Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Goldberg, Israel' 'Diski-Posner, Yael' 'Patra, Goutam Kumar' _publ_contact_author_name 'Prof Israel Goldberg' _publ_contact_author_address ; School of Chemistry Tel Aviv University Ramat Aviv Campus Tel Aviv 69978 ISRAEL ; _publ_contact_author_email 'GOLDBERG@POST.TAU.AC.IL' _publ_section_title ; Crystal-engineering of metalloporphyrin assemblies. New supramolecular architectures mediated by bipyridyl ligands ; data_Compound-4 _database_code_CSD 182545 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C44 H28 N4 O4 Zn), 3(C12 H10 N4), 13(C6 H5 N O2)' _chemical_formula_sum 'C202 H151 N33 O34 Zn2' _chemical_formula_weight 3715.30 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 13.6390(3) _cell_length_b 14.9790(3) _cell_length_c 23.0890(6) _cell_angle_alpha 79.3850(8) _cell_angle_beta 75.3600(8) _cell_angle_gamma 87.3800(16) _cell_volume 4485.80(18) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 12479 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 27.89 _exptl_crystal_description 'needles' _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1926 _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.7 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19762 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0944 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.89 _reflns_number_total 19762 _reflns_number_gt 12479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'SIR-97' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+6.9067P] 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 19762 _refine_ls_number_parameters 1229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1309 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.2008 _refine_ls_wR_factor_gt 0.1706 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.496 _refine_ls_shift/su_mean 0.085 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 0.7396(2) 0.59152(19) 0.27828(12) 0.0211(6) Uani 1 1 d . . . N2 N 0.8927(2) 0.45646(19) 0.24602(13) 0.0230(6) Uani 1 1 d . . . N3 N 0.7453(2) 0.31446(19) 0.30629(12) 0.0211(6) Uani 1 1 d . . . N4 N 0.5928(2) 0.44971(18) 0.34015(12) 0.0208(6) Uani 1 1 d . . . C5 C 0.5328(2) 0.5232(2) 0.35282(15) 0.0234(7) Uani 1 1 d . . . C6 C 0.5616(2) 0.6145(2) 0.33250(15) 0.0213(7) Uani 1 1 d . . . C7 C 0.6582(2) 0.6450(2) 0.29691(15) 0.0212(7) Uani 1 1 d . . . C8 C 0.6859(3) 0.7397(2) 0.27521(16) 0.0241(7) Uani 1 1 d . . . H8 H 0.6431 0.7907 0.2816 0.029 Uiso 1 1 calc R . . C9 C 0.7844(3) 0.7418(2) 0.24405(17) 0.0274(8) Uani 1 1 d . . . H9 H 0.8234 0.7946 0.2241 0.033 Uiso 1 1 calc R . . C10 C 0.8193(2) 0.6488(2) 0.24662(15) 0.0226(7) Uani 1 1 d . . . C11 C 0.9184(2) 0.6231(2) 0.22129(16) 0.0232(7) Uani 1 1 d . . . C12 C 0.9517(3) 0.5333(2) 0.22122(16) 0.0248(8) Uani 1 1 d . . . C13 C 1.0539(3) 0.5058(3) 0.19529(18) 0.0320(9) Uani 1 1 d . . . H13 H 1.1099 0.5452 0.1757 0.038 Uiso 1 1 calc R . . C14 C 1.0558(3) 0.4141(3) 0.20388(19) 0.0330(9) Uani 1 1 d . . . H14 H 1.1127 0.3771 0.1908 0.040 Uiso 1 1 calc R . . C15 C 0.9544(2) 0.3828(2) 0.23681(17) 0.0260(8) Uani 1 1 d . . . C16 C 0.9255(2) 0.2913(2) 0.25692(16) 0.0245(7) Uani 1 1 d . . . C17 C 0.8290(2) 0.2606(2) 0.29123(16) 0.0228(7) Uani 1 1 d . . . C18 C 0.8046(3) 0.1676(2) 0.31953(17) 0.0271(8) Uani 1 1 d . . . H18 H 0.8495 0.1173 0.3166 0.033 Uiso 1 1 calc R . . C19 C 0.7066(3) 0.1649(2) 0.35094(17) 0.0271(8) Uani 1 1 d . . . H19 H 0.6694 0.1126 0.3741 0.033 Uiso 1 1 calc R . . C20 C 0.6689(2) 0.2568(2) 0.34258(15) 0.0223(7) Uani 1 1 d . . . C21 C 0.5701(2) 0.2835(2) 0.36950(15) 0.0214(7) Uani 1 1 d . . . C22 C 0.5367(2) 0.3731(2) 0.36971(15) 0.0229(7) Uani 1 1 d . . . C23 C 0.4373(3) 0.3998(2) 0.40196(16) 0.0263(8) Uani 1 1 d . . . H23 H 0.3837 0.3603 0.4258 0.032 Uiso 1 1 calc R . . C24 C 0.4354(3) 0.4918(2) 0.39171(16) 0.0272(8) Uani 1 1 d . . . H24 H 0.3802 0.5289 0.4072 0.033 Uiso 1 1 calc R . . C25 C 0.4866(2) 0.6854(2) 0.35322(15) 0.0221(7) Uani 1 1 d . . . C26 C 0.5064(2) 0.7427(2) 0.38981(15) 0.0219(7) Uani 1 1 d . . . H26 H 0.5697 0.7383 0.4003 0.026 Uiso 1 1 calc R . . C27 C 0.4366(2) 0.8060(2) 0.41143(16) 0.0224(7) Uani 1 1 d . . . H27 H 0.4523 0.8447 0.4362 0.027 Uiso 1 1 calc R . . C28 C 0.3431(2) 0.8130(2) 0.39685(16) 0.0230(7) Uani 1 1 d . . . C29 C 0.3224(3) 0.7583(2) 0.35920(17) 0.0272(8) Uani 1 1 d . . . H29 H 0.2597 0.7641 0.3480 0.033 Uiso 1 1 calc R . . C30 C 0.3931(3) 0.6952(2) 0.33780(16) 0.0259(8) Uani 1 1 d . . . H30 H 0.3779 0.6577 0.3122 0.031 Uiso 1 1 calc R . . O31 O 0.27604(17) 0.87598(16) 0.42088(11) 0.0277(6) Uani 1 1 d . . . H31 H 0.2070 0.8633 0.4199 0.070(16) Uiso 1 1 d R . . C32 C 0.9962(2) 0.6967(2) 0.19500(16) 0.0245(8) Uani 1 1 d . . . C33 C 1.0176(3) 0.7538(2) 0.23122(18) 0.0288(8) Uani 1 1 d . . . H33 H 0.9810 0.7468 0.2727 0.035 Uiso 1 1 calc R . . C34 C 1.0916(3) 0.8213(3) 0.20826(19) 0.0340(9) Uani 1 1 d . . . H34 H 1.1045 0.8603 0.2337 0.041 Uiso 1 1 calc R . . C35 C 1.1459(3) 0.8309(3) 0.1481(2) 0.0397(10) Uani 1 1 d . . . C36 C 1.1259(3) 0.7746(3) 0.1116(2) 0.0446(11) Uani 1 1 d . . . H36 H 1.1635 0.7809 0.0703 0.054 Uiso 1 1 calc R . . C37 C 1.0511(3) 0.7087(3) 0.13484(19) 0.0378(10) Uani 1 1 d . . . H37 H 1.0372 0.6710 0.1090 0.045 Uiso 1 1 calc R . . O38 O 1.2211(2) 0.8950(2) 0.12331(15) 0.0543(9) Uani 1 1 d . . . H38 H 1.2159 0.9479 0.1477 0.13(3) Uiso 1 1 d R . . C39 C 1.0036(3) 0.2204(2) 0.24066(17) 0.0260(8) Uani 1 1 d . . . C40 C 0.9911(3) 0.1620(2) 0.20287(18) 0.0296(8) Uani 1 1 d . . . H40 H 0.9315 0.1661 0.1884 0.036 Uiso 1 1 calc R . . C41 C 1.0644(3) 0.0974(3) 0.18580(19) 0.0322(9) Uani 1 1 d . . . H41 H 1.0547 0.0583 0.1597 0.039 Uiso 1 1 calc R . . C42 C 1.1515(3) 0.0903(2) 0.20708(19) 0.0316(9) Uani 1 1 d . . . C43 C 1.1643(3) 0.1470(2) 0.24566(18) 0.0313(9) Uani 1 1 d . . . H43 H 1.2232 0.1420 0.2608 0.038 Uiso 1 1 calc R . . C44 C 1.0910(3) 0.2111(3) 0.26207(18) 0.0306(8) Uani 1 1 d . . . H44 H 1.1006 0.2497 0.2886 0.037 Uiso 1 1 calc R . . O45 O 1.22160(19) 0.02533(18) 0.18970(14) 0.0404(7) Uani 1 1 d . . . H45 H 1.2962 0.0330 0.1934 0.11(2) Uiso 1 1 d R . . C46 C 0.4980(2) 0.2075(2) 0.40264(16) 0.0232(7) Uani 1 1 d . . . C47 C 0.4594(3) 0.1941(2) 0.46573(16) 0.0266(8) Uani 1 1 d . . . H47 H 0.4738 0.2377 0.4875 0.032 Uiso 1 1 calc R . . C48 C 0.4011(3) 0.1198(3) 0.49718(17) 0.0294(8) Uani 1 1 d . . . H48 H 0.3768 0.1123 0.5401 0.035 Uiso 1 1 calc R . . C49 C 0.3778(2) 0.0559(2) 0.46620(17) 0.0256(8) Uani 1 1 d . . . C50 C 0.4111(3) 0.0696(2) 0.40323(17) 0.0276(8) Uani 1 1 d . . . H50 H 0.3927 0.0279 0.3813 0.033 Uiso 1 1 calc R . . C51 C 0.4711(3) 0.1442(2) 0.37226(17) 0.0277(8) Uani 1 1 d . . . H51 H 0.4945 0.1523 0.3292 0.033 Uiso 1 1 calc R . . O52 O 0.32190(18) -0.01839(17) 0.49933(12) 0.0314(6) Uani 1 1 d . . . H52 H 0.3012 -0.0562 0.4755 0.09(2) Uiso 1 1 d R . . Zn53 Zn 0.73609(3) 0.45283(3) 0.280628(18) 0.01987(12) Uani 1 1 d . . . N54 N 0.6850(2) 0.45213(19) 0.19952(12) 0.0222(6) Uani 1 1 d . . . C55 C 0.6494(3) 0.5275(3) 0.17043(16) 0.0269(8) Uani 1 1 d . . . H55 H 0.6520 0.5830 0.1844 0.032 Uiso 1 1 calc R . . C56 C 0.6087(3) 0.5283(3) 0.12079(16) 0.0294(8) Uani 1 1 d . . . H56 H 0.5838 0.5830 0.1015 0.035 Uiso 1 1 calc R . . C57 C 0.6053(3) 0.4476(3) 0.10001(16) 0.0282(8) Uani 1 1 d . . . C58 C 0.6428(3) 0.3694(3) 0.12953(17) 0.0315(8) Uani 1 1 d . . . H58 H 0.6422 0.3132 0.1161 0.038 Uiso 1 1 calc R . . C59 C 0.6814(3) 0.3747(3) 0.17914(16) 0.0290(8) Uani 1 1 d . . . H59 H 0.7062 0.3208 0.1995 0.035 Uiso 1 1 calc R . . C60 C 0.5617(3) 0.4420(3) 0.04854(17) 0.0337(9) Uani 1 1 d . . . H60 H 0.5655 0.3866 0.0337 0.040 Uiso 1 1 calc R . . N61 N 0.5190(2) 0.5104(2) 0.02377(14) 0.0339(8) Uani 1 1 d . . . N62 N 1.0949(2) 0.8680(2) 0.39918(15) 0.0334(8) Uani 1 1 d . . . C63 C 1.0811(3) 0.9299(3) 0.35243(19) 0.0350(9) Uani 1 1 d . . . H63 H 1.1357 0.9696 0.3306 0.042 Uiso 1 1 calc R . . C64 C 0.9921(3) 0.9397(3) 0.33405(19) 0.0357(9) Uani 1 1 d . . . H64 H 0.9860 0.9844 0.3002 0.043 Uiso 1 1 calc R . . C65 C 0.9111(3) 0.8824(3) 0.36616(18) 0.0297(8) Uani 1 1 d . . . C66 C 0.9241(3) 0.8182(3) 0.41515(19) 0.0345(9) Uani 1 1 d . . . H66 H 0.8706 0.7780 0.4380 0.041 Uiso 1 1 calc R . . C67 C 1.0166(3) 0.8138(3) 0.43022(19) 0.0362(9) Uani 1 1 d . . . H67 H 1.0248 0.7702 0.4642 0.043 Uiso 1 1 calc R . . C68 C 0.8137(3) 0.8887(3) 0.34957(18) 0.0292(8) Uani 1 1 d . . . H68 H 0.7610 0.8467 0.3707 0.035 Uiso 1 1 calc R . . N69 N 0.8002(2) 0.9512(2) 0.30638(16) 0.0325(7) Uani 1 1 d . . . N70 N 0.7012(2) 0.9486(2) 0.29840(15) 0.0307(7) Uani 1 1 d . . . C71 C 0.6881(3) 1.0100(3) 0.25499(18) 0.0323(9) Uani 1 1 d . . . H71 H 0.7420 1.0502 0.2327 0.039 Uiso 1 1 calc R . . C72 C 0.5898(3) 1.0189(3) 0.23935(17) 0.0301(8) Uani 1 1 d . . . C73 C 0.5088(3) 0.9637(3) 0.27155(18) 0.0330(9) Uani 1 1 d . . . H73 H 0.5155 0.9176 0.3046 0.040 Uiso 1 1 calc R . . C74 C 0.4183(3) 0.9762(3) 0.25526(19) 0.0378(10) Uani 1 1 d . . . H74 H 0.3629 0.9382 0.2784 0.045 Uiso 1 1 calc R . . N75 N 0.4034(2) 1.0384(2) 0.20880(15) 0.0374(8) Uani 1 1 d . . . C76 C 0.4822(3) 1.0914(3) 0.1773(2) 0.0507(12) Uani 1 1 d . . . H76 H 0.4741 1.1358 0.1437 0.061 Uiso 1 1 calc R . . C77 C 0.5751(3) 1.0842(3) 0.1917(2) 0.0503(12) Uani 1 1 d . . . H77 H 0.6287 1.1243 0.1688 0.060 Uiso 1 1 calc R . . C78 C 0.9133(4) 1.4680(4) 0.0810(2) 0.0614(15) Uani 1 1 d . . . H78 H 0.9319 1.5044 0.1061 0.074 Uiso 1 1 calc R . . C79 C 0.9346(4) 1.3740(5) 0.0877(3) 0.0725(16) Uani 1 1 d . . . H79 H 0.9691 1.3457 0.1172 0.087 Uiso 1 1 calc R . . C80 C 0.9064(5) 1.3273(5) 0.0531(3) 0.0796(18) Uani 1 1 d . . . H80 H 0.9220 1.2643 0.0581 0.095 Uiso 1 1 calc R . . C81 C 0.8571(5) 1.3605(5) 0.0108(3) 0.085(2) Uani 1 1 d . . . H81 H 0.8364 1.3210 -0.0117 0.102 Uiso 1 1 calc R . . C82 C 0.8353(4) 1.4562(5) -0.0008(3) 0.0742(18) Uani 1 1 d . . . H82 H 0.8034 1.4837 -0.0317 0.089 Uiso 1 1 calc R . . C83 C 0.8656(4) 1.5040(4) 0.0375(3) 0.0650(15) Uani 1 1 d . . . N84 N 0.8424(5) 1.6019(5) 0.0295(4) 0.101(2) Uani 1 1 d . . . O85 O 0.8073(5) 1.6361(5) -0.0131(3) 0.144(3) Uani 1 1 d . . . O86 O 0.8609(4) 1.6445(4) 0.0673(3) 0.120(2) Uani 1 1 d . . . C87 C 0.6156(5) 0.5292(7) 0.7755(4) 0.103(3) Uani 1 1 d . . . H87 H 0.6036 0.4792 0.7582 0.124 Uiso 1 1 calc R . . C88 C 0.5941(4) 0.6182(8) 0.7506(3) 0.096(3) Uani 1 1 d . . . H88 H 0.5664 0.6296 0.7160 0.115 Uiso 1 1 calc R . . C89 C 0.6135(4) 0.6897(5) 0.7768(3) 0.0731(18) Uani 1 1 d . . . H89 H 0.6003 0.7505 0.7602 0.088 Uiso 1 1 calc R . . C90 C 0.6513(3) 0.6713(4) 0.8264(2) 0.0577(13) Uani 1 1 d . . . H90 H 0.6647 0.7202 0.8442 0.069 Uiso 1 1 calc R . . C91 C 0.6708(3) 0.5852(4) 0.8516(2) 0.0577(14) Uani 1 1 d . . . H91 H 0.6957 0.5738 0.8872 0.069 Uiso 1 1 calc R . . C92 C 0.6544(4) 0.5165(5) 0.8253(3) 0.0752(18) Uani 1 1 d . . . N93 N 0.6806(5) 0.4216(5) 0.8545(5) 0.112(2) Uani 1 1 d . . . O94 O 0.7043(4) 0.4162(4) 0.9041(3) 0.121(2) Uani 1 1 d . . . O95 O 0.6757(7) 0.3664(6) 0.8232(6) 0.236(5) Uani 1 1 d . . . C96 C 0.8639(6) 0.5220(8) 0.5626(3) 0.116(4) Uani 1 1 d . . . H96 H 0.8653 0.5519 0.5223 0.139 Uiso 1 1 calc R . . C97 C 0.8826(7) 0.4335(9) 0.5738(5) 0.136(4) Uani 1 1 d . . . H97 H 0.8922 0.3993 0.5420 0.163 Uiso 1 1 calc R . . C98 C 0.8883(4) 0.3909(6) 0.6313(3) 0.089(2) Uani 1 1 d . . . H98 H 0.9062 0.3285 0.6382 0.107 Uiso 1 1 calc R . . C99 C 0.8684(4) 0.4382(5) 0.6780(3) 0.0699(16) Uani 1 1 d . . . H99 H 0.8709 0.4085 0.7177 0.084 Uiso 1 1 calc R . . C100 C 0.8443(4) 0.5306(5) 0.6675(2) 0.0711(18) Uani 1 1 d . . . H100 H 0.8299 0.5648 0.6995 0.085 Uiso 1 1 calc R . . C101 C 0.8424(4) 0.5697(6) 0.6097(2) 0.079(2) Uani 1 1 d . . . N102 N 0.8153(5) 0.6663(6) 0.5979(3) 0.105(2) Uani 1 1 d . . . O103 O 0.8155(5) 0.7035(5) 0.5464(2) 0.161(3) Uani 1 1 d . . . O104 O 0.7913(4) 0.7088(4) 0.6422(3) 0.1155(19) Uani 1 1 d . . . C105 C 0.6943(3) 0.4766(3) 0.45721(18) 0.0418(10) Uani 1 1 d . . . H105 H 0.6392 0.5146 0.4715 0.050 Uiso 1 1 calc R . . C106 C 0.6865(4) 0.3828(4) 0.4730(2) 0.0526(12) Uani 1 1 d . . . H106 H 0.6254 0.3560 0.4989 0.063 Uiso 1 1 calc R . . C107 C 0.7656(5) 0.3282(4) 0.4518(2) 0.0572(14) Uani 1 1 d . . . H107 H 0.7592 0.2641 0.4634 0.069 Uiso 1 1 calc R . . C108 C 0.8551(4) 0.3660(4) 0.4135(2) 0.0553(13) Uani 1 1 d . . . H108 H 0.9094 0.3278 0.3984 0.066 Uiso 1 1 calc R . . C109 C 0.8652(3) 0.4597(3) 0.39731(19) 0.0443(11) Uani 1 1 d . . . H109 H 0.9260 0.4866 0.3712 0.053 Uiso 1 1 calc R . . C110 C 0.7842(3) 0.5129(3) 0.42028(17) 0.0333(9) Uani 1 1 d . . . N111 N 0.7947(3) 0.6122(3) 0.40496(15) 0.0394(8) Uani 1 1 d . . . O112 O 0.8735(2) 0.6444(2) 0.37020(14) 0.0553(9) Uani 1 1 d . . . O113 O 0.7253(2) 0.6593(2) 0.42849(15) 0.0509(8) Uani 1 1 d . . . C114 C 0.3689(4) 0.2212(4) 0.9406(3) 0.0666(15) Uani 1 1 d . . . H114 H 0.3086 0.2307 0.9701 0.080 Uiso 1 1 calc R . . C115 C 0.3668(5) 0.2182(4) 0.8814(3) 0.0716(16) Uani 1 1 d . . . H115 H 0.3047 0.2252 0.8696 0.086 Uiso 1 1 calc R . . C116 C 0.4552(6) 0.2050(5) 0.8400(3) 0.093(2) Uani 1 1 d . . . H116 H 0.4539 0.2045 0.7992 0.111 Uiso 1 1 calc R . . C117 C 0.5443(6) 0.1927(7) 0.8559(4) 0.120(3) Uani 1 1 d . . . H117 H 0.6043 0.1819 0.8266 0.144 Uiso 1 1 calc R . . C118 C 0.5479(5) 0.1959(6) 0.9148(3) 0.097(2) Uani 1 1 d . . . H118 H 0.6103 0.1885 0.9263 0.116 Uiso 1 1 calc R . . C119 C 0.4608(5) 0.2098(4) 0.9555(2) 0.0635(15) Uani 1 1 d . . . N120 N 0.4643(7) 0.2123(4) 1.0176(3) 0.100(2) Uani 1 1 d . . . O121 O 0.5448(6) 0.2151(4) 1.0303(3) 0.131(2) Uani 1 1 d . . . O122 O 0.3828(6) 0.2138(5) 1.0559(3) 0.155(3) Uani 1 1 d . . . C123 C 0.8032(4) 0.9982(3) -0.0006(3) 0.093(3) Uani 0.710(6) 1 d PG A 1 C124 C 0.8210(4) 0.9278(4) -0.0337(2) 0.067(2) Uani 0.710(6) 1 d PG A 1 C125 C 0.8834(4) 0.8559(3) -0.0187(2) 0.076(3) Uani 0.710(6) 1 d PG A 1 C126 C 0.9281(4) 0.8544(4) 0.0293(3) 0.070(3) Uani 0.710(6) 1 d PG A 1 C127 C 0.9103(4) 0.9248(5) 0.0624(2) 0.181(9) Uani 0.710(6) 1 d PG A 1 C128 C 0.8479(4) 0.9967(4) 0.0474(3) 0.069(3) Uani 0.710(6) 1 d PG A 1 N129 N 0.8311(5) 1.0629(7) 0.0784(4) 0.089(2) Uani 0.710(6) 1 d P A 1 O130 O 0.8704(5) 1.0589(6) 0.1242(3) 0.115(3) Uani 0.710(6) 1 d P A 1 O131 O 0.7791(5) 1.1374(5) 0.0672(4) 0.108(3) Uani 0.710(6) 1 d P A 1 C132 C 0.9959(5) 1.0236(4) 0.4872(3) 0.046(2) Uiso 0.50 1 d PG . . C133 C 1.0832(3) 1.0009(4) 0.5072(3) 0.0219(15) Uiso 0.50 1 d PG . . C134 C 1.0833(6) 0.9264(5) 0.5531(3) 0.065(3) Uiso 0.50 1 d PG . . C135 C 0.9960(8) 0.8746(6) 0.5790(4) 0.131(15) Uiso 0.50 1 d PG . . C136 C 0.9086(6) 0.8973(6) 0.5590(4) 0.096(4) Uiso 0.50 1 d PG . . C137 C 0.9085(4) 0.9718(5) 0.5131(4) 0.052(3) Uiso 0.50 1 d PG . . N138 N 0.9951(9) 1.1075(9) 0.4374(7) 0.077(4) Uiso 0.50 1 d P . . O139 O 0.9081(13) 1.1304(12) 0.4332(8) 0.177(6) Uiso 0.50 1 d P . . O140 O 1.0610(11) 1.1381(9) 0.4189(6) 0.108(4) Uiso 0.50 1 d P . . C'23 C 0.8796(11) 0.9858(10) 0.1109(7) 0.028(3) Uiso 0.290(4) 1 d P A 2 C'24 C 0.9229(14) 0.9035(13) 0.0613(9) 0.044(5) Uiso 0.290(4) 1 d P A 2 C'25 C 0.8616(11) 0.9298(11) 0.0102(7) 0.034(4) Uiso 0.290(4) 1 d P A 2 C'26 C 0.8046(16) 1.0087(15) 0.0085(10) 0.068(6) Uiso 0.290(4) 1 d P A 2 C'28 C 0.8337(14) 1.0614(14) 0.0770(9) 0.051(5) Uiso 0.290(4) 1 d P A 2 N'29 N 0.7849(11) 1.1196(10) 0.0768(7) 0.044(4) Uiso 0.290(4) 1 d P A 2 O'30 O 0.7921(6) 1.1569(6) 0.1294(4) 0.022(2) Uiso 0.290(4) 1 d P A 2 O'31 O 0.7268(8) 1.1719(8) 0.0518(5) 0.040(3) Uiso 0.290(4) 1 d P A 2 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 0.0213(15) 0.0204(15) 0.0223(15) -0.0042(12) -0.0058(11) -0.0033(11) N2 0.0228(15) 0.0183(15) 0.0289(16) -0.0033(12) -0.0088(12) 0.0000(12) N3 0.0209(14) 0.0191(15) 0.0240(15) -0.0032(12) -0.0071(11) -0.0016(11) N4 0.0233(15) 0.0179(15) 0.0219(15) -0.0048(12) -0.0056(11) -0.0011(11) C5 0.0229(18) 0.0262(19) 0.0218(18) -0.0089(15) -0.0034(14) -0.0014(14) C6 0.0249(18) 0.0202(17) 0.0212(18) -0.0074(14) -0.0078(14) 0.0001(14) C7 0.0194(17) 0.0227(18) 0.0235(18) -0.0072(14) -0.0068(13) 0.0012(14) C8 0.0238(18) 0.0204(18) 0.0283(19) -0.0056(15) -0.0063(14) 0.0009(14) C9 0.029(2) 0.0185(18) 0.033(2) -0.0024(15) -0.0050(15) -0.0038(14) C10 0.0249(18) 0.0216(18) 0.0216(18) -0.0045(14) -0.0051(14) -0.0030(14) C11 0.0192(17) 0.0236(19) 0.0266(19) -0.0044(15) -0.0053(14) -0.0007(14) C12 0.0239(18) 0.0249(19) 0.0250(19) -0.0030(15) -0.0052(14) -0.0050(14) C13 0.0233(19) 0.026(2) 0.042(2) -0.0044(17) 0.0006(16) -0.0025(15) C14 0.0238(19) 0.026(2) 0.046(2) -0.0031(18) -0.0035(16) -0.0014(15) C15 0.0203(18) 0.0246(19) 0.035(2) -0.0065(16) -0.0086(15) 0.0004(14) C16 0.0212(18) 0.0214(18) 0.032(2) -0.0046(15) -0.0096(14) 0.0016(14) C17 0.0234(18) 0.0197(18) 0.0274(19) -0.0028(15) -0.0112(14) -0.0012(14) C18 0.0271(19) 0.0195(18) 0.034(2) -0.0004(15) -0.0097(15) 0.0001(14) C19 0.029(2) 0.0202(18) 0.032(2) -0.0007(15) -0.0096(15) -0.0019(15) C20 0.0253(18) 0.0216(18) 0.0219(18) -0.0024(14) -0.0098(14) -0.0032(14) C21 0.0261(18) 0.0207(17) 0.0184(17) -0.0021(14) -0.0082(13) -0.0014(14) C22 0.0241(18) 0.0227(18) 0.0228(18) -0.0055(15) -0.0060(14) -0.0022(14) C23 0.0246(18) 0.0254(19) 0.027(2) -0.0065(15) -0.0024(14) -0.0016(15) C24 0.0251(19) 0.026(2) 0.027(2) -0.0071(16) 0.0017(14) -0.0038(15) C25 0.0236(18) 0.0169(17) 0.0249(19) -0.0045(14) -0.0031(14) -0.0027(13) C26 0.0199(17) 0.0220(18) 0.0258(19) -0.0044(15) -0.0089(14) -0.0006(13) C27 0.0231(18) 0.0203(18) 0.0254(19) -0.0079(15) -0.0057(14) -0.0016(14) C28 0.0237(18) 0.0183(17) 0.0258(19) -0.0020(14) -0.0050(14) -0.0010(14) C29 0.0187(17) 0.029(2) 0.038(2) -0.0103(17) -0.0116(15) 0.0014(14) C30 0.0258(19) 0.0242(19) 0.031(2) -0.0100(16) -0.0086(15) 0.0000(15) O31 0.0201(13) 0.0248(13) 0.0406(15) -0.0134(11) -0.0072(10) 0.0023(10) C32 0.0227(18) 0.0186(18) 0.029(2) -0.0036(15) 0.0002(14) -0.0018(14) C33 0.0235(19) 0.027(2) 0.034(2) -0.0090(16) -0.0017(15) -0.0014(15) C34 0.030(2) 0.027(2) 0.045(2) -0.0115(18) -0.0045(17) -0.0015(16) C35 0.031(2) 0.024(2) 0.056(3) -0.0084(19) 0.0053(18) -0.0072(16) C36 0.048(3) 0.035(2) 0.040(2) -0.010(2) 0.0131(19) -0.0122(19) C37 0.043(2) 0.028(2) 0.038(2) -0.0093(18) 0.0027(18) -0.0114(17) O38 0.0427(18) 0.0340(17) 0.071(2) -0.0132(16) 0.0190(15) -0.0199(14) C39 0.0204(18) 0.0203(18) 0.035(2) -0.0006(16) -0.0064(14) -0.0005(14) C40 0.0185(18) 0.025(2) 0.044(2) -0.0024(17) -0.0085(15) 0.0013(14) C41 0.026(2) 0.025(2) 0.047(2) -0.0106(18) -0.0097(17) 0.0028(15) C42 0.0228(19) 0.0199(19) 0.049(2) -0.0041(17) -0.0058(16) 0.0028(15) C43 0.0210(18) 0.025(2) 0.047(2) 0.0001(17) -0.0116(16) 0.0014(15) C44 0.0270(19) 0.025(2) 0.040(2) -0.0070(17) -0.0100(16) 0.0007(15) O45 0.0241(14) 0.0301(15) 0.068(2) -0.0138(14) -0.0111(13) 0.0083(11) C46 0.0214(17) 0.0216(18) 0.0263(19) -0.0038(15) -0.0060(14) -0.0001(14) C47 0.033(2) 0.027(2) 0.0219(19) -0.0050(15) -0.0077(15) -0.0067(15) C48 0.033(2) 0.031(2) 0.0230(19) -0.0027(16) -0.0052(15) -0.0077(16) C49 0.0207(18) 0.0219(18) 0.033(2) -0.0027(15) -0.0063(14) -0.0025(14) C50 0.0281(19) 0.0252(19) 0.032(2) -0.0106(16) -0.0068(15) -0.0039(15) C51 0.030(2) 0.028(2) 0.0246(19) -0.0084(16) -0.0042(15) -0.0053(15) O52 0.0281(13) 0.0258(14) 0.0376(15) -0.0035(12) -0.0029(11) -0.0097(11) Zn53 0.0201(2) 0.0189(2) 0.0215(2) -0.00354(15) -0.00672(15) -0.00061(15) N54 0.0208(15) 0.0257(16) 0.0207(15) -0.0036(12) -0.0068(11) -0.0003(12) C55 0.0277(19) 0.030(2) 0.0245(19) -0.0038(16) -0.0096(15) -0.0005(15) C56 0.0253(19) 0.036(2) 0.027(2) -0.0024(17) -0.0104(15) 0.0023(16) C57 0.0252(19) 0.039(2) 0.0224(19) -0.0061(16) -0.0078(14) -0.0024(16) C58 0.037(2) 0.033(2) 0.027(2) -0.0062(17) -0.0120(16) -0.0057(17) C59 0.036(2) 0.027(2) 0.026(2) -0.0005(16) -0.0126(16) -0.0010(16) C60 0.031(2) 0.046(3) 0.027(2) -0.0102(18) -0.0087(16) -0.0060(18) N61 0.0308(17) 0.050(2) 0.0256(17) -0.0075(16) -0.0148(13) 0.0009(15) N62 0.0263(17) 0.0361(19) 0.044(2) -0.0174(16) -0.0128(14) 0.0060(14) C63 0.0227(19) 0.037(2) 0.045(2) -0.0083(19) -0.0075(17) 0.0027(16) C64 0.029(2) 0.037(2) 0.043(2) -0.0067(19) -0.0116(17) 0.0023(17) C65 0.0270(19) 0.027(2) 0.039(2) -0.0148(17) -0.0089(16) 0.0027(15) C66 0.032(2) 0.033(2) 0.041(2) -0.0088(18) -0.0112(17) -0.0022(17) C67 0.033(2) 0.038(2) 0.042(2) -0.0115(19) -0.0147(18) 0.0075(18) C68 0.0238(19) 0.026(2) 0.039(2) -0.0095(17) -0.0076(16) 0.0013(15) N69 0.0236(16) 0.0259(17) 0.051(2) -0.0086(16) -0.0139(14) 0.0018(13) N70 0.0230(16) 0.0234(17) 0.049(2) -0.0086(15) -0.0131(14) 0.0026(12) C71 0.031(2) 0.025(2) 0.043(2) -0.0044(18) -0.0139(17) -0.0003(16) C72 0.032(2) 0.026(2) 0.034(2) -0.0058(16) -0.0105(16) 0.0039(16) C73 0.026(2) 0.035(2) 0.032(2) 0.0038(17) -0.0054(16) 0.0066(16) C74 0.026(2) 0.043(2) 0.039(2) 0.0015(19) -0.0043(17) 0.0046(17) N75 0.0305(18) 0.042(2) 0.039(2) -0.0046(16) -0.0126(15) 0.0134(15) C76 0.048(3) 0.050(3) 0.049(3) 0.017(2) -0.020(2) -0.001(2) C77 0.049(3) 0.045(3) 0.055(3) 0.011(2) -0.024(2) -0.010(2) C78 0.056(3) 0.081(4) 0.043(3) -0.025(3) 0.010(2) -0.017(3) C79 0.074(4) 0.084(5) 0.054(4) -0.026(3) 0.002(3) -0.003(3) C80 0.073(4) 0.082(5) 0.071(4) -0.013(4) 0.002(3) 0.004(3) C81 0.074(4) 0.110(6) 0.067(4) -0.057(4) 0.021(3) -0.024(4) C82 0.047(3) 0.125(6) 0.050(3) -0.027(4) -0.005(2) 0.002(3) C83 0.046(3) 0.065(4) 0.065(4) -0.007(3) 0.017(3) -0.002(3) N84 0.065(4) 0.091(5) 0.119(6) -0.007(4) 0.022(4) -0.006(3) O85 0.111(5) 0.149(6) 0.124(5) 0.043(4) -0.002(4) 0.044(4) O86 0.088(4) 0.079(4) 0.177(6) -0.036(4) 0.011(4) -0.017(3) C87 0.042(4) 0.157(8) 0.124(7) -0.099(6) 0.010(4) -0.011(4) C88 0.031(3) 0.217(10) 0.048(3) -0.048(5) -0.007(2) 0.004(4) C89 0.047(3) 0.112(5) 0.051(3) 0.006(3) -0.009(2) -0.003(3) C90 0.042(3) 0.073(4) 0.055(3) -0.010(3) -0.008(2) -0.015(2) C91 0.030(2) 0.086(4) 0.051(3) -0.005(3) -0.001(2) -0.011(2) C92 0.030(3) 0.095(5) 0.094(5) -0.030(4) 0.006(3) -0.007(3) N93 0.062(4) 0.089(5) 0.176(8) -0.039(6) -0.002(4) -0.016(3) O94 0.070(3) 0.126(5) 0.141(5) -0.004(4) 0.006(3) 0.011(3) O95 0.221(10) 0.130(7) 0.381(16) -0.126(9) -0.061(9) 0.009(6) C96 0.108(6) 0.212(11) 0.037(4) -0.033(6) -0.012(3) -0.089(7) C97 0.109(6) 0.221(12) 0.098(7) -0.087(9) -0.008(5) -0.076(8) C98 0.048(3) 0.156(7) 0.081(5) -0.065(5) -0.011(3) -0.030(4) C99 0.043(3) 0.103(5) 0.064(4) -0.022(4) -0.009(2) 0.007(3) C100 0.044(3) 0.131(6) 0.039(3) -0.019(3) -0.006(2) -0.017(3) C101 0.060(3) 0.131(6) 0.043(3) 0.016(4) -0.020(3) -0.055(4) N102 0.106(4) 0.147(6) 0.067(4) 0.029(4) -0.051(3) -0.077(4) O103 0.211(6) 0.204(7) 0.070(3) 0.070(4) -0.081(4) -0.135(5) O104 0.135(4) 0.123(5) 0.089(4) 0.035(3) -0.057(3) -0.054(4) C105 0.041(2) 0.054(3) 0.030(2) -0.001(2) -0.0124(18) -0.009(2) C106 0.062(3) 0.059(3) 0.036(3) 0.005(2) -0.015(2) -0.025(3) C107 0.098(4) 0.046(3) 0.037(3) -0.003(2) -0.034(3) -0.014(3) C108 0.077(4) 0.059(3) 0.037(3) -0.019(2) -0.022(2) 0.009(3) C109 0.043(2) 0.060(3) 0.033(2) -0.011(2) -0.0119(18) -0.008(2) C110 0.037(2) 0.042(2) 0.022(2) -0.0017(17) -0.0111(16) -0.0093(18) N111 0.043(2) 0.049(2) 0.0310(19) -0.0030(17) -0.0203(16) -0.0117(18) O112 0.061(2) 0.064(2) 0.0387(18) -0.0033(16) -0.0064(15) -0.0334(17) O113 0.0473(19) 0.051(2) 0.059(2) -0.0066(16) -0.0238(16) 0.0058(16) C114 0.074(4) 0.054(3) 0.070(4) -0.005(3) -0.021(3) 0.015(3) C115 0.087(4) 0.061(4) 0.082(4) -0.019(3) -0.048(4) 0.019(3) C116 0.115(6) 0.109(6) 0.074(4) -0.045(4) -0.049(4) 0.049(5) C117 0.096(6) 0.191(9) 0.083(5) -0.053(6) -0.033(4) 0.065(6) C118 0.064(4) 0.146(7) 0.086(5) -0.024(5) -0.032(4) 0.027(4) C119 0.095(4) 0.053(3) 0.052(3) -0.011(3) -0.035(3) 0.008(3) N120 0.189(7) 0.061(3) 0.067(4) -0.007(3) -0.068(5) 0.021(4) O121 0.221(7) 0.098(4) 0.108(4) 0.016(3) -0.121(5) -0.039(4) O122 0.219(7) 0.182(7) 0.059(3) -0.035(4) -0.036(4) 0.097(6) C123 0.090(7) 0.066(6) 0.083(7) 0.012(5) 0.037(5) -0.010(5) C124 0.091(6) 0.046(5) 0.055(5) -0.007(4) -0.004(4) 0.001(4) C125 0.088(6) 0.047(5) 0.080(6) 0.006(4) -0.006(5) -0.004(4) C126 0.061(5) 0.068(6) 0.069(5) 0.036(4) -0.026(4) -0.027(4) C127 0.041(5) 0.055(6) 0.38(2) -0.037(10) 0.064(9) -0.015(4) C128 0.060(5) 0.074(6) 0.060(5) -0.026(5) 0.025(4) -0.042(4) N129 0.053(4) 0.121(7) 0.076(5) -0.007(5) 0.011(4) -0.022(4) O130 0.086(5) 0.193(9) 0.078(5) -0.055(5) -0.013(4) -0.038(5) O131 0.073(4) 0.065(4) 0.167(7) -0.038(4) 0.018(4) -0.011(3) _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 C7 1.366(4) . ? N1 C10 1.380(4) . ? N1 Zn53 2.071(3) . ? N2 C15 1.373(4) . ? N2 C12 1.382(4) . ? N2 Zn53 2.082(3) . ? N3 C17 1.376(4) . ? N3 C20 1.382(4) . ? N3 Zn53 2.055(3) . ? N4 C5 1.371(4) . ? N4 C22 1.377(4) . ? N4 Zn53 2.083(3) . ? C5 C6 1.403(5) . ? C5 C24 1.446(5) . ? C6 C7 1.409(5) . ? C6 C25 1.498(5) . ? C7 C8 1.449(5) . ? C8 C9 1.353(5) . ? C8 H8 0.9500 . ? C9 C10 1.446(5) . ? C9 H9 0.9500 . ? C10 C11 1.398(5) . ? C11 C12 1.399(5) . ? C11 C32 1.498(5) . ? C12 C13 1.446(5) . ? C13 C14 1.352(5) . ? C13 H13 0.9500 . ? C14 C15 1.452(5) . ? C14 H14 0.9500 . ? C15 C16 1.403(5) . ? C16 C17 1.402(5) . ? C16 C39 1.498(5) . ? C17 C18 1.440(5) . ? C18 C19 1.349(5) . ? C18 H18 0.9500 . ? C19 C20 1.443(5) . ? C19 H19 0.9500 . ? C20 C21 1.408(5) . ? C21 C22 1.398(5) . ? C21 C46 1.500(5) . ? C22 C23 1.450(5) . ? C23 C24 1.355(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.388(5) . ? C25 C30 1.404(5) . ? C26 C27 1.380(5) . ? C26 H26 0.9500 . ? C27 C28 1.395(5) . ? C27 H27 0.9500 . ? C28 O31 1.375(4) . ? C28 C29 1.384(5) . ? C29 C30 1.384(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? O31 H31 0.9762 . ? C32 C37 1.385(5) . ? C32 C33 1.389(5) . ? C33 C34 1.395(5) . ? C33 H33 0.9500 . ? C34 C35 1.384(6) . ? C34 H34 0.9500 . ? C35 C36 1.377(6) . ? C35 O38 1.376(5) . ? C36 C37 1.388(6) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? O38 H38 1.0437 . ? C39 C40 1.388(5) . ? C39 C44 1.394(5) . ? C40 C41 1.394(5) . ? C40 H40 0.9500 . ? C41 C42 1.389(5) . ? C41 H41 0.9500 . ? C42 O45 1.374(4) . ? C42 C43 1.385(6) . ? C43 C44 1.385(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? O45 H45 1.0548 . ? C46 C51 1.389(5) . ? C46 C47 1.398(5) . ? C47 C48 1.374(5) . ? C47 H47 0.9500 . ? C48 C49 1.388(5) . ? C48 H48 0.9500 . ? C49 O52 1.369(4) . ? C49 C50 1.388(5) . ? C50 C51 1.388(5) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? O52 H52 0.9536 . ? Zn53 N54 2.159(3) . ? N54 C59 1.337(5) . ? N54 C55 1.341(5) . ? C55 C56 1.392(5) . ? C55 H55 0.9500 . ? C56 C57 1.387(5) . ? C56 H56 0.9500 . ? C57 C58 1.387(5) . ? C57 C60 1.474(5) . ? C58 C59 1.391(5) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 N61 1.269(5) . ? C60 H60 0.9500 . ? N61 N61 1.413(6) 2_665 ? N62 C63 1.333(5) . ? N62 C67 1.338(5) . ? C63 C64 1.377(5) . ? C63 H63 0.9500 . ? C64 C65 1.394(6) . ? C64 H64 0.9500 . ? C65 C66 1.386(6) . ? C65 C68 1.468(5) . ? C66 C67 1.387(5) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 N69 1.280(5) . ? C68 H68 0.9500 . ? N69 N70 1.412(4) . ? N70 C71 1.272(5) . ? C71 C72 1.468(5) . ? C71 H71 0.9500 . ? C72 C73 1.377(5) . ? C72 C77 1.381(6) . ? C73 C74 1.374(5) . ? C73 H73 0.9500 . ? C74 N75 1.336(5) . ? C74 H74 0.9500 . ? N75 C76 1.335(6) . ? C76 C77 1.384(6) . ? C76 H76 0.9500 . ? C77 H77 0.9500 . ? C78 C83 1.350(8) . ? C78 C79 1.413(9) . ? C78 H78 0.9500 . ? C79 C80 1.289(9) . ? C79 H79 0.9500 . ? C80 C81 1.332(10) . ? C80 H80 0.9500 . ? C81 C82 1.441(10) . ? C81 H81 0.9500 . ? C82 C83 1.383(8) . ? C82 H82 0.9500 . ? C83 N84 1.473(9) . ? N84 O85 1.221(9) . ? N84 O86 1.249(9) . ? C87 C92 1.362(11) . ? C87 C88 1.401(11) . ? C87 H87 0.9500 . ? C88 C89 1.389(10) . ? C88 H88 0.9500 . ? C89 C90 1.349(7) . ? C89 H89 0.9500 . ? C90 C91 1.358(8) . ? C90 H90 0.9500 . ? C91 C92 1.340(8) . ? C91 H91 0.9500 . ? C92 N93 1.524(10) . ? N93 O95 1.208(10) . ? N93 O94 1.255(9) . ? C96 C97 1.328(14) . ? C96 C101 1.374(11) . ? C96 H96 0.9500 . ? C97 C98 1.382(13) . ? C97 H97 0.9500 . ? C98 C99 1.363(8) . ? C98 H98 0.9500 . ? C99 C100 1.399(9) . ? C99 H99 0.9500 . ? C100 C101 1.362(8) . ? C100 H100 0.9500 . ? C101 N102 1.470(10) . ? N102 O103 1.216(7) . ? N102 O104 1.267(9) . ? C105 C110 1.373(6) . ? C105 C106 1.388(7) . ? C105 H105 0.9500 . ? C106 C107 1.367(7) . ? C106 H106 0.9500 . ? C107 C108 1.388(7) . ? C107 H107 0.9500 . ? C108 C109 1.388(7) . ? C108 H108 0.9500 . ? C109 C110 1.384(6) . ? C109 H109 0.9500 . ? C110 N111 1.470(6) . ? N111 O112 1.225(4) . ? N111 O113 1.228(5) . ? C114 C119 1.378(8) . ? C114 C115 1.382(8) . ? C114 H114 0.9500 . ? C115 C116 1.368(9) . ? C115 H115 0.9500 . ? C116 C117 1.349(9) . ? C116 H116 0.9500 . ? C117 C118 1.384(9) . ? C117 H117 0.9500 . ? C118 C119 1.351(9) . ? C118 H118 0.9500 . ? C119 N120 1.453(8) . ? N120 O121 1.209(9) . ? N120 O122 1.235(9) . ? C123 C124 1.3900 . ? C123 C128 1.3900 . ? C124 C125 1.3900 . ? C125 C126 1.3900 . ? C126 C127 1.3900 . ? C127 C128 1.3900 . ? C128 N129 1.307(10) . ? N129 O130 1.291(9) . ? N129 O131 1.316(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 N1 C10 107.1(3) . . ? C7 N1 Zn53 126.0(2) . . ? C10 N1 Zn53 125.7(2) . . ? C15 N2 C12 107.2(3) . . ? C15 N2 Zn53 126.0(2) . . ? C12 N2 Zn53 126.4(2) . . ? C17 N3 C20 106.1(3) . . ? C17 N3 Zn53 127.0(2) . . ? C20 N3 Zn53 126.9(2) . . ? C5 N4 C22 107.0(3) . . ? C5 N4 Zn53 126.5(2) . . ? C22 N4 Zn53 126.2(2) . . ? N4 C5 C6 125.6(3) . . ? N4 C5 C24 109.4(3) . . ? C6 C5 C24 125.0(3) . . ? C5 C6 C7 125.0(3) . . ? C5 C6 C25 117.8(3) . . ? C7 C6 C25 117.1(3) . . ? N1 C7 C6 126.2(3) . . ? N1 C7 C8 109.6(3) . . ? C6 C7 C8 124.2(3) . . ? C9 C8 C7 106.9(3) . . ? C9 C8 H8 126.5 . . ? C7 C8 H8 126.6 . . ? C8 C9 C10 107.5(3) . . ? C8 C9 H9 126.2 . . ? C10 C9 H9 126.3 . . ? N1 C10 C11 126.5(3) . . ? N1 C10 C9 108.9(3) . . ? C11 C10 C9 124.6(3) . . ? C10 C11 C12 124.9(3) . . ? C10 C11 C32 117.7(3) . . ? C12 C11 C32 117.3(3) . . ? N2 C12 C11 125.8(3) . . ? N2 C12 C13 108.7(3) . . ? C11 C12 C13 125.4(3) . . ? C14 C13 C12 107.8(3) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? C13 C14 C15 106.9(3) . . ? C13 C14 H14 126.5 . . ? C15 C14 H14 126.5 . . ? N2 C15 C16 125.8(3) . . ? N2 C15 C14 109.2(3) . . ? C16 C15 C14 124.9(3) . . ? C17 C16 C15 125.3(3) . . ? C17 C16 C39 117.0(3) . . ? C15 C16 C39 117.7(3) . . ? N3 C17 C16 125.7(3) . . ? N3 C17 C18 109.7(3) . . ? C16 C17 C18 124.5(3) . . ? C19 C18 C17 107.6(3) . . ? C19 C18 H18 126.2 . . ? C17 C18 H18 126.2 . . ? C18 C19 C20 106.9(3) . . ? C18 C19 H19 126.6 . . ? C20 C19 H19 126.5 . . ? N3 C20 C21 125.4(3) . . ? N3 C20 C19 109.8(3) . . ? C21 C20 C19 124.7(3) . . ? C22 C21 C20 125.5(3) . . ? C22 C21 C46 119.0(3) . . ? C20 C21 C46 115.4(3) . . ? N4 C22 C21 125.7(3) . . ? N4 C22 C23 109.3(3) . . ? C21 C22 C23 125.0(3) . . ? C24 C23 C22 106.9(3) . . ? C24 C23 H23 126.5 . . ? C22 C23 H23 126.5 . . ? C23 C24 C5 107.4(3) . . ? C23 C24 H24 126.3 . . ? C5 C24 H24 126.3 . . ? C26 C25 C30 117.4(3) . . ? C26 C25 C6 120.9(3) . . ? C30 C25 C6 121.6(3) . . ? C27 C26 C25 121.8(3) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C26 C27 C28 119.8(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? O31 C28 C29 123.4(3) . . ? O31 C28 C27 117.0(3) . . ? C29 C28 C27 119.6(3) . . ? C28 C29 C30 120.0(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 121.3(3) . . ? C29 C30 H30 119.4 . . ? C25 C30 H30 119.3 . . ? C28 O31 H31 111.3 . . ? C37 C32 C33 117.7(3) . . ? C37 C32 C11 121.8(3) . . ? C33 C32 C11 120.5(3) . . ? C32 C33 C34 121.7(4) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 119.3(4) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C36 C35 O38 118.3(4) . . ? C36 C35 C34 119.9(4) . . ? O38 C35 C34 121.9(4) . . ? C35 C36 C37 120.2(4) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C32 C37 C36 121.4(4) . . ? C32 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C35 O38 H38 113.4 . . ? C40 C39 C44 117.7(3) . . ? C40 C39 C16 120.4(3) . . ? C44 C39 C16 121.8(3) . . ? C39 C40 C41 121.3(3) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C40 119.9(4) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? O45 C42 C43 122.2(3) . . ? O45 C42 C41 118.2(3) . . ? C43 C42 C41 119.6(3) . . ? C44 C43 C42 119.9(3) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.1 . . ? C43 C44 C39 121.6(4) . . ? C43 C44 H44 119.2 . . ? C39 C44 H44 119.2 . . ? C42 O45 H45 118.0 . . ? C51 C46 C47 117.0(3) . . ? C51 C46 C21 121.3(3) . . ? C47 C46 C21 121.7(3) . . ? C48 C47 C46 122.1(3) . . ? C48 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? C47 C48 C49 120.0(3) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? O52 C49 C48 118.2(3) . . ? O52 C49 C50 122.5(3) . . ? C48 C49 C50 119.2(3) . . ? C51 C50 C49 120.0(3) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C46 121.6(3) . . ? C50 C51 H51 119.2 . . ? C46 C51 H51 119.2 . . ? C49 O52 H52 114.6 . . ? N3 Zn53 N1 163.09(11) . . ? N3 Zn53 N4 89.04(11) . . ? N1 Zn53 N4 88.43(11) . . ? N3 Zn53 N2 88.85(11) . . ? N1 Zn53 N2 88.44(11) . . ? N4 Zn53 N2 162.13(11) . . ? N3 Zn53 N54 97.24(11) . . ? N1 Zn53 N54 99.66(11) . . ? N4 Zn53 N54 96.55(11) . . ? N2 Zn53 N54 101.32(11) . . ? C59 N54 C55 117.7(3) . . ? C59 N54 Zn53 120.7(2) . . ? C55 N54 Zn53 121.4(2) . . ? N54 C55 C56 123.1(4) . . ? N54 C55 H55 118.5 . . ? C56 C55 H55 118.4 . . ? C57 C56 C55 118.7(4) . . ? C57 C56 H56 120.7 . . ? C55 C56 H56 120.7 . . ? C58 C57 C56 118.6(3) . . ? C58 C57 C60 119.2(4) . . ? C56 C57 C60 122.2(4) . . ? C57 C58 C59 118.9(4) . . ? C57 C58 H58 120.6 . . ? C59 C58 H58 120.6 . . ? N54 C59 C58 123.0(3) . . ? N54 C59 H59 118.5 . . ? C58 C59 H59 118.5 . . ? N61 C60 C57 120.9(4) . . ? N61 C60 H60 119.5 . . ? C57 C60 H60 119.6 . . ? C60 N61 N61 111.5(4) . 2_665 ? C63 N62 C67 117.5(3) . . ? N62 C63 C64 123.7(4) . . ? N62 C63 H63 118.1 . . ? C64 C63 H63 118.1 . . ? C63 C64 C65 118.6(4) . . ? C63 C64 H64 120.7 . . ? C65 C64 H64 120.7 . . ? C66 C65 C64 118.3(4) . . ? C66 C65 C68 119.7(4) . . ? C64 C65 C68 121.9(4) . . ? C65 C66 C67 118.8(4) . . ? C65 C66 H66 120.6 . . ? C67 C66 H66 120.6 . . ? N62 C67 C66 123.1(4) . . ? N62 C67 H67 118.5 . . ? C66 C67 H67 118.4 . . ? N69 C68 C65 119.6(4) . . ? N69 C68 H68 120.2 . . ? C65 C68 H68 120.2 . . ? C68 N69 N70 111.5(3) . . ? C71 N70 N69 111.5(3) . . ? N70 C71 C72 120.0(4) . . ? N70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C73 C72 C77 117.4(4) . . ? C73 C72 C71 121.9(4) . . ? C77 C72 C71 120.7(4) . . ? C74 C73 C72 119.2(4) . . ? C74 C73 H73 120.4 . . ? C72 C73 H73 120.4 . . ? N75 C74 C73 124.0(4) . . ? N75 C74 H74 118.0 . . ? C73 C74 H74 118.0 . . ? C76 N75 C74 116.8(3) . . ? N75 C76 C77 122.6(4) . . ? N75 C76 H76 118.7 . . ? C77 C76 H76 118.7 . . ? C72 C77 C76 120.0(4) . . ? C72 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C83 C78 C79 117.5(6) . . ? C83 C78 H78 121.3 . . ? C79 C78 H78 121.2 . . ? C80 C79 C78 118.9(7) . . ? C80 C79 H79 120.5 . . ? C78 C79 H79 120.6 . . ? C79 C80 C81 125.0(7) . . ? C79 C80 H80 117.5 . . ? C81 C80 H80 117.5 . . ? C80 C81 C82 120.1(6) . . ? C80 C81 H81 120.0 . . ? C82 C81 H81 120.0 . . ? C83 C82 C81 113.3(6) . . ? C83 C82 H82 123.3 . . ? C81 C82 H82 123.4 . . ? C78 C83 C82 125.2(6) . . ? C78 C83 N84 118.7(7) . . ? C82 C83 N84 116.2(7) . . ? O85 N84 O86 124.4(8) . . ? O85 N84 C83 118.7(8) . . ? O86 N84 C83 116.9(8) . . ? C92 C87 C88 118.1(7) . . ? C92 C87 H87 121.0 . . ? C88 C87 H87 121.0 . . ? C89 C88 C87 119.3(6) . . ? C89 C88 H88 120.3 . . ? C87 C88 H88 120.4 . . ? C90 C89 C88 119.0(7) . . ? C90 C89 H89 120.5 . . ? C88 C89 H89 120.5 . . ? C89 C90 C91 122.2(6) . . ? C89 C90 H90 118.9 . . ? C91 C90 H90 118.9 . . ? C92 C91 C90 118.7(6) . . ? C92 C91 H91 120.6 . . ? C90 C91 H91 120.6 . . ? C91 C92 C87 122.7(7) . . ? C91 C92 N93 116.4(7) . . ? C87 C92 N93 120.9(8) . . ? O95 N93 O94 133.1(11) . . ? O95 N93 C92 111.2(10) . . ? O94 N93 C92 115.7(7) . . ? C97 C96 C101 119.4(9) . . ? C97 C96 H96 120.3 . . ? C101 C96 H96 120.4 . . ? C96 C97 C98 120.6(8) . . ? C96 C97 H97 119.7 . . ? C98 C97 H97 119.7 . . ? C99 C98 C97 120.1(9) . . ? C99 C98 H98 119.9 . . ? C97 C98 H98 120.0 . . ? C98 C99 C100 119.9(7) . . ? C98 C99 H99 120.0 . . ? C100 C99 H99 120.0 . . ? C101 C100 C99 117.5(6) . . ? C101 C100 H100 121.3 . . ? C99 C100 H100 121.2 . . ? C100 C101 C96 122.4(9) . . ? C100 C101 N102 118.3(7) . . ? C96 C101 N102 119.3(7) . . ? O103 N102 O104 121.5(9) . . ? O103 N102 C101 119.6(8) . . ? O104 N102 C101 118.9(6) . . ? C110 C105 C106 118.0(5) . . ? C110 C105 H105 121.0 . . ? C106 C105 H105 121.0 . . ? C107 C106 C105 120.9(5) . . ? C107 C106 H106 119.5 . . ? C105 C106 H106 119.6 . . ? C106 C107 C108 120.3(5) . . ? C106 C107 H107 119.8 . . ? C108 C107 H107 119.8 . . ? C107 C108 C109 119.9(5) . . ? C107 C108 H108 120.0 . . ? C109 C108 H108 120.0 . . ? C110 C109 C108 118.2(4) . . ? C110 C109 H109 120.9 . . ? C108 C109 H109 120.9 . . ? C105 C110 C109 122.6(4) . . ? C105 C110 N111 118.5(4) . . ? C109 C110 N111 118.8(4) . . ? O112 N111 O113 122.9(4) . . ? O112 N111 C110 118.3(4) . . ? O113 N111 C110 118.8(3) . . ? C119 C114 C115 118.1(6) . . ? C119 C114 H114 120.9 . . ? C115 C114 H114 120.9 . . ? C116 C115 C114 119.3(6) . . ? C116 C115 H115 120.3 . . ? C114 C115 H115 120.3 . . ? C117 C116 C115 121.6(6) . . ? C117 C116 H116 119.2 . . ? C115 C116 H116 119.2 . . ? C116 C117 C118 119.9(7) . . ? C116 C117 H117 120.0 . . ? C118 C117 H117 120.1 . . ? C119 C118 C117 118.5(6) . . ? C119 C118 H118 120.8 . . ? C117 C118 H118 120.7 . . ? C118 C119 C114 122.5(6) . . ? C118 C119 N120 118.6(6) . . ? C114 C119 N120 118.9(6) . . ? O121 N120 O122 122.0(7) . . ? O121 N120 C119 120.4(8) . . ? O122 N120 C119 117.6(7) . . ? C124 C123 C128 120.0 . . ? C125 C124 C123 120.0 . . ? C124 C125 C126 120.0 . . ? C125 C126 C127 120.0 . . ? C128 C127 C126 120.0 . . ? N129 C128 C127 120.1(7) . . ? N129 C128 C123 119.9(7) . . ? C127 C128 C123 120.0 . . ? O130 N129 C128 119.1(9) . . ? O130 N129 O131 114.2(9) . . ? C128 N129 O131 126.6(9) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.143 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.079 #======END===================================================== data_Compound-5 _database_code_CSD 182546 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C44 H28 N4 O4 Zn), C10 H8 N2, 12(C6 H5 N O2)' _chemical_formula_sum 'C170 H124 N22 O32 Zn2' _chemical_formula_weight 3117.65 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 'orthorhombic' _symmetry_space_group_name_H-M 'Cmca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x+1/2, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x-1/2, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z-1/2' _cell_length_a 28.2500(6) _cell_length_b 26.4570(9) _cell_length_c 41.4810(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 31003.3(16) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4448 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 25.72 _exptl_crystal_description 'chunks' _exptl_crystal_colour 'red-violet' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12912 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.5 deg. Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14428 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2143 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.72 _reflns_number_total 14428 _reflns_number_gt 4448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'SHELXS-86 (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^)+(0.1028P)^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 14428 _refine_ls_number_parameters 549 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1829 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.2219 _refine_ls_wR_factor_gt 0.1872 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _refine_ls_shift/su_max 0.558 _refine_ls_shift/su_mean 0.056 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 0.0000 0.28160(19) 0.20294(12) 0.0404(14) Uani 1 2 d S . . N2 N 0.07218(13) 0.20644(14) 0.19237(8) 0.0386(10) Uani 1 1 d . . . N3 N 0.0000 0.13360(18) 0.18065(13) 0.0400(14) Uani 1 2 d S . . C4 C 0.02304(15) 0.05297(19) 0.16967(12) 0.0549(15) Uani 1 1 d . . . H4 H 0.0424 0.0245 0.1650 0.066 Uiso 1 1 calc R . . C5 C 0.03964(19) 0.10092(18) 0.17746(12) 0.0468(14) Uani 1 1 d . . . C6 C 0.08513(19) 0.11532(18) 0.18015(12) 0.0483(14) Uani 1 1 d . . . C7 C 0.09984(17) 0.1669(2) 0.18689(12) 0.0501(14) Uani 1 1 d . . . C8 C 0.14970(19) 0.17997(19) 0.19014(12) 0.0541(15) Uani 1 1 d . . . H8 H 0.1763 0.1583 0.1877 0.065 Uiso 1 1 calc R . . C9 C 0.14977(16) 0.2308(2) 0.19759(12) 0.0551(15) Uani 1 1 d . . . H9 H 0.1769 0.2511 0.2014 0.066 Uiso 1 1 calc R . . C10 C 0.10129(16) 0.2474(2) 0.19853(12) 0.0478(14) Uani 1 1 d . . . C11 C 0.08707(17) 0.29650(18) 0.20528(11) 0.0389(12) Uani 1 1 d . . . C12 C 0.03866(18) 0.3144(2) 0.20703(12) 0.0543(14) Uani 1 1 d . . . C13 C 0.02287(15) 0.36403(19) 0.21475(11) 0.0548(15) Uani 1 1 d . . . H13 H 0.0426 0.3923 0.2192 0.066 Uiso 1 1 calc R . . C14 C 0.12349(16) 0.07802(17) 0.17702(13) 0.0382(13) Uani 1 1 d . . . C15 C 0.1393(3) 0.0608(3) 0.14981(18) 0.131(3) Uani 1 1 d . . . H15 H 0.1279 0.0759 0.1306 0.158 Uiso 1 1 calc R . . C16 C 0.1727(3) 0.0206(3) 0.14670(19) 0.142(4) Uani 1 1 d . . . H16 H 0.1824 0.0110 0.1257 0.170 Uiso 1 1 calc R . . C17 C 0.1895(2) -0.0023(2) 0.17002(18) 0.0626(17) Uani 1 1 d . . . C18 C 0.1777(2) 0.0171(3) 0.2013(2) 0.124(3) Uani 1 1 d . . . H18 H 0.1905 0.0022 0.2202 0.149 Uiso 1 1 calc R . . C19 C 0.1460(2) 0.0597(3) 0.20334(18) 0.117(3) Uani 1 1 d . . . H19 H 0.1407 0.0753 0.2237 0.140 Uiso 1 1 calc R . . O20 O 0.22191(12) -0.03977(12) 0.17054(10) 0.0801(13) Uani 1 1 d . . . H20 H 0.2375 -0.0421 0.1539 0.120 Uiso 1 1 d R . . C21 C 0.12355(17) 0.33521(17) 0.21057(14) 0.0474(14) Uani 1 1 d . . . C22 C 0.1434(3) 0.3463(3) 0.23918(16) 0.157(4) Uani 1 1 d . . . H22 H 0.1339 0.3275 0.2576 0.188 Uiso 1 1 calc R . . C23 C 0.1778(3) 0.3847(3) 0.24300(17) 0.178(5) Uani 1 1 d . . . H23 H 0.1903 0.3912 0.2639 0.214 Uiso 1 1 calc R . . C24 C 0.1923(2) 0.4105(2) 0.21961(16) 0.0634(17) Uani 1 1 d . . . C25 C 0.1759(3) 0.4015(3) 0.1890(2) 0.173(5) Uani 1 1 d . . . H25 H 0.1865 0.4207 0.1710 0.207 Uiso 1 1 calc R . . C26 C 0.1426(3) 0.3626(4) 0.18564(17) 0.193(5) Uani 1 1 d . . . H26 H 0.1325 0.3545 0.1644 0.232 Uiso 1 1 calc R . . O27 O 0.22584(12) 0.44757(12) 0.22310(9) 0.0770(12) Uani 1 1 d . . . H27 H 0.2418 0.4515 0.2068 0.116 Uiso 1 1 d R . . Zn28 Zn 0.0000 0.20964(3) 0.185162(19) 0.0422(3) Uani 1 2 d S . . N29 N 0.0000 0.23462(19) 0.13625(14) 0.0520(16) Uani 1 2 d S . . C30 C 0.03981(19) 0.2442(2) 0.12077(16) 0.0802(19) Uani 1 1 d . . . H30 H 0.0692 0.2384 0.1313 0.096 Uiso 1 1 calc R . . C31 C 0.0398(2) 0.2628(3) 0.08917(16) 0.112(3) Uani 1 1 d . . . H31 H 0.0689 0.2700 0.0787 0.134 Uiso 1 1 calc R . . C32 C 0.0000 0.2702(3) 0.07398(19) 0.063(2) Uani 1 2 d S . . C33 C 0.0000 0.2849(3) 0.03782(17) 0.0517(19) Uani 1 2 d S . . C34 C 0.04138(18) 0.2935(2) 0.02129(13) 0.0779(19) Uani 1 1 d . . . H34 H 0.0708 0.2888 0.0319 0.093 Uiso 1 1 calc R . . C35 C 0.04093(18) 0.3085(2) -0.00984(14) 0.0717(17) Uani 1 1 d . . . H35 H 0.0703 0.3138 -0.0204 0.086 Uiso 1 1 calc R . . N36 N 0.0000 0.31627(18) -0.02676(14) 0.0479(15) Uani 1 2 d S . . N37 N 0.0000 0.3854(2) -0.09240(14) 0.0520(16) Uani 1 2 d S . . N38 N 0.07251(14) 0.30998(18) -0.08562(9) 0.0544(12) Uani 1 1 d . . . N39 N 0.0000 0.2368(2) -0.07758(15) 0.0615(18) Uani 1 2 d S . . C40 C 0.02302(17) 0.1531(2) -0.06705(14) 0.080(2) Uani 1 1 d . . . H40 H 0.0422 0.1240 -0.0638 0.096 Uiso 1 1 calc R . . C41 C 0.0413(2) 0.2046(2) -0.07285(14) 0.0691(17) Uani 1 1 d . . . C42 C 0.0854(2) 0.2212(2) -0.07567(13) 0.0573(15) Uani 1 1 d . . . C43 C 0.1012(2) 0.2692(2) -0.08251(13) 0.0595(16) Uani 1 1 d . . . C44 C 0.15146(19) 0.2845(3) -0.08421(13) 0.0720(18) Uani 1 1 d . . . H44 H 0.1785 0.2637 -0.0814 0.086 Uiso 1 1 calc R . . C45 C 0.15067(18) 0.3362(2) -0.09074(13) 0.0611(16) Uani 1 1 d . . . H45 H 0.1774 0.3571 -0.0948 0.073 Uiso 1 1 calc R . . C46 C 0.1015(2) 0.3522(2) -0.09011(12) 0.0518(14) Uani 1 1 d . . . C47 C 0.0865(2) 0.4016(2) -0.09538(13) 0.0634(16) Uani 1 1 d . . . C48 C 0.03833(19) 0.4164(2) -0.09851(12) 0.0548(15) Uani 1 1 d . . . C49 C 0.02388(15) 0.4696(2) -0.10389(12) 0.0602(16) Uani 1 1 d . . . H49 H 0.0441 0.4979 -0.1068 0.072 Uiso 1 1 calc R . . C50 C 0.1221(2) 0.1820(2) -0.07053(16) 0.0752(18) Uani 1 1 d . . . C51 C 0.1418(2) 0.1597(3) -0.09583(18) 0.111(3) Uani 1 1 d . . . H51 H 0.1308 0.1694 -0.1166 0.133 Uiso 1 1 calc R . . C52 C 0.1798(3) 0.1206(3) -0.0945(2) 0.128(3) Uani 1 1 d . . . H52 H 0.1925 0.1048 -0.1132 0.154 Uiso 1 1 calc R . . C53 C 0.1937(3) 0.1102(3) -0.0656(3) 0.152(4) Uani 1 1 d . . . C54 C 0.1738(4) 0.1380(5) -0.0379(2) 0.250(7) Uani 1 1 d . . . H54 H 0.1882 0.1349 -0.0172 0.300 Uiso 1 1 calc R . . C55 C 0.1364(4) 0.1670(4) -0.0414(2) 0.216(6) Uani 1 1 d . . . H55 H 0.1192 0.1774 -0.0229 0.259 Uiso 1 1 calc R . . O56 O 0.2308(3) 0.0773(3) -0.06162(17) 0.257(4) Uani 1 1 d . . . H56 H 0.2425 0.0811 -0.0432 0.386 Uiso 1 1 calc R . . C57 C 0.12304(19) 0.4415(2) -0.10230(14) 0.0581(15) Uani 1 1 d . . . C58 C 0.1367(3) 0.4722(3) -0.07844(17) 0.144(4) Uani 1 1 d . . . H58 H 0.1226 0.4689 -0.0577 0.173 Uiso 1 1 calc R . . C59 C 0.1689(3) 0.5065(3) -0.0832(2) 0.158(4) Uani 1 1 d . . . H59 H 0.1759 0.5289 -0.0660 0.190 Uiso 1 1 calc R . . C60 C 0.1927(2) 0.5124(2) -0.11055(19) 0.0733(19) Uani 1 1 d . . . C61 C 0.1827(3) 0.4806(3) -0.13263(17) 0.127(3) Uani 1 1 d . . . H61 H 0.2000 0.4828 -0.1522 0.152 Uiso 1 1 calc R . . C62 C 0.1489(2) 0.4432(3) -0.13025(16) 0.133(3) Uani 1 1 d . . . H62 H 0.1438 0.4197 -0.1472 0.160 Uiso 1 1 calc R . . O63 O 0.22780(14) 0.54768(15) -0.11538(10) 0.0889(14) Uani 1 1 d . . . H63 H 0.2405 0.5548 -0.0977 0.133 Uiso 1 1 calc R . . Zn64 Zn 0.0000 0.31361(3) -0.078429(19) 0.0496(3) Uani 1 2 d S . . 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 0.028(3) 0.041(4) 0.053(4) 0.001(3) 0.000 0.000 N2 0.049(3) 0.019(2) 0.048(3) 0.0041(19) -0.009(2) 0.007(2) N3 0.028(3) 0.034(3) 0.059(4) 0.010(3) 0.000 0.000 C4 0.047(3) 0.053(3) 0.065(4) 0.010(3) -0.001(3) 0.011(3) C5 0.050(4) 0.036(4) 0.054(4) -0.001(3) 0.004(3) -0.017(3) C6 0.049(4) 0.029(3) 0.067(4) 0.001(3) -0.001(3) 0.003(3) C7 0.029(3) 0.060(4) 0.061(4) 0.000(3) 0.000(3) 0.005(3) C8 0.063(4) 0.032(4) 0.067(4) 0.005(3) 0.005(3) -0.003(3) C9 0.023(3) 0.062(4) 0.081(4) 0.016(3) 0.002(3) 0.012(3) C10 0.026(3) 0.046(4) 0.071(4) 0.008(3) -0.002(3) -0.004(3) C11 0.035(3) 0.035(3) 0.046(3) 0.001(3) -0.011(2) -0.003(3) C12 0.038(3) 0.069(4) 0.055(4) 0.010(3) 0.000(3) -0.006(3) C13 0.058(4) 0.053(3) 0.053(4) -0.010(3) -0.004(3) 0.002(3) C14 0.027(3) 0.026(3) 0.062(4) 0.006(3) -0.002(3) 0.008(2) C15 0.146(7) 0.156(7) 0.091(6) 0.011(5) 0.020(5) 0.128(6) C16 0.189(9) 0.159(8) 0.077(6) 0.017(5) 0.024(6) 0.123(7) C17 0.055(4) 0.040(4) 0.093(6) 0.006(4) 0.025(4) 0.019(3) C18 0.109(6) 0.124(6) 0.140(8) 0.078(5) 0.035(5) 0.092(5) C19 0.109(6) 0.133(6) 0.109(6) 0.032(5) 0.041(5) 0.101(5) O20 0.054(3) 0.058(2) 0.128(4) 0.005(2) 0.031(2) 0.021(2) C21 0.046(3) 0.036(3) 0.060(4) 0.002(3) -0.015(3) -0.004(3) C22 0.237(10) 0.181(8) 0.052(5) 0.023(5) -0.023(5) -0.167(7) C23 0.256(10) 0.205(8) 0.074(6) 0.049(6) -0.065(6) -0.212(8) C24 0.059(4) 0.049(4) 0.082(5) 0.034(4) -0.005(4) -0.010(3) C25 0.211(10) 0.189(8) 0.118(7) 0.052(6) -0.062(7) -0.188(8) C26 0.191(9) 0.342(13) 0.047(5) 0.056(6) -0.033(5) -0.195(9) O27 0.054(2) 0.059(2) 0.117(4) 0.011(2) -0.006(2) -0.033(2) Zn28 0.0354(5) 0.0429(5) 0.0484(5) 0.0023(4) 0.000 0.000 N29 0.054(4) 0.046(4) 0.057(4) 0.003(3) 0.000 0.000 C30 0.044(4) 0.111(5) 0.085(5) 0.040(4) 0.009(3) 0.003(4) C31 0.046(4) 0.227(8) 0.061(5) 0.049(5) -0.005(4) 0.000(5) C32 0.049(6) 0.090(6) 0.048(6) 0.006(4) 0.000 0.000 C33 0.061(5) 0.064(5) 0.029(4) 0.019(4) 0.000 0.000 C34 0.047(4) 0.146(6) 0.040(4) 0.038(4) -0.008(3) 0.017(4) C35 0.042(4) 0.109(5) 0.064(4) 0.008(4) -0.005(3) -0.022(3) N36 0.053(4) 0.041(4) 0.050(4) -0.005(3) 0.000 0.000 N37 0.032(4) 0.063(4) 0.061(4) 0.011(3) 0.000 0.000 N38 0.053(3) 0.065(3) 0.046(3) -0.003(2) -0.001(2) -0.003(3) N39 0.063(5) 0.051(4) 0.070(5) -0.009(3) 0.000 0.000 C40 0.086(5) 0.040(3) 0.114(5) -0.007(3) 0.001(3) 0.004(3) C41 0.071(5) 0.062(5) 0.074(4) -0.017(3) 0.015(4) -0.013(4) C42 0.048(4) 0.053(4) 0.071(4) 0.001(3) -0.007(3) -0.006(3) C43 0.050(4) 0.037(4) 0.091(5) 0.000(3) -0.003(3) 0.006(3) C44 0.036(4) 0.103(5) 0.077(5) -0.004(4) 0.018(3) -0.008(4) C45 0.038(4) 0.068(4) 0.077(4) 0.000(3) -0.006(3) -0.001(3) C46 0.051(4) 0.037(4) 0.067(4) 0.005(3) 0.004(3) 0.003(3) C47 0.046(4) 0.089(5) 0.055(4) -0.018(3) 0.013(3) -0.014(4) C48 0.049(4) 0.071(4) 0.045(4) 0.018(3) 0.004(3) 0.012(3) C49 0.058(4) 0.074(4) 0.049(3) 0.015(3) -0.006(3) -0.013(3) C50 0.092(5) 0.068(4) 0.066(5) 0.004(4) 0.005(4) 0.036(4) C51 0.095(6) 0.149(7) 0.088(6) -0.015(5) -0.023(4) 0.087(5) C52 0.138(8) 0.117(7) 0.130(8) 0.029(6) -0.010(6) 0.010(6) C53 0.173(9) 0.134(7) 0.150(9) 0.068(7) 0.044(8) 0.127(7) C54 0.265(14) 0.415(18) 0.071(7) 0.014(9) 0.007(8) 0.191(13) C55 0.256(12) 0.274(11) 0.117(8) 0.059(7) 0.026(7) 0.252(10) O56 0.305(9) 0.246(8) 0.220(8) 0.033(6) 0.043(7) 0.236(7) C57 0.052(4) 0.066(4) 0.057(4) -0.004(3) -0.001(3) -0.001(3) C58 0.146(7) 0.180(8) 0.107(6) -0.095(6) 0.070(5) -0.138(6) C59 0.117(7) 0.216(9) 0.142(8) -0.111(7) 0.062(6) -0.106(7) C60 0.052(4) 0.070(5) 0.098(6) -0.004(4) 0.005(4) -0.028(4) C61 0.139(7) 0.196(8) 0.045(4) 0.018(5) 0.002(4) -0.114(6) C62 0.099(6) 0.239(9) 0.062(5) -0.017(5) 0.026(4) -0.118(6) O63 0.056(3) 0.072(3) 0.139(4) -0.015(3) -0.002(3) -0.008(2) Zn64 0.0469(6) 0.0583(6) 0.0436(6) -0.0011(4) 0.000 0.000 _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 C12 1.406(5) . ? N1 C12 1.406(5) 11 ? N1 Zn28 2.042(5) . ? N2 C7 1.326(5) . ? N2 C10 1.385(5) . ? N2 Zn28 2.063(4) . ? N3 C5 1.421(5) 11 ? N3 C5 1.421(5) . ? N3 Zn28 2.021(5) . ? C4 C4 1.302(8) 11 ? C4 C5 1.390(6) . ? C4 H4 0.9500 . ? C5 C6 1.345(6) . ? C6 C7 1.453(6) . ? C6 C14 1.471(6) . ? C7 C8 1.457(6) . ? C8 C9 1.379(6) . ? C8 H8 0.9500 . ? C9 C10 1.439(6) . ? C9 H9 0.9500 . ? C10 C11 1.387(6) . ? C11 C12 1.450(6) . ? C11 C21 1.469(6) . ? C12 C13 1.422(6) . ? C13 C13 1.292(9) 11 ? C13 H13 0.9500 . ? C14 C15 1.297(7) . ? C14 C19 1.353(7) . ? C15 C16 1.425(8) . ? C15 H15 0.9500 . ? C16 C17 1.236(7) . ? C16 H16 0.9500 . ? C17 O20 1.350(6) . ? C17 C18 1.433(8) . ? C18 C19 1.445(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? O20 H20 0.8195 . ? C21 C22 1.344(7) . ? C21 C26 1.373(7) . ? C22 C23 1.416(7) . ? C22 H22 0.9500 . ? C23 C24 1.255(7) . ? C23 H23 0.9500 . ? C24 O27 1.371(6) . ? C24 C25 1.373(8) . ? C25 C26 1.401(8) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? O27 H27 0.8186 . ? Zn28 N2 2.063(4) 11 ? Zn28 N29 2.134(6) . ? N29 C30 1.320(5) . ? N29 C30 1.320(5) 11 ? C30 C31 1.400(8) . ? C30 H30 0.9500 . ? C31 C32 1.303(6) . ? C31 H31 0.9500 . ? C32 C31 1.303(6) 11 ? C32 C33 1.549(9) . ? C33 C34 1.374(6) 11 ? C33 C34 1.374(6) . ? C34 C35 1.351(7) . ? C34 H34 0.9500 . ? C35 N36 1.368(6) . ? C35 H35 0.9500 . ? N36 C35 1.368(6) 11 ? N36 Zn64 2.144(6) . ? N37 C48 1.382(6) 11 ? N37 C48 1.383(6) . ? N37 Zn64 1.985(6) . ? N38 C43 1.355(6) . ? N38 C46 1.398(6) . ? N38 Zn64 2.072(4) . ? N39 C41 1.456(6) 11 ? N39 C41 1.456(6) . ? N39 Zn64 2.034(6) . ? C40 C40 1.301(10) 11 ? C40 C41 1.478(7) . ? C40 H40 0.9500 . ? C41 C42 1.327(7) . ? C42 C43 1.375(7) . ? C42 C50 1.481(7) . ? C43 C44 1.479(7) . ? C44 C45 1.393(7) . ? C44 H44 0.9500 . ? C45 C46 1.453(6) . ? C45 H45 0.9500 . ? C46 C47 1.390(7) . ? C47 C48 1.422(6) . ? C47 C57 1.505(7) . ? C48 C49 1.481(6) . ? C49 C49 1.349(9) 11 ? C49 H49 0.9500 . ? C50 C51 1.328(7) . ? C50 C55 1.334(9) . ? C51 C52 1.490(9) . ? C51 H51 0.9500 . ? C52 C53 1.292(10) . ? C52 H52 0.9500 . ? C53 O56 1.373(8) . ? C53 C54 1.477(11) . ? C54 C55 1.313(10) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? O56 H56 0.8580 . ? C57 C58 1.336(7) . ? C57 C62 1.372(7) . ? C58 C59 1.301(8) . ? C58 H58 0.9500 . ? C59 C60 1.326(8) . ? C59 H59 0.9500 . ? C60 C61 1.275(7) . ? C60 O63 1.378(6) . ? C61 C62 1.377(8) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? O63 H63 0.8400 . ? Zn64 N38 2.072(4) 11 ? 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 C12 N1 C12 102.0(6) . 11 ? C12 N1 Zn28 128.3(3) . . ? C12 N1 Zn28 128.3(3) 11 . ? C7 N2 C10 107.5(4) . . ? C7 N2 Zn28 126.2(3) . . ? C10 N2 Zn28 125.6(3) . . ? C5 N3 C5 104.0(5) 11 . ? C5 N3 Zn28 127.9(3) 11 . ? C5 N3 Zn28 127.9(3) . . ? C4 C4 C5 109.7(3) 11 . ? C4 C4 H4 125.1 11 . ? C5 C4 H4 125.1 . . ? C6 C5 C4 126.9(5) . . ? C6 C5 N3 124.9(4) . . ? C4 C5 N3 108.1(5) . . ? C5 C6 C7 123.7(5) . . ? C5 C6 C14 120.4(4) . . ? C7 C6 C14 115.8(4) . . ? N2 C7 C6 127.3(5) . . ? N2 C7 C8 111.5(5) . . ? C6 C7 C8 121.2(5) . . ? C9 C8 C7 104.7(5) . . ? C9 C8 H8 127.6 . . ? C7 C8 H8 127.6 . . ? C8 C9 C10 107.7(5) . . ? C8 C9 H9 126.2 . . ? C10 C9 H9 126.2 . . ? N2 C10 C11 126.7(4) . . ? N2 C10 C9 108.7(5) . . ? C11 C10 C9 124.6(5) . . ? C10 C11 C12 126.1(4) . . ? C10 C11 C21 118.6(4) . . ? C12 C11 C21 115.2(4) . . ? N1 C12 C13 110.7(5) . . ? N1 C12 C11 121.6(5) . . ? C13 C12 C11 127.5(5) . . ? C13 C13 C12 108.3(3) 11 . ? C13 C13 H13 125.9 11 . ? C12 C13 H13 125.9 . . ? C15 C14 C19 114.5(5) . . ? C15 C14 C6 124.5(5) . . ? C19 C14 C6 120.9(5) . . ? C14 C15 C16 124.7(6) . . ? C14 C15 H15 117.7 . . ? C16 C15 H15 117.7 . . ? C17 C16 C15 123.3(7) . . ? C17 C16 H16 118.4 . . ? C15 C16 H16 118.4 . . ? C16 C17 O20 129.3(7) . . ? C16 C17 C18 116.4(6) . . ? O20 C17 C18 113.9(6) . . ? C17 C18 C19 118.4(6) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C14 C19 C18 121.6(7) . . ? C14 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C17 O20 H20 114.0 . . ? C22 C21 C26 112.7(5) . . ? C22 C21 C11 125.2(5) . . ? C26 C21 C11 122.0(5) . . ? C21 C22 C23 122.8(6) . . ? C21 C22 H22 118.6 . . ? C23 C22 H22 118.6 . . ? C24 C23 C22 121.9(6) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 O27 122.2(6) . . ? C23 C24 C25 120.7(6) . . ? O27 C24 C25 117.1(5) . . ? C24 C25 C26 116.4(7) . . ? C24 C25 H25 121.8 . . ? C26 C25 H25 121.8 . . ? C21 C26 C25 125.2(7) . . ? C21 C26 H26 117.4 . . ? C25 C26 H26 117.4 . . ? C24 O27 H27 112.6 . . ? N3 Zn28 N1 164.1(2) . . ? N3 Zn28 N2 88.42(11) . 11 ? N1 Zn28 N2 89.20(11) . 11 ? N3 Zn28 N2 88.42(11) . . ? N1 Zn28 N2 89.20(11) . . ? N2 Zn28 N2 162.68(19) 11 . ? N3 Zn28 N29 102.7(2) . . ? N1 Zn28 N29 93.1(2) . . ? N2 Zn28 N29 98.65(10) 11 . ? N2 Zn28 N29 98.66(10) . . ? C30 N29 C30 116.9(7) . 11 ? C30 N29 Zn28 121.5(4) . . ? C30 N29 Zn28 121.5(4) 11 . ? N29 C30 C31 121.5(6) . . ? N29 C30 H30 119.2 . . ? C31 C30 H30 119.3 . . ? C32 C31 C30 120.4(6) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C31 119.1(8) . 11 ? C31 C32 C33 120.4(4) . . ? C31 C32 C33 120.4(4) 11 . ? C34 C33 C34 116.6(6) 11 . ? C34 C33 C32 121.6(3) 11 . ? C34 C33 C32 121.6(3) . . ? C35 C34 C33 121.2(5) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 N36 122.9(5) . . ? C34 C35 H35 118.6 . . ? N36 C35 H35 118.6 . . ? C35 N36 C35 115.3(6) 11 . ? C35 N36 Zn64 120.5(3) 11 . ? C35 N36 Zn64 120.5(3) . . ? C48 N37 C48 103.1(6) 11 . ? C48 N37 Zn64 128.4(3) 11 . ? C48 N37 Zn64 128.4(3) . . ? C43 N38 C46 107.4(5) . . ? C43 N38 Zn64 127.9(4) . . ? C46 N38 Zn64 124.1(4) . . ? C41 N39 C41 106.4(6) 11 . ? C41 N39 Zn64 125.8(3) 11 . ? C41 N39 Zn64 125.8(3) . . ? C40 C40 C41 110.4(3) 11 . ? C40 C40 H40 124.8 11 . ? C41 C40 H40 124.8 . . ? C42 C41 N39 123.2(5) . . ? C42 C41 C40 130.3(6) . . ? N39 C41 C40 106.3(5) . . ? C41 C42 C43 128.9(6) . . ? C41 C42 C50 114.4(5) . . ? C43 C42 C50 116.8(5) . . ? N38 C43 C42 124.1(5) . . ? N38 C43 C44 110.5(5) . . ? C42 C43 C44 125.0(6) . . ? C45 C44 C43 105.2(5) . . ? C45 C44 H44 127.4 . . ? C43 C44 H44 127.4 . . ? C44 C45 C46 107.3(5) . . ? C44 C45 H45 126.3 . . ? C46 C45 H45 126.3 . . ? C47 C46 N38 126.4(5) . . ? C47 C46 C45 124.2(5) . . ? N38 C46 C45 109.2(5) . . ? C46 C47 C48 124.4(5) . . ? C46 C47 C57 118.7(5) . . ? C48 C47 C57 116.4(5) . . ? N37 C48 C47 124.7(5) . . ? N37 C48 C49 112.1(5) . . ? C47 C48 C49 122.7(5) . . ? C49 C49 C48 106.0(3) 11 . ? C49 C49 H49 127.0 11 . ? C48 C49 H49 127.0 . . ? C51 C50 C55 117.0(6) . . ? C51 C50 C42 119.5(6) . . ? C55 C50 C42 123.5(6) . . ? C50 C51 C52 125.7(7) . . ? C50 C51 H51 117.2 . . ? C52 C51 H51 117.2 . . ? C53 C52 C51 113.6(8) . . ? C53 C52 H52 123.2 . . ? C51 C52 H52 123.2 . . ? C52 C53 O56 118.6(10) . . ? C52 C53 C54 120.1(8) . . ? O56 C53 C54 120.8(10) . . ? C55 C54 C53 120.6(9) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.8 . . ? C54 C55 C50 121.4(8) . . ? C54 C55 H55 119.3 . . ? C50 C55 H55 119.3 . . ? C53 O56 H56 111.8 . . ? C58 C57 C62 116.9(6) . . ? C58 C57 C47 118.9(5) . . ? C62 C57 C47 123.4(5) . . ? C59 C58 C57 120.8(7) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C58 C59 C60 124.5(7) . . ? C58 C59 H59 117.7 . . ? C60 C59 H59 117.7 . . ? C61 C60 C59 115.1(6) . . ? C61 C60 O63 120.1(7) . . ? C59 C60 O63 124.7(7) . . ? C60 C61 C62 125.0(7) . . ? C60 C61 H61 117.5 . . ? C62 C61 H61 117.5 . . ? C57 C62 C61 117.0(7) . . ? C57 C62 H62 121.5 . . ? C61 C62 H62 121.5 . . ? C60 O63 H63 109.4 . . ? N37 Zn64 N39 164.0(2) . . ? N37 Zn64 N38 90.14(14) . 11 ? N39 Zn64 N38 87.48(14) . 11 ? N37 Zn64 N38 90.13(14) . . ? N39 Zn64 N38 87.49(14) . . ? N38 Zn64 N38 162.6(2) 11 . ? N37 Zn64 N36 105.1(2) . . ? N39 Zn64 N36 90.9(2) . . ? N38 Zn64 N36 98.36(11) 11 . ? N38 Zn64 N36 98.36(11) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.72 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.370 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.076 #===============END====================================================