# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Roesky, Peter' _publ_contact_author_email roesky@kit.edu _publ_section_title ; Dimeric Complexes of Lithium and Sodium Forming a Tetrametalla-cyclobuta[1,2:1,4:2,3:3,4]tetracyclopentane Structure ; loop_ _publ_author_name P.Roesky J.Jenter # Attachment '- deposit.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 753230' #TrackingRef '- deposit.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H76 Li2 N6' _chemical_formula_weight 895.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Li Li 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 '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 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 77.222(15) _cell_length_b 15.608(3) _cell_length_c 18.684(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.85(3) _cell_angle_gamma 90.00 _cell_volume 22359(8) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.632 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.133 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7744 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45705 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -89 _diffrn_reflns_limit_h_max 90 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 24.61 _reflns_number_total 18020 _reflns_number_gt 9745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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. 'C59 and C60 were calculated isotropically to due disorder problems' ; _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^)+(0.1345P)^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 18020 _refine_ls_number_parameters 1247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1572 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.2499 _refine_ls_wR_factor_gt 0.2177 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 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 C1 C 0.21814(5) 0.3845(3) 0.10942(19) 0.0462(9) Uani 1 1 d . . . H1 H 0.2286 0.4172 0.1164 0.055 Uiso 1 1 calc R . . C2 C 0.21703(5) 0.3149(2) 0.05972(19) 0.0434(9) Uani 1 1 d . . . C3 C 0.22813(6) 0.3041(3) 0.0060(2) 0.0576(11) Uani 1 1 d . . . H3 H 0.2380 0.3378 -0.0012 0.069 Uiso 1 1 calc R . . C4 C 0.22165(5) 0.2337(3) -0.0346(2) 0.0543(11) Uani 1 1 d . . . H4 H 0.2261 0.2104 -0.0757 0.065 Uiso 1 1 calc R . . C5 C 0.20724(5) 0.2041(2) -0.00280(18) 0.0430(9) Uani 1 1 d . . . C6 C 0.19810(5) 0.1261(2) -0.02133(19) 0.0459(9) Uani 1 1 d . . . H6 H 0.1997 0.0992 -0.0656 0.055 Uiso 1 1 calc R . . C7 C 0.20753(5) 0.4800(2) 0.1897(2) 0.0448(9) Uani 1 1 d . . . C8 C 0.20987(5) 0.5612(2) 0.1597(2) 0.0466(9) Uani 1 1 d . . . C9 C 0.21125(6) 0.6312(3) 0.2068(2) 0.0589(11) Uani 1 1 d . . . H9 H 0.2129 0.6867 0.1880 0.071 Uiso 1 1 calc R . . C10 C 0.21026(6) 0.6224(3) 0.2791(2) 0.0619(12) Uani 1 1 d . . . H10 H 0.2112 0.6712 0.3097 0.074 Uiso 1 1 calc R . . C11 C 0.20786(7) 0.5418(3) 0.3072(2) 0.0635(12) Uani 1 1 d . . . H11 H 0.2072 0.5359 0.3574 0.076 Uiso 1 1 calc R . . C12 C 0.20635(6) 0.4695(3) 0.2637(2) 0.0516(10) Uani 1 1 d . . . C13 C 0.18076(6) 0.0074(3) -0.00213(19) 0.0502(10) Uani 1 1 d . . . C14 C 0.16259(6) -0.0010(3) -0.0106(2) 0.0645(12) Uani 1 1 d . . . C15 C 0.15547(8) -0.0809(4) -0.0278(3) 0.0850(17) Uani 1 1 d . . . H15 H 0.1432 -0.0879 -0.0335 0.102 Uiso 1 1 calc R . . C16 C 0.16614(10) -0.1514(4) -0.0369(3) 0.0917(19) Uani 1 1 d . . . H16 H 0.1611 -0.2060 -0.0484 0.110 Uiso 1 1 calc R . . C17 C 0.18410(9) -0.1408(3) -0.0289(2) 0.0784(16) Uani 1 1 d . . . H17 H 0.1913 -0.1887 -0.0361 0.094 Uiso 1 1 calc R . . C18 C 0.19193(6) -0.0623(3) -0.0106(2) 0.0571(11) Uani 1 1 d . . . C19 C 0.21106(6) 0.5772(3) 0.0806(2) 0.0545(10) Uani 1 1 d . . . H19 H 0.2094 0.5207 0.0554 0.065 Uiso 1 1 calc R . . C20 C 0.22919(7) 0.6098(4) 0.0684(3) 0.0824(16) Uani 1 1 d . . . H20A H 0.2308 0.6681 0.0877 0.124 Uiso 1 1 calc R . . H20B H 0.2302 0.6103 0.0166 0.124 Uiso 1 1 calc R . . H20C H 0.2381 0.5720 0.0931 0.124 Uiso 1 1 calc R . . C21 C 0.19679(6) 0.6369(3) 0.0465(2) 0.0697(13) Uani 1 1 d . . . H21A H 0.1854 0.6099 0.0482 0.105 Uiso 1 1 calc R . . H21B H 0.1985 0.6480 -0.0037 0.105 Uiso 1 1 calc R . . H21C H 0.1973 0.6910 0.0733 0.105 Uiso 1 1 calc R . . C22 C 0.20361(7) 0.3831(3) 0.2961(2) 0.0698(14) Uani 1 1 d . . . H22 H 0.2031 0.3396 0.2566 0.084 Uiso 1 1 calc R . . C23 C 0.21874(9) 0.3590(4) 0.3531(3) 0.105(2) Uani 1 1 d . . . H23A H 0.2297 0.3612 0.3318 0.158 Uiso 1 1 calc R . . H23B H 0.2169 0.3009 0.3707 0.158 Uiso 1 1 calc R . . H23C H 0.2192 0.3995 0.3934 0.158 Uiso 1 1 calc R . . C24 C 0.18614(8) 0.3798(4) 0.3282(3) 0.0914(18) Uani 1 1 d . . . H24A H 0.1866 0.4191 0.3693 0.137 Uiso 1 1 calc R . . H24B H 0.1841 0.3213 0.3444 0.137 Uiso 1 1 calc R . . H24C H 0.1767 0.3968 0.2914 0.137 Uiso 1 1 calc R . . C25 C 0.15103(7) 0.0769(4) -0.0010(3) 0.0863(16) Uani 1 1 d . . . H25 H 0.1584 0.1292 -0.0039 0.104 Uiso 1 1 calc R . . C26 C 0.13595(10) 0.0834(6) -0.0607(4) 0.142(3) Uani 1 1 d . . . H26A H 0.1405 0.0845 -0.1075 0.213 Uiso 1 1 calc R . . H26B H 0.1294 0.1360 -0.0546 0.213 Uiso 1 1 calc R . . H26C H 0.1283 0.0337 -0.0585 0.213 Uiso 1 1 calc R . . C27 C 0.14499(9) 0.0762(4) 0.0727(4) 0.109(2) Uani 1 1 d . . . H27A H 0.1382 0.0240 0.0784 0.163 Uiso 1 1 calc R . . H27B H 0.1377 0.1265 0.0782 0.163 Uiso 1 1 calc R . . H27C H 0.1551 0.0774 0.1096 0.163 Uiso 1 1 calc R . . C28 C 0.21176(7) -0.0573(3) 0.0011(2) 0.0681(13) Uani 1 1 d . . . H28 H 0.2150 0.0012 0.0200 0.082 Uiso 1 1 calc R . . C29 C 0.21970(8) -0.0687(4) -0.0702(3) 0.0960(19) Uani 1 1 d . . . H29A H 0.2159 -0.1235 -0.0923 0.144 Uiso 1 1 calc R . . H29B H 0.2325 -0.0680 -0.0604 0.144 Uiso 1 1 calc R . . H29C H 0.2158 -0.0217 -0.1031 0.144 Uiso 1 1 calc R . . C30 C 0.21973(9) -0.1227(4) 0.0573(3) 0.0924(17) Uani 1 1 d . . . H30A H 0.2146 -0.1150 0.1023 0.139 Uiso 1 1 calc R . . H30B H 0.2324 -0.1139 0.0663 0.139 Uiso 1 1 calc R . . H30C H 0.2173 -0.1809 0.0391 0.139 Uiso 1 1 calc R . . C31 C 0.15082(5) 0.3460(2) 0.12118(19) 0.0458(9) Uani 1 1 d . . . H31 H 0.1392 0.3671 0.1172 0.055 Uiso 1 1 calc R . . C32 C 0.15567(5) 0.2781(2) 0.17030(19) 0.0423(9) Uani 1 1 d . . . C33 C 0.14618(5) 0.2514(3) 0.2260(2) 0.0563(11) Uani 1 1 d . . . H33 H 0.1350 0.2710 0.2350 0.068 Uiso 1 1 calc R . . C34 C 0.15641(5) 0.1909(3) 0.2652(2) 0.0532(10) Uani 1 1 d . . . H34 H 0.1538 0.1618 0.3072 0.064 Uiso 1 1 calc R . . C35 C 0.17152(5) 0.1812(2) 0.23030(18) 0.0430(9) Uani 1 1 d . . . C36 C 0.18446(5) 0.1171(2) 0.24705(19) 0.0447(9) Uani 1 1 d . . . H36 H 0.1852 0.0898 0.2928 0.054 Uiso 1 1 calc R . . C37 C 0.15579(5) 0.4496(2) 0.0352(2) 0.0419(9) Uani 1 1 d . . . C38 C 0.15144(5) 0.5288(2) 0.0649(2) 0.0473(9) Uani 1 1 d . . . C39 C 0.14669(5) 0.5953(3) 0.0159(2) 0.0576(11) Uani 1 1 d . . . H39 H 0.1435 0.6493 0.0338 0.069 Uiso 1 1 calc R . . C40 C 0.14646(6) 0.5844(3) -0.0571(3) 0.0642(12) Uani 1 1 d . . . H40 H 0.1432 0.6307 -0.0889 0.077 Uiso 1 1 calc R . . C41 C 0.15091(6) 0.5063(3) -0.0843(2) 0.0646(12) Uani 1 1 d . . . H41 H 0.1508 0.4993 -0.1349 0.078 Uiso 1 1 calc R . . C42 C 0.15559(5) 0.4377(3) -0.0385(2) 0.0514(10) Uani 1 1 d . . . C43 C 0.20671(5) 0.0243(2) 0.2241(2) 0.0467(9) Uani 1 1 d . . . C44 C 0.20001(6) -0.0557(2) 0.2415(2) 0.0513(10) Uani 1 1 d . . . C45 C 0.21198(7) -0.1195(3) 0.2650(2) 0.0644(12) Uani 1 1 d . . . H45 H 0.2079 -0.1742 0.2778 0.077 Uiso 1 1 calc R . . C46 C 0.22962(7) -0.1042(4) 0.2698(3) 0.0785(15) Uani 1 1 d . . . H46 H 0.2375 -0.1477 0.2887 0.094 Uiso 1 1 calc R . . C47 C 0.23614(7) -0.0285(3) 0.2483(3) 0.0756(14) Uani 1 1 d . . . H47 H 0.2484 -0.0205 0.2502 0.091 Uiso 1 1 calc R . . C48 C 0.22464(6) 0.0375(3) 0.2235(2) 0.0616(12) Uani 1 1 d . . . C49 C 0.15183(5) 0.5446(3) 0.1458(2) 0.0546(10) Uani 1 1 d . . . H49 H 0.1579 0.4950 0.1715 0.066 Uiso 1 1 calc R . . C50 C 0.16171(7) 0.6253(3) 0.1709(3) 0.0780(15) Uani 1 1 d . . . H50A H 0.1737 0.6216 0.1586 0.117 Uiso 1 1 calc R . . H50B H 0.1619 0.6310 0.2232 0.117 Uiso 1 1 calc R . . H50C H 0.1559 0.6752 0.1470 0.117 Uiso 1 1 calc R . . C51 C 0.13342(6) 0.5486(4) 0.1678(3) 0.0764(15) Uani 1 1 d . . . H51A H 0.1341 0.5543 0.2203 0.115 Uiso 1 1 calc R . . H51B H 0.1271 0.4959 0.1525 0.115 Uiso 1 1 calc R . . H51C H 0.1272 0.5980 0.1447 0.115 Uiso 1 1 calc R . . C52 C 0.16019(6) 0.3515(3) -0.0693(2) 0.0613(12) Uani 1 1 d . . . H52 H 0.1618 0.3099 -0.0283 0.074 Uiso 1 1 calc R . . C53 C 0.14576(7) 0.3170(4) -0.1241(3) 0.0896(17) Uani 1 1 d . . . H53A H 0.1350 0.3107 -0.1014 0.134 Uiso 1 1 calc R . . H53B H 0.1492 0.2611 -0.1416 0.134 Uiso 1 1 calc R . . H53C H 0.1437 0.3569 -0.1647 0.134 Uiso 1 1 calc R . . C54 C 0.17744(7) 0.3573(4) -0.1002(3) 0.0853(16) Uani 1 1 d . . . H54A H 0.1765 0.3997 -0.1392 0.128 Uiso 1 1 calc R . . H54B H 0.1803 0.3012 -0.1192 0.128 Uiso 1 1 calc R . . H54C H 0.1866 0.3746 -0.0622 0.128 Uiso 1 1 calc R . . C55 C 0.18050(6) -0.0772(3) 0.2293(2) 0.0550(10) Uani 1 1 d . . . H55 H 0.1743 -0.0249 0.2089 0.066 Uiso 1 1 calc R . . C56 C 0.17674(8) -0.1481(3) 0.1749(3) 0.0838(16) Uani 1 1 d . . . H56A H 0.1826 -0.2006 0.1934 0.126 Uiso 1 1 calc R . . H56B H 0.1810 -0.1316 0.1296 0.126 Uiso 1 1 calc R . . H56C H 0.1641 -0.1581 0.1665 0.126 Uiso 1 1 calc R . . C57 C 0.17319(7) -0.0985(4) 0.2996(3) 0.0813(15) Uani 1 1 d . . . H57A H 0.1795 -0.1478 0.3226 0.122 Uiso 1 1 calc R . . H57B H 0.1608 -0.1124 0.2894 0.122 Uiso 1 1 calc R . . H57C H 0.1747 -0.0490 0.3321 0.122 Uiso 1 1 calc R . . C58 C 0.23129(7) 0.1231(4) 0.1975(3) 0.0921(19) Uani 1 1 d . . . H58 H 0.2208 0.1535 0.1735 0.111 Uiso 1 1 calc R . . C59 C 0.24326(9) 0.1132(4) 0.1411(4) 0.110(2) Uiso 1 1 d . . . H59A H 0.2471 0.1699 0.1267 0.165 Uiso 1 1 calc R . . H59B H 0.2371 0.0839 0.0991 0.165 Uiso 1 1 calc R . . H59C H 0.2535 0.0794 0.1604 0.165 Uiso 1 1 calc R . . C60 C 0.23829(11) 0.1786(5) 0.2589(4) 0.126(2) Uiso 1 1 d . . . H60A H 0.2491 0.1538 0.2828 0.189 Uiso 1 1 calc R . . H60B H 0.2297 0.1827 0.2934 0.189 Uiso 1 1 calc R . . H60C H 0.2407 0.2359 0.2410 0.189 Uiso 1 1 calc R . . C61 C 0.06961(5) 0.1323(2) 0.40346(18) 0.0409(8) Uani 1 1 d . . . H61 H 0.0702 0.1044 0.3586 0.049 Uiso 1 1 calc R . . C62 C 0.08018(5) 0.2060(2) 0.41964(18) 0.0381(8) Uani 1 1 d . . . C63 C 0.09461(5) 0.2291(3) 0.3845(2) 0.0494(10) Uani 1 1 d . . . H63 H 0.0984 0.2024 0.3434 0.059 Uiso 1 1 calc R . . C64 C 0.10216(5) 0.2982(2) 0.42174(19) 0.0469(10) Uani 1 1 d . . . H64 H 0.1122 0.3288 0.4113 0.056 Uiso 1 1 calc R . . C65 C 0.09219(4) 0.3146(2) 0.47801(18) 0.0384(8) Uani 1 1 d . . . C66 C 0.09482(5) 0.3856(2) 0.52727(18) 0.0403(8) Uani 1 1 d . . . H66 H 0.1056 0.4157 0.5307 0.048 Uiso 1 1 calc R . . C67 C 0.05048(5) 0.0223(2) 0.42423(19) 0.0471(10) Uani 1 1 d . . . C68 C 0.03223(6) 0.0228(3) 0.4160(2) 0.0602(12) Uani 1 1 d . . . C69 C 0.02361(7) -0.0543(4) 0.3971(2) 0.0767(16) Uani 1 1 d . . . H69 H 0.0112 -0.0561 0.3902 0.092 Uiso 1 1 calc R . . C70 C 0.03322(9) -0.1283(3) 0.3884(3) 0.0860(19) Uani 1 1 d . . . H70 H 0.0272 -0.1805 0.3765 0.103 Uiso 1 1 calc R . . C71 C 0.05103(8) -0.1279(3) 0.3964(3) 0.0746(15) Uani 1 1 d . . . H71 H 0.0572 -0.1793 0.3892 0.090 Uiso 1 1 calc R . . C72 C 0.06029(6) -0.0524(3) 0.4151(2) 0.0557(11) Uani 1 1 d . . . C73 C 0.08692(5) 0.4829(2) 0.61176(19) 0.0418(9) Uani 1 1 d . . . C74 C 0.08634(5) 0.4717(3) 0.6856(2) 0.0493(10) Uani 1 1 d . . . C75 C 0.09009(6) 0.5422(3) 0.7310(2) 0.0616(12) Uani 1 1 d . . . H75 H 0.0901 0.5356 0.7816 0.074 Uiso 1 1 calc R . . C76 C 0.09376(7) 0.6206(3) 0.7037(2) 0.0671(13) Uani 1 1 d . . . H76 H 0.0964 0.6676 0.7354 0.081 Uiso 1 1 calc R . . C77 C 0.09371(6) 0.6318(3) 0.6305(2) 0.0619(12) Uani 1 1 d . . . H77 H 0.0960 0.6869 0.6123 0.074 Uiso 1 1 calc R . . C78 C 0.09037(5) 0.5633(2) 0.5825(2) 0.0477(9) Uani 1 1 d . . . C79 C 0.02199(6) 0.1047(3) 0.4266(3) 0.0739(14) Uani 1 1 d . . . H79 H 0.0300 0.1544 0.4221 0.089 Uiso 1 1 calc R . . C80 C 0.01645(9) 0.1068(4) 0.5023(3) 0.104(2) Uani 1 1 d . . . H80A H 0.0102 0.1604 0.5090 0.156 Uiso 1 1 calc R . . H80B H 0.0268 0.1035 0.5380 0.156 Uiso 1 1 calc R . . H80C H 0.0088 0.0581 0.5085 0.156 Uiso 1 1 calc R . . C81 C 0.00622(9) 0.1155(6) 0.3698(4) 0.127(3) Uani 1 1 d . . . H81A H -0.0017 0.0666 0.3720 0.190 Uiso 1 1 calc R . . H81B H 0.0101 0.1183 0.3219 0.190 Uiso 1 1 calc R . . H81C H 0.0001 0.1685 0.3791 0.190 Uiso 1 1 calc R . . C82 C 0.08027(7) -0.0555(3) 0.4264(2) 0.0623(12) Uani 1 1 d . . . H82 H 0.0845 0.0036 0.4400 0.075 Uiso 1 1 calc R . . C83 C 0.08726(9) -0.1148(4) 0.4876(3) 0.0983(19) Uani 1 1 d . . . H83A H 0.0843 -0.1742 0.4741 0.147 Uiso 1 1 calc R . . H83B H 0.0820 -0.0998 0.5311 0.147 Uiso 1 1 calc R . . H83C H 0.1000 -0.1086 0.4970 0.147 Uiso 1 1 calc R . . C84 C 0.08741(8) -0.0783(4) 0.3564(3) 0.101(2) Uani 1 1 d . . . H84A H 0.1002 -0.0749 0.3635 0.151 Uiso 1 1 calc R . . H84B H 0.0828 -0.0381 0.3185 0.151 Uiso 1 1 calc R . . H84C H 0.0838 -0.1367 0.3421 0.151 Uiso 1 1 calc R . . C85 C 0.08195(6) 0.3849(3) 0.7168(2) 0.0598(12) Uani 1 1 d . . . H85 H 0.0800 0.3437 0.6757 0.072 Uiso 1 1 calc R . . C86 C 0.06527(7) 0.3884(3) 0.7517(3) 0.0847(16) Uani 1 1 d . . . H86A H 0.0624 0.3309 0.7679 0.127 Uiso 1 1 calc R . . H86B H 0.0558 0.4092 0.7166 0.127 Uiso 1 1 calc R . . H86C H 0.0668 0.4273 0.7931 0.127 Uiso 1 1 calc R . . C87 C 0.09695(8) 0.3508(4) 0.7686(4) 0.107(2) Uani 1 1 d . . . H87A H 0.1075 0.3472 0.7440 0.160 Uiso 1 1 calc R . . H87B H 0.0940 0.2937 0.7852 0.160 Uiso 1 1 calc R . . H87C H 0.0991 0.3894 0.8101 0.160 Uiso 1 1 calc R . . C88 C 0.09025(6) 0.5806(3) 0.5021(2) 0.0570(11) Uani 1 1 d . . . H88 H 0.0882 0.5245 0.4766 0.068 Uiso 1 1 calc R . . C89 C 0.10757(7) 0.6138(4) 0.4858(3) 0.0891(18) Uani 1 1 d . . . H89A H 0.1169 0.5758 0.5075 0.134 Uiso 1 1 calc R . . H89B H 0.1094 0.6716 0.5057 0.134 Uiso 1 1 calc R . . H89C H 0.1078 0.6156 0.4335 0.134 Uiso 1 1 calc R . . C90 C 0.07552(8) 0.6404(4) 0.4725(3) 0.0853(16) Uani 1 1 d . . . H90A H 0.0766 0.6538 0.4220 0.128 Uiso 1 1 calc R . . H90B H 0.0762 0.6935 0.5007 0.128 Uiso 1 1 calc R . . H90C H 0.0643 0.6124 0.4757 0.128 Uiso 1 1 calc R . . C91 C 0.05817(5) 0.1329(2) 0.67689(18) 0.0417(9) Uani 1 1 d . . . H91 H 0.0582 0.1059 0.7225 0.050 Uiso 1 1 calc R . . C92 C 0.04601(5) 0.2001(2) 0.65797(18) 0.0395(8) Uani 1 1 d . . . C93 C 0.03106(5) 0.2156(3) 0.6920(2) 0.0524(10) Uani 1 1 d . . . H93 H 0.0279 0.1879 0.7338 0.063 Uiso 1 1 calc R . . C94 C 0.02186(5) 0.2790(3) 0.6526(2) 0.0563(11) Uani 1 1 d . . . H94 H 0.0111 0.3033 0.6617 0.068 Uiso 1 1 calc R . . C95 C 0.03165(5) 0.3005(2) 0.59636(18) 0.0406(9) Uani 1 1 d . . . C96 C 0.02777(5) 0.3681(2) 0.54577(18) 0.0427(9) Uani 1 1 d . . . H96 H 0.0165 0.3930 0.5414 0.051 Uiso 1 1 calc R . . C97 C 0.07964(5) 0.0332(2) 0.65758(19) 0.0442(9) Uani 1 1 d . . . C98 C 0.07160(6) -0.0459(3) 0.6680(2) 0.0497(10) Uani 1 1 d . . . C99 C 0.08257(7) -0.1152(3) 0.6901(2) 0.0641(13) Uani 1 1 d . . . H99 H 0.0775 -0.1693 0.6986 0.077 Uiso 1 1 calc R . . C100 C 0.10043(8) -0.1064(3) 0.6995(3) 0.0747(15) Uani 1 1 d . . . H100 H 0.1076 -0.1544 0.7140 0.090 Uiso 1 1 calc R . . C101 C 0.10807(6) -0.0284(3) 0.6880(2) 0.0664(13) Uani 1 1 d . . . H101 H 0.1204 -0.0231 0.6950 0.080 Uiso 1 1 calc R . . C102 C 0.09789(5) 0.0424(3) 0.6663(2) 0.0529(10) Uani 1 1 d . . . C103 C 0.03397(5) 0.4679(2) 0.45994(19) 0.0423(9) Uani 1 1 d . . . C104 C 0.02953(5) 0.5478(3) 0.4874(2) 0.0497(10) Uani 1 1 d . . . C105 C 0.02532(6) 0.6132(3) 0.4391(3) 0.0636(12) Uani 1 1 d . . . H105 H 0.0222 0.6675 0.4567 0.076 Uiso 1 1 calc R . . C106 C 0.02543(6) 0.6021(3) 0.3656(3) 0.0679(13) Uani 1 1 d . . . H106 H 0.0225 0.6483 0.3333 0.081 Uiso 1 1 calc R . . C107 C 0.02986(6) 0.5238(3) 0.3397(2) 0.0624(12) Uani 1 1 d . . . H107 H 0.0299 0.5165 0.2892 0.075 Uiso 1 1 calc R . . C108 C 0.03426(5) 0.4551(3) 0.3853(2) 0.0504(10) Uani 1 1 d . . . C109 C 0.05185(6) -0.0600(3) 0.6550(2) 0.0581(11) Uani 1 1 d . . . H109 H 0.0465 -0.0049 0.6361 0.070 Uiso 1 1 calc R . . C110 C 0.04695(8) -0.1284(4) 0.5982(3) 0.0883(17) Uani 1 1 d . . . H11A H 0.0517 -0.1837 0.6156 0.132 Uiso 1 1 calc R . . H11B H 0.0517 -0.1130 0.5536 0.132 Uiso 1 1 calc R . . H11C H 0.0342 -0.1324 0.5886 0.132 Uiso 1 1 calc R . . C111 C 0.04415(7) -0.0809(4) 0.7238(3) 0.0881(17) Uani 1 1 d . . . H11D H 0.0479 -0.0377 0.7605 0.132 Uiso 1 1 calc R . . H11E H 0.0482 -0.1375 0.7412 0.132 Uiso 1 1 calc R . . H11F H 0.0314 -0.0811 0.7143 0.132 Uiso 1 1 calc R . . C112 C 0.10625(6) 0.1284(3) 0.6530(3) 0.0642(12) Uani 1 1 d . . . H112 H 0.0972 0.1738 0.6566 0.077 Uiso 1 1 calc R . . C113 C 0.12182(8) 0.1489(5) 0.7091(4) 0.112(2) Uani 1 1 d . . . H11G H 0.1182 0.1455 0.7575 0.168 Uiso 1 1 calc R . . H11H H 0.1260 0.2069 0.7007 0.168 Uiso 1 1 calc R . . H11I H 0.1312 0.1075 0.7048 0.168 Uiso 1 1 calc R . . C114 C 0.11142(8) 0.1317(4) 0.5768(3) 0.0931(19) Uani 1 1 d . . . H11J H 0.1208 0.0904 0.5725 0.140 Uiso 1 1 calc R . . H11K H 0.1155 0.1895 0.5668 0.140 Uiso 1 1 calc R . . H11L H 0.1013 0.1172 0.5421 0.140 Uiso 1 1 calc R . . C115 C 0.02993(6) 0.5644(3) 0.5690(2) 0.0602(11) Uani 1 1 d . . . H115 H 0.0344 0.5109 0.5942 0.072 Uiso 1 1 calc R . . C116 C 0.04215(10) 0.6355(5) 0.5962(3) 0.114(2) Uani 1 1 d . . . H11M H 0.0382 0.6895 0.5731 0.171 Uiso 1 1 calc R . . H11N H 0.0539 0.6225 0.5847 0.171 Uiso 1 1 calc R . . H11O H 0.0423 0.6409 0.6486 0.171 Uiso 1 1 calc R . . C117 C 0.01191(8) 0.5791(5) 0.5891(3) 0.110(2) Uani 1 1 d . . . H11P H 0.0122 0.5768 0.6417 0.166 Uiso 1 1 calc R . . H11Q H 0.0041 0.5345 0.5672 0.166 Uiso 1 1 calc R . . H11R H 0.0077 0.6354 0.5717 0.166 Uiso 1 1 calc R . . C118 C 0.03910(6) 0.3685(3) 0.3559(2) 0.0588(12) Uani 1 1 d . . . H118 H 0.0413 0.3286 0.3978 0.071 Uiso 1 1 calc R . . C119 C 0.05569(7) 0.3734(3) 0.3207(3) 0.0784(15) Uani 1 1 d . . . H11S H 0.0537 0.4085 0.2771 0.118 Uiso 1 1 calc R . . H11T H 0.0592 0.3155 0.3080 0.118 Uiso 1 1 calc R . . H11U H 0.0649 0.3992 0.3544 0.118 Uiso 1 1 calc R . . C120 C 0.02437(8) 0.3304(4) 0.3047(3) 0.0952(18) Uani 1 1 d . . . H12A H 0.0143 0.3201 0.3306 0.143 Uiso 1 1 calc R . . H12B H 0.0282 0.2762 0.2854 0.143 Uiso 1 1 calc R . . H12C H 0.0211 0.3704 0.2649 0.143 Uiso 1 1 calc R . . Li1 Li 0.18894(9) 0.1615(4) 0.1104(3) 0.0492(15) Uani 1 1 d . . . Li2 Li 0.18541(8) 0.3248(4) 0.1133(3) 0.0445(14) Uani 1 1 d . . . Li3 Li 0.06349(8) 0.1720(4) 0.5389(3) 0.0436(14) Uani 1 1 d . . . Li4 Li 0.06161(8) 0.3356(4) 0.5371(3) 0.0428(13) Uani 1 1 d . . . N1 N 0.20541(4) 0.40466(19) 0.14540(15) 0.0429(7) Uani 1 1 d . . . N2 N 0.20413(4) 0.25429(18) 0.05554(14) 0.0391(7) Uani 1 1 d . . . N3 N 0.18775(4) 0.0904(2) 0.01917(16) 0.0461(8) Uani 1 1 d . . . N4 N 0.16171(4) 0.38019(19) 0.08156(15) 0.0408(7) Uani 1 1 d . . . N5 N 0.17125(4) 0.23431(19) 0.17179(15) 0.0397(7) Uani 1 1 d . . . N6 N 0.19530(4) 0.09437(19) 0.20248(16) 0.0447(7) Uani 1 1 d . . . N7 N 0.05921(4) 0.10099(19) 0.44609(15) 0.0423(7) Uani 1 1 d . . . N8 N 0.07850(4) 0.25868(17) 0.47761(14) 0.0331(6) Uani 1 1 d . . . N9 N 0.08319(4) 0.40969(18) 0.56680(15) 0.0380(7) Uani 1 1 d . . . N10 N 0.06922(4) 0.10690(18) 0.63476(15) 0.0385(7) Uani 1 1 d . . . N11 N 0.04655(4) 0.25231(18) 0.59873(14) 0.0359(7) Uani 1 1 d . . . N12 N 0.03886(4) 0.39662(19) 0.50599(15) 0.0406(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 C1 0.043(2) 0.054(2) 0.041(2) -0.0009(18) 0.0057(17) -0.0018(18) C2 0.047(2) 0.044(2) 0.041(2) -0.0020(17) 0.0135(17) -0.0002(17) C3 0.057(2) 0.059(3) 0.062(3) -0.003(2) 0.026(2) -0.006(2) C4 0.061(2) 0.060(3) 0.046(2) -0.002(2) 0.023(2) 0.001(2) C5 0.054(2) 0.044(2) 0.0320(18) -0.0007(16) 0.0094(17) 0.0028(18) C6 0.056(2) 0.049(2) 0.0331(19) 0.0010(17) 0.0076(18) 0.0089(19) C7 0.048(2) 0.043(2) 0.042(2) -0.0042(17) 0.0026(17) 0.0007(18) C8 0.051(2) 0.046(2) 0.042(2) -0.0002(18) 0.0053(18) 0.0005(18) C9 0.072(3) 0.048(2) 0.057(3) -0.002(2) 0.010(2) -0.003(2) C10 0.081(3) 0.056(3) 0.048(2) -0.012(2) 0.004(2) -0.001(2) C11 0.094(3) 0.056(3) 0.040(2) -0.004(2) 0.008(2) -0.001(2) C12 0.071(3) 0.047(2) 0.037(2) -0.0022(18) 0.008(2) -0.001(2) C13 0.072(3) 0.044(2) 0.0326(19) -0.0024(17) 0.0010(19) -0.008(2) C14 0.071(3) 0.069(3) 0.052(3) 0.009(2) 0.004(2) -0.017(3) C15 0.096(4) 0.090(4) 0.068(3) 0.009(3) 0.003(3) -0.040(4) C16 0.144(6) 0.070(4) 0.057(3) -0.001(3) -0.002(4) -0.035(4) C17 0.134(5) 0.050(3) 0.052(3) -0.006(2) 0.012(3) -0.013(3) C18 0.086(3) 0.046(2) 0.040(2) -0.0062(18) 0.008(2) -0.002(2) C19 0.067(3) 0.054(2) 0.044(2) 0.0038(19) 0.008(2) 0.000(2) C20 0.071(3) 0.112(4) 0.067(3) 0.018(3) 0.016(3) -0.005(3) C21 0.078(3) 0.079(3) 0.051(3) 0.010(2) 0.006(2) 0.008(3) C22 0.117(4) 0.055(3) 0.040(2) 0.002(2) 0.022(3) -0.005(3) C23 0.131(5) 0.107(5) 0.079(4) 0.030(4) 0.020(4) 0.026(4) C24 0.113(5) 0.089(4) 0.075(3) 0.003(3) 0.025(3) -0.030(4) C25 0.058(3) 0.092(4) 0.109(4) 0.008(3) 0.014(3) -0.011(3) C26 0.107(5) 0.208(9) 0.110(5) 0.025(6) 0.009(5) 0.034(6) C27 0.118(5) 0.104(5) 0.106(5) -0.030(4) 0.024(4) -0.016(4) C28 0.091(4) 0.055(3) 0.058(3) -0.001(2) 0.007(3) 0.013(3) C29 0.104(4) 0.103(4) 0.086(4) -0.007(3) 0.036(4) 0.030(4) C30 0.113(5) 0.076(4) 0.085(4) 0.012(3) -0.003(3) 0.016(3) C31 0.047(2) 0.048(2) 0.042(2) 0.0023(18) 0.0069(18) 0.0037(18) C32 0.0406(19) 0.044(2) 0.044(2) 0.0042(17) 0.0105(17) 0.0008(17) C33 0.052(2) 0.068(3) 0.053(2) 0.004(2) 0.023(2) 0.004(2) C34 0.061(2) 0.061(3) 0.041(2) 0.010(2) 0.018(2) 0.002(2) C35 0.050(2) 0.047(2) 0.0337(19) 0.0072(17) 0.0113(17) 0.0022(18) C36 0.055(2) 0.046(2) 0.0330(19) 0.0044(17) 0.0060(17) -0.0029(18) C37 0.0391(19) 0.042(2) 0.044(2) 0.0044(17) 0.0061(17) 0.0043(16) C38 0.043(2) 0.048(2) 0.050(2) 0.0044(19) 0.0024(18) 0.0050(18) C39 0.051(2) 0.052(2) 0.070(3) 0.004(2) 0.006(2) 0.009(2) C40 0.063(3) 0.064(3) 0.066(3) 0.027(2) 0.009(2) 0.011(2) C41 0.069(3) 0.078(3) 0.048(2) 0.015(2) 0.012(2) 0.020(3) C42 0.057(2) 0.059(3) 0.039(2) 0.0074(19) 0.0103(19) 0.014(2) C43 0.054(2) 0.044(2) 0.042(2) 0.0085(18) 0.0043(18) 0.0047(19) C44 0.067(3) 0.044(2) 0.043(2) 0.0042(18) 0.006(2) 0.008(2) C45 0.088(4) 0.043(2) 0.061(3) 0.007(2) 0.000(3) 0.010(2) C46 0.083(4) 0.079(4) 0.072(3) 0.008(3) 0.003(3) 0.033(3) C47 0.067(3) 0.083(4) 0.077(3) 0.007(3) 0.008(3) 0.010(3) C48 0.058(3) 0.068(3) 0.060(3) 0.013(2) 0.015(2) 0.011(2) C49 0.053(2) 0.057(3) 0.052(2) -0.009(2) 0.002(2) 0.009(2) C50 0.076(3) 0.081(3) 0.077(3) -0.030(3) 0.007(3) -0.012(3) C51 0.072(3) 0.102(4) 0.056(3) -0.019(3) 0.014(2) -0.001(3) C52 0.080(3) 0.067(3) 0.039(2) 0.003(2) 0.015(2) 0.019(2) C53 0.090(4) 0.097(4) 0.085(4) -0.019(3) 0.022(3) 0.005(3) C54 0.074(3) 0.098(4) 0.086(4) -0.008(3) 0.019(3) 0.025(3) C55 0.068(3) 0.050(2) 0.045(2) 0.0065(19) 0.000(2) -0.007(2) C56 0.102(4) 0.073(3) 0.074(3) -0.017(3) 0.005(3) -0.017(3) C57 0.078(3) 0.101(4) 0.063(3) 0.017(3) 0.005(3) -0.025(3) C58 0.064(3) 0.096(4) 0.121(5) 0.042(4) 0.031(3) -0.001(3) C61 0.053(2) 0.040(2) 0.0300(18) -0.0048(16) 0.0059(17) -0.0034(17) C62 0.046(2) 0.0357(19) 0.0333(18) -0.0048(16) 0.0066(16) -0.0032(16) C63 0.060(2) 0.052(2) 0.040(2) -0.0114(18) 0.0197(19) -0.003(2) C64 0.049(2) 0.051(2) 0.044(2) -0.0071(18) 0.0199(18) -0.0127(18) C65 0.0375(18) 0.040(2) 0.0374(19) -0.0011(16) 0.0032(16) -0.0027(16) C66 0.0401(19) 0.042(2) 0.0388(19) -0.0024(17) 0.0058(16) -0.0071(16) C67 0.065(3) 0.045(2) 0.0333(19) -0.0078(17) 0.0109(18) -0.016(2) C68 0.070(3) 0.064(3) 0.050(2) -0.007(2) 0.022(2) -0.025(2) C69 0.086(3) 0.088(4) 0.059(3) -0.016(3) 0.020(3) -0.050(3) C70 0.142(6) 0.061(3) 0.061(3) -0.021(3) 0.033(3) -0.048(4) C71 0.114(4) 0.053(3) 0.061(3) -0.012(2) 0.027(3) -0.023(3) C72 0.085(3) 0.043(2) 0.041(2) -0.0014(18) 0.017(2) -0.013(2) C73 0.047(2) 0.042(2) 0.0363(19) -0.0097(16) 0.0042(17) -0.0043(17) C74 0.060(2) 0.050(2) 0.040(2) -0.0063(18) 0.0105(19) -0.003(2) C75 0.084(3) 0.064(3) 0.038(2) -0.014(2) 0.015(2) -0.006(2) C76 0.089(3) 0.054(3) 0.060(3) -0.026(2) 0.016(3) -0.016(2) C77 0.085(3) 0.040(2) 0.062(3) -0.011(2) 0.013(2) -0.011(2) C78 0.054(2) 0.043(2) 0.046(2) -0.0002(18) 0.0070(19) -0.0014(18) C79 0.054(3) 0.075(3) 0.096(4) -0.014(3) 0.023(3) -0.022(2) C80 0.122(5) 0.107(5) 0.091(4) -0.041(4) 0.046(4) -0.024(4) C81 0.086(4) 0.172(8) 0.119(5) -0.007(5) -0.002(4) 0.007(5) C82 0.089(3) 0.050(2) 0.049(2) -0.003(2) 0.014(2) 0.003(2) C83 0.126(5) 0.095(4) 0.072(3) 0.013(3) 0.003(4) 0.007(4) C84 0.102(4) 0.142(6) 0.060(3) -0.024(3) 0.015(3) 0.022(4) C85 0.086(3) 0.054(3) 0.042(2) -0.002(2) 0.018(2) -0.010(2) C86 0.087(4) 0.082(4) 0.092(4) -0.002(3) 0.036(3) -0.019(3) C87 0.100(4) 0.107(5) 0.113(5) 0.059(4) 0.011(4) 0.003(4) C88 0.075(3) 0.047(2) 0.049(2) 0.010(2) 0.010(2) -0.004(2) C89 0.069(3) 0.144(5) 0.054(3) 0.025(3) 0.008(2) -0.022(3) C90 0.098(4) 0.084(4) 0.071(3) 0.017(3) 0.000(3) 0.008(3) C91 0.053(2) 0.043(2) 0.0296(18) 0.0023(16) 0.0073(17) -0.0041(18) C92 0.047(2) 0.042(2) 0.0300(17) 0.0022(16) 0.0060(16) 0.0008(17) C93 0.056(2) 0.061(3) 0.044(2) 0.013(2) 0.0198(19) 0.006(2) C94 0.050(2) 0.070(3) 0.053(2) 0.015(2) 0.022(2) 0.017(2) C95 0.0385(19) 0.048(2) 0.0358(19) 0.0051(17) 0.0079(16) 0.0039(17) C96 0.0408(19) 0.051(2) 0.0364(19) 0.0053(17) 0.0046(16) 0.0082(17) C97 0.058(2) 0.043(2) 0.0311(18) 0.0030(16) 0.0060(17) 0.0056(18) C98 0.068(3) 0.048(2) 0.0339(19) 0.0055(18) 0.0072(19) 0.002(2) C99 0.096(4) 0.043(2) 0.055(3) 0.012(2) 0.016(3) 0.013(2) C100 0.097(4) 0.066(3) 0.062(3) 0.023(2) 0.014(3) 0.034(3) C101 0.063(3) 0.073(3) 0.065(3) 0.019(2) 0.015(2) 0.027(3) C102 0.056(2) 0.060(3) 0.044(2) 0.008(2) 0.0112(19) 0.008(2) C103 0.043(2) 0.042(2) 0.042(2) 0.0046(17) 0.0049(17) 0.0093(17) C104 0.052(2) 0.048(2) 0.049(2) 0.0071(19) 0.0068(19) 0.0085(19) C105 0.067(3) 0.049(3) 0.078(3) 0.008(2) 0.020(3) 0.012(2) C106 0.073(3) 0.066(3) 0.067(3) 0.027(2) 0.016(2) 0.018(2) C107 0.073(3) 0.068(3) 0.048(2) 0.020(2) 0.016(2) 0.018(2) C108 0.055(2) 0.058(2) 0.040(2) 0.0082(19) 0.0126(19) 0.009(2) C109 0.080(3) 0.044(2) 0.049(2) 0.0052(19) 0.003(2) -0.006(2) C110 0.113(4) 0.077(4) 0.076(3) -0.013(3) 0.017(3) -0.027(3) C111 0.085(4) 0.124(5) 0.057(3) 0.019(3) 0.015(3) -0.015(3) C112 0.051(2) 0.068(3) 0.076(3) 0.009(2) 0.013(2) 0.005(2) C113 0.087(4) 0.138(6) 0.106(5) 0.014(4) -0.011(4) -0.033(4) C114 0.107(4) 0.086(4) 0.091(4) 0.043(3) 0.034(4) 0.015(3) C115 0.074(3) 0.056(3) 0.051(2) -0.012(2) 0.011(2) 0.004(2) C116 0.133(6) 0.121(5) 0.090(4) -0.031(4) 0.014(4) -0.035(5) C117 0.083(4) 0.183(7) 0.066(3) -0.031(4) 0.014(3) 0.027(4) C118 0.079(3) 0.061(3) 0.038(2) 0.005(2) 0.014(2) 0.017(2) C119 0.081(3) 0.079(3) 0.078(3) 0.004(3) 0.026(3) 0.022(3) C120 0.093(4) 0.095(4) 0.100(4) -0.027(4) 0.019(4) 0.005(3) Li1 0.059(4) 0.055(4) 0.033(3) 0.006(3) 0.005(3) 0.002(3) Li2 0.049(3) 0.043(3) 0.042(3) 0.001(3) 0.006(3) 0.006(3) Li3 0.053(3) 0.044(3) 0.034(3) 0.001(3) 0.009(3) 0.002(3) Li4 0.043(3) 0.039(3) 0.047(3) 0.006(3) 0.008(3) -0.002(3) N1 0.0491(17) 0.0461(18) 0.0338(15) -0.0012(14) 0.0063(14) 0.0036(15) N2 0.0435(17) 0.0427(17) 0.0317(15) 0.0032(13) 0.0075(13) 0.0027(14) N3 0.0553(19) 0.0456(18) 0.0378(16) 0.0002(14) 0.0070(15) -0.0014(15) N4 0.0438(16) 0.0430(17) 0.0356(15) 0.0030(14) 0.0051(14) 0.0058(14) N5 0.0435(16) 0.0424(17) 0.0337(15) 0.0041(13) 0.0063(13) 0.0004(14) N6 0.0526(18) 0.0407(17) 0.0416(17) 0.0069(14) 0.0086(15) 0.0023(15) N7 0.0547(18) 0.0386(16) 0.0338(15) -0.0019(13) 0.0061(14) -0.0083(15) N8 0.0385(15) 0.0327(15) 0.0287(14) -0.0020(12) 0.0057(12) -0.0026(13) N9 0.0468(17) 0.0353(16) 0.0314(15) -0.0014(13) 0.0027(13) -0.0025(13) N10 0.0468(17) 0.0353(16) 0.0328(15) 0.0033(13) 0.0024(13) 0.0017(13) N11 0.0391(15) 0.0390(16) 0.0298(14) 0.0027(13) 0.0055(13) -0.0002(13) N12 0.0436(16) 0.0461(18) 0.0323(15) 0.0055(14) 0.0047(13) 0.0044(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 C1 N1 1.294(4) . ? C1 C2 1.425(5) . ? C2 N2 1.369(5) . ? C2 C3 1.406(5) . ? C3 C4 1.393(6) . ? C4 C5 1.401(5) . ? C5 N2 1.386(4) . ? C5 C6 1.429(5) . ? C6 N3 1.291(4) . ? C7 C12 1.406(5) . ? C7 C8 1.406(5) . ? C7 N1 1.437(5) . ? C8 C9 1.399(6) . ? C8 C19 1.512(5) . ? C9 C10 1.369(6) . ? C10 C11 1.385(6) . ? C11 C12 1.387(6) . ? C12 C22 1.504(6) . ? C13 C14 1.399(6) . ? C13 C18 1.410(6) . ? C13 N3 1.441(5) . ? C14 C15 1.387(7) . ? C14 C25 1.532(7) . ? C15 C16 1.396(8) . ? C16 C17 1.387(9) . ? C17 C18 1.390(6) . ? C18 C28 1.523(7) . ? C19 C21 1.523(6) . ? C19 C20 1.532(6) . ? C22 C23 1.531(8) . ? C22 C24 1.541(7) . ? C25 C27 1.505(8) . ? C25 C26 1.517(9) . ? C28 C30 1.539(7) . ? C28 C29 1.542(6) . ? C31 N4 1.300(4) . ? C31 C32 1.423(5) . ? C32 N5 1.381(4) . ? C32 C33 1.406(5) . ? C33 C34 1.383(6) . ? C34 C35 1.411(5) . ? C35 N5 1.370(4) . ? C35 C36 1.422(5) . ? C36 N6 1.299(4) . ? C37 C42 1.388(5) . ? C37 C38 1.412(5) . ? C37 N4 1.428(5) . ? C38 C39 1.402(6) . ? C38 C49 1.528(5) . ? C39 C40 1.372(6) . ? C40 C41 1.380(6) . ? C41 C42 1.391(6) . ? C42 C52 1.522(6) . ? C43 C48 1.401(6) . ? C43 C44 1.404(5) . ? C43 N6 1.432(5) . ? C44 C45 1.394(6) . ? C44 C55 1.534(6) . ? C45 C46 1.375(7) . ? C46 C47 1.364(7) . ? C47 C48 1.403(7) . ? C48 C58 1.531(7) . ? C49 C50 1.517(6) . ? C49 C51 1.528(6) . ? C52 C54 1.517(6) . ? C52 C53 1.520(7) . ? C55 C56 1.507(6) . ? C55 C57 1.527(6) . ? C58 C60 1.487(9) . ? C58 C59 1.490(7) . ? C61 N7 1.292(4) . ? C61 C62 1.423(5) . ? C62 N8 1.378(4) . ? C62 C63 1.405(5) . ? C63 C64 1.375(5) . ? C64 C65 1.399(4) . ? C65 N8 1.370(4) . ? C65 C66 1.439(5) . ? C66 N9 1.285(4) . ? C67 C68 1.400(6) . ? C67 C72 1.411(6) . ? C67 N7 1.437(5) . ? C68 C69 1.400(6) . ? C68 C79 1.528(7) . ? C69 C70 1.394(8) . ? C70 C71 1.365(8) . ? C71 C72 1.402(6) . ? C72 C82 1.533(7) . ? C73 C74 1.397(5) . ? C73 C78 1.408(5) . ? C73 N9 1.426(4) . ? C74 C75 1.397(6) . ? C74 C85 1.529(5) . ? C75 C76 1.369(6) . ? C76 C77 1.378(6) . ? C77 C78 1.399(6) . ? C78 C88 1.525(5) . ? C79 C80 1.526(7) . ? C79 C81 1.526(9) . ? C82 C83 1.519(7) . ? C82 C84 1.521(6) . ? C85 C86 1.512(6) . ? C85 C87 1.515(8) . ? C88 C89 1.499(6) . ? C88 C90 1.524(7) . ? C91 N10 1.294(4) . ? C91 C92 1.424(5) . ? C92 N11 1.379(4) . ? C92 C93 1.404(5) . ? C93 C94 1.378(6) . ? C94 C95 1.406(4) . ? C95 N11 1.371(4) . ? C95 C96 1.424(5) . ? C96 N12 1.279(4) . ? C97 C98 1.405(5) . ? C97 C102 1.407(6) . ? C97 N10 1.439(5) . ? C98 C99 1.405(6) . ? C98 C109 1.531(6) . ? C99 C100 1.377(7) . ? C100 C101 1.382(7) . ? C101 C102 1.388(6) . ? C102 C112 1.522(6) . ? C103 C104 1.407(5) . ? C103 C108 1.411(5) . ? C103 N12 1.429(5) . ? C104 C105 1.375(6) . ? C104 C115 1.543(5) . ? C105 C106 1.386(6) . ? C106 C107 1.371(6) . ? C107 C108 1.387(6) . ? C108 C118 1.522(6) . ? C109 C111 1.515(6) . ? C109 C110 1.522(6) . ? C112 C114 1.524(6) . ? C112 C113 1.531(8) . ? C115 C117 1.501(7) . ? C115 C116 1.506(7) . ? C118 C119 1.509(6) . ? C118 C120 1.518(7) . ? 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 C1 C2 122.3(4) . . ? N2 C2 C3 112.2(3) . . ? N2 C2 C1 123.4(3) . . ? C3 C2 C1 124.2(3) . . ? C4 C3 C2 105.9(3) . . ? C3 C4 C5 106.3(3) . . ? N2 C5 C4 111.6(3) . . ? N2 C5 C6 123.0(3) . . ? C4 C5 C6 124.9(3) . . ? N3 C6 C5 123.2(3) . . ? C12 C7 C8 121.6(3) . . ? C12 C7 N1 117.1(3) . . ? C8 C7 N1 121.3(3) . . ? C9 C8 C7 117.1(3) . . ? C9 C8 C19 118.5(4) . . ? C7 C8 C19 124.3(3) . . ? C10 C9 C8 122.3(4) . . ? C9 C10 C11 119.4(4) . . ? C10 C11 C12 121.5(4) . . ? C11 C12 C7 118.1(4) . . ? C11 C12 C22 120.0(3) . . ? C7 C12 C22 121.9(4) . . ? C14 C13 C18 122.3(4) . . ? C14 C13 N3 116.9(4) . . ? C18 C13 N3 120.7(4) . . ? C15 C14 C13 118.4(5) . . ? C15 C14 C25 121.4(5) . . ? C13 C14 C25 120.2(4) . . ? C14 C15 C16 120.9(6) . . ? C17 C16 C15 119.3(5) . . ? C16 C17 C18 122.1(5) . . ? C17 C18 C13 117.0(5) . . ? C17 C18 C28 118.8(5) . . ? C13 C18 C28 124.2(4) . . ? C8 C19 C21 112.5(3) . . ? C8 C19 C20 111.3(4) . . ? C21 C19 C20 111.3(4) . . ? C12 C22 C23 111.6(5) . . ? C12 C22 C24 111.0(4) . . ? C23 C22 C24 110.6(4) . . ? C27 C25 C26 112.3(5) . . ? C27 C25 C14 110.4(5) . . ? C26 C25 C14 111.9(6) . . ? C18 C28 C30 112.2(4) . . ? C18 C28 C29 111.5(4) . . ? C30 C28 C29 110.2(4) . . ? N4 C31 C32 122.3(3) . . ? N5 C32 C33 111.6(3) . . ? N5 C32 C31 122.9(3) . . ? C33 C32 C31 125.3(3) . . ? C34 C33 C32 106.2(3) . . ? C33 C34 C35 106.3(3) . . ? N5 C35 C34 111.7(3) . . ? N5 C35 C36 123.0(3) . . ? C34 C35 C36 124.9(3) . . ? N6 C36 C35 122.8(3) . . ? C42 C37 C38 122.1(4) . . ? C42 C37 N4 117.7(3) . . ? C38 C37 N4 120.1(3) . . ? C39 C38 C37 116.6(4) . . ? C39 C38 C49 119.9(4) . . ? C37 C38 C49 123.5(3) . . ? C40 C39 C38 121.9(4) . . ? C39 C40 C41 120.0(4) . . ? C40 C41 C42 120.7(4) . . ? C37 C42 C41 118.6(4) . . ? C37 C42 C52 121.1(4) . . ? C41 C42 C52 120.3(4) . . ? C48 C43 C44 121.6(4) . . ? C48 C43 N6 117.5(3) . . ? C44 C43 N6 120.8(4) . . ? C45 C44 C43 117.3(4) . . ? C45 C44 C55 119.5(4) . . ? C43 C44 C55 122.9(4) . . ? C46 C45 C44 120.8(4) . . ? C47 C46 C45 121.9(5) . . ? C46 C47 C48 119.5(5) . . ? C43 C48 C47 118.5(4) . . ? C43 C48 C58 120.0(4) . . ? C47 C48 C58 121.5(4) . . ? C50 C49 C51 109.5(4) . . ? C50 C49 C38 112.9(4) . . ? C51 C49 C38 111.4(4) . . ? C54 C52 C53 111.7(4) . . ? C54 C52 C42 110.3(4) . . ? C53 C52 C42 112.5(4) . . ? C56 C55 C57 111.0(4) . . ? C56 C55 C44 111.6(4) . . ? C57 C55 C44 112.2(4) . . ? C60 C58 C59 114.0(5) . . ? C60 C58 C48 111.6(5) . . ? C59 C58 C48 113.2(5) . . ? N7 C61 C62 123.9(3) . . ? N8 C62 C63 111.6(3) . . ? N8 C62 C61 122.9(3) . . ? C63 C62 C61 125.1(3) . . ? C64 C63 C62 106.1(3) . . ? C63 C64 C65 106.6(3) . . ? N8 C65 C64 111.9(3) . . ? N8 C65 C66 123.0(3) . . ? C64 C65 C66 125.0(3) . . ? N9 C66 C65 122.5(3) . . ? C68 C67 C72 122.7(4) . . ? C68 C67 N7 117.3(4) . . ? C72 C67 N7 120.0(4) . . ? C67 C68 C69 117.7(5) . . ? C67 C68 C79 121.4(4) . . ? C69 C68 C79 120.9(4) . . ? C70 C69 C68 119.9(5) . . ? C71 C70 C69 121.8(5) . . ? C70 C71 C72 120.5(5) . . ? C71 C72 C67 117.4(5) . . ? C71 C72 C82 118.8(4) . . ? C67 C72 C82 123.8(4) . . ? C74 C73 C78 121.6(3) . . ? C74 C73 N9 117.0(3) . . ? C78 C73 N9 121.3(3) . . ? C73 C74 C75 118.2(4) . . ? C73 C74 C85 121.4(3) . . ? C75 C74 C85 120.3(3) . . ? C76 C75 C74 120.9(4) . . ? C75 C76 C77 120.5(4) . . ? C76 C77 C78 121.2(4) . . ? C77 C78 C73 117.5(3) . . ? C77 C78 C88 118.4(4) . . ? C73 C78 C88 124.1(3) . . ? C80 C79 C81 110.7(5) . . ? C80 C79 C68 110.2(5) . . ? C81 C79 C68 112.6(5) . . ? C83 C82 C84 111.8(4) . . ? C83 C82 C72 112.6(4) . . ? C84 C82 C72 110.6(4) . . ? C86 C85 C87 111.3(4) . . ? C86 C85 C74 111.8(4) . . ? C87 C85 C74 111.6(4) . . ? C89 C88 C90 111.1(4) . . ? C89 C88 C78 111.2(4) . . ? C90 C88 C78 112.5(4) . . ? N10 C91 C92 122.9(3) . . ? N11 C92 C93 111.5(3) . . ? N11 C92 C91 123.5(3) . . ? C93 C92 C91 124.6(3) . . ? C94 C93 C92 106.4(3) . . ? C93 C94 C95 106.4(3) . . ? N11 C95 C94 111.6(3) . . ? N11 C95 C96 122.5(3) . . ? C94 C95 C96 125.7(3) . . ? N12 C96 C95 122.8(3) . . ? C98 C97 C102 121.8(4) . . ? C98 C97 N10 120.1(4) . . ? C102 C97 N10 118.0(3) . . ? C97 C98 C99 117.1(4) . . ? C97 C98 C109 123.5(4) . . ? C99 C98 C109 119.3(4) . . ? C100 C99 C98 121.4(4) . . ? C99 C100 C101 120.5(4) . . ? C100 C101 C102 120.7(5) . . ? C101 C102 C97 118.4(4) . . ? C101 C102 C112 120.9(4) . . ? C97 C102 C112 120.7(4) . . ? C104 C103 C108 121.3(3) . . ? C104 C103 N12 121.9(3) . . ? C108 C103 N12 116.8(3) . . ? C105 C104 C103 117.9(4) . . ? C105 C104 C115 119.9(4) . . ? C103 C104 C115 122.2(4) . . ? C104 C105 C106 121.9(4) . . ? C107 C106 C105 119.5(4) . . ? C106 C107 C108 121.6(4) . . ? C107 C108 C103 117.8(4) . . ? C107 C108 C118 121.1(4) . . ? C103 C108 C118 121.1(3) . . ? C111 C109 C110 110.5(4) . . ? C111 C109 C98 112.3(4) . . ? C110 C109 C98 111.8(4) . . ? C102 C112 C114 110.2(4) . . ? C102 C112 C113 112.7(4) . . ? C114 C112 C113 111.1(4) . . ? C117 C115 C116 111.4(5) . . ? C117 C115 C104 111.3(4) . . ? C116 C115 C104 113.3(4) . . ? C119 C118 C120 110.9(4) . . ? C119 C118 C108 111.8(4) . . ? C120 C118 C108 112.2(4) . . ? C1 N1 C7 117.2(3) . . ? C2 N2 C5 104.0(3) . . ? C6 N3 C13 117.7(3) . . ? C31 N4 C37 118.4(3) . . ? C35 N5 C32 104.2(3) . . ? C36 N6 C43 116.8(3) . . ? C61 N7 C67 116.9(3) . . ? C65 N8 C62 103.8(2) . . ? C66 N9 C73 117.9(3) . . ? C91 N10 C97 117.2(3) . . ? C95 N11 C92 104.2(3) . . ? C96 N12 C103 118.3(3) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 24.61 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.445 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.059 #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 753231' #TrackingRef '- deposit.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70.50 H88 N6 Na2' _chemical_formula_weight 1065.45 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.205(2) _cell_length_b 12.304(3) _cell_length_c 24.047(5) _cell_angle_alpha 83.20(3) _cell_angle_beta 80.33(3) _cell_angle_gamma 80.59(3) _cell_volume 3210.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.258 _exptl_crystal_size_mid 0.182 _exptl_crystal_size_min 0.139 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1150 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26156 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12534 _reflns_number_gt 7886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.1101P)^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 12534 _refine_ls_number_parameters 725 _refine_ls_number_restraints 202 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1976 _refine_ls_wR_factor_gt 0.1774 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.472 _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 C1 C 1.0014(3) 0.4332(3) 0.09652(14) 0.0362(8) Uani 1 1 d D . . H1 H 0.9952 0.4380 0.0574 0.043 Uiso 1 1 calc R . . C2 C 0.9383(3) 0.5251(3) 0.12659(13) 0.0340(8) Uani 1 1 d D . . C3 C 0.8952(3) 0.6271(3) 0.09870(14) 0.0390(8) Uani 1 1 d D . . H3 H 0.8962 0.6439 0.0591 0.047 Uiso 1 1 calc R . . C4 C 0.8510(3) 0.6984(3) 0.14028(14) 0.0375(8) Uani 1 1 d D . . H4 H 0.8173 0.7743 0.1352 0.045 Uiso 1 1 calc R . . C5 C 0.8665(3) 0.6349(3) 0.19132(13) 0.0326(7) Uani 1 1 d D . . C6 C 0.8165(3) 0.6808(3) 0.24645(14) 0.0355(8) Uani 1 1 d D . . H6 H 0.7921 0.7586 0.2457 0.043 Uiso 1 1 calc R . . C7 C 1.1289(4) 0.2703(3) 0.07618(14) 0.0388(8) Uani 1 1 d . . . C8 C 1.0754(4) 0.1801(3) 0.06614(15) 0.0441(9) Uani 1 1 d . . . C9 C 1.1426(5) 0.1067(4) 0.02914(18) 0.0573(12) Uani 1 1 d . . . H9 H 1.1079 0.0453 0.0219 0.069 Uiso 1 1 calc R . . C10 C 1.2587(5) 0.1208(5) 0.00264(19) 0.0662(14) Uani 1 1 d . . . H10 H 1.3034 0.0694 -0.0225 0.079 Uiso 1 1 calc R . . C11 C 1.3101(5) 0.2102(4) 0.01283(18) 0.0593(12) Uani 1 1 d . . . H11 H 1.3903 0.2194 -0.0056 0.071 Uiso 1 1 calc R . . C12 C 1.2469(4) 0.2868(4) 0.04941(16) 0.0471(10) Uani 1 1 d . . . C13 C 0.7468(4) 0.6855(3) 0.34147(14) 0.0397(9) Uani 1 1 d . . . C14 C 0.8157(4) 0.6853(4) 0.38512(16) 0.0498(10) Uani 1 1 d . B . C15 C 0.7622(5) 0.7456(4) 0.43129(18) 0.0638(13) Uani 1 1 d . . . H15 H 0.8074 0.7473 0.4612 0.077 Uiso 1 1 calc R . . C16 C 0.6449(5) 0.8025(4) 0.43395(19) 0.0632(14) Uani 1 1 d . . . H16 H 0.6108 0.8447 0.4650 0.076 Uiso 1 1 calc R . . C17 C 0.5770(4) 0.7981(4) 0.39171(18) 0.0528(11) Uani 1 1 d . . . H17 H 0.4956 0.8360 0.3946 0.063 Uiso 1 1 calc R . . C18 C 0.6251(4) 0.7392(3) 0.34462(16) 0.0430(9) Uani 1 1 d . . . C19 C 1.3038(4) 0.3861(4) 0.05828(18) 0.0548(11) Uani 1 1 d . . . H19 H 1.2588 0.4156 0.0942 0.066 Uiso 1 1 calc R . . C20 C 1.4380(6) 0.3570(6) 0.0652(3) 0.098(2) Uani 1 1 d . . . H20A H 1.4471 0.2981 0.0961 0.148 Uiso 1 1 calc R . . H20B H 1.4678 0.4226 0.0741 0.148 Uiso 1 1 calc R . . H20C H 1.4857 0.3315 0.0299 0.148 Uiso 1 1 calc R . . C21 C 1.2881(6) 0.4774(5) 0.0113(3) 0.0811(16) Uani 1 1 d . . . H21A H 1.3253 0.5403 0.0183 0.122 Uiso 1 1 calc R . . H21B H 1.2007 0.5011 0.0099 0.122 Uiso 1 1 calc R . . H21C H 1.3281 0.4503 -0.0250 0.122 Uiso 1 1 calc R . . C22 C 0.9453(4) 0.1653(4) 0.09256(17) 0.0488(10) Uani 1 1 d . . . H22 H 0.9245 0.2049 0.1277 0.059 Uiso 1 1 calc R . . C23 C 0.9295(5) 0.0439(4) 0.1093(2) 0.0697(14) Uani 1 1 d . . . H23A H 0.8443 0.0393 0.1263 0.105 Uiso 1 1 calc R . . H23B H 0.9838 0.0117 0.1369 0.105 Uiso 1 1 calc R . . H23C H 0.9502 0.0030 0.0756 0.105 Uiso 1 1 calc R . . C24 C 0.8565(5) 0.2174(5) 0.0528(2) 0.0701(14) Uani 1 1 d . . . H24A H 0.7730 0.2077 0.0705 0.105 Uiso 1 1 calc R . . H24B H 0.8768 0.1819 0.0174 0.105 Uiso 1 1 calc R . . H24C H 0.8620 0.2966 0.0448 0.105 Uiso 1 1 calc R . . C25 C 0.9451(5) 0.6241(4) 0.38282(19) 0.0604(12) Uani 1 1 d D . . H25 H 0.9631 0.5715 0.3528 0.072 Uiso 1 1 calc R A 1 C26A C 1.0487(14) 0.7119(13) 0.3723(7) 0.091(5) Uiso 0.50 1 d P B 1 H26A H 1.0426 0.7578 0.3364 0.137 Uiso 0.50 1 calc PR B 1 H26B H 1.1311 0.6697 0.3710 0.137 Uiso 0.50 1 calc PR B 1 H26C H 1.0328 0.7595 0.4035 0.137 Uiso 0.50 1 calc PR B 1 C26B C 1.027(3) 0.677(3) 0.3458(14) 0.077(15) Uiso 0.25 1 d PD B 2 H26D H 0.9886 0.7115 0.3129 0.115 Uiso 0.25 1 calc PR B 2 H26E H 1.0984 0.6236 0.3332 0.115 Uiso 0.25 1 calc PR B 2 H26F H 1.0524 0.7342 0.3644 0.115 Uiso 0.25 1 calc PR B 2 C26C C 1.031(2) 0.692(3) 0.3532(13) 0.043(7) Uiso 0.25 1 d P B 3 H26G H 1.0018 0.7274 0.3183 0.064 Uiso 0.25 1 calc PR B 3 H26H H 1.1101 0.6458 0.3438 0.064 Uiso 0.25 1 calc PR B 3 H26I H 1.0391 0.7483 0.3771 0.064 Uiso 0.25 1 calc PR B 3 C27 C 0.9735(7) 0.5659(6) 0.4383(3) 0.097(2) Uani 1 1 d . B . H27A H 0.9133 0.5161 0.4532 0.146 Uiso 1 1 calc R . . H27B H 0.9702 0.6205 0.4653 0.146 Uiso 1 1 calc R . . H27C H 1.0556 0.5228 0.4329 0.146 Uiso 1 1 calc R . . C28 C 0.5434(4) 0.7336(4) 0.30120(19) 0.0497(10) Uani 1 1 d . . . H28 H 0.5858 0.6759 0.2757 0.060 Uiso 1 1 calc R . . C29 C 0.5208(5) 0.8431(4) 0.2643(2) 0.0684(13) Uani 1 1 d . . . H29A H 0.4682 0.8352 0.2367 0.103 Uiso 1 1 calc R . . H29B H 0.5992 0.8625 0.2441 0.103 Uiso 1 1 calc R . . H29C H 0.4807 0.9016 0.2883 0.103 Uiso 1 1 calc R . . C30 C 0.4187(5) 0.6995(4) 0.3286(2) 0.0693(14) Uani 1 1 d . . . H30A H 0.3694 0.6965 0.2990 0.104 Uiso 1 1 calc R . . H30B H 0.3758 0.7539 0.3545 0.104 Uiso 1 1 calc R . . H30C H 0.4318 0.6265 0.3497 0.104 Uiso 1 1 calc R . . C31 C 1.2840(3) 0.4710(3) 0.27226(15) 0.0380(8) Uani 1 1 d . . . H31 H 1.3424 0.5050 0.2858 0.046 Uiso 1 1 calc R . . C32 C 1.2102(3) 0.4056(3) 0.31430(15) 0.0379(8) Uani 1 1 d . . . C33 C 1.2470(4) 0.3631(4) 0.36595(17) 0.0519(11) Uani 1 1 d . . . H33 H 1.3170 0.3766 0.3800 0.062 Uiso 1 1 calc R . . C34 C 1.1613(4) 0.2975(4) 0.39271(16) 0.0523(11) Uani 1 1 d . . . H34 H 1.1617 0.2556 0.4285 0.063 Uiso 1 1 calc R . . C35 C 1.0743(4) 0.3051(3) 0.35673(14) 0.0388(8) Uani 1 1 d . . . C36 C 0.9629(4) 0.2563(3) 0.37175(15) 0.0394(8) Uani 1 1 d . . . H36 H 0.9563 0.2056 0.4047 0.047 Uiso 1 1 calc R . . C37 C 1.3705(3) 0.5521(3) 0.18727(15) 0.0375(8) Uani 1 1 d . . . C38 C 1.3295(4) 0.6525(4) 0.15717(16) 0.0446(9) Uani 1 1 d . . . C39 C 1.4171(4) 0.7161(4) 0.12844(19) 0.0583(12) Uani 1 1 d . . . H39 H 1.3913 0.7843 0.1079 0.070 Uiso 1 1 calc R . . C40 C 1.5404(4) 0.6819(4) 0.12927(19) 0.0592(12) Uani 1 1 d . . . H40 H 1.5985 0.7278 0.1108 0.071 Uiso 1 1 calc R . . C41 C 1.5790(4) 0.5813(4) 0.15691(17) 0.0482(10) Uani 1 1 d . . . H41 H 1.6642 0.5575 0.1563 0.058 Uiso 1 1 calc R . . C42 C 1.4965(3) 0.5135(3) 0.18582(15) 0.0401(8) Uani 1 1 d . . . C43 C 0.7663(3) 0.2257(3) 0.36680(15) 0.0375(8) Uani 1 1 d . . . C44 C 0.7477(4) 0.1314(3) 0.34346(17) 0.0453(9) Uani 1 1 d . D . C45 C 0.6394(5) 0.0892(4) 0.3632(2) 0.0639(13) Uani 1 1 d . . . H45 H 0.6248 0.0253 0.3482 0.077 Uiso 1 1 calc R . . C46 C 0.5528(5) 0.1377(5) 0.4038(3) 0.0743(16) Uani 1 1 d . . . H46 H 0.4786 0.1081 0.4161 0.089 Uiso 1 1 calc R . . C47 C 0.5730(5) 0.2281(4) 0.4266(2) 0.0670(14) Uani 1 1 d . . . H47 H 0.5133 0.2597 0.4554 0.080 Uiso 1 1 calc R . . C48 C 0.6793(4) 0.2753(3) 0.40836(17) 0.0493(10) Uani 1 1 d . . . C49 C 1.5477(4) 0.4019(3) 0.21279(18) 0.0472(9) Uani 1 1 d . . . H49 H 1.4792 0.3571 0.2243 0.057 Uiso 1 1 calc R . . C50 C 1.6466(5) 0.3386(5) 0.1715(2) 0.0719(14) Uani 1 1 d . . . H50A H 1.6775 0.2672 0.1904 0.108 Uiso 1 1 calc R . . H50B H 1.7140 0.3819 0.1591 0.108 Uiso 1 1 calc R . . H50C H 1.6114 0.3264 0.1385 0.108 Uiso 1 1 calc R . . C51 C 1.6018(5) 0.4147(5) 0.2665(2) 0.0641(13) Uani 1 1 d . . . H51A H 1.6338 0.3415 0.2832 0.096 Uiso 1 1 calc R . . H51B H 1.5375 0.4510 0.2940 0.096 Uiso 1 1 calc R . . H51C H 1.6681 0.4596 0.2561 0.096 Uiso 1 1 calc R . . C52 C 1.1950(4) 0.6948(4) 0.15797(19) 0.0523(10) Uani 1 1 d . . . H52 H 1.1502 0.6293 0.1654 0.063 Uiso 1 1 calc R . . C53 C 1.1656(5) 0.7568(5) 0.1021(2) 0.0735(15) Uani 1 1 d . . . H53A H 1.0773 0.7819 0.1052 0.110 Uiso 1 1 calc R . . H53B H 1.1911 0.7074 0.0717 0.110 Uiso 1 1 calc R . . H53C H 1.2094 0.8209 0.0933 0.110 Uiso 1 1 calc R . . C54 C 1.1486(6) 0.7674(7) 0.2062(3) 0.098(2) Uani 1 1 d . . . H54A H 1.0612 0.7943 0.2065 0.147 Uiso 1 1 calc R . . H54B H 1.1939 0.8305 0.2010 0.147 Uiso 1 1 calc R . . H54C H 1.1607 0.7242 0.2423 0.147 Uiso 1 1 calc R . . C55 C 0.8462(5) 0.0773(4) 0.29938(19) 0.0599(13) Uani 1 1 d . . . H55 H 0.8848 0.1379 0.2751 0.072 Uiso 1 1 calc R C 1 C56A C 0.9385(9) 0.0052(8) 0.3212(4) 0.059(2) Uiso 0.50 1 d P D 1 H56A H 0.9976 -0.0254 0.2901 0.089 Uiso 0.50 1 calc PR D 1 H56B H 0.9035 -0.0550 0.3456 0.089 Uiso 0.50 1 calc PR D 1 H56C H 0.9799 0.0449 0.3435 0.089 Uiso 0.50 1 calc PR D 1 C57A C 0.7804(10) 0.0152(9) 0.2586(4) 0.064(2) Uiso 0.50 1 d P D 1 H57A H 0.7149 0.0676 0.2437 0.096 Uiso 0.50 1 calc PR D 1 H57B H 0.7458 -0.0475 0.2806 0.096 Uiso 0.50 1 calc PR D 1 H57C H 0.8412 -0.0114 0.2270 0.096 Uiso 0.50 1 calc PR D 1 C56B C 0.8489(13) -0.0446(11) 0.2966(6) 0.086(3) Uiso 0.50 1 d P D 2 H56D H 0.8345 -0.0813 0.3350 0.130 Uiso 0.50 1 calc PR D 2 H56E H 0.9291 -0.0762 0.2773 0.130 Uiso 0.50 1 calc PR D 2 H56F H 0.7850 -0.0559 0.2755 0.130 Uiso 0.50 1 calc PR D 2 C57B C 0.8634(12) 0.1423(10) 0.2462(5) 0.079(3) Uiso 0.50 1 d P D 2 H57D H 0.8605 0.2199 0.2526 0.118 Uiso 0.50 1 calc PR D 2 H57E H 0.7985 0.1360 0.2246 0.118 Uiso 0.50 1 calc PR D 2 H57F H 0.9432 0.1155 0.2248 0.118 Uiso 0.50 1 calc PR D 2 C58 C 0.6968(5) 0.3774(4) 0.4344(2) 0.0638(14) Uani 1 1 d . . . H58 H 0.7729 0.4036 0.4129 0.077 Uiso 1 1 calc R . . C59 C 0.5926(7) 0.4707(5) 0.4285(2) 0.0851(19) Uani 1 1 d . . . H59A H 0.6073 0.5347 0.4457 0.128 Uiso 1 1 calc R . . H59B H 0.5157 0.4467 0.4478 0.128 Uiso 1 1 calc R . . H59C H 0.5871 0.4913 0.3883 0.128 Uiso 1 1 calc R . . C60 C 0.7152(7) 0.3518(6) 0.4957(3) 0.0900(19) Uani 1 1 d . . . H60A H 0.7268 0.4194 0.5107 0.135 Uiso 1 1 calc R . . H60B H 0.7878 0.2960 0.4984 0.135 Uiso 1 1 calc R . . H60C H 0.6432 0.3234 0.5178 0.135 Uiso 1 1 calc R . . C61 C 0.5296(9) 0.0375(8) 0.1226(4) 0.144(4) Uani 1 1 d U . . H61A H 0.6052 0.0514 0.1341 0.216 Uiso 1 1 calc R . . H61B H 0.5190 0.0791 0.0860 0.216 Uiso 1 1 calc R . . H61C H 0.5343 -0.0418 0.1192 0.216 Uiso 1 1 calc R . . C62 C 0.4227(6) 0.0737(4) 0.1663(3) 0.0769(16) Uani 1 1 d U . . C63 C 0.4337(8) 0.1204(5) 0.2172(4) 0.109(3) Uani 1 1 d U . . H63 H 0.5108 0.1327 0.2247 0.131 Uiso 1 1 calc R . . C64 C 0.3223(9) 0.1477(5) 0.2565(3) 0.095(2) Uani 1 1 d U . . H64 H 0.3254 0.1785 0.2906 0.114 Uiso 1 1 calc R . . C65 C 0.2156(8) 0.1295(6) 0.2446(4) 0.104(2) Uani 1 1 d U . . H65 H 0.1433 0.1468 0.2708 0.125 Uiso 1 1 calc R . . C66 C 0.2079(8) 0.0890(7) 0.1985(4) 0.109(2) Uani 1 1 d U . . H66 H 0.1303 0.0767 0.1917 0.130 Uiso 1 1 calc R . . C67 C 0.3066(7) 0.0639(6) 0.1600(3) 0.0889(18) Uani 1 1 d U . . H67 H 0.2949 0.0374 0.1261 0.107 Uiso 1 1 calc R . . N1 N 1.0648(3) 0.3459(3) 0.11634(12) 0.0374(7) Uani 1 1 d . . . N2 N 0.9200(3) 0.5289(2) 0.18471(11) 0.0319(6) Uani 1 1 d . . . N3 N 0.8037(3) 0.6249(2) 0.29445(12) 0.0367(7) Uani 1 1 d . . . N4 N 1.2799(3) 0.4887(3) 0.21904(12) 0.0359(7) Uani 1 1 d . . . N5 N 1.1030(3) 0.3712(2) 0.30751(11) 0.0329(6) Uani 1 1 d . . . N6 N 0.8728(3) 0.2762(2) 0.34409(12) 0.0359(7) Uani 1 1 d . . . Na1 Na 0.89365(14) 0.43972(11) 0.28177(6) 0.0394(4) Uani 1 1 d . . . Na2 Na 1.13129(15) 0.38088(15) 0.20209(6) 0.0503(4) Uani 1 1 d . . . C151 C 0.9161(11) 0.0004(15) 0.5001(7) 0.135(5) Uani 0.50 1 d PGDU E -1 H151 H 0.8295 0.0064 0.5078 0.162 Uiso 0.50 1 calc PR E -1 C152 C 0.9791(15) -0.0393(13) 0.4499(6) 0.188(7) Uani 0.50 1 d PGDU E -1 H152 H 0.9354 -0.0605 0.4233 0.226 Uiso 0.50 1 calc PR E -1 C153 C 1.1059(15) -0.0480(13) 0.4386(6) 0.211(7) Uani 0.50 1 d PGDU E -1 C154 C 1.1698(11) -0.0170(13) 0.4775(8) 0.163(6) Uani 0.50 1 d PGDU E -1 H154 H 1.2565 -0.0230 0.4698 0.195 Uiso 0.50 1 calc PR E -1 C155 C 1.1069(15) 0.0227(14) 0.5277(7) 0.160(6) Uani 0.50 1 d PGDU E -1 H155 H 1.1506 0.0439 0.5543 0.192 Uiso 0.50 1 calc PR E -1 C156 C 0.9801(15) 0.0315(15) 0.5390(6) 0.159(6) Uani 0.50 1 d PGDU E -1 H156 H 0.9371 0.0586 0.5732 0.191 Uiso 0.50 1 calc PR E -1 C157 C 1.1485(19) -0.0542(16) 0.4054(7) 0.266(10) Uani 0.50 1 d PGDU E -1 H15A H 1.2356 -0.0591 0.4080 0.400 Uiso 0.50 1 calc PR E -1 H15B H 1.1238 0.0106 0.3798 0.400 Uiso 0.50 1 calc PR E -1 H15C H 1.1344 -0.1213 0.3907 0.400 Uiso 0.50 1 calc PR E -1 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 C1 0.038(2) 0.045(2) 0.0271(16) -0.0046(15) -0.0045(14) -0.0110(17) C2 0.0309(19) 0.043(2) 0.0295(16) -0.0035(14) -0.0034(13) -0.0102(15) C3 0.039(2) 0.049(2) 0.0290(17) 0.0011(15) -0.0049(14) -0.0083(17) C4 0.037(2) 0.0357(19) 0.0390(18) 0.0029(15) -0.0054(15) -0.0085(15) C5 0.0343(19) 0.0340(18) 0.0307(16) -0.0022(14) -0.0041(14) -0.0103(15) C6 0.040(2) 0.0292(17) 0.0381(18) -0.0030(14) -0.0044(15) -0.0084(15) C7 0.046(2) 0.042(2) 0.0276(16) -0.0053(15) -0.0053(15) -0.0027(17) C8 0.055(3) 0.045(2) 0.0334(18) -0.0074(16) -0.0072(16) -0.0066(19) C9 0.072(3) 0.053(3) 0.048(2) -0.017(2) -0.003(2) -0.008(2) C10 0.075(4) 0.069(3) 0.049(2) -0.024(2) 0.009(2) 0.001(3) C11 0.052(3) 0.072(3) 0.049(2) -0.011(2) 0.008(2) -0.005(2) C12 0.051(3) 0.052(2) 0.0359(19) -0.0055(17) 0.0018(17) -0.0081(19) C13 0.053(2) 0.0318(18) 0.0328(17) -0.0026(14) -0.0003(16) -0.0094(17) C14 0.067(3) 0.047(2) 0.0343(19) -0.0054(17) -0.0071(18) -0.005(2) C15 0.090(4) 0.064(3) 0.038(2) -0.012(2) -0.008(2) -0.007(3) C16 0.087(4) 0.055(3) 0.044(2) -0.018(2) 0.015(2) -0.015(3) C17 0.058(3) 0.041(2) 0.055(2) -0.0091(19) 0.012(2) -0.013(2) C18 0.050(2) 0.0307(19) 0.046(2) -0.0032(16) 0.0043(17) -0.0114(17) C19 0.050(3) 0.070(3) 0.045(2) -0.012(2) 0.0069(18) -0.021(2) C20 0.081(4) 0.092(5) 0.135(6) 0.009(4) -0.047(4) -0.034(4) C21 0.086(4) 0.063(3) 0.099(4) 0.005(3) -0.022(3) -0.026(3) C22 0.054(3) 0.056(3) 0.041(2) -0.0144(18) -0.0039(18) -0.016(2) C23 0.081(4) 0.062(3) 0.071(3) -0.007(2) -0.006(3) -0.026(3) C24 0.061(3) 0.083(4) 0.068(3) -0.004(3) -0.016(2) -0.013(3) C25 0.079(3) 0.058(3) 0.045(2) -0.013(2) -0.024(2) 0.006(2) C27 0.089(5) 0.106(5) 0.094(4) 0.028(4) -0.038(4) -0.011(4) C28 0.046(2) 0.041(2) 0.063(3) -0.0106(19) -0.0040(19) -0.0075(18) C29 0.067(3) 0.058(3) 0.081(3) 0.006(3) -0.020(3) -0.009(2) C30 0.056(3) 0.059(3) 0.095(4) -0.012(3) -0.004(3) -0.017(2) C31 0.0306(19) 0.042(2) 0.045(2) -0.0070(16) -0.0058(15) -0.0128(16) C32 0.035(2) 0.044(2) 0.0379(18) -0.0054(15) -0.0062(15) -0.0125(16) C33 0.044(2) 0.075(3) 0.042(2) 0.002(2) -0.0148(17) -0.021(2) C34 0.050(3) 0.070(3) 0.0366(19) 0.0134(19) -0.0112(17) -0.018(2) C35 0.040(2) 0.043(2) 0.0328(17) 0.0029(15) -0.0022(15) -0.0114(16) C36 0.043(2) 0.040(2) 0.0342(17) 0.0044(15) 0.0007(15) -0.0138(17) C37 0.034(2) 0.043(2) 0.0384(18) -0.0008(15) -0.0056(15) -0.0158(16) C38 0.038(2) 0.052(2) 0.046(2) 0.0069(18) -0.0094(16) -0.0163(18) C39 0.048(3) 0.062(3) 0.064(3) 0.025(2) -0.014(2) -0.023(2) C40 0.041(3) 0.074(3) 0.061(3) 0.020(2) -0.006(2) -0.027(2) C41 0.031(2) 0.066(3) 0.047(2) 0.0017(19) -0.0028(16) -0.0141(19) C42 0.033(2) 0.049(2) 0.0404(19) -0.0016(16) -0.0066(15) -0.0133(17) C43 0.037(2) 0.0340(19) 0.0397(18) 0.0068(15) -0.0010(15) -0.0112(15) C44 0.049(2) 0.035(2) 0.051(2) 0.0022(17) -0.0014(18) -0.0145(17) C45 0.066(3) 0.051(3) 0.078(3) -0.003(2) 0.000(3) -0.032(2) C46 0.050(3) 0.070(3) 0.100(4) -0.001(3) 0.014(3) -0.032(3) C47 0.059(3) 0.058(3) 0.077(3) -0.007(2) 0.024(2) -0.022(2) C48 0.048(2) 0.044(2) 0.051(2) 0.0002(18) 0.0107(18) -0.0142(19) C49 0.036(2) 0.045(2) 0.062(2) -0.0045(19) -0.0058(18) -0.0095(17) C50 0.049(3) 0.071(3) 0.094(4) -0.022(3) -0.009(3) 0.003(2) C51 0.057(3) 0.068(3) 0.066(3) 0.009(2) -0.022(2) -0.001(2) C52 0.039(2) 0.051(2) 0.067(3) 0.009(2) -0.0130(19) -0.0127(19) C53 0.052(3) 0.082(4) 0.085(4) 0.018(3) -0.025(3) -0.010(3) C54 0.055(4) 0.135(6) 0.101(5) -0.038(4) -0.007(3) 0.008(4) C55 0.080(3) 0.038(2) 0.058(3) -0.0065(19) 0.015(2) -0.022(2) C58 0.072(3) 0.055(3) 0.059(3) -0.015(2) 0.024(2) -0.022(2) C59 0.132(6) 0.051(3) 0.063(3) -0.008(2) 0.003(3) -0.004(3) C60 0.109(5) 0.082(4) 0.083(4) -0.020(3) -0.020(3) -0.014(4) C61 0.117(6) 0.114(6) 0.160(7) 0.019(5) 0.053(5) 0.002(5) C62 0.081(4) 0.048(3) 0.089(4) 0.011(3) 0.003(3) 0.000(3) C63 0.118(6) 0.056(3) 0.163(7) 0.022(4) -0.050(5) -0.030(4) C64 0.144(7) 0.054(3) 0.087(4) -0.020(3) -0.009(4) -0.011(4) C65 0.109(6) 0.072(4) 0.126(6) -0.017(4) 0.002(5) -0.010(4) C66 0.099(5) 0.111(6) 0.106(5) -0.007(4) 0.001(4) -0.006(4) C67 0.093(5) 0.092(4) 0.074(4) -0.002(3) -0.009(3) 0.000(4) N1 0.0400(18) 0.0400(17) 0.0330(15) -0.0080(13) -0.0027(13) -0.0076(14) N2 0.0320(16) 0.0350(16) 0.0301(14) -0.0032(11) -0.0041(11) -0.0099(12) N3 0.0430(18) 0.0334(16) 0.0339(15) -0.0044(12) -0.0034(12) -0.0076(13) N4 0.0304(16) 0.0398(17) 0.0384(16) -0.0011(13) -0.0031(12) -0.0119(13) N5 0.0318(16) 0.0356(16) 0.0317(14) -0.0021(12) -0.0017(11) -0.0104(12) N6 0.0339(17) 0.0330(16) 0.0395(15) 0.0030(12) 0.0000(13) -0.0111(13) Na1 0.0416(8) 0.0325(7) 0.0407(7) 0.0032(6) -0.0015(6) -0.0049(6) Na2 0.0472(10) 0.0753(12) 0.0356(7) -0.0095(7) -0.0045(6) -0.0293(8) C151 0.179(10) 0.080(8) 0.153(9) 0.035(7) -0.056(7) -0.038(9) C152 0.222(10) 0.152(12) 0.205(11) -0.031(10) -0.052(9) -0.037(11) C153 0.225(10) 0.193(13) 0.213(11) -0.039(10) -0.019(8) -0.020(11) C154 0.189(10) 0.094(9) 0.195(10) 0.035(8) -0.027(7) -0.029(9) C155 0.178(9) 0.124(11) 0.189(10) 0.017(9) -0.044(9) -0.062(10) C156 0.176(9) 0.133(11) 0.178(10) 0.000(9) -0.047(8) -0.043(10) C157 0.276(13) 0.286(17) 0.227(11) -0.052(13) -0.005(10) -0.023(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 C1 N1 1.277(5) . ? C1 C2 1.435(5) . ? C1 Na2 3.086(4) . ? C2 N2 1.383(4) . ? C2 C3 1.404(5) . ? C3 C4 1.383(5) . ? C4 C5 1.395(5) . ? C5 N2 1.359(5) . ? C5 C6 1.488(5) . ? C5 Na1 3.056(4) . ? C6 N3 1.271(4) . ? C6 Na1 3.013(4) . ? C7 C12 1.406(6) . ? C7 C8 1.407(5) . ? C7 N1 1.440(5) . ? C8 C9 1.385(6) . ? C8 C22 1.520(6) . ? C9 C10 1.378(7) . ? C10 C11 1.386(7) . ? C11 C12 1.390(6) . ? C12 C19 1.519(6) . ? C13 C14 1.403(6) . ? C13 C18 1.409(6) . ? C13 N3 1.429(5) . ? C14 C15 1.403(6) . ? C14 C25 1.515(7) . ? C15 C16 1.380(8) . ? C16 C17 1.378(7) . ? C17 C18 1.400(6) . ? C18 C28 1.514(6) . ? C19 C21 1.508(7) . ? C19 C20 1.520(8) . ? C22 C24 1.510(7) . ? C22 C23 1.532(7) . ? C25 C26B 1.36(2) . ? C25 C26C 1.42(2) . ? C25 C27 1.497(7) . ? C25 C26A 1.681(16) . ? C28 C29 1.533(7) . ? C28 C30 1.542(6) . ? C31 N4 1.280(5) . ? C31 C32 1.448(5) . ? C31 Na2 3.006(4) . ? C32 N5 1.377(4) . ? C32 C33 1.390(5) . ? C32 Na2 3.040(4) . ? C33 C34 1.382(6) . ? C34 C35 1.394(6) . ? C35 N5 1.377(4) . ? C35 C36 1.446(5) . ? C35 Na1 3.084(4) . ? C36 N6 1.276(5) . ? C36 Na1 3.035(4) . ? C37 C38 1.405(6) . ? C37 C42 1.410(6) . ? C37 N4 1.443(4) . ? C38 C39 1.396(5) . ? C38 C52 1.510(6) . ? C39 C40 1.379(7) . ? C40 C41 1.374(7) . ? C41 C42 1.390(5) . ? C42 C49 1.513(6) . ? C43 C48 1.394(6) . ? C43 C44 1.406(5) . ? C43 N6 1.432(4) . ? C44 C45 1.386(6) . ? C44 C55 1.523(6) . ? C45 C46 1.372(7) . ? C46 C47 1.363(7) . ? C47 C48 1.392(6) . ? C48 C58 1.522(6) . ? C49 C50 1.534(7) . ? C49 C51 1.549(6) . ? C52 C54 1.518(8) . ? C52 C53 1.524(7) . ? C55 C56A 1.380(11) . ? C55 C57B 1.428(12) . ? C55 C56B 1.505(14) . ? C55 C57A 1.642(11) . ? C58 C59 1.509(8) . ? C58 C60 1.514(8) . ? C61 C62 1.499(9) . ? C62 C67 1.361(9) . ? C62 C63 1.445(10) . ? C63 C64 1.450(11) . ? C64 C65 1.335(11) . ? C65 C66 1.289(11) . ? C66 C67 1.336(10) . ? N1 Na2 2.413(3) . ? N2 Na1 2.451(3) . ? N2 Na2 2.800(4) . ? N3 Na1 2.369(3) . ? N4 Na2 2.404(3) . ? N5 Na2 2.492(3) . ? N5 Na1 2.513(3) . ? N6 Na1 2.382(3) . ? Na1 Na2 3.045(2) . ? C151 C152 1.3900 . ? C151 C156 1.3900 . ? C152 C153 1.3900 . ? C153 C157 0.8647 . ? C153 C154 1.3900 . ? C154 C155 1.3900 . ? C155 C156 1.3900 . ? 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 C1 C2 127.5(3) . . ? N1 C1 Na2 47.41(18) . . ? C2 C1 Na2 82.4(2) . . ? N2 C2 C3 111.5(3) . . ? N2 C2 C1 126.0(3) . . ? C3 C2 C1 122.4(3) . . ? C4 C3 C2 106.5(3) . . ? C3 C4 C5 105.2(3) . . ? N2 C5 C4 113.6(3) . . ? N2 C5 C6 125.5(3) . . ? C4 C5 C6 120.7(3) . . ? N2 C5 Na1 51.44(16) . . ? C4 C5 Na1 162.6(2) . . ? C6 C5 Na1 74.23(19) . . ? N3 C6 C5 125.6(3) . . ? N3 C6 Na1 48.40(19) . . ? C5 C6 Na1 77.4(2) . . ? C12 C7 C8 121.5(4) . . ? C12 C7 N1 118.3(3) . . ? C8 C7 N1 120.2(3) . . ? C9 C8 C7 118.2(4) . . ? C9 C8 C22 120.1(4) . . ? C7 C8 C22 121.6(3) . . ? C10 C9 C8 121.4(4) . . ? C9 C10 C11 119.8(4) . . ? C10 C11 C12 121.4(4) . . ? C11 C12 C7 117.8(4) . . ? C11 C12 C19 120.3(4) . . ? C7 C12 C19 121.9(4) . . ? C14 C13 C18 121.7(3) . . ? C14 C13 N3 117.1(4) . . ? C18 C13 N3 121.1(3) . . ? C15 C14 C13 118.0(4) . . ? C15 C14 C25 120.1(4) . . ? C13 C14 C25 121.8(4) . . ? C16 C15 C14 121.0(5) . . ? C17 C16 C15 120.1(4) . . ? C16 C17 C18 121.7(5) . . ? C17 C18 C13 117.4(4) . . ? C17 C18 C28 118.8(4) . . ? C13 C18 C28 123.8(3) . . ? C21 C19 C12 111.5(4) . . ? C21 C19 C20 110.2(4) . . ? C12 C19 C20 113.1(5) . . ? C24 C22 C8 110.4(4) . . ? C24 C22 C23 109.7(4) . . ? C8 C22 C23 113.0(4) . . ? C26B C25 C26C 11(2) . . ? C26B C25 C27 122.9(18) . . ? C26C C25 C27 116.4(14) . . ? C26B C25 C14 112.2(19) . . ? C26C C25 C14 110.7(12) . . ? C27 C25 C14 114.1(5) . . ? C26B C25 C26A 32.2(16) . . ? C26C C25 C26A 21.1(14) . . ? C27 C25 C26A 98.7(7) . . ? C14 C25 C26A 111.6(7) . . ? C18 C28 C29 112.5(4) . . ? C18 C28 C30 112.4(4) . . ? C29 C28 C30 108.7(4) . . ? N4 C31 C32 127.8(3) . . ? N4 C31 Na2 50.47(17) . . ? C32 C31 Na2 77.4(2) . . ? N5 C32 C33 112.0(3) . . ? N5 C32 C31 125.8(3) . . ? C33 C32 C31 122.1(3) . . ? N5 C32 Na2 53.97(17) . . ? C33 C32 Na2 152.6(3) . . ? C31 C32 Na2 74.9(2) . . ? C34 C33 C32 106.3(3) . . ? C33 C34 C35 106.3(3) . . ? N5 C35 C34 111.8(3) . . ? N5 C35 C36 124.5(3) . . ? C34 C35 C36 123.5(3) . . ? N5 C35 Na1 53.14(18) . . ? C34 C35 Na1 151.9(3) . . ? C36 C35 Na1 74.4(2) . . ? N6 C36 C35 125.0(3) . . ? N6 C36 Na1 48.16(18) . . ? C35 C36 Na1 78.2(2) . . ? C38 C37 C42 121.1(3) . . ? C38 C37 N4 118.1(3) . . ? C42 C37 N4 120.8(3) . . ? C39 C38 C37 118.0(4) . . ? C39 C38 C52 120.1(4) . . ? C37 C38 C52 121.8(3) . . ? C40 C39 C38 121.4(4) . . ? C41 C40 C39 119.8(4) . . ? C40 C41 C42 121.7(4) . . ? C41 C42 C37 117.9(4) . . ? C41 C42 C49 117.9(4) . . ? C37 C42 C49 124.1(3) . . ? C48 C43 C44 121.5(3) . . ? C48 C43 N6 119.6(3) . . ? C44 C43 N6 118.8(3) . . ? C45 C44 C43 117.7(4) . . ? C45 C44 C55 122.2(4) . . ? C43 C44 C55 120.1(3) . . ? C46 C45 C44 121.4(4) . . ? C47 C46 C45 120.2(4) . . ? C46 C47 C48 121.3(5) . . ? C47 C48 C43 117.9(4) . . ? C47 C48 C58 119.4(4) . . ? C43 C48 C58 122.7(4) . . ? C42 C49 C50 111.9(4) . . ? C42 C49 C51 111.0(4) . . ? C50 C49 C51 109.2(4) . . ? C38 C52 C54 110.0(4) . . ? C38 C52 C53 113.3(4) . . ? C54 C52 C53 110.4(5) . . ? C56A C55 C57B 123.8(8) . . ? C56A C55 C56B 62.0(7) . . ? C57B C55 C56B 115.9(8) . . ? C56A C55 C44 114.9(5) . . ? C57B C55 C44 114.2(6) . . ? C56B C55 C44 116.0(6) . . ? C56A C55 C57A 110.7(6) . . ? C57B C55 C57A 76.9(6) . . ? C56B C55 C57A 51.1(6) . . ? C44 C55 C57A 108.7(5) . . ? C59 C58 C60 110.5(4) . . ? C59 C58 C48 112.0(5) . . ? C60 C58 C48 112.1(4) . . ? C67 C62 C63 115.2(6) . . ? C67 C62 C61 121.1(7) . . ? C63 C62 C61 123.7(8) . . ? C62 C63 C64 117.3(7) . . ? C65 C64 C63 119.7(7) . . ? C66 C65 C64 121.8(8) . . ? C65 C66 C67 121.5(9) . . ? C66 C67 C62 124.4(7) . . ? C1 N1 C7 116.8(3) . . ? C1 N1 Na2 109.7(2) . . ? C7 N1 Na2 126.5(3) . . ? C5 N2 C2 103.2(3) . . ? C5 N2 Na1 102.9(2) . . ? C2 N2 Na1 151.7(2) . . ? C5 N2 Na2 141.9(2) . . ? C2 N2 Na2 94.9(2) . . ? Na1 N2 Na2 70.51(9) . . ? C6 N3 C13 116.0(3) . . ? C6 N3 Na1 107.9(2) . . ? C13 N3 Na1 136.0(2) . . ? C31 N4 C37 115.0(3) . . ? C31 N4 Na2 105.3(2) . . ? C37 N4 Na2 139.1(2) . . ? C35 N5 C32 103.6(3) . . ? C35 N5 Na2 144.3(2) . . ? C32 N5 Na2 99.5(2) . . ? C35 N5 Na1 100.9(2) . . ? C32 N5 Na1 143.0(2) . . ? Na2 N5 Na1 74.94(10) . . ? C36 N6 C43 117.7(3) . . ? C36 N6 Na1 108.3(2) . . ? C43 N6 Na1 130.2(2) . . ? N3 Na1 N6 129.42(12) . . ? N3 Na1 N2 77.65(11) . . ? N6 Na1 N2 148.89(12) . . ? N3 Na1 N5 119.51(12) . . ? N6 Na1 N5 74.44(11) . . ? N2 Na1 N5 107.71(11) . . ? N3 Na1 C6 23.65(9) . . ? N6 Na1 C6 151.80(12) . . ? N2 Na1 C6 54.03(10) . . ? N5 Na1 C6 121.18(11) . . ? N3 Na1 C36 128.01(11) . . ? N6 Na1 C36 23.53(10) . . ? N2 Na1 C36 151.87(12) . . ? N5 Na1 C36 52.51(10) . . ? C6 Na1 C36 150.31(11) . . ? N3 Na1 Na2 122.63(10) . . ? N6 Na1 Na2 104.47(10) . . ? N2 Na1 Na2 60.12(9) . . ? N5 Na1 Na2 52.23(7) . . ? C6 Na1 Na2 103.43(9) . . ? C36 Na1 Na2 92.95(9) . . ? N3 Na1 C5 51.97(10) . . ? N6 Na1 C5 165.94(12) . . ? N2 Na1 C5 25.69(9) . . ? N5 Na1 C5 118.11(11) . . ? C6 Na1 C5 28.38(9) . . ? C36 Na1 C5 170.34(11) . . ? Na2 Na1 C5 80.94(9) . . ? N3 Na1 C35 123.31(12) . . ? N6 Na1 C35 50.48(10) . . ? N2 Na1 C35 133.02(11) . . ? N5 Na1 C35 26.00(9) . . ? C6 Na1 C35 136.39(11) . . ? C36 Na1 C35 27.32(10) . . ? Na2 Na1 C35 74.24(8) . . ? C5 Na1 C35 143.04(11) . . ? N4 Na2 N1 132.28(12) . . ? N4 Na2 N5 77.21(10) . . ? N1 Na2 N5 150.05(11) . . ? N4 Na2 N2 107.04(12) . . ? N1 Na2 N2 70.69(11) . . ? N5 Na2 N2 98.30(11) . . ? N4 Na2 C31 24.24(10) . . ? N1 Na2 C31 156.38(12) . . ? N5 Na2 C31 53.47(10) . . ? N2 Na2 C31 111.88(11) . . ? N4 Na2 C32 51.94(10) . . ? N1 Na2 C32 175.14(12) . . ? N5 Na2 C32 26.55(9) . . ? N2 Na2 C32 111.29(11) . . ? C31 Na2 C32 27.72(10) . . ? N4 Na2 Na1 109.01(10) . . ? N1 Na2 Na1 103.97(10) . . ? N5 Na2 Na1 52.84(8) . . ? N2 Na2 Na1 49.37(7) . . ? C31 Na2 Na1 93.80(9) . . ? C32 Na2 Na1 75.06(9) . . ? N4 Na2 C1 121.92(11) . . ? N1 Na2 C1 22.93(10) . . ? N5 Na2 C1 145.13(12) . . ? N2 Na2 C1 50.22(10) . . ? C31 Na2 C1 143.82(12) . . ? C32 Na2 C1 160.50(13) . . ? Na1 Na2 C1 92.32(9) . . ? C152 C151 C156 120.0 . . ? C153 C152 C151 120.0 . . ? C157 C153 C152 124.3 . . ? C157 C153 C154 113.6 . . ? C152 C153 C154 120.0 . . ? C155 C154 C153 120.0 . . ? C154 C155 C156 120.0 . . ? C155 C156 C151 120.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.760 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.051