Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Dr Qingdao Zeng' _publ_contact_author_address ; Institute of Chemistry Center for Molecular Science Beijing B 100080 CHINA ; _publ_contact_author_email STMZQD@ICCAS.AC.CN _publ_section_title ; Bipyridine conformation controls the solid-state supramolecular chemistry of zinc(II) phthalocyanine with bipyridines ; loop_ _publ_author_name 'Qingdao Zeng' 'Chunli Bai' 'Yan Li' 'Baocheng Ma' 'Hongwei Ma' ; Chun-Ying Shu ; 'Chen Wang' 'Dongxia Wu' data_c _database_code_depnum_ccdc_archive 'CCDC 249308' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H44 N18 O0.96 Zn2' _chemical_formula_weight 1355.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 29.649(6) _cell_length_b 21.016(4) _cell_length_c 12.252(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.14(3) _cell_angle_gamma 90.00 _cell_volume 7629(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27686 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2775 _exptl_absorpt_coefficient_mu 0.682 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6737 _exptl_absorpt_correction_T_max 0.8812 _exptl_absorpt_process_details Abscor _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Raxis Rapid IP Area Detector' _diffrn_measurement_method '\w oscillation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27686 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8810 _reflns_number_gt 5295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid Auto(Rigaku 2001)' _computing_cell_refinement 'Rapid Auto(Rigaku 2001)' _computing_data_reduction 'Rapid Auto(Rigaku 2001)' _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^)+(0.1478P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(6) _refine_ls_number_reflns 8810 _refine_ls_number_parameters 786 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1197 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2265 _refine_ls_wR_factor_gt 0.2050 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.11753(3) 0.85118(5) 0.08743(8) 0.0540(3) Uani 1 1 d . . . Zn2 Zn -0.19516(3) 1.30062(6) 0.30561(8) 0.0555(3) Uani 1 1 d . . . N1 N 0.0991(2) 0.7663(4) 0.1521(7) 0.0603(19) Uani 1 1 d . . . N2 N 0.1284(3) 0.7792(4) 0.3347(6) 0.0575(18) Uani 1 1 d . . . N3 N 0.1587(2) 0.8623(4) 0.2213(6) 0.0545(17) Uani 1 1 d . . . N4 N 0.2035(2) 0.9517(4) 0.1640(6) 0.0555(17) Uani 1 1 d . . . N5 N 0.1586(3) 0.9128(3) 0.0125(6) 0.0526(16) Uani 1 1 d . . . N6 N 0.1320(3) 0.8970(4) -0.1769(6) 0.0618(19) Uani 1 1 d . . . N7 N 0.0992(2) 0.8162(4) -0.0632(6) 0.0583(18) Uani 1 1 d . . . N8 N 0.0625(2) 0.7176(4) -0.0122(6) 0.0555(17) Uani 1 1 d . . . N11 N -0.2380(2) 1.2424(4) 0.3866(6) 0.0600(19) Uani 1 1 d . . . N12 N -0.2089(3) 1.2574(4) 0.5710(6) 0.067(2) Uani 1 1 d . . . N13 N -0.1737(3) 1.3352(4) 0.4519(6) 0.0616(19) Uani 1 1 d . . . N14 N -0.1329(3) 1.4281(4) 0.3949(7) 0.071(2) Uani 1 1 d . . . N15 N -0.1727(3) 1.3825(4) 0.2402(6) 0.0616(19) Uani 1 1 d . . . N16 N -0.2057(3) 1.3716(4) 0.0569(7) 0.064(2) Uani 1 1 d . . . N17 N -0.2375(2) 1.2918(4) 0.1728(6) 0.0585(18) Uani 1 1 d . . . N18 N -0.2843(3) 1.2027(4) 0.2335(7) 0.0606(19) Uani 1 1 d . . . C1 C 0.0740(3) 0.7200(4) 0.0930(7) 0.052(2) Uani 1 1 d . . . C2 C 0.0650(3) 0.6698(5) 0.1727(9) 0.066(2) Uani 1 1 d . . . C3 C 0.0408(4) 0.6130(5) 0.1604(10) 0.077(3) Uani 1 1 d . . . H3A H 0.0293 0.6000 0.0924 0.093 Uiso 1 1 calc R . . C4 C 0.0344(4) 0.5765(5) 0.2545(11) 0.079(3) Uani 1 1 d . . . H4B H 0.0183 0.5385 0.2492 0.095 Uiso 1 1 calc R . . C5 C 0.0515(4) 0.5961(5) 0.3533(10) 0.076(3) Uani 1 1 d . . . H5A H 0.0470 0.5710 0.4144 0.092 Uiso 1 1 calc R . . C6 C 0.0746(4) 0.6501(5) 0.3654(9) 0.073(3) Uani 1 1 d . . . H6B H 0.0857 0.6627 0.4340 0.087 Uiso 1 1 calc R . . C7 C 0.0820(3) 0.6884(5) 0.2713(7) 0.059(2) Uani 1 1 d . . . C8 C 0.1046(3) 0.7481(5) 0.2559(7) 0.054(2) Uani 1 1 d . . . C9 C 0.1532(3) 0.8298(5) 0.3178(7) 0.060(2) Uani 1 1 d . . . C10 C 0.1831(3) 0.8592(6) 0.4051(7) 0.066(2) Uani 1 1 d . . . C11 C 0.1904(3) 0.8462(6) 0.5135(7) 0.071(3) Uani 1 1 d . . . H11A H 0.1760 0.8124 0.5470 0.085 Uiso 1 1 calc R . . C12 C 0.2189(5) 0.8839(7) 0.5688(10) 0.090(3) Uani 1 1 d . . . H12B H 0.2237 0.8770 0.6433 0.108 Uiso 1 1 calc R . . C13 C 0.2434(4) 0.9362(8) 0.5168(10) 0.090(4) Uani 1 1 d . . . H13A H 0.2643 0.9597 0.5586 0.108 Uiso 1 1 calc R . . C14 C 0.2365(3) 0.9511(6) 0.4098(8) 0.072(3) Uani 1 1 d . . . H14B H 0.2508 0.9849 0.3765 0.086 Uiso 1 1 calc R . . C15 C 0.2063(3) 0.9115(5) 0.3550(8) 0.065(2) Uani 1 1 d . . . C16 C 0.1888(3) 0.9097(5) 0.2390(8) 0.059(2) Uani 1 1 d . . . C17 C 0.1910(3) 0.9503(4) 0.0610(8) 0.056(2) Uani 1 1 d . . . C18 C 0.2104(3) 0.9914(5) -0.0209(8) 0.061(2) Uani 1 1 d . . . C19 C 0.2432(4) 1.0380(5) -0.0145(10) 0.076(3) Uani 1 1 d . . . H19A H 0.2563 1.0509 0.0520 0.091 Uiso 1 1 calc R . . C20 C 0.2559(4) 1.0655(6) -0.1161(11) 0.093(4) Uani 1 1 d . . . H20A H 0.2790 1.0954 -0.1156 0.111 Uiso 1 1 calc R . . C21 C 0.2347(4) 1.0490(6) -0.2156(11) 0.087(3) Uani 1 1 d . . . H21A H 0.2431 1.0687 -0.2796 0.104 Uiso 1 1 calc R . . C22 C 0.2017(4) 1.0038(5) -0.2191(8) 0.078(3) Uani 1 1 d . . . H22A H 0.1884 0.9912 -0.2855 0.093 Uiso 1 1 calc R . . C23 C 0.1880(3) 0.9764(4) -0.1202(8) 0.062(2) Uani 1 1 d . . . C24 C 0.1573(3) 0.9257(5) -0.0975(8) 0.064(2) Uani 1 1 d . . . C25 C 0.1064(3) 0.8451(4) -0.1587(6) 0.0509(18) Uani 1 1 d . . . C26 C 0.0857(3) 0.8099(5) -0.2459(8) 0.062(2) Uani 1 1 d . . . C27 C 0.0846(4) 0.8200(5) -0.3594(9) 0.077(3) Uani 1 1 d . . . H27A H 0.1002 0.8533 -0.3910 0.092 Uiso 1 1 calc R . . C28 C 0.0579(4) 0.7754(7) -0.4239(8) 0.088(4) Uani 1 1 d . . . H28A H 0.0528 0.7827 -0.4983 0.105 Uiso 1 1 calc R . . C29 C 0.0396(4) 0.7216(7) -0.3760(8) 0.083(3) Uani 1 1 d . . . H29A H 0.0242 0.6924 -0.4209 0.100 Uiso 1 1 calc R . . C30 C 0.0431(3) 0.7094(6) -0.2667(8) 0.071(3) Uani 1 1 d . . . H30A H 0.0316 0.6724 -0.2367 0.086 Uiso 1 1 calc R . . C31 C 0.0667(3) 0.7591(5) -0.1976(8) 0.064(2) Uani 1 1 d . . . C32 C 0.0752(3) 0.7626(5) -0.0837(8) 0.059(2) Uani 1 1 d . . . N9 N 0.0649(2) 0.9138(3) 0.1328(5) 0.067(2) Uiso 1 1 d GD . . C33 C 0.0729(2) 0.9789(4) 0.1273(7) 0.103(4) Uiso 1 1 d GD . . H33A H 0.1009 0.9938 0.1074 0.124 Uiso 1 1 calc R . . C34 C 0.0389(3) 1.0217(3) 0.1516(7) 0.140(6) Uiso 1 1 d GD . . H34A H 0.0443 1.0652 0.1479 0.168 Uiso 1 1 calc R . . C35 C -0.0030(3) 0.9994(4) 0.1814(5) 0.093(3) Uiso 1 1 d GD . . C36 C -0.0110(2) 0.9343(5) 0.1869(7) 0.126(5) Uiso 1 1 d GD . . H36A H -0.0391 0.9194 0.2068 0.151 Uiso 1 1 calc R . . C37 C 0.0229(3) 0.8915(3) 0.1626(7) 0.118(5) Uiso 1 1 d GD . . H37A H 0.0176 0.8480 0.1663 0.142 Uiso 1 1 calc R . . C38 C -0.0437(7) 1.0437(14) 0.2015(18) 0.178(9) Uiso 1 1 d D . . H38A H -0.0676 1.0348 0.1475 0.214 Uiso 1 1 calc R . . H38B H -0.0552 1.0349 0.2730 0.214 Uiso 1 1 calc R . . C39 C -0.0320(8) 1.1084(13) 0.1955(18) 0.176(8) Uiso 1 1 d D . . H39A H -0.0242 1.1195 0.1217 0.211 Uiso 1 1 calc R . . H39B H -0.0063 1.1175 0.2442 0.211 Uiso 1 1 calc R . . C40 C -0.0753(3) 1.1481(5) 0.2312(9) 0.121(5) Uiso 1 1 d GD . . C41 C -0.0652(2) 1.2127(5) 0.2357(8) 0.122(5) Uiso 1 1 d GD . . H41A H -0.0359 1.2265 0.2240 0.146 Uiso 1 1 calc R . . C42 C -0.0987(3) 1.2565(4) 0.2576(8) 0.120(5) Uiso 1 1 d GD . . H42A H -0.0920 1.2997 0.2606 0.144 Uiso 1 1 calc R . . N10 N -0.1424(2) 1.2358(4) 0.2751(6) 0.066(2) Uiso 1 1 d GD . . C43 C -0.1525(3) 1.1713(4) 0.2706(8) 0.138(6) Uiso 1 1 d GD . . H43A H -0.1817 1.1574 0.2823 0.165 Uiso 1 1 calc R . . C44 C -0.1189(4) 1.1274(3) 0.2486(10) 0.138(6) Uiso 1 1 d G . . H44A H -0.1257 1.0842 0.2456 0.166 Uiso 1 1 calc R . . C45 C -0.2692(3) 1.2049(4) 0.3354(8) 0.056(2) Uani 1 1 d . . . C46 C -0.2860(3) 1.1606(4) 0.4229(8) 0.055(2) Uani 1 1 d . . . C47 C -0.3184(4) 1.1113(5) 0.4154(10) 0.074(3) Uani 1 1 d . . . H47A H -0.3330 1.1004 0.3494 0.088 Uiso 1 1 calc R . . C48 C -0.3271(4) 1.0802(5) 0.5108(9) 0.074(3) Uani 1 1 d . . . H48A H -0.3480 1.0473 0.5101 0.089 Uiso 1 1 calc R . . C49 C -0.3054(4) 1.0972(6) 0.6069(9) 0.073(3) Uani 1 1 d . . . H49A H -0.3118 1.0749 0.6700 0.088 Uiso 1 1 calc R . . C50 C -0.2752(4) 1.1450(5) 0.6136(9) 0.071(3) Uani 1 1 d . . . H50A H -0.2612 1.1566 0.6800 0.085 Uiso 1 1 calc R . . C51 C -0.2656(3) 1.1763(5) 0.5168(8) 0.059(2) Uani 1 1 d . . . C52 C -0.2348(3) 1.2294(4) 0.4927(7) 0.057(2) Uani 1 1 d . . . C53 C -0.1822(4) 1.3061(6) 0.5498(8) 0.071(3) Uani 1 1 d . . . C54 C -0.1580(3) 1.3434(6) 0.6375(7) 0.068(3) Uani 1 1 d . . . C55 C -0.1551(4) 1.3377(7) 0.7500(9) 0.086(3) Uani 1 1 d . . . H55A H -0.1698 1.3042 0.7832 0.103 Uiso 1 1 calc R . . C56 C -0.1322(6) 1.3779(8) 0.8101(12) 0.125(6) Uani 1 1 d . . . H56A H -0.1314 1.3742 0.8858 0.150 Uiso 1 1 calc R . . C57 C -0.1075(6) 1.4295(9) 0.7569(11) 0.122(6) Uani 1 1 d . . . H57A H -0.0896 1.4571 0.7989 0.146 Uiso 1 1 calc R . . C58 C -0.1109(4) 1.4368(7) 0.6480(10) 0.090(3) Uani 1 1 d . . . H58A H -0.0968 1.4708 0.6147 0.108 Uiso 1 1 calc R . . C59 C -0.1352(4) 1.3938(5) 0.5869(7) 0.067(3) Uani 1 1 d . . . C60 C -0.1480(4) 1.3870(5) 0.4696(8) 0.065(3) Uani 1 1 d . . . C61 C -0.1446(3) 1.4250(4) 0.2915(8) 0.062(2) Uani 1 1 d . . . C62 C -0.1320(3) 1.4737(4) 0.2119(8) 0.061(2) Uani 1 1 d . . . C63 C -0.1043(4) 1.5264(6) 0.2148(11) 0.083(3) Uani 1 1 d . . . H63A H -0.0903 1.5384 0.2808 0.099 Uiso 1 1 calc R . . C64 C -0.0971(4) 1.5605(6) 0.1260(12) 0.091(4) Uani 1 1 d . . . H64A H -0.0764 1.5939 0.1297 0.109 Uiso 1 1 calc R . . C65 C -0.1199(4) 1.5472(6) 0.0278(12) 0.089(4) Uani 1 1 d . . . H65A H -0.1164 1.5739 -0.0318 0.106 Uiso 1 1 calc R . . C66 C -0.1488(4) 1.4932(6) 0.0167(10) 0.080(3) Uani 1 1 d . . . H66A H -0.1634 1.4821 -0.0491 0.096 Uiso 1 1 calc R . . C67 C -0.1535(4) 1.4582(4) 0.1129(9) 0.071(3) Uani 1 1 d . . . C68 C -0.1797(3) 1.3994(4) 0.1321(8) 0.060(2) Uani 1 1 d . . . C69 C -0.2329(3) 1.3229(5) 0.0760(8) 0.063(2) Uani 1 1 d . . . C70 C -0.2616(3) 1.2937(5) -0.0037(8) 0.063(2) Uani 1 1 d . . . C71 C -0.2681(4) 1.3046(6) -0.1173(8) 0.075(3) Uani 1 1 d . . . H71A H -0.2529 1.3376 -0.1507 0.090 Uiso 1 1 calc R . . C72 C -0.2976(3) 1.2651(6) -0.1790(9) 0.073(3) Uani 1 1 d . . . H72A H -0.3026 1.2718 -0.2535 0.087 Uiso 1 1 calc R . . C73 C -0.3188(4) 1.2170(6) -0.1272(10) 0.078(3) Uani 1 1 d . . . H73A H -0.3380 1.1906 -0.1681 0.094 Uiso 1 1 calc R . . C74 C -0.3129(3) 1.2056(5) -0.0159(8) 0.066(2) Uani 1 1 d . . . H74A H -0.3282 1.1726 0.0170 0.079 Uiso 1 1 calc R . . C75 C -0.2833(3) 1.2449(5) 0.0463(7) 0.053(2) Uani 1 1 d . . . C76 C -0.2686(3) 1.2440(4) 0.1566(7) 0.057(2) Uani 1 1 d . . . O1W O 0.0000 1.3925(15) 1.0000 0.123 Uiso 0.55(3) 2 d SP . . O2W O -0.1430(12) 1.1696(18) 0.898(3) 0.127 Uiso 0.311(19) 1 d P . . O3W O -0.051(3) 1.387(5) 0.566(7) 0.160 Uiso 0.16(2) 1 d P . . O4W O 0.0000 1.382(3) 0.5000 0.108 Uiso 0.23(3) 2 d SP . . O5W O 0.0000 0.961(4) 0.5000 0.112 Uiso 0.20(3) 2 d SP . . 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 0.0614(5) 0.0437(5) 0.0573(5) 0.0005(4) 0.0077(4) 0.0030(4) Zn2 0.0683(6) 0.0410(5) 0.0580(6) 0.0008(4) 0.0114(4) 0.0031(4) N1 0.056(4) 0.041(4) 0.083(5) -0.001(4) 0.002(4) 0.009(3) N2 0.066(5) 0.052(4) 0.056(4) 0.007(3) 0.014(3) 0.008(4) N3 0.065(4) 0.047(4) 0.052(4) 0.001(3) 0.006(3) 0.010(3) N4 0.060(4) 0.052(4) 0.054(4) -0.001(3) -0.002(3) 0.000(3) N5 0.070(4) 0.032(3) 0.056(4) 0.002(3) 0.008(3) 0.000(3) N6 0.077(5) 0.059(5) 0.050(4) 0.000(4) -0.002(4) 0.002(4) N7 0.055(4) 0.058(5) 0.062(4) 0.000(3) 0.006(3) 0.000(3) N8 0.055(4) 0.048(4) 0.065(5) -0.003(3) 0.011(3) 0.001(3) N11 0.058(4) 0.053(4) 0.069(5) 0.003(4) 0.011(4) 0.001(4) N12 0.087(6) 0.058(5) 0.057(4) 0.009(4) 0.015(4) -0.011(4) N13 0.074(5) 0.053(5) 0.059(4) -0.003(3) 0.012(4) -0.003(4) N14 0.080(5) 0.064(5) 0.068(5) -0.013(4) 0.006(4) -0.018(4) N15 0.078(5) 0.053(4) 0.054(4) 0.004(4) 0.013(4) -0.001(4) N16 0.079(5) 0.051(5) 0.063(5) 0.000(4) 0.017(4) 0.002(4) N17 0.068(4) 0.053(5) 0.055(4) 0.004(4) 0.005(3) 0.007(4) N18 0.061(4) 0.052(4) 0.070(5) 0.001(4) 0.019(4) 0.007(3) C1 0.052(5) 0.042(4) 0.063(5) 0.000(4) 0.013(4) 0.002(3) C2 0.064(6) 0.051(5) 0.084(7) -0.001(5) 0.021(5) 0.015(4) C3 0.081(7) 0.045(5) 0.108(8) 0.004(5) 0.040(6) 0.000(5) C4 0.082(7) 0.048(5) 0.109(8) 0.006(6) 0.029(6) 0.001(5) C5 0.077(7) 0.067(7) 0.087(8) 0.024(6) 0.023(5) 0.005(5) C6 0.097(7) 0.044(5) 0.078(6) 0.010(5) 0.026(5) 0.014(5) C7 0.056(5) 0.060(5) 0.064(5) 0.003(4) 0.020(4) 0.010(4) C8 0.056(5) 0.056(5) 0.052(5) 0.005(4) 0.013(4) 0.011(4) C9 0.062(5) 0.063(6) 0.054(5) -0.004(4) 0.003(4) 0.016(4) C10 0.067(5) 0.077(7) 0.056(5) -0.001(5) 0.006(4) 0.015(5) C11 0.081(6) 0.084(7) 0.050(5) 0.012(5) 0.009(4) 0.025(6) C12 0.111(9) 0.091(9) 0.068(7) -0.004(6) 0.004(7) 0.014(7) C13 0.064(7) 0.127(11) 0.079(8) -0.021(8) -0.008(6) 0.015(7) C14 0.056(5) 0.089(8) 0.069(6) -0.013(6) -0.007(5) -0.005(5) C15 0.068(6) 0.059(6) 0.069(6) 0.001(5) 0.021(5) 0.014(5) C16 0.052(5) 0.056(5) 0.069(6) -0.002(5) 0.008(4) 0.006(4) C17 0.059(5) 0.045(5) 0.066(6) 0.000(4) 0.018(4) 0.001(4) C18 0.059(5) 0.055(5) 0.068(6) 0.004(4) 0.005(4) 0.007(4) C19 0.074(7) 0.069(7) 0.085(7) 0.017(6) -0.001(5) -0.008(5) C20 0.095(8) 0.075(7) 0.110(9) 0.017(7) 0.013(7) -0.029(6) C21 0.081(7) 0.076(7) 0.105(9) 0.021(7) 0.023(6) -0.019(6) C22 0.114(9) 0.059(6) 0.059(6) 0.008(5) 0.004(5) -0.003(6) C23 0.071(6) 0.037(4) 0.079(7) 0.007(4) 0.018(5) 0.004(4) C24 0.070(6) 0.058(6) 0.066(6) 0.002(5) 0.012(5) 0.005(5) C25 0.063(5) 0.045(4) 0.044(4) -0.003(4) 0.002(3) 0.009(4) C26 0.063(5) 0.056(6) 0.067(6) 0.009(5) 0.006(4) 0.008(4) C27 0.079(7) 0.071(7) 0.080(7) -0.011(5) 0.008(5) -0.005(5) C28 0.093(7) 0.123(10) 0.046(5) -0.002(6) -0.008(5) -0.031(7) C29 0.075(6) 0.118(10) 0.057(6) -0.021(6) 0.008(5) -0.023(6) C30 0.057(5) 0.082(7) 0.076(6) -0.008(5) 0.007(4) -0.019(5) C31 0.051(5) 0.066(6) 0.077(6) -0.009(5) 0.014(4) -0.004(4) C32 0.058(5) 0.052(5) 0.067(6) 0.001(4) 0.009(4) 0.002(4) C45 0.064(5) 0.044(5) 0.061(5) 0.002(4) 0.006(4) 0.002(4) C46 0.058(5) 0.038(4) 0.071(6) 0.002(4) 0.020(4) 0.005(4) C47 0.073(7) 0.052(6) 0.097(8) -0.003(5) 0.020(6) 0.004(5) C48 0.075(6) 0.057(6) 0.090(8) 0.018(5) 0.025(6) -0.005(5) C49 0.090(7) 0.070(7) 0.062(6) 0.008(5) 0.021(5) 0.000(6) C50 0.082(7) 0.051(5) 0.081(7) 0.005(5) 0.025(5) 0.004(5) C51 0.069(6) 0.055(5) 0.053(5) 0.002(4) 0.017(4) 0.007(4) C52 0.080(6) 0.044(5) 0.049(5) -0.001(4) 0.013(4) 0.014(4) C53 0.089(7) 0.061(6) 0.063(6) -0.002(6) 0.005(5) 0.000(6) C54 0.075(6) 0.069(7) 0.059(5) -0.012(5) 0.007(4) -0.010(5) C55 0.099(8) 0.098(9) 0.063(6) 0.015(6) 0.005(5) -0.026(7) C56 0.184(16) 0.106(11) 0.085(9) -0.013(8) -0.008(10) -0.040(11) C57 0.156(14) 0.130(13) 0.080(9) -0.020(9) 0.007(8) -0.066(11) C58 0.115(9) 0.083(8) 0.072(7) -0.018(6) 0.002(6) -0.011(7) C59 0.084(7) 0.067(6) 0.050(5) -0.002(5) -0.002(4) 0.003(5) C60 0.093(7) 0.044(5) 0.059(5) -0.003(4) 0.014(5) -0.005(5) C61 0.075(6) 0.043(5) 0.068(6) -0.004(4) 0.021(5) -0.006(4) C62 0.079(6) 0.035(4) 0.069(6) -0.002(4) 0.005(5) 0.008(4) C63 0.084(7) 0.064(7) 0.100(8) 0.004(6) -0.002(6) -0.013(6) C64 0.091(8) 0.072(7) 0.112(10) 0.014(7) 0.042(7) -0.010(6) C65 0.082(8) 0.068(7) 0.118(10) 0.033(7) 0.037(7) 0.009(6) C66 0.082(7) 0.068(7) 0.092(8) 0.018(6) 0.024(6) 0.004(6) C67 0.091(7) 0.033(4) 0.092(7) 0.011(5) 0.033(6) 0.006(4) C68 0.071(6) 0.042(5) 0.068(6) 0.002(4) 0.017(5) 0.005(4) C69 0.074(6) 0.053(5) 0.063(6) -0.001(4) 0.018(5) 0.004(4) C70 0.075(6) 0.054(6) 0.060(5) 0.006(5) 0.008(4) 0.019(5) C71 0.084(7) 0.069(6) 0.071(6) -0.003(6) -0.004(5) 0.011(6) C72 0.075(6) 0.081(7) 0.060(6) 0.005(5) -0.017(5) 0.009(6) C73 0.072(7) 0.084(8) 0.077(8) -0.008(6) -0.020(6) 0.012(6) C74 0.064(6) 0.064(6) 0.069(6) 0.001(5) 0.010(5) 0.009(5) C75 0.053(5) 0.052(5) 0.055(5) 0.000(4) 0.001(4) 0.008(4) C76 0.061(5) 0.046(5) 0.067(6) 0.001(4) 0.018(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N5 2.021(7) . ? Zn1 N3 2.022(7) . ? Zn1 N1 2.034(8) . ? Zn1 N7 2.042(8) . ? Zn1 N9 2.132(6) . ? Zn2 N13 2.015(8) . ? Zn2 N15 2.022(8) . ? Zn2 N17 2.027(7) . ? Zn2 N11 2.046(8) . ? Zn2 N10 2.118(7) . ? N1 C8 1.332(11) . ? N1 C1 1.410(11) . ? N2 C9 1.315(12) . ? N2 C8 1.344(12) . ? N3 C16 1.350(12) . ? N3 C9 1.380(12) . ? N4 C17 1.303(11) . ? N4 C16 1.357(12) . ? N5 C17 1.362(12) . ? N5 C24 1.374(12) . ? N6 C24 1.350(12) . ? N6 C25 1.351(12) . ? N7 C25 1.342(11) . ? N7 C32 1.351(11) . ? N8 C1 1.322(11) . ? N8 C32 1.353(11) . ? N11 C52 1.329(11) . ? N11 C45 1.351(12) . ? N12 C53 1.326(14) . ? N12 C52 1.341(13) . ? N13 C60 1.342(13) . ? N13 C53 1.378(12) . ? N14 C61 1.303(13) . ? N14 C60 1.348(13) . ? N15 C61 1.359(12) . ? N15 C68 1.379(12) . ? N16 C68 1.317(13) . ? N16 C69 1.328(12) . ? N17 C69 1.367(12) . ? N17 C76 1.371(12) . ? N18 C45 1.311(12) . ? N18 C76 1.376(11) . ? C1 C2 1.467(13) . ? C2 C7 1.350(14) . ? C2 C3 1.399(15) . ? C3 C4 1.404(15) . ? C4 C5 1.360(16) . ? C5 C6 1.330(16) . ? C6 C7 1.430(13) . ? C7 C8 1.438(13) . ? C9 C10 1.496(14) . ? C10 C11 1.365(13) . ? C10 C15 1.447(15) . ? C11 C12 1.327(17) . ? C12 C13 1.48(2) . ? C13 C14 1.355(16) . ? C14 C15 1.377(14) . ? C15 C16 1.495(14) . ? C17 C18 1.459(13) . ? C18 C19 1.379(14) . ? C18 C23 1.401(14) . ? C19 C20 1.437(16) . ? C20 C21 1.393(17) . ? C21 C22 1.363(15) . ? C22 C23 1.415(14) . ? C23 C24 1.434(13) . ? C25 C26 1.419(13) . ? C26 C31 1.355(14) . ? C26 C27 1.407(14) . ? C27 C28 1.444(15) . ? C28 C29 1.393(17) . ? C29 C30 1.364(14) . ? C30 C31 1.500(14) . ? C31 C32 1.411(13) . ? N9 C33 1.3900 . ? N9 C37 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C35 C38 1.55(2) . ? C36 C37 1.3900 . ? C38 C39 1.41(3) . ? C39 C40 1.60(2) . ? C40 C41 1.3900 . ? C40 C44 1.3900 . ? C41 C42 1.3900 . ? C42 N10 1.3900 . ? N10 C43 1.3900 . ? C43 C44 1.3900 . ? C45 C46 1.519(12) . ? C46 C51 1.321(14) . ? C46 C47 1.414(14) . ? C47 C48 1.372(15) . ? C48 C49 1.367(16) . ? C49 C50 1.348(15) . ? C50 C51 1.395(13) . ? C51 C52 1.480(13) . ? C53 C54 1.491(14) . ? C54 C55 1.383(14) . ? C54 C59 1.412(15) . ? C55 C56 1.295(18) . ? C56 C57 1.48(2) . ? C57 C58 1.342(17) . ? C58 C59 1.362(16) . ? C59 C60 1.481(13) . ? C61 C62 1.472(13) . ? C62 C63 1.378(15) . ? C62 C67 1.388(15) . ? C63 C64 1.327(16) . ? C64 C65 1.388(18) . ? C65 C66 1.424(17) . ? C66 C67 1.400(14) . ? C67 C68 1.484(13) . ? C69 C70 1.412(14) . ? C70 C75 1.367(14) . ? C70 C71 1.416(14) . ? C71 C72 1.407(15) . ? C72 C73 1.359(16) . ? C73 C74 1.389(15) . ? C74 C75 1.408(14) . ? C75 C76 1.405(13) . ? O3W O4W 1.74(8) . ? O4W O3W 1.74(8) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zn1 N3 86.5(3) . . ? N5 Zn1 N1 156.0(3) . . ? N3 Zn1 N1 87.0(3) . . ? N5 Zn1 N7 88.0(3) . . ? N3 Zn1 N7 155.2(3) . . ? N1 Zn1 N7 88.3(3) . . ? N5 Zn1 N9 100.5(3) . . ? N3 Zn1 N9 98.2(3) . . ? N1 Zn1 N9 103.3(3) . . ? N7 Zn1 N9 106.6(3) . . ? N13 Zn2 N15 87.0(3) . . ? N13 Zn2 N17 155.9(3) . . ? N15 Zn2 N17 87.9(3) . . ? N13 Zn2 N11 88.0(3) . . ? N15 Zn2 N11 157.0(3) . . ? N17 Zn2 N11 87.5(3) . . ? N13 Zn2 N10 100.3(3) . . ? N15 Zn2 N10 102.8(3) . . ? N17 Zn2 N10 103.8(3) . . ? N11 Zn2 N10 100.2(3) . . ? C8 N1 C1 109.6(8) . . ? C8 N1 Zn1 126.8(6) . . ? C1 N1 Zn1 123.4(6) . . ? C9 N2 C8 124.2(8) . . ? C16 N3 C9 109.0(8) . . ? C16 N3 Zn1 126.2(6) . . ? C9 N3 Zn1 123.5(6) . . ? C17 N4 C16 123.6(8) . . ? C17 N5 C24 107.8(7) . . ? C17 N5 Zn1 126.9(6) . . ? C24 N5 Zn1 125.3(6) . . ? C24 N6 C25 122.9(8) . . ? C25 N7 C32 108.4(8) . . ? C25 N7 Zn1 125.4(6) . . ? C32 N7 Zn1 126.1(6) . . ? C1 N8 C32 122.4(8) . . ? C52 N11 C45 110.9(8) . . ? C52 N11 Zn2 125.0(7) . . ? C45 N11 Zn2 123.3(6) . . ? C53 N12 C52 121.9(8) . . ? C60 N13 C53 109.9(8) . . ? C60 N13 Zn2 126.5(6) . . ? C53 N13 Zn2 123.6(7) . . ? C61 N14 C60 122.9(9) . . ? C61 N15 C68 110.1(8) . . ? C61 N15 Zn2 125.5(6) . . ? C68 N15 Zn2 124.0(7) . . ? C68 N16 C69 124.1(9) . . ? C69 N17 C76 108.3(8) . . ? C69 N17 Zn2 125.0(7) . . ? C76 N17 Zn2 125.2(6) . . ? C45 N18 C76 121.1(8) . . ? N8 C1 N1 129.7(8) . . ? N8 C1 C2 125.1(8) . . ? N1 C1 C2 105.1(8) . . ? C7 C2 C3 121.1(10) . . ? C7 C2 C1 108.5(9) . . ? C3 C2 C1 130.3(10) . . ? C2 C3 C4 117.6(12) . . ? C5 C4 C3 120.4(11) . . ? C6 C5 C4 122.2(10) . . ? C5 C6 C7 119.0(11) . . ? C2 C7 C6 119.6(10) . . ? C2 C7 C8 107.2(8) . . ? C6 C7 C8 133.2(9) . . ? N1 C8 N2 126.1(8) . . ? N1 C8 C7 109.6(8) . . ? N2 C8 C7 124.3(8) . . ? N2 C9 N3 128.3(9) . . ? N2 C9 C10 122.8(9) . . ? N3 C9 C10 108.8(9) . . ? C11 C10 C15 120.4(10) . . ? C11 C10 C9 132.8(11) . . ? C15 C10 C9 106.8(8) . . ? C12 C11 C10 116.8(12) . . ? C11 C12 C13 122.7(11) . . ? C14 C13 C12 121.9(12) . . ? C13 C14 C15 114.0(12) . . ? C14 C15 C10 124.2(10) . . ? C14 C15 C16 132.5(10) . . ? C10 C15 C16 103.3(9) . . ? N3 C16 N4 126.8(8) . . ? N3 C16 C15 112.1(8) . . ? N4 C16 C15 121.1(8) . . ? N4 C17 N5 127.4(8) . . ? N4 C17 C18 123.2(9) . . ? N5 C17 C18 109.5(8) . . ? C19 C18 C23 121.4(9) . . ? C19 C18 C17 132.6(10) . . ? C23 C18 C17 106.1(8) . . ? C18 C19 C20 116.3(11) . . ? C21 C20 C19 122.3(10) . . ? C22 C21 C20 120.0(10) . . ? C21 C22 C23 119.1(11) . . ? C18 C23 C22 120.6(9) . . ? C18 C23 C24 106.4(9) . . ? C22 C23 C24 132.3(10) . . ? N6 C24 N5 127.8(9) . . ? N6 C24 C23 122.2(9) . . ? N5 C24 C23 110.1(9) . . ? N7 C25 N6 128.2(8) . . ? N7 C25 C26 110.0(8) . . ? N6 C25 C26 121.7(7) . . ? C31 C26 C27 123.7(10) . . ? C31 C26 C25 104.9(8) . . ? C27 C26 C25 131.3(9) . . ? C26 C27 C28 115.9(10) . . ? C29 C28 C27 120.7(9) . . ? C30 C29 C28 123.3(10) . . ? C29 C30 C31 116.1(10) . . ? C26 C31 C32 109.2(9) . . ? C26 C31 C30 119.7(9) . . ? C32 C31 C30 131.1(9) . . ? N7 C32 N8 128.4(9) . . ? N7 C32 C31 107.5(8) . . ? N8 C32 C31 124.0(9) . . ? C33 N9 C37 120.0 . . ? C33 N9 Zn1 117.8(4) . . ? C37 N9 Zn1 122.1(4) . . ? N9 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 C38 123.2(12) . . ? C36 C35 C38 116.6(12) . . ? C37 C36 C35 120.0 . . ? C36 C37 N9 120.0 . . ? C39 C38 C35 112.2(19) . . ? C38 C39 C40 106.6(19) . . ? C41 C40 C44 120.0 . . ? C41 C40 C39 110.1(12) . . ? C44 C40 C39 129.7(12) . . ? C40 C41 C42 120.0 . . ? N10 C42 C41 120.0 . . ? C42 N10 C43 120.0 . . ? C42 N10 Zn2 121.6(4) . . ? C43 N10 Zn2 118.3(4) . . ? C44 C43 N10 120.0 . . ? C43 C44 C40 120.0 . . ? N18 C45 N11 131.8(9) . . ? N18 C45 C46 122.7(8) . . ? N11 C45 C46 105.5(8) . . ? C51 C46 C47 121.8(9) . . ? C51 C46 C45 108.1(8) . . ? C47 C46 C45 130.1(10) . . ? C48 C47 C46 116.2(11) . . ? C49 C48 C47 120.9(11) . . ? C50 C49 C48 122.5(10) . . ? C49 C50 C51 117.1(11) . . ? C46 C51 C50 121.5(10) . . ? C46 C51 C52 106.3(8) . . ? C50 C51 C52 132.2(9) . . ? N11 C52 N12 128.9(9) . . ? N11 C52 C51 109.1(8) . . ? N12 C52 C51 121.9(8) . . ? N12 C53 N13 130.0(9) . . ? N12 C53 C54 122.6(9) . . ? N13 C53 C54 107.2(9) . . ? C55 C54 C59 119.3(10) . . ? C55 C54 C53 133.0(10) . . ? C59 C54 C53 107.7(8) . . ? C56 C55 C54 121.5(12) . . ? C55 C56 C57 119.1(13) . . ? C58 C57 C56 120.2(13) . . ? C57 C58 C59 119.2(13) . . ? C58 C59 C54 120.6(9) . . ? C58 C59 C60 135.2(11) . . ? C54 C59 C60 104.1(9) . . ? N13 C60 N14 127.8(9) . . ? N13 C60 C59 111.0(8) . . ? N14 C60 C59 121.1(9) . . ? N14 C61 N15 128.3(8) . . ? N14 C61 C62 122.9(9) . . ? N15 C61 C62 108.5(9) . . ? C63 C62 C67 117.7(10) . . ? C63 C62 C61 135.1(10) . . ? C67 C62 C61 107.2(8) . . ? C64 C63 C62 121.8(12) . . ? C63 C64 C65 120.8(12) . . ? C64 C65 C66 121.1(11) . . ? C67 C66 C65 114.6(12) . . ? C62 C67 C66 123.7(10) . . ? C62 C67 C68 106.4(8) . . ? C66 C67 C68 129.8(11) . . ? N16 C68 N15 128.5(9) . . ? N16 C68 C67 123.7(9) . . ? N15 C68 C67 107.8(9) . . ? N16 C69 N17 127.1(10) . . ? N16 C69 C70 124.5(9) . . ? N17 C69 C70 108.3(9) . . ? C75 C70 C69 107.3(8) . . ? C75 C70 C71 120.9(10) . . ? C69 C70 C71 131.7(10) . . ? C72 C71 C70 119.4(11) . . ? C73 C72 C71 118.4(10) . . ? C72 C73 C74 123.0(11) . . ? C73 C74 C75 118.8(10) . . ? C70 C75 C76 107.9(8) . . ? C70 C75 C74 119.5(9) . . ? C76 C75 C74 132.6(9) . . ? N17 C76 N18 127.3(9) . . ? N17 C76 C75 108.2(8) . . ? N18 C76 C75 124.5(9) . . ? O3W O4W O3W 173(8) . 2_556 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.706 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.105 data_a _database_code_depnum_ccdc_archive 'CCDC 249309' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H56 N20 O2 Zn2' _chemical_formula_weight 1484.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.886(2) _cell_length_b 12.317(3) _cell_length_c 14.535(3) _cell_angle_alpha 65.05(3) _cell_angle_beta 76.62(3) _cell_angle_gamma 70.07(3) _cell_volume 1652.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 15867 _cell_measurement_theta_min 0.988 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.312 _exptl_crystal_size_mid 0.227 _exptl_crystal_size_min 0.088 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8488 _exptl_absorpt_correction_T_max 1.1432 _exptl_absorpt_process_details abscor _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Ragaku Raxis Rapid IP' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7474 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7474 _reflns_number_gt 5737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid Auto (Rigaku 2001)' _computing_cell_refinement 'Rapid Auto (Rigaku 2001)' _computing_data_reduction 'Rapid Auto (Rigaku 2001)' _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^)+(0.0724P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7474 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.011 _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 Zn1 Zn 0.35786(3) 0.56916(2) 0.39278(2) 0.02384(9) Uani 1 1 d . . . O1 O 0.1845(3) 0.1822(2) 0.0291(2) 0.0718(7) Uani 1 1 d . . . N1 N 0.49883(19) 0.49299(18) 0.30378(15) 0.0274(4) Uani 1 1 d . . . N2 N 0.47059(18) 0.67555(17) 0.37984(15) 0.0260(4) Uani 1 1 d . . . N3 N 0.26074(18) 0.60249(17) 0.51723(14) 0.0257(4) Uani 1 1 d . . . N4 N 0.28843(19) 0.42074(17) 0.44134(14) 0.0260(4) Uani 1 1 d . . . N5 N 0.4097(2) 0.33138(18) 0.31631(15) 0.0308(4) Uani 1 1 d . . . N6 N 0.62948(19) 0.63933(18) 0.24145(15) 0.0292(4) Uani 1 1 d . . . N7 N 0.34460(19) 0.76930(17) 0.50091(15) 0.0290(4) Uani 1 1 d . . . N8 N 0.13188(18) 0.45470(17) 0.58140(15) 0.0279(4) Uani 1 1 d . . . N9 N 0.23490(18) 0.69811(17) 0.27284(14) 0.0262(4) Uani 1 1 d . . . N10 N 0.3951(3) 0.1516(3) 0.0490(2) 0.0551(7) Uani 1 1 d . . . C1 C 0.4911(2) 0.4039(2) 0.27516(18) 0.0300(5) Uani 1 1 d . . . C2 C 0.5866(3) 0.3992(3) 0.1879(2) 0.0395(6) Uani 1 1 d . . . C3 C 0.6183(4) 0.3255(3) 0.1311(3) 0.0634(10) Uani 1 1 d . . . H3A H 0.5761 0.2648 0.1467 0.076 Uiso 1 1 calc R . . C4 C 0.7149(5) 0.3454(4) 0.0504(3) 0.0897(16) Uani 1 1 d . . . H4A H 0.7379 0.2977 0.0105 0.108 Uiso 1 1 calc R . . C5 C 0.7786(4) 0.4357(4) 0.0279(3) 0.0804(14) Uani 1 1 d . . . H5B H 0.8429 0.4475 -0.0273 0.096 Uiso 1 1 calc R . . C6 C 0.7486(3) 0.5081(3) 0.0851(2) 0.0531(8) Uani 1 1 d . . . H6B H 0.7921 0.5677 0.0700 0.064 Uiso 1 1 calc R . . C7 C 0.6514(3) 0.4889(2) 0.1659(2) 0.0370(6) Uani 1 1 d . . . C8 C 0.5937(2) 0.5465(2) 0.24028(18) 0.0297(5) Uani 1 1 d . . . C9 C 0.5728(2) 0.6974(2) 0.30578(18) 0.0261(5) Uani 1 1 d . . . C10 C 0.6096(2) 0.8015(2) 0.30480(18) 0.0282(5) Uani 1 1 d . . . C11 C 0.7051(2) 0.8617(2) 0.2453(2) 0.0351(6) Uani 1 1 d . . . H11A H 0.7635 0.8351 0.1962 0.042 Uiso 1 1 calc R . . C12 C 0.7093(3) 0.9627(3) 0.2622(2) 0.0409(6) Uani 1 1 d . . . H12A H 0.7708 1.0058 0.2228 0.049 Uiso 1 1 calc R . . C13 C 0.6245(3) 1.0013(2) 0.3364(2) 0.0415(6) Uani 1 1 d . . . H13A H 0.6302 1.0695 0.3458 0.050 Uiso 1 1 calc R . . C14 C 0.5315(3) 0.9404(2) 0.3968(2) 0.0337(5) Uani 1 1 d . . . H14A H 0.4752 0.9657 0.4473 0.040 Uiso 1 1 calc R . . C15 C 0.5252(2) 0.8399(2) 0.37923(18) 0.0278(5) Uani 1 1 d . . . C16 C 0.4391(2) 0.7589(2) 0.42597(17) 0.0257(5) Uani 1 1 d . . . C17 C 0.2659(2) 0.6951(2) 0.54384(18) 0.0273(5) Uani 1 1 d . . . C18 C 0.1683(2) 0.7018(2) 0.62980(18) 0.0298(5) Uani 1 1 d . . . C19 C 0.1338(3) 0.7786(3) 0.6845(2) 0.0391(6) Uani 1 1 d . . . H19A H 0.1750 0.8403 0.6681 0.047 Uiso 1 1 calc R . . C20 C 0.0363(3) 0.7597(3) 0.7641(2) 0.0482(7) Uani 1 1 d . . . H20A H 0.0106 0.8101 0.8019 0.058 Uiso 1 1 calc R . . C21 C -0.0247(3) 0.6672(3) 0.7893(2) 0.0482(7) Uani 1 1 d . . . H21A H -0.0902 0.6567 0.8436 0.058 Uiso 1 1 calc R . . C22 C 0.0102(3) 0.5899(3) 0.7347(2) 0.0395(6) Uani 1 1 d . . . H22A H -0.0302 0.5275 0.7517 0.047 Uiso 1 1 calc R . . C23 C 0.1069(2) 0.6092(2) 0.65448(18) 0.0302(5) Uani 1 1 d . . . C24 C 0.1673(2) 0.5482(2) 0.58153(17) 0.0266(5) Uani 1 1 d . . . C25 C 0.1890(2) 0.3965(2) 0.51660(17) 0.0257(5) Uani 1 1 d . . . C26 C 0.1521(2) 0.2926(2) 0.51727(18) 0.0276(5) Uani 1 1 d . . . C27 C 0.0596(2) 0.2308(2) 0.5783(2) 0.0344(5) Uani 1 1 d . . . H27A H 0.0056 0.2540 0.6305 0.041 Uiso 1 1 calc R . . C28 C 0.0504(3) 0.1334(2) 0.5587(2) 0.0411(6) Uani 1 1 d . . . H28A H -0.0113 0.0907 0.5984 0.049 Uiso 1 1 calc R . . C29 C 0.1307(3) 0.0979(2) 0.4816(2) 0.0392(6) Uani 1 1 d . . . H29A H 0.1224 0.0317 0.4706 0.047 Uiso 1 1 calc R . . C30 C 0.2230(3) 0.1591(2) 0.4206(2) 0.0331(5) Uani 1 1 d . . . H30A H 0.2765 0.1361 0.3682 0.040 Uiso 1 1 calc R . . C31 C 0.2329(2) 0.2570(2) 0.44076(18) 0.0274(5) Uani 1 1 d . . . C32 C 0.3186(2) 0.3387(2) 0.39326(18) 0.0270(5) Uani 1 1 d . . . C33 C 0.2240(3) 0.8198(2) 0.2322(2) 0.0358(6) Uani 1 1 d . . . H33A H 0.2697 0.8501 0.2583 0.043 Uiso 1 1 calc R . . C34 C 0.1496(3) 0.9027(2) 0.1543(2) 0.0396(6) Uani 1 1 d . . . H34A H 0.1453 0.9868 0.1289 0.048 Uiso 1 1 calc R . . C35 C 0.0802(2) 0.8604(2) 0.11341(18) 0.0308(5) Uani 1 1 d . . . C36 C 0.0892(3) 0.7345(2) 0.15704(19) 0.0339(5) Uani 1 1 d . . . H36A H 0.0426 0.7020 0.1337 0.041 Uiso 1 1 calc R . . C37 C 0.1669(3) 0.6575(2) 0.23490(19) 0.0332(5) Uani 1 1 d . . . H37A H 0.1724 0.5729 0.2624 0.040 Uiso 1 1 calc R . . C38 C 0.0025(3) 0.9408(2) 0.02738(19) 0.0364(6) Uani 1 1 d . . . H38A H -0.0475 0.9059 0.0097 0.044 Uiso 1 1 calc R . . C39 C 0.3677(4) 0.1316(5) 0.1555(3) 0.0958(15) Uani 1 1 d . . . H39A H 0.2781 0.1291 0.1777 0.144 Uiso 1 1 calc R . . H39B H 0.3813 0.1983 0.1661 0.144 Uiso 1 1 calc R . . H39C H 0.4253 0.0540 0.1938 0.144 Uiso 1 1 calc R . . C40 C 0.5249(4) 0.1575(5) -0.0002(3) 0.0863(13) Uani 1 1 d . . . H40A H 0.5287 0.1708 -0.0707 0.129 Uiso 1 1 calc R . . H40B H 0.5878 0.0806 0.0326 0.129 Uiso 1 1 calc R . . H40C H 0.5449 0.2250 0.0046 0.129 Uiso 1 1 calc R . . C41 C 0.2975(4) 0.1774(3) -0.0037(2) 0.0599(9) Uani 1 1 d . . . H41B H 0.3185 0.1933 -0.0731 0.072 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 Zn1 0.02790(14) 0.02091(14) 0.02413(14) -0.00883(10) -0.00435(10) -0.00681(10) O1 0.0796(18) 0.0723(17) 0.0688(16) -0.0048(13) -0.0227(14) -0.0451(15) N1 0.0313(10) 0.0244(9) 0.0290(10) -0.0121(8) -0.0025(8) -0.0084(8) N2 0.0291(10) 0.0248(9) 0.0269(10) -0.0122(8) -0.0052(8) -0.0060(8) N3 0.0297(10) 0.0229(9) 0.0267(10) -0.0111(8) -0.0041(8) -0.0070(8) N4 0.0329(10) 0.0208(9) 0.0246(10) -0.0089(8) -0.0036(8) -0.0068(8) N5 0.0406(11) 0.0264(10) 0.0301(11) -0.0142(9) -0.0007(9) -0.0122(9) N6 0.0299(10) 0.0269(10) 0.0320(11) -0.0132(9) -0.0014(8) -0.0077(9) N7 0.0358(11) 0.0237(10) 0.0287(10) -0.0103(8) -0.0055(8) -0.0075(9) N8 0.0315(10) 0.0247(10) 0.0278(10) -0.0103(8) -0.0020(8) -0.0082(9) N9 0.0258(9) 0.0243(9) 0.0238(9) -0.0047(8) -0.0050(8) -0.0051(8) N10 0.0628(17) 0.0623(17) 0.0416(14) -0.0189(13) -0.0125(13) -0.0150(14) C1 0.0347(12) 0.0275(12) 0.0295(12) -0.0140(10) -0.0001(10) -0.0084(10) C2 0.0492(15) 0.0382(14) 0.0372(15) -0.0208(12) 0.0081(12) -0.0190(13) C3 0.087(2) 0.067(2) 0.063(2) -0.0487(19) 0.0320(19) -0.047(2) C4 0.126(4) 0.099(3) 0.088(3) -0.078(3) 0.062(3) -0.076(3) C5 0.105(3) 0.091(3) 0.074(3) -0.063(2) 0.059(2) -0.065(3) C6 0.065(2) 0.0518(18) 0.0538(19) -0.0327(16) 0.0219(16) -0.0320(17) C7 0.0437(14) 0.0336(13) 0.0372(14) -0.0185(12) 0.0036(12) -0.0132(12) C8 0.0330(12) 0.0253(11) 0.0304(12) -0.0106(10) -0.0023(10) -0.0081(10) C9 0.0271(11) 0.0228(11) 0.0289(12) -0.0077(9) -0.0086(9) -0.0063(9) C10 0.0299(12) 0.0240(11) 0.0310(12) -0.0074(10) -0.0109(10) -0.0065(10) C11 0.0323(13) 0.0382(14) 0.0373(14) -0.0148(12) -0.0026(11) -0.0123(11) C12 0.0446(15) 0.0386(14) 0.0438(16) -0.0100(13) -0.0051(12) -0.0232(13) C13 0.0519(16) 0.0317(13) 0.0493(17) -0.0133(13) -0.0149(13) -0.0177(13) C14 0.0418(14) 0.0297(12) 0.0351(13) -0.0137(11) -0.0098(11) -0.0107(11) C15 0.0309(12) 0.0250(11) 0.0283(12) -0.0083(10) -0.0102(9) -0.0062(10) C16 0.0308(11) 0.0216(10) 0.0257(11) -0.0063(9) -0.0108(9) -0.0065(9) C17 0.0323(12) 0.0236(11) 0.0261(12) -0.0098(10) -0.0060(10) -0.0051(10) C18 0.0358(13) 0.0253(11) 0.0275(12) -0.0107(10) -0.0040(10) -0.0063(10) C19 0.0496(15) 0.0345(13) 0.0391(15) -0.0200(12) 0.0022(12) -0.0152(12) C20 0.0621(19) 0.0441(16) 0.0460(17) -0.0318(14) 0.0091(14) -0.0143(15) C21 0.0540(17) 0.0508(17) 0.0426(16) -0.0268(14) 0.0171(14) -0.0204(15) C22 0.0447(15) 0.0372(14) 0.0387(15) -0.0168(12) 0.0065(12) -0.0177(13) C23 0.0356(12) 0.0254(12) 0.0287(12) -0.0109(10) -0.0059(10) -0.0047(10) C24 0.0293(11) 0.0236(11) 0.0250(11) -0.0089(9) -0.0047(9) -0.0038(10) C25 0.0282(11) 0.0208(10) 0.0262(11) -0.0058(9) -0.0080(9) -0.0050(9) C26 0.0290(11) 0.0232(11) 0.0307(12) -0.0095(10) -0.0091(10) -0.0040(10) C27 0.0328(12) 0.0328(13) 0.0386(14) -0.0134(11) -0.0011(11) -0.0118(11) C28 0.0397(14) 0.0360(14) 0.0522(17) -0.0158(13) -0.0006(12) -0.0195(12) C29 0.0447(15) 0.0322(13) 0.0507(16) -0.0199(13) -0.0077(13) -0.0151(12) C30 0.0376(13) 0.0290(12) 0.0366(14) -0.0158(11) -0.0065(11) -0.0076(11) C31 0.0313(12) 0.0226(11) 0.0281(12) -0.0076(10) -0.0077(10) -0.0066(10) C32 0.0318(12) 0.0208(10) 0.0277(12) -0.0084(9) -0.0068(9) -0.0052(9) C33 0.0404(14) 0.0310(13) 0.0373(14) -0.0038(11) -0.0157(11) -0.0151(12) C34 0.0481(15) 0.0252(12) 0.0414(15) 0.0010(11) -0.0209(12) -0.0119(12) C35 0.0309(12) 0.0305(12) 0.0262(12) -0.0053(10) -0.0076(10) -0.0065(10) C36 0.0390(13) 0.0298(12) 0.0344(13) -0.0104(11) -0.0132(11) -0.0071(11) C37 0.0436(14) 0.0251(12) 0.0312(13) -0.0078(10) -0.0114(11) -0.0085(11) C38 0.0383(13) 0.0351(13) 0.0332(13) -0.0047(11) -0.0173(11) -0.0082(12) C39 0.072(3) 0.161(5) 0.055(2) -0.049(3) -0.012(2) -0.020(3) C40 0.070(3) 0.125(4) 0.070(3) -0.046(3) 0.002(2) -0.027(3) C41 0.095(3) 0.0557(19) 0.0379(17) -0.0063(15) -0.0140(17) -0.041(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N3 2.001(2) . ? Zn1 N4 2.0044(19) . ? Zn1 N1 2.008(2) . ? Zn1 N2 2.0100(19) . ? Zn1 N9 2.156(2) . ? O1 C41 1.202(4) . ? N1 C1 1.360(3) . ? N1 C8 1.365(3) . ? N2 C16 1.362(3) . ? N2 C9 1.369(3) . ? N3 C24 1.361(3) . ? N3 C17 1.371(3) . ? N4 C25 1.362(3) . ? N4 C32 1.371(3) . ? N5 C32 1.324(3) . ? N5 C1 1.335(3) . ? N6 C9 1.328(3) . ? N6 C8 1.336(3) . ? N7 C16 1.330(3) . ? N7 C17 1.328(3) . ? N8 C25 1.335(3) . ? N8 C24 1.334(3) . ? N9 C37 1.333(3) . ? N9 C33 1.332(3) . ? N10 C41 1.326(4) . ? N10 C39 1.435(4) . ? N10 C40 1.440(5) . ? C1 C2 1.450(3) . ? C2 C3 1.383(4) . ? C2 C7 1.395(4) . ? C3 C4 1.380(4) . ? C4 C5 1.392(5) . ? C5 C6 1.376(4) . ? C6 C7 1.385(4) . ? C7 C8 1.447(3) . ? C9 C10 1.461(3) . ? C10 C15 1.383(3) . ? C10 C11 1.396(3) . ? C11 C12 1.383(4) . ? C12 C13 1.383(4) . ? C13 C14 1.382(4) . ? C14 C15 1.392(3) . ? C15 C16 1.451(3) . ? C17 C18 1.453(3) . ? C18 C19 1.387(3) . ? C18 C23 1.392(3) . ? C19 C20 1.376(4) . ? C20 C21 1.387(4) . ? C21 C22 1.389(4) . ? C22 C23 1.375(4) . ? C23 C24 1.461(3) . ? C25 C26 1.463(3) . ? C26 C27 1.385(3) . ? C26 C31 1.378(3) . ? C27 C28 1.384(3) . ? C28 C29 1.383(4) . ? C29 C30 1.379(4) . ? C30 C31 1.397(3) . ? C31 C32 1.455(3) . ? C33 C34 1.366(4) . ? C34 C35 1.390(3) . ? C35 C36 1.382(3) . ? C35 C38 1.461(3) . ? C36 C37 1.374(3) . ? C38 C38 1.323(5) 2_575 ? 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 N4 88.33(8) . . ? N3 Zn1 N1 160.00(8) . . ? N4 Zn1 N1 88.25(8) . . ? N3 Zn1 N2 88.19(8) . . ? N4 Zn1 N2 160.15(8) . . ? N1 Zn1 N2 88.36(8) . . ? N3 Zn1 N9 104.36(8) . . ? N4 Zn1 N9 100.58(8) . . ? N1 Zn1 N9 95.64(8) . . ? N2 Zn1 N9 99.21(8) . . ? C1 N1 C8 108.9(2) . . ? C1 N1 Zn1 124.12(16) . . ? C8 N1 Zn1 124.31(15) . . ? C16 N2 C9 108.80(19) . . ? C16 N2 Zn1 124.96(16) . . ? C9 N2 Zn1 124.52(15) . . ? C24 N3 C17 108.95(19) . . ? C24 N3 Zn1 125.64(15) . . ? C17 N3 Zn1 124.94(16) . . ? C25 N4 C32 108.74(19) . . ? C25 N4 Zn1 125.53(15) . . ? C32 N4 Zn1 124.96(15) . . ? C32 N5 C1 123.5(2) . . ? C9 N6 C8 123.8(2) . . ? C16 N7 C17 123.5(2) . . ? C25 N8 C24 123.3(2) . . ? C37 N9 C33 116.9(2) . . ? C37 N9 Zn1 120.36(15) . . ? C33 N9 Zn1 122.77(16) . . ? C41 N10 C39 119.3(3) . . ? C41 N10 C40 121.5(3) . . ? C39 N10 C40 118.8(3) . . ? N5 C1 N1 127.9(2) . . ? N5 C1 C2 123.2(2) . . ? N1 C1 C2 108.8(2) . . ? C3 C2 C7 121.4(3) . . ? C3 C2 C1 131.7(3) . . ? C7 C2 C1 106.9(2) . . ? C4 C3 C2 117.5(3) . . ? C3 C4 C5 121.1(3) . . ? C6 C5 C4 121.6(3) . . ? C5 C6 C7 117.6(3) . . ? C6 C7 C2 120.8(2) . . ? C6 C7 C8 133.1(2) . . ? C2 C7 C8 106.1(2) . . ? N6 C8 N1 127.5(2) . . ? N6 C8 C7 123.1(2) . . ? N1 C8 C7 109.3(2) . . ? N6 C9 N2 127.6(2) . . ? N6 C9 C10 123.6(2) . . ? N2 C9 C10 108.7(2) . . ? C15 C10 C11 121.0(2) . . ? C15 C10 C9 106.4(2) . . ? C11 C10 C9 132.6(2) . . ? C12 C11 C10 117.2(2) . . ? C11 C12 C13 121.6(2) . . ? C14 C13 C12 121.3(2) . . ? C13 C14 C15 117.4(2) . . ? C10 C15 C14 121.3(2) . . ? C10 C15 C16 107.0(2) . . ? C14 C15 C16 131.6(2) . . ? N7 C16 N2 127.4(2) . . ? N7 C16 C15 123.5(2) . . ? N2 C16 C15 109.0(2) . . ? N7 C17 N3 127.9(2) . . ? N7 C17 C18 123.4(2) . . ? N3 C17 C18 108.8(2) . . ? C19 C18 C23 121.4(2) . . ? C19 C18 C17 131.7(2) . . ? C23 C18 C17 106.9(2) . . ? C20 C19 C18 117.2(2) . . ? C19 C20 C21 121.6(3) . . ? C20 C21 C22 121.2(3) . . ? C23 C22 C21 117.5(3) . . ? C22 C23 C18 121.2(2) . . ? C22 C23 C24 132.6(2) . . ? C18 C23 C24 106.2(2) . . ? N8 C24 N3 127.8(2) . . ? N8 C24 C23 123.1(2) . . ? N3 C24 C23 109.10(19) . . ? N8 C25 N4 127.6(2) . . ? N8 C25 C26 123.6(2) . . ? N4 C25 C26 108.9(2) . . ? C27 C26 C31 121.0(2) . . ? C27 C26 C25 132.3(2) . . ? C31 C26 C25 106.6(2) . . ? C26 C27 C28 117.6(2) . . ? C29 C28 C27 121.5(2) . . ? C30 C29 C28 121.1(2) . . ? C29 C30 C31 117.4(2) . . ? C26 C31 C30 121.3(2) . . ? C26 C31 C32 107.0(2) . . ? C30 C31 C32 131.7(2) . . ? N5 C32 N4 127.5(2) . . ? N5 C32 C31 123.7(2) . . ? N4 C32 C31 108.8(2) . . ? N9 C33 C34 123.8(2) . . ? C33 C34 C35 119.5(2) . . ? C36 C35 C34 116.7(2) . . ? C36 C35 C38 119.7(2) . . ? C34 C35 C38 123.6(2) . . ? C37 C36 C35 120.0(2) . . ? N9 C37 C36 123.1(2) . . ? C38 C38 C35 125.3(3) 2_575 . ? O1 C41 N10 126.6(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.315 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.074 data_c _database_code_depnum_ccdc_archive 'CCDC 249310' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H30 N10 Zn' _chemical_formula_weight 776.16 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)/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 9.2854(19) _cell_length_b 20.135(4) _cell_length_c 18.572(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.15(3) _cell_angle_gamma 90.00 _cell_volume 3472.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17243 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.48 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6377 _exptl_absorpt_correction_T_max 0.7926 _exptl_absorpt_process_details abscor _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis Rapid IP' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17243 _diffrn_reflns_av_R_equivalents 0.078 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7246 _reflns_number_gt 3723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid Auto(Rigaku 2001)' _computing_cell_refinement 'Rapid Auto(Rigaku 2001)' _computing_data_reduction 'Rapid Auto(Rigaku 2001)' _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^)+(0.1530P)^2^+0.4015P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7246 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1505 _refine_ls_R_factor_gt 0.0872 _refine_ls_wR_factor_ref 0.2878 _refine_ls_wR_factor_gt 0.2524 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.15107(8) 0.15493(4) -0.01816(4) 0.0574(3) Uani 1 1 d . . . N1 N 0.0451(6) 0.1616(3) 0.0761(3) 0.0565(13) Uani 1 1 d . . . N2 N -0.1614(5) 0.0920(3) 0.0495(3) 0.0563(12) Uani 1 1 d . . . N3 N 0.0115(6) 0.0837(3) -0.0482(3) 0.0576(13) Uani 1 1 d . . . N4 N 0.1233(5) 0.0459(3) -0.1575(3) 0.0581(13) Uani 1 1 d . . . N5 N 0.2882(6) 0.1181(3) -0.0916(3) 0.0606(13) Uani 1 1 d . . . N6 N 0.5030(6) 0.1781(3) -0.0592(3) 0.0602(14) Uani 1 1 d . . . N7 N 0.3223(6) 0.1984(3) 0.0309(3) 0.0599(13) Uani 1 1 d . . . N8 N 0.2088(6) 0.2316(3) 0.1442(3) 0.0590(13) Uani 1 1 d . . . N9 N 0.0512(5) 0.2351(3) -0.0740(3) 0.0580(13) Uani 1 1 d . . . N10 N -0.8314(8) 0.4628(5) 0.0291(4) 0.099(2) Uani 1 1 d . . . C1 C 0.0898(7) 0.1989(3) 0.1340(4) 0.0599(16) Uani 1 1 d . . . C2 C -0.0218(7) 0.1944(3) 0.1905(3) 0.0566(15) Uani 1 1 d . . . C3 C -0.0368(8) 0.2216(4) 0.2575(4) 0.0713(19) Uani 1 1 d . . . H3A H 0.0341 0.2494 0.2761 0.086 Uiso 1 1 calc R . . C4 C -0.1581(8) 0.2074(4) 0.2968(4) 0.075(2) Uani 1 1 d . . . H4B H -0.1710 0.2273 0.3415 0.090 Uiso 1 1 calc R . . C5 C -0.2613(8) 0.1639(4) 0.2711(4) 0.077(2) Uani 1 1 d . . . H5A H -0.3396 0.1533 0.3000 0.092 Uiso 1 1 calc R . . C6 C -0.2506(8) 0.1350(4) 0.2017(4) 0.0696(18) Uani 1 1 d . . . H6B H -0.3204 0.1064 0.1835 0.084 Uiso 1 1 calc R . . C7 C -0.1290(7) 0.1524(3) 0.1629(3) 0.0581(15) Uani 1 1 d . . . C8 C -0.0819(7) 0.1326(3) 0.0903(3) 0.0578(15) Uani 1 1 d . . . C9 C -0.1154(7) 0.0693(3) -0.0140(4) 0.0593(16) Uani 1 1 d . . . C10 C -0.1968(7) 0.0235(3) -0.0581(3) 0.0565(15) Uani 1 1 d . . . C11 C -0.3324(7) -0.0058(4) -0.0469(4) 0.0661(17) Uani 1 1 d . . . H11A H -0.3861 0.0025 -0.0057 0.079 Uiso 1 1 calc R . . C12 C -0.3808(8) -0.0473(4) -0.1002(4) 0.076(2) Uani 1 1 d . . . H12A H -0.4701 -0.0676 -0.0950 0.091 Uiso 1 1 calc R . . C13 C -0.3031(9) -0.0598(4) -0.1602(4) 0.076(2) Uani 1 1 d . . . H13A H -0.3413 -0.0878 -0.1952 0.092 Uiso 1 1 calc R . . C14 C -0.1700(8) -0.0324(3) -0.1710(4) 0.0681(18) Uani 1 1 d . . . H14A H -0.1172 -0.0421 -0.2122 0.082 Uiso 1 1 calc R . . C15 C -0.1158(7) 0.0104(3) -0.1184(3) 0.0577(15) Uani 1 1 d . . . C16 C 0.0161(7) 0.0479(3) -0.1100(4) 0.0596(16) Uani 1 1 d . . . C17 C 0.2505(7) 0.0771(3) -0.1472(3) 0.0557(15) Uani 1 1 d . . . C18 C 0.3698(7) 0.0710(3) -0.1962(4) 0.0605(16) Uani 1 1 d . . . C19 C 0.3869(8) 0.0377(4) -0.2610(4) 0.0724(19) Uani 1 1 d . . . H19A H 0.3134 0.0118 -0.2802 0.087 Uiso 1 1 calc R . . C20 C 0.5168(9) 0.0445(4) -0.2957(4) 0.080(2) Uani 1 1 d . . . H20A H 0.5302 0.0234 -0.3397 0.096 Uiso 1 1 calc R . . C21 C 0.6283(10) 0.0818(4) -0.2669(5) 0.088(3) Uani 1 1 d . . . H21A H 0.7150 0.0850 -0.2917 0.106 Uiso 1 1 calc R . . C22 C 0.6125(9) 0.1140(4) -0.2030(4) 0.077(2) Uani 1 1 d . . . H22A H 0.6880 0.1385 -0.1835 0.092 Uiso 1 1 calc R . . C23 C 0.4825(7) 0.1094(3) -0.1676(4) 0.0649(17) Uani 1 1 d . . . C24 C 0.4264(7) 0.1384(3) -0.1024(4) 0.0577(15) Uani 1 1 d . . . C25 C 0.4536(7) 0.2038(3) 0.0016(4) 0.0628(17) Uani 1 1 d . . . C26 C 0.5448(7) 0.2433(3) 0.0505(4) 0.0617(17) Uani 1 1 d . . . C27 C 0.6871(7) 0.2644(4) 0.0465(4) 0.0684(18) Uani 1 1 d . . . H27A H 0.7460 0.2526 0.0082 0.082 Uiso 1 1 calc R . . C28 C 0.7368(9) 0.3039(4) 0.1021(5) 0.084(2) Uani 1 1 d . . . H28A H 0.8311 0.3194 0.1009 0.101 Uiso 1 1 calc R . . C29 C 0.6507(9) 0.3209(4) 0.1591(4) 0.079(2) Uani 1 1 d . . . H29A H 0.6892 0.3472 0.1956 0.094 Uiso 1 1 calc R . . C30 C 0.5076(8) 0.3004(4) 0.1644(4) 0.0677(18) Uani 1 1 d . . . H30A H 0.4488 0.3129 0.2025 0.081 Uiso 1 1 calc R . . C31 C 0.4597(7) 0.2606(3) 0.1098(4) 0.0628(17) Uani 1 1 d . . . C32 C 0.3163(6) 0.2303(3) 0.0957(3) 0.0563(15) Uani 1 1 d . . . C33 C 0.0469(8) 0.2945(4) -0.0488(4) 0.0724(19) Uani 1 1 d . . . H33A H 0.1077 0.3041 -0.0104 0.087 Uiso 1 1 calc R . . C34 C -0.0400(8) 0.3453(4) -0.0737(4) 0.074(2) Uani 1 1 d . . . H34A H -0.0360 0.3873 -0.0529 0.089 Uiso 1 1 calc R . . C35 C -0.1309(8) 0.3325(4) -0.1289(4) 0.072(2) Uani 1 1 d . . . C36 C -0.1261(8) 0.2706(4) -0.1608(4) 0.075(2) Uani 1 1 d . . . H36A H -0.1828 0.2606 -0.2007 0.090 Uiso 1 1 calc R . . C37 C -0.0355(9) 0.2247(4) -0.1317(4) 0.078(2) Uani 1 1 d . . . H37A H -0.0329 0.1829 -0.1530 0.093 Uiso 1 1 calc R . . C38 C -0.2417(9) 0.3821(4) -0.1529(4) 0.081(2) Uani 1 1 d . . . H38A H -0.2776 0.3699 -0.2002 0.098 Uiso 1 1 calc R . . H38B H -0.1978 0.4257 -0.1565 0.098 Uiso 1 1 calc R . . C39 C -0.3676(7) 0.3847(4) -0.0994(4) 0.0700(18) Uani 1 1 d . . . H39A H -0.4161 0.3420 -0.0991 0.084 Uiso 1 1 calc R . . H39B H -0.3299 0.3926 -0.0514 0.084 Uiso 1 1 calc R . . C40 C -0.4766(9) 0.4388(4) -0.1179(4) 0.080(2) Uani 1 1 d . . . H40A H -0.4267 0.4811 -0.1208 0.096 Uiso 1 1 calc R . . H40B H -0.5174 0.4296 -0.1650 0.096 Uiso 1 1 calc R . . C41 C -0.5980(8) 0.4449(4) -0.0639(4) 0.0718(19) Uani 1 1 d . . . C42 C -0.6148(9) 0.4035(5) -0.0085(5) 0.089(2) Uani 1 1 d . . . H42A H -0.5514 0.3684 -0.0006 0.107 Uiso 1 1 calc R . . C43 C -0.7335(11) 0.4150(5) 0.0379(5) 0.100(3) Uani 1 1 d . . . H43A H -0.7437 0.3871 0.0775 0.120 Uiso 1 1 calc R . . C44 C -0.8095(10) 0.5017(6) -0.0266(5) 0.103(3) Uani 1 1 d . . . H44A H -0.8764 0.5351 -0.0352 0.124 Uiso 1 1 calc R . . C45 C -0.6967(8) 0.4967(4) -0.0729(5) 0.085(2) Uani 1 1 d . . . H45A H -0.6853 0.5274 -0.1100 0.102 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 Zn1 0.0501(4) 0.0666(5) 0.0556(5) -0.0012(3) -0.0033(3) -0.0039(3) N1 0.053(3) 0.064(3) 0.052(3) -0.001(2) -0.004(2) -0.007(2) N2 0.047(3) 0.065(3) 0.057(3) 0.002(2) -0.004(2) -0.007(2) N3 0.054(3) 0.066(3) 0.053(3) -0.007(2) -0.006(2) -0.001(2) N4 0.048(3) 0.065(3) 0.061(3) 0.001(2) -0.004(2) 0.008(2) N5 0.054(3) 0.069(3) 0.058(3) 0.006(3) 0.002(2) 0.005(3) N6 0.049(3) 0.058(3) 0.074(4) 0.010(3) -0.006(3) 0.000(2) N7 0.048(3) 0.070(3) 0.062(3) 0.000(3) -0.006(2) -0.009(3) N8 0.058(3) 0.061(3) 0.059(3) -0.001(2) -0.007(3) -0.003(3) N9 0.045(3) 0.071(4) 0.058(3) 0.001(3) 0.001(2) 0.005(2) N10 0.072(5) 0.131(7) 0.093(6) -0.027(5) -0.002(4) 0.016(5) C1 0.057(4) 0.061(4) 0.061(4) -0.002(3) -0.007(3) -0.003(3) C2 0.053(4) 0.063(4) 0.054(4) -0.001(3) 0.000(3) 0.000(3) C3 0.067(4) 0.075(5) 0.072(4) -0.014(4) -0.014(4) -0.001(4) C4 0.058(4) 0.095(5) 0.073(5) -0.018(4) 0.002(4) -0.007(4) C5 0.057(4) 0.106(6) 0.066(4) -0.005(4) 0.012(3) -0.008(4) C6 0.056(4) 0.083(5) 0.070(4) -0.002(4) 0.012(3) -0.004(3) C7 0.059(4) 0.064(4) 0.052(3) -0.004(3) -0.002(3) 0.000(3) C8 0.049(4) 0.062(4) 0.062(4) 0.006(3) -0.006(3) -0.003(3) C9 0.050(4) 0.067(4) 0.061(4) -0.004(3) -0.008(3) 0.002(3) C10 0.054(4) 0.065(4) 0.051(3) 0.001(3) -0.007(3) 0.001(3) C11 0.056(4) 0.072(4) 0.070(4) -0.001(3) -0.009(3) -0.010(3) C12 0.066(5) 0.078(5) 0.083(5) -0.002(4) -0.017(4) -0.002(4) C13 0.078(5) 0.070(4) 0.081(5) -0.019(4) -0.032(4) 0.000(4) C14 0.074(5) 0.063(4) 0.068(4) -0.008(3) -0.014(4) -0.003(3) C15 0.054(4) 0.057(4) 0.063(4) 0.004(3) -0.009(3) 0.006(3) C16 0.058(4) 0.062(4) 0.059(4) 0.004(3) -0.012(3) 0.002(3) C17 0.049(3) 0.054(3) 0.064(4) -0.004(3) -0.003(3) 0.002(3) C18 0.057(4) 0.062(4) 0.063(4) 0.002(3) -0.005(3) 0.013(3) C19 0.064(4) 0.092(5) 0.061(4) -0.003(4) 0.000(3) 0.010(4) C20 0.074(5) 0.099(6) 0.065(4) -0.011(4) -0.005(4) 0.021(4) C21 0.087(6) 0.096(6) 0.081(6) 0.008(5) 0.037(5) 0.025(5) C22 0.075(5) 0.071(5) 0.085(5) 0.015(4) -0.005(4) 0.009(4) C23 0.059(4) 0.061(4) 0.074(4) 0.012(3) 0.004(3) 0.011(3) C24 0.055(4) 0.054(3) 0.064(4) 0.007(3) 0.004(3) 0.003(3) C25 0.061(4) 0.064(4) 0.064(4) 0.008(3) -0.007(3) -0.006(3) C26 0.056(4) 0.057(4) 0.072(4) 0.017(3) -0.019(3) -0.013(3) C27 0.057(4) 0.070(4) 0.078(5) 0.021(4) -0.012(3) -0.002(3) C28 0.058(4) 0.084(5) 0.112(7) 0.018(5) -0.023(5) -0.022(4) C29 0.077(5) 0.085(5) 0.074(5) 0.002(4) -0.008(4) -0.026(4) C30 0.066(4) 0.072(4) 0.065(4) 0.003(3) -0.010(3) -0.012(3) C31 0.060(4) 0.061(4) 0.067(4) 0.008(3) -0.009(3) -0.014(3) C32 0.044(3) 0.067(4) 0.058(4) 0.007(3) -0.003(3) -0.003(3) C33 0.060(4) 0.079(5) 0.078(5) -0.009(4) -0.002(4) -0.011(4) C34 0.068(5) 0.073(5) 0.082(5) -0.016(4) 0.002(4) -0.004(4) C35 0.060(4) 0.091(5) 0.067(4) -0.001(4) 0.020(4) -0.006(4) C36 0.066(5) 0.081(5) 0.077(5) -0.002(4) -0.008(4) 0.009(4) C37 0.088(5) 0.071(5) 0.074(5) 0.002(4) -0.014(4) 0.014(4) C38 0.077(5) 0.085(5) 0.082(5) 0.008(4) 0.006(4) 0.009(4) C39 0.055(4) 0.069(4) 0.086(5) 0.008(4) -0.001(3) 0.010(3) C40 0.079(5) 0.081(5) 0.079(5) 0.015(4) 0.005(4) 0.004(4) C41 0.076(5) 0.072(4) 0.068(4) -0.001(4) -0.004(4) -0.002(4) C42 0.081(6) 0.097(6) 0.089(6) 0.005(5) 0.009(5) 0.006(5) C43 0.101(7) 0.107(7) 0.093(6) -0.004(5) 0.004(5) -0.002(6) C44 0.097(7) 0.130(8) 0.084(6) -0.010(6) -0.006(5) 0.054(6) C45 0.069(5) 0.090(6) 0.095(6) -0.003(4) -0.013(4) 0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N5 2.009(5) . ? Zn1 N3 2.010(5) . ? Zn1 N1 2.015(5) . ? Zn1 N7 2.029(5) . ? Zn1 N9 2.130(5) . ? N1 C8 1.344(8) . ? N1 C1 1.376(8) . ? N2 C8 1.335(8) . ? N2 C9 1.337(8) . ? N3 C16 1.357(8) . ? N3 C9 1.370(8) . ? N4 C16 1.333(8) . ? N4 C17 1.351(8) . ? N5 C24 1.363(8) . ? N5 C17 1.368(8) . ? N6 C25 1.325(9) . ? N6 C24 1.337(9) . ? N7 C25 1.341(9) . ? N7 C32 1.365(8) . ? N8 C1 1.300(8) . ? N8 C32 1.347(8) . ? N9 C33 1.285(9) . ? N9 C37 1.354(8) . ? N10 C44 1.314(12) . ? N10 C43 1.334(12) . ? C1 C2 1.479(9) . ? C2 C3 1.366(9) . ? C2 C7 1.402(9) . ? C3 C4 1.375(10) . ? C4 C5 1.382(10) . ? C5 C6 1.418(10) . ? C6 C7 1.387(9) . ? C7 C8 1.473(9) . ? C9 C10 1.446(9) . ? C10 C15 1.377(9) . ? C10 C11 1.406(9) . ? C11 C12 1.371(10) . ? C12 C13 1.353(11) . ? C13 C14 1.368(10) . ? C14 C15 1.396(9) . ? C15 C16 1.447(9) . ? C17 C18 1.441(9) . ? C18 C19 1.387(10) . ? C18 C23 1.406(10) . ? C19 C20 1.376(10) . ? C20 C21 1.385(12) . ? C21 C22 1.361(11) . ? C22 C23 1.379(10) . ? C23 C24 1.441(9) . ? C25 C26 1.474(9) . ? C26 C27 1.390(9) . ? C26 C31 1.400(10) . ? C27 C28 1.382(11) . ? C28 C29 1.371(12) . ? C29 C30 1.396(10) . ? C30 C31 1.366(9) . ? C31 C32 1.487(9) . ? C33 C34 1.382(11) . ? C34 C35 1.352(11) . ? C35 C36 1.381(10) . ? C35 C38 1.501(11) . ? C36 C37 1.360(10) . ? C38 C39 1.537(10) . ? C39 C40 1.526(10) . ? C40 C41 1.516(11) . ? C41 C42 1.334(11) . ? C41 C45 1.398(10) . ? C42 C43 1.420(12) . ? C44 C45 1.361(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zn1 N3 87.6(2) . . ? N5 Zn1 N1 157.8(2) . . ? N3 Zn1 N1 88.4(2) . . ? N5 Zn1 N7 88.1(2) . . ? N3 Zn1 N7 159.4(2) . . ? N1 Zn1 N7 88.0(2) . . ? N5 Zn1 N9 103.0(2) . . ? N3 Zn1 N9 97.2(2) . . ? N1 Zn1 N9 99.2(2) . . ? N7 Zn1 N9 103.4(2) . . ? C8 N1 C1 110.3(5) . . ? C8 N1 Zn1 125.0(4) . . ? C1 N1 Zn1 124.7(4) . . ? C8 N2 C9 122.2(6) . . ? C16 N3 C9 107.9(5) . . ? C16 N3 Zn1 126.3(5) . . ? C9 N3 Zn1 125.3(4) . . ? C16 N4 C17 123.1(6) . . ? C24 N5 C17 107.9(5) . . ? C24 N5 Zn1 126.1(5) . . ? C17 N5 Zn1 125.0(4) . . ? C25 N6 C24 124.1(6) . . ? C25 N7 C32 111.0(5) . . ? C25 N7 Zn1 124.4(5) . . ? C32 N7 Zn1 124.5(4) . . ? C1 N8 C32 121.6(6) . . ? C33 N9 C37 114.4(6) . . ? C33 N9 Zn1 122.8(5) . . ? C37 N9 Zn1 121.7(5) . . ? C44 N10 C43 114.8(8) . . ? N8 C1 N1 130.2(6) . . ? N8 C1 C2 121.7(6) . . ? N1 C1 C2 108.1(5) . . ? C3 C2 C7 120.1(6) . . ? C3 C2 C1 133.9(6) . . ? C7 C2 C1 106.0(5) . . ? C2 C3 C4 119.0(7) . . ? C3 C4 C5 121.1(7) . . ? C4 C5 C6 121.6(7) . . ? C7 C6 C5 115.3(7) . . ? C6 C7 C2 122.7(6) . . ? C6 C7 C8 130.6(6) . . ? C2 C7 C8 106.7(6) . . ? N2 C8 N1 129.6(6) . . ? N2 C8 C7 121.4(6) . . ? N1 C8 C7 109.0(6) . . ? N2 C9 N3 127.8(6) . . ? N2 C9 C10 123.4(6) . . ? N3 C9 C10 108.8(6) . . ? C15 C10 C11 122.1(6) . . ? C15 C10 C9 107.3(6) . . ? C11 C10 C9 130.6(6) . . ? C12 C11 C10 116.2(7) . . ? C13 C12 C11 122.2(7) . . ? C12 C13 C14 122.1(7) . . ? C13 C14 C15 118.0(7) . . ? C10 C15 C14 119.4(6) . . ? C10 C15 C16 106.0(6) . . ? C14 C15 C16 134.6(7) . . ? N4 C16 N3 127.0(6) . . ? N4 C16 C15 123.1(6) . . ? N3 C16 C15 109.9(6) . . ? N4 C17 N5 127.6(6) . . ? N4 C17 C18 123.0(6) . . ? N5 C17 C18 109.5(5) . . ? C19 C18 C23 120.5(7) . . ? C19 C18 C17 132.8(7) . . ? C23 C18 C17 106.7(6) . . ? C20 C19 C18 117.4(7) . . ? C19 C20 C21 121.9(7) . . ? C22 C21 C20 120.8(8) . . ? C21 C22 C23 118.7(8) . . ? C22 C23 C18 120.5(7) . . ? C22 C23 C24 133.8(7) . . ? C18 C23 C24 105.7(6) . . ? N6 C24 N5 126.1(6) . . ? N6 C24 C23 123.6(6) . . ? N5 C24 C23 110.3(6) . . ? N6 C25 N7 129.1(6) . . ? N6 C25 C26 122.5(6) . . ? N7 C25 C26 108.4(6) . . ? C27 C26 C31 120.3(6) . . ? C27 C26 C25 132.6(7) . . ? C31 C26 C25 107.1(6) . . ? C28 C27 C26 116.8(8) . . ? C29 C28 C27 121.8(7) . . ? C28 C29 C30 122.5(7) . . ? C31 C30 C29 115.4(7) . . ? C30 C31 C26 123.1(6) . . ? C30 C31 C32 131.3(7) . . ? C26 C31 C32 105.5(6) . . ? N8 C32 N7 129.1(6) . . ? N8 C32 C31 122.6(6) . . ? N7 C32 C31 108.1(6) . . ? N9 C33 C34 126.0(7) . . ? C35 C34 C33 118.3(7) . . ? C34 C35 C36 118.5(7) . . ? C34 C35 C38 121.6(7) . . ? C36 C35 C38 119.7(7) . . ? C37 C36 C35 117.6(7) . . ? N9 C37 C36 125.1(7) . . ? C35 C38 C39 110.7(6) . . ? C40 C39 C38 112.6(6) . . ? C41 C40 C39 113.7(6) . . ? C42 C41 C45 118.8(8) . . ? C42 C41 C40 123.2(8) . . ? C45 C41 C40 118.0(7) . . ? C41 C42 C43 117.3(9) . . ? N10 C43 C42 125.0(9) . . ? N10 C44 C45 125.2(9) . . ? C44 C45 C41 118.9(9) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.466 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.123