# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Key Lab for Polyoxometalate Science Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_phone +86-431-85098620 _publ_contact_author_fax +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #================================ data_1 _database_code_depnum_ccdc_archive 'CCDC 879383' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H70 Mn N6 O8' _chemical_formula_weight 1442.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.2241(18) _cell_length_b 15.7921(7) _cell_length_c 20.0361(11) _cell_angle_alpha 90 _cell_angle_beta 102.581(6) _cell_angle_gamma 90 _cell_volume 7171.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3012 _exptl_absorpt_coefficient_mu 0.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.74 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28547 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 25.03 _reflns_number_total 12591 _reflns_number_gt 5980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The low ratio of observed/unique reflections may be attributed to the weak diffraction of the crystals. The distances of O6---H6A and O7---H7A were restrained to 0.82+-0.02 \%A. The distance of H6A...H7A was restrained to 2.1+-0.02 \%A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12591 _refine_ls_number_parameters 970 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1923 _refine_ls_wR_factor_gt 0.1738 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.76503(3) 0.00967(3) 0.16671(3) 0.0550(2) Uani 1 1 d . . . C1 C 0.4971(2) 0.3644(3) 0.0944(3) 0.0856(15) Uani 1 1 d . . . H1A H 0.4821 0.3706 0.0455 0.103 Uiso 1 1 calc R . . H1B H 0.4653 0.3777 0.1171 0.103 Uiso 1 1 calc R . . C2 C 0.5169(2) 0.2729(3) 0.1104(2) 0.0715(13) Uani 1 1 d . . . C3 C 0.50296(19) 0.2284(3) 0.1635(3) 0.0652(12) Uani 1 1 d . . . C4 C 0.5237(2) 0.1453(3) 0.1800(3) 0.0747(13) Uani 1 1 d . . . C5 C 0.5551(2) 0.1073(3) 0.1372(4) 0.0916(17) Uani 1 1 d . . . H5 H 0.5676 0.0516 0.1454 0.110 Uiso 1 1 calc R . . C6 C 0.5681(3) 0.1501(5) 0.0829(4) 0.104(2) Uani 1 1 d . . . H6 H 0.5890 0.1231 0.0543 0.125 Uiso 1 1 calc R . . C7 C 0.5504(2) 0.2333(4) 0.0702(3) 0.0921(16) Uani 1 1 d . . . H7 H 0.5610 0.2628 0.0345 0.111 Uiso 1 1 calc R . . C8 C 0.5139(2) 0.0996(3) 0.2425(3) 0.0990(18) Uani 1 1 d . . . H8A H 0.5005 0.0424 0.2297 0.119 Uiso 1 1 calc R . . H8B H 0.4828 0.1281 0.2592 0.119 Uiso 1 1 calc R . . C9 C 0.5688(2) 0.0953(3) 0.2998(3) 0.0808(14) Uani 1 1 d . . . C10 C 0.6028(3) 0.0218(3) 0.3119(3) 0.0920(16) Uani 1 1 d . . . H10 H 0.5908 -0.0267 0.2864 0.110 Uiso 1 1 calc R . . C11 C 0.6543(3) 0.0211(4) 0.3617(3) 0.1038(19) Uani 1 1 d . . . H11 H 0.6764 -0.0284 0.3702 0.125 Uiso 1 1 calc R . . C12 C 0.6728(3) 0.0921(4) 0.3984(3) 0.0979(17) Uani 1 1 d . . . H12 H 0.7078 0.0905 0.4314 0.118 Uiso 1 1 calc R . . C13 C 0.6410(3) 0.1668(3) 0.3878(3) 0.0816(14) Uani 1 1 d . . . C14 C 0.5881(2) 0.1667(3) 0.3395(3) 0.0780(14) Uani 1 1 d . . . C15 C 0.6632(3) 0.2463(4) 0.4284(3) 0.1037(19) Uani 1 1 d . . . H15A H 0.6305 0.2719 0.4439 0.124 Uiso 1 1 calc R . . H15B H 0.6923 0.2296 0.4687 0.124 Uiso 1 1 calc R . . C16 C 0.6903(3) 0.3122(3) 0.3906(2) 0.0781(14) Uani 1 1 d . . . C17 C 0.7486(3) 0.3109(4) 0.3892(3) 0.0968(18) Uani 1 1 d . . . H17 H 0.7719 0.2671 0.4113 0.116 Uiso 1 1 calc R . . C18 C 0.7742(3) 0.3716(4) 0.3566(3) 0.1040(19) Uani 1 1 d . . . H18 H 0.8145 0.3696 0.3581 0.125 Uiso 1 1 calc R . . C19 C 0.7405(3) 0.4354(3) 0.3216(3) 0.0891(16) Uani 1 1 d . . . H19 H 0.7578 0.4757 0.2984 0.107 Uiso 1 1 calc R . . C20 C 0.6809(2) 0.4402(3) 0.3208(2) 0.0729(13) Uani 1 1 d . . . C21 C 0.6554(2) 0.3778(3) 0.3540(2) 0.0720(13) Uani 1 1 d . . . C22 C 0.6435(2) 0.5122(2) 0.2838(3) 0.0808(15) Uani 1 1 d . . . H22A H 0.6118 0.5239 0.3070 0.097 Uiso 1 1 calc R . . H22B H 0.6678 0.5627 0.2870 0.097 Uiso 1 1 calc R . . C23 C 0.6174(2) 0.4949(3) 0.2101(3) 0.0739(13) Uani 1 1 d . . . C24 C 0.6431(3) 0.5311(3) 0.1617(4) 0.108(2) Uani 1 1 d . . . H24 H 0.6751 0.5671 0.1759 0.129 Uiso 1 1 calc R . . C25 C 0.6235(3) 0.5164(4) 0.0929(4) 0.127(2) Uani 1 1 d . . . H25 H 0.6423 0.5411 0.0612 0.153 Uiso 1 1 calc R . . C26 C 0.5743(3) 0.4633(4) 0.0715(3) 0.1112(19) Uani 1 1 d . . . H26 H 0.5598 0.4537 0.0250 0.133 Uiso 1 1 calc R . . C27 C 0.5477(2) 0.4257(3) 0.1180(3) 0.0792(14) Uani 1 1 d . . . C28 C 0.5694(2) 0.4412(3) 0.1875(2) 0.0663(12) Uani 1 1 d . . . C29 C 0.7516(3) -0.3616(4) 0.0056(3) 0.1086(19) Uani 1 1 d . . . H29A H 0.7619 -0.4082 -0.0211 0.130 Uiso 1 1 calc R . . H29B H 0.7093 -0.3630 0.0016 0.130 Uiso 1 1 calc R . . C30 C 0.7679(3) -0.2797(4) -0.0238(2) 0.0887(16) Uani 1 1 d . . . C31 C 0.7265(3) -0.2136(5) -0.0359(3) 0.115(2) Uani 1 1 d . . . H31 H 0.6896 -0.2212 -0.0257 0.137 Uiso 1 1 calc R . . C32 C 0.7396(5) -0.1396(6) -0.0620(4) 0.143(4) Uani 1 1 d . . . H32 H 0.7118 -0.0964 -0.0705 0.172 Uiso 1 1 calc R . . C33 C 0.7936(5) -0.1279(4) -0.0760(3) 0.128(3) Uani 1 1 d . . . H33 H 0.8023 -0.0763 -0.0939 0.154 Uiso 1 1 calc R . . C34 C 0.8370(3) -0.1922(3) -0.0640(2) 0.0915(18) Uani 1 1 d . . . C35 C 0.8223(3) -0.2686(3) -0.0391(2) 0.0779(15) Uani 1 1 d . . . C36 C 0.8974(4) -0.1786(3) -0.0772(3) 0.112(2) Uani 1 1 d . . . H36A H 0.9086 -0.2284 -0.0997 0.134 Uiso 1 1 calc R . . H36B H 0.8960 -0.1311 -0.1082 0.134 Uiso 1 1 calc R . . C37 C 0.9429(3) -0.1620(3) -0.0147(3) 0.0874(17) Uani 1 1 d . . . C38 C 0.9524(3) -0.0821(3) 0.0155(3) 0.104(2) Uani 1 1 d . . . H38 H 0.9299 -0.0367 -0.0054 0.125 Uiso 1 1 calc R . . C39 C 0.9935(4) -0.0681(4) 0.0746(4) 0.110(2) Uani 1 1 d . . . H39 H 0.9971 -0.0145 0.0943 0.132 Uiso 1 1 calc R . . C40 C 1.0290(3) -0.1316(4) 0.1046(3) 0.0974(17) Uani 1 1 d . . . H40 H 1.0581 -0.1214 0.1436 0.117 Uiso 1 1 calc R . . C41 C 1.0214(3) -0.2130(3) 0.0759(3) 0.0830(15) Uani 1 1 d . . . C42 C 0.9784(3) -0.2276(3) 0.0186(3) 0.0786(15) Uani 1 1 d . . . C43 C 1.0616(3) -0.2835(4) 0.1077(3) 0.1007(17) Uani 1 1 d . . . H43A H 1.1001 -0.2596 0.1270 0.121 Uiso 1 1 calc R . . H43B H 1.0663 -0.3225 0.0718 0.121 Uiso 1 1 calc R . . C44 C 1.0415(3) -0.3334(3) 0.1633(3) 0.0885(16) Uani 1 1 d . . . C45 C 1.0656(3) -0.3157(4) 0.2306(4) 0.113(2) Uani 1 1 d . . . H45 H 1.0963 -0.2767 0.2414 0.136 Uiso 1 1 calc R . . C46 C 1.0447(4) -0.3553(5) 0.2829(3) 0.120(2) Uani 1 1 d . . . H46 H 1.0620 -0.3436 0.3284 0.145 Uiso 1 1 calc R . . C47 C 0.9982(4) -0.4121(4) 0.2670(4) 0.118(2) Uani 1 1 d . . . H47 H 0.9840 -0.4382 0.3019 0.141 Uiso 1 1 calc R . . C48 C 0.9731(3) -0.4299(3) 0.2006(3) 0.0871(16) Uani 1 1 d . . . C49 C 0.9947(3) -0.3922(3) 0.1480(3) 0.0787(14) Uani 1 1 d . . . C50 C 0.9194(3) -0.4867(3) 0.1852(3) 0.1046(19) Uani 1 1 d . . . H50A H 0.9187 -0.5213 0.2250 0.126 Uiso 1 1 calc R . . H50B H 0.9223 -0.5243 0.1478 0.126 Uiso 1 1 calc R . . C51 C 0.8614(2) -0.4364(3) 0.1659(3) 0.0785(14) Uani 1 1 d . . . C52 C 0.8406(3) -0.3952(4) 0.2153(3) 0.1000(18) Uani 1 1 d . . . H52 H 0.8599 -0.4020 0.2608 0.120 Uiso 1 1 calc R . . C53 C 0.7911(3) -0.3428(4) 0.1996(3) 0.1019(19) Uani 1 1 d . . . H53 H 0.7778 -0.3148 0.2342 0.122 Uiso 1 1 calc R . . C54 C 0.7619(2) -0.3329(3) 0.1316(3) 0.0946(17) Uani 1 1 d . . . H54 H 0.7288 -0.2983 0.1206 0.114 Uiso 1 1 calc R . . C55 C 0.7818(2) -0.3746(3) 0.0801(3) 0.0779(14) Uani 1 1 d . . . C56 C 0.8317(3) -0.4281(3) 0.0990(3) 0.0766(14) Uani 1 1 d . . . C57 C 0.67075(19) 0.0083(2) 0.0235(2) 0.0609(11) Uani 1 1 d . . . H57 H 0.6943 0.0508 0.0116 0.073 Uiso 1 1 calc R . . C58 C 0.6202(2) -0.0139(3) -0.0234(2) 0.0705(12) Uani 1 1 d . . . H58 H 0.6104 0.0131 -0.0656 0.085 Uiso 1 1 calc R . . C59 C 0.5848(2) -0.0759(3) -0.0072(2) 0.0782(14) Uani 1 1 d . . . H59 H 0.5505 -0.0917 -0.0383 0.094 Uiso 1 1 calc R . . C60 C 0.60064(19) -0.1157(3) 0.0570(2) 0.0657(12) Uani 1 1 d . . . C61 C 0.65207(16) -0.0881(2) 0.10166(17) 0.0441(9) Uani 1 1 d . . . C62 C 0.5663(2) -0.1811(4) 0.0781(3) 0.103(2) Uani 1 1 d . . . H62 H 0.5320 -0.1992 0.0484 0.124 Uiso 1 1 calc R . . C63 C 0.5823(2) -0.2169(4) 0.1392(3) 0.0996(18) Uani 1 1 d . . . H63 H 0.5593 -0.2603 0.1511 0.120 Uiso 1 1 calc R . . C64 C 0.63339(19) -0.1905(3) 0.1868(2) 0.0615(11) Uani 1 1 d . . . C65 C 0.66815(16) -0.1252(2) 0.16850(18) 0.0432(9) Uani 1 1 d . . . C66 C 0.6515(2) -0.2259(3) 0.2518(2) 0.0703(13) Uani 1 1 d . . . H66 H 0.6298 -0.2694 0.2659 0.084 Uiso 1 1 calc R . . C67 C 0.7006(2) -0.1965(3) 0.2939(2) 0.0692(12) Uani 1 1 d . . . H67 H 0.7137 -0.2208 0.3368 0.083 Uiso 1 1 calc R . . C68 C 0.7318(2) -0.1300(3) 0.2734(2) 0.0620(11) Uani 1 1 d . . . H68 H 0.7651 -0.1098 0.3039 0.074 Uiso 1 1 calc R . . C69 C 0.68813(19) 0.1630(3) 0.2109(2) 0.0640(12) Uani 1 1 d . . . H69 H 0.6717 0.1214 0.2338 0.077 Uiso 1 1 calc R . . C70 C 0.6687(2) 0.2459(3) 0.2136(2) 0.0714(12) Uani 1 1 d . . . H70 H 0.6392 0.2587 0.2369 0.086 Uiso 1 1 calc R . . C71 C 0.6928(2) 0.3073(3) 0.1822(2) 0.0719(13) Uani 1 1 d . . . H71 H 0.6801 0.3630 0.1835 0.086 Uiso 1 1 calc R . . C72 C 0.7374(2) 0.2868(2) 0.1473(2) 0.0593(11) Uani 1 1 d . . . C73 C 0.75449(17) 0.2021(2) 0.14467(18) 0.0499(10) Uani 1 1 d . . . C74 C 0.79791(17) 0.1787(2) 0.10720(17) 0.0455(9) Uani 1 1 d . . . C75 C 0.7668(2) 0.3501(3) 0.1157(2) 0.0742(13) Uani 1 1 d . . . H75 H 0.7562 0.4066 0.1177 0.089 Uiso 1 1 calc R . . C76 C 0.8095(2) 0.3289(3) 0.0833(2) 0.0686(12) Uani 1 1 d . . . H76 H 0.8290 0.3715 0.0648 0.082 Uiso 1 1 calc R . . C77 C 0.82577(18) 0.2429(2) 0.07634(18) 0.0502(10) Uani 1 1 d . . . C78 C 0.8683(2) 0.2175(3) 0.0408(2) 0.0614(11) Uani 1 1 d . . . H78 H 0.8889 0.2580 0.0217 0.074 Uiso 1 1 calc R . . C79 C 0.8797(2) 0.1346(3) 0.0340(2) 0.0660(12) Uani 1 1 d . . . H79 H 0.9068 0.1172 0.0088 0.079 Uiso 1 1 calc R . . C80 C 0.84969(19) 0.0753(2) 0.0658(2) 0.0598(11) Uani 1 1 d . . . H80 H 0.8580 0.0182 0.0617 0.072 Uiso 1 1 calc R . . C81 C 0.8122(2) 0.0670(3) 0.3245(2) 0.0704(12) Uani 1 1 d . . . H81 H 0.7815 0.1061 0.3166 0.084 Uiso 1 1 calc R . . C82 C 0.8460(3) 0.0580(3) 0.3906(2) 0.0838(15) Uani 1 1 d . . . H82 H 0.8364 0.0879 0.4267 0.101 Uiso 1 1 calc R . . C83 C 0.8933(3) 0.0051(3) 0.4016(2) 0.0746(13) Uani 1 1 d . . . H83 H 0.9174 0.0006 0.4451 0.090 Uiso 1 1 calc R . . C84 C 0.9052(2) -0.0412(3) 0.3493(2) 0.0622(11) Uani 1 1 d . . . C85 C 0.86811(19) -0.0337(2) 0.2841(2) 0.0537(10) Uani 1 1 d . . . C86 C 0.9539(2) -0.0990(3) 0.3584(2) 0.0801(14) Uani 1 1 d . . . H86 H 0.9811 -0.1008 0.4000 0.096 Uiso 1 1 calc R . . C87 C 0.9608(2) -0.1513(3) 0.3065(3) 0.0790(14) Uani 1 1 d . . . H87 H 0.9923 -0.1891 0.3135 0.095 Uiso 1 1 calc R . . C88 C 0.9202(2) -0.1487(2) 0.2416(2) 0.0575(11) Uani 1 1 d . . . C89 C 0.87558(17) -0.0890(2) 0.23027(17) 0.0482(10) Uani 1 1 d . . . C90 C 0.9235(2) -0.2067(3) 0.1899(3) 0.0719(13) Uani 1 1 d . . . H90 H 0.9530 -0.2475 0.1962 0.086 Uiso 1 1 calc R . . C91 C 0.8823(2) -0.2021(3) 0.1299(2) 0.0688(12) Uani 1 1 d . . . H91 H 0.8837 -0.2403 0.0950 0.083 Uiso 1 1 calc R . . C92 C 0.8381(2) -0.1409(2) 0.12046(19) 0.0535(11) Uani 1 1 d . . . H92 H 0.8102 -0.1391 0.0795 0.064 Uiso 1 1 calc R . . N1 N 0.71621(14) -0.09357(17) 0.21168(14) 0.0486(8) Uani 1 1 d . . . N2 N 0.68780(13) -0.02745(17) 0.08459(14) 0.0461(7) Uani 1 1 d . . . N3 N 0.83537(15) -0.08480(19) 0.16938(16) 0.0583(9) Uani 1 1 d . . . N4 N 0.82212(16) 0.0217(2) 0.27248(16) 0.0592(9) Uani 1 1 d . . . N5 N 0.81014(14) 0.09618(18) 0.10147(15) 0.0506(8) Uani 1 1 d . . . N6 N 0.72973(15) 0.13995(19) 0.17686(16) 0.0569(9) Uani 1 1 d . . . O1 O 0.55206(15) 0.2357(2) 0.32899(19) 0.0941(10) Uani 1 1 d . . . O2 O 0.59687(16) 0.38091(18) 0.35106(15) 0.0799(9) Uani 1 1 d . . . H2 H 0.5873 0.3409 0.3724 0.120 Uiso 1 1 calc R . . O3 O 0.54109(13) 0.40366(17) 0.23112(16) 0.0720(8) Uani 1 1 d . . . H3 H 0.5570 0.4166 0.2704 0.108 Uiso 1 1 calc R . . O4 O 0.46814(14) 0.26453(19) 0.20252(17) 0.0841(9) Uani 1 1 d . . . H4 H 0.4828 0.3111 0.2205 0.126 Uiso 1 1 d R . . O5 O 0.86156(16) -0.33424(18) -0.02900(15) 0.0849(10) Uani 1 1 d . . . H5A H 0.8468 -0.3752 -0.0140 0.127 Uiso 1 1 calc R . . O8 O 0.85014(19) -0.47297(19) 0.04928(18) 0.1007(12) Uani 1 1 d . . . O6 O 0.96987(19) -0.3074(2) -0.00582(18) 0.0977(12) Uani 1 1 d D . . H6A H 0.9355(14) -0.322(4) -0.024(3) 0.146 Uiso 1 1 d D . . O7 O 0.97115(17) -0.4167(2) 0.08577(19) 0.0886(10) Uani 1 1 d D . . H7A H 0.982(2) -0.377(3) 0.067(3) 0.133 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0580(4) 0.0527(4) 0.0515(4) 0.0073(3) 0.0057(3) -0.0152(3) C1 0.076(4) 0.090(3) 0.078(3) 0.001(3) -0.010(3) -0.005(3) C2 0.045(3) 0.093(3) 0.070(3) -0.023(3) -0.003(2) -0.011(2) C3 0.040(3) 0.069(3) 0.085(3) -0.020(3) 0.010(2) -0.014(2) C4 0.041(3) 0.067(3) 0.110(4) -0.018(3) 0.003(3) -0.016(2) C5 0.065(4) 0.076(3) 0.126(5) -0.047(4) 0.005(3) -0.004(3) C6 0.067(4) 0.127(6) 0.114(5) -0.063(4) 0.009(4) 0.003(4) C7 0.070(4) 0.126(5) 0.076(3) -0.033(3) 0.005(3) -0.022(3) C8 0.065(4) 0.063(3) 0.170(6) -0.006(3) 0.028(4) -0.015(2) C9 0.064(4) 0.068(3) 0.116(4) 0.019(3) 0.032(3) -0.005(3) C10 0.095(5) 0.065(3) 0.127(5) 0.022(3) 0.047(4) -0.004(3) C11 0.104(5) 0.094(4) 0.120(5) 0.035(4) 0.041(4) 0.031(4) C12 0.106(5) 0.103(4) 0.083(4) 0.025(3) 0.016(3) 0.025(4) C13 0.083(4) 0.091(4) 0.074(3) 0.018(3) 0.025(3) 0.016(3) C14 0.065(4) 0.076(3) 0.104(4) 0.021(3) 0.041(3) 0.012(3) C15 0.121(5) 0.121(5) 0.065(3) 0.007(3) 0.011(3) 0.032(4) C16 0.084(4) 0.087(3) 0.055(3) -0.017(3) -0.004(3) 0.018(3) C17 0.082(5) 0.094(4) 0.098(4) -0.004(3) -0.017(3) 0.022(4) C18 0.066(4) 0.108(4) 0.122(5) -0.029(4) -0.016(4) 0.012(4) C19 0.071(4) 0.076(3) 0.108(4) -0.021(3) -0.006(3) -0.010(3) C20 0.070(4) 0.058(3) 0.082(3) -0.035(2) -0.002(3) 0.000(3) C21 0.066(4) 0.076(3) 0.069(3) -0.038(3) 0.005(3) 0.007(3) C22 0.074(3) 0.043(2) 0.114(4) -0.024(2) -0.005(3) 0.000(2) C23 0.069(3) 0.044(2) 0.104(4) 0.001(3) 0.008(3) 0.004(2) C24 0.093(5) 0.081(4) 0.136(6) 0.009(4) -0.005(4) -0.020(3) C25 0.126(6) 0.119(5) 0.137(6) 0.044(4) 0.028(5) -0.032(4) C26 0.111(5) 0.123(5) 0.091(4) 0.027(4) 0.004(4) -0.013(4) C27 0.074(4) 0.072(3) 0.086(4) 0.014(3) 0.005(3) 0.000(3) C28 0.067(3) 0.047(2) 0.080(3) -0.001(2) 0.004(3) 0.004(2) C29 0.080(4) 0.143(5) 0.090(4) -0.038(4) -0.009(3) -0.005(4) C30 0.105(5) 0.095(4) 0.054(3) -0.017(3) -0.007(3) 0.021(4) C31 0.120(6) 0.149(6) 0.059(4) -0.029(4) -0.015(3) 0.050(5) C32 0.188(9) 0.164(8) 0.063(4) -0.031(4) -0.007(5) 0.098(8) C33 0.237(10) 0.087(4) 0.052(3) 0.009(3) 0.011(5) 0.076(6) C34 0.154(6) 0.076(4) 0.045(3) 0.004(2) 0.021(3) 0.040(4) C35 0.121(5) 0.067(3) 0.042(3) -0.007(2) 0.010(3) 0.030(3) C36 0.210(8) 0.077(3) 0.061(4) 0.023(3) 0.057(4) 0.033(4) C37 0.152(5) 0.052(3) 0.079(4) 0.024(3) 0.071(4) 0.023(3) C38 0.170(7) 0.054(3) 0.116(5) 0.007(3) 0.089(5) 0.005(3) C39 0.157(7) 0.062(3) 0.138(6) -0.019(4) 0.088(5) -0.021(4) C40 0.105(5) 0.084(4) 0.122(5) -0.015(3) 0.066(4) -0.019(4) C41 0.092(4) 0.075(3) 0.100(4) 0.005(3) 0.061(4) 0.005(3) C42 0.111(5) 0.072(3) 0.071(3) -0.009(3) 0.058(3) -0.009(3) C43 0.081(4) 0.116(4) 0.115(5) -0.011(4) 0.044(3) -0.020(4) C44 0.082(4) 0.092(4) 0.085(4) 0.002(3) 0.005(3) 0.018(3) C45 0.098(5) 0.131(5) 0.110(5) 0.001(4) 0.021(4) 0.027(4) C46 0.126(6) 0.139(6) 0.082(5) 0.003(4) -0.010(4) 0.057(5) C47 0.136(7) 0.120(5) 0.092(5) 0.027(4) 0.016(4) 0.029(5) C48 0.097(4) 0.081(3) 0.078(4) 0.023(3) 0.008(3) 0.028(3) C49 0.084(4) 0.079(3) 0.078(4) 0.022(3) 0.026(3) 0.031(3) C50 0.136(6) 0.077(3) 0.106(4) 0.048(3) 0.040(4) 0.016(4) C51 0.102(4) 0.058(3) 0.087(4) 0.016(3) 0.045(3) -0.013(3) C52 0.115(5) 0.109(4) 0.086(4) 0.004(3) 0.042(4) -0.027(4) C53 0.113(5) 0.115(5) 0.096(5) -0.032(4) 0.063(4) -0.035(4) C54 0.071(4) 0.100(4) 0.121(5) -0.024(4) 0.040(4) -0.018(3) C55 0.067(4) 0.076(3) 0.094(4) -0.018(3) 0.026(3) -0.022(3) C56 0.105(4) 0.056(3) 0.076(3) 0.000(3) 0.035(3) -0.020(3) C57 0.069(3) 0.061(2) 0.051(2) 0.013(2) 0.009(2) -0.011(2) C58 0.074(3) 0.088(3) 0.043(2) 0.012(2) 0.000(2) -0.006(3) C59 0.073(3) 0.100(3) 0.052(3) 0.005(2) -0.009(2) -0.018(3) C60 0.057(3) 0.080(3) 0.055(3) 0.004(2) 0.002(2) -0.021(2) C61 0.046(2) 0.044(2) 0.044(2) -0.0005(17) 0.0135(18) -0.0054(18) C62 0.075(4) 0.140(5) 0.083(4) 0.026(3) -0.012(3) -0.059(3) C63 0.078(4) 0.117(4) 0.097(4) 0.037(3) 0.004(3) -0.044(3) C64 0.052(3) 0.070(3) 0.064(3) 0.010(2) 0.016(2) -0.017(2) C65 0.043(2) 0.0445(19) 0.044(2) -0.0018(17) 0.0143(18) 0.0032(18) C66 0.062(3) 0.076(3) 0.078(3) 0.031(2) 0.028(3) -0.008(2) C67 0.071(3) 0.083(3) 0.058(3) 0.028(2) 0.023(3) -0.004(3) C68 0.066(3) 0.070(3) 0.048(2) 0.008(2) 0.010(2) -0.003(2) C69 0.051(3) 0.078(3) 0.065(3) 0.002(2) 0.018(2) -0.017(2) C70 0.070(3) 0.068(3) 0.080(3) -0.020(2) 0.024(3) 0.002(3) C71 0.071(3) 0.054(3) 0.090(3) -0.015(2) 0.016(3) -0.001(2) C72 0.059(3) 0.050(2) 0.068(3) -0.016(2) 0.014(2) -0.005(2) C73 0.049(3) 0.053(2) 0.046(2) -0.0046(18) 0.0079(19) -0.0160(19) C74 0.045(2) 0.045(2) 0.044(2) -0.0008(17) 0.0051(18) -0.0101(18) C75 0.087(4) 0.046(2) 0.094(3) -0.008(2) 0.029(3) -0.008(2) C76 0.085(4) 0.050(2) 0.073(3) 0.002(2) 0.023(3) -0.016(2) C77 0.055(3) 0.051(2) 0.044(2) 0.0033(18) 0.009(2) -0.008(2) C78 0.069(3) 0.063(3) 0.055(3) 0.011(2) 0.019(2) -0.014(2) C79 0.066(3) 0.071(3) 0.067(3) 0.008(2) 0.028(2) -0.004(2) C80 0.061(3) 0.045(2) 0.076(3) 0.000(2) 0.020(2) 0.001(2) C81 0.076(3) 0.075(3) 0.066(3) -0.019(2) 0.029(3) -0.011(2) C82 0.109(5) 0.095(4) 0.053(3) -0.020(3) 0.029(3) -0.025(3) C83 0.093(4) 0.081(3) 0.051(3) 0.001(2) 0.018(3) -0.007(3) C84 0.070(3) 0.067(3) 0.047(3) 0.007(2) 0.007(2) -0.013(2) C85 0.049(3) 0.055(2) 0.059(3) 0.002(2) 0.015(2) -0.007(2) C86 0.087(4) 0.082(3) 0.063(3) 0.013(3) -0.003(3) -0.007(3) C87 0.069(4) 0.078(3) 0.084(4) 0.019(3) 0.006(3) 0.004(2) C88 0.065(3) 0.052(2) 0.060(3) 0.005(2) 0.023(2) -0.002(2) C89 0.041(2) 0.067(2) 0.037(2) 0.0044(19) 0.0088(18) -0.013(2) C90 0.077(4) 0.060(3) 0.084(3) 0.015(2) 0.030(3) 0.007(2) C91 0.083(4) 0.062(3) 0.067(3) 0.005(2) 0.028(3) 0.004(3) C92 0.084(3) 0.0384(19) 0.044(2) -0.0087(17) 0.028(2) -0.002(2) N1 0.055(2) 0.0500(17) 0.0406(18) 0.0020(14) 0.0099(16) -0.0028(15) N2 0.050(2) 0.0491(17) 0.0393(17) 0.0061(14) 0.0091(14) -0.0066(15) N3 0.064(2) 0.0567(19) 0.056(2) 0.0050(16) 0.0164(18) -0.0107(16) N4 0.064(3) 0.063(2) 0.055(2) -0.0064(17) 0.0228(18) -0.0081(18) N5 0.049(2) 0.0469(18) 0.058(2) 0.0046(15) 0.0157(17) -0.0031(15) N6 0.055(2) 0.063(2) 0.055(2) -0.0073(16) 0.0156(18) -0.0161(17) O1 0.069(2) 0.087(2) 0.128(3) 0.003(2) 0.026(2) 0.0117(19) O2 0.083(3) 0.076(2) 0.082(2) -0.0239(16) 0.0211(18) 0.0132(17) O3 0.065(2) 0.0603(17) 0.087(2) -0.0113(16) 0.0098(17) 0.0006(15) O4 0.058(2) 0.079(2) 0.120(3) -0.0075(18) 0.030(2) -0.0006(16) O5 0.125(3) 0.0558(17) 0.079(2) 0.0007(15) 0.033(2) 0.0147(19) O8 0.151(4) 0.0624(19) 0.098(3) -0.0091(18) 0.047(2) 0.004(2) O6 0.149(4) 0.061(2) 0.089(2) -0.0124(18) 0.039(2) 0.013(2) O7 0.103(3) 0.086(2) 0.078(2) 0.0105(18) 0.023(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N3 2.204(3) . ? Mn1 N2 2.232(3) . ? Mn1 N6 2.240(3) . ? Mn1 N4 2.250(3) . ? Mn1 N1 2.281(3) . ? Mn1 N5 2.295(3) . ? C1 C27 1.517(7) . ? C1 C2 1.528(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.372(6) . ? C2 C7 1.385(7) . ? C3 O4 1.365(5) . ? C3 C4 1.413(6) . ? C4 C5 1.377(7) . ? C4 C8 1.506(7) . ? C5 C6 1.370(8) . ? C5 H5 0.9300 . ? C6 C7 1.384(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.521(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.395(7) . ? C9 C14 1.397(7) . ? C10 C11 1.379(8) . ? C10 H10 0.9300 . ? C11 C12 1.359(8) . ? C11 H11 0.9300 . ? C12 C13 1.384(7) . ? C12 H12 0.9300 . ? C13 C14 1.386(7) . ? C13 C15 1.524(7) . ? C14 O1 1.362(5) . ? C15 C16 1.503(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.360(7) . ? C16 C21 1.418(7) . ? C17 C18 1.366(8) . ? C17 H17 0.9300 . ? C18 C19 1.371(7) . ? C18 H18 0.9300 . ? C19 C20 1.384(7) . ? C19 H19 0.9300 . ? C20 C21 1.391(7) . ? C20 C22 1.521(6) . ? C21 O2 1.348(5) . ? C22 C23 1.495(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.369(8) . ? C23 C28 1.395(6) . ? C24 C25 1.373(8) . ? C24 H24 0.9300 . ? C25 C26 1.407(8) . ? C25 H25 0.9300 . ? C26 C27 1.362(7) . ? C26 H26 0.9300 . ? C27 C28 1.396(6) . ? C28 O3 1.341(5) . ? C29 C30 1.504(8) . ? C29 C55 1.518(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C35 1.375(8) . ? C30 C31 1.404(8) . ? C31 C32 1.344(10) . ? C31 H31 0.9300 . ? C32 C33 1.354(11) . ? C32 H32 0.9300 . ? C33 C34 1.415(8) . ? C33 H33 0.9300 . ? C34 C35 1.377(7) . ? C34 C36 1.497(8) . ? C35 O5 1.366(5) . ? C36 C37 1.476(8) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.395(7) . ? C37 C42 1.400(7) . ? C38 C39 1.367(9) . ? C38 H38 0.9300 . ? C39 C40 1.352(8) . ? C39 H39 0.9300 . ? C40 C41 1.404(7) . ? C40 H40 0.9300 . ? C41 C42 1.367(7) . ? C41 C43 1.504(7) . ? C42 O6 1.351(5) . ? C43 C44 1.519(7) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.372(8) . ? C44 C49 1.410(7) . ? C45 C46 1.397(9) . ? C45 H45 0.9300 . ? C46 C47 1.388(9) . ? C46 H46 0.9300 . ? C47 C48 1.361(8) . ? C47 H47 0.9300 . ? C48 C49 1.394(7) . ? C48 C50 1.513(8) . ? C49 O7 1.307(6) . ? C50 C51 1.538(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.359(7) . ? C51 C56 1.374(7) . ? C52 C53 1.395(8) . ? C52 H52 0.9300 . ? C53 C54 1.393(8) . ? C53 H53 0.9300 . ? C54 C55 1.386(7) . ? C54 H54 0.9300 . ? C55 C56 1.416(7) . ? C56 O8 1.365(6) . ? C57 N2 1.328(4) . ? C57 C58 1.380(6) . ? C57 H57 0.9300 . ? C58 C59 1.362(6) . ? C58 H58 0.9300 . ? C59 C60 1.407(6) . ? C59 H59 0.9300 . ? C60 C61 1.397(5) . ? C60 C62 1.425(6) . ? C61 N2 1.359(4) . ? C61 C65 1.434(5) . ? C62 C63 1.326(6) . ? C62 H62 0.9300 . ? C63 C64 1.414(6) . ? C63 H63 0.9300 . ? C64 C66 1.396(6) . ? C64 C65 1.407(5) . ? C65 N1 1.350(4) . ? C66 C67 1.345(6) . ? C66 H66 0.9300 . ? C67 C68 1.389(6) . ? C67 H67 0.9300 . ? C68 N1 1.340(5) . ? C68 H68 0.9300 . ? C69 N6 1.349(5) . ? C69 C70 1.390(6) . ? C69 H69 0.9300 . ? C70 C71 1.342(6) . ? C70 H70 0.9300 . ? C71 C72 1.409(6) . ? C71 H71 0.9300 . ? C72 C73 1.400(5) . ? C72 C75 1.435(6) . ? C73 N6 1.368(5) . ? C73 C74 1.431(5) . ? C74 N5 1.344(4) . ? C74 C77 1.416(5) . ? C75 C76 1.339(6) . ? C75 H75 0.9300 . ? C76 C77 1.425(5) . ? C76 H76 0.9300 . ? C77 C78 1.397(6) . ? C78 C79 1.348(5) . ? C78 H78 0.9300 . ? C79 C80 1.401(6) . ? C79 H79 0.9300 . ? C80 N5 1.322(5) . ? C80 H80 0.9300 . ? C81 N4 1.324(5) . ? C81 C82 1.392(6) . ? C81 H81 0.9300 . ? C82 C83 1.359(7) . ? C82 H82 0.9300 . ? C83 C84 1.355(6) . ? C83 H83 0.9300 . ? C84 C85 1.405(5) . ? C84 C86 1.434(6) . ? C85 N4 1.361(5) . ? C85 C89 1.426(5) . ? C86 C87 1.363(6) . ? C86 H86 0.9300 . ? C87 C88 1.433(6) . ? C87 H87 0.9300 . ? C88 C89 1.383(5) . ? C88 C90 1.396(6) . ? C89 N3 1.367(5) . ? C90 C91 1.366(6) . ? C90 H90 0.9300 . ? C91 C92 1.391(6) . ? C91 H91 0.9300 . ? C92 N3 1.333(4) . ? C92 H92 0.9300 . ? O2 H2 0.8200 . ? O3 H3 0.8200 . ? O4 H4 0.8558 . ? O5 H5A 0.8200 . ? O6 H6A 0.83(2) . ? O7 H7A 0.81(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Mn1 N2 108.21(12) . . ? N3 Mn1 N6 154.59(12) . . ? N2 Mn1 N6 93.26(11) . . ? N3 Mn1 N4 75.69(12) . . ? N2 Mn1 N4 158.54(11) . . ? N6 Mn1 N4 89.36(12) . . ? N3 Mn1 N1 86.34(11) . . ? N2 Mn1 N1 73.42(10) . . ? N6 Mn1 N1 113.42(12) . . ? N4 Mn1 N1 85.99(11) . . ? N3 Mn1 N5 89.36(11) . . ? N2 Mn1 N5 97.45(11) . . ? N6 Mn1 N5 74.13(12) . . ? N4 Mn1 N5 103.75(11) . . ? N1 Mn1 N5 168.06(11) . . ? C27 C1 C2 111.2(4) . . ? C27 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? C27 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C3 C2 C7 118.5(5) . . ? C3 C2 C1 122.4(5) . . ? C7 C2 C1 119.2(5) . . ? O4 C3 C2 120.0(4) . . ? O4 C3 C4 118.0(5) . . ? C2 C3 C4 122.0(5) . . ? C5 C4 C3 117.4(5) . . ? C5 C4 C8 120.4(5) . . ? C3 C4 C8 122.2(5) . . ? C6 C5 C4 121.2(5) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 120.4(6) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C2 120.3(6) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? C4 C8 C9 113.3(4) . . ? C4 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? C4 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C14 118.2(5) . . ? C10 C9 C8 121.3(5) . . ? C14 C9 C8 120.4(4) . . ? C11 C10 C9 120.1(6) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 120.4(5) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 121.7(6) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C14 117.9(5) . . ? C12 C13 C15 120.8(5) . . ? C14 C13 C15 121.3(5) . . ? O1 C14 C13 121.9(5) . . ? O1 C14 C9 116.6(5) . . ? C13 C14 C9 121.6(5) . . ? C16 C15 C13 115.6(4) . . ? C16 C15 H15A 108.4 . . ? C13 C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? C13 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C17 C16 C21 117.4(5) . . ? C17 C16 C15 121.8(5) . . ? C21 C16 C15 120.7(5) . . ? C16 C17 C18 122.6(5) . . ? C16 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C17 C18 C19 120.0(6) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 120.3(6) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 119.0(5) . . ? C19 C20 C22 120.6(5) . . ? C21 C20 C22 120.4(5) . . ? O2 C21 C20 118.9(5) . . ? O2 C21 C16 120.5(5) . . ? C20 C21 C16 120.6(5) . . ? C23 C22 C20 114.2(3) . . ? C23 C22 H22A 108.7 . . ? C20 C22 H22A 108.7 . . ? C23 C22 H22B 108.7 . . ? C20 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C24 C23 C28 117.7(5) . . ? C24 C23 C22 118.6(5) . . ? C28 C23 C22 123.7(5) . . ? C23 C24 C25 122.7(6) . . ? C23 C24 H24 118.7 . . ? C25 C24 H24 118.7 . . ? C24 C25 C26 118.4(6) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C27 C26 C25 120.7(6) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 119.2(5) . . ? C26 C27 C1 120.0(5) . . ? C28 C27 C1 120.6(5) . . ? O3 C28 C23 121.9(4) . . ? O3 C28 C27 116.8(4) . . ? C23 C28 C27 121.2(5) . . ? C30 C29 C55 113.6(4) . . ? C30 C29 H29A 108.8 . . ? C55 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? C55 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C35 C30 C31 119.7(6) . . ? C35 C30 C29 121.2(5) . . ? C31 C30 C29 119.1(7) . . ? C32 C31 C30 120.6(8) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 119.9(8) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 121.7(8) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 117.8(7) . . ? C35 C34 C36 120.4(5) . . ? C33 C34 C36 121.8(6) . . ? O5 C35 C30 119.1(5) . . ? O5 C35 C34 120.5(6) . . ? C30 C35 C34 120.4(5) . . ? C37 C36 C34 113.6(4) . . ? C37 C36 H36A 108.8 . . ? C34 C36 H36A 108.8 . . ? C37 C36 H36B 108.8 . . ? C34 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C38 C37 C42 116.2(6) . . ? C38 C37 C36 123.1(5) . . ? C42 C37 C36 120.7(5) . . ? C39 C38 C37 122.4(6) . . ? C39 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? C40 C39 C38 120.6(6) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 119.1(6) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C42 C41 C40 120.1(5) . . ? C42 C41 C43 120.3(5) . . ? C40 C41 C43 119.6(6) . . ? O6 C42 C41 118.9(5) . . ? O6 C42 C37 119.6(5) . . ? C41 C42 C37 121.5(5) . . ? C41 C43 C44 115.6(4) . . ? C41 C43 H43A 108.4 . . ? C44 C43 H43A 108.4 . . ? C41 C43 H43B 108.4 . . ? C44 C43 H43B 108.4 . . ? H43A C43 H43B 107.4 . . ? C45 C44 C49 118.5(6) . . ? C45 C44 C43 119.3(6) . . ? C49 C44 C43 121.9(5) . . ? C44 C45 C46 120.8(7) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C47 C46 C45 119.9(6) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C48 C47 C46 120.2(7) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C47 C48 C49 120.2(6) . . ? C47 C48 C50 118.6(6) . . ? C49 C48 C50 121.0(5) . . ? O7 C49 C48 116.7(6) . . ? O7 C49 C44 122.9(5) . . ? C48 C49 C44 120.3(5) . . ? C48 C50 C51 112.5(4) . . ? C48 C50 H50A 109.1 . . ? C51 C50 H50A 109.1 . . ? C48 C50 H50B 109.1 . . ? C51 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C52 C51 C56 118.8(6) . . ? C52 C51 C50 119.7(6) . . ? C56 C51 C50 121.4(5) . . ? C51 C52 C53 121.8(6) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C54 C53 C52 119.3(5) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C55 C54 C53 120.3(6) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C54 C55 C56 118.1(5) . . ? C54 C55 C29 120.6(5) . . ? C56 C55 C29 121.3(5) . . ? O8 C56 C51 119.4(5) . . ? O8 C56 C55 118.9(5) . . ? C51 C56 C55 121.7(5) . . ? N2 C57 C58 123.9(4) . . ? N2 C57 H57 118.0 . . ? C58 C57 H57 118.0 . . ? C59 C58 C57 119.3(4) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C58 C59 C60 119.1(4) . . ? C58 C59 H59 120.4 . . ? C60 C59 H59 120.4 . . ? C61 C60 C59 117.6(4) . . ? C61 C60 C62 119.4(4) . . ? C59 C60 C62 122.9(4) . . ? N2 C61 C60 122.8(3) . . ? N2 C61 C65 118.3(3) . . ? C60 C61 C65 118.9(3) . . ? C63 C62 C60 121.4(4) . . ? C63 C62 H62 119.3 . . ? C60 C62 H62 119.3 . . ? C62 C63 C64 121.5(4) . . ? C62 C63 H63 119.3 . . ? C64 C63 H63 119.3 . . ? C66 C64 C65 117.7(4) . . ? C66 C64 C63 123.3(4) . . ? C65 C64 C63 119.0(4) . . ? N1 C65 C64 123.0(3) . . ? N1 C65 C61 117.3(3) . . ? C64 C65 C61 119.7(3) . . ? C67 C66 C64 119.2(4) . . ? C67 C66 H66 120.4 . . ? C64 C66 H66 120.4 . . ? C66 C67 C68 120.2(4) . . ? C66 C67 H67 119.9 . . ? C68 C67 H67 119.9 . . ? N1 C68 C67 122.9(4) . . ? N1 C68 H68 118.5 . . ? C67 C68 H68 118.5 . . ? N6 C69 C70 123.3(4) . . ? N6 C69 H69 118.4 . . ? C70 C69 H69 118.4 . . ? C71 C70 C69 119.3(4) . . ? C71 C70 H70 120.3 . . ? C69 C70 H70 120.3 . . ? C70 C71 C72 119.6(4) . . ? C70 C71 H71 120.2 . . ? C72 C71 H71 120.2 . . ? C73 C72 C71 119.0(4) . . ? C73 C72 C75 118.9(4) . . ? C71 C72 C75 122.2(4) . . ? N6 C73 C72 121.1(4) . . ? N6 C73 C74 118.6(3) . . ? C72 C73 C74 120.3(3) . . ? N5 C74 C77 122.2(4) . . ? N5 C74 C73 118.8(3) . . ? C77 C74 C73 119.1(3) . . ? C76 C75 C72 121.0(4) . . ? C76 C75 H75 119.5 . . ? C72 C75 H75 119.5 . . ? C75 C76 C77 121.7(4) . . ? C75 C76 H76 119.2 . . ? C77 C76 H76 119.2 . . ? C78 C77 C74 117.3(3) . . ? C78 C77 C76 123.8(4) . . ? C74 C77 C76 119.0(4) . . ? C79 C78 C77 120.4(4) . . ? C79 C78 H78 119.8 . . ? C77 C78 H78 119.8 . . ? C78 C79 C80 118.4(4) . . ? C78 C79 H79 120.8 . . ? C80 C79 H79 120.8 . . ? N5 C80 C79 123.5(4) . . ? N5 C80 H80 118.3 . . ? C79 C80 H80 118.3 . . ? N4 C81 C82 122.3(5) . . ? N4 C81 H81 118.8 . . ? C82 C81 H81 118.8 . . ? C83 C82 C81 119.1(4) . . ? C83 C82 H82 120.5 . . ? C81 C82 H82 120.5 . . ? C84 C83 C82 120.0(4) . . ? C84 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? C83 C84 C85 119.1(5) . . ? C83 C84 C86 122.3(4) . . ? C85 C84 C86 118.6(4) . . ? N4 C85 C84 120.8(4) . . ? N4 C85 C89 119.0(4) . . ? C84 C85 C89 120.0(4) . . ? C87 C86 C84 120.6(4) . . ? C87 C86 H86 119.7 . . ? C84 C86 H86 119.7 . . ? C86 C87 C88 120.8(5) . . ? C86 C87 H87 119.6 . . ? C88 C87 H87 119.6 . . ? C89 C88 C90 119.1(4) . . ? C89 C88 C87 119.3(4) . . ? C90 C88 C87 121.6(4) . . ? N3 C89 C88 121.4(4) . . ? N3 C89 C85 118.2(4) . . ? C88 C89 C85 120.3(4) . . ? C91 C90 C88 118.5(4) . . ? C91 C90 H90 120.8 . . ? C88 C90 H90 120.8 . . ? C90 C91 C92 120.7(4) . . ? C90 C91 H91 119.6 . . ? C92 C91 H91 119.6 . . ? N3 C92 C91 120.9(4) . . ? N3 C92 H92 119.6 . . ? C91 C92 H92 119.6 . . ? C68 N1 C65 116.9(3) . . ? C68 N1 Mn1 127.8(3) . . ? C65 N1 Mn1 115.1(2) . . ? C57 N2 C61 117.1(3) . . ? C57 N2 Mn1 126.7(3) . . ? C61 N2 Mn1 115.9(2) . . ? C92 N3 C89 119.4(4) . . ? C92 N3 Mn1 125.9(3) . . ? C89 N3 Mn1 114.4(3) . . ? C81 N4 C85 118.5(4) . . ? C81 N4 Mn1 128.2(3) . . ? C85 N4 Mn1 112.7(2) . . ? C80 N5 C74 118.2(3) . . ? C80 N5 Mn1 128.0(2) . . ? C74 N5 Mn1 113.4(2) . . ? C69 N6 C73 117.8(3) . . ? C69 N6 Mn1 127.6(3) . . ? C73 N6 Mn1 114.6(3) . . ? C21 O2 H2 109.5 . . ? C28 O3 H3 109.5 . . ? C3 O4 H4 111.6 . . ? C35 O5 H5A 109.5 . . ? C42 O6 H6A 117(5) . . ? C49 O7 H7A 96(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C27 C1 C2 C3 103.9(5) . . . . ? C27 C1 C2 C7 -75.7(5) . . . . ? C7 C2 C3 O4 -177.5(4) . . . . ? C1 C2 C3 O4 2.9(6) . . . . ? C7 C2 C3 C4 2.6(6) . . . . ? C1 C2 C3 C4 -177.0(4) . . . . ? O4 C3 C4 C5 175.3(4) . . . . ? C2 C3 C4 C5 -4.9(6) . . . . ? O4 C3 C4 C8 -6.3(6) . . . . ? C2 C3 C4 C8 173.5(4) . . . . ? C3 C4 C5 C6 3.2(7) . . . . ? C8 C4 C5 C6 -175.3(5) . . . . ? C4 C5 C6 C7 0.7(8) . . . . ? C5 C6 C7 C2 -3.1(8) . . . . ? C3 C2 C7 C6 1.4(7) . . . . ? C1 C2 C7 C6 -179.0(4) . . . . ? C5 C4 C8 C9 73.9(6) . . . . ? C3 C4 C8 C9 -104.5(5) . . . . ? C4 C8 C9 C10 -101.4(5) . . . . ? C4 C8 C9 C14 75.3(6) . . . . ? C14 C9 C10 C11 -0.4(8) . . . . ? C8 C9 C10 C11 176.3(5) . . . . ? C9 C10 C11 C12 -1.3(9) . . . . ? C10 C11 C12 C13 0.6(9) . . . . ? C11 C12 C13 C14 1.8(8) . . . . ? C11 C12 C13 C15 -178.7(5) . . . . ? C12 C13 C14 O1 175.6(4) . . . . ? C15 C13 C14 O1 -3.9(7) . . . . ? C12 C13 C14 C9 -3.6(7) . . . . ? C15 C13 C14 C9 176.9(5) . . . . ? C10 C9 C14 O1 -176.3(4) . . . . ? C8 C9 C14 O1 6.9(7) . . . . ? C10 C9 C14 C13 2.9(7) . . . . ? C8 C9 C14 C13 -173.9(5) . . . . ? C12 C13 C15 C16 103.3(6) . . . . ? C14 C13 C15 C16 -77.2(7) . . . . ? C13 C15 C16 C17 -88.0(6) . . . . ? C13 C15 C16 C21 91.1(6) . . . . ? C21 C16 C17 C18 2.6(7) . . . . ? C15 C16 C17 C18 -178.3(5) . . . . ? C16 C17 C18 C19 -2.2(9) . . . . ? C17 C18 C19 C20 1.8(8) . . . . ? C18 C19 C20 C21 -2.1(7) . . . . ? C18 C19 C20 C22 178.3(4) . . . . ? C19 C20 C21 O2 -177.7(4) . . . . ? C22 C20 C21 O2 1.9(6) . . . . ? C19 C20 C21 C16 2.6(6) . . . . ? C22 C20 C21 C16 -177.7(4) . . . . ? C17 C16 C21 O2 177.5(4) . . . . ? C15 C16 C21 O2 -1.7(6) . . . . ? C17 C16 C21 C20 -2.9(6) . . . . ? C15 C16 C21 C20 178.0(4) . . . . ? C19 C20 C22 C23 88.7(5) . . . . ? C21 C20 C22 C23 -90.9(5) . . . . ? C20 C22 C23 C24 -102.3(5) . . . . ? C20 C22 C23 C28 75.2(6) . . . . ? C28 C23 C24 C25 -0.1(8) . . . . ? C22 C23 C24 C25 177.6(5) . . . . ? C23 C24 C25 C26 1.3(10) . . . . ? C24 C25 C26 C27 -1.5(10) . . . . ? C25 C26 C27 C28 0.6(9) . . . . ? C25 C26 C27 C1 -176.3(5) . . . . ? C2 C1 C27 C26 105.3(6) . . . . ? C2 C1 C27 C28 -71.6(6) . . . . ? C24 C23 C28 O3 -179.3(4) . . . . ? C22 C23 C28 O3 3.1(6) . . . . ? C24 C23 C28 C27 -0.8(7) . . . . ? C22 C23 C28 C27 -178.4(4) . . . . ? C26 C27 C28 O3 179.1(5) . . . . ? C1 C27 C28 O3 -4.0(6) . . . . ? C26 C27 C28 C23 0.5(7) . . . . ? C1 C27 C28 C23 177.4(4) . . . . ? C55 C29 C30 C35 73.5(6) . . . . ? C55 C29 C30 C31 -106.5(6) . . . . ? C35 C30 C31 C32 -0.2(8) . . . . ? C29 C30 C31 C32 179.9(5) . . . . ? C30 C31 C32 C33 -1.0(10) . . . . ? C31 C32 C33 C34 0.3(10) . . . . ? C32 C33 C34 C35 1.6(8) . . . . ? C32 C33 C34 C36 -177.9(6) . . . . ? C31 C30 C35 O5 -178.1(4) . . . . ? C29 C30 C35 O5 1.9(7) . . . . ? C31 C30 C35 C34 2.1(7) . . . . ? C29 C30 C35 C34 -178.0(4) . . . . ? C33 C34 C35 O5 177.5(4) . . . . ? C36 C34 C35 O5 -3.0(7) . . . . ? C33 C34 C35 C30 -2.7(7) . . . . ? C36 C34 C35 C30 176.8(5) . . . . ? C35 C34 C36 C37 -77.9(6) . . . . ? C33 C34 C36 C37 101.6(5) . . . . ? C34 C36 C37 C38 -82.6(6) . . . . ? C34 C36 C37 C42 96.0(6) . . . . ? C42 C37 C38 C39 -0.7(8) . . . . ? C36 C37 C38 C39 178.0(6) . . . . ? C37 C38 C39 C40 3.3(9) . . . . ? C38 C39 C40 C41 -2.8(9) . . . . ? C39 C40 C41 C42 -0.1(8) . . . . ? C39 C40 C41 C43 178.4(5) . . . . ? C40 C41 C42 O6 -176.4(4) . . . . ? C43 C41 C42 O6 5.1(7) . . . . ? C40 C41 C42 C37 2.7(7) . . . . ? C43 C41 C42 C37 -175.8(4) . . . . ? C38 C37 C42 O6 176.9(4) . . . . ? C36 C37 C42 O6 -1.8(7) . . . . ? C38 C37 C42 C41 -2.3(7) . . . . ? C36 C37 C42 C41 179.0(5) . . . . ? C42 C41 C43 C44 -91.9(6) . . . . ? C40 C41 C43 C44 89.6(6) . . . . ? C41 C43 C44 C45 -100.0(6) . . . . ? C41 C43 C44 C49 73.9(7) . . . . ? C49 C44 C45 C46 0.5(8) . . . . ? C43 C44 C45 C46 174.7(5) . . . . ? C44 C45 C46 C47 -1.3(9) . . . . ? C45 C46 C47 C48 0.5(10) . . . . ? C46 C47 C48 C49 1.1(9) . . . . ? C46 C47 C48 C50 -175.2(5) . . . . ? C47 C48 C49 O7 175.4(5) . . . . ? C50 C48 C49 O7 -8.3(7) . . . . ? C47 C48 C49 C44 -2.0(7) . . . . ? C50 C48 C49 C44 174.2(5) . . . . ? C45 C44 C49 O7 -176.1(5) . . . . ? C43 C44 C49 O7 9.9(8) . . . . ? C45 C44 C49 C48 1.2(7) . . . . ? C43 C44 C49 C48 -172.9(5) . . . . ? C47 C48 C50 C51 98.5(6) . . . . ? C49 C48 C50 C51 -77.7(6) . . . . ? C48 C50 C51 C52 -74.6(6) . . . . ? C48 C50 C51 C56 101.7(6) . . . . ? C56 C51 C52 C53 -2.0(8) . . . . ? C50 C51 C52 C53 174.3(5) . . . . ? C51 C52 C53 C54 0.6(8) . . . . ? C52 C53 C54 C55 -0.1(8) . . . . ? C53 C54 C55 C56 1.1(7) . . . . ? C53 C54 C55 C29 -177.7(5) . . . . ? C30 C29 C55 C54 77.8(6) . . . . ? C30 C29 C55 C56 -101.0(6) . . . . ? C52 C51 C56 O8 -176.3(4) . . . . ? C50 C51 C56 O8 7.4(6) . . . . ? C52 C51 C56 C55 3.1(7) . . . . ? C50 C51 C56 C55 -173.2(4) . . . . ? C54 C55 C56 O8 176.7(4) . . . . ? C29 C55 C56 O8 -4.5(7) . . . . ? C54 C55 C56 C51 -2.7(7) . . . . ? C29 C55 C56 C51 176.1(5) . . . . ? N2 C57 C58 C59 0.2(7) . . . . ? C57 C58 C59 C60 0.1(7) . . . . ? C58 C59 C60 C61 1.0(7) . . . . ? C58 C59 C60 C62 -179.9(5) . . . . ? C59 C60 C61 N2 -2.4(6) . . . . ? C62 C60 C61 N2 178.4(4) . . . . ? C59 C60 C61 C65 177.6(4) . . . . ? C62 C60 C61 C65 -1.6(6) . . . . ? C61 C60 C62 C63 -0.4(9) . . . . ? C59 C60 C62 C63 -179.5(6) . . . . ? C60 C62 C63 C64 1.4(10) . . . . ? C62 C63 C64 C66 179.5(5) . . . . ? C62 C63 C64 C65 -0.4(8) . . . . ? C66 C64 C65 N1 -2.8(6) . . . . ? C63 C64 C65 N1 177.1(4) . . . . ? C66 C64 C65 C61 178.6(4) . . . . ? C63 C64 C65 C61 -1.5(6) . . . . ? N2 C61 C65 N1 3.8(5) . . . . ? C60 C61 C65 N1 -176.2(3) . . . . ? N2 C61 C65 C64 -177.5(3) . . . . ? C60 C61 C65 C64 2.5(5) . . . . ? C65 C64 C66 C67 0.2(7) . . . . ? C63 C64 C66 C67 -179.7(5) . . . . ? C64 C66 C67 C68 1.9(7) . . . . ? C66 C67 C68 N1 -1.7(7) . . . . ? N6 C69 C70 C71 -1.5(6) . . . . ? C69 C70 C71 C72 -0.1(6) . . . . ? C70 C71 C72 C73 1.7(6) . . . . ? C70 C71 C72 C75 -176.9(4) . . . . ? C71 C72 C73 N6 -1.8(6) . . . . ? C75 C72 C73 N6 176.8(4) . . . . ? C71 C72 C73 C74 177.4(4) . . . . ? C75 C72 C73 C74 -4.0(6) . . . . ? N6 C73 C74 N5 4.0(5) . . . . ? C72 C73 C74 N5 -175.1(3) . . . . ? N6 C73 C74 C77 -177.1(3) . . . . ? C72 C73 C74 C77 3.7(5) . . . . ? C73 C72 C75 C76 0.9(7) . . . . ? C71 C72 C75 C76 179.5(4) . . . . ? C72 C75 C76 C77 2.6(7) . . . . ? N5 C74 C77 C78 -1.8(5) . . . . ? C73 C74 C77 C78 179.4(3) . . . . ? N5 C74 C77 C76 178.5(3) . . . . ? C73 C74 C77 C76 -0.3(5) . . . . ? C75 C76 C77 C78 177.4(4) . . . . ? C75 C76 C77 C74 -2.9(6) . . . . ? C74 C77 C78 C79 3.1(6) . . . . ? C76 C77 C78 C79 -177.3(4) . . . . ? C77 C78 C79 C80 -2.7(6) . . . . ? C78 C79 C80 N5 1.0(6) . . . . ? N4 C81 C82 C83 4.3(7) . . . . ? C81 C82 C83 C84 -3.2(7) . . . . ? C82 C83 C84 C85 -0.1(7) . . . . ? C82 C83 C84 C86 -179.0(4) . . . . ? C83 C84 C85 N4 2.6(6) . . . . ? C86 C84 C85 N4 -178.4(4) . . . . ? C83 C84 C85 C89 -172.5(4) . . . . ? C86 C84 C85 C89 6.4(6) . . . . ? C83 C84 C86 C87 172.7(4) . . . . ? C85 C84 C86 C87 -6.2(7) . . . . ? C84 C86 C87 C88 1.1(7) . . . . ? C86 C87 C88 C89 3.9(6) . . . . ? C86 C87 C88 C90 -174.3(4) . . . . ? C90 C88 C89 N3 -1.0(6) . . . . ? C87 C88 C89 N3 -179.2(3) . . . . ? C90 C88 C89 C85 174.7(3) . . . . ? C87 C88 C89 C85 -3.6(6) . . . . ? N4 C85 C89 N3 -1.1(5) . . . . ? C84 C85 C89 N3 174.2(3) . . . . ? N4 C85 C89 C88 -176.8(3) . . . . ? C84 C85 C89 C88 -1.6(5) . . . . ? C89 C88 C90 C91 -0.1(6) . . . . ? C87 C88 C90 C91 178.2(4) . . . . ? C88 C90 C91 C92 0.2(6) . . . . ? C90 C91 C92 N3 0.7(6) . . . . ? C67 C68 N1 C65 -0.8(6) . . . . ? C67 C68 N1 Mn1 -175.6(3) . . . . ? C64 C65 N1 C68 3.0(5) . . . . ? C61 C65 N1 C68 -178.3(3) . . . . ? C64 C65 N1 Mn1 178.5(3) . . . . ? C61 C65 N1 Mn1 -2.8(4) . . . . ? N3 Mn1 N1 C68 65.7(3) . . . . ? N2 Mn1 N1 C68 176.0(3) . . . . ? N6 Mn1 N1 C68 -97.7(3) . . . . ? N4 Mn1 N1 C68 -10.2(3) . . . . ? N5 Mn1 N1 C68 134.9(5) . . . . ? N3 Mn1 N1 C65 -109.2(2) . . . . ? N2 Mn1 N1 C65 1.0(2) . . . . ? N6 Mn1 N1 C65 87.3(2) . . . . ? N4 Mn1 N1 C65 174.9(3) . . . . ? N5 Mn1 N1 C65 -40.1(7) . . . . ? C58 C57 N2 C61 -1.5(6) . . . . ? C58 C57 N2 Mn1 -175.4(3) . . . . ? C60 C61 N2 C57 2.6(5) . . . . ? C65 C61 N2 C57 -177.4(3) . . . . ? C60 C61 N2 Mn1 177.2(3) . . . . ? C65 C61 N2 Mn1 -2.8(4) . . . . ? N3 Mn1 N2 C57 -104.7(3) . . . . ? N6 Mn1 N2 C57 61.5(3) . . . . ? N4 Mn1 N2 C57 158.1(3) . . . . ? N1 Mn1 N2 C57 174.9(3) . . . . ? N5 Mn1 N2 C57 -12.9(3) . . . . ? N3 Mn1 N2 C61 81.3(3) . . . . ? N6 Mn1 N2 C61 -112.5(3) . . . . ? N4 Mn1 N2 C61 -15.9(5) . . . . ? N1 Mn1 N2 C61 0.9(2) . . . . ? N5 Mn1 N2 C61 173.1(2) . . . . ? C91 C92 N3 C89 -1.7(5) . . . . ? C91 C92 N3 Mn1 -174.9(3) . . . . ? C88 C89 N3 C92 1.8(5) . . . . ? C85 C89 N3 C92 -173.9(3) . . . . ? C88 C89 N3 Mn1 175.8(3) . . . . ? C85 C89 N3 Mn1 0.1(4) . . . . ? N2 Mn1 N3 C92 16.0(3) . . . . ? N6 Mn1 N3 C92 -130.3(3) . . . . ? N4 Mn1 N3 C92 174.0(3) . . . . ? N1 Mn1 N3 C92 87.2(3) . . . . ? N5 Mn1 N3 C92 -81.7(3) . . . . ? N2 Mn1 N3 C89 -157.5(2) . . . . ? N6 Mn1 N3 C89 56.2(4) . . . . ? N4 Mn1 N3 C89 0.5(2) . . . . ? N1 Mn1 N3 C89 -86.3(2) . . . . ? N5 Mn1 N3 C89 104.9(2) . . . . ? C82 C81 N4 C85 -1.8(6) . . . . ? C82 C81 N4 Mn1 168.9(3) . . . . ? C84 C85 N4 C81 -1.7(6) . . . . ? C89 C85 N4 C81 173.6(3) . . . . ? C84 C85 N4 Mn1 -173.8(3) . . . . ? C89 C85 N4 Mn1 1.5(4) . . . . ? N3 Mn1 N4 C81 -172.2(3) . . . . ? N2 Mn1 N4 C81 -68.7(5) . . . . ? N6 Mn1 N4 C81 28.6(3) . . . . ? N1 Mn1 N4 C81 -84.9(3) . . . . ? N5 Mn1 N4 C81 102.1(3) . . . . ? N3 Mn1 N4 C85 -1.0(2) . . . . ? N2 Mn1 N4 C85 102.4(4) . . . . ? N6 Mn1 N4 C85 -160.3(3) . . . . ? N1 Mn1 N4 C85 86.2(3) . . . . ? N5 Mn1 N4 C85 -86.8(3) . . . . ? C79 C80 N5 C74 0.3(6) . . . . ? C79 C80 N5 Mn1 -172.3(3) . . . . ? C77 C74 N5 C80 0.2(5) . . . . ? C73 C74 N5 C80 179.0(3) . . . . ? C77 C74 N5 Mn1 173.8(3) . . . . ? C73 C74 N5 Mn1 -7.4(4) . . . . ? N3 Mn1 N5 C80 18.5(3) . . . . ? N2 Mn1 N5 C80 -89.8(3) . . . . ? N6 Mn1 N5 C80 178.9(3) . . . . ? N4 Mn1 N5 C80 93.6(3) . . . . ? N1 Mn1 N5 C80 -50.4(7) . . . . ? N3 Mn1 N5 C74 -154.4(2) . . . . ? N2 Mn1 N5 C74 97.3(2) . . . . ? N6 Mn1 N5 C74 6.0(2) . . . . ? N4 Mn1 N5 C74 -79.3(3) . . . . ? N1 Mn1 N5 C74 136.7(5) . . . . ? C70 C69 N6 C73 1.4(6) . . . . ? C70 C69 N6 Mn1 -179.3(3) . . . . ? C72 C73 N6 C69 0.3(5) . . . . ? C74 C73 N6 C69 -178.9(3) . . . . ? C72 C73 N6 Mn1 -179.2(3) . . . . ? C74 C73 N6 Mn1 1.7(4) . . . . ? N3 Mn1 N6 C69 -132.1(3) . . . . ? N2 Mn1 N6 C69 79.8(3) . . . . ? N4 Mn1 N6 C69 -78.9(3) . . . . ? N1 Mn1 N6 C69 6.5(4) . . . . ? N5 Mn1 N6 C69 176.6(3) . . . . ? N3 Mn1 N6 C73 47.3(4) . . . . ? N2 Mn1 N6 C73 -100.8(2) . . . . ? N4 Mn1 N6 C73 100.5(3) . . . . ? N1 Mn1 N6 C73 -174.1(2) . . . . ? N5 Mn1 N6 C73 -4.0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.82 1.97 2.517(5) 123.5 . O3 H3 O2 0.82 1.77 2.495(4) 146.5 . O4 H4 O3 0.86 1.97 2.757(4) 151.9 . O5 H5A O8 0.82 1.99 2.741(4) 152.3 . O7 H7A O6 0.81(2) 1.79(3) 2.515(5) 148(6) . O6 H6A O5 0.83(2) 1.71(4) 2.493(6) 156(7) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.506 _refine_diff_density_min -0.867 _refine_diff_density_rms 0.048 #===== data_2 _database_code_depnum_ccdc_archive 'CCDC 879384' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H70 Cd N6 O8' _chemical_formula_weight 1499.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.155(4) _cell_length_b 15.844(5) _cell_length_c 20.126(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.761(5) _cell_angle_gamma 90.00 _cell_volume 7201(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 2.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5249 _exptl_absorpt_correction_T_max 0.6179 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31632 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 67.04 _reflns_number_total 12663 _reflns_number_gt 8400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distances of O1---H1A and O2---H2A were restrained to 0.82+-0.02 \%A. The distance of O8---H8A was restrained to 0.82+-0.01 \%A. The distance of C44...H2A was restrained to 1.72+-0.02 \%A. The distance of C72...H8A was restrained to 1.62+-0.02 \%A. The distance of H8A...H7 was restrained to 2.02+-0.02 \%A. For C62, C61 and C60 atoms, SIMU restraint was used to make them behave similar anisotropic displacement parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1005P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12663 _refine_ls_number_parameters 977 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1' Cd 0.21179(17) -0.5184(2) 0.34177(18) 0.0558(8) Uiso 0.10 1 d P . . Cd1 Cd 0.237323(15) -0.48857(2) 0.331345(17) 0.04613(12) Uani 0.90 1 d P . . C1 C 0.3107(2) -0.3276(3) 0.2869(3) 0.0630(12) Uani 1 1 d . . . H1 H 0.3265 -0.3687 0.2631 0.076 Uiso 1 1 calc R . . C2 C 0.3298(2) -0.2456(3) 0.2844(3) 0.0706(14) Uani 1 1 d . . . H2 H 0.3593 -0.2322 0.2615 0.085 Uiso 1 1 calc R . . C3 C 0.3047(2) -0.1852(4) 0.3157(3) 0.0762(14) Uani 1 1 d . . . H3 H 0.3165 -0.1294 0.3138 0.091 Uiso 1 1 calc R . . C4 C 0.2604(2) -0.2063(3) 0.3518(3) 0.0626(11) Uani 1 1 d . . . C5 C 0.2313(3) -0.1445(3) 0.3844(3) 0.0760(14) Uani 1 1 d . . . H5 H 0.2419 -0.0880 0.3830 0.091 Uiso 1 1 calc R . . C6 C 0.1892(3) -0.1666(3) 0.4169(3) 0.0721(14) Uani 1 1 d . . . H6 H 0.1694 -0.1247 0.4354 0.086 Uiso 1 1 calc R . . C7 C 0.1739(2) -0.2529(3) 0.4238(2) 0.0559(10) Uani 1 1 d . . . C8 C 0.1316(2) -0.2797(3) 0.4597(2) 0.0645(12) Uani 1 1 d . . . H8 H 0.1105 -0.2399 0.4788 0.077 Uiso 1 1 calc R . . C9 C 0.1212(2) -0.3625(3) 0.4668(3) 0.0665(12) Uani 1 1 d . . . H70 H 0.0937 -0.3805 0.4912 0.080 Uiso 1 1 calc R . . C10 C 0.1529(2) -0.4212(3) 0.4365(3) 0.0627(12) Uani 1 1 d . . . H10 H 0.1462 -0.4784 0.4419 0.075 Uiso 1 1 calc R . . C11 C 0.20266(17) -0.3163(3) 0.3937(2) 0.0484(9) Uani 1 1 d . . . C12 C 0.24586(17) -0.2920(3) 0.3551(2) 0.0497(10) Uani 1 1 d . . . C13 C 0.3364(2) -0.4925(3) 0.4742(2) 0.0637(12) Uani 1 1 d . . . H13 H 0.3135 -0.4489 0.4857 0.076 Uiso 1 1 calc R . . C14 C 0.3876(2) -0.5163(4) 0.5205(3) 0.0771(15) Uani 1 1 d . . . H14 H 0.3991 -0.4889 0.5622 0.093 Uiso 1 1 calc R . . C15 C 0.4204(3) -0.5796(4) 0.5040(3) 0.0858(17) Uani 1 1 d . . . H15 H 0.4544 -0.5964 0.5350 0.103 Uiso 1 1 calc R . . C16 C 0.4043(2) -0.6208(4) 0.4407(3) 0.0703(13) Uani 1 1 d . . . C17 C 0.4380(3) -0.6871(5) 0.4198(4) 0.101(2) Uani 1 1 d . . . H17 H 0.4728 -0.7049 0.4490 0.121 Uiso 1 1 calc R . . C18 C 0.4206(3) -0.7238(4) 0.3596(4) 0.094(2) Uani 1 1 d . . . H18 H 0.4427 -0.7684 0.3482 0.112 Uiso 1 1 calc R . . C19 C 0.3689(2) -0.6967(3) 0.3116(3) 0.0621(12) Uani 1 1 d . . . C20 C 0.3496(2) -0.7335(4) 0.2475(3) 0.0701(14) Uani 1 1 d . . . H20 H 0.3707 -0.7779 0.2341 0.084 Uiso 1 1 calc R . . C21 C 0.3003(2) -0.7045(4) 0.2050(3) 0.0744(14) Uani 1 1 d . . . H21 H 0.2866 -0.7292 0.1626 0.089 Uiso 1 1 calc R . . C22 C 0.2699(2) -0.6366(3) 0.2258(2) 0.0634(12) Uani 1 1 d . . . H22 H 0.2364 -0.6163 0.1958 0.076 Uiso 1 1 calc R . . C23 C 0.33514(17) -0.6300(3) 0.3296(2) 0.0485(9) Uani 1 1 d . . . C24 C 0.35254(17) -0.5922(3) 0.3960(2) 0.0494(9) Uani 1 1 d . . . C25 C 0.1870(2) -0.4370(4) 0.1700(3) 0.0701(13) Uani 1 1 d . . . H25 H 0.2182 -0.3987 0.1780 0.084 Uiso 1 1 calc R . . C26 C 0.1530(3) -0.4460(4) 0.1040(3) 0.0828(17) Uani 1 1 d . . . H26 H 0.1632 -0.4172 0.0679 0.099 Uiso 1 1 calc R . . C27 C 0.1054(3) -0.4967(4) 0.0930(3) 0.0743(15) Uani 1 1 d . . . H27 H 0.0810 -0.5003 0.0497 0.089 Uiso 1 1 calc R . . C28 C 0.0921(2) -0.5441(3) 0.1466(2) 0.0626(12) Uani 1 1 d . . . C29 C 0.0434(3) -0.6011(4) 0.1377(3) 0.0774(15) Uani 1 1 d . . . H29 H 0.0163 -0.6031 0.0961 0.093 Uiso 1 1 calc R . . C30 C 0.0360(2) -0.6522(4) 0.1888(3) 0.0762(14) Uani 1 1 d . . . H30 H 0.0043 -0.6896 0.1819 0.091 Uiso 1 1 calc R . . C31 C 0.0768(2) -0.6491(3) 0.2535(3) 0.0608(11) Uani 1 1 d . . . C32 C 0.0728(2) -0.7064(3) 0.3058(3) 0.0702(13) Uani 1 1 d . . . H32 H 0.0428 -0.7466 0.2995 0.084 Uiso 1 1 calc R . . C33 C 0.1135(2) -0.7019(4) 0.3657(3) 0.0720(13) Uani 1 1 d . . . H33 H 0.1120 -0.7401 0.4004 0.086 Uiso 1 1 calc R . . C34 C 0.1573(2) -0.6410(3) 0.3753(2) 0.0575(11) Uani 1 1 d . . . H34 H 0.1845 -0.6382 0.4169 0.069 Uiso 1 1 calc R . . C35 C 0.12208(17) -0.5895(3) 0.2657(2) 0.0522(10) Uani 1 1 d . . . C36 C 0.13061(19) -0.5355(3) 0.2115(2) 0.0515(10) Uani 1 1 d . . . C37 C 0.1672(3) -0.9248(3) 0.3996(3) 0.0753(15) Uani 1 1 d . . . C38 C 0.2164(3) -0.8728(4) 0.4172(3) 0.0812(16) Uani 1 1 d . . . C39 C 0.2358(3) -0.8310(5) 0.3656(4) 0.101(2) Uani 1 1 d . . . H39 H 0.2684 -0.7952 0.3759 0.121 Uiso 1 1 calc R . . C40 C 0.2057(4) -0.8434(5) 0.2975(4) 0.108(3) Uani 1 1 d . . . H40 H 0.2195 -0.8174 0.2626 0.130 Uiso 1 1 calc R . . C41 C 0.1562(3) -0.8935(5) 0.2822(4) 0.097(2) Uani 1 1 d . . . H41 H 0.1362 -0.8996 0.2370 0.116 Uiso 1 1 calc R . . C42 C 0.1356(3) -0.9347(4) 0.3318(3) 0.0827(16) Uani 1 1 d . . . C43 C 0.0785(3) -0.9857(4) 0.3150(4) 0.103(2) Uani 1 1 d . . . H43A H 0.0790 -1.0218 0.2762 0.124 Uiso 1 1 calc R . . H43B H 0.0765 -1.0218 0.3534 0.124 Uiso 1 1 calc R . . C44 C 0.0027(3) -0.8907(4) 0.3512(3) 0.0738(14) Uani 1 1 d D . . C45 C 0.0242(3) -0.9306(4) 0.2991(3) 0.0835(16) Uani 1 1 d . . . C46 C -0.0040(4) -0.9107(6) 0.2321(4) 0.114(3) Uani 1 1 d . . . H46 H 0.0091 -0.9362 0.1965 0.137 Uiso 1 1 calc R . . C47 C -0.0505(4) -0.8546(6) 0.2170(4) 0.118(3) Uani 1 1 d . . . H47 H -0.0687 -0.8426 0.1720 0.141 Uiso 1 1 calc R . . C48 C -0.0692(3) -0.8171(5) 0.2692(4) 0.103(2) Uani 1 1 d . . . H48 H -0.1004 -0.7790 0.2589 0.124 Uiso 1 1 calc R . . C49 C -0.0440(3) -0.8332(4) 0.3367(3) 0.0833(16) Uani 1 1 d . . . C50 C -0.0639(3) -0.7841(5) 0.3916(4) 0.095(2) Uani 1 1 d . . . H50A H -0.1031 -0.7616 0.3728 0.115 Uiso 1 1 calc R . . H50B H -0.0674 -0.8228 0.4278 0.115 Uiso 1 1 calc R . . C51 C 0.0199(3) -0.7264(4) 0.4790(3) 0.0802(16) Uani 1 1 d . . . C52 C -0.0245(3) -0.7128(4) 0.4220(4) 0.0829(17) Uani 1 1 d . . . C53 C -0.0320(3) -0.6313(5) 0.3930(4) 0.102(2) Uani 1 1 d . . . H53 H -0.0610 -0.6214 0.3538 0.122 Uiso 1 1 calc R . . C54 C 0.0036(5) -0.5672(5) 0.4230(5) 0.116(3) Uani 1 1 d . . . H54 H -0.0009 -0.5137 0.4035 0.139 Uiso 1 1 calc R . . C55 C 0.0452(4) -0.5803(4) 0.4807(4) 0.104(2) Uani 1 1 d . . . H55 H 0.0681 -0.5349 0.5005 0.125 Uiso 1 1 calc R . . C56 C 0.0548(3) -0.6586(4) 0.5113(3) 0.0880(19) Uani 1 1 d . . . C57 C 0.1024(4) -0.6731(4) 0.5744(3) 0.113(3) Uani 1 1 d . . . H57A H 0.1041 -0.6245 0.6041 0.135 Uiso 1 1 calc R . . H57B H 0.0918 -0.7217 0.5984 0.135 Uiso 1 1 calc R . . C58 C 0.1771(3) -0.7656(4) 0.5359(3) 0.0842(18) Uani 1 1 d . . . C59 C 0.1622(4) -0.6873(4) 0.5608(3) 0.095(2) Uani 1 1 d . . . C60 C 0.2034(4) -0.6235(6) 0.5707(3) 0.122(2) Uani 1 1 d U . . H60 H 0.1937 -0.5718 0.5870 0.146 Uiso 1 1 calc R . . C61 C 0.2578(4) -0.6339(6) 0.5573(4) 0.1226(19) Uani 1 1 d U . . H61 H 0.2853 -0.5902 0.5657 0.147 Uiso 1 1 calc R . . C62 C 0.2720(4) -0.7075(6) 0.5318(3) 0.121(2) Uani 1 1 d U . . H62 H 0.3090 -0.7137 0.5216 0.145 Uiso 1 1 calc R . . C63 C 0.2313(3) -0.7762(5) 0.5202(3) 0.0907(19) Uani 1 1 d . . . C64 C 0.2480(3) -0.8587(6) 0.4911(4) 0.113(3) Uani 1 1 d . . . H64A H 0.2386 -0.9049 0.5185 0.136 Uiso 1 1 calc R . . H64B H 0.2904 -0.8593 0.4943 0.136 Uiso 1 1 calc R . . C65 C 0.4114(2) -0.3354(4) 0.1644(3) 0.0754(15) Uani 1 1 d . . . C66 C 0.4289(2) -0.4053(4) 0.2059(3) 0.0778(16) Uani 1 1 d . . . C67 C 0.3956(3) -0.4782(4) 0.1933(4) 0.0904(19) Uani 1 1 d . . . H67 H 0.4074 -0.5258 0.2199 0.108 Uiso 1 1 calc R . . C68 C 0.3449(3) -0.4818(5) 0.1416(4) 0.098(2) Uani 1 1 d . . . H68 H 0.3230 -0.5313 0.1336 0.118 Uiso 1 1 calc R . . C69 C 0.3275(3) -0.4120(5) 0.1027(4) 0.097(2) Uani 1 1 d . . . H69 H 0.2935 -0.4147 0.0681 0.116 Uiso 1 1 calc R . . C70 C 0.3592(3) -0.3371(4) 0.1133(3) 0.0796(15) Uani 1 1 d . . . C71 C 0.3394(3) -0.2580(5) 0.0705(3) 0.098(2) Uani 1 1 d . . . H71A H 0.3736 -0.2342 0.0568 0.118 Uiso 1 1 calc R . . H71B H 0.3113 -0.2747 0.0294 0.118 Uiso 1 1 calc R . . C72 C 0.3464(2) -0.1236(4) 0.1403(3) 0.0750(15) Uani 1 1 d D . . C73 C 0.3113(3) -0.1895(4) 0.1058(3) 0.0840(17) Uani 1 1 d . . . C74 C 0.2519(3) -0.1921(5) 0.1070(4) 0.101(2) Uani 1 1 d . . . H74 H 0.2287 -0.2364 0.0857 0.121 Uiso 1 1 calc R . . C75 C 0.2262(3) -0.1297(5) 0.1394(4) 0.105(2) Uani 1 1 d . . . H75 H 0.1862 -0.1320 0.1396 0.126 Uiso 1 1 calc R . . C76 C 0.2606(3) -0.0645(4) 0.1708(4) 0.0899(18) Uani 1 1 d . . . H76 H 0.2432 -0.0224 0.1920 0.108 Uiso 1 1 calc R . . C77 C 0.3211(3) -0.0598(4) 0.1719(3) 0.0790(16) Uani 1 1 d . . . C78 C 0.3578(3) 0.0119(4) 0.2069(4) 0.0872(18) Uani 1 1 d . . . H78A H 0.3337 0.0626 0.2007 0.105 Uiso 1 1 calc R . . H78B H 0.3905 0.0211 0.1849 0.105 Uiso 1 1 calc R . . C79 C 0.4311(2) -0.0536(3) 0.3058(3) 0.0694(13) Uani 1 1 d . . . C80 C 0.3824(2) -0.0007(3) 0.2823(4) 0.0751(15) Uani 1 1 d . . . C81 C 0.3565(3) 0.0389(5) 0.3290(5) 0.105(2) Uani 1 1 d . . . H81 H 0.3247 0.0750 0.3134 0.126 Uiso 1 1 calc R . . C82 C 0.3758(4) 0.0271(5) 0.3973(5) 0.116(3) Uani 1 1 d . . . H82 H 0.3570 0.0540 0.4278 0.139 Uiso 1 1 calc R . . C83 C 0.4235(4) -0.0253(5) 0.4207(4) 0.105(2) Uani 1 1 d . . . H83 H 0.4368 -0.0330 0.4674 0.126 Uiso 1 1 calc R . . C84 C 0.4522(3) -0.0668(4) 0.3764(3) 0.0794(15) Uani 1 1 d . . . C85 C 0.5019(2) -0.1283(4) 0.4019(3) 0.0855(16) Uani 1 1 d . . . H85A H 0.5171 -0.1196 0.4503 0.103 Uiso 1 1 calc R . . H85B H 0.5338 -0.1176 0.3789 0.103 Uiso 1 1 calc R . . C86 C 0.49460(19) -0.2682(4) 0.3375(3) 0.0685(13) Uani 1 1 d . . . C87 C 0.4817(2) -0.2195(4) 0.3896(3) 0.0701(13) Uani 1 1 d . . . C88 C 0.4476(2) -0.2536(4) 0.4309(3) 0.0814(16) Uani 1 1 d . . . H88 H 0.4381 -0.2214 0.4657 0.098 Uiso 1 1 calc R . . C89 C 0.4275(3) -0.3346(5) 0.4209(4) 0.0932(19) Uani 1 1 d . . . H89 H 0.4055 -0.3578 0.4497 0.112 Uiso 1 1 calc R . . C90 C 0.4397(2) -0.3825(4) 0.3682(4) 0.0875(19) Uani 1 1 d . . . H90 H 0.4253 -0.4374 0.3618 0.105 Uiso 1 1 calc R . . C91 C 0.4735(2) -0.3500(3) 0.3242(3) 0.0709(14) Uani 1 1 d . . . C92 C 0.4828(2) -0.4001(4) 0.2636(4) 0.0910(19) Uani 1 1 d . . . H92A H 0.5148 -0.3746 0.2467 0.109 Uiso 1 1 calc R . . H92B H 0.4949 -0.4569 0.2784 0.109 Uiso 1 1 calc R . . N1 N 0.16143(16) -0.5861(2) 0.32654(19) 0.0546(8) Uani 1 1 d . . . N2 N 0.17616(16) -0.4815(3) 0.22154(18) 0.0565(9) Uani 1 1 d . . . N3 N 0.28664(15) -0.5999(2) 0.28609(18) 0.0507(8) Uani 1 1 d . . . N4 N 0.31892(15) -0.5300(2) 0.41397(17) 0.0499(8) Uani 1 1 d . . . N5 N 0.19143(15) -0.3991(2) 0.40117(19) 0.0533(9) Uani 1 1 d . . . N6 N 0.27062(15) -0.3509(2) 0.3219(2) 0.0558(9) Uani 1 1 d . . . O3 O 0.1497(2) -0.9696(3) 0.4503(2) 0.0998(14) Uani 1 1 d . . . O4 O 0.1381(2) -0.8303(2) 0.5272(2) 0.0873(11) Uani 1 1 d . . . H4A H 0.1527 -0.8715 0.5125 0.131 Uiso 1 1 calc R . . O6 O 0.45946(15) -0.0939(2) 0.2638(2) 0.0752(10) Uani 1 1 d . . . H6A H 0.4438 -0.0822 0.2242 0.113 Uiso 1 1 calc R . . O7 O 0.44731(17) -0.2668(3) 0.1755(2) 0.0906(12) Uani 1 1 d . . . H7 H 0.4273 -0.2239 0.1667 0.136 Uiso 1 1 calc RD . . O1 O 0.0308(3) -0.8047(3) 0.5052(2) 0.0992(13) Uani 1 1 d D . . H1A H 0.020(4) -0.833(5) 0.470(3) 0.149 Uiso 1 1 d D . . O2 O 0.02670(18) -0.9131(3) 0.4150(2) 0.0830(10) Uani 1 1 d D . . H2A H 0.0616(12) -0.923(5) 0.4137(19) 0.125 Uiso 1 1 d D . . O5 O 0.53088(16) -0.2340(3) 0.2982(2) 0.0900(12) Uani 1 1 d . . . O8 O 0.40479(18) -0.1211(3) 0.1437(2) 0.0863(11) Uani 1 1 d D . . H8A H 0.4019(11) -0.1251(17) 0.1027(6) 0.129 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04807(19) 0.04124(19) 0.04736(18) -0.00160(15) 0.00680(13) 0.00465(15) C1 0.054(2) 0.066(3) 0.072(3) 0.005(3) 0.018(2) 0.013(2) C2 0.074(3) 0.068(3) 0.071(3) 0.020(3) 0.018(3) 0.004(3) C3 0.082(3) 0.063(3) 0.084(4) 0.017(3) 0.017(3) 0.000(3) C4 0.070(3) 0.054(3) 0.062(3) 0.010(2) 0.009(2) 0.007(2) C5 0.099(4) 0.046(3) 0.083(4) 0.002(3) 0.022(3) 0.004(3) C6 0.091(3) 0.052(3) 0.074(3) -0.005(3) 0.021(3) 0.016(3) C7 0.067(3) 0.047(3) 0.052(2) -0.003(2) 0.009(2) 0.010(2) C8 0.074(3) 0.068(3) 0.054(3) -0.011(2) 0.020(2) 0.016(2) C9 0.071(3) 0.067(3) 0.065(3) -0.003(3) 0.025(2) 0.001(2) C10 0.070(3) 0.054(3) 0.067(3) -0.001(2) 0.021(2) -0.001(2) C11 0.050(2) 0.045(2) 0.046(2) -0.0034(18) 0.0017(17) 0.0109(17) C12 0.050(2) 0.049(2) 0.047(2) 0.0058(19) 0.0033(18) 0.0129(18) C13 0.076(3) 0.058(3) 0.051(2) -0.013(2) 0.002(2) 0.007(2) C14 0.083(3) 0.090(4) 0.050(3) -0.016(3) -0.004(2) 0.007(3) C15 0.079(3) 0.101(5) 0.063(3) -0.009(3) -0.015(3) 0.022(3) C16 0.062(3) 0.081(4) 0.062(3) -0.008(3) 0.000(2) 0.018(2) C17 0.083(4) 0.116(5) 0.088(4) -0.022(4) -0.015(3) 0.051(4) C18 0.077(3) 0.102(5) 0.096(5) -0.026(4) 0.005(3) 0.043(3) C19 0.061(3) 0.062(3) 0.065(3) -0.011(2) 0.018(2) 0.012(2) C20 0.065(3) 0.072(3) 0.077(3) -0.024(3) 0.024(3) 0.007(2) C21 0.082(3) 0.083(4) 0.059(3) -0.023(3) 0.017(3) 0.000(3) C22 0.070(3) 0.071(3) 0.046(2) -0.012(2) 0.006(2) 0.005(2) C23 0.052(2) 0.050(2) 0.044(2) -0.0013(19) 0.0110(18) 0.0022(18) C24 0.049(2) 0.047(2) 0.051(2) 0.0001(19) 0.0080(18) 0.0050(18) C25 0.083(3) 0.071(3) 0.058(3) 0.018(3) 0.020(3) 0.012(3) C26 0.113(5) 0.090(4) 0.051(3) 0.015(3) 0.030(3) 0.029(4) C27 0.091(4) 0.087(4) 0.041(2) -0.005(3) 0.004(2) 0.015(3) C28 0.073(3) 0.063(3) 0.049(3) -0.003(2) 0.007(2) 0.015(2) C29 0.083(3) 0.075(4) 0.062(3) -0.022(3) -0.009(3) 0.010(3) C30 0.073(3) 0.076(4) 0.074(4) -0.014(3) 0.001(3) -0.006(3) C31 0.065(3) 0.056(3) 0.062(3) -0.010(2) 0.016(2) 0.005(2) C32 0.080(3) 0.059(3) 0.076(4) -0.010(3) 0.028(3) -0.008(2) C33 0.087(3) 0.069(3) 0.063(3) 0.000(3) 0.023(3) -0.003(3) C34 0.081(3) 0.049(3) 0.045(2) 0.007(2) 0.017(2) 0.003(2) C35 0.047(2) 0.066(3) 0.042(2) -0.004(2) 0.0072(18) 0.0125(19) C36 0.054(2) 0.051(3) 0.048(2) -0.0009(19) 0.0064(19) 0.0115(19) C37 0.100(4) 0.055(3) 0.077(4) 0.002(3) 0.032(3) 0.014(3) C38 0.076(3) 0.083(4) 0.086(4) 0.015(3) 0.022(3) 0.021(3) C39 0.085(4) 0.118(6) 0.108(6) 0.018(5) 0.041(4) 0.014(4) C40 0.119(6) 0.128(6) 0.098(5) 0.031(5) 0.067(5) 0.032(5) C41 0.111(5) 0.104(5) 0.086(4) -0.004(4) 0.045(4) 0.011(4) C42 0.100(4) 0.069(4) 0.087(4) -0.016(3) 0.037(3) 0.015(3) C43 0.129(6) 0.082(4) 0.107(5) -0.048(4) 0.045(5) -0.011(4) C44 0.079(3) 0.074(4) 0.072(4) -0.015(3) 0.024(3) -0.022(3) C45 0.097(4) 0.079(4) 0.072(4) -0.019(3) 0.013(3) -0.028(3) C46 0.144(7) 0.129(7) 0.068(4) -0.039(4) 0.019(5) -0.052(6) C47 0.112(6) 0.144(8) 0.082(5) -0.004(5) -0.010(4) -0.054(6) C48 0.092(4) 0.117(6) 0.096(5) -0.002(5) 0.009(4) -0.030(4) C49 0.071(3) 0.096(4) 0.079(4) -0.003(3) 0.008(3) -0.024(3) C50 0.077(4) 0.105(5) 0.110(5) -0.001(4) 0.033(4) 0.009(3) C51 0.113(4) 0.062(4) 0.078(4) 0.004(3) 0.048(4) -0.003(3) C52 0.095(4) 0.071(4) 0.099(5) -0.002(3) 0.056(4) 0.003(3) C53 0.120(5) 0.089(5) 0.115(6) 0.010(4) 0.065(5) 0.029(4) C54 0.185(8) 0.062(4) 0.127(7) 0.011(5) 0.090(7) 0.018(5) C55 0.169(7) 0.058(4) 0.105(6) -0.014(4) 0.074(6) -0.009(4) C56 0.145(5) 0.057(3) 0.082(4) -0.015(3) 0.067(4) -0.011(3) C57 0.215(9) 0.070(4) 0.065(4) -0.022(3) 0.055(5) -0.037(5) C58 0.122(5) 0.081(4) 0.042(3) 0.007(3) 0.001(3) -0.034(4) C59 0.153(6) 0.080(4) 0.049(3) -0.008(3) 0.017(4) -0.040(4) C60 0.164(4) 0.122(4) 0.062(3) 0.007(3) -0.012(3) -0.063(4) C61 0.162(4) 0.124(4) 0.064(3) 0.011(2) -0.015(3) -0.064(4) C62 0.158(4) 0.126(4) 0.062(3) 0.013(3) -0.013(3) -0.063(4) C63 0.106(5) 0.096(5) 0.056(3) 0.019(3) -0.014(3) -0.018(4) C64 0.078(4) 0.155(8) 0.096(5) 0.039(5) -0.007(3) 0.004(4) C65 0.067(3) 0.079(4) 0.086(4) -0.013(3) 0.029(3) -0.014(3) C66 0.070(3) 0.066(4) 0.102(4) -0.014(3) 0.029(3) 0.007(3) C67 0.097(4) 0.064(3) 0.117(5) -0.017(4) 0.038(4) 0.001(3) C68 0.104(5) 0.079(4) 0.117(6) -0.025(4) 0.033(5) -0.015(4) C69 0.100(4) 0.100(5) 0.086(4) -0.027(4) 0.014(4) -0.028(4) C70 0.086(4) 0.093(4) 0.061(3) -0.013(3) 0.019(3) -0.012(3) C71 0.122(5) 0.109(5) 0.058(3) -0.003(4) 0.006(3) -0.024(4) C72 0.076(3) 0.071(4) 0.070(3) 0.033(3) -0.001(3) -0.007(3) C73 0.094(4) 0.082(4) 0.063(3) 0.019(3) -0.010(3) -0.012(3) C74 0.085(4) 0.102(5) 0.096(5) 0.017(4) -0.024(3) -0.020(4) C75 0.070(4) 0.105(5) 0.121(6) 0.019(5) -0.021(4) -0.002(4) C76 0.078(4) 0.074(4) 0.101(5) 0.021(4) -0.014(3) 0.002(3) C77 0.080(3) 0.063(4) 0.080(4) 0.030(3) -0.012(3) -0.008(3) C78 0.087(4) 0.056(3) 0.107(5) 0.026(3) -0.006(3) 0.000(3) C79 0.070(3) 0.050(3) 0.082(4) 0.002(3) 0.002(3) -0.012(2) C80 0.070(3) 0.045(3) 0.103(4) 0.001(3) 0.002(3) -0.006(2) C81 0.101(5) 0.074(4) 0.130(7) -0.004(5) 0.008(5) 0.015(4) C82 0.127(6) 0.097(5) 0.123(7) -0.023(5) 0.025(5) 0.025(5) C83 0.123(5) 0.100(5) 0.084(4) -0.024(4) 0.003(4) 0.005(4) C84 0.083(3) 0.065(3) 0.083(4) -0.006(3) 0.001(3) -0.007(3) C85 0.069(3) 0.096(4) 0.078(4) 0.000(3) -0.016(3) 0.002(3) C86 0.047(2) 0.072(3) 0.080(3) 0.016(3) 0.001(2) 0.009(2) C87 0.056(3) 0.077(4) 0.069(3) 0.013(3) -0.004(2) 0.011(2) C88 0.077(3) 0.094(5) 0.067(3) 0.017(3) 0.002(3) 0.005(3) C89 0.082(4) 0.114(6) 0.080(4) 0.025(4) 0.007(3) 0.005(4) C90 0.067(3) 0.069(4) 0.113(5) 0.033(4) -0.007(3) 0.002(3) C91 0.052(2) 0.063(3) 0.092(4) 0.012(3) 0.003(2) 0.018(2) C92 0.066(3) 0.067(4) 0.138(6) 0.001(4) 0.018(3) 0.018(3) N1 0.063(2) 0.048(2) 0.051(2) -0.0001(17) 0.0094(17) -0.0019(16) N2 0.064(2) 0.061(2) 0.0413(18) 0.0100(17) 0.0049(16) 0.0109(18) N3 0.061(2) 0.046(2) 0.0454(19) -0.0082(16) 0.0119(16) 0.0073(15) N4 0.0572(19) 0.047(2) 0.0403(18) -0.0017(15) -0.0011(15) 0.0127(15) N5 0.061(2) 0.048(2) 0.053(2) -0.0058(17) 0.0158(17) 0.0137(16) N6 0.056(2) 0.049(2) 0.062(2) 0.0018(18) 0.0114(18) 0.0057(16) O3 0.149(4) 0.065(2) 0.093(3) 0.011(2) 0.045(3) -0.004(3) O4 0.125(3) 0.061(2) 0.077(2) -0.009(2) 0.026(2) -0.022(2) O6 0.0676(19) 0.070(2) 0.084(3) 0.010(2) 0.0071(18) -0.0066(17) O7 0.076(2) 0.081(3) 0.116(3) 0.002(2) 0.023(2) -0.009(2) O1 0.163(4) 0.058(3) 0.081(3) 0.001(2) 0.036(3) -0.017(3) O2 0.086(2) 0.087(3) 0.077(3) -0.006(2) 0.019(2) -0.005(2) O5 0.068(2) 0.092(3) 0.115(3) 0.006(3) 0.030(2) -0.001(2) O8 0.095(3) 0.080(3) 0.082(3) 0.021(2) 0.016(2) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1' Cd1 0.820(4) . ? Cd1' N1 1.564(6) . ? Cd1' N5 2.341(5) . ? Cd1' N2 2.449(5) . ? Cd1' C34 2.489(6) . ? Cd1' C35 2.554(6) . ? Cd1' N4 2.590(5) . ? Cd1' N3 2.605(5) . ? Cd1 N4 2.319(3) . ? Cd1 N1 2.326(4) . ? Cd1 N6 2.336(4) . ? Cd1 N2 2.349(4) . ? Cd1 N3 2.389(3) . ? Cd1 N5 2.403(3) . ? C1 N6 1.334(6) . ? C1 C2 1.377(8) . ? C1 H1 0.9300 . ? C2 C3 1.344(8) . ? C2 H2 0.9300 . ? C3 C4 1.422(7) . ? C3 H3 0.9300 . ? C4 C12 1.404(7) . ? C4 C5 1.427(7) . ? C5 C6 1.335(8) . ? C5 H5 0.9300 . ? C6 C7 1.427(7) . ? C6 H6 0.9300 . ? C7 C8 1.407(7) . ? C7 C11 1.414(6) . ? C8 C9 1.347(7) . ? C8 H8 0.9300 . ? C9 C10 1.404(7) . ? C9 H70 0.9300 . ? C10 N5 1.305(6) . ? C10 H10 0.9300 . ? C11 N5 1.351(6) . ? C11 C12 1.447(6) . ? C12 N6 1.347(6) . ? C13 N4 1.330(6) . ? C13 C14 1.389(8) . ? C13 H13 0.9300 . ? C14 C15 1.342(8) . ? C14 H14 0.9300 . ? C15 C16 1.406(8) . ? C15 H15 0.9300 . ? C16 C24 1.406(7) . ? C16 C17 1.426(8) . ? C17 C18 1.323(9) . ? C17 H17 0.9300 . ? C18 C19 1.428(8) . ? C18 H18 0.9300 . ? C19 C20 1.396(7) . ? C19 C23 1.409(6) . ? C20 C21 1.347(8) . ? C20 H20 0.9300 . ? C21 C22 1.397(7) . ? C21 H21 0.9300 . ? C22 N3 1.324(6) . ? C22 H22 0.9300 . ? C23 N3 1.350(5) . ? C23 C24 1.437(6) . ? C24 N4 1.355(5) . ? C25 N2 1.323(6) . ? C25 C26 1.394(9) . ? C25 H25 0.9300 . ? C26 C27 1.342(9) . ? C26 H26 0.9300 . ? C27 C28 1.403(8) . ? C27 H27 0.9300 . ? C28 C36 1.416(7) . ? C28 C29 1.425(8) . ? C29 C30 1.349(9) . ? C29 H29 0.9300 . ? C30 C31 1.430(8) . ? C30 H30 0.9300 . ? C31 C35 1.392(7) . ? C31 C32 1.409(7) . ? C32 C33 1.358(8) . ? C32 H32 0.9300 . ? C33 C34 1.382(7) . ? C33 H33 0.9300 . ? C34 N1 1.331(6) . ? C34 H34 0.9300 . ? C35 N1 1.356(6) . ? C35 C36 1.434(6) . ? C36 N2 1.338(6) . ? C37 O3 1.374(7) . ? C37 C38 1.387(9) . ? C37 C42 1.407(9) . ? C38 C39 1.387(9) . ? C38 C64 1.523(10) . ? C39 C40 1.407(11) . ? C39 H39 0.9300 . ? C40 C41 1.373(11) . ? C40 H40 0.9300 . ? C41 C42 1.365(9) . ? C41 H41 0.9300 . ? C42 C43 1.523(10) . ? C43 C45 1.506(10) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 O2 1.330(7) . ? C44 C49 1.394(9) . ? C44 C45 1.406(8) . ? C45 C46 1.397(11) . ? C46 C47 1.377(13) . ? C46 H46 0.9300 . ? C47 C48 1.358(12) . ? C47 H47 0.9300 . ? C48 C49 1.379(10) . ? C48 H48 0.9300 . ? C49 C50 1.505(9) . ? C50 C52 1.495(10) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O1 1.350(7) . ? C51 C52 1.377(10) . ? C51 C56 1.415(9) . ? C52 C53 1.412(10) . ? C53 C54 1.361(12) . ? C53 H53 0.9300 . ? C54 C55 1.351(13) . ? C54 H54 0.9300 . ? C55 C56 1.382(10) . ? C55 H55 0.9300 . ? C56 C57 1.503(11) . ? C57 C59 1.485(11) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 O4 1.352(7) . ? C58 C63 1.373(10) . ? C58 C59 1.408(10) . ? C59 C60 1.374(9) . ? C60 C61 1.355(13) . ? C60 H60 0.9300 . ? C61 C62 1.343(13) . ? C61 H61 0.9300 . ? C62 C63 1.425(10) . ? C62 H62 0.9300 . ? C63 C64 1.515(12) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 O7 1.356(7) . ? C65 C66 1.393(9) . ? C65 C70 1.405(8) . ? C66 C67 1.380(9) . ? C66 C92 1.507(10) . ? C67 C68 1.387(11) . ? C67 H67 0.9300 . ? C68 C69 1.364(11) . ? C68 H68 0.9300 . ? C69 C70 1.387(9) . ? C69 H69 0.9300 . ? C70 C71 1.532(10) . ? C71 C73 1.520(10) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 O8 1.340(7) . ? C72 C77 1.391(9) . ? C72 C73 1.408(8) . ? C73 C74 1.381(9) . ? C74 C75 1.388(11) . ? C74 H74 0.9300 . ? C75 C76 1.369(10) . ? C75 H75 0.9300 . ? C76 C77 1.400(8) . ? C76 H76 0.9300 . ? C77 C78 1.497(9) . ? C78 C80 1.512(10) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 O6 1.341(7) . ? C79 C80 1.400(8) . ? C79 C84 1.413(9) . ? C80 C81 1.372(10) . ? C81 C82 1.362(12) . ? C81 H81 0.9300 . ? C82 C83 1.377(11) . ? C82 H82 0.9300 . ? C83 C84 1.391(9) . ? C83 H83 0.9300 . ? C84 C85 1.509(8) . ? C85 C87 1.522(9) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 O5 1.386(6) . ? C86 C87 1.387(8) . ? C86 C91 1.391(8) . ? C87 C88 1.377(8) . ? C88 C89 1.364(10) . ? C88 H88 0.9300 . ? C89 C90 1.383(10) . ? C89 H89 0.9300 . ? C90 C91 1.401(9) . ? C90 H90 0.9300 . ? C91 C92 1.511(9) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? O4 H4A 0.8200 . ? O6 H6A 0.8200 . ? O7 H7 0.8200 . ? O1 H1A 0.83(2) . ? O2 H2A 0.83(2) . ? O8 H8A 0.814(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cd1 Cd1' N1 153.4(4) . . ? Cd1 Cd1' N5 84.4(3) . . ? N1 Cd1' N5 115.4(2) . . ? Cd1 Cd1' N2 73.4(3) . . ? N1 Cd1' N2 84.0(2) . . ? N5 Cd1' N2 104.47(19) . . ? Cd1 Cd1' C34 163.2(3) . . ? N1 Cd1' C34 28.1(2) . . ? N5 Cd1' C34 108.7(2) . . ? N2 Cd1' C34 112.0(2) . . ? Cd1 Cd1' C35 129.7(3) . . ? N1 Cd1' C35 26.82(19) . . ? N5 Cd1' C35 115.70(19) . . ? N2 Cd1' C35 57.39(16) . . ? C34 Cd1' C35 54.87(18) . . ? Cd1 Cd1' N4 61.9(2) . . ? N1 Cd1' N4 129.9(3) . . ? N5 Cd1' N4 92.66(17) . . ? N2 Cd1' N4 130.0(2) . . ? C34 Cd1' N4 105.84(19) . . ? C35 Cd1' N4 149.0(2) . . ? Cd1 Cd1' N3 65.8(2) . . ? N1 Cd1' N3 96.5(2) . . ? N5 Cd1' N3 148.1(2) . . ? N2 Cd1' N3 78.71(15) . . ? C34 Cd1' N3 98.95(18) . . ? C35 Cd1' N3 93.09(16) . . ? N4 Cd1' N3 63.92(14) . . ? Cd1' Cd1 N4 99.9(3) . . ? Cd1' Cd1 N1 17.5(3) . . ? N4 Cd1 N1 109.28(13) . . ? Cd1' Cd1 N6 146.1(3) . . ? N4 Cd1 N6 95.24(13) . . ? N1 Cd1 N6 151.31(13) . . ? Cd1' Cd1 N2 87.1(3) . . ? N4 Cd1 N2 156.12(12) . . ? N1 Cd1 N2 72.52(13) . . ? N6 Cd1 N2 91.15(14) . . ? Cd1' Cd1 N3 96.0(3) . . ? N4 Cd1 N3 71.46(12) . . ? N1 Cd1 N3 85.05(12) . . ? N6 Cd1 N3 117.69(12) . . ? N2 Cd1 N3 85.19(13) . . ? Cd1' Cd1 N5 75.8(3) . . ? N4 Cd1 N5 98.23(12) . . ? N1 Cd1 N5 89.37(13) . . ? N6 Cd1 N5 72.12(13) . . ? N2 Cd1 N5 105.64(13) . . ? N3 Cd1 N5 165.75(12) . . ? N6 C1 C2 123.1(5) . . ? N6 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.6(5) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 120.5(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C12 C4 C3 117.3(4) . . ? C12 C4 C5 120.0(4) . . ? C3 C4 C5 122.7(5) . . ? C6 C5 C4 121.0(5) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 121.5(5) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C11 117.0(4) . . ? C8 C7 C6 123.7(4) . . ? C11 C7 C6 119.3(4) . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118.5(4) . . ? C8 C9 H70 120.7 . . ? C10 C9 H70 120.7 . . ? N5 C10 C9 122.9(5) . . ? N5 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N5 C11 C7 121.4(4) . . ? N5 C11 C12 119.4(3) . . ? C7 C11 C12 119.2(4) . . ? N6 C12 C4 120.9(4) . . ? N6 C12 C11 120.1(4) . . ? C4 C12 C11 118.9(4) . . ? N4 C13 C14 122.2(4) . . ? N4 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C15 C14 C13 118.8(5) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 121.4(5) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C24 116.5(4) . . ? C15 C16 C17 123.9(5) . . ? C24 C16 C17 119.5(5) . . ? C18 C17 C16 121.2(5) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 121.8(5) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C23 117.9(4) . . ? C20 C19 C18 123.3(4) . . ? C23 C19 C18 118.7(5) . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 119.0(5) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N3 C22 C21 123.2(5) . . ? N3 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? N3 C23 C19 121.8(4) . . ? N3 C23 C24 118.6(3) . . ? C19 C23 C24 119.6(4) . . ? N4 C24 C16 121.5(4) . . ? N4 C24 C23 119.5(4) . . ? C16 C24 C23 119.0(4) . . ? N2 C25 C26 121.9(6) . . ? N2 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 119.2(5) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 120.4(5) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C36 117.2(5) . . ? C27 C28 C29 123.0(5) . . ? C36 C28 C29 119.8(5) . . ? C30 C29 C28 121.0(5) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 120.2(5) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C35 C31 C32 118.4(5) . . ? C35 C31 C30 120.3(5) . . ? C32 C31 C30 121.3(5) . . ? C33 C32 C31 118.9(5) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C34 120.3(5) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? N1 C34 C33 121.6(5) . . ? N1 C34 Cd1' 33.5(2) . . ? C33 C34 Cd1' 155.1(4) . . ? N1 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? Cd1' C34 H34 85.7 . . ? N1 C35 C31 121.1(4) . . ? N1 C35 C36 119.0(4) . . ? C31 C35 C36 119.7(4) . . ? N1 C35 Cd1' 31.4(2) . . ? C31 C35 Cd1' 152.4(4) . . ? C36 C35 Cd1' 87.8(3) . . ? N2 C36 C28 121.0(4) . . ? N2 C36 C35 120.2(4) . . ? C28 C36 C35 118.6(4) . . ? O3 C37 C38 118.6(6) . . ? O3 C37 C42 119.1(6) . . ? C38 C37 C42 122.3(6) . . ? C39 C38 C37 118.5(6) . . ? C39 C38 C64 119.8(7) . . ? C37 C38 C64 121.8(6) . . ? C38 C39 C40 119.3(7) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C41 C40 C39 120.6(6) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C42 C41 C40 121.4(7) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C41 C42 C37 117.8(6) . . ? C41 C42 C43 121.2(7) . . ? C37 C42 C43 121.0(6) . . ? C45 C43 C42 112.5(5) . . ? C45 C43 H43A 109.1 . . ? C42 C43 H43A 109.1 . . ? C45 C43 H43B 109.1 . . ? C42 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? O2 C44 C49 121.1(5) . . ? O2 C44 C45 117.3(6) . . ? C49 C44 C45 121.5(6) . . ? C46 C45 C44 116.8(7) . . ? C46 C45 C43 121.8(7) . . ? C44 C45 C43 121.2(6) . . ? C47 C46 C45 122.3(7) . . ? C47 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C48 C47 C46 118.6(8) . . ? C48 C47 H47 120.7 . . ? C46 C47 H47 120.7 . . ? C47 C48 C49 122.9(8) . . ? C47 C48 H48 118.6 . . ? C49 C48 H48 118.6 . . ? C48 C49 C44 117.8(7) . . ? C48 C49 C50 119.7(7) . . ? C44 C49 C50 122.2(6) . . ? C52 C50 C49 115.6(5) . . ? C52 C50 H50A 108.4 . . ? C49 C50 H50A 108.4 . . ? C52 C50 H50B 108.4 . . ? C49 C50 H50B 108.4 . . ? H50A C50 H50B 107.4 . . ? O1 C51 C52 120.8(6) . . ? O1 C51 C56 118.6(7) . . ? C52 C51 C56 120.7(6) . . ? C51 C52 C53 119.2(7) . . ? C51 C52 C50 119.8(6) . . ? C53 C52 C50 121.0(7) . . ? C54 C53 C52 119.5(8) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C55 C54 C53 120.9(8) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C54 C55 C56 122.4(8) . . ? C54 C55 H55 118.8 . . ? C56 C55 H55 118.8 . . ? C55 C56 C51 117.2(7) . . ? C55 C56 C57 122.0(7) . . ? C51 C56 C57 120.7(6) . . ? C59 C57 C56 114.1(5) . . ? C59 C57 H57A 108.7 . . ? C56 C57 H57A 108.7 . . ? C59 C57 H57B 108.7 . . ? C56 C57 H57B 108.7 . . ? H57A C57 H57B 107.6 . . ? O4 C58 C63 119.7(6) . . ? O4 C58 C59 120.4(7) . . ? C63 C58 C59 119.9(6) . . ? C60 C59 C58 118.9(8) . . ? C60 C59 C57 120.5(7) . . ? C58 C59 C57 120.6(6) . . ? C61 C60 C59 121.9(9) . . ? C61 C60 H60 119.1 . . ? C59 C60 H60 119.1 . . ? C62 C61 C60 119.9(8) . . ? C62 C61 H61 120.1 . . ? C60 C61 H61 120.1 . . ? C61 C62 C63 121.2(9) . . ? C61 C62 H62 119.4 . . ? C63 C62 H62 119.4 . . ? C58 C63 C62 118.2(8) . . ? C58 C63 C64 121.3(6) . . ? C62 C63 C64 120.5(8) . . ? C63 C64 C38 113.4(6) . . ? C63 C64 H64A 108.9 . . ? C38 C64 H64A 108.9 . . ? C63 C64 H64B 108.9 . . ? C38 C64 H64B 108.9 . . ? H64A C64 H64B 107.7 . . ? O7 C65 C66 116.9(5) . . ? O7 C65 C70 122.2(6) . . ? C66 C65 C70 120.9(5) . . ? C67 C66 C65 118.6(6) . . ? C67 C66 C92 121.4(6) . . ? C65 C66 C92 120.0(5) . . ? C66 C67 C68 121.2(7) . . ? C66 C67 H67 119.4 . . ? C68 C67 H67 119.4 . . ? C69 C68 C67 119.5(7) . . ? C69 C68 H68 120.3 . . ? C67 C68 H68 120.3 . . ? C68 C69 C70 121.7(7) . . ? C68 C69 H69 119.1 . . ? C70 C69 H69 119.1 . . ? C69 C70 C65 118.0(7) . . ? C69 C70 C71 122.1(6) . . ? C65 C70 C71 119.9(6) . . ? C73 C71 C70 115.2(5) . . ? C73 C71 H71A 108.5 . . ? C70 C71 H71A 108.5 . . ? C73 C71 H71B 108.5 . . ? C70 C71 H71B 108.5 . . ? H71A C71 H71B 107.5 . . ? O8 C72 C77 118.5(5) . . ? O8 C72 C73 120.9(6) . . ? C77 C72 C73 120.7(5) . . ? C74 C73 C72 118.7(7) . . ? C74 C73 C71 121.3(6) . . ? C72 C73 C71 119.9(6) . . ? C73 C74 C75 121.2(7) . . ? C73 C74 H74 119.4 . . ? C75 C74 H74 119.4 . . ? C76 C75 C74 119.3(6) . . ? C76 C75 H75 120.4 . . ? C74 C75 H75 120.4 . . ? C75 C76 C77 121.6(7) . . ? C75 C76 H76 119.2 . . ? C77 C76 H76 119.2 . . ? C72 C77 C76 118.3(6) . . ? C72 C77 C78 121.0(5) . . ? C76 C77 C78 120.7(6) . . ? C77 C78 C80 114.9(5) . . ? C77 C78 H78A 108.5 . . ? C80 C78 H78A 108.5 . . ? C77 C78 H78B 108.5 . . ? C80 C78 H78B 108.5 . . ? H78A C78 H78B 107.5 . . ? O6 C79 C80 122.8(5) . . ? O6 C79 C84 117.1(5) . . ? C80 C79 C84 120.1(6) . . ? C81 C80 C79 118.9(7) . . ? C81 C80 C78 120.1(6) . . ? C79 C80 C78 121.0(6) . . ? C82 C81 C80 122.1(7) . . ? C82 C81 H81 118.9 . . ? C80 C81 H81 118.9 . . ? C81 C82 C83 119.3(8) . . ? C81 C82 H82 120.4 . . ? C83 C82 H82 120.4 . . ? C82 C83 C84 121.7(8) . . ? C82 C83 H83 119.2 . . ? C84 C83 H83 119.2 . . ? C83 C84 C79 117.9(6) . . ? C83 C84 C85 121.7(6) . . ? C79 C84 C85 120.4(6) . . ? C84 C85 C87 112.0(4) . . ? C84 C85 H85A 109.2 . . ? C87 C85 H85A 109.2 . . ? C84 C85 H85B 109.2 . . ? C87 C85 H85B 109.2 . . ? H85A C85 H85B 107.9 . . ? O5 C86 C87 118.3(5) . . ? O5 C86 C91 119.1(5) . . ? C87 C86 C91 122.6(5) . . ? C88 C87 C86 119.1(6) . . ? C88 C87 C85 118.2(6) . . ? C86 C87 C85 122.7(5) . . ? C89 C88 C87 120.1(6) . . ? C89 C88 H88 120.0 . . ? C87 C88 H88 120.0 . . ? C88 C89 C90 120.7(6) . . ? C88 C89 H89 119.7 . . ? C90 C89 H89 119.7 . . ? C89 C90 C91 121.3(6) . . ? C89 C90 H90 119.4 . . ? C91 C90 H90 119.4 . . ? C86 C91 C90 116.3(6) . . ? C86 C91 C92 122.5(5) . . ? C90 C91 C92 121.1(6) . . ? C66 C92 C91 114.1(4) . . ? C66 C92 H92A 108.7 . . ? C91 C92 H92A 108.7 . . ? C66 C92 H92B 108.7 . . ? C91 C92 H92B 108.7 . . ? H92A C92 H92B 107.6 . . ? C34 N1 C35 119.8(4) . . ? C34 N1 Cd1' 118.4(4) . . ? C35 N1 Cd1' 121.8(4) . . ? C34 N1 Cd1 125.5(3) . . ? C35 N1 Cd1 114.5(3) . . ? Cd1' N1 Cd1 9.08(14) . . ? C25 N2 C36 120.1(4) . . ? C25 N2 Cd1 125.7(4) . . ? C36 N2 Cd1 113.8(3) . . ? C25 N2 Cd1' 145.2(4) . . ? C36 N2 Cd1' 94.5(3) . . ? Cd1 N2 Cd1' 19.54(10) . . ? C22 N3 C23 118.2(4) . . ? C22 N3 Cd1 127.3(3) . . ? C23 N3 Cd1 114.4(3) . . ? C22 N3 Cd1' 121.6(3) . . ? C23 N3 Cd1' 115.7(3) . . ? Cd1 N3 Cd1' 18.25(9) . . ? C13 N4 C24 119.4(4) . . ? C13 N4 Cd1 124.3(3) . . ? C24 N4 Cd1 116.1(3) . . ? C13 N4 Cd1' 122.7(3) . . ? C24 N4 Cd1' 115.9(3) . . ? Cd1 N4 Cd1' 18.17(9) . . ? C10 N5 C11 119.6(4) . . ? C10 N5 Cd1' 107.4(3) . . ? C11 N5 Cd1' 131.4(3) . . ? C10 N5 Cd1 127.1(3) . . ? C11 N5 Cd1 112.7(3) . . ? Cd1' N5 Cd1 19.85(11) . . ? C1 N6 C12 119.5(4) . . ? C1 N6 Cd1 125.6(3) . . ? C12 N6 Cd1 115.0(3) . . ? C58 O4 H4A 109.5 . . ? C79 O6 H6A 109.5 . . ? C65 O7 H7 109.5 . . ? C51 O1 H1A 99(7) . . ? C44 O2 H2A 103(2) . . ? C72 O8 H8A 95.1(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cd1' Cd1 N4 -123.9(8) . . . . ? N5 Cd1' Cd1 N4 96.05(14) . . . . ? N2 Cd1' Cd1 N4 -157.01(13) . . . . ? C34 Cd1' Cd1 N4 -45.8(12) . . . . ? C35 Cd1' Cd1 N4 -145.0(3) . . . . ? N3 Cd1' Cd1 N4 -72.16(13) . . . . ? N5 Cd1' Cd1 N1 -140.0(9) . . . . ? N2 Cd1' Cd1 N1 -33.1(8) . . . . ? C34 Cd1' Cd1 N1 78.1(13) . . . . ? C35 Cd1' Cd1 N1 -21.0(6) . . . . ? N4 Cd1' Cd1 N1 123.9(8) . . . . ? N3 Cd1' Cd1 N1 51.8(8) . . . . ? N1 Cd1' Cd1 N6 120.8(7) . . . . ? N5 Cd1' Cd1 N6 -19.2(5) . . . . ? N2 Cd1' Cd1 N6 87.7(4) . . . . ? C34 Cd1' Cd1 N6 -161.1(8) . . . . ? C35 Cd1' Cd1 N6 99.8(5) . . . . ? N4 Cd1' Cd1 N6 -115.2(4) . . . . ? N3 Cd1' Cd1 N6 172.6(4) . . . . ? N1 Cd1' Cd1 N2 33.1(8) . . . . ? N5 Cd1' Cd1 N2 -106.94(15) . . . . ? C34 Cd1' Cd1 N2 111.2(11) . . . . ? C35 Cd1' Cd1 N2 12.0(3) . . . . ? N4 Cd1' Cd1 N2 157.01(13) . . . . ? N3 Cd1' Cd1 N2 84.85(13) . . . . ? N1 Cd1' Cd1 N3 -51.8(8) . . . . ? N5 Cd1' Cd1 N3 168.21(13) . . . . ? N2 Cd1' Cd1 N3 -84.85(13) . . . . ? C34 Cd1' Cd1 N3 26.3(12) . . . . ? C35 Cd1' Cd1 N3 -72.8(3) . . . . ? N4 Cd1' Cd1 N3 72.16(13) . . . . ? N1 Cd1' Cd1 N5 140.0(9) . . . . ? N2 Cd1' Cd1 N5 106.94(15) . . . . ? C34 Cd1' Cd1 N5 -141.9(12) . . . . ? C35 Cd1' Cd1 N5 119.0(4) . . . . ? N4 Cd1' Cd1 N5 -96.05(14) . . . . ? N3 Cd1' Cd1 N5 -168.21(13) . . . . ? N6 C1 C2 C3 -3.5(8) . . . . ? C1 C2 C3 C4 1.2(8) . . . . ? C2 C3 C4 C12 2.3(8) . . . . ? C2 C3 C4 C5 -178.3(6) . . . . ? C12 C4 C5 C6 -1.7(8) . . . . ? C3 C4 C5 C6 178.9(6) . . . . ? C4 C5 C6 C7 3.7(9) . . . . ? C5 C6 C7 C8 177.4(5) . . . . ? C5 C6 C7 C11 -2.1(8) . . . . ? C11 C7 C8 C9 2.5(7) . . . . ? C6 C7 C8 C9 -177.0(5) . . . . ? C7 C8 C9 C10 -1.1(8) . . . . ? C8 C9 C10 N5 -0.8(8) . . . . ? C8 C7 C11 N5 -2.3(6) . . . . ? C6 C7 C11 N5 177.3(4) . . . . ? C8 C7 C11 C12 178.9(4) . . . . ? C6 C7 C11 C12 -1.5(7) . . . . ? C3 C4 C12 N6 -3.9(7) . . . . ? C5 C4 C12 N6 176.7(5) . . . . ? C3 C4 C12 C11 177.5(4) . . . . ? C5 C4 C12 C11 -1.9(7) . . . . ? N5 C11 C12 N6 6.0(6) . . . . ? C7 C11 C12 N6 -175.2(4) . . . . ? N5 C11 C12 C4 -175.4(4) . . . . ? C7 C11 C12 C4 3.4(6) . . . . ? N4 C13 C14 C15 -0.4(9) . . . . ? C13 C14 C15 C16 1.1(10) . . . . ? C14 C15 C16 C24 0.1(9) . . . . ? C14 C15 C16 C17 178.6(7) . . . . ? C15 C16 C17 C18 179.9(7) . . . . ? C24 C16 C17 C18 -1.7(11) . . . . ? C16 C17 C18 C19 2.6(12) . . . . ? C17 C18 C19 C20 179.5(7) . . . . ? C17 C18 C19 C23 -1.0(10) . . . . ? C23 C19 C20 C21 0.4(8) . . . . ? C18 C19 C20 C21 179.9(6) . . . . ? C19 C20 C21 C22 1.2(8) . . . . ? C20 C21 C22 N3 -1.3(8) . . . . ? C20 C19 C23 N3 -2.2(7) . . . . ? C18 C19 C23 N3 178.3(5) . . . . ? C20 C19 C23 C24 178.1(4) . . . . ? C18 C19 C23 C24 -1.4(7) . . . . ? C15 C16 C24 N4 -2.1(8) . . . . ? C17 C16 C24 N4 179.4(5) . . . . ? C15 C16 C24 C23 177.8(5) . . . . ? C17 C16 C24 C23 -0.8(8) . . . . ? N3 C23 C24 N4 2.4(6) . . . . ? C19 C23 C24 N4 -177.9(4) . . . . ? N3 C23 C24 C16 -177.5(4) . . . . ? C19 C23 C24 C16 2.3(6) . . . . ? N2 C25 C26 C27 4.8(8) . . . . ? C25 C26 C27 C28 -4.0(8) . . . . ? C26 C27 C28 C36 0.4(7) . . . . ? C26 C27 C28 C29 -177.9(5) . . . . ? C27 C28 C29 C30 172.7(5) . . . . ? C36 C28 C29 C30 -5.5(8) . . . . ? C28 C29 C30 C31 0.9(8) . . . . ? C29 C30 C31 C35 4.3(8) . . . . ? C29 C30 C31 C32 -174.8(5) . . . . ? C35 C31 C32 C33 -0.7(7) . . . . ? C30 C31 C32 C33 178.4(5) . . . . ? C31 C32 C33 C34 1.3(8) . . . . ? C32 C33 C34 N1 -1.0(7) . . . . ? C32 C33 C34 Cd1' -0.1(12) . . . . ? Cd1 Cd1' C34 N1 -111.3(12) . . . . ? N5 Cd1' C34 N1 109.1(4) . . . . ? N2 Cd1' C34 N1 -5.7(4) . . . . ? C35 Cd1' C34 N1 0.4(3) . . . . ? N4 Cd1' C34 N1 -152.4(4) . . . . ? N3 Cd1' C34 N1 -87.1(4) . . . . ? Cd1 Cd1' C34 C33 -112.7(13) . . . . ? N1 Cd1' C34 C33 -1.4(8) . . . . ? N5 Cd1' C34 C33 107.8(8) . . . . ? N2 Cd1' C34 C33 -7.1(9) . . . . ? C35 Cd1' C34 C33 -1.0(8) . . . . ? N4 Cd1' C34 C33 -153.8(8) . . . . ? N3 Cd1' C34 C33 -88.5(8) . . . . ? C32 C31 C35 N1 -0.3(6) . . . . ? C30 C31 C35 N1 -179.4(4) . . . . ? C32 C31 C35 C36 174.3(4) . . . . ? C30 C31 C35 C36 -4.8(6) . . . . ? C32 C31 C35 Cd1' -1.8(9) . . . . ? C30 C31 C35 Cd1' 179.0(5) . . . . ? Cd1 Cd1' C35 N1 159.1(6) . . . . ? N5 Cd1' C35 N1 -95.9(4) . . . . ? N2 Cd1' C35 N1 172.9(4) . . . . ? C34 Cd1' C35 N1 -0.4(3) . . . . ? N4 Cd1' C35 N1 58.2(5) . . . . ? N3 Cd1' C35 N1 98.4(4) . . . . ? Cd1 Cd1' C35 C31 161.7(6) . . . . ? N1 Cd1' C35 C31 2.5(6) . . . . ? N5 Cd1' C35 C31 -93.4(7) . . . . ? N2 Cd1' C35 C31 175.4(7) . . . . ? C34 Cd1' C35 C31 2.1(6) . . . . ? N4 Cd1' C35 C31 60.7(8) . . . . ? N3 Cd1' C35 C31 100.9(7) . . . . ? Cd1 Cd1' C35 C36 -15.0(5) . . . . ? N1 Cd1' C35 C36 -174.1(5) . . . . ? N5 Cd1' C35 C36 90.0(3) . . . . ? N2 Cd1' C35 C36 -1.3(2) . . . . ? C34 Cd1' C35 C36 -174.5(3) . . . . ? N4 Cd1' C35 C36 -115.9(4) . . . . ? N3 Cd1' C35 C36 -75.7(3) . . . . ? C27 C28 C36 N2 2.7(6) . . . . ? C29 C28 C36 N2 -179.0(4) . . . . ? C27 C28 C36 C35 -173.5(4) . . . . ? C29 C28 C36 C35 4.8(6) . . . . ? N1 C35 C36 N2 -1.3(6) . . . . ? C31 C35 C36 N2 -176.0(4) . . . . ? Cd1' C35 C36 N2 2.2(4) . . . . ? N1 C35 C36 C28 175.0(4) . . . . ? C31 C35 C36 C28 0.3(6) . . . . ? Cd1' C35 C36 C28 178.5(4) . . . . ? O3 C37 C38 C39 176.8(5) . . . . ? C42 C37 C38 C39 -1.7(8) . . . . ? O3 C37 C38 C64 -5.2(8) . . . . ? C42 C37 C38 C64 176.3(6) . . . . ? C37 C38 C39 C40 -0.8(9) . . . . ? C64 C38 C39 C40 -178.9(7) . . . . ? C38 C39 C40 C41 2.7(10) . . . . ? C39 C40 C41 C42 -1.9(10) . . . . ? C40 C41 C42 C37 -0.6(9) . . . . ? C40 C41 C42 C43 176.1(6) . . . . ? O3 C37 C42 C41 -176.0(5) . . . . ? C38 C37 C42 C41 2.5(8) . . . . ? O3 C37 C42 C43 7.3(8) . . . . ? C38 C37 C42 C43 -174.2(5) . . . . ? C41 C42 C43 C45 -73.7(7) . . . . ? C37 C42 C43 C45 102.8(7) . . . . ? O2 C44 C45 C46 175.9(5) . . . . ? C49 C44 C45 C46 -0.8(8) . . . . ? O2 C44 C45 C43 -9.6(8) . . . . ? C49 C44 C45 C43 173.7(5) . . . . ? C42 C43 C45 C46 96.6(7) . . . . ? C42 C43 C45 C44 -77.6(8) . . . . ? C44 C45 C46 C47 0.2(10) . . . . ? C43 C45 C46 C47 -174.3(7) . . . . ? C45 C46 C47 C48 0.4(11) . . . . ? C46 C47 C48 C49 -0.4(11) . . . . ? C47 C48 C49 C44 -0.1(10) . . . . ? C47 C48 C49 C50 175.2(7) . . . . ? O2 C44 C49 C48 -175.8(5) . . . . ? C45 C44 C49 C48 0.8(8) . . . . ? O2 C44 C49 C50 9.1(8) . . . . ? C45 C44 C49 C50 -174.4(5) . . . . ? C48 C49 C50 C52 -100.1(7) . . . . ? C44 C49 C50 C52 75.0(8) . . . . ? O1 C51 C52 C53 -175.5(5) . . . . ? C56 C51 C52 C53 4.7(8) . . . . ? O1 C51 C52 C50 4.4(8) . . . . ? C56 C51 C52 C50 -175.4(5) . . . . ? C49 C50 C52 C51 -91.6(7) . . . . ? C49 C50 C52 C53 88.3(7) . . . . ? C51 C52 C53 C54 -1.9(8) . . . . ? C50 C52 C53 C54 178.2(5) . . . . ? C52 C53 C54 C55 -1.2(10) . . . . ? C53 C54 C55 C56 1.5(11) . . . . ? C54 C55 C56 C51 1.2(9) . . . . ? C54 C55 C56 C57 178.1(6) . . . . ? O1 C51 C56 C55 175.8(5) . . . . ? C52 C51 C56 C55 -4.3(8) . . . . ? O1 C51 C56 C57 -1.1(8) . . . . ? C52 C51 C56 C57 178.8(5) . . . . ? C55 C56 C57 C59 -82.9(7) . . . . ? C51 C56 C57 C59 93.9(7) . . . . ? O4 C58 C59 C60 178.4(5) . . . . ? C63 C58 C59 C60 -1.8(9) . . . . ? O4 C58 C59 C57 -3.3(9) . . . . ? C63 C58 C59 C57 176.4(6) . . . . ? C56 C57 C59 C60 101.7(7) . . . . ? C56 C57 C59 C58 -76.6(8) . . . . ? C58 C59 C60 C61 -0.2(10) . . . . ? C57 C59 C60 C61 -178.4(7) . . . . ? C59 C60 C61 C62 1.9(11) . . . . ? C60 C61 C62 C63 -1.7(11) . . . . ? O4 C58 C63 C62 -178.2(5) . . . . ? C59 C58 C63 C62 2.0(8) . . . . ? O4 C58 C63 C64 1.8(8) . . . . ? C59 C58 C63 C64 -178.0(6) . . . . ? C61 C62 C63 C58 -0.3(10) . . . . ? C61 C62 C63 C64 179.7(7) . . . . ? C58 C63 C64 C38 73.1(8) . . . . ? C62 C63 C64 C38 -106.9(7) . . . . ? C39 C38 C64 C63 77.9(8) . . . . ? C37 C38 C64 C63 -100.1(8) . . . . ? O7 C65 C66 C67 -175.8(5) . . . . ? C70 C65 C66 C67 3.9(8) . . . . ? O7 C65 C66 C92 4.6(7) . . . . ? C70 C65 C66 C92 -175.8(5) . . . . ? C65 C66 C67 C68 -1.8(9) . . . . ? C92 C66 C67 C68 177.9(6) . . . . ? C66 C67 C68 C69 -0.1(10) . . . . ? C67 C68 C69 C70 -0.1(10) . . . . ? C68 C69 C70 C65 2.1(9) . . . . ? C68 C69 C70 C71 -179.0(6) . . . . ? O7 C65 C70 C69 175.6(5) . . . . ? C66 C65 C70 C69 -4.0(8) . . . . ? O7 C65 C70 C71 -3.2(8) . . . . ? C66 C65 C70 C71 177.1(5) . . . . ? C69 C70 C71 C73 104.3(7) . . . . ? C65 C70 C71 C73 -76.8(7) . . . . ? O8 C72 C73 C74 176.4(5) . . . . ? C77 C72 C73 C74 -3.5(8) . . . . ? O8 C72 C73 C71 -1.2(8) . . . . ? C77 C72 C73 C71 178.9(5) . . . . ? C70 C71 C73 C74 -84.0(7) . . . . ? C70 C71 C73 C72 93.5(7) . . . . ? C72 C73 C74 C75 2.3(9) . . . . ? C71 C73 C74 C75 179.9(6) . . . . ? C73 C74 C75 C76 -0.2(11) . . . . ? C74 C75 C76 C77 -0.8(10) . . . . ? O8 C72 C77 C76 -177.3(5) . . . . ? C73 C72 C77 C76 2.5(8) . . . . ? O8 C72 C77 C78 2.1(8) . . . . ? C73 C72 C77 C78 -178.1(5) . . . . ? C75 C76 C77 C72 -0.4(9) . . . . ? C75 C76 C77 C78 -179.8(6) . . . . ? C72 C77 C78 C80 -93.2(7) . . . . ? C76 C77 C78 C80 86.2(7) . . . . ? O6 C79 C80 C81 -179.2(5) . . . . ? C84 C79 C80 C81 1.1(8) . . . . ? O6 C79 C80 C78 1.9(7) . . . . ? C84 C79 C80 C78 -177.8(5) . . . . ? C77 C78 C80 C81 -102.4(7) . . . . ? C77 C78 C80 C79 76.4(7) . . . . ? C79 C80 C81 C82 -1.3(11) . . . . ? C78 C80 C81 C82 177.6(7) . . . . ? C80 C81 C82 C83 1.0(13) . . . . ? C81 C82 C83 C84 -0.4(13) . . . . ? C82 C83 C84 C79 0.2(11) . . . . ? C82 C83 C84 C85 -176.1(7) . . . . ? O6 C79 C84 C83 179.8(5) . . . . ? C80 C79 C84 C83 -0.5(8) . . . . ? O6 C79 C84 C85 -3.9(7) . . . . ? C80 C79 C84 C85 175.8(5) . . . . ? C83 C84 C85 C87 103.4(7) . . . . ? C79 C84 C85 C87 -72.8(7) . . . . ? O5 C86 C87 C88 -177.5(4) . . . . ? C91 C86 C87 C88 1.3(7) . . . . ? O5 C86 C87 C85 4.6(7) . . . . ? C91 C86 C87 C85 -176.5(5) . . . . ? C84 C85 C87 C88 -74.8(7) . . . . ? C84 C85 C87 C86 103.1(6) . . . . ? C86 C87 C88 C89 0.8(8) . . . . ? C85 C87 C88 C89 178.8(5) . . . . ? C87 C88 C89 C90 -1.9(9) . . . . ? C88 C89 C90 C91 0.8(9) . . . . ? O5 C86 C91 C90 176.6(4) . . . . ? C87 C86 C91 C90 -2.3(7) . . . . ? O5 C86 C91 C92 -6.9(7) . . . . ? C87 C86 C91 C92 174.2(5) . . . . ? C89 C90 C91 C86 1.2(8) . . . . ? C89 C90 C91 C92 -175.3(5) . . . . ? C67 C66 C92 C91 -105.0(6) . . . . ? C65 C66 C92 C91 74.6(7) . . . . ? C86 C91 C92 C66 -103.2(6) . . . . ? C90 C91 C92 C66 73.1(7) . . . . ? C33 C34 N1 C35 0.0(6) . . . . ? Cd1' C34 N1 C35 -179.3(6) . . . . ? C33 C34 N1 Cd1' 179.3(4) . . . . ? C33 C34 N1 Cd1 -174.0(3) . . . . ? Cd1' C34 N1 Cd1 6.71(15) . . . . ? C31 C35 N1 C34 0.7(6) . . . . ? C36 C35 N1 C34 -174.0(4) . . . . ? Cd1' C35 N1 C34 179.3(6) . . . . ? C31 C35 N1 Cd1' -178.6(3) . . . . ? C36 C35 N1 Cd1' 6.7(6) . . . . ? C31 C35 N1 Cd1 175.3(3) . . . . ? C36 C35 N1 Cd1 0.6(5) . . . . ? Cd1' C35 N1 Cd1 -6.10(17) . . . . ? Cd1 Cd1' N1 C34 142.9(8) . . . . ? N5 Cd1' N1 C34 -82.1(4) . . . . ? N2 Cd1' N1 C34 174.6(3) . . . . ? C35 Cd1' N1 C34 -179.3(6) . . . . ? N4 Cd1' N1 C34 35.5(5) . . . . ? N3 Cd1' N1 C34 96.8(3) . . . . ? Cd1 Cd1' N1 C35 -37.7(10) . . . . ? N5 Cd1' N1 C35 97.2(4) . . . . ? N2 Cd1' N1 C35 -6.0(4) . . . . ? C34 Cd1' N1 C35 179.3(6) . . . . ? N4 Cd1' N1 C35 -145.1(3) . . . . ? N3 Cd1' N1 C35 -83.9(4) . . . . ? N5 Cd1' N1 Cd1 134.9(10) . . . . ? N2 Cd1' N1 Cd1 31.7(8) . . . . ? C34 Cd1' N1 Cd1 -142.9(8) . . . . ? C35 Cd1' N1 Cd1 37.7(10) . . . . ? N4 Cd1' N1 Cd1 -107.4(9) . . . . ? N3 Cd1' N1 Cd1 -46.2(8) . . . . ? Cd1' Cd1 N1 C34 -40.6(8) . . . . ? N4 Cd1 N1 C34 19.3(4) . . . . ? N6 Cd1 N1 C34 -127.9(4) . . . . ? N2 Cd1 N1 C34 174.2(4) . . . . ? N3 Cd1 N1 C34 87.7(3) . . . . ? N5 Cd1 N1 C34 -79.2(3) . . . . ? Cd1' Cd1 N1 C35 145.1(9) . . . . ? N4 Cd1 N1 C35 -154.9(3) . . . . ? N6 Cd1 N1 C35 57.9(4) . . . . ? N2 Cd1 N1 C35 0.0(3) . . . . ? N3 Cd1 N1 C35 -86.5(3) . . . . ? N5 Cd1 N1 C35 106.6(3) . . . . ? N4 Cd1 N1 Cd1' 60.0(8) . . . . ? N6 Cd1 N1 Cd1' -87.3(9) . . . . ? N2 Cd1 N1 Cd1' -145.2(8) . . . . ? N3 Cd1 N1 Cd1' 128.3(8) . . . . ? N5 Cd1 N1 Cd1' -38.5(8) . . . . ? C26 C25 N2 C36 -1.7(7) . . . . ? C26 C25 N2 Cd1 170.3(4) . . . . ? C26 C25 N2 Cd1' 172.0(4) . . . . ? C28 C36 N2 C25 -2.0(6) . . . . ? C35 C36 N2 C25 174.1(4) . . . . ? C28 C36 N2 Cd1 -175.0(3) . . . . ? C35 C36 N2 Cd1 1.2(5) . . . . ? C28 C36 N2 Cd1' -178.5(4) . . . . ? C35 C36 N2 Cd1' -2.3(4) . . . . ? Cd1' Cd1 N2 C25 177.0(4) . . . . ? N4 Cd1 N2 C25 -74.8(5) . . . . ? N1 Cd1 N2 C25 -173.1(4) . . . . ? N6 Cd1 N2 C25 30.9(4) . . . . ? N3 Cd1 N2 C25 -86.8(4) . . . . ? N5 Cd1 N2 C25 102.7(4) . . . . ? Cd1' Cd1 N2 C36 -10.5(4) . . . . ? N4 Cd1 N2 C36 97.7(4) . . . . ? N1 Cd1 N2 C36 -0.6(3) . . . . ? N6 Cd1 N2 C36 -156.6(3) . . . . ? N3 Cd1 N2 C36 85.7(3) . . . . ? N5 Cd1 N2 C36 -84.8(3) . . . . ? N4 Cd1 N2 Cd1' 108.2(4) . . . . ? N1 Cd1 N2 Cd1' 9.9(3) . . . . ? N6 Cd1 N2 Cd1' -146.1(3) . . . . ? N3 Cd1 N2 Cd1' 96.2(3) . . . . ? N5 Cd1 N2 Cd1' -74.3(3) . . . . ? Cd1 Cd1' N2 C25 -4.2(6) . . . . ? N1 Cd1' N2 C25 -170.0(6) . . . . ? N5 Cd1' N2 C25 75.2(6) . . . . ? C34 Cd1' N2 C25 -167.3(6) . . . . ? C35 Cd1' N2 C25 -173.3(6) . . . . ? N4 Cd1' N2 C25 -31.0(7) . . . . ? N3 Cd1' N2 C25 -72.1(6) . . . . ? Cd1 Cd1' N2 C36 170.4(3) . . . . ? N1 Cd1' N2 C36 4.6(3) . . . . ? N5 Cd1' N2 C36 -110.2(3) . . . . ? C34 Cd1' N2 C36 7.3(3) . . . . ? C35 Cd1' N2 C36 1.3(2) . . . . ? N4 Cd1' N2 C36 143.6(3) . . . . ? N3 Cd1' N2 C36 102.5(3) . . . . ? N1 Cd1' N2 Cd1 -165.8(4) . . . . ? N5 Cd1' N2 Cd1 79.5(3) . . . . ? C34 Cd1' N2 Cd1 -163.1(3) . . . . ? C35 Cd1' N2 Cd1 -169.0(3) . . . . ? N4 Cd1' N2 Cd1 -26.73(19) . . . . ? N3 Cd1' N2 Cd1 -67.9(2) . . . . ? C21 C22 N3 C23 -0.4(7) . . . . ? C21 C22 N3 Cd1 -176.7(4) . . . . ? C21 C22 N3 Cd1' -155.6(4) . . . . ? C19 C23 N3 C22 2.2(6) . . . . ? C24 C23 N3 C22 -178.1(4) . . . . ? C19 C23 N3 Cd1 178.9(3) . . . . ? C24 C23 N3 Cd1 -1.4(5) . . . . ? C19 C23 N3 Cd1' 158.8(4) . . . . ? C24 C23 N3 Cd1' -21.5(5) . . . . ? Cd1' Cd1 N3 C22 78.1(5) . . . . ? N4 Cd1 N3 C22 176.6(4) . . . . ? N1 Cd1 N3 C22 64.4(4) . . . . ? N6 Cd1 N3 C22 -97.2(4) . . . . ? N2 Cd1 N3 C22 -8.5(4) . . . . ? N5 Cd1 N3 C22 131.6(5) . . . . ? Cd1' Cd1 N3 C23 -98.3(4) . . . . ? N4 Cd1 N3 C23 0.2(3) . . . . ? N1 Cd1 N3 C23 -112.0(3) . . . . ? N6 Cd1 N3 C23 86.4(3) . . . . ? N2 Cd1 N3 C23 175.1(3) . . . . ? N5 Cd1 N3 C23 -44.8(6) . . . . ? N4 Cd1 N3 Cd1' 98.5(3) . . . . ? N1 Cd1 N3 Cd1' -13.7(3) . . . . ? N6 Cd1 N3 Cd1' -175.3(3) . . . . ? N2 Cd1 N3 Cd1' -86.6(3) . . . . ? N5 Cd1 N3 Cd1' 53.5(5) . . . . ? Cd1 Cd1' N3 C22 -114.0(4) . . . . ? N1 Cd1' N3 C22 45.3(4) . . . . ? N5 Cd1' N3 C22 -136.5(4) . . . . ? N2 Cd1' N3 C22 -37.3(4) . . . . ? C34 Cd1' N3 C22 73.5(4) . . . . ? C35 Cd1' N3 C22 18.6(4) . . . . ? N4 Cd1' N3 C22 176.9(4) . . . . ? Cd1 Cd1' N3 C23 90.3(4) . . . . ? N1 Cd1' N3 C23 -110.5(3) . . . . ? N5 Cd1' N3 C23 67.7(5) . . . . ? N2 Cd1' N3 C23 167.0(3) . . . . ? C34 Cd1' N3 C23 -82.3(3) . . . . ? C35 Cd1' N3 C23 -137.2(3) . . . . ? N4 Cd1' N3 C23 21.1(3) . . . . ? N1 Cd1' N3 Cd1 159.3(4) . . . . ? N5 Cd1' N3 Cd1 -22.6(3) . . . . ? N2 Cd1' N3 Cd1 76.7(3) . . . . ? C34 Cd1' N3 Cd1 -172.5(3) . . . . ? C35 Cd1' N3 Cd1 132.6(3) . . . . ? N4 Cd1' N3 Cd1 -69.2(2) . . . . ? C14 C13 N4 C24 -1.5(7) . . . . ? C14 C13 N4 Cd1 -176.0(4) . . . . ? C14 C13 N4 Cd1' 162.2(4) . . . . ? C16 C24 N4 C13 2.8(7) . . . . ? C23 C24 N4 C13 -177.1(4) . . . . ? C16 C24 N4 Cd1 177.7(4) . . . . ? C23 C24 N4 Cd1 -2.1(5) . . . . ? C16 C24 N4 Cd1' -162.0(4) . . . . ? C23 C24 N4 Cd1' 18.1(5) . . . . ? Cd1' Cd1 N4 C13 -91.3(4) . . . . ? N1 Cd1 N4 C13 -106.6(4) . . . . ? N6 Cd1 N4 C13 58.2(4) . . . . ? N2 Cd1 N4 C13 163.1(4) . . . . ? N3 Cd1 N4 C13 175.7(4) . . . . ? N5 Cd1 N4 C13 -14.4(4) . . . . ? Cd1' Cd1 N4 C24 94.0(4) . . . . ? N1 Cd1 N4 C24 78.7(3) . . . . ? N6 Cd1 N4 C24 -116.5(3) . . . . ? N2 Cd1 N4 C24 -11.6(5) . . . . ? N3 Cd1 N4 C24 1.0(3) . . . . ? N5 Cd1 N4 C24 170.9(3) . . . . ? N1 Cd1 N4 Cd1' -15.3(3) . . . . ? N6 Cd1 N4 Cd1' 149.5(3) . . . . ? N2 Cd1 N4 Cd1' -105.6(4) . . . . ? N3 Cd1 N4 Cd1' -93.0(3) . . . . ? N5 Cd1 N4 Cd1' 76.9(3) . . . . ? Cd1 Cd1' N4 C13 100.8(4) . . . . ? N1 Cd1' N4 C13 -108.2(4) . . . . ? N5 Cd1' N4 C13 18.6(4) . . . . ? N2 Cd1' N4 C13 130.1(4) . . . . ? C34 Cd1' N4 C13 -91.7(4) . . . . ? C35 Cd1' N4 C13 -138.2(4) . . . . ? N3 Cd1' N4 C13 176.0(4) . . . . ? Cd1 Cd1' N4 C24 -95.0(4) . . . . ? N1 Cd1' N4 C24 56.1(4) . . . . ? N5 Cd1' N4 C24 -177.1(3) . . . . ? N2 Cd1' N4 C24 -65.7(4) . . . . ? C34 Cd1' N4 C24 72.6(3) . . . . ? C35 Cd1' N4 C24 26.1(6) . . . . ? N3 Cd1' N4 C24 -19.8(3) . . . . ? N1 Cd1' N4 Cd1 151.0(5) . . . . ? N5 Cd1' N4 Cd1 -82.2(3) . . . . ? N2 Cd1' N4 Cd1 29.3(2) . . . . ? C34 Cd1' N4 Cd1 167.5(3) . . . . ? C35 Cd1' N4 Cd1 121.0(5) . . . . ? N3 Cd1' N4 Cd1 75.2(2) . . . . ? C9 C10 N5 C11 1.1(7) . . . . ? C9 C10 N5 Cd1' -166.1(4) . . . . ? C9 C10 N5 Cd1 -169.2(4) . . . . ? C7 C11 N5 C10 0.5(6) . . . . ? C12 C11 N5 C10 179.3(4) . . . . ? C7 C11 N5 Cd1' 164.2(3) . . . . ? C12 C11 N5 Cd1' -17.1(6) . . . . ? C7 C11 N5 Cd1 172.2(3) . . . . ? C12 C11 N5 Cd1 -9.1(5) . . . . ? Cd1 Cd1' N5 C10 -172.7(4) . . . . ? N1 Cd1' N5 C10 25.9(4) . . . . ? N2 Cd1' N5 C10 116.1(3) . . . . ? C34 Cd1' N5 C10 -3.6(4) . . . . ? C35 Cd1' N5 C10 55.7(4) . . . . ? N4 Cd1' N5 C10 -111.3(3) . . . . ? N3 Cd1' N5 C10 -152.1(4) . . . . ? Cd1 Cd1' N5 C11 22.2(5) . . . . ? N1 Cd1' N5 C11 -139.2(4) . . . . ? N2 Cd1' N5 C11 -49.0(4) . . . . ? C34 Cd1' N5 C11 -168.7(4) . . . . ? C35 Cd1' N5 C11 -109.4(4) . . . . ? N4 Cd1' N5 C11 83.6(4) . . . . ? N3 Cd1' N5 C11 42.8(6) . . . . ? N1 Cd1' N5 Cd1 -161.4(4) . . . . ? N2 Cd1' N5 Cd1 -71.2(3) . . . . ? C34 Cd1' N5 Cd1 169.1(4) . . . . ? C35 Cd1' N5 Cd1 -131.6(4) . . . . ? N4 Cd1' N5 Cd1 61.4(2) . . . . ? N3 Cd1' N5 Cd1 20.6(2) . . . . ? Cd1' Cd1 N5 C10 8.7(4) . . . . ? N4 Cd1 N5 C10 -89.5(4) . . . . ? N1 Cd1 N5 C10 19.9(4) . . . . ? N6 Cd1 N5 C10 177.6(4) . . . . ? N2 Cd1 N5 C10 91.5(4) . . . . ? N3 Cd1 N5 C10 -46.9(7) . . . . ? Cd1' Cd1 N5 C11 -162.1(4) . . . . ? N4 Cd1 N5 C11 99.7(3) . . . . ? N1 Cd1 N5 C11 -151.0(3) . . . . ? N6 Cd1 N5 C11 6.8(3) . . . . ? N2 Cd1 N5 C11 -79.3(3) . . . . ? N3 Cd1 N5 C11 142.3(4) . . . . ? N4 Cd1 N5 Cd1' -98.2(3) . . . . ? N1 Cd1 N5 Cd1' 11.2(3) . . . . ? N6 Cd1 N5 Cd1' 168.9(3) . . . . ? N2 Cd1 N5 Cd1' 82.8(3) . . . . ? N3 Cd1 N5 Cd1' -55.6(6) . . . . ? C2 C1 N6 C12 1.9(7) . . . . ? C2 C1 N6 Cd1 -178.4(4) . . . . ? C4 C12 N6 C1 1.9(6) . . . . ? C11 C12 N6 C1 -179.5(4) . . . . ? C4 C12 N6 Cd1 -177.8(3) . . . . ? C11 C12 N6 Cd1 0.8(5) . . . . ? Cd1' Cd1 N6 C1 -164.0(5) . . . . ? N4 Cd1 N6 C1 79.5(4) . . . . ? N1 Cd1 N6 C1 -131.4(4) . . . . ? N2 Cd1 N6 C1 -77.5(4) . . . . ? N3 Cd1 N6 C1 7.7(4) . . . . ? N5 Cd1 N6 C1 176.4(4) . . . . ? Cd1' Cd1 N6 C12 15.7(6) . . . . ? N4 Cd1 N6 C12 -100.9(3) . . . . ? N1 Cd1 N6 C12 48.2(5) . . . . ? N2 Cd1 N6 C12 102.2(3) . . . . ? N3 Cd1 N6 C12 -172.7(3) . . . . ? N5 Cd1 N6 C12 -3.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O3 0.83(2) 2.143(19) 2.920(7) 156(4) . O4 H4A O3 0.82 1.99 2.743(6) 152.8 . O6 H6A O8 0.82 1.78 2.506(6) 146.3 . O1 H1A O2 0.83(2) 1.71(5) 2.487(6) 154(10) . O7 H7 O8 0.82 1.74 2.536(6) 162.8 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 67.04 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.774 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.074 #===== data_3 _database_code_depnum_ccdc_archive 'CCDC 879385' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H70 N6 Ni O8' _chemical_formula_weight 1446.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.277(3) _cell_length_b 22.740(3) _cell_length_c 21.277(3) _cell_angle_alpha 90 _cell_angle_beta 93.441(14) _cell_angle_gamma 90 _cell_volume 7378.2(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8068 _exptl_absorpt_correction_T_max 0.8552 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81601 _diffrn_reflns_av_R_equivalents 0.1928 _diffrn_reflns_av_sigmaI/netI 0.0973 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 66.60 _reflns_number_total 12991 _reflns_number_gt 3864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The low ratio of observed/unique reflections may be attributed to the weak diffraction of the crystals. The alert ADPs may come from a large amount of disorder in the structure. The distances of O3---H3 and O4---H4 were restrained to 0.82+-0.02 \%A. The distance of C40---H40 was restrained to 0.90+-0.01 \%A. The distance of H6A...H50A was restrained to 2.00+-0.01 \%A. The distances of C3...H4 and C24...H3 were restrained to 1.71+-0.01 \%A. The distances of H3...H22B, H1...H3, H4...H8A and H7A...H36A were restrained to 2.02+-0.01 \%A. For all C atoms, SIMU restraint was used to make them behave similar anisotropic displacement parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12991 _refine_ls_number_parameters 922 _refine_ls_number_restraints 610 _refine_ls_R_factor_all 0.2101 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2524 _refine_ls_wR_factor_gt 0.2079 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.61109(8) 0.03165(4) 0.30072(4) 0.1146(5) Uani 1 1 d . . . C1 C 0.3905(6) 0.2763(4) 0.1472(4) 0.149(2) Uani 1 1 d U . . H1A H 0.3822 0.3092 0.1184 0.179 Uiso 1 1 calc R . . H1B H 0.3519 0.2819 0.1812 0.179 Uiso 1 1 calc R . . C2 C 0.3661(5) 0.2197(4) 0.1127(5) 0.136(2) Uani 1 1 d U . . C3 C 0.3754(5) 0.2134(5) 0.0499(5) 0.144(2) Uani 1 1 d DU . . C4 C 0.3589(5) 0.1592(5) 0.0170(4) 0.147(2) Uani 1 1 d U . . C5 C 0.3293(5) 0.1129(4) 0.0537(5) 0.152(3) Uani 1 1 d U . . H5 H 0.3160 0.0771 0.0344 0.182 Uiso 1 1 calc R . . C6 C 0.3196(6) 0.1182(4) 0.1153(5) 0.149(2) Uani 1 1 d U . . H6 H 0.2995 0.0863 0.1376 0.178 Uiso 1 1 calc R . . C7 C 0.3389(5) 0.1707(4) 0.1466(5) 0.145(2) Uani 1 1 d U . . H7 H 0.3339 0.1733 0.1899 0.174 Uiso 1 1 calc R . . C8 C 0.3749(6) 0.1513(5) -0.0507(4) 0.170(3) Uani 1 1 d U . . H8A H 0.3655 0.1886 -0.0721 0.204 Uiso 1 1 calc RD . . H8B H 0.3323 0.1236 -0.0690 0.204 Uiso 1 1 calc R . . C9 C 0.4648(8) 0.1297(6) -0.0623(4) 0.159(3) Uani 1 1 d U . . C10 C 0.5368(7) 0.1692(6) -0.0682(3) 0.142(3) Uani 1 1 d U . . C11 C 0.4827(8) 0.0701(6) -0.0662(4) 0.168(3) Uani 1 1 d U . . H11 H 0.4367 0.0436 -0.0632 0.202 Uiso 1 1 calc R . . C12 C 0.5650(8) 0.0483(5) -0.0744(4) 0.168(3) Uani 1 1 d U . . H12 H 0.5750 0.0080 -0.0760 0.201 Uiso 1 1 calc R . . C13 C 0.6345(7) 0.0888(5) -0.0804(3) 0.159(3) Uani 1 1 d U . . H13 H 0.6904 0.0749 -0.0871 0.191 Uiso 1 1 calc R . . C14 C 0.6204(7) 0.1486(5) -0.0766(3) 0.145(2) Uani 1 1 d U . . C15 C 0.6958(6) 0.1917(5) -0.0817(3) 0.154(3) Uani 1 1 d U . . H15A H 0.7395 0.1744 -0.1073 0.185 Uiso 1 1 calc R . . H15B H 0.6741 0.2271 -0.1027 0.185 Uiso 1 1 calc R . . C16 C 0.7385(6) 0.2079(5) -0.0177(4) 0.141(2) Uani 1 1 d U . . C17 C 0.7065(6) 0.2528(5) 0.0208(4) 0.141(2) Uani 1 1 d U . . C18 C 0.8111(6) 0.1756(5) 0.0056(4) 0.159(3) Uani 1 1 d U . . H18 H 0.8340 0.1464 -0.0192 0.191 Uiso 1 1 calc R . . C19 C 0.8490(6) 0.1863(5) 0.0646(5) 0.178(3) Uani 1 1 d U . . H19 H 0.8953 0.1632 0.0808 0.214 Uiso 1 1 calc R . . C20 C 0.8178(6) 0.2313(5) 0.0991(5) 0.169(3) Uani 1 1 d U . . H20 H 0.8470 0.2400 0.1376 0.203 Uiso 1 1 calc R . . C21 C 0.7459(5) 0.2647(4) 0.0804(4) 0.143(2) Uani 1 1 d U . . C22 C 0.7091(6) 0.3106(4) 0.1222(4) 0.148(2) Uani 1 1 d U . . H22A H 0.7566 0.3262 0.1496 0.177 Uiso 1 1 calc R . . H22B H 0.6863 0.3427 0.0960 0.177 Uiso 1 1 calc RD . . C23 C 0.6395(6) 0.2902(3) 0.1615(4) 0.131(2) Uani 1 1 d U . . C24 C 0.5534(7) 0.2954(3) 0.1388(4) 0.126(2) Uani 1 1 d DU . . C25 C 0.4837(7) 0.2757(3) 0.1735(4) 0.135(2) Uani 1 1 d U . . C26 C 0.5046(8) 0.2530(4) 0.2325(5) 0.152(3) Uani 1 1 d U . . H26 H 0.4598 0.2408 0.2572 0.183 Uiso 1 1 calc R . . C27 C 0.5869(8) 0.2480(4) 0.2548(5) 0.156(3) Uani 1 1 d U . . H27 H 0.5981 0.2317 0.2946 0.187 Uiso 1 1 calc R . . C28 C 0.6556(7) 0.2657(3) 0.2220(4) 0.144(3) Uani 1 1 d U . . H28 H 0.7127 0.2618 0.2392 0.172 Uiso 1 1 calc R . . C29 C 1.0431(9) -0.0597(7) 0.3591(6) 0.255(4) Uani 1 1 d U . . H29A H 1.1011 -0.0773 0.3597 0.306 Uiso 1 1 calc R . . H29B H 1.0451 -0.0296 0.3914 0.306 Uiso 1 1 calc R . . C30 C 1.0267(7) -0.0281(6) 0.2941(5) 0.249(4) Uani 1 1 d GU . . C31 C 0.9767(7) 0.0230(6) 0.2909(5) 0.276(5) Uani 1 1 d GU . . H31 H 0.9526 0.0375 0.3269 0.332 Uiso 1 1 calc R . . C32 C 0.9628(6) 0.0524(4) 0.2339(7) 0.279(5) Uani 1 1 d GU . . H32 H 0.9293 0.0865 0.2317 0.335 Uiso 1 1 calc R . . C33 C 0.9989(7) 0.0306(5) 0.1801(5) 0.277(5) Uani 1 1 d GU . . H33 H 0.9896 0.0503 0.1419 0.333 Uiso 1 1 calc R . . C34 C 1.0489(6) -0.0205(6) 0.1834(5) 0.252(4) Uani 1 1 d GU . . C35 C 1.0628(5) -0.0498(4) 0.2404(7) 0.239(4) Uani 1 1 d GU . . C36 C 1.0831(9) -0.0432(7) 0.1257(6) 0.255(4) Uani 1 1 d U . . H36A H 1.1411 -0.0589 0.1365 0.306 Uiso 1 1 calc RD . . H36B H 1.0906 -0.0101 0.0978 0.306 Uiso 1 1 calc R . . C37 C 0.9782(7) -0.1889(4) 0.0755(6) 0.234(4) Uani 1 1 d GU . . C38 C 1.0311(5) -0.1481(7) 0.1082(4) 0.215(4) Uani 1 1 d GU . . C39 C 1.0321(6) -0.0899(6) 0.0883(5) 0.242(4) Uani 1 1 d GU . . C40 C 0.9802(7) -0.0725(4) 0.0357(6) 0.244(4) Uani 1 1 d GDU . . H40 H 0.9809 -0.0336 0.0223 0.293 Uiso 1 1 calc RD . . C41 C 0.9273(6) -0.1133(6) 0.0029(4) 0.248(4) Uani 1 1 d GU . . H41 H 0.8926 -0.1017 -0.0323 0.298 Uiso 1 1 calc R . . C42 C 0.9263(6) -0.1715(5) 0.0229(5) 0.242(4) Uani 1 1 d GU . . H42 H 0.8909 -0.1989 0.0010 0.290 Uiso 1 1 calc R . . C43 C 0.9700(9) -0.2525(8) 0.0995(7) 0.252(4) Uani 1 1 d U . . H43A H 0.9442 -0.2775 0.0665 0.302 Uiso 1 1 calc R . . H43B H 1.0274 -0.2679 0.1127 0.302 Uiso 1 1 calc R . . C44 C 0.9483(5) -0.2590(4) 0.2139(6) 0.227(4) Uani 1 1 d GU . . C45 C 0.9144(7) -0.2507(4) 0.1525(5) 0.236(4) Uani 1 1 d GU . . C46 C 0.8250(8) -0.2416(4) 0.1404(4) 0.232(4) Uani 1 1 d GU . . H46 H 0.8023 -0.2361 0.0993 0.278 Uiso 1 1 calc R . . C47 C 0.7695(5) -0.2408(4) 0.1899(6) 0.237(4) Uani 1 1 d GU . . H47 H 0.7097 -0.2347 0.1818 0.284 Uiso 1 1 calc R . . C48 C 0.8034(7) -0.2491(4) 0.2513(5) 0.226(4) Uani 1 1 d GU . . H48 H 0.7663 -0.2485 0.2844 0.272 Uiso 1 1 calc R . . C49 C 0.8928(8) -0.2582(4) 0.2634(4) 0.231(4) Uani 1 1 d GU . . C50 C 0.9262(9) -0.2628(6) 0.3303(7) 0.244(4) Uani 1 1 d U . . H50A H 0.9860 -0.2772 0.3316 0.292 Uiso 1 1 calc RD . . H50B H 0.8913 -0.2917 0.3512 0.292 Uiso 1 1 calc R . . C51 C 0.9244(8) -0.2046(4) 0.3674(5) 0.230(4) Uani 1 1 d GU . . C52 C 0.9847(6) -0.1620(7) 0.3521(4) 0.228(4) Uani 1 1 d GU . . C53 C 0.9812(6) -0.1062(6) 0.3784(5) 0.241(4) Uani 1 1 d GU . . C54 C 0.9172(9) -0.0929(4) 0.4200(5) 0.258(5) Uani 1 1 d GU . . H54 H 0.9148 -0.0556 0.4376 0.310 Uiso 1 1 calc R . . C55 C 0.8569(6) -0.1356(7) 0.4353(3) 0.246(5) Uani 1 1 d GU . . H55 H 0.8141 -0.1267 0.4632 0.296 Uiso 1 1 calc R . . C56 C 0.8605(6) -0.1914(5) 0.4090(5) 0.238(4) Uani 1 1 d GU . . H56 H 0.8201 -0.2199 0.4193 0.286 Uiso 1 1 calc R . . C57 C 0.5075(7) 0.1333(4) 0.3585(3) 0.134(2) Uani 1 1 d U . . H57 H 0.5613 0.1498 0.3711 0.161 Uiso 1 1 calc R . . C58 C 0.4288(8) 0.1636(4) 0.3726(4) 0.151(3) Uani 1 1 d U . . H58 H 0.4327 0.1991 0.3943 0.182 Uiso 1 1 calc R . . C59 C 0.3514(8) 0.1419(5) 0.3555(4) 0.170(3) Uani 1 1 d U . . H59 H 0.3010 0.1623 0.3648 0.204 Uiso 1 1 calc R . . C60 C 0.3448(8) 0.0917(5) 0.3251(4) 0.152(3) Uani 1 1 d U . . C61 C 0.4249(7) 0.0595(4) 0.3112(3) 0.129(2) Uani 1 1 d U . . C62 C 0.2638(9) 0.0640(6) 0.3048(5) 0.186(3) Uani 1 1 d U . . H62 H 0.2103 0.0828 0.3089 0.223 Uiso 1 1 calc R . . C63 C 0.2674(9) 0.0139(6) 0.2816(5) 0.184(3) Uani 1 1 d U . . H63 H 0.2124 -0.0026 0.2722 0.221 Uiso 1 1 calc R . . C64 C 0.3369(8) -0.0231(5) 0.2666(4) 0.155(3) Uani 1 1 d U . . C65 C 0.4258(8) 0.0068(5) 0.2830(3) 0.137(3) Uani 1 1 d U . . C66 C 0.3452(10) -0.0731(5) 0.2402(5) 0.182(3) Uani 1 1 d U . . H66 H 0.2928 -0.0910 0.2263 0.218 Uiso 1 1 calc R . . C67 C 0.4187(8) -0.1041(4) 0.2293(3) 0.159(3) Uani 1 1 d U . . H67 H 0.4162 -0.1421 0.2130 0.191 Uiso 1 1 calc R . . C68 C 0.5066(7) -0.0727(3) 0.2456(3) 0.169(3) Uani 1 1 d U . . H68 H 0.5600 -0.0894 0.2367 0.203 Uiso 1 1 calc R . . C69 C 0.5644(4) 0.1110(3) 0.1864(3) 0.0952(17) Uani 1 1 d U . . H69 H 0.5238 0.1291 0.2110 0.114 Uiso 1 1 calc R . . C70 C 0.5718(5) 0.1303(3) 0.1248(3) 0.1068(18) Uani 1 1 d U . . H70 H 0.5372 0.1612 0.1090 0.128 Uiso 1 1 calc R . . C71 C 0.6281(5) 0.1046(3) 0.0886(3) 0.116(2) Uani 1 1 d U . . H71 H 0.6330 0.1170 0.0473 0.139 Uiso 1 1 calc R . . C72 C 0.6796(5) 0.0591(3) 0.1129(3) 0.1115(18) Uani 1 1 d U . . C73 C 0.6701(5) 0.0410(3) 0.1753(3) 0.0997(17) Uani 1 1 d U . . C74 C 0.7405(6) 0.0282(5) 0.0785(4) 0.149(2) Uani 1 1 d U . . H74 H 0.7490 0.0398 0.0374 0.179 Uiso 1 1 calc R . . C75 C 0.7864(6) -0.0170(5) 0.1026(5) 0.164(3) Uani 1 1 d U . . H75 H 0.8248 -0.0368 0.0776 0.197 Uiso 1 1 calc R . . C76 C 0.7781(6) -0.0354(4) 0.1648(5) 0.159(3) Uani 1 1 d U . . C77 C 0.8259(7) -0.0850(5) 0.1961(6) 0.191(3) Uani 1 1 d U . . H77 H 0.8650 -0.1080 0.1751 0.229 Uiso 1 1 calc R . . C78 C 0.8092(8) -0.0950(5) 0.2582(7) 0.204(4) Uani 1 1 d U . . H78 H 0.8422 -0.1239 0.2796 0.245 Uiso 1 1 calc R . . C79 C 0.7475(8) -0.0655(4) 0.2909(6) 0.198(4) Uani 1 1 d U . . H79 H 0.7367 -0.0767 0.3317 0.237 Uiso 1 1 calc R . . C80 C 0.7176(5) -0.0060(3) 0.2022(4) 0.124(2) Uani 1 1 d U . . C81 C 0.7449(6) 0.1329(4) 0.3168(4) 0.146(3) Uani 1 1 d U . . H81 H 0.7323 0.1413 0.2745 0.175 Uiso 1 1 calc R . . C82 C 0.8056(6) 0.1691(4) 0.3524(4) 0.158(3) Uani 1 1 d U . . H82 H 0.8315 0.2013 0.3340 0.190 Uiso 1 1 calc R . . C83 C 0.8245(6) 0.1557(4) 0.4132(4) 0.156(3) Uani 1 1 d U . . H83 H 0.8650 0.1786 0.4366 0.188 Uiso 1 1 calc R . . C84 C 0.7850(6) 0.1083(4) 0.4421(4) 0.144(2) Uani 1 1 d U . . C85 C 0.7249(5) 0.0741(3) 0.4028(3) 0.121(2) Uani 1 1 d U . . C86 C 0.7996(6) 0.0919(4) 0.5058(4) 0.159(3) Uani 1 1 d U . . H86 H 0.8393 0.1135 0.5314 0.191 Uiso 1 1 calc R . . C87 C 0.7589(7) 0.0473(4) 0.5300(4) 0.162(3) Uani 1 1 d U . . H87 H 0.7701 0.0386 0.5725 0.194 Uiso 1 1 calc R . . C88 C 0.6979(6) 0.0116(4) 0.4935(3) 0.143(2) Uani 1 1 d U . . C89 C 0.6821(5) 0.0256(3) 0.4294(3) 0.120(2) Uani 1 1 d U . . C90 C 0.6534(7) -0.0360(4) 0.5147(4) 0.172(3) Uani 1 1 d U . . H90 H 0.6628 -0.0473 0.5566 0.206 Uiso 1 1 calc R . . C91 C 0.5956(7) -0.0674(4) 0.4764(4) 0.170(3) Uani 1 1 d U . . H91 H 0.5653 -0.0994 0.4914 0.203 Uiso 1 1 calc R . . C92 C 0.5842(7) -0.0494(3) 0.4142(3) 0.156(3) Uani 1 1 d U . . H92 H 0.5453 -0.0705 0.3874 0.187 Uiso 1 1 calc R . . N1 N 0.5060(4) 0.0831(2) 0.3282(2) 0.1093(17) Uani 1 1 d . . . N2 N 0.5017(6) -0.0217(2) 0.2724(2) 0.127(2) Uani 1 1 d . . . N3 N 0.6245(4) -0.0051(3) 0.3916(2) 0.129(2) Uani 1 1 d . . . N4 N 0.7065(4) 0.0883(3) 0.3419(3) 0.1155(17) Uani 1 1 d . . . N5 N 0.7030(4) -0.0206(3) 0.2633(3) 0.141(2) Uani 1 1 d . . . N6 N 0.6126(4) 0.0683(2) 0.2107(2) 0.0931(14) Uani 1 1 d . . . O1 O 0.6358(4) 0.2833(3) -0.0015(3) 0.1592(19) Uani 1 1 d . . . H1 H 0.6219 0.3071 0.0251 0.239 Uiso 1 1 calc RD . . O2 O 0.5210(4) 0.2271(4) -0.0653(3) 0.177(2) Uani 1 1 d . . . O5 O 1.0815(5) -0.1693(6) 0.1588(5) 0.290(6) Uani 1 1 d . . . H5A H 1.0713 -0.2044 0.1633 0.435 Uiso 1 1 calc R . . O6 O 1.0505(5) -0.1752(4) 0.3075(5) 0.240(4) Uani 1 1 d . . . H6A H 1.0453 -0.2095 0.2960 0.359 Uiso 1 1 calc RD . . O7 O 1.1105(4) -0.1016(5) 0.2448(4) 0.247(5) Uani 1 1 d . . . H7A H 1.1245 -0.1114 0.2097 0.370 Uiso 1 1 calc RD . . O8 O 1.0385(7) -0.2658(6) 0.2288(6) 0.327(7) Uani 1 1 d . . . O3 O 0.5315(4) 0.3187(3) 0.0803(3) 0.164(2) Uani 1 1 d D . . H3 H 0.5541(9) 0.3524(6) 0.0870(7) 0.245 Uiso 1 1 d D . . O4 O 0.3989(4) 0.2612(3) 0.0151(3) 0.181(2) Uani 1 1 d D . . H4 H 0.428(2) 0.2445(12) -0.0107(8) 0.272 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.1751(10) 0.0799(6) 0.0827(6) 0.0185(5) -0.0435(6) -0.0326(7) C1 0.159(6) 0.115(5) 0.176(6) 0.004(4) 0.033(5) 0.004(5) C2 0.127(5) 0.122(5) 0.163(5) 0.012(5) 0.031(5) 0.006(4) C3 0.128(5) 0.149(6) 0.156(6) 0.025(6) 0.002(5) -0.009(5) C4 0.128(5) 0.168(6) 0.144(5) 0.001(5) -0.006(4) -0.020(5) C5 0.126(5) 0.150(6) 0.178(6) 0.000(6) -0.002(5) -0.026(5) C6 0.143(5) 0.125(5) 0.179(6) 0.010(5) 0.026(5) -0.001(5) C7 0.141(5) 0.122(5) 0.176(6) 0.013(5) 0.047(5) 0.005(5) C8 0.155(6) 0.211(7) 0.141(5) -0.011(5) -0.027(5) -0.036(6) C9 0.164(6) 0.212(7) 0.097(4) -0.008(5) -0.029(4) -0.021(6) C10 0.144(6) 0.209(7) 0.069(4) 0.007(4) -0.019(4) -0.033(6) C11 0.196(7) 0.208(7) 0.098(4) -0.010(5) -0.012(5) -0.027(7) C12 0.207(8) 0.203(8) 0.090(4) -0.004(5) -0.007(5) -0.015(7) C13 0.186(7) 0.212(8) 0.079(4) -0.007(5) -0.003(4) -0.008(6) C14 0.160(6) 0.206(6) 0.066(3) 0.008(4) -0.011(4) -0.019(6) C15 0.160(6) 0.211(7) 0.092(4) 0.015(4) 0.013(4) -0.024(5) C16 0.123(5) 0.197(6) 0.104(4) -0.002(4) 0.010(4) -0.024(5) C17 0.119(5) 0.174(6) 0.128(5) 0.004(5) 0.006(5) -0.009(5) C18 0.119(5) 0.218(7) 0.140(6) -0.032(5) 0.008(5) 0.006(5) C19 0.130(5) 0.225(7) 0.176(6) -0.057(6) -0.018(5) 0.022(5) C20 0.119(5) 0.209(7) 0.175(6) -0.061(5) -0.020(5) 0.016(5) C21 0.112(5) 0.170(6) 0.145(5) -0.024(4) -0.012(4) -0.006(4) C22 0.146(6) 0.144(5) 0.151(6) -0.028(5) -0.005(5) -0.010(5) C23 0.155(6) 0.103(4) 0.134(5) -0.019(4) -0.003(5) 0.003(4) C24 0.164(6) 0.087(4) 0.126(5) 0.001(4) 0.005(5) 0.008(4) C25 0.175(6) 0.084(4) 0.145(5) -0.004(4) 0.019(5) 0.004(4) C26 0.213(7) 0.097(4) 0.148(6) 0.001(4) 0.014(6) -0.006(5) C27 0.220(8) 0.099(5) 0.148(6) 0.002(4) -0.003(6) -0.007(6) C28 0.191(7) 0.097(5) 0.139(6) -0.026(4) -0.026(5) 0.008(5) C29 0.234(8) 0.313(9) 0.202(7) 0.030(7) -0.111(6) -0.058(7) C30 0.235(8) 0.279(9) 0.217(7) 0.039(7) -0.108(6) -0.085(7) C31 0.306(9) 0.260(10) 0.248(9) 0.028(8) -0.103(8) -0.103(8) C32 0.320(10) 0.242(9) 0.263(10) 0.050(8) -0.079(9) -0.113(8) C33 0.287(9) 0.269(10) 0.265(10) 0.077(8) -0.068(8) -0.117(8) C34 0.217(8) 0.287(9) 0.245(8) 0.070(8) -0.053(7) -0.091(7) C35 0.198(8) 0.279(9) 0.229(9) 0.062(8) -0.084(7) -0.109(7) C36 0.208(8) 0.310(10) 0.245(9) 0.066(8) -0.001(7) -0.074(7) C37 0.178(7) 0.305(9) 0.225(8) -0.009(7) 0.071(6) 0.021(7) C38 0.136(6) 0.303(10) 0.213(8) -0.003(8) 0.075(6) 0.006(7) C39 0.175(7) 0.330(9) 0.226(8) 0.032(7) 0.047(6) -0.036(7) C40 0.192(8) 0.330(11) 0.215(8) 0.033(8) 0.056(7) -0.032(8) C41 0.212(8) 0.329(11) 0.211(8) 0.001(8) 0.075(7) -0.001(9) C42 0.202(8) 0.314(10) 0.217(8) -0.024(8) 0.072(7) 0.023(8) C43 0.208(8) 0.281(9) 0.269(9) -0.013(8) 0.039(7) 0.025(8) C44 0.205(8) 0.210(7) 0.268(9) 0.033(8) 0.025(7) 0.037(7) C45 0.208(7) 0.221(7) 0.282(8) 0.008(7) 0.028(7) 0.014(7) C46 0.194(8) 0.216(8) 0.285(9) -0.006(8) 0.020(7) -0.037(8) C47 0.183(8) 0.233(8) 0.296(10) 0.020(8) 0.023(7) -0.054(7) C48 0.183(7) 0.219(7) 0.279(9) 0.059(8) 0.023(7) -0.042(7) C49 0.211(7) 0.208(6) 0.276(8) 0.083(7) 0.017(7) 0.005(7) C50 0.224(7) 0.248(8) 0.258(8) 0.100(7) 0.007(7) 0.017(8) C51 0.207(7) 0.269(8) 0.214(7) 0.118(7) -0.008(6) 0.010(7) C52 0.187(7) 0.280(10) 0.207(8) 0.109(7) -0.062(6) 0.020(8) C53 0.217(7) 0.308(9) 0.185(7) 0.060(7) -0.084(6) -0.020(7) C54 0.256(9) 0.339(10) 0.170(7) 0.046(8) -0.072(7) -0.013(8) C55 0.231(8) 0.331(11) 0.170(7) 0.063(8) -0.044(6) -0.010(9) C56 0.216(8) 0.302(10) 0.192(8) 0.117(7) -0.021(6) -0.003(8) C57 0.190(8) 0.116(6) 0.095(4) 0.018(4) -0.002(5) -0.032(5) C58 0.202(8) 0.136(6) 0.116(5) 0.009(4) 0.005(6) -0.031(6) C59 0.200(7) 0.182(7) 0.128(6) 0.024(5) 0.012(5) -0.029(7) C60 0.179(6) 0.168(6) 0.107(5) 0.031(4) 0.011(5) -0.050(6) C61 0.202(7) 0.120(5) 0.063(3) 0.019(4) -0.011(4) -0.059(5) C62 0.203(7) 0.210(8) 0.146(6) 0.027(6) 0.019(6) -0.045(7) C63 0.226(7) 0.179(8) 0.147(6) 0.021(6) 0.006(6) -0.061(7) C64 0.241(7) 0.131(6) 0.091(4) 0.013(4) -0.018(5) -0.066(6) C65 0.224(7) 0.114(6) 0.071(4) 0.027(4) -0.017(5) -0.070(6) C66 0.296(9) 0.136(7) 0.108(5) 0.026(5) -0.028(6) -0.078(7) C67 0.311(9) 0.082(5) 0.076(4) 0.019(4) -0.051(5) -0.075(5) C68 0.332(10) 0.084(5) 0.083(4) 0.023(4) -0.060(5) -0.075(6) C69 0.121(4) 0.080(4) 0.082(4) 0.010(3) -0.017(3) 0.010(3) C70 0.145(5) 0.095(4) 0.078(4) 0.019(3) -0.015(4) 0.016(4) C71 0.142(5) 0.124(5) 0.081(4) 0.006(4) -0.005(4) 0.013(4) C72 0.112(4) 0.118(4) 0.103(4) -0.016(4) -0.007(4) 0.012(4) C73 0.109(4) 0.093(4) 0.092(4) -0.006(3) -0.030(4) 0.011(4) C74 0.135(5) 0.166(6) 0.145(5) -0.027(5) -0.008(5) 0.021(5) C75 0.128(5) 0.179(6) 0.183(6) -0.067(6) -0.018(5) 0.030(5) C76 0.131(5) 0.152(5) 0.186(6) -0.045(5) -0.069(5) 0.031(4) C77 0.163(6) 0.169(6) 0.230(7) -0.047(6) -0.080(7) 0.059(5) C78 0.198(7) 0.160(6) 0.238(9) -0.012(7) -0.115(7) 0.066(6) C79 0.231(9) 0.127(7) 0.219(9) 0.006(6) -0.112(8) 0.051(6) C80 0.126(5) 0.108(5) 0.131(5) -0.020(4) -0.051(4) 0.021(4) C81 0.165(6) 0.131(6) 0.137(5) 0.039(5) -0.041(5) -0.057(5) C82 0.170(6) 0.139(5) 0.158(6) 0.029(5) -0.042(5) -0.062(5) C83 0.173(6) 0.134(5) 0.154(6) 0.011(5) -0.055(5) -0.051(5) C84 0.175(5) 0.126(5) 0.124(4) 0.012(4) -0.060(4) -0.037(4) C85 0.159(5) 0.100(4) 0.096(4) 0.016(3) -0.052(4) -0.031(4) C86 0.207(6) 0.146(6) 0.115(5) -0.002(4) -0.072(5) -0.033(5) C87 0.226(7) 0.147(6) 0.103(5) 0.009(4) -0.059(5) -0.027(5) C88 0.219(6) 0.122(5) 0.082(4) 0.013(3) -0.050(4) -0.033(4) C89 0.181(5) 0.094(4) 0.079(3) 0.016(3) -0.045(4) -0.031(4) C90 0.276(7) 0.148(6) 0.085(4) 0.029(4) -0.042(5) -0.041(6) C91 0.284(8) 0.126(5) 0.094(4) 0.032(4) -0.036(5) -0.060(5) C92 0.269(8) 0.097(5) 0.093(4) 0.026(4) -0.051(5) -0.061(5) N1 0.166(5) 0.088(4) 0.072(3) 0.006(3) -0.014(3) -0.044(4) N2 0.244(8) 0.062(4) 0.069(3) 0.013(3) -0.037(4) -0.045(4) N3 0.198(6) 0.090(4) 0.094(3) 0.021(3) -0.043(4) -0.057(4) N4 0.145(5) 0.097(4) 0.100(4) 0.025(3) -0.030(3) -0.036(3) N5 0.168(5) 0.102(4) 0.143(5) 0.010(4) -0.079(4) 0.020(4) N6 0.122(4) 0.073(3) 0.080(3) 0.005(3) -0.025(3) -0.006(3) O1 0.164(5) 0.161(5) 0.150(4) 0.019(4) -0.011(4) -0.010(4) O2 0.162(5) 0.190(6) 0.174(5) 0.031(5) -0.032(4) -0.017(5) O5 0.145(6) 0.50(2) 0.227(9) 0.068(10) 0.027(6) 0.052(8) O6 0.160(6) 0.292(10) 0.264(9) 0.108(8) -0.013(6) 0.053(6) O7 0.100(4) 0.321(11) 0.312(10) 0.100(9) -0.041(5) -0.041(5) O8 0.236(10) 0.347(15) 0.396(16) 0.076(12) 0.014(10) 0.154(11) O3 0.151(4) 0.170(5) 0.170(5) 0.050(4) 0.011(4) 0.014(4) O4 0.197(6) 0.176(6) 0.168(5) 0.047(4) -0.008(4) -0.027(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 2.037(7) . ? Ni1 N6 2.090(5) . ? Ni1 N4 2.097(5) . ? Ni1 N1 2.098(7) . ? Ni1 N3 2.105(5) . ? Ni1 N2 2.123(7) . ? C1 C25 1.498(12) . ? C1 C2 1.516(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.359(12) . ? C2 C7 1.405(12) . ? C3 O4 1.376(11) . ? C3 C4 1.432(13) . ? C4 C5 1.402(13) . ? C4 C8 1.485(12) . ? C5 C6 1.332(12) . ? C5 H5 0.9300 . ? C6 C7 1.389(12) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.494(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C11 1.385(14) . ? C9 C10 1.431(14) . ? C10 O2 1.341(12) . ? C10 C14 1.382(13) . ? C11 C12 1.373(13) . ? C11 H11 0.9300 . ? C12 C13 1.416(13) . ? C12 H12 0.9300 . ? C13 C14 1.379(13) . ? C13 H13 0.9300 . ? C14 C15 1.521(13) . ? C15 C16 1.519(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C18 1.396(12) . ? C16 C17 1.414(12) . ? C17 O1 1.347(10) . ? C17 C21 1.398(11) . ? C18 C19 1.373(12) . ? C18 H18 0.9300 . ? C19 C20 1.361(13) . ? C19 H19 0.9300 . ? C20 C21 1.375(12) . ? C20 H20 0.9300 . ? C21 C22 1.503(12) . ? C22 C23 1.466(11) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.378(11) . ? C23 C28 1.412(12) . ? C24 O3 1.376(9) . ? C24 C25 1.405(11) . ? C25 C26 1.378(12) . ? C26 C27 1.321(13) . ? C26 H26 0.9300 . ? C27 C28 1.356(12) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C53 1.492(15) . ? C29 C30 1.565(14) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 C36 1.458(17) . ? C35 O7 1.385(12) . ? C36 C39 1.514(17) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C37 C43 1.540(17) . ? C38 O5 1.372(11) . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C40 H40 0.9300 . ? C41 C42 1.3900 . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C45 1.452(14) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C44 O8 1.404(11) . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C46 H46 0.9300 . ? C47 C48 1.3900 . ? C47 H47 0.9300 . ? C48 C49 1.3900 . ? C48 H48 0.9300 . ? C49 C50 1.488(15) . ? C50 C51 1.541(17) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C52 O6 1.453(11) . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C54 H54 0.9300 . ? C55 C56 1.3900 . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 N1 1.310(9) . ? C57 C58 1.432(12) . ? C57 H57 0.9300 . ? C58 C59 1.312(12) . ? C58 H58 0.9300 . ? C59 C60 1.314(14) . ? C59 H59 0.9300 . ? C60 C62 1.433(14) . ? C60 C61 1.471(13) . ? C61 C65 1.340(12) . ? C61 N1 1.379(10) . ? C62 C63 1.244(15) . ? C62 H62 0.9300 . ? C63 C64 1.408(16) . ? C63 H63 0.9300 . ? C64 C66 1.276(14) . ? C64 C65 1.540(13) . ? C65 N2 1.359(11) . ? C66 C67 1.359(14) . ? C66 H66 0.9300 . ? C67 C68 1.541(13) . ? C67 H67 0.9300 . ? C68 N2 1.297(10) . ? C68 H68 0.9300 . ? C69 N6 1.307(7) . ? C69 C70 1.394(8) . ? C69 H69 0.9300 . ? C70 C71 1.324(9) . ? C70 H70 0.9300 . ? C71 C72 1.379(10) . ? C71 H71 0.9300 . ? C72 C73 1.406(9) . ? C72 C74 1.406(11) . ? C73 N6 1.342(8) . ? C73 C80 1.396(10) . ? C74 C75 1.331(13) . ? C74 H74 0.9300 . ? C75 C76 1.402(14) . ? C75 H75 0.9300 . ? C76 C80 1.421(12) . ? C76 C77 1.479(14) . ? C77 C78 1.380(17) . ? C77 H77 0.9300 . ? C78 C79 1.379(17) . ? C78 H78 0.9300 . ? C79 N5 1.343(10) . ? C79 H79 0.9300 . ? C80 N5 1.373(10) . ? C81 N4 1.301(9) . ? C81 C82 1.424(10) . ? C81 H81 0.9300 . ? C82 C83 1.343(11) . ? C82 H82 0.9300 . ? C83 C84 1.396(11) . ? C83 H83 0.9300 . ? C84 C86 1.410(11) . ? C84 C85 1.432(9) . ? C85 N4 1.349(8) . ? C85 C89 1.418(10) . ? C86 C87 1.312(12) . ? C86 H86 0.9300 . ? C87 C88 1.431(11) . ? C87 H87 0.9300 . ? C88 C90 1.369(11) . ? C88 C89 1.406(9) . ? C89 N3 1.351(8) . ? C90 C91 1.367(11) . ? C90 H90 0.9300 . ? C91 C92 1.386(9) . ? C91 H91 0.9300 . ? C92 N3 1.290(9) . ? C92 H92 0.9300 . ? O1 H1 0.8200 . ? O5 H5A 0.8200 . ? O6 H6A 0.8200 . ? O7 H7A 0.8200 . ? O3 H3 0.848(15) . ? O4 H4 0.82(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ni1 N6 80.1(3) . . ? N5 Ni1 N4 92.5(2) . . ? N6 Ni1 N4 95.3(2) . . ? N5 Ni1 N1 172.3(2) . . ? N6 Ni1 N1 94.8(2) . . ? N4 Ni1 N1 93.8(2) . . ? N5 Ni1 N3 95.5(3) . . ? N6 Ni1 N3 173.8(3) . . ? N4 Ni1 N3 80.4(2) . . ? N1 Ni1 N3 90.0(2) . . ? N5 Ni1 N2 96.0(3) . . ? N6 Ni1 N2 91.12(18) . . ? N4 Ni1 N2 170.1(3) . . ? N1 Ni1 N2 78.2(3) . . ? N3 Ni1 N2 93.7(2) . . ? C25 C1 C2 112.0(7) . . ? C25 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? C25 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C7 118.1(9) . . ? C3 C2 C1 122.0(9) . . ? C7 C2 C1 119.8(9) . . ? C2 C3 O4 119.4(10) . . ? C2 C3 C4 123.2(9) . . ? O4 C3 C4 117.4(9) . . ? C5 C4 C3 115.2(9) . . ? C5 C4 C8 121.9(10) . . ? C3 C4 C8 122.9(10) . . ? C6 C5 C4 122.6(10) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C7 121.1(9) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C2 119.7(9) . . ? C6 C7 H7 120.1 . . ? C2 C7 H7 120.1 . . ? C4 C8 C9 113.9(7) . . ? C4 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? C4 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C11 C9 C10 116.9(12) . . ? C11 C9 C8 121.2(12) . . ? C10 C9 C8 121.8(11) . . ? O2 C10 C14 120.6(10) . . ? O2 C10 C9 118.1(11) . . ? C14 C10 C9 121.3(12) . . ? C12 C11 C9 123.0(13) . . ? C12 C11 H11 118.5 . . ? C9 C11 H11 118.5 . . ? C11 C12 C13 118.3(12) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? C14 C13 C12 121.0(11) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C10 119.4(11) . . ? C13 C14 C15 120.6(11) . . ? C10 C14 C15 120.0(11) . . ? C16 C15 C14 112.2(6) . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C18 C16 C17 118.0(8) . . ? C18 C16 C15 118.7(9) . . ? C17 C16 C15 123.3(9) . . ? O1 C17 C21 120.8(9) . . ? O1 C17 C16 117.8(8) . . ? C21 C17 C16 121.4(9) . . ? C19 C18 C16 120.9(9) . . ? C19 C18 H18 119.5 . . ? C16 C18 H18 119.5 . . ? C20 C19 C18 119.0(10) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 124.0(9) . . ? C19 C20 H20 118.0 . . ? C21 C20 H20 118.0 . . ? C20 C21 C17 116.6(9) . . ? C20 C21 C22 122.3(8) . . ? C17 C21 C22 121.1(9) . . ? C23 C22 C21 115.3(8) . . ? C23 C22 H22A 108.5 . . ? C21 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? C21 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C24 C23 C28 117.6(9) . . ? C24 C23 C22 119.0(9) . . ? C28 C23 C22 123.5(9) . . ? O3 C24 C23 121.6(9) . . ? O3 C24 C25 116.6(8) . . ? C23 C24 C25 121.8(9) . . ? C26 C25 C24 117.1(10) . . ? C26 C25 C1 120.5(9) . . ? C24 C25 C1 122.3(9) . . ? C27 C26 C25 121.6(11) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C26 C27 C28 122.6(11) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C23 119.3(10) . . ? C27 C28 H28 120.4 . . ? C23 C28 H28 120.4 . . ? C53 C29 C30 119.8(7) . . ? C53 C29 H29A 107.4 . . ? C30 C29 H29A 107.4 . . ? C53 C29 H29B 107.4 . . ? C30 C29 H29B 107.4 . . ? H29A C29 H29B 106.9 . . ? C31 C30 C35 120.0 . . ? C31 C30 C29 119.1(12) . . ? C35 C30 C29 120.9(12) . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 C36 121.4(12) . . ? C33 C34 C36 118.6(12) . . ? O7 C35 C34 121.4(12) . . ? O7 C35 C30 118.6(12) . . ? C34 C35 C30 120.0 . . ? C34 C36 C39 119.4(9) . . ? C34 C36 H36A 107.5 . . ? C39 C36 H36A 107.5 . . ? C34 C36 H36B 107.5 . . ? C39 C36 H36B 107.5 . . ? H36A C36 H36B 107.0 . . ? C38 C37 C42 120.0 . . ? C38 C37 C43 121.1(12) . . ? C42 C37 C43 118.7(12) . . ? O5 C38 C39 123.9(13) . . ? O5 C38 C37 116.1(13) . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 C36 121.5(11) . . ? C40 C39 C36 118.3(11) . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C45 C43 C37 107.2(12) . . ? C45 C43 H43A 110.3 . . ? C37 C43 H43A 110.3 . . ? C45 C43 H43B 110.3 . . ? C37 C43 H43B 110.3 . . ? H43A C43 H43B 108.5 . . ? C45 C44 C49 120.0 . . ? C45 C44 O8 122.2(11) . . ? C49 C44 O8 117.8(11) . . ? C44 C45 C46 120.0 . . ? C44 C45 C43 121.6(11) . . ? C46 C45 C43 118.4(11) . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 C47 120.0 . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C44 120.0 . . ? C48 C49 C50 117.6(10) . . ? C44 C49 C50 122.3(10) . . ? C49 C50 C51 114.5(9) . . ? C49 C50 H50A 108.6 . . ? C51 C50 H50A 108.6 . . ? C49 C50 H50B 108.6 . . ? C51 C50 H50B 108.6 . . ? H50A C50 H50B 107.6 . . ? C52 C51 C56 120.0 . . ? C52 C51 C50 116.5(12) . . ? C56 C51 C50 123.1(12) . . ? C51 C52 C53 120.0 . . ? C51 C52 O6 120.3(12) . . ? C53 C52 O6 119.7(12) . . ? C52 C53 C54 120.0 . . ? C52 C53 C29 119.7(13) . . ? C54 C53 C29 120.2(13) . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? N1 C57 C58 122.2(9) . . ? N1 C57 H57 118.9 . . ? C58 C57 H57 118.9 . . ? C59 C58 C57 120.9(11) . . ? C59 C58 H58 119.5 . . ? C57 C58 H58 119.5 . . ? C58 C59 C60 120.3(13) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C59 C60 C62 124.8(14) . . ? C59 C60 C61 119.4(11) . . ? C62 C60 C61 115.8(11) . . ? C65 C61 N1 115.6(10) . . ? C65 C61 C60 124.5(10) . . ? N1 C61 C60 119.9(8) . . ? C63 C62 C60 117.7(15) . . ? C63 C62 H62 121.2 . . ? C60 C62 H62 121.2 . . ? C62 C63 C64 133.6(15) . . ? C62 C63 H63 113.2 . . ? C64 C63 H63 113.2 . . ? C66 C64 C63 136.7(13) . . ? C66 C64 C65 112.6(13) . . ? C63 C64 C65 110.5(10) . . ? C61 C65 N2 122.1(9) . . ? C61 C65 C64 117.7(11) . . ? N2 C65 C64 120.1(9) . . ? C64 C66 C67 129.9(13) . . ? C64 C66 H66 115.0 . . ? C67 C66 H66 115.0 . . ? C66 C67 C68 116.0(9) . . ? C66 C67 H67 122.0 . . ? C68 C67 H67 122.0 . . ? N2 C68 C67 116.2(10) . . ? N2 C68 H68 121.9 . . ? C67 C68 H68 121.9 . . ? N6 C69 C70 122.0(6) . . ? N6 C69 H69 119.0 . . ? C70 C69 H69 119.0 . . ? C71 C70 C69 120.1(6) . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C70 C71 C72 119.2(7) . . ? C70 C71 H71 120.4 . . ? C72 C71 H71 120.4 . . ? C71 C72 C73 119.0(7) . . ? C71 C72 C74 124.0(8) . . ? C73 C72 C74 117.0(8) . . ? N6 C73 C80 117.7(7) . . ? N6 C73 C72 120.2(6) . . ? C80 C73 C72 122.0(8) . . ? C75 C74 C72 122.4(10) . . ? C75 C74 H74 118.8 . . ? C72 C74 H74 118.8 . . ? C74 C75 C76 121.3(9) . . ? C74 C75 H75 119.4 . . ? C76 C75 H75 119.4 . . ? C75 C76 C80 119.1(9) . . ? C75 C76 C77 125.6(11) . . ? C80 C76 C77 115.3(11) . . ? C78 C77 C76 116.3(11) . . ? C78 C77 H77 121.9 . . ? C76 C77 H77 121.9 . . ? C79 C78 C77 125.0(11) . . ? C79 C78 H78 117.5 . . ? C77 C78 H78 117.5 . . ? N5 C79 C78 119.5(12) . . ? N5 C79 H79 120.2 . . ? C78 C79 H79 120.2 . . ? N5 C80 C73 117.5(8) . . ? N5 C80 C76 124.3(8) . . ? C73 C80 C76 118.1(9) . . ? N4 C81 C82 121.9(7) . . ? N4 C81 H81 119.1 . . ? C82 C81 H81 119.1 . . ? C83 C82 C81 118.5(8) . . ? C83 C82 H82 120.8 . . ? C81 C82 H82 120.8 . . ? C82 C83 C84 121.7(7) . . ? C82 C83 H83 119.2 . . ? C84 C83 H83 119.2 . . ? C83 C84 C86 125.4(7) . . ? C83 C84 C85 116.2(7) . . ? C86 C84 C85 118.5(8) . . ? N4 C85 C89 119.7(5) . . ? N4 C85 C84 121.4(6) . . ? C89 C85 C84 118.9(6) . . ? C87 C86 C84 122.1(7) . . ? C87 C86 H86 119.0 . . ? C84 C86 H86 119.0 . . ? C86 C87 C88 122.2(7) . . ? C86 C87 H87 118.9 . . ? C88 C87 H87 118.9 . . ? C90 C88 C89 116.1(7) . . ? C90 C88 C87 126.1(7) . . ? C89 C88 C87 117.8(7) . . ? N3 C89 C88 121.9(6) . . ? N3 C89 C85 117.6(5) . . ? C88 C89 C85 120.5(6) . . ? C91 C90 C88 122.1(7) . . ? C91 C90 H90 118.9 . . ? C88 C90 H90 118.9 . . ? C90 C91 C92 117.1(8) . . ? C90 C91 H91 121.4 . . ? C92 C91 H91 121.4 . . ? N3 C92 C91 123.4(7) . . ? N3 C92 H92 118.3 . . ? C91 C92 H92 118.3 . . ? C57 N1 C61 117.2(8) . . ? C57 N1 Ni1 129.2(6) . . ? C61 N1 Ni1 113.6(6) . . ? C68 N2 C65 124.9(9) . . ? C68 N2 Ni1 124.8(8) . . ? C65 N2 Ni1 110.2(5) . . ? C92 N3 C89 119.4(6) . . ? C92 N3 Ni1 129.1(4) . . ? C89 N3 Ni1 111.5(4) . . ? C81 N4 C85 120.4(6) . . ? C81 N4 Ni1 128.8(5) . . ? C85 N4 Ni1 110.7(4) . . ? C79 N5 C80 119.4(9) . . ? C79 N5 Ni1 127.9(8) . . ? C80 N5 Ni1 112.7(5) . . ? C69 N6 C73 119.5(5) . . ? C69 N6 Ni1 128.4(5) . . ? C73 N6 Ni1 112.0(4) . . ? C17 O1 H1 109.5 . . ? C38 O5 H5A 109.5 . . ? C52 O6 H6A 109.5 . . ? C35 O7 H7A 109.5 . . ? C24 O3 H3 97.0(11) . . ? C3 O4 H4 99.3(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 C1 C2 C3 -91.2(11) . . . . ? C25 C1 C2 C7 84.2(10) . . . . ? C7 C2 C3 O4 177.7(7) . . . . ? C1 C2 C3 O4 -6.9(12) . . . . ? C7 C2 C3 C4 -0.1(13) . . . . ? C1 C2 C3 C4 175.3(8) . . . . ? C2 C3 C4 C5 2.0(13) . . . . ? O4 C3 C4 C5 -175.8(8) . . . . ? C2 C3 C4 C8 -175.7(8) . . . . ? O4 C3 C4 C8 6.4(13) . . . . ? C3 C4 C5 C6 -1.8(13) . . . . ? C8 C4 C5 C6 176.0(8) . . . . ? C4 C5 C6 C7 -0.3(14) . . . . ? C5 C6 C7 C2 2.5(13) . . . . ? C3 C2 C7 C6 -2.2(12) . . . . ? C1 C2 C7 C6 -177.7(8) . . . . ? C5 C4 C8 C9 -87.1(11) . . . . ? C3 C4 C8 C9 90.5(12) . . . . ? C4 C8 C9 C11 90.8(11) . . . . ? C4 C8 C9 C10 -87.7(11) . . . . ? C11 C9 C10 O2 179.2(7) . . . . ? C8 C9 C10 O2 -2.3(11) . . . . ? C11 C9 C10 C14 -0.9(10) . . . . ? C8 C9 C10 C14 177.6(7) . . . . ? C10 C9 C11 C12 1.1(12) . . . . ? C8 C9 C11 C12 -177.5(8) . . . . ? C9 C11 C12 C13 -1.4(13) . . . . ? C11 C12 C13 C14 1.6(12) . . . . ? C12 C13 C14 C10 -1.5(11) . . . . ? C12 C13 C14 C15 178.6(6) . . . . ? O2 C10 C14 C13 -179.0(7) . . . . ? C9 C10 C14 C13 1.1(10) . . . . ? O2 C10 C14 C15 0.9(10) . . . . ? C9 C10 C14 C15 -179.0(6) . . . . ? C13 C14 C15 C16 -92.8(10) . . . . ? C10 C14 C15 C16 87.4(10) . . . . ? C14 C15 C16 C18 93.0(11) . . . . ? C14 C15 C16 C17 -84.6(12) . . . . ? C18 C16 C17 O1 -179.2(8) . . . . ? C15 C16 C17 O1 -1.5(13) . . . . ? C18 C16 C17 C21 -0.2(13) . . . . ? C15 C16 C17 C21 177.5(8) . . . . ? C17 C16 C18 C19 1.4(14) . . . . ? C15 C16 C18 C19 -176.4(9) . . . . ? C16 C18 C19 C20 -3.6(17) . . . . ? C18 C19 C20 C21 4.8(18) . . . . ? C19 C20 C21 C17 -3.6(16) . . . . ? C19 C20 C21 C22 174.8(10) . . . . ? O1 C17 C21 C20 -179.8(9) . . . . ? C16 C17 C21 C20 1.1(13) . . . . ? O1 C17 C21 C22 1.8(13) . . . . ? C16 C17 C21 C22 -177.2(8) . . . . ? C20 C21 C22 C23 -92.1(11) . . . . ? C17 C21 C22 C23 86.2(11) . . . . ? C21 C22 C23 C24 -92.1(9) . . . . ? C21 C22 C23 C28 88.4(10) . . . . ? C28 C23 C24 O3 -179.9(6) . . . . ? C22 C23 C24 O3 0.5(11) . . . . ? C28 C23 C24 C25 -1.7(11) . . . . ? C22 C23 C24 C25 178.8(7) . . . . ? O3 C24 C25 C26 -179.2(7) . . . . ? C23 C24 C25 C26 2.5(11) . . . . ? O3 C24 C25 C1 3.7(11) . . . . ? C23 C24 C25 C1 -174.6(7) . . . . ? C2 C1 C25 C26 -87.9(10) . . . . ? C2 C1 C25 C24 89.2(9) . . . . ? C24 C25 C26 C27 -2.2(12) . . . . ? C1 C25 C26 C27 174.9(8) . . . . ? C25 C26 C27 C28 1.2(14) . . . . ? C26 C27 C28 C23 -0.3(13) . . . . ? C24 C23 C28 C27 0.6(11) . . . . ? C22 C23 C28 C27 -179.9(8) . . . . ? C53 C29 C30 C31 90.6(15) . . . . ? C53 C29 C30 C35 -90.7(15) . . . . ? C35 C30 C31 C32 0.0 . . . . ? C29 C30 C31 C32 178.8(8) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C32 C33 C34 C36 177.8(9) . . . . ? C33 C34 C35 O7 178.4(8) . . . . ? C36 C34 C35 O7 0.6(9) . . . . ? C33 C34 C35 C30 0.0 . . . . ? C36 C34 C35 C30 -177.8(10) . . . . ? C31 C30 C35 O7 -178.4(8) . . . . ? C29 C30 C35 O7 2.8(9) . . . . ? C31 C30 C35 C34 0.0 . . . . ? C29 C30 C35 C34 -178.8(8) . . . . ? C35 C34 C36 C39 83.3(13) . . . . ? C33 C34 C36 C39 -94.5(13) . . . . ? C42 C37 C38 O5 -178.7(7) . . . . ? C43 C37 C38 O5 6.3(10) . . . . ? C42 C37 C38 C39 0.0 . . . . ? C43 C37 C38 C39 -175.0(9) . . . . ? O5 C38 C39 C40 178.6(8) . . . . ? C37 C38 C39 C40 0.0 . . . . ? O5 C38 C39 C36 -6.5(11) . . . . ? C37 C38 C39 C36 175.0(10) . . . . ? C34 C36 C39 C38 -75.4(15) . . . . ? C34 C36 C39 C40 99.6(11) . . . . ? C38 C39 C40 C41 0.0 . . . . ? C36 C39 C40 C41 -175.1(9) . . . . ? C39 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C37 0.0 . . . . ? C38 C37 C42 C41 0.0 . . . . ? C43 C37 C42 C41 175.1(9) . . . . ? C38 C37 C43 C45 75.2(13) . . . . ? C42 C37 C43 C45 -99.9(12) . . . . ? C49 C44 C45 C46 0.0 . . . . ? O8 C44 C45 C46 -177.2(11) . . . . ? C49 C44 C45 C43 -178.8(12) . . . . ? O8 C44 C45 C43 4.1(14) . . . . ? C37 C43 C45 C44 -108.0(12) . . . . ? C37 C43 C45 C46 73.2(13) . . . . ? C44 C45 C46 C47 0.0 . . . . ? C43 C45 C46 C47 178.8(11) . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C44 0.0 . . . . ? C47 C48 C49 C50 176.0(10) . . . . ? C45 C44 C49 C48 0.0 . . . . ? O8 C44 C49 C48 177.3(11) . . . . ? C45 C44 C49 C50 -175.8(10) . . . . ? O8 C44 C49 C50 1.5(12) . . . . ? C48 C49 C50 C51 -70.2(12) . . . . ? C44 C49 C50 C51 105.7(12) . . . . ? C49 C50 C51 C52 -71.0(12) . . . . ? C49 C50 C51 C56 101.7(10) . . . . ? C56 C51 C52 C53 0.0 . . . . ? C50 C51 C52 C53 173.0(8) . . . . ? C56 C51 C52 O6 -178.6(7) . . . . ? C50 C51 C52 O6 -5.6(8) . . . . ? C51 C52 C53 C54 0.0 . . . . ? O6 C52 C53 C54 178.6(7) . . . . ? C51 C52 C53 C29 -176.8(7) . . . . ? O6 C52 C53 C29 1.8(8) . . . . ? C30 C29 C53 C52 76.7(15) . . . . ? C30 C29 C53 C54 -100.1(14) . . . . ? C52 C53 C54 C55 0.0 . . . . ? C29 C53 C54 C55 176.8(7) . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? C50 C51 C56 C55 -172.5(9) . . . . ? N1 C57 C58 C59 -0.2(12) . . . . ? C57 C58 C59 C60 0.4(14) . . . . ? C58 C59 C60 C62 179.4(8) . . . . ? C58 C59 C60 C61 0.8(13) . . . . ? C59 C60 C61 C65 177.0(7) . . . . ? C62 C60 C61 C65 -1.7(11) . . . . ? C59 C60 C61 N1 -2.2(11) . . . . ? C62 C60 C61 N1 179.1(6) . . . . ? C59 C60 C62 C63 -173.6(10) . . . . ? C61 C60 C62 C63 5.0(13) . . . . ? C60 C62 C63 C64 -4.2(19) . . . . ? C62 C63 C64 C66 -175.7(12) . . . . ? C62 C63 C64 C65 -0.2(17) . . . . ? N1 C61 C65 N2 0.6(9) . . . . ? C60 C61 C65 N2 -178.7(7) . . . . ? N1 C61 C65 C64 176.6(5) . . . . ? C60 C61 C65 C64 -2.7(10) . . . . ? C66 C64 C65 C61 -179.7(7) . . . . ? C63 C64 C65 C61 3.7(10) . . . . ? C66 C64 C65 N2 -3.6(10) . . . . ? C63 C64 C65 N2 179.7(7) . . . . ? C63 C64 C66 C67 -179.3(10) . . . . ? C65 C64 C66 C67 5.2(14) . . . . ? C64 C66 C67 C68 -6.1(15) . . . . ? C66 C67 C68 N2 5.1(10) . . . . ? N6 C69 C70 C71 1.0(9) . . . . ? C69 C70 C71 C72 -0.6(10) . . . . ? C70 C71 C72 C73 0.6(10) . . . . ? C70 C71 C72 C74 179.0(7) . . . . ? C71 C72 C73 N6 -1.0(9) . . . . ? C74 C72 C73 N6 -179.5(6) . . . . ? C71 C72 C73 C80 177.6(6) . . . . ? C74 C72 C73 C80 -0.9(9) . . . . ? C71 C72 C74 C75 -177.1(8) . . . . ? C73 C72 C74 C75 1.3(12) . . . . ? C72 C74 C75 C76 -1.8(14) . . . . ? C74 C75 C76 C80 1.7(13) . . . . ? C74 C75 C76 C77 180.0(9) . . . . ? C75 C76 C77 C78 178.8(10) . . . . ? C80 C76 C77 C78 -2.8(13) . . . . ? C76 C77 C78 C79 5.1(18) . . . . ? C77 C78 C79 N5 -4.9(18) . . . . ? N6 C73 C80 N5 -0.8(9) . . . . ? C72 C73 C80 N5 -179.4(6) . . . . ? N6 C73 C80 C76 179.5(6) . . . . ? C72 C73 C80 C76 0.9(10) . . . . ? C75 C76 C80 N5 179.1(7) . . . . ? C77 C76 C80 N5 0.6(11) . . . . ? C75 C76 C80 C73 -1.2(11) . . . . ? C77 C76 C80 C73 -179.7(7) . . . . ? N4 C81 C82 C83 1.4(15) . . . . ? C81 C82 C83 C84 -1.3(16) . . . . ? C82 C83 C84 C86 -178.6(10) . . . . ? C82 C83 C84 C85 1.5(15) . . . . ? C83 C84 C85 N4 -1.6(13) . . . . ? C86 C84 C85 N4 178.4(8) . . . . ? C83 C84 C85 C89 -179.6(8) . . . . ? C86 C84 C85 C89 0.5(13) . . . . ? C83 C84 C86 C87 178.9(10) . . . . ? C85 C84 C86 C87 -1.2(15) . . . . ? C84 C86 C87 C88 1.0(17) . . . . ? C86 C87 C88 C90 179.3(11) . . . . ? C86 C87 C88 C89 0.0(15) . . . . ? C90 C88 C89 N3 1.7(13) . . . . ? C87 C88 C89 N3 -178.9(8) . . . . ? C90 C88 C89 C85 179.9(9) . . . . ? C87 C88 C89 C85 -0.7(13) . . . . ? N4 C85 C89 N3 0.8(12) . . . . ? C84 C85 C89 N3 178.7(8) . . . . ? N4 C85 C89 C88 -177.5(8) . . . . ? C84 C85 C89 C88 0.4(12) . . . . ? C89 C88 C90 C91 -1.2(16) . . . . ? C87 C88 C90 C91 179.4(10) . . . . ? C88 C90 C91 C92 0.6(17) . . . . ? C90 C91 C92 N3 -0.4(16) . . . . ? C58 C57 N1 C61 -1.2(9) . . . . ? C58 C57 N1 Ni1 178.7(5) . . . . ? C65 C61 N1 C57 -177.0(6) . . . . ? C60 C61 N1 C57 2.3(8) . . . . ? C65 C61 N1 Ni1 3.1(6) . . . . ? C60 C61 N1 Ni1 -177.6(5) . . . . ? N5 Ni1 N1 C57 -142.0(18) . . . . ? N6 Ni1 N1 C57 -93.6(5) . . . . ? N4 Ni1 N1 C57 2.0(5) . . . . ? N3 Ni1 N1 C57 82.4(5) . . . . ? N2 Ni1 N1 C57 176.2(6) . . . . ? N5 Ni1 N1 C61 38(2) . . . . ? N6 Ni1 N1 C61 86.3(4) . . . . ? N4 Ni1 N1 C61 -178.1(4) . . . . ? N3 Ni1 N1 C61 -97.7(4) . . . . ? N2 Ni1 N1 C61 -3.9(4) . . . . ? C67 C68 N2 C65 -4.5(9) . . . . ? C67 C68 N2 Ni1 179.6(4) . . . . ? C61 C65 N2 C68 179.8(6) . . . . ? C64 C65 N2 C68 3.9(10) . . . . ? C61 C65 N2 Ni1 -3.8(8) . . . . ? C64 C65 N2 Ni1 -179.7(4) . . . . ? N5 Ni1 N2 C68 5.5(5) . . . . ? N6 Ni1 N2 C68 85.7(5) . . . . ? N4 Ni1 N2 C68 -144.0(13) . . . . ? N1 Ni1 N2 C68 -179.6(5) . . . . ? N3 Ni1 N2 C68 -90.5(5) . . . . ? N5 Ni1 N2 C65 -170.9(5) . . . . ? N6 Ni1 N2 C65 -90.8(5) . . . . ? N4 Ni1 N2 C65 39.6(15) . . . . ? N1 Ni1 N2 C65 3.9(4) . . . . ? N3 Ni1 N2 C65 93.1(5) . . . . ? C91 C92 N3 C89 0.9(15) . . . . ? C91 C92 N3 Ni1 -176.3(8) . . . . ? C88 C89 N3 C92 -1.6(13) . . . . ? C85 C89 N3 C92 -179.8(8) . . . . ? C88 C89 N3 Ni1 176.1(7) . . . . ? C85 C89 N3 Ni1 -2.2(9) . . . . ? N5 Ni1 N3 C92 -88.9(8) . . . . ? N6 Ni1 N3 C92 -134.0(19) . . . . ? N4 Ni1 N3 C92 179.5(8) . . . . ? N1 Ni1 N3 C92 85.7(8) . . . . ? N2 Ni1 N3 C92 7.5(9) . . . . ? N5 Ni1 N3 C89 93.7(6) . . . . ? N6 Ni1 N3 C89 49(2) . . . . ? N4 Ni1 N3 C89 2.1(6) . . . . ? N1 Ni1 N3 C89 -91.7(6) . . . . ? N2 Ni1 N3 C89 -169.8(6) . . . . ? C82 C81 N4 C85 -1.6(14) . . . . ? C82 C81 N4 Ni1 176.7(7) . . . . ? C89 C85 N4 C81 179.7(8) . . . . ? C84 C85 N4 C81 1.7(12) . . . . ? C89 C85 N4 Ni1 1.1(9) . . . . ? C84 C85 N4 Ni1 -176.8(7) . . . . ? N5 Ni1 N4 C81 84.7(8) . . . . ? N6 Ni1 N4 C81 4.4(8) . . . . ? N1 Ni1 N4 C81 -90.8(8) . . . . ? N3 Ni1 N4 C81 179.9(8) . . . . ? N2 Ni1 N4 C81 -125.6(13) . . . . ? N5 Ni1 N4 C85 -96.9(5) . . . . ? N6 Ni1 N4 C85 -177.2(5) . . . . ? N1 Ni1 N4 C85 87.6(5) . . . . ? N3 Ni1 N4 C85 -1.7(5) . . . . ? N2 Ni1 N4 C85 52.8(16) . . . . ? C78 C79 N5 C80 2.2(13) . . . . ? C78 C79 N5 Ni1 -178.4(7) . . . . ? C73 C80 N5 C79 -180.0(7) . . . . ? C76 C80 N5 C79 -0.3(11) . . . . ? C73 C80 N5 Ni1 0.5(8) . . . . ? C76 C80 N5 Ni1 -179.8(6) . . . . ? N6 Ni1 N5 C79 -179.6(7) . . . . ? N4 Ni1 N5 C79 85.5(7) . . . . ? N1 Ni1 N5 C79 -130.5(17) . . . . ? N3 Ni1 N5 C79 4.8(7) . . . . ? N2 Ni1 N5 C79 -89.5(7) . . . . ? N6 Ni1 N5 C80 -0.1(5) . . . . ? N4 Ni1 N5 C80 -95.1(5) . . . . ? N1 Ni1 N5 C80 49(2) . . . . ? N3 Ni1 N5 C80 -175.7(5) . . . . ? N2 Ni1 N5 C80 89.9(5) . . . . ? C70 C69 N6 C73 -1.3(8) . . . . ? C70 C69 N6 Ni1 -178.9(4) . . . . ? C80 C73 N6 C69 -177.3(5) . . . . ? C72 C73 N6 C69 1.3(8) . . . . ? C80 C73 N6 Ni1 0.6(6) . . . . ? C72 C73 N6 Ni1 179.3(5) . . . . ? N5 Ni1 N6 C69 177.5(5) . . . . ? N4 Ni1 N6 C69 -90.9(5) . . . . ? N1 Ni1 N6 C69 3.3(5) . . . . ? N3 Ni1 N6 C69 -137(2) . . . . ? N2 Ni1 N6 C69 81.5(5) . . . . ? N5 Ni1 N6 C73 -0.2(4) . . . . ? N4 Ni1 N6 C73 91.4(4) . . . . ? N1 Ni1 N6 C73 -174.4(4) . . . . ? N3 Ni1 N6 C73 45(2) . . . . ? N2 Ni1 N6 C73 -96.2(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O3 0.82 1.88 2.559(9) 138.9 . O6 H6A O8 0.82 1.92 2.656(18) 149.1 . O7 H7A O5 0.82 1.80 2.413(16) 129.8 . O5 H5A O8 0.82 2.06 2.754(17) 142.8 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 66.60 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.405 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.051 #===== data_4 _database_code_depnum_ccdc_archive 'CCDC 879386' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H94 Co N6 O12' _chemical_formula_weight 1870.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 _symmetry_space_group_name_Hall 'R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 17.1320(4) _cell_length_b 17.1320(4) _cell_length_c 29.2524(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 7435.5(3) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2937 _exptl_absorpt_coefficient_mu 0.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11416 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 29.26 _reflns_number_total 6097 _reflns_number_gt 3525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distances of O1---H1A, O2---H2A, O3---H3A and O4---H4A were refined isotropically with restraints of O---H = 0.82+-0.02 \%A. The distances of H3A...H26B, H4...H1A and H4...H33A were restrained to 2.05+-0.01 \%A. The distance of C25...H3A was restrained to 1.72+-0.01 \%A For C21, C22, C23, C39 and C40 atoms, some anisotropic displacement ellipsoids were rather elongated which led us to use the SIMU/DELU restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1233P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.18(3) _refine_ls_number_reflns 6097 _refine_ls_number_parameters 431 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1256 _refine_ls_R_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.2411 _refine_ls_wR_factor_gt 0.2323 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.197 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 1.0000 1.06777(4) 0.0500(4) Uani 1 3 d S . . C1 C 0.0997(5) 1.1448(5) 1.1461(2) 0.0668(17) Uani 1 1 d . . . H1 H 0.0440 1.1199 1.1606 0.080 Uiso 1 1 calc R . . C2 C 0.1725(7) 1.2178(6) 1.1668(3) 0.079(2) Uani 1 1 d . . . H2 H 0.1669 1.2424 1.1941 0.095 Uiso 1 1 calc R . . C3 C 0.2518(7) 1.2508(6) 1.1445(3) 0.087(2) Uani 1 1 d . . . H3 H 0.3014 1.3002 1.1576 0.104 Uiso 1 1 calc R . . C4 C 0.2664(5) 1.2182(5) 1.1044(3) 0.0666(17) Uani 1 1 d . . . C5 C 0.3460(6) 1.2518(7) 1.0789(4) 0.101(3) Uani 1 1 d . . . H5 H 0.3957 1.3047 1.0892 0.122 Uiso 1 1 calc R . . C6 C 0.3569(5) 1.2136(6) 1.0402(3) 0.088(2) Uani 1 1 d . . . H6 H 0.4124 1.2366 1.0257 0.105 Uiso 1 1 calc R . . C7 C 0.2793(4) 1.1378(5) 1.0235(2) 0.0623(16) Uani 1 1 d . . . C8 C 0.2820(7) 1.0894(7) 0.9841(3) 0.099(3) Uani 1 1 d . . . H8 H 0.3357 1.1086 0.9684 0.119 Uiso 1 1 calc R . . C9 C 0.2034(6) 1.0134(6) 0.9696(3) 0.076(2) Uani 1 1 d . . . H9 H 0.2038 0.9800 0.9447 0.092 Uiso 1 1 calc R . . C10 C 0.1263(6) 0.9897(5) 0.9928(2) 0.074(2) Uani 1 1 d . . . H10 H 0.0739 0.9400 0.9821 0.088 Uiso 1 1 calc R . . C11 C 0.1952(4) 1.0994(4) 1.0453(2) 0.0569(15) Uani 1 1 d . . . C12 C 0.1874(5) 1.1430(4) 1.0866(2) 0.0561(14) Uani 1 1 d . . . C13 C 0.2869(7) 0.8299(6) 0.9870(2) 0.083(2) Uani 1 1 d . . . C14 C 0.1952(6) 0.7900(5) 0.9878(3) 0.079(2) Uani 1 1 d . . . C15 C 0.1522(8) 0.7982(8) 1.0259(4) 0.111(3) Uani 1 1 d . . . H15 H 0.0895 0.7690 1.0262 0.133 Uiso 1 1 calc R . . C16 C 0.1997(9) 0.8490(9) 1.0641(3) 0.124(4) Uani 1 1 d . . . H16 H 0.1709 0.8550 1.0897 0.149 Uiso 1 1 calc R . . C17 C 0.2871(9) 0.8873(7) 1.0614(3) 0.108(3) Uani 1 1 d . . . H17 H 0.3205 0.9219 1.0861 0.130 Uiso 1 1 calc R . . C18 C 0.3349(7) 0.8807(6) 1.0240(3) 0.093(2) Uani 1 1 d . . . C19 C 0.4402(8) 0.9269(7) 1.0245(3) 0.106(3) Uani 1 1 d . . . H19A H 0.4583 0.8908 1.0068 0.128 Uiso 1 1 calc R . . H19B H 0.4603 0.9292 1.0557 0.128 Uiso 1 1 calc R . . C20 C 0.4870(7) 1.0246(8) 1.0045(4) 0.111(4) Uani 1 1 d . . . C21 C 0.5181(7) 1.0978(9) 1.0340(6) 0.146(4) Uani 1 1 d U . . H21 H 0.5148 1.0876 1.0654 0.175 Uiso 1 1 calc R . . C22 C 0.5535(8) 1.1848(10) 1.0185(6) 0.159(4) Uani 1 1 d U . . H22 H 0.5730 1.2334 1.0384 0.191 Uiso 1 1 calc R . . C23 C 0.5583(7) 1.1954(10) 0.9716(6) 0.146(4) Uani 1 1 d U . . H23 H 0.5795 1.2535 0.9606 0.175 Uiso 1 1 calc R . . C24 C 0.5352(7) 1.1300(8) 0.9403(5) 0.120(4) Uani 1 1 d . . . C25 C 0.4936(6) 1.0369(9) 0.9597(4) 0.107(3) Uani 1 1 d D . . C26 C 0.5374(8) 1.1467(8) 0.8901(5) 0.134(4) Uani 1 1 d . . . H26A H 0.5845 1.2081 0.8840 0.160 Uiso 1 1 calc R . . H26B H 0.5536 1.1068 0.8745 0.160 Uiso 1 1 calc RD . . C27 C 0.3862(7) 1.0546(8) 0.8505(3) 0.097(3) Uani 1 1 d . . . C28 C 0.4540(7) 1.1338(8) 0.8707(5) 0.124(4) Uani 1 1 d . . . C29 C 0.4381(9) 1.2098(8) 0.8779(6) 0.140(5) Uani 1 1 d . . . H29 H 0.4775 1.2621 0.8937 0.168 Uiso 1 1 calc R . . C30 C 0.3660(12) 1.1962(10) 0.8606(7) 0.156(6) Uani 1 1 d . . . H30 H 0.3575 1.2458 0.8613 0.187 Uiso 1 1 calc R . . C31 C 0.2964(8) 1.1204(9) 0.8406(5) 0.126(4) Uani 1 1 d . . . H31 H 0.2442 1.1194 0.8308 0.151 Uiso 1 1 calc R . . C32 C 0.3069(8) 1.0470(6) 0.8358(3) 0.093(3) Uani 1 1 d . . . C33 C 0.2400(7) 0.9584(6) 0.8164(3) 0.088(2) Uani 1 1 d . . . H33A H 0.2707 0.9267 0.8064 0.106 Uiso 1 1 calc RD . . H33B H 0.2118 0.9679 0.7899 0.106 Uiso 1 1 calc R . . C34 C 0.1777(6) 0.8400(6) 0.8793(3) 0.086(2) Uani 1 1 d . . . C35 C 0.1649(7) 0.8984(6) 0.8523(2) 0.084(2) Uani 1 1 d . . . C36 C 0.0855(8) 0.9007(7) 0.8570(3) 0.097(3) Uani 1 1 d . . . H36 H 0.0735 0.9353 0.8368 0.116 Uiso 1 1 calc R . . C37 C 0.0268(6) 0.8549(9) 0.8895(4) 0.109(3) Uani 1 1 d . . . H37 H -0.0256 0.8583 0.8920 0.131 Uiso 1 1 calc R . . C38 C 0.0417(6) 0.8030(8) 0.9190(4) 0.102(3) Uani 1 1 d . . . H38 H -0.0002 0.7730 0.9421 0.122 Uiso 1 1 calc R . . C39 C 0.1184(6) 0.7927(5) 0.9163(3) 0.089(3) Uani 1 1 d U . . C40 C 0.1353(7) 0.7343(5) 0.9473(4) 0.096(3) Uani 1 1 d U . . H40A H 0.1650 0.7076 0.9305 0.115 Uiso 1 1 calc R . . H40B H 0.0784 0.6859 0.9587 0.115 Uiso 1 1 calc R . . N1 N 0.1047(4) 1.1062(4) 1.10486(18) 0.0635(16) Uani 1 1 d . . . N2 N 0.1190(4) 1.0302(4) 1.02870(17) 0.0611(15) Uani 1 1 d . . . O1 O 0.2589(5) 0.8382(5) 0.8760(3) 0.113(2) Uani 1 1 d D . . H1A H 0.272(9) 0.811(7) 0.857(4) 0.169 Uiso 1 1 d D . . O2 O 0.3279(5) 0.8209(5) 0.9495(2) 0.0970(17) Uani 1 1 d D . . H2A H 0.376(7) 0.856(10) 0.936(7) 0.145 Uiso 0.67 1 d PD . . O3 O 0.4704(5) 0.9721(5) 0.9279(2) 0.1045(18) Uani 1 1 d D . . H3A H 0.4569(19) 0.9922(14) 0.9061(5) 0.157 Uiso 1 1 d D . . O4 O 0.4061(7) 0.9887(6) 0.8445(3) 0.135(3) Uani 1 1 d D . . H4 H 0.362(3) 0.947(9) 0.857(3) 0.203 Uiso 0.67 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0549(5) 0.0549(5) 0.0402(6) 0.000 0.000 0.0275(3) C1 0.086(5) 0.079(5) 0.045(3) -0.013(3) -0.016(3) 0.048(4) C2 0.128(7) 0.088(6) 0.054(4) -0.017(4) -0.014(5) 0.079(6) C3 0.100(6) 0.083(5) 0.071(5) -0.032(4) -0.033(5) 0.042(5) C4 0.069(4) 0.077(4) 0.067(4) -0.006(4) -0.015(3) 0.046(4) C5 0.070(5) 0.095(6) 0.118(7) -0.022(6) 0.011(5) 0.025(5) C6 0.062(5) 0.113(6) 0.090(6) -0.016(5) -0.016(4) 0.046(5) C7 0.054(4) 0.067(4) 0.067(4) -0.010(3) 0.005(3) 0.032(3) C8 0.087(6) 0.126(8) 0.087(6) -0.008(5) 0.019(5) 0.055(6) C9 0.093(6) 0.077(5) 0.054(4) -0.008(4) 0.003(4) 0.039(5) C10 0.100(6) 0.054(4) 0.067(4) -0.013(3) 0.005(4) 0.040(4) C11 0.057(4) 0.066(4) 0.052(3) -0.003(3) -0.007(3) 0.034(3) C12 0.074(4) 0.055(3) 0.048(3) -0.005(3) -0.007(3) 0.038(3) C13 0.136(8) 0.081(5) 0.047(4) 0.003(4) 0.017(4) 0.066(6) C14 0.095(6) 0.064(4) 0.068(5) 0.008(4) 0.009(4) 0.033(4) C15 0.090(6) 0.130(8) 0.103(7) -0.004(6) 0.021(6) 0.047(6) C16 0.120(9) 0.162(11) 0.070(6) 0.006(7) 0.038(6) 0.055(8) C17 0.152(10) 0.101(7) 0.077(6) -0.036(5) -0.001(6) 0.067(7) C18 0.097(6) 0.093(6) 0.100(6) -0.002(5) 0.012(5) 0.057(5) C19 0.153(9) 0.105(7) 0.074(5) -0.002(5) -0.005(5) 0.075(7) C20 0.087(6) 0.128(9) 0.131(9) -0.056(7) -0.022(6) 0.064(6) C21 0.078(5) 0.127(6) 0.199(9) -0.081(8) 0.010(6) 0.025(5) C22 0.089(5) 0.132(7) 0.217(9) -0.077(8) 0.006(7) 0.027(5) C23 0.078(5) 0.121(6) 0.213(9) -0.059(8) 0.004(7) 0.030(5) C24 0.067(5) 0.113(8) 0.160(11) 0.000(8) 0.026(6) 0.031(6) C25 0.061(5) 0.141(10) 0.123(9) -0.003(8) 0.004(5) 0.053(6) C26 0.105(9) 0.103(7) 0.169(12) 0.024(7) 0.062(8) 0.034(6) C27 0.091(6) 0.124(8) 0.099(6) 0.059(6) 0.047(5) 0.072(7) C28 0.072(6) 0.111(8) 0.204(12) 0.063(8) 0.062(7) 0.055(6) C29 0.081(7) 0.081(7) 0.249(17) 0.061(8) 0.033(8) 0.033(6) C30 0.109(11) 0.104(10) 0.229(17) 0.051(10) 0.056(11) 0.034(9) C31 0.092(7) 0.133(10) 0.189(11) 0.081(9) 0.046(7) 0.083(8) C32 0.143(8) 0.095(6) 0.067(4) 0.021(4) 0.041(5) 0.079(7) C33 0.133(7) 0.096(6) 0.059(4) 0.013(4) 0.015(4) 0.076(6) C34 0.104(7) 0.086(6) 0.068(5) -0.015(4) 0.011(4) 0.048(5) C35 0.111(7) 0.078(5) 0.044(4) -0.007(4) -0.002(4) 0.033(5) C36 0.132(9) 0.100(6) 0.066(5) -0.026(5) -0.024(6) 0.063(6) C37 0.075(6) 0.158(9) 0.093(7) -0.017(7) -0.001(5) 0.056(6) C38 0.052(5) 0.127(8) 0.079(6) -0.008(6) 0.003(4) 0.010(5) C39 0.080(6) 0.056(4) 0.099(6) -0.012(4) -0.016(5) 0.009(4) C40 0.093(6) 0.043(4) 0.123(7) -0.005(4) 0.030(5) 0.013(4) N1 0.087(4) 0.084(4) 0.045(3) -0.017(3) -0.017(3) 0.062(4) N2 0.057(3) 0.074(4) 0.041(3) -0.003(3) -0.001(2) 0.024(3) O1 0.124(5) 0.126(5) 0.113(5) 0.022(4) 0.026(4) 0.082(5) O2 0.109(5) 0.114(5) 0.075(4) -0.008(3) 0.013(3) 0.061(4) O3 0.124(5) 0.122(5) 0.083(4) -0.014(4) 0.003(3) 0.072(4) O4 0.192(8) 0.138(6) 0.137(6) 0.022(5) 0.027(5) 0.128(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.108(6) . ? Co1 N1 2.108(6) 3_465 ? Co1 N1 2.108(6) 2_675 ? Co1 N2 2.162(6) 3_465 ? Co1 N2 2.162(6) . ? Co1 N2 2.162(6) 2_675 ? C1 C2 1.388(12) . ? C1 N1 1.398(9) . ? C1 H1 0.9300 . ? C2 C3 1.351(13) . ? C2 H2 0.9300 . ? C3 C4 1.376(11) . ? C3 H3 0.9300 . ? C4 C5 1.401(12) . ? C4 C12 1.422(9) . ? C5 C6 1.366(13) . ? C5 H5 0.9300 . ? C6 C7 1.402(11) . ? C6 H6 0.9300 . ? C7 C11 1.402(9) . ? C7 C8 1.432(12) . ? C8 C9 1.391(13) . ? C8 H8 0.9300 . ? C9 C10 1.354(11) . ? C9 H9 0.9300 . ? C10 N2 1.299(9) . ? C10 H10 0.9300 . ? C11 N2 1.341(9) . ? C11 C12 1.461(9) . ? C12 N1 1.341(9) . ? C13 O2 1.352(9) . ? C13 C14 1.364(13) . ? C13 C18 1.374(13) . ? C14 C15 1.382(14) . ? C14 C40 1.547(13) . ? C15 C16 1.399(17) . ? C15 H15 0.9300 . ? C16 C17 1.302(16) . ? C16 H16 0.9300 . ? C17 C18 1.405(14) . ? C17 H17 0.9300 . ? C18 C19 1.566(15) . ? C19 C20 1.562(17) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C25 1.325(16) . ? C20 C21 1.390(15) . ? C21 C22 1.38(2) . ? C21 H21 0.9300 . ? C22 C23 1.38(2) . ? C22 H22 0.9300 . ? C23 C24 1.346(17) . ? C23 H23 0.9300 . ? C24 C25 1.496(17) . ? C24 C26 1.491(19) . ? C25 O3 1.346(14) . ? C26 C28 1.448(19) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O4 1.343(12) . ? C27 C32 1.367(14) . ? C27 C28 1.402(17) . ? C28 C29 1.473(17) . ? C29 C30 1.24(2) . ? C29 H29 0.9300 . ? C30 C31 1.38(2) . ? C30 H30 0.9300 . ? C31 C32 1.365(14) . ? C31 H31 0.9300 . ? C32 C33 1.483(14) . ? C33 C35 1.578(12) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.376(13) . ? C34 O1 1.410(12) . ? C34 C39 1.427(13) . ? C35 C36 1.387(14) . ? C36 C37 1.319(14) . ? C36 H36 0.9300 . ? C37 C38 1.353(16) . ? C37 H37 0.9300 . ? C38 C39 1.412(15) . ? C38 H38 0.9300 . ? C39 C40 1.482(14) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? O1 H1A 0.82(2) . ? O2 H2A 0.83(2) . ? O3 H3A 0.81(2) . ? O4 H4 0.82(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 95.9(2) . 3_465 ? N1 Co1 N1 95.9(2) . 2_675 ? N1 Co1 N1 95.9(2) 3_465 2_675 ? N1 Co1 N2 168.5(2) . 3_465 ? N1 Co1 N2 76.8(2) 3_465 3_465 ? N1 Co1 N2 93.7(2) 2_675 3_465 ? N1 Co1 N2 76.8(2) . . ? N1 Co1 N2 93.7(2) 3_465 . ? N1 Co1 N2 168.5(2) 2_675 . ? N2 Co1 N2 94.64(19) 3_465 . ? N1 Co1 N2 93.7(2) . 2_675 ? N1 Co1 N2 168.5(2) 3_465 2_675 ? N1 Co1 N2 76.8(2) 2_675 2_675 ? N2 Co1 N2 94.64(19) 3_465 2_675 ? N2 Co1 N2 94.64(19) . 2_675 ? C2 C1 N1 124.3(7) . . ? C2 C1 H1 117.9 . . ? N1 C1 H1 117.9 . . ? C3 C2 C1 115.4(7) . . ? C3 C2 H2 122.3 . . ? C1 C2 H2 122.3 . . ? C2 C3 C4 126.2(8) . . ? C2 C3 H3 116.9 . . ? C4 C3 H3 116.9 . . ? C3 C4 C5 128.7(8) . . ? C3 C4 C12 113.4(7) . . ? C5 C4 C12 117.9(7) . . ? C6 C5 C4 125.6(8) . . ? C6 C5 H5 117.2 . . ? C4 C5 H5 117.2 . . ? C5 C6 C7 116.0(8) . . ? C5 C6 H6 122.0 . . ? C7 C6 H6 122.0 . . ? C6 C7 C11 123.5(6) . . ? C6 C7 C8 121.8(7) . . ? C11 C7 C8 114.6(7) . . ? C9 C8 C7 119.4(7) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 118.0(7) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? N2 C10 C9 125.9(7) . . ? N2 C10 H10 117.1 . . ? C9 C10 H10 117.1 . . ? N2 C11 C7 124.6(6) . . ? N2 C11 C12 116.9(6) . . ? C7 C11 C12 118.2(6) . . ? N1 C12 C4 125.6(6) . . ? N1 C12 C11 115.9(5) . . ? C4 C12 C11 118.5(6) . . ? O2 C13 C14 119.4(8) . . ? O2 C13 C18 122.1(9) . . ? C14 C13 C18 118.5(7) . . ? C13 C14 C15 120.2(8) . . ? C13 C14 C40 122.5(7) . . ? C15 C14 C40 117.3(9) . . ? C14 C15 C16 122.2(10) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C17 C16 C15 115.4(9) . . ? C17 C16 H16 122.3 . . ? C15 C16 H16 122.3 . . ? C16 C17 C18 125.2(10) . . ? C16 C17 H17 117.4 . . ? C18 C17 H17 117.4 . . ? C13 C18 C17 118.4(10) . . ? C13 C18 C19 120.1(8) . . ? C17 C18 C19 121.4(9) . . ? C18 C19 C20 112.5(8) . . ? C18 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? C18 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C25 C20 C21 120.5(14) . . ? C25 C20 C19 119.8(9) . . ? C21 C20 C19 119.6(12) . . ? C22 C21 C20 122.4(16) . . ? C22 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? C21 C22 C23 115.9(13) . . ? C21 C22 H22 122.1 . . ? C23 C22 H22 122.1 . . ? C24 C23 C22 126.4(16) . . ? C24 C23 H23 116.8 . . ? C22 C23 H23 116.8 . . ? C23 C24 C25 114.5(13) . . ? C23 C24 C26 122.8(13) . . ? C25 C24 C26 122.0(11) . . ? C20 C25 O3 125.9(11) . . ? C20 C25 C24 120.2(12) . . ? O3 C25 C24 113.8(10) . . ? C28 C26 C24 115.3(9) . . ? C28 C26 H26A 108.4 . . ? C24 C26 H26A 108.4 . . ? C28 C26 H26B 108.4 . . ? C24 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? O4 C27 C32 122.5(11) . . ? O4 C27 C28 115.6(9) . . ? C32 C27 C28 121.9(9) . . ? C27 C28 C26 126.1(10) . . ? C27 C28 C29 119.1(11) . . ? C26 C28 C29 114.4(13) . . ? C30 C29 C28 112.4(15) . . ? C30 C29 H29 123.8 . . ? C28 C29 H29 123.8 . . ? C29 C30 C31 131.2(15) . . ? C29 C30 H30 114.4 . . ? C31 C30 H30 114.4 . . ? C32 C31 C30 117.5(11) . . ? C32 C31 H31 121.3 . . ? C30 C31 H31 121.3 . . ? C31 C32 C27 117.5(11) . . ? C31 C32 C33 126.3(11) . . ? C27 C32 C33 116.2(8) . . ? C32 C33 C35 112.0(6) . . ? C32 C33 H33A 109.2 . . ? C35 C33 H33A 109.2 . . ? C32 C33 H33B 109.2 . . ? C35 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 O1 119.6(8) . . ? C35 C34 C39 121.4(8) . . ? O1 C34 C39 118.1(8) . . ? C34 C35 C36 118.6(8) . . ? C34 C35 C33 118.8(9) . . ? C36 C35 C33 122.6(8) . . ? C37 C36 C35 121.5(10) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 C38 120.8(10) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C39 122.6(9) . . ? C37 C38 H38 118.7 . . ? C39 C38 H38 118.7 . . ? C38 C39 C34 114.5(9) . . ? C38 C39 C40 124.0(9) . . ? C34 C39 C40 121.5(9) . . ? C39 C40 C14 110.2(6) . . ? C39 C40 H40A 109.6 . . ? C14 C40 H40A 109.6 . . ? C39 C40 H40B 109.6 . . ? C14 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C12 N1 C1 115.0(6) . . ? C12 N1 Co1 116.3(4) . . ? C1 N1 Co1 128.7(5) . . ? C10 N2 C11 116.9(6) . . ? C10 N2 Co1 129.1(5) . . ? C11 N2 Co1 113.9(4) . . ? C34 O1 H1A 128(10) . . ? C13 O2 H2A 132(10) . . ? C25 O3 H3A 102.9(19) . . ? C27 O4 H4 100(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.6(11) . . . . ? C1 C2 C3 C4 -0.8(12) . . . . ? C2 C3 C4 C5 177.1(9) . . . . ? C2 C3 C4 C12 0.2(12) . . . . ? C3 C4 C5 C6 176.8(10) . . . . ? C12 C4 C5 C6 -6.4(14) . . . . ? C4 C5 C6 C7 4.5(15) . . . . ? C5 C6 C7 C11 -2.4(12) . . . . ? C5 C6 C7 C8 -177.8(9) . . . . ? C6 C7 C8 C9 178.7(8) . . . . ? C11 C7 C8 C9 2.9(13) . . . . ? C7 C8 C9 C10 1.8(14) . . . . ? C8 C9 C10 N2 -2.1(13) . . . . ? C6 C7 C11 N2 175.9(7) . . . . ? C8 C7 C11 N2 -8.4(10) . . . . ? C6 C7 C11 C12 2.4(10) . . . . ? C8 C7 C11 C12 178.1(7) . . . . ? C3 C4 C12 N1 1.9(10) . . . . ? C5 C4 C12 N1 -175.3(8) . . . . ? C3 C4 C12 C11 -176.8(6) . . . . ? C5 C4 C12 C11 6.0(10) . . . . ? N2 C11 C12 N1 2.9(8) . . . . ? C7 C11 C12 N1 176.9(6) . . . . ? N2 C11 C12 C4 -178.2(6) . . . . ? C7 C11 C12 C4 -4.2(8) . . . . ? O2 C13 C14 C15 179.8(9) . . . . ? C18 C13 C14 C15 -2.3(13) . . . . ? O2 C13 C14 C40 -0.2(11) . . . . ? C18 C13 C14 C40 177.8(8) . . . . ? C13 C14 C15 C16 1.9(17) . . . . ? C40 C14 C15 C16 -178.2(11) . . . . ? C14 C15 C16 C17 -0.5(19) . . . . ? C15 C16 C17 C18 0(2) . . . . ? O2 C13 C18 C17 179.3(9) . . . . ? C14 C13 C18 C17 1.5(13) . . . . ? O2 C13 C18 C19 -2.7(13) . . . . ? C14 C13 C18 C19 179.4(8) . . . . ? C16 C17 C18 C13 -0.1(17) . . . . ? C16 C17 C18 C19 -178.0(11) . . . . ? C13 C18 C19 C20 91.2(10) . . . . ? C17 C18 C19 C20 -91.0(11) . . . . ? C18 C19 C20 C25 -80.3(11) . . . . ? C18 C19 C20 C21 97.0(11) . . . . ? C25 C20 C21 C22 2.5(17) . . . . ? C19 C20 C21 C22 -174.8(10) . . . . ? C20 C21 C22 C23 -1.4(18) . . . . ? C21 C22 C23 C24 -3(2) . . . . ? C22 C23 C24 C25 5.4(18) . . . . ? C22 C23 C24 C26 176.2(12) . . . . ? C21 C20 C25 O3 176.3(9) . . . . ? C19 C20 C25 O3 -6.4(14) . . . . ? C21 C20 C25 C24 0.4(14) . . . . ? C19 C20 C25 C24 177.7(9) . . . . ? C23 C24 C25 C20 -4.0(14) . . . . ? C26 C24 C25 C20 -174.9(10) . . . . ? C23 C24 C25 O3 179.6(9) . . . . ? C26 C24 C25 O3 8.7(14) . . . . ? C23 C24 C26 C28 -91.4(14) . . . . ? C25 C24 C26 C28 78.8(14) . . . . ? O4 C27 C28 C26 -7.4(16) . . . . ? C32 C27 C28 C26 175.5(10) . . . . ? O4 C27 C28 C29 179.2(10) . . . . ? C32 C27 C28 C29 2.2(15) . . . . ? C24 C26 C28 C27 -93.8(15) . . . . ? C24 C26 C28 C29 79.8(13) . . . . ? C27 C28 C29 C30 -6.2(18) . . . . ? C26 C28 C29 C30 179.8(13) . . . . ? C28 C29 C30 C31 8(3) . . . . ? C29 C30 C31 C32 -4(3) . . . . ? C30 C31 C32 C27 -1.0(15) . . . . ? C30 C31 C32 C33 178.3(10) . . . . ? O4 C27 C32 C31 -175.4(8) . . . . ? C28 C27 C32 C31 1.4(13) . . . . ? O4 C27 C32 C33 5.2(12) . . . . ? C28 C27 C32 C33 -178.0(8) . . . . ? C31 C32 C33 C35 -79.9(11) . . . . ? C27 C32 C33 C35 99.4(9) . . . . ? O1 C34 C35 C36 -178.3(8) . . . . ? C39 C34 C35 C36 -9.6(12) . . . . ? O1 C34 C35 C33 3.0(11) . . . . ? C39 C34 C35 C33 171.7(8) . . . . ? C32 C33 C35 C34 -91.5(9) . . . . ? C32 C33 C35 C36 89.9(10) . . . . ? C34 C35 C36 C37 6.4(13) . . . . ? C33 C35 C36 C37 -174.9(8) . . . . ? C35 C36 C37 C38 -0.8(15) . . . . ? C36 C37 C38 C39 -1.9(16) . . . . ? C37 C38 C39 C34 -1.1(14) . . . . ? C37 C38 C39 C40 -178.0(9) . . . . ? C35 C34 C39 C38 6.9(12) . . . . ? O1 C34 C39 C38 175.8(8) . . . . ? C35 C34 C39 C40 -176.1(7) . . . . ? O1 C34 C39 C40 -7.2(12) . . . . ? C38 C39 C40 C14 -94.3(10) . . . . ? C34 C39 C40 C14 89.0(10) . . . . ? C13 C14 C40 C39 -92.1(10) . . . . ? C15 C14 C40 C39 88.0(10) . . . . ? C4 C12 N1 C1 -3.1(9) . . . . ? C11 C12 N1 C1 175.7(5) . . . . ? C4 C12 N1 Co1 176.3(5) . . . . ? C11 C12 N1 Co1 -5.0(7) . . . . ? C2 C1 N1 C12 2.4(9) . . . . ? C2 C1 N1 Co1 -176.9(5) . . . . ? N1 Co1 N1 C12 96.4(6) 3_465 . . . ? N1 Co1 N1 C12 -167.1(5) 2_675 . . . ? N2 Co1 N1 C12 46.5(15) 3_465 . . . ? N2 Co1 N1 C12 4.0(5) . . . . ? N2 Co1 N1 C12 -89.9(4) 2_675 . . . ? N1 Co1 N1 C1 -84.3(4) 3_465 . . . ? N1 Co1 N1 C1 12.2(6) 2_675 . . . ? N2 Co1 N1 C1 -134.2(11) 3_465 . . . ? N2 Co1 N1 C1 -176.8(6) . . . . ? N2 Co1 N1 C1 89.3(6) 2_675 . . . ? C9 C10 N2 C11 -2.9(11) . . . . ? C9 C10 N2 Co1 178.9(6) . . . . ? C7 C11 N2 C10 8.4(10) . . . . ? C12 C11 N2 C10 -178.0(6) . . . . ? C7 C11 N2 Co1 -173.1(5) . . . . ? C12 C11 N2 Co1 0.5(7) . . . . ? N1 Co1 N2 C10 175.9(7) . . . . ? N1 Co1 N2 C10 80.8(7) 3_465 . . . ? N1 Co1 N2 C10 -132.7(12) 2_675 . . . ? N2 Co1 N2 C10 3.7(6) 3_465 . . . ? N2 Co1 N2 C10 -91.4(5) 2_675 . . . ? N1 Co1 N2 C11 -2.3(5) . . . . ? N1 Co1 N2 C11 -97.5(5) 3_465 . . . ? N1 Co1 N2 C11 49.0(14) 2_675 . . . ? N2 Co1 N2 C11 -174.6(5) 3_465 . . . ? N2 Co1 N2 C11 90.4(6) 2_675 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A O4 0.81(2) 1.988(19) 2.750(11) 156(2) . O2 H2A O3 0.83(2) 1.85(10) 2.597(10) 150(20) . O4 H4 O1 0.82(2) 1.90(4) 2.712(13) 170(17) . _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.084 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.085 #===== data_5 _database_code_depnum_ccdc_archive 'CCDC 879387' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H74 Co N6 O10' _chemical_formula_weight 1122.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 18.3920(3) _cell_length_b 18.9660(3) _cell_length_c 15.8660(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5534.42(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2380 _exptl_absorpt_coefficient_mu 0.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9084 _exptl_absorpt_correction_T_max 0.9353 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40604 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 29.28 _reflns_number_total 6944 _reflns_number_gt 3884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distance of O1---H1WA was refined isotropically with restraints of O---H = 0.85+-0.02 \%A. The distance of O1---H1WB was refined isotropically with restraints of O---H = 0.85+-0.01 \%A. The distance of O3---H3 was refined isotropically with restraints of O---H = 0.82+-0.02 \%A. The distance of H1WA...H1WB was restrained to 1.44+-0.02 \%A. The distance of H3...H24B was restrained to 2.10+-0.02 \%A. The distance of C25...H3 was restrained to 1.71+-0.01 \%A. For C5 and C6 atoms, some anisotropic displacement ellipsoids were rather elongated which led us to use the DELU restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6944 _refine_ls_number_parameters 366 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.883 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.197909(18) 0.2500 0.04297(12) Uani 1 2 d S . . C1 C 0.12751(13) 0.27976(15) 0.31870(18) 0.0772(7) Uani 1 1 d . . . H1A H 0.1444 0.3252 0.3388 0.093 Uiso 1 1 calc R . . H1B H 0.1542 0.2434 0.3485 0.093 Uiso 1 1 calc R . . C2 C 0.14163(13) 0.27388(15) 0.22869(18) 0.0753(7) Uani 1 1 d . . . H2A H 0.1937 0.2720 0.2191 0.090 Uiso 1 1 calc R . . H2B H 0.1228 0.3152 0.2001 0.090 Uiso 1 1 calc R . . C3 C -0.0290(2) 0.04407(14) 0.2182(2) 0.1267(16) Uani 1 1 d . . . H3A H -0.0236 0.0036 0.1814 0.152 Uiso 1 1 calc R . . H3B H -0.0760 0.0409 0.2457 0.152 Uiso 1 1 calc R . . C4 C 0.14875(9) 0.23909(10) 0.55418(10) 0.0388(4) Uani 1 1 d . . . C5 C 0.17818(9) 0.17420(10) 0.52884(11) 0.0404(4) Uani 1 1 d U . . C6 C 0.13276(11) 0.11686(11) 0.51969(13) 0.0536(5) Uani 1 1 d U . . H6 H 0.1523 0.0738 0.5032 0.064 Uiso 1 1 calc R . . C7 C 0.05890(11) 0.12189(12) 0.53442(14) 0.0596(6) Uani 1 1 d . . . H7 H 0.0291 0.0826 0.5286 0.072 Uiso 1 1 calc R . . C8 C 0.03011(11) 0.18621(11) 0.55790(13) 0.0543(5) Uani 1 1 d . . . H8 H -0.0197 0.1899 0.5671 0.065 Uiso 1 1 calc R . . C9 C 0.07334(9) 0.24517(10) 0.56803(11) 0.0426(4) Uani 1 1 d . . . C10 C 0.03972(10) 0.31487(10) 0.59443(12) 0.0489(5) Uani 1 1 d . . . H10A H -0.0063 0.3056 0.6221 0.059 Uiso 1 1 calc R . . H10B H 0.0715 0.3374 0.6351 0.059 Uiso 1 1 calc R . . C11 C 0.08173(8) 0.41158(9) 0.49498(11) 0.0371(4) Uani 1 1 d . . . C12 C 0.02696(9) 0.36501(9) 0.52192(11) 0.0394(4) Uani 1 1 d . . . C13 C -0.03924(9) 0.36617(10) 0.47980(12) 0.0445(4) Uani 1 1 d . . . H13 H -0.0760 0.3356 0.4966 0.053 Uiso 1 1 calc R . . C14 C -0.05148(9) 0.41170(10) 0.41355(13) 0.0471(5) Uani 1 1 d . . . H14 H -0.0963 0.4119 0.3864 0.056 Uiso 1 1 calc R . . C15 C 0.00261(9) 0.45668(9) 0.38785(12) 0.0440(4) Uani 1 1 d . . . H15 H -0.0060 0.4872 0.3431 0.053 Uiso 1 1 calc R . . C16 C 0.07001(9) 0.45737(9) 0.42749(11) 0.0386(4) Uani 1 1 d . . . C17 C 0.12771(9) 0.50993(9) 0.40014(12) 0.0428(4) Uani 1 1 d . . . H17A H 0.1037 0.5494 0.3730 0.051 Uiso 1 1 calc R . . H17B H 0.1518 0.5279 0.4501 0.051 Uiso 1 1 calc R . . C18 C 0.24854(9) 0.44885(9) 0.37095(11) 0.0379(4) Uani 1 1 d . . . C19 C 0.18526(9) 0.48153(8) 0.34057(11) 0.0371(4) Uani 1 1 d . . . C20 C 0.17757(10) 0.48886(9) 0.25405(12) 0.0438(4) Uani 1 1 d . . . H20 H 0.1364 0.5111 0.2327 0.053 Uiso 1 1 calc R . . C21 C 0.22949(11) 0.46403(10) 0.19891(12) 0.0488(5) Uani 1 1 d . . . H21 H 0.2241 0.4708 0.1412 0.059 Uiso 1 1 calc R . . C22 C 0.28964(10) 0.42898(10) 0.23001(12) 0.0458(5) Uani 1 1 d . . . H22 H 0.3240 0.4111 0.1926 0.055 Uiso 1 1 calc R . . C23 C 0.29971(9) 0.41993(9) 0.31594(11) 0.0395(4) Uani 1 1 d . . . C24 C 0.36180(9) 0.37501(10) 0.34923(12) 0.0460(5) Uani 1 1 d . . . H24A H 0.4034 0.3792 0.3119 0.055 Uiso 1 1 calc R . . H24B H 0.3761 0.3918 0.4045 0.055 Uiso 1 1 calc RD . . C25 C 0.31536(9) 0.26791(10) 0.43070(11) 0.0383(4) Uani 1 1 d D . . C26 C 0.33905(9) 0.29836(10) 0.35517(11) 0.0417(4) Uani 1 1 d . . . C27 C 0.33665(11) 0.25717(11) 0.28297(13) 0.0526(5) Uani 1 1 d . . . H27 H 0.3544 0.2757 0.2327 0.063 Uiso 1 1 calc R . . C28 C 0.30888(12) 0.18984(11) 0.28340(14) 0.0575(6) Uani 1 1 d . . . H28 H 0.3076 0.1633 0.2341 0.069 Uiso 1 1 calc R . . C29 C 0.28296(10) 0.16219(10) 0.35808(12) 0.0482(5) Uani 1 1 d . . . H29 H 0.2629 0.1172 0.3583 0.058 Uiso 1 1 calc R . . C30 C 0.28619(9) 0.20002(9) 0.43252(11) 0.0387(4) Uani 1 1 d . . . C31 C 0.25951(10) 0.16682(10) 0.51373(11) 0.0464(4) Uani 1 1 d . . . H31A H 0.2852 0.1882 0.5606 0.056 Uiso 1 1 calc R . . H31B H 0.2718 0.1171 0.5131 0.056 Uiso 1 1 calc R . . N1 N 0.04904(10) 0.27238(11) 0.33660(12) 0.0683(5) Uani 1 1 d . . . H1C H 0.0342 0.3172 0.3262 0.082 Uiso 1 1 d R . . H1D H 0.0399 0.2625 0.3834 0.082 Uiso 1 1 d R . . N2 N 0.10753(10) 0.21045(10) 0.19338(12) 0.0676(5) Uani 1 1 d . . . H2C H 0.0980 0.2129 0.1439 0.081 Uiso 1 1 d R . . H2D H 0.1396 0.1795 0.2128 0.081 Uiso 1 1 d R . . N3 N -0.02499(13) 0.10862(12) 0.16900(14) 0.0844(6) Uani 1 1 d . . . H3C H -0.0705 0.1213 0.1481 0.101 Uiso 1 1 d R . . H3D H 0.0195 0.1076 0.1365 0.101 Uiso 1 1 d R . . O1 O 0.14636(6) 0.41206(7) 0.53657(8) 0.0455(3) Uani 1 1 d . . . H1 H 0.1731 0.4419 0.5157 0.068 Uiso 1 1 calc R . . O2 O 0.19243(6) 0.29497(7) 0.56671(8) 0.0450(3) Uani 1 1 d . . . H2 H 0.2347 0.2837 0.5573 0.068 Uiso 1 1 calc R . . O4 O 0.26201(6) 0.44619(7) 0.45559(7) 0.0517(3) Uani 1 1 d . . . O1W O 0.37822(13) 0.42939(12) 0.58692(16) 0.1131(8) Uani 1 1 d D . . H1WA H 0.364(2) 0.4546(19) 0.5453(17) 0.170 Uiso 1 1 d D . . H1WB H 0.3439(17) 0.425(2) 0.624(2) 0.170 Uiso 1 1 d D . . O3 O 0.32196(7) 0.30426(7) 0.50470(8) 0.0481(3) Uani 1 1 d D . . H3 H 0.3054(11) 0.3385(6) 0.4946(9) 0.072 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0518(2) 0.0434(2) 0.03372(19) 0.000 0.00143(15) 0.000 C1 0.0572(14) 0.0828(17) 0.092(2) -0.0329(15) -0.0189(13) 0.0064(12) C2 0.0521(13) 0.0849(17) 0.0889(19) 0.0130(15) -0.0127(13) -0.0110(13) C3 0.189(5) 0.0590(15) 0.132(3) -0.0280(17) 0.073(3) -0.043(2) C4 0.0394(10) 0.0521(11) 0.0250(8) 0.0081(7) -0.0017(7) -0.0023(8) C5 0.0409(10) 0.0487(11) 0.0317(9) 0.0092(8) -0.0024(8) 0.0009(8) C6 0.0611(12) 0.0496(12) 0.0500(12) 0.0096(9) -0.0005(10) 0.0036(10) C7 0.0546(12) 0.0563(13) 0.0678(14) 0.0140(11) -0.0003(11) -0.0139(11) C8 0.0410(10) 0.0668(14) 0.0550(12) 0.0124(10) 0.0076(10) -0.0068(10) C9 0.0391(10) 0.0570(12) 0.0317(9) 0.0063(8) 0.0047(8) -0.0022(9) C10 0.0382(10) 0.0678(13) 0.0408(10) -0.0026(9) 0.0124(8) -0.0024(9) C11 0.0285(8) 0.0426(10) 0.0403(9) -0.0142(8) 0.0032(7) 0.0015(7) C12 0.0325(8) 0.0467(10) 0.0390(10) -0.0108(8) 0.0080(8) 0.0027(8) C13 0.0285(9) 0.0471(11) 0.0578(12) -0.0117(9) 0.0086(9) -0.0002(8) C14 0.0305(9) 0.0496(11) 0.0612(12) -0.0122(10) -0.0042(9) 0.0061(8) C15 0.0393(10) 0.0414(10) 0.0513(11) -0.0061(8) -0.0027(9) 0.0086(8) C16 0.0337(9) 0.0372(9) 0.0448(10) -0.0120(8) 0.0037(8) 0.0047(7) C17 0.0410(10) 0.0348(9) 0.0527(11) -0.0065(8) -0.0035(8) 0.0004(8) C18 0.0352(9) 0.0387(9) 0.0396(10) -0.0021(7) -0.0035(8) -0.0080(7) C19 0.0339(9) 0.0299(9) 0.0475(10) -0.0045(7) 0.0000(8) -0.0065(7) C20 0.0419(10) 0.0385(10) 0.0510(11) 0.0009(8) -0.0111(9) -0.0002(8) C21 0.0559(12) 0.0524(12) 0.0382(10) 0.0010(8) -0.0055(9) -0.0054(10) C22 0.0463(10) 0.0480(11) 0.0430(11) 0.0013(8) 0.0074(9) -0.0012(9) C23 0.0331(9) 0.0408(10) 0.0446(10) 0.0002(8) 0.0024(8) -0.0055(7) C24 0.0284(8) 0.0611(12) 0.0486(11) 0.0059(9) 0.0075(8) 0.0010(8) C25 0.0280(8) 0.0505(11) 0.0364(10) 0.0011(8) -0.0027(7) 0.0081(8) C26 0.0302(8) 0.0538(11) 0.0410(10) 0.0046(9) 0.0036(8) 0.0103(8) C27 0.0585(12) 0.0590(13) 0.0403(10) 0.0075(10) 0.0121(10) 0.0198(10) C28 0.0768(14) 0.0533(13) 0.0424(11) -0.0048(9) 0.0047(11) 0.0228(11) C29 0.0525(11) 0.0412(10) 0.0508(12) 0.0010(9) 0.0004(9) 0.0164(9) C30 0.0320(8) 0.0473(10) 0.0369(9) 0.0065(8) -0.0029(7) 0.0147(8) C31 0.0456(10) 0.0502(11) 0.0434(10) 0.0092(8) -0.0052(9) 0.0109(9) N1 0.0594(11) 0.0819(13) 0.0634(11) -0.0280(10) -0.0104(9) 0.0124(10) N2 0.0672(12) 0.0813(13) 0.0541(11) -0.0081(9) 0.0123(9) -0.0054(10) N3 0.0986(15) 0.0784(14) 0.0762(14) -0.0255(11) 0.0170(12) -0.0215(12) O1 0.0359(6) 0.0583(8) 0.0423(7) -0.0051(6) -0.0020(5) -0.0093(6) O2 0.0327(6) 0.0600(8) 0.0423(7) -0.0038(6) 0.0020(5) -0.0023(6) O4 0.0397(7) 0.0768(9) 0.0386(7) -0.0047(6) -0.0066(6) 0.0022(6) O1W 0.1312(18) 0.0848(14) 0.1233(18) 0.0034(13) -0.0802(15) 0.0042(13) O3 0.0457(7) 0.0589(8) 0.0398(7) -0.0001(6) -0.0075(6) -0.0040(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.1671(17) . ? Co1 N1 2.1671(17) 4 ? Co1 N3 2.175(2) . ? Co1 N3 2.175(2) 4 ? Co1 N2 2.1852(18) . ? Co1 N2 2.1852(17) 4 ? C1 C2 1.456(4) . ? C1 N1 1.478(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.468(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N3 1.454(4) . ? C3 C3 1.469(7) 4 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O2 1.345(2) . ? C4 C5 1.403(3) . ? C4 C9 1.409(2) . ? C5 C6 1.379(3) . ? C5 C31 1.521(2) . ? C6 C7 1.382(3) . ? C6 H6 0.9300 . ? C7 C8 1.381(3) . ? C7 H7 0.9300 . ? C8 C9 1.381(3) . ? C8 H8 0.9300 . ? C9 C10 1.518(3) . ? C10 C12 1.511(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O1 1.3597(19) . ? C11 C16 1.395(3) . ? C11 C12 1.406(2) . ? C12 C13 1.389(2) . ? C13 C14 1.379(3) . ? C13 H13 0.9300 . ? C14 C15 1.372(3) . ? C14 H14 0.9300 . ? C15 C16 1.390(2) . ? C15 H15 0.9300 . ? C16 C17 1.519(2) . ? C17 C19 1.518(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.367(2) . ? C18 C23 1.396(2) . ? C18 C19 1.404(2) . ? C19 C20 1.387(2) . ? C20 C21 1.378(3) . ? C20 H20 0.9300 . ? C21 C22 1.382(3) . ? C21 H21 0.9300 . ? C22 C23 1.387(3) . ? C22 H22 0.9300 . ? C23 C24 1.519(2) . ? C24 C26 1.516(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O3 1.367(2) . ? C25 C30 1.395(3) . ? C25 C26 1.400(2) . ? C26 C27 1.387(3) . ? C27 C28 1.375(3) . ? C27 H27 0.9300 . ? C28 C29 1.381(3) . ? C28 H28 0.9300 . ? C29 C30 1.383(3) . ? C29 H29 0.9300 . ? C30 C31 1.516(2) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? N1 H1C 0.9069 . ? N1 H1D 0.7835 . ? N2 H2C 0.8056 . ? N2 H2D 0.8884 . ? N3 H3C 0.9311 . ? N3 H3D 0.9677 . ? O1 H1 0.8200 . ? O2 H2 0.8200 . ? O1W H1WA 0.856(18) . ? O1W H1WB 0.864(10) . ? O3 H3 0.735(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 98.65(11) . 4 ? N1 Co1 N3 165.94(8) . . ? N1 Co1 N3 92.57(9) 4 . ? N1 Co1 N3 92.57(9) . 4 ? N1 Co1 N3 165.94(8) 4 4 ? N3 Co1 N3 77.73(13) . 4 ? N1 Co1 N2 79.22(7) . . ? N1 Co1 N2 92.58(7) 4 . ? N3 Co1 N2 91.90(8) . . ? N3 Co1 N2 97.84(8) 4 . ? N1 Co1 N2 92.58(7) . 4 ? N1 Co1 N2 79.22(7) 4 4 ? N3 Co1 N2 97.84(8) . 4 ? N3 Co1 N2 91.90(8) 4 4 ? N2 Co1 N2 167.50(11) . 4 ? C2 C1 N1 110.83(19) . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C1 C2 N2 111.2(2) . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? N2 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N3 C3 C3 109.4(2) . 4 ? N3 C3 H3A 109.8 . . ? C3 C3 H3A 109.8 4 . ? N3 C3 H3B 109.8 . . ? C3 C3 H3B 109.8 4 . ? H3A C3 H3B 108.2 . . ? O2 C4 C5 120.22(15) . . ? O2 C4 C9 120.04(17) . . ? C5 C4 C9 119.74(16) . . ? C6 C5 C4 119.23(16) . . ? C6 C5 C31 120.43(17) . . ? C4 C5 C31 120.33(16) . . ? C5 C6 C7 121.5(2) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C8 C7 C6 118.92(19) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C8 C9 121.72(18) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C8 C9 C4 118.83(18) . . ? C8 C9 C10 120.17(16) . . ? C4 C9 C10 121.00(16) . . ? C12 C10 C9 113.65(14) . . ? C12 C10 H10A 108.8 . . ? C9 C10 H10A 108.8 . . ? C12 C10 H10B 108.8 . . ? C9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? O1 C11 C16 120.22(15) . . ? O1 C11 C12 118.88(16) . . ? C16 C11 C12 120.90(15) . . ? C13 C12 C11 118.14(17) . . ? C13 C12 C10 120.83(16) . . ? C11 C12 C10 121.03(16) . . ? C14 C13 C12 121.31(17) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C15 C14 C13 119.83(17) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 121.18(18) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C11 118.62(16) . . ? C15 C16 C17 119.99(17) . . ? C11 C16 C17 121.30(15) . . ? C19 C17 C16 115.61(14) . . ? C19 C17 H17A 108.4 . . ? C16 C17 H17A 108.4 . . ? C19 C17 H17B 108.4 . . ? C16 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? O4 C18 C23 118.53(15) . . ? O4 C18 C19 120.26(15) . . ? C23 C18 C19 121.19(16) . . ? C20 C19 C18 117.94(16) . . ? C20 C19 C17 120.64(16) . . ? C18 C19 C17 121.40(16) . . ? C21 C20 C19 121.56(17) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 119.50(17) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 121.17(17) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.43(16) . . ? C22 C23 C24 120.77(16) . . ? C18 C23 C24 120.65(16) . . ? C26 C24 C23 110.60(14) . . ? C26 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C26 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? O3 C25 C30 118.81(15) . . ? O3 C25 C26 119.97(16) . . ? C30 C25 C26 121.20(17) . . ? C27 C26 C25 117.70(17) . . ? C27 C26 C24 119.84(17) . . ? C25 C26 C24 122.33(17) . . ? C28 C27 C26 122.04(19) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C28 C29 119.0(2) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C28 C29 C30 121.40(19) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C29 C30 C25 118.53(17) . . ? C29 C30 C31 119.77(17) . . ? C25 C30 C31 121.70(16) . . ? C30 C31 C5 114.46(14) . . ? C30 C31 H31A 108.6 . . ? C5 C31 H31A 108.6 . . ? C30 C31 H31B 108.6 . . ? C5 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? C1 N1 Co1 110.27(13) . . ? C1 N1 H1C 99.8 . . ? Co1 N1 H1C 111.7 . . ? C1 N1 H1D 114.5 . . ? Co1 N1 H1D 110.8 . . ? H1C N1 H1D 109.3 . . ? C2 N2 Co1 108.61(15) . . ? C2 N2 H2C 114.7 . . ? Co1 N2 H2C 102.2 . . ? C2 N2 H2D 97.2 . . ? Co1 N2 H2D 112.7 . . ? H2C N2 H2D 121.4 . . ? C3 N3 Co1 110.42(17) . . ? C3 N3 H3C 111.2 . . ? Co1 N3 H3C 101.5 . . ? C3 N3 H3D 108.2 . . ? Co1 N3 H3D 98.7 . . ? H3C N3 H3D 125.1 . . ? C11 O1 H1 109.5 . . ? C4 O2 H2 109.5 . . ? H1WA O1W H1WB 111(3) . . ? C25 O3 H3 102.8(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -50.9(3) . . . . ? O2 C4 C5 C6 177.37(16) . . . . ? C9 C4 C5 C6 -1.4(2) . . . . ? O2 C4 C5 C31 -1.2(2) . . . . ? C9 C4 C5 C31 -179.94(15) . . . . ? C4 C5 C6 C7 0.4(3) . . . . ? C31 C5 C6 C7 178.89(17) . . . . ? C5 C6 C7 C8 0.8(3) . . . . ? C6 C7 C8 C9 -0.9(3) . . . . ? C7 C8 C9 C4 -0.2(3) . . . . ? C7 C8 C9 C10 -179.62(18) . . . . ? O2 C4 C9 C8 -177.47(16) . . . . ? C5 C4 C9 C8 1.3(2) . . . . ? O2 C4 C9 C10 2.0(2) . . . . ? C5 C4 C9 C10 -179.24(15) . . . . ? C8 C9 C10 C12 -99.4(2) . . . . ? C4 C9 C10 C12 81.1(2) . . . . ? O1 C11 C12 C13 178.75(14) . . . . ? C16 C11 C12 C13 -0.4(2) . . . . ? O1 C11 C12 C10 -1.5(2) . . . . ? C16 C11 C12 C10 179.41(15) . . . . ? C9 C10 C12 C13 92.36(19) . . . . ? C9 C10 C12 C11 -87.4(2) . . . . ? C11 C12 C13 C14 -0.2(2) . . . . ? C10 C12 C13 C14 -179.99(16) . . . . ? C12 C13 C14 C15 0.4(3) . . . . ? C13 C14 C15 C16 0.0(3) . . . . ? C14 C15 C16 C11 -0.5(3) . . . . ? C14 C15 C16 C17 -177.36(16) . . . . ? O1 C11 C16 C15 -178.37(14) . . . . ? C12 C11 C16 C15 0.7(2) . . . . ? O1 C11 C16 C17 -1.6(2) . . . . ? C12 C11 C16 C17 177.51(15) . . . . ? C15 C16 C17 C19 -98.89(19) . . . . ? C11 C16 C17 C19 84.4(2) . . . . ? O4 C18 C19 C20 173.88(15) . . . . ? C23 C18 C19 C20 -4.6(2) . . . . ? O4 C18 C19 C17 -4.5(2) . . . . ? C23 C18 C19 C17 177.01(15) . . . . ? C16 C17 C19 C20 94.2(2) . . . . ? C16 C17 C19 C18 -87.5(2) . . . . ? C18 C19 C20 C21 1.0(3) . . . . ? C17 C19 C20 C21 179.41(16) . . . . ? C19 C20 C21 C22 2.1(3) . . . . ? C20 C21 C22 C23 -1.7(3) . . . . ? C21 C22 C23 C18 -1.8(3) . . . . ? C21 C22 C23 C24 173.74(18) . . . . ? O4 C18 C23 C22 -173.54(16) . . . . ? C19 C18 C23 C22 5.0(2) . . . . ? O4 C18 C23 C24 10.9(2) . . . . ? C19 C18 C23 C24 -170.52(16) . . . . ? C22 C23 C24 C26 -87.4(2) . . . . ? C18 C23 C24 C26 88.0(2) . . . . ? O3 C25 C26 C27 174.84(15) . . . . ? C30 C25 C26 C27 -3.8(2) . . . . ? O3 C25 C26 C24 -9.4(2) . . . . ? C30 C25 C26 C24 171.90(15) . . . . ? C23 C24 C26 C27 77.9(2) . . . . ? C23 C24 C26 C25 -97.8(2) . . . . ? C25 C26 C27 C28 3.1(3) . . . . ? C24 C26 C27 C28 -172.74(18) . . . . ? C26 C27 C28 C29 -0.4(3) . . . . ? C27 C28 C29 C30 -1.8(3) . . . . ? C28 C29 C30 C25 1.0(3) . . . . ? C28 C29 C30 C31 -177.90(17) . . . . ? O3 C25 C30 C29 -176.86(15) . . . . ? C26 C25 C30 C29 1.8(2) . . . . ? O3 C25 C30 C31 2.1(2) . . . . ? C26 C25 C30 C31 -179.25(15) . . . . ? C29 C30 C31 C5 -85.3(2) . . . . ? C25 C30 C31 C5 95.8(2) . . . . ? C6 C5 C31 C30 106.6(2) . . . . ? C4 C5 C31 C30 -74.9(2) . . . . ? C2 C1 N1 Co1 34.7(3) . . . . ? N1 Co1 N1 C1 -100.61(18) 4 . . . ? N3 Co1 N1 C1 42.0(4) . . . . ? N3 Co1 N1 C1 87.88(18) 4 . . . ? N2 Co1 N1 C1 -9.61(17) . . . . ? N2 Co1 N1 C1 179.90(17) 4 . . . ? C1 C2 N2 Co1 40.5(2) . . . . ? N1 Co1 N2 C2 -16.13(16) . . . . ? N1 Co1 N2 C2 82.19(16) 4 . . . ? N3 Co1 N2 C2 174.85(17) . . . . ? N3 Co1 N2 C2 -107.27(17) 4 . . . ? N2 Co1 N2 C2 33.59(15) 4 . . . ? C3 C3 N3 Co1 -40.2(4) 4 . . . ? N1 Co1 N3 C3 61.4(4) . . . . ? N1 Co1 N3 C3 -155.6(2) 4 . . . ? N3 Co1 N3 C3 14.14(18) 4 . . . ? N2 Co1 N3 C3 111.7(2) . . . . ? N2 Co1 N3 C3 -76.1(2) 4 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O3 0.82 1.85 2.5835(18) 148.1 . O1 H1 O4 0.82 1.89 2.5678(17) 138.7 . O1W H1WA O4 0.856(18) 2.36(3) 3.002(2) 132(3) . N3 H3D O1W 0.97 2.16 3.083(3) 159.8 2_554 O3 H3 O4 0.735(14) 2.278(14) 3.0113(19) 175.1(17) . _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.408 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.041 #===== data_6 _database_code_depnum_ccdc_archive 'CCDC 879388' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130 H140 N12 O17 Zn2' _chemical_formula_weight 2273.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.772(4) _cell_length_b 17.601(3) _cell_length_c 19.969(5) _cell_angle_alpha 90 _cell_angle_beta 91.723(5) _cell_angle_gamma 90 _cell_volume 5892(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8777 _exptl_absorpt_correction_T_max 0.9062 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22477 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.1934 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.35 _reflns_number_total 10701 _reflns_number_gt 3707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The low ratio of observed/unique reflections may be attributed to the weak diffraction of the crystals. The distances of H4...H7B, H8...H56A and H5...H8 were refined isotropically with restraints of 2.02+-0.02 \%A. The distance of H2A...H28A was restrained to 2.02+-0.01 \%A. The distance of O1W...O7 was restrained to 3.10+-0.01 \%A. The distance of C62...C63 was restrained to 1.50+-0.01 \%A. For N6, C64, C65, N3, C62, C63, C35, C28, C62, C63, C19, C20, C31, C32 and C33, some anisotropic displacement ellipsoids were rather elongated which led us to use the SIMU/DELU restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10701 _refine_ls_number_parameters 734 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1758 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1846 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.00805(5) 0.28335(4) 0.75505(3) 0.0592(3) Uani 1 1 d . . . C1 C -0.3748(5) 0.3428(4) 0.8165(4) 0.094(2) Uani 1 1 d . . . H1 H -0.3793 0.3063 0.8499 0.113 Uiso 1 1 calc R . . C2 C -0.3575(5) 0.4177(5) 0.8333(3) 0.084(2) Uani 1 1 d . . . H2 H -0.3496 0.4307 0.8781 0.100 Uiso 1 1 calc R . . C3 C -0.3517(4) 0.4738(3) 0.7844(3) 0.0599(17) Uani 1 1 d . . . C4 C -0.3652(3) 0.4511(4) 0.7181(3) 0.0583(16) Uani 1 1 d . . . C5 C -0.3810(3) 0.3763(4) 0.7011(3) 0.0570(16) Uani 1 1 d . . . C6 C -0.3849(4) 0.3234(4) 0.7517(3) 0.0723(19) Uani 1 1 d . . . H6 H -0.3947 0.2728 0.7408 0.087 Uiso 1 1 calc R . . C7 C -0.3341(4) 0.5543(4) 0.8033(3) 0.078(2) Uani 1 1 d . . . H7A H -0.3542 0.5645 0.8474 0.093 Uiso 1 1 calc R . . H7B H -0.3611 0.5881 0.7717 0.093 Uiso 1 1 calc RD . . C8 C -0.2448(5) 0.5696(3) 0.8034(4) 0.072(2) Uani 1 1 d . . . C9 C -0.1979(6) 0.5497(4) 0.8594(4) 0.088(2) Uani 1 1 d . . . H9 H -0.2228 0.5307 0.8969 0.105 Uiso 1 1 calc R . . C10 C -0.1146(6) 0.5572(4) 0.8613(4) 0.096(2) Uani 1 1 d . . . H10 H -0.0847 0.5447 0.8997 0.116 Uiso 1 1 calc R . . C11 C -0.0782(5) 0.5834(4) 0.8053(5) 0.085(2) Uani 1 1 d . . . H11 H -0.0229 0.5872 0.8054 0.102 Uiso 1 1 calc R . . C12 C -0.1217(5) 0.6039(3) 0.7493(4) 0.0708(19) Uani 1 1 d . . . C13 C -0.2046(5) 0.5986(3) 0.7498(4) 0.0655(17) Uani 1 1 d . . . C14 C -0.0793(4) 0.6279(3) 0.6874(4) 0.081(2) Uani 1 1 d . . . H14A H -0.0325 0.6572 0.7005 0.098 Uiso 1 1 calc R . . H14B H -0.1143 0.6604 0.6606 0.098 Uiso 1 1 calc R . . C15 C -0.0539(4) 0.5603(3) 0.6450(3) 0.0600(16) Uani 1 1 d . . . C16 C 0.0225(4) 0.5329(4) 0.6499(4) 0.0732(19) Uani 1 1 d . . . H16 H 0.0586 0.5569 0.6791 0.088 Uiso 1 1 calc R . . C17 C 0.0479(4) 0.4729(4) 0.6146(4) 0.0747(19) Uani 1 1 d . . . H17 H 0.1004 0.4563 0.6196 0.090 Uiso 1 1 calc R . . C18 C -0.0049(5) 0.4362(4) 0.5706(4) 0.077(2) Uani 1 1 d . . . H18 H 0.0120 0.3943 0.5464 0.092 Uiso 1 1 calc R . . C19 C -0.0842(4) 0.4623(4) 0.5626(3) 0.0604(17) Uani 1 1 d U . . C20 C -0.1072(4) 0.5250(3) 0.6008(3) 0.0556(16) Uani 1 1 d U . . C21 C -0.1403(4) 0.4241(4) 0.5107(3) 0.0700(19) Uani 1 1 d . . . H21A H -0.1086 0.4007 0.4765 0.084 Uiso 1 1 calc R . . H21B H -0.1733 0.4628 0.4892 0.084 Uiso 1 1 calc R . . C22 C -0.1950(4) 0.3631(4) 0.5405(3) 0.0614(17) Uani 1 1 d . . . C23 C -0.1746(4) 0.2879(4) 0.5410(3) 0.083(2) Uani 1 1 d . . . H23 H -0.1266 0.2736 0.5224 0.099 Uiso 1 1 calc R . . C24 C -0.2217(5) 0.2327(4) 0.5676(4) 0.096(3) Uani 1 1 d . . . H24 H -0.2062 0.1820 0.5673 0.116 Uiso 1 1 calc R . . C25 C -0.2922(5) 0.2545(4) 0.5946(3) 0.080(2) Uani 1 1 d . . . H25 H -0.3247 0.2173 0.6127 0.096 Uiso 1 1 calc R . . C26 C -0.3173(4) 0.3291(4) 0.5963(3) 0.0614(17) Uani 1 1 d . . . C27 C -0.2670(4) 0.3845(3) 0.5684(3) 0.0553(15) Uani 1 1 d . . . C28 C -0.3938(3) 0.3514(3) 0.6292(3) 0.0648(17) Uani 1 1 d . . . H28A H -0.4188 0.3925 0.6039 0.078 Uiso 1 1 calc RD . . H28B H -0.4301 0.3085 0.6278 0.078 Uiso 1 1 calc R . . C29 C 0.1856(6) 0.1723(9) 0.4994(5) 0.122(4) Uani 1 1 d . . . C30 C 0.1136(10) 0.2066(8) 0.4845(5) 0.170(5) Uani 1 1 d . . . H30 H 0.1101 0.2534 0.4631 0.204 Uiso 1 1 calc R . . C31 C 0.0417(10) 0.1640(13) 0.5048(8) 0.197(9) Uani 1 1 d U . . H31 H -0.0094 0.1833 0.4973 0.236 Uiso 1 1 calc R . . C32 C 0.0544(12) 0.0939(12) 0.5355(9) 0.197(8) Uani 1 1 d U . . H32 H 0.0088 0.0664 0.5450 0.236 Uiso 1 1 calc R . . C33 C 0.1213(8) 0.0619(10) 0.5525(7) 0.145(6) Uani 1 1 d U . . C34 C 0.1900(10) 0.1015(8) 0.5318(6) 0.138(5) Uani 1 1 d . . . C35 C 0.1299(7) -0.0078(7) 0.5933(7) 0.181(6) Uani 1 1 d . . . H35A H 0.1801 -0.0324 0.5840 0.217 Uiso 1 1 calc R . . H35B H 0.0871 -0.0428 0.5816 0.217 Uiso 1 1 calc R . . C36 C 0.1275(4) 0.0115(3) 0.6664(3) 0.129(4) Uani 1 1 d G . . C37 C 0.1971(3) 0.0298(3) 0.7023(4) 0.120(4) Uani 1 1 d G . . C38 C 0.1934(3) 0.0530(3) 0.7687(3) 0.101(3) Uani 1 1 d G . . C39 C 0.1201(4) 0.0577(3) 0.7991(3) 0.094(2) Uani 1 1 d G . . H39 H 0.1176 0.0732 0.8436 0.112 Uiso 1 1 calc R . . C40 C 0.0505(3) 0.0394(3) 0.7632(3) 0.106(3) Uani 1 1 d G . . H40 H 0.0015 0.0426 0.7835 0.127 Uiso 1 1 calc R . . C41 C 0.0542(3) 0.0162(3) 0.6968(3) 0.115(3) Uani 1 1 d G . . H41 H 0.0077 0.0040 0.6727 0.137 Uiso 1 1 calc R . . C42 C 0.2693(5) 0.0683(4) 0.8100(5) 0.118(3) Uani 1 1 d . . . H42A H 0.3111 0.0352 0.7943 0.141 Uiso 1 1 calc R . . H42B H 0.2601 0.0551 0.8563 0.141 Uiso 1 1 calc R . . C43 C 0.2988(5) 0.1503(5) 0.8075(5) 0.091(2) Uani 1 1 d . . . C44 C 0.2825(6) 0.1982(7) 0.8566(5) 0.116(3) Uani 1 1 d . . . H44 H 0.2517 0.1818 0.8917 0.139 Uiso 1 1 calc R . . C45 C 0.3097(6) 0.2703(7) 0.8565(4) 0.135(4) Uani 1 1 d . . . H45 H 0.2984 0.3029 0.8916 0.161 Uiso 1 1 calc R . . C46 C 0.3550(5) 0.2954(5) 0.8035(4) 0.109(3) Uani 1 1 d . . . H46 H 0.3748 0.3448 0.8043 0.131 Uiso 1 1 calc R . . C47 C 0.3709(4) 0.2499(4) 0.7510(4) 0.0745(19) Uani 1 1 d . . . C48 C 0.3432(4) 0.1751(5) 0.7528(4) 0.077(2) Uani 1 1 d . . . C49 C 0.4177(4) 0.2779(4) 0.6919(3) 0.0767(19) Uani 1 1 d . . . H49A H 0.4505 0.3208 0.7060 0.092 Uiso 1 1 calc R . . H49B H 0.4529 0.2378 0.6775 0.092 Uiso 1 1 calc R . . C50 C 0.3639(4) 0.3018(3) 0.6337(3) 0.0589(17) Uani 1 1 d . . . C51 C 0.3344(5) 0.3745(4) 0.6307(4) 0.076(2) Uani 1 1 d . . . H51 H 0.3487 0.4090 0.6642 0.091 Uiso 1 1 calc R . . C52 C 0.2850(6) 0.3968(4) 0.5798(5) 0.098(3) Uani 1 1 d . . . H52 H 0.2666 0.4466 0.5780 0.118 Uiso 1 1 calc R . . C53 C 0.2622(5) 0.3466(5) 0.5315(4) 0.086(2) Uani 1 1 d . . . H53 H 0.2270 0.3623 0.4974 0.103 Uiso 1 1 calc R . . C54 C 0.2892(5) 0.2752(4) 0.5318(3) 0.075(2) Uani 1 1 d . . . C55 C 0.3395(4) 0.2532(4) 0.5831(4) 0.072(2) Uani 1 1 d . . . C56 C 0.2600(6) 0.2201(5) 0.4785(3) 0.114(3) Uani 1 1 d . . . H56A H 0.3031 0.1856 0.4682 0.136 Uiso 1 1 calc RD . . H56B H 0.2462 0.2483 0.4380 0.136 Uiso 1 1 calc R . . C57 C -0.0416(4) 0.1773(3) 0.8711(3) 0.0548(15) Uani 1 1 d . . . H57 H -0.0833 0.1526 0.8484 0.066 Uiso 1 1 calc R A . C58 C 0.0450(6) 0.2075(4) 0.9475(3) 0.111(3) Uani 1 1 d . . . H58 H 0.0755 0.2086 0.9872 0.133 Uiso 1 1 calc R A . C59 C 0.0533(6) 0.2527(4) 0.8954(4) 0.105(3) Uani 1 1 d . A . H59 H 0.0907 0.2915 0.8927 0.126 Uiso 1 1 calc R . . C60 C -0.0435(4) 0.0965(3) 0.9748(3) 0.0662(18) Uani 1 1 d . . . H60A H -0.0953 0.0794 0.9581 0.079 Uiso 1 1 calc R A . H60B H -0.0495 0.1147 1.0203 0.079 Uiso 1 1 calc R . . C61 C 0.0133(4) 0.0310(3) 0.9756(2) 0.0570(16) Uani 1 1 d . . . H61A H 0.0662 0.0486 0.9890 0.068 Uiso 1 1 calc R . . H61B H 0.0159 0.0098 0.9309 0.068 Uiso 1 1 calc R . . C62 C 0.1149(8) 0.2339(7) 0.6679(6) 0.168(4) Uani 1 1 d DU . . H62A H 0.1167 0.2489 0.6212 0.202 Uiso 1 1 calc R A . H62B H 0.1455 0.1873 0.6723 0.202 Uiso 1 1 calc R . . C63 C 0.1575(7) 0.2905(8) 0.7056(7) 0.173(4) Uani 1 1 d DU A . N1 N -0.0013(3) 0.2339(3) 0.8461(2) 0.0613(14) Uani 1 1 d . A . N2 N -0.0157(3) 0.1594(3) 0.9326(2) 0.0635(14) Uani 1 1 d . A . N3 N 0.0344(6) 0.2148(4) 0.6800(4) 0.153(3) Uani 1 1 d U A . H3A H 0.0298 0.1657 0.6920 0.183 Uiso 1 1 d R . . H3B H 0.0049 0.2221 0.6422 0.183 Uiso 1 1 d R . . N4 N 0.1153(9) 0.3127(11) 0.7509(7) 0.107(5) Uani 0.55 1 d P A . N4' N 0.1024(14) 0.3520(10) 0.7506(11) 0.102(8) Uiso 0.45 1 d P A . C64 C -0.1797(6) 0.3255(6) 0.7660(6) 0.092(3) Uani 0.75(2) 1 d PU A 1 C65 C -0.1456(7) 0.3895(7) 0.7365(8) 0.091(3) Uani 0.75(2) 1 d PU A 1 N5 N -0.0529(6) 0.3921(4) 0.7527(7) 0.093(4) Uani 0.75(2) 1 d P A 1 N6 N -0.1422(6) 0.2599(5) 0.7389(6) 0.088(3) Uani 0.75(2) 1 d PU A 1 C64' C -0.170(2) 0.339(2) 0.715(2) 0.093(13) Uiso 0.25(2) 1 d P A 2 C65' C -0.131(3) 0.391(2) 0.780(2) 0.108(14) Uiso 0.25(2) 1 d P A 2 N5' N -0.069(3) 0.389(2) 0.787(2) 0.116(15) Uiso 0.25(2) 1 d P A 2 N6' N -0.114(2) 0.2562(16) 0.7092(15) 0.097(11) Uiso 0.25(2) 1 d P A 2 O1 O -0.1837(3) 0.5493(2) 0.5940(2) 0.0716(12) Uani 1 1 d . . . H1A H -0.1903 0.5858 0.6187 0.107 Uiso 1 1 calc R . . O2 O -0.2888(2) 0.4583(2) 0.56816(19) 0.0680(12) Uani 1 1 d . . . H2A H -0.3320 0.4627 0.5859 0.102 Uiso 1 1 calc RD . . O3 O -0.3655(3) 0.5064(2) 0.6697(2) 0.0743(13) Uani 1 1 d . . . O4 O -0.2475(3) 0.6250(2) 0.6950(2) 0.0882(14) Uani 1 1 d . . . H4 H -0.2953 0.6200 0.7012 0.132 Uiso 1 1 calc RD . . O5 O 0.3717(4) 0.1804(3) 0.5861(3) 0.136(2) Uani 1 1 d . . . H5 H 0.3550 0.1556 0.5539 0.204 Uiso 1 1 calc RD . . O6 O 0.3621(3) 0.1278(3) 0.7024(3) 0.0978(17) Uani 1 1 d . . . H6A H 0.3428 0.0857 0.7090 0.147 Uiso 1 1 calc R . . O7 O 0.2657(4) 0.0252(3) 0.6719(4) 0.168(3) Uani 1 1 d D . . O8 O 0.2601(5) 0.0685(4) 0.5391(3) 0.137(3) Uani 1 1 d . . . H8 H 0.2946 0.0965 0.5246 0.206 Uiso 1 1 calc RD . . O1W O 0.3914(6) -0.0717(5) 0.6273(5) 0.100(3) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0635(5) 0.0603(4) 0.0539(4) 0.0091(4) -0.0003(3) 0.0132(4) C1 0.125(8) 0.078(5) 0.078(5) 0.020(4) -0.013(5) -0.015(5) C2 0.094(6) 0.100(6) 0.057(4) 0.005(4) -0.008(4) 0.003(5) C3 0.047(4) 0.062(4) 0.071(4) 0.001(4) 0.006(3) 0.006(3) C4 0.036(4) 0.068(4) 0.072(4) 0.016(4) 0.006(3) 0.008(3) C5 0.035(4) 0.073(4) 0.063(4) 0.013(4) -0.008(3) -0.003(3) C6 0.070(5) 0.074(4) 0.072(5) 0.015(4) -0.014(4) -0.011(4) C7 0.063(5) 0.077(5) 0.094(5) -0.008(4) 0.010(4) 0.006(4) C8 0.082(6) 0.054(4) 0.080(5) -0.009(4) 0.004(5) -0.001(4) C9 0.094(7) 0.080(5) 0.089(6) -0.022(4) 0.005(6) 0.007(5) C10 0.098(8) 0.097(6) 0.092(6) -0.013(5) -0.029(6) 0.020(5) C11 0.072(6) 0.075(5) 0.107(6) -0.005(5) -0.023(6) -0.001(4) C12 0.070(6) 0.048(4) 0.094(5) -0.009(4) -0.002(5) -0.006(4) C13 0.060(5) 0.045(4) 0.090(5) 0.002(3) -0.022(5) 0.006(3) C14 0.059(5) 0.059(4) 0.126(6) 0.010(4) -0.013(4) -0.019(3) C15 0.039(4) 0.062(4) 0.079(4) 0.024(3) -0.007(4) -0.012(3) C16 0.047(5) 0.076(5) 0.097(5) 0.013(4) 0.000(4) -0.014(4) C17 0.038(4) 0.094(5) 0.092(5) 0.022(4) -0.003(4) -0.009(4) C18 0.067(6) 0.085(5) 0.081(5) 0.020(4) 0.026(5) 0.006(4) C19 0.050(5) 0.079(4) 0.053(4) 0.027(3) -0.005(3) -0.016(4) C20 0.046(5) 0.058(4) 0.063(4) 0.022(3) -0.001(4) 0.008(3) C21 0.063(5) 0.090(4) 0.057(4) 0.016(4) 0.010(4) -0.006(4) C22 0.064(5) 0.079(5) 0.041(3) 0.004(3) -0.001(3) -0.006(4) C23 0.080(6) 0.087(5) 0.082(4) 0.000(4) 0.023(4) 0.016(5) C24 0.122(8) 0.068(5) 0.101(5) 0.003(4) 0.030(5) 0.000(5) C25 0.092(6) 0.070(4) 0.079(5) 0.010(4) 0.019(4) -0.023(4) C26 0.060(5) 0.070(4) 0.054(3) 0.008(3) -0.012(3) -0.018(4) C27 0.059(5) 0.062(4) 0.044(3) 0.006(3) -0.011(3) -0.004(3) C28 0.044(4) 0.083(4) 0.067(4) 0.013(3) -0.007(3) -0.013(3) C29 0.060(7) 0.219(13) 0.086(6) -0.083(8) -0.010(6) 0.022(8) C30 0.143(13) 0.277(16) 0.089(7) -0.074(8) -0.001(8) -0.013(13) C31 0.092(10) 0.34(2) 0.157(13) -0.109(14) -0.034(9) 0.048(15) C32 0.122(12) 0.28(2) 0.189(16) -0.128(14) -0.023(12) -0.037(13) C33 0.085(8) 0.199(14) 0.151(10) -0.093(10) 0.026(8) -0.055(10) C34 0.182(16) 0.116(9) 0.117(8) -0.065(7) 0.005(9) 0.015(10) C35 0.167(12) 0.125(9) 0.256(14) -0.087(10) 0.095(11) -0.092(8) C36 0.104(8) 0.084(6) 0.202(10) -0.057(6) 0.067(8) -0.046(5) C37 0.061(6) 0.060(5) 0.241(12) -0.013(6) 0.061(8) -0.011(4) C38 0.045(5) 0.061(5) 0.196(9) 0.055(5) 0.020(6) 0.009(4) C39 0.056(5) 0.086(5) 0.139(6) 0.042(5) 0.017(5) -0.003(4) C40 0.052(6) 0.089(5) 0.177(9) 0.011(6) 0.024(6) -0.015(4) C41 0.067(6) 0.097(6) 0.181(9) -0.033(6) 0.016(6) -0.038(5) C42 0.043(5) 0.118(6) 0.191(9) 0.097(6) -0.020(5) -0.006(4) C43 0.050(5) 0.123(7) 0.098(6) 0.060(6) -0.018(5) -0.012(5) C44 0.084(7) 0.175(10) 0.088(6) 0.064(7) -0.016(5) -0.031(7) C45 0.138(10) 0.197(11) 0.068(5) 0.024(7) 0.005(5) -0.035(8) C46 0.122(8) 0.125(7) 0.079(5) 0.016(5) -0.024(5) -0.040(6) C47 0.049(5) 0.092(5) 0.081(5) 0.024(4) -0.031(4) -0.020(4) C48 0.038(4) 0.088(5) 0.103(6) 0.027(5) -0.022(4) 0.001(4) C49 0.058(5) 0.074(4) 0.098(5) 0.017(4) -0.009(4) -0.020(4) C50 0.053(4) 0.057(4) 0.068(4) 0.011(3) 0.010(4) -0.002(3) C51 0.096(6) 0.054(4) 0.077(5) 0.005(4) 0.009(5) 0.002(4) C52 0.135(9) 0.061(5) 0.098(6) 0.022(5) -0.006(6) 0.021(5) C53 0.098(7) 0.087(6) 0.071(5) 0.031(5) -0.007(4) 0.012(5) C54 0.087(6) 0.094(6) 0.043(4) 0.003(4) 0.005(4) 0.017(5) C55 0.072(5) 0.056(4) 0.088(5) -0.006(4) 0.015(5) 0.018(4) C56 0.122(8) 0.157(8) 0.062(4) -0.024(5) -0.004(5) 0.017(7) C57 0.060(5) 0.059(4) 0.045(3) 0.010(3) -0.011(3) 0.000(3) C58 0.166(9) 0.091(5) 0.072(4) 0.031(4) -0.064(5) -0.059(6) C59 0.150(9) 0.075(5) 0.084(5) 0.041(4) -0.058(5) -0.056(5) C60 0.080(5) 0.063(4) 0.056(3) 0.018(3) 0.003(3) -0.007(4) C61 0.069(5) 0.058(4) 0.044(3) 0.013(3) -0.001(3) -0.006(3) C62 0.163(9) 0.176(8) 0.168(7) -0.011(6) 0.077(7) 0.067(7) C63 0.109(9) 0.204(10) 0.208(10) 0.017(8) 0.047(8) 0.053(8) N1 0.072(4) 0.054(3) 0.057(3) 0.016(2) -0.012(3) -0.007(3) N2 0.073(4) 0.056(3) 0.060(3) 0.015(3) -0.017(3) -0.012(3) N3 0.207(9) 0.125(5) 0.131(5) -0.002(4) 0.079(6) 0.036(6) N4 0.075(10) 0.144(15) 0.104(10) -0.040(10) 0.027(8) -0.008(10) C64 0.067(5) 0.092(5) 0.115(7) 0.006(4) 0.000(4) 0.010(3) C65 0.068(5) 0.091(5) 0.115(7) 0.008(4) -0.001(4) 0.014(4) N5 0.119(9) 0.041(4) 0.121(8) 0.013(5) 0.028(7) 0.008(4) N6 0.065(5) 0.089(5) 0.111(7) 0.002(4) 0.000(4) 0.004(3) O1 0.058(3) 0.069(3) 0.087(3) 0.014(2) -0.019(2) 0.004(2) O2 0.045(3) 0.081(3) 0.079(3) 0.024(2) 0.003(2) 0.001(2) O3 0.072(3) 0.065(3) 0.086(3) 0.019(2) 0.004(3) 0.009(2) O4 0.051(3) 0.089(3) 0.124(4) 0.015(3) -0.015(3) -0.005(3) O5 0.147(6) 0.097(4) 0.161(5) -0.050(4) -0.054(4) 0.055(4) O6 0.052(3) 0.068(3) 0.173(5) 0.032(3) 0.007(3) -0.004(2) O7 0.084(5) 0.099(4) 0.325(9) -0.069(5) 0.098(6) -0.019(3) O8 0.120(6) 0.111(5) 0.184(6) -0.035(4) 0.039(5) -0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.016(4) . ? Zn1 N6' 2.03(3) . ? Zn1 N5 2.057(7) . ? Zn1 N3 2.067(6) . ? Zn1 N4 2.137(14) . ? Zn1 N4' 2.22(2) . ? Zn1 N5' 2.22(4) . ? Zn1 N6 2.300(9) . ? C1 C6 1.344(9) . ? C1 C2 1.389(9) . ? C1 H1 0.9300 . ? C2 C3 1.394(8) . ? C2 H2 0.9300 . ? C3 C4 1.396(8) . ? C3 C7 1.493(8) . ? C4 O3 1.371(6) . ? C4 C5 1.383(8) . ? C5 C6 1.377(8) . ? C5 C28 1.511(8) . ? C6 H6 0.9300 . ? C7 C8 1.523(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.379(9) . ? C8 C9 1.392(10) . ? C9 C10 1.404(10) . ? C9 H9 0.9300 . ? C10 C11 1.369(10) . ? C10 H10 0.9300 . ? C11 C12 1.365(10) . ? C11 H11 0.9300 . ? C12 C13 1.394(9) . ? C12 C14 1.504(9) . ? C13 O4 1.373(7) . ? C14 C15 1.530(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.371(9) . ? C15 C20 1.384(8) . ? C16 C17 1.345(9) . ? C16 H16 0.9300 . ? C17 C18 1.389(9) . ? C17 H17 0.9300 . ? C18 C19 1.412(9) . ? C18 H18 0.9300 . ? C19 C20 1.402(8) . ? C19 C21 1.534(8) . ? C20 O1 1.355(7) . ? C21 C22 1.542(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.367(8) . ? C22 C27 1.397(8) . ? C23 C24 1.369(9) . ? C23 H23 0.9300 . ? C24 C25 1.370(9) . ? C24 H24 0.9300 . ? C25 C26 1.380(8) . ? C25 H25 0.9300 . ? C26 C27 1.415(8) . ? C26 C28 1.511(8) . ? C27 O2 1.349(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.375(16) . ? C29 C34 1.405(14) . ? C29 C56 1.573(13) . ? C30 C31 1.49(2) . ? C30 H30 0.9300 . ? C31 C32 1.39(2) . ? C31 H31 0.9300 . ? C32 C33 1.29(2) . ? C32 H32 0.9300 . ? C33 C34 1.417(16) . ? C33 C35 1.478(18) . ? C34 O8 1.316(14) . ? C35 C36 1.500(12) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.3900 . ? C36 C41 1.3900 . ? C37 O7 1.320(6) . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C38 C42 1.520(9) . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 C41 1.3900 . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.528(11) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.328(11) . ? C43 C48 1.410(10) . ? C44 C45 1.348(12) . ? C44 H44 0.9300 . ? C45 C46 1.392(11) . ? C45 H45 0.9300 . ? C46 C47 1.353(10) . ? C46 H46 0.9300 . ? C47 C48 1.398(9) . ? C47 C49 1.520(9) . ? C48 O6 1.351(8) . ? C49 C50 1.510(9) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.373(8) . ? C50 C55 1.376(9) . ? C51 C52 1.349(10) . ? C51 H51 0.9300 . ? C52 C53 1.354(10) . ? C52 H52 0.9300 . ? C53 C54 1.337(9) . ? C53 H53 0.9300 . ? C54 C55 1.364(9) . ? C54 C56 1.510(10) . ? C55 O5 1.390(8) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 N1 1.311(7) . ? C57 N2 1.329(7) . ? C57 H57 0.9300 . ? C58 C59 1.321(8) . ? C58 N2 1.351(8) . ? C58 H58 0.9300 . ? C59 N1 1.365(8) . ? C59 H59 0.9300 . ? C60 N2 1.476(7) . ? C60 C61 1.494(8) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C61 1.536(9) 3_557 ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 N3 1.419(14) . ? C62 C63 1.427(9) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 N4 1.229(16) . ? C63 N4' 1.70(2) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 N4' 0.73(2) . ? C64 C65 1.401(18) . ? C64 N6 1.430(13) . ? C65 N5 1.580(15) . ? C64' C65' 1.70(7) . ? C64' N6' 1.74(5) . ? C65' N5' 1.05(6) . ? O1 H1A 0.8200 . ? O2 H2A 0.8200 . ? O4 H4 0.8200 . ? O5 H5 0.8200 . ? O6 H6A 0.8200 . ? O8 H8 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N6' 109.3(9) . . ? N1 Zn1 N5 115.6(4) . . ? N6' Zn1 N5 84.0(9) . . ? N1 Zn1 N3 113.0(3) . . ? N6' Zn1 N3 81.4(10) . . ? N5 Zn1 N3 131.4(5) . . ? N1 Zn1 N4 96.4(5) . . ? N6' Zn1 N4 150.9(10) . . ? N5 Zn1 N4 97.3(6) . . ? N3 Zn1 N4 76.0(5) . . ? N1 Zn1 N4' 104.3(6) . . ? N6' Zn1 N4' 146.2(10) . . ? N5 Zn1 N4' 78.3(6) . . ? N3 Zn1 N4' 89.0(6) . . ? N4 Zn1 N4' 19.1(6) . . ? N1 Zn1 N5' 96.4(11) . . ? N6' Zn1 N5' 85.6(15) . . ? N5 Zn1 N5' 19.8(9) . . ? N3 Zn1 N5' 150.4(11) . . ? N4 Zn1 N5' 105.3(14) . . ? N4' Zn1 N5' 87.1(14) . . ? N1 Zn1 N6 94.4(3) . . ? N6' Zn1 N6 19.3(8) . . ? N5 Zn1 N6 79.0(4) . . ? N3 Zn1 N6 98.6(4) . . ? N4 Zn1 N6 169.1(5) . . ? N4' Zn1 N6 155.1(6) . . ? N5' Zn1 N6 74.6(13) . . ? C6 C1 C2 119.5(7) . . ? C6 C1 H1 120.3 . . ? C2 C1 H1 120.3 . . ? C1 C2 C3 121.5(6) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 116.7(6) . . ? C2 C3 C7 120.9(6) . . ? C4 C3 C7 122.4(6) . . ? O3 C4 C5 120.5(6) . . ? O3 C4 C3 117.6(6) . . ? C5 C4 C3 121.9(5) . . ? C6 C5 C4 118.5(6) . . ? C6 C5 C28 119.5(6) . . ? C4 C5 C28 122.0(5) . . ? C1 C6 C5 121.8(6) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C3 C7 C8 110.8(5) . . ? C3 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C13 C8 C9 116.1(8) . . ? C13 C8 C7 124.6(8) . . ? C9 C8 C7 119.2(7) . . ? C8 C9 C10 122.3(8) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C11 C10 C9 118.6(8) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C12 C11 C10 121.2(8) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 119.0(7) . . ? C11 C12 C14 119.6(8) . . ? C13 C12 C14 121.4(7) . . ? O4 C13 C8 119.2(7) . . ? O4 C13 C12 118.0(7) . . ? C8 C13 C12 122.8(7) . . ? C12 C14 C15 112.5(5) . . ? C12 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? C12 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C20 118.2(6) . . ? C16 C15 C14 120.6(7) . . ? C20 C15 C14 121.2(6) . . ? C17 C16 C15 123.3(7) . . ? C17 C16 H16 118.3 . . ? C15 C16 H16 118.3 . . ? C16 C17 C18 119.4(7) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C17 C18 C19 120.1(7) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 117.9(6) . . ? C20 C19 C21 122.6(6) . . ? C18 C19 C21 119.4(6) . . ? O1 C20 C15 120.8(6) . . ? O1 C20 C19 118.0(6) . . ? C15 C20 C19 121.2(6) . . ? C19 C21 C22 113.9(4) . . ? C19 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? C19 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C27 118.6(5) . . ? C23 C22 C21 121.6(6) . . ? C27 C22 C21 119.8(6) . . ? C22 C23 C24 122.8(6) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C23 C24 C25 118.1(6) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? C24 C25 C26 122.9(6) . . ? C24 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C25 C26 C27 117.4(6) . . ? C25 C26 C28 121.4(5) . . ? C27 C26 C28 121.1(6) . . ? O2 C27 C22 119.7(5) . . ? O2 C27 C26 120.0(5) . . ? C22 C27 C26 120.3(6) . . ? C5 C28 C26 113.0(5) . . ? C5 C28 H28A 109.0 . . ? C26 C28 H28A 109.0 . . ? C5 C28 H28B 109.0 . . ? C26 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C34 121.5(14) . . ? C30 C29 C56 114.0(14) . . ? C34 C29 C56 124.5(11) . . ? C29 C30 C31 115.8(15) . . ? C29 C30 H30 122.1 . . ? C31 C30 H30 122.1 . . ? C32 C31 C30 116.9(17) . . ? C32 C31 H31 121.6 . . ? C30 C31 H31 121.6 . . ? C33 C32 C31 128(2) . . ? C33 C32 H32 115.8 . . ? C31 C32 H32 115.8 . . ? C32 C33 C34 114.6(19) . . ? C32 C33 C35 125.2(16) . . ? C34 C33 C35 120.1(14) . . ? O8 C34 C29 118.5(13) . . ? O8 C34 C33 118.8(14) . . ? C29 C34 C33 122.6(15) . . ? C33 C35 C36 110.1(8) . . ? C33 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? C33 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.2 . . ? C37 C36 C41 120.0 . . ? C37 C36 C35 120.6(6) . . ? C41 C36 C35 119.2(7) . . ? O7 C37 C38 121.4(6) . . ? O7 C37 C36 118.6(6) . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 C42 120.5(6) . . ? C39 C38 C42 119.3(6) . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C36 120.0 . . ? C40 C41 H41 120.0 . . ? C36 C41 H41 120.0 . . ? C38 C42 C43 114.6(6) . . ? C38 C42 H42A 108.6 . . ? C43 C42 H42A 108.6 . . ? C38 C42 H42B 108.6 . . ? C43 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C44 C43 C48 120.1(8) . . ? C44 C43 C42 120.1(8) . . ? C48 C43 C42 119.8(9) . . ? C43 C44 C45 121.3(9) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C44 C45 C46 119.5(10) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C47 C46 C45 121.7(9) . . ? C47 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C46 C47 C48 117.8(7) . . ? C46 C47 C49 121.9(7) . . ? C48 C47 C49 120.3(7) . . ? O6 C48 C47 118.5(6) . . ? O6 C48 C43 121.9(8) . . ? C47 C48 C43 119.6(8) . . ? C50 C49 C47 112.2(5) . . ? C50 C49 H49A 109.2 . . ? C47 C49 H49A 109.2 . . ? C50 C49 H49B 109.2 . . ? C47 C49 H49B 109.2 . . ? H49A C49 H49B 107.9 . . ? C51 C50 C55 116.7(7) . . ? C51 C50 C49 119.9(6) . . ? C55 C50 C49 123.4(6) . . ? C52 C51 C50 121.1(7) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C53 120.0(7) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 121.5(7) . . ? C54 C53 H53 119.3 . . ? C52 C53 H53 119.3 . . ? C53 C54 C55 118.2(7) . . ? C53 C54 C56 119.9(8) . . ? C55 C54 C56 121.8(7) . . ? C54 C55 C50 122.6(6) . . ? C54 C55 O5 121.7(7) . . ? C50 C55 O5 115.8(7) . . ? C54 C56 C29 113.5(6) . . ? C54 C56 H56A 108.9 . . ? C29 C56 H56A 108.9 . . ? C54 C56 H56B 108.9 . . ? C29 C56 H56B 108.9 . . ? H56A C56 H56B 107.7 . . ? N1 C57 N2 111.9(6) . . ? N1 C57 H57 124.0 . . ? N2 C57 H57 124.0 . . ? C59 C58 N2 107.5(6) . . ? C59 C58 H58 126.2 . . ? N2 C58 H58 126.2 . . ? C58 C59 N1 109.7(6) . . ? C58 C59 H59 125.1 . . ? N1 C59 H59 125.1 . . ? N2 C60 C61 111.9(5) . . ? N2 C60 H60A 109.2 . . ? C61 C60 H60A 109.2 . . ? N2 C60 H60B 109.2 . . ? C61 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? C60 C61 C61 111.0(6) . 3_557 ? C60 C61 H61A 109.4 . . ? C61 C61 H61A 109.4 3_557 . ? C60 C61 H61B 109.4 . . ? C61 C61 H61B 109.4 3_557 . ? H61A C61 H61B 108.0 . . ? N3 C62 C63 122.6(10) . . ? N3 C62 H62A 106.7 . . ? C63 C62 H62A 106.7 . . ? N3 C62 H62B 106.7 . . ? C63 C62 H62B 106.7 . . ? H62A C62 H62B 106.6 . . ? N4 C63 C62 108.7(13) . . ? N4 C63 N4' 22.1(12) . . ? C62 C63 N4' 116.9(12) . . ? C57 N1 C59 104.7(5) . . ? C57 N1 Zn1 130.9(5) . . ? C59 N1 Zn1 124.3(4) . . ? C57 N2 C58 106.2(5) . . ? C57 N2 C60 127.3(6) . . ? C58 N2 C60 126.4(6) . . ? C62 N3 Zn1 109.6(7) . . ? C62 N3 H3A 111.2 . . ? Zn1 N3 H3A 109.5 . . ? C62 N3 H3B 108.8 . . ? Zn1 N3 H3B 109.5 . . ? H3A N3 H3B 108.2 . . ? N4' N4 C63 118(3) . . ? N4' N4 Zn1 87(3) . . ? C63 N4 Zn1 122.1(12) . . ? N4 N4' C63 40(2) . . ? N4 N4' Zn1 74(3) . . ? C63 N4' Zn1 98.2(10) . . ? C65 C64 N6 107.4(9) . . ? C64 C65 N5 110.4(9) . . ? C65 N5 Zn1 109.5(6) . . ? C64 N6 Zn1 104.0(6) . . ? C65' C64' N6' 108(3) . . ? N5' C65' C64' 117(4) . . ? C65' N5' Zn1 116(4) . . ? C64' N6' Zn1 103.9(18) . . ? C20 O1 H1A 109.5 . . ? C27 O2 H2A 109.5 . . ? C13 O4 H4 109.5 . . ? C55 O5 H5 109.5 . . ? C48 O6 H6A 109.5 . . ? C34 O8 H8 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.2(12) . . . . ? C1 C2 C3 C4 0.9(10) . . . . ? C1 C2 C3 C7 179.2(7) . . . . ? C2 C3 C4 O3 175.4(5) . . . . ? C7 C3 C4 O3 -2.8(8) . . . . ? C2 C3 C4 C5 -2.1(9) . . . . ? C7 C3 C4 C5 179.6(5) . . . . ? O3 C4 C5 C6 -176.2(5) . . . . ? C3 C4 C5 C6 1.3(9) . . . . ? O3 C4 C5 C28 3.9(8) . . . . ? C3 C4 C5 C28 -178.6(5) . . . . ? C2 C1 C6 C5 -2.1(12) . . . . ? C4 C5 C6 C1 0.9(10) . . . . ? C28 C5 C6 C1 -179.2(7) . . . . ? C2 C3 C7 C8 92.2(7) . . . . ? C4 C3 C7 C8 -89.6(8) . . . . ? C3 C7 C8 C13 93.7(7) . . . . ? C3 C7 C8 C9 -82.4(7) . . . . ? C13 C8 C9 C10 -1.0(9) . . . . ? C7 C8 C9 C10 175.5(6) . . . . ? C8 C9 C10 C11 -1.7(10) . . . . ? C9 C10 C11 C12 1.9(10) . . . . ? C10 C11 C12 C13 0.6(10) . . . . ? C10 C11 C12 C14 -176.3(6) . . . . ? C9 C8 C13 O4 -174.9(5) . . . . ? C7 C8 C13 O4 8.9(9) . . . . ? C9 C8 C13 C12 3.5(9) . . . . ? C7 C8 C13 C12 -172.7(6) . . . . ? C11 C12 C13 O4 175.0(5) . . . . ? C14 C12 C13 O4 -8.1(8) . . . . ? C11 C12 C13 C8 -3.4(9) . . . . ? C14 C12 C13 C8 173.4(5) . . . . ? C11 C12 C14 C15 83.4(8) . . . . ? C13 C12 C14 C15 -93.4(7) . . . . ? C12 C14 C15 C16 -98.0(7) . . . . ? C12 C14 C15 C20 81.8(8) . . . . ? C20 C15 C16 C17 -0.9(9) . . . . ? C14 C15 C16 C17 179.0(5) . . . . ? C15 C16 C17 C18 0.1(9) . . . . ? C16 C17 C18 C19 0.8(9) . . . . ? C17 C18 C19 C20 -0.8(8) . . . . ? C17 C18 C19 C21 176.4(5) . . . . ? C16 C15 C20 O1 179.6(5) . . . . ? C14 C15 C20 O1 -0.2(8) . . . . ? C16 C15 C20 C19 0.8(8) . . . . ? C14 C15 C20 C19 -179.1(5) . . . . ? C18 C19 C20 O1 -178.8(4) . . . . ? C21 C19 C20 O1 4.1(7) . . . . ? C18 C19 C20 C15 0.1(7) . . . . ? C21 C19 C20 C15 -177.0(5) . . . . ? C20 C19 C21 C22 -85.8(7) . . . . ? C18 C19 C21 C22 97.2(6) . . . . ? C19 C21 C22 C23 -94.4(7) . . . . ? C19 C21 C22 C27 85.2(7) . . . . ? C27 C22 C23 C24 -0.1(11) . . . . ? C21 C22 C23 C24 179.5(7) . . . . ? C22 C23 C24 C25 0.2(12) . . . . ? C23 C24 C25 C26 -0.2(12) . . . . ? C24 C25 C26 C27 0.1(10) . . . . ? C24 C25 C26 C28 -177.3(7) . . . . ? C23 C22 C27 O2 -179.6(6) . . . . ? C21 C22 C27 O2 0.9(8) . . . . ? C23 C22 C27 C26 0.0(9) . . . . ? C21 C22 C27 C26 -179.6(5) . . . . ? C25 C26 C27 O2 179.5(6) . . . . ? C28 C26 C27 O2 -3.0(8) . . . . ? C25 C26 C27 C22 0.0(9) . . . . ? C28 C26 C27 C22 177.4(5) . . . . ? C6 C5 C28 C26 -90.8(6) . . . . ? C4 C5 C28 C26 89.1(7) . . . . ? C25 C26 C28 C5 94.4(7) . . . . ? C27 C26 C28 C5 -82.9(7) . . . . ? C34 C29 C30 C31 0.0(13) . . . . ? C56 C29 C30 C31 -178.7(8) . . . . ? C29 C30 C31 C32 -1.0(18) . . . . ? C30 C31 C32 C33 4(3) . . . . ? C31 C32 C33 C34 -6(2) . . . . ? C31 C32 C33 C35 171.0(15) . . . . ? C30 C29 C34 O8 173.9(8) . . . . ? C56 C29 C34 O8 -7.5(13) . . . . ? C30 C29 C34 C33 -1.6(14) . . . . ? C56 C29 C34 C33 177.0(8) . . . . ? C32 C33 C34 O8 -171.3(11) . . . . ? C35 C33 C34 O8 11.7(14) . . . . ? C32 C33 C34 C29 4.2(15) . . . . ? C35 C33 C34 C29 -172.8(9) . . . . ? C32 C33 C35 C36 -83.4(15) . . . . ? C34 C33 C35 C36 93.3(11) . . . . ? C33 C35 C36 C37 -88.8(10) . . . . ? C33 C35 C36 C41 86.5(9) . . . . ? C41 C36 C37 O7 -179.5(5) . . . . ? C35 C36 C37 O7 -4.3(8) . . . . ? C41 C36 C37 C38 0.0 . . . . ? C35 C36 C37 C38 175.3(7) . . . . ? O7 C37 C38 C39 179.5(5) . . . . ? C36 C37 C38 C39 0.0 . . . . ? O7 C37 C38 C42 -4.5(6) . . . . ? C36 C37 C38 C42 176.0(5) . . . . ? C37 C38 C39 C40 0.0 . . . . ? C42 C38 C39 C40 -176.1(5) . . . . ? C38 C39 C40 C41 0.0 . . . . ? C39 C40 C41 C36 0.0 . . . . ? C37 C36 C41 C40 0.0 . . . . ? C35 C36 C41 C40 -175.3(7) . . . . ? C37 C38 C42 C43 90.7(8) . . . . ? C39 C38 C42 C43 -93.2(7) . . . . ? C38 C42 C43 C44 98.5(10) . . . . ? C38 C42 C43 C48 -81.4(9) . . . . ? C48 C43 C44 C45 -2.1(14) . . . . ? C42 C43 C44 C45 178.0(8) . . . . ? C43 C44 C45 C46 0.9(15) . . . . ? C44 C45 C46 C47 1.6(15) . . . . ? C45 C46 C47 C48 -2.7(12) . . . . ? C45 C46 C47 C49 177.8(8) . . . . ? C46 C47 C48 O6 -176.6(7) . . . . ? C49 C47 C48 O6 2.9(10) . . . . ? C46 C47 C48 C43 1.5(10) . . . . ? C49 C47 C48 C43 -179.0(6) . . . . ? C44 C43 C48 O6 178.9(7) . . . . ? C42 C43 C48 O6 -1.2(10) . . . . ? C44 C43 C48 C47 0.9(11) . . . . ? C42 C43 C48 C47 -179.2(6) . . . . ? C46 C47 C49 C50 -97.8(8) . . . . ? C48 C47 C49 C50 82.7(8) . . . . ? C47 C49 C50 C51 86.7(7) . . . . ? C47 C49 C50 C55 -90.9(7) . . . . ? C55 C50 C51 C52 -1.0(9) . . . . ? C49 C50 C51 C52 -178.8(6) . . . . ? C50 C51 C52 C53 1.6(11) . . . . ? C51 C52 C53 C54 -1.7(12) . . . . ? C52 C53 C54 C55 1.3(11) . . . . ? C52 C53 C54 C56 177.7(7) . . . . ? C53 C54 C55 C50 -0.7(10) . . . . ? C56 C54 C55 C50 -177.1(6) . . . . ? C53 C54 C55 O5 -178.4(6) . . . . ? C56 C54 C55 O5 5.2(10) . . . . ? C51 C50 C55 C54 0.6(9) . . . . ? C49 C50 C55 C54 178.2(6) . . . . ? C51 C50 C55 O5 178.4(6) . . . . ? C49 C50 C55 O5 -4.0(9) . . . . ? C53 C54 C56 C29 -92.5(9) . . . . ? C55 C54 C56 C29 83.8(11) . . . . ? C30 C29 C56 C54 88.1(9) . . . . ? C34 C29 C56 C54 -90.6(10) . . . . ? N2 C58 C59 N1 -0.6(10) . . . . ? N2 C60 C61 C61 175.3(6) . . . 3_557 ? N3 C62 C63 N4 5(2) . . . . ? N3 C62 C63 N4' -16.9(19) . . . . ? N2 C57 N1 C59 0.0(7) . . . . ? N2 C57 N1 Zn1 176.7(4) . . . . ? C58 C59 N1 C57 0.4(9) . . . . ? C58 C59 N1 Zn1 -176.6(6) . . . . ? N6' Zn1 N1 C57 18.2(11) . . . . ? N5 Zn1 N1 C57 110.7(6) . . . . ? N3 Zn1 N1 C57 -70.5(6) . . . . ? N4 Zn1 N1 C57 -148.0(7) . . . . ? N4' Zn1 N1 C57 -165.6(7) . . . . ? N5' Zn1 N1 C57 105.8(14) . . . . ? N6 Zn1 N1 C57 30.8(6) . . . . ? N6' Zn1 N1 C59 -165.7(11) . . . . ? N5 Zn1 N1 C59 -73.1(7) . . . . ? N3 Zn1 N1 C59 105.7(7) . . . . ? N4 Zn1 N1 C59 28.2(8) . . . . ? N4' Zn1 N1 C59 10.5(8) . . . . ? N5' Zn1 N1 C59 -78.1(15) . . . . ? N6 Zn1 N1 C59 -153.0(6) . . . . ? N1 C57 N2 C58 -0.3(7) . . . . ? N1 C57 N2 C60 -176.4(5) . . . . ? C59 C58 N2 C57 0.6(9) . . . . ? C59 C58 N2 C60 176.7(6) . . . . ? C61 C60 N2 C57 102.2(7) . . . . ? C61 C60 N2 C58 -73.1(8) . . . . ? C63 C62 N3 Zn1 2.3(15) . . . . ? N1 Zn1 N3 C62 -96.5(7) . . . . ? N6' Zn1 N3 C62 156.2(11) . . . . ? N5 Zn1 N3 C62 82.1(9) . . . . ? N4 Zn1 N3 C62 -5.4(9) . . . . ? N4' Zn1 N3 C62 8.7(9) . . . . ? N5' Zn1 N3 C62 91(3) . . . . ? N6 Zn1 N3 C62 164.9(8) . . . . ? C62 C63 N4 N4' -116(4) . . . . ? C62 C63 N4 Zn1 -11(2) . . . . ? N4' C63 N4 Zn1 105(4) . . . . ? N1 Zn1 N4 N4' -116(3) . . . . ? N6' Zn1 N4 N4' 92(3) . . . . ? N5 Zn1 N4 N4' 1(3) . . . . ? N3 Zn1 N4 N4' 132(3) . . . . ? N5' Zn1 N4 N4' -18(3) . . . . ? N6 Zn1 N4 N4' 70(4) . . . . ? N1 Zn1 N4 C63 122.3(15) . . . . ? N6' Zn1 N4 C63 -30(3) . . . . ? N5 Zn1 N4 C63 -120.8(16) . . . . ? N3 Zn1 N4 C63 10.1(15) . . . . ? N4' Zn1 N4 C63 -122(4) . . . . ? N5' Zn1 N4 C63 -139.2(19) . . . . ? N6 Zn1 N4 C63 -51(4) . . . . ? Zn1 N4 N4' C63 -125(3) . . . . ? C63 N4 N4' Zn1 125(3) . . . . ? C62 C63 N4' N4 73(4) . . . . ? N4 C63 N4' Zn1 -53(3) . . . . ? C62 C63 N4' Zn1 20.0(15) . . . . ? N1 Zn1 N4' N4 67(3) . . . . ? N6' Zn1 N4' N4 -119(3) . . . . ? N5 Zn1 N4' N4 -179(3) . . . . ? N3 Zn1 N4' N4 -46(3) . . . . ? N5' Zn1 N4' N4 163(3) . . . . ? N6 Zn1 N4' N4 -154.9(18) . . . . ? N1 Zn1 N4' C63 99.0(9) . . . . ? N6' Zn1 N4' C63 -87(2) . . . . ? N5 Zn1 N4' C63 -147.2(11) . . . . ? N3 Zn1 N4' C63 -14.5(9) . . . . ? N4 Zn1 N4' C63 32(2) . . . . ? N5' Zn1 N4' C63 -165.1(14) . . . . ? N6 Zn1 N4' C63 -123.1(13) . . . . ? N6 C64 C65 N5 -60.1(15) . . . . ? C64 C65 N5 Zn1 35.3(15) . . . . ? N1 Zn1 N5 C65 -93.8(9) . . . . ? N6' Zn1 N5 C65 14.7(11) . . . . ? N3 Zn1 N5 C65 87.7(10) . . . . ? N4 Zn1 N5 C65 165.5(9) . . . . ? N4' Zn1 N5 C65 165.8(11) . . . . ? N5' Zn1 N5 C65 -79(4) . . . . ? N6 Zn1 N5 C65 -4.1(8) . . . . ? C65 C64 N6 Zn1 52.2(11) . . . . ? N1 Zn1 N6 C64 90.1(6) . . . . ? N6' Zn1 N6 C64 -129(3) . . . . ? N5 Zn1 N6 C64 -25.2(7) . . . . ? N3 Zn1 N6 C64 -155.8(6) . . . . ? N4 Zn1 N6 C64 -96(3) . . . . ? N4' Zn1 N6 C64 -49.2(18) . . . . ? N5' Zn1 N6 C64 -5.4(12) . . . . ? N6' C64' C65' N5' 36(5) . . . . ? C64' C65' N5' Zn1 -28(6) . . . . ? N1 Zn1 N5' C65' -98(4) . . . . ? N6' Zn1 N5' C65' 11(4) . . . . ? N5 Zn1 N5' C65' 95(5) . . . . ? N3 Zn1 N5' C65' 75(6) . . . . ? N4 Zn1 N5' C65' 163(4) . . . . ? N4' Zn1 N5' C65' 158(4) . . . . ? N6 Zn1 N5' C65' -5(4) . . . . ? C65' C64' N6' Zn1 -23(3) . . . . ? N1 Zn1 N6' C64' 105.4(16) . . . . ? N5 Zn1 N6' C64' -9.7(16) . . . . ? N3 Zn1 N6' C64' -143.2(17) . . . . ? N4 Zn1 N6' C64' -104(2) . . . . ? N4' Zn1 N6' C64' -68(2) . . . . ? N5' Zn1 N6' C64' 10.1(19) . . . . ? N6 Zn1 N6' C64' 64(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O4 0.82 1.95 2.668(6) 145.7 . O2 H2A O3 0.82 1.94 2.577(5) 133.8 . O4 H4 O3 0.82 2.39 2.910(6) 121.6 . O5 H5 O8 0.82 2.22 2.857(8) 134.3 . O6 H6A O7 0.82 1.82 2.486(8) 138.0 . O8 H8 O5 0.82 2.30 2.857(8) 126.2 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.862 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.064 #===== data_7 _database_code_depnum_ccdc_archive 'CCDC 879389' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C154 H146 N4 Na6 O59 Zn6' _chemical_formula_weight 3526.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.767(3) _cell_length_b 17.448(4) _cell_length_c 17.880(8) _cell_angle_alpha 116.355(4) _cell_angle_beta 96.267(3) _cell_angle_gamma 102.994(5) _cell_volume 3905(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8225 _exptl_absorpt_correction_T_max 0.8624 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28835 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0967 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 29.22 _reflns_number_total 17847 _reflns_number_gt 9140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distances of O1W---H1A, O1W---H1B, O3W---H3A and O3W---H3B were restrained to 0.87+-0.02 \%A. The distance of H1A...H1B was refined restrained to 1.44+-0.02 \%A. The distance of H1A...H3A was restrained to 2.42+-0.01 \%A. The distances of O4W...O11 and O11...O4W' were restrained to 3.12+-0.01 \%A. For O21 and C68, some anisotropic displacement ellipsoids were rather elongated which led us to use the DELU restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17847 _refine_ls_number_parameters 1054 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 0.844 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.27453(3) -0.12598(2) -0.10672(2) 0.04072(12) Uani 1 1 d . . . Zn2 Zn -0.05416(2) -0.42003(2) -0.10116(2) 0.03337(10) Uani 1 1 d . . . Zn3 Zn 0.42954(3) -0.03166(3) 0.06346(2) 0.05163(14) Uani 1 1 d . . . Na1 Na -0.15979(8) -0.77810(7) -0.20785(7) 0.0331(3) Uani 1 1 d . . . Na2 Na 0.32013(8) -0.32038(8) -0.24735(7) 0.0366(3) Uani 1 1 d . . . Na3 Na -0.15924(9) -0.59330(9) -0.03295(8) 0.0481(4) Uani 1 1 d . . . C1 C -0.1395(2) -0.97892(19) -0.22761(17) 0.0301(7) Uani 1 1 d . . . C2 C -0.2183(2) -1.0553(2) -0.27664(18) 0.0334(8) Uani 1 1 d . . . C3 C -0.1994(3) -1.1368(2) -0.3226(2) 0.0414(9) Uani 1 1 d . . . H3 H -0.2502 -1.1895 -0.3549 0.050 Uiso 1 1 calc R . . C4 C -0.1071(3) -1.1404(2) -0.3210(2) 0.0469(9) Uani 1 1 d . . . H4 H -0.0960 -1.1956 -0.3493 0.056 Uiso 1 1 calc R . . C5 C -0.0316(2) -1.0630(2) -0.27779(19) 0.0388(8) Uani 1 1 d . . . H5 H 0.0303 -1.0660 -0.2794 0.047 Uiso 1 1 calc R . . C6 C -0.0457(2) -0.9802(2) -0.23152(18) 0.0329(7) Uani 1 1 d . . . C7 C 0.0399(2) -0.8949(2) -0.19489(19) 0.0368(8) Uani 1 1 d . . . H7A H 0.0251 -0.8446 -0.1514 0.044 Uiso 1 1 calc R . . H7B H 0.0951 -0.9030 -0.1682 0.044 Uiso 1 1 calc R . . C8 C 0.0625(2) -0.8753(2) -0.26737(19) 0.0363(8) Uani 1 1 d . . . C9 C 0.1058(3) -0.9283(2) -0.3275(2) 0.0506(10) Uani 1 1 d . . . H9 H 0.1280 -0.9704 -0.3193 0.061 Uiso 1 1 calc R . . C10 C 0.1158(3) -0.9187(2) -0.3988(2) 0.0574(11) Uani 1 1 d . . . H10 H 0.1462 -0.9534 -0.4376 0.069 Uiso 1 1 calc R . . C11 C 0.0814(3) -0.8583(2) -0.4133(2) 0.0485(10) Uani 1 1 d . . . H11 H 0.0851 -0.8550 -0.4635 0.058 Uiso 1 1 calc R . . C12 C 0.0411(2) -0.8022(2) -0.35341(19) 0.0353(8) Uani 1 1 d . . . C13 C 0.0359(2) -0.80993(19) -0.27993(18) 0.0299(7) Uani 1 1 d . . . C14 C 0.0012(2) -0.7376(2) -0.3710(2) 0.0411(9) Uani 1 1 d . . . H14A H -0.0086 -0.6935 -0.3181 0.049 Uiso 1 1 calc R . . H14B H 0.0474 -0.7059 -0.3903 0.049 Uiso 1 1 calc R . . C15 C -0.0922(2) -0.7853(2) -0.43825(19) 0.0377(8) Uani 1 1 d . . . C16 C -0.0943(3) -0.8239(2) -0.5262(2) 0.0492(10) Uani 1 1 d . . . H16 H -0.0371 -0.8161 -0.5433 0.059 Uiso 1 1 calc R . . C17 C -0.1790(3) -0.8728(2) -0.5878(2) 0.0518(10) Uani 1 1 d . . . H17 H -0.1796 -0.8936 -0.6456 0.062 Uiso 1 1 calc R . . C18 C -0.2619(3) -0.8906(2) -0.5634(2) 0.0473(9) Uani 1 1 d . . . H18 H -0.3180 -0.9279 -0.6057 0.057 Uiso 1 1 calc R . . C19 C -0.2659(2) -0.8548(2) -0.47665(19) 0.0380(8) Uani 1 1 d . . . C20 C -0.1786(2) -0.79856(19) -0.41640(17) 0.0325(8) Uani 1 1 d . . . C21 C -0.3556(2) -0.8797(2) -0.4498(2) 0.0425(9) Uani 1 1 d . . . H21A H -0.4103 -0.8869 -0.4905 0.051 Uiso 1 1 calc R . . H21B H -0.3533 -0.8318 -0.3937 0.051 Uiso 1 1 calc R . . C22 C -0.3673(2) -0.9661(2) -0.4459(2) 0.0391(8) Uani 1 1 d . . . C23 C -0.3955(2) -1.0478(2) -0.5221(2) 0.0469(9) Uani 1 1 d . . . H23 H -0.4082 -1.0481 -0.5743 0.056 Uiso 1 1 calc R . . C24 C -0.4048(2) -1.1278(2) -0.5220(2) 0.0508(10) Uani 1 1 d . . . H24 H -0.4253 -1.1814 -0.5737 0.061 Uiso 1 1 calc R . . C25 C -0.3840(2) -1.1287(2) -0.4458(2) 0.0433(9) Uani 1 1 d . . . H25 H -0.3908 -1.1832 -0.4463 0.052 Uiso 1 1 calc R . . C26 C -0.3525(2) -1.0486(2) -0.36702(19) 0.0346(8) Uani 1 1 d . . . C27 C -0.3483(2) -0.9689(2) -0.36876(19) 0.0356(8) Uani 1 1 d . . . C28 C -0.3192(2) -1.0506(2) -0.28532(19) 0.0367(8) Uani 1 1 d . . . H28A H -0.3613 -1.1024 -0.2860 0.044 Uiso 1 1 calc R . . H28B H -0.3219 -0.9970 -0.2363 0.044 Uiso 1 1 calc R . . C29 C -0.1346(2) -0.8694(2) -0.08535(17) 0.0356(8) Uani 1 1 d . . . H29A H -0.1020 -0.8052 -0.0549 0.043 Uiso 1 1 calc R . . H29B H -0.0898 -0.8984 -0.0747 0.043 Uiso 1 1 calc R . . C30 C -0.2167(2) -0.8871(2) -0.04655(19) 0.0350(8) Uani 1 1 d . . . C31 C 0.0695(2) -0.6732(2) -0.14994(18) 0.0393(8) Uani 1 1 d . . . H31A H 0.0809 -0.6258 -0.1655 0.047 Uiso 1 1 calc R . . H31B H 0.1293 -0.6860 -0.1414 0.047 Uiso 1 1 calc R . . C32 C 0.0355(2) -0.64265(19) -0.06797(18) 0.0299(7) Uani 1 1 d . . . C33 C -0.1942(3) -0.6671(2) -0.31189(19) 0.0445(9) Uani 1 1 d . . . H33A H -0.2622 -0.6751 -0.3251 0.053 Uiso 1 1 calc R . . H33B H -0.1657 -0.6468 -0.3488 0.053 Uiso 1 1 calc R . . C34 C -0.1505(2) -0.5959(2) -0.21903(19) 0.0316(7) Uani 1 1 d . . . C35 C -0.3952(2) -0.8643(2) -0.2519(2) 0.0444(9) Uani 1 1 d . . . H35A H -0.4262 -0.9106 -0.2388 0.053 Uiso 1 1 calc R . . H35B H -0.4424 -0.8612 -0.2918 0.053 Uiso 1 1 calc R . . C36 C -0.3582(3) -0.7747(2) -0.1699(2) 0.0532(11) Uani 1 1 d . . . C37 C 0.5092(2) -0.3897(2) -0.20580(19) 0.0399(9) Uani 1 1 d . . . C38 C 0.4858(2) -0.4695(2) -0.20147(19) 0.0427(9) Uani 1 1 d . . . C39 C 0.5520(3) -0.5165(3) -0.2150(2) 0.0548(10) Uani 1 1 d . . . H39 H 0.5390 -0.5695 -0.2117 0.066 Uiso 1 1 calc R . . C40 C 0.6366(3) -0.4860(3) -0.2332(2) 0.0553(11) Uani 1 1 d . . . H40 H 0.6827 -0.5154 -0.2373 0.066 Uiso 1 1 calc R . . C41 C 0.6530(2) -0.4119(3) -0.2452(2) 0.0526(10) Uani 1 1 d . . . H41 H 0.7082 -0.3946 -0.2618 0.063 Uiso 1 1 calc R . . C42 C 0.5892(2) -0.3623(2) -0.23326(19) 0.0414(9) Uani 1 1 d . . . C43 C 0.6025(2) -0.2862(2) -0.2548(2) 0.0453(9) Uani 1 1 d . . . H43A H 0.5753 -0.2420 -0.2177 0.054 Uiso 1 1 calc R . . H43B H 0.6704 -0.2570 -0.2439 0.054 Uiso 1 1 calc R . . C44 C 0.5553(2) -0.3195(2) -0.3479(2) 0.0365(8) Uani 1 1 d . . . C45 C 0.5961(2) -0.3666(2) -0.4136(2) 0.0452(9) Uani 1 1 d . . . H45 H 0.6535 -0.3763 -0.3996 0.054 Uiso 1 1 calc R . . C46 C 0.5538(3) -0.3991(2) -0.4983(2) 0.0491(10) Uani 1 1 d . . . H46 H 0.5825 -0.4303 -0.5410 0.059 Uiso 1 1 calc R . . C47 C 0.4687(3) -0.3856(2) -0.5201(2) 0.0443(9) Uani 1 1 d . . . H47 H 0.4405 -0.4080 -0.5778 0.053 Uiso 1 1 calc R . . C48 C 0.4240(2) -0.33927(19) -0.45791(19) 0.0345(8) Uani 1 1 d . . . C49 C 0.4702(2) -0.30434(19) -0.37203(18) 0.0334(8) Uani 1 1 d . . . C50 C 0.3267(2) -0.3307(2) -0.48539(19) 0.0377(8) Uani 1 1 d . . . H50A H 0.3144 -0.2825 -0.4372 0.045 Uiso 1 1 calc R . . H50B H 0.3276 -0.3155 -0.5314 0.045 Uiso 1 1 calc R . . C51 C 0.2469(2) -0.4179(2) -0.51597(18) 0.0327(7) Uani 1 1 d . . . C52 C 0.2194(2) -0.4839(2) -0.60143(19) 0.0393(8) Uani 1 1 d . . . H52 H 0.2466 -0.4724 -0.6414 0.047 Uiso 1 1 calc R . . C53 C 0.1533(2) -0.5655(2) -0.6287(2) 0.0431(9) Uani 1 1 d . . . H53 H 0.1332 -0.6077 -0.6868 0.052 Uiso 1 1 calc R . . C54 C 0.1170(2) -0.5845(2) -0.5689(2) 0.0422(9) Uani 1 1 d . . . H54 H 0.0755 -0.6414 -0.5870 0.051 Uiso 1 1 calc R . . C55 C 0.1406(2) -0.5210(2) -0.48255(19) 0.0344(8) Uani 1 1 d . . . C56 C 0.2011(2) -0.43557(19) -0.45913(17) 0.0299(7) Uani 1 1 d . . . C57 C 0.1121(2) -0.5448(2) -0.4149(2) 0.0399(9) Uani 1 1 d . . . H57A H 0.1061 -0.4923 -0.3668 0.048 Uiso 1 1 calc R . . H57B H 0.0506 -0.5912 -0.4389 0.048 Uiso 1 1 calc R . . C58 C 0.2455(2) -0.5306(2) -0.3011(2) 0.0371(8) Uani 1 1 d . . . C59 C 0.1870(2) -0.5778(2) -0.3844(2) 0.0381(8) Uani 1 1 d . . . C60 C 0.2010(2) -0.6578(2) -0.4402(2) 0.0480(10) Uani 1 1 d . . . H60 H 0.1638 -0.6902 -0.4963 0.058 Uiso 1 1 calc R . . C61 C 0.2671(3) -0.6908(3) -0.4159(3) 0.0571(11) Uani 1 1 d . . . H61 H 0.2735 -0.7455 -0.4544 0.069 Uiso 1 1 calc R . . C62 C 0.3239(3) -0.6427(2) -0.3340(3) 0.0533(10) Uani 1 1 d . . . H62 H 0.3688 -0.6654 -0.3173 0.064 Uiso 1 1 calc R . . C63 C 0.3161(2) -0.5605(2) -0.2751(2) 0.0439(9) Uani 1 1 d . . . C64 C 0.3893(2) -0.5063(3) -0.1890(2) 0.0496(9) Uani 1 1 d . . . H64A H 0.3689 -0.4571 -0.1504 0.060 Uiso 1 1 calc R . . H64B H 0.3941 -0.5442 -0.1633 0.060 Uiso 1 1 calc R . . C65 C 0.4900(3) -0.2689(3) -0.0892(2) 0.0521(10) Uani 1 1 d . . . H65A H 0.5562 -0.2364 -0.0805 0.063 Uiso 1 1 calc R . . H65B H 0.4887 -0.3001 -0.0557 0.063 Uiso 1 1 calc R . . C66 C 0.4342(2) -0.2034(2) -0.0579(2) 0.0380(8) Uani 1 1 d . . . C67 C 0.4287(2) -0.1703(2) -0.29654(19) 0.0402(8) Uani 1 1 d . . . H67A H 0.3632 -0.1688 -0.3045 0.048 Uiso 1 1 calc R . . H67B H 0.4552 -0.1612 -0.3403 0.048 Uiso 1 1 calc R . . C68 C 0.4859(2) -0.0946(2) -0.2088(2) 0.0419(8) Uani 1 1 d U . . C69 C 0.1374(2) -0.3289(2) -0.3682(2) 0.0420(9) Uani 1 1 d . . . H69A H 0.0797 -0.3742 -0.3763 0.050 Uiso 1 1 calc R . . H69B H 0.1272 -0.3133 -0.4135 0.050 Uiso 1 1 calc R . . C70 C 0.1547(2) -0.2465(2) -0.28238(19) 0.0360(8) Uani 1 1 d . . . C71 C 0.1999(3) -0.4436(3) -0.1709(2) 0.0529(10) Uani 1 1 d . . . H71A H 0.2469 -0.3960 -0.1195 0.063 Uiso 1 1 calc R . . H71B H 0.1948 -0.4996 -0.1701 0.063 Uiso 1 1 calc R . . C72 C 0.1059(2) -0.4266(2) -0.1681(2) 0.0385(8) Uani 1 1 d . . . C73 C -0.0408(2) -0.2510(2) -0.1143(2) 0.0413(9) Uani 1 1 d . . . H73 H 0.0082 -0.2568 -0.1430 0.050 Uiso 1 1 calc R . . C74 C -0.1502(3) -0.2747(3) -0.0508(2) 0.0505(10) Uani 1 1 d . . . H74 H -0.1911 -0.3009 -0.0267 0.061 Uiso 1 1 calc R . . C75 C -0.1481(3) -0.1991(3) -0.0529(2) 0.0536(10) Uani 1 1 d . . . H75 H -0.1872 -0.1635 -0.0311 0.064 Uiso 1 1 calc R . . C76 C -0.0511(3) -0.1091(2) -0.1120(2) 0.0527(10) Uani 1 1 d . . . H76A H -0.1086 -0.0964 -0.1284 0.063 Uiso 1 1 calc R . . H76B H -0.0229 -0.1287 -0.1611 0.063 Uiso 1 1 calc R . . C77 C 0.0189(3) -0.0225(2) -0.0390(2) 0.0476(9) Uani 1 1 d . . . H77A H 0.0756 -0.0355 -0.0215 0.057 Uiso 1 1 calc R . . H77B H 0.0382 0.0194 -0.0604 0.057 Uiso 1 1 calc R . . N1 N -0.08208(19) -0.30780(17) -0.08992(16) 0.0388(7) Uani 1 1 d . . . N2 N -0.0788(2) -0.18340(18) -0.09236(17) 0.0422(7) Uani 1 1 d . . . O1 O -0.15649(14) -0.89793(12) -0.17599(11) 0.0308(5) Uani 1 1 d . . . O2 O -0.00109(13) -0.75225(12) -0.21756(12) 0.0326(5) Uani 1 1 d . . . O3 O -0.18043(14) -0.75184(12) -0.33010(11) 0.0325(5) Uani 1 1 d . . . O2W O -0.3103(2) -0.5724(2) -0.00961(18) 0.0604(10) Uani 0.80 1 d P . . O2W' O -0.3419(7) -0.5108(6) -0.0184(6) 0.028(2) Uiso 0.20 1 d P . . O4 O -0.31882(14) -0.88759(13) -0.29111(12) 0.0356(5) Uani 1 1 d . . . O5 O -0.30061(16) -0.92563(16) -0.08997(13) 0.0498(7) Uani 1 1 d . . . O6 O -0.19019(15) -0.85752(15) 0.03377(12) 0.0425(6) Uani 1 1 d . . . O7 O 0.09456(15) -0.57440(13) -0.00170(12) 0.0397(6) Uani 1 1 d . . . O8 O -0.04281(15) -0.68429(13) -0.06652(12) 0.0356(5) Uani 1 1 d . . . O9 O -0.14916(15) -0.51835(14) -0.20471(13) 0.0394(6) Uani 1 1 d . . . O10 O -0.11897(19) -0.61661(14) -0.16680(13) 0.0506(7) Uani 1 1 d . . . O11 O -0.42031(18) -0.74147(19) -0.13944(19) 0.0874(11) Uani 1 1 d D . . O12 O -0.27105(17) -0.74053(17) -0.13668(16) 0.0658(9) Uani 1 1 d . . . O13 O 0.23362(15) -0.44871(14) -0.24521(13) 0.0386(5) Uani 1 1 d . . . O14 O 0.45179(14) -0.33381(14) -0.17884(12) 0.0387(6) Uani 1 1 d . . . O15 O 0.42883(14) -0.25634(13) -0.30739(12) 0.0343(5) Uani 1 1 d . . . O16 O 0.21580(13) -0.36580(13) -0.37519(11) 0.0325(5) Uani 1 1 d . . . O17 O 0.0667(2) -0.4060(2) -0.21664(18) 0.0722(8) Uani 1 1 d . . . O18 O 0.07337(15) -0.43276(15) -0.10640(13) 0.0413(6) Uani 1 1 d . . . O19 O 0.35619(15) -0.21662(14) -0.10336(13) 0.0398(6) Uani 1 1 d . . . O20 O 0.47440(16) -0.13820(15) 0.01646(13) 0.0474(6) Uani 1 1 d . . . O21 O 0.53203(17) -0.10824(16) -0.15592(14) 0.0525(7) Uani 1 1 d U . . O22 O 0.48254(18) -0.01807(16) -0.19275(15) 0.0570(7) Uani 1 1 d . . . O23 O 0.23330(15) -0.22123(14) -0.22882(12) 0.0390(6) Uani 1 1 d . . . O24 O 0.09128(17) -0.21000(16) -0.27178(15) 0.0536(7) Uani 1 1 d . . . O5W O -0.2755(13) -0.0901(12) -0.0646(11) 0.278(7) Uiso 0.50 1 d P . . O1W O 0.1998(2) -0.04503(18) -0.13724(16) 0.0603(7) Uani 1 1 d D . . H1A H 0.246(2) -0.033(3) -0.157(2) 0.090 Uiso 1 1 d D . . H1B H 0.1501(19) -0.088(2) -0.178(2) 0.090 Uiso 1 1 d D . . O3W O 0.3196(3) 0.0354(3) -0.2023(3) 0.1062(12) Uani 1 1 d D . . H3A H 0.339(4) 0.0959(15) -0.157(3) 0.159 Uiso 1 1 d D . . H3B H 0.367(4) 0.008(4) -0.214(4) 0.159 Uiso 1 1 d D . . O4W O -0.6280(5) -0.7781(6) -0.1928(9) 0.310(8) Uani 0.70 1 d PD . . O4W' O -0.6186(6) -0.7849(9) -0.1382(7) 0.081(4) Uiso 0.30 1 d PD . . O25 O 0.39125(18) -0.02622(15) -0.04176(15) 0.0494(7) Uani 1 1 d . . . H25A H 0.363(3) 0.009(3) -0.037(3) 0.074 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0463(2) 0.0372(2) 0.02516(18) 0.00825(17) 0.00812(17) 0.00362(18) Zn2 0.0354(2) 0.0305(2) 0.03098(19) 0.01294(16) 0.00562(16) 0.00952(16) Zn3 0.0608(3) 0.0446(2) 0.02710(19) 0.00465(18) 0.00354(19) 0.0065(2) Na1 0.0341(6) 0.0316(6) 0.0312(6) 0.0138(5) 0.0080(5) 0.0091(5) Na2 0.0368(6) 0.0391(7) 0.0312(6) 0.0151(6) 0.0048(5) 0.0126(6) Na3 0.0498(8) 0.0513(8) 0.0344(7) 0.0138(6) 0.0085(6) 0.0154(7) C1 0.0423(18) 0.0283(16) 0.0257(14) 0.0164(13) 0.0088(14) 0.0141(15) C2 0.0424(19) 0.0309(17) 0.0274(15) 0.0161(14) 0.0095(14) 0.0076(15) C3 0.055(2) 0.0269(17) 0.0360(17) 0.0134(15) 0.0065(16) 0.0077(16) C4 0.070(3) 0.0307(19) 0.0396(18) 0.0131(16) 0.0126(18) 0.0232(19) C5 0.0453(19) 0.042(2) 0.0376(17) 0.0223(16) 0.0130(16) 0.0215(17) C6 0.0421(18) 0.0342(18) 0.0273(15) 0.0186(14) 0.0062(14) 0.0137(15) C7 0.0364(17) 0.0374(18) 0.0344(16) 0.0156(15) 0.0061(14) 0.0125(15) C8 0.0345(17) 0.0306(17) 0.0372(17) 0.0116(15) 0.0108(15) 0.0074(15) C9 0.060(2) 0.042(2) 0.058(2) 0.0235(18) 0.028(2) 0.0252(18) C10 0.073(3) 0.047(2) 0.059(2) 0.0202(19) 0.042(2) 0.029(2) C11 0.059(2) 0.042(2) 0.0441(19) 0.0171(17) 0.0282(18) 0.0148(19) C12 0.0350(17) 0.0273(16) 0.0379(17) 0.0128(14) 0.0136(15) 0.0031(14) C13 0.0246(15) 0.0249(16) 0.0333(16) 0.0091(13) 0.0110(13) 0.0043(13) C14 0.047(2) 0.0303(17) 0.0453(19) 0.0188(16) 0.0199(17) 0.0064(16) C15 0.056(2) 0.0282(17) 0.0345(17) 0.0185(14) 0.0156(16) 0.0134(16) C16 0.072(3) 0.046(2) 0.048(2) 0.0278(18) 0.033(2) 0.031(2) C17 0.088(3) 0.047(2) 0.0265(17) 0.0168(17) 0.016(2) 0.031(2) C18 0.073(3) 0.0373(19) 0.0272(16) 0.0121(15) 0.0019(18) 0.0222(19) C19 0.055(2) 0.0292(17) 0.0306(16) 0.0134(14) 0.0039(16) 0.0192(16) C20 0.055(2) 0.0237(16) 0.0244(15) 0.0132(13) 0.0110(15) 0.0185(15) C21 0.0421(19) 0.045(2) 0.0330(17) 0.0134(16) -0.0028(15) 0.0182(17) C22 0.0293(17) 0.041(2) 0.0365(17) 0.0127(16) -0.0010(14) 0.0098(15) C23 0.044(2) 0.049(2) 0.0313(17) 0.0105(17) -0.0040(16) 0.0115(18) C24 0.051(2) 0.038(2) 0.0374(19) 0.0016(17) -0.0039(17) 0.0085(17) C25 0.0352(18) 0.0333(18) 0.045(2) 0.0080(16) 0.0029(16) 0.0075(15) C26 0.0232(15) 0.0360(19) 0.0349(17) 0.0108(15) 0.0045(14) 0.0062(14) C27 0.0258(16) 0.0330(18) 0.0339(17) 0.0079(15) 0.0010(14) 0.0050(14) C28 0.0353(17) 0.0317(17) 0.0377(17) 0.0154(15) 0.0094(15) 0.0033(15) C29 0.0417(18) 0.0345(17) 0.0250(15) 0.0130(14) 0.0038(14) 0.0066(15) C30 0.047(2) 0.0266(16) 0.0295(16) 0.0103(14) 0.0138(16) 0.0128(16) C31 0.0386(18) 0.0313(17) 0.0342(17) 0.0077(15) 0.0111(15) 0.0024(15) C32 0.0357(18) 0.0261(16) 0.0325(16) 0.0157(14) 0.0093(15) 0.0136(15) C33 0.064(2) 0.0336(19) 0.0328(17) 0.0115(15) 0.0026(17) 0.0233(17) C34 0.0325(17) 0.0308(18) 0.0298(16) 0.0113(14) 0.0092(14) 0.0129(14) C35 0.0346(18) 0.045(2) 0.0436(19) 0.0148(17) 0.0101(16) 0.0088(16) C36 0.046(2) 0.047(2) 0.051(2) 0.0072(18) 0.0219(19) 0.0161(19) C37 0.0321(18) 0.052(2) 0.0313(16) 0.0145(16) 0.0022(14) 0.0209(17) C38 0.046(2) 0.058(2) 0.0321(17) 0.0235(17) 0.0113(16) 0.0266(18) C39 0.069(3) 0.068(3) 0.048(2) 0.034(2) 0.018(2) 0.043(2) C40 0.050(2) 0.083(3) 0.046(2) 0.030(2) 0.0151(18) 0.045(2) C41 0.037(2) 0.074(3) 0.045(2) 0.023(2) 0.0102(17) 0.025(2) C42 0.0318(18) 0.049(2) 0.0319(16) 0.0101(16) 0.0016(15) 0.0148(16) C43 0.0278(17) 0.046(2) 0.0448(19) 0.0122(17) 0.0011(15) 0.0038(16) C44 0.0289(17) 0.0311(17) 0.0390(17) 0.0126(15) 0.0079(15) 0.0001(14) C45 0.0371(18) 0.043(2) 0.052(2) 0.0204(18) 0.0139(17) 0.0116(16) C46 0.051(2) 0.045(2) 0.048(2) 0.0162(18) 0.0242(18) 0.0141(18) C47 0.056(2) 0.0385(19) 0.0291(16) 0.0123(15) 0.0100(16) 0.0064(18) C48 0.0379(18) 0.0263(16) 0.0325(16) 0.0130(14) 0.0058(15) 0.0014(14) C49 0.0338(17) 0.0280(16) 0.0288(15) 0.0095(14) 0.0107(14) -0.0003(14) C50 0.049(2) 0.0313(17) 0.0310(16) 0.0164(14) 0.0051(15) 0.0089(15) C51 0.0341(17) 0.0310(17) 0.0265(15) 0.0100(14) 0.0011(14) 0.0099(14) C52 0.0430(19) 0.043(2) 0.0303(16) 0.0171(15) 0.0060(15) 0.0141(17) C53 0.0422(19) 0.039(2) 0.0286(16) 0.0033(15) 0.0004(15) 0.0095(17) C54 0.0321(17) 0.0299(17) 0.0428(19) 0.0054(16) -0.0029(16) 0.0024(15) C55 0.0240(15) 0.0335(17) 0.0369(17) 0.0105(15) 0.0033(14) 0.0087(14) C56 0.0255(15) 0.0325(17) 0.0234(14) 0.0060(13) 0.0004(13) 0.0124(14) C57 0.0311(17) 0.0368(18) 0.0445(18) 0.0161(16) 0.0120(15) 0.0036(15) C58 0.0394(18) 0.0365(18) 0.0458(19) 0.0249(16) 0.0242(16) 0.0131(16) C59 0.0350(18) 0.0382(19) 0.0437(18) 0.0233(16) 0.0165(16) 0.0047(15) C60 0.041(2) 0.038(2) 0.055(2) 0.0164(18) 0.0153(18) 0.0055(17) C61 0.065(3) 0.041(2) 0.072(3) 0.026(2) 0.030(2) 0.023(2) C62 0.057(2) 0.048(2) 0.069(3) 0.033(2) 0.022(2) 0.0282(19) C63 0.0427(19) 0.049(2) 0.053(2) 0.0332(18) 0.0182(17) 0.0163(17) C64 0.058(2) 0.063(2) 0.050(2) 0.0386(19) 0.0207(18) 0.031(2) C65 0.045(2) 0.066(2) 0.0317(17) 0.0126(18) 0.0019(16) 0.0194(19) C66 0.0374(18) 0.0404(19) 0.0329(17) 0.0157(16) 0.0117(16) 0.0090(16) C67 0.0412(19) 0.0322(18) 0.0354(17) 0.0101(15) 0.0067(15) 0.0048(15) C68 0.040(2) 0.036(2) 0.0388(18) 0.0105(15) 0.0206(15) 0.0050(16) C69 0.0411(19) 0.0421(19) 0.0368(17) 0.0104(16) 0.0046(15) 0.0229(16) C70 0.0389(19) 0.0359(18) 0.0312(16) 0.0151(15) 0.0071(16) 0.0113(16) C71 0.054(2) 0.081(3) 0.055(2) 0.047(2) 0.0301(19) 0.036(2) C72 0.0410(19) 0.0386(19) 0.0317(17) 0.0128(16) 0.0090(16) 0.0136(16) C73 0.046(2) 0.0360(19) 0.0356(17) 0.0146(16) 0.0057(16) 0.0098(17) C74 0.047(2) 0.050(2) 0.063(2) 0.0316(19) 0.0214(19) 0.0190(19) C75 0.056(2) 0.050(2) 0.068(2) 0.031(2) 0.026(2) 0.0287(19) C76 0.080(3) 0.038(2) 0.044(2) 0.0232(17) 0.0113(19) 0.0214(19) C77 0.063(2) 0.042(2) 0.048(2) 0.0282(17) 0.0151(18) 0.0205(18) N1 0.0444(16) 0.0305(15) 0.0369(14) 0.0153(13) 0.0018(13) 0.0093(13) N2 0.0554(18) 0.0339(16) 0.0373(15) 0.0167(13) 0.0079(14) 0.0165(14) O1 0.0384(12) 0.0283(11) 0.0253(10) 0.0126(9) 0.0084(9) 0.0097(9) O2 0.0331(11) 0.0261(11) 0.0274(10) 0.0040(9) 0.0098(9) 0.0071(9) O3 0.0485(13) 0.0253(11) 0.0238(10) 0.0099(9) 0.0090(9) 0.0156(10) O2W 0.0543(19) 0.063(2) 0.0405(16) 0.0023(16) 0.0049(15) 0.0273(17) O4 0.0320(11) 0.0327(12) 0.0287(10) 0.0057(9) 0.0041(9) 0.0071(10) O5 0.0413(14) 0.0603(15) 0.0289(11) 0.0110(11) 0.0080(11) 0.0046(12) O6 0.0425(13) 0.0510(14) 0.0280(11) 0.0164(11) 0.0089(10) 0.0095(11) O7 0.0449(13) 0.0315(12) 0.0257(11) 0.0053(10) 0.0047(10) 0.0011(11) O8 0.0391(13) 0.0344(12) 0.0292(11) 0.0133(10) 0.0092(10) 0.0077(10) O9 0.0480(13) 0.0251(12) 0.0345(11) 0.0071(10) -0.0040(10) 0.0143(10) O10 0.0879(19) 0.0321(13) 0.0281(11) 0.0110(10) 0.0027(12) 0.0251(13) O11 0.0480(16) 0.0713(19) 0.092(2) -0.0054(17) 0.0265(16) 0.0180(15) O12 0.0367(14) 0.0543(16) 0.0595(16) -0.0092(13) 0.0128(13) 0.0077(13) O13 0.0399(12) 0.0475(13) 0.0388(12) 0.0258(11) 0.0186(10) 0.0171(11) O14 0.0348(12) 0.0468(13) 0.0315(11) 0.0128(10) 0.0064(10) 0.0212(11) O15 0.0346(11) 0.0305(12) 0.0297(11) 0.0100(9) 0.0060(9) 0.0061(10) O16 0.0320(11) 0.0341(12) 0.0239(10) 0.0074(9) 0.0028(9) 0.0127(10) O17 0.0756(19) 0.119(3) 0.0670(17) 0.0632(18) 0.0372(15) 0.0621(19) O18 0.0385(12) 0.0532(14) 0.0338(11) 0.0196(11) 0.0155(10) 0.0163(11) O19 0.0376(12) 0.0366(12) 0.0330(11) 0.0078(10) 0.0034(10) 0.0111(10) O20 0.0446(13) 0.0499(14) 0.0289(12) 0.0071(11) 0.0048(10) 0.0085(12) O21 0.0539(15) 0.0485(15) 0.0334(12) 0.0076(11) 0.0079(11) 0.0045(12) O22 0.0623(16) 0.0322(14) 0.0539(15) 0.0042(12) 0.0220(13) 0.0057(12) O23 0.0437(13) 0.0365(12) 0.0294(11) 0.0079(10) 0.0041(10) 0.0185(11) O24 0.0456(14) 0.0489(15) 0.0540(14) 0.0112(12) 0.0074(12) 0.0241(12) O1W 0.0699(18) 0.0552(17) 0.0541(15) 0.0213(13) 0.0181(14) 0.0257(14) O3W 0.086(3) 0.106(3) 0.143(3) 0.082(3) 0.016(3) 0.019(2) O4W 0.164(8) 0.209(9) 0.46(2) 0.122(11) 0.162(11) -0.066(7) O25 0.0590(17) 0.0373(14) 0.0379(12) 0.0134(12) 0.0036(12) 0.0041(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O25 1.941(2) . ? Zn1 O6 1.965(2) 2_545 ? Zn1 O23 1.983(2) . ? Zn1 O1W 2.182(3) . ? Zn1 O19 2.210(2) . ? Zn1 Zn3 3.0896(11) . ? Zn1 Na2 3.4793(14) . ? Zn1 H25A 2.12(4) . ? Zn2 O18 1.953(2) . ? Zn2 O9 1.9670(19) . ? Zn2 N1 2.019(3) . ? Zn2 O7 2.030(2) 2_545 ? Zn2 Na3 3.6416(16) 2_545 ? Zn3 O25 1.954(3) . ? Zn3 O20 1.972(2) . ? Zn3 O5 2.068(2) 2_545 ? Zn3 O21 2.145(2) 2_655 ? Zn3 O22 2.200(3) 2_655 ? Zn3 C68 2.477(3) 2_655 ? Na1 O12 2.225(3) . ? Na1 O2 2.326(2) . ? Na1 O1 2.407(2) . ? Na1 O3 2.426(3) . ? Na1 O4 2.465(2) . ? Na1 O8 2.480(2) . ? Na1 O10 2.479(3) . ? Na1 C36 3.087(4) . ? Na1 Na3 3.3475(18) . ? Na2 O14 2.297(2) . ? Na2 O16 2.302(2) . ? Na2 O19 2.306(2) . ? Na2 O23 2.308(3) . ? Na2 O13 2.334(3) . ? Na2 O15 2.369(2) . ? Na2 C66 3.090(3) . ? Na3 O2W 2.391(3) . ? Na3 O10 2.409(3) . ? Na3 O12 2.441(3) . ? Na3 O18 2.463(3) 2_545 ? Na3 O8 2.539(3) . ? Na3 O7 2.620(3) 2_545 ? Na3 Zn2 3.6416(16) 2_545 ? C1 C2 1.393(4) . ? C1 C6 1.400(4) . ? C1 O1 1.401(3) . ? C2 C3 1.403(4) . ? C2 C28 1.506(4) . ? C3 C4 1.377(5) . ? C3 H3 0.9300 . ? C4 C5 1.368(4) . ? C4 H4 0.9300 . ? C5 C6 1.389(4) . ? C5 H5 0.9300 . ? C6 C7 1.532(4) . ? C7 C8 1.531(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.384(5) . ? C8 C9 1.397(4) . ? C9 C10 1.377(5) . ? C9 H9 0.9300 . ? C10 C11 1.375(5) . ? C10 H10 0.9300 . ? C11 C12 1.390(4) . ? C11 H11 0.9300 . ? C12 C13 1.388(4) . ? C12 C14 1.512(5) . ? C13 O2 1.393(3) . ? C14 C15 1.508(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.374(4) . ? C15 C16 1.403(4) . ? C16 C17 1.375(5) . ? C16 H16 0.9300 . ? C17 C18 1.360(5) . ? C17 H17 0.9300 . ? C18 C19 1.406(4) . ? C18 H18 0.9300 . ? C19 C20 1.405(4) . ? C19 C21 1.496(5) . ? C20 O3 1.396(3) . ? C21 C22 1.512(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.395(4) . ? C22 C27 1.401(5) . ? C23 C24 1.370(5) . ? C23 H23 0.9300 . ? C24 C25 1.372(5) . ? C24 H24 0.9300 . ? C25 C26 1.404(4) . ? C25 H25 0.9300 . ? C26 C27 1.392(5) . ? C26 C28 1.508(5) . ? C27 O4 1.404(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O1 1.441(3) . ? C29 C30 1.500(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O5 1.242(4) . ? C30 O6 1.269(4) . ? C31 O2 1.432(3) . ? C31 C32 1.508(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O8 1.229(3) . ? C32 O7 1.280(3) . ? C33 O3 1.433(4) . ? C33 C34 1.514(4) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O10 1.225(4) . ? C34 O9 1.255(4) . ? C35 O4 1.433(4) . ? C35 C36 1.515(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O11 1.241(4) . ? C36 O12 1.241(4) . ? C37 O14 1.395(4) . ? C37 C38 1.398(5) . ? C37 C42 1.395(5) . ? C38 C39 1.387(5) . ? C38 C64 1.508(5) . ? C39 C40 1.376(5) . ? C39 H39 0.9300 . ? C40 C41 1.376(6) . ? C40 H40 0.9300 . ? C41 C42 1.389(5) . ? C41 H41 0.9300 . ? C42 C43 1.518(5) . ? C43 C44 1.516(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.391(4) . ? C44 C49 1.403(5) . ? C45 C46 1.370(5) . ? C45 H45 0.9300 . ? C46 C47 1.376(5) . ? C46 H46 0.9300 . ? C47 C48 1.388(4) . ? C47 H47 0.9300 . ? C48 C49 1.396(4) . ? C48 C50 1.528(5) . ? C49 O15 1.391(3) . ? C50 C51 1.521(4) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.385(4) . ? C51 C56 1.386(4) . ? C52 C53 1.369(4) . ? C52 H52 0.9300 . ? C53 C54 1.378(5) . ? C53 H53 0.9300 . ? C54 C55 1.386(4) . ? C54 H54 0.9300 . ? C55 C56 1.400(4) . ? C55 C57 1.513(5) . ? C56 O16 1.403(3) . ? C57 C59 1.512(5) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C63 1.389(5) . ? C58 O13 1.398(4) . ? C58 C59 1.398(4) . ? C59 C60 1.389(5) . ? C60 C61 1.362(5) . ? C60 H60 0.9300 . ? C61 C62 1.370(5) . ? C61 H61 0.9300 . ? C62 C63 1.392(5) . ? C62 H62 0.9300 . ? C63 C64 1.523(5) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 O14 1.440(4) . ? C65 C66 1.501(5) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 O19 1.246(4) . ? C66 O20 1.263(3) . ? C67 O15 1.427(4) . ? C67 C68 1.513(4) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 O21 1.243(4) . ? C68 O22 1.250(4) . ? C68 Zn3 2.477(3) 2_655 ? C69 O16 1.437(4) . ? C69 C70 1.509(4) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 O24 1.233(4) . ? C70 O23 1.269(4) . ? C71 O13 1.443(4) . ? C71 C72 1.485(5) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 O17 1.216(4) . ? C72 O18 1.286(4) . ? C73 N1 1.310(4) . ? C73 N2 1.339(4) . ? C73 H73 0.9300 . ? C74 C75 1.330(5) . ? C74 N1 1.376(4) . ? C74 H74 0.9300 . ? C75 N2 1.351(4) . ? C75 H75 0.9300 . ? C76 N2 1.473(4) . ? C76 C77 1.519(5) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 C77 1.505(6) 2 ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? O2W O2W' 1.324(11) . ? O5 Zn3 2.068(2) 2_545 ? O6 Zn1 1.965(2) 2_545 ? O7 Zn2 2.030(2) 2_545 ? O7 Na3 2.620(3) 2_545 ? O18 Na3 2.463(3) 2_545 ? O21 Zn3 2.145(2) 2_655 ? O22 Zn3 2.200(3) 2_655 ? O1W H1A 0.828(18) . ? O1W H1B 0.888(18) . ? O3W H3A 0.95(2) . ? O3W H3B 0.92(2) . ? O4W O4W' 1.033(16) . ? O25 H25A 0.80(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O25 Zn1 O6 112.84(10) . 2_545 ? O25 Zn1 O23 131.75(10) . . ? O6 Zn1 O23 114.93(9) 2_545 . ? O25 Zn1 O1W 93.47(11) . . ? O6 Zn1 O1W 93.01(10) 2_545 . ? O23 Zn1 O1W 90.47(9) . . ? O25 Zn1 O19 88.11(10) . . ? O6 Zn1 O19 97.58(9) 2_545 . ? O23 Zn1 O19 79.48(8) . . ? O1W Zn1 O19 167.73(9) . . ? O25 Zn1 Zn3 37.66(8) . . ? O6 Zn1 Zn3 82.65(7) 2_545 . ? O23 Zn1 Zn3 146.40(7) . . ? O1W Zn1 Zn3 118.20(7) . . ? O19 Zn1 Zn3 69.56(5) . . ? O25 Zn1 Na2 112.03(8) . . ? O6 Zn1 Na2 114.57(7) 2_545 . ? O23 Zn1 Na2 39.09(7) . . ? O1W Zn1 Na2 128.47(7) . . ? O19 Zn1 Na2 40.63(6) . . ? Zn3 Zn1 Na2 108.28(3) . . ? O25 Zn1 H25A 22.1(12) . . ? O6 Zn1 H25A 106.4(12) 2_545 . ? O23 Zn1 H25A 136.0(12) . . ? O1W Zn1 H25A 72.4(12) . . ? O19 Zn1 H25A 110.1(12) . . ? Zn3 Zn1 H25A 50.9(13) . . ? Na2 Zn1 H25A 130.9(12) . . ? O18 Zn2 O9 110.08(9) . . ? O18 Zn2 N1 120.89(11) . . ? O9 Zn2 N1 104.35(10) . . ? O18 Zn2 O7 111.76(9) . 2_545 ? O9 Zn2 O7 107.20(9) . 2_545 ? N1 Zn2 O7 101.48(10) . 2_545 ? O18 Zn2 Na3 39.30(7) . 2_545 ? O9 Zn2 Na3 133.70(7) . 2_545 ? N1 Zn2 Na3 121.07(7) . 2_545 ? O7 Zn2 Na3 73.94(7) 2_545 2_545 ? O25 Zn3 O20 99.76(10) . . ? O25 Zn3 O5 103.51(10) . 2_545 ? O20 Zn3 O5 104.99(10) . 2_545 ? O25 Zn3 O21 99.80(10) . 2_655 ? O20 Zn3 O21 145.10(10) . 2_655 ? O5 Zn3 O21 98.14(9) 2_545 2_655 ? O25 Zn3 O22 154.55(10) . 2_655 ? O20 Zn3 O22 91.30(10) . 2_655 ? O5 Zn3 O22 95.53(9) 2_545 2_655 ? O21 Zn3 O22 60.36(10) 2_655 2_655 ? O25 Zn3 C68 128.06(12) . 2_655 ? O20 Zn3 C68 118.96(12) . 2_655 ? O5 Zn3 C68 98.56(9) 2_545 2_655 ? O21 Zn3 C68 30.12(11) 2_655 2_655 ? O22 Zn3 C68 30.26(11) 2_655 2_655 ? O25 Zn3 Zn1 37.37(7) . . ? O20 Zn3 Zn1 87.43(6) . . ? O5 Zn3 Zn1 72.89(7) 2_545 . ? O21 Zn3 Zn1 124.70(8) 2_655 . ? O22 Zn3 Zn1 167.54(7) 2_655 . ? C68 Zn3 Zn1 153.60(10) 2_655 . ? O12 Na1 O2 150.78(8) . . ? O12 Na1 O1 94.22(10) . . ? O2 Na1 O1 92.57(8) . . ? O12 Na1 O3 108.79(11) . . ? O2 Na1 O3 83.00(8) . . ? O1 Na1 O3 140.09(8) . . ? O12 Na1 O4 69.46(8) . . ? O2 Na1 O4 139.75(8) . . ? O1 Na1 O4 78.29(8) . . ? O3 Na1 O4 79.94(8) . . ? O12 Na1 O8 86.33(9) . . ? O2 Na1 O8 66.32(7) . . ? O1 Na1 O8 83.20(8) . . ? O3 Na1 O8 129.10(8) . . ? O4 Na1 O8 148.02(9) . . ? O12 Na1 O10 79.71(10) . . ? O2 Na1 O10 80.98(9) . . ? O1 Na1 O10 151.89(8) . . ? O3 Na1 O10 66.62(7) . . ? O4 Na1 O10 123.52(9) . . ? O8 Na1 O10 69.11(8) . . ? O12 Na1 C36 19.60(8) . . ? O2 Na1 C36 169.26(9) . . ? O1 Na1 C36 93.59(10) . . ? O3 Na1 C36 97.77(10) . . ? O4 Na1 C36 50.46(8) . . ? O8 Na1 C36 105.72(9) . . ? O10 Na1 C36 89.48(10) . . ? O12 Na1 Na3 46.80(6) . . ? O2 Na1 Na3 104.48(6) . . ? O1 Na1 Na3 111.25(7) . . ? O3 Na1 Na3 108.24(7) . . ? O4 Na1 Na3 115.42(7) . . ? O8 Na1 Na3 48.91(6) . . ? O10 Na1 Na3 45.90(6) . . ? C36 Na1 Na3 65.04(7) . . ? O14 Na2 O16 147.51(9) . . ? O14 Na2 O19 71.66(8) . . ? O16 Na2 O19 140.71(10) . . ? O14 Na2 O23 141.02(8) . . ? O16 Na2 O23 69.90(8) . . ? O19 Na2 O23 71.21(8) . . ? O14 Na2 O13 85.90(9) . . ? O16 Na2 O13 89.13(8) . . ? O19 Na2 O13 100.29(9) . . ? O23 Na2 O13 112.02(9) . . ? O14 Na2 O15 85.42(9) . . ? O16 Na2 O15 82.16(8) . . ? O19 Na2 O15 105.68(9) . . ? O23 Na2 O15 93.48(9) . . ? O13 Na2 O15 148.35(9) . . ? O14 Na2 C66 51.25(9) . . ? O16 Na2 C66 160.27(10) . . ? O19 Na2 C66 20.90(8) . . ? O23 Na2 C66 90.51(9) . . ? O13 Na2 C66 100.86(9) . . ? O15 Na2 C66 97.19(9) . . ? O14 Na2 Zn1 108.75(6) . . ? O16 Na2 Zn1 102.71(7) . . ? O19 Na2 Zn1 38.61(6) . . ? O23 Na2 Zn1 32.80(5) . . ? O13 Na2 Zn1 113.26(7) . . ? O15 Na2 Zn1 98.34(7) . . ? C66 Na2 Zn1 57.75(7) . . ? O2W Na3 O10 119.93(11) . . ? O2W Na3 O12 77.96(10) . . ? O10 Na3 O12 77.04(9) . . ? O2W Na3 O18 104.13(10) . 2_545 ? O10 Na3 O18 135.56(10) . 2_545 ? O12 Na3 O18 120.59(11) . 2_545 ? O2W Na3 O8 153.59(12) . . ? O10 Na3 O8 69.24(8) . . ? O12 Na3 O8 80.67(8) . . ? O18 Na3 O8 73.91(8) 2_545 . ? O2W Na3 O7 89.53(11) . 2_545 ? O10 Na3 O7 80.69(8) . 2_545 ? O12 Na3 O7 144.17(11) . 2_545 ? O18 Na3 O7 94.92(8) 2_545 2_545 ? O8 Na3 O7 116.84(8) . 2_545 ? O2W Na3 Na1 117.84(8) . . ? O10 Na3 Na1 47.65(6) . . ? O12 Na3 Na1 41.63(6) . . ? O18 Na3 Na1 116.78(8) 2_545 . ? O8 Na3 Na1 47.43(5) . . ? O7 Na3 Na1 128.06(7) 2_545 . ? O2W Na3 Zn2 134.26(9) . 2_545 ? O10 Na3 Zn2 105.57(8) . 2_545 ? O12 Na3 Zn2 119.26(9) . 2_545 ? O18 Na3 Zn2 30.14(5) 2_545 2_545 ? O8 Na3 Zn2 48.27(5) . 2_545 ? O7 Na3 Zn2 93.54(6) 2_545 2_545 ? Na1 Na3 Zn2 95.44(5) . 2_545 ? C2 C1 C6 122.2(3) . . ? C2 C1 O1 118.0(3) . . ? C6 C1 O1 119.7(3) . . ? C1 C2 C3 117.0(3) . . ? C1 C2 C28 122.0(3) . . ? C3 C2 C28 120.8(3) . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 117.7(3) . . ? C5 C6 C7 118.7(3) . . ? C1 C6 C7 123.3(3) . . ? C8 C7 C6 109.6(2) . . ? C8 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? C8 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C13 C8 C9 117.3(3) . . ? C13 C8 C7 122.4(3) . . ? C9 C8 C7 120.1(3) . . ? C10 C9 C8 120.7(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.6(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 120.3(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 118.0(3) . . ? C13 C12 C14 122.1(3) . . ? C11 C12 C14 119.8(3) . . ? C8 C13 C12 122.7(3) . . ? C8 C13 O2 118.2(3) . . ? C12 C13 O2 119.0(3) . . ? C15 C14 C12 111.9(2) . . ? C15 C14 H14A 109.2 . . ? C12 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C12 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C20 C15 C16 117.0(3) . . ? C20 C15 C14 121.6(3) . . ? C16 C15 C14 121.2(3) . . ? C17 C16 C15 121.4(3) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C18 C17 C16 119.5(3) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 122.4(3) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C20 C19 C18 115.6(3) . . ? C20 C19 C21 121.9(3) . . ? C18 C19 C21 122.3(3) . . ? C15 C20 O3 118.5(3) . . ? C15 C20 C19 123.5(3) . . ? O3 C20 C19 118.0(3) . . ? C19 C21 C22 110.9(3) . . ? C19 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C27 117.2(3) . . ? C23 C22 C21 119.6(3) . . ? C27 C22 C21 123.2(3) . . ? C24 C23 C22 121.8(3) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 121.0(4) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 117.6(3) . . ? C27 C26 C28 122.5(3) . . ? C25 C26 C28 119.8(3) . . ? C26 C27 C22 122.2(3) . . ? C26 C27 O4 119.2(3) . . ? C22 C27 O4 118.5(3) . . ? C26 C28 C2 110.5(3) . . ? C26 C28 H28A 109.6 . . ? C2 C28 H28A 109.6 . . ? C26 C28 H28B 109.6 . . ? C2 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? O1 C29 C30 117.4(3) . . ? O1 C29 H29A 107.9 . . ? C30 C29 H29A 107.9 . . ? O1 C29 H29B 107.9 . . ? C30 C29 H29B 107.9 . . ? H29A C29 H29B 107.2 . . ? O5 C30 O6 125.3(3) . . ? O5 C30 C29 122.2(3) . . ? O6 C30 C29 112.5(3) . . ? O2 C31 C32 109.7(2) . . ? O2 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O2 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? O8 C32 O7 123.8(3) . . ? O8 C32 C31 120.5(3) . . ? O7 C32 C31 115.6(3) . . ? O3 C33 C34 112.6(3) . . ? O3 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? O3 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? O10 C34 O9 126.6(3) . . ? O10 C34 C33 119.9(3) . . ? O9 C34 C33 113.5(3) . . ? O4 C35 C36 111.1(3) . . ? O4 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? O4 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? O11 C36 O12 124.4(3) . . ? O11 C36 C35 115.7(3) . . ? O12 C36 C35 119.9(3) . . ? O11 C36 Na1 157.4(3) . . ? O12 C36 Na1 36.99(16) . . ? C35 C36 Na1 84.73(19) . . ? O14 C37 C38 118.4(3) . . ? O14 C37 C42 118.8(3) . . ? C38 C37 C42 122.7(3) . . ? C39 C38 C37 117.3(3) . . ? C39 C38 C64 121.5(4) . . ? C37 C38 C64 121.0(3) . . ? C40 C39 C38 121.0(4) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C41 119.9(4) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C40 C41 C42 121.8(4) . . ? C40 C41 H41 119.1 . . ? C42 C41 H41 119.1 . . ? C41 C42 C37 116.5(4) . . ? C41 C42 C43 121.6(3) . . ? C37 C42 C43 121.7(3) . . ? C44 C43 C42 111.8(3) . . ? C44 C43 H43A 109.3 . . ? C42 C43 H43A 109.3 . . ? C44 C43 H43B 109.3 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 107.9 . . ? C45 C44 C49 117.0(3) . . ? C45 C44 C43 120.6(3) . . ? C49 C44 C43 122.4(3) . . ? C46 C45 C44 121.7(4) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C45 C46 C47 119.9(3) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C48 121.5(3) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C47 C48 C49 117.4(3) . . ? C47 C48 C50 119.6(3) . . ? C49 C48 C50 123.0(3) . . ? O15 C49 C48 119.5(3) . . ? O15 C49 C44 118.1(3) . . ? C48 C49 C44 122.3(3) . . ? C51 C50 C48 111.1(3) . . ? C51 C50 H50A 109.4 . . ? C48 C50 H50A 109.4 . . ? C51 C50 H50B 109.4 . . ? C48 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C52 C51 C56 117.4(3) . . ? C52 C51 C50 121.1(3) . . ? C56 C51 C50 121.4(2) . . ? C53 C52 C51 121.8(3) . . ? C53 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C52 C53 C54 119.1(3) . . ? C52 C53 H53 120.4 . . ? C54 C53 H53 120.4 . . ? C53 C54 C55 121.9(3) . . ? C53 C54 H54 119.1 . . ? C55 C54 H54 119.1 . . ? C54 C55 C56 116.8(3) . . ? C54 C55 C57 122.1(3) . . ? C56 C55 C57 120.8(3) . . ? C51 C56 C55 122.2(3) . . ? C51 C56 O16 119.1(3) . . ? C55 C56 O16 118.7(3) . . ? C59 C57 C55 109.7(3) . . ? C59 C57 H57A 109.7 . . ? C55 C57 H57A 109.7 . . ? C59 C57 H57B 109.7 . . ? C55 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? C63 C58 O13 120.6(3) . . ? C63 C58 C59 122.1(3) . . ? O13 C58 C59 117.1(3) . . ? C60 C59 C58 116.8(3) . . ? C60 C59 C57 120.1(3) . . ? C58 C59 C57 123.1(3) . . ? C61 C60 C59 122.5(4) . . ? C61 C60 H60 118.7 . . ? C59 C60 H60 118.7 . . ? C60 C61 C62 119.3(4) . . ? C60 C61 H61 120.4 . . ? C62 C61 H61 120.4 . . ? C61 C62 C63 121.6(4) . . ? C61 C62 H62 119.2 . . ? C63 C62 H62 119.2 . . ? C58 C63 C62 117.6(3) . . ? C58 C63 C64 124.0(3) . . ? C62 C63 C64 118.2(3) . . ? C38 C64 C63 110.1(3) . . ? C38 C64 H64A 109.6 . . ? C63 C64 H64A 109.6 . . ? C38 C64 H64B 109.6 . . ? C63 C64 H64B 109.6 . . ? H64A C64 H64B 108.2 . . ? O14 C65 C66 111.9(3) . . ? O14 C65 H65A 109.2 . . ? C66 C65 H65A 109.2 . . ? O14 C65 H65B 109.2 . . ? C66 C65 H65B 109.2 . . ? H65A C65 H65B 107.9 . . ? O19 C66 O20 126.4(3) . . ? O19 C66 C65 120.6(3) . . ? O20 C66 C65 113.0(3) . . ? O19 C66 Na2 41.31(14) . . ? O20 C66 Na2 163.5(3) . . ? C65 C66 Na2 80.55(17) . . ? O15 C67 C68 112.4(3) . . ? O15 C67 H67A 109.1 . . ? C68 C67 H67A 109.1 . . ? O15 C67 H67B 109.1 . . ? C68 C67 H67B 109.1 . . ? H67A C67 H67B 107.9 . . ? O21 C68 O22 122.5(3) . . ? O21 C68 C67 122.0(3) . . ? O22 C68 C67 115.6(4) . . ? O21 C68 Zn3 60.00(18) . 2_655 ? O22 C68 Zn3 62.50(18) . 2_655 ? C67 C68 Zn3 176.5(3) . 2_655 ? O16 C69 C70 112.5(2) . . ? O16 C69 H69A 109.1 . . ? C70 C69 H69A 109.1 . . ? O16 C69 H69B 109.1 . . ? C70 C69 H69B 109.1 . . ? H69A C69 H69B 107.8 . . ? O24 C70 O23 126.5(3) . . ? O24 C70 C69 116.5(3) . . ? O23 C70 C69 117.0(3) . . ? O13 C71 C72 114.1(3) . . ? O13 C71 H71A 108.7 . . ? C72 C71 H71A 108.7 . . ? O13 C71 H71B 108.7 . . ? C72 C71 H71B 108.7 . . ? H71A C71 H71B 107.6 . . ? O17 C72 O18 124.6(3) . . ? O17 C72 C71 123.4(3) . . ? O18 C72 C71 112.0(3) . . ? N1 C73 N2 110.7(3) . . ? N1 C73 H73 124.6 . . ? N2 C73 H73 124.6 . . ? C75 C74 N1 108.9(3) . . ? C75 C74 H74 125.6 . . ? N1 C74 H74 125.6 . . ? C74 C75 N2 107.4(3) . . ? C74 C75 H75 126.3 . . ? N2 C75 H75 126.3 . . ? N2 C76 C77 115.1(3) . . ? N2 C76 H76A 108.5 . . ? C77 C76 H76A 108.5 . . ? N2 C76 H76B 108.5 . . ? C77 C76 H76B 108.5 . . ? H76A C76 H76B 107.5 . . ? C77 C77 C76 115.1(4) 2 . ? C77 C77 H77A 108.5 2 . ? C76 C77 H77A 108.5 . . ? C77 C77 H77B 108.5 2 . ? C76 C77 H77B 108.5 . . ? H77A C77 H77B 107.5 . . ? C73 N1 C74 105.9(3) . . ? C73 N1 Zn2 129.5(3) . . ? C74 N1 Zn2 124.6(3) . . ? C73 N2 C75 107.1(3) . . ? C73 N2 C76 125.2(3) . . ? C75 N2 C76 127.7(3) . . ? C1 O1 C29 114.5(2) . . ? C1 O1 Na1 127.73(17) . . ? C29 O1 Na1 113.67(17) . . ? C13 O2 C31 114.3(2) . . ? C13 O2 Na1 126.73(15) . . ? C31 O2 Na1 118.70(16) . . ? C20 O3 C33 109.4(2) . . ? C20 O3 Na1 135.37(18) . . ? C33 O3 Na1 115.19(16) . . ? O2W' O2W Na3 123.6(5) . . ? C27 O4 C35 114.2(2) . . ? C27 O4 Na1 132.14(17) . . ? C35 O4 Na1 113.65(15) . . ? C30 O5 Zn3 134.0(2) . 2_545 ? C30 O6 Zn1 125.0(2) . 2_545 ? C32 O7 Zn2 105.70(18) . 2_545 ? C32 O7 Na3 130.4(2) . 2_545 ? Zn2 O7 Na3 109.96(8) 2_545 2_545 ? C32 O8 Na1 115.30(19) . . ? C32 O8 Na3 113.4(2) . . ? Na1 O8 Na3 83.66(8) . . ? C34 O9 Zn2 114.9(2) . . ? C34 O10 Na3 129.4(2) . . ? C34 O10 Na1 118.48(19) . . ? Na3 O10 Na1 86.45(9) . . ? C36 O12 Na1 123.4(2) . . ? C36 O12 Na3 138.2(2) . . ? Na1 O12 Na3 91.58(9) . . ? C58 O13 C71 116.6(3) . . ? C58 O13 Na2 117.49(17) . . ? C71 O13 Na2 121.7(2) . . ? C37 O14 C65 109.6(2) . . ? C37 O14 Na2 134.03(17) . . ? C65 O14 Na2 116.31(19) . . ? C49 O15 C67 115.7(2) . . ? C49 O15 Na2 124.84(18) . . ? C67 O15 Na2 116.53(18) . . ? C56 O16 C69 110.2(2) . . ? C56 O16 Na2 132.91(18) . . ? C69 O16 Na2 115.67(16) . . ? C72 O18 Zn2 115.7(2) . . ? C72 O18 Na3 130.2(2) . 2_545 ? Zn2 O18 Na3 110.57(10) . 2_545 ? C66 O19 Zn1 132.8(2) . . ? C66 O19 Na2 117.8(2) . . ? Zn1 O19 Na2 100.76(10) . . ? C66 O20 Zn3 121.0(2) . . ? C68 O21 Zn3 89.9(2) . 2_655 ? C68 O22 Zn3 87.2(2) . 2_655 ? C70 O23 Zn1 128.4(2) . . ? C70 O23 Na2 119.43(19) . . ? Zn1 O23 Na2 108.10(10) . . ? Zn1 O1W H1A 86(3) . . ? Zn1 O1W H1B 100(3) . . ? H1A O1W H1B 112(3) . . ? H3A O3W H3B 117(6) . . ? Zn1 O25 Zn3 104.96(12) . . ? Zn1 O25 H25A 91(3) . . ? Zn3 O25 H25A 115(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Zn1 Zn3 O25 -143.87(14) 2_545 . . . ? O23 Zn1 Zn3 O25 91.11(18) . . . . ? O1W Zn1 Zn3 O25 -54.39(15) . . . . ? O19 Zn1 Zn3 O25 115.17(14) . . . . ? Na2 Zn1 Zn3 O25 102.62(13) . . . . ? O25 Zn1 Zn3 O20 -109.78(14) . . . . ? O6 Zn1 Zn3 O20 106.35(10) 2_545 . . . ? O23 Zn1 Zn3 O20 -18.67(14) . . . . ? O1W Zn1 Zn3 O20 -164.17(11) . . . . ? O19 Zn1 Zn3 O20 5.40(9) . . . . ? Na2 Zn1 Zn3 O20 -7.16(7) . . . . ? O25 Zn1 Zn3 O5 143.68(15) . . . 2_545 ? O6 Zn1 Zn3 O5 -0.19(11) 2_545 . . 2_545 ? O23 Zn1 Zn3 O5 -125.21(15) . . . 2_545 ? O1W Zn1 Zn3 O5 89.29(11) . . . 2_545 ? O19 Zn1 Zn3 O5 -101.15(10) . . . 2_545 ? Na2 Zn1 Zn3 O5 -113.70(8) . . . 2_545 ? O25 Zn1 Zn3 O21 55.57(15) . . . 2_655 ? O6 Zn1 Zn3 O21 -88.30(11) 2_545 . . 2_655 ? O23 Zn1 Zn3 O21 146.68(15) . . . 2_655 ? O1W Zn1 Zn3 O21 1.18(12) . . . 2_655 ? O19 Zn1 Zn3 O21 170.74(10) . . . 2_655 ? Na2 Zn1 Zn3 O21 158.18(8) . . . 2_655 ? O25 Zn1 Zn3 O22 165.8(4) . . . 2_655 ? O6 Zn1 Zn3 O22 21.9(3) 2_545 . . 2_655 ? O23 Zn1 Zn3 O22 -103.1(4) . . . 2_655 ? O1W Zn1 Zn3 O22 111.4(3) . . . 2_655 ? O19 Zn1 Zn3 O22 -79.0(3) . . . 2_655 ? Na2 Zn1 Zn3 O22 -91.6(3) . . . 2_655 ? O25 Zn1 Zn3 C68 69.3(2) . . . 2_655 ? O6 Zn1 Zn3 C68 -74.55(19) 2_545 . . 2_655 ? O23 Zn1 Zn3 C68 160.4(2) . . . 2_655 ? O1W Zn1 Zn3 C68 14.9(2) . . . 2_655 ? O19 Zn1 Zn3 C68 -175.50(19) . . . 2_655 ? Na2 Zn1 Zn3 C68 171.94(18) . . . 2_655 ? O25 Zn1 Na2 O14 41.52(12) . . . . ? O6 Zn1 Na2 O14 -88.68(10) 2_545 . . . ? O23 Zn1 Na2 O14 171.40(13) . . . . ? O1W Zn1 Na2 O14 155.40(12) . . . . ? O19 Zn1 Na2 O14 -16.75(11) . . . . ? Zn3 Zn1 Na2 O14 1.48(8) . . . . ? O25 Zn1 Na2 O16 -130.24(10) . . . . ? O6 Zn1 Na2 O16 99.56(10) 2_545 . . . ? O23 Zn1 Na2 O16 -0.35(12) . . . . ? O1W Zn1 Na2 O16 -16.36(12) . . . . ? O19 Zn1 Na2 O16 171.50(11) . . . . ? Zn3 Zn1 Na2 O16 -170.27(6) . . . . ? O25 Zn1 Na2 O19 58.26(13) . . . . ? O6 Zn1 Na2 O19 -71.93(12) 2_545 . . . ? O23 Zn1 Na2 O19 -171.85(14) . . . . ? O1W Zn1 Na2 O19 172.14(13) . . . . ? Zn3 Zn1 Na2 O19 18.23(9) . . . . ? O25 Zn1 Na2 O23 -129.89(14) . . . . ? O6 Zn1 Na2 O23 99.91(13) 2_545 . . . ? O1W Zn1 Na2 O23 -16.01(14) . . . . ? O19 Zn1 Na2 O23 171.85(14) . . . . ? Zn3 Zn1 Na2 O23 -169.92(11) . . . . ? O25 Zn1 Na2 O13 135.17(11) . . . . ? O6 Zn1 Na2 O13 4.97(10) 2_545 . . . ? O23 Zn1 Na2 O13 -94.95(13) . . . . ? O1W Zn1 Na2 O13 -110.95(12) . . . . ? O19 Zn1 Na2 O13 76.90(11) . . . . ? Zn3 Zn1 Na2 O13 95.13(7) . . . . ? O25 Zn1 Na2 O15 -46.46(11) . . . . ? O6 Zn1 Na2 O15 -176.66(9) 2_545 . . . ? O23 Zn1 Na2 O15 83.43(12) . . . . ? O1W Zn1 Na2 O15 67.42(11) . . . . ? O19 Zn1 Na2 O15 -104.72(11) . . . . ? Zn3 Zn1 Na2 O15 -86.49(6) . . . . ? O25 Zn1 Na2 C66 46.81(11) . . . . ? O6 Zn1 Na2 C66 -83.38(10) 2_545 . . . ? O23 Zn1 Na2 C66 176.70(13) . . . . ? O1W Zn1 Na2 C66 160.69(12) . . . . ? O19 Zn1 Na2 C66 -11.45(11) . . . . ? Zn3 Zn1 Na2 C66 6.78(7) . . . . ? O12 Na1 Na3 O2W -18.29(16) . . . . ? O2 Na1 Na3 O2W 167.96(13) . . . . ? O1 Na1 Na3 O2W -93.40(13) . . . . ? O3 Na1 Na3 O2W 80.68(13) . . . . ? O4 Na1 Na3 O2W -6.63(14) . . . . ? O8 Na1 Na3 O2W -152.90(14) . . . . ? O10 Na1 Na3 O2W 106.38(15) . . . . ? C36 Na1 Na3 O2W -9.53(15) . . . . ? O12 Na1 Na3 O10 -124.66(15) . . . . ? O2 Na1 Na3 O10 61.59(11) . . . . ? O1 Na1 Na3 O10 160.22(11) . . . . ? O3 Na1 Na3 O10 -25.70(10) . . . . ? O4 Na1 Na3 O10 -113.00(12) . . . . ? O8 Na1 Na3 O10 100.73(11) . . . . ? C36 Na1 Na3 O10 -115.91(13) . . . . ? O2 Na1 Na3 O12 -173.75(14) . . . . ? O1 Na1 Na3 O12 -75.12(13) . . . . ? O3 Na1 Na3 O12 98.96(14) . . . . ? O4 Na1 Na3 O12 11.66(13) . . . . ? O8 Na1 Na3 O12 -134.61(14) . . . . ? O10 Na1 Na3 O12 124.66(15) . . . . ? C36 Na1 Na3 O12 8.75(15) . . . . ? O12 Na1 Na3 O18 106.87(14) . . . 2_545 ? O2 Na1 Na3 O18 -66.88(10) . . . 2_545 ? O1 Na1 Na3 O18 31.75(10) . . . 2_545 ? O3 Na1 Na3 O18 -154.17(9) . . . 2_545 ? O4 Na1 Na3 O18 118.53(10) . . . 2_545 ? O8 Na1 Na3 O18 -27.74(9) . . . 2_545 ? O10 Na1 Na3 O18 -128.47(12) . . . 2_545 ? C36 Na1 Na3 O18 115.62(12) . . . 2_545 ? O12 Na1 Na3 O8 134.61(14) . . . . ? O2 Na1 Na3 O8 -39.14(9) . . . . ? O1 Na1 Na3 O8 59.50(9) . . . . ? O3 Na1 Na3 O8 -126.43(10) . . . . ? O4 Na1 Na3 O8 146.27(11) . . . . ? O10 Na1 Na3 O8 -100.73(11) . . . . ? C36 Na1 Na3 O8 143.36(12) . . . . ? O12 Na1 Na3 O7 -131.98(15) . . . 2_545 ? O2 Na1 Na3 O7 54.27(11) . . . 2_545 ? O1 Na1 Na3 O7 152.90(9) . . . 2_545 ? O3 Na1 Na3 O7 -33.02(11) . . . 2_545 ? O4 Na1 Na3 O7 -120.32(11) . . . 2_545 ? O8 Na1 Na3 O7 93.41(11) . . . 2_545 ? O10 Na1 Na3 O7 -7.32(11) . . . 2_545 ? C36 Na1 Na3 O7 -123.23(13) . . . 2_545 ? O12 Na1 Na3 Zn2 129.20(13) . . . 2_545 ? O2 Na1 Na3 Zn2 -44.55(8) . . . 2_545 ? O1 Na1 Na3 Zn2 54.08(7) . . . 2_545 ? O3 Na1 Na3 Zn2 -131.84(6) . . . 2_545 ? O4 Na1 Na3 Zn2 140.86(7) . . . 2_545 ? O8 Na1 Na3 Zn2 -5.41(7) . . . 2_545 ? O10 Na1 Na3 Zn2 -106.14(9) . . . 2_545 ? C36 Na1 Na3 Zn2 137.95(10) . . . 2_545 ? C6 C1 C2 C3 7.7(4) . . . . ? O1 C1 C2 C3 -175.2(3) . . . . ? C6 C1 C2 C28 -168.2(3) . . . . ? O1 C1 C2 C28 8.8(4) . . . . ? C1 C2 C3 C4 -1.7(5) . . . . ? C28 C2 C3 C4 174.3(3) . . . . ? C2 C3 C4 C5 -3.6(5) . . . . ? C3 C4 C5 C6 3.1(5) . . . . ? C4 C5 C6 C1 2.6(5) . . . . ? C4 C5 C6 C7 -171.7(3) . . . . ? C2 C1 C6 C5 -8.2(5) . . . . ? O1 C1 C6 C5 174.8(3) . . . . ? C2 C1 C6 C7 165.8(3) . . . . ? O1 C1 C6 C7 -11.2(4) . . . . ? C5 C6 C7 C8 75.7(4) . . . . ? C1 C6 C7 C8 -98.3(3) . . . . ? C6 C7 C8 C13 102.2(3) . . . . ? C6 C7 C8 C9 -73.3(4) . . . . ? C13 C8 C9 C10 -3.8(5) . . . . ? C7 C8 C9 C10 171.9(3) . . . . ? C8 C9 C10 C11 -1.6(6) . . . . ? C9 C10 C11 C12 3.9(5) . . . . ? C10 C11 C12 C13 -0.8(5) . . . . ? C10 C11 C12 C14 -178.5(3) . . . . ? C9 C8 C13 C12 7.2(4) . . . . ? C7 C8 C13 C12 -168.5(3) . . . . ? C9 C8 C13 O2 -175.5(3) . . . . ? C7 C8 C13 O2 8.8(4) . . . . ? C11 C12 C13 C8 -4.9(4) . . . . ? C14 C12 C13 C8 172.8(3) . . . . ? C11 C12 C13 O2 177.8(3) . . . . ? C14 C12 C13 O2 -4.5(4) . . . . ? C13 C12 C14 C15 -104.1(3) . . . . ? C11 C12 C14 C15 73.6(4) . . . . ? C12 C14 C15 C20 90.2(4) . . . . ? C12 C14 C15 C16 -85.0(4) . . . . ? C20 C15 C16 C17 0.0(5) . . . . ? C14 C15 C16 C17 175.3(3) . . . . ? C15 C16 C17 C18 -5.5(6) . . . . ? C16 C17 C18 C19 5.2(6) . . . . ? C17 C18 C19 C20 0.5(5) . . . . ? C17 C18 C19 C21 -175.5(3) . . . . ? C16 C15 C20 O3 -171.9(3) . . . . ? C14 C15 C20 O3 12.7(5) . . . . ? C16 C15 C20 C19 6.1(5) . . . . ? C14 C15 C20 C19 -169.2(3) . . . . ? C18 C19 C20 C15 -6.4(5) . . . . ? C21 C19 C20 C15 169.6(3) . . . . ? C18 C19 C20 O3 171.7(3) . . . . ? C21 C19 C20 O3 -12.3(5) . . . . ? C20 C19 C21 C22 -91.8(4) . . . . ? C18 C19 C21 C22 84.0(4) . . . . ? C19 C21 C22 C23 -74.6(4) . . . . ? C19 C21 C22 C27 103.2(3) . . . . ? C27 C22 C23 C24 0.3(5) . . . . ? C21 C22 C23 C24 178.3(3) . . . . ? C22 C23 C24 C25 -1.7(5) . . . . ? C23 C24 C25 C26 -0.3(5) . . . . ? C24 C25 C26 C27 3.4(5) . . . . ? C24 C25 C26 C28 -172.8(3) . . . . ? C25 C26 C27 C22 -4.8(5) . . . . ? C28 C26 C27 C22 171.3(3) . . . . ? C25 C26 C27 O4 178.9(3) . . . . ? C28 C26 C27 O4 -5.0(4) . . . . ? C23 C22 C27 C26 3.0(5) . . . . ? C21 C22 C27 C26 -174.9(3) . . . . ? C23 C22 C27 O4 179.3(3) . . . . ? C21 C22 C27 O4 1.4(5) . . . . ? C27 C26 C28 C2 -96.6(3) . . . . ? C25 C26 C28 C2 79.5(3) . . . . ? C1 C2 C28 C26 96.7(3) . . . . ? C3 C2 C28 C26 -79.0(4) . . . . ? O1 C29 C30 O5 0.7(5) . . . . ? O1 C29 C30 O6 -178.4(3) . . . . ? O2 C31 C32 O8 -0.2(4) . . . . ? O2 C31 C32 O7 177.1(3) . . . . ? O3 C33 C34 O10 -8.4(5) . . . . ? O3 C33 C34 O9 170.0(3) . . . . ? O4 C35 C36 O11 168.0(4) . . . . ? O4 C35 C36 O12 -13.8(5) . . . . ? O4 C35 C36 Na1 -1.9(3) . . . . ? O12 Na1 C36 O11 41.6(7) . . . . ? O2 Na1 C36 O11 9.2(13) . . . . ? O1 Na1 C36 O11 134.1(8) . . . . ? O3 Na1 C36 O11 -84.2(8) . . . . ? O4 Na1 C36 O11 -154.3(9) . . . . ? O8 Na1 C36 O11 50.2(9) . . . . ? O10 Na1 C36 O11 -17.9(9) . . . . ? Na3 Na1 C36 O11 22.3(8) . . . . ? O2 Na1 C36 O12 -32.4(8) . . . . ? O1 Na1 C36 O12 92.5(3) . . . . ? O3 Na1 C36 O12 -125.9(3) . . . . ? O4 Na1 C36 O12 164.1(4) . . . . ? O8 Na1 C36 O12 8.5(4) . . . . ? O10 Na1 C36 O12 -59.5(3) . . . . ? Na3 Na1 C36 O12 -19.3(3) . . . . ? O12 Na1 C36 C35 -162.7(5) . . . . ? O2 Na1 C36 C35 164.8(5) . . . . ? O1 Na1 C36 C35 -70.2(2) . . . . ? O3 Na1 C36 C35 71.4(2) . . . . ? O4 Na1 C36 C35 1.36(19) . . . . ? O8 Na1 C36 C35 -154.2(2) . . . . ? O10 Na1 C36 C35 137.7(2) . . . . ? Na3 Na1 C36 C35 178.0(2) . . . . ? O14 C37 C38 C39 -169.7(3) . . . . ? C42 C37 C38 C39 8.2(5) . . . . ? O14 C37 C38 C64 14.7(4) . . . . ? C42 C37 C38 C64 -167.5(3) . . . . ? C37 C38 C39 C40 -0.9(5) . . . . ? C64 C38 C39 C40 174.7(3) . . . . ? C38 C39 C40 C41 -5.4(5) . . . . ? C39 C40 C41 C42 4.9(5) . . . . ? C40 C41 C42 C37 2.0(5) . . . . ? C40 C41 C42 C43 -174.0(3) . . . . ? O14 C37 C42 C41 169.2(3) . . . . ? C38 C37 C42 C41 -8.7(4) . . . . ? O14 C37 C42 C43 -14.8(4) . . . . ? C38 C37 C42 C43 167.3(3) . . . . ? C41 C42 C43 C44 88.0(4) . . . . ? C37 C42 C43 C44 -87.8(4) . . . . ? C42 C43 C44 C45 -74.2(4) . . . . ? C42 C43 C44 C49 106.2(4) . . . . ? C49 C44 C45 C46 -1.8(5) . . . . ? C43 C44 C45 C46 178.5(3) . . . . ? C44 C45 C46 C47 -0.2(5) . . . . ? C45 C46 C47 C48 0.1(5) . . . . ? C46 C47 C48 C49 2.0(5) . . . . ? C46 C47 C48 C50 -176.4(3) . . . . ? C47 C48 C49 O15 179.1(3) . . . . ? C50 C48 C49 O15 -2.6(4) . . . . ? C47 C48 C49 C44 -4.1(5) . . . . ? C50 C48 C49 C44 174.2(3) . . . . ? C45 C44 C49 O15 -179.2(3) . . . . ? C43 C44 C49 O15 0.5(4) . . . . ? C45 C44 C49 C48 4.0(5) . . . . ? C43 C44 C49 C48 -176.4(3) . . . . ? C47 C48 C50 C51 76.6(4) . . . . ? C49 C48 C50 C51 -101.7(3) . . . . ? C48 C50 C51 C52 -89.9(4) . . . . ? C48 C50 C51 C56 88.0(4) . . . . ? C56 C51 C52 C53 -3.4(5) . . . . ? C50 C51 C52 C53 174.6(3) . . . . ? C51 C52 C53 C54 -3.6(5) . . . . ? C52 C53 C54 C55 4.4(5) . . . . ? C53 C54 C55 C56 1.9(5) . . . . ? C53 C54 C55 C57 -171.5(3) . . . . ? C52 C51 C56 C55 10.1(5) . . . . ? C50 C51 C56 C55 -167.9(3) . . . . ? C52 C51 C56 O16 -170.1(3) . . . . ? C50 C51 C56 O16 11.9(4) . . . . ? C54 C55 C56 C51 -9.3(5) . . . . ? C57 C55 C56 C51 164.2(3) . . . . ? C54 C55 C56 O16 170.9(3) . . . . ? C57 C55 C56 O16 -15.6(4) . . . . ? C54 C55 C57 C59 86.8(3) . . . . ? C56 C55 C57 C59 -86.3(3) . . . . ? C63 C58 C59 C60 1.5(5) . . . . ? O13 C58 C59 C60 178.3(3) . . . . ? C63 C58 C59 C57 -177.8(3) . . . . ? O13 C58 C59 C57 -1.0(4) . . . . ? C55 C57 C59 C60 -66.2(4) . . . . ? C55 C57 C59 C58 113.0(3) . . . . ? C58 C59 C60 C61 1.1(5) . . . . ? C57 C59 C60 C61 -179.6(3) . . . . ? C59 C60 C61 C62 -1.7(6) . . . . ? C60 C61 C62 C63 -0.3(6) . . . . ? O13 C58 C63 C62 180.0(3) . . . . ? C59 C58 C63 C62 -3.3(5) . . . . ? O13 C58 C63 C64 -4.5(5) . . . . ? C59 C58 C63 C64 172.3(3) . . . . ? C61 C62 C63 C58 2.7(5) . . . . ? C61 C62 C63 C64 -173.1(3) . . . . ? C39 C38 C64 C63 -91.6(4) . . . . ? C37 C38 C64 C63 83.9(4) . . . . ? C58 C63 C64 C38 -105.3(4) . . . . ? C62 C63 C64 C38 70.2(4) . . . . ? O14 C65 C66 O19 10.8(5) . . . . ? O14 C65 C66 O20 -170.0(3) . . . . ? O14 C65 C66 Na2 0.1(3) . . . . ? O14 Na2 C66 O19 -166.1(3) . . . . ? O16 Na2 C66 O19 28.9(4) . . . . ? O23 Na2 C66 O19 22.1(2) . . . . ? O13 Na2 C66 O19 -90.4(2) . . . . ? O15 Na2 C66 O19 115.7(2) . . . . ? Zn1 Na2 C66 O19 20.3(2) . . . . ? O14 Na2 C66 O20 146.2(8) . . . . ? O16 Na2 C66 O20 -18.8(10) . . . . ? O19 Na2 C66 O20 -47.7(7) . . . . ? O23 Na2 C66 O20 -25.6(8) . . . . ? O13 Na2 C66 O20 -138.1(8) . . . . ? O15 Na2 C66 O20 68.0(8) . . . . ? Zn1 Na2 C66 O20 -27.3(8) . . . . ? O14 Na2 C66 C65 -0.09(19) . . . . ? O16 Na2 C66 C65 -165.1(3) . . . . ? O19 Na2 C66 C65 166.0(4) . . . . ? O23 Na2 C66 C65 -171.9(2) . . . . ? O13 Na2 C66 C65 75.6(2) . . . . ? O15 Na2 C66 C65 -78.3(2) . . . . ? Zn1 Na2 C66 C65 -173.7(2) . . . . ? O15 C67 C68 O21 4.3(4) . . . . ? O15 C67 C68 O22 -174.7(3) . . . . ? O15 C67 C68 Zn3 -119(5) . . . 2_655 ? O16 C69 C70 O24 178.9(3) . . . . ? O16 C69 C70 O23 -0.3(4) . . . . ? O13 C71 C72 O17 -10.0(5) . . . . ? O13 C71 C72 O18 172.6(3) . . . . ? N1 C74 C75 N2 -0.5(4) . . . . ? N2 C76 C77 C77 -65.0(5) . . . 2 ? N2 C73 N1 C74 0.3(3) . . . . ? N2 C73 N1 Zn2 -178.0(2) . . . . ? C75 C74 N1 C73 0.1(4) . . . . ? C75 C74 N1 Zn2 178.5(2) . . . . ? O18 Zn2 N1 C73 26.9(3) . . . . ? O9 Zn2 N1 C73 -97.6(3) . . . . ? O7 Zn2 N1 C73 151.1(3) 2_545 . . . ? Na3 Zn2 N1 C73 73.0(3) 2_545 . . . ? O18 Zn2 N1 C74 -151.1(2) . . . . ? O9 Zn2 N1 C74 84.4(3) . . . . ? O7 Zn2 N1 C74 -26.9(3) 2_545 . . . ? Na3 Zn2 N1 C74 -105.0(2) 2_545 . . . ? N1 C73 N2 C75 -0.6(4) . . . . ? N1 C73 N2 C76 -178.2(3) . . . . ? C74 C75 N2 C73 0.7(4) . . . . ? C74 C75 N2 C76 178.2(3) . . . . ? C77 C76 N2 C73 -98.5(4) . . . . ? C77 C76 N2 C75 84.4(5) . . . . ? C2 C1 O1 C29 106.4(3) . . . . ? C6 C1 O1 C29 -76.5(3) . . . . ? C2 C1 O1 Na1 -98.2(3) . . . . ? C6 C1 O1 Na1 79.0(3) . . . . ? C30 C29 O1 C1 -100.3(3) . . . . ? C30 C29 O1 Na1 100.7(3) . . . . ? O12 Na1 O1 C1 147.1(2) . . . . ? O2 Na1 O1 C1 -61.3(2) . . . . ? O3 Na1 O1 C1 20.8(3) . . . . ? O4 Na1 O1 C1 79.1(2) . . . . ? O8 Na1 O1 C1 -127.1(2) . . . . ? O10 Na1 O1 C1 -136.9(2) . . . . ? C36 Na1 O1 C1 127.5(2) . . . . ? Na3 Na1 O1 C1 -168.0(2) . . . . ? O12 Na1 O1 C29 -57.28(19) . . . . ? O2 Na1 O1 C29 94.29(18) . . . . ? O3 Na1 O1 C29 176.45(18) . . . . ? O4 Na1 O1 C29 -125.28(19) . . . . ? O8 Na1 O1 C29 28.51(18) . . . . ? O10 Na1 O1 C29 18.7(3) . . . . ? C36 Na1 O1 C29 -76.92(19) . . . . ? Na3 Na1 O1 C29 -12.34(19) . . . . ? C8 C13 O2 C31 88.7(3) . . . . ? C12 C13 O2 C31 -93.9(3) . . . . ? C8 C13 O2 Na1 -85.8(3) . . . . ? C12 C13 O2 Na1 91.6(3) . . . . ? C32 C31 O2 C13 -150.2(3) . . . . ? C32 C31 O2 Na1 24.8(3) . . . . ? O12 Na1 O2 C13 170.5(3) . . . . ? O1 Na1 O2 C13 67.1(2) . . . . ? O3 Na1 O2 C13 -73.1(2) . . . . ? O4 Na1 O2 C13 -7.8(3) . . . . ? O8 Na1 O2 C13 148.5(3) . . . . ? O10 Na1 O2 C13 -140.4(2) . . . . ? C36 Na1 O2 C13 -167.9(6) . . . . ? Na3 Na1 O2 C13 179.8(2) . . . . ? O12 Na1 O2 C31 -3.8(4) . . . . ? O1 Na1 O2 C31 -107.2(2) . . . . ? O3 Na1 O2 C31 112.6(2) . . . . ? O4 Na1 O2 C31 178.0(2) . . . . ? O8 Na1 O2 C31 -25.8(2) . . . . ? O10 Na1 O2 C31 45.3(2) . . . . ? C36 Na1 O2 C31 17.8(7) . . . . ? Na3 Na1 O2 C31 5.5(2) . . . . ? C15 C20 O3 C33 89.1(3) . . . . ? C19 C20 O3 C33 -89.0(3) . . . . ? C15 C20 O3 Na1 -87.8(3) . . . . ? C19 C20 O3 Na1 94.0(3) . . . . ? C34 C33 O3 C20 -151.8(3) . . . . ? C34 C33 O3 Na1 25.8(3) . . . . ? O12 Na1 O3 C20 -136.9(3) . . . . ? O2 Na1 O3 C20 70.6(3) . . . . ? O1 Na1 O3 C20 -15.0(3) . . . . ? O4 Na1 O3 C20 -72.8(3) . . . . ? O8 Na1 O3 C20 122.2(3) . . . . ? O10 Na1 O3 C20 153.8(3) . . . . ? C36 Na1 O3 C20 -120.2(3) . . . . ? Na3 Na1 O3 C20 173.6(2) . . . . ? O12 Na1 O3 C33 46.3(2) . . . . ? O2 Na1 O3 C33 -106.2(2) . . . . ? O1 Na1 O3 C33 168.2(2) . . . . ? O4 Na1 O3 C33 110.4(2) . . . . ? O8 Na1 O3 C33 -54.6(2) . . . . ? O10 Na1 O3 C33 -23.0(2) . . . . ? C36 Na1 O3 C33 63.0(2) . . . . ? Na3 Na1 O3 C33 -3.2(2) . . . . ? O10 Na3 O2W O2W' -53.9(5) . . . . ? O12 Na3 O2W O2W' -121.1(5) . . . . ? O18 Na3 O2W O2W' 120.0(5) 2_545 . . . ? O8 Na3 O2W O2W' -157.8(5) . . . . ? O7 Na3 O2W O2W' 25.1(5) 2_545 . . . ? Na1 Na3 O2W O2W' -108.8(5) . . . . ? Zn2 Na3 O2W O2W' 119.6(5) 2_545 . . . ? C26 C27 O4 C35 -89.4(4) . . . . ? C22 C27 O4 C35 94.1(3) . . . . ? C26 C27 O4 Na1 89.4(3) . . . . ? C22 C27 O4 Na1 -87.0(3) . . . . ? C36 C35 O4 C27 -178.3(3) . . . . ? C36 C35 O4 Na1 2.6(4) . . . . ? O12 Na1 O4 C27 -174.8(3) . . . . ? O2 Na1 O4 C27 4.3(3) . . . . ? O1 Na1 O4 C27 -75.7(3) . . . . ? O3 Na1 O4 C27 70.7(3) . . . . ? O8 Na1 O4 C27 -131.6(3) . . . . ? O10 Na1 O4 C27 123.7(3) . . . . ? C36 Na1 O4 C27 179.6(3) . . . . ? Na3 Na1 O4 C27 176.2(3) . . . . ? O12 Na1 O4 C35 4.1(2) . . . . ? O2 Na1 O4 C35 -176.9(2) . . . . ? O1 Na1 O4 C35 103.2(2) . . . . ? O3 Na1 O4 C35 -110.5(2) . . . . ? O8 Na1 O4 C35 47.2(3) . . . . ? O10 Na1 O4 C35 -57.4(2) . . . . ? C36 Na1 O4 C35 -1.6(2) . . . . ? Na3 Na1 O4 C35 -5.0(2) . . . . ? O6 C30 O5 Zn3 -5.2(5) . . . 2_545 ? C29 C30 O5 Zn3 175.9(2) . . . 2_545 ? O5 C30 O6 Zn1 5.0(5) . . . 2_545 ? C29 C30 O6 Zn1 -175.9(2) . . . 2_545 ? O8 C32 O7 Zn2 18.8(4) . . . 2_545 ? C31 C32 O7 Zn2 -158.4(2) . . . 2_545 ? O8 C32 O7 Na3 -116.0(3) . . . 2_545 ? C31 C32 O7 Na3 66.7(4) . . . 2_545 ? O7 C32 O8 Na1 160.8(2) . . . . ? C31 C32 O8 Na1 -22.2(4) . . . . ? O7 C32 O8 Na3 66.7(4) . . . . ? C31 C32 O8 Na3 -116.2(3) . . . . ? O12 Na1 O8 C32 -144.2(2) . . . . ? O2 Na1 O8 C32 25.3(2) . . . . ? O1 Na1 O8 C32 121.1(2) . . . . ? O3 Na1 O8 C32 -32.9(3) . . . . ? O4 Na1 O8 C32 175.9(2) . . . . ? O10 Na1 O8 C32 -63.8(2) . . . . ? C36 Na1 O8 C32 -147.1(2) . . . . ? Na3 Na1 O8 C32 -112.9(2) . . . . ? O12 Na1 O8 Na3 -31.33(10) . . . . ? O2 Na1 O8 Na3 138.14(9) . . . . ? O1 Na1 O8 Na3 -126.03(8) . . . . ? O3 Na1 O8 Na3 80.00(11) . . . . ? O4 Na1 O8 Na3 -71.26(18) . . . . ? O10 Na1 O8 Na3 49.05(8) . . . . ? C36 Na1 O8 Na3 -34.20(11) . . . . ? O2W Na3 O8 C32 179.8(2) . . . . ? O10 Na3 O8 C32 63.9(2) . . . . ? O12 Na3 O8 C32 143.5(2) . . . . ? O18 Na3 O8 C32 -90.8(2) 2_545 . . . ? O7 Na3 O8 C32 -3.4(2) 2_545 . . . ? Na1 Na3 O8 C32 114.9(2) . . . . ? Zn2 Na3 O8 C32 -72.37(19) 2_545 . . . ? O2W Na3 O8 Na1 64.9(2) . . . . ? O10 Na3 O8 Na1 -50.94(8) . . . . ? O12 Na3 O8 Na1 28.64(9) . . . . ? O18 Na3 O8 Na1 154.37(9) 2_545 . . . ? O7 Na3 O8 Na1 -118.26(8) 2_545 . . . ? Zn2 Na3 O8 Na1 172.77(9) 2_545 . . . ? O10 C34 O9 Zn2 20.1(4) . . . . ? C33 C34 O9 Zn2 -158.2(2) . . . . ? O18 Zn2 O9 C34 55.5(2) . . . . ? N1 Zn2 O9 C34 -173.4(2) . . . . ? O7 Zn2 O9 C34 -66.3(2) 2_545 . . . ? Na3 Zn2 O9 C34 17.7(3) 2_545 . . . ? O9 C34 O10 Na3 57.7(5) . . . . ? C33 C34 O10 Na3 -124.1(3) . . . . ? O9 C34 O10 Na1 168.5(2) . . . . ? C33 C34 O10 Na1 -13.3(4) . . . . ? O2W Na3 O10 C34 22.8(3) . . . . ? O12 Na3 O10 C34 90.5(3) . . . . ? O18 Na3 O10 C34 -148.8(3) 2_545 . . . ? O8 Na3 O10 C34 175.3(3) . . . . ? O7 Na3 O10 C34 -61.3(3) 2_545 . . . ? Na1 Na3 O10 C34 124.6(3) . . . . ? Zn2 Na3 O10 C34 -152.4(3) 2_545 . . . ? O2W Na3 O10 Na1 -101.80(12) . . . . ? O12 Na3 O10 Na1 -34.10(9) . . . . ? O18 Na3 O10 Na1 86.63(14) 2_545 . . . ? O8 Na3 O10 Na1 50.70(7) . . . . ? O7 Na3 O10 Na1 174.16(9) 2_545 . . . ? Zn2 Na3 O10 Na1 83.06(7) 2_545 . . . ? O12 Na1 O10 C34 -96.1(3) . . . . ? O2 Na1 O10 C34 105.9(2) . . . . ? O1 Na1 O10 C34 -175.7(2) . . . . ? O3 Na1 O10 C34 19.7(2) . . . . ? O4 Na1 O10 C34 -39.3(3) . . . . ? O8 Na1 O10 C34 173.9(3) . . . . ? C36 Na1 O10 C34 -79.0(3) . . . . ? Na3 Na1 O10 C34 -133.6(3) . . . . ? O12 Na1 O10 Na3 37.54(10) . . . . ? O2 Na1 O10 Na3 -120.43(9) . . . . ? O1 Na1 O10 Na3 -42.0(2) . . . . ? O3 Na1 O10 Na3 153.34(11) . . . . ? O4 Na1 O10 Na3 94.31(10) . . . . ? O8 Na1 O10 Na3 -52.43(8) . . . . ? C36 Na1 O10 Na3 54.64(10) . . . . ? O11 C36 O12 Na1 -162.0(4) . . . . ? C35 C36 O12 Na1 19.9(5) . . . . ? O11 C36 O12 Na3 -20.1(7) . . . . ? C35 C36 O12 Na3 161.9(3) . . . . ? Na1 C36 O12 Na3 141.9(6) . . . . ? O2 Na1 O12 C36 168.2(3) . . . . ? O1 Na1 O12 C36 -88.9(3) . . . . ? O3 Na1 O12 C36 58.0(3) . . . . ? O4 Na1 O12 C36 -13.0(3) . . . . ? O8 Na1 O12 C36 -171.8(3) . . . . ? O10 Na1 O12 C36 118.8(3) . . . . ? Na3 Na1 O12 C36 155.7(4) . . . . ? O2 Na1 O12 Na3 12.5(3) . . . . ? O1 Na1 O12 Na3 115.42(10) . . . . ? O3 Na1 O12 Na3 -97.70(10) . . . . ? O4 Na1 O12 Na3 -168.76(13) . . . . ? O8 Na1 O12 Na3 32.52(10) . . . . ? O10 Na1 O12 Na3 -36.89(10) . . . . ? C36 Na1 O12 Na3 -155.7(4) . . . . ? O2W Na3 O12 C36 14.5(4) . . . . ? O10 Na3 O12 C36 -110.4(4) . . . . ? O18 Na3 O12 C36 114.0(4) 2_545 . . . ? O8 Na3 O12 C36 178.9(4) . . . . ? O7 Na3 O12 C36 -57.4(5) 2_545 . . . ? Na1 Na3 O12 C36 -149.0(5) . . . . ? Zn2 Na3 O12 C36 148.8(4) 2_545 . . . ? O2W Na3 O12 Na1 163.52(14) . . . . ? O10 Na3 O12 Na1 38.59(11) . . . . ? O18 Na3 O12 Na1 -97.05(12) 2_545 . . . ? O8 Na3 O12 Na1 -32.09(10) . . . . ? O7 Na3 O12 Na1 91.56(17) 2_545 . . . ? Zn2 Na3 O12 Na1 -62.17(12) 2_545 . . . ? C63 C58 O13 C71 -67.4(4) . . . . ? C59 C58 O13 C71 115.7(3) . . . . ? C63 C58 O13 Na2 90.0(3) . . . . ? C59 C58 O13 Na2 -86.9(3) . . . . ? C72 C71 O13 C58 -117.6(3) . . . . ? C72 C71 O13 Na2 86.0(3) . . . . ? O14 Na2 O13 C58 -72.7(2) . . . . ? O16 Na2 O13 C58 75.1(2) . . . . ? O19 Na2 O13 C58 -143.3(2) . . . . ? O23 Na2 O13 C58 143.0(2) . . . . ? O15 Na2 O13 C58 1.7(3) . . . . ? C66 Na2 O13 C58 -122.0(2) . . . . ? Zn1 Na2 O13 C58 178.6(2) . . . . ? O14 Na2 O13 C71 83.4(2) . . . . ? O16 Na2 O13 C71 -128.7(2) . . . . ? O19 Na2 O13 C71 12.9(2) . . . . ? O23 Na2 O13 C71 -60.8(2) . . . . ? O15 Na2 O13 C71 157.8(2) . . . . ? C66 Na2 O13 C71 34.2(2) . . . . ? Zn1 Na2 O13 C71 -25.2(2) . . . . ? C38 C37 O14 C65 91.9(3) . . . . ? C42 C37 O14 C65 -86.1(3) . . . . ? C38 C37 O14 Na2 -92.1(4) . . . . ? C42 C37 O14 Na2 89.9(3) . . . . ? C66 C65 O14 C37 176.6(3) . . . . ? C66 C65 O14 Na2 -0.2(4) . . . . ? O16 Na2 O14 C37 -5.1(4) . . . . ? O19 Na2 O14 C37 179.1(3) . . . . ? O23 Na2 O14 C37 -162.6(3) . . . . ? O13 Na2 O14 C37 76.8(3) . . . . ? O15 Na2 O14 C37 -72.7(3) . . . . ? C66 Na2 O14 C37 -175.7(3) . . . . ? Zn1 Na2 O14 C37 -170.0(3) . . . . ? O16 Na2 O14 C65 170.8(2) . . . . ? O19 Na2 O14 C65 -5.1(2) . . . . ? O23 Na2 O14 C65 13.2(3) . . . . ? O13 Na2 O14 C65 -107.3(2) . . . . ? O15 Na2 O14 C65 103.1(2) . . . . ? C66 Na2 O14 C65 0.1(2) . . . . ? Zn1 Na2 O14 C65 5.9(2) . . . . ? C48 C49 O15 C67 -70.0(3) . . . . ? C44 C49 O15 C67 113.1(3) . . . . ? C48 C49 O15 Na2 89.8(3) . . . . ? C44 C49 O15 Na2 -87.1(3) . . . . ? C68 C67 O15 C49 -117.7(3) . . . . ? C68 C67 O15 Na2 80.8(3) . . . . ? O14 Na2 O15 C49 74.0(2) . . . . ? O16 Na2 O15 C49 -75.9(2) . . . . ? O19 Na2 O15 C49 143.5(2) . . . . ? O23 Na2 O15 C49 -145.0(2) . . . . ? O13 Na2 O15 C49 -0.5(3) . . . . ? C66 Na2 O15 C49 124.0(2) . . . . ? Zn1 Na2 O15 C49 -177.7(2) . . . . ? O14 Na2 O15 C67 -126.28(19) . . . . ? O16 Na2 O15 C67 83.82(19) . . . . ? O19 Na2 O15 C67 -56.8(2) . . . . ? O23 Na2 O15 C67 14.66(19) . . . . ? O13 Na2 O15 C67 159.2(2) . . . . ? C66 Na2 O15 C67 -76.3(2) . . . . ? Zn1 Na2 O15 C67 -17.97(19) . . . . ? C51 C56 O16 C69 99.2(3) . . . . ? C55 C56 O16 C69 -81.1(3) . . . . ? C51 C56 O16 Na2 -94.5(3) . . . . ? C55 C56 O16 Na2 85.3(3) . . . . ? C70 C69 O16 C56 -173.2(3) . . . . ? C70 C69 O16 Na2 17.8(3) . . . . ? O14 Na2 O16 C56 9.8(3) . . . . ? O19 Na2 O16 C56 -176.5(2) . . . . ? O23 Na2 O16 C56 174.9(3) . . . . ? O13 Na2 O16 C56 -71.2(3) . . . . ? O15 Na2 O16 C56 78.3(2) . . . . ? C66 Na2 O16 C56 167.8(3) . . . . ? Zn1 Na2 O16 C56 175.2(2) . . . . ? O14 Na2 O16 C69 175.6(2) . . . . ? O19 Na2 O16 C69 -10.7(3) . . . . ? O23 Na2 O16 C69 -19.3(2) . . . . ? O13 Na2 O16 C69 94.6(2) . . . . ? O15 Na2 O16 C69 -115.9(2) . . . . ? C66 Na2 O16 C69 -26.5(4) . . . . ? Zn1 Na2 O16 C69 -19.1(2) . . . . ? O17 C72 O18 Zn2 6.8(4) . . . . ? C71 C72 O18 Zn2 -175.9(2) . . . . ? O17 C72 O18 Na3 -149.6(3) . . . 2_545 ? C71 C72 O18 Na3 27.8(4) . . . 2_545 ? O9 Zn2 O18 C72 63.5(2) . . . . ? N1 Zn2 O18 C72 -58.3(2) . . . . ? O7 Zn2 O18 C72 -177.53(19) 2_545 . . . ? Na3 Zn2 O18 C72 -160.9(3) 2_545 . . . ? O9 Zn2 O18 Na3 -135.63(10) . . . 2_545 ? N1 Zn2 O18 Na3 102.62(13) . . . 2_545 ? O7 Zn2 O18 Na3 -16.62(13) 2_545 . . 2_545 ? O20 C66 O19 Zn1 23.9(5) . . . . ? C65 C66 O19 Zn1 -157.0(3) . . . . ? Na2 C66 O19 Zn1 -140.9(4) . . . . ? O20 C66 O19 Na2 164.9(3) . . . . ? C65 C66 O19 Na2 -16.1(4) . . . . ? O25 Zn1 O19 C66 17.5(3) . . . . ? O6 Zn1 O19 C66 -95.3(3) 2_545 . . . ? O23 Zn1 O19 C66 150.6(3) . . . . ? O1W Zn1 O19 C66 115.2(5) . . . . ? Zn3 Zn1 O19 C66 -16.1(3) . . . . ? Na2 Zn1 O19 C66 145.4(3) . . . . ? O25 Zn1 O19 Na2 -127.92(11) . . . . ? O6 Zn1 O19 Na2 119.28(9) 2_545 . . . ? O23 Zn1 O19 Na2 5.22(9) . . . . ? O1W Zn1 O19 Na2 -30.3(5) . . . . ? Zn3 Zn1 O19 Na2 -161.52(9) . . . . ? O14 Na2 O19 C66 11.4(2) . . . . ? O16 Na2 O19 C66 -165.1(2) . . . . ? O23 Na2 O19 C66 -156.6(3) . . . . ? O13 Na2 O19 C66 93.5(2) . . . . ? O15 Na2 O19 C66 -68.2(2) . . . . ? Zn1 Na2 O19 C66 -151.9(3) . . . . ? O14 Na2 O19 Zn1 163.29(11) . . . . ? O16 Na2 O19 Zn1 -13.17(18) . . . . ? O23 Na2 O19 Zn1 -4.65(8) . . . . ? O13 Na2 O19 Zn1 -114.57(9) . . . . ? O15 Na2 O19 Zn1 83.69(10) . . . . ? C66 Na2 O19 Zn1 151.9(3) . . . . ? O19 C66 O20 Zn3 -12.6(5) . . . . ? C65 C66 O20 Zn3 168.2(2) . . . . ? Na2 C66 O20 Zn3 24.7(9) . . . . ? O25 Zn3 O20 C66 -34.8(3) . . . . ? O5 Zn3 O20 C66 72.2(2) 2_545 . . . ? O21 Zn3 O20 C66 -158.1(2) 2_655 . . . ? O22 Zn3 O20 C66 168.2(2) 2_655 . . . ? C68 Zn3 O20 C66 -178.9(2) 2_655 . . . ? Zn1 Zn3 O20 C66 0.6(2) . . . . ? O22 C68 O21 Zn3 2.4(3) . . . 2_655 ? C67 C68 O21 Zn3 -176.6(3) . . . 2_655 ? O21 C68 O22 Zn3 -2.3(3) . . . 2_655 ? C67 C68 O22 Zn3 176.7(2) . . . 2_655 ? O24 C70 O23 Zn1 8.5(5) . . . . ? C69 C70 O23 Zn1 -172.3(2) . . . . ? O24 C70 O23 Na2 162.9(3) . . . . ? C69 C70 O23 Na2 -17.9(4) . . . . ? O25 Zn1 O23 C70 -130.9(3) . . . . ? O6 Zn1 O23 C70 57.8(3) 2_545 . . . ? O1W Zn1 O23 C70 -35.8(3) . . . . ? O19 Zn1 O23 C70 151.3(3) . . . . ? Zn3 Zn1 O23 C70 174.2(2) . . . . ? Na2 Zn1 O23 C70 156.7(3) . . . . ? O25 Zn1 O23 Na2 72.45(16) . . . . ? O6 Zn1 O23 Na2 -98.92(12) 2_545 . . . ? O1W Zn1 O23 Na2 167.53(11) . . . . ? O19 Zn1 O23 Na2 -5.39(9) . . . . ? Zn3 Zn1 O23 Na2 17.48(18) . . . . ? O14 Na2 O23 C70 -172.1(2) . . . . ? O16 Na2 O23 C70 20.5(2) . . . . ? O19 Na2 O23 C70 -153.8(2) . . . . ? O13 Na2 O23 C70 -60.0(2) . . . . ? O15 Na2 O23 C70 100.8(2) . . . . ? C66 Na2 O23 C70 -161.9(2) . . . . ? Zn1 Na2 O23 C70 -159.1(3) . . . . ? O14 Na2 O23 Zn1 -13.0(2) . . . . ? O16 Na2 O23 Zn1 179.63(12) . . . . ? O19 Na2 O23 Zn1 5.36(9) . . . . ? O13 Na2 O23 Zn1 99.15(11) . . . . ? O15 Na2 O23 Zn1 -100.03(10) . . . . ? C66 Na2 O23 Zn1 -2.79(11) . . . . ? O6 Zn1 O25 Zn3 39.38(15) 2_545 . . . ? O23 Zn1 O25 Zn3 -132.13(12) . . . . ? O1W Zn1 O25 Zn3 134.13(12) . . . . ? O19 Zn1 O25 Zn3 -58.05(11) . . . . ? Na2 Zn1 O25 Zn3 -91.70(11) . . . . ? O20 Zn3 O25 Zn1 72.53(13) . . . . ? O5 Zn3 O25 Zn1 -35.60(13) 2_545 . . . ? O21 Zn3 O25 Zn1 -136.52(11) 2_655 . . . ? O22 Zn3 O25 Zn1 -172.94(17) 2_655 . . . ? C68 Zn3 O25 Zn1 -148.11(11) 2_655 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1A O3W 0.828(18) 1.93(3) 2.690(5) 152(5) . O1W H1B O24 0.888(18) 1.94(3) 2.753(3) 152(4) . _diffrn_measured_fraction_theta_max 0.841 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.974 _refine_diff_density_min -0.867 _refine_diff_density_rms 0.073 #===== data_8 _database_code_depnum_ccdc_archive 'CCDC 879390' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C152 H144 N6 Na6 O59 Zn6' _chemical_formula_weight 3528.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.772(5) _cell_length_b 17.442(4) _cell_length_c 17.887(6) _cell_angle_alpha 115.964(2) _cell_angle_beta 96.529(7) _cell_angle_gamma 103.069(5) _cell_volume 3915(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7783 _exptl_absorpt_correction_T_max 0.8306 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21347 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13139 _reflns_number_gt 8965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distances of O1W---H1A and O1W---H1B were restrained to 0.87+-0.02 \%A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13139 _refine_ls_number_parameters 1062 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.77686(3) 0.37355(3) -0.10723(2) 0.03713(12) Uani 1 1 d . . . Zn2 Zn 0.55112(3) -0.07780(2) 0.10284(2) 0.03147(11) Uani 1 1 d . . . Zn3 Zn 0.93473(3) 0.46553(3) 0.06223(3) 0.05048(14) Uani 1 1 d . . . Na1 Na 0.65843(9) 0.27860(8) 0.20679(8) 0.0331(3) Uani 1 1 d . . . Na2 Na 0.17884(9) -0.17849(8) 0.24707(8) 0.0340(3) Uani 1 1 d . . . Na3 Na 0.33853(11) -0.09395(11) -0.03401(9) 0.0566(4) Uani 1 1 d . . . C1 C 0.6401(2) 0.4800(2) 0.22687(19) 0.0288(7) Uani 1 1 d . . . C2 C 0.7180(2) 0.5563(2) 0.27593(19) 0.0319(8) Uani 1 1 d . . . C3 C 0.7003(3) 0.6372(2) 0.3221(2) 0.0426(9) Uani 1 1 d . . . H3 H 0.7514 0.6895 0.3546 0.051 Uiso 1 1 calc R . . C4 C 0.6073(3) 0.6407(2) 0.3203(2) 0.0444(9) Uani 1 1 d . . . H4 H 0.5962 0.6956 0.3487 0.053 Uiso 1 1 calc R . . C5 C 0.5324(3) 0.5637(2) 0.2768(2) 0.0405(9) Uani 1 1 d . . . H5 H 0.4705 0.5667 0.2781 0.049 Uiso 1 1 calc R . . C6 C 0.5457(2) 0.4802(2) 0.23001(19) 0.0318(7) Uani 1 1 d . . . C7 C 0.4599(2) 0.3957(2) 0.1921(2) 0.0368(8) Uani 1 1 d . . . H7A H 0.4748 0.3458 0.1488 0.044 Uiso 1 1 calc R . . H7B H 0.4053 0.4045 0.1650 0.044 Uiso 1 1 calc R . . C8 C 0.4359(2) 0.3752(2) 0.2635(2) 0.0367(8) Uani 1 1 d . . . C9 C 0.3920(3) 0.4271(3) 0.3224(3) 0.0525(11) Uani 1 1 d . . . H9 H 0.3691 0.4686 0.3135 0.063 Uiso 1 1 calc R . . C10 C 0.3822(3) 0.4175(3) 0.3939(3) 0.0557(11) Uani 1 1 d . . . H10 H 0.3522 0.4524 0.4325 0.067 Uiso 1 1 calc R . . C11 C 0.4160(3) 0.3575(3) 0.4084(2) 0.0505(10) Uani 1 1 d . . . H11 H 0.4115 0.3540 0.4583 0.061 Uiso 1 1 calc R . . C12 C 0.4571(2) 0.3011(2) 0.3498(2) 0.0359(8) Uani 1 1 d . . . C13 C 0.4618(2) 0.3099(2) 0.2762(2) 0.0307(8) Uani 1 1 d . . . C14 C 0.4963(3) 0.2363(2) 0.3676(2) 0.0424(9) Uani 1 1 d . . . H14A H 0.4500 0.2043 0.3867 0.051 Uiso 1 1 calc R . . H14B H 0.5067 0.1926 0.3153 0.051 Uiso 1 1 calc R . . C15 C 0.5891(3) 0.2848(2) 0.4352(2) 0.0378(8) Uani 1 1 d . . . C16 C 0.5906(3) 0.3216(3) 0.5231(2) 0.0490(10) Uani 1 1 d . . . H16 H 0.5333 0.3125 0.5396 0.059 Uiso 1 1 calc R . . C17 C 0.6751(3) 0.3707(3) 0.5847(2) 0.0530(11) Uani 1 1 d . . . H17 H 0.6750 0.3915 0.6423 0.064 Uiso 1 1 calc R . . C18 C 0.7600(3) 0.3894(2) 0.5618(2) 0.0454(9) Uani 1 1 d . . . H18 H 0.8161 0.4259 0.6043 0.055 Uiso 1 1 calc R . . C19 C 0.7631(3) 0.3541(2) 0.4755(2) 0.0383(8) Uani 1 1 d . . . C20 C 0.6771(3) 0.2986(2) 0.4147(2) 0.0340(8) Uani 1 1 d . . . C21 C 0.8542(3) 0.3794(2) 0.4493(2) 0.0435(9) Uani 1 1 d . . . H21A H 0.8520 0.3318 0.3936 0.052 Uiso 1 1 calc R . . H21B H 0.9085 0.3862 0.4902 0.052 Uiso 1 1 calc R . . C22 C 0.8673(2) 0.4663(2) 0.4454(2) 0.0371(8) Uani 1 1 d . . . C23 C 0.8956(3) 0.5477(3) 0.5213(2) 0.0472(9) Uani 1 1 d . . . H23 H 0.9080 0.5479 0.5735 0.057 Uiso 1 1 calc R . . C24 C 0.9054(3) 0.6278(3) 0.5205(2) 0.0488(10) Uani 1 1 d . . . H24 H 0.9261 0.6815 0.5717 0.059 Uiso 1 1 calc R . . C25 C 0.8847(3) 0.6284(2) 0.4448(2) 0.0430(9) Uani 1 1 d . . . H25 H 0.8917 0.6829 0.4451 0.052 Uiso 1 1 calc R . . C26 C 0.8534(2) 0.5494(2) 0.3666(2) 0.0347(8) Uani 1 1 d . . . C27 C 0.8484(2) 0.4694(2) 0.3689(2) 0.0356(8) Uani 1 1 d . . . C28 C 0.8198(2) 0.5524(2) 0.2851(2) 0.0374(8) Uani 1 1 d . . . H28A H 0.8229 0.4995 0.2361 0.045 Uiso 1 1 calc R . . H28B H 0.8617 0.6048 0.2863 0.045 Uiso 1 1 calc R . . C29 C 0.6359(2) 0.3724(2) 0.08505(19) 0.0341(8) Uani 1 1 d . . . H29A H 0.5936 0.4038 0.0748 0.041 Uiso 1 1 calc R . . H29B H 0.6006 0.3089 0.0543 0.041 Uiso 1 1 calc R . . C30 C 0.7196(3) 0.3876(2) 0.0463(2) 0.0305(7) Uani 1 1 d . . . C31 C 0.4294(2) 0.1739(2) 0.1467(2) 0.0403(9) Uani 1 1 d . . . H31A H 0.3697 0.1866 0.1378 0.048 Uiso 1 1 calc R . . H31B H 0.4177 0.1262 0.1620 0.048 Uiso 1 1 calc R . . C32 C 0.4637(2) 0.1442(2) 0.0655(2) 0.0314(7) Uani 1 1 d . . . C33 C 0.6940(3) 0.1675(2) 0.3109(2) 0.0433(9) Uani 1 1 d . . . H33A H 0.6676 0.1474 0.3488 0.052 Uiso 1 1 calc R . . H33B H 0.7623 0.1755 0.3224 0.052 Uiso 1 1 calc R . . C34 C 0.6479(2) 0.0972(2) 0.2196(2) 0.0312(8) Uani 1 1 d . . . C35 C 0.8959(3) 0.3656(2) 0.2529(2) 0.0442(9) Uani 1 1 d . . . H35A H 0.9434 0.3638 0.2937 0.053 Uiso 1 1 calc R . . H35B H 0.9264 0.4113 0.2387 0.053 Uiso 1 1 calc R . . C36 C 0.8589(3) 0.2752(3) 0.1724(3) 0.0544(11) Uani 1 1 d . . . C37 C -0.0108(2) -0.1078(2) 0.2057(2) 0.0363(8) Uani 1 1 d . . . C38 C 0.0129(3) -0.0284(3) 0.2023(2) 0.0403(9) Uani 1 1 d . . . C39 C -0.0534(3) 0.0189(3) 0.2160(2) 0.0524(11) Uani 1 1 d . . . H39 H -0.0404 0.0722 0.2132 0.063 Uiso 1 1 calc R . . C40 C -0.1378(3) -0.0123(3) 0.2338(2) 0.0552(11) Uani 1 1 d . . . H40 H -0.1840 0.0169 0.2380 0.066 Uiso 1 1 calc R . . C41 C -0.1541(3) -0.0867(3) 0.2453(2) 0.0522(11) Uani 1 1 d . . . H41 H -0.2095 -0.1047 0.2613 0.063 Uiso 1 1 calc R . . C42 C -0.0895(2) -0.1359(2) 0.2334(2) 0.0399(9) Uani 1 1 d . . . C43 C -0.1031(2) -0.2120(2) 0.2545(2) 0.0437(9) Uani 1 1 d . . . H43A H -0.0762 -0.2561 0.2174 0.052 Uiso 1 1 calc R . . H43B H -0.1711 -0.2410 0.2435 0.052 Uiso 1 1 calc R . . C44 C -0.0559(2) -0.1800(2) 0.3471(2) 0.0354(8) Uani 1 1 d . . . C45 C -0.0961(3) -0.1329(2) 0.4122(2) 0.0419(9) Uani 1 1 d . . . H45 H -0.1528 -0.1222 0.3982 0.050 Uiso 1 1 calc R . . C46 C -0.0542(3) -0.1015(2) 0.4971(2) 0.0475(10) Uani 1 1 d . . . H46 H -0.0832 -0.0711 0.5395 0.057 Uiso 1 1 calc R . . C47 C 0.0312(3) -0.1152(2) 0.5193(2) 0.0434(9) Uani 1 1 d . . . H47 H 0.0597 -0.0929 0.5768 0.052 Uiso 1 1 calc R . . C48 C 0.0753(2) -0.1623(2) 0.4564(2) 0.0333(8) Uani 1 1 d . . . C49 C 0.0289(2) -0.1956(2) 0.3715(2) 0.0312(8) Uani 1 1 d . . . C50 C 0.1728(2) -0.1701(2) 0.4845(2) 0.0376(8) Uani 1 1 d . . . H50A H 0.1716 -0.1859 0.5301 0.045 Uiso 1 1 calc R . . H50B H 0.1853 -0.2178 0.4366 0.045 Uiso 1 1 calc R . . C51 C 0.2526(2) -0.0837(2) 0.51546(19) 0.0307(7) Uani 1 1 d . . . C52 C 0.2804(3) -0.0183(2) 0.6005(2) 0.0383(8) Uani 1 1 d . . . H52 H 0.2530 -0.0300 0.6402 0.046 Uiso 1 1 calc R . . C53 C 0.3468(3) 0.0630(2) 0.6278(2) 0.0422(9) Uani 1 1 d . . . H53 H 0.3676 0.1041 0.6860 0.051 Uiso 1 1 calc R . . C54 C 0.3829(2) 0.0839(2) 0.5688(2) 0.0392(8) Uani 1 1 d . . . H54 H 0.4237 0.1411 0.5869 0.047 Uiso 1 1 calc R . . C55 C 0.3589(2) 0.0202(2) 0.4827(2) 0.0347(8) Uani 1 1 d . . . C56 C 0.2985(2) -0.0642(2) 0.45875(18) 0.0287(7) Uani 1 1 d . . . C57 C 0.3876(2) 0.0464(2) 0.4161(2) 0.0386(8) Uani 1 1 d . . . H57A H 0.4489 0.0932 0.4408 0.046 Uiso 1 1 calc R . . H57B H 0.3943 -0.0050 0.3678 0.046 Uiso 1 1 calc R . . C58 C 0.2540(2) 0.0331(2) 0.3033(2) 0.0352(8) Uani 1 1 d . . . C59 C 0.3121(2) 0.0796(2) 0.3855(2) 0.0357(8) Uani 1 1 d . . . C60 C 0.2987(3) 0.1589(2) 0.4417(2) 0.0454(9) Uani 1 1 d . . . H60 H 0.3361 0.1907 0.4977 0.054 Uiso 1 1 calc R . . C61 C 0.2322(3) 0.1918(3) 0.4176(3) 0.0546(11) Uani 1 1 d . . . H61 H 0.2256 0.2460 0.4562 0.066 Uiso 1 1 calc R . . C62 C 0.1753(3) 0.1445(3) 0.3360(3) 0.0516(10) Uani 1 1 d . . . H62 H 0.1303 0.1676 0.3198 0.062 Uiso 1 1 calc R . . C63 C 0.1825(3) 0.0634(2) 0.2768(2) 0.0414(9) Uani 1 1 d . . . C64 C 0.1100(3) 0.0098(3) 0.1907(2) 0.0468(10) Uani 1 1 d . . . H64A H 0.1050 0.0481 0.1652 0.056 Uiso 1 1 calc R . . H64B H 0.1310 -0.0387 0.1523 0.056 Uiso 1 1 calc R . . C65 C 0.0101(3) -0.2262(3) 0.0887(2) 0.0464(10) Uani 1 1 d . . . H65A H 0.0140 -0.1937 0.0563 0.056 Uiso 1 1 calc R . . H65B H -0.0568 -0.2582 0.0783 0.056 Uiso 1 1 calc R . . C66 C 0.0650(3) -0.2925(2) 0.0582(2) 0.0356(8) Uani 1 1 d . . . C67 C 0.0688(3) -0.3298(2) 0.2951(2) 0.0395(8) Uani 1 1 d . . . H67A H 0.0408 -0.3398 0.3378 0.047 Uiso 1 1 calc R . . H67B H 0.1341 -0.3317 0.3040 0.047 Uiso 1 1 calc R . . C68 C 0.0121(3) -0.4043(3) 0.2061(3) 0.0471(10) Uani 1 1 d . . . C69 C 0.3615(2) -0.1703(2) 0.3681(2) 0.0400(9) Uani 1 1 d . . . H69A H 0.3707 -0.1875 0.4124 0.048 Uiso 1 1 calc R . . H69B H 0.4196 -0.1245 0.3777 0.048 Uiso 1 1 calc R . . C70 C 0.3448(2) -0.2512(2) 0.2813(2) 0.0336(8) Uani 1 1 d . . . C71 C 0.2982(3) -0.0519(3) 0.1726(2) 0.0512(10) Uani 1 1 d . . . H71A H 0.3055 0.0052 0.1736 0.061 Uiso 1 1 calc R . . H71B H 0.2499 -0.0976 0.1212 0.061 Uiso 1 1 calc R . . C72 C 0.3914(3) -0.0722(2) 0.1683(2) 0.0372(8) Uani 1 1 d . . . C73 C 0.5290(2) -0.2483(2) 0.1193(2) 0.0352(8) Uani 1 1 d . . . H73 H 0.4792 -0.2419 0.1468 0.042 Uiso 1 1 calc R . . C74 C 0.6394(3) -0.2286(3) 0.0596(3) 0.0507(10) Uani 1 1 d . . . H74 H 0.6825 -0.2029 0.0367 0.061 Uiso 1 1 calc R . . C75 C 0.5377(3) -0.3926(2) 0.1137(2) 0.0466(9) Uani 1 1 d . . . H75A H 0.5035 -0.3779 0.1588 0.056 Uiso 1 1 calc R . . H75B H 0.5957 -0.4018 0.1346 0.056 Uiso 1 1 calc R . . C76 C 0.4755(3) -0.4805(2) 0.0359(2) 0.0406(9) Uani 1 1 d . . . H76A H 0.4541 -0.5245 0.0547 0.049 Uiso 1 1 calc R . . H76B H 0.4190 -0.4706 0.0131 0.049 Uiso 1 1 calc R . . N1 N 0.5745(2) -0.19104(18) 0.09595(17) 0.0350(7) Uani 1 1 d . . . N2 N 0.5647(2) -0.31604(18) 0.09780(18) 0.0387(7) Uani 1 1 d . . . N3 N 0.6364(2) -0.3036(2) 0.0595(2) 0.0556(9) Uani 1 1 d . . . O1 O 0.65694(15) 0.39949(14) 0.17509(12) 0.0298(5) Uani 1 1 d . . . O2 O 0.49967(15) 0.25227(14) 0.21453(13) 0.0335(5) Uani 1 1 d . . . O3 O 0.67928(16) 0.25200(14) 0.32884(13) 0.0329(5) Uani 1 1 d . . . O2W O 0.1884(3) -0.0738(3) -0.0107(2) 0.0687(11) Uani 0.80 1 d P . . O2W' O 0.1593(8) -0.0081(8) -0.0159(7) 0.038(3) Uani 0.20 1 d P . . O4 O 0.81808(15) 0.38839(15) 0.29101(13) 0.0359(5) Uani 1 1 d . . . O3W' O 1.1386(10) 0.2688(11) 0.2294(11) 0.128(6) Uani 0.30 1 d P . . O3W O 1.1088(4) 0.2961(4) 0.1728(6) 0.146(3) Uani 0.70 1 d P . . O5 O 0.80299(18) 0.42410(18) 0.08955(14) 0.0470(6) Uani 1 1 d . . . O6 O 0.69183(17) 0.35809(16) -0.03405(14) 0.0411(6) Uani 1 1 d . . . O7 O 0.40517(17) 0.07585(15) -0.00076(14) 0.0412(6) Uani 1 1 d . . . O8 O 0.54291(16) 0.18525(15) 0.06462(13) 0.0365(5) Uani 1 1 d . . . O9 O 0.64703(17) 0.01895(15) 0.20621(14) 0.0392(6) Uani 1 1 d . . . O10 O 0.6151(2) 0.11563(16) 0.16618(15) 0.0507(7) Uani 1 1 d . . . O11 O 0.9227(2) 0.2423(2) 0.1436(2) 0.0908(12) Uani 1 1 d . . . O12 O 0.7719(2) 0.24006(19) 0.13956(18) 0.0667(9) Uani 1 1 d . . . O13 O 0.26520(16) -0.04848(15) 0.24633(14) 0.0371(6) Uani 1 1 d . . . O14 O 0.04752(16) -0.16322(15) 0.17918(13) 0.0361(5) Uani 1 1 d . . . O15 O 0.07014(15) -0.24349(14) 0.30647(13) 0.0337(5) Uani 1 1 d . . . O16 O 0.28317(15) -0.13334(14) 0.37500(12) 0.0312(5) Uani 1 1 d . . . O17 O 0.4293(2) -0.0940(2) 0.21660(19) 0.0699(9) Uani 1 1 d . . . O18 O 0.42330(16) -0.06603(16) 0.10635(14) 0.0413(6) Uani 1 1 d . . . O19 O 0.14175(16) -0.28075(15) 0.10381(14) 0.0387(6) Uani 1 1 d . . . O20 O 0.02473(17) -0.35685(16) -0.01658(14) 0.0443(6) Uani 1 1 d . . . O21 O -0.0334(2) -0.38903(18) 0.15479(16) 0.0547(7) Uani 1 1 d . . . O22 O 0.0152(2) -0.48101(17) 0.18980(16) 0.0553(7) Uani 1 1 d . . . O23 O 0.26529(16) -0.27786(15) 0.22879(13) 0.0368(5) Uani 1 1 d . . . O24 O 0.40992(18) -0.28501(18) 0.26998(16) 0.0556(7) Uani 1 1 d . . . O1W O 0.7052(2) 0.4544(2) -0.13898(19) 0.0624(8) Uani 1 1 d D . . H1A H 0.741(3) 0.482(3) -0.160(3) 0.094 Uiso 1 1 d D . . H1B H 0.657(3) 0.410(3) -0.183(2) 0.094 Uiso 1 1 d D . . O25 O 0.89423(18) 0.47313(16) -0.04182(15) 0.0408(6) Uani 1 1 d . . . O4W O 0.7920(7) -0.3824(7) 0.0320(6) 0.059(3) Uiso 0.30 1 d P . . O4W' O 0.7753(9) -0.4065(9) 0.0539(8) 0.042(3) Uiso 0.20 1 d P . . O5W O 0.8209(3) 0.5284(3) -0.2120(3) 0.0982(12) Uani 1 1 d . . . H25A H 0.881(5) 0.513(5) -0.021(4) 0.147 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0426(2) 0.0343(2) 0.0232(2) 0.00710(17) 0.00898(18) 0.00508(19) Zn2 0.0328(2) 0.0291(2) 0.0317(2) 0.01309(17) 0.00829(17) 0.01104(17) Zn3 0.0597(3) 0.0542(3) 0.0266(2) 0.0084(2) 0.0066(2) 0.0228(2) Na1 0.0339(7) 0.0320(7) 0.0325(7) 0.0142(6) 0.0094(6) 0.0106(6) Na2 0.0348(7) 0.0354(7) 0.0296(7) 0.0128(6) 0.0053(6) 0.0137(6) Na3 0.0583(10) 0.0610(11) 0.0413(8) 0.0172(8) 0.0099(8) 0.0186(8) C1 0.0395(19) 0.0292(18) 0.0244(16) 0.0159(15) 0.0114(15) 0.0141(16) C2 0.039(2) 0.0316(19) 0.0253(17) 0.0153(15) 0.0088(15) 0.0080(16) C3 0.054(2) 0.031(2) 0.0359(19) 0.0139(17) 0.0054(18) 0.0067(18) C4 0.061(3) 0.031(2) 0.039(2) 0.0118(17) 0.011(2) 0.020(2) C5 0.048(2) 0.047(2) 0.037(2) 0.0230(18) 0.0137(18) 0.025(2) C6 0.040(2) 0.0323(19) 0.0266(17) 0.0167(15) 0.0072(15) 0.0129(16) C7 0.0364(19) 0.038(2) 0.0350(19) 0.0177(16) 0.0069(16) 0.0111(16) C8 0.0337(19) 0.033(2) 0.0373(19) 0.0124(16) 0.0134(17) 0.0073(16) C9 0.062(3) 0.049(2) 0.062(3) 0.030(2) 0.033(2) 0.030(2) C10 0.071(3) 0.050(3) 0.060(3) 0.024(2) 0.045(2) 0.034(2) C11 0.063(3) 0.047(2) 0.043(2) 0.0193(19) 0.032(2) 0.016(2) C12 0.0350(19) 0.0308(19) 0.0365(19) 0.0128(16) 0.0139(16) 0.0049(15) C13 0.0258(17) 0.0280(18) 0.0303(17) 0.0076(15) 0.0113(15) 0.0052(14) C14 0.053(2) 0.033(2) 0.045(2) 0.0213(18) 0.023(2) 0.0086(18) C15 0.053(2) 0.0274(19) 0.037(2) 0.0184(16) 0.0152(19) 0.0129(17) C16 0.072(3) 0.045(2) 0.043(2) 0.025(2) 0.032(2) 0.026(2) C17 0.091(3) 0.045(2) 0.026(2) 0.0146(19) 0.017(2) 0.031(2) C18 0.067(3) 0.038(2) 0.0269(19) 0.0111(17) 0.0020(19) 0.022(2) C19 0.052(2) 0.028(2) 0.0311(18) 0.0097(16) 0.0045(17) 0.0175(17) C20 0.058(2) 0.0251(18) 0.0235(17) 0.0125(15) 0.0122(17) 0.0190(17) C21 0.044(2) 0.044(2) 0.0341(19) 0.0121(17) -0.0009(17) 0.0175(18) C22 0.0303(18) 0.039(2) 0.0327(19) 0.0110(16) 0.0007(16) 0.0103(16) C23 0.048(2) 0.048(2) 0.0315(19) 0.0112(18) -0.0034(17) 0.0121(19) C24 0.048(2) 0.038(2) 0.037(2) 0.0021(18) -0.0023(18) 0.0089(18) C25 0.037(2) 0.035(2) 0.042(2) 0.0102(17) 0.0035(17) 0.0064(17) C26 0.0256(17) 0.033(2) 0.0352(19) 0.0103(16) 0.0068(15) 0.0046(15) C27 0.0257(17) 0.033(2) 0.0329(19) 0.0054(16) 0.0039(15) 0.0056(15) C28 0.037(2) 0.032(2) 0.0364(19) 0.0137(16) 0.0111(17) 0.0026(16) C29 0.041(2) 0.0321(19) 0.0245(17) 0.0123(15) 0.0042(15) 0.0065(16) C30 0.041(2) 0.0256(18) 0.0272(18) 0.0119(15) 0.0103(17) 0.0140(16) C31 0.037(2) 0.032(2) 0.0351(19) 0.0064(16) 0.0119(17) 0.0000(16) C32 0.037(2) 0.0269(19) 0.0308(18) 0.0136(16) 0.0099(16) 0.0116(16) C33 0.062(2) 0.029(2) 0.0328(19) 0.0085(16) 0.0015(18) 0.0211(18) C34 0.0318(18) 0.0277(19) 0.0306(18) 0.0095(15) 0.0083(15) 0.0119(15) C35 0.033(2) 0.048(2) 0.043(2) 0.0153(19) 0.0095(18) 0.0129(18) C36 0.046(3) 0.051(3) 0.052(2) 0.010(2) 0.020(2) 0.017(2) C37 0.0320(19) 0.047(2) 0.0254(17) 0.0098(16) 0.0034(15) 0.0226(17) C38 0.042(2) 0.052(2) 0.0296(18) 0.0178(18) 0.0081(17) 0.0248(19) C39 0.065(3) 0.065(3) 0.044(2) 0.029(2) 0.016(2) 0.044(2) C40 0.051(3) 0.081(3) 0.045(2) 0.027(2) 0.015(2) 0.047(2) C41 0.036(2) 0.073(3) 0.046(2) 0.022(2) 0.0137(19) 0.028(2) C42 0.0310(19) 0.048(2) 0.0275(18) 0.0062(17) 0.0018(16) 0.0161(17) C43 0.0246(18) 0.047(2) 0.042(2) 0.0098(18) 0.0053(17) 0.0058(17) C44 0.0293(18) 0.0302(19) 0.0339(19) 0.0096(15) 0.0061(16) -0.0011(15) C45 0.034(2) 0.042(2) 0.048(2) 0.0180(18) 0.0151(18) 0.0121(17) C46 0.050(2) 0.044(2) 0.045(2) 0.0153(19) 0.025(2) 0.0154(19) C47 0.053(2) 0.039(2) 0.0300(19) 0.0126(17) 0.0107(18) 0.0051(18) C48 0.0365(19) 0.0253(18) 0.0300(18) 0.0106(15) 0.0071(16) 0.0012(15) C49 0.0302(18) 0.0243(18) 0.0298(18) 0.0082(14) 0.0110(15) 0.0002(14) C50 0.046(2) 0.034(2) 0.0315(18) 0.0166(16) 0.0071(17) 0.0095(17) C51 0.0327(18) 0.0312(19) 0.0263(17) 0.0121(15) 0.0030(15) 0.0124(15) C52 0.044(2) 0.043(2) 0.0270(18) 0.0143(17) 0.0089(16) 0.0149(18) C53 0.038(2) 0.044(2) 0.0261(18) 0.0023(16) 0.0023(16) 0.0116(18) C54 0.0298(19) 0.031(2) 0.038(2) 0.0040(16) 0.0026(16) 0.0045(15) C55 0.0259(17) 0.034(2) 0.0360(19) 0.0103(16) 0.0061(15) 0.0096(16) C56 0.0246(16) 0.0304(19) 0.0211(16) 0.0045(14) -0.0005(14) 0.0102(15) C57 0.0293(18) 0.038(2) 0.040(2) 0.0134(17) 0.0128(17) 0.0043(16) C58 0.0376(19) 0.0305(19) 0.044(2) 0.0201(17) 0.0226(18) 0.0117(16) C59 0.0314(19) 0.034(2) 0.040(2) 0.0174(17) 0.0148(17) 0.0042(16) C60 0.044(2) 0.035(2) 0.049(2) 0.0137(18) 0.0180(19) 0.0076(18) C61 0.062(3) 0.036(2) 0.063(3) 0.017(2) 0.026(2) 0.020(2) C62 0.059(3) 0.045(2) 0.062(3) 0.027(2) 0.024(2) 0.029(2) C63 0.045(2) 0.044(2) 0.047(2) 0.0272(19) 0.0183(19) 0.0174(18) C64 0.055(2) 0.055(3) 0.047(2) 0.032(2) 0.021(2) 0.029(2) C65 0.041(2) 0.056(3) 0.0288(19) 0.0058(18) 0.0004(17) 0.0241(19) C66 0.035(2) 0.039(2) 0.0292(19) 0.0129(17) 0.0109(17) 0.0100(17) C67 0.0347(19) 0.030(2) 0.041(2) 0.0082(16) 0.0094(17) 0.0047(16) C68 0.047(2) 0.036(2) 0.040(2) 0.0053(19) 0.028(2) 0.0003(18) C69 0.0339(19) 0.039(2) 0.0363(19) 0.0070(16) 0.0024(16) 0.0178(17) C70 0.035(2) 0.0316(19) 0.0308(18) 0.0111(15) 0.0082(17) 0.0126(16) C71 0.053(2) 0.080(3) 0.048(2) 0.042(2) 0.031(2) 0.037(2) C72 0.041(2) 0.038(2) 0.0328(19) 0.0141(17) 0.0142(18) 0.0161(17) C73 0.0365(19) 0.031(2) 0.0360(19) 0.0139(16) 0.0063(16) 0.0116(16) C74 0.051(2) 0.046(2) 0.070(3) 0.032(2) 0.030(2) 0.023(2) C75 0.067(3) 0.037(2) 0.041(2) 0.0210(18) 0.013(2) 0.021(2) C76 0.050(2) 0.036(2) 0.045(2) 0.0241(18) 0.0134(18) 0.0164(18) N1 0.0363(16) 0.0277(16) 0.0348(15) 0.0110(13) 0.0031(13) 0.0096(13) N2 0.0489(18) 0.0308(17) 0.0360(16) 0.0147(13) 0.0090(15) 0.0149(14) N3 0.057(2) 0.045(2) 0.080(2) 0.0333(19) 0.032(2) 0.0274(18) O1 0.0385(13) 0.0273(12) 0.0235(11) 0.0118(10) 0.0074(10) 0.0105(10) O2 0.0325(12) 0.0300(13) 0.0263(11) 0.0040(10) 0.0109(10) 0.0070(10) O3 0.0470(14) 0.0265(12) 0.0248(11) 0.0102(10) 0.0100(11) 0.0147(11) O2W 0.055(2) 0.079(3) 0.048(2) 0.0053(19) 0.0076(18) 0.034(2) O2W' 0.043(7) 0.051(8) 0.033(6) 0.024(6) 0.003(6) 0.033(6) O4 0.0307(12) 0.0337(13) 0.0311(12) 0.0069(11) 0.0053(10) 0.0072(11) O3W' 0.095(10) 0.149(13) 0.206(16) 0.155(14) -0.009(10) 0.031(9) O3W 0.050(3) 0.101(5) 0.296(10) 0.105(6) 0.049(5) 0.017(3) O5 0.0379(15) 0.0623(18) 0.0288(13) 0.0136(12) 0.0073(12) 0.0115(13) O6 0.0413(14) 0.0503(16) 0.0241(13) 0.0135(11) 0.0082(11) 0.0094(12) O7 0.0430(14) 0.0344(14) 0.0280(12) 0.0048(11) 0.0078(11) 0.0008(12) O8 0.0392(14) 0.0373(14) 0.0298(12) 0.0134(11) 0.0131(11) 0.0092(12) O9 0.0472(15) 0.0269(13) 0.0369(13) 0.0096(11) -0.0002(11) 0.0164(11) O10 0.088(2) 0.0361(15) 0.0272(13) 0.0128(12) 0.0029(13) 0.0292(15) O11 0.0471(18) 0.079(2) 0.093(2) -0.0076(19) 0.0246(19) 0.0228(17) O12 0.0379(17) 0.0587(19) 0.0587(18) -0.0077(15) 0.0097(14) 0.0112(14) O13 0.0420(14) 0.0411(14) 0.0364(13) 0.0207(11) 0.0206(12) 0.0176(12) O14 0.0334(13) 0.0427(14) 0.0291(12) 0.0104(11) 0.0066(11) 0.0208(11) O15 0.0344(13) 0.0279(13) 0.0300(12) 0.0072(10) 0.0097(11) 0.0067(10) O16 0.0292(12) 0.0341(13) 0.0226(11) 0.0061(10) 0.0045(10) 0.0129(10) O17 0.075(2) 0.113(3) 0.0658(19) 0.058(2) 0.0395(18) 0.065(2) O18 0.0375(13) 0.0520(16) 0.0368(13) 0.0197(12) 0.0178(12) 0.0173(12) O19 0.0332(14) 0.0383(14) 0.0330(13) 0.0060(11) 0.0038(11) 0.0159(11) O20 0.0413(14) 0.0464(16) 0.0283(13) 0.0048(12) 0.0041(11) 0.0131(12) O21 0.0647(19) 0.0471(17) 0.0286(14) 0.0058(13) 0.0094(14) 0.0020(14) O22 0.0622(18) 0.0307(16) 0.0521(16) 0.0034(13) 0.0258(15) 0.0057(13) O23 0.0369(14) 0.0383(14) 0.0268(12) 0.0071(11) 0.0031(11) 0.0168(11) O24 0.0413(15) 0.0507(17) 0.0553(16) 0.0048(13) 0.0048(13) 0.0258(14) O1W 0.068(2) 0.064(2) 0.063(2) 0.0318(16) 0.0142(16) 0.0318(18) O25 0.0418(14) 0.0374(15) 0.0325(13) 0.0097(12) 0.0054(11) 0.0094(12) O5W 0.081(3) 0.108(3) 0.116(3) 0.072(3) 0.011(2) 0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O25 1.947(3) . ? Zn1 O6 1.973(2) . ? Zn1 O23 1.986(2) 2_655 ? Zn1 O1W 2.161(3) . ? Zn1 O19 2.240(2) 2_655 ? Zn1 Zn3 3.1052(10) . ? Zn1 Na2 3.4912(14) 2_655 ? Zn2 O18 1.950(2) . ? Zn2 O9 1.966(2) . ? Zn2 O7 2.016(2) 2_655 ? Zn2 N1 2.035(3) . ? Zn2 Na3 3.6308(19) . ? Zn3 O25 1.959(3) . ? Zn3 O20 1.972(2) 2_655 ? Zn3 O5 2.107(2) . ? Zn3 O22 2.123(3) 1_665 ? Zn3 O21 2.237(3) 1_665 ? Zn3 C68 2.475(4) 1_665 ? Na1 O12 2.229(3) . ? Na1 O2 2.318(2) . ? Na1 O1 2.415(2) . ? Na1 O3 2.424(2) . ? Na1 O4 2.474(3) . ? Na1 O8 2.482(3) . ? Na1 O10 2.506(3) . ? Na1 C36 3.100(4) . ? Na1 Na3 3.3626(19) 2_655 ? Na2 O19 2.299(3) . ? Na2 O14 2.300(3) . ? Na2 O16 2.303(2) . ? Na2 O23 2.311(2) . ? Na2 O13 2.343(3) . ? Na2 O15 2.369(2) . ? Na2 C66 3.084(4) . ? Na2 C70 3.121(4) . ? Na2 Zn1 3.4912(13) 2_655 ? Na3 O2W 2.377(4) . ? Na3 O10 2.430(3) 2_655 ? Na3 O12 2.435(3) 2_655 ? Na3 O18 2.459(3) . ? Na3 O8 2.573(3) 2_655 ? Na3 O7 2.665(3) . ? Na3 Na1 3.3626(19) 2_655 ? C1 C2 1.386(5) . ? C1 O1 1.401(3) . ? C1 C6 1.403(4) . ? C2 C3 1.392(5) . ? C2 C28 1.514(5) . ? C3 C4 1.386(5) . ? C3 H3 0.9300 . ? C4 C5 1.360(5) . ? C4 H4 0.9300 . ? C5 C6 1.401(5) . ? C5 H5 0.9300 . ? C6 C7 1.523(5) . ? C7 C8 1.528(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.379(5) . ? C8 C9 1.391(4) . ? C9 C10 1.379(5) . ? C9 H9 0.9300 . ? C10 C11 1.364(5) . ? C10 H10 0.9300 . ? C11 C12 1.395(4) . ? C11 H11 0.9300 . ? C12 C13 1.398(5) . ? C12 C14 1.512(5) . ? C13 O2 1.401(3) . ? C14 C15 1.503(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.388(5) . ? C15 C16 1.410(5) . ? C16 C17 1.372(6) . ? C16 H16 0.9300 . ? C17 C18 1.376(6) . ? C17 H17 0.9300 . ? C18 C19 1.399(5) . ? C18 H18 0.9300 . ? C19 C20 1.394(5) . ? C19 C21 1.511(5) . ? C20 O3 1.396(3) . ? C21 C22 1.517(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.391(5) . ? C22 C23 1.396(5) . ? C23 C24 1.379(5) . ? C23 H23 0.9300 . ? C24 C25 1.358(5) . ? C24 H24 0.9300 . ? C25 C26 1.395(5) . ? C25 H25 0.9300 . ? C26 C27 1.400(5) . ? C26 C28 1.512(5) . ? C27 O4 1.410(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O1 1.438(4) . ? C29 C30 1.513(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O5 1.232(4) . ? C30 O6 1.274(4) . ? C31 O2 1.428(4) . ? C31 C32 1.503(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O8 1.232(4) . ? C32 O7 1.279(4) . ? C33 O3 1.439(4) . ? C33 C34 1.500(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O10 1.218(4) . ? C34 O9 1.275(4) . ? C35 O4 1.446(4) . ? C35 C36 1.517(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O12 1.237(5) . ? C36 O11 1.257(4) . ? C37 C38 1.380(5) . ? C37 C42 1.387(5) . ? C37 O14 1.403(4) . ? C38 C39 1.394(5) . ? C38 C64 1.517(5) . ? C39 C40 1.373(6) . ? C39 H39 0.9300 . ? C40 C41 1.373(6) . ? C40 H40 0.9300 . ? C41 C42 1.397(5) . ? C41 H41 0.9300 . ? C42 C43 1.511(5) . ? C43 C44 1.513(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.387(4) . ? C44 C49 1.403(5) . ? C45 C46 1.376(5) . ? C45 H45 0.9300 . ? C46 C47 1.383(5) . ? C46 H46 0.9300 . ? C47 C48 1.402(4) . ? C47 H47 0.9300 . ? C48 C49 1.388(5) . ? C48 C50 1.526(5) . ? C49 O15 1.401(3) . ? C50 C51 1.511(5) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.382(4) . ? C51 C56 1.399(4) . ? C52 C53 1.366(5) . ? C52 H52 0.9300 . ? C53 C54 1.381(5) . ? C53 H53 0.9300 . ? C54 C55 1.390(5) . ? C54 H54 0.9300 . ? C55 C56 1.384(5) . ? C55 C57 1.521(5) . ? C56 O16 1.403(3) . ? C57 C59 1.519(5) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.383(5) . ? C58 O13 1.401(4) . ? C58 C63 1.407(5) . ? C59 C60 1.384(5) . ? C60 C61 1.363(6) . ? C60 H60 0.9300 . ? C61 C62 1.367(6) . ? C61 H61 0.9300 . ? C62 C63 1.385(5) . ? C62 H62 0.9300 . ? C63 C64 1.519(5) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 O14 1.448(4) . ? C65 C66 1.505(5) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 O19 1.237(4) . ? C66 O20 1.267(4) . ? C67 O15 1.423(4) . ? C67 C68 1.522(5) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 O21 1.233(5) . ? C68 O22 1.251(5) . ? C68 Zn3 2.475(4) 1_445 ? C69 O16 1.438(4) . ? C69 C70 1.516(4) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 O24 1.229(4) . ? C70 O23 1.264(4) . ? C71 O13 1.438(4) . ? C71 C72 1.499(5) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 O17 1.217(4) . ? C72 O18 1.288(4) . ? C73 N1 1.323(4) . ? C73 N2 1.324(4) . ? C73 H73 0.9300 . ? C74 N3 1.298(5) . ? C74 N1 1.350(4) . ? C74 H74 0.9300 . ? C75 N2 1.464(4) . ? C75 C76 1.529(5) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 C76 1.518(6) 2_645 ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? N2 N3 1.352(4) . ? O2W O2W' 1.348(11) . ? O3W' O3W 1.362(13) . ? O7 Zn2 2.016(2) 2_655 ? O8 Na3 2.573(3) 2_655 ? O10 Na3 2.430(3) 2_655 ? O12 Na3 2.435(3) 2_655 ? O19 Zn1 2.240(2) 2_655 ? O20 Zn3 1.972(2) 2_655 ? O21 Zn3 2.237(3) 1_445 ? O22 Zn3 2.123(3) 1_445 ? O23 Zn1 1.986(2) 2_655 ? O1W H1A 0.866(19) . ? O1W H1B 0.90(2) . ? O25 H25A 0.71(6) . ? O4W O4W' 0.715(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O25 Zn1 O6 112.41(10) . . ? O25 Zn1 O23 132.32(9) . 2_655 ? O6 Zn1 O23 114.80(10) . 2_655 ? O25 Zn1 O1W 93.06(12) . . ? O6 Zn1 O1W 93.46(11) . . ? O23 Zn1 O1W 90.47(11) 2_655 . ? O25 Zn1 O19 88.45(10) . 2_655 ? O6 Zn1 O19 98.01(9) . 2_655 ? O23 Zn1 O19 78.97(9) 2_655 2_655 ? O1W Zn1 O19 166.89(10) . 2_655 ? O25 Zn1 Zn3 37.48(8) . . ? O6 Zn1 Zn3 83.18(7) . . ? O23 Zn1 Zn3 145.46(7) 2_655 . ? O1W Zn1 Zn3 118.91(9) . . ? O19 Zn1 Zn3 69.08(6) 2_655 . ? O25 Zn1 Na2 112.25(7) . 2_655 ? O6 Zn1 Na2 114.95(8) . 2_655 ? O23 Zn1 Na2 38.91(7) 2_655 2_655 ? O1W Zn1 Na2 128.08(9) . 2_655 ? O19 Zn1 Na2 40.34(6) 2_655 2_655 ? Zn3 Zn1 Na2 107.43(3) . 2_655 ? O18 Zn2 O9 111.16(9) . . ? O18 Zn2 O7 113.63(10) . 2_655 ? O9 Zn2 O7 107.34(10) . 2_655 ? O18 Zn2 N1 118.42(11) . . ? O9 Zn2 N1 103.50(10) . . ? O7 Zn2 N1 101.67(10) 2_655 . ? O18 Zn2 Na3 39.43(7) . . ? O9 Zn2 Na3 135.27(7) . . ? O7 Zn2 Na3 75.47(8) 2_655 . ? N1 Zn2 Na3 119.94(8) . . ? O25 Zn3 O20 101.81(10) . 2_655 ? O25 Zn3 O5 102.26(10) . . ? O20 Zn3 O5 103.90(10) 2_655 . ? O25 Zn3 O22 153.10(11) . 1_665 ? O20 Zn3 O22 94.83(10) 2_655 1_665 ? O5 Zn3 O22 93.94(10) . 1_665 ? O25 Zn3 O21 96.74(11) . 1_665 ? O20 Zn3 O21 149.70(11) 2_655 1_665 ? O5 Zn3 O21 95.20(10) . 1_665 ? O22 Zn3 O21 60.12(11) 1_665 1_665 ? O25 Zn3 C68 125.03(13) . 1_665 ? O20 Zn3 C68 123.03(13) 2_655 1_665 ? O5 Zn3 C68 96.45(10) . 1_665 ? O22 Zn3 C68 30.37(13) 1_665 1_665 ? O21 Zn3 C68 29.79(12) 1_665 1_665 ? O25 Zn3 Zn1 37.20(8) . . ? O20 Zn3 Zn1 87.77(7) 2_655 . ? O5 Zn3 Zn1 72.45(7) . . ? O22 Zn3 Zn1 166.36(7) 1_665 . ? O21 Zn3 Zn1 120.72(9) 1_665 . ? C68 Zn3 Zn1 149.17(11) 1_665 . ? O12 Na1 O2 151.02(11) . . ? O12 Na1 O1 95.61(11) . . ? O2 Na1 O1 92.78(8) . . ? O12 Na1 O3 106.68(11) . . ? O2 Na1 O3 83.64(8) . . ? O1 Na1 O3 139.89(8) . . ? O12 Na1 O4 69.03(9) . . ? O2 Na1 O4 139.95(8) . . ? O1 Na1 O4 77.85(8) . . ? O3 Na1 O4 79.64(8) . . ? O12 Na1 O8 86.94(10) . . ? O2 Na1 O8 66.51(8) . . ? O1 Na1 O8 83.50(8) . . ? O3 Na1 O8 129.61(9) . . ? O4 Na1 O8 147.61(8) . . ? O12 Na1 O10 79.36(11) . . ? O2 Na1 O10 80.34(9) . . ? O1 Na1 O10 152.21(9) . . ? O3 Na1 O10 66.52(8) . . ? O4 Na1 O10 123.99(10) . . ? O8 Na1 O10 69.03(8) . . ? O12 Na1 C36 19.21(10) . . ? O2 Na1 C36 169.14(10) . . ? O1 Na1 C36 93.91(10) . . ? O3 Na1 C36 96.65(10) . . ? O4 Na1 C36 50.24(9) . . ? O8 Na1 C36 105.79(10) . . ? O10 Na1 C36 89.79(10) . . ? O12 Na1 Na3 46.34(8) . 2_655 ? O2 Na1 Na3 104.93(7) . 2_655 ? O1 Na1 Na3 111.89(7) . 2_655 ? O3 Na1 Na3 107.59(7) . 2_655 ? O4 Na1 Na3 114.75(7) . 2_655 ? O8 Na1 Na3 49.46(6) . 2_655 ? O10 Na1 Na3 46.11(6) . 2_655 ? C36 Na1 Na3 64.57(8) . 2_655 ? O19 Na2 O14 71.70(8) . . ? O19 Na2 O16 141.30(9) . . ? O14 Na2 O16 146.90(9) . . ? O19 Na2 O23 71.54(9) . . ? O14 Na2 O23 141.47(10) . . ? O16 Na2 O23 70.16(8) . . ? O19 Na2 O13 100.81(9) . . ? O14 Na2 O13 85.28(9) . . ? O16 Na2 O13 88.86(9) . . ? O23 Na2 O13 112.67(9) . . ? O19 Na2 O15 105.47(9) . . ? O14 Na2 O15 85.71(9) . . ? O16 Na2 O15 82.14(9) . . ? O23 Na2 O15 93.19(9) . . ? O13 Na2 O15 147.86(9) . . ? O19 Na2 C66 20.69(8) . . ? O14 Na2 C66 51.43(8) . . ? O16 Na2 C66 160.87(9) . . ? O23 Na2 C66 90.80(9) . . ? O13 Na2 C66 100.73(9) . . ? O15 Na2 C66 97.50(9) . . ? O19 Na2 C70 90.09(9) . . ? O14 Na2 C70 161.67(9) . . ? O16 Na2 C70 51.22(8) . . ? O23 Na2 C70 20.83(8) . . ? O13 Na2 C70 100.63(9) . . ? O15 Na2 C70 97.54(9) . . ? C66 Na2 C70 110.26(9) . . ? O19 Na2 Zn1 39.12(6) . 2_655 ? O14 Na2 Zn1 109.26(7) . 2_655 ? O16 Na2 Zn1 102.83(6) . 2_655 ? O23 Na2 Zn1 32.67(6) . 2_655 ? O13 Na2 Zn1 114.36(6) . 2_655 ? O15 Na2 Zn1 97.74(7) . 2_655 ? C66 Na2 Zn1 58.15(7) . 2_655 ? C70 Na2 Zn1 52.47(6) . 2_655 ? O2W Na3 O10 122.21(13) . 2_655 ? O2W Na3 O12 78.59(12) . 2_655 ? O10 Na3 O12 77.08(10) 2_655 2_655 ? O2W Na3 O18 103.00(11) . . ? O10 Na3 O18 134.25(11) 2_655 . ? O12 Na3 O18 122.14(12) 2_655 . ? O2W Na3 O8 153.13(14) . 2_655 ? O10 Na3 O8 68.74(8) 2_655 2_655 ? O12 Na3 O8 80.78(10) 2_655 2_655 ? O18 Na3 O8 73.98(8) . 2_655 ? O2W Na3 O7 90.16(12) . . ? O10 Na3 O7 79.72(9) 2_655 . ? O12 Na3 O7 143.04(12) 2_655 . ? O18 Na3 O7 94.61(9) . . ? O8 Na3 O7 116.59(9) 2_655 . ? O2W Na3 Na1 118.85(11) . 2_655 ? O10 Na3 Na1 48.02(7) 2_655 2_655 ? O12 Na3 Na1 41.48(7) 2_655 2_655 ? O18 Na3 Na1 116.88(8) . 2_655 ? O8 Na3 Na1 47.16(6) 2_655 2_655 ? O7 Na3 Na1 127.52(7) . 2_655 ? O2W Na3 Zn2 133.24(10) . . ? O10 Na3 Zn2 104.22(9) 2_655 . ? O12 Na3 Zn2 120.28(10) 2_655 . ? O18 Na3 Zn2 30.24(5) . . ? O8 Na3 Zn2 48.31(6) 2_655 . ? O7 Na3 Zn2 93.07(7) . . ? Na1 Na3 Zn2 95.28(5) 2_655 . ? C2 C1 O1 118.5(3) . . ? C2 C1 C6 122.2(3) . . ? O1 C1 C6 119.2(3) . . ? C1 C2 C3 118.0(3) . . ? C1 C2 C28 121.9(3) . . ? C3 C2 C28 119.9(3) . . ? C4 C3 C2 120.8(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 122.1(3) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 116.6(3) . . ? C5 C6 C7 119.1(3) . . ? C1 C6 C7 124.1(3) . . ? C6 C7 C8 109.1(3) . . ? C6 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? C6 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C13 C8 C9 117.3(3) . . ? C13 C8 C7 122.4(3) . . ? C9 C8 C7 120.2(3) . . ? C10 C9 C8 120.7(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 121.3(3) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 116.4(3) . . ? C11 C12 C14 120.8(3) . . ? C13 C12 C14 122.8(3) . . ? C8 C13 C12 123.3(3) . . ? C8 C13 O2 118.5(3) . . ? C12 C13 O2 118.1(3) . . ? C15 C14 C12 111.0(3) . . ? C15 C14 H14A 109.4 . . ? C12 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C12 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C20 C15 C16 116.7(4) . . ? C20 C15 C14 122.0(3) . . ? C16 C15 C14 121.3(3) . . ? C17 C16 C15 121.1(3) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 117.0(3) . . ? C20 C19 C21 121.3(3) . . ? C18 C19 C21 121.6(3) . . ? C15 C20 C19 123.3(3) . . ? C15 C20 O3 117.9(3) . . ? C19 C20 O3 118.7(3) . . ? C19 C21 C22 111.2(3) . . ? C19 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C19 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C27 C22 C23 117.1(3) . . ? C27 C22 C21 123.2(3) . . ? C23 C22 C21 119.6(3) . . ? C24 C23 C22 121.4(3) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 121.8(4) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C27 117.1(3) . . ? C25 C26 C28 119.7(3) . . ? C27 C26 C28 123.1(3) . . ? C22 C27 C26 122.5(3) . . ? C22 C27 O4 118.7(3) . . ? C26 C27 O4 118.7(3) . . ? C26 C28 C2 110.5(2) . . ? C26 C28 H28A 109.6 . . ? C2 C28 H28A 109.6 . . ? C26 C28 H28B 109.6 . . ? C2 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? O1 C29 C30 117.4(3) . . ? O1 C29 H29A 107.9 . . ? C30 C29 H29A 107.9 . . ? O1 C29 H29B 107.9 . . ? C30 C29 H29B 107.9 . . ? H29A C29 H29B 107.2 . . ? O5 C30 O6 126.3(3) . . ? O5 C30 C29 122.3(3) . . ? O6 C30 C29 111.3(3) . . ? O2 C31 C32 110.0(3) . . ? O2 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O2 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? O8 C32 O7 123.5(3) . . ? O8 C32 C31 120.7(3) . . ? O7 C32 C31 115.7(3) . . ? O3 C33 C34 111.9(3) . . ? O3 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? O3 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? O10 C34 O9 125.6(3) . . ? O10 C34 C33 121.9(3) . . ? O9 C34 C33 112.6(3) . . ? O4 C35 C36 110.4(3) . . ? O4 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? O4 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? O12 C36 O11 124.9(4) . . ? O12 C36 C35 120.2(3) . . ? O11 C36 C35 114.9(4) . . ? O12 C36 Na1 36.38(17) . . ? O11 C36 Na1 157.9(3) . . ? C35 C36 Na1 85.20(19) . . ? C38 C37 C42 123.4(3) . . ? C38 C37 O14 118.2(3) . . ? C42 C37 O14 118.4(3) . . ? C37 C38 C39 117.3(3) . . ? C37 C38 C64 121.6(3) . . ? C39 C38 C64 120.9(4) . . ? C40 C39 C38 120.6(4) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C41 C40 C39 120.0(3) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 121.5(4) . . ? C40 C41 H41 119.2 . . ? C42 C41 H41 119.2 . . ? C37 C42 C41 116.2(4) . . ? C37 C42 C43 122.7(3) . . ? C41 C42 C43 121.1(3) . . ? C42 C43 C44 112.0(3) . . ? C42 C43 H43A 109.2 . . ? C44 C43 H43A 109.2 . . ? C42 C43 H43B 109.2 . . ? C44 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C45 C44 C49 117.0(3) . . ? C45 C44 C43 120.3(3) . . ? C49 C44 C43 122.8(3) . . ? C46 C45 C44 121.8(3) . . ? C46 C45 H45 119.1 . . ? C44 C45 H45 119.1 . . ? C45 C46 C47 119.8(3) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C46 C47 C48 121.0(3) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C49 C48 C47 117.2(3) . . ? C49 C48 C50 123.8(3) . . ? C47 C48 C50 118.9(3) . . ? C48 C49 O15 119.2(3) . . ? C48 C49 C44 123.0(3) . . ? O15 C49 C44 117.7(3) . . ? C51 C50 C48 111.9(3) . . ? C51 C50 H50A 109.2 . . ? C48 C50 H50A 109.2 . . ? C51 C50 H50B 109.2 . . ? C48 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? C52 C51 C56 116.8(3) . . ? C52 C51 C50 121.5(3) . . ? C56 C51 C50 121.6(3) . . ? C53 C52 C51 121.9(3) . . ? C53 C52 H52 119.0 . . ? C51 C52 H52 119.0 . . ? C52 C53 C54 119.8(3) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C53 C54 C55 120.7(3) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C56 C55 C54 117.7(3) . . ? C56 C55 C57 121.2(3) . . ? C54 C55 C57 120.6(3) . . ? C55 C56 C51 122.4(3) . . ? C55 C56 O16 119.2(3) . . ? C51 C56 O16 118.4(3) . . ? C59 C57 C55 109.9(2) . . ? C59 C57 H57A 109.7 . . ? C55 C57 H57A 109.7 . . ? C59 C57 H57B 109.7 . . ? C55 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? C59 C58 O13 118.2(3) . . ? C59 C58 C63 122.1(3) . . ? O13 C58 C63 119.7(3) . . ? C58 C59 C60 117.6(3) . . ? C58 C59 C57 122.8(3) . . ? C60 C59 C57 119.6(3) . . ? C61 C60 C59 122.0(4) . . ? C61 C60 H60 119.0 . . ? C59 C60 H60 119.0 . . ? C60 C61 C62 119.4(4) . . ? C60 C61 H61 120.3 . . ? C62 C61 H61 120.3 . . ? C61 C62 C63 122.0(4) . . ? C61 C62 H62 119.0 . . ? C63 C62 H62 119.0 . . ? C62 C63 C58 116.9(4) . . ? C62 C63 C64 119.1(3) . . ? C58 C63 C64 123.9(3) . . ? C38 C64 C63 109.9(3) . . ? C38 C64 H64A 109.7 . . ? C63 C64 H64A 109.7 . . ? C38 C64 H64B 109.7 . . ? C63 C64 H64B 109.7 . . ? H64A C64 H64B 108.2 . . ? O14 C65 C66 111.4(3) . . ? O14 C65 H65A 109.3 . . ? C66 C65 H65A 109.3 . . ? O14 C65 H65B 109.3 . . ? C66 C65 H65B 109.3 . . ? H65A C65 H65B 108.0 . . ? O19 C66 O20 126.5(3) . . ? O19 C66 C65 120.8(3) . . ? O20 C66 C65 112.7(3) . . ? O19 C66 Na2 41.03(15) . . ? O20 C66 Na2 163.6(3) . . ? C65 C66 Na2 80.99(19) . . ? O15 C67 C68 112.2(3) . . ? O15 C67 H67A 109.2 . . ? C68 C67 H67A 109.2 . . ? O15 C67 H67B 109.2 . . ? C68 C67 H67B 109.2 . . ? H67A C67 H67B 107.9 . . ? O21 C68 O22 123.3(4) . . ? O21 C68 C67 121.6(4) . . ? O22 C68 C67 115.1(4) . . ? O21 C68 Zn3 64.3(2) . 1_445 ? O22 C68 Zn3 59.1(2) . 1_445 ? C67 C68 Zn3 173.0(3) . 1_445 ? O16 C69 C70 112.5(3) . . ? O16 C69 H69A 109.1 . . ? C70 C69 H69A 109.1 . . ? O16 C69 H69B 109.1 . . ? C70 C69 H69B 109.1 . . ? H69A C69 H69B 107.8 . . ? O24 C70 O23 126.7(3) . . ? O24 C70 C69 116.2(3) . . ? O23 C70 C69 117.1(3) . . ? O24 C70 Na2 160.7(2) . . ? O23 C70 Na2 40.55(15) . . ? C69 C70 Na2 78.87(18) . . ? O13 C71 C72 113.5(3) . . ? O13 C71 H71A 108.9 . . ? C72 C71 H71A 108.9 . . ? O13 C71 H71B 108.9 . . ? C72 C71 H71B 108.9 . . ? H71A C71 H71B 107.7 . . ? O17 C72 O18 125.4(3) . . ? O17 C72 C71 122.9(3) . . ? O18 C72 C71 111.6(3) . . ? N1 C73 N2 109.9(3) . . ? N1 C73 H73 125.1 . . ? N2 C73 H73 125.1 . . ? N3 C74 N1 114.2(3) . . ? N3 C74 H74 122.9 . . ? N1 C74 H74 122.9 . . ? N2 C75 C76 115.0(3) . . ? N2 C75 H75A 108.5 . . ? C76 C75 H75A 108.5 . . ? N2 C75 H75B 108.5 . . ? C76 C75 H75B 108.5 . . ? H75A C75 H75B 107.5 . . ? C76 C76 C75 114.9(4) 2_645 . ? C76 C76 H76A 108.5 2_645 . ? C75 C76 H76A 108.5 . . ? C76 C76 H76B 108.5 2_645 . ? C75 C76 H76B 108.5 . . ? H76A C76 H76B 107.5 . . ? C73 N1 C74 103.1(3) . . ? C73 N1 Zn2 130.5(2) . . ? C74 N1 Zn2 126.3(2) . . ? C73 N2 N3 109.4(3) . . ? C73 N2 C75 128.2(3) . . ? N3 N2 C75 122.4(3) . . ? C74 N3 N2 103.5(3) . . ? C1 O1 C29 114.6(2) . . ? C1 O1 Na1 127.22(16) . . ? C29 O1 Na1 114.02(18) . . ? C13 O2 C31 114.3(2) . . ? C13 O2 Na1 126.73(18) . . ? C31 O2 Na1 118.76(16) . . ? C20 O3 C33 109.9(2) . . ? C20 O3 Na1 135.01(18) . . ? C33 O3 Na1 115.06(17) . . ? O2W' O2W Na3 122.6(6) . . ? C27 O4 C35 113.4(2) . . ? C27 O4 Na1 132.63(18) . . ? C35 O4 Na1 114.02(19) . . ? C30 O5 Zn3 133.5(2) . . ? C30 O6 Zn1 124.3(2) . . ? C32 O7 Zn2 106.19(19) . 2_655 ? C32 O7 Na3 130.3(2) . . ? Zn2 O7 Na3 108.78(9) 2_655 . ? C32 O8 Na1 115.0(2) . . ? C32 O8 Na3 114.1(2) . 2_655 ? Na1 O8 Na3 83.38(8) . 2_655 ? C34 O9 Zn2 113.5(2) . . ? C34 O10 Na3 128.3(2) . 2_655 ? C34 O10 Na1 116.7(2) . . ? Na3 O10 Na1 85.87(9) 2_655 . ? C36 O12 Na1 124.4(2) . . ? C36 O12 Na3 138.5(3) . 2_655 ? Na1 O12 Na3 92.17(11) . 2_655 ? C58 O13 C71 116.6(3) . . ? C58 O13 Na2 117.67(17) . . ? C71 O13 Na2 121.7(2) . . ? C37 O14 C65 109.0(2) . . ? C37 O14 Na2 134.79(19) . . ? C65 O14 Na2 116.12(18) . . ? C49 O15 C67 115.5(2) . . ? C49 O15 Na2 124.71(18) . . ? C67 O15 Na2 117.05(17) . . ? C56 O16 C69 110.0(2) . . ? C56 O16 Na2 133.42(17) . . ? C69 O16 Na2 115.38(17) . . ? C72 O18 Zn2 114.9(2) . . ? C72 O18 Na3 131.0(2) . . ? Zn2 O18 Na3 110.33(9) . . ? C66 O19 Zn1 133.1(2) . 2_655 ? C66 O19 Na2 118.28(19) . . ? Zn1 O19 Na2 100.54(10) 2_655 . ? C66 O20 Zn3 120.9(2) . 2_655 ? C68 O21 Zn3 85.9(2) . 1_445 ? C68 O22 Zn3 90.5(3) . 1_445 ? C70 O23 Zn1 128.28(19) . 2_655 ? C70 O23 Na2 118.6(2) . . ? Zn1 O23 Na2 108.42(11) 2_655 . ? Zn1 O1W H1A 110(4) . . ? Zn1 O1W H1B 99(4) . . ? H1A O1W H1B 106(5) . . ? Zn1 O25 Zn3 105.32(12) . . ? Zn1 O25 H25A 108(6) . . ? Zn3 O25 H25A 96(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Zn1 Zn3 O25 -141.89(13) . . . . ? O23 Zn1 Zn3 O25 93.26(16) 2_655 . . . ? O1W Zn1 Zn3 O25 -51.70(14) . . . . ? O19 Zn1 Zn3 O25 116.81(12) 2_655 . . . ? Na2 Zn1 Zn3 O25 104.05(11) 2_655 . . . ? O25 Zn1 Zn3 O20 -112.95(13) . . . 2_655 ? O6 Zn1 Zn3 O20 105.16(10) . . . 2_655 ? O23 Zn1 Zn3 O20 -19.69(15) 2_655 . . 2_655 ? O1W Zn1 Zn3 O20 -164.65(12) . . . 2_655 ? O19 Zn1 Zn3 O20 3.86(9) 2_655 . . 2_655 ? Na2 Zn1 Zn3 O20 -8.90(7) 2_655 . . 2_655 ? O25 Zn1 Zn3 O5 141.72(13) . . . . ? O6 Zn1 Zn3 O5 -0.17(11) . . . . ? O23 Zn1 Zn3 O5 -125.02(15) 2_655 . . . ? O1W Zn1 Zn3 O5 90.02(12) . . . . ? O19 Zn1 Zn3 O5 -101.47(10) 2_655 . . . ? Na2 Zn1 Zn3 O5 -114.23(8) 2_655 . . . ? O25 Zn1 Zn3 O22 145.7(3) . . . 1_665 ? O6 Zn1 Zn3 O22 3.8(3) . . . 1_665 ? O23 Zn1 Zn3 O22 -121.1(3) 2_655 . . 1_665 ? O1W Zn1 Zn3 O22 94.0(3) . . . 1_665 ? O19 Zn1 Zn3 O22 -97.5(3) 2_655 . . 1_665 ? Na2 Zn1 Zn3 O22 -110.3(3) 2_655 . . 1_665 ? O25 Zn1 Zn3 O21 56.16(13) . . . 1_665 ? O6 Zn1 Zn3 O21 -85.73(11) . . . 1_665 ? O23 Zn1 Zn3 O21 149.42(14) 2_655 . . 1_665 ? O1W Zn1 Zn3 O21 4.46(12) . . . 1_665 ? O19 Zn1 Zn3 O21 172.97(10) 2_655 . . 1_665 ? Na2 Zn1 Zn3 O21 160.21(8) 2_655 . . 1_665 ? O25 Zn1 Zn3 C68 69.19(19) . . . 1_665 ? O6 Zn1 Zn3 C68 -72.70(18) . . . 1_665 ? O23 Zn1 Zn3 C68 162.45(19) 2_655 . . 1_665 ? O1W Zn1 Zn3 C68 17.49(19) . . . 1_665 ? O19 Zn1 Zn3 C68 -174.00(17) 2_655 . . 1_665 ? Na2 Zn1 Zn3 C68 173.24(16) 2_655 . . 1_665 ? O18 Zn2 Na3 O2W 0.78(19) . . . . ? O9 Zn2 Na3 O2W -64.37(19) . . . . ? O7 Zn2 Na3 O2W -164.50(18) 2_655 . . . ? N1 Zn2 Na3 O2W 100.23(18) . . . . ? O18 Zn2 Na3 O10 174.05(15) . . . 2_655 ? O9 Zn2 Na3 O10 108.90(12) . . . 2_655 ? O7 Zn2 Na3 O10 8.78(10) 2_655 . . 2_655 ? N1 Zn2 Na3 O10 -86.49(12) . . . 2_655 ? O18 Zn2 Na3 O12 -102.79(15) . . . 2_655 ? O9 Zn2 Na3 O12 -167.94(12) . . . 2_655 ? O7 Zn2 Na3 O12 91.94(11) 2_655 . . 2_655 ? N1 Zn2 Na3 O12 -3.34(13) . . . 2_655 ? O9 Zn2 Na3 O18 -65.15(16) . . . . ? O7 Zn2 Na3 O18 -165.27(14) 2_655 . . . ? N1 Zn2 Na3 O18 99.45(15) . . . . ? O18 Zn2 Na3 O8 -142.56(14) . . . 2_655 ? O9 Zn2 Na3 O8 152.29(12) . . . 2_655 ? O7 Zn2 Na3 O8 52.16(10) 2_655 . . 2_655 ? N1 Zn2 Na3 O8 -43.11(11) . . . 2_655 ? O18 Zn2 Na3 O7 93.89(13) . . . . ? O9 Zn2 Na3 O7 28.74(12) . . . . ? O7 Zn2 Na3 O7 -71.39(9) 2_655 . . . ? N1 Zn2 Na3 O7 -166.66(10) . . . . ? O18 Zn2 Na3 Na1 -137.98(13) . . . 2_655 ? O9 Zn2 Na3 Na1 156.87(10) . . . 2_655 ? O7 Zn2 Na3 Na1 56.74(8) 2_655 . . 2_655 ? N1 Zn2 Na3 Na1 -38.53(10) . . . 2_655 ? O1 C1 C2 C3 175.3(3) . . . . ? C6 C1 C2 C3 -7.3(5) . . . . ? O1 C1 C2 C28 -9.0(4) . . . . ? C6 C1 C2 C28 168.4(3) . . . . ? C1 C2 C3 C4 1.3(5) . . . . ? C28 C2 C3 C4 -174.5(3) . . . . ? C2 C3 C4 C5 3.7(5) . . . . ? C3 C4 C5 C6 -2.8(5) . . . . ? C4 C5 C6 C1 -2.8(5) . . . . ? C4 C5 C6 C7 172.5(3) . . . . ? C2 C1 C6 C5 8.0(4) . . . . ? O1 C1 C6 C5 -174.6(3) . . . . ? C2 C1 C6 C7 -167.1(3) . . . . ? O1 C1 C6 C7 10.3(4) . . . . ? C5 C6 C7 C8 -75.7(4) . . . . ? C1 C6 C7 C8 99.3(3) . . . . ? C6 C7 C8 C13 -101.8(4) . . . . ? C6 C7 C8 C9 73.8(4) . . . . ? C13 C8 C9 C10 5.0(6) . . . . ? C7 C8 C9 C10 -170.8(4) . . . . ? C8 C9 C10 C11 0.5(7) . . . . ? C9 C10 C11 C12 -3.2(7) . . . . ? C10 C11 C12 C13 0.2(6) . . . . ? C10 C11 C12 C14 178.6(4) . . . . ? C9 C8 C13 C12 -8.2(5) . . . . ? C7 C8 C13 C12 167.5(3) . . . . ? C9 C8 C13 O2 175.4(3) . . . . ? C7 C8 C13 O2 -8.9(5) . . . . ? C11 C12 C13 C8 5.7(5) . . . . ? C14 C12 C13 C8 -172.6(3) . . . . ? C11 C12 C13 O2 -177.9(3) . . . . ? C14 C12 C13 O2 3.8(5) . . . . ? C11 C12 C14 C15 -73.6(4) . . . . ? C13 C12 C14 C15 104.6(4) . . . . ? C12 C14 C15 C20 -91.0(4) . . . . ? C12 C14 C15 C16 86.6(4) . . . . ? C20 C15 C16 C17 1.8(5) . . . . ? C14 C15 C16 C17 -175.9(3) . . . . ? C15 C16 C17 C18 3.7(6) . . . . ? C16 C17 C18 C19 -4.1(6) . . . . ? C17 C18 C19 C20 -1.0(5) . . . . ? C17 C18 C19 C21 175.4(3) . . . . ? C16 C15 C20 C19 -7.3(5) . . . . ? C14 C15 C20 C19 170.4(3) . . . . ? C16 C15 C20 O3 170.6(3) . . . . ? C14 C15 C20 O3 -11.7(5) . . . . ? C18 C19 C20 C15 6.9(5) . . . . ? C21 C19 C20 C15 -169.5(3) . . . . ? C18 C19 C20 O3 -171.0(3) . . . . ? C21 C19 C20 O3 12.6(5) . . . . ? C20 C19 C21 C22 91.9(4) . . . . ? C18 C19 C21 C22 -84.4(4) . . . . ? C19 C21 C22 C27 -102.5(4) . . . . ? C19 C21 C22 C23 74.6(4) . . . . ? C27 C22 C23 C24 -0.7(5) . . . . ? C21 C22 C23 C24 -178.0(3) . . . . ? C22 C23 C24 C25 1.9(6) . . . . ? C23 C24 C25 C26 0.0(6) . . . . ? C24 C25 C26 C27 -3.0(5) . . . . ? C24 C25 C26 C28 172.6(3) . . . . ? C23 C22 C27 C26 -2.4(5) . . . . ? C21 C22 C27 C26 174.7(3) . . . . ? C23 C22 C27 O4 -179.0(3) . . . . ? C21 C22 C27 O4 -1.8(5) . . . . ? C25 C26 C27 C22 4.2(5) . . . . ? C28 C26 C27 C22 -171.2(3) . . . . ? C25 C26 C27 O4 -179.2(3) . . . . ? C28 C26 C27 O4 5.4(4) . . . . ? C25 C26 C28 C2 -80.0(4) . . . . ? C27 C26 C28 C2 95.3(4) . . . . ? C1 C2 C28 C26 -96.5(3) . . . . ? C3 C2 C28 C26 79.1(4) . . . . ? O1 C29 C30 O5 -2.1(5) . . . . ? O1 C29 C30 O6 177.8(3) . . . . ? O2 C31 C32 O8 1.1(5) . . . . ? O2 C31 C32 O7 -177.9(3) . . . . ? O3 C33 C34 O10 10.0(5) . . . . ? O3 C33 C34 O9 -169.5(3) . . . . ? O4 C35 C36 O12 13.3(6) . . . . ? O4 C35 C36 O11 -167.6(4) . . . . ? O4 C35 C36 Na1 2.8(3) . . . . ? O2 Na1 C36 O12 32.0(8) . . . . ? O1 Na1 C36 O12 -95.8(4) . . . . ? O3 Na1 C36 O12 122.9(4) . . . . ? O4 Na1 C36 O12 -166.5(4) . . . . ? O8 Na1 C36 O12 -11.5(4) . . . . ? O10 Na1 C36 O12 56.6(4) . . . . ? Na3 Na1 C36 O12 16.6(3) 2_655 . . . ? O12 Na1 C36 O11 -39.2(8) . . . . ? O2 Na1 C36 O11 -7.2(13) . . . . ? O1 Na1 C36 O11 -135.1(9) . . . . ? O3 Na1 C36 O11 83.7(9) . . . . ? O4 Na1 C36 O11 154.3(10) . . . . ? O8 Na1 C36 O11 -50.7(9) . . . . ? O10 Na1 C36 O11 17.4(9) . . . . ? Na3 Na1 C36 O11 -22.6(9) 2_655 . . . ? O12 Na1 C36 C35 164.5(5) . . . . ? O2 Na1 C36 C35 -163.5(5) . . . . ? O1 Na1 C36 C35 68.7(2) . . . . ? O3 Na1 C36 C35 -72.6(2) . . . . ? O4 Na1 C36 C35 -1.99(19) . . . . ? O8 Na1 C36 C35 153.0(2) . . . . ? O10 Na1 C36 C35 -138.9(2) . . . . ? Na3 Na1 C36 C35 -178.9(3) 2_655 . . . ? C42 C37 C38 C39 -9.3(5) . . . . ? O14 C37 C38 C39 170.4(3) . . . . ? C42 C37 C38 C64 166.3(3) . . . . ? O14 C37 C38 C64 -14.1(5) . . . . ? C37 C38 C39 C40 1.2(5) . . . . ? C64 C38 C39 C40 -174.4(4) . . . . ? C38 C39 C40 C41 5.5(6) . . . . ? C39 C40 C41 C42 -4.6(6) . . . . ? C38 C37 C42 C41 10.1(5) . . . . ? O14 C37 C42 C41 -169.6(3) . . . . ? C38 C37 C42 C43 -166.7(3) . . . . ? O14 C37 C42 C43 13.6(5) . . . . ? C40 C41 C42 C37 -2.9(5) . . . . ? C40 C41 C42 C43 174.0(4) . . . . ? C37 C42 C43 C44 88.3(4) . . . . ? C41 C42 C43 C44 -88.4(4) . . . . ? C42 C43 C44 C45 73.5(4) . . . . ? C42 C43 C44 C49 -106.3(4) . . . . ? C49 C44 C45 C46 1.0(5) . . . . ? C43 C44 C45 C46 -178.9(3) . . . . ? C44 C45 C46 C47 1.3(6) . . . . ? C45 C46 C47 C48 -1.1(6) . . . . ? C46 C47 C48 C49 -1.2(5) . . . . ? C46 C47 C48 C50 175.9(3) . . . . ? C47 C48 C49 O15 -179.7(3) . . . . ? C50 C48 C49 O15 3.4(5) . . . . ? C47 C48 C49 C44 3.6(5) . . . . ? C50 C48 C49 C44 -173.4(3) . . . . ? C45 C44 C49 C48 -3.5(5) . . . . ? C43 C44 C49 C48 176.4(3) . . . . ? C45 C44 C49 O15 179.7(3) . . . . ? C43 C44 C49 O15 -0.4(5) . . . . ? C49 C48 C50 C51 101.2(4) . . . . ? C47 C48 C50 C51 -75.7(4) . . . . ? C48 C50 C51 C52 89.8(4) . . . . ? C48 C50 C51 C56 -86.8(4) . . . . ? C56 C51 C52 C53 2.3(5) . . . . ? C50 C51 C52 C53 -174.4(3) . . . . ? C51 C52 C53 C54 4.8(5) . . . . ? C52 C53 C54 C55 -5.7(5) . . . . ? C53 C54 C55 C56 -0.5(5) . . . . ? C53 C54 C55 C57 171.8(3) . . . . ? C54 C55 C56 C51 7.9(5) . . . . ? C57 C55 C56 C51 -164.3(3) . . . . ? C54 C55 C56 O16 -171.4(3) . . . . ? C57 C55 C56 O16 16.4(4) . . . . ? C52 C51 C56 C55 -8.8(5) . . . . ? C50 C51 C56 C55 167.9(3) . . . . ? C52 C51 C56 O16 170.5(3) . . . . ? C50 C51 C56 O16 -12.8(4) . . . . ? C56 C55 C57 C59 85.3(4) . . . . ? C54 C55 C57 C59 -86.7(4) . . . . ? O13 C58 C59 C60 -178.4(3) . . . . ? C63 C58 C59 C60 -0.9(5) . . . . ? O13 C58 C59 C57 0.6(4) . . . . ? C63 C58 C59 C57 178.0(3) . . . . ? C55 C57 C59 C58 -112.0(3) . . . . ? C55 C57 C59 C60 67.0(4) . . . . ? C58 C59 C60 C61 -1.2(5) . . . . ? C57 C59 C60 C61 179.8(3) . . . . ? C59 C60 C61 C62 1.5(6) . . . . ? C60 C61 C62 C63 0.4(6) . . . . ? C61 C62 C63 C58 -2.4(5) . . . . ? C61 C62 C63 C64 173.5(3) . . . . ? C59 C58 C63 C62 2.7(5) . . . . ? O13 C58 C63 C62 -179.9(3) . . . . ? C59 C58 C63 C64 -173.0(3) . . . . ? O13 C58 C63 C64 4.5(5) . . . . ? C37 C38 C64 C63 -84.2(4) . . . . ? C39 C38 C64 C63 91.2(4) . . . . ? C62 C63 C64 C38 -70.5(4) . . . . ? C58 C63 C64 C38 105.1(4) . . . . ? O14 C65 C66 O19 -12.0(5) . . . . ? O14 C65 C66 O20 169.2(3) . . . . ? O14 C65 C66 Na2 -1.4(3) . . . . ? O14 Na2 C66 O19 167.2(3) . . . . ? O16 Na2 C66 O19 -26.8(4) . . . . ? O23 Na2 C66 O19 -21.1(2) . . . . ? O13 Na2 C66 O19 92.2(3) . . . . ? O15 Na2 C66 O19 -114.4(2) . . . . ? C70 Na2 C66 O19 -13.5(3) . . . . ? Zn1 Na2 C66 O19 -19.9(2) 2_655 . . . ? O19 Na2 C66 O20 45.9(7) . . . . ? O14 Na2 C66 O20 -146.8(8) . . . . ? O16 Na2 C66 O20 19.2(10) . . . . ? O23 Na2 C66 O20 24.9(8) . . . . ? O13 Na2 C66 O20 138.1(8) . . . . ? O15 Na2 C66 O20 -68.4(8) . . . . ? C70 Na2 C66 O20 32.5(8) . . . . ? Zn1 Na2 C66 O20 26.0(8) 2_655 . . . ? O19 Na2 C66 C65 -166.2(4) . . . . ? O14 Na2 C66 C65 1.1(2) . . . . ? O16 Na2 C66 C65 167.1(3) . . . . ? O23 Na2 C66 C65 172.8(2) . . . . ? O13 Na2 C66 C65 -74.0(2) . . . . ? O15 Na2 C66 C65 79.4(2) . . . . ? C70 Na2 C66 C65 -179.6(2) . . . . ? Zn1 Na2 C66 C65 173.9(2) 2_655 . . . ? O15 C67 C68 O21 -5.9(4) . . . . ? O15 C67 C68 O22 174.1(3) . . . . ? O15 C67 C68 Zn3 142(2) . . . 1_445 ? O16 C69 C70 O24 178.2(3) . . . . ? O16 C69 C70 O23 -2.9(4) . . . . ? O16 C69 C70 Na2 11.1(2) . . . . ? O19 Na2 C70 O24 29.7(8) . . . . ? O14 Na2 C70 O24 36.2(9) . . . . ? O16 Na2 C70 O24 -151.1(8) . . . . ? O23 Na2 C70 O24 56.3(7) . . . . ? O13 Na2 C70 O24 -71.3(8) . . . . ? O15 Na2 C70 O24 135.3(8) . . . . ? C66 Na2 C70 O24 34.4(8) . . . . ? Zn1 Na2 C70 O24 41.4(7) 2_655 . . . ? O19 Na2 C70 O23 -26.6(2) . . . . ? O14 Na2 C70 O23 -20.1(4) . . . . ? O16 Na2 C70 O23 152.6(3) . . . . ? O13 Na2 C70 O23 -127.6(2) . . . . ? O15 Na2 C70 O23 79.1(2) . . . . ? C66 Na2 C70 O23 -21.8(2) . . . . ? Zn1 Na2 C70 O23 -14.94(19) 2_655 . . . ? O19 Na2 C70 C69 172.7(2) . . . . ? O14 Na2 C70 C69 179.1(3) . . . . ? O16 Na2 C70 C69 -8.16(18) . . . . ? O23 Na2 C70 C69 -160.8(3) . . . . ? O13 Na2 C70 C69 71.7(2) . . . . ? O15 Na2 C70 C69 -81.7(2) . . . . ? C66 Na2 C70 C69 177.40(19) . . . . ? Zn1 Na2 C70 C69 -175.7(2) 2_655 . . . ? O13 C71 C72 O17 8.3(6) . . . . ? O13 C71 C72 O18 -173.6(3) . . . . ? N2 C75 C76 C76 66.4(5) . . . 2_645 ? N2 C73 N1 C74 -0.2(4) . . . . ? N2 C73 N1 Zn2 175.9(2) . . . . ? N3 C74 N1 C73 0.0(5) . . . . ? N3 C74 N1 Zn2 -176.3(3) . . . . ? O18 Zn2 N1 C73 -23.9(3) . . . . ? O9 Zn2 N1 C73 99.6(3) . . . . ? O7 Zn2 N1 C73 -149.1(3) 2_655 . . . ? Na3 Zn2 N1 C73 -69.3(3) . . . . ? O18 Zn2 N1 C74 151.3(3) . . . . ? O9 Zn2 N1 C74 -85.2(3) . . . . ? O7 Zn2 N1 C74 26.1(3) 2_655 . . . ? Na3 Zn2 N1 C74 105.9(3) . . . . ? N1 C73 N2 N3 0.3(4) . . . . ? N1 C73 N2 C75 178.0(3) . . . . ? C76 C75 N2 C73 103.4(4) . . . . ? C76 C75 N2 N3 -79.2(4) . . . . ? N1 C74 N3 N2 0.2(5) . . . . ? C73 N2 N3 C74 -0.3(4) . . . . ? C75 N2 N3 C74 -178.2(4) . . . . ? C2 C1 O1 C29 -105.6(3) . . . . ? C6 C1 O1 C29 76.9(3) . . . . ? C2 C1 O1 Na1 99.1(3) . . . . ? C6 C1 O1 Na1 -78.5(3) . . . . ? C30 C29 O1 C1 102.8(3) . . . . ? C30 C29 O1 Na1 -98.4(3) . . . . ? O12 Na1 O1 C1 -146.3(2) . . . . ? O2 Na1 O1 C1 61.5(2) . . . . ? O3 Na1 O1 C1 -21.9(3) . . . . ? O4 Na1 O1 C1 -79.2(2) . . . . ? O8 Na1 O1 C1 127.4(2) . . . . ? O10 Na1 O1 C1 135.9(3) . . . . ? C36 Na1 O1 C1 -127.1(2) . . . . ? Na3 Na1 O1 C1 168.8(2) 2_655 . . . ? O12 Na1 O1 C29 58.2(2) . . . . ? O2 Na1 O1 C29 -94.02(19) . . . . ? O3 Na1 O1 C29 -177.44(19) . . . . ? O4 Na1 O1 C29 125.31(19) . . . . ? O8 Na1 O1 C29 -28.05(19) . . . . ? O10 Na1 O1 C29 -19.6(3) . . . . ? C36 Na1 O1 C29 77.4(2) . . . . ? Na3 Na1 O1 C29 13.3(2) 2_655 . . . ? C8 C13 O2 C31 -88.6(4) . . . . ? C12 C13 O2 C31 94.8(4) . . . . ? C8 C13 O2 Na1 85.5(3) . . . . ? C12 C13 O2 Na1 -91.1(3) . . . . ? C32 C31 O2 C13 149.6(3) . . . . ? C32 C31 O2 Na1 -25.0(4) . . . . ? O12 Na1 O2 C13 -173.5(3) . . . . ? O1 Na1 O2 C13 -66.7(2) . . . . ? O3 Na1 O2 C13 73.2(2) . . . . ? O4 Na1 O2 C13 7.7(3) . . . . ? O8 Na1 O2 C13 -148.4(3) . . . . ? O10 Na1 O2 C13 140.4(2) . . . . ? C36 Na1 O2 C13 165.4(6) . . . . ? Na3 Na1 O2 C13 179.8(2) 2_655 . . . ? O12 Na1 O2 C31 0.4(4) . . . . ? O1 Na1 O2 C31 107.2(2) . . . . ? O3 Na1 O2 C31 -112.9(2) . . . . ? O4 Na1 O2 C31 -178.4(2) . . . . ? O8 Na1 O2 C31 25.5(2) . . . . ? O10 Na1 O2 C31 -45.7(2) . . . . ? C36 Na1 O2 C31 -20.8(7) . . . . ? Na3 Na1 O2 C31 -6.3(2) 2_655 . . . ? C15 C20 O3 C33 -90.1(3) . . . . ? C19 C20 O3 C33 87.8(4) . . . . ? C15 C20 O3 Na1 87.1(3) . . . . ? C19 C20 O3 Na1 -94.9(3) . . . . ? C34 C33 O3 C20 149.9(3) . . . . ? C34 C33 O3 Na1 -27.9(4) . . . . ? O12 Na1 O3 C20 137.2(3) . . . . ? O2 Na1 O3 C20 -70.5(3) . . . . ? O1 Na1 O3 C20 16.2(3) . . . . ? O4 Na1 O3 C20 72.9(3) . . . . ? O8 Na1 O3 C20 -122.7(3) . . . . ? O10 Na1 O3 C20 -152.7(3) . . . . ? C36 Na1 O3 C20 120.4(3) . . . . ? Na3 Na1 O3 C20 -174.2(3) 2_655 . . . ? O12 Na1 O3 C33 -45.7(2) . . . . ? O2 Na1 O3 C33 106.6(2) . . . . ? O1 Na1 O3 C33 -166.6(2) . . . . ? O4 Na1 O3 C33 -109.9(2) . . . . ? O8 Na1 O3 C33 54.4(3) . . . . ? O10 Na1 O3 C33 24.4(2) . . . . ? C36 Na1 O3 C33 -62.5(2) . . . . ? Na3 Na1 O3 C33 2.9(2) 2_655 . . . ? O10 Na3 O2W O2W' -56.6(6) 2_655 . . . ? O12 Na3 O2W O2W' -123.3(6) 2_655 . . . ? O18 Na3 O2W O2W' 116.0(6) . . . . ? O8 Na3 O2W O2W' -163.8(6) 2_655 . . . ? O7 Na3 O2W O2W' 21.3(6) . . . . ? Na1 Na3 O2W O2W' -112.9(6) 2_655 . . . ? Zn2 Na3 O2W O2W' 115.6(6) . . . . ? C22 C27 O4 C35 -93.6(4) . . . . ? C26 C27 O4 C35 89.7(3) . . . . ? C22 C27 O4 Na1 86.8(4) . . . . ? C26 C27 O4 Na1 -89.9(3) . . . . ? C36 C35 O4 C27 176.5(3) . . . . ? C36 C35 O4 Na1 -3.8(4) . . . . ? O12 Na1 O4 C27 177.1(3) . . . . ? O2 Na1 O4 C27 -3.5(3) . . . . ? O1 Na1 O4 C27 76.2(3) . . . . ? O3 Na1 O4 C27 -70.4(3) . . . . ? O8 Na1 O4 C27 132.4(3) . . . . ? O10 Na1 O4 C27 -122.7(3) . . . . ? C36 Na1 O4 C27 -178.2(3) . . . . ? Na3 Na1 O4 C27 -175.1(2) 2_655 . . . ? O12 Na1 O4 C35 -2.4(2) . . . . ? O2 Na1 O4 C35 176.9(2) . . . . ? O1 Na1 O4 C35 -103.4(2) . . . . ? O3 Na1 O4 C35 110.0(2) . . . . ? O8 Na1 O4 C35 -47.1(3) . . . . ? O10 Na1 O4 C35 57.8(2) . . . . ? C36 Na1 O4 C35 2.3(2) . . . . ? Na3 Na1 O4 C35 5.3(2) 2_655 . . . ? O6 C30 O5 Zn3 5.6(5) . . . . ? C29 C30 O5 Zn3 -174.4(2) . . . . ? O25 Zn3 O5 C30 20.0(3) . . . . ? O20 Zn3 O5 C30 -85.6(3) 2_655 . . . ? O22 Zn3 O5 C30 178.4(3) 1_665 . . . ? O21 Zn3 O5 C30 118.1(3) 1_665 . . . ? C68 Zn3 O5 C30 148.0(3) 1_665 . . . ? Zn1 Zn3 O5 C30 -2.5(3) . . . . ? O5 C30 O6 Zn1 -5.4(5) . . . . ? C29 C30 O6 Zn1 174.7(2) . . . . ? O25 Zn1 O6 C30 -21.4(3) . . . . ? O23 Zn1 O6 C30 151.7(2) 2_655 . . . ? O1W Zn1 O6 C30 -116.1(3) . . . . ? O19 Zn1 O6 C30 70.2(3) 2_655 . . . ? Zn3 Zn1 O6 C30 2.6(2) . . . . ? Na2 Zn1 O6 C30 108.7(2) 2_655 . . . ? O8 C32 O7 Zn2 -17.6(4) . . . 2_655 ? C31 C32 O7 Zn2 161.4(2) . . . 2_655 ? O8 C32 O7 Na3 115.7(3) . . . . ? C31 C32 O7 Na3 -65.4(4) . . . . ? O2W Na3 O7 C32 105.3(3) . . . . ? O10 Na3 O7 C32 -132.0(3) 2_655 . . . ? O12 Na3 O7 C32 176.3(2) 2_655 . . . ? O18 Na3 O7 C32 2.2(3) . . . . ? O8 Na3 O7 C32 -72.2(3) 2_655 . . . ? Na1 Na3 O7 C32 -127.1(2) 2_655 . . . ? Zn2 Na3 O7 C32 -28.1(2) . . . . ? O2W Na3 O7 Zn2 -122.36(13) . . . 2_655 ? O10 Na3 O7 Zn2 0.41(11) 2_655 . . 2_655 ? O12 Na3 O7 Zn2 -51.3(2) 2_655 . . 2_655 ? O18 Na3 O7 Zn2 134.58(11) . . . 2_655 ? O8 Na3 O7 Zn2 60.21(13) 2_655 . . 2_655 ? Na1 Na3 O7 Zn2 5.26(15) 2_655 . . 2_655 ? Zn2 Na3 O7 Zn2 104.31(10) . . . 2_655 ? O7 C32 O8 Na1 -160.3(3) . . . . ? C31 C32 O8 Na1 20.8(4) . . . . ? O7 C32 O8 Na3 -66.3(4) . . . 2_655 ? C31 C32 O8 Na3 114.8(3) . . . 2_655 ? O12 Na1 O8 C32 143.7(2) . . . . ? O2 Na1 O8 C32 -24.4(2) . . . . ? O1 Na1 O8 C32 -120.3(2) . . . . ? O3 Na1 O8 C32 34.5(3) . . . . ? O4 Na1 O8 C32 -175.1(2) . . . . ? O10 Na1 O8 C32 64.0(2) . . . . ? C36 Na1 O8 C32 147.5(2) . . . . ? Na3 Na1 O8 C32 113.5(2) 2_655 . . . ? O12 Na1 O8 Na3 30.24(11) . . . 2_655 ? O2 Na1 O8 Na3 -137.85(10) . . . 2_655 ? O1 Na1 O8 Na3 126.25(8) . . . 2_655 ? O3 Na1 O8 Na3 -78.95(11) . . . 2_655 ? O4 Na1 O8 Na3 71.35(17) . . . 2_655 ? O10 Na1 O8 Na3 -49.53(8) . . . 2_655 ? C36 Na1 O8 Na3 34.01(11) . . . 2_655 ? O10 C34 O9 Zn2 -19.7(4) . . . . ? C33 C34 O9 Zn2 159.9(2) . . . . ? O18 Zn2 O9 C34 -55.5(2) . . . . ? O7 Zn2 O9 C34 69.3(2) 2_655 . . . ? N1 Zn2 O9 C34 176.3(2) . . . . ? Na3 Zn2 O9 C34 -17.4(3) . . . . ? O9 C34 O10 Na3 -60.9(5) . . . 2_655 ? C33 C34 O10 Na3 119.6(3) . . . 2_655 ? O9 C34 O10 Na1 -167.9(2) . . . . ? C33 C34 O10 Na1 12.6(4) . . . . ? O12 Na1 O10 C34 93.7(2) . . . . ? O2 Na1 O10 C34 -107.0(2) . . . . ? O1 Na1 O10 C34 175.5(2) . . . . ? O3 Na1 O10 C34 -19.8(2) . . . . ? O4 Na1 O10 C34 38.2(3) . . . . ? O8 Na1 O10 C34 -175.5(3) . . . . ? C36 Na1 O10 C34 77.5(2) . . . . ? Na3 Na1 O10 C34 131.2(3) 2_655 . . . ? O12 Na1 O10 Na3 -37.45(11) . . . 2_655 ? O2 Na1 O10 Na3 121.76(10) . . . 2_655 ? O1 Na1 O10 Na3 44.3(2) . . . 2_655 ? O3 Na1 O10 Na3 -151.03(11) . . . 2_655 ? O4 Na1 O10 Na3 -92.99(11) . . . 2_655 ? O8 Na1 O10 Na3 53.34(8) . . . 2_655 ? C36 Na1 O10 Na3 -53.68(11) . . . 2_655 ? O11 C36 O12 Na1 163.1(4) . . . . ? C35 C36 O12 Na1 -17.9(6) . . . . ? O11 C36 O12 Na3 15.6(8) . . . 2_655 ? C35 C36 O12 Na3 -165.4(3) . . . 2_655 ? Na1 C36 O12 Na3 -147.5(6) . . . 2_655 ? O2 Na1 O12 C36 -168.1(3) . . . . ? O1 Na1 O12 C36 85.8(4) . . . . ? O3 Na1 O12 C36 -60.5(4) . . . . ? O4 Na1 O12 C36 11.1(4) . . . . ? O8 Na1 O12 C36 168.9(4) . . . . ? O10 Na1 O12 C36 -121.9(4) . . . . ? Na3 Na1 O12 C36 -159.1(4) 2_655 . . . ? O2 Na1 O12 Na3 -8.9(3) . . . 2_655 ? O1 Na1 O12 Na3 -115.09(11) . . . 2_655 ? O3 Na1 O12 Na3 98.63(12) . . . 2_655 ? O4 Na1 O12 Na3 170.22(14) . . . 2_655 ? O8 Na1 O12 Na3 -31.94(11) . . . 2_655 ? O10 Na1 O12 Na3 37.29(11) . . . 2_655 ? C36 Na1 O12 Na3 159.1(4) . . . 2_655 ? C59 C58 O13 C71 -115.4(3) . . . . ? C63 C58 O13 C71 67.0(4) . . . . ? C59 C58 O13 Na2 86.9(3) . . . . ? C63 C58 O13 Na2 -90.6(3) . . . . ? C72 C71 O13 C58 119.4(3) . . . . ? C72 C71 O13 Na2 -83.9(4) . . . . ? O19 Na2 O13 C58 143.7(2) . . . . ? O14 Na2 O13 C58 73.4(2) . . . . ? O16 Na2 O13 C58 -74.0(2) . . . . ? O23 Na2 O13 C58 -141.9(2) . . . . ? O15 Na2 O13 C58 -0.8(3) . . . . ? C66 Na2 O13 C58 122.7(2) . . . . ? C70 Na2 O13 C58 -124.1(2) . . . . ? Zn1 Na2 O13 C58 -177.6(2) 2_655 . . . ? O19 Na2 O13 C71 -12.7(2) . . . . ? O14 Na2 O13 C71 -83.1(2) . . . . ? O16 Na2 O13 C71 129.5(2) . . . . ? O23 Na2 O13 C71 61.6(3) . . . . ? O15 Na2 O13 C71 -157.3(2) . . . . ? C66 Na2 O13 C71 -33.8(2) . . . . ? C70 Na2 O13 C71 79.4(2) . . . . ? Zn1 Na2 O13 C71 25.9(2) 2_655 . . . ? C38 C37 O14 C65 -91.2(4) . . . . ? C42 C37 O14 C65 88.4(4) . . . . ? C38 C37 O14 Na2 92.1(4) . . . . ? C42 C37 O14 Na2 -88.3(4) . . . . ? C66 C65 O14 C37 -175.3(3) . . . . ? C66 C65 O14 Na2 2.1(4) . . . . ? O19 Na2 O14 C37 180.0(3) . . . . ? O16 Na2 O14 C37 3.6(4) . . . . ? O23 Na2 O14 C37 161.9(3) . . . . ? O13 Na2 O14 C37 -77.0(3) . . . . ? O15 Na2 O14 C37 72.1(3) . . . . ? C66 Na2 O14 C37 175.3(3) . . . . ? C70 Na2 O14 C37 173.2(3) . . . . ? Zn1 Na2 O14 C37 168.8(3) 2_655 . . . ? O19 Na2 O14 C65 3.5(2) . . . . ? O16 Na2 O14 C65 -172.9(2) . . . . ? O23 Na2 O14 C65 -14.6(3) . . . . ? O13 Na2 O14 C65 106.5(2) . . . . ? O15 Na2 O14 C65 -104.4(2) . . . . ? C66 Na2 O14 C65 -1.2(2) . . . . ? C70 Na2 O14 C65 -3.3(4) . . . . ? Zn1 Na2 O14 C65 -7.7(3) 2_655 . . . ? C48 C49 O15 C67 70.4(4) . . . . ? C44 C49 O15 C67 -112.7(3) . . . . ? C48 C49 O15 Na2 -90.1(3) . . . . ? C44 C49 O15 Na2 86.8(3) . . . . ? C68 C67 O15 C49 118.7(3) . . . . ? C68 C67 O15 Na2 -79.3(3) . . . . ? O19 Na2 O15 C49 -143.4(2) . . . . ? O14 Na2 O15 C49 -73.8(2) . . . . ? O16 Na2 O15 C49 75.4(2) . . . . ? O23 Na2 O15 C49 144.8(2) . . . . ? O13 Na2 O15 C49 0.3(3) . . . . ? C66 Na2 O15 C49 -123.9(2) . . . . ? C70 Na2 O15 C49 124.4(2) . . . . ? Zn1 Na2 O15 C49 177.4(2) 2_655 . . . ? O19 Na2 O15 C67 56.4(2) . . . . ? O14 Na2 O15 C67 126.1(2) . . . . ? O16 Na2 O15 C67 -84.8(2) . . . . ? O23 Na2 O15 C67 -15.3(2) . . . . ? O13 Na2 O15 C67 -159.9(2) . . . . ? C66 Na2 O15 C67 75.9(2) . . . . ? C70 Na2 O15 C67 -35.8(2) . . . . ? Zn1 Na2 O15 C67 17.2(2) 2_655 . . . ? C55 C56 O16 C69 80.7(3) . . . . ? C51 C56 O16 C69 -98.6(3) . . . . ? C55 C56 O16 Na2 -85.6(3) . . . . ? C51 C56 O16 Na2 95.1(3) . . . . ? C70 C69 O16 C56 174.6(3) . . . . ? C70 C69 O16 Na2 -16.4(4) . . . . ? O19 Na2 O16 C56 176.4(2) . . . . ? O14 Na2 O16 C56 -9.1(4) . . . . ? O23 Na2 O16 C56 -174.9(3) . . . . ? O13 Na2 O16 C56 70.5(3) . . . . ? O15 Na2 O16 C56 -78.6(3) . . . . ? C66 Na2 O16 C56 -168.8(3) . . . . ? C70 Na2 O16 C56 175.1(3) . . . . ? Zn1 Na2 O16 C56 -174.8(2) 2_655 . . . ? O19 Na2 O16 C69 10.7(3) . . . . ? O14 Na2 O16 C69 -174.8(2) . . . . ? O23 Na2 O16 C69 19.4(2) . . . . ? O13 Na2 O16 C69 -95.3(2) . . . . ? O15 Na2 O16 C69 115.7(2) . . . . ? C66 Na2 O16 C69 25.4(4) . . . . ? C70 Na2 O16 C69 9.3(2) . . . . ? Zn1 Na2 O16 C69 19.5(2) 2_655 . . . ? O17 C72 O18 Zn2 -8.6(5) . . . . ? C71 C72 O18 Zn2 173.4(2) . . . . ? O17 C72 O18 Na3 147.1(3) . . . . ? C71 C72 O18 Na3 -30.9(4) . . . . ? O9 Zn2 O18 C72 -62.5(3) . . . . ? O7 Zn2 O18 C72 176.2(2) 2_655 . . . ? N1 Zn2 O18 C72 57.1(3) . . . . ? Na3 Zn2 O18 C72 160.7(3) . . . . ? O9 Zn2 O18 Na3 136.78(11) . . . . ? O7 Zn2 O18 Na3 15.58(15) 2_655 . . . ? N1 Zn2 O18 Na3 -103.61(13) . . . . ? O2W Na3 O18 C72 24.0(3) . . . . ? O10 Na3 O18 C72 -164.6(3) 2_655 . . . ? O12 Na3 O18 C72 -60.5(3) 2_655 . . . ? O8 Na3 O18 C72 -128.4(3) 2_655 . . . ? O7 Na3 O18 C72 115.3(3) . . . . ? Na1 Na3 O18 C72 -108.2(3) 2_655 . . . ? Zn2 Na3 O18 C72 -156.6(3) . . . . ? O2W Na3 O18 Zn2 -179.42(14) . . . . ? O10 Na3 O18 Zn2 -8.1(2) 2_655 . . . ? O12 Na3 O18 Zn2 96.02(14) 2_655 . . . ? O8 Na3 O18 Zn2 28.18(11) 2_655 . . . ? O7 Na3 O18 Zn2 -88.19(11) . . . . ? Na1 Na3 O18 Zn2 48.35(14) 2_655 . . . ? O20 C66 O19 Zn1 -23.5(5) . . . 2_655 ? C65 C66 O19 Zn1 157.9(3) . . . 2_655 ? Na2 C66 O19 Zn1 141.9(4) . . . 2_655 ? O20 C66 O19 Na2 -165.4(3) . . . . ? C65 C66 O19 Na2 16.0(4) . . . . ? O14 Na2 O19 C66 -10.5(2) . . . . ? O16 Na2 O19 C66 166.3(2) . . . . ? O23 Na2 O19 C66 157.7(3) . . . . ? O13 Na2 O19 C66 -91.8(3) . . . . ? O15 Na2 O19 C66 69.5(3) . . . . ? C70 Na2 O19 C66 167.4(2) . . . . ? Zn1 Na2 O19 C66 152.7(3) 2_655 . . . ? O14 Na2 O19 Zn1 -163.19(11) . . . 2_655 ? O16 Na2 O19 Zn1 13.64(19) . . . 2_655 ? O23 Na2 O19 Zn1 5.03(9) . . . 2_655 ? O13 Na2 O19 Zn1 115.51(10) . . . 2_655 ? O15 Na2 O19 Zn1 -83.17(10) . . . 2_655 ? C66 Na2 O19 Zn1 -152.7(3) . . . 2_655 ? C70 Na2 O19 Zn1 14.68(10) . . . 2_655 ? O19 C66 O20 Zn3 14.6(5) . . . 2_655 ? C65 C66 O20 Zn3 -166.7(2) . . . 2_655 ? Na2 C66 O20 Zn3 -21.4(9) . . . 2_655 ? O22 C68 O21 Zn3 -4.1(3) . . . 1_445 ? C67 C68 O21 Zn3 175.9(3) . . . 1_445 ? O21 C68 O22 Zn3 4.3(3) . . . 1_445 ? C67 C68 O22 Zn3 -175.7(2) . . . 1_445 ? O24 C70 O23 Zn1 -7.2(5) . . . 2_655 ? C69 C70 O23 Zn1 174.1(2) . . . 2_655 ? Na2 C70 O23 Zn1 152.8(3) . . . 2_655 ? O24 C70 O23 Na2 -159.9(3) . . . . ? C69 C70 O23 Na2 21.3(4) . . . . ? O19 Na2 O23 C70 151.9(2) . . . . ? O14 Na2 O23 C70 170.0(2) . . . . ? O16 Na2 O23 C70 -22.4(2) . . . . ? O13 Na2 O23 C70 57.6(2) . . . . ? O15 Na2 O23 C70 -102.9(2) . . . . ? C66 Na2 O23 C70 159.6(2) . . . . ? Zn1 Na2 O23 C70 157.7(3) 2_655 . . . ? O19 Na2 O23 Zn1 -5.88(10) . . . 2_655 ? O14 Na2 O23 Zn1 12.3(2) . . . 2_655 ? O16 Na2 O23 Zn1 179.83(12) . . . 2_655 ? O13 Na2 O23 Zn1 -100.17(12) . . . 2_655 ? O15 Na2 O23 Zn1 99.37(11) . . . 2_655 ? C66 Na2 O23 Zn1 1.82(11) . . . 2_655 ? C70 Na2 O23 Zn1 -157.7(3) . . . 2_655 ? O6 Zn1 O25 Zn3 41.52(13) . . . . ? O23 Zn1 O25 Zn3 -130.04(11) 2_655 . . . ? O1W Zn1 O25 Zn3 136.53(11) . . . . ? O19 Zn1 O25 Zn3 -56.51(10) 2_655 . . . ? Na2 Zn1 O25 Zn3 -89.91(9) 2_655 . . . ? O20 Zn3 O25 Zn1 70.06(12) 2_655 . . . ? O5 Zn3 O25 Zn1 -37.19(12) . . . . ? O22 Zn3 O25 Zn1 -162.90(16) 1_665 . . . ? O21 Zn3 O25 Zn1 -134.03(11) 1_665 . . . ? C68 Zn3 O25 Zn1 -144.20(12) 1_665 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1A O5W 0.866(19) 1.84(2) 2.697(5) 173(5) . O1W H1B O24 0.90(2) 1.96(3) 2.806(4) 155(5) 2_655 O25 H25A O4W 0.71(6) 2.41(6) 3.104(10) 164(8) 1_565 O25 H25A O4W' 0.71(6) 2.46(6) 3.104(12) 151(8) 1_565 _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.059 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.067 #===== data_9 _database_code_depnum_ccdc_archive 'CCDC 879391' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H84 Co4 Na2 O39' _chemical_formula_weight 1855.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.788(3) _cell_length_b 18.229(6) _cell_length_c 21.761(7) _cell_angle_alpha 90 _cell_angle_beta 98.766(4) _cell_angle_gamma 90 _cell_volume 4229(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1916 _exptl_absorpt_coefficient_mu 0.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7988 _exptl_absorpt_correction_T_max 0.8590 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18698 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 29.35 _reflns_number_total 9771 _reflns_number_gt 6237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distances of O3---H3A, O3W---H3B, O1W---H1A, O1W---H1B, O2W---H2A, O2W---H2B, O4W---H4A and O4W---H4B were restrained to 0.82+-0.01 \%A. The distance of O13---H13 was restrained to 0.89+-0.02 \%A. The distances of H3A...H3B, H2A...H2B and H1A...H1B were restrained to 1.44+-0.02 \%A. The distance of H4A...H4B was restrained to 1.44+-0.01 \%A. The distance of O5W...O11 was restrained to 3.02+-0.01 \%A. The distance of H2B...H4A was restrained to 2.50+-0.02 \%A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9771 _refine_ls_number_parameters 568 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.78356(4) 0.11861(2) -0.03338(2) 0.02844(13) Uani 1 1 d . . . Co2 Co 1.09436(4) 0.05714(2) -0.01828(2) 0.02647(13) Uani 1 1 d . . . Na1 Na 0.71658(12) 0.21947(7) 0.07945(6) 0.0338(3) Uani 1 1 d . . . C1 C 0.4383(3) 0.2405(2) 0.13562(18) 0.0368(8) Uani 1 1 d . . . C2 C 0.3827(3) 0.3085(2) 0.12038(19) 0.0415(9) Uani 1 1 d . . . C3 C 0.3138(4) 0.3395(2) 0.1634(2) 0.0515(11) Uani 1 1 d . . . H3 H 0.2725 0.3838 0.1539 0.062 Uiso 1 1 calc R . . C4 C 0.3057(4) 0.3062(3) 0.2188(2) 0.0585(12) Uani 1 1 d . . . H4 H 0.2581 0.3275 0.2463 0.070 Uiso 1 1 calc R . . C5 C 0.3671(4) 0.2419(3) 0.2343(2) 0.0530(11) Uani 1 1 d . . . H5 H 0.3619 0.2203 0.2725 0.064 Uiso 1 1 calc R . . C6 C 0.4376(3) 0.2079(2) 0.19357(18) 0.0387(8) Uani 1 1 d . . . C7 C 0.5179(4) 0.1413(2) 0.21627(18) 0.0408(9) Uani 1 1 d . . . H7A H 0.5397 0.1148 0.1808 0.049 Uiso 1 1 calc R . . H7B H 0.4700 0.1085 0.2388 0.049 Uiso 1 1 calc R . . C8 C 0.7505(3) 0.17253(18) 0.23584(15) 0.0327(8) Uani 1 1 d . . . C9 C 0.6379(4) 0.16453(19) 0.25869(16) 0.0364(8) Uani 1 1 d . . . C10 C 0.6350(4) 0.1806(2) 0.32047(18) 0.0446(9) Uani 1 1 d . . . H10 H 0.5608 0.1747 0.3368 0.053 Uiso 1 1 calc R . . C11 C 0.7416(4) 0.2054(2) 0.35813(18) 0.0469(10) Uani 1 1 d . . . H11 H 0.7399 0.2142 0.4001 0.056 Uiso 1 1 calc R . . C12 C 0.8506(4) 0.2172(2) 0.33367(17) 0.0432(9) Uani 1 1 d . . . H12 H 0.9204 0.2362 0.3590 0.052 Uiso 1 1 calc R . . C13 C 0.8580(4) 0.20112(18) 0.27152(16) 0.0359(8) Uani 1 1 d . . . C14 C 0.9741(3) 0.2191(2) 0.24483(18) 0.0399(9) Uani 1 1 d . . . H14A H 0.9778 0.1887 0.2086 0.048 Uiso 1 1 calc R . . H14B H 1.0472 0.2083 0.2753 0.048 Uiso 1 1 calc R . . C15 C 0.9760(3) 0.2996(2) 0.22643(17) 0.0365(8) Uani 1 1 d . . . C16 C 1.0083(4) 0.3529(2) 0.27244(19) 0.0451(9) Uani 1 1 d . . . H16 H 1.0352 0.3386 0.3133 0.054 Uiso 1 1 calc R . . C17 C 1.0005(4) 0.4264(2) 0.2573(2) 0.0513(11) Uani 1 1 d . . . H17 H 1.0257 0.4616 0.2876 0.062 Uiso 1 1 calc R . . C18 C 0.9556(4) 0.4478(2) 0.1977(2) 0.0493(10) Uani 1 1 d . . . H18 H 0.9480 0.4976 0.1886 0.059 Uiso 1 1 calc R . . C19 C 0.9212(3) 0.3971(2) 0.15069(18) 0.0398(8) Uani 1 1 d . . . C20 C 0.9395(3) 0.32307(19) 0.16548(17) 0.0342(8) Uani 1 1 d . . . C21 C 0.8582(4) 0.4223(2) 0.0865(2) 0.0514(10) Uani 1 1 d . . . H21A H 0.9021 0.4646 0.0735 0.062 Uiso 1 1 calc R . . H21B H 0.8621 0.3834 0.0565 0.062 Uiso 1 1 calc R . . C22 C 0.6227(4) 0.39470(18) 0.06775(17) 0.0409(9) Uani 1 1 d . . . C23 C 0.7223(4) 0.44211(19) 0.08862(18) 0.0451(9) Uani 1 1 d . . . C24 C 0.6908(5) 0.5088(2) 0.1137(2) 0.0576(12) Uani 1 1 d . . . H24 H 0.7532 0.5432 0.1262 0.069 Uiso 1 1 calc R . . C25 C 0.5706(5) 0.5243(2) 0.1203(2) 0.0612(12) Uani 1 1 d . . . H25 H 0.5518 0.5690 0.1373 0.073 Uiso 1 1 calc R . . C26 C 0.4754(5) 0.4743(2) 0.1018(2) 0.0580(12) Uani 1 1 d . . . H26 H 0.3935 0.4857 0.1068 0.070 Uiso 1 1 calc R . . C27 C 0.5004(4) 0.4076(2) 0.07604(18) 0.0439(9) Uani 1 1 d . . . C28 C 0.3981(4) 0.3497(2) 0.06200(19) 0.0464(10) Uani 1 1 d . . . H28A H 0.3195 0.3732 0.0452 0.056 Uiso 1 1 calc R . . H28B H 0.4201 0.3158 0.0311 0.056 Uiso 1 1 calc R . . C29 C 0.4500(3) 0.1388(2) 0.0671(2) 0.0425(9) Uani 1 1 d . . . H29A H 0.4331 0.1085 0.1015 0.051 Uiso 1 1 calc R . . H29B H 0.5132 0.1139 0.0475 0.051 Uiso 1 1 calc R . . C30 C 0.3312(3) 0.1437(2) 0.02033(16) 0.0344(8) Uani 1 1 d . . . C31 C 0.8006(4) 0.07899(19) 0.16981(16) 0.0372(8) Uani 1 1 d . . . H31A H 0.7436 0.0453 0.1858 0.045 Uiso 1 1 calc R . . H31B H 0.8823 0.0743 0.1953 0.045 Uiso 1 1 calc R . . C32 C 0.8109(3) 0.05867(17) 0.10241(15) 0.0286(7) Uani 1 1 d . . . C33 C 1.0319(3) 0.2451(2) 0.09945(18) 0.0395(9) Uani 1 1 d . . . H33A H 1.0873 0.2261 0.1352 0.047 Uiso 1 1 calc R . . H33B H 1.0741 0.2854 0.0821 0.047 Uiso 1 1 calc R . . C34 C 1.0010(3) 0.18532(19) 0.05122(16) 0.0302(7) Uani 1 1 d . . . C35 C 0.6337(5) 0.3382(2) -0.02805(18) 0.0515(11) Uani 1 1 d . . . H35A H 0.6879 0.3770 -0.0389 0.062 Uiso 1 1 calc R . . H35B H 0.5476 0.3523 -0.0427 0.062 Uiso 1 1 calc R . . C36 C 0.6631(3) 0.2676(2) -0.05984(18) 0.0391(8) Uani 1 1 d . . . O1 O 0.5016(2) 0.20703(12) 0.09184(11) 0.0344(5) Uani 1 1 d . . . O2 O 0.7558(2) 0.15281(12) 0.17385(10) 0.0334(5) Uani 1 1 d . . . O1W O 0.8231(2) 0.15487(15) -0.12093(11) 0.0448(6) Uani 1 1 d D . . H1A H 0.7805 0.1948 -0.1293 0.067 Uiso 1 1 d RD . . H1B H 0.8320 0.1407 -0.1498 0.067 Uiso 1 1 d RD . . O3 O 0.9171(2) 0.27069(13) 0.11816(11) 0.0346(5) Uani 1 1 d . . . O2W O 0.6421(2) 0.04774(14) -0.07184(13) 0.0473(7) Uani 1 1 d D . . H2A H 0.6572 0.0004 -0.0518 0.071 Uiso 1 1 d RD . . H2B H 0.6161 0.0561 -0.0389 0.071 Uiso 1 1 d RD . . O4 O 0.6511(2) 0.32952(12) 0.03778(11) 0.0390(6) Uani 1 1 d . . . O3W O 1.0876(2) 0.15018(14) -0.08123(11) 0.0390(6) Uani 1 1 d D . . H3A H 1.0982 0.1385 -0.1179 0.058 Uiso 1 1 d RD . . H3B H 1.1470 0.1781 -0.0568 0.058 Uiso 1 1 d RD . . O5 O 0.2869(3) 0.20210(14) -0.00082(13) 0.0509(7) Uani 1 1 d . . . O6 O 0.2859(2) 0.07947(13) 0.00587(12) 0.0352(5) Uani 1 1 d . . . O7 O 0.8752(2) 0.00296(13) 0.09711(10) 0.0341(5) Uani 1 1 d . . . O8 O 0.7544(2) 0.09747(13) 0.06000(10) 0.0352(5) Uani 1 1 d . . . O7W O 0.8834(10) 0.0329(6) -0.1849(5) 0.119(3) Uani 0.50 1 d P . . O9 O 1.0706(2) 0.12993(13) 0.05524(11) 0.0376(6) Uani 1 1 d . . . O10 O 0.9089(2) 0.19655(14) 0.01004(11) 0.0403(6) Uani 1 1 d . . . O11 O 0.6851(3) 0.27387(15) -0.11359(13) 0.0548(7) Uani 1 1 d D . . O12 O 0.6604(2) 0.20860(13) -0.03047(11) 0.0367(6) Uani 1 1 d . . . O6W O 0.6746(14) 0.4705(10) -0.2880(8) 0.087(5) Uani 0.25 1 d P . . O5W O 0.7990(11) 0.4051(5) -0.1534(5) 0.133(4) Uani 0.50 1 d PD . . O9W O 1.206(2) 0.0703(14) 0.1730(14) 0.158(12) Uani 0.25 1 d P . . O10W O 0.6452(6) 0.3784(4) 0.2498(3) 0.0600(16) Uani 0.50 1 d P . . O8W O 0.8211(7) -0.1081(4) 0.1917(3) 0.082(3) Uani 0.50 1 d P . . O4W O 0.3935(3) 0.0629(2) -0.10638(18) 0.0812(11) Uani 1 1 d D . . H4B H 0.344(5) 0.066(3) -0.078(2) 0.122 Uiso 1 1 d D . . H4A H 0.432(2) 0.1035(13) -0.110(2) 0.122 Uiso 1 1 d D . . O13 O 0.9046(2) 0.03372(12) -0.03907(10) 0.0263(5) Uani 1 1 d D . . H13 H 0.902(4) 0.030(2) -0.0765(9) 0.039 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0307(2) 0.0263(2) 0.0263(2) -0.00212(18) -0.00182(18) -0.00126(19) Co2 0.0270(2) 0.0244(2) 0.0276(2) -0.00321(18) 0.00290(18) -0.00291(18) Na1 0.0374(7) 0.0260(6) 0.0351(7) -0.0011(6) -0.0038(6) 0.0016(6) C1 0.0243(16) 0.0358(19) 0.048(2) -0.0121(17) -0.0022(15) -0.0035(15) C2 0.0313(18) 0.0345(19) 0.052(2) -0.0091(18) -0.0135(17) 0.0004(16) C3 0.037(2) 0.046(2) 0.067(3) -0.017(2) -0.008(2) 0.0068(18) C4 0.040(2) 0.066(3) 0.069(3) -0.021(3) 0.007(2) 0.003(2) C5 0.044(2) 0.059(3) 0.057(3) -0.008(2) 0.010(2) 0.001(2) C6 0.0358(18) 0.0365(19) 0.042(2) -0.0055(17) 0.0008(16) -0.0038(16) C7 0.048(2) 0.0342(19) 0.041(2) 0.0011(17) 0.0093(18) -0.0046(17) C8 0.047(2) 0.0237(16) 0.0262(17) -0.0018(13) 0.0011(16) 0.0089(15) C9 0.050(2) 0.0263(17) 0.0319(19) -0.0007(15) 0.0021(17) 0.0075(16) C10 0.062(3) 0.038(2) 0.035(2) -0.0002(17) 0.0105(19) 0.0104(19) C11 0.072(3) 0.040(2) 0.0273(19) -0.0026(16) 0.003(2) 0.017(2) C12 0.058(2) 0.037(2) 0.0309(19) -0.0049(16) -0.0054(18) 0.0120(18) C13 0.047(2) 0.0274(17) 0.0296(18) -0.0034(14) -0.0053(16) 0.0131(16) C14 0.0396(19) 0.038(2) 0.038(2) -0.0097(16) -0.0067(16) 0.0149(16) C15 0.0282(17) 0.039(2) 0.040(2) -0.0128(17) -0.0020(15) 0.0051(15) C16 0.042(2) 0.051(2) 0.040(2) -0.0147(19) -0.0047(17) 0.0024(19) C17 0.056(2) 0.043(2) 0.053(3) -0.024(2) 0.001(2) -0.0086(19) C18 0.059(3) 0.036(2) 0.051(2) -0.0115(19) 0.002(2) -0.0077(19) C19 0.0377(19) 0.0361(19) 0.044(2) -0.0086(17) 0.0014(17) -0.0079(16) C20 0.0291(16) 0.0353(18) 0.0366(19) -0.0140(16) 0.0003(15) -0.0030(15) C21 0.063(3) 0.035(2) 0.054(3) -0.0054(19) -0.001(2) -0.013(2) C22 0.060(2) 0.0194(16) 0.038(2) 0.0000(15) -0.0082(18) 0.0023(16) C23 0.063(3) 0.0248(17) 0.043(2) -0.0012(16) -0.0062(19) -0.0046(18) C24 0.074(3) 0.0247(19) 0.067(3) -0.0078(19) -0.013(2) -0.004(2) C25 0.082(3) 0.027(2) 0.069(3) -0.009(2) -0.010(3) 0.010(2) C26 0.066(3) 0.027(2) 0.075(3) -0.004(2) -0.009(2) 0.010(2) C27 0.054(2) 0.0261(18) 0.045(2) -0.0013(17) -0.0133(18) 0.0069(17) C28 0.046(2) 0.0315(19) 0.054(2) -0.0055(18) -0.0148(19) 0.0076(17) C29 0.0385(19) 0.0298(18) 0.055(2) -0.0121(17) -0.0060(18) -0.0051(16) C30 0.0350(18) 0.0341(19) 0.0341(19) -0.0032(16) 0.0051(15) -0.0035(16) C31 0.053(2) 0.0279(17) 0.0296(18) -0.0033(14) 0.0021(16) 0.0094(16) C32 0.0331(16) 0.0230(16) 0.0304(17) -0.0051(14) 0.0070(14) -0.0068(14) C33 0.0305(17) 0.043(2) 0.044(2) -0.0176(17) 0.0034(16) -0.0029(16) C34 0.0297(17) 0.0319(17) 0.0288(17) -0.0017(14) 0.0038(14) -0.0076(15) C35 0.078(3) 0.034(2) 0.038(2) 0.0041(17) -0.006(2) 0.009(2) C36 0.0407(19) 0.0324(19) 0.038(2) -0.0002(17) -0.0139(17) 0.0015(16) O1 0.0335(12) 0.0277(12) 0.0397(14) -0.0085(10) -0.0018(11) -0.0044(10) O2 0.0492(14) 0.0255(11) 0.0248(12) -0.0044(10) 0.0030(11) 0.0077(11) O1W 0.0541(16) 0.0497(16) 0.0303(13) 0.0055(12) 0.0051(12) 0.0051(13) O3 0.0291(12) 0.0349(13) 0.0376(13) -0.0122(11) -0.0019(10) -0.0026(10) O2W 0.0399(14) 0.0406(15) 0.0564(17) -0.0026(13) -0.0083(13) -0.0065(12) O4 0.0554(16) 0.0229(12) 0.0340(13) -0.0035(10) -0.0085(12) 0.0017(11) O3W 0.0434(14) 0.0387(13) 0.0340(13) 0.0017(11) 0.0034(11) -0.0043(12) O5 0.0589(18) 0.0339(14) 0.0523(17) 0.0066(13) -0.0159(14) -0.0115(13) O6 0.0285(12) 0.0283(12) 0.0461(15) -0.0050(11) -0.0024(11) -0.0059(10) O7 0.0410(13) 0.0318(12) 0.0295(13) -0.0071(10) 0.0050(11) 0.0072(11) O8 0.0469(14) 0.0316(12) 0.0270(12) 0.0020(10) 0.0055(11) 0.0069(11) O7W 0.141(9) 0.106(7) 0.115(8) -0.007(6) 0.033(7) 0.021(7) O9 0.0397(13) 0.0340(13) 0.0372(14) -0.0090(11) 0.0001(11) 0.0040(11) O10 0.0415(14) 0.0365(14) 0.0385(14) -0.0079(11) -0.0078(12) -0.0045(11) O11 0.077(2) 0.0490(16) 0.0350(15) 0.0055(13) -0.0031(14) 0.0106(15) O12 0.0392(13) 0.0287(12) 0.0392(14) -0.0031(11) -0.0038(11) 0.0010(11) O6W 0.060(9) 0.089(12) 0.099(12) 0.053(10) -0.035(8) -0.024(9) O5W 0.195(11) 0.087(6) 0.142(9) -0.003(6) 0.107(8) -0.051(7) O9W 0.091(14) 0.141(19) 0.21(3) 0.064(19) -0.095(16) -0.039(14) O10W 0.057(4) 0.074(4) 0.045(3) -0.003(3) -0.007(3) -0.010(3) O8W 0.115(6) 0.111(6) 0.023(3) 0.020(3) 0.016(3) 0.074(5) O4W 0.052(2) 0.121(3) 0.074(2) 0.004(2) 0.0179(18) -0.008(2) O13 0.0265(10) 0.0292(11) 0.0222(11) -0.0024(10) 0.0002(9) -0.0011(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O13 2.041(2) . ? Co1 O2W 2.076(3) . ? Co1 O10 2.086(2) . ? Co1 O12 2.118(2) . ? Co1 O1W 2.120(2) . ? Co1 O8 2.138(2) . ? Co1 Na1 3.2360(16) . ? Co2 O13 2.072(2) . ? Co2 O13 2.073(2) 3_755 ? Co2 O6 2.093(2) 1_655 ? Co2 O7 2.103(2) 3_755 ? Co2 O9 2.124(2) . ? Co2 O3W 2.174(2) . ? Na1 O4 2.269(3) . ? Na1 O8 2.312(3) . ? Na1 O2 2.368(3) . ? Na1 O12 2.385(3) . ? Na1 O1 2.386(3) . ? Na1 O3 2.389(3) . ? Na1 O10 2.778(3) . ? Na1 C32 3.118(4) . ? Na1 C36 3.124(4) . ? C1 O1 1.394(4) . ? C1 C2 1.394(5) . ? C1 C6 1.396(5) . ? C2 C3 1.399(6) . ? C2 C28 1.508(6) . ? C3 C4 1.366(7) . ? C3 H3 0.9300 . ? C4 C5 1.363(7) . ? C4 H4 0.9300 . ? C5 C6 1.397(5) . ? C5 H5 0.9300 . ? C6 C7 1.529(5) . ? C7 C9 1.531(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.388(5) . ? C8 C13 1.395(5) . ? C8 O2 1.406(4) . ? C9 C10 1.381(5) . ? C10 C11 1.383(6) . ? C10 H10 0.9300 . ? C11 C12 1.379(6) . ? C11 H11 0.9300 . ? C12 C13 1.398(5) . ? C12 H12 0.9300 . ? C13 C14 1.495(5) . ? C14 C15 1.522(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.392(5) . ? C15 C16 1.400(5) . ? C16 C17 1.380(6) . ? C16 H16 0.9300 . ? C17 C18 1.370(6) . ? C17 H17 0.9300 . ? C18 C19 1.388(5) . ? C18 H18 0.9300 . ? C19 C20 1.394(5) . ? C19 C21 1.528(6) . ? C20 O3 1.398(4) . ? C21 C23 1.517(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.379(6) . ? C22 C23 1.400(5) . ? C22 O4 1.411(4) . ? C23 C24 1.397(5) . ? C24 C25 1.355(7) . ? C24 H24 0.9300 . ? C25 C26 1.387(6) . ? C25 H25 0.9300 . ? C26 C27 1.382(5) . ? C26 H26 0.9300 . ? C27 C28 1.524(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O1 1.433(4) . ? C29 C30 1.513(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O5 1.227(4) . ? C30 O6 1.290(4) . ? C31 O2 1.437(4) . ? C31 C32 1.533(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O7 1.245(4) . ? C32 O8 1.246(4) . ? C33 O3 1.438(4) . ? C33 C34 1.515(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O10 1.249(4) . ? C34 O9 1.253(4) . ? C35 O4 1.425(4) . ? C35 C36 1.517(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O11 1.234(5) . ? C36 O12 1.254(4) . ? O1W H1A 0.8650 . ? O1W H1B 0.6997 . ? O2W H2A 0.9689 . ? O2W H2B 0.8230 . ? O3W H3A 0.8505 . ? O3W H3B 0.9212 . ? O6 Co2 2.093(2) 1_455 ? O7 Co2 2.103(2) 3_755 ? O7W O6W 1.385(18) 2_644 ? O6W O9W 1.21(3) 4_565 ? O6W O7W 1.385(18) 2_654 ? O9W O6W 1.21(3) 4_666 ? O10W O8W 1.292(8) 2_655 ? O8W O10W 1.292(8) 2_645 ? O4W H4B 0.873(11) . ? O4W H4A 0.862(11) . ? O13 Co2 2.073(2) 3_755 ? O13 H13 0.813(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Co1 O2W 86.65(10) . . ? O13 Co1 O10 99.63(10) . . ? O2W Co1 O10 173.03(10) . . ? O13 Co1 O12 177.78(9) . . ? O2W Co1 O12 93.91(10) . . ? O10 Co1 O12 79.94(10) . . ? O13 Co1 O1W 87.92(10) . . ? O2W Co1 O1W 93.89(11) . . ? O10 Co1 O1W 89.39(10) . . ? O12 Co1 O1W 89.90(10) . . ? O13 Co1 O8 96.28(9) . . ? O2W Co1 O8 93.74(11) . . ? O10 Co1 O8 82.62(10) . . ? O12 Co1 O8 85.83(9) . . ? O1W Co1 O8 171.49(10) . . ? O13 Co1 Na1 134.09(7) . . ? O2W Co1 Na1 115.09(8) . . ? O10 Co1 Na1 58.24(7) . . ? O12 Co1 Na1 47.44(7) . . ? O1W Co1 Na1 127.11(8) . . ? O8 Co1 Na1 45.50(7) . . ? O13 Co2 O13 83.19(9) . 3_755 ? O13 Co2 O6 178.01(9) . 1_655 ? O13 Co2 O6 95.15(9) 3_755 1_655 ? O13 Co2 O7 89.22(9) . 3_755 ? O13 Co2 O7 95.03(9) 3_755 3_755 ? O6 Co2 O7 92.01(9) 1_655 3_755 ? O13 Co2 O9 93.71(9) . . ? O13 Co2 O9 92.06(9) 3_755 . ? O6 Co2 O9 85.25(9) 1_655 . ? O7 Co2 O9 172.61(9) 3_755 . ? O13 Co2 O3W 94.93(9) . . ? O13 Co2 O3W 177.64(9) 3_755 . ? O6 Co2 O3W 86.76(9) 1_655 . ? O7 Co2 O3W 83.50(10) 3_755 . ? O9 Co2 O3W 89.48(10) . . ? O4 Na1 O8 146.11(11) . . ? O4 Na1 O2 143.47(10) . . ? O8 Na1 O2 69.64(9) . . ? O4 Na1 O12 69.92(9) . . ? O8 Na1 O12 76.19(9) . . ? O2 Na1 O12 144.27(10) . . ? O4 Na1 O1 83.12(10) . . ? O8 Na1 O1 97.52(9) . . ? O2 Na1 O1 84.34(9) . . ? O12 Na1 O1 90.16(9) . . ? O4 Na1 O3 90.32(10) . . ? O8 Na1 O3 105.37(10) . . ? O2 Na1 O3 82.09(9) . . ? O12 Na1 O3 117.65(10) . . ? O1 Na1 O3 147.25(10) . . ? O4 Na1 O10 97.39(10) . . ? O8 Na1 O10 65.71(8) . . ? O2 Na1 O10 110.18(9) . . ? O12 Na1 O10 62.53(9) . . ? O1 Na1 O10 150.06(9) . . ? O3 Na1 O10 62.55(8) . . ? O4 Na1 C32 165.73(10) . . ? O8 Na1 C32 20.38(8) . . ? O2 Na1 C32 50.80(8) . . ? O12 Na1 C32 96.28(9) . . ? O1 Na1 C32 101.05(9) . . ? O3 Na1 C32 93.15(9) . . ? O10 Na1 C32 72.13(8) . . ? O4 Na1 C36 50.48(9) . . ? O8 Na1 C36 95.99(10) . . ? O2 Na1 C36 165.43(10) . . ? O12 Na1 C36 21.39(9) . . ? O1 Na1 C36 95.58(10) . . ? O3 Na1 C36 104.82(10) . . ? O10 Na1 C36 63.74(9) . . ? C32 Na1 C36 115.29(10) . . ? O4 Na1 Co1 106.92(8) . . ? O8 Na1 Co1 41.28(6) . . ? O2 Na1 Co1 109.61(7) . . ? O12 Na1 Co1 40.86(6) . . ? O1 Na1 Co1 111.41(7) . . ? O3 Na1 Co1 101.22(7) . . ? O10 Na1 Co1 39.68(5) . . ? C32 Na1 Co1 58.82(7) . . ? C36 Na1 Co1 56.84(7) . . ? O1 C1 C2 117.7(3) . . ? O1 C1 C6 120.1(3) . . ? C2 C1 C6 122.1(3) . . ? C1 C2 C3 117.0(4) . . ? C1 C2 C28 123.0(3) . . ? C3 C2 C28 120.0(4) . . ? C4 C3 C2 121.6(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 117.5(4) . . ? C1 C6 C7 123.3(3) . . ? C5 C6 C7 118.9(4) . . ? C6 C7 C9 111.1(3) . . ? C6 C7 H7A 109.4 . . ? C9 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? C9 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C13 122.6(3) . . ? C9 C8 O2 118.9(3) . . ? C13 C8 O2 118.5(3) . . ? C10 C9 C8 118.5(4) . . ? C10 C9 C7 120.2(3) . . ? C8 C9 C7 121.2(3) . . ? C9 C10 C11 120.4(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.2(4) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 121.2(4) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C8 C13 C12 116.9(4) . . ? C8 C13 C14 122.7(3) . . ? C12 C13 C14 120.3(3) . . ? C13 C14 C15 111.1(3) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C20 C15 C16 118.2(4) . . ? C20 C15 C14 122.2(3) . . ? C16 C15 C14 119.5(3) . . ? C17 C16 C15 120.2(4) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 121.6(4) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C18 C19 C20 117.5(4) . . ? C18 C19 C21 120.4(4) . . ? C20 C19 C21 122.0(3) . . ? C15 C20 C19 121.8(3) . . ? C15 C20 O3 118.9(3) . . ? C19 C20 O3 119.2(3) . . ? C23 C21 C19 109.9(3) . . ? C23 C21 H21A 109.7 . . ? C19 C21 H21A 109.7 . . ? C23 C21 H21B 109.7 . . ? C19 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C27 C22 C23 123.7(3) . . ? C27 C22 O4 118.9(3) . . ? C23 C22 O4 117.4(4) . . ? C24 C23 C22 116.3(4) . . ? C24 C23 C21 120.9(4) . . ? C22 C23 C21 122.7(3) . . ? C25 C24 C23 121.1(4) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.7(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 120.9(4) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C22 C27 C26 117.0(4) . . ? C22 C27 C28 122.3(3) . . ? C26 C27 C28 120.6(4) . . ? C2 C28 C27 110.3(3) . . ? C2 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? C2 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? O1 C29 C30 116.3(3) . . ? O1 C29 H29A 108.2 . . ? C30 C29 H29A 108.2 . . ? O1 C29 H29B 108.2 . . ? C30 C29 H29B 108.2 . . ? H29A C29 H29B 107.4 . . ? O5 C30 O6 125.8(3) . . ? O5 C30 C29 123.0(3) . . ? O6 C30 C29 111.2(3) . . ? O2 C31 C32 111.0(3) . . ? O2 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? O2 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? O7 C32 O8 127.7(3) . . ? O7 C32 C31 114.1(3) . . ? O8 C32 C31 118.2(3) . . ? O7 C32 Na1 157.6(2) . . ? O8 C32 Na1 40.24(15) . . ? C31 C32 Na1 81.76(19) . . ? O3 C33 C34 108.8(3) . . ? O3 C33 H33A 109.9 . . ? C34 C33 H33A 109.9 . . ? O3 C33 H33B 109.9 . . ? C34 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O10 C34 O9 125.8(3) . . ? O10 C34 C33 116.5(3) . . ? O9 C34 C33 117.7(3) . . ? O4 C35 C36 111.1(3) . . ? O4 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? O4 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? O11 C36 O12 125.8(4) . . ? O11 C36 C35 116.0(3) . . ? O12 C36 C35 118.2(3) . . ? O11 C36 Na1 155.8(3) . . ? O12 C36 Na1 43.91(17) . . ? C35 C36 Na1 79.4(2) . . ? C1 O1 C29 115.7(3) . . ? C1 O1 Na1 128.39(19) . . ? C29 O1 Na1 111.6(2) . . ? C8 O2 C31 111.2(2) . . ? C8 O2 Na1 132.31(19) . . ? C31 O2 Na1 116.40(19) . . ? Co1 O1W H1A 106.2 . . ? Co1 O1W H1B 140.0 . . ? H1A O1W H1B 105.2 . . ? C20 O3 C33 111.8(2) . . ? C20 O3 Na1 124.88(19) . . ? C33 O3 Na1 123.08(19) . . ? Co1 O2W H2A 108.0 . . ? Co1 O2W H2B 82.0 . . ? H2A O2W H2B 80.2 . . ? C22 O4 C35 111.5(3) . . ? C22 O4 Na1 129.5(2) . . ? C35 O4 Na1 119.0(2) . . ? Co2 O3W H3A 113.6 . . ? Co2 O3W H3B 96.6 . . ? H3A O3W H3B 119.9 . . ? C30 O6 Co2 124.1(2) . 1_455 ? C32 O7 Co2 131.2(2) . 3_755 ? C32 O8 Co1 132.8(2) . . ? C32 O8 Na1 119.4(2) . . ? Co1 O8 Na1 93.23(9) . . ? C34 O9 Co2 126.2(2) . . ? C34 O10 Co1 127.1(2) . . ? C34 O10 Na1 102.3(2) . . ? Co1 O10 Na1 82.08(9) . . ? C36 O12 Co1 125.9(2) . . ? C36 O12 Na1 114.7(2) . . ? Co1 O12 Na1 91.70(9) . . ? O9W O6W O7W 111.1(18) 4_565 2_654 ? H4B O4W H4A 111(4) . . ? Co1 O13 Co2 116.77(11) . . ? Co1 O13 Co2 120.94(10) . 3_755 ? Co2 O13 Co2 96.81(9) . 3_755 ? Co1 O13 H13 101(3) . . ? Co2 O13 H13 97(3) . . ? Co2 O13 H13 123(3) 3_755 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 Co1 Na1 O4 152.00(11) . . . . ? O2W Co1 Na1 O4 -96.66(12) . . . . ? O10 Co1 Na1 O4 81.02(12) . . . . ? O12 Co1 Na1 O4 -25.80(12) . . . . ? O1W Co1 Na1 O4 19.96(13) . . . . ? O8 Co1 Na1 O4 -165.62(13) . . . . ? O13 Co1 Na1 O8 -42.38(14) . . . . ? O2W Co1 Na1 O8 68.96(13) . . . . ? O10 Co1 Na1 O8 -113.36(13) . . . . ? O12 Co1 Na1 O8 139.82(14) . . . . ? O1W Co1 Na1 O8 -174.42(13) . . . . ? O13 Co1 Na1 O2 -27.31(12) . . . . ? O2W Co1 Na1 O2 84.02(12) . . . . ? O10 Co1 Na1 O2 -98.29(12) . . . . ? O12 Co1 Na1 O2 154.89(12) . . . . ? O1W Co1 Na1 O2 -159.35(11) . . . . ? O8 Co1 Na1 O2 15.07(11) . . . . ? O13 Co1 Na1 O12 177.80(12) . . . . ? O2W Co1 Na1 O12 -70.87(13) . . . . ? O10 Co1 Na1 O12 106.82(13) . . . . ? O1W Co1 Na1 O12 45.76(13) . . . . ? O8 Co1 Na1 O12 -139.82(14) . . . . ? O13 Co1 Na1 O1 -118.87(11) . . . . ? O2W Co1 Na1 O1 -7.53(12) . . . . ? O10 Co1 Na1 O1 170.15(12) . . . . ? O12 Co1 Na1 O1 63.33(12) . . . . ? O1W Co1 Na1 O1 109.09(12) . . . . ? O8 Co1 Na1 O1 -76.49(12) . . . . ? O13 Co1 Na1 O3 58.20(12) . . . . ? O2W Co1 Na1 O3 169.54(11) . . . . ? O10 Co1 Na1 O3 -12.78(10) . . . . ? O12 Co1 Na1 O3 -119.60(12) . . . . ? O1W Co1 Na1 O3 -73.84(12) . . . . ? O8 Co1 Na1 O3 100.58(12) . . . . ? O13 Co1 Na1 O10 70.98(12) . . . . ? O2W Co1 Na1 O10 -177.68(12) . . . . ? O12 Co1 Na1 O10 -106.82(13) . . . . ? O1W Co1 Na1 O10 -61.06(13) . . . . ? O8 Co1 Na1 O10 113.36(13) . . . . ? O13 Co1 Na1 C32 -28.67(12) . . . . ? O2W Co1 Na1 C32 82.67(11) . . . . ? O10 Co1 Na1 C32 -99.65(11) . . . . ? O12 Co1 Na1 C32 153.53(12) . . . . ? O1W Co1 Na1 C32 -160.71(12) . . . . ? O8 Co1 Na1 C32 13.71(12) . . . . ? O13 Co1 Na1 C36 158.68(12) . . . . ? O2W Co1 Na1 C36 -89.98(12) . . . . ? O10 Co1 Na1 C36 87.70(12) . . . . ? O12 Co1 Na1 C36 -19.11(12) . . . . ? O1W Co1 Na1 C36 26.65(13) . . . . ? O8 Co1 Na1 C36 -158.94(13) . . . . ? O1 C1 C2 C3 176.6(3) . . . . ? C6 C1 C2 C3 -6.6(5) . . . . ? O1 C1 C2 C28 -5.8(5) . . . . ? C6 C1 C2 C28 170.9(3) . . . . ? C1 C2 C3 C4 2.6(6) . . . . ? C28 C2 C3 C4 -175.0(4) . . . . ? C2 C3 C4 C5 1.1(7) . . . . ? C3 C4 C5 C6 -1.1(7) . . . . ? O1 C1 C6 C5 -176.6(3) . . . . ? C2 C1 C6 C5 6.7(5) . . . . ? O1 C1 C6 C7 8.6(5) . . . . ? C2 C1 C6 C7 -168.0(3) . . . . ? C4 C5 C6 C1 -2.7(6) . . . . ? C4 C5 C6 C7 172.3(4) . . . . ? C1 C6 C7 C9 97.9(4) . . . . ? C5 C6 C7 C9 -76.7(4) . . . . ? C13 C8 C9 C10 -4.8(5) . . . . ? O2 C8 C9 C10 176.9(3) . . . . ? C13 C8 C9 C7 172.9(3) . . . . ? O2 C8 C9 C7 -5.4(5) . . . . ? C6 C7 C9 C10 80.6(4) . . . . ? C6 C7 C9 C8 -97.0(4) . . . . ? C8 C9 C10 C11 1.2(5) . . . . ? C7 C9 C10 C11 -176.5(3) . . . . ? C9 C10 C11 C12 2.7(6) . . . . ? C10 C11 C12 C13 -3.2(6) . . . . ? C9 C8 C13 C12 4.2(5) . . . . ? O2 C8 C13 C12 -177.4(3) . . . . ? C9 C8 C13 C14 -171.7(3) . . . . ? O2 C8 C13 C14 6.7(5) . . . . ? C11 C12 C13 C8 -0.2(5) . . . . ? C11 C12 C13 C14 175.8(3) . . . . ? C8 C13 C14 C15 94.6(4) . . . . ? C12 C13 C14 C15 -81.1(4) . . . . ? C13 C14 C15 C20 -98.2(4) . . . . ? C13 C14 C15 C16 77.8(4) . . . . ? C20 C15 C16 C17 1.7(5) . . . . ? C14 C15 C16 C17 -174.6(3) . . . . ? C15 C16 C17 C18 3.0(6) . . . . ? C16 C17 C18 C19 -2.3(6) . . . . ? C17 C18 C19 C20 -3.0(6) . . . . ? C17 C18 C19 C21 173.3(4) . . . . ? C16 C15 C20 C19 -7.2(5) . . . . ? C14 C15 C20 C19 168.9(3) . . . . ? C16 C15 C20 O3 174.7(3) . . . . ? C14 C15 C20 O3 -9.2(5) . . . . ? C18 C19 C20 C15 7.8(5) . . . . ? C21 C19 C20 C15 -168.4(3) . . . . ? C18 C19 C20 O3 -174.0(3) . . . . ? C21 C19 C20 O3 9.8(5) . . . . ? C18 C19 C21 C23 -75.5(4) . . . . ? C20 C19 C21 C23 100.6(4) . . . . ? C27 C22 C23 C24 -6.2(6) . . . . ? O4 C22 C23 C24 175.2(3) . . . . ? C27 C22 C23 C21 171.9(4) . . . . ? O4 C22 C23 C21 -6.8(5) . . . . ? C19 C21 C23 C24 77.9(5) . . . . ? C19 C21 C23 C22 -100.1(4) . . . . ? C22 C23 C24 C25 3.4(6) . . . . ? C21 C23 C24 C25 -174.7(4) . . . . ? C23 C24 C25 C26 -0.4(7) . . . . ? C24 C25 C26 C27 -0.3(7) . . . . ? C23 C22 C27 C26 5.6(6) . . . . ? O4 C22 C27 C26 -175.8(3) . . . . ? C23 C22 C27 C28 -170.2(4) . . . . ? O4 C22 C27 C28 8.4(6) . . . . ? C25 C26 C27 C22 -2.2(7) . . . . ? C25 C26 C27 C28 173.7(4) . . . . ? C1 C2 C28 C27 -97.7(4) . . . . ? C3 C2 C28 C27 79.8(4) . . . . ? C22 C27 C28 C2 95.1(4) . . . . ? C26 C27 C28 C2 -80.5(5) . . . . ? O1 C29 C30 O5 7.4(5) . . . . ? O1 C29 C30 O6 -173.5(3) . . . . ? O2 C31 C32 O7 164.3(3) . . . . ? O2 C31 C32 O8 -16.8(4) . . . . ? O2 C31 C32 Na1 0.8(3) . . . . ? O4 Na1 C32 O7 43.2(9) . . . . ? O8 Na1 C32 O7 67.3(6) . . . . ? O2 Na1 C32 O7 -137.7(7) . . . . ? O12 Na1 C32 O7 57.7(6) . . . . ? O1 Na1 C32 O7 149.1(6) . . . . ? O3 Na1 C32 O7 -60.6(6) . . . . ? O10 Na1 C32 O7 -0.8(6) . . . . ? C36 Na1 C32 O7 47.5(7) . . . . ? Co1 Na1 C32 O7 40.7(6) . . . . ? O4 Na1 C32 O8 -24.1(5) . . . . ? O2 Na1 C32 O8 155.0(3) . . . . ? O12 Na1 C32 O8 -9.6(2) . . . . ? O1 Na1 C32 O8 81.8(2) . . . . ? O3 Na1 C32 O8 -127.9(2) . . . . ? O10 Na1 C32 O8 -68.1(2) . . . . ? C36 Na1 C32 O8 -19.9(3) . . . . ? Co1 Na1 C32 O8 -26.7(2) . . . . ? O4 Na1 C32 C31 -179.6(4) . . . . ? O8 Na1 C32 C31 -155.6(4) . . . . ? O2 Na1 C32 C31 -0.59(19) . . . . ? O12 Na1 C32 C31 -165.2(2) . . . . ? O1 Na1 C32 C31 -73.8(2) . . . . ? O3 Na1 C32 C31 76.5(2) . . . . ? O10 Na1 C32 C31 136.4(2) . . . . ? C36 Na1 C32 C31 -175.44(19) . . . . ? Co1 Na1 C32 C31 177.8(2) . . . . ? O3 C33 C34 O10 43.2(4) . . . . ? O3 C33 C34 O9 -138.1(3) . . . . ? O4 C35 C36 O11 -160.5(3) . . . . ? O4 C35 C36 O12 21.0(5) . . . . ? O4 C35 C36 Na1 -0.3(3) . . . . ? O4 Na1 C36 O11 132.4(7) . . . . ? O8 Na1 C36 O11 -53.1(7) . . . . ? O2 Na1 C36 O11 -62.4(9) . . . . ? O12 Na1 C36 O11 -75.3(7) . . . . ? O1 Na1 C36 O11 -151.3(7) . . . . ? O3 Na1 C36 O11 54.5(7) . . . . ? O10 Na1 C36 O11 6.0(6) . . . . ? C32 Na1 C36 O11 -46.3(7) . . . . ? Co1 Na1 C36 O11 -39.3(6) . . . . ? O4 Na1 C36 O12 -152.3(3) . . . . ? O8 Na1 C36 O12 22.2(3) . . . . ? O2 Na1 C36 O12 13.0(6) . . . . ? O1 Na1 C36 O12 -76.0(3) . . . . ? O3 Na1 C36 O12 129.8(2) . . . . ? O10 Na1 C36 O12 81.3(3) . . . . ? C32 Na1 C36 O12 29.0(3) . . . . ? Co1 Na1 C36 O12 36.0(2) . . . . ? O4 Na1 C36 C35 0.2(2) . . . . ? O8 Na1 C36 C35 174.7(2) . . . . ? O2 Na1 C36 C35 165.5(4) . . . . ? O12 Na1 C36 C35 152.6(4) . . . . ? O1 Na1 C36 C35 76.6(2) . . . . ? O3 Na1 C36 C35 -77.6(3) . . . . ? O10 Na1 C36 C35 -126.1(3) . . . . ? C32 Na1 C36 C35 -178.4(2) . . . . ? Co1 Na1 C36 C35 -171.5(3) . . . . ? C2 C1 O1 C29 -116.1(3) . . . . ? C6 C1 O1 C29 67.1(4) . . . . ? C2 C1 O1 Na1 89.3(4) . . . . ? C6 C1 O1 Na1 -87.5(4) . . . . ? C30 C29 O1 C1 74.8(4) . . . . ? C30 C29 O1 Na1 -126.3(3) . . . . ? O4 Na1 O1 C1 -75.5(3) . . . . ? O8 Na1 O1 C1 138.6(3) . . . . ? O2 Na1 O1 C1 70.1(3) . . . . ? O12 Na1 O1 C1 -145.3(3) . . . . ? O3 Na1 O1 C1 4.3(4) . . . . ? O10 Na1 O1 C1 -168.4(3) . . . . ? C32 Na1 O1 C1 118.3(3) . . . . ? C36 Na1 O1 C1 -124.5(3) . . . . ? Co1 Na1 O1 C1 179.0(3) . . . . ? O4 Na1 O1 C29 129.0(2) . . . . ? O8 Na1 O1 C29 -16.8(2) . . . . ? O2 Na1 O1 C29 -85.4(2) . . . . ? O12 Na1 O1 C29 59.3(2) . . . . ? O3 Na1 O1 C29 -151.2(2) . . . . ? O10 Na1 O1 C29 36.1(3) . . . . ? C32 Na1 O1 C29 -37.2(2) . . . . ? C36 Na1 O1 C29 80.0(2) . . . . ? Co1 Na1 O1 C29 23.5(2) . . . . ? C9 C8 O2 C31 -94.9(4) . . . . ? C13 C8 O2 C31 86.6(4) . . . . ? C9 C8 O2 Na1 89.1(4) . . . . ? C13 C8 O2 Na1 -89.4(4) . . . . ? C32 C31 O2 C8 -177.9(3) . . . . ? C32 C31 O2 Na1 -1.2(4) . . . . ? O4 Na1 O2 C8 -3.8(4) . . . . ? O8 Na1 O2 C8 -174.4(3) . . . . ? O12 Na1 O2 C8 -156.6(3) . . . . ? O1 Na1 O2 C8 -74.2(3) . . . . ? O3 Na1 O2 C8 75.9(3) . . . . ? O10 Na1 O2 C8 132.7(3) . . . . ? C32 Na1 O2 C8 176.5(3) . . . . ? C36 Na1 O2 C8 -164.6(4) . . . . ? Co1 Na1 O2 C8 175.0(3) . . . . ? O4 Na1 O2 C31 -179.7(2) . . . . ? O8 Na1 O2 C31 9.7(2) . . . . ? O12 Na1 O2 C31 27.6(3) . . . . ? O1 Na1 O2 C31 109.9(2) . . . . ? O3 Na1 O2 C31 -100.0(2) . . . . ? O10 Na1 O2 C31 -43.1(3) . . . . ? C32 Na1 O2 C31 0.7(2) . . . . ? C36 Na1 O2 C31 19.5(6) . . . . ? Co1 Na1 O2 C31 -0.8(3) . . . . ? C15 C20 O3 C33 -80.1(4) . . . . ? C19 C20 O3 C33 101.7(4) . . . . ? C15 C20 O3 Na1 93.9(3) . . . . ? C19 C20 O3 Na1 -84.3(4) . . . . ? C34 C33 O3 C20 176.4(3) . . . . ? C34 C33 O3 Na1 2.3(4) . . . . ? O4 Na1 O3 C20 68.2(3) . . . . ? O8 Na1 O3 C20 -142.2(3) . . . . ? O2 Na1 O3 C20 -75.9(3) . . . . ? O12 Na1 O3 C20 135.6(3) . . . . ? O1 Na1 O3 C20 -9.5(4) . . . . ? O10 Na1 O3 C20 166.4(3) . . . . ? C32 Na1 O3 C20 -125.6(3) . . . . ? C36 Na1 O3 C20 117.2(3) . . . . ? Co1 Na1 O3 C20 175.5(2) . . . . ? O4 Na1 O3 C33 -118.5(3) . . . . ? O8 Na1 O3 C33 31.1(3) . . . . ? O2 Na1 O3 C33 97.4(3) . . . . ? O12 Na1 O3 C33 -51.1(3) . . . . ? O1 Na1 O3 C33 163.8(3) . . . . ? O10 Na1 O3 C33 -20.3(3) . . . . ? C32 Na1 O3 C33 47.7(3) . . . . ? C36 Na1 O3 C33 -69.5(3) . . . . ? Co1 Na1 O3 C33 -11.1(3) . . . . ? C27 C22 O4 C35 86.7(4) . . . . ? C23 C22 O4 C35 -94.6(4) . . . . ? C27 C22 O4 Na1 -93.2(4) . . . . ? C23 C22 O4 Na1 85.5(4) . . . . ? C36 C35 O4 C22 -179.4(3) . . . . ? C36 C35 O4 Na1 0.5(5) . . . . ? O8 Na1 O4 C22 169.8(3) . . . . ? O2 Na1 O4 C22 5.7(4) . . . . ? O12 Na1 O4 C22 169.2(3) . . . . ? O1 Na1 O4 C22 76.5(3) . . . . ? O3 Na1 O4 C22 -71.3(3) . . . . ? O10 Na1 O4 C22 -133.7(3) . . . . ? C32 Na1 O4 C22 -175.5(4) . . . . ? C36 Na1 O4 C22 179.6(3) . . . . ? Co1 Na1 O4 C22 -173.2(3) . . . . ? O8 Na1 O4 C35 -10.1(4) . . . . ? O2 Na1 O4 C35 -174.1(3) . . . . ? O12 Na1 O4 C35 -10.7(3) . . . . ? O1 Na1 O4 C35 -103.4(3) . . . . ? O3 Na1 O4 C35 108.8(3) . . . . ? O10 Na1 O4 C35 46.5(3) . . . . ? C32 Na1 O4 C35 4.6(6) . . . . ? C36 Na1 O4 C35 -0.3(3) . . . . ? Co1 Na1 O4 C35 7.0(3) . . . . ? O5 C30 O6 Co2 -32.5(5) . . . 1_455 ? C29 C30 O6 Co2 148.4(2) . . . 1_455 ? O8 C32 O7 Co2 -6.5(5) . . . 3_755 ? C31 C32 O7 Co2 172.2(2) . . . 3_755 ? Na1 C32 O7 Co2 -55.3(8) . . . 3_755 ? O7 C32 O8 Co1 -26.1(5) . . . . ? C31 C32 O8 Co1 155.3(2) . . . . ? Na1 C32 O8 Co1 127.6(4) . . . . ? O7 C32 O8 Na1 -153.7(3) . . . . ? C31 C32 O8 Na1 27.7(4) . . . . ? O13 Co1 O8 C32 14.6(3) . . . . ? O2W Co1 O8 C32 101.7(3) . . . . ? O10 Co1 O8 C32 -84.3(3) . . . . ? O12 Co1 O8 C32 -164.7(3) . . . . ? Na1 Co1 O8 C32 -136.2(3) . . . . ? O13 Co1 O8 Na1 150.86(9) . . . . ? O2W Co1 O8 Na1 -122.11(11) . . . . ? O10 Co1 O8 Na1 51.92(10) . . . . ? O12 Co1 O8 Na1 -28.46(10) . . . . ? O4 Na1 O8 C32 169.6(2) . . . . ? O2 Na1 O8 C32 -20.5(2) . . . . ? O12 Na1 O8 C32 170.1(2) . . . . ? O1 Na1 O8 C32 -101.5(2) . . . . ? O3 Na1 O8 C32 54.8(3) . . . . ? O10 Na1 O8 C32 104.4(2) . . . . ? C36 Na1 O8 C32 162.0(2) . . . . ? Co1 Na1 O8 C32 144.4(3) . . . . ? O4 Na1 O8 Co1 25.2(2) . . . . ? O2 Na1 O8 Co1 -164.86(11) . . . . ? O12 Na1 O8 Co1 25.76(9) . . . . ? O1 Na1 O8 Co1 114.06(10) . . . . ? O3 Na1 O8 Co1 -89.58(11) . . . . ? O10 Na1 O8 Co1 -40.02(8) . . . . ? C32 Na1 O8 Co1 -144.4(3) . . . . ? C36 Na1 O8 Co1 17.61(11) . . . . ? O10 C34 O9 Co2 21.6(5) . . . . ? C33 C34 O9 Co2 -157.1(2) . . . . ? O13 Co2 O9 C34 -56.1(3) . . . . ? O13 Co2 O9 C34 -139.5(3) 3_755 . . . ? O6 Co2 O9 C34 125.6(3) 1_655 . . . ? O3W Co2 O9 C34 38.8(3) . . . . ? O9 C34 O10 Co1 35.1(5) . . . . ? C33 C34 O10 Co1 -146.3(2) . . . . ? O9 C34 O10 Na1 124.4(3) . . . . ? C33 C34 O10 Na1 -57.0(3) . . . . ? O13 Co1 O10 C34 -37.0(3) . . . . ? O12 Co1 O10 C34 145.2(3) . . . . ? O1W Co1 O10 C34 -124.8(3) . . . . ? O8 Co1 O10 C34 58.2(3) . . . . ? Na1 Co1 O10 C34 99.5(3) . . . . ? O13 Co1 O10 Na1 -136.47(8) . . . . ? O12 Co1 O10 Na1 45.73(8) . . . . ? O1W Co1 O10 Na1 135.74(9) . . . . ? O8 Co1 O10 Na1 -41.32(8) . . . . ? O4 Na1 O10 C34 126.0(2) . . . . ? O8 Na1 O10 C34 -84.7(2) . . . . ? O2 Na1 O10 C34 -29.7(2) . . . . ? O12 Na1 O10 C34 -171.3(2) . . . . ? O1 Na1 O10 C34 -145.0(2) . . . . ? O3 Na1 O10 C34 39.5(2) . . . . ? C32 Na1 O10 C34 -64.0(2) . . . . ? C36 Na1 O10 C34 164.8(2) . . . . ? Co1 Na1 O10 C34 -126.4(2) . . . . ? O4 Na1 O10 Co1 -107.65(10) . . . . ? O8 Na1 O10 Co1 41.64(9) . . . . ? O2 Na1 O10 Co1 96.71(10) . . . . ? O12 Na1 O10 Co1 -44.89(8) . . . . ? O1 Na1 O10 Co1 -18.6(2) . . . . ? O3 Na1 O10 Co1 165.85(11) . . . . ? C32 Na1 O10 Co1 62.40(9) . . . . ? C36 Na1 O10 Co1 -68.86(10) . . . . ? O11 C36 O12 Co1 38.8(5) . . . . ? C35 C36 O12 Co1 -142.9(3) . . . . ? Na1 C36 O12 Co1 -111.9(3) . . . . ? O11 C36 O12 Na1 150.7(3) . . . . ? C35 C36 O12 Na1 -30.9(4) . . . . ? O2W Co1 O12 C36 -116.5(3) . . . . ? O10 Co1 O12 C36 66.8(3) . . . . ? O1W Co1 O12 C36 -22.6(3) . . . . ? O8 Co1 O12 C36 150.0(3) . . . . ? Na1 Co1 O12 C36 122.5(3) . . . . ? O2W Co1 O12 Na1 120.95(10) . . . . ? O10 Co1 O12 Na1 -55.76(9) . . . . ? O1W Co1 O12 Na1 -145.16(10) . . . . ? O8 Co1 O12 Na1 27.47(9) . . . . ? O4 Na1 O12 C36 22.4(2) . . . . ? O8 Na1 O12 C36 -157.2(3) . . . . ? O2 Na1 O12 C36 -174.5(2) . . . . ? O1 Na1 O12 C36 105.0(3) . . . . ? O3 Na1 O12 C36 -56.9(3) . . . . ? O10 Na1 O12 C36 -87.7(3) . . . . ? C32 Na1 O12 C36 -153.8(2) . . . . ? Co1 Na1 O12 C36 -131.3(3) . . . . ? O4 Na1 O12 Co1 153.69(12) . . . . ? O8 Na1 O12 Co1 -25.99(9) . . . . ? O2 Na1 O12 Co1 -43.2(2) . . . . ? O1 Na1 O12 Co1 -123.70(9) . . . . ? O3 Na1 O12 Co1 74.34(11) . . . . ? O10 Na1 O12 Co1 43.54(8) . . . . ? C32 Na1 O12 Co1 -22.56(10) . . . . ? C36 Na1 O12 Co1 131.3(3) . . . . ? O2W Co1 O13 Co2 172.46(13) . . . . ? O10 Co1 O13 Co2 -10.59(13) . . . . ? O1W Co1 O13 Co2 78.44(12) . . . . ? O8 Co1 O13 Co2 -94.14(12) . . . . ? Na1 Co1 O13 Co2 -65.21(14) . . . . ? O2W Co1 O13 Co2 -70.32(14) . . . 3_755 ? O10 Co1 O13 Co2 106.63(13) . . . 3_755 ? O1W Co1 O13 Co2 -164.34(13) . . . 3_755 ? O8 Co1 O13 Co2 23.08(13) . . . 3_755 ? Na1 Co1 O13 Co2 52.00(16) . . . 3_755 ? O13 Co2 O13 Co1 129.81(15) 3_755 . . . ? O7 Co2 O13 Co1 -135.03(12) 3_755 . . . ? O9 Co2 O13 Co1 38.18(12) . . . . ? O3W Co2 O13 Co1 -51.62(12) . . . . ? O13 Co2 O13 Co2 0.0 3_755 . . 3_755 ? O7 Co2 O13 Co2 95.15(10) 3_755 . . 3_755 ? O9 Co2 O13 Co2 -91.63(10) . . . 3_755 ? O3W Co2 O13 Co2 178.57(9) . . . 3_755 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13 O7W 0.813(19) 2.34(2) 3.147(10) 174(4) . O1W H1A O11 0.86 1.83 2.650(4) 156.5 . O1W H1B O7W 0.70 2.21 2.754(10) 135.6 . O2W H2A O6 0.97 1.82 2.775(4) 168.3 3_655 O2W H2B O8 0.82 2.54 3.076(4) 124.0 . O3W H3A O8W 0.85 2.02 2.839(6) 162.2 3_755 O3W H3B O5 0.92 1.84 2.726(4) 160.2 1_655 O4W H4B O6 0.873(11) 2.04(3) 2.876(4) 160(6) . _diffrn_measured_fraction_theta_max 0.841 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.948 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.097 #===== data_10 _database_code_depnum_ccdc_archive 'CCDC 879392' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H56 Cu3 Na2 O24' _chemical_formula_weight 1541.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.724(3) _cell_length_b 18.516(5) _cell_length_c 17.637(6) _cell_angle_alpha 90 _cell_angle_beta 99.769(5) _cell_angle_gamma 90 _cell_volume 3129.5(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1578 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7683 _exptl_absorpt_correction_T_max 0.8164 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20455 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5715 _reflns_number_gt 3247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5715 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.821 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.40965(4) -0.05333(2) 0.00376(2) 0.02447(13) Uani 1 1 d . . . Cu2 Cu -1.0000 0.0000 0.0000 0.03564(19) Uani 1 2 d S . . Na1 Na -0.99775(14) -0.00879(7) 0.18287(7) 0.0311(3) Uani 1 1 d . . . C1 C -0.8486(4) -0.20318(19) 0.2609(2) 0.0287(9) Uani 1 1 d . . . H1A H -0.8747 -0.1924 0.2066 0.034 Uiso 1 1 calc R . . H1B H -0.8045 -0.2503 0.2659 0.034 Uiso 1 1 calc R . . C2 C -1.0852(4) -0.15638(19) 0.2749(2) 0.0260(8) Uani 1 1 d . . . C3 C -0.9780(4) -0.20385(19) 0.2988(2) 0.0271(9) Uani 1 1 d . . . C4 C -0.9887(4) -0.24781(19) 0.3614(2) 0.0366(10) Uani 1 1 d . . . H4 H -0.9193 -0.2815 0.3781 0.044 Uiso 1 1 calc R . . C5 C -1.1017(4) -0.2417(2) 0.3990(2) 0.0406(11) Uani 1 1 d . . . H5 H -1.1110 -0.2733 0.4388 0.049 Uiso 1 1 calc R . . C6 C -1.2001(4) -0.1895(2) 0.3780(2) 0.0407(10) Uani 1 1 d . . . H6 H -1.2728 -0.1843 0.4057 0.049 Uiso 1 1 calc R . . C7 C -1.1934(4) -0.1439(2) 0.3162(2) 0.0306(9) Uani 1 1 d . . . C8 C -1.2889(4) -0.0789(2) 0.2990(2) 0.0339(10) Uani 1 1 d . . . H8A H -1.3800 -0.0903 0.3113 0.041 Uiso 1 1 calc R . . H8B H -1.3004 -0.0675 0.2446 0.041 Uiso 1 1 calc R . . C9 C -1.1795(4) 0.0479(2) 0.3127(2) 0.0299(9) Uani 1 1 d . . . C10 C -1.2280(4) -0.0136(2) 0.3462(2) 0.0307(9) Uani 1 1 d . . . C11 C -1.2174(4) -0.0141(2) 0.4253(2) 0.0404(10) Uani 1 1 d . . . H11 H -1.2489 -0.0544 0.4488 0.049 Uiso 1 1 calc R . . C12 C -1.1624(4) 0.0425(3) 0.4700(2) 0.0468(11) Uani 1 1 d . . . H12 H -1.1576 0.0408 0.5230 0.056 Uiso 1 1 calc R . . C13 C -1.1144(4) 0.1016(2) 0.4365(2) 0.0463(11) Uani 1 1 d . . . H13 H -1.0774 0.1401 0.4673 0.056 Uiso 1 1 calc R . . C14 C -1.1193(4) 0.1058(2) 0.3570(2) 0.0344(9) Uani 1 1 d . . . C15 C -1.0529(4) 0.1702(2) 0.3234(2) 0.0414(10) Uani 1 1 d . . . H15A H -1.0864 0.1725 0.2685 0.050 Uiso 1 1 calc R . . H15B H -1.0808 0.2143 0.3463 0.050 Uiso 1 1 calc R . . C16 C -0.8262(4) 0.12476(19) 0.2904(2) 0.0308(9) Uani 1 1 d . . . C17 C -0.8953(4) 0.1650(2) 0.3379(2) 0.0353(10) Uani 1 1 d . . . C18 C -0.8127(5) 0.1969(2) 0.4024(2) 0.0429(11) Uani 1 1 d . . . H18 H -0.8550 0.2259 0.4348 0.051 Uiso 1 1 calc R . . C19 C -0.6722(5) 0.1862(2) 0.4183(2) 0.0441(11) Uani 1 1 d . . . H19 H -0.6191 0.2099 0.4597 0.053 Uiso 1 1 calc R . . C20 C -0.6089(5) 0.1406(2) 0.3737(2) 0.0443(11) Uani 1 1 d . . . H20 H -0.5134 0.1323 0.3864 0.053 Uiso 1 1 calc R . . C21 C -0.6849(4) 0.1063(2) 0.3094(2) 0.0330(10) Uani 1 1 d . . . C22 C -0.6232(4) 0.0476(2) 0.2673(2) 0.0358(9) Uani 1 1 d . . . H22A H -0.5242 0.0562 0.2696 0.043 Uiso 1 1 calc R . . H22B H -0.6673 0.0474 0.2137 0.043 Uiso 1 1 calc R . . C23 C -0.7204(3) -0.08152(19) 0.26348(19) 0.0248(8) Uani 1 1 d . . . C24 C -0.6452(4) -0.0257(2) 0.3038(2) 0.0300(9) Uani 1 1 d . . . C25 C -0.5886(4) -0.0377(2) 0.3801(2) 0.0363(10) Uani 1 1 d . . . H25 H -0.5387 -0.0008 0.4083 0.044 Uiso 1 1 calc R . . C26 C -0.6041(4) -0.1023(2) 0.4151(2) 0.0430(11) Uani 1 1 d . . . H26 H -0.5608 -0.1101 0.4656 0.052 Uiso 1 1 calc R . . C27 C -0.6840(4) -0.1560(2) 0.3754(2) 0.0365(10) Uani 1 1 d . . . H27 H -0.6959 -0.1995 0.3999 0.044 Uiso 1 1 calc R . . C28 C -0.7469(4) -0.14625(19) 0.2994(2) 0.0272(9) Uani 1 1 d . . . C29 C -1.1602(4) -0.1555(2) 0.1409(2) 0.0344(9) Uani 1 1 d . . . H29A H -1.2578 -0.1588 0.1460 0.041 Uiso 1 1 calc R . . H29B H -1.1240 -0.2042 0.1393 0.041 Uiso 1 1 calc R . . C30 C -1.1477(4) -0.11698(19) 0.0672(2) 0.0277(9) Uani 1 1 d . . . C31 C -1.2854(4) 0.0931(2) 0.1893(2) 0.0306(9) Uani 1 1 d . . . H31A H -1.2390 0.1348 0.1719 0.037 Uiso 1 1 calc R . . H31B H -1.3495 0.1103 0.2219 0.037 Uiso 1 1 calc R . . C32 C -1.3667(3) 0.0550(2) 0.12065(18) 0.0232(8) Uani 1 1 d . . . C33 C -0.9069(4) 0.1549(2) 0.1604(2) 0.0430(11) Uani 1 1 d . . . H33A H -0.8138 0.1626 0.1490 0.052 Uiso 1 1 calc R . . H33B H -0.9387 0.2002 0.1791 0.052 Uiso 1 1 calc R . . C34 C -1.0025(4) 0.1335(2) 0.0883(2) 0.0333(9) Uani 1 1 d . . . C35 C -0.7202(4) -0.11512(18) 0.13243(19) 0.0279(9) Uani 1 1 d . . . H35A H -0.7959 -0.1403 0.1002 0.034 Uiso 1 1 calc R . . H35B H -0.6591 -0.1511 0.1605 0.034 Uiso 1 1 calc R . . C36 C -0.6400(4) -0.0722(2) 0.0824(2) 0.0271(9) Uani 1 1 d . . . O1 O -1.0842(2) -0.11806(12) 0.20677(12) 0.0259(6) Uani 1 1 d . . . O2 O -1.1835(2) 0.04727(13) 0.23334(12) 0.0287(6) Uani 1 1 d . . . O3 O -0.9011(3) 0.10025(13) 0.22045(13) 0.0332(6) Uani 1 1 d . . . O4 O -0.7768(2) -0.07033(12) 0.18634(12) 0.0265(6) Uani 1 1 d . . . O5 O -1.0443(2) -0.07446(13) 0.07052(13) 0.0306(6) Uani 1 1 d . . . O6 O -1.2400(2) -0.12934(13) 0.01070(13) 0.0311(6) Uani 1 1 d . . . O7 O -1.3216(2) -0.00312(13) 0.09937(13) 0.0309(6) Uani 1 1 d . . . O8 O -1.4739(3) 0.08739(13) 0.08958(14) 0.0349(6) Uani 1 1 d . . . O9 O -1.0206(3) 0.06537(13) 0.08004(13) 0.0387(7) Uani 1 1 d . . . O10 O -1.0529(3) 0.18026(15) 0.04438(16) 0.0558(8) Uani 1 1 d . . . O11 O -0.6867(2) -0.01184(13) 0.05913(13) 0.0343(6) Uani 1 1 d . . . O12 O -0.5323(3) -0.10234(14) 0.06577(14) 0.0377(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0225(2) 0.0248(2) 0.0253(2) 0.0002(2) 0.00195(17) 0.0020(2) Cu2 0.0497(5) 0.0316(4) 0.0257(4) -0.0009(3) 0.0065(3) -0.0063(3) Na1 0.0373(9) 0.0263(8) 0.0303(8) 0.0006(6) 0.0073(6) -0.0029(7) C1 0.034(2) 0.022(2) 0.031(2) 0.0064(17) 0.0070(17) 0.0075(17) C2 0.031(2) 0.022(2) 0.026(2) 0.0014(16) 0.0074(17) -0.0062(17) C3 0.032(2) 0.020(2) 0.029(2) 0.0001(17) 0.0070(17) -0.0030(17) C4 0.053(3) 0.023(2) 0.035(2) 0.0046(19) 0.009(2) 0.0056(19) C5 0.067(3) 0.026(2) 0.033(2) 0.0101(18) 0.021(2) -0.003(2) C6 0.046(3) 0.040(3) 0.042(3) -0.002(2) 0.025(2) -0.008(2) C7 0.028(2) 0.032(2) 0.033(2) -0.0032(19) 0.0088(17) -0.0068(18) C8 0.027(2) 0.040(2) 0.036(2) -0.0002(18) 0.0092(18) 0.0007(18) C9 0.027(2) 0.037(2) 0.025(2) -0.0025(19) 0.0029(16) 0.0117(19) C10 0.019(2) 0.040(3) 0.033(2) -0.0025(19) 0.0067(17) 0.0098(18) C11 0.035(2) 0.048(3) 0.041(3) 0.004(2) 0.013(2) 0.004(2) C12 0.052(3) 0.065(3) 0.026(2) -0.004(2) 0.011(2) 0.003(2) C13 0.048(3) 0.053(3) 0.036(3) -0.021(2) 0.003(2) 0.003(2) C14 0.035(2) 0.036(2) 0.032(2) -0.0073(19) 0.0048(18) 0.0111(19) C15 0.055(3) 0.031(2) 0.035(2) -0.0127(19) 0.000(2) 0.004(2) C16 0.045(3) 0.023(2) 0.022(2) -0.0029(17) 0.0020(18) -0.0145(19) C17 0.047(3) 0.028(2) 0.028(2) 0.0023(18) -0.0003(19) -0.0036(19) C18 0.068(3) 0.031(2) 0.028(2) -0.0048(18) 0.002(2) -0.009(2) C19 0.059(3) 0.039(3) 0.026(2) -0.002(2) -0.013(2) -0.013(2) C20 0.047(3) 0.043(3) 0.038(3) 0.004(2) -0.006(2) -0.011(2) C21 0.041(3) 0.029(2) 0.026(2) 0.0042(18) -0.0014(18) -0.0124(19) C22 0.031(2) 0.040(2) 0.037(2) -0.005(2) 0.0055(17) -0.010(2) C23 0.0173(19) 0.032(2) 0.026(2) -0.0013(17) 0.0073(16) 0.0087(16) C24 0.021(2) 0.037(2) 0.034(2) -0.0025(18) 0.0077(17) 0.0041(17) C25 0.031(2) 0.044(3) 0.034(2) -0.008(2) 0.0059(18) 0.0004(19) C26 0.038(3) 0.060(3) 0.028(2) 0.005(2) -0.0017(19) 0.013(2) C27 0.042(3) 0.034(2) 0.034(2) 0.0051(19) 0.0066(19) 0.011(2) C28 0.028(2) 0.027(2) 0.028(2) -0.0015(17) 0.0097(17) 0.0079(17) C29 0.037(2) 0.030(2) 0.035(2) 0.0005(18) 0.0030(18) -0.0049(19) C30 0.031(2) 0.026(2) 0.027(2) -0.0042(17) 0.0080(19) 0.0092(18) C31 0.026(2) 0.030(2) 0.033(2) 0.0008(18) -0.0015(17) 0.0015(17) C32 0.025(2) 0.021(2) 0.0239(19) -0.0008(17) 0.0068(16) -0.0043(18) C33 0.060(3) 0.032(2) 0.034(2) 0.003(2) 0.000(2) -0.014(2) C34 0.044(3) 0.031(3) 0.027(2) -0.001(2) 0.0122(18) 0.001(2) C35 0.033(2) 0.023(2) 0.029(2) 0.0002(17) 0.0095(17) 0.0012(17) C36 0.027(2) 0.028(2) 0.026(2) -0.0072(17) 0.0027(17) -0.0069(18) O1 0.0297(15) 0.0235(14) 0.0239(14) 0.0063(11) 0.0024(11) -0.0014(11) O2 0.0291(14) 0.0318(14) 0.0240(14) -0.0048(12) 0.0006(10) 0.0079(12) O3 0.0456(17) 0.0268(15) 0.0238(14) -0.0028(12) -0.0038(12) -0.0093(12) O4 0.0262(13) 0.0273(15) 0.0261(14) 0.0011(11) 0.0048(11) 0.0035(11) O5 0.0305(15) 0.0364(17) 0.0253(14) 0.0008(11) 0.0058(11) -0.0065(12) O6 0.0277(15) 0.0326(15) 0.0295(15) -0.0061(12) -0.0054(12) 0.0084(12) O7 0.0314(15) 0.0332(16) 0.0259(14) -0.0071(12) -0.0014(11) 0.0080(12) O8 0.0311(16) 0.0269(15) 0.0403(16) -0.0090(12) -0.0128(12) 0.0072(12) O9 0.0645(19) 0.0271(17) 0.0253(14) -0.0037(12) 0.0102(12) -0.0082(14) O10 0.081(2) 0.0384(18) 0.0438(19) 0.0071(15) -0.0025(16) 0.0131(16) O11 0.0405(17) 0.0302(16) 0.0354(16) 0.0102(12) 0.0150(12) 0.0052(13) O12 0.0351(16) 0.0326(16) 0.0492(17) 0.0109(13) 0.0182(13) 0.0024(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O8 1.938(2) 3_355 ? Cu1 O12 1.971(2) . ? Cu1 O11 1.979(2) 3_455 ? Cu1 O7 1.988(2) 1_655 ? Cu1 O6 2.156(2) 1_655 ? Cu1 Cu1 2.6317(10) 3_455 ? Cu2 O9 1.896(2) 3_355 ? Cu2 O9 1.896(2) . ? Cu2 O5 1.953(2) 3_355 ? Cu2 O5 1.953(2) . ? Cu2 Na1 3.2258(17) 3_355 ? Cu2 Na1 3.2258(17) . ? Na1 O9 2.255(3) . ? Na1 O1 2.258(3) . ? Na1 O3 2.278(3) . ? Na1 O5 2.303(3) . ? Na1 O2 2.383(3) . ? Na1 O4 2.424(3) . ? Na1 C30 3.049(4) . ? Na1 C34 3.115(4) . ? C1 C3 1.522(5) . ? C1 C28 1.524(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.374(5) . ? C2 O1 1.396(4) . ? C2 C7 1.397(5) . ? C3 C4 1.389(5) . ? C4 C5 1.381(5) . ? C4 H4 0.9300 . ? C5 C6 1.367(5) . ? C5 H5 0.9300 . ? C6 C7 1.388(5) . ? C6 H6 0.9300 . ? C7 C8 1.519(5) . ? C8 C10 1.530(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.394(4) . ? C9 C14 1.395(5) . ? C9 C10 1.400(5) . ? C10 C11 1.381(5) . ? C11 C12 1.366(6) . ? C11 H11 0.9300 . ? C12 C13 1.363(6) . ? C12 H12 0.9300 . ? C13 C14 1.397(5) . ? C13 H13 0.9300 . ? C14 C15 1.522(5) . ? C15 C17 1.514(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.378(5) . ? C16 O3 1.397(4) . ? C16 C21 1.401(5) . ? C17 C18 1.405(5) . ? C18 C19 1.362(6) . ? C18 H18 0.9300 . ? C19 C20 1.370(5) . ? C19 H19 0.9300 . ? C20 C21 1.397(5) . ? C20 H20 0.9300 . ? C21 C22 1.498(5) . ? C22 C24 1.532(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.390(5) . ? C23 O4 1.394(4) . ? C23 C28 1.400(5) . ? C24 C25 1.382(5) . ? C25 C26 1.367(5) . ? C25 H25 0.9300 . ? C26 C27 1.378(5) . ? C26 H26 0.9300 . ? C27 C28 1.387(5) . ? C27 H27 0.9300 . ? C29 O1 1.443(4) . ? C29 C30 1.507(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O6 1.243(4) . ? C30 O5 1.271(4) . ? C31 O2 1.430(4) . ? C31 C32 1.505(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O7 1.244(4) . ? C32 O8 1.246(4) . ? C33 O3 1.459(4) . ? C33 C34 1.497(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O10 1.208(4) . ? C34 O9 1.279(4) . ? C35 O4 1.439(4) . ? C35 C36 1.501(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O11 1.249(4) . ? C36 O12 1.264(4) . ? O6 Cu1 2.156(2) 1_455 ? O7 Cu1 1.988(2) 1_455 ? O8 Cu1 1.938(2) 3_355 ? O11 Cu1 1.979(2) 3_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Cu1 O12 90.01(11) 3_355 . ? O8 Cu1 O11 89.20(11) 3_355 3_455 ? O12 Cu1 O11 168.60(10) . 3_455 ? O8 Cu1 O7 168.01(10) 3_355 1_655 ? O12 Cu1 O7 87.64(11) . 1_655 ? O11 Cu1 O7 90.78(10) 3_455 1_655 ? O8 Cu1 O6 99.60(10) 3_355 1_655 ? O12 Cu1 O6 101.38(10) . 1_655 ? O11 Cu1 O6 89.97(10) 3_455 1_655 ? O7 Cu1 O6 92.39(9) 1_655 1_655 ? O8 Cu1 Cu1 84.98(7) 3_355 3_455 ? O12 Cu1 Cu1 84.93(8) . 3_455 ? O11 Cu1 Cu1 83.66(7) 3_455 3_455 ? O7 Cu1 Cu1 83.09(7) 1_655 3_455 ? O6 Cu1 Cu1 172.12(7) 1_655 3_455 ? O9 Cu2 O9 180.0(2) 3_355 . ? O9 Cu2 O5 85.06(10) 3_355 3_355 ? O9 Cu2 O5 94.94(10) . 3_355 ? O9 Cu2 O5 94.94(10) 3_355 . ? O9 Cu2 O5 85.06(10) . . ? O5 Cu2 O5 180.00(18) 3_355 . ? O9 Cu2 Na1 43.22(8) 3_355 3_355 ? O9 Cu2 Na1 136.78(8) . 3_355 ? O5 Cu2 Na1 44.97(7) 3_355 3_355 ? O5 Cu2 Na1 135.03(7) . 3_355 ? O9 Cu2 Na1 136.78(8) 3_355 . ? O9 Cu2 Na1 43.22(8) . . ? O5 Cu2 Na1 135.03(7) 3_355 . ? O5 Cu2 Na1 44.97(7) . . ? Na1 Cu2 Na1 180.00(5) 3_355 . ? O9 Na1 O1 134.95(11) . . ? O9 Na1 O3 70.97(9) . . ? O1 Na1 O3 152.66(10) . . ? O9 Na1 O5 69.60(9) . . ? O1 Na1 O5 70.28(9) . . ? O3 Na1 O5 136.83(10) . . ? O9 Na1 O2 93.30(10) . . ? O1 Na1 O2 89.47(9) . . ? O3 Na1 O2 78.85(9) . . ? O5 Na1 O2 120.05(10) . . ? O9 Na1 O4 105.82(10) . . ? O1 Na1 O4 86.02(9) . . ? O3 Na1 O4 95.11(10) . . ? O5 Na1 O4 79.47(9) . . ? O2 Na1 O4 156.97(10) . . ? O9 Na1 C30 83.74(10) . . ? O1 Na1 C30 52.07(9) . . ? O3 Na1 C30 154.71(10) . . ? O5 Na1 C30 22.39(8) . . ? O2 Na1 C30 103.28(10) . . ? O4 Na1 C30 91.67(9) . . ? O9 Na1 C34 20.58(9) . . ? O1 Na1 C34 152.35(11) . . ? O3 Na1 C34 51.24(9) . . ? O5 Na1 C34 90.16(10) . . ? O2 Na1 C34 83.58(10) . . ? O4 Na1 C34 110.10(10) . . ? C30 Na1 C34 103.61(11) . . ? O9 Na1 Cu2 35.14(6) . . ? O1 Na1 Cu2 106.99(7) . . ? O3 Na1 Cu2 100.29(7) . . ? O5 Na1 Cu2 36.82(6) . . ? O2 Na1 Cu2 118.33(7) . . ? O4 Na1 Cu2 84.52(6) . . ? C30 Na1 Cu2 56.11(7) . . ? C34 Na1 Cu2 54.88(7) . . ? C3 C1 C28 109.4(3) . . ? C3 C1 H1A 109.8 . . ? C28 C1 H1A 109.8 . . ? C3 C1 H1B 109.8 . . ? C28 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? C3 C2 O1 118.3(3) . . ? C3 C2 C7 123.0(3) . . ? O1 C2 C7 118.8(3) . . ? C2 C3 C4 117.6(3) . . ? C2 C3 C1 120.0(3) . . ? C4 C3 C1 122.2(3) . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 121.2(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C2 116.7(3) . . ? C6 C7 C8 122.0(3) . . ? C2 C7 C8 121.0(3) . . ? C7 C8 C10 110.6(3) . . ? C7 C8 H8A 109.5 . . ? C10 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C10 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O2 C9 C14 120.3(3) . . ? O2 C9 C10 117.5(3) . . ? C14 C9 C10 121.9(3) . . ? C11 C10 C9 117.3(4) . . ? C11 C10 C8 119.9(4) . . ? C9 C10 C8 122.8(3) . . ? C12 C11 C10 122.1(4) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C13 C12 C11 119.7(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 121.6(4) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C9 C14 C13 117.3(4) . . ? C9 C14 C15 123.4(3) . . ? C13 C14 C15 119.3(4) . . ? C17 C15 C14 111.7(3) . . ? C17 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C17 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C17 C16 O3 118.5(3) . . ? C17 C16 C21 123.1(3) . . ? O3 C16 C21 118.3(3) . . ? C16 C17 C18 116.7(4) . . ? C16 C17 C15 121.0(3) . . ? C18 C17 C15 122.2(4) . . ? C19 C18 C17 121.4(4) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 121.3(4) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C16 116.5(4) . . ? C20 C21 C22 122.1(4) . . ? C16 C21 C22 121.2(3) . . ? C21 C22 C24 109.8(3) . . ? C21 C22 H22A 109.7 . . ? C24 C22 H22A 109.7 . . ? C21 C22 H22B 109.7 . . ? C24 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C24 C23 O4 118.4(3) . . ? C24 C23 C28 121.7(3) . . ? O4 C23 C28 119.8(3) . . ? C25 C24 C23 117.9(3) . . ? C25 C24 C22 119.3(3) . . ? C23 C24 C22 122.8(3) . . ? C26 C25 C24 121.5(4) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C25 C26 C27 119.9(4) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C28 121.0(4) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C27 C28 C23 117.6(3) . . ? C27 C28 C1 119.1(3) . . ? C23 C28 C1 123.1(3) . . ? O1 C29 C30 111.2(3) . . ? O1 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? O1 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? O6 C30 O5 127.6(3) . . ? O6 C30 C29 116.8(3) . . ? O5 C30 C29 115.6(3) . . ? O6 C30 Na1 148.8(2) . . ? O5 C30 Na1 43.68(16) . . ? C29 C30 Na1 80.3(2) . . ? O2 C31 C32 112.3(3) . . ? O2 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? O2 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.9 . . ? O7 C32 O8 126.6(3) . . ? O7 C32 C31 119.0(3) . . ? O8 C32 C31 114.4(3) . . ? O3 C33 C34 112.0(3) . . ? O3 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? O3 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? O10 C34 O9 126.9(4) . . ? O10 C34 C33 118.7(4) . . ? O9 C34 C33 114.3(3) . . ? O10 C34 Na1 156.5(3) . . ? O9 C34 Na1 38.31(17) . . ? C33 C34 Na1 79.5(2) . . ? O4 C35 C36 112.2(3) . . ? O4 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? O4 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? O11 C36 O12 126.0(3) . . ? O11 C36 C35 118.1(3) . . ? O12 C36 C35 115.9(3) . . ? C2 O1 C29 111.7(2) . . ? C2 O1 Na1 132.3(2) . . ? C29 O1 Na1 115.86(19) . . ? C9 O2 C31 116.1(3) . . ? C9 O2 Na1 119.00(19) . . ? C31 O2 Na1 123.7(2) . . ? C16 O3 C33 111.4(3) . . ? C16 O3 Na1 132.2(2) . . ? C33 O3 Na1 116.2(2) . . ? C23 O4 C35 115.3(2) . . ? C23 O4 Na1 107.17(17) . . ? C35 O4 Na1 133.7(2) . . ? C30 O5 Cu2 131.7(2) . . ? C30 O5 Na1 113.9(2) . . ? Cu2 O5 Na1 98.21(11) . . ? C30 O6 Cu1 111.5(2) . 1_455 ? C32 O7 Cu1 122.5(2) . 1_455 ? C32 O8 Cu1 122.8(2) . 3_355 ? C34 O9 Cu2 133.2(2) . . ? C34 O9 Na1 121.1(2) . . ? Cu2 O9 Na1 101.63(12) . . ? C36 O11 Cu1 123.3(2) . 3_455 ? C36 O12 Cu1 121.9(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Cu2 Na1 O9 180.0 3_355 . . . ? O5 Cu2 Na1 O9 27.48(16) 3_355 . . . ? O5 Cu2 Na1 O9 -152.52(16) . . . . ? Na1 Cu2 Na1 O9 179(100) 3_355 . . . ? O9 Cu2 Na1 O1 -31.87(15) 3_355 . . . ? O9 Cu2 Na1 O1 148.13(15) . . . . ? O5 Cu2 Na1 O1 175.61(11) 3_355 . . . ? O5 Cu2 Na1 O1 -4.39(11) . . . . ? Na1 Cu2 Na1 O1 -32(100) 3_355 . . . ? O9 Cu2 Na1 O3 146.48(14) 3_355 . . . ? O9 Cu2 Na1 O3 -33.52(14) . . . . ? O5 Cu2 Na1 O3 -6.04(13) 3_355 . . . ? O5 Cu2 Na1 O3 173.96(13) . . . . ? Na1 Cu2 Na1 O3 146(100) 3_355 . . . ? O9 Cu2 Na1 O5 -27.48(16) 3_355 . . . ? O9 Cu2 Na1 O5 152.52(16) . . . . ? O5 Cu2 Na1 O5 180.0 3_355 . . . ? Na1 Cu2 Na1 O5 -28(100) 3_355 . . . ? O9 Cu2 Na1 O2 -130.72(14) 3_355 . . . ? O9 Cu2 Na1 O2 49.28(14) . . . . ? O5 Cu2 Na1 O2 76.76(13) 3_355 . . . ? O5 Cu2 Na1 O2 -103.24(13) . . . . ? Na1 Cu2 Na1 O2 -131(100) 3_355 . . . ? O9 Cu2 Na1 O4 52.26(13) 3_355 . . . ? O9 Cu2 Na1 O4 -127.74(13) . . . . ? O5 Cu2 Na1 O4 -100.26(12) 3_355 . . . ? O5 Cu2 Na1 O4 79.74(12) . . . . ? Na1 Cu2 Na1 O4 52(100) 3_355 . . . ? O9 Cu2 Na1 C30 -43.46(14) 3_355 . . . ? O9 Cu2 Na1 C30 136.54(14) . . . . ? O5 Cu2 Na1 C30 164.02(12) 3_355 . . . ? O5 Cu2 Na1 C30 -15.98(12) . . . . ? Na1 Cu2 Na1 C30 -44(100) 3_355 . . . ? O9 Cu2 Na1 C34 171.58(15) 3_355 . . . ? O9 Cu2 Na1 C34 -8.42(15) . . . . ? O5 Cu2 Na1 C34 19.06(14) 3_355 . . . ? O5 Cu2 Na1 C34 -160.94(14) . . . . ? Na1 Cu2 Na1 C34 171(100) 3_355 . . . ? O1 C2 C3 C4 -172.5(3) . . . . ? C7 C2 C3 C4 8.6(5) . . . . ? O1 C2 C3 C1 11.9(5) . . . . ? C7 C2 C3 C1 -166.9(3) . . . . ? C28 C1 C3 C2 85.0(4) . . . . ? C28 C1 C3 C4 -90.3(4) . . . . ? C2 C3 C4 C5 -2.0(6) . . . . ? C1 C3 C4 C5 173.5(3) . . . . ? C3 C4 C5 C6 -4.0(6) . . . . ? C4 C5 C6 C7 3.5(6) . . . . ? C5 C6 C7 C2 2.7(6) . . . . ? C5 C6 C7 C8 -171.1(4) . . . . ? C3 C2 C7 C6 -9.0(5) . . . . ? O1 C2 C7 C6 172.1(3) . . . . ? C3 C2 C7 C8 164.8(3) . . . . ? O1 C2 C7 C8 -14.0(5) . . . . ? C6 C7 C8 C10 85.2(4) . . . . ? C2 C7 C8 C10 -88.4(4) . . . . ? O2 C9 C10 C11 176.9(3) . . . . ? C14 C9 C10 C11 1.7(5) . . . . ? O2 C9 C10 C8 -2.2(5) . . . . ? C14 C9 C10 C8 -177.5(3) . . . . ? C7 C8 C10 C11 -66.7(4) . . . . ? C7 C8 C10 C9 112.4(4) . . . . ? C9 C10 C11 C12 0.1(5) . . . . ? C8 C10 C11 C12 179.2(4) . . . . ? C10 C11 C12 C13 -0.7(6) . . . . ? C11 C12 C13 C14 -0.3(6) . . . . ? O2 C9 C14 C13 -177.7(3) . . . . ? C10 C9 C14 C13 -2.6(5) . . . . ? O2 C9 C14 C15 -1.2(5) . . . . ? C10 C9 C14 C15 173.9(3) . . . . ? C12 C13 C14 C9 1.9(6) . . . . ? C12 C13 C14 C15 -174.8(4) . . . . ? C9 C14 C15 C17 -101.8(4) . . . . ? C13 C14 C15 C17 74.7(4) . . . . ? O3 C16 C17 C18 -171.5(3) . . . . ? C21 C16 C17 C18 9.5(5) . . . . ? O3 C16 C17 C15 12.2(5) . . . . ? C21 C16 C17 C15 -166.8(3) . . . . ? C14 C15 C17 C16 83.1(4) . . . . ? C14 C15 C17 C18 -92.9(4) . . . . ? C16 C17 C18 C19 -2.3(6) . . . . ? C15 C17 C18 C19 173.9(4) . . . . ? C17 C18 C19 C20 -3.5(6) . . . . ? C18 C19 C20 C21 2.5(6) . . . . ? C19 C20 C21 C16 4.2(5) . . . . ? C19 C20 C21 C22 -170.0(4) . . . . ? C17 C16 C21 C20 -10.4(5) . . . . ? O3 C16 C21 C20 170.6(3) . . . . ? C17 C16 C21 C22 163.8(3) . . . . ? O3 C16 C21 C22 -15.2(5) . . . . ? C20 C21 C22 C24 88.1(4) . . . . ? C16 C21 C22 C24 -85.8(4) . . . . ? O4 C23 C24 C25 -179.4(3) . . . . ? C28 C23 C24 C25 4.3(5) . . . . ? O4 C23 C24 C22 0.6(5) . . . . ? C28 C23 C24 C22 -175.7(3) . . . . ? C21 C22 C24 C25 -60.5(4) . . . . ? C21 C22 C24 C23 119.6(4) . . . . ? C23 C24 C25 C26 0.6(5) . . . . ? C22 C24 C25 C26 -179.3(3) . . . . ? C24 C25 C26 C27 -3.5(6) . . . . ? C25 C26 C27 C28 1.5(6) . . . . ? C26 C27 C28 C23 3.2(5) . . . . ? C26 C27 C28 C1 -172.5(3) . . . . ? C24 C23 C28 C27 -6.2(5) . . . . ? O4 C23 C28 C27 177.5(3) . . . . ? C24 C23 C28 C1 169.3(3) . . . . ? O4 C23 C28 C1 -6.9(5) . . . . ? C3 C1 C28 C27 66.8(4) . . . . ? C3 C1 C28 C23 -108.7(4) . . . . ? O1 C29 C30 O6 -157.9(3) . . . . ? O1 C29 C30 O5 21.0(4) . . . . ? O1 C29 C30 Na1 -5.5(2) . . . . ? O9 Na1 C30 O6 -39.4(5) . . . . ? O1 Na1 C30 O6 131.2(5) . . . . ? O3 Na1 C30 O6 -39.5(6) . . . . ? O5 Na1 C30 O6 -88.6(5) . . . . ? O2 Na1 C30 O6 52.5(5) . . . . ? O4 Na1 C30 O6 -145.2(5) . . . . ? C34 Na1 C30 O6 -34.0(5) . . . . ? Cu2 Na1 C30 O6 -62.9(5) . . . . ? O9 Na1 C30 O5 49.1(2) . . . . ? O1 Na1 C30 O5 -140.2(3) . . . . ? O3 Na1 C30 O5 49.1(4) . . . . ? O2 Na1 C30 O5 141.1(2) . . . . ? O4 Na1 C30 O5 -56.6(2) . . . . ? C34 Na1 C30 O5 54.6(2) . . . . ? Cu2 Na1 C30 O5 25.7(2) . . . . ? O9 Na1 C30 C29 -166.5(2) . . . . ? O1 Na1 C30 C29 4.12(18) . . . . ? O3 Na1 C30 C29 -166.5(2) . . . . ? O5 Na1 C30 C29 144.4(3) . . . . ? O2 Na1 C30 C29 -74.6(2) . . . . ? O4 Na1 C30 C29 87.8(2) . . . . ? C34 Na1 C30 C29 -161.1(2) . . . . ? Cu2 Na1 C30 C29 170.0(2) . . . . ? O2 C31 C32 O7 -15.2(4) . . . . ? O2 C31 C32 O8 166.3(3) . . . . ? O3 C33 C34 O10 156.1(4) . . . . ? O3 C33 C34 O9 -24.4(5) . . . . ? O3 C33 C34 Na1 -8.0(3) . . . . ? O9 Na1 C34 O10 61.5(7) . . . . ? O1 Na1 C34 O10 20.3(8) . . . . ? O3 Na1 C34 O10 -137.0(7) . . . . ? O5 Na1 C34 O10 64.1(7) . . . . ? O2 Na1 C34 O10 -56.2(7) . . . . ? O4 Na1 C34 O10 142.9(7) . . . . ? C30 Na1 C34 O10 46.0(7) . . . . ? Cu2 Na1 C34 O10 75.3(7) . . . . ? O1 Na1 C34 O9 -41.2(4) . . . . ? O3 Na1 C34 O9 161.5(3) . . . . ? O5 Na1 C34 O9 2.6(3) . . . . ? O2 Na1 C34 O9 -117.6(3) . . . . ? O4 Na1 C34 O9 81.4(3) . . . . ? C30 Na1 C34 O9 -15.5(3) . . . . ? Cu2 Na1 C34 O9 13.9(2) . . . . ? O9 Na1 C34 C33 -155.4(4) . . . . ? O1 Na1 C34 C33 163.4(3) . . . . ? O3 Na1 C34 C33 6.1(2) . . . . ? O5 Na1 C34 C33 -152.8(2) . . . . ? O2 Na1 C34 C33 86.9(2) . . . . ? O4 Na1 C34 C33 -74.0(2) . . . . ? C30 Na1 C34 C33 -170.9(2) . . . . ? Cu2 Na1 C34 C33 -141.6(2) . . . . ? O4 C35 C36 O11 -39.0(4) . . . . ? O4 C35 C36 O12 143.2(3) . . . . ? C3 C2 O1 C29 91.6(4) . . . . ? C7 C2 O1 C29 -89.5(4) . . . . ? C3 C2 O1 Na1 -92.2(4) . . . . ? C7 C2 O1 Na1 86.7(4) . . . . ? C30 C29 O1 C2 -175.0(3) . . . . ? C30 C29 O1 Na1 8.1(4) . . . . ? O9 Na1 O1 C2 -167.6(2) . . . . ? O3 Na1 O1 C2 -9.5(4) . . . . ? O5 Na1 O1 C2 164.2(3) . . . . ? O2 Na1 O1 C2 -73.5(3) . . . . ? O4 Na1 O1 C2 83.9(3) . . . . ? C30 Na1 O1 C2 179.2(3) . . . . ? C34 Na1 O1 C2 -148.5(3) . . . . ? Cu2 Na1 O1 C2 166.9(2) . . . . ? O9 Na1 O1 C29 8.5(3) . . . . ? O3 Na1 O1 C29 166.6(3) . . . . ? O5 Na1 O1 C29 -19.7(2) . . . . ? O2 Na1 O1 C29 102.6(2) . . . . ? O4 Na1 O1 C29 -100.0(2) . . . . ? C30 Na1 O1 C29 -4.7(2) . . . . ? C34 Na1 O1 C29 27.6(3) . . . . ? Cu2 Na1 O1 C29 -16.9(2) . . . . ? C14 C9 O2 C31 -75.9(4) . . . . ? C10 C9 O2 C31 108.8(3) . . . . ? C14 C9 O2 Na1 92.0(3) . . . . ? C10 C9 O2 Na1 -83.3(3) . . . . ? C32 C31 O2 C9 -133.0(3) . . . . ? C32 C31 O2 Na1 59.8(3) . . . . ? O9 Na1 O2 C9 -150.1(2) . . . . ? O1 Na1 O2 C9 74.9(2) . . . . ? O3 Na1 O2 C9 -80.2(2) . . . . ? O5 Na1 O2 C9 141.6(2) . . . . ? O4 Na1 O2 C9 -3.6(4) . . . . ? C30 Na1 O2 C9 125.6(2) . . . . ? C34 Na1 O2 C9 -131.9(2) . . . . ? Cu2 Na1 O2 C9 -176.0(2) . . . . ? O9 Na1 O2 C31 16.8(2) . . . . ? O1 Na1 O2 C31 -118.2(2) . . . . ? O3 Na1 O2 C31 86.7(2) . . . . ? O5 Na1 O2 C31 -51.5(3) . . . . ? O4 Na1 O2 C31 163.3(3) . . . . ? C30 Na1 O2 C31 -67.5(3) . . . . ? C34 Na1 O2 C31 35.0(2) . . . . ? Cu2 Na1 O2 C31 -9.1(3) . . . . ? C17 C16 O3 C33 85.0(4) . . . . ? C21 C16 O3 C33 -96.0(4) . . . . ? C17 C16 O3 Na1 -100.2(4) . . . . ? C21 C16 O3 Na1 78.8(4) . . . . ? C34 C33 O3 C16 -172.3(3) . . . . ? C34 C33 O3 Na1 12.1(4) . . . . ? O9 Na1 O3 C16 -174.6(3) . . . . ? O1 Na1 O3 C16 21.6(4) . . . . ? O5 Na1 O3 C16 -149.7(3) . . . . ? O2 Na1 O3 C16 87.9(3) . . . . ? O4 Na1 O3 C16 -69.7(3) . . . . ? C30 Na1 O3 C16 -174.6(3) . . . . ? C34 Na1 O3 C16 178.6(3) . . . . ? Cu2 Na1 O3 C16 -155.0(3) . . . . ? O9 Na1 O3 C33 -0.1(2) . . . . ? O1 Na1 O3 C33 -163.9(3) . . . . ? O5 Na1 O3 C33 24.9(3) . . . . ? O2 Na1 O3 C33 -97.6(3) . . . . ? O4 Na1 O3 C33 104.9(2) . . . . ? C30 Na1 O3 C33 0.0(4) . . . . ? C34 Na1 O3 C33 -6.9(2) . . . . ? Cu2 Na1 O3 C33 19.6(3) . . . . ? C24 C23 O4 C35 115.1(3) . . . . ? C28 C23 O4 C35 -68.6(4) . . . . ? C24 C23 O4 Na1 -83.8(3) . . . . ? C28 C23 O4 Na1 92.5(3) . . . . ? C36 C35 O4 C23 -113.4(3) . . . . ? C36 C35 O4 Na1 91.9(3) . . . . ? O9 Na1 O4 C23 146.2(2) . . . . ? O1 Na1 O4 C23 -78.0(2) . . . . ? O3 Na1 O4 C23 74.6(2) . . . . ? O5 Na1 O4 C23 -148.7(2) . . . . ? O2 Na1 O4 C23 1.2(4) . . . . ? C30 Na1 O4 C23 -129.8(2) . . . . ? C34 Na1 O4 C23 125.0(2) . . . . ? Cu2 Na1 O4 C23 174.45(19) . . . . ? O9 Na1 O4 C35 -57.7(3) . . . . ? O1 Na1 O4 C35 78.1(3) . . . . ? O3 Na1 O4 C35 -129.3(3) . . . . ? O5 Na1 O4 C35 7.4(3) . . . . ? O2 Na1 O4 C35 157.3(3) . . . . ? C30 Na1 O4 C35 26.3(3) . . . . ? C34 Na1 O4 C35 -78.9(3) . . . . ? Cu2 Na1 O4 C35 -29.4(3) . . . . ? O6 C30 O5 Cu2 11.9(5) . . . . ? C29 C30 O5 Cu2 -166.8(2) . . . . ? Na1 C30 O5 Cu2 -127.3(3) . . . . ? O6 C30 O5 Na1 139.2(3) . . . . ? C29 C30 O5 Na1 -39.6(4) . . . . ? O9 Cu2 O5 C30 -65.8(3) 3_355 . . . ? O9 Cu2 O5 C30 114.2(3) . . . . ? O5 Cu2 O5 C30 -63(37) 3_355 . . . ? Na1 Cu2 O5 C30 -47.3(3) 3_355 . . . ? Na1 Cu2 O5 C30 132.7(3) . . . . ? O9 Cu2 O5 Na1 161.51(11) 3_355 . . . ? O9 Cu2 O5 Na1 -18.49(11) . . . . ? O5 Cu2 O5 Na1 165(37) 3_355 . . . ? Na1 Cu2 O5 Na1 180.0 3_355 . . . ? O9 Na1 O5 C30 -126.7(2) . . . . ? O1 Na1 O5 C30 32.4(2) . . . . ? O3 Na1 O5 C30 -151.8(2) . . . . ? O2 Na1 O5 C30 -45.0(3) . . . . ? O4 Na1 O5 C30 121.9(2) . . . . ? C34 Na1 O5 C30 -127.6(2) . . . . ? Cu2 Na1 O5 C30 -143.1(3) . . . . ? O9 Na1 O5 Cu2 16.46(9) . . . . ? O1 Na1 O5 Cu2 175.54(12) . . . . ? O3 Na1 O5 Cu2 -8.70(19) . . . . ? O2 Na1 O5 Cu2 98.17(12) . . . . ? O4 Na1 O5 Cu2 -94.94(10) . . . . ? C30 Na1 O5 Cu2 143.1(3) . . . . ? C34 Na1 O5 Cu2 15.49(11) . . . . ? O5 C30 O6 Cu1 -87.4(4) . . . 1_455 ? C29 C30 O6 Cu1 91.3(3) . . . 1_455 ? Na1 C30 O6 Cu1 -26.8(6) . . . 1_455 ? O8 C32 O7 Cu1 4.4(5) . . . 1_455 ? C31 C32 O7 Cu1 -173.8(2) . . . 1_455 ? O7 C32 O8 Cu1 -2.6(5) . . . 3_355 ? C31 C32 O8 Cu1 175.7(2) . . . 3_355 ? O10 C34 O9 Cu2 53.3(6) . . . . ? C33 C34 O9 Cu2 -126.1(3) . . . . ? Na1 C34 O9 Cu2 -152.8(5) . . . . ? O10 C34 O9 Na1 -154.0(3) . . . . ? C33 C34 O9 Na1 26.7(4) . . . . ? O9 Cu2 O9 C34 -173(100) 3_355 . . . ? O5 Cu2 O9 C34 -4.5(4) 3_355 . . . ? O5 Cu2 O9 C34 175.5(4) . . . . ? Na1 Cu2 O9 C34 -23.6(4) 3_355 . . . ? Na1 Cu2 O9 C34 156.4(4) . . . . ? O9 Cu2 O9 Na1 31(100) 3_355 . . . ? O5 Cu2 O9 Na1 -160.90(11) 3_355 . . . ? O5 Cu2 O9 Na1 19.10(11) . . . . ? Na1 Cu2 O9 Na1 180.0 3_355 . . . ? O1 Na1 O9 C34 154.4(3) . . . . ? O3 Na1 O9 C34 -15.2(3) . . . . ? O5 Na1 O9 C34 -177.2(3) . . . . ? O2 Na1 O9 C34 61.9(3) . . . . ? O4 Na1 O9 C34 -105.2(3) . . . . ? C30 Na1 O9 C34 164.9(3) . . . . ? Cu2 Na1 O9 C34 -160.1(3) . . . . ? O1 Na1 O9 Cu2 -45.52(19) . . . . ? O3 Na1 O9 Cu2 144.92(14) . . . . ? O5 Na1 O9 Cu2 -17.16(10) . . . . ? O2 Na1 O9 Cu2 -138.07(11) . . . . ? O4 Na1 O9 Cu2 54.91(13) . . . . ? C30 Na1 O9 Cu2 -35.06(11) . . . . ? C34 Na1 O9 Cu2 160.1(3) . . . . ? O12 C36 O11 Cu1 -5.0(5) . . . 3_455 ? C35 C36 O11 Cu1 177.5(2) . . . 3_455 ? O11 C36 O12 Cu1 4.6(5) . . . . ? C35 C36 O12 Cu1 -177.9(2) . . . . ? O8 Cu1 O12 C36 -86.9(3) 3_355 . . . ? O11 Cu1 O12 C36 -0.9(7) 3_455 . . . ? O7 Cu1 O12 C36 81.4(3) 1_655 . . . ? O6 Cu1 O12 C36 173.3(3) 1_655 . . . ? Cu1 Cu1 O12 C36 -1.9(3) 3_455 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.403 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.067 #===== data_11 _database_code_depnum_ccdc_archive 'CCDC 879393' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C208 H264 Cu7 Na4 O61' _chemical_formula_weight 4276.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 53.4770(8) _cell_length_b 10.5650(3) _cell_length_c 38.1550(13) _cell_angle_alpha 90 _cell_angle_beta 95.734(2) _cell_angle_gamma 90 _cell_volume 21449.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8988 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8490 _exptl_absorpt_correction_T_max 0.8868 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41537 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.1562 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 63 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.03 _reflns_number_total 18832 _reflns_number_gt 8670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The low ratio of observed/unique reflections may be attributed to the weak diffraction of the crystals. The distances of O2W---H2A, O2W---H2B, O1W---H1C, O1W---H1D, O3W---H3A, O3W---H3B, O7W---H7A and O7W---H7B were restrained to 0.87+-0.01 \%A. The distances of H3A...H3B, H2A...H2B, H1C...H1D and H7A...H7B were restrained to 1.44+-0.02 \%A. The distance of Cu2...H2A was restrained to 2.60+-0.02 \%A. The distance of O9...O6W was restrained to 3.12+-0.01 \%A. For C44, C39, C40, C42, C43, C82, C84, C86, C90 and C92, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18832 _refine_ls_number_parameters 1372 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.1118 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.884 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.436947(9) -0.13737(5) 0.693014(14) 0.03673(16) Uani 1 1 d . . . Cu2 Cu 0.5000 -0.49287(7) 0.7500 0.0392(2) Uani 1 2 d SD . . Cu3 Cu 0.468471(9) -0.84867(5) 0.693152(13) 0.03163(15) Uani 1 1 d . . . Cu4 Cu 0.428921(10) -0.65112(5) 0.662039(15) 0.03692(15) Uani 1 1 d . . . Na1 Na 0.52871(3) -0.84046(15) 0.66252(4) 0.0347(4) Uani 1 1 d . . . Na2 Na 0.37662(3) -0.08127(16) 0.66367(5) 0.0436(5) Uani 1 1 d . . . C1 C 0.55238(8) -0.5360(4) 0.59566(11) 0.0317(11) Uani 1 1 d . . . H1A H 0.5413 -0.5272 0.6142 0.038 Uiso 1 1 calc R . . H1B H 0.5552 -0.4526 0.5862 0.038 Uiso 1 1 calc R . . C2 C 0.57725(8) -0.5925(4) 0.61073(12) 0.0320(11) Uani 1 1 d . . . C3 C 0.58025(7) -0.6539(4) 0.64299(11) 0.0302(10) Uani 1 1 d . . . C4 C 0.60261(8) -0.7161(4) 0.65473(11) 0.0330(11) Uani 1 1 d . . . C5 C 0.62223(8) -0.7115(4) 0.63320(13) 0.0415(12) Uani 1 1 d . . . H5 H 0.6373 -0.7513 0.6409 0.050 Uiso 1 1 calc R . . C6 C 0.62023(8) -0.6500(4) 0.60069(13) 0.0398(12) Uani 1 1 d . A . C7 C 0.59750(8) -0.5912(4) 0.59004(12) 0.0391(12) Uani 1 1 d . . . H7 H 0.5956 -0.5497 0.5684 0.047 Uiso 1 1 calc R . . C8 C 0.60643(8) -0.7957(4) 0.68802(12) 0.0371(12) Uani 1 1 d . . . H8A H 0.6215 -0.7680 0.7022 0.045 Uiso 1 1 calc R . . H8B H 0.5923 -0.7837 0.7018 0.045 Uiso 1 1 calc R . . C9 C 0.60878(8) -0.9342(4) 0.67935(11) 0.0324(11) Uani 1 1 d . . . C10 C 0.63183(8) -0.9888(4) 0.67384(12) 0.0392(12) Uani 1 1 d . . . H10 H 0.6463 -0.9403 0.6780 0.047 Uiso 1 1 calc R . . C11 C 0.63396(8) -1.1128(4) 0.66235(12) 0.0412(12) Uani 1 1 d . A . C12 C 0.61192(8) -1.1802(4) 0.65462(11) 0.0379(12) Uani 1 1 d . . . H12 H 0.6128 -1.2611 0.6452 0.045 Uiso 1 1 calc R . . C13 C 0.58859(7) -1.1323(4) 0.66031(10) 0.0295(10) Uani 1 1 d . . . C14 C 0.58766(7) -1.0123(4) 0.67446(10) 0.0283(11) Uani 1 1 d . . . C15 C 0.56473(8) -1.2024(4) 0.64751(11) 0.0334(11) Uani 1 1 d . . . H15A H 0.5520 -1.1874 0.6635 0.040 Uiso 1 1 calc R . . H15B H 0.5680 -1.2926 0.6471 0.040 Uiso 1 1 calc R . . C16 C 0.55522(7) -1.1572(4) 0.61083(11) 0.0267(10) Uani 1 1 d . . . C17 C 0.53433(7) -1.0800(4) 0.60351(12) 0.0267(10) Uani 1 1 d . . . C18 C 0.52771(7) -1.0309(4) 0.56994(12) 0.0271(10) Uani 1 1 d . . . C19 C 0.54237(8) -1.0652(4) 0.54358(11) 0.0306(11) Uani 1 1 d . . . H19 H 0.5379 -1.0351 0.5209 0.037 Uiso 1 1 calc R . . C20 C 0.56343(8) -1.1422(4) 0.54931(12) 0.0312(10) Uani 1 1 d . . . C21 C 0.56922(8) -1.1876(4) 0.58305(12) 0.0304(11) Uani 1 1 d . . . H21 H 0.5831 -1.2407 0.5875 0.036 Uiso 1 1 calc R . . C22 C 0.50604(7) -0.9379(3) 0.56131(11) 0.0294(11) Uani 1 1 d . . . H22A H 0.4944 -0.9712 0.5424 0.035 Uiso 1 1 calc R . . H22B H 0.4970 -0.9254 0.5818 0.035 Uiso 1 1 calc R . . C23 C 0.51684(7) -0.8130(4) 0.55024(11) 0.0266(10) Uani 1 1 d . . . C24 C 0.52493(7) -0.7215(4) 0.57462(11) 0.0262(10) Uani 1 1 d . . . C25 C 0.54018(7) -0.6204(4) 0.56690(11) 0.0276(10) Uani 1 1 d . . . C26 C 0.54465(8) -0.6058(4) 0.53157(12) 0.0353(12) Uani 1 1 d . . . H26 H 0.5547 -0.5389 0.5256 0.042 Uiso 1 1 calc R . . C27 C 0.53478(8) -0.6865(4) 0.50504(12) 0.0345(11) Uani 1 1 d . . . C28 C 0.52159(8) -0.7917(4) 0.51526(12) 0.0335(11) Uani 1 1 d . . . H28 H 0.5157 -0.8501 0.4982 0.040 Uiso 1 1 calc R . . C29 C 0.53795(10) -0.6656(4) 0.46587(12) 0.0474(13) Uani 1 1 d . . . C30 C 0.51108(10) -0.6507(5) 0.44582(14) 0.0697(16) Uani 1 1 d . . . H30A H 0.5013 -0.7251 0.4493 0.105 Uiso 1 1 calc R . . H30B H 0.5125 -0.6397 0.4211 0.105 Uiso 1 1 calc R . . H30C H 0.5030 -0.5781 0.4547 0.105 Uiso 1 1 calc R . . C31 C 0.55013(11) -0.7812(5) 0.45069(14) 0.0727(18) Uani 1 1 d . . . H31A H 0.5404 -0.8553 0.4548 0.109 Uiso 1 1 calc R . . H31B H 0.5669 -0.7911 0.4619 0.109 Uiso 1 1 calc R . . H31C H 0.5507 -0.7699 0.4258 0.109 Uiso 1 1 calc R . . C32 C 0.55267(13) -0.5472(5) 0.45936(14) 0.093(2) Uani 1 1 d . . . H32A H 0.5539 -0.5381 0.4346 0.140 Uiso 1 1 calc R . . H32B H 0.5692 -0.5533 0.4716 0.140 Uiso 1 1 calc R . . H32C H 0.5442 -0.4748 0.4678 0.140 Uiso 1 1 calc R . . C33 C 0.58002(9) -1.1664(4) 0.51945(13) 0.0486(13) Uani 1 1 d . . . C34 C 0.59614(14) -1.0505(6) 0.5160(2) 0.133(3) Uani 1 1 d . . . H34A H 0.5856 -0.9778 0.5114 0.199 Uiso 1 1 calc R . . H34B H 0.6063 -1.0623 0.4968 0.199 Uiso 1 1 calc R . . H34C H 0.6068 -1.0379 0.5374 0.199 Uiso 1 1 calc R . . C35 C 0.56399(13) -1.1876(6) 0.48435(16) 0.103(2) Uani 1 1 d . . . H35A H 0.5536 -1.2611 0.4861 0.154 Uiso 1 1 calc R . . H35B H 0.5748 -1.2001 0.4660 0.154 Uiso 1 1 calc R . . H35C H 0.5535 -1.1150 0.4790 0.154 Uiso 1 1 calc R . . C36 C 0.59638(12) -1.2813(6) 0.52611(15) 0.094(2) Uani 1 1 d . . . H36A H 0.5860 -1.3547 0.5279 0.141 Uiso 1 1 calc R . . H36B H 0.6070 -1.2704 0.5477 0.141 Uiso 1 1 calc R . . H36C H 0.6065 -1.2923 0.5070 0.141 Uiso 1 1 calc R . . C37 C 0.65962(9) -1.1700(5) 0.65640(14) 0.0522(14) Uani 1 1 d . . . C38 C 0.66093(16) -1.1873(11) 0.6177(2) 0.074(3) Uani 0.620(5) 1 d P A 1 H38A H 0.6473 -1.2404 0.6083 0.110 Uiso 0.620(5) 1 calc PR A 1 H38B H 0.6766 -1.2262 0.6138 0.110 Uiso 0.620(5) 1 calc PR A 1 H38C H 0.6597 -1.1064 0.6063 0.110 Uiso 0.620(5) 1 calc PR A 1 C39 C 0.66223(17) -1.3014(9) 0.6745(3) 0.088(3) Uani 0.620(5) 1 d PU A 1 H39A H 0.6486 -1.3548 0.6654 0.131 Uiso 0.620(5) 1 calc PR A 1 H39B H 0.6619 -1.2914 0.6995 0.131 Uiso 0.620(5) 1 calc PR A 1 H39C H 0.6779 -1.3394 0.6698 0.131 Uiso 0.620(5) 1 calc PR A 1 C40 C 0.68121(19) -1.0909(11) 0.6723(4) 0.097(4) Uani 0.620(5) 1 d PU A 1 H40A H 0.6800 -1.0809 0.6971 0.146 Uiso 0.620(5) 1 calc PR A 1 H40B H 0.6807 -1.0093 0.6612 0.146 Uiso 0.620(5) 1 calc PR A 1 H40C H 0.6968 -1.1320 0.6687 0.146 Uiso 0.620(5) 1 calc PR A 1 C42 C 0.6452(2) -0.7813(9) 0.5645(3) 0.081(3) Uani 0.620(5) 1 d PU A 1 H42A H 0.6478 -0.8380 0.5842 0.121 Uiso 0.620(5) 1 calc PR A 1 H42B H 0.6595 -0.7843 0.5512 0.121 Uiso 0.620(5) 1 calc PR A 1 H42C H 0.6304 -0.8061 0.5497 0.121 Uiso 0.620(5) 1 calc PR A 1 C43 C 0.66653(19) -0.6115(11) 0.5987(3) 0.096(4) Uani 0.620(5) 1 d PU A 1 H43A H 0.6647 -0.5265 0.6070 0.143 Uiso 0.620(5) 1 calc PR A 1 H43B H 0.6801 -0.6149 0.5841 0.143 Uiso 0.620(5) 1 calc PR A 1 H43C H 0.6700 -0.6672 0.6184 0.143 Uiso 0.620(5) 1 calc PR A 1 C44 C 0.6385(2) -0.5599(11) 0.5470(3) 0.095(4) Uani 0.620(5) 1 d PU A 1 H44A H 0.6370 -0.4758 0.5561 0.142 Uiso 0.620(5) 1 calc PR A 1 H44B H 0.6235 -0.5808 0.5322 0.142 Uiso 0.620(5) 1 calc PR A 1 H44C H 0.6527 -0.5641 0.5335 0.142 Uiso 0.620(5) 1 calc PR A 1 C86 C 0.2389(2) -0.2808(11) 0.7253(4) 0.109(4) Uani 0.620(5) 1 d PU A 1 H86A H 0.2392 -0.1960 0.7164 0.164 Uiso 0.620(5) 1 calc PR A 1 H86B H 0.2458 -0.2816 0.7496 0.164 Uiso 0.620(5) 1 calc PR A 1 H86C H 0.2220 -0.3113 0.7235 0.164 Uiso 0.620(5) 1 calc PR A 1 C87 C 0.24090(18) -0.3679(13) 0.6661(3) 0.113(5) Uani 0.620(5) 1 d P A 1 H87A H 0.2503 -0.4196 0.6514 0.170 Uiso 0.620(5) 1 calc PR A 1 H87B H 0.2397 -0.2835 0.6568 0.170 Uiso 0.620(5) 1 calc PR A 1 H87C H 0.2243 -0.4025 0.6667 0.170 Uiso 0.620(5) 1 calc PR A 1 C88 C 0.2549(2) -0.4983(13) 0.7176(5) 0.127(6) Uani 0.620(5) 1 d P A 1 H88A H 0.2640 -0.5509 0.7027 0.191 Uiso 0.620(5) 1 calc PR A 1 H88B H 0.2380 -0.5290 0.7175 0.191 Uiso 0.620(5) 1 calc PR A 1 H88C H 0.2631 -0.5005 0.7412 0.191 Uiso 0.620(5) 1 calc PR A 1 C82 C 0.2515(2) 0.0220(12) 0.6042(4) 0.123(5) Uani 0.620(5) 1 d PU A 1 H82A H 0.2346 0.0165 0.5932 0.185 Uiso 0.620(5) 1 calc PR A 1 H82B H 0.2553 -0.0519 0.6183 0.185 Uiso 0.620(5) 1 calc PR A 1 H82C H 0.2629 0.0274 0.5864 0.185 Uiso 0.620(5) 1 calc PR A 1 C83 C 0.23598(15) 0.1356(14) 0.6563(3) 0.103(5) Uani 0.620(5) 1 d P A 1 H83A H 0.2190 0.1350 0.6455 0.155 Uiso 0.620(5) 1 calc PR A 1 H83B H 0.2385 0.2086 0.6713 0.155 Uiso 0.620(5) 1 calc PR A 1 H83C H 0.2391 0.0603 0.6702 0.155 Uiso 0.620(5) 1 calc PR A 1 C84 C 0.2472(2) 0.2539(11) 0.6053(3) 0.105(4) Uani 0.620(5) 1 d PU A 1 H84A H 0.2299 0.2472 0.5958 0.157 Uiso 0.620(5) 1 calc PR A 1 H84B H 0.2577 0.2583 0.5864 0.157 Uiso 0.620(5) 1 calc PR A 1 H84C H 0.2494 0.3290 0.6195 0.157 Uiso 0.620(5) 1 calc PR A 1 C90 C 0.2678(2) -0.2748(11) 0.5584(3) 0.105(4) Uani 0.620(5) 1 d PU A 1 H90A H 0.2739 -0.1932 0.5522 0.158 Uiso 0.620(5) 1 calc PR A 1 H90B H 0.2671 -0.2787 0.5834 0.158 Uiso 0.620(5) 1 calc PR A 1 H90C H 0.2514 -0.2882 0.5466 0.158 Uiso 0.620(5) 1 calc PR A 1 C91 C 0.2746(3) -0.5030(11) 0.5566(4) 0.109(5) Uani 0.620(5) 1 d P A 1 H91A H 0.2869 -0.5675 0.5536 0.163 Uiso 0.620(5) 1 calc PR A 1 H91B H 0.2596 -0.5198 0.5413 0.163 Uiso 0.620(5) 1 calc PR A 1 H91C H 0.2707 -0.5028 0.5806 0.163 Uiso 0.620(5) 1 calc PR A 1 C92 C 0.2863(3) -0.3678(15) 0.5077(4) 0.138(6) Uani 0.620(5) 1 d PU A 1 H92A H 0.2937 -0.2887 0.5017 0.208 Uiso 0.620(5) 1 calc PR A 1 H92B H 0.2696 -0.3741 0.4959 0.208 Uiso 0.620(5) 1 calc PR A 1 H92C H 0.2964 -0.4364 0.5003 0.208 Uiso 0.620(5) 1 calc PR A 1 O10 O 0.4200(4) -0.4039(16) 0.6695(4) 0.081(5) Uani 0.620(5) 1 d P A 1 C38' C 0.6593(4) -1.273(2) 0.6338(7) 0.120(8) Uiso 0.380(5) 1 d P A 2 H38D H 0.6471 -1.2594 0.6141 0.179 Uiso 0.380(5) 1 calc PR A 2 H38E H 0.6551 -1.3481 0.6462 0.179 Uiso 0.380(5) 1 calc PR A 2 H38F H 0.6756 -1.2833 0.6257 0.179 Uiso 0.380(5) 1 calc PR A 2 C39' C 0.6771(3) -1.1708(14) 0.6897(4) 0.062(4) Uiso 0.380(5) 1 d P A 2 H39D H 0.6745 -1.0955 0.7030 0.092 Uiso 0.380(5) 1 calc PR A 2 H39E H 0.6941 -1.1735 0.6840 0.092 Uiso 0.380(5) 1 calc PR A 2 H39F H 0.6737 -1.2438 0.7034 0.092 Uiso 0.380(5) 1 calc PR A 2 C40' C 0.6764(3) -1.0615(17) 0.6357(6) 0.106(6) Uiso 0.380(5) 1 d P A 2 H40D H 0.6684 -1.0471 0.6123 0.159 Uiso 0.380(5) 1 calc PR A 2 H40E H 0.6931 -1.0924 0.6343 0.159 Uiso 0.380(5) 1 calc PR A 2 H40F H 0.6770 -0.9835 0.6487 0.159 Uiso 0.380(5) 1 calc PR A 2 C42' C 0.6636(3) -0.7403(16) 0.5910(5) 0.088(6) Uiso 0.380(5) 1 d P A 2 H42D H 0.6573 -0.8245 0.5936 0.132 Uiso 0.380(5) 1 calc PR A 2 H42E H 0.6709 -0.7101 0.6135 0.132 Uiso 0.380(5) 1 calc PR A 2 H42F H 0.6761 -0.7411 0.5747 0.132 Uiso 0.380(5) 1 calc PR A 2 C43' C 0.6523(3) -0.5260(14) 0.5739(5) 0.075(5) Uiso 0.380(5) 1 d P A 2 H43D H 0.6390 -0.4684 0.5663 0.112 Uiso 0.380(5) 1 calc PR A 2 H43E H 0.6644 -0.5270 0.5570 0.112 Uiso 0.380(5) 1 calc PR A 2 H43F H 0.6603 -0.4991 0.5964 0.112 Uiso 0.380(5) 1 calc PR A 2 C44' C 0.6306(3) -0.6973(19) 0.5396(5) 0.107(7) Uiso 0.380(5) 1 d P A 2 H44D H 0.6240 -0.7814 0.5411 0.161 Uiso 0.380(5) 1 calc PR A 2 H44E H 0.6435 -0.6968 0.5238 0.161 Uiso 0.380(5) 1 calc PR A 2 H44F H 0.6174 -0.6407 0.5309 0.161 Uiso 0.380(5) 1 calc PR A 2 C86' C 0.2350(3) -0.2738(18) 0.6895(6) 0.101(6) Uiso 0.380(5) 1 d P A 2 H86D H 0.2386 -0.1916 0.6995 0.152 Uiso 0.380(5) 1 calc PR A 2 H86E H 0.2188 -0.3015 0.6951 0.152 Uiso 0.380(5) 1 calc PR A 2 H86F H 0.2352 -0.2695 0.6644 0.152 Uiso 0.380(5) 1 calc PR A 2 C87' C 0.2509(5) -0.492(3) 0.6931(7) 0.114(10) Uiso 0.380(5) 1 d P A 2 H87D H 0.2638 -0.5444 0.7051 0.171 Uiso 0.380(5) 1 calc PR A 2 H87E H 0.2519 -0.4978 0.6682 0.171 Uiso 0.380(5) 1 calc PR A 2 H87F H 0.2347 -0.5211 0.6986 0.171 Uiso 0.380(5) 1 calc PR A 2 C88' C 0.2507(3) -0.3664(16) 0.7458(4) 0.074(5) Uiso 0.380(5) 1 d P A 2 H88D H 0.2525 -0.2821 0.7551 0.111 Uiso 0.380(5) 1 calc PR A 2 H88E H 0.2630 -0.4206 0.7580 0.111 Uiso 0.380(5) 1 calc PR A 2 H88F H 0.2342 -0.3974 0.7489 0.111 Uiso 0.380(5) 1 calc PR A 2 C82' C 0.2528(3) 0.1072(15) 0.5868(4) 0.078(5) Uiso 0.380(5) 1 d P A 2 H82D H 0.2622 0.1687 0.5750 0.117 Uiso 0.380(5) 1 calc PR A 2 H82E H 0.2356 0.1081 0.5769 0.117 Uiso 0.380(5) 1 calc PR A 2 H82F H 0.2598 0.0246 0.5839 0.117 Uiso 0.380(5) 1 calc PR A 2 C83' C 0.2382(4) 0.0440(18) 0.6427(6) 0.103(7) Uiso 0.380(5) 1 d P A 2 H83D H 0.2453 -0.0384 0.6401 0.155 Uiso 0.380(5) 1 calc PR A 2 H83E H 0.2216 0.0466 0.6305 0.155 Uiso 0.380(5) 1 calc PR A 2 H83F H 0.2373 0.0614 0.6672 0.155 Uiso 0.380(5) 1 calc PR A 2 C84' C 0.2439(3) 0.2820(13) 0.6288(5) 0.073(5) Uiso 0.380(5) 1 d P A 2 H84D H 0.2551 0.3381 0.6183 0.110 Uiso 0.380(5) 1 calc PR A 2 H84E H 0.2428 0.3064 0.6529 0.110 Uiso 0.380(5) 1 calc PR A 2 H84F H 0.2275 0.2867 0.6161 0.110 Uiso 0.380(5) 1 calc PR A 2 C90' C 0.2731(3) -0.2371(15) 0.5397(5) 0.082(5) Uiso 0.380(5) 1 d P A 2 H90D H 0.2715 -0.1939 0.5615 0.123 Uiso 0.380(5) 1 calc PR A 2 H90E H 0.2567 -0.2462 0.5270 0.123 Uiso 0.380(5) 1 calc PR A 2 H90F H 0.2837 -0.1891 0.5258 0.123 Uiso 0.380(5) 1 calc PR A 2 C91' C 0.2669(6) -0.441(3) 0.5669(10) 0.177(17) Uiso 0.380(5) 1 d P A 2 H91D H 0.2514 -0.4500 0.5521 0.266 Uiso 0.380(5) 1 calc PR A 2 H91E H 0.2640 -0.3930 0.5875 0.266 Uiso 0.380(5) 1 calc PR A 2 H91F H 0.2733 -0.5229 0.5738 0.266 Uiso 0.380(5) 1 calc PR A 2 C92' C 0.2894(4) -0.4270(18) 0.5106(5) 0.079(6) Uiso 0.380(5) 1 d P A 2 H92D H 0.2734 -0.4396 0.4971 0.118 Uiso 0.380(5) 1 calc PR A 2 H92E H 0.2982 -0.5061 0.5131 0.118 Uiso 0.380(5) 1 calc PR A 2 H92F H 0.2991 -0.3674 0.4987 0.118 Uiso 0.380(5) 1 calc PR A 2 O10' O 0.4111(7) -0.440(3) 0.6761(9) 0.107(11) Uani 0.380(5) 1 d P A 2 C41 C 0.64203(9) -0.6529(5) 0.57720(14) 0.0520(14) Uani 1 1 d . . . C45 C 0.49391(7) -0.6533(4) 0.60702(11) 0.0322(11) Uani 1 1 d . . . H45A H 0.4833 -0.6713 0.5854 0.039 Uiso 1 1 calc R . . H45B H 0.4985 -0.5646 0.6067 0.039 Uiso 1 1 calc R . . C46 C 0.47929(8) -0.6776(4) 0.63798(12) 0.0283(10) Uani 1 1 d . . . C47 C 0.50078(7) -1.1339(4) 0.63672(11) 0.0354(11) Uani 1 1 d . . . H47A H 0.5082 -1.2141 0.6445 0.043 Uiso 1 1 calc R . . H47B H 0.4906 -1.1480 0.6146 0.043 Uiso 1 1 calc R . . C48 C 0.48445(8) -1.0863(4) 0.66371(11) 0.0281(11) Uani 1 1 d . . . C49 C 0.53452(8) -0.5187(4) 0.69644(14) 0.0349(12) Uani 1 1 d . . . C50 C 0.56064(8) -0.5682(4) 0.69147(12) 0.0388(12) Uani 1 1 d . . . H50A H 0.5714 -0.4980 0.6864 0.047 Uiso 1 1 calc R . . H50B H 0.5678 -0.6080 0.7131 0.047 Uiso 1 1 calc R . . C51 C 0.54695(8) -0.9251(4) 0.74016(13) 0.0296(11) Uani 1 1 d . . . C52 C 0.56340(9) -1.0102(4) 0.72071(12) 0.0514(14) Uani 1 1 d . . . H52A H 0.5801 -1.0124 0.7331 0.062 Uiso 1 1 calc R . . H52B H 0.5567 -1.0956 0.7203 0.062 Uiso 1 1 calc R . . C53 C 0.36929(8) -0.1621(4) 0.55855(12) 0.0385(12) Uani 1 1 d . . . H53A H 0.3852 -0.1585 0.5732 0.046 Uiso 1 1 calc R . . H53B H 0.3725 -0.1927 0.5355 0.046 Uiso 1 1 calc R . . C54 C 0.35786(7) -0.0319(4) 0.55528(12) 0.0303(11) Uani 1 1 d . . . C55 C 0.34157(8) 0.0006(4) 0.52597(12) 0.0346(11) Uani 1 1 d . . . H55 H 0.3397 -0.0550 0.5070 0.041 Uiso 1 1 calc R . . C56 C 0.32790(8) 0.1130(4) 0.52387(12) 0.0349(11) Uani 1 1 d . . . C57 C 0.33030(8) 0.1896(4) 0.55300(12) 0.0351(11) Uani 1 1 d . . . H57 H 0.3208 0.2633 0.5525 0.042 Uiso 1 1 calc R . . C58 C 0.34628(7) 0.1634(4) 0.58350(11) 0.0283(10) Uani 1 1 d . . . C59 C 0.36092(7) 0.0546(4) 0.58289(11) 0.0272(11) Uani 1 1 d . A . C60 C 0.34552(8) 0.2410(4) 0.61668(11) 0.0327(11) Uani 1 1 d . . . H60A H 0.3414 0.3281 0.6105 0.039 Uiso 1 1 calc R . . H60B H 0.3619 0.2398 0.6301 0.039 Uiso 1 1 calc R . . C61 C 0.32601(8) 0.1881(4) 0.63909(12) 0.0318(11) Uani 1 1 d . . . C62 C 0.30061(8) 0.1948(4) 0.62662(12) 0.0400(12) Uani 1 1 d . . . H62 H 0.2962 0.2375 0.6056 0.048 Uiso 1 1 calc R . . C63 C 0.28178(8) 0.1417(4) 0.64370(13) 0.0433(12) Uani 1 1 d . A . C64 C 0.28877(8) 0.0798(4) 0.67485(13) 0.0424(12) Uani 1 1 d . . . H64 H 0.2763 0.0445 0.6870 0.051 Uiso 1 1 calc R . . C65 C 0.31387(8) 0.0672(4) 0.68919(12) 0.0355(11) Uani 1 1 d . . . C66 C 0.33240(8) 0.1232(4) 0.67070(12) 0.0315(11) Uani 1 1 d . . . C67 C 0.31957(8) -0.0142(4) 0.72202(11) 0.0379(12) Uani 1 1 d . . . H67A H 0.3372 -0.0074 0.7305 0.045 Uiso 1 1 calc R . . H67B H 0.3097 0.0148 0.7405 0.045 Uiso 1 1 calc R . . C68 C 0.31310(7) -0.1507(4) 0.71294(11) 0.0344(11) Uani 1 1 d . . . C69 C 0.33022(8) -0.2302(4) 0.69950(12) 0.0345(11) Uani 1 1 d . . . C70 C 0.32346(9) -0.3455(4) 0.68382(12) 0.0425(12) Uani 1 1 d . . . C71 C 0.29874(9) -0.3864(4) 0.68589(13) 0.0517(14) Uani 1 1 d . . . H71 H 0.2938 -0.4642 0.6761 0.062 Uiso 1 1 calc R . . C72 C 0.28139(9) -0.3153(5) 0.70189(14) 0.0512(14) Uani 1 1 d . A . C73 C 0.28865(8) -0.1976(4) 0.71435(12) 0.0435(13) Uani 1 1 d . . . H73 H 0.2769 -0.1470 0.7241 0.052 Uiso 1 1 calc R . . C74 C 0.34150(9) -0.4169(4) 0.66238(12) 0.0477(14) Uani 1 1 d . . . H74A H 0.3384 -0.5071 0.6636 0.057 Uiso 1 1 calc R . . H74B H 0.3587 -0.4011 0.6720 0.057 Uiso 1 1 calc R . . C75 C 0.33775(9) -0.3723(4) 0.62373(13) 0.0403(12) Uani 1 1 d . . . C76 C 0.31569(10) -0.3963(4) 0.60379(15) 0.0508(14) Uani 1 1 d . . . H76 H 0.3035 -0.4441 0.6136 0.061 Uiso 1 1 calc R . . C77 C 0.31056(9) -0.3528(4) 0.56974(15) 0.0509(13) Uani 1 1 d . A . C78 C 0.32901(10) -0.2804(4) 0.55571(13) 0.0465(13) Uani 1 1 d . . . H78 H 0.3259 -0.2507 0.5327 0.056 Uiso 1 1 calc R . . C79 C 0.35164(9) -0.2514(4) 0.57461(13) 0.0377(12) Uani 1 1 d . . . C80 C 0.35607(9) -0.3010(4) 0.60880(13) 0.0364(12) Uani 1 1 d . A . C81 C 0.25417(9) 0.1405(5) 0.62758(15) 0.0590(15) Uani 1 1 d . . . C85 C 0.25448(10) -0.3649(6) 0.70415(19) 0.0758(18) Uani 1 1 d . . . C89 C 0.28514(11) -0.3748(5) 0.54767(16) 0.0679(17) Uani 1 1 d . . . C93 C 0.31058(8) 0.1495(5) 0.49101(12) 0.0435(12) Uani 1 1 d . . . C94 C 0.32099(11) 0.2688(5) 0.47492(15) 0.0808(19) Uani 1 1 d . . . H94A H 0.3103 0.2925 0.4543 0.121 Uiso 1 1 calc R . . H94B H 0.3376 0.2522 0.4686 0.121 Uiso 1 1 calc R . . H94C H 0.3216 0.3364 0.4918 0.121 Uiso 1 1 calc R . . C95 C 0.30844(11) 0.0469(5) 0.46306(14) 0.0760(18) Uani 1 1 d . . . H95A H 0.2973 0.0746 0.4432 0.114 Uiso 1 1 calc R . . H95B H 0.3019 -0.0288 0.4726 0.114 Uiso 1 1 calc R . . H95C H 0.3247 0.0299 0.4557 0.114 Uiso 1 1 calc R . . C96 C 0.28404(9) 0.1770(6) 0.50123(14) 0.0763(18) Uani 1 1 d . . . H96A H 0.2732 0.1994 0.4806 0.114 Uiso 1 1 calc R . . H96B H 0.2847 0.2458 0.5177 0.114 Uiso 1 1 calc R . . H96C H 0.2776 0.1030 0.5118 0.114 Uiso 1 1 calc R . . C97 C 0.40269(7) 0.0843(4) 0.60719(12) 0.0361(11) Uani 1 1 d . . . H97A H 0.4008 0.1756 0.6064 0.043 Uiso 1 1 calc R . . H97B H 0.4083 0.0570 0.5850 0.043 Uiso 1 1 calc R . . C98 C 0.42220(8) 0.0489(4) 0.63679(11) 0.0313(11) Uani 1 1 d . . . C99 C 0.39679(8) -0.2314(4) 0.73342(12) 0.0330(11) Uani 1 1 d . A . C100 C 0.36858(8) -0.2436(5) 0.73329(13) 0.0490(14) Uani 1 1 d . . . H10A H 0.3642 -0.3322 0.7354 0.059 Uiso 1 1 calc R . . H10B H 0.3633 -0.1993 0.7535 0.059 Uiso 1 1 calc R . . C101 C 0.40981(11) -0.4352(6) 0.64206(18) 0.0543(15) Uani 1 1 d . . . C102 C 0.40054(9) -0.3297(4) 0.61713(14) 0.0547(15) Uani 1 1 d . A . H10C H 0.4136 -0.2667 0.6162 0.066 Uiso 1 1 calc R . . H10D H 0.3966 -0.3636 0.5936 0.066 Uiso 1 1 calc R . . C103 C 0.36762(9) 0.1889(5) 0.71073(13) 0.0631(16) Uani 1 1 d . . . H10E H 0.3695 0.1399 0.7323 0.076 Uiso 1 1 calc R . . H10F H 0.3556 0.2557 0.7138 0.076 Uiso 1 1 calc R . . C104 C 0.39243(8) 0.2482(5) 0.70527(14) 0.0421(13) Uani 1 1 d . . . O1 O 0.35766(5) 0.1079(3) 0.68231(8) 0.0357(7) Uani 1 1 d . . . O2 O 0.35537(5) -0.1928(3) 0.70175(8) 0.0368(8) Uani 1 1 d . . . O3 O 0.37845(6) -0.2717(3) 0.62903(8) 0.0400(8) Uani 1 1 d . . . O4 O 0.37865(5) 0.0268(2) 0.61160(7) 0.0328(7) Uani 1 1 d . . . O5 O 0.39870(5) 0.2594(3) 0.67440(8) 0.0439(8) Uani 1 1 d . . . O6 O 0.40449(7) 0.2896(4) 0.73175(10) 0.0743(12) Uani 1 1 d . . . O7 O 0.40989(5) -0.2983(3) 0.75428(8) 0.0418(8) Uani 1 1 d . . . O8 O 0.40437(5) -0.1511(3) 0.71177(7) 0.0315(7) Uani 1 1 d . . . O9 O 0.40957(5) -0.5453(3) 0.62793(8) 0.0469(9) Uani 1 1 d D A . O11 O 0.41707(5) -0.0464(3) 0.65545(8) 0.0388(8) Uani 1 1 d . . . O12 O 0.44146(5) 0.1132(3) 0.64088(8) 0.0414(8) Uani 1 1 d . . . O13 O 0.55974(5) -0.6582(2) 0.66319(7) 0.0304(7) Uani 1 1 d . . . O14 O 0.51630(5) -0.7295(2) 0.60809(7) 0.0284(7) Uani 1 1 d . . . O15 O 0.52032(5) -1.0446(2) 0.63144(7) 0.0276(7) Uani 1 1 d . . . O16 O 0.56491(5) -0.9678(2) 0.68536(7) 0.0315(7) Uani 1 1 d . . . O17 O 0.53158(5) -0.4927(3) 0.72826(8) 0.0437(8) Uani 1 1 d . . . O18 O 0.51883(6) -0.5036(3) 0.67108(9) 0.0570(10) Uani 1 1 d . . . O19 O 0.45896(5) -0.6166(2) 0.63666(7) 0.0345(7) Uani 1 1 d . . . O20 O 0.48783(5) -0.7550(2) 0.66087(7) 0.0303(7) Uani 1 1 d . . . O21 O 0.46524(5) -1.1522(3) 0.66552(7) 0.0375(7) Uani 1 1 d . . . O22 O 0.49077(5) -0.9888(3) 0.68078(7) 0.0317(7) Uani 1 1 d . . . O23 O 0.53570(6) -0.8379(3) 0.72501(8) 0.0413(8) Uani 1 1 d . . . O24 O 0.54703(5) -0.9541(3) 0.77281(8) 0.0342(7) Uani 1 1 d . . . O5W O 0.3220(3) -0.5880(12) 0.7623(4) 0.187(6) Uani 0.50 1 d P . . O6W O 0.39003(17) -0.6245(9) 0.55770(19) 0.104(3) Uani 0.50 1 d PD . . O6W' O 0.3723(2) -0.5530(12) 0.5488(3) 0.151(5) Uiso 0.50 1 d P . . O1W O 0.5000 -0.7036(4) 0.7500 0.0606(16) Uani 1 2 d SD . . H1C H 0.5132(14) -0.743(10) 0.743(3) 0.091 Uiso 0.50 1 d PD . . H1D H 0.4868(15) -0.725(10) 0.736(3) 0.091 Uiso 0.50 1 d PD . . O2W O 0.47861(5) -0.4720(3) 0.70548(8) 0.0405(8) Uani 1 1 d D . . H2B H 0.4895(6) -0.471(4) 0.6900(9) 0.061 Uiso 1 1 d D . . H2A H 0.4668(5) -0.528(3) 0.6981(7) 0.061 Uiso 1 1 d D . . O3W O 0.45255(6) -0.2595(3) 0.72693(9) 0.0438(8) Uani 1 1 d D . . H3A H 0.4579(8) -0.322(3) 0.7163(11) 0.066 Uiso 1 1 d D . . H3B H 0.4616(7) -0.216(4) 0.7407(11) 0.066 Uiso 1 1 d D . . O4W O 0.66514(19) -0.6361(11) 0.7153(4) 0.143(5) Uani 0.50 1 d P . . O7W O 0.38093(9) 0.4806(4) 0.76906(15) 0.1098(16) Uani 1 1 d D . . H7B H 0.3643(5) 0.458(7) 0.7692(19) 0.165 Uiso 1 1 d D . . H7A H 0.3861(12) 0.438(7) 0.7500(15) 0.165 Uiso 1 1 d D . . O25 O 0.45041(5) -0.6987(3) 0.70260(8) 0.0319(8) Uani 1 1 d . . . H25 H 0.4407(8) -0.688(4) 0.7150(12) 0.048 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0251(3) 0.0509(3) 0.0354(4) 0.0198(3) 0.0092(3) 0.0083(3) Cu2 0.0305(5) 0.0509(5) 0.0375(6) 0.000 0.0098(4) 0.000 Cu3 0.0277(3) 0.0439(3) 0.0246(3) 0.0117(3) 0.0090(2) 0.0088(3) Cu4 0.0302(3) 0.0449(3) 0.0354(4) 0.0060(3) 0.0020(3) 0.0016(3) Na1 0.0303(9) 0.0448(10) 0.0290(11) 0.0045(9) 0.0020(8) 0.0042(8) Na2 0.0292(10) 0.0619(12) 0.0406(12) 0.0215(10) 0.0085(9) 0.0039(8) C1 0.035(3) 0.031(2) 0.030(3) 0.006(2) 0.011(2) -0.003(2) C2 0.032(3) 0.032(2) 0.032(3) -0.005(2) 0.008(2) -0.008(2) C3 0.028(2) 0.036(2) 0.028(3) -0.005(2) 0.008(2) -0.001(2) C4 0.036(3) 0.042(3) 0.022(3) -0.006(2) 0.007(2) -0.005(2) C5 0.034(3) 0.043(3) 0.048(4) -0.007(3) 0.008(3) 0.003(2) C6 0.040(3) 0.039(3) 0.043(3) -0.006(3) 0.019(2) -0.003(2) C7 0.042(3) 0.042(3) 0.036(3) 0.000(2) 0.014(3) -0.002(2) C8 0.033(3) 0.050(3) 0.028(3) -0.007(2) 0.004(2) 0.002(2) C9 0.035(3) 0.045(3) 0.017(3) -0.001(2) 0.005(2) 0.008(2) C10 0.026(3) 0.057(3) 0.035(3) -0.001(3) 0.003(2) -0.003(2) C11 0.035(3) 0.057(3) 0.031(3) -0.006(2) 0.001(2) 0.019(3) C12 0.040(3) 0.046(3) 0.028(3) -0.006(2) 0.004(2) 0.009(2) C13 0.032(3) 0.041(3) 0.016(3) 0.004(2) 0.006(2) 0.008(2) C14 0.026(3) 0.045(3) 0.013(3) 0.006(2) 0.004(2) 0.017(2) C15 0.040(3) 0.036(2) 0.026(3) 0.006(2) 0.011(2) 0.008(2) C16 0.025(2) 0.029(2) 0.027(3) 0.001(2) 0.008(2) -0.004(2) C17 0.025(2) 0.027(2) 0.029(3) -0.004(2) 0.011(2) -0.006(2) C18 0.030(2) 0.027(2) 0.026(3) 0.000(2) 0.010(2) -0.007(2) C19 0.039(3) 0.031(2) 0.023(3) 0.002(2) 0.008(2) -0.002(2) C20 0.035(3) 0.029(2) 0.032(3) -0.003(2) 0.014(2) -0.003(2) C21 0.032(3) 0.029(2) 0.031(3) -0.002(2) 0.006(2) 0.006(2) C22 0.028(2) 0.039(3) 0.022(3) 0.005(2) 0.005(2) -0.004(2) C23 0.023(2) 0.031(2) 0.026(3) 0.004(2) 0.005(2) 0.0028(19) C24 0.026(2) 0.030(2) 0.024(3) 0.009(2) 0.007(2) 0.007(2) C25 0.030(2) 0.029(2) 0.025(3) 0.006(2) 0.006(2) 0.003(2) C26 0.040(3) 0.033(3) 0.035(3) 0.011(2) 0.013(2) -0.002(2) C27 0.043(3) 0.037(3) 0.024(3) 0.007(2) 0.008(2) 0.003(2) C28 0.041(3) 0.037(3) 0.022(3) -0.002(2) 0.004(2) 0.002(2) C29 0.073(4) 0.046(3) 0.026(3) 0.007(2) 0.018(3) -0.006(3) C30 0.093(5) 0.072(4) 0.043(4) 0.009(3) 0.001(3) 0.004(3) C31 0.096(5) 0.085(4) 0.043(4) 0.006(3) 0.035(3) 0.018(4) C32 0.148(6) 0.102(5) 0.032(4) 0.009(3) 0.018(4) -0.061(5) C33 0.061(3) 0.051(3) 0.038(3) 0.003(3) 0.027(3) 0.011(3) C34 0.141(7) 0.099(5) 0.181(8) -0.009(5) 0.130(7) -0.034(5) C35 0.122(6) 0.141(6) 0.049(5) -0.010(4) 0.031(4) 0.056(5) C36 0.120(5) 0.108(5) 0.063(5) 0.017(4) 0.055(4) 0.065(4) C37 0.038(3) 0.068(4) 0.051(4) -0.020(3) 0.002(3) 0.014(3) C38 0.051(6) 0.127(9) 0.047(7) 0.005(6) 0.030(5) 0.047(6) C39 0.071(5) 0.098(5) 0.097(5) 0.022(4) 0.023(4) 0.034(4) C40 0.076(5) 0.103(5) 0.113(6) -0.021(4) 0.008(4) 0.016(4) C42 0.091(5) 0.081(5) 0.079(5) -0.018(4) 0.049(4) -0.005(4) C43 0.077(5) 0.119(6) 0.095(5) -0.004(4) 0.029(4) -0.014(4) C44 0.087(5) 0.113(5) 0.092(5) 0.029(4) 0.044(4) 0.012(4) C86 0.091(5) 0.117(6) 0.123(6) -0.005(5) 0.030(4) -0.016(4) C87 0.044(6) 0.152(12) 0.140(12) 0.016(10) -0.010(7) -0.049(7) C88 0.055(7) 0.122(11) 0.204(19) 0.089(13) 0.007(9) -0.031(7) C82 0.123(5) 0.123(5) 0.124(5) -0.0008(11) 0.0113(11) -0.0003(11) C83 0.020(5) 0.216(15) 0.074(8) 0.010(9) 0.010(5) 0.029(7) C84 0.104(4) 0.105(4) 0.105(4) 0.0008(11) 0.0094(11) 0.0001(11) C90 0.105(4) 0.105(4) 0.105(4) -0.0003(11) 0.0099(11) 0.0003(11) C91 0.094(9) 0.070(8) 0.146(13) 0.030(9) -0.068(9) -0.056(8) C92 0.138(6) 0.138(6) 0.138(6) 0.0000(11) 0.0129(12) -0.0002(11) O10 0.150(13) 0.066(8) 0.019(7) -0.005(6) -0.026(8) 0.035(7) O10' 0.18(3) 0.10(2) 0.045(14) 0.028(10) 0.008(12) 0.067(17) C41 0.052(3) 0.053(3) 0.056(4) 0.002(3) 0.030(3) 0.005(3) C45 0.028(2) 0.042(3) 0.027(3) 0.011(2) 0.006(2) 0.009(2) C46 0.022(3) 0.033(3) 0.029(3) -0.002(2) 0.004(2) -0.006(2) C47 0.029(2) 0.045(3) 0.034(3) -0.002(2) 0.009(2) -0.004(2) C48 0.026(3) 0.036(3) 0.023(3) 0.014(2) 0.005(2) 0.009(2) C49 0.029(3) 0.042(3) 0.036(4) -0.006(3) 0.013(3) -0.005(2) C50 0.034(3) 0.057(3) 0.027(3) -0.005(2) 0.008(2) -0.003(2) C51 0.026(3) 0.035(3) 0.029(3) -0.008(2) 0.012(2) -0.008(2) C52 0.067(3) 0.066(3) 0.025(3) 0.013(3) 0.027(3) 0.029(3) C53 0.042(3) 0.044(3) 0.031(3) 0.001(2) 0.010(2) 0.007(2) C54 0.027(2) 0.035(3) 0.030(3) 0.011(2) 0.007(2) 0.005(2) C55 0.036(3) 0.041(3) 0.026(3) -0.001(2) 0.002(2) -0.001(2) C56 0.030(3) 0.046(3) 0.030(3) 0.009(2) 0.010(2) 0.000(2) C57 0.027(3) 0.045(3) 0.032(3) 0.008(2) -0.001(2) 0.009(2) C58 0.026(2) 0.032(3) 0.028(3) 0.001(2) 0.009(2) -0.007(2) C59 0.021(2) 0.038(3) 0.022(3) 0.013(2) 0.000(2) -0.001(2) C60 0.034(3) 0.033(2) 0.030(3) 0.006(2) -0.002(2) 0.005(2) C61 0.038(3) 0.030(3) 0.027(3) -0.003(2) 0.005(2) 0.002(2) C62 0.038(3) 0.047(3) 0.035(3) 0.007(2) 0.007(3) 0.012(2) C63 0.034(3) 0.055(3) 0.041(3) 0.002(3) 0.003(2) 0.012(2) C64 0.032(3) 0.055(3) 0.042(4) 0.002(3) 0.012(3) 0.004(2) C65 0.038(3) 0.041(3) 0.027(3) -0.007(2) 0.003(2) 0.001(2) C66 0.033(3) 0.034(3) 0.028(3) -0.007(2) 0.008(2) 0.003(2) C67 0.038(3) 0.048(3) 0.027(3) -0.001(2) 0.006(2) -0.002(2) C68 0.024(2) 0.048(3) 0.032(3) 0.006(2) 0.008(2) -0.004(2) C69 0.028(3) 0.042(3) 0.035(3) 0.015(2) 0.009(2) -0.007(2) C70 0.047(3) 0.040(3) 0.041(3) 0.010(3) 0.009(2) -0.001(3) C71 0.053(3) 0.044(3) 0.060(4) 0.003(3) 0.014(3) -0.021(3) C72 0.043(3) 0.062(4) 0.051(4) 0.003(3) 0.013(3) -0.015(3) C73 0.037(3) 0.052(3) 0.043(3) 0.004(3) 0.012(2) 0.002(2) C74 0.059(3) 0.038(3) 0.048(4) 0.004(3) 0.017(3) 0.001(2) C75 0.051(3) 0.028(3) 0.043(3) 0.006(2) 0.008(3) 0.003(2) C76 0.053(4) 0.038(3) 0.063(4) 0.003(3) 0.013(3) -0.007(3) C77 0.053(3) 0.036(3) 0.062(4) -0.004(3) -0.006(3) -0.003(3) C78 0.061(4) 0.040(3) 0.038(4) 0.003(2) 0.002(3) -0.003(3) C79 0.041(3) 0.036(3) 0.037(3) 0.004(2) 0.007(3) 0.013(2) C80 0.042(3) 0.030(3) 0.037(3) -0.004(2) 0.001(3) 0.008(2) C81 0.037(3) 0.071(4) 0.069(4) 0.012(3) 0.003(3) 0.003(3) C85 0.048(4) 0.085(4) 0.098(6) -0.009(4) 0.024(4) -0.025(3) C89 0.063(4) 0.067(4) 0.073(5) 0.003(3) 0.004(3) -0.016(3) C93 0.043(3) 0.058(3) 0.027(3) 0.004(3) -0.012(2) 0.005(3) C94 0.084(4) 0.101(5) 0.051(4) 0.041(4) -0.022(3) -0.011(4) C95 0.094(5) 0.084(4) 0.045(4) -0.007(3) -0.021(3) 0.020(4) C96 0.044(3) 0.121(5) 0.059(4) -0.003(4) -0.016(3) 0.011(3) C97 0.029(3) 0.044(3) 0.035(3) 0.010(2) 0.000(2) -0.002(2) C98 0.033(3) 0.042(3) 0.021(3) 0.007(2) 0.008(2) 0.013(2) C99 0.035(3) 0.037(3) 0.030(3) -0.004(2) 0.013(2) -0.001(2) C100 0.035(3) 0.068(3) 0.046(4) 0.018(3) 0.012(3) 0.003(3) C101 0.053(4) 0.054(4) 0.058(5) 0.000(4) 0.014(4) 0.029(3) C102 0.051(3) 0.055(3) 0.060(4) 0.006(3) 0.018(3) 0.021(3) C103 0.058(4) 0.104(4) 0.028(3) -0.005(3) 0.007(3) -0.027(3) C104 0.034(3) 0.068(3) 0.022(3) 0.001(3) -0.006(3) -0.019(2) O1 0.0282(17) 0.0465(18) 0.032(2) 0.0021(15) -0.0018(15) -0.0066(14) O2 0.0256(17) 0.0519(19) 0.034(2) 0.0150(16) 0.0064(15) 0.0003(14) O3 0.0395(19) 0.0455(18) 0.036(2) 0.0058(16) 0.0108(17) 0.0113(15) O4 0.0224(16) 0.0454(18) 0.0304(19) 0.0147(15) 0.0022(14) -0.0010(14) O5 0.0325(18) 0.068(2) 0.031(2) -0.0011(17) 0.0044(16) -0.0098(16) O6 0.062(2) 0.128(3) 0.035(2) -0.018(2) 0.014(2) -0.049(2) O7 0.0356(19) 0.052(2) 0.038(2) 0.0180(17) 0.0028(16) 0.0049(16) O8 0.0216(15) 0.0398(17) 0.0338(19) 0.0111(16) 0.0072(14) 0.0009(14) O9 0.0391(19) 0.055(2) 0.045(2) 0.0190(18) -0.0060(17) 0.0075(17) O11 0.0269(17) 0.0495(19) 0.040(2) 0.0223(17) 0.0028(15) 0.0053(15) O12 0.0298(18) 0.057(2) 0.035(2) 0.0138(16) -0.0061(15) -0.0132(16) O13 0.0289(16) 0.0385(16) 0.0250(18) -0.0043(15) 0.0094(14) -0.0035(14) O14 0.0283(16) 0.0374(16) 0.0207(18) 0.0063(14) 0.0084(14) 0.0058(13) O15 0.0263(16) 0.0375(16) 0.0207(18) -0.0008(13) 0.0114(14) -0.0041(13) O16 0.0306(17) 0.0470(18) 0.0187(18) 0.0031(14) 0.0114(14) 0.0109(14) O17 0.0264(17) 0.069(2) 0.038(2) -0.0110(18) 0.0129(16) -0.0052(15) O18 0.038(2) 0.094(3) 0.040(2) -0.006(2) 0.0073(19) 0.0091(19) O19 0.0266(17) 0.0439(18) 0.034(2) 0.0133(14) 0.0090(14) 0.0103(14) O20 0.0257(16) 0.0409(18) 0.0251(19) 0.0136(15) 0.0072(14) 0.0034(14) O21 0.0267(17) 0.0480(18) 0.041(2) 0.0104(16) 0.0166(15) 0.0035(15) O22 0.0282(17) 0.0398(18) 0.0281(19) 0.0065(16) 0.0080(14) 0.0100(14) O23 0.053(2) 0.0456(19) 0.027(2) -0.0037(17) 0.0107(16) 0.0162(17) O24 0.0366(18) 0.0457(18) 0.022(2) -0.0039(15) 0.0109(15) -0.0019(14) O5W 0.162(12) 0.136(10) 0.239(17) 0.031(11) -0.095(11) -0.019(9) O6W 0.107(7) 0.114(7) 0.094(7) -0.013(6) 0.028(6) 0.002(6) O1W 0.029(3) 0.048(3) 0.108(6) 0.000 0.027(4) 0.000 O2W 0.0273(18) 0.060(2) 0.034(2) -0.0095(17) 0.0043(15) 0.0000(15) O3W 0.040(2) 0.047(2) 0.043(3) 0.0090(17) 0.0011(17) 0.0113(16) O4W 0.082(7) 0.145(10) 0.197(13) -0.087(9) -0.011(8) -0.020(7) O7W 0.089(3) 0.094(3) 0.143(5) 0.022(3) 0.001(3) 0.009(3) O25 0.0270(18) 0.0484(18) 0.0212(19) 0.0079(15) 0.0072(14) 0.0094(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O21 1.932(3) 1_565 ? Cu1 O11 1.950(3) . ? Cu1 O8 1.954(2) . ? Cu1 O3W 1.955(3) . ? Cu1 Na2 3.3600(17) . ? Cu2 O17 1.954(3) 2_656 ? Cu2 O17 1.954(3) . ? Cu2 O2W 1.964(3) . ? Cu2 O2W 1.964(3) 2_656 ? Cu2 O1W 2.226(5) . ? Cu3 O25 1.908(3) . ? Cu3 O20 1.955(2) . ? Cu3 O24 1.957(3) 2_656 ? Cu3 O22 1.987(3) . ? Cu3 O12 2.377(3) 1_545 ? Cu3 Na1 3.5359(15) . ? Cu4 O25 1.901(3) . ? Cu4 O9 1.935(3) . ? Cu4 O5 1.970(3) 1_545 ? Cu4 O19 1.990(3) . ? Cu4 H25 2.09(5) . ? Na1 O20 2.360(3) . ? Na1 O23 2.377(3) . ? Na1 O14 2.419(3) . ? Na1 O16 2.445(3) . ? Na1 O15 2.481(3) . ? Na1 O13 2.540(3) . ? Na1 O22 2.709(3) . ? Na2 O11 2.247(3) . ? Na2 O2 2.263(3) . ? Na2 O4 2.304(3) . ? Na2 O8 2.360(3) . ? Na2 O1 2.381(3) . ? Na2 O3 2.414(3) . ? Na2 C98 3.063(5) . ? C1 C25 1.510(6) . ? C1 C2 1.518(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.387(6) . ? C2 C7 1.402(5) . ? C3 C4 1.398(6) . ? C3 O13 1.403(4) . ? C4 C5 1.397(5) . ? C4 C8 1.520(6) . ? C5 C6 1.395(6) . ? C5 H5 0.9300 . ? C6 C7 1.389(6) . ? C6 C41 1.540(6) . ? C7 H7 0.9300 . ? C8 C9 1.508(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.396(5) . ? C9 C14 1.396(6) . ? C10 C11 1.390(6) . ? C10 H10 0.9300 . ? C11 C12 1.384(6) . ? C11 C37 1.537(6) . ? C12 C13 1.384(5) . ? C12 H12 0.9300 . ? C13 C14 1.381(5) . ? C13 C15 1.513(6) . ? C14 O16 1.406(4) . ? C15 C16 1.517(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.389(5) . ? C16 C21 1.395(5) . ? C17 C18 1.394(5) . ? C17 O15 1.413(4) . ? C18 C19 1.384(5) . ? C18 C22 1.530(5) . ? C19 C20 1.388(5) . ? C19 H19 0.9300 . ? C20 C21 1.380(6) . ? C20 C33 1.534(6) . ? C21 H21 0.9300 . ? C22 C23 1.517(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.381(5) . ? C23 C28 1.402(5) . ? C24 C25 1.394(5) . ? C24 O14 1.403(4) . ? C25 C26 1.401(6) . ? C26 C27 1.387(6) . ? C26 H26 0.9300 . ? C27 C28 1.392(5) . ? C27 C29 1.537(6) . ? C28 H28 0.9300 . ? C29 C32 1.512(6) . ? C29 C31 1.525(6) . ? C29 C30 1.567(7) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C36 1.504(6) . ? C33 C34 1.511(7) . ? C33 C35 1.533(8) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38' 1.39(2) . ? C37 C38 1.495(9) . ? C37 C40 1.503(11) . ? C37 C39' 1.498(15) . ? C37 C39 1.551(10) . ? C37 C40' 1.698(18) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C42 C41 1.456(9) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C41 1.538(11) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C41 1.512(11) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C86 C85 1.506(11) . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 C85 1.557(13) . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 C85 1.499(12) . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C82 C81 1.536(12) . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 C81 1.538(10) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 C81 1.494(11) . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C90 C89 1.488(11) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 C89 1.519(11) . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 C89 1.536(16) . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? O10 C101 1.179(19) . ? C38' H38D 0.9600 . ? C38' H38E 0.9600 . ? C38' H38F 0.9600 . ? C39' H39D 0.9600 . ? C39' H39E 0.9600 . ? C39' H39F 0.9600 . ? C40' H40D 0.9600 . ? C40' H40E 0.9600 . ? C40' H40F 0.9600 . ? C42' C41 1.529(16) . ? C42' H42D 0.9600 . ? C42' H42E 0.9600 . ? C42' H42F 0.9600 . ? C43' C41 1.459(15) . ? C43' H43D 0.9600 . ? C43' H43E 0.9600 . ? C43' H43F 0.9600 . ? C44' C41 1.575(19) . ? C44' H44D 0.9600 . ? C44' H44E 0.9600 . ? C44' H44F 0.9600 . ? C86' C85 1.484(19) . ? C86' H86D 0.9600 . ? C86' H86E 0.9600 . ? C86' H86F 0.9600 . ? C87' C85 1.42(3) . ? C87' H87D 0.9600 . ? C87' H87E 0.9600 . ? C87' H87F 0.9600 . ? C88' C85 1.622(16) . ? C88' H88D 0.9600 . ? C88' H88E 0.9600 . ? C88' H88F 0.9600 . ? C82' C81 1.588(16) . ? C82' H82D 0.9600 . ? C82' H82E 0.9600 . ? C82' H82F 0.9600 . ? C83' C81 1.482(19) . ? C83' H83D 0.9600 . ? C83' H83E 0.9600 . ? C83' H83F 0.9600 . ? C84' C81 1.596(15) . ? C84' H84D 0.9600 . ? C84' H84E 0.9600 . ? C84' H84F 0.9600 . ? C90' C89 1.608(16) . ? C90' H90D 0.9600 . ? C90' H90E 0.9600 . ? C90' H90F 0.9600 . ? C91' C89 1.45(3) . ? C91' H91D 0.9600 . ? C91' H91E 0.9600 . ? C91' H91F 0.9600 . ? C92' C89 1.557(19) . ? C92' H92D 0.9600 . ? C92' H92E 0.9600 . ? C92' H92F 0.9600 . ? O10' C101 1.29(3) . ? C45 O14 1.440(4) . ? C45 C46 1.502(5) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 O20 1.249(5) . ? C46 O19 1.261(5) . ? C47 O15 1.436(4) . ? C47 C48 1.502(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O22 1.247(5) . ? C48 O21 1.249(5) . ? C49 O18 1.226(5) . ? C49 O17 1.270(5) . ? C49 C50 1.521(6) . ? C50 O13 1.435(5) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O23 1.215(5) . ? C51 O24 1.282(5) . ? C51 C52 1.504(5) . ? C52 O16 1.431(5) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.506(5) . ? C53 C79 1.507(6) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.390(6) . ? C54 C59 1.392(6) . ? C55 C56 1.393(6) . ? C55 H55 0.9300 . ? C56 C57 1.371(6) . ? C56 C93 1.532(6) . ? C57 C58 1.401(6) . ? C57 H57 0.9300 . ? C58 C59 1.392(5) . ? C58 C60 1.512(5) . ? C59 O4 1.406(5) . ? C60 C61 1.520(5) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.395(6) . ? C61 C66 1.400(6) . ? C62 C63 1.373(6) . ? C62 H62 0.9300 . ? C63 C64 1.376(6) . ? C63 C81 1.542(6) . ? C64 C65 1.404(6) . ? C64 H64 0.9300 . ? C65 C66 1.403(5) . ? C65 C67 1.525(6) . ? C66 O1 1.388(5) . ? C67 C68 1.515(6) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.378(5) . ? C68 C73 1.404(5) . ? C69 C70 1.390(6) . ? C69 O2 1.396(5) . ? C70 C71 1.400(6) . ? C70 C74 1.525(6) . ? C71 C72 1.382(6) . ? C71 H71 0.9300 . ? C72 C73 1.373(6) . ? C72 C85 1.542(6) . ? C73 H73 0.9300 . ? C74 C75 1.542(6) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C76 1.362(6) . ? C75 C80 1.401(6) . ? C76 C77 1.379(7) . ? C76 H76 0.9300 . ? C77 C78 1.397(6) . ? C77 C89 1.544(7) . ? C78 C79 1.380(6) . ? C78 H78 0.9300 . ? C79 C80 1.404(6) . ? C80 O3 1.393(5) . ? C93 C95 1.517(6) . ? C93 C94 1.531(6) . ? C93 C96 1.536(6) . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C96 H96A 0.9600 . ? C96 H96B 0.9600 . ? C96 H96C 0.9600 . ? C97 O4 1.447(4) . ? C97 C98 1.506(6) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 O12 1.231(5) . ? C98 O11 1.278(5) . ? C99 O7 1.230(5) . ? C99 O8 1.278(5) . ? C99 C100 1.514(6) . ? C100 O2 1.437(5) . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? C101 O9 1.282(6) . ? C101 C102 1.516(7) . ? C102 O3 1.444(5) . ? C102 H10C 0.9700 . ? C102 H10D 0.9700 . ? C103 O1 1.442(5) . ? C103 C104 1.500(6) . ? C103 H10E 0.9700 . ? C103 H10F 0.9700 . ? C104 O6 1.224(5) . ? C104 O5 1.262(5) . ? O5 Cu4 1.970(3) 1_565 ? O12 Cu3 2.377(3) 1_565 ? O21 Cu1 1.932(3) 1_545 ? O24 Cu3 1.957(3) 2_656 ? O5W O4W 1.162(13) 2_656 ? O6W O6W' 1.232(13) . ? O1W H1C 0.89(2) . ? O1W H1D 0.88(2) . ? O2W H2B 0.872(18) . ? O2W H2A 0.894(17) . ? O3W H3A 0.843(18) . ? O3W H3B 0.819(19) . ? O4W O5W 1.162(13) 2_656 ? O7W H7B 0.92(2) . ? O7W H7A 0.92(2) . ? O25 H25 0.74(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Cu1 O11 92.28(12) 1_565 . ? O21 Cu1 O8 165.54(13) 1_565 . ? O11 Cu1 O8 82.25(11) . . ? O21 Cu1 O3W 90.02(12) 1_565 . ? O11 Cu1 O3W 167.74(13) . . ? O8 Cu1 O3W 92.63(12) . . ? O21 Cu1 Na2 127.68(9) 1_565 . ? O11 Cu1 Na2 39.96(8) . . ? O8 Cu1 Na2 43.41(8) . . ? O3W Cu1 Na2 132.00(10) . . ? O17 Cu2 O17 179.9(2) 2_656 . ? O17 Cu2 O2W 85.05(12) 2_656 . ? O17 Cu2 O2W 94.94(12) . . ? O17 Cu2 O2W 94.94(12) 2_656 2_656 ? O17 Cu2 O2W 85.05(12) . 2_656 ? O2W Cu2 O2W 167.09(18) . 2_656 ? O17 Cu2 O1W 90.05(9) 2_656 . ? O17 Cu2 O1W 90.05(9) . . ? O2W Cu2 O1W 96.45(9) . . ? O2W Cu2 O1W 96.45(9) 2_656 . ? O25 Cu3 O20 90.50(11) . . ? O25 Cu3 O24 95.23(11) . 2_656 ? O20 Cu3 O24 172.83(11) . 2_656 ? O25 Cu3 O22 172.02(12) . . ? O20 Cu3 O22 81.91(11) . . ? O24 Cu3 O22 92.16(11) 2_656 . ? O25 Cu3 O12 91.30(12) . 1_545 ? O20 Cu3 O12 82.70(11) . 1_545 ? O24 Cu3 O12 101.43(11) 2_656 1_545 ? O22 Cu3 O12 90.18(11) . 1_545 ? O25 Cu3 Na1 122.49(9) . . ? O20 Cu3 Na1 38.94(8) . . ? O24 Cu3 Na1 133.92(8) 2_656 . ? O22 Cu3 Na1 49.58(8) . . ? O12 Cu3 Na1 102.95(7) 1_545 . ? O25 Cu4 O9 159.98(14) . . ? O25 Cu4 O5 96.98(12) . 1_545 ? O9 Cu4 O5 92.41(13) . 1_545 ? O25 Cu4 O19 89.60(11) . . ? O9 Cu4 O19 88.29(12) . . ? O5 Cu4 O19 157.78(12) 1_545 . ? O25 Cu4 H25 20.7(11) . . ? O9 Cu4 H25 147.9(12) . . ? O5 Cu4 H25 81.6(12) 1_545 . ? O19 Cu4 H25 108.9(12) . . ? O20 Na1 O23 94.29(11) . . ? O20 Na1 O14 67.54(9) . . ? O23 Na1 O14 149.09(12) . . ? O20 Na1 O16 156.65(11) . . ? O23 Na1 O16 66.99(10) . . ? O14 Na1 O16 135.39(10) . . ? O20 Na1 O15 101.37(11) . . ? O23 Na1 O15 119.50(11) . . ? O14 Na1 O15 89.42(10) . . ? O16 Na1 O15 77.93(10) . . ? O20 Na1 O13 108.22(10) . . ? O23 Na1 O13 86.78(11) . . ? O14 Na1 O13 76.37(10) . . ? O16 Na1 O13 85.43(10) . . ? O15 Na1 O13 138.65(10) . . ? O20 Na1 O22 60.85(9) . . ? O23 Na1 O22 78.20(10) . . ? O14 Na1 O22 110.66(10) . . ? O16 Na1 O22 100.17(10) . . ? O15 Na1 O22 61.03(9) . . ? O13 Na1 O22 160.23(11) . . ? O20 Na1 Cu3 31.38(7) . . ? O23 Na1 Cu3 74.09(8) . . ? O14 Na1 Cu3 96.60(7) . . ? O16 Na1 Cu3 125.71(8) . . ? O15 Na1 Cu3 90.54(7) . . ? O13 Na1 Cu3 129.12(8) . . ? O22 Na1 Cu3 33.95(6) . . ? O11 Na2 O2 136.66(13) . . ? O11 Na2 O4 70.69(11) . . ? O2 Na2 O4 151.87(13) . . ? O11 Na2 O8 67.70(10) . . ? O2 Na2 O8 69.82(11) . . ? O4 Na2 O8 138.20(11) . . ? O11 Na2 O1 110.41(12) . . ? O2 Na2 O1 89.38(11) . . ? O4 Na2 O1 84.24(11) . . ? O8 Na2 O1 106.47(12) . . ? O11 Na2 O3 88.17(11) . . ? O2 Na2 O3 88.16(11) . . ? O4 Na2 O3 86.15(11) . . ? O8 Na2 O3 96.24(11) . . ? O1 Na2 O3 154.73(13) . . ? O11 Na2 C98 21.62(10) . . ? O2 Na2 C98 156.37(14) . . ? O4 Na2 C98 51.76(11) . . ? O8 Na2 C98 86.63(11) . . ? O1 Na2 C98 95.75(11) . . ? O3 Na2 C98 96.53(11) . . ? O11 Na2 Cu1 33.89(8) . . ? O2 Na2 Cu1 102.78(9) . . ? O4 Na2 Cu1 104.39(8) . . ? O8 Na2 Cu1 34.68(6) . . ? O1 Na2 Cu1 118.16(10) . . ? O3 Na2 Cu1 86.87(9) . . ? C98 Na2 Cu1 54.64(9) . . ? C25 C1 C2 110.0(3) . . ? C25 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? C25 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C3 C2 C7 118.5(4) . . ? C3 C2 C1 122.6(4) . . ? C7 C2 C1 118.7(4) . . ? C2 C3 C4 121.6(4) . . ? C2 C3 O13 118.4(4) . . ? C4 C3 O13 119.9(4) . . ? C5 C4 C3 117.6(4) . . ? C5 C4 C8 117.7(4) . . ? C3 C4 C8 124.5(4) . . ? C6 C5 C4 122.9(4) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C7 C6 C5 117.1(4) . . ? C7 C6 C41 122.0(4) . . ? C5 C6 C41 120.8(4) . . ? C6 C7 C2 122.2(4) . . ? C6 C7 H7 118.9 . . ? C2 C7 H7 118.9 . . ? C9 C8 C4 111.1(4) . . ? C9 C8 H8A 109.4 . . ? C4 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C4 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C14 116.8(4) . . ? C10 C9 C8 121.9(4) . . ? C14 C9 C8 121.2(4) . . ? C11 C10 C9 122.6(4) . . ? C11 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C12 C11 C10 117.2(4) . . ? C12 C11 C37 121.4(4) . . ? C10 C11 C37 121.3(4) . . ? C11 C12 C13 122.7(4) . . ? C11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C14 C13 C12 117.8(4) . . ? C14 C13 C15 120.9(4) . . ? C12 C13 C15 120.9(4) . . ? C13 C14 C9 122.3(4) . . ? C13 C14 O16 119.2(4) . . ? C9 C14 O16 118.4(4) . . ? C13 C15 C16 109.7(3) . . ? C13 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? C13 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C21 117.7(4) . . ? C17 C16 C15 124.0(4) . . ? C21 C16 C15 118.2(4) . . ? C16 C17 C18 121.9(4) . . ? C16 C17 O15 118.7(4) . . ? C18 C17 O15 119.3(3) . . ? C19 C18 C17 117.4(4) . . ? C19 C18 C22 118.9(4) . . ? C17 C18 C22 123.6(3) . . ? C18 C19 C20 123.3(4) . . ? C18 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C21 C20 C19 117.0(4) . . ? C21 C20 C33 122.9(4) . . ? C19 C20 C33 120.0(4) . . ? C20 C21 C16 122.8(4) . . ? C20 C21 H21 118.6 . . ? C16 C21 H21 118.6 . . ? C23 C22 C18 108.5(3) . . ? C23 C22 H22A 110.0 . . ? C18 C22 H22A 110.0 . . ? C23 C22 H22B 110.0 . . ? C18 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? C24 C23 C28 117.0(4) . . ? C24 C23 C22 121.6(4) . . ? C28 C23 C22 121.0(4) . . ? C23 C24 C25 123.0(4) . . ? C23 C24 O14 117.5(3) . . ? C25 C24 O14 119.4(4) . . ? C24 C25 C26 116.6(4) . . ? C24 C25 C1 121.2(4) . . ? C26 C25 C1 122.1(4) . . ? C27 C26 C25 123.1(4) . . ? C27 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? C26 C27 C28 116.9(4) . . ? C26 C27 C29 123.4(4) . . ? C28 C27 C29 119.7(4) . . ? C27 C28 C23 122.7(4) . . ? C27 C28 H28 118.7 . . ? C23 C28 H28 118.7 . . ? C32 C29 C31 110.6(4) . . ? C32 C29 C27 112.9(4) . . ? C31 C29 C27 110.3(4) . . ? C32 C29 C30 107.7(4) . . ? C31 C29 C30 107.5(4) . . ? C27 C29 C30 107.7(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C34 110.0(5) . . ? C36 C33 C20 112.3(4) . . ? C34 C33 C20 107.9(4) . . ? C36 C33 C35 107.1(5) . . ? C34 C33 C35 108.4(5) . . ? C20 C33 C35 111.0(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38' C37 C38 44.8(9) . . ? C38' C37 C40 130.4(10) . . ? C38 C37 C40 110.9(7) . . ? C38' C37 C39' 119.3(12) . . ? C38 C37 C39' 138.5(7) . . ? C40 C37 C39' 43.4(6) . . ? C38' C37 C11 116.4(10) . . ? C38 C37 C11 108.9(5) . . ? C40 C37 C11 112.5(5) . . ? C39' C37 C11 111.5(6) . . ? C38' C37 C39 64.4(10) . . ? C38 C37 C39 108.6(6) . . ? C40 C37 C39 106.7(7) . . ? C39' C37 C39 66.2(7) . . ? C11 C37 C39 109.1(5) . . ? C38' C37 C40' 102.4(12) . . ? C38 C37 C40' 62.9(8) . . ? C40 C37 C40' 52.6(7) . . ? C39' C37 C40' 94.9(9) . . ? C11 C37 C40' 108.9(7) . . ? C39 C37 C40' 141.6(8) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C85 C87 H87A 109.5 . . ? C85 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C85 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C85 C88 H88A 109.5 . . ? C85 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C85 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C89 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C89 C91 H91A 109.5 . . ? C89 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C89 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C89 C92 H92A 109.5 . . ? C89 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C89 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C37 C38' H38D 109.5 . . ? C37 C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C37 C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? C37 C39' H39D 109.5 . . ? C37 C39' H39E 109.5 . . ? H39D C39' H39E 109.5 . . ? C37 C39' H39F 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? C37 C40' H40D 109.5 . . ? C37 C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C37 C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? C41 C42' H42D 109.5 . . ? C41 C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? C41 C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? C41 C43' H43D 109.5 . . ? C41 C43' H43E 109.5 . . ? H43D C43' H43E 109.5 . . ? C41 C43' H43F 109.5 . . ? H43D C43' H43F 109.5 . . ? H43E C43' H43F 109.5 . . ? C41 C44' H44D 109.5 . . ? C41 C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C41 C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? C85 C86' H86D 109.5 . . ? C85 C86' H86E 109.5 . . ? H86D C86' H86E 109.5 . . ? C85 C86' H86F 109.5 . . ? H86D C86' H86F 109.5 . . ? H86E C86' H86F 109.5 . . ? C85 C87' H87D 109.5 . . ? C85 C87' H87E 109.5 . . ? H87D C87' H87E 109.5 . . ? C85 C87' H87F 109.5 . . ? H87D C87' H87F 109.5 . . ? H87E C87' H87F 109.5 . . ? C85 C88' H88D 109.5 . . ? C85 C88' H88E 109.5 . . ? H88D C88' H88E 109.5 . . ? C85 C88' H88F 109.5 . . ? H88D C88' H88F 109.5 . . ? H88E C88' H88F 109.5 . . ? C81 C82' H82D 109.5 . . ? C81 C82' H82E 109.5 . . ? H82D C82' H82E 109.5 . . ? C81 C82' H82F 109.5 . . ? H82D C82' H82F 109.5 . . ? H82E C82' H82F 109.5 . . ? C81 C83' H83D 109.5 . . ? C81 C83' H83E 109.5 . . ? H83D C83' H83E 109.5 . . ? C81 C83' H83F 109.5 . . ? H83D C83' H83F 109.5 . . ? H83E C83' H83F 109.5 . . ? C81 C84' H84D 109.5 . . ? C81 C84' H84E 109.5 . . ? H84D C84' H84E 109.5 . . ? C81 C84' H84F 109.5 . . ? H84D C84' H84F 109.5 . . ? H84E C84' H84F 109.5 . . ? C89 C90' H90D 109.5 . . ? C89 C90' H90E 109.5 . . ? H90D C90' H90E 109.5 . . ? C89 C90' H90F 109.5 . . ? H90D C90' H90F 109.5 . . ? H90E C90' H90F 109.5 . . ? C89 C91' H91D 109.5 . . ? C89 C91' H91E 109.5 . . ? H91D C91' H91E 109.5 . . ? C89 C91' H91F 109.5 . . ? H91D C91' H91F 109.5 . . ? H91E C91' H91F 109.5 . . ? C89 C92' H92D 109.5 . . ? C89 C92' H92E 109.5 . . ? H92D C92' H92E 109.5 . . ? C89 C92' H92F 109.5 . . ? H92D C92' H92F 109.5 . . ? H92E C92' H92F 109.5 . . ? C42 C41 C43' 140.3(7) . . ? C42 C41 C44 111.2(7) . . ? C43' C41 C44 50.0(7) . . ? C42 C41 C42' 56.2(7) . . ? C43' C41 C42' 107.9(10) . . ? C44 C41 C42' 133.5(8) . . ? C42 C41 C43 108.7(7) . . ? C43' C41 C43 58.4(8) . . ? C44 C41 C43 104.9(7) . . ? C42' C41 C43 54.2(7) . . ? C42 C41 C6 109.4(5) . . ? C43' C41 C6 110.2(7) . . ? C44 C41 C6 112.7(5) . . ? C42' C41 C6 113.5(7) . . ? C43 C41 C6 109.8(5) . . ? C42 C41 C44' 57.7(8) . . ? C43' C41 C44' 108.1(11) . . ? C44 C41 C44' 59.4(8) . . ? C42' C41 C44' 110.2(10) . . ? C43 C41 C44' 143.4(8) . . ? C6 C41 C44' 106.8(7) . . ? O14 C45 C46 112.3(3) . . ? O14 C45 H45A 109.2 . . ? C46 C45 H45A 109.2 . . ? O14 C45 H45B 109.2 . . ? C46 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? O20 C46 O19 128.0(4) . . ? O20 C46 C45 118.6(4) . . ? O19 C46 C45 113.3(4) . . ? O15 C47 C48 110.9(3) . . ? O15 C47 H47A 109.5 . . ? C48 C47 H47A 109.5 . . ? O15 C47 H47B 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 108.0 . . ? O22 C48 O21 127.8(4) . . ? O22 C48 C47 119.3(4) . . ? O21 C48 C47 112.9(4) . . ? O18 C49 O17 125.9(4) . . ? O18 C49 C50 120.7(4) . . ? O17 C49 C50 113.4(4) . . ? O13 C50 C49 111.0(4) . . ? O13 C50 H50A 109.4 . . ? C49 C50 H50A 109.4 . . ? O13 C50 H50B 109.4 . . ? C49 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? O23 C51 O24 126.6(4) . . ? O23 C51 C52 120.3(4) . . ? O24 C51 C52 113.0(4) . . ? O16 C52 C51 111.6(4) . . ? O16 C52 H52A 109.3 . . ? C51 C52 H52A 109.3 . . ? O16 C52 H52B 109.3 . . ? C51 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? C54 C53 C79 109.9(3) . . ? C54 C53 H53A 109.7 . . ? C79 C53 H53A 109.7 . . ? C54 C53 H53B 109.7 . . ? C79 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? C55 C54 C59 117.6(4) . . ? C55 C54 C53 120.6(4) . . ? C59 C54 C53 121.4(4) . . ? C54 C55 C56 122.7(4) . . ? C54 C55 H55 118.7 . . ? C56 C55 H55 118.7 . . ? C57 C56 C55 116.8(4) . . ? C57 C56 C93 121.0(4) . . ? C55 C56 C93 122.2(4) . . ? C56 C57 C58 123.8(4) . . ? C56 C57 H57 118.1 . . ? C58 C57 H57 118.1 . . ? C59 C58 C57 116.5(4) . . ? C59 C58 C60 121.6(4) . . ? C57 C58 C60 121.5(4) . . ? C58 C59 C54 122.1(4) . . ? C58 C59 O4 119.7(4) . . ? C54 C59 O4 118.2(4) . . ? C58 C60 C61 110.5(3) . . ? C58 C60 H60A 109.6 . . ? C61 C60 H60A 109.6 . . ? C58 C60 H60B 109.6 . . ? C61 C60 H60B 109.6 . . ? H60A C60 H60B 108.1 . . ? C62 C61 C66 117.7(4) . . ? C62 C61 C60 119.3(4) . . ? C66 C61 C60 122.9(4) . . ? C63 C62 C61 123.6(4) . . ? C63 C62 H62 118.2 . . ? C61 C62 H62 118.2 . . ? C62 C63 C64 117.1(4) . . ? C62 C63 C81 122.2(4) . . ? C64 C63 C81 120.5(4) . . ? C63 C64 C65 123.2(4) . . ? C63 C64 H64 118.4 . . ? C65 C64 H64 118.4 . . ? C64 C65 C66 117.4(4) . . ? C64 C65 C67 118.5(4) . . ? C66 C65 C67 123.9(4) . . ? O1 C66 C61 118.6(4) . . ? O1 C66 C65 120.2(4) . . ? C61 C66 C65 121.1(4) . . ? C68 C67 C65 109.1(4) . . ? C68 C67 H67A 109.9 . . ? C65 C67 H67A 109.9 . . ? C68 C67 H67B 109.9 . . ? C65 C67 H67B 109.9 . . ? H67A C67 H67B 108.3 . . ? C69 C68 C73 117.1(4) . . ? C69 C68 C67 121.3(4) . . ? C73 C68 C67 121.3(4) . . ? C68 C69 C70 122.7(4) . . ? C68 C69 O2 118.5(4) . . ? C70 C69 O2 118.8(4) . . ? C69 C70 C71 116.9(4) . . ? C69 C70 C74 120.9(4) . . ? C71 C70 C74 122.0(4) . . ? C72 C71 C70 122.5(4) . . ? C72 C71 H71 118.8 . . ? C70 C71 H71 118.8 . . ? C73 C72 C71 117.7(4) . . ? C73 C72 C85 121.5(5) . . ? C71 C72 C85 120.7(5) . . ? C72 C73 C68 122.6(4) . . ? C72 C73 H73 118.7 . . ? C68 C73 H73 118.7 . . ? C70 C74 C75 109.5(4) . . ? C70 C74 H74A 109.8 . . ? C75 C74 H74A 109.8 . . ? C70 C74 H74B 109.8 . . ? C75 C74 H74B 109.8 . . ? H74A C74 H74B 108.2 . . ? C76 C75 C80 118.3(5) . . ? C76 C75 C74 120.0(4) . . ? C80 C75 C74 121.6(5) . . ? C75 C76 C77 122.9(5) . . ? C75 C76 H76 118.5 . . ? C77 C76 H76 118.5 . . ? C76 C77 C78 117.5(5) . . ? C76 C77 C89 123.0(5) . . ? C78 C77 C89 119.4(5) . . ? C79 C78 C77 122.5(5) . . ? C79 C78 H78 118.7 . . ? C77 C78 H78 118.7 . . ? C78 C79 C80 117.4(4) . . ? C78 C79 C53 118.6(4) . . ? C80 C79 C53 123.9(4) . . ? O3 C80 C75 119.4(4) . . ? O3 C80 C79 119.2(4) . . ? C75 C80 C79 121.2(4) . . ? C84 C81 C83' 130.6(10) . . ? C84 C81 C84' 36.7(6) . . ? C83' C81 C84' 114.8(10) . . ? C84 C81 C82 108.6(8) . . ? C83' C81 C82 69.0(9) . . ? C84' C81 C82 140.2(9) . . ? C84 C81 C63 113.3(6) . . ? C83' C81 C63 114.6(9) . . ? C84' C81 C63 107.4(7) . . ? C82 C81 C63 105.6(6) . . ? C84 C81 C83 107.0(7) . . ? C83' C81 C83 43.1(7) . . ? C84' C81 C83 76.4(8) . . ? C82 C81 C83 111.0(8) . . ? C63 C81 C83 111.4(5) . . ? C84 C81 C82' 68.7(8) . . ? C83' C81 C82' 104.8(11) . . ? C84' C81 C82' 104.7(9) . . ? C82 C81 C82' 42.1(6) . . ? C63 C81 C82' 109.9(7) . . ? C83 C81 C82' 136.0(8) . . ? C87' C85 C86' 115.8(14) . . ? C87' C85 C88 37.4(10) . . ? C86' C85 C88 136.5(9) . . ? C87' C85 C86 130.9(11) . . ? C86' C85 C86 54.3(8) . . ? C88 C85 C86 111.2(9) . . ? C87' C85 C72 113.9(11) . . ? C86' C85 C72 112.4(8) . . ? C88 C85 C72 110.8(6) . . ? C86 C85 C72 113.4(6) . . ? C87' C85 C87 70.6(11) . . ? C86' C85 C87 54.4(9) . . ? C88 C85 C87 106.8(9) . . ? C86 C85 C87 106.3(8) . . ? C72 C85 C87 107.8(5) . . ? C87' C85 C88' 104.8(12) . . ? C86' C85 C88' 102.9(11) . . ? C88 C85 C88' 69.8(9) . . ? C86 C85 C88' 49.4(7) . . ? C72 C85 C88' 105.5(7) . . ? C87 C85 C88' 145.1(8) . . ? C91' C89 C90 74.6(12) . . ? C91' C89 C91 34.6(13) . . ? C90 C89 C91 108.4(9) . . ? C91' C89 C92 128.3(16) . . ? C90 C89 C92 109.2(8) . . ? C91 C89 C92 108.6(9) . . ? C91' C89 C77 113.2(15) . . ? C90 C89 C77 106.3(6) . . ? C91 C89 C77 109.7(6) . . ? C92 C89 C77 114.5(7) . . ? C91' C89 C92' 117.0(15) . . ? C90 C89 C92' 130.8(10) . . ? C91 C89 C92' 88.8(10) . . ? C92 C89 C92' 24.4(9) . . ? C77 C89 C92' 110.4(8) . . ? C91' C89 C90' 104.6(14) . . ? C90 C89 C90' 33.0(7) . . ? C91 C89 C90' 134.3(9) . . ? C92 C89 C90' 79.9(9) . . ? C77 C89 C90' 106.4(7) . . ? C92' C89 C90' 103.9(10) . . ? C95 C93 C94 108.1(4) . . ? C95 C93 C56 113.1(4) . . ? C94 C93 C56 108.7(4) . . ? C95 C93 C96 107.9(4) . . ? C94 C93 C96 109.2(4) . . ? C56 C93 C96 109.8(4) . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C93 C95 H95A 109.5 . . ? C93 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C93 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C93 C96 H96A 109.5 . . ? C93 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C93 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? O4 C97 C98 111.4(3) . . ? O4 C97 H97A 109.3 . . ? C98 C97 H97A 109.3 . . ? O4 C97 H97B 109.3 . . ? C98 C97 H97B 109.3 . . ? H97A C97 H97B 108.0 . . ? O12 C98 O11 126.0(4) . . ? O12 C98 C97 117.8(4) . . ? O11 C98 C97 116.2(4) . . ? O12 C98 Na2 152.8(3) . . ? O11 C98 Na2 40.35(19) . . ? C97 C98 Na2 81.3(2) . . ? O7 C99 O8 127.1(4) . . ? O7 C99 C100 117.2(4) . . ? O8 C99 C100 115.8(4) . . ? O2 C100 C99 112.2(3) . . ? O2 C100 H10A 109.2 . . ? C99 C100 H10A 109.2 . . ? O2 C100 H10B 109.2 . . ? C99 C100 H10B 109.2 . . ? H10A C100 H10B 107.9 . . ? O10 C101 O9 127.8(10) . . ? O10 C101 O10' 31.3(19) . . ? O9 C101 O10' 112.6(16) . . ? O10 C101 C102 116.3(10) . . ? O9 C101 C102 114.5(6) . . ? O10' C101 C102 129.7(17) . . ? O3 C102 C101 110.0(4) . . ? O3 C102 H10C 109.7 . . ? C101 C102 H10C 109.7 . . ? O3 C102 H10D 109.7 . . ? C101 C102 H10D 109.7 . . ? H10C C102 H10D 108.2 . . ? O1 C103 C104 114.1(4) . . ? O1 C103 H10E 108.7 . . ? C104 C103 H10E 108.7 . . ? O1 C103 H10F 108.7 . . ? C104 C103 H10F 108.7 . . ? H10E C103 H10F 107.6 . . ? O6 C104 O5 124.7(4) . . ? O6 C104 C103 115.8(4) . . ? O5 C104 C103 119.3(4) . . ? C66 O1 C103 116.5(3) . . ? C66 O1 Na2 115.6(2) . . ? C103 O1 Na2 125.9(3) . . ? C69 O2 C100 109.6(3) . . ? C69 O2 Na2 130.6(3) . . ? C100 O2 Na2 119.7(2) . . ? C80 O3 C102 114.6(4) . . ? C80 O3 Na2 114.2(2) . . ? C102 O3 Na2 127.2(3) . . ? C59 O4 C97 111.1(3) . . ? C59 O4 Na2 133.6(2) . . ? C97 O4 Na2 115.3(2) . . ? C104 O5 Cu4 124.7(3) . 1_565 ? C99 O8 Cu1 129.6(3) . . ? C99 O8 Na2 119.7(3) . . ? Cu1 O8 Na2 101.92(12) . . ? C101 O9 Cu4 105.0(3) . . ? C98 O11 Cu1 131.7(3) . . ? C98 O11 Na2 118.0(3) . . ? Cu1 O11 Na2 106.15(13) . . ? C98 O12 Cu3 129.1(3) . 1_565 ? C3 O13 C50 114.9(3) . . ? C3 O13 Na1 124.4(2) . . ? C50 O13 Na1 118.9(2) . . ? C24 O14 C45 106.8(3) . . ? C24 O14 Na1 136.4(2) . . ? C45 O14 Na1 116.8(2) . . ? C17 O15 C47 112.4(3) . . ? C17 O15 Na1 120.4(2) . . ? C47 O15 Na1 127.1(2) . . ? C14 O16 C52 107.8(3) . . ? C14 O16 Na1 139.1(2) . . ? C52 O16 Na1 113.0(2) . . ? C49 O17 Cu2 126.9(3) . . ? C46 O19 Cu4 128.4(3) . . ? C46 O20 Cu3 126.3(2) . . ? C46 O20 Na1 122.8(2) . . ? Cu3 O20 Na1 109.69(13) . . ? C48 O21 Cu1 132.7(3) . 1_545 ? C48 O22 Cu3 127.0(3) . . ? C48 O22 Na1 121.0(2) . . ? Cu3 O22 Na1 96.47(11) . . ? C51 O23 Na1 119.3(3) . . ? C51 O24 Cu3 123.3(3) . 2_656 ? Cu2 O1W H1C 118(7) . . ? Cu2 O1W H1D 105(7) . . ? H1C O1W H1D 107(3) . . ? Cu2 O2W H2B 102(3) . . ? Cu2 O2W H2A 122.2(19) . . ? H2B O2W H2A 107(3) . . ? Cu1 O3W H3A 110(3) . . ? Cu1 O3W H3B 104(4) . . ? H3A O3W H3B 123(3) . . ? H7B O7W H7A 104(3) . . ? Cu4 O25 Cu3 110.01(15) . . ? Cu4 O25 H25 94(4) . . ? Cu3 O25 H25 130(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O25 Cu3 Na1 O20 -39.49(18) . . . . ? O24 Cu3 Na1 O20 -179.22(18) 2_656 . . . ? O22 Cu3 Na1 O20 139.48(18) . . . . ? O12 Cu3 Na1 O20 60.53(15) 1_545 . . . ? O25 Cu3 Na1 O23 88.59(14) . . . . ? O20 Cu3 Na1 O23 128.08(16) . . . . ? O24 Cu3 Na1 O23 -51.15(15) 2_656 . . . ? O22 Cu3 Na1 O23 -92.44(14) . . . . ? O12 Cu3 Na1 O23 -171.39(11) 1_545 . . . ? O25 Cu3 Na1 O14 -61.31(14) . . . . ? O20 Cu3 Na1 O14 -21.82(14) . . . . ? O24 Cu3 Na1 O14 158.96(14) 2_656 . . . ? O22 Cu3 Na1 O14 117.66(14) . . . . ? O12 Cu3 Na1 O14 38.71(10) 1_545 . . . ? O25 Cu3 Na1 O16 133.74(15) . . . . ? O20 Cu3 Na1 O16 173.22(18) . . . . ? O24 Cu3 Na1 O16 -6.00(18) 2_656 . . . ? O22 Cu3 Na1 O16 -47.29(15) . . . . ? O12 Cu3 Na1 O16 -126.25(12) 1_545 . . . ? O25 Cu3 Na1 O15 -150.78(13) . . . . ? O20 Cu3 Na1 O15 -111.30(16) . . . . ? O24 Cu3 Na1 O15 69.48(15) 2_656 . . . ? O22 Cu3 Na1 O15 28.18(13) . . . . ? O12 Cu3 Na1 O15 -50.77(10) 1_545 . . . ? O25 Cu3 Na1 O13 16.47(16) . . . . ? O20 Cu3 Na1 O13 55.96(16) . . . . ? O24 Cu3 Na1 O13 -123.26(16) 2_656 . . . ? O22 Cu3 Na1 O13 -164.56(16) . . . . ? O12 Cu3 Na1 O13 116.49(12) 1_545 . . . ? O25 Cu3 Na1 O22 -178.97(16) . . . . ? O20 Cu3 Na1 O22 -139.48(18) . . . . ? O24 Cu3 Na1 O22 41.29(17) 2_656 . . . ? O12 Cu3 Na1 O22 -78.95(13) 1_545 . . . ? O21 Cu1 Na2 O11 -32.48(19) 1_565 . . . ? O8 Cu1 Na2 O11 162.94(19) . . . . ? O3W Cu1 Na2 O11 -166.61(19) . . . . ? O21 Cu1 Na2 O2 146.29(14) 1_565 . . . ? O11 Cu1 Na2 O2 178.77(18) . . . . ? O8 Cu1 Na2 O2 -18.28(14) . . . . ? O3W Cu1 Na2 O2 12.17(17) . . . . ? O21 Cu1 Na2 O4 -26.33(15) 1_565 . . . ? O11 Cu1 Na2 O4 6.16(16) . . . . ? O8 Cu1 Na2 O4 169.10(16) . . . . ? O3W Cu1 Na2 O4 -160.45(15) . . . . ? O21 Cu1 Na2 O8 164.57(16) 1_565 . . . ? O11 Cu1 Na2 O8 -162.94(19) . . . . ? O3W Cu1 Na2 O8 30.45(18) . . . . ? O21 Cu1 Na2 O1 -117.46(14) 1_565 . . . ? O11 Cu1 Na2 O1 -84.98(17) . . . . ? O8 Cu1 Na2 O1 77.96(15) . . . . ? O3W Cu1 Na2 O1 108.42(16) . . . . ? O21 Cu1 Na2 O3 58.89(14) 1_565 . . . ? O11 Cu1 Na2 O3 91.38(16) . . . . ? O8 Cu1 Na2 O3 -105.68(14) . . . . ? O3W Cu1 Na2 O3 -75.23(16) . . . . ? O21 Cu1 Na2 C98 -41.38(15) 1_565 . . . ? O11 Cu1 Na2 C98 -8.90(17) . . . . ? O8 Cu1 Na2 C98 154.05(16) . . . . ? O3W Cu1 Na2 C98 -175.50(17) . . . . ? C25 C1 C2 C3 -103.7(4) . . . . ? C25 C1 C2 C7 71.2(5) . . . . ? C7 C2 C3 C4 -1.4(6) . . . . ? C1 C2 C3 C4 173.5(4) . . . . ? C7 C2 C3 O13 -178.2(3) . . . . ? C1 C2 C3 O13 -3.3(6) . . . . ? C2 C3 C4 C5 1.7(6) . . . . ? O13 C3 C4 C5 178.4(4) . . . . ? C2 C3 C4 C8 -173.9(4) . . . . ? O13 C3 C4 C8 2.8(6) . . . . ? C3 C4 C5 C6 -1.1(6) . . . . ? C8 C4 C5 C6 174.9(4) . . . . ? C4 C5 C6 C7 0.2(7) . . . . ? C4 C5 C6 C41 -177.2(4) . . . . ? C5 C6 C7 C2 0.2(6) . . . . ? C41 C6 C7 C2 177.5(4) . . . . ? C3 C2 C7 C6 0.5(6) . . . . ? C1 C2 C7 C6 -174.7(4) . . . . ? C5 C4 C8 C9 -65.1(5) . . . . ? C3 C4 C8 C9 110.5(5) . . . . ? C4 C8 C9 C10 87.1(5) . . . . ? C4 C8 C9 C14 -89.2(5) . . . . ? C14 C9 C10 C11 3.1(6) . . . . ? C8 C9 C10 C11 -173.3(4) . . . . ? C9 C10 C11 C12 3.3(7) . . . . ? C9 C10 C11 C37 179.8(4) . . . . ? C10 C11 C12 C13 -4.8(7) . . . . ? C37 C11 C12 C13 178.7(4) . . . . ? C11 C12 C13 C14 -0.3(6) . . . . ? C11 C12 C13 C15 172.6(4) . . . . ? C12 C13 C14 C9 7.3(6) . . . . ? C15 C13 C14 C9 -165.7(4) . . . . ? C12 C13 C14 O16 -170.8(3) . . . . ? C15 C13 C14 O16 16.3(6) . . . . ? C10 C9 C14 C13 -8.6(6) . . . . ? C8 C9 C14 C13 167.8(4) . . . . ? C10 C9 C14 O16 169.5(3) . . . . ? C8 C9 C14 O16 -14.1(6) . . . . ? C14 C13 C15 C16 81.2(5) . . . . ? C12 C13 C15 C16 -91.5(4) . . . . ? C13 C15 C16 C17 -106.6(4) . . . . ? C13 C15 C16 C21 68.7(5) . . . . ? C21 C16 C17 C18 -1.7(6) . . . . ? C15 C16 C17 C18 173.7(4) . . . . ? C21 C16 C17 O15 -178.0(3) . . . . ? C15 C16 C17 O15 -2.6(6) . . . . ? C16 C17 C18 C19 1.9(6) . . . . ? O15 C17 C18 C19 178.2(3) . . . . ? C16 C17 C18 C22 -175.4(4) . . . . ? O15 C17 C18 C22 0.9(6) . . . . ? C17 C18 C19 C20 -1.8(6) . . . . ? C22 C18 C19 C20 175.6(3) . . . . ? C18 C19 C20 C21 1.4(6) . . . . ? C18 C19 C20 C33 -174.6(4) . . . . ? C19 C20 C21 C16 -1.2(6) . . . . ? C33 C20 C21 C16 174.8(4) . . . . ? C17 C16 C21 C20 1.3(6) . . . . ? C15 C16 C21 C20 -174.3(4) . . . . ? C19 C18 C22 C23 -62.2(5) . . . . ? C17 C18 C22 C23 115.1(4) . . . . ? C18 C22 C23 C24 -87.1(4) . . . . ? C18 C22 C23 C28 85.7(5) . . . . ? C28 C23 C24 C25 -8.8(6) . . . . ? C22 C23 C24 C25 164.3(4) . . . . ? C28 C23 C24 O14 168.4(3) . . . . ? C22 C23 C24 O14 -18.5(5) . . . . ? C23 C24 C25 C26 7.7(6) . . . . ? O14 C24 C25 C26 -169.5(3) . . . . ? C23 C24 C25 C1 -168.9(4) . . . . ? O14 C24 C25 C1 13.9(5) . . . . ? C2 C1 C25 C24 86.5(4) . . . . ? C2 C1 C25 C26 -89.9(5) . . . . ? C24 C25 C26 C27 -0.3(6) . . . . ? C1 C25 C26 C27 176.3(4) . . . . ? C25 C26 C27 C28 -5.3(6) . . . . ? C25 C26 C27 C29 175.3(4) . . . . ? C26 C27 C28 C23 4.0(6) . . . . ? C29 C27 C28 C23 -176.5(4) . . . . ? C24 C23 C28 C27 2.8(6) . . . . ? C22 C23 C28 C27 -170.4(4) . . . . ? C26 C27 C29 C32 -0.7(7) . . . . ? C28 C27 C29 C32 179.9(4) . . . . ? C26 C27 C29 C31 123.5(5) . . . . ? C28 C27 C29 C31 -55.9(6) . . . . ? C26 C27 C29 C30 -119.4(5) . . . . ? C28 C27 C29 C30 61.1(5) . . . . ? C21 C20 C33 C36 22.8(7) . . . . ? C19 C20 C33 C36 -161.4(5) . . . . ? C21 C20 C33 C34 -98.6(6) . . . . ? C19 C20 C33 C34 77.2(6) . . . . ? C21 C20 C33 C35 142.7(5) . . . . ? C19 C20 C33 C35 -41.5(6) . . . . ? C12 C11 C37 C38' 18.5(14) . . . . ? C10 C11 C37 C38' -157.8(12) . . . . ? C12 C11 C37 C38 66.7(8) . . . . ? C10 C11 C37 C38 -109.6(7) . . . . ? C12 C11 C37 C40 -169.9(7) . . . . ? C10 C11 C37 C40 13.7(9) . . . . ? C12 C11 C37 C39' -122.9(8) . . . . ? C10 C11 C37 C39' 60.7(9) . . . . ? C12 C11 C37 C39 -51.7(7) . . . . ? C10 C11 C37 C39 131.9(6) . . . . ? C12 C11 C37 C40' 133.6(9) . . . . ? C10 C11 C37 C40' -42.7(10) . . . . ? C7 C6 C41 C42 -109.8(7) . . . . ? C5 C6 C41 C42 67.5(8) . . . . ? C7 C6 C41 C43' 68.5(10) . . . . ? C5 C6 C41 C43' -114.3(10) . . . . ? C7 C6 C41 C44 14.5(8) . . . . ? C5 C6 C41 C44 -168.3(7) . . . . ? C7 C6 C41 C42' -170.4(9) . . . . ? C5 C6 C41 C42' 6.8(10) . . . . ? C7 C6 C41 C43 131.0(6) . . . . ? C5 C6 C41 C43 -51.7(7) . . . . ? C7 C6 C41 C44' -48.7(10) . . . . ? C5 C6 C41 C44' 128.5(9) . . . . ? O14 C45 C46 O20 1.7(5) . . . . ? O14 C45 C46 O19 -176.6(3) . . . . ? O15 C47 C48 O22 -8.2(5) . . . . ? O15 C47 C48 O21 170.5(3) . . . . ? O18 C49 C50 O13 -34.7(6) . . . . ? O17 C49 C50 O13 147.3(4) . . . . ? O23 C51 C52 O16 4.4(6) . . . . ? O24 C51 C52 O16 -174.1(4) . . . . ? C79 C53 C54 C55 -85.8(5) . . . . ? C79 C53 C54 C59 86.9(5) . . . . ? C59 C54 C55 C56 -2.0(6) . . . . ? C53 C54 C55 C56 171.0(4) . . . . ? C54 C55 C56 C57 -2.8(6) . . . . ? C54 C55 C56 C93 178.2(4) . . . . ? C55 C56 C57 C58 2.7(6) . . . . ? C93 C56 C57 C58 -178.3(4) . . . . ? C56 C57 C58 C59 2.2(6) . . . . ? C56 C57 C58 C60 -171.2(4) . . . . ? C57 C58 C59 C54 -7.3(5) . . . . ? C60 C58 C59 C54 166.0(4) . . . . ? C57 C58 C59 O4 175.6(3) . . . . ? C60 C58 C59 O4 -11.0(5) . . . . ? C55 C54 C59 C58 7.3(6) . . . . ? C53 C54 C59 C58 -165.7(3) . . . . ? C55 C54 C59 O4 -175.6(3) . . . . ? C53 C54 C59 O4 11.4(5) . . . . ? C59 C58 C60 C61 -85.8(5) . . . . ? C57 C58 C60 C61 87.2(4) . . . . ? C58 C60 C61 C62 -66.8(5) . . . . ? C58 C60 C61 C66 107.9(5) . . . . ? C66 C61 C62 C63 0.2(6) . . . . ? C60 C61 C62 C63 175.1(4) . . . . ? C61 C62 C63 C64 0.4(7) . . . . ? C61 C62 C63 C81 -174.4(4) . . . . ? C62 C63 C64 C65 -1.1(7) . . . . ? C81 C63 C64 C65 173.8(4) . . . . ? C63 C64 C65 C66 1.1(7) . . . . ? C63 C64 C65 C67 -174.2(4) . . . . ? C62 C61 C66 O1 175.6(3) . . . . ? C60 C61 C66 O1 0.8(6) . . . . ? C62 C61 C66 C65 -0.1(6) . . . . ? C60 C61 C66 C65 -174.9(4) . . . . ? C64 C65 C66 O1 -176.1(4) . . . . ? C67 C65 C66 O1 -1.1(6) . . . . ? C64 C65 C66 C61 -0.5(6) . . . . ? C67 C65 C66 C61 174.6(4) . . . . ? C64 C65 C67 C68 65.6(5) . . . . ? C66 C65 C67 C68 -109.4(4) . . . . ? C65 C67 C68 C69 86.7(5) . . . . ? C65 C67 C68 C73 -86.5(5) . . . . ? C73 C68 C69 C70 7.9(6) . . . . ? C67 C68 C69 C70 -165.5(4) . . . . ? C73 C68 C69 O2 -172.2(4) . . . . ? C67 C68 C69 O2 14.4(6) . . . . ? C68 C69 C70 C71 -7.6(7) . . . . ? O2 C69 C70 C71 172.5(4) . . . . ? C68 C69 C70 C74 166.6(4) . . . . ? O2 C69 C70 C74 -13.3(6) . . . . ? C69 C70 C71 C72 1.6(7) . . . . ? C74 C70 C71 C72 -172.6(4) . . . . ? C70 C71 C72 C73 3.6(8) . . . . ? C70 C71 C72 C85 -178.9(5) . . . . ? C71 C72 C73 C68 -3.2(7) . . . . ? C85 C72 C73 C68 179.3(5) . . . . ? C69 C68 C73 C72 -2.3(7) . . . . ? C67 C68 C73 C72 171.2(4) . . . . ? C69 C70 C74 C75 -88.3(5) . . . . ? C71 C70 C74 C75 85.6(5) . . . . ? C70 C74 C75 C76 -65.8(5) . . . . ? C70 C74 C75 C80 110.7(5) . . . . ? C80 C75 C76 C77 -0.4(7) . . . . ? C74 C75 C76 C77 176.2(4) . . . . ? C75 C76 C77 C78 -0.4(7) . . . . ? C75 C76 C77 C89 -177.2(5) . . . . ? C76 C77 C78 C79 -0.4(7) . . . . ? C89 C77 C78 C79 176.5(4) . . . . ? C77 C78 C79 C80 2.0(7) . . . . ? C77 C78 C79 C53 -174.0(4) . . . . ? C54 C53 C79 C78 66.4(5) . . . . ? C54 C53 C79 C80 -109.3(5) . . . . ? C76 C75 C80 O3 177.9(4) . . . . ? C74 C75 C80 O3 1.3(6) . . . . ? C76 C75 C80 C79 2.2(6) . . . . ? C74 C75 C80 C79 -174.4(4) . . . . ? C78 C79 C80 O3 -178.6(4) . . . . ? C53 C79 C80 O3 -2.9(6) . . . . ? C78 C79 C80 C75 -2.9(6) . . . . ? C53 C79 C80 C75 172.9(4) . . . . ? C62 C63 C81 C84 -32.7(8) . . . . ? C64 C63 C81 C84 152.6(7) . . . . ? C62 C63 C81 C83' 159.7(10) . . . . ? C64 C63 C81 C83' -15.0(11) . . . . ? C62 C63 C81 C84' -71.5(9) . . . . ? C64 C63 C81 C84' 113.9(8) . . . . ? C62 C63 C81 C82 86.1(7) . . . . ? C64 C63 C81 C82 -88.6(7) . . . . ? C62 C63 C81 C83 -153.3(7) . . . . ? C64 C63 C81 C83 32.0(9) . . . . ? C62 C63 C81 C82' 42.0(9) . . . . ? C64 C63 C81 C82' -132.7(8) . . . . ? C73 C72 C85 C87' -174.4(13) . . . . ? C71 C72 C85 C87' 8.2(14) . . . . ? C73 C72 C85 C86' 51.4(13) . . . . ? C71 C72 C85 C86' -126.0(11) . . . . ? C73 C72 C85 C88 -133.9(10) . . . . ? C71 C72 C85 C88 48.7(11) . . . . ? C73 C72 C85 C86 -7.9(10) . . . . ? C71 C72 C85 C86 174.7(8) . . . . ? C73 C72 C85 C87 109.5(8) . . . . ? C71 C72 C85 C87 -67.9(8) . . . . ? C73 C72 C85 C88' -60.0(9) . . . . ? C71 C72 C85 C88' 122.6(8) . . . . ? C76 C77 C89 C91' 2.5(15) . . . . ? C78 C77 C89 C91' -174.2(14) . . . . ? C76 C77 C89 C90 82.4(8) . . . . ? C78 C77 C89 C90 -94.3(7) . . . . ? C76 C77 C89 C91 -34.6(10) . . . . ? C78 C77 C89 C91 148.7(9) . . . . ? C76 C77 C89 C92 -157.0(8) . . . . ? C78 C77 C89 C92 26.3(9) . . . . ? C76 C77 C89 C92' -130.9(9) . . . . ? C78 C77 C89 C92' 52.4(10) . . . . ? C76 C77 C89 C90' 116.9(8) . . . . ? C78 C77 C89 C90' -59.8(9) . . . . ? C57 C56 C93 C95 -174.2(4) . . . . ? C55 C56 C93 C95 4.7(6) . . . . ? C57 C56 C93 C94 65.6(5) . . . . ? C55 C56 C93 C94 -115.4(5) . . . . ? C57 C56 C93 C96 -53.7(6) . . . . ? C55 C56 C93 C96 125.2(5) . . . . ? O4 C97 C98 O12 -163.3(3) . . . . ? O4 C97 C98 O11 16.8(5) . . . . ? O4 C97 C98 Na2 -3.9(3) . . . . ? O11 Na2 C98 O12 -72.2(7) . . . . ? O2 Na2 C98 O12 -39.7(8) . . . . ? O4 Na2 C98 O12 140.0(7) . . . . ? O8 Na2 C98 O12 -44.3(6) . . . . ? O1 Na2 C98 O12 62.0(6) . . . . ? O3 Na2 C98 O12 -140.2(6) . . . . ? Cu1 Na2 C98 O12 -58.7(6) . . . . ? O2 Na2 C98 O11 32.5(5) . . . . ? O4 Na2 C98 O11 -147.8(4) . . . . ? O8 Na2 C98 O11 28.0(3) . . . . ? O1 Na2 C98 O11 134.2(3) . . . . ? O3 Na2 C98 O11 -67.9(3) . . . . ? Cu1 Na2 C98 O11 13.5(3) . . . . ? O11 Na2 C98 C97 150.7(4) . . . . ? O2 Na2 C98 C97 -176.8(3) . . . . ? O4 Na2 C98 C97 2.9(2) . . . . ? O8 Na2 C98 C97 178.7(2) . . . . ? O1 Na2 C98 C97 -75.1(2) . . . . ? O3 Na2 C98 C97 82.8(2) . . . . ? Cu1 Na2 C98 C97 164.2(3) . . . . ? O7 C99 C100 O2 -162.3(4) . . . . ? O8 C99 C100 O2 18.3(5) . . . . ? O10 C101 C102 O3 -74.1(13) . . . . ? O9 C101 C102 O3 118.1(5) . . . . ? O10' C101 C102 O3 -40(2) . . . . ? O1 C103 C104 O6 -161.7(5) . . . . ? O1 C103 C104 O5 22.7(7) . . . . ? C61 C66 O1 C103 103.6(4) . . . . ? C65 C66 O1 C103 -80.7(5) . . . . ? C61 C66 O1 Na2 -91.6(4) . . . . ? C65 C66 O1 Na2 84.2(4) . . . . ? C104 C103 O1 C66 -134.3(4) . . . . ? C104 C103 O1 Na2 62.6(5) . . . . ? O11 Na2 O1 C66 146.5(3) . . . . ? O2 Na2 O1 C66 -72.9(3) . . . . ? O4 Na2 O1 C66 79.6(3) . . . . ? O8 Na2 O1 C66 -141.6(3) . . . . ? O3 Na2 O1 C66 11.4(4) . . . . ? C98 Na2 O1 C66 130.2(3) . . . . ? Cu1 Na2 O1 C66 -177.1(2) . . . . ? O11 Na2 O1 C103 -50.2(3) . . . . ? O2 Na2 O1 C103 90.3(3) . . . . ? O4 Na2 O1 C103 -117.1(3) . . . . ? O8 Na2 O1 C103 21.6(3) . . . . ? O3 Na2 O1 C103 174.7(3) . . . . ? C98 Na2 O1 C103 -66.6(3) . . . . ? Cu1 Na2 O1 C103 -13.9(3) . . . . ? C68 C69 O2 C100 93.1(4) . . . . ? C70 C69 O2 C100 -87.0(5) . . . . ? C68 C69 O2 Na2 -90.5(4) . . . . ? C70 C69 O2 Na2 89.4(4) . . . . ? C99 C100 O2 C69 167.4(4) . . . . ? C99 C100 O2 Na2 -9.4(5) . . . . ? O11 Na2 O2 C69 -163.5(3) . . . . ? O4 Na2 O2 C69 0.2(5) . . . . ? O8 Na2 O2 C69 -175.4(4) . . . . ? O1 Na2 O2 C69 76.8(3) . . . . ? O3 Na2 O2 C69 -78.1(3) . . . . ? C98 Na2 O2 C69 179.8(3) . . . . ? Cu1 Na2 O2 C69 -164.5(3) . . . . ? O11 Na2 O2 C100 12.6(4) . . . . ? O4 Na2 O2 C100 176.3(3) . . . . ? O8 Na2 O2 C100 0.6(3) . . . . ? O1 Na2 O2 C100 -107.2(3) . . . . ? O3 Na2 O2 C100 98.0(3) . . . . ? C98 Na2 O2 C100 -4.2(5) . . . . ? Cu1 Na2 O2 C100 11.6(3) . . . . ? C75 C80 O3 C102 114.0(4) . . . . ? C79 C80 O3 C102 -70.2(5) . . . . ? C75 C80 O3 Na2 -86.8(4) . . . . ? C79 C80 O3 Na2 89.0(4) . . . . ? C101 C102 O3 C80 -107.1(5) . . . . ? C101 C102 O3 Na2 97.0(5) . . . . ? O11 Na2 O3 C80 -146.2(3) . . . . ? O2 Na2 O3 C80 77.0(3) . . . . ? O4 Na2 O3 C80 -75.5(3) . . . . ? O8 Na2 O3 C80 146.4(3) . . . . ? O1 Na2 O3 C80 -7.7(4) . . . . ? C98 Na2 O3 C80 -126.3(3) . . . . ? Cu1 Na2 O3 C80 179.9(3) . . . . ? O11 Na2 O3 C102 9.8(3) . . . . ? O2 Na2 O3 C102 -127.0(3) . . . . ? O4 Na2 O3 C102 80.5(3) . . . . ? O8 Na2 O3 C102 -57.6(3) . . . . ? O1 Na2 O3 C102 148.3(3) . . . . ? C98 Na2 O3 C102 29.7(3) . . . . ? Cu1 Na2 O3 C102 -24.1(3) . . . . ? C58 C59 O4 C97 -88.9(4) . . . . ? C54 C59 O4 C97 93.9(4) . . . . ? C58 C59 O4 Na2 88.0(4) . . . . ? C54 C59 O4 Na2 -89.1(4) . . . . ? C98 C97 O4 C59 -176.7(3) . . . . ? C98 C97 O4 Na2 5.7(4) . . . . ? O11 Na2 O4 C59 167.8(4) . . . . ? O2 Na2 O4 C59 -0.4(5) . . . . ? O8 Na2 O4 C59 173.5(3) . . . . ? O1 Na2 O4 C59 -78.2(3) . . . . ? O3 Na2 O4 C59 78.4(3) . . . . ? C98 Na2 O4 C59 179.8(4) . . . . ? Cu1 Na2 O4 C59 164.2(3) . . . . ? O11 Na2 O4 C97 -15.3(2) . . . . ? O2 Na2 O4 C97 176.4(3) . . . . ? O8 Na2 O4 C97 -9.7(3) . . . . ? O1 Na2 O4 C97 98.7(3) . . . . ? O3 Na2 O4 C97 -104.7(3) . . . . ? C98 Na2 O4 C97 -3.3(2) . . . . ? Cu1 Na2 O4 C97 -19.0(3) . . . . ? O6 C104 O5 Cu4 -1.3(7) . . . 1_565 ? C103 C104 O5 Cu4 173.9(3) . . . 1_565 ? O7 C99 O8 Cu1 20.4(6) . . . . ? C100 C99 O8 Cu1 -160.3(3) . . . . ? O7 C99 O8 Na2 161.6(4) . . . . ? C100 C99 O8 Na2 -19.0(5) . . . . ? O21 Cu1 O8 C99 88.7(6) 1_565 . . . ? O11 Cu1 O8 C99 157.2(4) . . . . ? O3W Cu1 O8 C99 -11.6(4) . . . . ? Na2 Cu1 O8 C99 146.2(4) . . . . ? O21 Cu1 O8 Na2 -57.5(5) 1_565 . . . ? O11 Cu1 O8 Na2 10.96(12) . . . . ? O3W Cu1 O8 Na2 -157.85(13) . . . . ? O11 Na2 O8 C99 -160.7(3) . . . . ? O2 Na2 O8 C99 10.5(3) . . . . ? O4 Na2 O8 C99 -166.4(3) . . . . ? O1 Na2 O8 C99 93.6(3) . . . . ? O3 Na2 O8 C99 -75.2(3) . . . . ? C98 Na2 O8 C99 -171.4(3) . . . . ? Cu1 Na2 O8 C99 -150.5(3) . . . . ? O11 Na2 O8 Cu1 -10.18(11) . . . . ? O2 Na2 O8 Cu1 160.98(14) . . . . ? O4 Na2 O8 Cu1 -15.9(2) . . . . ? O1 Na2 O8 Cu1 -115.95(12) . . . . ? O3 Na2 O8 Cu1 75.26(12) . . . . ? C98 Na2 O8 Cu1 -20.95(13) . . . . ? O10 C101 O9 Cu4 1.4(14) . . . . ? O10' C101 O9 Cu4 -31(2) . . . . ? C102 C101 O9 Cu4 167.6(3) . . . . ? O25 Cu4 O9 C101 -10.1(5) . . . . ? O5 Cu4 O9 C101 108.0(3) 1_545 . . . ? O19 Cu4 O9 C101 -94.2(3) . . . . ? O12 C98 O11 Cu1 -6.4(6) . . . . ? C97 C98 O11 Cu1 173.5(3) . . . . ? Na2 C98 O11 Cu1 -153.8(5) . . . . ? O12 C98 O11 Na2 147.4(3) . . . . ? C97 C98 O11 Na2 -32.6(5) . . . . ? O21 Cu1 O11 C98 -49.1(4) 1_565 . . . ? O8 Cu1 O11 C98 144.4(4) . . . . ? O3W Cu1 O11 C98 -149.7(5) . . . . ? Na2 Cu1 O11 C98 156.1(4) . . . . ? O21 Cu1 O11 Na2 154.83(14) 1_565 . . . ? O8 Cu1 O11 Na2 -11.74(13) . . . . ? O3W Cu1 O11 Na2 54.2(6) . . . . ? O2 Na2 O11 C98 -161.7(3) . . . . ? O4 Na2 O11 C98 26.3(3) . . . . ? O8 Na2 O11 C98 -149.6(3) . . . . ? O1 Na2 O11 C98 -49.5(3) . . . . ? O3 Na2 O11 C98 112.9(3) . . . . ? Cu1 Na2 O11 C98 -160.0(4) . . . . ? O2 Na2 O11 Cu1 -1.7(3) . . . . ? O4 Na2 O11 Cu1 -173.68(16) . . . . ? O8 Na2 O11 Cu1 10.39(12) . . . . ? O1 Na2 O11 Cu1 110.43(14) . . . . ? O3 Na2 O11 Cu1 -87.12(14) . . . . ? C98 Na2 O11 Cu1 160.0(4) . . . . ? O11 C98 O12 Cu3 -27.3(6) . . . 1_565 ? C97 C98 O12 Cu3 152.7(3) . . . 1_565 ? Na2 C98 O12 Cu3 22.3(8) . . . 1_565 ? C2 C3 O13 C50 -100.7(4) . . . . ? C4 C3 O13 C50 82.5(5) . . . . ? C2 C3 O13 Na1 94.7(4) . . . . ? C4 C3 O13 Na1 -82.1(4) . . . . ? C49 C50 O13 C3 143.9(4) . . . . ? C49 C50 O13 Na1 -50.6(4) . . . . ? O20 Na1 O13 C3 -136.6(3) . . . . ? O23 Na1 O13 C3 130.0(3) . . . . ? O14 Na1 O13 C3 -76.2(3) . . . . ? O16 Na1 O13 C3 62.8(3) . . . . ? O15 Na1 O13 C3 -3.1(4) . . . . ? O22 Na1 O13 C3 170.3(3) . . . . ? Cu3 Na1 O13 C3 -163.6(3) . . . . ? O20 Na1 O13 C50 59.4(3) . . . . ? O23 Na1 O13 C50 -34.0(3) . . . . ? O14 Na1 O13 C50 119.9(3) . . . . ? O16 Na1 O13 C50 -101.2(3) . . . . ? O15 Na1 O13 C50 -167.1(3) . . . . ? O22 Na1 O13 C50 6.4(5) . . . . ? Cu3 Na1 O13 C50 32.4(3) . . . . ? C23 C24 O14 C45 -92.4(4) . . . . ? C25 C24 O14 C45 84.9(4) . . . . ? C23 C24 O14 Na1 84.9(5) . . . . ? C25 C24 O14 Na1 -97.8(4) . . . . ? C46 C45 O14 C24 166.3(3) . . . . ? C46 C45 O14 Na1 -11.6(4) . . . . ? O20 Na1 O14 C24 -165.4(4) . . . . ? O23 Na1 O14 C24 136.8(3) . . . . ? O16 Na1 O14 C24 9.2(4) . . . . ? O15 Na1 O14 C24 -62.8(4) . . . . ? O13 Na1 O14 C24 78.0(3) . . . . ? O22 Na1 O14 C24 -121.4(3) . . . . ? Cu3 Na1 O14 C24 -153.3(3) . . . . ? O20 Na1 O14 C45 11.7(2) . . . . ? O23 Na1 O14 C45 -46.1(4) . . . . ? O16 Na1 O14 C45 -173.6(2) . . . . ? O15 Na1 O14 C45 114.3(3) . . . . ? O13 Na1 O14 C45 -104.9(3) . . . . ? O22 Na1 O14 C45 55.7(3) . . . . ? Cu3 Na1 O14 C45 23.8(3) . . . . ? C16 C17 O15 C47 -88.9(4) . . . . ? C18 C17 O15 C47 94.6(4) . . . . ? C16 C17 O15 Na1 95.2(3) . . . . ? C18 C17 O15 Na1 -81.2(4) . . . . ? C48 C47 O15 C17 -173.6(3) . . . . ? C48 C47 O15 Na1 2.0(5) . . . . ? O20 Na1 O15 C17 129.8(3) . . . . ? O23 Na1 O15 C17 -128.6(3) . . . . ? O14 Na1 O15 C17 62.8(3) . . . . ? O16 Na1 O15 C17 -74.1(3) . . . . ? O13 Na1 O15 C17 -5.6(3) . . . . ? O22 Na1 O15 C17 177.0(3) . . . . ? Cu3 Na1 O15 C17 159.4(3) . . . . ? O20 Na1 O15 C47 -45.4(3) . . . . ? O23 Na1 O15 C47 56.2(3) . . . . ? O14 Na1 O15 C47 -112.4(3) . . . . ? O16 Na1 O15 C47 110.7(3) . . . . ? O13 Na1 O15 C47 179.2(3) . . . . ? O22 Na1 O15 C47 1.8(3) . . . . ? Cu3 Na1 O15 C47 -15.8(3) . . . . ? C13 C14 O16 C52 85.8(4) . . . . ? C9 C14 O16 C52 -92.3(4) . . . . ? C13 C14 O16 Na1 -95.5(4) . . . . ? C9 C14 O16 Na1 86.4(5) . . . . ? C51 C52 O16 C14 154.5(4) . . . . ? C51 C52 O16 Na1 -24.6(5) . . . . ? O20 Na1 O16 C14 166.9(4) . . . . ? O23 Na1 O16 C14 -154.2(4) . . . . ? O14 Na1 O16 C14 -0.5(5) . . . . ? O15 Na1 O16 C14 76.1(4) . . . . ? O13 Na1 O16 C14 -65.8(4) . . . . ? O22 Na1 O16 C14 133.3(4) . . . . ? Cu3 Na1 O16 C14 158.0(4) . . . . ? O20 Na1 O16 C52 -14.4(5) . . . . ? O23 Na1 O16 C52 24.5(3) . . . . ? O14 Na1 O16 C52 178.2(3) . . . . ? O15 Na1 O16 C52 -105.2(3) . . . . ? O13 Na1 O16 C52 112.9(3) . . . . ? O22 Na1 O16 C52 -47.9(3) . . . . ? Cu3 Na1 O16 C52 -23.3(3) . . . . ? O18 C49 O17 Cu2 28.5(7) . . . . ? C50 C49 O17 Cu2 -153.6(3) . . . . ? O17 Cu2 O17 C49 -106(53) 2_656 . . . ? O2W Cu2 O17 C49 -22.2(4) . . . . ? O2W Cu2 O17 C49 170.8(4) 2_656 . . . ? O1W Cu2 O17 C49 74.3(4) . . . . ? O20 C46 O19 Cu4 -18.0(6) . . . . ? C45 C46 O19 Cu4 160.1(3) . . . . ? O25 Cu4 O19 C46 38.6(3) . . . . ? O9 Cu4 O19 C46 -161.3(4) . . . . ? O5 Cu4 O19 C46 -69.1(5) 1_545 . . . ? O19 C46 O20 Cu3 21.7(6) . . . . ? C45 C46 O20 Cu3 -156.4(3) . . . . ? O19 C46 O20 Na1 -172.0(3) . . . . ? C45 C46 O20 Na1 9.9(5) . . . . ? O25 Cu3 O20 C46 -44.7(3) . . . . ? O24 Cu3 O20 C46 172.3(9) 2_656 . . . ? O22 Cu3 O20 C46 137.8(3) . . . . ? O12 Cu3 O20 C46 46.6(3) 1_545 . . . ? Na1 Cu3 O20 C46 167.8(4) . . . . ? O25 Cu3 O20 Na1 147.56(14) . . . . ? O24 Cu3 O20 Na1 4.5(11) 2_656 . . . ? O22 Cu3 O20 Na1 -29.97(14) . . . . ? O12 Cu3 O20 Na1 -121.19(13) 1_545 . . . ? O23 Na1 O20 C46 142.3(3) . . . . ? O14 Na1 O20 C46 -11.8(3) . . . . ? O16 Na1 O20 C46 177.7(3) . . . . ? O15 Na1 O20 C46 -96.4(3) . . . . ? O13 Na1 O20 C46 54.3(3) . . . . ? O22 Na1 O20 C46 -143.7(3) . . . . ? Cu3 Na1 O20 C46 -168.3(4) . . . . ? O23 Na1 O20 Cu3 -49.39(15) . . . . ? O14 Na1 O20 Cu3 156.45(15) . . . . ? O16 Na1 O20 Cu3 -14.0(4) . . . . ? O15 Na1 O20 Cu3 71.86(14) . . . . ? O13 Na1 O20 Cu3 -137.41(12) . . . . ? O22 Na1 O20 Cu3 24.55(11) . . . . ? O22 C48 O21 Cu1 1.2(7) . . . 1_545 ? C47 C48 O21 Cu1 -177.4(3) . . . 1_545 ? O21 C48 O22 Cu3 -40.0(6) . . . . ? C47 C48 O22 Cu3 138.5(3) . . . . ? O21 C48 O22 Na1 -168.0(3) . . . . ? C47 C48 O22 Na1 10.5(5) . . . . ? O25 Cu3 O22 C48 -130.9(9) . . . . ? O20 Cu3 O22 C48 -112.8(3) . . . . ? O24 Cu3 O22 C48 71.2(3) 2_656 . . . ? O12 Cu3 O22 C48 -30.2(3) 1_545 . . . ? Na1 Cu3 O22 C48 -137.2(4) . . . . ? O25 Cu3 O22 Na1 6.3(10) . . . . ? O20 Cu3 O22 Na1 24.36(11) . . . . ? O24 Cu3 O22 Na1 -151.59(12) 2_656 . . . ? O12 Cu3 O22 Na1 106.96(10) 1_545 . . . ? O20 Na1 O22 C48 117.9(3) . . . . ? O23 Na1 O22 C48 -140.3(3) . . . . ? O14 Na1 O22 C48 70.6(3) . . . . ? O16 Na1 O22 C48 -76.6(3) . . . . ? O15 Na1 O22 C48 -6.6(3) . . . . ? O13 Na1 O22 C48 178.4(3) . . . . ? Cu3 Na1 O22 C48 140.7(3) . . . . ? O20 Na1 O22 Cu3 -22.79(11) . . . . ? O23 Na1 O22 Cu3 78.99(12) . . . . ? O14 Na1 O22 Cu3 -70.10(13) . . . . ? O16 Na1 O22 Cu3 142.68(11) . . . . ? O15 Na1 O22 Cu3 -147.33(14) . . . . ? O13 Na1 O22 Cu3 37.6(4) . . . . ? O24 C51 O23 Na1 -161.8(3) . . . . ? C52 C51 O23 Na1 19.9(5) . . . . ? O20 Na1 O23 C51 141.4(3) . . . . ? O14 Na1 O23 C51 -167.0(3) . . . . ? O16 Na1 O23 C51 -24.2(3) . . . . ? O15 Na1 O23 C51 35.8(3) . . . . ? O13 Na1 O23 C51 -110.6(3) . . . . ? O22 Na1 O23 C51 82.4(3) . . . . ? Cu3 Na1 O23 C51 117.1(3) . . . . ? O23 C51 O24 Cu3 -7.3(6) . . . 2_656 ? C52 C51 O24 Cu3 171.1(3) . . . 2_656 ? O9 Cu4 O25 Cu3 -149.7(3) . . . . ? O5 Cu4 O25 Cu3 92.94(15) 1_545 . . . ? O19 Cu4 O25 Cu3 -65.78(14) . . . . ? O20 Cu3 O25 Cu4 69.13(14) . . . . ? O24 Cu3 O25 Cu4 -115.19(15) 2_656 . . . ? O22 Cu3 O25 Cu4 87.0(10) . . . . ? O12 Cu3 O25 Cu4 -13.58(14) 1_545 . . . ? Na1 Cu3 O25 Cu4 92.69(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1C O23 0.89(2) 1.75(3) 2.633(4) 171(11) . O1W H1D O25 0.88(2) 2.22(4) 3.058(3) 158(9) . O2W H2B O18 0.872(18) 1.82(2) 2.650(4) 158(4) . O2W H2A O25 0.894(17) 2.02(3) 2.827(4) 150(3) . O2W H2A O19 0.894(17) 2.52(3) 3.127(4) 126(2) . O3W H3A O2W 0.843(18) 2.00(3) 2.807(4) 161(4) . O7W H7B O4W 0.92(2) 2.01(4) 2.871(11) 157(7) 2_666 O7W H7A O6 0.92(2) 2.02(5) 2.836(6) 148(8) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.786 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.063 #===== data_12 _database_code_depnum_ccdc_archive 'CCDC 879394' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H67 Na O16 Zn2' _chemical_formula_weight 1101.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.2387(6) _cell_length_b 25.4087(7) _cell_length_c 18.6362(5) _cell_angle_alpha 90 _cell_angle_beta 97.552(2) _cell_angle_gamma 90 _cell_volume 11378.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4624 _exptl_absorpt_coefficient_mu 0.914 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8174 _exptl_absorpt_correction_T_max 0.8676 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25289 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.1279 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 29.18 _reflns_number_total 13034 _reflns_number_gt 5513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The low ratio of observed/unique reflections may be attributed to the weak diffraction of the crystals. The distances of O1W---H1C and O1W---H1D were restrained to 0.85+-0.02 \%A. The distance of O13---H13 was restrained to 0.88+-0.02 \%A. The distance of H1C...H1D was restrained to 1.44+-0.02 \%A. For C30, C31, C32, C34 and C38 atoms, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13034 _refine_ls_number_parameters 675 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1350 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1770 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.01733(2) 1.10855(2) 0.05857(3) 0.05149(18) Uani 1 1 d . . . Zn2 Zn -0.04435(2) 1.01017(2) 0.11049(3) 0.05670(19) Uani 1 1 d . . . Na1 Na 0.14678(6) 1.10929(6) 0.13952(8) 0.0412(4) Uani 1 1 d . . . C1 C 0.24588(18) 0.99308(16) 0.0890(2) 0.0440(10) Uani 1 1 d . . . H1A H 0.2069 0.9994 0.0720 0.053 Uiso 1 1 calc R . . H1B H 0.2580 0.9630 0.0631 0.053 Uiso 1 1 calc R . . C2 C 0.33803(18) 1.03946(18) 0.0872(2) 0.0500(11) Uani 1 1 d . . . H2 H 0.3550 1.0071 0.0983 0.060 Uiso 1 1 calc R . . C3 C 0.28013(16) 1.04145(16) 0.0746(2) 0.0414(10) Uani 1 1 d . . . C4 C 0.25598(15) 1.09000(16) 0.0560(2) 0.0361(9) Uani 1 1 d . . . C5 C 0.28793(16) 1.13532(16) 0.0538(2) 0.0375(9) Uani 1 1 d . . . C6 C 0.34500(17) 1.13022(17) 0.0673(2) 0.0444(10) Uani 1 1 d . . . H6 H 0.3667 1.1602 0.0649 0.053 Uiso 1 1 calc R . . C7 C 0.37155(17) 1.08322(19) 0.0840(2) 0.0505(11) Uani 1 1 d . . . C8 C 0.26151(16) 1.18933(15) 0.0407(2) 0.0374(9) Uani 1 1 d . . . H8A H 0.2787 1.2077 0.0037 0.045 Uiso 1 1 calc R . . H8B H 0.2221 1.1855 0.0237 0.045 Uiso 1 1 calc R . . C9 C 0.26905(16) 1.22110(14) 0.1102(2) 0.0358(9) Uani 1 1 d . . . C10 C 0.22877(16) 1.22074(14) 0.1574(2) 0.0355(9) Uani 1 1 d . . . C11 C 0.23859(16) 1.24270(14) 0.2261(2) 0.0363(9) Uani 1 1 d . . . C12 C 0.28844(18) 1.26951(16) 0.2444(2) 0.0440(10) Uani 1 1 d . . . H12 H 0.2952 1.2850 0.2899 0.053 Uiso 1 1 calc R . . C13 C 0.32883(17) 1.27428(16) 0.1980(2) 0.0419(10) Uani 1 1 d . . . C14 C 0.31813(16) 1.24876(16) 0.1315(2) 0.0404(10) Uani 1 1 d . . . H14 H 0.3448 1.2502 0.1001 0.048 Uiso 1 1 calc R . . C15 C 0.19923(17) 1.23348(16) 0.2813(2) 0.0432(10) Uani 1 1 d . . . H15A H 0.1619 1.2275 0.2568 0.052 Uiso 1 1 calc R . . H15B H 0.1984 1.2643 0.3118 0.052 Uiso 1 1 calc R . . C16 C 0.21840(17) 1.18576(16) 0.3278(2) 0.0422(10) Uani 1 1 d . . . C17 C 0.19522(16) 1.13572(16) 0.3170(2) 0.0388(10) Uani 1 1 d . . . C18 C 0.22096(18) 1.09164(16) 0.3522(2) 0.0435(10) Uani 1 1 d . . . C19 C 0.26812(19) 1.10006(19) 0.4023(2) 0.0509(11) Uani 1 1 d . . . H19 H 0.2855 1.0711 0.4260 0.061 Uiso 1 1 calc R . . C20 C 0.29021(19) 1.1493(2) 0.4185(2) 0.0535(12) Uani 1 1 d . . . C21 C 0.26453(18) 1.19136(17) 0.3806(2) 0.0476(11) Uani 1 1 d . . . H21 H 0.2787 1.2250 0.3908 0.057 Uiso 1 1 calc R . . C22 C 0.19871(18) 1.03631(16) 0.3379(2) 0.0490(11) Uani 1 1 d . . . H22A H 0.1606 1.0383 0.3145 0.059 Uiso 1 1 calc R . . H22B H 0.1986 1.0182 0.3836 0.059 Uiso 1 1 calc R . . C23 C 0.21853(16) 1.00423(14) 0.2147(2) 0.0399(10) Uani 1 1 d . . . C24 C 0.25355(16) 0.98197(15) 0.1694(2) 0.0401(10) Uani 1 1 d . . . C25 C 0.29908(18) 0.95343(17) 0.2019(3) 0.0502(11) Uani 1 1 d . . . H25 H 0.3218 0.9366 0.1724 0.060 Uiso 1 1 calc R . . C26 C 0.31205(18) 0.94902(17) 0.2763(3) 0.0505(11) Uani 1 1 d . . . C27 C 0.27956(18) 0.97667(16) 0.3188(2) 0.0477(11) Uani 1 1 d . . . H27 H 0.2894 0.9763 0.3688 0.057 Uiso 1 1 calc R . . C28 C 0.23302(17) 1.00489(15) 0.2903(2) 0.0442(10) Uani 1 1 d . . . C29 C 0.4346(2) 1.0796(2) 0.1017(3) 0.0711(15) Uani 1 1 d . . . C30 C 0.4517(7) 1.1118(7) 0.1721(10) 0.170(6) Uani 0.68 1 d PU . . C31 C 0.4646(6) 1.1115(6) 0.0466(8) 0.148(5) Uani 0.68 1 d PU . . C32 C 0.4504(6) 1.0453(6) 0.1701(8) 0.151(5) Uani 0.68 1 d PU . . C34 C 0.4054(5) 0.9572(4) 0.3515(7) 0.096(3) Uani 0.68 1 d PU . . C35 C 0.3802(5) 0.8759(4) 0.2560(5) 0.099(4) Uani 0.68 1 d P . . C38 C 0.3840(4) 1.1947(4) 0.4504(6) 0.090(3) Uani 0.68 1 d PU . . C39 C 0.3211(5) 1.1889(7) 0.5408(6) 0.126(5) Uani 0.68 1 d P . . C30' C 0.4651(8) 1.1299(8) 0.1153(11) 0.084(5) Uiso 0.32 1 d P . . C31' C 0.4581(7) 1.0391(7) 0.0469(10) 0.071(4) Uiso 0.32 1 d P . . C32' C 0.4588(8) 1.0263(8) 0.1009(12) 0.085(5) Uiso 0.32 1 d P . . C34' C 0.4144(8) 0.9505(8) 0.3185(12) 0.071(5) Uiso 0.32 1 d P . . C35' C 0.4095(17) 0.9101(17) 0.254(2) 0.183(17) Uiso 0.32 1 d P . . C38' C 0.3909(9) 1.1689(9) 0.4287(12) 0.087(6) Uiso 0.32 1 d P . . C39' C 0.3274(17) 1.1581(14) 0.544(2) 0.141(15) Uiso 0.32 1 d P . . C33 C 0.3617(2) 0.9159(2) 0.3109(3) 0.0674(14) Uani 1 1 d . . . C36 C 0.3446(3) 0.8827(3) 0.3730(4) 0.104(2) Uani 1 1 d . . . H36A H 0.3103 0.8648 0.3569 0.156 Uiso 1 1 calc R . . H36B H 0.3397 0.9051 0.4131 0.156 Uiso 1 1 calc R . . H36C H 0.3731 0.8572 0.3879 0.156 Uiso 1 1 calc R . . C37 C 0.3417(2) 1.1576(2) 0.4755(3) 0.0709(15) Uani 1 1 d . . . C40 C 0.3707(3) 1.1053(3) 0.5019(5) 0.139(3) Uani 1 1 d . . . C41 C 0.38208(19) 1.30418(19) 0.2218(3) 0.0581(13) Uani 1 1 d . . . C42 C 0.4187(2) 1.3098(3) 0.1614(3) 0.0859(18) Uani 1 1 d . . . H42A H 0.4521 1.3286 0.1794 0.129 Uiso 1 1 calc R . . H42B H 0.3988 1.3288 0.1217 0.129 Uiso 1 1 calc R . . H42C H 0.4283 1.2755 0.1453 0.129 Uiso 1 1 calc R . . C43 C 0.3687(3) 1.3606(3) 0.2424(4) 0.106(2) Uani 1 1 d . . . H43A H 0.4027 1.3792 0.2579 0.159 Uiso 1 1 calc R . . H43B H 0.3461 1.3600 0.2811 0.159 Uiso 1 1 calc R . . H43C H 0.3488 1.3781 0.2012 0.159 Uiso 1 1 calc R . . C44 C 0.4140(3) 1.2767(4) 0.2854(4) 0.150(4) Uani 1 1 d . . . H44A H 0.4478 1.2956 0.3006 0.226 Uiso 1 1 calc R . . H44B H 0.4227 1.2415 0.2719 0.226 Uiso 1 1 calc R . . H44C H 0.3918 1.2755 0.3245 0.226 Uiso 1 1 calc R . . C45 C 0.13854(17) 1.23421(17) 0.0989(3) 0.0509(11) Uani 1 1 d . . . H45A H 0.1551 1.2518 0.0607 0.061 Uiso 1 1 calc R . . H45B H 0.1300 1.2606 0.1333 0.061 Uiso 1 1 calc R . . C46 C 0.08617(18) 1.20720(19) 0.0674(3) 0.0500(11) Uani 1 1 d . . . C47 C 0.12437(17) 0.98920(16) 0.1840(3) 0.0533(12) Uani 1 1 d . . . H47A H 0.1235 0.9755 0.2324 0.064 Uiso 1 1 calc R . . H47B H 0.1309 0.9600 0.1527 0.064 Uiso 1 1 calc R . . C48 C 0.06870(18) 1.01479(18) 0.1569(2) 0.0486(11) Uani 1 1 d . . . C49 C 0.17743(17) 1.08371(19) -0.0324(2) 0.0499(11) Uani 1 1 d . . . H49A H 0.2014 1.0584 -0.0519 0.060 Uiso 1 1 calc R . . H49B H 0.1787 1.1162 -0.0595 0.060 Uiso 1 1 calc R . . C50 C 0.11942(17) 1.06335(16) -0.0420(2) 0.0411(10) Uani 1 1 d . . . C51 C 0.09748(16) 1.14974(17) 0.2881(2) 0.0457(11) Uani 1 1 d . . . H51A H 0.0728 1.1594 0.2449 0.055 Uiso 1 1 calc R . . H51B H 0.1070 1.1817 0.3154 0.055 Uiso 1 1 calc R . . C52 C 0.06603(16) 1.11366(17) 0.3335(2) 0.0382(9) Uani 1 1 d . . . O1 O 0.17715(10) 1.19704(10) 0.13431(14) 0.0373(6) Uani 1 1 d . . . O2 O 0.14743(11) 1.12824(10) 0.26653(14) 0.0403(7) Uani 1 1 d . . . O3 O 0.16871(10) 1.02668(10) 0.18492(15) 0.0433(7) Uani 1 1 d . . . O4 O 0.19790(10) 1.09336(10) 0.04186(13) 0.0364(6) Uani 1 1 d . . . O5 O 0.07607(11) 1.16329(12) 0.08982(16) 0.0497(7) Uani 1 1 d . . . O6 O 0.05600(16) 1.23289(16) 0.0197(2) 0.0976(14) Uani 1 1 d . . . O9 O 0.06526(11) 1.06188(11) 0.14372(15) 0.0459(7) Uani 1 1 d . . . O10 O 0.02853(12) 0.98212(12) 0.1490(2) 0.0735(11) Uani 1 1 d . . . O11 O 0.08969(15) 1.07215(17) 0.0050(2) 0.0856(12) Uani 1 1 d . . . O12 O 0.10399(12) 1.04092(13) -0.10087(17) 0.0562(8) Uani 1 1 d . . . O8 O 0.07296(12) 1.06479(12) 0.32930(17) 0.0531(8) Uani 1 1 d . . . O7 O 0.03363(12) 1.13722(12) 0.36886(17) 0.0571(8) Uani 1 1 d . . . O2W O -0.0099(6) 1.2461(6) 0.3140(8) 0.173(5) Uiso 0.50 1 d P . . O3W O -0.0243(8) 1.2722(8) 0.1423(11) 0.221(7) Uiso 0.50 1 d P . . O4W O 0.1189(3) 0.8880(3) 0.0509(4) 0.101(2) Uiso 0.60 1 d P . . O4W' O 0.1597(5) 0.8660(4) 0.0182(6) 0.100(3) Uiso 0.40 1 d P . . O1W O -0.01168(16) 1.1567(2) -0.0308(2) 0.0912(12) Uani 1 1 d D . . H1D H -0.0402(19) 1.170(2) -0.017(4) 0.137 Uiso 1 1 d D . . H1C H -0.014(3) 1.1269(16) -0.050(4) 0.137 Uiso 1 1 d D . . O13 O -0.03293(15) 1.04990(16) 0.02405(18) 0.0759(11) Uani 1 1 d D . . H13 H -0.024(3) 1.066(2) -0.013(2) 0.114 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0325(3) 0.0725(4) 0.0505(3) -0.0079(3) 0.0092(2) -0.0116(2) Zn2 0.0349(3) 0.0585(3) 0.0800(4) -0.0284(3) 0.0198(3) -0.0117(2) Na1 0.0324(8) 0.0408(9) 0.0518(10) 0.0058(7) 0.0108(7) -0.0022(7) C1 0.042(2) 0.039(2) 0.051(3) -0.008(2) 0.0047(19) 0.0042(19) C2 0.045(3) 0.055(3) 0.049(3) -0.005(2) 0.002(2) 0.007(2) C3 0.036(2) 0.045(3) 0.043(2) -0.008(2) 0.0051(18) 0.0020(19) C4 0.031(2) 0.046(2) 0.032(2) -0.0073(18) 0.0063(16) -0.0047(19) C5 0.038(2) 0.049(2) 0.025(2) -0.0035(18) 0.0049(17) -0.0030(19) C6 0.037(2) 0.054(3) 0.043(2) 0.000(2) 0.0057(19) -0.005(2) C7 0.037(2) 0.070(3) 0.044(3) -0.009(2) 0.0020(19) 0.001(2) C8 0.039(2) 0.043(2) 0.031(2) 0.0063(18) 0.0061(17) -0.0069(18) C9 0.040(2) 0.033(2) 0.035(2) 0.0058(17) 0.0066(18) -0.0055(17) C10 0.035(2) 0.029(2) 0.042(2) 0.0090(18) 0.0038(18) -0.0029(17) C11 0.040(2) 0.031(2) 0.038(2) 0.0035(18) 0.0084(17) 0.0024(18) C12 0.053(3) 0.040(2) 0.039(2) -0.0054(19) 0.006(2) -0.010(2) C13 0.041(2) 0.041(2) 0.043(3) 0.002(2) 0.0039(19) -0.0064(19) C14 0.034(2) 0.045(2) 0.044(2) 0.0016(19) 0.0100(18) -0.0082(18) C15 0.046(3) 0.040(2) 0.046(3) -0.002(2) 0.014(2) -0.0010(19) C16 0.049(3) 0.042(2) 0.040(2) 0.0007(19) 0.022(2) 0.004(2) C17 0.039(2) 0.047(3) 0.033(2) -0.0009(19) 0.0168(19) 0.0024(19) C18 0.051(3) 0.046(2) 0.039(2) 0.003(2) 0.023(2) 0.003(2) C19 0.052(3) 0.057(3) 0.045(3) 0.015(2) 0.011(2) 0.009(2) C20 0.051(3) 0.072(3) 0.039(3) 0.004(2) 0.010(2) -0.003(2) C21 0.055(3) 0.044(3) 0.044(3) 0.002(2) 0.011(2) -0.001(2) C22 0.051(3) 0.046(3) 0.052(3) 0.013(2) 0.018(2) 0.001(2) C23 0.034(2) 0.028(2) 0.057(3) 0.0023(19) 0.005(2) 0.0000(17) C24 0.035(2) 0.031(2) 0.054(3) -0.0016(19) 0.0044(19) 0.0003(18) C25 0.047(3) 0.041(3) 0.063(3) 0.000(2) 0.012(2) 0.012(2) C26 0.044(3) 0.040(2) 0.065(3) 0.004(2) 0.001(2) 0.008(2) C27 0.049(3) 0.042(2) 0.052(3) 0.007(2) 0.005(2) 0.004(2) C28 0.043(3) 0.032(2) 0.061(3) 0.008(2) 0.017(2) 0.0020(19) C29 0.044(3) 0.095(4) 0.072(4) -0.003(3) -0.001(2) 0.000(3) C30 0.169(6) 0.172(6) 0.169(6) -0.003(2) 0.018(2) 0.000(2) C31 0.147(5) 0.149(5) 0.148(5) 0.0012(10) 0.0197(12) -0.0001(10) C32 0.150(5) 0.151(5) 0.151(5) 0.0010(10) 0.0186(12) -0.0001(10) C34 0.093(4) 0.097(4) 0.097(4) 0.001(2) 0.009(2) 0.0003(19) C35 0.115(8) 0.104(8) 0.074(6) -0.004(5) -0.009(5) 0.095(7) C38 0.088(3) 0.091(3) 0.090(3) 0.0021(19) 0.0090(19) -0.0045(19) C39 0.117(9) 0.192(15) 0.059(6) -0.068(8) -0.024(6) 0.047(10) C33 0.062(3) 0.062(3) 0.076(4) 0.011(3) -0.002(3) 0.027(3) C36 0.097(5) 0.087(5) 0.124(6) 0.043(4) 0.001(4) 0.031(4) C37 0.066(3) 0.085(4) 0.058(3) 0.020(3) -0.002(3) -0.006(3) C40 0.102(6) 0.124(7) 0.172(8) 0.050(6) -0.057(5) -0.002(5) C41 0.053(3) 0.062(3) 0.058(3) -0.005(2) 0.003(2) -0.023(2) C42 0.063(4) 0.109(5) 0.087(4) -0.011(3) 0.014(3) -0.047(3) C43 0.107(5) 0.089(5) 0.129(6) -0.037(4) 0.037(4) -0.042(4) C44 0.081(5) 0.222(10) 0.130(6) 0.077(6) -0.053(4) -0.073(6) C45 0.041(3) 0.042(3) 0.069(3) 0.014(2) 0.005(2) 0.004(2) C46 0.038(3) 0.056(3) 0.056(3) 0.009(2) 0.005(2) -0.001(2) C47 0.039(3) 0.035(2) 0.086(4) 0.004(2) 0.007(2) -0.008(2) C48 0.037(3) 0.046(3) 0.065(3) -0.010(2) 0.015(2) -0.008(2) C49 0.040(2) 0.069(3) 0.040(3) -0.009(2) 0.0015(19) -0.014(2) C50 0.036(2) 0.050(3) 0.038(3) -0.002(2) 0.0084(19) -0.0076(19) C51 0.038(2) 0.050(3) 0.052(3) 0.011(2) 0.016(2) 0.0054(19) C52 0.030(2) 0.049(3) 0.036(2) 0.009(2) 0.0039(17) 0.0009(19) O1 0.0315(15) 0.0335(14) 0.0465(16) 0.0057(12) 0.0044(12) -0.0058(12) O2 0.0353(16) 0.0481(16) 0.0408(16) 0.0068(13) 0.0167(13) 0.0024(12) O3 0.0281(15) 0.0372(15) 0.0652(19) 0.0067(13) 0.0076(13) -0.0007(12) O4 0.0308(15) 0.0438(15) 0.0344(15) -0.0058(12) 0.0030(11) -0.0010(12) O5 0.0369(17) 0.0467(18) 0.064(2) 0.0112(15) 0.0009(14) -0.0053(13) O6 0.073(3) 0.095(3) 0.112(3) 0.051(3) -0.036(2) -0.015(2) O9 0.0406(17) 0.0451(19) 0.0519(18) -0.0031(14) 0.0056(13) -0.0041(13) O10 0.0286(17) 0.0465(19) 0.146(3) -0.010(2) 0.0144(18) -0.0056(14) O11 0.061(2) 0.131(3) 0.070(2) -0.031(2) 0.0261(19) -0.018(2) O12 0.0478(18) 0.067(2) 0.054(2) -0.0183(17) 0.0067(15) -0.0212(15) O8 0.0407(18) 0.054(2) 0.068(2) 0.0198(16) 0.0195(15) 0.0036(14) O7 0.0450(18) 0.065(2) 0.067(2) 0.0045(16) 0.0313(16) -0.0011(15) O1W 0.066(3) 0.127(4) 0.076(3) 0.022(3) -0.008(2) -0.021(2) O13 0.066(2) 0.113(3) 0.052(2) -0.033(2) 0.0215(18) -0.037(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O13 1.978(3) . ? Zn1 O5 2.021(3) . ? Zn1 O7 2.080(3) 2 ? Zn1 O1W 2.112(5) . ? Zn1 O9 2.188(3) . ? Zn1 O11 2.322(4) . ? Zn1 Zn2 3.1303(8) . ? Zn1 Na1 3.2981(16) . ? Zn1 H1C 2.12(8) . ? Zn1 H13 1.90(7) . ? Zn2 O12 1.934(3) 5_575 ? Zn2 O13 1.951(4) . ? Zn2 O10 1.952(3) . ? Zn2 O8 1.967(3) 2 ? Na1 O5 2.294(3) . ? Na1 O3 2.299(3) . ? Na1 O9 2.324(3) . ? Na1 O1 2.354(3) . ? Na1 O4 2.367(3) . ? Na1 O2 2.413(3) . ? Na1 O11 2.860(4) . ? Na1 C48 3.100(5) . ? Na1 C46 3.104(5) . ? C1 C24 1.513(6) . ? C1 C3 1.526(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C7 1.383(6) . ? C2 C3 1.393(6) . ? C2 H2 0.9300 . ? C3 C4 1.390(6) . ? C4 C5 1.391(5) . ? C4 O4 1.400(4) . ? C5 C6 1.379(5) . ? C5 C8 1.521(5) . ? C6 C7 1.373(6) . ? C6 H6 0.9300 . ? C7 C29 1.524(6) . ? C8 C9 1.516(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.394(5) . ? C9 C10 1.398(5) . ? C10 C11 1.387(5) . ? C10 O1 1.404(4) . ? C11 C12 1.390(6) . ? C11 C15 1.510(5) . ? C12 C13 1.395(6) . ? C12 H12 0.9300 . ? C13 C14 1.391(6) . ? C13 C41 1.513(6) . ? C14 H14 0.9300 . ? C15 C16 1.527(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.394(6) . ? C16 C21 1.396(6) . ? C17 C18 1.402(6) . ? C17 O2 1.406(5) . ? C18 C19 1.395(6) . ? C18 C22 1.517(6) . ? C19 C20 1.377(6) . ? C19 H19 0.9300 . ? C20 C21 1.384(6) . ? C20 C37 1.545(7) . ? C21 H21 0.9300 . ? C22 C28 1.519(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O3 1.384(5) . ? C23 C24 1.394(6) . ? C23 C28 1.406(6) . ? C24 C25 1.391(6) . ? C25 C26 1.386(6) . ? C25 H25 0.9300 . ? C26 C27 1.381(6) . ? C26 C33 1.539(6) . ? C27 C28 1.382(6) . ? C27 H27 0.9300 . ? C29 C32' 1.48(2) . ? C29 C30' 1.48(2) . ? C29 C32 1.550(16) . ? C29 C30 1.555(18) . ? C29 C31 1.559(15) . ? C29 C31' 1.604(18) . ? C30 C30' 1.24(2) . ? C30 C32 1.69(2) . ? C31 C30' 1.36(2) . ? C31 C31' 1.85(2) . ? C32 C32' 1.42(2) . ? C34 C34' 0.70(2) . ? C34 C33 1.608(12) . ? C35 C35' 1.13(4) . ? C35 C33 1.550(10) . ? C38 C38' 0.80(2) . ? C38 C37 1.512(11) . ? C39 C39' 0.80(4) . ? C39 C37 1.589(12) . ? C31' C32' 1.06(2) . ? C34' C33 1.54(2) . ? C34' C35' 1.58(4) . ? C35' C33 1.68(4) . ? C38' C37 1.59(2) . ? C39' C37 1.37(4) . ? C39' C40 1.93(4) . ? C33 C36 1.533(8) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C40 1.553(9) . ? C41 C44 1.499(8) . ? C41 C42 1.529(7) . ? C41 C43 1.530(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 O1 1.429(5) . ? C45 C46 1.494(6) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 O5 1.228(5) . ? C46 O6 1.256(5) . ? C47 O3 1.434(5) . ? C47 C48 1.523(6) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O9 1.222(5) . ? C48 O10 1.273(5) . ? C49 O4 1.429(5) . ? C49 C50 1.487(6) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O11 1.226(5) . ? C50 O12 1.249(5) . ? C51 O2 1.433(4) . ? C51 C52 1.519(5) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 O7 1.244(5) . ? C52 O8 1.257(5) . ? O12 Zn2 1.934(3) 5_575 ? O8 Zn2 1.967(3) 2 ? O7 Zn1 2.080(3) 2 ? O2W O3W 1.270(19) 2 ? O3W O2W 1.270(19) 2 ? O4W O4W' 1.350(12) . ? O1W H1D 0.841(19) . ? O1W H1C 0.835(19) . ? O13 H13 0.86(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Zn1 O5 173.14(14) . . ? O13 Zn1 O7 94.72(13) . 2 ? O5 Zn1 O7 91.58(12) . 2 ? O13 Zn1 O1W 93.04(17) . . ? O5 Zn1 O1W 88.70(14) . . ? O7 Zn1 O1W 98.36(16) 2 . ? O13 Zn1 O9 94.20(15) . . ? O5 Zn1 O9 82.95(11) . . ? O7 Zn1 O9 91.29(12) 2 . ? O1W Zn1 O9 167.42(13) . . ? O13 Zn1 O11 91.59(14) . . ? O5 Zn1 O11 81.65(12) . . ? O7 Zn1 O11 165.09(14) 2 . ? O1W Zn1 O11 94.78(17) . . ? O9 Zn1 O11 74.76(13) . . ? O13 Zn1 Zn2 36.89(10) . . ? O5 Zn1 Zn2 143.87(9) . . ? O7 Zn1 Zn2 74.34(9) 2 . ? O1W Zn1 Zn2 125.70(10) . . ? O9 Zn1 Zn2 64.71(7) . . ? O11 Zn1 Zn2 103.50(11) . . ? O13 Zn1 Na1 131.40(13) . . ? O5 Zn1 Na1 43.31(8) . . ? O7 Zn1 Na1 108.14(9) 2 . ? O1W Zn1 Na1 123.76(10) . . ? O9 Zn1 Na1 44.68(8) . . ? O11 Zn1 Na1 58.13(10) . . ? Zn2 Zn1 Na1 109.12(3) . . ? O13 Zn1 H1C 74.0(13) . . ? O5 Zn1 H1C 106.1(14) . . ? O7 Zn1 H1C 111.7(14) 2 . ? O1W Zn1 H1C 22.8(7) . . ? O9 Zn1 H1C 154.6(9) . . ? O11 Zn1 H1C 83.0(15) . . ? Zn2 Zn1 H1C 110.0(14) . . ? Na1 Zn1 H1C 129.8(18) . . ? O13 Zn1 H13 25.4(16) . . ? O5 Zn1 H13 151.9(17) . . ? O7 Zn1 H13 111.0(17) 2 . ? O1W Zn1 H13 71.7(13) . . ? O9 Zn1 H13 112.3(16) . . ? O11 Zn1 H13 79.8(18) . . ? Zn2 Zn1 H13 62.2(15) . . ? Na1 Zn1 H13 135(2) . . ? H1C Zn1 H13 50.4(14) . . ? O12 Zn2 O13 117.15(14) 5_575 . ? O12 Zn2 O10 114.73(14) 5_575 . ? O13 Zn2 O10 105.82(16) . . ? O12 Zn2 O8 102.19(12) 5_575 2 ? O13 Zn2 O8 101.82(15) . 2 ? O10 Zn2 O8 114.69(14) . 2 ? O12 Zn2 Zn1 152.75(10) 5_575 . ? O13 Zn2 Zn1 37.48(10) . . ? O10 Zn2 Zn1 87.66(10) . . ? O8 Zn2 Zn1 80.30(9) 2 . ? O5 Na1 O3 144.99(11) . . ? O5 Na1 O9 74.34(11) . . ? O3 Na1 O9 70.78(10) . . ? O5 Na1 O1 68.77(10) . . ? O3 Na1 O1 145.24(11) . . ? O9 Na1 O1 139.83(11) . . ? O5 Na1 O4 103.34(11) . . ? O3 Na1 O4 90.45(10) . . ? O9 Na1 O4 118.06(11) . . ? O1 Na1 O4 86.11(10) . . ? O5 Na1 O2 100.65(11) . . ? O3 Na1 O2 81.37(10) . . ? O9 Na1 O2 88.07(10) . . ? O1 Na1 O2 83.67(10) . . ? O4 Na1 O2 148.38(11) . . ? O5 Na1 O11 66.02(12) . . ? O3 Na1 O11 94.77(12) . . ? O9 Na1 O11 62.81(10) . . ? O1 Na1 O11 113.21(12) . . ? O4 Na1 O11 60.75(10) . . ? O2 Na1 O11 149.95(11) . . ? O5 Na1 C48 94.09(12) . . ? O3 Na1 C48 50.90(11) . . ? O9 Na1 C48 20.25(10) . . ? O1 Na1 C48 159.44(11) . . ? O4 Na1 C48 109.64(11) . . ? O2 Na1 C48 88.71(11) . . ? O11 Na1 C48 66.70(12) . . ? O5 Na1 C46 19.90(10) . . ? O3 Na1 C46 164.67(12) . . ? O9 Na1 C46 94.24(12) . . ? O1 Na1 C46 49.90(11) . . ? O4 Na1 C46 93.99(11) . . ? O2 Na1 C46 101.93(12) . . ? O11 Na1 C46 74.79(13) . . ? C48 Na1 C46 113.91(13) . . ? O5 Na1 Zn1 37.17(7) . . ? O3 Na1 Zn1 108.85(8) . . ? O9 Na1 Zn1 41.45(8) . . ? O1 Na1 Zn1 105.69(8) . . ? O4 Na1 Zn1 102.12(8) . . ? O2 Na1 Zn1 109.44(8) . . ? O11 Na1 Zn1 43.57(8) . . ? C48 Na1 Zn1 59.09(9) . . ? C46 Na1 Zn1 55.86(9) . . ? C24 C1 C3 109.0(3) . . ? C24 C1 H1A 109.9 . . ? C3 C1 H1A 109.9 . . ? C24 C1 H1B 109.9 . . ? C3 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C7 C2 C3 123.2(4) . . ? C7 C2 H2 118.4 . . ? C3 C2 H2 118.4 . . ? C4 C3 C2 117.2(4) . . ? C4 C3 C1 122.5(4) . . ? C2 C3 C1 120.0(4) . . ? C3 C4 C5 121.6(4) . . ? C3 C4 O4 118.8(3) . . ? C5 C4 O4 119.6(4) . . ? C6 C5 C4 117.8(4) . . ? C6 C5 C8 120.3(4) . . ? C4 C5 C8 121.8(4) . . ? C7 C6 C5 123.5(4) . . ? C7 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? C6 C7 C2 116.7(4) . . ? C6 C7 C29 121.9(4) . . ? C2 C7 C29 121.4(4) . . ? C9 C8 C5 110.0(3) . . ? C9 C8 H8A 109.7 . . ? C5 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C5 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C14 C9 C10 117.7(4) . . ? C14 C9 C8 121.0(3) . . ? C10 C9 C8 121.2(3) . . ? C11 C10 C9 121.9(4) . . ? C11 C10 O1 119.6(3) . . ? C9 C10 O1 118.5(3) . . ? C10 C11 C12 117.5(3) . . ? C10 C11 C15 121.2(4) . . ? C12 C11 C15 121.0(4) . . ? C11 C12 C13 123.2(4) . . ? C11 C12 H12 118.4 . . ? C13 C12 H12 118.4 . . ? C14 C13 C12 116.6(4) . . ? C14 C13 C41 123.2(4) . . ? C12 C13 C41 120.1(4) . . ? C13 C14 C9 122.8(4) . . ? C13 C14 H14 118.6 . . ? C9 C14 H14 118.6 . . ? C11 C15 C16 109.7(3) . . ? C11 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? C11 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C21 117.7(4) . . ? C17 C16 C15 123.7(4) . . ? C21 C16 C15 118.4(4) . . ? C16 C17 C18 121.0(4) . . ? C16 C17 O2 120.1(4) . . ? C18 C17 O2 118.8(4) . . ? C19 C18 C17 117.8(4) . . ? C19 C18 C22 120.1(4) . . ? C17 C18 C22 122.2(4) . . ? C20 C19 C18 123.1(4) . . ? C20 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? C19 C20 C21 117.0(4) . . ? C19 C20 C37 122.1(4) . . ? C21 C20 C37 120.9(4) . . ? C20 C21 C16 123.0(4) . . ? C20 C21 H21 118.5 . . ? C16 C21 H21 118.5 . . ? C18 C22 C28 112.4(3) . . ? C18 C22 H22A 109.1 . . ? C28 C22 H22A 109.1 . . ? C18 C22 H22B 109.1 . . ? C28 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? O3 C23 C24 119.5(4) . . ? O3 C23 C28 119.1(3) . . ? C24 C23 C28 121.3(4) . . ? C25 C24 C23 117.4(4) . . ? C25 C24 C1 121.0(4) . . ? C23 C24 C1 121.3(4) . . ? C26 C25 C24 122.7(4) . . ? C26 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C27 C26 C25 117.5(4) . . ? C27 C26 C33 120.7(4) . . ? C25 C26 C33 121.7(4) . . ? C26 C27 C28 122.8(4) . . ? C26 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C27 C28 C23 117.6(4) . . ? C27 C28 C22 122.0(4) . . ? C23 C28 C22 120.4(4) . . ? C32' C29 C30' 127.1(11) . . ? C32' C29 C7 116.2(9) . . ? C30' C29 C7 116.6(9) . . ? C32' C29 C32 55.7(9) . . ? C30' C29 C32 106.3(10) . . ? C7 C29 C32 110.1(7) . . ? C32' C29 C30 115.4(11) . . ? C30' C29 C30 48.0(9) . . ? C7 C29 C30 107.3(7) . . ? C32 C29 C30 66.0(8) . . ? C32' C29 C31 104.5(10) . . ? C30' C29 C31 53.1(9) . . ? C7 C29 C31 111.6(7) . . ? C32 C29 C31 138.3(8) . . ? C30 C29 C31 100.7(9) . . ? C32' C29 C31' 39.8(8) . . ? C30' C29 C31' 116.8(11) . . ? C7 C29 C31' 109.4(7) . . ? C32 C29 C31' 95.3(9) . . ? C30 C29 C31' 142.8(9) . . ? C31 C29 C31' 71.3(9) . . ? C30' C30 C29 62.9(13) . . ? C30' C30 C32 111.0(16) . . ? C29 C30 C32 56.9(8) . . ? C30' C31 C29 60.5(11) . . ? C30' C31 C31' 109.3(14) . . ? C29 C31 C31' 55.5(8) . . ? C32' C32 C29 59.5(10) . . ? C32' C32 C30 110.8(14) . . ? C29 C32 C30 57.2(8) . . ? C34' C34 C33 72(2) . . ? C35' C35 C33 76(2) . . ? C38' C38 C37 80.7(19) . . ? C39' C39 C37 59(3) . . ? C30 C30' C31 135(2) . . ? C30 C30' C29 69.1(13) . . ? C31 C30' C29 66.4(11) . . ? C32' C31' C29 63.5(14) . . ? C32' C31' C31 108.6(18) . . ? C29 C31' C31 53.2(7) . . ? C31' C32' C32 141(2) . . ? C31' C32' C29 76.7(16) . . ? C32 C32' C29 64.8(11) . . ? C34 C34' C33 82(2) . . ? C34 C34' C35' 146(3) . . ? C33 C34' C35' 65.3(17) . . ? C35 C35' C34' 117(3) . . ? C35 C35' C33 63(2) . . ? C34' C35' C33 56.3(16) . . ? C38 C38' C37 69.5(18) . . ? C39 C39' C37 90(4) . . ? C39 C39' C40 139(5) . . ? C37 C39' C40 52.8(14) . . ? C36 C33 C26 110.1(4) . . ? C36 C33 C34' 123.3(9) . . ? C26 C33 C34' 108.7(8) . . ? C36 C33 C35 105.5(6) . . ? C26 C33 C35 111.1(5) . . ? C34' C33 C35 97.2(10) . . ? C36 C33 C34 103.4(6) . . ? C26 C33 C34 105.7(5) . . ? C34' C33 C34 25.6(7) . . ? C35 C33 C34 120.6(7) . . ? C36 C33 C35' 135.1(15) . . ? C26 C33 C35' 110.3(15) . . ? C34' C33 C35' 58.4(15) . . ? C35 C33 C35' 40.6(14) . . ? C34 C33 C35' 83.7(15) . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39' C37 C38 123.4(18) . . ? C39' C37 C20 111.2(17) . . ? C38 C37 C20 113.1(5) . . ? C39' C37 C40 82.7(15) . . ? C38 C37 C40 109.6(6) . . ? C20 C37 C40 113.0(5) . . ? C39' C37 C39 30.2(15) . . ? C38 C37 C39 102.6(9) . . ? C20 C37 C39 106.7(6) . . ? C40 C37 C39 111.2(8) . . ? C39' C37 C38' 144.2(19) . . ? C38 C37 C38' 29.8(8) . . ? C20 C37 C38' 104.0(9) . . ? C40 C37 C38' 89.3(9) . . ? C39 C37 C38' 131.6(12) . . ? C37 C40 C39' 44.5(12) . . ? C44 C41 C13 109.3(4) . . ? C44 C41 C42 109.7(5) . . ? C13 C41 C42 112.7(4) . . ? C44 C41 C43 110.0(6) . . ? C13 C41 C43 110.1(4) . . ? C42 C41 C43 105.1(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O1 C45 C46 110.4(3) . . ? O1 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? O1 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? O5 C46 O6 126.1(4) . . ? O5 C46 C45 118.7(4) . . ? O6 C46 C45 115.1(4) . . ? O5 C46 Na1 39.5(2) . . ? O6 C46 Na1 157.1(4) . . ? C45 C46 Na1 82.5(2) . . ? O3 C47 C48 110.5(3) . . ? O3 C47 H47A 109.6 . . ? C48 C47 H47A 109.6 . . ? O3 C47 H47B 109.6 . . ? C48 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? O9 C48 O10 125.7(4) . . ? O9 C48 C47 121.2(4) . . ? O10 C48 C47 113.0(4) . . ? O9 C48 Na1 41.17(19) . . ? O10 C48 Na1 163.9(4) . . ? C47 C48 Na1 80.7(2) . . ? O4 C49 C50 112.3(3) . . ? O4 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? O4 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.9 . . ? O11 C50 O12 125.1(4) . . ? O11 C50 C49 119.1(4) . . ? O12 C50 C49 115.7(4) . . ? O2 C51 C52 115.5(3) . . ? O2 C51 H51A 108.4 . . ? C52 C51 H51A 108.4 . . ? O2 C51 H51B 108.4 . . ? C52 C51 H51B 108.4 . . ? H51A C51 H51B 107.5 . . ? O7 C52 O8 127.4(4) . . ? O7 C52 C51 113.8(4) . . ? O8 C52 C51 118.8(3) . . ? C10 O1 C45 111.2(3) . . ? C10 O1 Na1 131.6(2) . . ? C45 O1 Na1 117.1(2) . . ? C17 O2 C51 114.4(3) . . ? C17 O2 Na1 125.6(2) . . ? C51 O2 Na1 117.0(2) . . ? C23 O3 C47 110.1(3) . . ? C23 O3 Na1 132.2(2) . . ? C47 O3 Na1 117.7(2) . . ? C4 O4 C49 112.6(3) . . ? C4 O4 Na1 118.7(2) . . ? C49 O4 Na1 128.6(2) . . ? C46 O5 Zn1 133.8(3) . . ? C46 O5 Na1 120.6(3) . . ? Zn1 O5 Na1 99.52(13) . . ? C48 O9 Zn1 133.8(3) . . ? C48 O9 Na1 118.6(3) . . ? Zn1 O9 Na1 93.87(11) . . ? C48 O10 Zn2 116.5(3) . . ? C50 O11 Zn1 158.2(4) . . ? C50 O11 Na1 115.1(3) . . ? Zn1 O11 Na1 78.29(11) . . ? C50 O12 Zn2 121.5(3) . 5_575 ? C52 O8 Zn2 127.0(3) . 2 ? C52 O7 Zn1 130.3(3) . 2 ? Zn1 O1W H1D 101(6) . . ? Zn1 O1W H1C 79(6) . . ? H1D O1W H1C 118(4) . . ? Zn2 O13 Zn1 105.63(15) . . ? Zn2 O13 H13 173(5) . . ? Zn1 O13 H13 72(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 Zn1 Zn2 O12 -26.5(3) . . . 5_575 ? O5 Zn1 Zn2 O12 164.9(2) . . . 5_575 ? O7 Zn1 Zn2 O12 94.5(2) 2 . . 5_575 ? O1W Zn1 Zn2 O12 5.4(3) . . . 5_575 ? O9 Zn1 Zn2 O12 -166.4(2) . . . 5_575 ? O11 Zn1 Zn2 O12 -100.7(2) . . . 5_575 ? Na1 Zn1 Zn2 O12 -161.3(2) . . . 5_575 ? O5 Zn1 Zn2 O13 -168.5(2) . . . . ? O7 Zn1 Zn2 O13 121.1(2) 2 . . . ? O1W Zn1 Zn2 O13 31.9(3) . . . . ? O9 Zn1 Zn2 O13 -139.8(2) . . . . ? O11 Zn1 Zn2 O13 -74.2(2) . . . . ? Na1 Zn1 Zn2 O13 -134.8(2) . . . . ? O13 Zn1 Zn2 O10 120.1(2) . . . . ? O5 Zn1 Zn2 O10 -48.43(19) . . . . ? O7 Zn1 Zn2 O10 -118.84(15) 2 . . . ? O1W Zn1 Zn2 O10 152.0(2) . . . . ? O9 Zn1 Zn2 O10 -19.74(14) . . . . ? O11 Zn1 Zn2 O10 45.90(15) . . . . ? Na1 Zn1 Zn2 O10 -14.66(12) . . . . ? O13 Zn1 Zn2 O8 -124.4(2) . . . 2 ? O5 Zn1 Zn2 O8 67.11(17) . . . 2 ? O7 Zn1 Zn2 O8 -3.31(13) 2 . . 2 ? O1W Zn1 Zn2 O8 -92.4(2) . . . 2 ? O9 Zn1 Zn2 O8 95.79(12) . . . 2 ? O11 Zn1 Zn2 O8 161.44(14) . . . 2 ? Na1 Zn1 Zn2 O8 100.88(10) . . . 2 ? O13 Zn1 Na1 O5 173.92(17) . . . . ? O7 Zn1 Na1 O5 -72.23(16) 2 . . . ? O1W Zn1 Na1 O5 41.5(2) . . . . ? O9 Zn1 Na1 O5 -144.92(17) . . . . ? O11 Zn1 Na1 O5 114.22(18) . . . . ? Zn2 Zn1 Na1 O5 -151.46(13) . . . . ? O13 Zn1 Na1 O3 -16.93(16) . . . . ? O5 Zn1 Na1 O3 169.15(16) . . . . ? O7 Zn1 Na1 O3 96.92(13) 2 . . . ? O1W Zn1 Na1 O3 -149.32(19) . . . . ? O9 Zn1 Na1 O3 24.24(13) . . . . ? O11 Zn1 Na1 O3 -76.63(15) . . . . ? Zn2 Zn1 Na1 O3 17.70(9) . . . . ? O13 Zn1 Na1 O9 -41.17(16) . . . . ? O5 Zn1 Na1 O9 144.92(17) . . . . ? O7 Zn1 Na1 O9 72.68(14) 2 . . . ? O1W Zn1 Na1 O9 -173.6(2) . . . . ? O11 Zn1 Na1 O9 -100.87(17) . . . . ? Zn2 Zn1 Na1 O9 -6.54(11) . . . . ? O13 Zn1 Na1 O1 167.08(14) . . . . ? O5 Zn1 Na1 O1 -6.83(14) . . . . ? O7 Zn1 Na1 O1 -79.07(12) 2 . . . ? O1W Zn1 Na1 O1 34.69(19) . . . . ? O9 Zn1 Na1 O1 -151.75(14) . . . . ? O11 Zn1 Na1 O1 107.38(15) . . . . ? Zn2 Zn1 Na1 O1 -158.29(7) . . . . ? O13 Zn1 Na1 O4 77.76(15) . . . . ? O5 Zn1 Na1 O4 -96.16(15) . . . . ? O7 Zn1 Na1 O4 -168.39(12) 2 . . . ? O1W Zn1 Na1 O4 -54.64(19) . . . . ? O9 Zn1 Na1 O4 118.92(14) . . . . ? O11 Zn1 Na1 O4 18.06(14) . . . . ? Zn2 Zn1 Na1 O4 112.38(8) . . . . ? O13 Zn1 Na1 O2 -104.19(15) . . . . ? O5 Zn1 Na1 O2 81.89(15) . . . . ? O7 Zn1 Na1 O2 9.65(13) 2 . . . ? O1W Zn1 Na1 O2 123.41(19) . . . . ? O9 Zn1 Na1 O2 -63.03(13) . . . . ? O11 Zn1 Na1 O2 -163.89(16) . . . . ? Zn2 Zn1 Na1 O2 -69.57(8) . . . . ? O13 Zn1 Na1 O11 59.70(18) . . . . ? O5 Zn1 Na1 O11 -114.22(18) . . . . ? O7 Zn1 Na1 O11 173.55(16) 2 . . . ? O1W Zn1 Na1 O11 -72.7(2) . . . . ? O9 Zn1 Na1 O11 100.87(17) . . . . ? Zn2 Zn1 Na1 O11 94.33(13) . . . . ? O13 Zn1 Na1 C48 -28.04(15) . . . . ? O5 Zn1 Na1 C48 158.05(16) . . . . ? O7 Zn1 Na1 C48 85.81(13) 2 . . . ? O1W Zn1 Na1 C48 -160.4(2) . . . . ? O9 Zn1 Na1 C48 13.13(14) . . . . ? O11 Zn1 Na1 C48 -87.74(16) . . . . ? Zn2 Zn1 Na1 C48 6.59(9) . . . . ? O13 Zn1 Na1 C46 164.34(16) . . . . ? O5 Zn1 Na1 C46 -9.57(16) . . . . ? O7 Zn1 Na1 C46 -81.81(14) 2 . . . ? O1W Zn1 Na1 C46 32.0(2) . . . . ? O9 Zn1 Na1 C46 -154.49(15) . . . . ? O11 Zn1 Na1 C46 104.65(17) . . . . ? Zn2 Zn1 Na1 C46 -161.03(11) . . . . ? C7 C2 C3 C4 1.9(6) . . . . ? C7 C2 C3 C1 -171.8(4) . . . . ? C24 C1 C3 C4 -106.8(4) . . . . ? C24 C1 C3 C2 66.5(5) . . . . ? C2 C3 C4 C5 -3.4(6) . . . . ? C1 C3 C4 C5 170.2(4) . . . . ? C2 C3 C4 O4 179.0(3) . . . . ? C1 C3 C4 O4 -7.4(6) . . . . ? C3 C4 C5 C6 3.1(6) . . . . ? O4 C4 C5 C6 -179.3(3) . . . . ? C3 C4 C5 C8 -173.9(3) . . . . ? O4 C4 C5 C8 3.7(5) . . . . ? C4 C5 C6 C7 -1.3(6) . . . . ? C8 C5 C6 C7 175.8(4) . . . . ? C5 C6 C7 C2 -0.1(6) . . . . ? C5 C6 C7 C29 -177.4(4) . . . . ? C3 C2 C7 C6 -0.2(6) . . . . ? C3 C2 C7 C29 177.1(4) . . . . ? C6 C5 C8 C9 -69.5(4) . . . . ? C4 C5 C8 C9 107.5(4) . . . . ? C5 C8 C9 C14 83.4(4) . . . . ? C5 C8 C9 C10 -92.1(4) . . . . ? C14 C9 C10 C11 -5.9(6) . . . . ? C8 C9 C10 C11 169.8(3) . . . . ? C14 C9 C10 O1 174.5(3) . . . . ? C8 C9 C10 O1 -9.8(5) . . . . ? C9 C10 C11 C12 5.6(6) . . . . ? O1 C10 C11 C12 -174.8(3) . . . . ? C9 C10 C11 C15 -168.7(4) . . . . ? O1 C10 C11 C15 10.9(5) . . . . ? C10 C11 C12 C13 -1.3(6) . . . . ? C15 C11 C12 C13 173.0(4) . . . . ? C11 C12 C13 C14 -2.5(6) . . . . ? C11 C12 C13 C41 179.9(4) . . . . ? C12 C13 C14 C9 2.1(6) . . . . ? C41 C13 C14 C9 179.7(4) . . . . ? C10 C9 C14 C13 1.9(6) . . . . ? C8 C9 C14 C13 -173.8(4) . . . . ? C10 C11 C15 C16 92.3(4) . . . . ? C12 C11 C15 C16 -81.9(5) . . . . ? C11 C15 C16 C17 -99.8(4) . . . . ? C11 C15 C16 C21 74.9(5) . . . . ? C21 C16 C17 C18 -6.9(5) . . . . ? C15 C16 C17 C18 167.9(3) . . . . ? C21 C16 C17 O2 177.5(3) . . . . ? C15 C16 C17 O2 -7.7(5) . . . . ? C16 C17 C18 C19 4.7(5) . . . . ? O2 C17 C18 C19 -179.7(3) . . . . ? C16 C17 C18 C22 -176.1(3) . . . . ? O2 C17 C18 C22 -0.4(5) . . . . ? C17 C18 C19 C20 0.0(6) . . . . ? C22 C18 C19 C20 -179.3(4) . . . . ? C18 C19 C20 C21 -2.1(6) . . . . ? C18 C19 C20 C37 178.6(4) . . . . ? C19 C20 C21 C16 -0.3(6) . . . . ? C37 C20 C21 C16 179.0(4) . . . . ? C17 C16 C21 C20 4.7(6) . . . . ? C15 C16 C21 C20 -170.4(4) . . . . ? C19 C18 C22 C28 -76.8(5) . . . . ? C17 C18 C22 C28 104.0(4) . . . . ? O3 C23 C24 C25 -171.1(3) . . . . ? C28 C23 C24 C25 9.6(5) . . . . ? O3 C23 C24 C1 15.1(5) . . . . ? C28 C23 C24 C1 -164.2(4) . . . . ? C3 C1 C24 C25 -83.6(4) . . . . ? C3 C1 C24 C23 89.9(4) . . . . ? C23 C24 C25 C26 -3.6(6) . . . . ? C1 C24 C25 C26 170.2(4) . . . . ? C24 C25 C26 C27 -3.4(6) . . . . ? C24 C25 C26 C33 178.2(4) . . . . ? C25 C26 C27 C28 4.8(6) . . . . ? C33 C26 C27 C28 -176.8(4) . . . . ? C26 C27 C28 C23 0.9(6) . . . . ? C26 C27 C28 C22 -178.3(4) . . . . ? O3 C23 C28 C27 172.3(3) . . . . ? C24 C23 C28 C27 -8.3(6) . . . . ? O3 C23 C28 C22 -8.5(5) . . . . ? C24 C23 C28 C22 170.8(4) . . . . ? C18 C22 C28 C27 86.9(5) . . . . ? C18 C22 C28 C23 -92.2(5) . . . . ? C6 C7 C29 C32' -165.4(10) . . . . ? C2 C7 C29 C32' 17.5(11) . . . . ? C6 C7 C29 C30' 12.6(11) . . . . ? C2 C7 C29 C30' -164.5(10) . . . . ? C6 C7 C29 C32 133.8(7) . . . . ? C2 C7 C29 C32 -43.3(8) . . . . ? C6 C7 C29 C30 63.7(9) . . . . ? C2 C7 C29 C30 -113.4(8) . . . . ? C6 C7 C29 C31 -45.7(8) . . . . ? C2 C7 C29 C31 137.1(7) . . . . ? C6 C7 C29 C31' -122.7(8) . . . . ? C2 C7 C29 C31' 60.2(9) . . . . ? C32' C29 C30 C30' 118.1(15) . . . . ? C7 C29 C30 C30' -110.6(13) . . . . ? C32 C29 C30 C30' 144.6(15) . . . . ? C31 C29 C30 C30' 6.2(14) . . . . ? C31' C29 C30 C30' 79(2) . . . . ? C32' C29 C30 C32 -26.5(12) . . . . ? C30' C29 C30 C32 -144.6(15) . . . . ? C7 C29 C30 C32 104.8(8) . . . . ? C31 C29 C30 C32 -138.4(9) . . . . ? C31' C29 C30 C32 -65.2(17) . . . . ? C32' C29 C31 C30' -125.8(13) . . . . ? C7 C29 C31 C30' 107.8(11) . . . . ? C32 C29 C31 C30' -71.6(16) . . . . ? C30 C29 C31 C30' -5.8(13) . . . . ? C31' C29 C31 C30' -148.2(13) . . . . ? C32' C29 C31 C31' 22.3(11) . . . . ? C30' C29 C31 C31' 148.2(13) . . . . ? C7 C29 C31 C31' -104.0(8) . . . . ? C32 C29 C31 C31' 76.6(14) . . . . ? C30 C29 C31 C31' 142.4(10) . . . . ? C30' C29 C32 C32' -124.2(13) . . . . ? C7 C29 C32 C32' 108.7(11) . . . . ? C30 C29 C32 C32' -150.8(13) . . . . ? C31 C29 C32 C32' -72.0(16) . . . . ? C31' C29 C32 C32' -4.2(12) . . . . ? C32' C29 C32 C30 150.8(13) . . . . ? C30' C29 C32 C30 26.6(11) . . . . ? C7 C29 C32 C30 -100.6(8) . . . . ? C31 C29 C32 C30 78.8(14) . . . . ? C31' C29 C32 C30 146.6(10) . . . . ? C30' C30 C32 C32' -7(2) . . . . ? C29 C30 C32 C32' 26.7(12) . . . . ? C30' C30 C32 C29 -33.5(14) . . . . ? C29 C30 C30' C31 -10(2) . . . . ? C32 C30 C30' C31 21(3) . . . . ? C32 C30 C30' C29 31.3(12) . . . . ? C29 C31 C30' C30 10(2) . . . . ? C31' C31 C30' C30 -17(3) . . . . ? C31' C31 C30' C29 -27.4(11) . . . . ? C32' C29 C30' C30 -92.5(17) . . . . ? C7 C29 C30' C30 89.8(13) . . . . ? C32 C29 C30' C30 -33.4(14) . . . . ? C31 C29 C30' C30 -172.3(17) . . . . ? C31' C29 C30' C30 -138.3(13) . . . . ? C32' C29 C30' C31 79.9(16) . . . . ? C7 C29 C30' C31 -97.9(10) . . . . ? C32 C29 C30' C31 138.9(10) . . . . ? C30 C29 C30' C31 172.3(17) . . . . ? C31' C29 C30' C31 34.1(14) . . . . ? C30' C29 C31' C32' 116.7(17) . . . . ? C7 C29 C31' C32' -108.1(15) . . . . ? C32 C29 C31' C32' 5.4(16) . . . . ? C30 C29 C31' C32' 62(2) . . . . ? C31 C29 C31' C32' 144.9(16) . . . . ? C32' C29 C31' C31 -144.9(16) . . . . ? C30' C29 C31' C31 -28.2(12) . . . . ? C7 C29 C31' C31 107.0(7) . . . . ? C32 C29 C31' C31 -139.5(9) . . . . ? C30 C29 C31' C31 -83.1(16) . . . . ? C30' C31 C31' C32' -4(2) . . . . ? C29 C31 C31' C32' -32.9(15) . . . . ? C30' C31 C31' C29 29.1(12) . . . . ? C29 C31' C32' C32 -9(3) . . . . ? C31 C31' C32' C32 20(4) . . . . ? C31 C31' C32' C29 29.1(12) . . . . ? C29 C32 C32' C31' 10(3) . . . . ? C30 C32 C32' C31' -16(4) . . . . ? C30 C32 C32' C29 -26.0(11) . . . . ? C30' C29 C32' C31' -88.6(19) . . . . ? C7 C29 C32' C31' 89.2(15) . . . . ? C32 C29 C32' C31' -173.5(19) . . . . ? C30 C29 C32' C31' -143.9(14) . . . . ? C31 C29 C32' C31' -34.2(16) . . . . ? C30' C29 C32' C32 84.8(15) . . . . ? C7 C29 C32' C32 -97.4(10) . . . . ? C30 C29 C32' C32 29.6(13) . . . . ? C31 C29 C32' C32 139.2(10) . . . . ? C31' C29 C32' C32 173.5(19) . . . . ? C33 C34 C34' C35' -17(5) . . . . ? C33 C35 C35' C34' 18(3) . . . . ? C34 C34' C35' C35 0(8) . . . . ? C33 C34' C35' C35 -19(3) . . . . ? C34 C34' C35' C33 19(5) . . . . ? C37 C39 C39' C40 23(4) . . . . ? C27 C26 C33 C36 46.1(6) . . . . ? C25 C26 C33 C36 -135.6(5) . . . . ? C27 C26 C33 C34' -91.6(10) . . . . ? C25 C26 C33 C34' 86.7(10) . . . . ? C27 C26 C33 C35 162.6(7) . . . . ? C25 C26 C33 C35 -19.1(8) . . . . ? C27 C26 C33 C34 -64.9(7) . . . . ? C25 C26 C33 C34 113.4(6) . . . . ? C27 C26 C33 C35' -153.9(16) . . . . ? C25 C26 C33 C35' 24.4(17) . . . . ? C34 C34' C33 C36 -43(2) . . . . ? C35' C34' C33 C36 126.2(18) . . . . ? C34 C34' C33 C26 88(2) . . . . ? C35' C34' C33 C26 -102.9(18) . . . . ? C34 C34' C33 C35 -157(2) . . . . ? C35' C34' C33 C35 12.3(18) . . . . ? C35' C34' C33 C34 170(3) . . . . ? C34 C34' C33 C35' -170(3) . . . . ? C35' C35 C33 C36 -144(2) . . . . ? C35' C35 C33 C26 97(2) . . . . ? C35' C35 C33 C34' -16(2) . . . . ? C35' C35 C33 C34 -27(2) . . . . ? C34' C34 C33 C36 144(2) . . . . ? C34' C34 C33 C26 -100(2) . . . . ? C34' C34 C33 C35 26(2) . . . . ? C34' C34 C33 C35' 9(3) . . . . ? C35 C35' C33 C36 54(3) . . . . ? C34' C35' C33 C36 -107.2(19) . . . . ? C35 C35' C33 C26 -99.1(19) . . . . ? C34' C35' C33 C26 99.9(13) . . . . ? C35 C35' C33 C34' 161(3) . . . . ? C34' C35' C33 C35 -161(3) . . . . ? C35 C35' C33 C34 156(2) . . . . ? C34' C35' C33 C34 -4.5(13) . . . . ? C39 C39' C37 C38 52(4) . . . . ? C40 C39' C37 C38 -108.7(12) . . . . ? C39 C39' C37 C20 -87(4) . . . . ? C40 C39' C37 C20 111.9(8) . . . . ? C39 C39' C37 C40 161(4) . . . . ? C40 C39' C37 C39 -161(4) . . . . ? C39 C39' C37 C38' 83(5) . . . . ? C40 C39' C37 C38' -78(3) . . . . ? C38' C38 C37 C39' 144(3) . . . . ? C38' C38 C37 C20 -77.7(19) . . . . ? C38' C38 C37 C40 49(2) . . . . ? C38' C38 C37 C39 167.7(19) . . . . ? C19 C20 C37 C39' -81.4(17) . . . . ? C21 C20 C37 C39' 99.4(17) . . . . ? C19 C20 C37 C38 134.9(6) . . . . ? C21 C20 C37 C38 -44.3(8) . . . . ? C19 C20 C37 C40 9.6(7) . . . . ? C21 C20 C37 C40 -169.7(5) . . . . ? C19 C20 C37 C39 -113.0(9) . . . . ? C21 C20 C37 C39 67.8(9) . . . . ? C19 C20 C37 C38' 104.9(10) . . . . ? C21 C20 C37 C38' -74.4(10) . . . . ? C39' C39 C37 C38 -137(4) . . . . ? C39' C39 C37 C20 104(4) . . . . ? C39' C39 C37 C40 -20(4) . . . . ? C39' C39 C37 C38' -129(4) . . . . ? C38 C38' C37 C39' -58(4) . . . . ? C38 C38' C37 C20 112.1(17) . . . . ? C38 C38' C37 C40 -134.3(18) . . . . ? C38 C38' C37 C39 -16(2) . . . . ? C38 C37 C40 C39' 122.9(18) . . . . ? C20 C37 C40 C39' -110.0(18) . . . . ? C39 C37 C40 C39' 10(2) . . . . ? C38' C37 C40 C39' 145.0(19) . . . . ? C39 C39' C40 C37 -30(6) . . . . ? C14 C13 C41 C44 -114.1(6) . . . . ? C12 C13 C41 C44 63.4(7) . . . . ? C14 C13 C41 C42 8.1(7) . . . . ? C12 C13 C41 C42 -174.5(4) . . . . ? C14 C13 C41 C43 125.0(5) . . . . ? C12 C13 C41 C43 -57.5(6) . . . . ? O1 C45 C46 O5 18.7(6) . . . . ? O1 C45 C46 O6 -162.0(4) . . . . ? O1 C45 C46 Na1 2.6(3) . . . . ? O3 Na1 C46 O5 12.6(7) . . . . ? O9 Na1 C46 O5 0.6(3) . . . . ? O1 Na1 C46 O5 -159.4(4) . . . . ? O4 Na1 C46 O5 119.1(3) . . . . ? O2 Na1 C46 O5 -88.4(3) . . . . ? O11 Na1 C46 O5 60.9(3) . . . . ? C48 Na1 C46 O5 5.6(4) . . . . ? Zn1 Na1 C46 O5 17.2(3) . . . . ? O5 Na1 C46 O6 -60.7(8) . . . . ? O3 Na1 C46 O6 -48.1(11) . . . . ? O9 Na1 C46 O6 -60.1(9) . . . . ? O1 Na1 C46 O6 139.9(9) . . . . ? O4 Na1 C46 O6 58.4(9) . . . . ? O2 Na1 C46 O6 -149.1(8) . . . . ? O11 Na1 C46 O6 0.2(8) . . . . ? C48 Na1 C46 O6 -55.1(9) . . . . ? Zn1 Na1 C46 O6 -43.5(8) . . . . ? O5 Na1 C46 C45 157.5(5) . . . . ? O3 Na1 C46 C45 170.1(4) . . . . ? O9 Na1 C46 C45 158.0(3) . . . . ? O1 Na1 C46 C45 -1.9(2) . . . . ? O4 Na1 C46 C45 -83.4(3) . . . . ? O2 Na1 C46 C45 69.1(3) . . . . ? O11 Na1 C46 C45 -141.6(3) . . . . ? C48 Na1 C46 C45 163.0(2) . . . . ? Zn1 Na1 C46 C45 174.7(3) . . . . ? O3 C47 C48 O9 -4.7(6) . . . . ? O3 C47 C48 O10 174.2(4) . . . . ? O3 C47 C48 Na1 3.0(3) . . . . ? O5 Na1 C48 O9 -12.7(3) . . . . ? O3 Na1 C48 O9 167.8(4) . . . . ? O1 Na1 C48 O9 19.9(5) . . . . ? O4 Na1 C48 O9 -118.4(3) . . . . ? O2 Na1 C48 O9 87.9(3) . . . . ? O11 Na1 C48 O9 -74.3(3) . . . . ? C46 Na1 C48 O9 -14.6(3) . . . . ? Zn1 Na1 C48 O9 -25.7(3) . . . . ? O5 Na1 C48 O10 27.6(11) . . . . ? O3 Na1 C48 O10 -151.9(12) . . . . ? O9 Na1 C48 O10 40.3(10) . . . . ? O1 Na1 C48 O10 60.2(13) . . . . ? O4 Na1 C48 O10 -78.1(11) . . . . ? O2 Na1 C48 O10 128.2(11) . . . . ? O11 Na1 C48 O10 -34.0(11) . . . . ? C46 Na1 C48 O10 25.7(12) . . . . ? Zn1 Na1 C48 O10 14.5(11) . . . . ? O5 Na1 C48 C47 177.3(3) . . . . ? O3 Na1 C48 C47 -2.2(2) . . . . ? O9 Na1 C48 C47 -170.1(5) . . . . ? O1 Na1 C48 C47 -150.2(3) . . . . ? O4 Na1 C48 C47 71.5(3) . . . . ? O2 Na1 C48 C47 -82.1(3) . . . . ? O11 Na1 C48 C47 115.6(3) . . . . ? C46 Na1 C48 C47 175.4(3) . . . . ? Zn1 Na1 C48 C47 164.2(3) . . . . ? O4 C49 C50 O11 22.8(6) . . . . ? O4 C49 C50 O12 -161.4(4) . . . . ? O2 C51 C52 O7 159.6(4) . . . . ? O2 C51 C52 O8 -23.5(5) . . . . ? C11 C10 O1 C45 90.3(4) . . . . ? C9 C10 O1 C45 -90.1(4) . . . . ? C11 C10 O1 Na1 -92.8(4) . . . . ? C9 C10 O1 Na1 86.8(4) . . . . ? C46 C45 O1 C10 173.6(3) . . . . ? C46 C45 O1 Na1 -3.7(4) . . . . ? O5 Na1 O1 C10 178.1(3) . . . . ? O3 Na1 O1 C10 9.2(4) . . . . ? O9 Na1 O1 C10 153.5(3) . . . . ? O4 Na1 O1 C10 -76.0(3) . . . . ? O2 Na1 O1 C10 74.1(3) . . . . ? O11 Na1 O1 C10 -131.8(3) . . . . ? C48 Na1 O1 C10 142.9(4) . . . . ? C46 Na1 O1 C10 -174.5(3) . . . . ? Zn1 Na1 O1 C10 -177.5(3) . . . . ? O5 Na1 O1 C45 -5.2(3) . . . . ? O3 Na1 O1 C45 -174.1(3) . . . . ? O9 Na1 O1 C45 -29.8(3) . . . . ? O4 Na1 O1 C45 100.8(3) . . . . ? O2 Na1 O1 C45 -109.2(3) . . . . ? O11 Na1 O1 C45 45.0(3) . . . . ? C48 Na1 O1 C45 -40.3(5) . . . . ? C46 Na1 O1 C45 2.2(3) . . . . ? Zn1 Na1 O1 C45 -0.8(3) . . . . ? C16 C17 O2 C51 -71.0(4) . . . . ? C18 C17 O2 C51 113.3(4) . . . . ? C16 C17 O2 Na1 88.6(4) . . . . ? C18 C17 O2 Na1 -87.1(4) . . . . ? C52 C51 O2 C17 -87.3(4) . . . . ? C52 C51 O2 Na1 111.2(3) . . . . ? O5 Na1 O2 C17 -137.4(3) . . . . ? O3 Na1 O2 C17 78.1(3) . . . . ? O9 Na1 O2 C17 149.0(3) . . . . ? O1 Na1 O2 C17 -70.4(3) . . . . ? O4 Na1 O2 C17 1.5(4) . . . . ? O11 Na1 O2 C17 162.7(3) . . . . ? C48 Na1 O2 C17 128.7(3) . . . . ? C46 Na1 O2 C17 -117.1(3) . . . . ? Zn1 Na1 O2 C17 -174.9(3) . . . . ? O5 Na1 O2 C51 21.8(3) . . . . ? O3 Na1 O2 C51 -122.7(2) . . . . ? O9 Na1 O2 C51 -51.9(3) . . . . ? O1 Na1 O2 C51 88.8(2) . . . . ? O4 Na1 O2 C51 160.7(3) . . . . ? O11 Na1 O2 C51 -38.1(4) . . . . ? C48 Na1 O2 C51 -72.1(3) . . . . ? C46 Na1 O2 C51 42.1(3) . . . . ? Zn1 Na1 O2 C51 -15.7(3) . . . . ? C24 C23 O3 C47 94.8(4) . . . . ? C28 C23 O3 C47 -85.8(4) . . . . ? C24 C23 O3 Na1 -85.2(4) . . . . ? C28 C23 O3 Na1 94.1(4) . . . . ? C48 C47 O3 C23 175.5(4) . . . . ? C48 C47 O3 Na1 -4.5(5) . . . . ? O5 Na1 O3 C23 -178.2(3) . . . . ? O9 Na1 O3 C23 -172.9(3) . . . . ? O1 Na1 O3 C23 -16.4(4) . . . . ? O4 Na1 O3 C23 67.4(3) . . . . ? O2 Na1 O3 C23 -81.9(3) . . . . ? O11 Na1 O3 C23 128.1(3) . . . . ? C48 Na1 O3 C23 -177.3(4) . . . . ? C46 Na1 O3 C23 174.4(5) . . . . ? Zn1 Na1 O3 C23 170.4(3) . . . . ? O5 Na1 O3 C47 1.8(4) . . . . ? O9 Na1 O3 C47 7.1(3) . . . . ? O1 Na1 O3 C47 163.6(3) . . . . ? O4 Na1 O3 C47 -112.6(3) . . . . ? O2 Na1 O3 C47 98.0(3) . . . . ? O11 Na1 O3 C47 -52.0(3) . . . . ? C48 Na1 O3 C47 2.6(3) . . . . ? C46 Na1 O3 C47 -5.7(6) . . . . ? Zn1 Na1 O3 C47 -9.7(3) . . . . ? C3 C4 O4 C49 -89.0(4) . . . . ? C5 C4 O4 C49 93.4(4) . . . . ? C3 C4 O4 Na1 88.1(4) . . . . ? C5 C4 O4 Na1 -89.5(4) . . . . ? C50 C49 O4 C4 153.9(4) . . . . ? C50 C49 O4 Na1 -22.8(5) . . . . ? O5 Na1 O4 C4 142.9(2) . . . . ? O3 Na1 O4 C4 -69.5(3) . . . . ? O9 Na1 O4 C4 -137.9(2) . . . . ? O1 Na1 O4 C4 75.8(2) . . . . ? O2 Na1 O4 C4 4.6(4) . . . . ? O11 Na1 O4 C4 -164.8(3) . . . . ? C48 Na1 O4 C4 -117.7(3) . . . . ? C46 Na1 O4 C4 125.2(3) . . . . ? Zn1 Na1 O4 C4 -178.9(2) . . . . ? O5 Na1 O4 C49 -40.5(3) . . . . ? O3 Na1 O4 C49 107.0(3) . . . . ? O9 Na1 O4 C49 38.7(3) . . . . ? O1 Na1 O4 C49 -107.6(3) . . . . ? O2 Na1 O4 C49 -178.8(3) . . . . ? O11 Na1 O4 C49 11.8(3) . . . . ? C48 Na1 O4 C49 58.9(3) . . . . ? C46 Na1 O4 C49 -58.3(3) . . . . ? Zn1 Na1 O4 C49 -2.4(3) . . . . ? O6 C46 O5 Zn1 8.7(8) . . . . ? C45 C46 O5 Zn1 -172.1(3) . . . . ? Na1 C46 O5 Zn1 -146.5(5) . . . . ? O6 C46 O5 Na1 155.1(4) . . . . ? C45 C46 O5 Na1 -25.7(6) . . . . ? O13 Zn1 O5 C46 109.4(12) . . . . ? O7 Zn1 O5 C46 -93.7(4) 2 . . . ? O1W Zn1 O5 C46 4.6(4) . . . . ? O9 Zn1 O5 C46 175.2(4) . . . . ? O11 Zn1 O5 C46 99.7(4) . . . . ? Zn2 Zn1 O5 C46 -158.9(3) . . . . ? Na1 Zn1 O5 C46 151.2(5) . . . . ? O13 Zn1 O5 Na1 -41.7(12) . . . . ? O7 Zn1 O5 Na1 115.13(13) 2 . . . ? O1W Zn1 O5 Na1 -146.54(17) . . . . ? O9 Zn1 O5 Na1 24.03(11) . . . . ? O11 Zn1 O5 Na1 -51.52(14) . . . . ? Zn2 Zn1 O5 Na1 49.96(19) . . . . ? O3 Na1 O5 C46 -174.2(3) . . . . ? O9 Na1 O5 C46 -179.4(4) . . . . ? O1 Na1 O5 C46 16.8(3) . . . . ? O4 Na1 O5 C46 -63.6(4) . . . . ? O2 Na1 O5 C46 95.6(3) . . . . ? O11 Na1 O5 C46 -112.7(4) . . . . ? C48 Na1 O5 C46 -174.9(3) . . . . ? Zn1 Na1 O5 C46 -156.1(4) . . . . ? O3 Na1 O5 Zn1 -18.1(3) . . . . ? O9 Na1 O5 Zn1 -23.28(11) . . . . ? O1 Na1 O5 Zn1 172.94(14) . . . . ? O4 Na1 O5 Zn1 92.55(12) . . . . ? O2 Na1 O5 Zn1 -108.21(12) . . . . ? O11 Na1 O5 Zn1 43.47(12) . . . . ? C48 Na1 O5 Zn1 -18.76(13) . . . . ? C46 Na1 O5 Zn1 156.1(4) . . . . ? O10 C48 O9 Zn1 -38.3(7) . . . . ? C47 C48 O9 Zn1 140.4(4) . . . . ? Na1 C48 O9 Zn1 128.9(4) . . . . ? O10 C48 O9 Na1 -167.2(4) . . . . ? C47 C48 O9 Na1 11.5(5) . . . . ? O13 Zn1 O9 C48 13.5(4) . . . . ? O5 Zn1 O9 C48 -160.2(4) . . . . ? O7 Zn1 O9 C48 108.4(4) 2 . . . ? O1W Zn1 O9 C48 -111.4(8) . . . . ? O11 Zn1 O9 C48 -77.0(4) . . . . ? Zn2 Zn1 O9 C48 36.4(3) . . . . ? Na1 Zn1 O9 C48 -136.8(4) . . . . ? O13 Zn1 O9 Na1 150.33(12) . . . . ? O5 Zn1 O9 Na1 -23.40(11) . . . . ? O7 Zn1 O9 Na1 -114.84(12) 2 . . . ? O1W Zn1 O9 Na1 25.4(7) . . . . ? O11 Zn1 O9 Na1 59.82(12) . . . . ? Zn2 Zn1 O9 Na1 173.17(11) . . . . ? O5 Na1 O9 C48 166.9(3) . . . . ? O3 Na1 O9 C48 -10.0(3) . . . . ? O1 Na1 O9 C48 -169.3(3) . . . . ? O4 Na1 O9 C48 69.9(3) . . . . ? O2 Na1 O9 C48 -91.5(3) . . . . ? O11 Na1 O9 C48 96.2(3) . . . . ? C46 Na1 O9 C48 166.7(3) . . . . ? Zn1 Na1 O9 C48 145.7(4) . . . . ? O5 Na1 O9 Zn1 21.14(10) . . . . ? O3 Na1 O9 Zn1 -155.71(13) . . . . ? O1 Na1 O9 Zn1 44.9(2) . . . . ? O4 Na1 O9 Zn1 -75.87(13) . . . . ? O2 Na1 O9 Zn1 122.77(10) . . . . ? O11 Na1 O9 Zn1 -49.56(12) . . . . ? C48 Na1 O9 Zn1 -145.7(4) . . . . ? C46 Na1 O9 Zn1 20.94(13) . . . . ? O9 C48 O10 Zn2 1.4(6) . . . . ? C47 C48 O10 Zn2 -177.5(3) . . . . ? Na1 C48 O10 Zn2 -30.3(13) . . . . ? O12 Zn2 O10 C48 -179.2(3) 5_575 . . . ? O13 Zn2 O10 C48 50.1(4) . . . . ? O8 Zn2 O10 C48 -61.3(4) 2 . . . ? Zn1 Zn2 O10 C48 16.9(3) . . . . ? O12 C50 O11 Zn1 -64.7(11) . . . . ? C49 C50 O11 Zn1 110.6(8) . . . . ? O12 C50 O11 Na1 170.6(3) . . . . ? C49 C50 O11 Na1 -14.1(5) . . . . ? O13 Zn1 O11 C50 89.9(9) . . . . ? O5 Zn1 O11 C50 -91.3(9) . . . . ? O7 Zn1 O11 C50 -155.0(7) 2 . . . ? O1W Zn1 O11 C50 -3.3(9) . . . . ? O9 Zn1 O11 C50 -176.2(9) . . . . ? Zn2 Zn1 O11 C50 125.2(9) . . . . ? Na1 Zn1 O11 C50 -130.5(9) . . . . ? O13 Zn1 O11 Na1 -139.62(14) . . . . ? O5 Zn1 O11 Na1 39.22(10) . . . . ? O7 Zn1 O11 Na1 -24.5(6) 2 . . . ? O1W Zn1 O11 Na1 127.20(13) . . . . ? O9 Zn1 O11 Na1 -45.70(10) . . . . ? Zn2 Zn1 O11 Na1 -104.32(7) . . . . ? O5 Na1 O11 C50 124.7(4) . . . . ? O3 Na1 O11 C50 -85.7(4) . . . . ? O9 Na1 O11 C50 -151.2(4) . . . . ? O1 Na1 O11 C50 73.2(4) . . . . ? O4 Na1 O11 C50 2.2(3) . . . . ? O2 Na1 O11 C50 -166.7(3) . . . . ? C48 Na1 O11 C50 -129.2(4) . . . . ? C46 Na1 O11 C50 105.8(4) . . . . ? Zn1 Na1 O11 C50 161.8(4) . . . . ? O5 Na1 O11 Zn1 -37.09(10) . . . . ? O3 Na1 O11 Zn1 112.49(12) . . . . ? O9 Na1 O11 Zn1 46.97(10) . . . . ? O1 Na1 O11 Zn1 -88.63(12) . . . . ? O4 Na1 O11 Zn1 -159.67(16) . . . . ? O2 Na1 O11 Zn1 31.5(3) . . . . ? C48 Na1 O11 Zn1 68.97(12) . . . . ? C46 Na1 O11 Zn1 -56.08(12) . . . . ? O11 C50 O12 Zn2 -28.5(6) . . . 5_575 ? C49 C50 O12 Zn2 156.0(3) . . . 5_575 ? O7 C52 O8 Zn2 -11.0(6) . . . 2 ? C51 C52 O8 Zn2 172.6(3) . . . 2 ? O8 C52 O7 Zn1 5.5(7) . . . 2 ? C51 C52 O7 Zn1 -177.9(3) . . . 2 ? O12 Zn2 O13 Zn1 166.71(14) 5_575 . . . ? O10 Zn2 O13 Zn1 -64.0(2) . . . . ? O8 Zn2 O13 Zn1 56.24(19) 2 . . . ? O5 Zn1 O13 Zn2 100.9(11) . . . . ? O7 Zn1 O13 Zn2 -55.86(19) 2 . . . ? O1W Zn1 O13 Zn2 -154.5(2) . . . . ? O9 Zn1 O13 Zn2 35.78(18) . . . . ? O11 Zn1 O13 Zn2 110.61(18) . . . . ? Na1 Zn1 O13 Zn2 63.43(19) . . . . ? _diffrn_measured_fraction_theta_max 0.846 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.446 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.088 #===== data_13 _database_code_depnum_ccdc_archive 'CCDC 879395' #TrackingRef '- Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H122 Na2 O26 Pb4' _chemical_formula_weight 2662.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.957(5) _cell_length_b 12.644(4) _cell_length_c 21.490(3) _cell_angle_alpha 86.158(4) _cell_angle_beta 82.931(6) _cell_angle_gamma 67.840(7) _cell_volume 2735.7(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1302 _exptl_absorpt_coefficient_mu 6.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3057 _exptl_absorpt_correction_T_max 0.4010 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17793 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.1329 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.40 _reflns_number_total 9911 _reflns_number_gt 5471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. For C43, C43', C44, C44', C30, C30', C31, C31', C32, C32' C42 and C42', some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9911 _refine_ls_number_parameters 646 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1052 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.93585(5) 0.64327(4) 0.949131(17) 0.04151(16) Uani 1 1 d . . . Pb2 Pb 0.67757(5) 0.50022(5) 1.06102(2) 0.0568(2) Uani 0.90 1 d P . . Pb2' Pb 0.6378(4) 0.6051(4) 1.02707(15) 0.0403(12) Uani 0.10 1 d P . . Na1 Na 1.0021(3) 0.3079(3) 0.85501(14) 0.0202(8) Uani 1 1 d . . . C1 C 0.6513(10) 0.3409(9) 0.6475(4) 0.030(2) Uani 1 1 d . . . C2 C 0.7402(10) 0.3958(9) 0.6410(4) 0.030(2) Uani 1 1 d . . . H2 H 0.7638 0.4202 0.6012 0.035 Uiso 1 1 calc R . . C3 C 0.7957(9) 0.4160(8) 0.6917(4) 0.026(2) Uani 1 1 d . . . C4 C 0.7575(9) 0.3811(8) 0.7506(4) 0.025(2) Uani 1 1 d . . . C5 C 0.6704(10) 0.3235(8) 0.7601(4) 0.028(2) Uani 1 1 d . . . C6 C 0.6192(10) 0.3058(9) 0.7069(4) 0.031(2) Uani 1 1 d . . . H6 H 0.5601 0.2683 0.7121 0.038 Uiso 1 1 calc R . . C7 C 0.6401(10) 0.2740(9) 0.8240(4) 0.032(2) Uani 1 1 d . . . H7A H 0.5485 0.2803 0.8296 0.038 Uiso 1 1 calc R . . H7B H 0.6534 0.3164 0.8569 0.038 Uiso 1 1 calc R . . C8 C 0.7330(9) 0.1473(8) 0.8284(4) 0.025(2) Uani 1 1 d . . . C9 C 0.8469(9) 0.1121(8) 0.8580(4) 0.024(2) Uani 1 1 d . . . C10 C 0.9366(9) -0.0016(9) 0.8547(4) 0.027(2) Uani 1 1 d . . . C11 C 0.9036(10) -0.0801(8) 0.8262(4) 0.027(2) Uani 1 1 d . . . H11 H 0.9605 -0.1563 0.8257 0.033 Uiso 1 1 calc R . . C12 C 0.7854(10) -0.0470(9) 0.7978(4) 0.029(2) Uani 1 1 d . . . C13 C 0.7059(10) 0.0653(9) 0.7999(4) 0.029(2) Uani 1 1 d . . . H13 H 0.6279 0.0885 0.7809 0.035 Uiso 1 1 calc R . . C14 C 1.0759(9) -0.0392(9) 0.8783(4) 0.034(2) Uani 1 1 d . . . H14A H 1.0768 0.0166 0.9069 0.040 Uiso 1 1 calc R . . H14B H 1.0969 -0.1122 0.9005 0.040 Uiso 1 1 calc R . . C15 C 1.1781(10) -0.0490(9) 0.8219(4) 0.029(2) Uani 1 1 d . . . C16 C 1.2235(10) -0.1428(9) 0.7836(4) 0.031(2) Uani 1 1 d . . . H16 H 1.1986 -0.2046 0.7949 0.038 Uiso 1 1 calc R . . C17 C 1.3073(10) -0.1462(9) 0.7275(4) 0.034(3) Uani 1 1 d . . . C18 C 1.3398(10) -0.0515(9) 0.7116(4) 0.031(2) Uani 1 1 d . . . H18 H 1.3916 -0.0518 0.6739 0.037 Uiso 1 1 calc R . . C19 C 1.2999(10) 0.0430(9) 0.7484(4) 0.032(2) Uani 1 1 d . . . C20 C 1.2232(9) 0.0410(9) 0.8054(4) 0.028(2) Uani 1 1 d . . . C21 C 1.3305(10) 0.1460(9) 0.7285(4) 0.035(3) Uani 1 1 d . . . H21A H 1.4217 0.1225 0.7098 0.042 Uiso 1 1 calc R . . H21B H 1.3213 0.1906 0.7651 0.042 Uiso 1 1 calc R . . C22 C 1.2376(10) 0.2210(9) 0.6808(4) 0.029(2) Uani 1 1 d . . . C23 C 1.2543(10) 0.1849(9) 0.6196(4) 0.036(3) Uani 1 1 d . . . H23 H 1.3252 0.1183 0.6077 0.043 Uiso 1 1 calc R . . C24 C 1.1687(11) 0.2447(10) 0.5756(4) 0.043(3) Uani 1 1 d . . . C25 C 1.0575(11) 0.3368(9) 0.5974(4) 0.037(3) Uani 1 1 d . . . H25 H 0.9953 0.3749 0.5697 0.044 Uiso 1 1 calc R . . C26 C 1.1306(10) 0.3175(9) 0.6988(4) 0.028(2) Uani 1 1 d . . . C27 C 1.0343(10) 0.3748(8) 0.6577(4) 0.029(2) Uani 1 1 d . . . C28 C 0.9039(10) 0.4666(9) 0.6809(4) 0.033(2) Uani 1 1 d . . . H28A H 0.8799 0.5288 0.6502 0.039 Uiso 1 1 calc R . . H28B H 0.9125 0.4967 0.7198 0.039 Uiso 1 1 calc R . . C29 C 1.3549(11) -0.2527(10) 0.6863(5) 0.045(3) Uani 1 1 d . . . C30 C 1.474(3) -0.262(3) 0.6393(12) 0.050(7) Uani 0.50 1 d PU . . C30' C 1.430(3) -0.235(3) 0.6236(13) 0.047(8) Uiso 0.50 1 d P . . C31' C 1.400(4) -0.367(3) 0.7293(17) 0.077(12) Uiso 0.50 1 d P . . C31 C 1.453(3) -0.356(3) 0.7248(13) 0.056(8) Uani 0.50 1 d PU . . C32' C 1.233(3) -0.256(3) 0.6541(14) 0.062(9) Uiso 0.50 1 d P . . C32 C 1.231(3) -0.290(3) 0.6797(15) 0.064(8) Uani 0.50 1 d PU . . C33 C 0.7480(11) -0.1334(10) 0.7647(4) 0.037(3) Uani 1 1 d . . . C34 C 0.8557(13) -0.2519(10) 0.7612(6) 0.056(3) Uani 1 1 d . . . H34A H 0.8774 -0.2795 0.8027 0.085 Uiso 1 1 calc R . . H34B H 0.9332 -0.2486 0.7362 0.085 Uiso 1 1 calc R . . H34C H 0.8247 -0.3027 0.7425 0.085 Uiso 1 1 calc R . . C35 C 0.7145(14) -0.0905(11) 0.6980(5) 0.057(4) Uani 1 1 d . . . H35A H 0.6465 -0.0154 0.6997 0.085 Uiso 1 1 calc R . . H35B H 0.6837 -0.1415 0.6794 0.085 Uiso 1 1 calc R . . H35C H 0.7923 -0.0877 0.6731 0.085 Uiso 1 1 calc R . . C36 C 0.6229(12) -0.1416(11) 0.8039(6) 0.055(3) Uani 1 1 d . . . H36A H 0.5540 -0.0671 0.8068 0.083 Uiso 1 1 calc R . . H36B H 0.6441 -0.1709 0.8452 0.083 Uiso 1 1 calc R . . H36C H 0.5932 -0.1918 0.7838 0.083 Uiso 1 1 calc R . . C37 C 0.5910(11) 0.3191(10) 0.5904(4) 0.038(3) Uani 1 1 d . . . C38 C 0.6394(15) 0.3647(14) 0.5302(5) 0.073(5) Uani 1 1 d . . . H38A H 0.6186 0.4451 0.5336 0.110 Uiso 1 1 calc R . . H38B H 0.5971 0.3521 0.4964 0.110 Uiso 1 1 calc R . . H38C H 0.7337 0.3261 0.5220 0.110 Uiso 1 1 calc R . . C39 C 0.6179(14) 0.1954(11) 0.5868(5) 0.062(4) Uani 1 1 d . . . H39A H 0.5853 0.1689 0.6258 0.093 Uiso 1 1 calc R . . H39B H 0.7116 0.1540 0.5788 0.093 Uiso 1 1 calc R . . H39C H 0.5741 0.1832 0.5535 0.093 Uiso 1 1 calc R . . C40 C 0.4419(12) 0.3804(13) 0.5994(6) 0.065(4) Uani 1 1 d . . . H40A H 0.4207 0.4611 0.6016 0.097 Uiso 1 1 calc R . . H40B H 0.4069 0.3536 0.6377 0.097 Uiso 1 1 calc R . . H40C H 0.4037 0.3654 0.5648 0.097 Uiso 1 1 calc R . . C41 C 1.1883(13) 0.2064(12) 0.5074(5) 0.058(4) Uani 1 1 d . . . C42' C 1.309(4) 0.092(4) 0.4983(18) 0.080(13) Uiso 0.50 1 d P . . C42 C 1.334(3) 0.125(3) 0.4865(13) 0.054(8) Uani 0.50 1 d PU . . C43' C 1.095(3) 0.141(3) 0.5024(14) 0.074(9) Uiso 0.50 1 d P . . C43 C 1.065(3) 0.210(3) 0.4843(14) 0.078(9) Uani 0.50 1 d PU . . C44 C 1.211(3) 0.309(2) 0.4639(9) 0.046(6) Uani 0.50 1 d PU . . C44' C 1.134(5) 0.303(4) 0.462(2) 0.123(16) Uiso 0.50 1 d P . . C45 C 1.1613(12) 0.4505(10) 0.7633(4) 0.040(3) Uani 1 1 d . . . H45A H 1.0878 0.5213 0.7564 0.048 Uiso 1 1 calc R . . H45B H 1.2314 0.4445 0.7298 0.048 Uiso 1 1 calc R . . C46 C 1.2097(17) 0.4569(16) 0.8231(6) 0.075(5) Uani 1 1 d . . . C47 C 1.2726(11) 0.1116(10) 0.8946(5) 0.041(3) Uani 1 1 d . . . H47A H 1.3544 0.1200 0.8770 0.049 Uiso 1 1 calc R . . H47B H 1.2945 0.0337 0.9105 0.049 Uiso 1 1 calc R . . C48 C 1.2114(14) 0.1905(12) 0.9466(6) 0.058(3) Uani 1 1 d . . . C49 C 0.7222(11) 0.5121(9) 0.8304(4) 0.036(3) Uani 1 1 d . . . H49A H 0.6428 0.5046 0.8522 0.043 Uiso 1 1 calc R . . H49B H 0.6957 0.5703 0.7977 0.043 Uiso 1 1 calc R . . C50 C 0.7918(14) 0.5471(10) 0.8749(5) 0.045(3) Uani 1 1 d . . . C51 C 0.8428(12) 0.1859(9) 0.9582(4) 0.042(3) Uani 1 1 d . . . H51A H 0.9197 0.1332 0.9770 0.050 Uiso 1 1 calc R . . H51B H 0.7721 0.1568 0.9670 0.050 Uiso 1 1 calc R . . C79 C 0.8010(14) 0.2984(10) 0.9865(5) 0.053(3) Uani 1 1 d . . . O1 O 1.1185(6) 0.3574(6) 0.7589(3) 0.0308(16) Uani 1 1 d . . . O2 O 0.8061(6) 0.4060(6) 0.8031(3) 0.0298(16) Uani 1 1 d . . . O3 O 0.8754(7) 0.1911(6) 0.8908(3) 0.0302(16) Uani 1 1 d . . . O4 O 1.1865(6) 0.1322(6) 0.8462(3) 0.0321(16) Uani 1 1 d . . . O5 O 1.2617(10) 0.3598(10) 0.8535(4) 0.079(3) Uani 1 1 d . . . O6 O 1.2025(11) 0.5514(8) 0.8412(4) 0.076(3) Uani 1 1 d . . . O7 O 0.9210(10) 0.4951(7) 0.8760(3) 0.059(2) Uani 1 1 d . . . O8 O 0.7261(8) 0.6301(7) 0.9078(3) 0.052(2) Uani 1 1 d . . . O9 O 0.8247(8) 0.3017(7) 1.0428(3) 0.046(2) Uani 1 1 d . . . O10 O 0.7327(10) 0.3877(8) 0.9555(4) 0.072(3) Uani 1 1 d . . . O11 O 1.2816(9) 0.1900(9) 0.9887(4) 0.081(3) Uani 1 1 d . . . O12 O 1.0898(10) 0.2546(8) 0.9469(3) 0.061(2) Uani 1 1 d . . . O13 O 0.8665(8) 0.5345(7) 1.0270(3) 0.047(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0669(3) 0.0371(3) 0.0290(2) -0.00163(17) -0.01291(18) -0.0264(2) Pb2 0.0549(4) 0.0536(4) 0.0575(3) -0.0200(3) -0.0022(3) -0.0133(3) Pb2' 0.024(2) 0.074(3) 0.0110(17) 0.0020(17) 0.0075(14) -0.008(2) Na1 0.0163(19) 0.0104(19) 0.0314(18) 0.0099(14) -0.0066(14) -0.0024(16) C1 0.036(6) 0.030(6) 0.023(5) -0.004(4) -0.010(4) -0.011(5) C2 0.038(6) 0.030(6) 0.018(5) 0.000(4) -0.007(4) -0.008(5) C3 0.026(6) 0.019(6) 0.027(5) -0.002(4) -0.003(4) -0.003(5) C4 0.021(6) 0.020(6) 0.030(5) -0.004(4) -0.014(4) 0.001(5) C5 0.028(6) 0.023(6) 0.026(5) -0.003(4) -0.003(4) -0.002(5) C6 0.033(6) 0.029(6) 0.036(6) -0.008(4) -0.002(4) -0.015(5) C7 0.037(6) 0.029(6) 0.033(5) -0.005(4) 0.002(4) -0.018(5) C8 0.022(6) 0.028(6) 0.020(4) -0.001(4) 0.005(4) -0.006(5) C9 0.033(6) 0.024(6) 0.015(4) -0.002(4) 0.002(4) -0.014(5) C10 0.030(6) 0.030(6) 0.021(5) 0.000(4) -0.007(4) -0.009(5) C11 0.036(6) 0.015(5) 0.029(5) 0.000(4) -0.004(4) -0.007(5) C12 0.029(6) 0.025(6) 0.032(5) -0.007(4) 0.002(4) -0.010(5) C13 0.023(6) 0.029(7) 0.034(5) 0.000(4) -0.013(4) -0.005(5) C14 0.036(6) 0.031(6) 0.030(5) 0.004(4) -0.010(4) -0.006(5) C15 0.027(6) 0.029(6) 0.027(5) -0.002(4) -0.006(4) -0.005(5) C16 0.033(6) 0.025(6) 0.033(5) -0.005(4) -0.007(4) -0.006(5) C17 0.030(6) 0.036(7) 0.030(5) -0.016(4) -0.004(4) -0.003(5) C18 0.026(6) 0.037(7) 0.026(5) -0.006(4) 0.003(4) -0.008(5) C19 0.032(6) 0.036(7) 0.028(5) -0.003(4) -0.011(4) -0.010(5) C20 0.026(6) 0.027(6) 0.024(5) -0.008(4) -0.007(4) 0.002(5) C21 0.035(6) 0.037(7) 0.034(5) -0.005(4) -0.005(4) -0.015(6) C22 0.030(6) 0.038(7) 0.025(5) -0.001(4) 0.000(4) -0.021(5) C23 0.035(7) 0.034(7) 0.030(5) -0.005(4) 0.004(4) -0.005(5) C24 0.050(8) 0.048(8) 0.031(6) -0.010(5) 0.005(5) -0.021(6) C25 0.043(7) 0.037(7) 0.030(5) 0.002(5) -0.012(5) -0.014(6) C26 0.036(6) 0.026(6) 0.025(5) -0.005(4) -0.002(4) -0.016(5) C27 0.042(7) 0.019(6) 0.030(5) -0.004(4) 0.004(4) -0.015(5) C28 0.046(7) 0.031(6) 0.027(5) 0.000(4) -0.004(4) -0.020(6) C29 0.051(8) 0.032(7) 0.050(6) -0.024(5) 0.000(5) -0.010(6) C30 0.052(11) 0.047(11) 0.043(10) -0.007(8) 0.007(8) -0.010(8) C31 0.054(11) 0.050(11) 0.056(11) -0.008(8) -0.009(8) -0.009(9) C32 0.075(12) 0.058(11) 0.071(12) -0.016(8) -0.013(9) -0.035(9) C33 0.044(7) 0.037(7) 0.037(5) -0.004(5) -0.010(5) -0.020(6) C34 0.068(9) 0.025(7) 0.081(8) -0.006(6) -0.020(7) -0.018(7) C35 0.092(10) 0.043(8) 0.036(6) -0.012(5) -0.018(6) -0.021(7) C36 0.049(8) 0.051(9) 0.073(8) -0.003(6) -0.009(6) -0.025(7) C37 0.051(8) 0.049(8) 0.022(5) -0.004(4) -0.009(4) -0.026(6) C38 0.090(11) 0.118(14) 0.034(7) 0.011(7) -0.027(6) -0.060(10) C39 0.091(11) 0.052(9) 0.050(7) -0.017(6) -0.023(7) -0.027(8) C40 0.054(9) 0.084(11) 0.068(8) 0.010(7) -0.036(7) -0.032(8) C41 0.059(9) 0.070(10) 0.035(6) -0.021(6) -0.003(5) -0.011(8) C42 0.055(11) 0.054(11) 0.044(10) -0.013(8) 0.011(8) -0.013(9) C43 0.079(12) 0.089(12) 0.067(11) -0.018(9) -0.017(9) -0.028(9) C44 0.057(10) 0.050(10) 0.027(8) 0.002(7) 0.010(7) -0.019(8) C45 0.061(8) 0.041(7) 0.032(5) -0.006(5) -0.006(5) -0.032(6) C46 0.117(13) 0.089(13) 0.035(7) -0.005(7) 0.019(7) -0.064(11) C47 0.036(7) 0.038(7) 0.046(6) -0.008(5) -0.023(5) -0.004(6) C48 0.054(9) 0.043(9) 0.071(9) -0.019(6) -0.003(7) -0.010(8) C49 0.045(7) 0.037(7) 0.032(5) 0.002(4) -0.006(5) -0.021(6) C50 0.067(9) 0.036(8) 0.032(6) -0.001(5) -0.007(6) -0.020(7) C51 0.062(8) 0.041(7) 0.016(5) -0.004(4) 0.004(4) -0.015(6) C79 0.101(11) 0.029(7) 0.036(7) -0.008(5) 0.003(6) -0.033(7) O1 0.042(4) 0.033(4) 0.020(3) -0.008(3) 0.002(3) -0.016(4) O2 0.038(4) 0.024(4) 0.028(3) -0.007(3) -0.012(3) -0.008(3) O3 0.046(4) 0.032(4) 0.018(3) -0.005(3) 0.000(3) -0.021(4) O4 0.036(4) 0.030(4) 0.029(3) -0.010(3) -0.010(3) -0.007(3) O5 0.103(8) 0.080(8) 0.062(6) -0.025(5) -0.024(5) -0.035(7) O6 0.152(10) 0.061(7) 0.044(5) -0.021(4) 0.002(5) -0.075(7) O7 0.087(7) 0.042(6) 0.053(5) -0.018(4) -0.020(4) -0.024(5) O8 0.061(5) 0.043(5) 0.046(4) -0.025(4) -0.005(4) -0.008(4) O9 0.066(6) 0.041(5) 0.031(4) -0.013(3) 0.000(3) -0.020(4) O10 0.102(8) 0.058(7) 0.051(5) -0.016(5) -0.013(5) -0.020(6) O11 0.077(7) 0.103(9) 0.057(5) -0.034(5) -0.040(5) -0.012(6) O12 0.080(7) 0.050(6) 0.052(5) -0.014(4) -0.019(4) -0.017(6) O13 0.052(5) 0.048(5) 0.045(4) 0.009(4) -0.012(3) -0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O13 2.331(7) . ? Pb1 O13 2.540(8) 2_767 ? Pb1 O7 2.587(7) . ? Pb1 O12 2.588(8) 2_767 ? Pb1 O8 2.629(8) . ? Pb1 Pb2' 3.666(4) . ? Pb2 Pb2' 1.412(4) . ? Pb2 O13 2.296(7) . ? Pb2 O9 2.444(8) . ? Pb2 O6 2.532(9) 2_767 ? Pb2 O10 2.642(8) . ? Pb2' O13 2.322(9) . ? Pb2' O8 2.668(8) . ? Na1 O7 2.249(9) . ? Na1 O12 2.253(8) . ? Na1 O4 2.372(7) . ? Na1 O2 2.407(7) . ? Na1 O3 2.414(7) . ? Na1 O1 2.463(7) . ? Na1 C50 3.052(14) . ? Na1 C48 3.080(15) . ? C1 C6 1.372(13) . ? C1 C2 1.382(14) . ? C1 C37 1.551(12) . ? C2 C3 1.393(13) . ? C2 H2 0.9300 . ? C3 C4 1.382(12) . ? C3 C28 1.534(14) . ? C4 C5 1.392(14) . ? C4 O2 1.405(10) . ? C5 C6 1.399(13) . ? C5 C7 1.523(13) . ? C6 H6 0.9300 . ? C7 C8 1.544(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.378(13) . ? C8 C9 1.378(13) . ? C9 C10 1.402(13) . ? C9 O3 1.407(11) . ? C10 C11 1.379(13) . ? C10 C14 1.557(13) . ? C11 C12 1.405(13) . ? C11 H11 0.9300 . ? C12 C13 1.358(14) . ? C12 C33 1.542(14) . ? C13 H13 0.9300 . ? C14 C15 1.522(13) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.384(13) . ? C15 C20 1.411(14) . ? C16 C17 1.415(13) . ? C16 H16 0.9300 . ? C17 C18 1.383(14) . ? C17 C29 1.545(14) . ? C18 C19 1.375(14) . ? C18 H18 0.9300 . ? C19 C20 1.402(13) . ? C19 C21 1.487(14) . ? C20 O4 1.401(11) . ? C21 C22 1.545(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C26 1.373(14) . ? C22 C23 1.388(13) . ? C23 C24 1.391(15) . ? C23 H23 0.9300 . ? C24 C25 1.388(15) . ? C24 C41 1.537(14) . ? C25 C27 1.372(13) . ? C25 H25 0.9300 . ? C26 O1 1.392(10) . ? C26 C27 1.409(14) . ? C27 C28 1.512(14) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.52(3) . ? C29 C30' 1.54(3) . ? C29 C32' 1.59(3) . ? C29 C31 1.60(3) . ? C29 C31' 1.61(4) . ? C29 C32 1.62(3) . ? C30 C30' 0.60(3) . ? C31' C31 0.65(4) . ? C32' C32 0.68(4) . ? C33 C34 1.517(16) . ? C33 C35 1.537(14) . ? C33 C36 1.552(16) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C39 1.484(16) . ? C37 C38 1.500(15) . ? C37 C40 1.514(16) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C43 1.48(3) . ? C41 C44' 1.50(5) . ? C41 C42' 1.55(4) . ? C41 C43' 1.56(4) . ? C41 C42 1.57(3) . ? C41 C44 1.63(3) . ? C42' C42 0.60(5) . ? C43' C43 0.90(4) . ? C43 C44' 1.65(6) . ? C44 C44' 0.88(5) . ? C45 O1 1.433(12) . ? C45 C46 1.469(17) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 O6 1.253(17) . ? C46 O5 1.310(18) . ? C47 O4 1.435(11) . ? C47 C48 1.469(16) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O11 1.256(15) . ? C48 O12 1.270(15) . ? C49 O2 1.425(12) . ? C49 C50 1.477(15) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O8 1.234(13) . ? C50 O7 1.320(14) . ? C51 O3 1.451(10) . ? C51 C79 1.470(15) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C79 O9 1.275(13) . ? C79 O10 1.289(15) . ? O6 Pb2 2.532(9) 2_767 ? O12 Pb1 2.588(8) 2_767 ? O13 Pb1 2.540(8) 2_767 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Pb1 O13 71.0(3) . 2_767 ? O13 Pb1 O7 83.0(3) . . ? O13 Pb1 O7 77.7(3) 2_767 . ? O13 Pb1 O12 74.4(3) . 2_767 ? O13 Pb1 O12 96.9(3) 2_767 2_767 ? O7 Pb1 O12 157.2(3) . 2_767 ? O13 Pb1 O8 76.8(3) . . ? O13 Pb1 O8 121.6(2) 2_767 . ? O7 Pb1 O8 50.7(3) . . ? O12 Pb1 O8 119.6(3) 2_767 . ? O13 Pb1 Pb2' 37.9(2) . . ? O13 Pb1 Pb2' 107.38(18) 2_767 . ? O7 Pb1 Pb2' 80.4(2) . . ? O12 Pb1 Pb2' 80.2(2) 2_767 . ? O8 Pb1 Pb2' 46.65(18) . . ? Pb2' Pb2 O13 73.2(2) . . ? Pb2' Pb2 O9 137.9(2) . . ? O13 Pb2 O9 82.8(3) . . ? Pb2' Pb2 O6 128.4(3) . 2_767 ? O13 Pb2 O6 78.9(3) . 2_767 ? O9 Pb2 O6 77.8(3) . 2_767 ? Pb2' Pb2 O10 90.4(3) . . ? O13 Pb2 O10 83.8(3) . . ? O9 Pb2 O10 52.5(3) . . ? O6 Pb2 O10 129.0(3) 2_767 . ? Pb2 Pb2' O13 71.2(2) . . ? Pb2 Pb2' O8 124.0(3) . . ? O13 Pb2' O8 76.2(3) . . ? Pb2 Pb2' Pb1 108.21(18) . . ? O13 Pb2' Pb1 38.10(18) . . ? O8 Pb2' Pb1 45.76(18) . . ? O7 Na1 O12 93.9(3) . . ? O7 Na1 O4 148.6(3) . . ? O12 Na1 O4 68.8(3) . . ? O7 Na1 O2 69.8(3) . . ? O12 Na1 O2 147.0(3) . . ? O4 Na1 O2 137.6(3) . . ? O7 Na1 O3 120.4(3) . . ? O12 Na1 O3 84.5(3) . . ? O4 Na1 O3 85.1(3) . . ? O2 Na1 O3 80.1(2) . . ? O7 Na1 O1 86.5(3) . . ? O12 Na1 O1 124.3(3) . . ? O4 Na1 O1 82.7(2) . . ? O2 Na1 O1 84.3(2) . . ? O3 Na1 O1 140.9(2) . . ? O7 Na1 C50 23.1(3) . . ? O12 Na1 C50 105.7(3) . . ? O4 Na1 C50 171.5(3) . . ? O2 Na1 C50 50.1(3) . . ? O3 Na1 C50 101.1(3) . . ? O1 Na1 C50 95.8(3) . . ? O7 Na1 C48 106.3(3) . . ? O12 Na1 C48 21.1(3) . . ? O4 Na1 C48 50.3(3) . . ? O2 Na1 C48 167.9(3) . . ? O3 Na1 C48 92.8(3) . . ? O1 Na1 C48 107.1(3) . . ? C50 Na1 C48 122.9(3) . . ? C6 C1 C2 117.0(8) . . ? C6 C1 C37 121.2(9) . . ? C2 C1 C37 121.8(8) . . ? C1 C2 C3 122.7(8) . . ? C1 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? C4 C3 C2 117.8(9) . . ? C4 C3 C28 121.7(8) . . ? C2 C3 C28 120.3(8) . . ? C3 C4 C5 122.2(8) . . ? C3 C4 O2 119.1(8) . . ? C5 C4 O2 118.7(8) . . ? C4 C5 C6 116.7(8) . . ? C4 C5 C7 121.9(8) . . ? C6 C5 C7 121.2(9) . . ? C1 C6 C5 123.6(9) . . ? C1 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? C5 C7 C8 109.1(7) . . ? C5 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? C5 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C13 C8 C9 117.6(9) . . ? C13 C8 C7 120.0(8) . . ? C9 C8 C7 122.4(9) . . ? C8 C9 C10 120.7(8) . . ? C8 C9 O3 119.9(8) . . ? C10 C9 O3 119.4(8) . . ? C11 C10 C9 118.9(9) . . ? C11 C10 C14 119.3(9) . . ? C9 C10 C14 121.7(9) . . ? C10 C11 C12 121.2(9) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 116.9(9) . . ? C13 C12 C33 121.2(9) . . ? C11 C12 C33 121.9(9) . . ? C12 C13 C8 124.4(9) . . ? C12 C13 H13 117.8 . . ? C8 C13 H13 117.8 . . ? C15 C14 C10 108.7(7) . . ? C15 C14 H14A 110.0 . . ? C10 C14 H14A 110.0 . . ? C15 C14 H14B 110.0 . . ? C10 C14 H14B 110.0 . . ? H14A C14 H14B 108.3 . . ? C16 C15 C20 118.2(9) . . ? C16 C15 C14 121.3(10) . . ? C20 C15 C14 120.4(9) . . ? C15 C16 C17 121.2(10) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 117.6(9) . . ? C18 C17 C29 123.3(9) . . ? C16 C17 C29 119.1(10) . . ? C19 C18 C17 123.8(9) . . ? C19 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? C18 C19 C20 117.1(10) . . ? C18 C19 C21 122.6(9) . . ? C20 C19 C21 120.3(9) . . ? O4 C20 C19 119.4(9) . . ? O4 C20 C15 118.9(8) . . ? C19 C20 C15 121.7(9) . . ? C19 C21 C22 111.6(8) . . ? C19 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? C19 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C26 C22 C23 118.6(9) . . ? C26 C22 C21 121.4(8) . . ? C23 C22 C21 119.6(9) . . ? C22 C23 C24 122.4(10) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C25 C24 C23 116.3(9) . . ? C25 C24 C41 120.8(10) . . ? C23 C24 C41 122.6(10) . . ? C27 C25 C24 123.6(10) . . ? C27 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? C22 C26 O1 118.5(8) . . ? C22 C26 C27 121.1(8) . . ? O1 C26 C27 120.4(9) . . ? C25 C27 C26 117.5(9) . . ? C25 C27 C28 121.0(9) . . ? C26 C27 C28 121.1(8) . . ? C27 C28 C3 109.6(8) . . ? C27 C28 H28A 109.8 . . ? C3 C28 H28A 109.8 . . ? C27 C28 H28B 109.8 . . ? C3 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C30' 22.6(13) . . ? C30 C29 C17 113.4(14) . . ? C30' C29 C17 111.7(14) . . ? C30 C29 C32' 112.7(17) . . ? C30' C29 C32' 93.6(16) . . ? C17 C29 C32' 109.3(14) . . ? C30 C29 C31 87.4(18) . . ? C30' C29 C31 108.9(17) . . ? C17 C29 C31 106.9(13) . . ? C32' C29 C31 125.7(19) . . ? C30 C29 C31' 106.3(19) . . ? C30' C29 C31' 125.0(19) . . ? C17 C29 C31' 110.2(16) . . ? C32' C29 C31' 105(2) . . ? C31 C29 C31' 23.4(15) . . ? C30 C29 C32 129.6(17) . . ? C30' C29 C32 114.7(17) . . ? C17 C29 C32 109.3(13) . . ? C32' C29 C32 24.3(13) . . ? C31 C29 C32 104.8(19) . . ? C31' C29 C32 82.1(19) . . ? C30' C30 C29 80(5) . . ? C30 C30' C29 77(4) . . ? C31 C31' C29 78(5) . . ? C31' C31 C29 79(5) . . ? C32 C32' C29 80(4) . . ? C32' C32 C29 75(4) . . ? C34 C33 C35 108.8(9) . . ? C34 C33 C12 113.4(9) . . ? C35 C33 C12 110.4(9) . . ? C34 C33 C36 108.5(10) . . ? C35 C33 C36 109.1(10) . . ? C12 C33 C36 106.5(9) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C38 111.5(10) . . ? C39 C37 C40 107.1(10) . . ? C38 C37 C40 106.9(10) . . ? C39 C37 C1 109.9(9) . . ? C38 C37 C1 112.2(9) . . ? C40 C37 C1 109.1(9) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C44' 67(2) . . ? C43 C41 C24 113.5(15) . . ? C44' C41 C24 113(2) . . ? C43 C41 C42' 116(2) . . ? C44' C41 C42' 130(2) . . ? C24 C41 C42' 110.0(17) . . ? C43 C41 C43' 34.2(15) . . ? C44' C41 C43' 101(2) . . ? C24 C41 C43' 107.7(14) . . ? C42' C41 C43' 89(2) . . ? C43 C41 C42 127.7(19) . . ? C44' C41 C42 113(2) . . ? C24 C41 C42 112.9(14) . . ? C42' C41 C42 22.1(17) . . ? C43' C41 C42 108(2) . . ? C43 C41 C44 99.0(19) . . ? C44' C41 C44 32.3(18) . . ? C24 C41 C44 106.0(12) . . ? C42' C41 C44 111.5(18) . . ? C43' C41 C44 130.9(17) . . ? C42 C41 C44 90.1(17) . . ? C42 C42' C41 81(6) . . ? C42' C42 C41 77(6) . . ? C43 C43' C41 68(3) . . ? C43' C43 C41 78(3) . . ? C43' C43 C44' 133(4) . . ? C41 C43 C44' 57(2) . . ? C44' C44 C41 66(4) . . ? C44 C44' C41 82(4) . . ? C44 C44' C43 137(5) . . ? C41 C44' C43 56(2) . . ? O1 C45 C46 115.2(9) . . ? O1 C45 H45A 108.5 . . ? C46 C45 H45A 108.5 . . ? O1 C45 H45B 108.5 . . ? C46 C45 H45B 108.5 . . ? H45A C45 H45B 107.5 . . ? O6 C46 O5 124.3(13) . . ? O6 C46 C45 119.7(14) . . ? O5 C46 C45 116.1(13) . . ? O4 C47 C48 111.8(9) . . ? O4 C47 H47A 109.3 . . ? C48 C47 H47A 109.3 . . ? O4 C47 H47B 109.3 . . ? C48 C47 H47B 109.3 . . ? H47A C47 H47B 107.9 . . ? O11 C48 O12 123.7(12) . . ? O11 C48 C47 118.2(12) . . ? O12 C48 C47 118.1(11) . . ? O11 C48 Na1 153.8(10) . . ? O12 C48 Na1 39.7(6) . . ? C47 C48 Na1 82.5(7) . . ? O2 C49 C50 110.5(9) . . ? O2 C49 H49A 109.6 . . ? C50 C49 H49A 109.6 . . ? O2 C49 H49B 109.6 . . ? C50 C49 H49B 109.6 . . ? H49A C49 H49B 108.1 . . ? O8 C50 O7 122.0(11) . . ? O8 C50 C49 117.5(12) . . ? O7 C50 C49 120.4(10) . . ? O8 C50 Na1 152.4(8) . . ? O7 C50 Na1 41.9(5) . . ? C49 C50 Na1 84.3(7) . . ? O3 C51 C79 112.0(9) . . ? O3 C51 H51A 109.2 . . ? C79 C51 H51A 109.2 . . ? O3 C51 H51B 109.2 . . ? C79 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? O9 C79 O10 123.1(11) . . ? O9 C79 C51 117.9(11) . . ? O10 C79 C51 118.7(10) . . ? C26 O1 C45 115.6(7) . . ? C26 O1 Na1 127.5(6) . . ? C45 O1 Na1 116.1(5) . . ? C4 O2 C49 112.9(7) . . ? C4 O2 Na1 133.2(5) . . ? C49 O2 Na1 113.8(5) . . ? C9 O3 C51 113.7(7) . . ? C9 O3 Na1 129.8(5) . . ? C51 O3 Na1 115.6(6) . . ? C20 O4 C47 113.4(7) . . ? C20 O4 Na1 132.4(5) . . ? C47 O4 Na1 114.0(6) . . ? C46 O6 Pb2 103.5(10) . 2_767 ? C50 O7 Na1 115.1(7) . . ? C50 O7 Pb1 93.4(6) . . ? Na1 O7 Pb1 143.2(4) . . ? C50 O8 Pb1 93.6(7) . . ? C50 O8 Pb2' 121.8(7) . . ? Pb1 O8 Pb2' 87.6(2) . . ? C79 O9 Pb2 96.6(7) . . ? C79 O10 Pb2 87.2(6) . . ? C48 O12 Na1 119.2(8) . . ? C48 O12 Pb1 97.9(7) . 2_767 ? Na1 O12 Pb1 134.4(4) . 2_767 ? Pb2 O13 Pb2' 35.59(16) . . ? Pb2 O13 Pb1 138.0(3) . . ? Pb2' O13 Pb1 104.0(3) . . ? Pb2 O13 Pb1 107.9(3) . 2_767 ? Pb2' O13 Pb1 142.9(4) . 2_767 ? Pb1 O13 Pb1 109.0(3) . 2_767 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Pb2 Pb2' O13 -57.9(4) . . . . ? O6 Pb2 Pb2' O13 60.3(4) 2_767 . . . ? O10 Pb2 Pb2' O13 -83.5(3) . . . . ? O13 Pb2 Pb2' O8 57.7(3) . . . . ? O9 Pb2 Pb2' O8 -0.2(5) . . . . ? O6 Pb2 Pb2' O8 118.0(4) 2_767 . . . ? O10 Pb2 Pb2' O8 -25.8(4) . . . . ? O13 Pb2 Pb2' Pb1 9.3(2) . . . . ? O9 Pb2 Pb2' Pb1 -48.6(4) . . . . ? O6 Pb2 Pb2' Pb1 69.6(4) 2_767 . . . ? O10 Pb2 Pb2' Pb1 -74.2(3) . . . . ? O13 Pb1 Pb2' Pb2 -14.3(3) . . . . ? O13 Pb1 Pb2' Pb2 2.8(3) 2_767 . . . ? O7 Pb1 Pb2' Pb2 76.5(3) . . . . ? O12 Pb1 Pb2' Pb2 -91.4(3) 2_767 . . . ? O8 Pb1 Pb2' Pb2 120.1(4) . . . . ? O13 Pb1 Pb2' O13 17.1(5) 2_767 . . . ? O7 Pb1 Pb2' O13 90.9(4) . . . . ? O12 Pb1 Pb2' O13 -77.1(4) 2_767 . . . ? O8 Pb1 Pb2' O13 134.5(4) . . . . ? O13 Pb1 Pb2' O8 -134.5(4) . . . . ? O13 Pb1 Pb2' O8 -117.4(3) 2_767 . . . ? O7 Pb1 Pb2' O8 -43.6(3) . . . . ? O12 Pb1 Pb2' O8 148.4(3) 2_767 . . . ? C6 C1 C2 C3 -0.2(15) . . . . ? C37 C1 C2 C3 -179.9(10) . . . . ? C1 C2 C3 C4 -1.2(15) . . . . ? C1 C2 C3 C28 173.9(9) . . . . ? C2 C3 C4 C5 2.4(14) . . . . ? C28 C3 C4 C5 -172.7(9) . . . . ? C2 C3 C4 O2 -176.5(8) . . . . ? C28 C3 C4 O2 8.5(13) . . . . ? C3 C4 C5 C6 -2.1(14) . . . . ? O2 C4 C5 C6 176.7(8) . . . . ? C3 C4 C5 C7 173.3(9) . . . . ? O2 C4 C5 C7 -7.8(13) . . . . ? C2 C1 C6 C5 0.5(15) . . . . ? C37 C1 C6 C5 -179.9(10) . . . . ? C4 C5 C6 C1 0.6(15) . . . . ? C7 C5 C6 C1 -174.8(9) . . . . ? C4 C5 C7 C8 -94.2(11) . . . . ? C6 C5 C7 C8 81.0(11) . . . . ? C5 C7 C8 C13 -78.9(11) . . . . ? C5 C7 C8 C9 98.6(10) . . . . ? C13 C8 C9 C10 5.0(13) . . . . ? C7 C8 C9 C10 -172.5(8) . . . . ? C13 C8 C9 O3 -176.4(8) . . . . ? C7 C8 C9 O3 6.1(12) . . . . ? C8 C9 C10 C11 -5.8(13) . . . . ? O3 C9 C10 C11 175.6(8) . . . . ? C8 C9 C10 C14 169.9(8) . . . . ? O3 C9 C10 C14 -8.7(12) . . . . ? C9 C10 C11 C12 3.2(13) . . . . ? C14 C10 C11 C12 -172.6(8) . . . . ? C10 C11 C12 C13 -0.1(13) . . . . ? C10 C11 C12 C33 179.1(9) . . . . ? C11 C12 C13 C8 -0.7(14) . . . . ? C33 C12 C13 C8 -179.8(9) . . . . ? C9 C8 C13 C12 -1.8(14) . . . . ? C7 C8 C13 C12 175.8(8) . . . . ? C11 C10 C14 C15 75.2(11) . . . . ? C9 C10 C14 C15 -100.5(10) . . . . ? C10 C14 C15 C16 -78.1(11) . . . . ? C10 C14 C15 C20 98.3(10) . . . . ? C20 C15 C16 C17 -3.4(14) . . . . ? C14 C15 C16 C17 173.1(8) . . . . ? C15 C16 C17 C18 -1.3(14) . . . . ? C15 C16 C17 C29 -179.8(9) . . . . ? C16 C17 C18 C19 2.7(15) . . . . ? C29 C17 C18 C19 -178.9(10) . . . . ? C17 C18 C19 C20 0.8(15) . . . . ? C17 C18 C19 C21 -176.7(9) . . . . ? C18 C19 C20 O4 176.3(8) . . . . ? C21 C19 C20 O4 -6.1(13) . . . . ? C18 C19 C20 C15 -5.8(14) . . . . ? C21 C19 C20 C15 171.8(9) . . . . ? C16 C15 C20 O4 -175.0(8) . . . . ? C14 C15 C20 O4 8.5(13) . . . . ? C16 C15 C20 C19 7.1(14) . . . . ? C14 C15 C20 C19 -169.4(8) . . . . ? C18 C19 C21 C22 78.1(12) . . . . ? C20 C19 C21 C22 -99.3(10) . . . . ? C19 C21 C22 C26 100.4(11) . . . . ? C19 C21 C22 C23 -73.2(12) . . . . ? C26 C22 C23 C24 1.9(16) . . . . ? C21 C22 C23 C24 175.7(10) . . . . ? C22 C23 C24 C25 -6.2(16) . . . . ? C22 C23 C24 C41 178.8(11) . . . . ? C23 C24 C25 C27 4.7(17) . . . . ? C41 C24 C25 C27 179.8(11) . . . . ? C23 C22 C26 O1 -176.2(9) . . . . ? C21 C22 C26 O1 10.2(14) . . . . ? C23 C22 C26 C27 4.2(15) . . . . ? C21 C22 C26 C27 -169.5(9) . . . . ? C24 C25 C27 C26 1.0(16) . . . . ? C24 C25 C27 C28 -172.7(10) . . . . ? C22 C26 C27 C25 -5.6(14) . . . . ? O1 C26 C27 C25 174.7(9) . . . . ? C22 C26 C27 C28 168.1(9) . . . . ? O1 C26 C27 C28 -11.6(14) . . . . ? C25 C27 C28 C3 74.1(11) . . . . ? C26 C27 C28 C3 -99.4(10) . . . . ? C4 C3 C28 C27 98.2(10) . . . . ? C2 C3 C28 C27 -76.7(11) . . . . ? C18 C17 C29 C30 18.9(19) . . . . ? C16 C17 C29 C30 -162.7(15) . . . . ? C18 C17 C29 C30' -5.6(18) . . . . ? C16 C17 C29 C30' 172.8(14) . . . . ? C18 C17 C29 C32' -107.8(16) . . . . ? C16 C17 C29 C32' 70.6(17) . . . . ? C18 C17 C29 C31 113.4(17) . . . . ? C16 C17 C29 C31 -68.1(17) . . . . ? C18 C17 C29 C31' 137.9(17) . . . . ? C16 C17 C29 C31' -43.7(19) . . . . ? C18 C17 C29 C32 -133.6(16) . . . . ? C16 C17 C29 C32 44.8(17) . . . . ? C17 C29 C30 C30' -91(5) . . . . ? C32' C29 C30 C30' 34(5) . . . . ? C31 C29 C30 C30' 162(5) . . . . ? C31' C29 C30 C30' 148(5) . . . . ? C32 C29 C30 C30' 55(6) . . . . ? C17 C29 C30' C30 99(5) . . . . ? C32' C29 C30' C30 -149(5) . . . . ? C31 C29 C30' C30 -19(5) . . . . ? C31' C29 C30' C30 -38(6) . . . . ? C32 C29 C30' C30 -136(5) . . . . ? C30 C29 C31' C31 37(5) . . . . ? C30' C29 C31' C31 52(6) . . . . ? C17 C29 C31' C31 -86(5) . . . . ? C32' C29 C31' C31 157(5) . . . . ? C32 C29 C31' C31 166(5) . . . . ? C30 C29 C31 C31' -144(5) . . . . ? C30' C29 C31 C31' -137(5) . . . . ? C17 C29 C31 C31' 102(5) . . . . ? C32' C29 C31 C31' -28(6) . . . . ? C32 C29 C31 C31' -14(5) . . . . ? C30 C29 C32' C32 139(4) . . . . ? C30' C29 C32' C32 151(4) . . . . ? C17 C29 C32' C32 -94(4) . . . . ? C31 C29 C32' C32 35(5) . . . . ? C31' C29 C32' C32 24(5) . . . . ? C30 C29 C32 C32' -52(5) . . . . ? C30' C29 C32 C32' -32(5) . . . . ? C17 C29 C32 C32' 94(4) . . . . ? C31 C29 C32 C32' -151(4) . . . . ? C31' C29 C32 C32' -157(5) . . . . ? C13 C12 C33 C34 173.9(9) . . . . ? C11 C12 C33 C34 -5.2(13) . . . . ? C13 C12 C33 C35 51.4(13) . . . . ? C11 C12 C33 C35 -127.7(10) . . . . ? C13 C12 C33 C36 -66.9(12) . . . . ? C11 C12 C33 C36 114.0(10) . . . . ? C6 C1 C37 C39 -55.5(13) . . . . ? C2 C1 C37 C39 124.1(11) . . . . ? C6 C1 C37 C38 179.9(11) . . . . ? C2 C1 C37 C38 -0.5(15) . . . . ? C6 C1 C37 C40 61.6(13) . . . . ? C2 C1 C37 C40 -118.7(11) . . . . ? C25 C24 C41 C43 -40(2) . . . . ? C23 C24 C41 C43 135(2) . . . . ? C25 C24 C41 C44' 34(3) . . . . ? C23 C24 C41 C44' -151(2) . . . . ? C25 C24 C41 C42' -172.0(19) . . . . ? C23 C24 C41 C42' 3(2) . . . . ? C25 C24 C41 C43' -76.3(19) . . . . ? C23 C24 C41 C43' 98.5(18) . . . . ? C25 C24 C41 C42 164.4(17) . . . . ? C23 C24 C41 C42 -21(2) . . . . ? C25 C24 C41 C44 67.3(17) . . . . ? C23 C24 C41 C44 -117.8(15) . . . . ? C43 C41 C42' C42 128(6) . . . . ? C44' C41 C42' C42 46(7) . . . . ? C24 C41 C42' C42 -102(6) . . . . ? C43' C41 C42' C42 149(6) . . . . ? C44 C41 C42' C42 15(6) . . . . ? C43 C41 C42 C42' -64(7) . . . . ? C44' C41 C42 C42' -143(6) . . . . ? C24 C41 C42 C42' 87(6) . . . . ? C43' C41 C42 C42' -32(6) . . . . ? C44 C41 C42 C42' -166(6) . . . . ? C44' C41 C43' C43 -13(4) . . . . ? C24 C41 C43' C43 106(3) . . . . ? C42' C41 C43' C43 -143(3) . . . . ? C42 C41 C43' C43 -132(3) . . . . ? C44 C41 C43' C43 -25(4) . . . . ? C41 C43' C43 C44' 15(4) . . . . ? C44' C41 C43 C43' 167(4) . . . . ? C24 C41 C43 C43' -87(3) . . . . ? C42' C41 C43 C43' 42(4) . . . . ? C42 C41 C43 C43' 64(4) . . . . ? C44 C41 C43 C43' 161(3) . . . . ? C24 C41 C43 C44' 106(2) . . . . ? C42' C41 C43 C44' -125(3) . . . . ? C43' C41 C43 C44' -167(4) . . . . ? C42 C41 C43 C44' -103(3) . . . . ? C44 C41 C43 C44' -5(2) . . . . ? C43 C41 C44 C44' 9(4) . . . . ? C24 C41 C44 C44' -108(4) . . . . ? C42' C41 C44 C44' 132(4) . . . . ? C43' C41 C44 C44' 23(5) . . . . ? C42 C41 C44 C44' 138(4) . . . . ? C41 C44 C44' C43 -12(5) . . . . ? C43 C41 C44' C44 -170(4) . . . . ? C24 C41 C44' C44 83(4) . . . . ? C42' C41 C44' C44 -64(5) . . . . ? C43' C41 C44' C44 -162(4) . . . . ? C42 C41 C44' C44 -47(4) . . . . ? C24 C41 C44' C43 -106.9(19) . . . . ? C42' C41 C44' C43 106(3) . . . . ? C43' C41 C44' C43 8(2) . . . . ? C42 C41 C44' C43 123(2) . . . . ? C44 C41 C44' C43 170(4) . . . . ? C43' C43 C44' C44 -3(10) . . . . ? C41 C43 C44' C44 15(6) . . . . ? C43' C43 C44' C41 -18(5) . . . . ? O1 C45 C46 O6 -153.5(12) . . . . ? O1 C45 C46 O5 28.2(18) . . . . ? O4 C47 C48 O11 -172.2(11) . . . . ? O4 C47 C48 O12 8.6(17) . . . . ? O4 C47 C48 Na1 -9.4(8) . . . . ? O7 Na1 C48 O11 -5(2) . . . . ? O12 Na1 C48 O11 -61(2) . . . . ? O4 Na1 C48 O11 151(2) . . . . ? O2 Na1 C48 O11 -74(3) . . . . ? O3 Na1 C48 O11 -128(2) . . . . ? O1 Na1 C48 O11 86(2) . . . . ? C50 Na1 C48 O11 -23(2) . . . . ? O7 Na1 C48 O12 56.0(10) . . . . ? O4 Na1 C48 O12 -147.9(11) . . . . ? O2 Na1 C48 O12 -13(2) . . . . ? O3 Na1 C48 O12 -66.8(10) . . . . ? O1 Na1 C48 O12 147.4(9) . . . . ? C50 Na1 C48 O12 38.4(11) . . . . ? O7 Na1 C48 C47 -149.2(7) . . . . ? O12 Na1 C48 C47 154.8(14) . . . . ? O4 Na1 C48 C47 6.8(6) . . . . ? O2 Na1 C48 C47 141.9(14) . . . . ? O3 Na1 C48 C47 88.0(7) . . . . ? O1 Na1 C48 C47 -57.9(8) . . . . ? C50 Na1 C48 C47 -166.8(7) . . . . ? O2 C49 C50 O8 -171.3(9) . . . . ? O2 C49 C50 O7 12.8(14) . . . . ? O2 C49 C50 Na1 -9.2(7) . . . . ? O7 Na1 C50 O8 -65.1(19) . . . . ? O12 Na1 C50 O8 -4(2) . . . . ? O2 Na1 C50 O8 151(2) . . . . ? O3 Na1 C50 O8 84(2) . . . . ? O1 Na1 C50 O8 -131.7(19) . . . . ? C48 Na1 C50 O8 -17(2) . . . . ? O12 Na1 C50 O7 61.5(7) . . . . ? O2 Na1 C50 O7 -144.2(8) . . . . ? O3 Na1 C50 O7 148.8(7) . . . . ? O1 Na1 C50 O7 -66.6(7) . . . . ? C48 Na1 C50 O7 48.1(8) . . . . ? O7 Na1 C50 C49 150.9(10) . . . . ? O12 Na1 C50 C49 -147.6(6) . . . . ? O2 Na1 C50 C49 6.7(5) . . . . ? O3 Na1 C50 C49 -60.3(6) . . . . ? O1 Na1 C50 C49 84.3(6) . . . . ? C48 Na1 C50 C49 -161.0(6) . . . . ? O3 C51 C79 O9 -149.9(10) . . . . ? O3 C51 C79 O10 35.8(16) . . . . ? C22 C26 O1 C45 99.5(11) . . . . ? C27 C26 O1 C45 -80.9(11) . . . . ? C22 C26 O1 Na1 -90.7(10) . . . . ? C27 C26 O1 Na1 88.9(10) . . . . ? C46 C45 O1 C26 -151.6(11) . . . . ? C46 C45 O1 Na1 37.4(13) . . . . ? O7 Na1 O1 C26 -136.5(7) . . . . ? O12 Na1 O1 C26 131.2(7) . . . . ? O4 Na1 O1 C26 73.0(7) . . . . ? O2 Na1 O1 C26 -66.5(7) . . . . ? O3 Na1 O1 C26 0.2(9) . . . . ? C50 Na1 O1 C26 -115.4(7) . . . . ? C48 Na1 O1 C26 117.6(7) . . . . ? O7 Na1 O1 C45 33.2(7) . . . . ? O12 Na1 O1 C45 -59.1(8) . . . . ? O4 Na1 O1 C45 -117.2(7) . . . . ? O2 Na1 O1 C45 103.2(7) . . . . ? O3 Na1 O1 C45 169.9(6) . . . . ? C50 Na1 O1 C45 54.3(7) . . . . ? C48 Na1 O1 C45 -72.7(7) . . . . ? C3 C4 O2 C49 91.0(10) . . . . ? C5 C4 O2 C49 -87.9(10) . . . . ? C3 C4 O2 Na1 -88.2(10) . . . . ? C5 C4 O2 Na1 93.0(10) . . . . ? C50 C49 O2 C4 -166.5(8) . . . . ? C50 C49 O2 Na1 12.8(10) . . . . ? O7 Na1 O2 C4 157.5(8) . . . . ? O12 Na1 O2 C4 -138.3(8) . . . . ? O4 Na1 O2 C4 -3.5(9) . . . . ? O3 Na1 O2 C4 -74.8(8) . . . . ? O1 Na1 O2 C4 69.1(8) . . . . ? C50 Na1 O2 C4 171.6(9) . . . . ? C48 Na1 O2 C4 -129.8(15) . . . . ? O7 Na1 O2 C49 -21.6(6) . . . . ? O12 Na1 O2 C49 42.6(9) . . . . ? O4 Na1 O2 C49 177.3(6) . . . . ? O3 Na1 O2 C49 106.0(6) . . . . ? O1 Na1 O2 C49 -110.0(6) . . . . ? C50 Na1 O2 C49 -7.5(6) . . . . ? C48 Na1 O2 C49 51.1(18) . . . . ? C8 C9 O3 C51 100.3(10) . . . . ? C10 C9 O3 C51 -81.1(10) . . . . ? C8 C9 O3 Na1 -91.6(9) . . . . ? C10 C9 O3 Na1 87.0(9) . . . . ? C79 C51 O3 C9 -147.7(10) . . . . ? C79 C51 O3 Na1 42.4(11) . . . . ? O7 Na1 O3 C9 132.2(7) . . . . ? O12 Na1 O3 C9 -136.4(8) . . . . ? O4 Na1 O3 C9 -67.3(7) . . . . ? O2 Na1 O3 C9 72.9(7) . . . . ? O1 Na1 O3 C9 4.8(9) . . . . ? C50 Na1 O3 C9 118.7(7) . . . . ? C48 Na1 O3 C9 -117.0(7) . . . . ? O7 Na1 O3 C51 -59.8(7) . . . . ? O12 Na1 O3 C51 31.5(7) . . . . ? O4 Na1 O3 C51 100.7(6) . . . . ? O2 Na1 O3 C51 -119.2(6) . . . . ? O1 Na1 O3 C51 172.8(6) . . . . ? C50 Na1 O3 C51 -73.4(7) . . . . ? C48 Na1 O3 C51 50.9(7) . . . . ? C19 C20 O4 C47 -96.4(10) . . . . ? C15 C20 O4 C47 85.6(11) . . . . ? C19 C20 O4 Na1 88.6(10) . . . . ? C15 C20 O4 Na1 -89.4(10) . . . . ? C48 C47 O4 C20 -162.7(10) . . . . ? C48 C47 O4 Na1 13.3(12) . . . . ? O7 Na1 O4 C20 -144.1(8) . . . . ? O12 Na1 O4 C20 155.6(9) . . . . ? O2 Na1 O4 C20 0.1(10) . . . . ? O3 Na1 O4 C20 69.6(8) . . . . ? O1 Na1 O4 C20 -73.2(8) . . . . ? C48 Na1 O4 C20 167.4(9) . . . . ? O7 Na1 O4 C47 40.9(9) . . . . ? O12 Na1 O4 C47 -19.4(7) . . . . ? O2 Na1 O4 C47 -174.9(6) . . . . ? O3 Na1 O4 C47 -105.4(7) . . . . ? O1 Na1 O4 C47 111.8(7) . . . . ? C48 Na1 O4 C47 -7.6(7) . . . . ? O5 C46 O6 Pb2 3.9(17) . . . 2_767 ? C45 C46 O6 Pb2 -174.3(10) . . . 2_767 ? O8 C50 O7 Na1 150.3(9) . . . . ? C49 C50 O7 Na1 -34.1(12) . . . . ? O8 C50 O7 Pb1 -5.8(11) . . . . ? C49 C50 O7 Pb1 169.8(9) . . . . ? Na1 C50 O7 Pb1 -156.1(6) . . . . ? O12 Na1 O7 C50 -122.0(7) . . . . ? O4 Na1 O7 C50 -176.3(6) . . . . ? O2 Na1 O7 C50 28.6(6) . . . . ? O3 Na1 O7 C50 -36.1(8) . . . . ? O1 Na1 O7 C50 113.8(7) . . . . ? C48 Na1 O7 C50 -139.4(7) . . . . ? O12 Na1 O7 Pb1 15.4(7) . . . . ? O4 Na1 O7 Pb1 -38.9(10) . . . . ? O2 Na1 O7 Pb1 166.0(8) . . . . ? O3 Na1 O7 Pb1 101.3(7) . . . . ? O1 Na1 O7 Pb1 -108.8(7) . . . . ? C50 Na1 O7 Pb1 137.4(12) . . . . ? C48 Na1 O7 Pb1 -2.0(8) . . . . ? O13 Pb1 O7 C50 81.6(6) . . . . ? O13 Pb1 O7 C50 153.7(6) 2_767 . . . ? O12 Pb1 O7 C50 75.4(10) 2_767 . . . ? O8 Pb1 O7 C50 3.0(6) . . . . ? Pb2' Pb1 O7 C50 43.4(6) . . . . ? O13 Pb1 O7 Na1 -60.5(7) . . . . ? O13 Pb1 O7 Na1 11.5(7) 2_767 . . . ? O12 Pb1 O7 Na1 -66.7(12) 2_767 . . . ? O8 Pb1 O7 Na1 -139.2(8) . . . . ? Pb2' Pb1 O7 Na1 -98.8(7) . . . . ? O7 C50 O8 Pb1 5.7(11) . . . . ? C49 C50 O8 Pb1 -170.0(8) . . . . ? Na1 C50 O8 Pb1 51.2(19) . . . . ? O7 C50 O8 Pb2' -83.7(12) . . . . ? C49 C50 O8 Pb2' 100.6(10) . . . . ? Na1 C50 O8 Pb2' -38(2) . . . . ? O13 Pb1 O8 C50 -94.9(7) . . . . ? O13 Pb1 O8 C50 -37.3(7) 2_767 . . . ? O7 Pb1 O8 C50 -3.2(6) . . . . ? O12 Pb1 O8 C50 -158.1(6) 2_767 . . . ? Pb2' Pb1 O8 C50 -121.7(7) . . . . ? O13 Pb1 O8 Pb2' 26.8(3) . . . . ? O13 Pb1 O8 Pb2' 84.3(3) 2_767 . . . ? O7 Pb1 O8 Pb2' 118.5(4) . . . . ? O12 Pb1 O8 Pb2' -36.4(4) 2_767 . . . ? Pb2 Pb2' O8 C50 10.3(10) . . . . ? O13 Pb2' O8 C50 65.8(9) . . . . ? Pb1 Pb2' O8 C50 92.7(9) . . . . ? Pb2 Pb2' O8 Pb1 -82.5(4) . . . . ? O13 Pb2' O8 Pb1 -27.0(3) . . . . ? O10 C79 O9 Pb2 8.5(14) . . . . ? C51 C79 O9 Pb2 -165.5(10) . . . . ? Pb2' Pb2 O9 C79 -37.3(8) . . . . ? O13 Pb2 O9 C79 -92.2(7) . . . . ? O6 Pb2 O9 C79 -172.3(7) 2_767 . . . ? O10 Pb2 O9 C79 -4.4(7) . . . . ? O9 C79 O10 Pb2 -7.8(13) . . . . ? C51 C79 O10 Pb2 166.1(11) . . . . ? Pb2' Pb2 O10 C79 163.0(8) . . . . ? O13 Pb2 O10 C79 89.9(8) . . . . ? O9 Pb2 O10 C79 4.3(7) . . . . ? O6 Pb2 O10 C79 19.5(9) 2_767 . . . ? O11 C48 O12 Na1 152.2(11) . . . . ? C47 C48 O12 Na1 -28.6(16) . . . . ? O11 C48 O12 Pb1 -0.3(15) . . . 2_767 ? C47 C48 O12 Pb1 178.9(10) . . . 2_767 ? Na1 C48 O12 Pb1 -152.5(9) . . . 2_767 ? O7 Na1 O12 C48 -127.1(10) . . . . ? O4 Na1 O12 C48 26.0(9) . . . . ? O2 Na1 O12 C48 175.1(8) . . . . ? O3 Na1 O12 C48 112.8(10) . . . . ? O1 Na1 O12 C48 -38.6(11) . . . . ? C50 Na1 O12 C48 -147.2(10) . . . . ? O7 Na1 O12 Pb1 13.2(6) . . . 2_767 ? O4 Na1 O12 Pb1 166.2(7) . . . 2_767 ? O2 Na1 O12 Pb1 -44.7(9) . . . 2_767 ? O3 Na1 O12 Pb1 -106.9(6) . . . 2_767 ? O1 Na1 O12 Pb1 101.7(6) . . . 2_767 ? C50 Na1 O12 Pb1 -7.0(7) . . . 2_767 ? C48 Na1 O12 Pb1 140.3(13) . . . 2_767 ? O9 Pb2 O13 Pb2' 145.1(2) . . . . ? O6 Pb2 O13 Pb2' -136.0(3) 2_767 . . . ? O10 Pb2 O13 Pb2' 92.2(3) . . . . ? Pb2' Pb2 O13 Pb1 -21.1(5) . . . . ? O9 Pb2 O13 Pb1 123.9(5) . . . . ? O6 Pb2 O13 Pb1 -157.2(6) 2_767 . . . ? O10 Pb2 O13 Pb1 71.1(5) . . . . ? Pb2' Pb2 O13 Pb1 -171.6(3) . . . 2_767 ? O9 Pb2 O13 Pb1 -26.5(3) . . . 2_767 ? O6 Pb2 O13 Pb1 52.4(3) 2_767 . . 2_767 ? O10 Pb2 O13 Pb1 -79.3(3) . . . 2_767 ? O8 Pb2' O13 Pb2 -133.8(3) . . . . ? Pb1 Pb2' O13 Pb2 -165.6(3) . . . . ? Pb2 Pb2' O13 Pb1 165.6(3) . . . . ? O8 Pb2' O13 Pb1 31.8(3) . . . . ? Pb2 Pb2' O13 Pb1 13.4(5) . . . 2_767 ? O8 Pb2' O13 Pb1 -120.5(6) . . . 2_767 ? Pb1 Pb2' O13 Pb1 -152.2(7) . . . 2_767 ? O13 Pb1 O13 Pb2 -150.2(7) 2_767 . . . ? O7 Pb1 O13 Pb2 -70.9(6) . . . . ? O12 Pb1 O13 Pb2 106.6(6) 2_767 . . . ? O8 Pb1 O13 Pb2 -19.7(5) . . . . ? Pb2' Pb1 O13 Pb2 12.5(3) . . . . ? O13 Pb1 O13 Pb2' -162.7(5) 2_767 . . . ? O7 Pb1 O13 Pb2' -83.4(3) . . . . ? O12 Pb1 O13 Pb2' 94.1(4) 2_767 . . . ? O8 Pb1 O13 Pb2' -32.2(3) . . . . ? O13 Pb1 O13 Pb1 0.000(1) 2_767 . . 2_767 ? O7 Pb1 O13 Pb1 79.3(3) . . . 2_767 ? O12 Pb1 O13 Pb1 -103.2(3) 2_767 . . 2_767 ? O8 Pb1 O13 Pb1 130.5(3) . . . 2_767 ? Pb2' Pb1 O13 Pb1 162.7(5) . . . 2_767 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.935 _refine_diff_density_min -1.771 _refine_diff_density_rms 0.168