# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Xiao-Juan Yang' _publ_contact_author_email YANGXJ@LZB.AC.CN _publ_section_title ; Zinc Compounds With or Without Zn-Zn Bond: Alkali Metal Reduction of LZnCl2 (L = alpha-diimine ligands) ; loop_ _publ_author_name 'Xiao-Juan Yang' 'Yu-Heng Deng' 'Yanyan Liu' 'Biao Wu' 'Peiju Yang' ; Jie Yu ; 'Chunxi Zhang' # Attachment 'zn.cif' data_ZnNa _database_code_depnum_ccdc_archive 'CCDC 722598' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H102 N4 Na2 O3 Zn2' _chemical_formula_weight 1152.22 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3505(10) _cell_length_b 12.6247(10) _cell_length_c 12.8227(10) _cell_angle_alpha 75.6590(10) _cell_angle_beta 65.0610(10) _cell_angle_gamma 69.1820(10) _cell_volume 1683.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3466 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 24.73 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10300 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.33 _reflns_number_total 7554 _reflns_number_gt 5359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0643P)^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 7554 _refine_ls_number_parameters 340 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.047 _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 Zn Zn 0.44716(3) 0.09850(2) 0.50382(2) 0.04320(11) Uani 1 1 d . . . Na Na 0.50716(13) 0.23402(13) 0.61512(11) 0.0784(4) Uani 1 1 d . . . N1 N 0.48814(18) 0.24594(16) 0.42293(16) 0.0428(5) Uani 1 1 d . . . N2 N 0.31018(19) 0.19845(17) 0.62168(17) 0.0462(5) Uani 1 1 d . . . C1 C 0.3909(2) 0.3364(2) 0.4767(2) 0.0475(6) Uani 1 1 d . . . H1A H 0.3884 0.4155 0.4429 0.057 Uiso 1 1 calc R . . C2 C 0.3011(3) 0.3127(2) 0.5767(2) 0.0498(6) Uani 1 1 d . . . H2A H 0.2326 0.3741 0.6183 0.060 Uiso 1 1 calc R . . C3 C 0.5583(2) 0.2704(2) 0.3042(2) 0.0447(6) Uani 1 1 d . . . C4 C 0.6887(3) 0.2484(2) 0.2664(2) 0.0514(6) Uani 1 1 d . . . C5 C 0.7563(3) 0.2718(3) 0.1492(2) 0.0650(8) Uani 1 1 d . . . H5A H 0.8424 0.2553 0.1239 0.078 Uiso 1 1 calc R . . C6 C 0.6995(3) 0.3184(3) 0.0703(2) 0.0695(9) Uani 1 1 d . . . H6A H 0.7462 0.3351 -0.0073 0.083 Uiso 1 1 calc R . . C7 C 0.5730(3) 0.3401(3) 0.1070(2) 0.0635(8) Uani 1 1 d . . . H7A H 0.5346 0.3722 0.0533 0.076 Uiso 1 1 calc R . . C8 C 0.5001(3) 0.3155(2) 0.2225(2) 0.0524(7) Uani 1 1 d . . . C9 C 0.7525(3) 0.2042(3) 0.3534(3) 0.0661(8) Uani 1 1 d . . . H9A H 0.7104 0.1509 0.4124 0.079 Uiso 1 1 calc R . . C10 C 0.7338(4) 0.3024(4) 0.4143(3) 0.0945(12) Uani 1 1 d . . . H10A H 0.7739 0.2742 0.4697 0.142 Uiso 1 1 calc R . . H10B H 0.6464 0.3361 0.4534 0.142 Uiso 1 1 calc R . . H10C H 0.7695 0.3589 0.3582 0.142 Uiso 1 1 calc R . . C11 C 0.8906(3) 0.1395(4) 0.3029(4) 0.1045(14) Uani 1 1 d . . . H11A H 0.9004 0.0782 0.2650 0.157 Uiso 1 1 calc R . . H11B H 0.9225 0.1091 0.3641 0.157 Uiso 1 1 calc R . . H11C H 0.9357 0.1906 0.2479 0.157 Uiso 1 1 calc R . . C12 C 0.3625(3) 0.3345(3) 0.2541(3) 0.0637(8) Uani 1 1 d . . . H12A H 0.3283 0.3086 0.3369 0.076 Uiso 1 1 calc R . . C13 C 0.2921(4) 0.4601(4) 0.2374(4) 0.1125(15) Uani 1 1 d . . . H13A H 0.3090 0.5033 0.2777 0.169 Uiso 1 1 calc R . . H13B H 0.2042 0.4685 0.2677 0.169 Uiso 1 1 calc R . . H13C H 0.3185 0.4874 0.1564 0.169 Uiso 1 1 calc R . . C14 C 0.3386(4) 0.2624(4) 0.1906(4) 0.1065(14) Uani 1 1 d . . . H14A H 0.3825 0.1837 0.2040 0.160 Uiso 1 1 calc R . . H14B H 0.3675 0.2874 0.1091 0.160 Uiso 1 1 calc R . . H14C H 0.2509 0.2708 0.2189 0.160 Uiso 1 1 calc R . . C15 C 0.1962(3) 0.1770(2) 0.7037(2) 0.0508(6) Uani 1 1 d . . . C16 C 0.1835(3) 0.1362(2) 0.8196(2) 0.0583(7) Uani 1 1 d . . . C17 C 0.0692(4) 0.1174(3) 0.8974(3) 0.0774(10) Uani 1 1 d . . . H17A H 0.0601 0.0891 0.9739 0.093 Uiso 1 1 calc R . . C18 C -0.0281(3) 0.1392(3) 0.8644(3) 0.0860(11) Uani 1 1 d . . . H18A H -0.1032 0.1275 0.9182 0.103 Uiso 1 1 calc R . . C19 C -0.0151(3) 0.1787(3) 0.7510(3) 0.0811(10) Uani 1 1 d . . . H19A H -0.0820 0.1935 0.7285 0.097 Uiso 1 1 calc R . . C20 C 0.0965(3) 0.1971(3) 0.6692(3) 0.0622(8) Uani 1 1 d . . . C21 C 0.2882(3) 0.1123(3) 0.8608(2) 0.0720(9) Uani 1 1 d . . . H21A H 0.3435 0.1578 0.8067 0.086 Uiso 1 1 calc R . . C22 C 0.2465(5) 0.1457(4) 0.9820(4) 0.1257(17) Uani 1 1 d . . . H22A H 0.2001 0.2249 0.9838 0.189 Uiso 1 1 calc R . . H22B H 0.3184 0.1330 1.0001 0.189 Uiso 1 1 calc R . . H22C H 0.1949 0.1002 1.0380 0.189 Uiso 1 1 calc R . . C23 C 0.3635(4) -0.0102(4) 0.8567(4) 0.1187(16) Uani 1 1 d . . . H23A H 0.3900 -0.0308 0.7807 0.178 Uiso 1 1 calc R . . H23B H 0.3137 -0.0573 0.9125 0.178 Uiso 1 1 calc R . . H23C H 0.4353 -0.0212 0.8744 0.178 Uiso 1 1 calc R . . C24 C 0.1074(3) 0.2331(3) 0.5437(3) 0.0731(9) Uani 1 1 d . . . H24A H 0.1882 0.2486 0.5002 0.088 Uiso 1 1 calc R . . C25 C 0.0084(5) 0.3409(4) 0.5278(4) 0.1329(19) Uani 1 1 d . . . H25A H 0.0202 0.3597 0.4472 0.199 Uiso 1 1 calc R . . H25B H 0.0144 0.4022 0.5550 0.199 Uiso 1 1 calc R . . H25C H -0.0724 0.3293 0.5712 0.199 Uiso 1 1 calc R . . C26 C 0.1071(5) 0.1379(4) 0.4918(4) 0.1161(16) Uani 1 1 d . . . H26A H 0.1714 0.0703 0.5013 0.174 Uiso 1 1 calc R . . H26B H 0.1220 0.1602 0.4109 0.174 Uiso 1 1 calc R . . H26C H 0.0276 0.1226 0.5304 0.174 Uiso 1 1 calc R . . C27 C 0.6427(5) 0.1582(6) 0.8060(4) 0.134(2) Uani 1 1 d . . . H27A H 0.5946 0.1271 0.8818 0.161 Uiso 1 1 calc R . . H27B H 0.6983 0.1902 0.8153 0.161 Uiso 1 1 calc R . . C28 C 0.7155(5) 0.0673(5) 0.7306(5) 0.139(2) Uani 1 1 d . . . H28A H 0.7681 0.0076 0.7656 0.209 Uiso 1 1 calc R . . H28B H 0.7661 0.0975 0.6569 0.209 Uiso 1 1 calc R . . H28C H 0.6601 0.0372 0.7199 0.209 Uiso 1 1 calc R . . C29 C 0.4908(6) 0.3418(5) 0.8217(4) 0.136(2) Uani 1 1 d . . . H29A H 0.5474 0.3762 0.8262 0.163 Uiso 1 1 calc R . . H29B H 0.4415 0.3170 0.9000 0.163 Uiso 1 1 calc R . . C30 C 0.4094(6) 0.4257(4) 0.7672(5) 0.152(2) Uani 1 1 d . . . H30A H 0.3635 0.4895 0.8113 0.227 Uiso 1 1 calc R . . H30B H 0.3524 0.3921 0.7640 0.227 Uiso 1 1 calc R . . H30C H 0.4582 0.4510 0.6901 0.227 Uiso 1 1 calc R . . C32 C -0.0156(7) 0.5026(9) 0.1724(8) 0.223(4) Uani 1 1 d D . . H32A H 0.0236 0.5123 0.2187 0.335 Uiso 1 1 calc R . . H32B H -0.0180 0.4250 0.1864 0.335 Uiso 1 1 calc R . . H32C H -0.0990 0.5528 0.1925 0.335 Uiso 1 1 calc R . . O1 O 0.5617(3) 0.2444(2) 0.7574(2) 0.0831(7) Uani 1 1 d . . . O2 O 0.0000 0.5000 0.0000 0.301(7) Uani 1 2 d SD . . C31 C 0.0535(13) 0.5287(16) 0.0533(10) 0.52(2) Uani 1 1 d D . . H31B H 0.0480 0.6093 0.0347 0.622 Uiso 1 1 calc R . . H31A H 0.1405 0.4847 0.0328 0.622 Uiso 1 1 calc R . . 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 Zn 0.04575(19) 0.04192(17) 0.03616(16) -0.00470(11) -0.01030(12) -0.01169(12) Na 0.0905(9) 0.1039(10) 0.0589(7) -0.0133(7) -0.0381(7) -0.0327(8) N1 0.0461(12) 0.0430(11) 0.0339(10) -0.0029(8) -0.0088(9) -0.0150(9) N2 0.0455(12) 0.0450(12) 0.0363(10) -0.0065(9) -0.0047(9) -0.0110(9) C1 0.0585(16) 0.0402(13) 0.0398(13) -0.0035(10) -0.0139(12) -0.0155(12) C2 0.0518(16) 0.0457(14) 0.0432(14) -0.0111(11) -0.0107(12) -0.0085(12) C3 0.0544(16) 0.0405(13) 0.0359(12) -0.0038(10) -0.0115(11) -0.0166(11) C4 0.0505(16) 0.0503(15) 0.0474(15) -0.0032(12) -0.0117(12) -0.0170(12) C5 0.0556(18) 0.071(2) 0.0518(17) -0.0036(14) -0.0040(14) -0.0209(15) C6 0.076(2) 0.080(2) 0.0367(15) -0.0022(14) -0.0032(14) -0.0292(17) C7 0.079(2) 0.0695(19) 0.0404(15) 0.0014(13) -0.0202(15) -0.0263(16) C8 0.0593(17) 0.0552(16) 0.0400(13) -0.0052(11) -0.0158(12) -0.0164(13) C9 0.0558(18) 0.079(2) 0.0594(18) 0.0097(15) -0.0217(15) -0.0263(16) C10 0.108(3) 0.124(3) 0.078(2) 0.001(2) -0.046(2) -0.058(3) C11 0.062(2) 0.118(3) 0.110(3) 0.013(3) -0.032(2) -0.017(2) C12 0.0597(19) 0.082(2) 0.0489(16) -0.0001(14) -0.0239(14) -0.0198(16) C13 0.080(3) 0.098(3) 0.140(4) 0.003(3) -0.049(3) -0.005(2) C14 0.093(3) 0.150(4) 0.100(3) -0.031(3) -0.034(2) -0.052(3) C15 0.0493(16) 0.0483(15) 0.0407(13) -0.0101(11) -0.0020(11) -0.0123(12) C16 0.0630(19) 0.0561(16) 0.0425(14) -0.0070(12) -0.0042(13) -0.0198(14) C17 0.084(3) 0.076(2) 0.0461(17) -0.0041(15) 0.0047(16) -0.0311(19) C18 0.057(2) 0.091(3) 0.077(2) -0.0089(19) 0.0124(18) -0.0289(19) C19 0.0525(19) 0.088(2) 0.084(3) -0.004(2) -0.0106(17) -0.0205(18) C20 0.0529(18) 0.0617(18) 0.0595(18) -0.0059(14) -0.0104(14) -0.0156(14) C21 0.092(2) 0.085(2) 0.0398(15) 0.0064(15) -0.0150(15) -0.045(2) C22 0.162(5) 0.145(5) 0.082(3) -0.030(3) -0.054(3) -0.035(4) C23 0.113(4) 0.107(4) 0.148(4) -0.039(3) -0.071(3) -0.001(3) C24 0.062(2) 0.090(2) 0.065(2) 0.0021(17) -0.0229(16) -0.0278(18) C25 0.143(4) 0.114(4) 0.115(4) 0.009(3) -0.065(3) 0.000(3) C26 0.158(5) 0.126(4) 0.078(3) -0.008(3) -0.047(3) -0.053(3) C27 0.125(4) 0.207(6) 0.096(3) -0.003(4) -0.069(3) -0.052(4) C28 0.130(4) 0.138(5) 0.141(5) 0.010(4) -0.073(4) -0.018(4) C29 0.208(6) 0.150(5) 0.095(3) -0.038(3) -0.061(4) -0.082(5) C30 0.222(7) 0.085(3) 0.170(6) -0.042(4) -0.092(5) -0.027(4) C32 0.115(6) 0.302(13) 0.240(10) -0.102(9) -0.025(6) -0.048(6) O1 0.1086(19) 0.1057(19) 0.0608(14) -0.0046(13) -0.0421(14) -0.0501(16) O2 0.144(9) 0.397(18) 0.391(17) -0.083(12) -0.075(10) -0.115(11) C31 0.179(13) 0.37(2) 0.90(6) 0.21(3) -0.177(19) -0.175(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 Zn N2 2.0024(19) . ? Zn N1 2.0167(19) . ? Zn Zn 2.3673(6) 2_656 ? Zn Na 2.9181(13) . ? Na O1 2.241(2) . ? Na N1 2.536(2) . ? Na C1 2.565(3) . ? Na N2 2.591(3) . ? Na C2 2.593(3) . ? Na C30 3.064(5) . ? Na C10 3.123(4) . ? N1 C1 1.392(3) . ? N1 C3 1.417(3) . ? N2 C2 1.398(3) . ? N2 C15 1.429(3) . ? C1 C2 1.345(3) . ? C1 H1A 0.9800 . ? C2 H2A 0.9800 . ? C3 C8 1.410(4) . ? C3 C4 1.413(4) . ? C4 C5 1.392(4) . ? C4 C9 1.517(4) . ? C5 C6 1.369(4) . ? C5 H5A 0.9300 . ? C6 C7 1.370(4) . ? C6 H6A 0.9300 . ? C7 C8 1.395(4) . ? C7 H7A 0.9300 . ? C8 C12 1.512(4) . ? C9 C10 1.525(5) . ? C9 C11 1.529(5) . ? C9 H9A 0.9800 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.525(5) . ? C12 C14 1.529(5) . ? C12 H12A 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.401(4) . ? C15 C16 1.406(4) . ? C16 C17 1.406(4) . ? C16 C21 1.505(4) . ? C17 C18 1.354(5) . ? C17 H17A 0.9300 . ? C18 C19 1.376(5) . ? C18 H18A 0.9300 . ? C19 C20 1.392(4) . ? C19 H19A 0.9300 . ? C20 C24 1.520(4) . ? C21 C23 1.495(5) . ? C21 C22 1.535(5) . ? C21 H21A 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.509(5) . ? C24 C26 1.514(6) . ? C24 H24A 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O1 1.410(5) . ? C27 C28 1.464(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O1 1.445(5) . ? C29 C30 1.446(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C32 C31 1.421(9) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? O2 C31 1.307(9) . ? O2 C31 1.307(9) 2_565 ? C31 H31B 0.9700 . ? C31 H31A 0.9700 . ? 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 N2 Zn N1 83.35(8) . . ? N2 Zn Zn 137.12(6) . 2_656 ? N1 Zn Zn 136.26(6) . 2_656 ? N2 Zn Na 60.17(7) . . ? N1 Zn Na 58.49(6) . . ? Zn Zn Na 120.01(3) 2_656 . ? O1 Na N1 165.62(10) . . ? O1 Na C1 148.08(11) . . ? N1 Na C1 31.68(7) . . ? O1 Na N2 131.08(10) . . ? N1 Na N2 62.82(7) . . ? C1 Na N2 54.38(8) . . ? O1 Na C2 133.92(11) . . ? N1 Na C2 54.58(8) . . ? C1 Na C2 30.23(8) . . ? N2 Na C2 31.29(7) . . ? O1 Na Zn 148.39(9) . . ? N1 Na Zn 42.69(5) . . ? C1 Na Zn 60.96(6) . . ? N2 Na Zn 42.10(5) . . ? C2 Na Zn 60.57(6) . . ? O1 Na C30 50.49(13) . . ? N1 Na C30 127.84(14) . . ? C1 Na C30 98.09(14) . . ? N2 Na C30 105.29(14) . . ? C2 Na C30 88.24(14) . . ? Zn Na C30 146.95(14) . . ? O1 Na C10 95.17(10) . . ? N1 Na C10 70.70(8) . . ? C1 Na C10 84.48(10) . . ? N2 Na C10 133.46(9) . . ? C2 Na C10 114.43(10) . . ? Zn Na C10 102.05(8) . . ? C30 Na C10 100.77(15) . . ? C1 N1 C3 116.23(19) . . ? C1 N1 Zn 108.93(15) . . ? C3 N1 Zn 127.40(15) . . ? C1 N1 Na 75.32(13) . . ? C3 N1 Na 136.81(16) . . ? Zn N1 Na 78.83(7) . . ? C2 N2 C15 115.0(2) . . ? C2 N2 Zn 109.19(15) . . ? C15 N2 Zn 127.49(17) . . ? C2 N2 Na 74.44(15) . . ? C15 N2 Na 140.11(17) . . ? Zn N2 Na 77.72(7) . . ? C2 C1 N1 118.4(2) . . ? C2 C1 Na 76.02(16) . . ? N1 C1 Na 73.01(14) . . ? C2 C1 H1A 120.8 . . ? N1 C1 H1A 120.8 . . ? Na C1 H1A 120.8 . . ? C1 C2 N2 118.4(2) . . ? C1 C2 Na 73.74(16) . . ? N2 C2 Na 74.28(14) . . ? C1 C2 H2A 120.8 . . ? N2 C2 H2A 120.8 . . ? Na C2 H2A 120.8 . . ? C8 C3 C4 119.2(2) . . ? C8 C3 N1 121.0(2) . . ? C4 C3 N1 119.8(2) . . ? C5 C4 C3 119.1(3) . . ? C5 C4 C9 120.8(3) . . ? C3 C4 C9 120.0(2) . . ? C6 C5 C4 121.8(3) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C5 C6 C7 119.1(3) . . ? C5 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 . . ? C6 C7 C8 122.1(3) . . ? C6 C7 H7A 119.0 . . ? C8 C7 H7A 119.0 . . ? C7 C8 C3 118.7(3) . . ? C7 C8 C12 118.6(2) . . ? C3 C8 C12 122.7(2) . . ? C4 C9 C10 109.6(3) . . ? C4 C9 C11 114.5(3) . . ? C10 C9 C11 110.8(3) . . ? C4 C9 H9A 107.2 . . ? C10 C9 H9A 107.2 . . ? C11 C9 H9A 107.2 . . ? C9 C10 Na 88.5(2) . . ? C9 C10 H10A 109.5 . . ? Na C10 H10A 84.8 . . ? C9 C10 H10B 109.5 . . ? Na C10 H10B 41.2 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? Na C10 H10C 150.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 C13 112.7(3) . . ? C8 C12 C14 112.1(3) . . ? C13 C12 C14 111.2(3) . . ? C8 C12 H12A 106.8 . . ? C13 C12 H12A 106.8 . . ? C14 C12 H12A 106.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 119.7(3) . . ? C20 C15 N2 120.1(2) . . ? C16 C15 N2 120.2(3) . . ? C17 C16 C15 118.2(3) . . ? C17 C16 C21 120.1(3) . . ? C15 C16 C21 121.8(3) . . ? C18 C17 C16 122.1(3) . . ? C18 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? C17 C18 C19 119.5(3) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C18 C19 C20 121.2(4) . . ? C18 C19 H19A 119.4 . . ? C20 C19 H19A 119.4 . . ? C19 C20 C15 119.3(3) . . ? C19 C20 C24 118.4(3) . . ? C15 C20 C24 122.2(3) . . ? C23 C21 C16 111.2(3) . . ? C23 C21 C22 109.6(3) . . ? C16 C21 C22 114.3(3) . . ? C23 C21 H21A 107.1 . . ? C16 C21 H21A 107.1 . . ? C22 C21 H21A 107.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 110.4(4) . . ? C25 C24 C20 113.2(3) . . ? C26 C24 C20 111.2(3) . . ? C25 C24 H24A 107.3 . . ? C26 C24 H24A 107.3 . . ? C20 C24 H24A 107.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C27 C28 109.9(4) . . ? O1 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? O1 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1 C29 C30 111.0(4) . . ? 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 . . ? C29 C30 Na 80.7(3) . . ? C29 C30 H30A 109.5 . . ? Na C30 H30A 168.1 . . ? C29 C30 H30B 109.5 . . ? Na C30 H30B 60.1 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? Na C30 H30C 71.4 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 O1 C29 114.4(4) . . ? C27 O1 Na 127.6(3) . . ? C29 O1 Na 117.1(3) . . ? C31 O2 C31 180.0(7) . 2_565 ? O2 C31 C32 103.5(7) . . ? O2 C31 H31B 111.1 . . ? C32 C31 H31B 111.1 . . ? O2 C31 H31A 111.1 . . ? C32 C31 H31A 111.1 . . ? H31B C31 H31A 109.0 . . ? 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 N2 Zn Na O1 94.12(19) . . . . ? N1 Zn Na O1 -164.6(2) . . . . ? Zn Zn Na O1 -36.00(19) 2_656 . . . ? N2 Zn Na N1 -101.24(10) . . . . ? Zn Zn Na N1 128.64(7) 2_656 . . . ? N2 Zn Na C1 -67.72(9) . . . . ? N1 Zn Na C1 33.52(9) . . . . ? Zn Zn Na C1 162.16(7) 2_656 . . . ? N1 Zn Na N2 101.24(10) . . . . ? Zn Zn Na N2 -130.12(7) 2_656 . . . ? N2 Zn Na C2 -32.95(9) . . . . ? N1 Zn Na C2 68.29(9) . . . . ? Zn Zn Na C2 -163.06(7) 2_656 . . . ? N2 Zn Na C30 -11.6(2) . . . . ? N1 Zn Na C30 89.6(2) . . . . ? Zn Zn Na C30 -141.8(2) 2_656 . . . ? N2 Zn Na C10 -144.36(11) . . . . ? N1 Zn Na C10 -43.12(10) . . . . ? Zn Zn Na C10 85.52(9) 2_656 . . . ? N2 Zn N1 C1 -11.12(16) . . . . ? Zn Zn N1 C1 -172.07(13) 2_656 . . . ? Na Zn N1 C1 -70.07(15) . . . . ? N2 Zn N1 C3 -159.4(2) . . . . ? Zn Zn N1 C3 39.7(2) 2_656 . . . ? Na Zn N1 C3 141.7(2) . . . . ? N2 Zn N1 Na 58.94(8) . . . . ? Zn Zn N1 Na -102.00(7) 2_656 . . . ? O1 Na N1 C1 -100.8(5) . . . . ? N2 Na N1 C1 65.51(14) . . . . ? C2 Na N1 C1 29.97(14) . . . . ? Zn Na N1 C1 113.18(15) . . . . ? C30 Na N1 C1 -23.1(2) . . . . ? C10 Na N1 C1 -111.91(16) . . . . ? O1 Na N1 C3 12.1(6) . . . . ? C1 Na N1 C3 112.9(3) . . . . ? N2 Na N1 C3 178.4(2) . . . . ? C2 Na N1 C3 142.8(2) . . . . ? Zn Na N1 C3 -134.0(2) . . . . ? C30 Na N1 C3 89.7(3) . . . . ? C10 Na N1 C3 0.9(2) . . . . ? O1 Na N1 Zn 146.0(4) . . . . ? C1 Na N1 Zn -113.18(15) . . . . ? N2 Na N1 Zn -47.67(6) . . . . ? C2 Na N1 Zn -83.21(9) . . . . ? C30 Na N1 Zn -136.32(17) . . . . ? C10 Na N1 Zn 134.91(11) . . . . ? N1 Zn N2 C2 11.17(17) . . . . ? Zn Zn N2 C2 171.79(13) 2_656 . . . ? Na Zn N2 C2 68.50(16) . . . . ? N1 Zn N2 C15 157.3(2) . . . . ? Zn Zn N2 C15 -42.1(3) 2_656 . . . ? Na Zn N2 C15 -145.4(2) . . . . ? N1 Zn N2 Na -57.34(7) . . . . ? Zn Zn N2 Na 103.29(8) 2_656 . . . ? O1 Na N2 C2 109.72(18) . . . . ? N1 Na N2 C2 -65.81(14) . . . . ? C1 Na N2 C2 -29.81(13) . . . . ? Zn Na N2 C2 -114.19(15) . . . . ? C30 Na N2 C2 59.26(18) . . . . ? C10 Na N2 C2 -62.5(2) . . . . ? O1 Na N2 C15 -0.8(3) . . . . ? N1 Na N2 C15 -176.3(3) . . . . ? C1 Na N2 C15 -140.3(3) . . . . ? C2 Na N2 C15 -110.5(3) . . . . ? Zn Na N2 C15 135.3(3) . . . . ? C30 Na N2 C15 -51.2(3) . . . . ? C10 Na N2 C15 -173.0(2) . . . . ? O1 Na N2 Zn -136.09(13) . . . . ? N1 Na N2 Zn 48.38(6) . . . . ? C1 Na N2 Zn 84.38(9) . . . . ? C2 Na N2 Zn 114.19(15) . . . . ? C30 Na N2 Zn 173.45(13) . . . . ? C10 Na N2 Zn 51.72(15) . . . . ? C3 N1 C1 C2 161.6(2) . . . . ? Zn N1 C1 C2 9.3(3) . . . . ? Na N1 C1 C2 -63.1(2) . . . . ? C3 N1 C1 Na -135.3(2) . . . . ? Zn N1 C1 Na 72.44(10) . . . . ? O1 Na C1 C2 -81.4(3) . . . . ? N1 Na C1 C2 126.1(2) . . . . ? N2 Na C1 C2 30.84(14) . . . . ? Zn Na C1 C2 80.59(15) . . . . ? C30 Na C1 C2 -72.2(2) . . . . ? C10 Na C1 C2 -172.33(17) . . . . ? O1 Na C1 N1 152.5(2) . . . . ? N2 Na C1 N1 -95.22(14) . . . . ? C2 Na C1 N1 -126.1(2) . . . . ? Zn Na C1 N1 -45.47(11) . . . . ? C30 Na C1 N1 161.73(18) . . . . ? C10 Na C1 N1 61.61(15) . . . . ? N1 C1 C2 N2 0.1(4) . . . . ? Na C1 C2 N2 -61.4(2) . . . . ? N1 C1 C2 Na 61.5(2) . . . . ? C15 N2 C2 C1 -160.4(3) . . . . ? Zn N2 C2 C1 -9.6(3) . . . . ? Na N2 C2 C1 61.1(2) . . . . ? C15 N2 C2 Na 138.5(2) . . . . ? Zn N2 C2 Na -70.69(11) . . . . ? O1 Na C2 C1 133.47(18) . . . . ? N1 Na C2 C1 -31.40(14) . . . . ? N2 Na C2 C1 -126.6(2) . . . . ? Zn Na C2 C1 -82.02(15) . . . . ? C30 Na C2 C1 109.42(19) . . . . ? C10 Na C2 C1 8.38(19) . . . . ? O1 Na C2 N2 -99.90(18) . . . . ? N1 Na C2 N2 95.23(14) . . . . ? C1 Na C2 N2 126.6(2) . . . . ? Zn Na C2 N2 44.61(11) . . . . ? C30 Na C2 N2 -123.96(18) . . . . ? C10 Na C2 N2 135.01(15) . . . . ? C1 N1 C3 C8 -56.8(3) . . . . ? Zn N1 C3 C8 89.5(3) . . . . ? Na N1 C3 C8 -153.2(2) . . . . ? C1 N1 C3 C4 123.8(3) . . . . ? Zn N1 C3 C4 -89.9(3) . . . . ? Na N1 C3 C4 27.4(3) . . . . ? C8 C3 C4 C5 -0.1(4) . . . . ? N1 C3 C4 C5 179.3(2) . . . . ? C8 C3 C4 C9 177.6(3) . . . . ? N1 C3 C4 C9 -3.0(4) . . . . ? C3 C4 C5 C6 1.8(4) . . . . ? C9 C4 C5 C6 -175.9(3) . . . . ? C4 C5 C6 C7 -1.6(5) . . . . ? C5 C6 C7 C8 -0.4(5) . . . . ? C6 C7 C8 C3 2.1(4) . . . . ? C6 C7 C8 C12 -175.8(3) . . . . ? C4 C3 C8 C7 -1.8(4) . . . . ? N1 C3 C8 C7 178.8(2) . . . . ? C4 C3 C8 C12 176.0(3) . . . . ? N1 C3 C8 C12 -3.4(4) . . . . ? C5 C4 C9 C10 99.2(3) . . . . ? C3 C4 C9 C10 -78.5(3) . . . . ? C5 C4 C9 C11 -26.0(4) . . . . ? C3 C4 C9 C11 156.3(3) . . . . ? C4 C9 C10 Na 95.8(2) . . . . ? C11 C9 C10 Na -136.9(2) . . . . ? O1 Na C10 C9 133.9(2) . . . . ? N1 Na C10 C9 -48.88(19) . . . . ? C1 Na C10 C9 -78.2(2) . . . . ? N2 Na C10 C9 -52.0(3) . . . . ? C2 Na C10 C9 -82.4(2) . . . . ? Zn Na C10 C9 -19.5(2) . . . . ? C30 Na C10 C9 -175.4(2) . . . . ? C7 C8 C12 C13 -66.3(4) . . . . ? C3 C8 C12 C13 116.0(3) . . . . ? C7 C8 C12 C14 60.2(4) . . . . ? C3 C8 C12 C14 -117.6(3) . . . . ? C2 N2 C15 C20 64.7(3) . . . . ? Zn N2 C15 C20 -79.8(3) . . . . ? Na N2 C15 C20 160.2(2) . . . . ? C2 N2 C15 C16 -115.1(3) . . . . ? Zn N2 C15 C16 100.4(3) . . . . ? Na N2 C15 C16 -19.6(4) . . . . ? C20 C15 C16 C17 -0.4(4) . . . . ? N2 C15 C16 C17 179.4(3) . . . . ? C20 C15 C16 C21 179.4(3) . . . . ? N2 C15 C16 C21 -0.8(4) . . . . ? C15 C16 C17 C18 -1.2(5) . . . . ? C21 C16 C17 C18 179.1(3) . . . . ? C16 C17 C18 C19 1.4(6) . . . . ? C17 C18 C19 C20 -0.2(6) . . . . ? C18 C19 C20 C15 -1.3(5) . . . . ? C18 C19 C20 C24 175.9(3) . . . . ? C16 C15 C20 C19 1.6(4) . . . . ? N2 C15 C20 C19 -178.2(3) . . . . ? C16 C15 C20 C24 -175.6(3) . . . . ? N2 C15 C20 C24 4.6(4) . . . . ? C17 C16 C21 C23 85.9(4) . . . . ? C15 C16 C21 C23 -93.9(4) . . . . ? C17 C16 C21 C22 -38.9(4) . . . . ? C15 C16 C21 C22 141.3(3) . . . . ? C19 C20 C24 C25 56.9(5) . . . . ? C15 C20 C24 C25 -125.9(4) . . . . ? C19 C20 C24 C26 -68.0(4) . . . . ? C15 C20 C24 C26 109.2(4) . . . . ? O1 C29 C30 Na 6.5(4) . . . . ? O1 Na C30 C29 -5.1(3) . . . . ? N1 Na C30 C29 -166.7(3) . . . . ? C1 Na C30 C29 -178.8(4) . . . . ? N2 Na C30 C29 126.1(4) . . . . ? C2 Na C30 C29 152.6(4) . . . . ? Zn Na C30 C29 134.1(3) . . . . ? C10 Na C30 C29 -92.9(4) . . . . ? C28 C27 O1 C29 -176.4(5) . . . . ? C28 C27 O1 Na 15.4(6) . . . . ? C30 C29 O1 C27 -179.4(5) . . . . ? C30 C29 O1 Na -9.9(6) . . . . ? N1 Na O1 C27 -97.2(5) . . . . ? C1 Na O1 C27 -174.6(3) . . . . ? N2 Na O1 C27 99.0(4) . . . . ? C2 Na O1 C27 141.7(3) . . . . ? Zn Na O1 C27 36.5(4) . . . . ? C30 Na O1 C27 173.6(4) . . . . ? C10 Na O1 C27 -86.7(4) . . . . ? N1 Na O1 C29 94.8(5) . . . . ? C1 Na O1 C29 17.5(4) . . . . ? N2 Na O1 C29 -69.0(3) . . . . ? C2 Na O1 C29 -26.3(4) . . . . ? Zn Na O1 C29 -131.5(3) . . . . ? C30 Na O1 C29 5.6(3) . . . . ? C10 Na O1 C29 105.3(3) . . . . ? C31 O2 C31 C32 0.0(14) 2_565 . . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.449 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.049 ###### data_ZnK _database_code_depnum_ccdc_archive 'CCDC 722599' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H128 K2 N6 O2 Zn2' _chemical_formula_weight 1486.88 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' K K 0.2009 0.2494 '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 P2(1)/n 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 12.913(3) _cell_length_b 13.519(3) _cell_length_c 25.206(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.80(3) _cell_angle_gamma 90.00 _cell_volume 4395.0(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1161 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24381 _diffrn_reflns_av_R_equivalents 0.1278 _diffrn_reflns_av_sigmaI/netI 0.2296 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.47 _reflns_number_total 9022 _reflns_number_gt 3005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0657P)^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 9022 _refine_ls_number_parameters 442 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2036 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 0.818 _refine_ls_restrained_S_all 0.819 _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 Zn1 Zn -0.11978(4) 0.39459(4) 0.60885(2) 0.0455(2) Uani 1 1 d . . . K1 K -0.08436(11) 0.32457(11) 0.74981(5) 0.0859(5) Uani 1 1 d . . . N1 N -0.1850(3) 0.2818(3) 0.64251(16) 0.0481(11) Uani 1 1 d . . . N2 N -0.1832(3) 0.4769(3) 0.66235(15) 0.0471(11) Uani 1 1 d . . . N3 N -0.0302(3) 0.4074(3) 0.55373(15) 0.0482(11) Uani 1 1 d . . . C1 C -0.2604(4) 0.3215(4) 0.67546(19) 0.0529(15) Uani 1 1 d . . . H1A H -0.3217 0.2823 0.6832 0.063 Uiso 1 1 calc R . . C2 C -0.2586(4) 0.4189(4) 0.68572(19) 0.0499(14) Uani 1 1 d . . . H2A H -0.3160 0.4502 0.7034 0.060 Uiso 1 1 calc R . . C3 C -0.2098(4) 0.1899(4) 0.6186(2) 0.0474(14) Uani 1 1 d . . . C4 C -0.3002(5) 0.1787(4) 0.5848(2) 0.0565(15) Uani 1 1 d . . . C5 C -0.3250(5) 0.0856(5) 0.5634(2) 0.0788(19) Uani 1 1 d . . . H5A H -0.3849 0.0778 0.5418 0.095 Uiso 1 1 calc R . . C6 C -0.2618(6) 0.0062(5) 0.5738(3) 0.083(2) Uani 1 1 d . . . H6A H -0.2799 -0.0556 0.5601 0.099 Uiso 1 1 calc R . . C7 C -0.1717(5) 0.0173(5) 0.6045(3) 0.0713(19) Uani 1 1 d . . . H7A H -0.1280 -0.0367 0.6099 0.086 Uiso 1 1 calc R . . C8 C -0.1444(4) 0.1074(5) 0.6275(2) 0.0569(15) Uani 1 1 d . . . C9 C -0.3698(5) 0.2652(4) 0.5687(2) 0.0679(17) Uani 1 1 d . . . H9A H -0.3456 0.3217 0.5904 0.081 Uiso 1 1 calc R . . C10 C -0.4836(5) 0.2508(6) 0.5798(3) 0.130(3) Uani 1 1 d . . . H10A H -0.4896 0.2333 0.6165 0.195 Uiso 1 1 calc R . . H10B H -0.5122 0.1989 0.5576 0.195 Uiso 1 1 calc R . . H10C H -0.5208 0.3111 0.5724 0.195 Uiso 1 1 calc R . . C11 C -0.3555(5) 0.2942(5) 0.5106(3) 0.109(2) Uani 1 1 d . . . H11A H -0.2834 0.3057 0.5055 0.163 Uiso 1 1 calc R . . H11B H -0.3942 0.3534 0.5024 0.163 Uiso 1 1 calc R . . H11C H -0.3801 0.2416 0.4877 0.163 Uiso 1 1 calc R . . C12 C -0.0485(4) 0.1137(4) 0.6643(2) 0.0665(16) Uani 1 1 d . . . H12A H -0.0319 0.1841 0.6684 0.080 Uiso 1 1 calc R . . C13 C -0.0720(5) 0.0756(5) 0.7190(3) 0.120(3) Uani 1 1 d . . . H13A H -0.1328 0.1080 0.7309 0.181 Uiso 1 1 calc R . . H13B H -0.0143 0.0891 0.7434 0.181 Uiso 1 1 calc R . . H13C H -0.0839 0.0055 0.7173 0.181 Uiso 1 1 calc R . . C14 C 0.0470(5) 0.0643(5) 0.6447(3) 0.125(3) Uani 1 1 d . . . H14A H 0.1035 0.0729 0.6705 0.187 Uiso 1 1 calc R . . H14B H 0.0645 0.0935 0.6116 0.187 Uiso 1 1 calc R . . H14C H 0.0337 -0.0050 0.6396 0.187 Uiso 1 1 calc R . . C15 C -0.2019(4) 0.5810(4) 0.6633(2) 0.0493(14) Uani 1 1 d . . . C16 C -0.1383(4) 0.6427(4) 0.6956(2) 0.0540(15) Uani 1 1 d . . . C17 C -0.1581(5) 0.7435(5) 0.6966(2) 0.0725(19) Uani 1 1 d . . . H17A H -0.1170 0.7840 0.7188 0.087 Uiso 1 1 calc R . . C18 C -0.2354(6) 0.7841(5) 0.6662(3) 0.080(2) Uani 1 1 d . . . H18A H -0.2454 0.8522 0.6665 0.096 Uiso 1 1 calc R . . C19 C -0.2993(6) 0.7254(5) 0.6350(3) 0.082(2) Uani 1 1 d . . . H19A H -0.3548 0.7538 0.6156 0.099 Uiso 1 1 calc R . . C20 C -0.2828(5) 0.6232(4) 0.6315(2) 0.0592(16) Uani 1 1 d . . . C21 C -0.0535(5) 0.5973(4) 0.7304(2) 0.0699(17) Uani 1 1 d . . . H21A H -0.0270 0.5403 0.7113 0.084 Uiso 1 1 calc R . . C22 C 0.0392(5) 0.6666(6) 0.7435(3) 0.124(3) Uani 1 1 d . . . H22A H 0.0681 0.6884 0.7111 0.187 Uiso 1 1 calc R . . H22B H 0.0912 0.6316 0.7646 0.187 Uiso 1 1 calc R . . H22C H 0.0162 0.7228 0.7630 0.187 Uiso 1 1 calc R . . C23 C -0.0972(5) 0.5584(4) 0.7815(2) 0.091(2) Uani 1 1 d . . . H23A H -0.0424 0.5293 0.8033 0.137 Uiso 1 1 calc R . . H23B H -0.1492 0.5094 0.7730 0.137 Uiso 1 1 calc R . . H23C H -0.1275 0.6120 0.8003 0.137 Uiso 1 1 calc R . . C24 C -0.3506(5) 0.5608(5) 0.5947(2) 0.0735(18) Uani 1 1 d . . . H24A H -0.3236 0.4931 0.5970 0.088 Uiso 1 1 calc R . . C25 C -0.4632(5) 0.5569(6) 0.6103(3) 0.117(3) Uani 1 1 d . . . H25A H -0.4660 0.5322 0.6459 0.176 Uiso 1 1 calc R . . H25B H -0.5019 0.5138 0.5864 0.176 Uiso 1 1 calc R . . H25C H -0.4925 0.6221 0.6084 0.176 Uiso 1 1 calc R . . C26 C -0.3434(5) 0.5948(5) 0.5362(2) 0.103(2) Uani 1 1 d . . . H26A H -0.2721 0.5954 0.5271 0.154 Uiso 1 1 calc R . . H26B H -0.3718 0.6601 0.5322 0.154 Uiso 1 1 calc R . . H26C H -0.3817 0.5499 0.5132 0.154 Uiso 1 1 calc R . . C27 C -0.0342(3) 0.4872(4) 0.51842(19) 0.0457(13) Uani 1 1 d . . . H27A H -0.0915 0.5284 0.5205 0.055 Uiso 1 1 calc R . . C28 C 0.0538(4) 0.3400(4) 0.5485(2) 0.0487(14) Uani 1 1 d . . . C29 C 0.1424(4) 0.3507(4) 0.5830(2) 0.0612(17) Uani 1 1 d . . . C30 C 0.2204(5) 0.2804(5) 0.5796(3) 0.088(2) Uani 1 1 d . . . H30A H 0.2794 0.2849 0.6022 0.105 Uiso 1 1 calc R . . C31 C 0.2120(5) 0.2054(5) 0.5440(3) 0.088(2) Uani 1 1 d . . . H31A H 0.2651 0.1591 0.5431 0.105 Uiso 1 1 calc R . . C32 C 0.1271(6) 0.1955(4) 0.5089(3) 0.080(2) Uani 1 1 d . . . H32A H 0.1241 0.1446 0.4840 0.096 Uiso 1 1 calc R . . C33 C 0.0464(5) 0.2626(4) 0.5114(2) 0.0596(16) Uani 1 1 d . . . C34 C 0.1557(5) 0.4344(5) 0.6214(3) 0.080(2) Uani 1 1 d . . . H34A H 0.0931 0.4751 0.6171 0.096 Uiso 1 1 calc R . . C35 C 0.2445(7) 0.4991(7) 0.6090(3) 0.173(4) Uani 1 1 d . . . H35A H 0.2492 0.5529 0.6338 0.259 Uiso 1 1 calc R . . H35B H 0.2341 0.5248 0.5736 0.259 Uiso 1 1 calc R . . H35C H 0.3076 0.4614 0.6115 0.259 Uiso 1 1 calc R . . C36 C 0.1629(7) 0.4012(6) 0.6778(3) 0.169(4) Uani 1 1 d . . . H36A H 0.1041 0.3605 0.6847 0.253 Uiso 1 1 calc R . . H36B H 0.1639 0.4578 0.7007 0.253 Uiso 1 1 calc R . . H36C H 0.2254 0.3637 0.6842 0.253 Uiso 1 1 calc R . . C37 C -0.0478(5) 0.2517(5) 0.4728(2) 0.0740(18) Uani 1 1 d . . . H37A H -0.0989 0.3015 0.4821 0.089 Uiso 1 1 calc R . . C38 C -0.0977(5) 0.1516(5) 0.4766(3) 0.107(2) Uani 1 1 d . . . H38A H -0.1163 0.1402 0.5125 0.160 Uiso 1 1 calc R . . H38B H -0.0498 0.1015 0.4665 0.160 Uiso 1 1 calc R . . H38C H -0.1588 0.1491 0.4534 0.160 Uiso 1 1 calc R . . C39 C -0.0195(5) 0.2707(5) 0.4135(3) 0.105(2) Uani 1 1 d . . . H39A H 0.0109 0.3352 0.4106 0.158 Uiso 1 1 calc R . . H39B H -0.0813 0.2670 0.3907 0.158 Uiso 1 1 calc R . . H39C H 0.0290 0.2216 0.4029 0.158 Uiso 1 1 calc R . . C40 C 0.0559(9) 0.3870(11) 0.8766(6) 0.219(7) Uani 1 1 d . . . H40A H 0.0655 0.3404 0.9056 0.263 Uiso 1 1 calc R . . H40B H -0.0144 0.4124 0.8760 0.263 Uiso 1 1 calc R . . C41 C 0.1327(10) 0.4685(9) 0.8815(6) 0.320(10) Uani 1 1 d . . . H41A H 0.1240 0.5037 0.9140 0.481 Uiso 1 1 calc R . . H41B H 0.1223 0.5130 0.8520 0.481 Uiso 1 1 calc R . . H41C H 0.2015 0.4416 0.8815 0.481 Uiso 1 1 calc R . . C42 C 0.1720(10) 0.2899(10) 0.8277(6) 0.235(7) Uani 1 1 d D . . H42A H 0.2278 0.3347 0.8196 0.282 Uiso 1 1 calc R . . H42B H 0.1873 0.2621 0.8627 0.282 Uiso 1 1 calc R . . C43 C 0.1645(10) 0.2090(10) 0.7874(5) 0.250(7) Uani 1 1 d D . . H43A H 0.2273 0.1708 0.7893 0.375 Uiso 1 1 calc R . . H43B H 0.1545 0.2371 0.7526 0.375 Uiso 1 1 calc R . . H43C H 0.1068 0.1669 0.7945 0.375 Uiso 1 1 calc R . . O1 O 0.0773(6) 0.3422(6) 0.8274(3) 0.152(3) 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 Zn1 0.0504(4) 0.0475(4) 0.0401(4) 0.0053(3) 0.0166(3) 0.0043(4) K1 0.0851(10) 0.1032(12) 0.0686(10) -0.0095(9) -0.0059(8) 0.0183(9) N1 0.061(3) 0.038(3) 0.047(3) 0.000(2) 0.015(2) 0.001(2) N2 0.059(3) 0.038(3) 0.046(3) -0.001(2) 0.018(2) 0.001(2) N3 0.054(3) 0.041(3) 0.051(3) 0.019(2) 0.023(2) 0.011(2) C1 0.057(4) 0.062(4) 0.041(4) 0.000(3) 0.014(3) -0.002(3) C2 0.055(4) 0.051(4) 0.045(4) -0.003(3) 0.012(3) 0.007(3) C3 0.045(4) 0.054(4) 0.044(4) 0.007(3) 0.012(3) -0.005(3) C4 0.075(4) 0.047(4) 0.049(4) -0.008(3) 0.019(3) -0.002(4) C5 0.074(5) 0.087(5) 0.076(5) -0.016(4) 0.016(4) -0.009(4) C6 0.098(6) 0.053(5) 0.100(6) -0.017(4) 0.030(5) -0.021(4) C7 0.066(5) 0.061(5) 0.089(5) 0.010(4) 0.029(4) 0.006(4) C8 0.071(4) 0.042(3) 0.061(4) 0.008(4) 0.030(3) -0.002(4) C9 0.071(5) 0.075(4) 0.056(4) 0.003(3) -0.003(3) 0.007(4) C10 0.067(5) 0.161(7) 0.164(8) 0.053(6) 0.029(5) 0.023(5) C11 0.106(6) 0.118(6) 0.103(6) 0.021(5) 0.008(5) 0.022(5) C12 0.067(4) 0.065(4) 0.068(4) 0.011(4) 0.010(3) 0.013(4) C13 0.125(6) 0.165(8) 0.071(5) 0.047(5) 0.001(4) -0.024(6) C14 0.081(5) 0.138(7) 0.157(8) -0.026(6) 0.024(5) 0.029(5) C15 0.062(4) 0.050(4) 0.038(3) 0.004(3) 0.025(3) 0.004(3) C16 0.071(4) 0.051(4) 0.041(4) -0.002(3) 0.019(3) 0.002(3) C17 0.102(6) 0.062(5) 0.055(5) 0.002(4) 0.019(4) -0.002(4) C18 0.131(7) 0.047(4) 0.067(5) 0.004(4) 0.048(5) -0.003(5) C19 0.104(6) 0.064(5) 0.083(5) 0.023(4) 0.034(4) 0.033(4) C20 0.068(4) 0.059(4) 0.051(4) 0.001(3) 0.011(3) 0.012(4) C21 0.079(4) 0.061(4) 0.069(5) -0.013(4) 0.008(4) 0.001(4) C22 0.111(6) 0.142(7) 0.118(7) -0.008(6) -0.016(5) -0.040(6) C23 0.129(6) 0.081(5) 0.063(5) 0.003(4) -0.006(4) 0.018(4) C24 0.082(5) 0.077(4) 0.060(5) 0.018(4) -0.006(4) 0.024(4) C25 0.077(5) 0.176(8) 0.099(6) 0.011(5) 0.012(4) -0.003(5) C26 0.103(5) 0.125(6) 0.080(5) 0.003(5) -0.004(4) 0.006(5) C27 0.035(3) 0.048(3) 0.056(4) 0.000(3) 0.015(2) 0.011(3) C28 0.058(4) 0.044(3) 0.046(4) 0.011(3) 0.023(3) 0.010(3) C29 0.045(4) 0.068(4) 0.072(5) 0.020(4) 0.017(3) 0.018(3) C30 0.073(5) 0.101(6) 0.091(6) 0.004(5) 0.017(4) 0.001(5) C31 0.072(5) 0.086(6) 0.106(6) 0.023(5) 0.015(5) 0.036(4) C32 0.087(5) 0.065(5) 0.091(6) -0.017(4) 0.030(4) 0.017(4) C33 0.064(4) 0.057(4) 0.061(4) 0.002(3) 0.025(3) 0.009(3) C34 0.051(4) 0.097(5) 0.092(6) -0.025(5) 0.009(4) 0.001(4) C35 0.159(9) 0.187(9) 0.177(10) -0.081(8) 0.050(7) -0.075(8) C36 0.223(11) 0.220(10) 0.065(6) -0.012(7) 0.019(6) 0.018(8) C37 0.078(5) 0.083(5) 0.063(5) -0.024(4) 0.023(4) 0.006(4) C38 0.111(6) 0.114(6) 0.097(6) -0.013(5) 0.022(5) -0.037(5) C39 0.124(6) 0.110(6) 0.082(6) 0.009(4) 0.005(5) -0.010(5) C40 0.157(11) 0.234(16) 0.261(16) 0.179(14) -0.040(13) -0.002(11) C41 0.229(14) 0.182(12) 0.53(3) 0.067(15) -0.215(16) -0.068(11) C42 0.147(11) 0.218(16) 0.33(2) 0.023(12) -0.117(12) 0.059(10) C43 0.220(15) 0.245(18) 0.28(2) 0.058(13) 0.011(13) 0.068(13) O1 0.141(6) 0.180(6) 0.131(6) 0.012(5) -0.034(5) 0.009(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 Zn1 N3 1.859(4) . ? Zn1 N1 1.955(4) . ? Zn1 N2 1.959(4) . ? Zn1 K1 3.6836(17) . ? K1 O1 2.799(7) . ? K1 C1 2.875(5) . ? K1 C2 2.990(5) . ? K1 N1 2.999(4) . ? K1 N2 3.234(4) . ? K1 C23 3.267(6) . ? K1 C18 3.267(6) 2_446 ? N1 C3 1.411(6) . ? N1 C1 1.415(6) . ? N2 C2 1.402(6) . ? N2 C15 1.428(6) . ? N3 C27 1.398(5) . ? N3 C28 1.428(6) . ? C1 C2 1.342(6) . ? C1 H1A 0.9800 . ? C2 H2A 0.9800 . ? C3 C8 1.410(7) . ? C3 C4 1.419(7) . ? C4 C5 1.400(7) . ? C4 C9 1.519(7) . ? C5 C6 1.366(8) . ? C5 H5A 0.9300 . ? C6 C7 1.373(8) . ? C6 H6A 0.9300 . ? C7 C8 1.387(7) . ? C7 H7A 0.9300 . ? C8 C12 1.514(7) . ? C9 C10 1.522(8) . ? C9 C11 1.535(7) . ? C9 H9A 0.9800 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.506(7) . ? C12 C13 1.517(7) . ? C12 H12A 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.402(7) . ? C15 C20 1.407(7) . ? C16 C17 1.387(7) . ? C16 C21 1.501(7) . ? C17 C18 1.345(8) . ? C17 H17A 0.9300 . ? C18 C19 1.367(8) . ? C18 K1 3.267(6) 2_456 ? C18 H18A 0.9300 . ? C19 C20 1.401(7) . ? C19 H19A 0.9300 . ? C20 C24 1.504(7) . ? C21 C23 1.524(7) . ? C21 C22 1.543(8) . ? C21 H21A 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.525(8) . ? C24 C26 1.551(7) . ? C24 H24A 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C27 1.357(8) 3_566 ? C27 H27A 0.9300 . ? C28 C33 1.404(7) . ? C28 C29 1.411(7) . ? C29 C30 1.392(8) . ? C29 C34 1.491(8) . ? C30 C31 1.356(8) . ? C30 H30A 0.9300 . ? C31 C32 1.381(8) . ? C31 H31A 0.9300 . ? C32 C33 1.385(7) . ? C32 H32A 0.9300 . ? C33 C37 1.527(8) . ? C34 C36 1.489(8) . ? C34 C35 1.488(8) . ? C34 H34A 0.9800 . ? 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 1.505(7) . ? C37 C39 1.577(7) . ? C37 H37A 0.9800 . ? 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 O1 1.420(15) . ? C40 C41 1.484(13) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.493(8) . ? C42 O1 1.412(12) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? 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 Zn1 N1 133.96(17) . . ? N3 Zn1 N2 139.27(17) . . ? N1 Zn1 N2 86.62(17) . . ? N3 Zn1 K1 133.82(13) . . ? N1 Zn1 K1 54.34(13) . . ? N2 Zn1 K1 61.21(12) . . ? O1 K1 C1 174.5(2) . . ? O1 K1 C2 148.9(2) . . ? C1 K1 C2 26.36(12) . . ? O1 K1 N1 157.17(19) . . ? C1 K1 N1 27.78(11) . . ? C2 K1 N1 46.64(12) . . ? O1 K1 N2 132.67(18) . . ? C1 K1 N2 44.91(13) . . ? C2 K1 N2 25.66(10) . . ? N1 K1 N2 50.86(10) . . ? O1 K1 C23 78.0(2) . . ? C1 K1 C23 97.21(16) . . ? C2 K1 C23 70.95(15) . . ? N1 K1 C23 112.45(14) . . ? N2 K1 C23 61.77(13) . . ? O1 K1 C18 95.3(2) . 2_446 ? C1 K1 C18 81.61(19) . 2_446 ? C2 K1 C18 83.13(19) . 2_446 ? N1 K1 C18 105.11(18) . 2_446 ? N2 K1 C18 106.17(17) . 2_446 ? C23 K1 C18 87.58(16) . 2_446 ? O1 K1 Zn1 134.81(17) . . ? C1 K1 Zn1 47.01(10) . . ? C2 K1 Zn1 46.74(10) . . ? N1 K1 Zn1 31.98(7) . . ? N2 K1 Zn1 32.06(7) . . ? C23 K1 Zn1 88.94(11) . . ? C18 K1 Zn1 127.51(17) 2_446 . ? C3 N1 C1 115.8(4) . . ? C3 N1 Zn1 126.5(3) . . ? C1 N1 Zn1 106.4(3) . . ? C3 N1 K1 129.4(3) . . ? C1 N1 K1 71.2(3) . . ? Zn1 N1 K1 93.68(15) . . ? C2 N2 C15 115.0(4) . . ? C2 N2 Zn1 107.0(3) . . ? C15 N2 Zn1 130.5(3) . . ? C2 N2 K1 67.4(3) . . ? C15 N2 K1 132.6(3) . . ? Zn1 N2 K1 86.73(14) . . ? C27 N3 C28 116.0(4) . . ? C27 N3 Zn1 122.9(3) . . ? C28 N3 Zn1 120.8(3) . . ? C2 C1 N1 118.6(5) . . ? C2 C1 K1 81.6(3) . . ? N1 C1 K1 81.0(3) . . ? C2 C1 H1A 119.9 . . ? N1 C1 H1A 119.9 . . ? K1 C1 H1A 119.9 . . ? C1 C2 N2 118.3(5) . . ? C1 C2 K1 72.0(3) . . ? N2 C2 K1 86.9(3) . . ? C1 C2 H2A 120.3 . . ? N2 C2 H2A 120.3 . . ? K1 C2 H2A 120.3 . . ? C8 C3 N1 120.5(5) . . ? C8 C3 C4 118.6(5) . . ? N1 C3 C4 120.9(5) . . ? C5 C4 C3 119.6(6) . . ? C5 C4 C9 117.9(6) . . ? C3 C4 C9 122.5(5) . . ? C6 C5 C4 120.6(6) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C5 C6 C7 120.2(6) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C7 C8 121.5(6) . . ? C6 C7 H7A 119.2 . . ? C8 C7 H7A 119.2 . . ? C7 C8 C3 119.4(6) . . ? C7 C8 C12 119.3(6) . . ? C3 C8 C12 121.2(5) . . ? C4 C9 C10 114.6(5) . . ? C4 C9 C11 110.8(5) . . ? C10 C9 C11 111.8(5) . . ? C4 C9 H9A 106.4 . . ? C10 C9 H9A 106.4 . . ? C11 C9 H9A 106.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C8 115.7(5) . . ? C14 C12 C13 110.5(6) . . ? C8 C12 C13 110.1(5) . . ? C14 C12 H12A 106.7 . . ? C8 C12 H12A 106.7 . . ? C13 C12 H12A 106.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 119.1(5) . . ? C16 C15 N2 120.1(5) . . ? C20 C15 N2 120.8(5) . . ? C17 C16 C15 119.5(6) . . ? C17 C16 C21 121.4(6) . . ? C15 C16 C21 119.1(5) . . ? C18 C17 C16 121.5(7) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C17 C18 C19 120.2(6) . . ? C17 C18 K1 103.4(4) . 2_456 ? C19 C18 K1 92.4(4) . 2_456 ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? K1 C18 H18A 74.1 2_456 . ? C18 C19 C20 121.2(7) . . ? C18 C19 H19A 119.4 . . ? C20 C19 H19A 119.4 . . ? C19 C20 C15 118.4(6) . . ? C19 C20 C24 120.4(6) . . ? C15 C20 C24 121.2(5) . . ? C16 C21 C23 110.2(5) . . ? C16 C21 C22 114.4(5) . . ? C23 C21 C22 110.1(5) . . ? C16 C21 H21A 107.3 . . ? C23 C21 H21A 107.3 . . ? C22 C21 H21A 107.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 K1 95.9(4) . . ? C21 C23 H23A 109.5 . . ? K1 C23 H23A 72.5 . . ? C21 C23 H23B 109.5 . . ? K1 C23 H23B 47.2 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? K1 C23 H23C 151.4 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 C25 113.2(5) . . ? C20 C24 C26 111.1(5) . . ? C25 C24 C26 111.0(5) . . ? C20 C24 H24A 107.1 . . ? C25 C24 H24A 107.1 . . ? C26 C24 H24A 107.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 C27 N3 128.9(6) 3_566 . ? C27 C27 H27A 115.5 3_566 . ? N3 C27 H27A 115.5 . . ? C33 C28 C29 121.0(5) . . ? C33 C28 N3 120.7(5) . . ? C29 C28 N3 118.3(5) . . ? C30 C29 C28 117.4(6) . . ? C30 C29 C34 119.8(6) . . ? C28 C29 C34 122.8(5) . . ? C31 C30 C29 121.1(7) . . ? C31 C30 H30A 119.5 . . ? C29 C30 H30A 119.5 . . ? C30 C31 C32 122.2(7) . . ? C30 C31 H31A 118.9 . . ? C32 C31 H31A 118.9 . . ? C31 C32 C33 118.9(6) . . ? C31 C32 H32A 120.6 . . ? C33 C32 H32A 120.6 . . ? C32 C33 C28 119.5(6) . . ? C32 C33 C37 119.0(6) . . ? C28 C33 C37 121.5(5) . . ? C36 C34 C35 111.4(7) . . ? C36 C34 C29 112.9(6) . . ? C35 C34 C29 112.1(6) . . ? C36 C34 H34A 106.7 . . ? C35 C34 H34A 106.7 . . ? C29 C34 H34A 106.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C33 112.1(5) . . ? C38 C37 C39 109.1(5) . . ? C33 C37 C39 112.0(5) . . ? C38 C37 H37A 107.8 . . ? C33 C37 H37A 107.8 . . ? C39 C37 H37A 107.8 . . ? 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 . . ? O1 C40 C41 103.4(13) . . ? O1 C40 H40A 111.1 . . ? C41 C40 H40A 111.1 . . ? O1 C40 H40B 111.1 . . ? C41 C40 H40B 111.1 . . ? H40A C40 H40B 109.0 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 O1 109.5(11) . . ? C43 C42 H42A 109.8 . . ? O1 C42 H42A 109.8 . . ? C43 C42 H42B 109.8 . . ? O1 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 O1 C42 114.4(10) . . ? C40 O1 K1 118.4(7) . . ? C42 O1 K1 125.3(7) . . ? 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 N3 Zn1 K1 O1 29.8(3) . . . . ? N1 Zn1 K1 O1 149.5(3) . . . . ? N2 Zn1 K1 O1 -102.3(3) . . . . ? N3 Zn1 K1 C1 -157.5(2) . . . . ? N1 Zn1 K1 C1 -37.75(19) . . . . ? N2 Zn1 K1 C1 70.4(2) . . . . ? N3 Zn1 K1 C2 166.1(2) . . . . ? N1 Zn1 K1 C2 -74.16(19) . . . . ? N2 Zn1 K1 C2 33.98(17) . . . . ? N3 Zn1 K1 N1 -119.7(2) . . . . ? N2 Zn1 K1 N1 108.1(2) . . . . ? N3 Zn1 K1 N2 132.2(2) . . . . ? N1 Zn1 K1 N2 -108.1(2) . . . . ? N3 Zn1 K1 C23 101.7(2) . . . . ? N1 Zn1 K1 C23 -138.63(19) . . . . ? N2 Zn1 K1 C23 -30.49(18) . . . . ? N3 Zn1 K1 C18 -172.2(2) . . . 2_446 ? N1 Zn1 K1 C18 -52.5(2) . . . 2_446 ? N2 Zn1 K1 C18 55.6(2) . . . 2_446 ? N3 Zn1 N1 C3 -27.5(5) . . . . ? N2 Zn1 N1 C3 156.5(4) . . . . ? K1 Zn1 N1 C3 -146.9(5) . . . . ? N3 Zn1 N1 C1 -169.0(3) . . . . ? N2 Zn1 N1 C1 15.0(3) . . . . ? K1 Zn1 N1 C1 71.5(3) . . . . ? N3 Zn1 N1 K1 119.5(2) . . . . ? N2 Zn1 N1 K1 -56.54(14) . . . . ? O1 K1 N1 C3 77.4(6) . . . . ? C1 K1 N1 C3 -108.4(5) . . . . ? C2 K1 N1 C3 -140.1(4) . . . . ? N2 K1 N1 C3 -174.0(4) . . . . ? C23 K1 N1 C3 -168.9(4) . . . . ? C18 K1 N1 C3 -75.2(4) 2_446 . . . ? Zn1 K1 N1 C3 145.4(4) . . . . ? O1 K1 N1 C1 -174.1(5) . . . . ? C2 K1 N1 C1 -31.6(3) . . . . ? N2 K1 N1 C1 -65.5(3) . . . . ? C23 K1 N1 C1 -60.5(3) . . . . ? C18 K1 N1 C1 33.2(3) 2_446 . . . ? Zn1 K1 N1 C1 -106.1(3) . . . . ? O1 K1 N1 Zn1 -68.0(5) . . . . ? C1 K1 N1 Zn1 106.1(3) . . . . ? C2 K1 N1 Zn1 74.49(18) . . . . ? N2 K1 N1 Zn1 40.57(12) . . . . ? C23 K1 N1 Zn1 45.6(2) . . . . ? C18 K1 N1 Zn1 139.32(16) 2_446 . . . ? N3 Zn1 N2 C2 169.9(3) . . . . ? N1 Zn1 N2 C2 -14.5(3) . . . . ? K1 Zn1 N2 C2 -65.2(3) . . . . ? N3 Zn1 N2 C15 22.5(6) . . . . ? N1 Zn1 N2 C15 -161.9(5) . . . . ? K1 Zn1 N2 C15 147.4(5) . . . . ? N3 Zn1 N2 K1 -124.9(2) . . . . ? N1 Zn1 N2 K1 50.66(14) . . . . ? O1 K1 N2 C2 -140.5(3) . . . . ? C1 K1 N2 C2 32.6(3) . . . . ? N1 K1 N2 C2 69.5(3) . . . . ? C23 K1 N2 C2 -105.2(3) . . . . ? C18 K1 N2 C2 -27.0(3) 2_446 . . . ? Zn1 K1 N2 C2 110.0(3) . . . . ? O1 K1 N2 C15 -36.7(5) . . . . ? C1 K1 N2 C15 136.4(4) . . . . ? C2 K1 N2 C15 103.8(5) . . . . ? N1 K1 N2 C15 173.3(4) . . . . ? C23 K1 N2 C15 -1.3(4) . . . . ? C18 K1 N2 C15 76.8(4) 2_446 . . . ? Zn1 K1 N2 C15 -146.2(5) . . . . ? O1 K1 N2 Zn1 109.5(3) . . . . ? C1 K1 N2 Zn1 -77.41(19) . . . . ? C2 K1 N2 Zn1 -110.0(3) . . . . ? N1 K1 N2 Zn1 -40.47(13) . . . . ? C23 K1 N2 Zn1 144.8(2) . . . . ? C18 K1 N2 Zn1 -137.01(17) 2_446 . . . ? N1 Zn1 N3 C27 145.4(4) . . . . ? N2 Zn1 N3 C27 -40.7(5) . . . . ? K1 Zn1 N3 C27 -135.9(3) . . . . ? N1 Zn1 N3 C28 -40.7(5) . . . . ? N2 Zn1 N3 C28 133.1(4) . . . . ? K1 Zn1 N3 C28 37.9(5) . . . . ? C3 N1 C1 C2 -159.3(5) . . . . ? Zn1 N1 C1 C2 -13.0(6) . . . . ? K1 N1 C1 C2 75.3(5) . . . . ? C3 N1 C1 K1 125.4(4) . . . . ? Zn1 N1 C1 K1 -88.3(2) . . . . ? O1 K1 C1 C2 35(2) . . . . ? N1 K1 C1 C2 -120.9(4) . . . . ? N2 K1 C1 C2 -31.7(3) . . . . ? C23 K1 C1 C2 5.0(3) . . . . ? C18 K1 C1 C2 91.5(3) 2_446 . . . ? Zn1 K1 C1 C2 -76.8(3) . . . . ? O1 K1 C1 N1 155.8(19) . . . . ? C2 K1 C1 N1 120.9(4) . . . . ? N2 K1 C1 N1 89.2(3) . . . . ? C23 K1 C1 N1 125.8(3) . . . . ? C18 K1 C1 N1 -147.7(3) 2_446 . . . ? Zn1 K1 C1 N1 44.1(2) . . . . ? N1 C1 C2 N2 1.3(7) . . . . ? K1 C1 C2 N2 76.2(4) . . . . ? N1 C1 C2 K1 -74.9(4) . . . . ? C15 N2 C2 C1 164.4(5) . . . . ? Zn1 N2 C2 C1 11.3(6) . . . . ? K1 N2 C2 C1 -67.7(4) . . . . ? C15 N2 C2 K1 -128.0(4) . . . . ? Zn1 N2 C2 K1 78.9(2) . . . . ? O1 K1 C2 C1 -173.8(4) . . . . ? N1 K1 C2 C1 33.4(3) . . . . ? N2 K1 C2 C1 121.1(4) . . . . ? C23 K1 C2 C1 -174.8(3) . . . . ? C18 K1 C2 C1 -85.0(3) 2_446 . . . ? Zn1 K1 C2 C1 77.9(3) . . . . ? O1 K1 C2 N2 65.0(5) . . . . ? C1 K1 C2 N2 -121.1(4) . . . . ? N1 K1 C2 N2 -87.7(3) . . . . ? C23 K1 C2 N2 64.1(3) . . . . ? C18 K1 C2 N2 153.9(3) 2_446 . . . ? Zn1 K1 C2 N2 -43.2(2) . . . . ? C1 N1 C3 C8 -121.8(5) . . . . ? Zn1 N1 C3 C8 99.7(5) . . . . ? K1 N1 C3 C8 -35.6(6) . . . . ? C1 N1 C3 C4 58.8(6) . . . . ? Zn1 N1 C3 C4 -79.7(5) . . . . ? K1 N1 C3 C4 145.0(4) . . . . ? C8 C3 C4 C5 3.1(7) . . . . ? N1 C3 C4 C5 -177.5(4) . . . . ? C8 C3 C4 C9 -174.1(5) . . . . ? N1 C3 C4 C9 5.3(7) . . . . ? C3 C4 C5 C6 -1.3(8) . . . . ? C9 C4 C5 C6 176.0(5) . . . . ? C4 C5 C6 C7 -1.7(9) . . . . ? C5 C6 C7 C8 2.8(9) . . . . ? C6 C7 C8 C3 -0.9(8) . . . . ? C6 C7 C8 C12 175.3(5) . . . . ? N1 C3 C8 C7 178.6(4) . . . . ? C4 C3 C8 C7 -2.0(7) . . . . ? N1 C3 C8 C12 2.4(7) . . . . ? C4 C3 C8 C12 -178.2(4) . . . . ? C5 C4 C9 C10 56.5(7) . . . . ? C3 C4 C9 C10 -126.2(6) . . . . ? C5 C4 C9 C11 -71.0(7) . . . . ? C3 C4 C9 C11 106.2(6) . . . . ? C7 C8 C12 C14 46.3(7) . . . . ? C3 C8 C12 C14 -137.5(6) . . . . ? C7 C8 C12 C13 -79.8(7) . . . . ? C3 C8 C12 C13 96.4(6) . . . . ? C2 N2 C15 C16 110.6(5) . . . . ? Zn1 N2 C15 C16 -104.0(5) . . . . ? K1 N2 C15 C16 29.1(6) . . . . ? C2 N2 C15 C20 -70.4(6) . . . . ? Zn1 N2 C15 C20 75.0(6) . . . . ? K1 N2 C15 C20 -151.9(4) . . . . ? C20 C15 C16 C17 1.7(7) . . . . ? N2 C15 C16 C17 -179.3(4) . . . . ? C20 C15 C16 C21 178.7(5) . . . . ? N2 C15 C16 C21 -2.3(7) . . . . ? C15 C16 C17 C18 -1.7(9) . . . . ? C21 C16 C17 C18 -178.6(6) . . . . ? C16 C17 C18 C19 2.6(10) . . . . ? C16 C17 C18 K1 103.4(5) . . . 2_456 ? C17 C18 C19 C20 -3.4(10) . . . . ? K1 C18 C19 C20 -110.5(5) 2_456 . . . ? C18 C19 C20 C15 3.3(9) . . . . ? C18 C19 C20 C24 -176.8(6) . . . . ? C16 C15 C20 C19 -2.5(7) . . . . ? N2 C15 C20 C19 178.6(4) . . . . ? C16 C15 C20 C24 177.7(5) . . . . ? N2 C15 C20 C24 -1.3(7) . . . . ? C17 C16 C21 C23 94.9(6) . . . . ? C15 C16 C21 C23 -82.1(6) . . . . ? C17 C16 C21 C22 -29.8(8) . . . . ? C15 C16 C21 C22 153.2(5) . . . . ? C16 C21 C23 K1 106.3(4) . . . . ? C22 C21 C23 K1 -126.6(4) . . . . ? O1 K1 C23 C21 107.2(4) . . . . ? C1 K1 C23 C21 -75.6(4) . . . . ? C2 K1 C23 C21 -73.3(4) . . . . ? N1 K1 C23 C21 -51.5(4) . . . . ? N2 K1 C23 C21 -47.1(3) . . . . ? C18 K1 C23 C21 -156.9(4) 2_446 . . . ? Zn1 K1 C23 C21 -29.3(4) . . . . ? C19 C20 C24 C25 -65.4(7) . . . . ? C15 C20 C24 C25 114.5(6) . . . . ? C19 C20 C24 C26 60.2(7) . . . . ? C15 C20 C24 C26 -119.9(6) . . . . ? C28 N3 C27 C27 -4.1(9) . . . 3_566 ? Zn1 N3 C27 C27 170.0(6) . . . 3_566 ? C27 N3 C28 C33 -84.6(6) . . . . ? Zn1 N3 C28 C33 101.2(5) . . . . ? C27 N3 C28 C29 97.9(5) . . . . ? Zn1 N3 C28 C29 -76.3(5) . . . . ? C33 C28 C29 C30 -1.6(8) . . . . ? N3 C28 C29 C30 175.9(5) . . . . ? C33 C28 C29 C34 177.1(5) . . . . ? N3 C28 C29 C34 -5.5(8) . . . . ? C28 C29 C30 C31 0.9(9) . . . . ? C34 C29 C30 C31 -177.8(6) . . . . ? C29 C30 C31 C32 0.9(10) . . . . ? C30 C31 C32 C33 -2.1(10) . . . . ? C31 C32 C33 C28 1.3(9) . . . . ? C31 C32 C33 C37 -179.8(6) . . . . ? C29 C28 C33 C32 0.5(8) . . . . ? N3 C28 C33 C32 -176.9(5) . . . . ? C29 C28 C33 C37 -178.3(5) . . . . ? N3 C28 C33 C37 4.3(7) . . . . ? C30 C29 C34 C36 -63.9(8) . . . . ? C28 C29 C34 C36 117.5(7) . . . . ? C30 C29 C34 C35 62.9(8) . . . . ? C28 C29 C34 C35 -115.7(7) . . . . ? C32 C33 C37 C38 56.8(7) . . . . ? C28 C33 C37 C38 -124.4(5) . . . . ? C32 C33 C37 C39 -66.2(7) . . . . ? C28 C33 C37 C39 112.6(6) . . . . ? C41 C40 O1 C42 70.2(12) . . . . ? C41 C40 O1 K1 -124.4(7) . . . . ? C43 C42 O1 C40 152.3(13) . . . . ? C43 C42 O1 K1 -11.9(17) . . . . ? C1 K1 O1 C40 21(3) . . . . ? C2 K1 O1 C40 50.1(10) . . . . ? N1 K1 O1 C40 171.0(6) . . . . ? N2 K1 O1 C40 82.3(9) . . . . ? C23 K1 O1 C40 50.9(8) . . . . ? C18 K1 O1 C40 -35.4(8) 2_446 . . . ? Zn1 K1 O1 C40 127.2(8) . . . . ? C1 K1 O1 C42 -175.8(18) . . . . ? C2 K1 O1 C42 -146.3(9) . . . . ? N1 K1 O1 C42 -25.4(12) . . . . ? N2 K1 O1 C42 -114.0(9) . . . . ? C23 K1 O1 C42 -145.4(10) . . . . ? C18 K1 O1 C42 128.2(9) 2_446 . . . ? Zn1 K1 O1 C42 -69.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.507 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.064 ############ data_LK _database_code_depnum_ccdc_archive 'CCDC 722600' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 K2 N2 O' _chemical_formula_weight 526.87 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' K K 0.2009 0.2494 '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 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 13.166(4) _cell_length_b 17.945(5) _cell_length_c 13.192(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.645(6) _cell_angle_gamma 90.00 _cell_volume 3052.7(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 red _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8672 _exptl_absorpt_correction_T_max 0.8922 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15775 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.1011 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.73 _reflns_number_total 5780 _reflns_number_gt 2869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0862P)^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 5780 _refine_ls_number_parameters 316 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1629 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.892 _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 N1 N -0.14923(19) 0.03114(13) 0.06438(18) 0.0406(6) Uani 1 1 d . . . N2 N -0.3237(2) -0.06140(13) -0.05552(18) 0.0405(6) Uani 1 1 d . . . C1 C -0.1605(2) -0.04583(17) 0.0693(2) 0.0422(8) Uani 1 1 d . . . H1A H -0.1084 -0.0716 0.1137 0.051 Uiso 1 1 calc R . . C2 C -0.2394(3) -0.08660(17) 0.0162(2) 0.0433(8) Uani 1 1 d . . . H2A H -0.2368 -0.1376 0.0293 0.052 Uiso 1 1 calc R . . C3 C -0.0833(2) 0.06517(16) 0.1443(2) 0.0393(7) Uani 1 1 d . . . C4 C -0.0591(3) 0.03966(18) 0.2491(2) 0.0481(8) Uani 1 1 d . . . C5 C 0.0208(3) 0.0730(2) 0.3185(3) 0.0587(10) Uani 1 1 d . . . H5A H 0.0397 0.0527 0.3845 0.070 Uiso 1 1 calc R . . C6 C 0.0732(3) 0.1341(2) 0.2950(3) 0.0708(11) Uani 1 1 d . . . H6A H 0.1286 0.1539 0.3424 0.085 Uiso 1 1 calc R . . C7 C 0.0407(3) 0.1657(2) 0.1978(3) 0.0614(10) Uani 1 1 d . . . H7A H 0.0720 0.2096 0.1823 0.074 Uiso 1 1 calc R . . C8 C -0.0359(2) 0.13465(17) 0.1238(3) 0.0467(8) Uani 1 1 d . . . K2 K -0.65194(6) -0.05460(4) -0.07178(7) 0.0722(3) Uani 1 1 d . . . C9 C -0.4079(2) -0.10706(15) -0.0817(2) 0.0385(7) Uani 1 1 d . . . C10 C -0.4465(2) -0.15602(17) -0.0117(2) 0.0458(8) Uani 1 1 d . . . C11 C -0.5265(3) -0.20489(18) -0.0506(3) 0.0578(10) Uani 1 1 d . . . H11 H -0.5471 -0.2390 -0.0056 0.069 Uiso 1 1 calc R . . C12 C -0.5765(3) -0.20518(19) -0.1522(3) 0.0657(11) Uani 1 1 d . . . H12 H -0.6296 -0.2389 -0.1758 0.079 Uiso 1 1 calc R . . C13 C -0.5461(3) -0.15411(19) -0.2190(3) 0.0570(9) Uani 1 1 d . . . H13 H -0.5811 -0.1526 -0.2876 0.068 Uiso 1 1 calc R . . C14 C -0.4652(2) -0.10557(16) -0.1860(2) 0.0426(8) Uani 1 1 d . . . C15 C -0.0743(3) 0.17324(18) 0.0221(3) 0.0558(9) Uani 1 1 d . . . H15A H -0.0935 0.1345 -0.0306 0.067 Uiso 1 1 calc R . . C16 C -0.1721(3) 0.2180(3) 0.0260(3) 0.0898(14) Uani 1 1 d . . . H16A H -0.2223 0.1862 0.0476 0.135 Uiso 1 1 calc R . . H16B H -0.2002 0.2377 -0.0415 0.135 Uiso 1 1 calc R . . H16C H -0.1550 0.2583 0.0743 0.135 Uiso 1 1 calc R . . C17 C 0.0046(3) 0.2243(2) -0.0140(3) 0.0890(14) Uani 1 1 d . . . H17A H 0.0657 0.1963 -0.0182 0.134 Uiso 1 1 calc R . . H17B H 0.0226 0.2644 0.0344 0.134 Uiso 1 1 calc R . . H17C H -0.0252 0.2443 -0.0810 0.134 Uiso 1 1 calc R . . C18 C -0.1283(3) -0.0141(2) 0.2935(3) 0.0625(10) Uani 1 1 d . . . H18A H -0.1822 -0.0312 0.2359 0.075 Uiso 1 1 calc R . . C19 C -0.1824(3) 0.0275(3) 0.3686(3) 0.0985(15) Uani 1 1 d . . . H19A H -0.2270 -0.0062 0.3956 0.148 Uiso 1 1 calc R . . H19B H -0.2229 0.0676 0.3329 0.148 Uiso 1 1 calc R . . H19C H -0.1314 0.0473 0.4246 0.148 Uiso 1 1 calc R . . C20 C -0.0752(4) -0.0821(2) 0.3453(3) 0.1034(15) Uani 1 1 d . . . H20A H -0.0433 -0.1090 0.2971 0.155 Uiso 1 1 calc R . . H20B H -0.1252 -0.1134 0.3682 0.155 Uiso 1 1 calc R . . H20C H -0.0230 -0.0674 0.4037 0.155 Uiso 1 1 calc R . . C21 C -0.4073(3) -0.15395(19) 0.1061(2) 0.0558(9) Uani 1 1 d . . . H21A H -0.3558 -0.1139 0.1218 0.067 Uiso 1 1 calc R . . C22 C -0.4968(3) -0.1358(2) 0.1609(3) 0.0933(14) Uani 1 1 d . . . H22A H -0.5287 -0.0897 0.1346 0.140 Uiso 1 1 calc R . . H22B H -0.4704 -0.1313 0.2340 0.140 Uiso 1 1 calc R . . H22C H -0.5473 -0.1751 0.1483 0.140 Uiso 1 1 calc R . . C23 C -0.3553(3) -0.2268(2) 0.1497(3) 0.0800(12) Uani 1 1 d . . . H23A H -0.2988 -0.2379 0.1161 0.120 Uiso 1 1 calc R . . H23B H -0.4050 -0.2666 0.1374 0.120 Uiso 1 1 calc R . . H23C H -0.3295 -0.2216 0.2228 0.120 Uiso 1 1 calc R . . C24 C -0.4280(3) -0.05553(18) -0.2644(2) 0.0522(9) Uani 1 1 d . . . H24A H -0.3925 -0.0127 -0.2268 0.063 Uiso 1 1 calc R . . C25 C -0.3490(3) -0.0980(2) -0.3121(3) 0.0791(13) Uani 1 1 d . . . H25A H -0.3253 -0.0668 -0.3618 0.119 Uiso 1 1 calc R . . H25B H -0.3807 -0.1420 -0.3459 0.119 Uiso 1 1 calc R . . H25C H -0.2911 -0.1118 -0.2587 0.119 Uiso 1 1 calc R . . C26 C -0.5145(3) -0.0256(3) -0.3491(3) 0.0984(15) Uani 1 1 d . . . H26A H -0.5634 0.0014 -0.3182 0.148 Uiso 1 1 calc R . . H26B H -0.5490 -0.0664 -0.3889 0.148 Uiso 1 1 calc R . . H26C H -0.4856 0.0070 -0.3935 0.148 Uiso 1 1 calc R . . O1 O -0.2242(3) 0.09781(19) -0.2802(3) 0.1134(11) Uani 1 1 d . . . K1 K -0.15220(6) -0.01035(4) -0.14196(5) 0.0535(3) Uani 1 1 d . . . C27 C -0.2258(8) 0.1718(4) -0.2624(4) 0.210(4) Uani 1 1 d D . . H27A H -0.1735 0.1838 -0.2016 0.253 Uiso 1 1 calc R . . H27B H -0.2929 0.1855 -0.2483 0.253 Uiso 1 1 calc R . . C28 C -0.2067(4) 0.2141(3) -0.3490(4) 0.1163(18) Uani 1 1 d D . . H28A H -0.2527 0.2567 -0.3627 0.140 Uiso 1 1 calc R . . H28B H -0.1354 0.2311 -0.3375 0.140 Uiso 1 1 calc R . . C29 C -0.2280(6) 0.1611(3) -0.4322(4) 0.143(2) Uani 1 1 d D . . H29A H -0.1690 0.1567 -0.4655 0.172 Uiso 1 1 calc R . . H29B H -0.2879 0.1766 -0.4835 0.172 Uiso 1 1 calc R . . C30 C -0.2482(6) 0.0906(3) -0.3862(5) 0.172(3) Uani 1 1 d . . . H30A H -0.3206 0.0771 -0.4086 0.206 Uiso 1 1 calc R . . H30B H -0.2062 0.0516 -0.4080 0.206 Uiso 1 1 calc R . . 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 N1 0.0576(17) 0.0334(15) 0.0311(14) -0.0019(11) 0.0096(13) -0.0026(12) N2 0.0494(17) 0.0391(16) 0.0320(14) -0.0019(12) 0.0057(13) -0.0046(13) C1 0.054(2) 0.044(2) 0.0274(16) 0.0000(14) 0.0061(16) -0.0016(16) C2 0.059(2) 0.0353(18) 0.0393(19) -0.0014(15) 0.0182(18) -0.0049(17) C3 0.0397(18) 0.0437(19) 0.0345(18) -0.0074(15) 0.0071(15) 0.0061(15) C4 0.059(2) 0.051(2) 0.0338(19) -0.0089(16) 0.0087(17) 0.0044(17) C5 0.061(2) 0.070(3) 0.041(2) -0.0125(19) 0.0005(19) 0.009(2) C6 0.065(3) 0.080(3) 0.063(3) -0.034(2) 0.003(2) -0.005(2) C7 0.058(2) 0.054(2) 0.074(3) -0.020(2) 0.017(2) -0.0100(19) C8 0.050(2) 0.0400(19) 0.051(2) -0.0100(16) 0.0128(18) -0.0010(16) K2 0.0639(6) 0.0674(6) 0.0895(7) -0.0286(5) 0.0255(5) 0.0037(4) C9 0.051(2) 0.0271(16) 0.0401(18) -0.0102(14) 0.0165(16) 0.0000(15) C10 0.058(2) 0.0363(18) 0.0466(19) -0.0053(15) 0.0194(17) 0.0000(16) C11 0.063(2) 0.044(2) 0.072(3) -0.0104(19) 0.027(2) -0.0095(18) C12 0.060(3) 0.050(2) 0.088(3) -0.026(2) 0.019(2) -0.0161(19) C13 0.061(2) 0.056(2) 0.054(2) -0.0176(18) 0.0118(19) -0.0034(19) C14 0.048(2) 0.0414(19) 0.0385(19) -0.0138(15) 0.0089(16) -0.0015(16) C15 0.071(2) 0.041(2) 0.057(2) -0.0006(17) 0.017(2) -0.0046(18) C16 0.077(3) 0.111(4) 0.082(3) 0.030(3) 0.019(2) 0.023(3) C17 0.089(3) 0.071(3) 0.113(4) 0.026(3) 0.036(3) -0.001(2) C18 0.081(3) 0.071(3) 0.0343(19) 0.0009(17) 0.0091(19) -0.004(2) C19 0.103(3) 0.139(4) 0.064(3) -0.018(3) 0.041(3) -0.008(3) C20 0.148(4) 0.084(3) 0.076(3) 0.028(3) 0.019(3) -0.001(3) C21 0.074(2) 0.055(2) 0.044(2) 0.0026(16) 0.0258(19) -0.0038(18) C22 0.117(3) 0.109(3) 0.071(3) -0.009(2) 0.058(3) 0.005(3) C23 0.106(3) 0.074(3) 0.064(3) 0.023(2) 0.026(2) 0.012(2) C24 0.065(2) 0.053(2) 0.0374(19) -0.0053(16) 0.0069(18) -0.0032(18) C25 0.104(3) 0.067(3) 0.080(3) -0.019(2) 0.051(3) -0.012(2) C26 0.108(4) 0.108(4) 0.067(3) 0.022(3) -0.012(3) -0.011(3) O1 0.182(3) 0.085(2) 0.080(2) 0.0369(18) 0.043(2) 0.019(2) K1 0.0758(6) 0.0506(5) 0.0382(4) 0.0009(3) 0.0212(4) 0.0006(4) C27 0.451(14) 0.109(5) 0.082(4) 0.016(4) 0.079(6) 0.071(7) C28 0.145(5) 0.071(3) 0.142(5) 0.007(3) 0.051(4) -0.011(3) C29 0.277(8) 0.076(4) 0.087(4) 0.023(3) 0.063(5) 0.026(4) C30 0.310(9) 0.102(5) 0.102(5) 0.003(4) 0.040(5) -0.077(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 N1 C3 1.367(4) . ? N1 C1 1.392(4) . ? N1 K2 2.673(3) 3_455 ? N1 K1 2.815(2) . ? N2 C9 1.366(4) . ? N2 C2 1.382(4) . ? N2 K2 2.734(2) 3_455 ? N2 K1 2.877(2) . ? C1 C2 1.345(4) . ? C1 K1 2.883(3) . ? C1 K2 3.062(3) 3_455 ? C1 H1A 0.9300 . ? C2 K1 2.917(3) . ? C2 K2 3.071(3) 3_455 ? C2 H2A 0.9300 . ? C3 C4 1.429(4) . ? C3 C8 1.444(4) . ? C3 K1 3.259(3) 3 ? C3 K2 3.429(3) 3_455 ? C4 C5 1.383(5) . ? C4 C18 1.522(4) . ? C4 K1 3.406(3) 3 ? C5 C6 1.364(5) . ? C5 K1 3.362(3) 3 ? C5 H5A 0.9300 . ? C6 C7 1.388(5) . ? C6 K1 3.307(3) 3 ? C6 H6A 0.9300 . ? C7 C8 1.372(4) . ? C7 K1 3.303(3) 3 ? C7 H7A 0.9300 . ? C8 C15 1.504(4) . ? C8 K1 3.305(3) 3 ? K2 N1 2.673(3) 3_455 ? K2 N2 2.734(2) 3_455 ? K2 C1 3.062(3) 3_455 ? K2 C2 3.071(3) 3_455 ? K2 C12 3.137(3) . ? K2 C11 3.145(3) . ? K2 C13 3.162(3) . ? K2 C10 3.224(3) . ? K2 C14 3.263(3) . ? K2 C9 3.375(3) . ? K2 C3 3.429(3) 3_455 ? K2 C9 3.535(3) 3_455 ? C9 C14 1.429(4) . ? C9 C10 1.440(4) . ? C9 K2 3.535(3) 3_455 ? C10 C11 1.387(4) . ? C10 C21 1.536(4) . ? C11 C12 1.369(5) . ? C11 H11 0.9300 . ? C12 C13 1.386(5) . ? C12 H12 0.9300 . ? C13 C14 1.377(4) . ? C13 H13 0.9300 . ? C14 C24 1.523(4) . ? C15 C16 1.527(5) . ? C15 C17 1.531(5) . ? C15 H15A 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.501(5) . ? C18 C19 1.527(5) . ? C18 H18A 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C23 1.533(5) . ? C21 C22 1.537(4) . ? C21 H21A 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C26 1.523(5) . ? C24 C25 1.525(4) . ? C24 H24A 0.9800 . ? C25 K1 3.446(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? O1 C27 1.349(6) . ? O1 C30 1.376(6) . ? O1 K1 2.701(3) . ? K1 C3 3.259(3) 3 ? K1 C7 3.303(3) 3 ? K1 C8 3.305(3) 3 ? K1 C6 3.307(3) 3 ? K1 C5 3.362(3) 3 ? K1 C4 3.406(3) 3 ? C27 C28 1.436(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.435(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.451(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? 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 C3 N1 C1 117.7(3) . . ? C3 N1 K2 112.05(16) . 3_455 ? C1 N1 K2 92.29(17) . 3_455 ? C3 N1 K1 138.33(17) . . ? C1 N1 K1 78.59(15) . . ? K2 N1 K1 104.74(9) 3_455 . ? C9 N2 C2 118.4(2) . . ? C9 N2 K2 114.99(16) . 3_455 ? C2 N2 K2 90.35(16) . 3_455 ? C9 N2 K1 138.82(17) . . ? C2 N2 K1 77.83(15) . . ? K2 N2 K1 101.52(8) 3_455 . ? C2 C1 N1 126.4(3) . . ? C2 C1 K1 78.03(17) . . ? N1 C1 K1 73.16(14) . . ? C2 C1 K2 77.67(19) . 3_455 ? N1 C1 K2 60.70(15) . 3_455 ? K1 C1 K2 93.92(9) . 3_455 ? C2 C1 H1A 116.8 . . ? N1 C1 H1A 116.8 . . ? K1 C1 H1A 123.5 . . ? K2 C1 H1A 141.2 3_455 . ? C1 C2 N2 127.4(3) . . ? C1 C2 K1 75.15(16) . . ? N2 C2 K1 74.59(15) . . ? C1 C2 K2 76.98(18) . 3_455 ? N2 C2 K2 62.91(15) . 3_455 ? K1 C2 K2 93.05(9) . 3_455 ? C1 C2 H2A 116.3 . . ? N2 C2 H2A 116.3 . . ? K1 C2 H2A 126.1 . . ? K2 C2 H2A 140.2 3_455 . ? N1 C3 C4 125.9(3) . . ? N1 C3 C8 118.2(3) . . ? C4 C3 C8 115.9(3) . . ? N1 C3 K1 108.35(16) . 3 ? C4 C3 K1 83.44(17) . 3 ? C8 C3 K1 79.08(16) . 3 ? N1 C3 K2 46.26(13) . 3_455 ? C4 C3 K2 105.53(19) . 3_455 ? C8 C3 K2 116.7(2) . 3_455 ? K1 C3 K2 153.66(10) 3 3_455 ? C5 C4 C3 119.5(3) . . ? C5 C4 C18 116.9(3) . . ? C3 C4 C18 122.8(3) . . ? C5 C4 K1 76.45(18) . 3 ? C3 C4 K1 71.92(16) . 3 ? C18 C4 K1 131.6(2) . 3 ? C6 C5 C4 123.3(3) . . ? C6 C5 K1 75.93(19) . 3 ? C4 C5 K1 79.98(18) . 3 ? C6 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? K1 C5 H5A 116.0 3 . ? C5 C6 C7 117.6(4) . . ? C5 C6 K1 80.5(2) . 3 ? C7 C6 K1 77.69(19) . 3 ? C5 C6 H6A 121.2 . . ? C7 C6 H6A 121.2 . . ? K1 C6 H6A 111.4 3 . ? C8 C7 C6 122.4(4) . . ? C8 C7 K1 78.12(19) . 3 ? C6 C7 K1 78.1(2) . 3 ? C8 C7 H7A 118.8 . . ? C6 C7 H7A 118.8 . . ? K1 C7 H7A 115.4 3 . ? C7 C8 C3 120.0(3) . . ? C7 C8 C15 120.9(3) . . ? C3 C8 C15 119.0(3) . . ? C7 C8 K1 77.91(19) . 3 ? C3 C8 K1 75.51(16) . 3 ? C15 C8 K1 119.19(18) . 3 ? N1 K2 N2 67.69(8) 3_455 3_455 ? N1 K2 C1 27.02(7) 3_455 3_455 ? N2 K2 C1 49.50(8) 3_455 3_455 ? N1 K2 C2 49.77(8) 3_455 3_455 ? N2 K2 C2 26.74(7) 3_455 3_455 ? C1 K2 C2 25.34(8) 3_455 3_455 ? N1 K2 C12 121.84(9) 3_455 . ? N2 K2 C12 161.45(10) 3_455 . ? C1 K2 C12 145.25(10) 3_455 . ? C2 K2 C12 170.49(10) 3_455 . ? N1 K2 C11 129.24(9) 3_455 . ? N2 K2 C11 136.29(10) 3_455 . ? C1 K2 C11 156.03(9) 3_455 . ? C2 K2 C11 161.44(10) 3_455 . ? C12 K2 C11 25.17(9) . . ? N1 K2 C13 131.92(9) 3_455 . ? N2 K2 C13 158.17(9) 3_455 . ? C1 K2 C13 142.69(9) 3_455 . ? C2 K2 C13 153.79(9) 3_455 . ? C12 K2 C13 25.41(9) . . ? C11 K2 C13 44.08(10) . . ? N1 K2 C10 149.25(8) 3_455 . ? N2 K2 C10 118.39(9) 3_455 . ? C1 K2 C10 165.46(8) 3_455 . ? C2 K2 C10 144.64(9) 3_455 . ? C12 K2 C10 44.72(9) . . ? C11 K2 C10 25.12(8) . . ? C13 K2 C10 51.69(9) . . ? N1 K2 C14 153.63(8) 3_455 . ? N2 K2 C14 133.61(8) 3_455 . ? C1 K2 C14 148.67(8) 3_455 . ? C2 K2 C14 140.57(8) 3_455 . ? C12 K2 C14 44.18(8) . . ? C11 K2 C14 50.92(8) . . ? C13 K2 C14 24.68(7) . . ? C10 K2 C14 44.12(8) . . ? N1 K2 C9 172.87(8) 3_455 . ? N2 K2 C9 117.83(7) 3_455 . ? C1 K2 C9 160.09(8) 3_455 . ? C2 K2 C9 137.09(8) 3_455 . ? C12 K2 C9 51.51(8) . . ? C11 K2 C9 43.74(8) . . ? C13 K2 C9 43.74(8) . . ? C10 K2 C9 25.06(7) . . ? C14 K2 C9 24.78(7) . . ? N1 K2 C3 21.69(6) 3_455 3_455 ? N2 K2 C3 88.56(7) 3_455 3_455 ? C1 K2 C3 42.19(8) 3_455 3_455 ? C2 K2 C3 67.41(8) 3_455 3_455 ? C12 K2 C3 103.39(9) . 3_455 ? C11 K2 C3 117.61(9) . 3_455 ? C13 K2 C3 110.29(8) . 3_455 ? C10 K2 C3 142.45(8) . 3_455 ? C14 K2 C3 132.38(8) . 3_455 ? C9 K2 C3 153.59(7) . 3_455 ? N1 K2 C9 87.51(7) 3_455 3_455 ? N2 K2 C9 20.51(6) 3_455 3_455 ? C1 K2 C9 66.30(8) 3_455 3_455 ? C2 K2 C9 41.13(8) 3_455 3_455 ? C12 K2 C9 148.37(9) . 3_455 ? C11 K2 C9 126.89(9) . 3_455 ? C13 K2 C9 137.76(8) . 3_455 ? C10 K2 C9 104.08(8) . 3_455 ? C14 K2 C9 113.13(7) . 3_455 ? C9 K2 C9 98.46(6) . 3_455 ? C3 K2 C9 107.58(7) 3_455 3_455 ? N2 C9 C14 118.4(3) . . ? N2 C9 C10 125.2(3) . . ? C14 C9 C10 116.3(3) . . ? N2 C9 K2 123.59(17) . . ? C14 C9 K2 73.21(16) . . ? C10 C9 K2 71.57(17) . . ? N2 C9 K2 44.51(12) . 3_455 ? C14 C9 K2 123.32(19) . 3_455 ? C10 C9 K2 101.53(17) . 3_455 ? K2 C9 K2 81.54(6) . 3_455 ? C11 C10 C9 119.2(3) . . ? C11 C10 C21 117.7(3) . . ? C9 C10 C21 123.0(3) . . ? C11 C10 K2 74.27(19) . . ? C9 C10 K2 83.37(18) . . ? C21 C10 K2 109.22(17) . . ? C12 C11 C10 122.9(3) . . ? C12 C11 K2 77.1(2) . . ? C10 C11 K2 80.61(19) . . ? C12 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? K2 C11 H11 113.9 . . ? C11 C12 C13 118.5(3) . . ? C11 C12 K2 77.8(2) . . ? C13 C12 K2 78.30(19) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? K2 C12 H12 113.9 . . ? C14 C13 C12 121.5(3) . . ? C14 C13 K2 81.80(17) . . ? C12 C13 K2 76.29(19) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? K2 C13 H13 112.8 . . ? C13 C14 C9 121.1(3) . . ? C13 C14 C24 119.5(3) . . ? C9 C14 C24 119.0(3) . . ? C13 C14 K2 73.52(17) . . ? C9 C14 K2 82.01(15) . . ? C24 C14 K2 121.56(19) . . ? C8 C15 C16 110.3(3) . . ? C8 C15 C17 115.2(3) . . ? C16 C15 C17 108.9(3) . . ? C8 C15 H15A 107.4 . . ? C16 C15 H15A 107.4 . . ? C17 C15 H15A 107.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C4 115.5(3) . . ? C20 C18 C19 109.8(3) . . ? C4 C18 C19 109.5(3) . . ? C20 C18 H18A 107.2 . . ? C4 C18 H18A 107.2 . . ? C19 C18 H18A 107.2 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C10 113.1(3) . . ? C23 C21 C22 109.3(3) . . ? C10 C21 C22 110.3(3) . . ? C23 C21 H21A 108.0 . . ? C10 C21 H21A 108.0 . . ? C22 C21 H21A 108.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C14 114.3(3) . . ? C26 C24 C25 110.2(3) . . ? C14 C24 C25 109.0(3) . . ? C26 C24 H24A 107.7 . . ? C14 C24 H24A 107.7 . . ? C25 C24 H24A 107.7 . . ? C24 C25 K1 89.4(2) . . ? C24 C25 H25A 109.5 . . ? K1 C25 H25A 82.8 . . ? C24 C25 H25B 109.5 . . ? K1 C25 H25B 151.3 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? K1 C25 H25C 42.2 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 O1 C30 105.2(4) . . ? C27 O1 K1 127.2(4) . . ? C30 O1 K1 126.6(3) . . ? O1 K1 N1 113.42(10) . . ? O1 K1 N2 107.44(9) . . ? N1 K1 N2 63.88(7) . . ? O1 K1 C1 137.31(10) . . ? N1 K1 C1 28.25(8) . . ? N2 K1 C1 50.24(8) . . ? O1 K1 C2 133.23(10) . . ? N1 K1 C2 50.43(8) . . ? N2 K1 C2 27.58(7) . . ? C1 K1 C2 26.82(8) . . ? O1 K1 C3 114.55(9) . 3 ? N1 K1 C3 105.17(7) . 3 ? N2 K1 C3 137.06(8) . 3 ? C1 K1 C3 99.47(8) . 3 ? C2 K1 C3 112.19(9) . 3 ? O1 K1 C7 124.56(11) . 3 ? N1 K1 C7 121.26(9) . 3 ? N2 K1 C7 103.86(8) . 3 ? C1 K1 C7 97.74(10) . 3 ? C2 K1 C7 91.17(9) . 3 ? C3 K1 C7 43.65(8) 3 3 ? O1 K1 C8 133.61(9) . 3 ? N1 K1 C8 104.15(8) . 3 ? N2 K1 C8 113.13(8) . 3 ? C1 K1 C8 87.42(8) . 3 ? C2 K1 C8 91.65(9) . 3 ? C3 K1 C8 25.41(7) 3 3 ? C7 K1 C8 23.97(8) 3 3 ? O1 K1 C6 100.43(11) . 3 ? N1 K1 C6 145.42(10) . 3 ? N2 K1 C6 113.39(9) . 3 ? C1 K1 C6 121.34(10) . 3 ? C2 K1 C6 109.85(10) . 3 ? C3 K1 C6 51.26(9) 3 3 ? C7 K1 C6 24.25(9) 3 3 ? C8 K1 C6 42.92(9) 3 3 ? O1 K1 C5 86.10(10) . 3 ? N1 K1 C5 148.16(8) . 3 ? N2 K1 C5 136.30(9) . 3 ? C1 K1 C5 136.16(9) . 3 ? C2 K1 C5 132.10(9) . 3 ? C3 K1 C5 43.02(8) 3 3 ? C7 K1 C5 41.36(9) 3 3 ? C8 K1 C5 48.85(8) 3 3 ? C6 K1 C5 23.59(8) 3 3 ? O1 K1 C4 92.04(9) . 3 ? N1 K1 C4 126.09(8) . 3 ? N2 K1 C4 152.55(8) . 3 ? C1 K1 C4 124.11(9) . 3 ? C2 K1 C4 134.16(9) . 3 ? C3 K1 C4 24.64(7) 3 3 ? C7 K1 C4 48.70(8) 3 3 ? C8 K1 C4 42.54(8) 3 3 ? C6 K1 C4 42.18(9) 3 3 ? C5 K1 C4 23.57(8) 3 3 ? O1 K1 C25 76.85(11) . . ? N1 K1 C25 127.77(8) . . ? N2 K1 C25 64.28(8) . . ? C1 K1 C25 111.03(9) . . ? C2 K1 C25 84.23(9) . . ? C3 K1 C25 116.59(8) 3 . ? C7 K1 C25 77.25(10) 3 . ? C8 K1 C25 101.13(9) 3 . ? C6 K1 C25 65.41(9) 3 . ? C5 K1 C25 79.67(9) 3 . ? C4 K1 C25 103.23(8) 3 . ? O1 C27 C28 111.7(5) . . ? O1 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? O1 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C29 C28 C27 102.7(5) . . ? C29 C28 H28A 111.2 . . ? C27 C28 H28A 111.2 . . ? C29 C28 H28B 111.2 . . ? C27 C28 H28B 111.2 . . ? H28A C28 H28B 109.1 . . ? C28 C29 C30 106.4(4) . . ? C28 C29 H29A 110.5 . . ? C30 C29 H29A 110.5 . . ? C28 C29 H29B 110.5 . . ? C30 C29 H29B 110.5 . . ? H29A C29 H29B 108.6 . . ? O1 C30 C29 108.6(4) . . ? O1 C30 H30A 110.0 . . ? C29 C30 H30A 110.0 . . ? O1 C30 H30B 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? 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 C3 N1 C1 C2 160.5(3) . . . . ? K2 N1 C1 C2 44.1(3) 3_455 . . . ? K1 N1 C1 C2 -60.5(3) . . . . ? C3 N1 C1 K1 -139.0(2) . . . . ? K2 N1 C1 K1 104.58(8) 3_455 . . . ? C3 N1 C1 K2 116.4(2) . . . 3_455 ? K1 N1 C1 K2 -104.58(8) . . . 3_455 ? N1 C1 C2 N2 1.7(4) . . . . ? K1 C1 C2 N2 -56.7(3) . . . . ? K2 C1 C2 N2 40.1(3) 3_455 . . . ? N1 C1 C2 K1 58.4(2) . . . . ? K2 C1 C2 K1 96.77(7) 3_455 . . . ? N1 C1 C2 K2 -38.4(2) . . . 3_455 ? K1 C1 C2 K2 -96.77(7) . . . 3_455 ? C9 N2 C2 C1 -163.7(3) . . . . ? K2 N2 C2 C1 -44.8(3) 3_455 . . . ? K1 N2 C2 C1 56.9(3) . . . . ? C9 N2 C2 K1 139.4(2) . . . . ? K2 N2 C2 K1 -101.72(7) 3_455 . . . ? C9 N2 C2 K2 -118.9(2) . . . 3_455 ? K1 N2 C2 K2 101.72(7) . . . 3_455 ? C1 N1 C3 C4 -28.7(4) . . . . ? K2 N1 C3 C4 76.5(3) 3_455 . . . ? K1 N1 C3 C4 -133.3(3) . . . . ? C1 N1 C3 C8 153.8(2) . . . . ? K2 N1 C3 C8 -101.1(2) 3_455 . . . ? K1 N1 C3 C8 49.1(4) . . . . ? C1 N1 C3 K1 66.6(2) . . . 3 ? K2 N1 C3 K1 171.69(8) 3_455 . . 3 ? K1 N1 C3 K1 -38.1(3) . . . 3 ? C1 N1 C3 K2 -105.1(2) . . . 3_455 ? K1 N1 C3 K2 150.2(3) . . . 3_455 ? N1 C3 C4 C5 170.0(3) . . . . ? C8 C3 C4 C5 -12.4(4) . . . . ? K1 C3 C4 C5 62.1(3) 3 . . . ? K2 C3 C4 C5 -143.2(2) 3_455 . . . ? N1 C3 C4 C18 -20.4(4) . . . . ? C8 C3 C4 C18 157.2(3) . . . . ? K1 C3 C4 C18 -128.4(3) 3 . . . ? K2 C3 C4 C18 26.4(3) 3_455 . . . ? N1 C3 C4 K1 107.9(3) . . . 3 ? C8 C3 C4 K1 -74.5(2) . . . 3 ? K2 C3 C4 K1 154.74(12) 3_455 . . 3 ? C3 C4 C5 C6 6.0(5) . . . . ? C18 C4 C5 C6 -164.2(3) . . . . ? K1 C4 C5 C6 65.7(3) 3 . . . ? C3 C4 C5 K1 -59.8(2) . . . 3 ? C18 C4 C5 K1 130.1(3) . . . 3 ? C4 C5 C6 C7 2.9(5) . . . . ? K1 C5 C6 C7 70.6(3) 3 . . . ? C4 C5 C6 K1 -67.7(3) . . . 3 ? C5 C6 C7 C8 -4.8(5) . . . . ? K1 C6 C7 C8 67.4(3) 3 . . . ? C5 C6 C7 K1 -72.2(3) . . . 3 ? C6 C7 C8 C3 -2.2(5) . . . . ? K1 C7 C8 C3 65.2(2) 3 . . . ? C6 C7 C8 C15 175.6(3) . . . . ? K1 C7 C8 C15 -116.9(3) 3 . . . ? C6 C7 C8 K1 -67.4(3) . . . 3 ? N1 C3 C8 C7 -171.6(3) . . . . ? C4 C3 C8 C7 10.6(4) . . . . ? K1 C3 C8 C7 -66.5(3) 3 . . . ? K2 C3 C8 C7 135.9(2) 3_455 . . . ? N1 C3 C8 C15 10.5(4) . . . . ? C4 C3 C8 C15 -167.3(3) . . . . ? K1 C3 C8 C15 115.6(2) 3 . . . ? K2 C3 C8 C15 -42.0(3) 3_455 . . . ? N1 C3 C8 K1 -105.1(2) . . . 3 ? C4 C3 C8 K1 77.1(2) . . . 3 ? K2 C3 C8 K1 -157.60(14) 3_455 . . 3 ? C2 N2 C9 C14 -145.0(3) . . . . ? K2 N2 C9 C14 109.9(2) 3_455 . . . ? K1 N2 C9 C14 -40.2(4) . . . . ? C2 N2 C9 C10 36.7(4) . . . . ? K2 N2 C9 C10 -68.3(3) 3_455 . . . ? K1 N2 C9 C10 141.5(2) . . . . ? C2 N2 C9 K2 127.0(2) . . . . ? K2 N2 C9 K2 21.9(3) 3_455 . . . ? K1 N2 C9 K2 -128.24(19) . . . . ? C2 N2 C9 K2 105.1(3) . . . 3_455 ? K1 N2 C9 K2 -150.2(4) . . . 3_455 ? N1 K2 C9 N2 -162.1(5) 3_455 . . . ? N2 K2 C9 N2 -22.5(3) 3_455 . . . ? C1 K2 C9 N2 23.1(4) 3_455 . . . ? C2 K2 C9 N2 1.2(3) 3_455 . . . ? C12 K2 C9 N2 175.7(3) . . . . ? C11 K2 C9 N2 -151.6(3) . . . . ? C13 K2 C9 N2 142.7(3) . . . . ? C10 K2 C9 N2 -120.6(3) . . . . ? C14 K2 C9 N2 113.3(3) . . . . ? C3 K2 C9 N2 155.1(2) 3_455 . . . ? C9 K2 C9 N2 -15.34(19) 3_455 . . . ? N1 K2 C9 C14 84.6(6) 3_455 . . . ? N2 K2 C9 C14 -135.84(17) 3_455 . . . ? C1 K2 C9 C14 -90.2(3) 3_455 . . . ? C2 K2 C9 C14 -112.10(19) 3_455 . . . ? C12 K2 C9 C14 62.37(19) . . . . ? C11 K2 C9 C14 95.1(2) . . . . ? C13 K2 C9 C14 29.32(17) . . . . ? C10 K2 C9 C14 126.1(3) . . . . ? C3 K2 C9 C14 41.7(3) 3_455 . . . ? C9 K2 C9 C14 -128.69(18) 3_455 . . . ? N1 K2 C9 C10 -41.5(7) 3_455 . . . ? N2 K2 C9 C10 98.07(18) 3_455 . . . ? C1 K2 C9 C10 143.7(2) 3_455 . . . ? C2 K2 C9 C10 121.81(19) 3_455 . . . ? C12 K2 C9 C10 -63.72(19) . . . . ? C11 K2 C9 C10 -31.03(17) . . . . ? C13 K2 C9 C10 -96.8(2) . . . . ? C14 K2 C9 C10 -126.1(3) . . . . ? C3 K2 C9 C10 -84.4(2) 3_455 . . . ? C9 K2 C9 C10 105.22(18) 3_455 . . . ? N1 K2 C9 K2 -146.7(6) 3_455 . . 3_455 ? N2 K2 C9 K2 -7.16(9) 3_455 . . 3_455 ? C1 K2 C9 K2 38.5(2) 3_455 . . 3_455 ? C2 K2 C9 K2 16.59(13) 3_455 . . 3_455 ? C12 K2 C9 K2 -168.94(13) . . . 3_455 ? C11 K2 C9 K2 -136.25(14) . . . 3_455 ? C13 K2 C9 K2 158.00(13) . . . 3_455 ? C10 K2 C9 K2 -105.22(18) . . . 3_455 ? C14 K2 C9 K2 128.69(18) . . . 3_455 ? C3 K2 C9 K2 170.42(15) 3_455 . . 3_455 ? C9 K2 C9 K2 0.0 3_455 . . 3_455 ? N2 C9 C10 C11 -173.6(3) . . . . ? C14 C9 C10 C11 8.1(4) . . . . ? K2 C9 C10 C11 67.8(3) . . . . ? K2 C9 C10 C11 144.7(2) 3_455 . . . ? N2 C9 C10 C21 9.9(4) . . . . ? C14 C9 C10 C21 -168.3(3) . . . . ? K2 C9 C10 C21 -108.6(3) . . . . ? K2 C9 C10 C21 -31.7(3) 3_455 . . . ? N2 C9 C10 K2 118.6(3) . . . . ? C14 C9 C10 K2 -59.7(2) . . . . ? K2 C9 C10 K2 76.92(9) 3_455 . . . ? N1 K2 C10 C11 47.8(3) 3_455 . . . ? N2 K2 C10 C11 141.53(19) 3_455 . . . ? C1 K2 C10 C11 110.5(4) 3_455 . . . ? C2 K2 C10 C11 148.6(2) 3_455 . . . ? C12 K2 C10 C11 -28.81(19) . . . . ? C13 K2 C10 C11 -61.9(2) . . . . ? C14 K2 C10 C11 -93.8(2) . . . . ? C9 K2 C10 C11 -122.9(3) . . . . ? C3 K2 C10 C11 10.5(2) 3_455 . . . ? C9 K2 C10 C11 157.36(19) 3_455 . . . ? N1 K2 C10 C9 170.74(17) 3_455 . . . ? N2 K2 C10 C9 -95.57(17) 3_455 . . . ? C1 K2 C10 C9 -126.6(3) 3_455 . . . ? C2 K2 C10 C9 -88.5(2) 3_455 . . . ? C12 K2 C10 C9 94.1(2) . . . . ? C11 K2 C10 C9 122.9(3) . . . . ? C13 K2 C10 C9 61.04(17) . . . . ? C14 K2 C10 C9 29.11(15) . . . . ? C3 K2 C10 C9 133.43(17) 3_455 . . . ? C9 K2 C10 C9 -79.73(18) 3_455 . . . ? N1 K2 C10 C21 -66.6(3) 3_455 . . . ? N2 K2 C10 C21 27.1(2) 3_455 . . . ? C1 K2 C10 C21 -3.9(5) 3_455 . . . ? C2 K2 C10 C21 34.2(3) 3_455 . . . ? C12 K2 C10 C21 -143.2(2) . . . . ? C11 K2 C10 C21 -114.4(3) . . . . ? C13 K2 C10 C21 -176.3(2) . . . . ? C14 K2 C10 C21 151.8(2) . . . . ? C9 K2 C10 C21 122.7(3) . . . . ? C3 K2 C10 C21 -103.9(2) 3_455 . . . ? C9 K2 C10 C21 43.0(2) 3_455 . . . ? C9 C10 C11 C12 -5.0(5) . . . . ? C21 C10 C11 C12 171.6(3) . . . . ? K2 C10 C11 C12 67.8(3) . . . . ? C9 C10 C11 K2 -72.8(2) . . . . ? C21 C10 C11 K2 103.8(2) . . . . ? N1 K2 C11 C12 82.2(2) 3_455 . . . ? N2 K2 C11 C12 -179.50(18) 3_455 . . . ? C1 K2 C11 C12 88.2(3) 3_455 . . . ? C2 K2 C11 C12 161.4(3) 3_455 . . . ? C13 K2 C11 C12 -31.20(19) . . . . ? C10 K2 C11 C12 -127.1(3) . . . . ? C14 K2 C11 C12 -63.6(2) . . . . ? C9 K2 C11 C12 -96.2(2) . . . . ? C3 K2 C11 C12 60.1(2) 3_455 . . . ? C9 K2 C11 C12 -154.95(19) 3_455 . . . ? N1 K2 C11 C10 -150.71(17) 3_455 . . . ? N2 K2 C11 C10 -52.4(2) 3_455 . . . ? C1 K2 C11 C10 -144.6(2) 3_455 . . . ? C2 K2 C11 C10 -71.5(3) 3_455 . . . ? C12 K2 C11 C10 127.1(3) . . . . ? C13 K2 C11 C10 95.9(2) . . . . ? C14 K2 C11 C10 63.50(18) . . . . ? C9 K2 C11 C10 30.96(16) . . . . ? C3 K2 C11 C10 -172.78(17) 3_455 . . . ? C9 K2 C11 C10 -27.8(2) 3_455 . . . ? C10 C11 C12 C13 -0.3(5) . . . . ? K2 C11 C12 C13 69.3(3) . . . . ? C10 C11 C12 K2 -69.6(3) . . . . ? N1 K2 C12 C11 -115.4(2) 3_455 . . . ? N2 K2 C12 C11 1.1(4) 3_455 . . . ? C1 K2 C12 C11 -134.6(2) 3_455 . . . ? C2 K2 C12 C11 -142.0(5) 3_455 . . . ? C13 K2 C12 C11 122.9(3) . . . . ? C10 K2 C12 C11 28.75(18) . . . . ? C14 K2 C12 C11 93.6(2) . . . . ? C9 K2 C12 C11 61.4(2) . . . . ? C3 K2 C12 C11 -127.9(2) 3_455 . . . ? C9 K2 C12 C11 40.2(3) 3_455 . . . ? N1 K2 C12 C13 121.7(2) 3_455 . . . ? N2 K2 C12 C13 -121.8(3) 3_455 . . . ? C1 K2 C12 C13 102.5(2) 3_455 . . . ? C2 K2 C12 C13 95.1(6) 3_455 . . . ? C11 K2 C12 C13 -122.9(3) . . . . ? C10 K2 C12 C13 -94.1(2) . . . . ? C14 K2 C12 C13 -29.3(2) . . . . ? C9 K2 C12 C13 -61.5(2) . . . . ? C3 K2 C12 C13 109.3(2) 3_455 . . . ? C9 K2 C12 C13 -82.7(3) 3_455 . . . ? C11 C12 C13 C14 2.3(5) . . . . ? K2 C12 C13 C14 71.3(3) . . . . ? C11 C12 C13 K2 -69.0(3) . . . . ? N1 K2 C13 C14 158.44(18) 3_455 . . . ? N2 K2 C13 C14 8.1(4) 3_455 . . . ? C1 K2 C13 C14 121.3(2) 3_455 . . . ? C2 K2 C13 C14 76.6(3) 3_455 . . . ? C12 K2 C13 C14 -125.3(3) . . . . ? C11 K2 C13 C14 -94.4(2) . . . . ? C10 K2 C13 C14 -61.9(2) . . . . ? C9 K2 C13 C14 -29.44(18) . . . . ? C3 K2 C13 C14 156.41(19) 3_455 . . . ? C9 K2 C13 C14 4.0(3) 3_455 . . . ? N1 K2 C13 C12 -76.3(3) 3_455 . . . ? N2 K2 C13 C12 133.4(3) 3_455 . . . ? C1 K2 C13 C12 -113.4(2) 3_455 . . . ? C2 K2 C13 C12 -158.1(2) 3_455 . . . ? C11 K2 C13 C12 30.9(2) . . . . ? C10 K2 C13 C12 63.4(2) . . . . ? C14 K2 C13 C12 125.3(3) . . . . ? C9 K2 C13 C12 95.9(3) . . . . ? C3 K2 C13 C12 -78.3(2) 3_455 . . . ? C9 K2 C13 C12 129.3(2) 3_455 . . . ? C12 C13 C14 C9 1.3(5) . . . . ? K2 C13 C14 C9 69.7(2) . . . . ? C12 C13 C14 C24 174.3(3) . . . . ? K2 C13 C14 C24 -117.4(3) . . . . ? C12 C13 C14 K2 -68.4(3) . . . . ? N2 C9 C14 C13 175.2(3) . . . . ? C10 C9 C14 C13 -6.4(4) . . . . ? K2 C9 C14 C13 -65.2(2) . . . . ? K2 C9 C14 C13 -132.7(2) 3_455 . . . ? N2 C9 C14 C24 2.2(4) . . . . ? C10 C9 C14 C24 -179.4(2) . . . . ? K2 C9 C14 C24 121.8(3) . . . . ? K2 C9 C14 C24 54.3(3) 3_455 . . . ? N2 C9 C14 K2 -119.6(2) . . . . ? C10 C9 C14 K2 58.8(2) . . . . ? K2 C9 C14 K2 -67.52(15) 3_455 . . . ? N1 K2 C14 C13 -38.0(3) 3_455 . . . ? N2 K2 C14 C13 -175.9(2) 3_455 . . . ? C1 K2 C14 C13 -95.1(3) 3_455 . . . ? C2 K2 C14 C13 -137.4(2) 3_455 . . . ? C12 K2 C14 C13 30.2(2) . . . . ? C11 K2 C14 C13 63.3(2) . . . . ? C10 K2 C14 C13 96.4(2) . . . . ? C9 K2 C14 C13 125.8(3) . . . . ? C3 K2 C14 C13 -30.5(2) 3_455 . . . ? C9 K2 C14 C13 -177.1(2) 3_455 . . . ? N1 K2 C14 C9 -163.84(18) 3_455 . . . ? N2 K2 C14 C9 58.3(2) 3_455 . . . ? C1 K2 C14 C9 139.10(19) 3_455 . . . ? C2 K2 C14 C9 96.7(2) 3_455 . . . ? C12 K2 C14 C9 -95.7(2) . . . . ? C11 K2 C14 C9 -62.52(18) . . . . ? C13 K2 C14 C9 -125.8(3) . . . . ? C10 K2 C14 C9 -29.45(16) . . . . ? C3 K2 C14 C9 -156.37(15) 3_455 . . . ? C9 K2 C14 C9 57.1(2) 3_455 . . . ? N1 K2 C14 C24 76.9(3) 3_455 . . . ? N2 K2 C14 C24 -61.0(3) 3_455 . . . ? C1 K2 C14 C24 19.8(3) 3_455 . . . ? C2 K2 C14 C24 -22.6(3) 3_455 . . . ? C12 K2 C14 C24 145.1(3) . . . . ? C11 K2 C14 C24 178.2(3) . . . . ? C13 K2 C14 C24 114.9(3) . . . . ? C10 K2 C14 C24 -148.7(3) . . . . ? C9 K2 C14 C24 -119.3(3) . . . . ? C3 K2 C14 C24 84.3(3) 3_455 . . . ? C9 K2 C14 C24 -62.2(2) 3_455 . . . ? C7 C8 C15 C16 -96.2(4) . . . . ? C3 C8 C15 C16 81.6(4) . . . . ? K1 C8 C15 C16 170.6(2) 3 . . . ? C7 C8 C15 C17 27.6(4) . . . . ? C3 C8 C15 C17 -154.5(3) . . . . ? K1 C8 C15 C17 -65.6(3) 3 . . . ? C5 C4 C18 C20 -62.9(4) . . . . ? C3 C4 C18 C20 127.3(3) . . . . ? K1 C4 C18 C20 32.8(4) 3 . . . ? C5 C4 C18 C19 61.6(4) . . . . ? C3 C4 C18 C19 -108.2(4) . . . . ? K1 C4 C18 C19 157.3(3) 3 . . . ? C11 C10 C21 C23 65.7(4) . . . . ? C9 C10 C21 C23 -117.8(3) . . . . ? K2 C10 C21 C23 147.6(2) . . . . ? C11 C10 C21 C22 -57.1(4) . . . . ? C9 C10 C21 C22 119.4(3) . . . . ? K2 C10 C21 C22 24.8(3) . . . . ? C13 C14 C24 C26 37.8(4) . . . . ? C9 C14 C24 C26 -149.1(3) . . . . ? K2 C14 C24 C26 -50.2(4) . . . . ? C13 C14 C24 C25 -86.0(4) . . . . ? C9 C14 C24 C25 87.1(3) . . . . ? K2 C14 C24 C25 -174.0(2) . . . . ? C26 C24 C25 K1 135.8(3) . . . . ? C14 C24 C25 K1 -98.0(2) . . . . ? C27 O1 K1 N1 23.1(6) . . . . ? C30 O1 K1 N1 -170.3(4) . . . . ? C27 O1 K1 N2 91.6(6) . . . . ? C30 O1 K1 N2 -101.8(5) . . . . ? C27 O1 K1 C1 42.0(6) . . . . ? C30 O1 K1 C1 -151.4(4) . . . . ? C27 O1 K1 C2 80.1(6) . . . . ? C30 O1 K1 C2 -113.4(5) . . . . ? C27 O1 K1 C3 -97.6(6) . . . 3 ? C30 O1 K1 C3 68.9(5) . . . 3 ? C27 O1 K1 C7 -147.0(6) . . . 3 ? C30 O1 K1 C7 19.6(5) . . . 3 ? C27 O1 K1 C8 -118.2(6) . . . 3 ? C30 O1 K1 C8 48.4(5) . . . 3 ? C27 O1 K1 C6 -149.6(6) . . . 3 ? C30 O1 K1 C6 16.9(5) . . . 3 ? C27 O1 K1 C5 -130.8(6) . . . 3 ? C30 O1 K1 C5 35.7(5) . . . 3 ? C27 O1 K1 C4 -108.0(6) . . . 3 ? C30 O1 K1 C4 58.6(5) . . . 3 ? C27 O1 K1 C25 148.9(6) . . . . ? C30 O1 K1 C25 -44.6(5) . . . . ? C3 N1 K1 O1 -88.6(3) . . . . ? C1 N1 K1 O1 152.38(18) . . . . ? K2 N1 K1 O1 63.01(12) 3_455 . . . ? C3 N1 K1 N2 172.7(3) . . . . ? C1 N1 K1 N2 53.67(17) . . . . ? K2 N1 K1 N2 -35.70(8) 3_455 . . . ? C3 N1 K1 C1 119.0(4) . . . . ? K2 N1 K1 C1 -89.37(18) 3_455 . . . ? C3 N1 K1 C2 143.8(3) . . . . ? C1 N1 K1 C2 24.77(16) . . . . ? K2 N1 K1 C2 -64.60(11) 3_455 . . . ? C3 N1 K1 C3 37.3(3) . . . 3 ? C1 N1 K1 C3 -81.71(17) . . . 3 ? K2 N1 K1 C3 -171.08(8) 3_455 . . 3 ? C3 N1 K1 C7 81.9(3) . . . 3 ? C1 N1 K1 C7 -37.15(19) . . . 3 ? K2 N1 K1 C7 -126.52(9) 3_455 . . 3 ? C3 N1 K1 C8 63.6(3) . . . 3 ? C1 N1 K1 C8 -55.45(18) . . . 3 ? K2 N1 K1 C8 -144.82(8) 3_455 . . 3 ? C3 N1 K1 C6 78.8(3) . . . 3 ? C1 N1 K1 C6 -40.2(2) . . . 3 ? K2 N1 K1 C6 -129.59(15) 3_455 . . 3 ? C3 N1 K1 C5 35.3(4) . . . 3 ? C1 N1 K1 C5 -83.8(2) . . . 3 ? K2 N1 K1 C5 -173.14(14) 3_455 . . 3 ? C3 N1 K1 C4 22.8(3) . . . 3 ? C1 N1 K1 C4 -96.29(18) . . . 3 ? K2 N1 K1 C4 174.34(8) 3_455 . . 3 ? C3 N1 K1 C25 -179.8(3) . . . . ? C1 N1 K1 C25 61.1(2) . . . . ? K2 N1 K1 C25 -28.25(13) 3_455 . . . ? C9 N2 K1 O1 78.8(3) . . . . ? C2 N2 K1 O1 -161.64(17) . . . . ? K2 N2 K1 O1 -73.79(12) 3_455 . . . ? C9 N2 K1 N1 -173.1(3) . . . . ? C2 N2 K1 N1 -53.58(16) . . . . ? K2 N2 K1 N1 34.26(8) 3_455 . . . ? C9 N2 K1 C1 -143.4(3) . . . . ? C2 N2 K1 C1 -23.84(15) . . . . ? K2 N2 K1 C1 64.01(10) 3_455 . . . ? C9 N2 K1 C2 -119.6(4) . . . . ? K2 N2 K1 C2 87.84(17) 3_455 . . . ? C9 N2 K1 C3 -88.8(3) . . . 3 ? C2 N2 K1 C3 30.7(2) . . . 3 ? K2 N2 K1 C3 118.57(10) 3_455 . . 3 ? C9 N2 K1 C7 -54.8(3) . . . 3 ? C2 N2 K1 C7 64.74(18) . . . 3 ? K2 N2 K1 C7 152.58(10) 3_455 . . 3 ? C9 N2 K1 C8 -78.2(3) . . . 3 ? C2 N2 K1 C8 41.38(18) . . . 3 ? K2 N2 K1 C8 129.23(9) 3_455 . . 3 ? C9 N2 K1 C6 -31.2(3) . . . 3 ? C2 N2 K1 C6 88.32(18) . . . 3 ? K2 N2 K1 C6 176.17(10) 3_455 . . 3 ? C9 N2 K1 C5 -24.2(4) . . . 3 ? C2 N2 K1 C5 95.33(19) . . . 3 ? K2 N2 K1 C5 -176.83(10) 3_455 . . 3 ? C9 N2 K1 C4 -54.5(4) . . . 3 ? C2 N2 K1 C4 65.1(2) . . . 3 ? K2 N2 K1 C4 152.90(14) 3_455 . . 3 ? C9 N2 K1 C25 13.4(3) . . . . ? C2 N2 K1 C25 132.95(18) . . . . ? K2 N2 K1 C25 -139.21(11) 3_455 . . . ? C2 C1 K1 O1 95.4(2) . . . . ? N1 C1 K1 O1 -38.9(2) . . . . ? K2 C1 K1 O1 18.92(19) 3_455 . . . ? C2 C1 K1 N1 134.3(3) . . . . ? K2 C1 K1 N1 57.77(15) 3_455 . . . ? C2 C1 K1 N2 24.50(17) . . . . ? N1 C1 K1 N2 -109.78(19) . . . . ? K2 C1 K1 N2 -52.01(8) 3_455 . . . ? N1 C1 K1 C2 -134.3(3) . . . . ? K2 C1 K1 C2 -76.51(19) 3_455 . . . ? C2 C1 K1 C3 -121.25(19) . . . 3 ? N1 C1 K1 C3 104.47(16) . . . 3 ? K2 C1 K1 C3 162.24(8) 3_455 . . 3 ? C2 C1 K1 C7 -77.1(2) . . . 3 ? N1 C1 K1 C7 148.60(17) . . . 3 ? K2 C1 K1 C7 -153.62(9) 3_455 . . 3 ? C2 C1 K1 C8 -98.80(19) . . . 3 ? N1 C1 K1 C8 126.92(17) . . . 3 ? K2 C1 K1 C8 -175.31(9) 3_455 . . 3 ? C2 C1 K1 C6 -71.1(2) . . . 3 ? N1 C1 K1 C6 154.59(16) . . . 3 ? K2 C1 K1 C6 -147.64(9) 3_455 . . 3 ? C2 C1 K1 C5 -94.9(2) . . . 3 ? N1 C1 K1 C5 130.79(17) . . . 3 ? K2 C1 K1 C5 -171.43(10) 3_455 . . 3 ? C2 C1 K1 C4 -121.68(19) . . . 3 ? N1 C1 K1 C4 104.04(17) . . . 3 ? K2 C1 K1 C4 161.81(8) 3_455 . . 3 ? C2 C1 K1 C25 2.1(2) . . . . ? N1 C1 K1 C25 -132.14(16) . . . . ? K2 C1 K1 C25 -74.37(10) 3_455 . . . ? C1 C2 K1 O1 -112.1(2) . . . . ? N2 C2 K1 O1 24.4(2) . . . . ? K2 C2 K1 O1 -36.45(17) 3_455 . . . ? C1 C2 K1 N1 -26.08(17) . . . . ? N2 C2 K1 N1 110.40(18) . . . . ? K2 C2 K1 N1 49.59(8) 3_455 . . . ? C1 C2 K1 N2 -136.5(3) . . . . ? K2 C2 K1 N2 -60.81(14) 3_455 . . . ? N2 C2 K1 C1 136.5(3) . . . . ? K2 C2 K1 C1 75.67(18) 3_455 . . . ? C1 C2 K1 C3 65.6(2) . . . 3 ? N2 C2 K1 C3 -157.92(15) . . . 3 ? K2 C2 K1 C3 141.27(8) 3_455 . . 3 ? C1 C2 K1 C7 105.0(2) . . . 3 ? N2 C2 K1 C7 -118.57(17) . . . 3 ? K2 C2 K1 C7 -179.38(10) 3_455 . . 3 ? C1 C2 K1 C8 80.98(19) . . . 3 ? N2 C2 K1 C8 -142.54(16) . . . 3 ? K2 C2 K1 C8 156.65(9) 3_455 . . 3 ? C1 C2 K1 C6 120.77(19) . . . 3 ? N2 C2 K1 C6 -102.75(17) . . . 3 ? K2 C2 K1 C6 -163.56(9) 3_455 . . 3 ? C1 C2 K1 C5 111.5(2) . . . 3 ? N2 C2 K1 C5 -111.99(17) . . . 3 ? K2 C2 K1 C5 -172.80(9) 3_455 . . 3 ? C1 C2 K1 C4 79.2(2) . . . 3 ? N2 C2 K1 C4 -144.37(15) . . . 3 ? K2 C2 K1 C4 154.82(9) 3_455 . . 3 ? C1 C2 K1 C25 -178.0(2) . . . . ? N2 C2 K1 C25 -41.51(16) . . . . ? K2 C2 K1 C25 -102.32(10) 3_455 . . . ? C24 C25 K1 O1 -74.6(2) . . . . ? C24 C25 K1 N1 35.0(2) . . . . ? C24 C25 K1 N2 42.39(18) . . . . ? C24 C25 K1 C1 61.3(2) . . . . ? C24 C25 K1 C2 62.3(2) . . . . ? C24 C25 K1 C3 174.27(18) . . . 3 ? C24 C25 K1 C7 154.8(2) . . . 3 ? C24 C25 K1 C8 152.86(19) . . . 3 ? C24 C25 K1 C6 177.2(2) . . . 3 ? C24 C25 K1 C5 -163.0(2) . . . 3 ? C24 C25 K1 C4 -163.63(19) . . . 3 ? C30 O1 C27 C28 -24.7(9) . . . . ? K1 O1 C27 C28 144.1(5) . . . . ? O1 C27 C28 C29 18.7(9) . . . . ? C27 C28 C29 C30 -5.3(8) . . . . ? C27 O1 C30 C29 20.3(8) . . . . ? K1 O1 C30 C29 -148.7(4) . . . . ? C28 C29 C30 O1 -9.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.73 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.357 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.057 ########## data_ZnL2 _database_code_depnum_ccdc_archive 'CCDC 722601' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H48 N4 Zn' _chemical_formula_weight 650.19 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' 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 P2(1)/c 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 30.0006(7) _cell_length_b 7.5969(2) _cell_length_c 16.3834(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.8170(10) _cell_angle_gamma 90.00 _cell_volume 3592.59(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4557 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 28.51 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7677 _exptl_absorpt_correction_T_max 0.8642 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18193 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6295 _reflns_number_gt 4288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0541P)^2^+1.9066P] 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 6295 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Zn Zn 0.247078(10) 0.50226(5) 0.49804(2) 0.03320(12) Uani 1 1 d . . . N1 N 0.21098(8) 0.3408(3) 0.55316(16) 0.0355(6) Uani 1 1 d . . . N2 N 0.29338(8) 0.2997(3) 0.51841(15) 0.0353(6) Uani 1 1 d . . . N3 N 0.29240(8) 0.7079(3) 0.52326(15) 0.0348(6) Uani 1 1 d . . . N4 N 0.21062(8) 0.6609(3) 0.40659(15) 0.0357(6) Uani 1 1 d . . . C1 C 0.23692(11) 0.1997(5) 0.5815(2) 0.0437(8) Uani 1 1 d . . . H1A H 0.2260 0.1128 0.6110 0.052 Uiso 1 1 calc R . . C2 C 0.28017(10) 0.1816(4) 0.5672(2) 0.0412(8) Uani 1 1 d . . . H2A H 0.2996 0.0888 0.5913 0.049 Uiso 1 1 calc R . . C3 C 0.16310(10) 0.3297(4) 0.55091(19) 0.0365(7) Uani 1 1 d . . . C4 C 0.14811(10) 0.3811(4) 0.6211(2) 0.0401(8) Uani 1 1 d . . . C5 C 0.10163(12) 0.3624(5) 0.6175(2) 0.0536(9) Uani 1 1 d . . . H5A H 0.0916 0.3960 0.6642 0.064 Uiso 1 1 calc R . . C6 C 0.06968(11) 0.2957(5) 0.5471(3) 0.0575(10) Uani 1 1 d . . . C7 C 0.08548(12) 0.2498(5) 0.4778(2) 0.0559(10) Uani 1 1 d . . . H7A H 0.0644 0.2068 0.4293 0.067 Uiso 1 1 calc R . . C8 C 0.13134(11) 0.2656(4) 0.4782(2) 0.0425(8) Uani 1 1 d . . . C9 C 0.18155(12) 0.4549(5) 0.6995(2) 0.0555(10) Uani 1 1 d . . . H9A H 0.2121 0.4587 0.6915 0.083 Uiso 1 1 calc R . . H9B H 0.1818 0.3814 0.7472 0.083 Uiso 1 1 calc R . . H9C H 0.1721 0.5718 0.7097 0.083 Uiso 1 1 calc R . . C10 C 0.01965(14) 0.2703(7) 0.5468(3) 0.0947(17) Uani 1 1 d . . . H10A H 0.0025 0.2226 0.4932 0.142 Uiso 1 1 calc R . . H10B H 0.0066 0.3817 0.5557 0.142 Uiso 1 1 calc R . . H10C H 0.0180 0.1906 0.5914 0.142 Uiso 1 1 calc R . . C11 C 0.14633(13) 0.2137(5) 0.4003(2) 0.0582(10) Uani 1 1 d . . . H11A H 0.1199 0.1733 0.3568 0.087 Uiso 1 1 calc R . . H11B H 0.1689 0.1212 0.4147 0.087 Uiso 1 1 calc R . . H11C H 0.1596 0.3138 0.3799 0.087 Uiso 1 1 calc R . . C12 C 0.33672(10) 0.2822(4) 0.50027(19) 0.0348(7) Uani 1 1 d . . . C13 C 0.33696(11) 0.2898(5) 0.4148(2) 0.0451(8) Uani 1 1 d . . . C14 C 0.37866(13) 0.2728(5) 0.3945(2) 0.0585(10) Uani 1 1 d . . . H14A H 0.3787 0.2772 0.3378 0.070 Uiso 1 1 calc R . . C15 C 0.42004(13) 0.2498(6) 0.4554(3) 0.0623(11) Uani 1 1 d . . . C16 C 0.41898(12) 0.2464(5) 0.5390(2) 0.0591(11) Uani 1 1 d . . . H16A H 0.4467 0.2325 0.5809 0.071 Uiso 1 1 calc R . . C17 C 0.37871(11) 0.2626(5) 0.5632(2) 0.0431(8) Uani 1 1 d . . . C18 C 0.29292(13) 0.3162(6) 0.3458(2) 0.0710(13) Uani 1 1 d . . . H18A H 0.2996 0.3165 0.2917 0.107 Uiso 1 1 calc R . . H18B H 0.2792 0.4266 0.3540 0.107 Uiso 1 1 calc R . . H18C H 0.2717 0.2223 0.3474 0.107 Uiso 1 1 calc R . . C19 C 0.46517(15) 0.2324(8) 0.4313(3) 0.105(2) Uani 1 1 d . . . H19A H 0.4903 0.2180 0.4817 0.158 Uiso 1 1 calc R . . H19B H 0.4702 0.3364 0.4018 0.158 Uiso 1 1 calc R . . H19C H 0.4636 0.1317 0.3953 0.158 Uiso 1 1 calc R . . C20 C 0.38168(13) 0.2628(6) 0.6573(2) 0.0608(11) Uani 1 1 d . . . H20A H 0.4133 0.2465 0.6895 0.091 Uiso 1 1 calc R . . H20B H 0.3631 0.1687 0.6695 0.091 Uiso 1 1 calc R . . H20C H 0.3705 0.3731 0.6724 0.091 Uiso 1 1 calc R . . C21 C 0.27891(10) 0.8247(4) 0.46097(19) 0.0417(8) Uani 1 1 d . . . H21A H 0.2980 0.9183 0.4561 0.050 Uiso 1 1 calc R . . C22 C 0.23573(11) 0.8040(4) 0.4033(2) 0.0418(8) Uani 1 1 d . . . H22A H 0.2244 0.8899 0.3625 0.050 Uiso 1 1 calc R . . C23 C 0.33592(10) 0.7287(4) 0.58471(18) 0.0342(7) Uani 1 1 d . . . C24 C 0.33617(11) 0.7213(5) 0.6702(2) 0.0444(8) Uani 1 1 d . . . C25 C 0.37768(12) 0.7416(5) 0.7324(2) 0.0563(10) Uani 1 1 d . . . H25A H 0.3776 0.7377 0.7891 0.068 Uiso 1 1 calc R . . C26 C 0.41910(12) 0.7675(6) 0.7127(2) 0.0602(11) Uani 1 1 d . . . C27 C 0.41813(12) 0.7723(5) 0.6282(2) 0.0564(10) Uani 1 1 d . . . H27A H 0.4458 0.7896 0.6140 0.068 Uiso 1 1 calc R . . C28 C 0.37751(11) 0.7523(4) 0.5635(2) 0.0426(8) Uani 1 1 d . . . C29 C 0.29206(13) 0.6889(6) 0.6952(2) 0.0678(12) Uani 1 1 d . . . H29A H 0.2986 0.6894 0.7559 0.102 Uiso 1 1 calc R . . H29B H 0.2794 0.5767 0.6736 0.102 Uiso 1 1 calc R . . H29C H 0.2701 0.7799 0.6719 0.102 Uiso 1 1 calc R . . C30 C 0.46418(15) 0.7898(8) 0.7821(3) 0.1047(19) Uani 1 1 d . . . H30A H 0.4892 0.8073 0.7568 0.157 Uiso 1 1 calc R . . H30B H 0.4700 0.6862 0.8169 0.157 Uiso 1 1 calc R . . H30C H 0.4618 0.8901 0.8163 0.157 Uiso 1 1 calc R . . C31 C 0.38089(13) 0.7516(6) 0.4726(2) 0.0596(11) Uani 1 1 d . . . H31A H 0.4125 0.7713 0.4723 0.089 Uiso 1 1 calc R . . H31B H 0.3617 0.8433 0.4411 0.089 Uiso 1 1 calc R . . H31C H 0.3707 0.6398 0.4469 0.089 Uiso 1 1 calc R . . C32 C 0.16242(10) 0.6665(4) 0.36054(19) 0.0348(7) Uani 1 1 d . . . C33 C 0.14826(10) 0.6138(4) 0.27555(19) 0.0391(8) Uani 1 1 d . . . C34 C 0.10132(12) 0.6236(5) 0.2330(2) 0.0526(9) Uani 1 1 d . . . H34A H 0.0915 0.5880 0.1766 0.063 Uiso 1 1 calc R . . C35 C 0.06889(11) 0.6845(6) 0.2717(2) 0.0585(10) Uani 1 1 d . . . C36 C 0.08405(12) 0.7344(5) 0.3561(2) 0.0548(10) Uani 1 1 d . . . H36A H 0.0625 0.7749 0.3831 0.066 Uiso 1 1 calc R . . C37 C 0.13027(11) 0.7257(4) 0.4014(2) 0.0408(8) Uani 1 1 d . . . C38 C 0.18233(12) 0.5457(5) 0.2310(2) 0.0543(10) Uani 1 1 d . . . H38A H 0.2129 0.5477 0.2693 0.081 Uiso 1 1 calc R . . H38B H 0.1815 0.6186 0.1828 0.081 Uiso 1 1 calc R . . H38D H 0.1743 0.4271 0.2125 0.081 Uiso 1 1 calc R . . C39 C 0.01827(13) 0.6992(8) 0.2225(3) 0.0961(17) Uani 1 1 d . . . H39A H 0.0008 0.7450 0.2589 0.144 Uiso 1 1 calc R . . H39D H 0.0066 0.5850 0.2023 0.144 Uiso 1 1 calc R . . H39B H 0.0153 0.7770 0.1751 0.144 Uiso 1 1 calc R . . C40 C 0.14463(13) 0.7813(5) 0.4938(2) 0.0566(10) Uani 1 1 d . . . H40D H 0.1177 0.8164 0.5107 0.085 Uiso 1 1 calc R . . H40A H 0.1658 0.8783 0.5009 0.085 Uiso 1 1 calc R . . H40B H 0.1594 0.6843 0.5282 0.085 Uiso 1 1 calc R . . 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 Zn 0.02963(18) 0.0358(2) 0.03364(19) 0.00552(17) 0.00771(13) 0.00052(16) N1 0.0327(13) 0.0362(15) 0.0406(15) 0.0039(12) 0.0150(11) -0.0006(11) N2 0.0338(14) 0.0373(15) 0.0362(15) 0.0027(12) 0.0120(11) 0.0040(12) N3 0.0329(14) 0.0366(15) 0.0334(14) 0.0012(12) 0.0063(11) -0.0036(11) N4 0.0314(13) 0.0384(15) 0.0338(14) 0.0054(12) 0.0026(10) 0.0008(11) C1 0.0463(19) 0.045(2) 0.0431(19) 0.0097(16) 0.0179(15) -0.0013(16) C2 0.0382(17) 0.0403(19) 0.0455(19) 0.0096(16) 0.0121(14) 0.0067(15) C3 0.0371(17) 0.0353(18) 0.0392(18) 0.0044(15) 0.0140(13) -0.0006(14) C4 0.0395(18) 0.042(2) 0.0404(18) 0.0021(15) 0.0143(14) -0.0005(15) C5 0.051(2) 0.064(3) 0.054(2) 0.001(2) 0.0273(17) 0.0011(18) C6 0.0323(18) 0.072(3) 0.068(3) 0.004(2) 0.0150(17) -0.0036(18) C7 0.042(2) 0.070(3) 0.049(2) -0.001(2) 0.0010(16) -0.0097(18) C8 0.0437(19) 0.046(2) 0.0377(18) -0.0014(16) 0.0102(14) -0.0025(15) C9 0.059(2) 0.066(3) 0.044(2) -0.0091(18) 0.0185(17) -0.0065(18) C10 0.045(2) 0.130(5) 0.115(4) 0.004(4) 0.030(2) -0.007(3) C11 0.068(3) 0.065(3) 0.046(2) -0.0085(19) 0.0229(18) -0.015(2) C12 0.0315(16) 0.0378(18) 0.0364(17) 0.0025(14) 0.0114(13) 0.0041(13) C13 0.0428(19) 0.059(2) 0.0344(18) 0.0028(17) 0.0112(14) 0.0033(16) C14 0.056(2) 0.083(3) 0.044(2) 0.008(2) 0.0267(18) 0.014(2) C15 0.042(2) 0.084(3) 0.067(3) 0.013(2) 0.0262(18) 0.0117(19) C16 0.0328(18) 0.086(3) 0.055(2) 0.011(2) 0.0052(16) 0.0101(18) C17 0.0378(19) 0.053(2) 0.0369(18) 0.0000(17) 0.0083(14) 0.0045(15) C18 0.057(2) 0.116(4) 0.037(2) 0.005(2) 0.0054(17) 0.010(2) C19 0.061(3) 0.162(6) 0.110(4) 0.030(4) 0.052(3) 0.027(3) C20 0.054(2) 0.083(3) 0.040(2) -0.001(2) 0.0043(16) 0.008(2) C21 0.0392(18) 0.041(2) 0.0416(19) 0.0066(16) 0.0061(14) -0.0072(15) C22 0.0441(18) 0.042(2) 0.0358(18) 0.0099(15) 0.0050(14) -0.0002(15) C23 0.0301(16) 0.0377(18) 0.0331(16) -0.0002(14) 0.0059(12) -0.0025(13) C24 0.0424(18) 0.055(2) 0.0355(18) -0.0023(16) 0.0111(14) -0.0024(16) C25 0.054(2) 0.082(3) 0.0281(17) 0.0005(19) 0.0041(15) -0.004(2) C26 0.042(2) 0.081(3) 0.048(2) -0.005(2) -0.0046(16) -0.0071(19) C27 0.0323(18) 0.078(3) 0.059(2) -0.002(2) 0.0115(16) -0.0077(17) C28 0.0405(19) 0.049(2) 0.0393(19) -0.0021(16) 0.0125(15) -0.0035(15) C29 0.053(2) 0.113(4) 0.043(2) -0.001(2) 0.0208(17) -0.008(2) C30 0.054(3) 0.167(6) 0.071(3) -0.005(3) -0.019(2) -0.019(3) C31 0.053(2) 0.086(3) 0.047(2) -0.006(2) 0.0241(17) -0.009(2) C32 0.0342(16) 0.0322(17) 0.0353(17) 0.0062(14) 0.0053(13) 0.0005(13) C33 0.0405(18) 0.041(2) 0.0334(17) 0.0026(15) 0.0068(13) 0.0003(14) C34 0.048(2) 0.065(3) 0.0374(19) -0.0010(18) -0.0020(15) 0.0010(18) C35 0.0337(19) 0.077(3) 0.057(2) 0.002(2) -0.0007(16) 0.0023(18) C36 0.0386(19) 0.067(3) 0.061(2) 0.004(2) 0.0185(17) 0.0086(17) C37 0.0412(18) 0.046(2) 0.0353(18) 0.0015(15) 0.0104(14) 0.0057(15) C38 0.057(2) 0.061(3) 0.045(2) -0.0044(18) 0.0157(16) 0.0055(18) C39 0.038(2) 0.139(5) 0.096(4) -0.005(3) -0.008(2) 0.006(3) C40 0.064(2) 0.066(3) 0.040(2) -0.0003(19) 0.0154(17) 0.014(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 Zn N4 2.000(2) . ? Zn N1 2.007(2) . ? Zn N3 2.038(2) . ? Zn N2 2.039(2) . ? N1 C1 1.332(4) . ? N1 C3 1.429(4) . ? N2 C2 1.332(4) . ? N2 C12 1.417(4) . ? N3 C21 1.329(4) . ? N3 C23 1.424(4) . ? N4 C22 1.332(4) . ? N4 C32 1.438(3) . ? C1 C2 1.387(4) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C8 1.394(4) . ? C3 C4 1.400(4) . ? C4 C5 1.387(4) . ? C4 C9 1.506(4) . ? C5 C6 1.380(5) . ? C5 H5A 0.9300 . ? C6 C7 1.389(5) . ? C6 C10 1.512(5) . ? C7 C8 1.379(5) . ? C7 H7A 0.9300 . ? C8 C11 1.518(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C17 1.401(4) . ? C12 C13 1.403(4) . ? C13 C14 1.386(5) . ? C13 C18 1.501(5) . ? C14 C15 1.375(5) . ? C14 H14A 0.9300 . ? C15 C16 1.378(5) . ? C15 C19 1.515(5) . ? C16 C17 1.376(5) . ? C16 H16A 0.9300 . ? C17 C20 1.520(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.388(4) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C28 1.395(4) . ? C23 C24 1.399(4) . ? C24 C25 1.386(5) . ? C24 C29 1.508(5) . ? C25 C26 1.380(5) . ? C25 H25A 0.9300 . ? C26 C27 1.377(5) . ? C26 C30 1.520(5) . ? C27 C28 1.388(5) . ? C27 H27A 0.9300 . ? C28 C31 1.521(5) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 C37 1.390(4) . ? C32 C33 1.399(4) . ? C33 C34 1.393(4) . ? C33 C38 1.501(4) . ? C34 C35 1.379(5) . ? C34 H34A 0.9300 . ? C35 C36 1.385(5) . ? C35 C39 1.517(5) . ? C36 C37 1.384(4) . ? C36 H36A 0.9300 . ? C37 C40 1.517(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38D 0.9600 . ? C39 H39A 0.9600 . ? C39 H39D 0.9600 . ? C39 H39B 0.9600 . ? C40 H40D 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? 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 N4 Zn N1 116.96(10) . . ? N4 Zn N3 83.59(10) . . ? N1 Zn N3 142.14(10) . . ? N4 Zn N2 141.87(10) . . ? N1 Zn N2 83.81(10) . . ? N3 Zn N2 99.11(10) . . ? C1 N1 C3 116.7(3) . . ? C1 N1 Zn 108.3(2) . . ? C3 N1 Zn 133.4(2) . . ? C2 N2 C12 120.2(3) . . ? C2 N2 Zn 107.81(19) . . ? C12 N2 Zn 131.3(2) . . ? C21 N3 C23 119.8(3) . . ? C21 N3 Zn 108.02(19) . . ? C23 N3 Zn 131.4(2) . . ? C22 N4 C32 117.0(2) . . ? C22 N4 Zn 108.78(19) . . ? C32 N4 Zn 132.6(2) . . ? N1 C1 C2 120.4(3) . . ? N1 C1 H1A 119.8 . . ? C2 C1 H1A 119.8 . . ? N2 C2 C1 118.6(3) . . ? N2 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C8 C3 C4 120.1(3) . . ? C8 C3 N1 119.4(3) . . ? C4 C3 N1 120.5(3) . . ? C5 C4 C3 118.8(3) . . ? C5 C4 C9 120.2(3) . . ? C3 C4 C9 121.1(3) . . ? C6 C5 C4 122.3(3) . . ? C6 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? C5 C6 C7 117.5(3) . . ? C5 C6 C10 120.8(4) . . ? C7 C6 C10 121.7(4) . . ? C8 C7 C6 122.4(3) . . ? C8 C7 H7A 118.8 . . ? C6 C7 H7A 118.8 . . ? C7 C8 C3 118.9(3) . . ? C7 C8 C11 119.8(3) . . ? C3 C8 C11 121.3(3) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 119.4(3) . . ? C17 C12 N2 123.2(3) . . ? C13 C12 N2 117.4(3) . . ? C14 C13 C12 119.1(3) . . ? C14 C13 C18 119.9(3) . . ? C12 C13 C18 121.0(3) . . ? C15 C14 C13 122.2(3) . . ? C15 C14 H14A 118.9 . . ? C13 C14 H14A 118.9 . . ? C14 C15 C16 117.5(3) . . ? C14 C15 C19 121.1(4) . . ? C16 C15 C19 121.4(4) . . ? C17 C16 C15 123.0(3) . . ? C17 C16 H16A 118.5 . . ? C15 C16 H16A 118.5 . . ? C16 C17 C12 118.8(3) . . ? C16 C17 C20 118.6(3) . . ? C12 C17 C20 122.6(3) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 118.6(3) . . ? N3 C21 H21A 120.7 . . ? C22 C21 H21A 120.7 . . ? N4 C22 C21 119.9(3) . . ? N4 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C28 C23 C24 119.6(3) . . ? C28 C23 N3 123.3(3) . . ? C24 C23 N3 117.2(3) . . ? C25 C24 C23 119.3(3) . . ? C25 C24 C29 119.8(3) . . ? C23 C24 C29 120.8(3) . . ? C26 C25 C24 122.0(3) . . ? C26 C25 H25A 119.0 . . ? C24 C25 H25A 119.0 . . ? C27 C26 C25 117.7(3) . . ? C27 C26 C30 121.3(4) . . ? C25 C26 C30 121.0(4) . . ? C26 C27 C28 122.6(3) . . ? C26 C27 H27A 118.7 . . ? C28 C27 H27A 118.7 . . ? C27 C28 C23 118.8(3) . . ? C27 C28 C31 118.0(3) . . ? C23 C28 C31 123.1(3) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 120.6(3) . . ? C37 C32 N4 119.2(3) . . ? C33 C32 N4 120.2(3) . . ? C34 C33 C32 118.3(3) . . ? C34 C33 C38 120.3(3) . . ? C32 C33 C38 121.4(3) . . ? C35 C34 C33 122.1(3) . . ? C35 C34 H34A 118.9 . . ? C33 C34 H34A 118.9 . . ? C34 C35 C36 118.1(3) . . ? C34 C35 C39 120.6(4) . . ? C36 C35 C39 121.3(4) . . ? C37 C36 C35 122.0(3) . . ? C37 C36 H36A 119.0 . . ? C35 C36 H36A 119.0 . . ? C36 C37 C32 118.9(3) . . ? C36 C37 C40 119.5(3) . . ? C32 C37 C40 121.7(3) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38D 109.5 . . ? H38A C38 H38D 109.5 . . ? H38B C38 H38D 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39D 109.5 . . ? H39A C39 H39D 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? H39D C39 H39B 109.5 . . ? C37 C40 H40D 109.5 . . ? C37 C40 H40A 109.5 . . ? H40D C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40D C40 H40B 109.5 . . ? H40A C40 H40B 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 N4 Zn N1 C1 152.8(2) . . . . ? N3 Zn N1 C1 -90.5(3) . . . . ? N2 Zn N1 C1 6.4(2) . . . . ? N4 Zn N1 C3 -11.3(3) . . . . ? N3 Zn N1 C3 105.4(3) . . . . ? N2 Zn N1 C3 -157.7(3) . . . . ? N4 Zn N2 C2 -136.1(2) . . . . ? N1 Zn N2 C2 -9.2(2) . . . . ? N3 Zn N2 C2 132.7(2) . . . . ? N4 Zn N2 C12 53.8(3) . . . . ? N1 Zn N2 C12 -179.3(3) . . . . ? N3 Zn N2 C12 -37.4(3) . . . . ? N4 Zn N3 C21 -9.3(2) . . . . ? N1 Zn N3 C21 -136.1(2) . . . . ? N2 Zn N3 C21 132.3(2) . . . . ? N4 Zn N3 C23 -178.9(3) . . . . ? N1 Zn N3 C23 54.3(3) . . . . ? N2 Zn N3 C23 -37.3(3) . . . . ? N1 Zn N4 C22 153.0(2) . . . . ? N3 Zn N4 C22 6.4(2) . . . . ? N2 Zn N4 C22 -90.2(3) . . . . ? N1 Zn N4 C32 -11.8(3) . . . . ? N3 Zn N4 C32 -158.3(3) . . . . ? N2 Zn N4 C32 105.1(3) . . . . ? C3 N1 C1 C2 164.5(3) . . . . ? Zn N1 C1 C2 -2.6(4) . . . . ? C12 N2 C2 C1 -178.0(3) . . . . ? Zn N2 C2 C1 10.6(4) . . . . ? N1 C1 C2 N2 -5.9(5) . . . . ? C1 N1 C3 C8 -89.6(4) . . . . ? Zn N1 C3 C8 73.4(4) . . . . ? C1 N1 C3 C4 89.9(4) . . . . ? Zn N1 C3 C4 -107.1(3) . . . . ? C8 C3 C4 C5 1.7(5) . . . . ? N1 C3 C4 C5 -177.7(3) . . . . ? C8 C3 C4 C9 -178.4(3) . . . . ? N1 C3 C4 C9 2.1(5) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? C9 C4 C5 C6 179.9(4) . . . . ? C4 C5 C6 C7 -1.2(6) . . . . ? C4 C5 C6 C10 177.5(4) . . . . ? C5 C6 C7 C8 1.3(6) . . . . ? C10 C6 C7 C8 -177.4(4) . . . . ? C6 C7 C8 C3 0.1(6) . . . . ? C6 C7 C8 C11 -179.8(4) . . . . ? C4 C3 C8 C7 -1.7(5) . . . . ? N1 C3 C8 C7 177.8(3) . . . . ? C4 C3 C8 C11 178.3(3) . . . . ? N1 C3 C8 C11 -2.3(5) . . . . ? C2 N2 C12 C17 -53.1(4) . . . . ? Zn N2 C12 C17 115.9(3) . . . . ? C2 N2 C12 C13 128.6(3) . . . . ? Zn N2 C12 C13 -62.4(4) . . . . ? C17 C12 C13 C14 1.8(5) . . . . ? N2 C12 C13 C14 -179.9(3) . . . . ? C17 C12 C13 C18 -178.1(4) . . . . ? N2 C12 C13 C18 0.3(5) . . . . ? C12 C13 C14 C15 -0.4(6) . . . . ? C18 C13 C14 C15 179.5(4) . . . . ? C13 C14 C15 C16 -0.9(6) . . . . ? C13 C14 C15 C19 -179.8(4) . . . . ? C14 C15 C16 C17 0.8(6) . . . . ? C19 C15 C16 C17 179.7(4) . . . . ? C15 C16 C17 C12 0.5(6) . . . . ? C15 C16 C17 C20 -178.1(4) . . . . ? C13 C12 C17 C16 -1.8(5) . . . . ? N2 C12 C17 C16 179.9(3) . . . . ? C13 C12 C17 C20 176.8(3) . . . . ? N2 C12 C17 C20 -1.5(5) . . . . ? C23 N3 C21 C22 -178.2(3) . . . . ? Zn N3 C21 C22 10.8(4) . . . . ? C32 N4 C22 C21 164.9(3) . . . . ? Zn N4 C22 C21 -2.6(4) . . . . ? N3 C21 C22 N4 -6.0(5) . . . . ? C21 N3 C23 C28 -52.3(4) . . . . ? Zn N3 C23 C28 116.3(3) . . . . ? C21 N3 C23 C24 129.0(3) . . . . ? Zn N3 C23 C24 -62.4(4) . . . . ? C28 C23 C24 C25 1.5(5) . . . . ? N3 C23 C24 C25 -179.7(3) . . . . ? C28 C23 C24 C29 -177.6(3) . . . . ? N3 C23 C24 C29 1.2(5) . . . . ? C23 C24 C25 C26 -0.6(6) . . . . ? C29 C24 C25 C26 178.5(4) . . . . ? C24 C25 C26 C27 -0.1(6) . . . . ? C24 C25 C26 C30 179.9(4) . . . . ? C25 C26 C27 C28 0.0(6) . . . . ? C30 C26 C27 C28 180.0(4) . . . . ? C26 C27 C28 C23 0.9(6) . . . . ? C26 C27 C28 C31 -177.3(4) . . . . ? C24 C23 C28 C27 -1.7(5) . . . . ? N3 C23 C28 C27 179.7(3) . . . . ? C24 C23 C28 C31 176.4(3) . . . . ? N3 C23 C28 C31 -2.2(5) . . . . ? C22 N4 C32 C37 -90.6(4) . . . . ? Zn N4 C32 C37 73.1(4) . . . . ? C22 N4 C32 C33 89.0(4) . . . . ? Zn N4 C32 C33 -107.2(3) . . . . ? C37 C32 C33 C34 0.5(5) . . . . ? N4 C32 C33 C34 -179.1(3) . . . . ? C37 C32 C33 C38 -178.6(3) . . . . ? N4 C32 C33 C38 1.8(5) . . . . ? C32 C33 C34 C35 0.5(5) . . . . ? C38 C33 C34 C35 179.6(4) . . . . ? C33 C34 C35 C36 -1.0(6) . . . . ? C33 C34 C35 C39 177.9(4) . . . . ? C34 C35 C36 C37 0.4(6) . . . . ? C39 C35 C36 C37 -178.4(4) . . . . ? C35 C36 C37 C32 0.6(6) . . . . ? C35 C36 C37 C40 -179.6(4) . . . . ? C33 C32 C37 C36 -1.0(5) . . . . ? N4 C32 C37 C36 178.6(3) . . . . ? C33 C32 C37 C40 179.2(3) . . . . ? N4 C32 C37 C40 -1.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.480 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.054 ########### data_ZnL2Na2 _database_code_depnum_ccdc_archive 'CCDC 722602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H72 N4 Na2 O2 Zn' _chemical_formula_weight 896.49 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' 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 Orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.267(2) _cell_length_b 12.2088(17) _cell_length_c 12.6174(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2813.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3225 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 20.82 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16206 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.44 _reflns_number_total 6498 _reflns_number_gt 3202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 -0.075 227 54 ' ' 2 1.000 0.500 0.425 227 54 ' ' _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^)+(0.1444P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 6498 _refine_ls_number_parameters 276 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1646 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2530 _refine_ls_wR_factor_gt 0.2028 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.013 _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 Zn Zn 0.5000 0.5000 0.45223(14) 0.0503(3) Uani 1 2 d S . . Na Na 0.41446(18) 0.6411(3) 0.3172(3) 0.0824(10) Uani 1 1 d . . . O O 0.3474(4) 0.7757(6) 0.2462(6) 0.120(2) Uani 1 1 d . . . N1 N 0.4540(3) 0.6403(4) 0.5077(5) 0.0580(15) Uani 1 1 d . . . N2 N 0.5485(3) 0.6106(5) 0.3488(5) 0.0636(16) Uani 1 1 d . . . C1 C 0.4974(3) 0.7310(5) 0.4739(7) 0.060(3) Uani 1 1 d . . . C2 C 0.5446(4) 0.7161(6) 0.3937(7) 0.0671(19) Uani 1 1 d . . . C3 C 0.4801(5) 0.8419(6) 0.5241(9) 0.091(3) Uani 1 1 d . . . H3A H 0.5159 0.8581 0.5776 0.137 Uiso 1 1 calc R . . H3B H 0.4324 0.8396 0.5557 0.137 Uiso 1 1 calc R . . H3C H 0.4813 0.8978 0.4705 0.137 Uiso 1 1 calc R . . C4 C 0.5894(4) 0.8079(6) 0.3438(8) 0.084(2) Uani 1 1 d . . . H4A H 0.6332 0.8193 0.3843 0.125 Uiso 1 1 calc R . . H4B H 0.5610 0.8741 0.3430 0.125 Uiso 1 1 calc R . . H4C H 0.6022 0.7882 0.2725 0.125 Uiso 1 1 calc R . . C5 C 0.4244(4) 0.6504(6) 0.6117(7) 0.063(2) Uani 1 1 d . . . C6 C 0.3491(4) 0.6770(5) 0.6255(7) 0.068(2) Uani 1 1 d . . . C7 C 0.3196(5) 0.6900(6) 0.7227(8) 0.081(2) Uani 1 1 d . . . H7A H 0.2699 0.7049 0.7288 0.097 Uiso 1 1 calc R . . C8 C 0.3600(6) 0.6820(7) 0.8101(9) 0.100(3) Uani 1 1 d . . . C9 C 0.4388(5) 0.6627(8) 0.8009(8) 0.094(3) Uani 1 1 d . . . H9A H 0.4686 0.6601 0.8605 0.113 Uiso 1 1 calc R . . C10 C 0.4673(4) 0.6482(6) 0.6998(7) 0.070(2) Uani 1 1 d . . . C11 C 0.6141(4) 0.5851(5) 0.2879(6) 0.0641(19) Uani 1 1 d . . . C12 C 0.6113(5) 0.5811(7) 0.1780(8) 0.084(2) Uani 1 1 d . . . C13 C 0.6719(6) 0.5478(8) 0.1245(8) 0.092(3) Uani 1 1 d . . . H13A H 0.6695 0.5424 0.0511 0.111 Uiso 1 1 calc R . . C14 C 0.7356(6) 0.5222(8) 0.1731(11) 0.099(3) Uani 1 1 d . . . C15 C 0.7385(4) 0.5331(7) 0.2811(9) 0.082(3) Uani 1 1 d . . . H15A H 0.7824 0.5190 0.3158 0.099 Uiso 1 1 calc R . . C16 C 0.6785(4) 0.5641(6) 0.3400(7) 0.0664(19) Uani 1 1 d . . . C17 C 0.2996(4) 0.6969(7) 0.5294(9) 0.092(3) Uani 1 1 d . . . H17A H 0.2510 0.7139 0.5531 0.139 Uiso 1 1 calc R . . H17B H 0.2983 0.6322 0.4861 0.139 Uiso 1 1 calc R . . H17C H 0.3184 0.7570 0.4887 0.139 Uiso 1 1 calc R . . C18 C 0.3290(8) 0.7019(13) 0.9246(9) 0.159(6) Uani 1 1 d . . . H18A H 0.2770 0.7127 0.9209 0.239 Uiso 1 1 calc R . . H18B H 0.3516 0.7658 0.9545 0.239 Uiso 1 1 calc R . . H18C H 0.3395 0.6395 0.9682 0.239 Uiso 1 1 calc R . . C19 C 0.5500(4) 0.6336(8) 0.6921(9) 0.096(3) Uani 1 1 d . . . H19A H 0.5636 0.6236 0.6192 0.144 Uiso 1 1 calc R . . H19B H 0.5645 0.5706 0.7324 0.144 Uiso 1 1 calc R . . H19C H 0.5740 0.6975 0.7197 0.144 Uiso 1 1 calc R . . C20 C 0.5456(7) 0.6240(10) 0.1195(9) 0.122(4) Uani 1 1 d . . . H20A H 0.5085 0.6448 0.1695 0.183 Uiso 1 1 calc R . . H20B H 0.5268 0.5679 0.0736 0.183 Uiso 1 1 calc R . . H20C H 0.5595 0.6866 0.0781 0.183 Uiso 1 1 calc R . . C21 C 0.8029(7) 0.4836(11) 0.1101(13) 0.145(6) Uani 1 1 d . . . H21A H 0.8431 0.4720 0.1578 0.217 Uiso 1 1 calc R . . H21B H 0.8160 0.5384 0.0590 0.217 Uiso 1 1 calc R . . H21C H 0.7916 0.4163 0.0744 0.217 Uiso 1 1 calc R . . C22 C 0.6827(4) 0.5806(6) 0.4618(9) 0.081(2) Uani 1 1 d . . . H22A H 0.7310 0.5624 0.4862 0.121 Uiso 1 1 calc R . . H22B H 0.6476 0.5338 0.4958 0.121 Uiso 1 1 calc R . . H22C H 0.6721 0.6556 0.4787 0.121 Uiso 1 1 calc R . . C23 C 0.3758(9) 0.8826(12) 0.245(2) 0.233(12) Uani 1 1 d . . . H23A H 0.4044 0.8960 0.3082 0.280 Uiso 1 1 calc R . . H23B H 0.4071 0.8927 0.1835 0.280 Uiso 1 1 calc R . . C24 C 0.3161(10) 0.9548(13) 0.240(2) 0.221(10) Uani 1 1 d . . . H24A H 0.3165 0.9941 0.1734 0.265 Uiso 1 1 calc R . . H24B H 0.3195 1.0079 0.2972 0.265 Uiso 1 1 calc R . . C25 C 0.2481(7) 0.8915(11) 0.2503(17) 0.167(6) Uani 1 1 d . . . H25A H 0.2289 0.8943 0.3219 0.200 Uiso 1 1 calc R . . H25B H 0.2110 0.9168 0.2011 0.200 Uiso 1 1 calc R . . C26 C 0.2740(7) 0.7817(9) 0.2231(12) 0.135(4) Uani 1 1 d . . . H26A H 0.2473 0.7272 0.2636 0.162 Uiso 1 1 calc R . . H26B H 0.2661 0.7676 0.1484 0.162 Uiso 1 1 calc R . . 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 Zn 0.0438(4) 0.0326(4) 0.0744(6) 0.000 0.000 0.0004(4) Na 0.0741(19) 0.0623(18) 0.111(3) 0.0100(19) -0.0143(19) 0.0067(15) O 0.117(5) 0.088(5) 0.154(7) 0.028(5) -0.023(5) 0.020(4) N1 0.048(3) 0.036(3) 0.089(4) 0.000(3) 0.006(3) 0.002(2) N2 0.060(3) 0.043(3) 0.088(5) -0.003(3) 0.018(3) -0.010(2) C1 0.060(4) 0.037(3) 0.083(8) -0.002(3) 0.004(4) 0.000(3) C2 0.057(4) 0.043(4) 0.101(6) 0.003(4) 0.007(4) -0.006(3) C3 0.087(5) 0.037(4) 0.149(8) -0.011(5) 0.024(5) -0.002(4) C4 0.085(5) 0.045(4) 0.121(7) 0.016(4) 0.010(5) -0.010(4) C5 0.061(4) 0.046(4) 0.080(6) 0.005(4) 0.008(4) 0.009(3) C6 0.067(4) 0.041(4) 0.095(6) -0.006(4) 0.010(4) 0.002(3) C7 0.086(6) 0.062(5) 0.094(7) 0.005(5) 0.029(6) 0.005(4) C8 0.113(7) 0.077(6) 0.111(8) -0.001(6) 0.055(7) 0.018(5) C9 0.104(6) 0.093(7) 0.086(7) -0.005(5) 0.002(5) 0.020(5) C10 0.060(4) 0.067(4) 0.084(6) -0.012(4) 0.001(4) 0.014(4) C11 0.065(4) 0.046(4) 0.081(6) 0.003(4) 0.017(4) 0.002(3) C12 0.090(6) 0.073(5) 0.087(6) 0.004(5) 0.021(5) -0.016(4) C13 0.104(7) 0.077(6) 0.097(7) 0.005(5) 0.030(6) -0.006(6) C14 0.099(7) 0.076(7) 0.123(9) -0.014(5) 0.056(7) -0.021(5) C15 0.061(4) 0.069(5) 0.116(8) 0.002(5) 0.025(5) -0.009(4) C16 0.056(4) 0.055(4) 0.088(6) 0.004(4) 0.006(4) -0.011(3) C17 0.065(5) 0.066(5) 0.146(9) 0.000(6) 0.000(5) 0.011(4) C18 0.195(13) 0.176(13) 0.107(11) 0.012(8) 0.056(9) 0.073(11) C19 0.074(5) 0.099(7) 0.116(8) -0.032(6) -0.010(5) 0.014(5) C20 0.145(10) 0.140(10) 0.081(7) 0.029(7) -0.026(7) 0.005(8) C21 0.103(9) 0.152(13) 0.180(14) -0.024(9) 0.076(9) -0.021(7) C22 0.063(4) 0.071(4) 0.110(7) 0.003(6) -0.002(5) -0.009(3) C23 0.156(11) 0.111(10) 0.43(3) 0.104(15) -0.110(17) 0.005(9) C24 0.195(17) 0.078(8) 0.39(3) 0.000(15) -0.079(19) -0.002(11) C25 0.108(9) 0.115(10) 0.277(19) -0.016(11) -0.047(11) 0.008(7) C26 0.134(9) 0.083(7) 0.189(12) 0.009(8) -0.074(9) 0.002(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 Zn N1 2.032(5) . ? Zn N1 2.032(5) 2_665 ? Zn N2 2.077(6) 2_665 ? Zn N2 2.077(6) . ? Zn Na 2.883(4) . ? Zn Na 2.883(4) 2_665 ? Na O 2.236(7) . ? Na N2 2.509(7) . ? Na N1 2.510(7) . ? Na C1 2.722(9) . ? Na C2 2.724(8) . ? Na C11 2.835(7) 2_665 ? Na C16 3.041(8) 2_665 ? O C26 1.374(11) . ? O C23 1.404(15) . ? N1 C1 1.427(8) . ? N1 C5 1.426(10) . ? N2 C2 1.409(9) . ? N2 C11 1.456(9) . ? C1 C2 1.341(11) . ? C1 C3 1.528(10) . ? C2 C4 1.525(10) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.360(11) . ? C5 C6 1.424(10) . ? C6 C7 1.349(11) . ? C6 C17 1.533(12) . ? C7 C8 1.329(14) . ? C7 H7A 0.9300 . ? C8 C9 1.464(14) . ? C8 C18 1.570(15) . ? C9 C10 1.389(12) . ? C9 H9A 0.9300 . ? C10 C19 1.524(11) . ? C11 C16 1.372(10) . ? C11 C12 1.389(12) . ? C11 Na 2.835(7) 2_665 ? C12 C13 1.358(12) . ? C12 C20 1.503(14) . ? C13 C14 1.352(15) . ? C13 H13A 0.9300 . ? C14 C15 1.369(15) . ? C14 C21 1.538(14) . ? C15 C16 1.376(10) . ? C15 H15A 0.9300 . ? C16 C22 1.551(13) . ? C16 Na 3.041(8) 2_665 ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.40(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.47(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.462(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? 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 Zn N1 139.7(4) . 2_665 ? N1 Zn N2 126.0(2) . 2_665 ? N1 Zn N2 81.1(2) 2_665 2_665 ? N1 Zn N2 81.1(2) . . ? N1 Zn N2 126.0(2) 2_665 . ? N2 Zn N2 102.1(3) 2_665 . ? N1 Zn Na 58.39(19) . . ? N1 Zn Na 158.62(19) 2_665 . ? N2 Zn Na 77.64(18) 2_665 . ? N2 Zn Na 58.09(19) . . ? N1 Zn Na 158.62(19) . 2_665 ? N1 Zn Na 58.39(19) 2_665 2_665 ? N2 Zn Na 58.09(19) 2_665 2_665 ? N2 Zn Na 77.64(18) . 2_665 ? Na Zn Na 107.55(17) . 2_665 ? O Na N2 135.0(3) . . ? O Na N1 123.0(3) . . ? N2 Na N1 64.3(2) . . ? O Na C1 107.4(3) . . ? N2 Na C1 53.2(2) . . ? N1 Na C1 31.3(2) . . ? O Na C2 111.9(3) . . ? N2 Na C2 30.9(2) . . ? N1 Na C2 53.9(2) . . ? C1 Na C2 28.5(2) . . ? O Na C11 124.2(3) . 2_665 ? N2 Na C11 93.2(2) . 2_665 ? N1 Na C11 100.0(2) . 2_665 ? C1 Na C11 126.1(2) . 2_665 ? C2 Na C11 122.3(2) . 2_665 ? O Na Zn 166.5(3) . . ? N2 Na Zn 44.65(15) . . ? N1 Na Zn 43.58(13) . . ? C1 Na Zn 60.66(16) . . ? C2 Na Zn 61.20(17) . . ? C11 Na Zn 66.08(15) 2_665 . ? O Na C16 109.7(3) . 2_665 ? N2 Na C16 114.1(2) . 2_665 ? N1 Na C16 93.8(2) . 2_665 ? C1 Na C16 125.1(3) . 2_665 ? C2 Na C16 136.9(2) . 2_665 ? C11 Na C16 26.7(2) 2_665 2_665 ? Zn Na C16 75.78(16) . 2_665 ? C26 O C23 107.9(8) . . ? C26 O Na 131.2(7) . . ? C23 O Na 119.1(7) . . ? C1 N1 C5 114.7(6) . . ? C1 N1 Zn 108.8(4) . . ? C5 N1 Zn 123.2(4) . . ? C1 N1 Na 82.6(5) . . ? C5 N1 Na 140.6(4) . . ? Zn N1 Na 78.0(2) . . ? C2 N2 C11 116.8(6) . . ? C2 N2 Zn 108.6(5) . . ? C11 N2 Zn 122.9(4) . . ? C2 N2 Na 83.0(4) . . ? C11 N2 Na 138.6(5) . . ? Zn N2 Na 77.27(19) . . ? C2 C1 N1 118.4(6) . . ? C2 C1 C3 124.4(6) . . ? N1 C1 C3 116.7(6) . . ? C2 C1 Na 75.8(5) . . ? N1 C1 Na 66.1(4) . . ? C3 C1 Na 122.9(5) . . ? C1 C2 N2 117.5(6) . . ? C1 C2 C4 123.8(7) . . ? N2 C2 C4 118.5(7) . . ? C1 C2 Na 75.7(4) . . ? N2 C2 Na 66.1(4) . . ? C4 C2 Na 124.7(6) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 117.5(8) . . ? C10 C5 N1 122.1(7) . . ? C6 C5 N1 119.9(7) . . ? C7 C6 C5 121.5(8) . . ? C7 C6 C17 117.7(7) . . ? C5 C6 C17 120.7(7) . . ? C8 C7 C6 121.6(8) . . ? C8 C7 H7A 119.2 . . ? C6 C7 H7A 119.2 . . ? C7 C8 C9 119.4(9) . . ? C7 C8 C18 123.5(9) . . ? C9 C8 C18 116.9(11) . . ? C10 C9 C8 117.6(9) . . ? C10 C9 H9A 121.2 . . ? C8 C9 H9A 121.2 . . ? C5 C10 C9 122.1(7) . . ? C5 C10 C19 121.4(8) . . ? C9 C10 C19 116.5(8) . . ? C16 C11 C12 120.2(7) . . ? C16 C11 N2 119.5(7) . . ? C12 C11 N2 120.3(7) . . ? C16 C11 Na 85.0(4) . 2_665 ? C12 C11 Na 95.1(5) . 2_665 ? N2 C11 Na 89.3(4) . 2_665 ? C13 C12 C11 118.5(9) . . ? C13 C12 C20 120.7(10) . . ? C11 C12 C20 120.4(8) . . ? C14 C13 C12 123.0(10) . . ? C14 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C13 C14 C15 117.5(9) . . ? C13 C14 C21 121.6(13) . . ? C15 C14 C21 120.9(13) . . ? C14 C15 C16 122.2(9) . . ? C14 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? C11 C16 C15 118.3(8) . . ? C11 C16 C22 119.5(6) . . ? C15 C16 C22 122.1(7) . . ? C11 C16 Na 68.2(4) . 2_665 ? C15 C16 Na 99.6(5) . 2_665 ? C22 C16 Na 103.2(4) . 2_665 ? C6 C17 H17A 109.5 . . ? C6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C8 C18 H18A 109.5 . . ? C8 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C8 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C10 C19 H19A 109.5 . . ? C10 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C10 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C12 C20 H20A 109.5 . . ? C12 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C12 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 109.5 . . ? C14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 O 107.4(13) . . ? C24 C23 H23A 110.2 . . ? O C23 H23A 110.2 . . ? C24 C23 H23B 110.2 . . ? O C23 H23B 110.2 . . ? H23A C23 H23B 108.5 . . ? C23 C24 C25 108.8(14) . . ? C23 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? C23 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C26 C25 C24 100.8(12) . . ? C26 C25 H25A 111.6 . . ? C24 C25 H25A 111.6 . . ? C26 C25 H25B 111.6 . . ? C24 C25 H25B 111.6 . . ? H25A C25 H25B 109.4 . . ? O C26 C25 108.4(9) . . ? O C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? 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 N1 Zn Na O 4.4(11) . . . . ? N1 Zn Na O 156.6(11) 2_665 . . . ? N2 Zn Na O 151.7(11) 2_665 . . . ? N2 Zn Na O -95.3(11) . . . . ? Na Zn Na O -157.8(11) 2_665 . . . ? N1 Zn Na N2 99.7(3) . . . . ? N1 Zn Na N2 -108.1(5) 2_665 . . . ? N2 Zn Na N2 -113.0(3) 2_665 . . . ? Na Zn Na N2 -62.5(2) 2_665 . . . ? N1 Zn Na N1 152.2(4) 2_665 . . . ? N2 Zn Na N1 147.3(2) 2_665 . . . ? N2 Zn Na N1 -99.7(3) . . . . ? Na Zn Na N1 -162.2(2) 2_665 . . . ? N1 Zn Na C1 33.8(2) . . . . ? N1 Zn Na C1 -174.0(5) 2_665 . . . ? N2 Zn Na C1 -178.9(3) 2_665 . . . ? N2 Zn Na C1 -65.9(3) . . . . ? Na Zn Na C1 -128.41(19) 2_665 . . . ? N1 Zn Na C2 66.5(3) . . . . ? N1 Zn Na C2 -141.2(5) 2_665 . . . ? N2 Zn Na C2 -146.1(3) 2_665 . . . ? N2 Zn Na C2 -33.2(3) . . . . ? Na Zn Na C2 -95.7(2) 2_665 . . . ? N1 Zn Na C11 -137.9(3) . . . 2_665 ? N1 Zn Na C11 14.3(5) 2_665 . . 2_665 ? N2 Zn Na C11 9.4(2) 2_665 . . 2_665 ? N2 Zn Na C11 122.4(3) . . . 2_665 ? Na Zn Na C11 59.89(19) 2_665 . . 2_665 ? N1 Zn Na C16 -111.5(2) . . . 2_665 ? N1 Zn Na C16 40.7(5) 2_665 . . 2_665 ? N2 Zn Na C16 35.8(2) 2_665 . . 2_665 ? N2 Zn Na C16 148.8(3) . . . 2_665 ? Na Zn Na C16 86.29(18) 2_665 . . 2_665 ? N2 Na O C26 173.3(10) . . . . ? N1 Na O C26 -101.4(11) . . . . ? C1 Na O C26 -131.7(11) . . . . ? C2 Na O C26 -161.7(10) . . . . ? C11 Na O C26 32.4(12) 2_665 . . . ? Zn Na O C26 -105.0(14) . . . . ? C16 Na O C26 7.1(11) 2_665 . . . ? N2 Na O C23 -24.2(15) . . . . ? N1 Na O C23 61.0(14) . . . . ? C1 Na O C23 30.8(14) . . . . ? C2 Na O C23 0.8(14) . . . . ? C11 Na O C23 -165.1(14) 2_665 . . . ? Zn Na O C23 57.4(18) . . . . ? C16 Na O C23 169.5(14) 2_665 . . . ? N1 Zn N1 C1 117.4(5) 2_665 . . . ? N2 Zn N1 C1 -118.5(5) 2_665 . . . ? N2 Zn N1 C1 -19.9(5) . . . . ? Na Zn N1 C1 -77.8(5) . . . . ? Na Zn N1 C1 -24.7(8) 2_665 . . . ? N1 Zn N1 C5 -21.2(5) 2_665 . . . ? N2 Zn N1 C5 102.9(6) 2_665 . . . ? N2 Zn N1 C5 -158.5(6) . . . . ? Na Zn N1 C5 143.6(6) . . . . ? Na Zn N1 C5 -163.4(5) 2_665 . . . ? N1 Zn N1 Na -164.78(16) 2_665 . . . ? N2 Zn N1 Na -40.7(3) 2_665 . . . ? N2 Zn N1 Na 57.9(2) . . . . ? Na Zn N1 Na 53.0(5) 2_665 . . . ? O Na N1 C1 -67.7(4) . . . . ? N2 Na N1 C1 60.8(3) . . . . ? C2 Na N1 C1 26.7(3) . . . . ? C11 Na N1 C1 149.6(3) 2_665 . . . ? Zn Na N1 C1 111.1(4) . . . . ? C16 Na N1 C1 175.8(3) 2_665 . . . ? O Na N1 C5 52.7(7) . . . . ? N2 Na N1 C5 -178.8(7) . . . . ? C1 Na N1 C5 120.4(8) . . . . ? C2 Na N1 C5 147.1(7) . . . . ? C11 Na N1 C5 -90.1(7) 2_665 . . . ? Zn Na N1 C5 -128.5(7) . . . . ? C16 Na N1 C5 -63.9(6) 2_665 . . . ? O Na N1 Zn -178.8(3) . . . . ? N2 Na N1 Zn -50.25(18) . . . . ? C1 Na N1 Zn -111.1(4) . . . . ? C2 Na N1 Zn -84.4(2) . . . . ? C11 Na N1 Zn 38.5(2) 2_665 . . . ? C16 Na N1 Zn 64.7(2) 2_665 . . . ? N1 Zn N2 C2 19.8(5) . . . . ? N1 Zn N2 C2 -127.4(5) 2_665 . . . ? N2 Zn N2 C2 144.9(5) 2_665 . . . ? Na Zn N2 C2 78.0(5) . . . . ? Na Zn N2 C2 -162.0(5) 2_665 . . . ? N1 Zn N2 C11 161.5(6) . . . . ? N1 Zn N2 C11 14.3(7) 2_665 . . . ? N2 Zn N2 C11 -73.4(5) 2_665 . . . ? Na Zn N2 C11 -140.4(6) . . . . ? Na Zn N2 C11 -20.4(5) 2_665 . . . ? N1 Zn N2 Na -58.2(2) . . . . ? N1 Zn N2 Na 154.6(2) 2_665 . . . ? N2 Zn N2 Na 66.92(17) 2_665 . . . ? Na Zn N2 Na 120.01(19) 2_665 . . . ? O Na N2 C2 49.9(6) . . . . ? N1 Na N2 C2 -62.0(4) . . . . ? C1 Na N2 C2 -27.5(4) . . . . ? C11 Na N2 C2 -161.6(5) 2_665 . . . ? Zn Na N2 C2 -110.9(5) . . . . ? C16 Na N2 C2 -144.3(5) 2_665 . . . ? O Na N2 C11 -73.3(7) . . . . ? N1 Na N2 C11 174.8(7) . . . . ? C1 Na N2 C11 -150.6(7) . . . . ? C2 Na N2 C11 -123.2(8) . . . . ? C11 Na N2 C11 75.3(6) 2_665 . . . ? Zn Na N2 C11 125.9(7) . . . . ? C16 Na N2 C11 92.5(7) 2_665 . . . ? O Na N2 Zn 160.9(4) . . . . ? N1 Na N2 Zn 48.96(19) . . . . ? C1 Na N2 Zn 83.5(3) . . . . ? C2 Na N2 Zn 110.9(5) . . . . ? C11 Na N2 Zn -50.6(2) 2_665 . . . ? C16 Na N2 Zn -33.4(3) 2_665 . . . ? C5 N1 C1 C2 160.1(7) . . . . ? Zn N1 C1 C2 17.6(9) . . . . ? Na N1 C1 C2 -57.0(7) . . . . ? C5 N1 C1 C3 -26.6(10) . . . . ? Zn N1 C1 C3 -169.1(6) . . . . ? Na N1 C1 C3 116.3(7) . . . . ? C5 N1 C1 Na -142.9(5) . . . . ? Zn N1 C1 Na 74.6(3) . . . . ? O Na C1 C2 -104.0(5) . . . . ? N2 Na C1 C2 29.7(4) . . . . ? N1 Na C1 C2 130.5(6) . . . . ? C11 Na C1 C2 92.3(5) 2_665 . . . ? Zn Na C1 C2 82.9(4) . . . . ? C16 Na C1 C2 125.3(4) 2_665 . . . ? O Na C1 N1 125.6(4) . . . . ? N2 Na C1 N1 -100.8(4) . . . . ? C2 Na C1 N1 -130.5(6) . . . . ? C11 Na C1 N1 -38.1(4) 2_665 . . . ? Zn Na C1 N1 -47.5(3) . . . . ? C16 Na C1 N1 -5.2(4) 2_665 . . . ? O Na C1 C3 18.1(7) . . . . ? N2 Na C1 C3 151.8(7) . . . . ? N1 Na C1 C3 -107.4(7) . . . . ? C2 Na C1 C3 122.1(8) . . . . ? C11 Na C1 C3 -145.6(6) 2_665 . . . ? Zn Na C1 C3 -155.0(7) . . . . ? C16 Na C1 C3 -112.6(6) 2_665 . . . ? N1 C1 C2 N2 -0.6(11) . . . . ? C3 C1 C2 N2 -173.3(7) . . . . ? Na C1 C2 N2 -52.9(6) . . . . ? N1 C1 C2 C4 174.6(7) . . . . ? C3 C1 C2 C4 2.0(13) . . . . ? Na C1 C2 C4 122.4(8) . . . . ? N1 C1 C2 Na 52.3(6) . . . . ? C3 C1 C2 Na -120.4(8) . . . . ? C11 N2 C2 C1 -160.6(7) . . . . ? Zn N2 C2 C1 -16.3(8) . . . . ? Na N2 C2 C1 57.7(7) . . . . ? C11 N2 C2 C4 23.9(10) . . . . ? Zn N2 C2 C4 168.2(6) . . . . ? Na N2 C2 C4 -117.8(7) . . . . ? C11 N2 C2 Na 141.7(6) . . . . ? Zn N2 C2 Na -74.0(3) . . . . ? O Na C2 C1 86.4(5) . . . . ? N2 Na C2 C1 -129.3(7) . . . . ? N1 Na C2 C1 -29.3(4) . . . . ? C11 Na C2 C1 -107.4(5) 2_665 . . . ? Zn Na C2 C1 -80.8(4) . . . . ? C16 Na C2 C1 -78.0(5) 2_665 . . . ? O Na C2 N2 -144.3(5) . . . . ? N1 Na C2 N2 100.0(4) . . . . ? C1 Na C2 N2 129.3(7) . . . . ? C11 Na C2 N2 21.9(6) 2_665 . . . ? Zn Na C2 N2 48.5(4) . . . . ? C16 Na C2 N2 51.3(6) 2_665 . . . ? O Na C2 C4 -35.1(8) . . . . ? N2 Na C2 C4 109.2(9) . . . . ? N1 Na C2 C4 -150.8(7) . . . . ? C1 Na C2 C4 -121.5(8) . . . . ? C11 Na C2 C4 131.2(6) 2_665 . . . ? Zn Na C2 C4 157.7(7) . . . . ? C16 Na C2 C4 160.5(6) 2_665 . . . ? C1 N1 C5 C10 -68.4(9) . . . . ? Zn N1 C5 C10 68.1(9) . . . . ? Na N1 C5 C10 -178.0(5) . . . . ? C1 N1 C5 C6 103.8(7) . . . . ? Zn N1 C5 C6 -119.7(6) . . . . ? Na N1 C5 C6 -5.8(10) . . . . ? C10 C5 C6 C7 -5.7(11) . . . . ? N1 C5 C6 C7 -178.3(7) . . . . ? C10 C5 C6 C17 171.4(7) . . . . ? N1 C5 C6 C17 -1.1(10) . . . . ? C5 C6 C7 C8 2.1(12) . . . . ? C17 C6 C7 C8 -175.1(8) . . . . ? C6 C7 C8 C9 2.3(13) . . . . ? C6 C7 C8 C18 177.0(10) . . . . ? C7 C8 C9 C10 -3.0(14) . . . . ? C18 C8 C9 C10 -178.1(10) . . . . ? C6 C5 C10 C9 4.9(12) . . . . ? N1 C5 C10 C9 177.3(8) . . . . ? C6 C5 C10 C19 -172.9(6) . . . . ? N1 C5 C10 C19 -0.6(11) . . . . ? C8 C9 C10 C5 -0.8(13) . . . . ? C8 C9 C10 C19 177.2(8) . . . . ? C2 N2 C11 C16 75.1(9) . . . . ? Zn N2 C11 C16 -63.7(8) . . . . ? Na N2 C11 C16 -173.4(5) . . . . ? C2 N2 C11 C12 -105.4(8) . . . . ? Zn N2 C11 C12 115.8(7) . . . . ? Na N2 C11 C12 6.1(11) . . . . ? C2 N2 C11 Na 159.0(6) . . . 2_665 ? Zn N2 C11 Na 20.2(5) . . . 2_665 ? Na N2 C11 Na -89.5(6) . . . 2_665 ? C16 C11 C12 C13 5.1(12) . . . . ? N2 C11 C12 C13 -174.4(7) . . . . ? Na C11 C12 C13 -82.1(8) 2_665 . . . ? C16 C11 C12 C20 -168.6(8) . . . . ? N2 C11 C12 C20 11.9(12) . . . . ? Na C11 C12 C20 104.2(8) 2_665 . . . ? C11 C12 C13 C14 -2.5(14) . . . . ? C20 C12 C13 C14 171.1(10) . . . . ? C12 C13 C14 C15 -1.3(15) . . . . ? C12 C13 C14 C21 179.3(9) . . . . ? C13 C14 C15 C16 2.8(14) . . . . ? C21 C14 C15 C16 -177.9(8) . . . . ? C12 C11 C16 C15 -3.8(11) . . . . ? N2 C11 C16 C15 175.8(6) . . . . ? Na C11 C16 C15 89.3(7) 2_665 . . . ? C12 C11 C16 C22 173.7(7) . . . . ? N2 C11 C16 C22 -6.8(9) . . . . ? Na C11 C16 C22 -93.2(6) 2_665 . . . ? C12 C11 C16 Na -93.1(7) . . . 2_665 ? N2 C11 C16 Na 86.4(5) . . . 2_665 ? C14 C15 C16 C11 -0.3(12) . . . . ? C14 C15 C16 C22 -177.7(8) . . . . ? C14 C15 C16 Na 70.1(9) . . . 2_665 ? C26 O C23 C24 11(3) . . . . ? Na O C23 C24 -155.4(16) . . . . ? O C23 C24 C25 6(3) . . . . ? C23 C24 C25 C26 -19(3) . . . . ? C23 O C26 C25 -23.7(19) . . . . ? Na O C26 C25 140.2(11) . . . . ? C24 C25 C26 O 25.9(19) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.446 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.150 ########END