Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author ; Priv. Doz. Dr. Katja Heinze Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Germany ; _publ_contact_author_phone '049 6221 54-8587' _publ_contact_author_fax '049 6221 54-5707' _publ_contact_author_email katja.heinze@urz.uni-heidelberg.de _publ_requested_coeditor_name 'Anja Reinhart' #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Structural and Photophysical Studies of trans-AB2C substituted Porphyrin Ligands and their Zinc and Copper Complexes ; _publ_section_abstract ; Structural and Photophysical Studies of trans-AB2C substituted Porphyrin Ligands and their Zinc and Copper Complexes ; _publ_author_address ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; _publ_contact_author_name 'Priv. Doz. Dr. Katja Heinze' loop_ _publ_author_name K.Heinze A.Reinhart #============================================================================== data_ar92 _database_code_depnum_ccdc_archive 'CCDC 659519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5-(4-nitrophenyl)-15-(carbomethoxyphenyl)-10,20-bis(phenyl)porphyrin ; _chemical_name_common ;5-(4-nitrophenyl)-15-(carbomethoxyphenyl)-10,20- bis(phenyl)porphyrin ; _chemical_melting_point 410 _chemical_formula_moiety 'C46 H31 N5 O4' _chemical_formula_sum 'C46 H31 N5 O4' _chemical_formula_weight 717.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 6.5450(9) _cell_length_b 12.5885(18) _cell_length_c 23.214(3) _cell_angle_alpha 96.636(3) _cell_angle_beta 91.808(3) _cell_angle_gamma 102.738(3) _cell_volume 1849.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.084 _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 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart1000' _diffrn_measurement_method 'O-Scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44414 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8483 _reflns_number_gt 5109 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0880P)^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 8483 _refine_ls_number_parameters 503 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1417 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 O1 O 1.7335(2) 0.71855(12) 0.05515(6) 0.0252(3) Uani 1 1 d . . . O2 O 1.5061(2) 0.62946(11) -0.01847(6) 0.0207(3) Uani 1 1 d . . . O3 O -0.6404(2) 0.34006(13) 0.54295(6) 0.0324(4) Uani 1 1 d . . . O4 O -0.8504(2) 0.25603(13) 0.46968(7) 0.0347(4) Uani 1 1 d . . . N1 N 0.6956(2) 0.61977(12) 0.26726(6) 0.0136(3) Uani 1 1 d . . . N2 N 0.2950(2) 0.56939(12) 0.32262(6) 0.0129(3) Uani 1 1 d . . . N3 N 0.1903(2) 0.34445(12) 0.26516(6) 0.0140(3) Uani 1 1 d . . . N4 N 0.5919(2) 0.39493(12) 0.20973(6) 0.0137(3) Uani 1 1 d . . . N5 N -0.6799(3) 0.31054(14) 0.49085(8) 0.0217(4) Uani 1 1 d . . . C1 C 0.8573(3) 0.62665(15) 0.23057(8) 0.0138(4) Uani 1 1 d . . . C2 C 0.9672(3) 0.73932(15) 0.23646(8) 0.0168(4) Uani 1 1 d . . . H2 H 1.0870 0.7690 0.2165 0.0193(19) Uiso 1 1 calc R . . C3 C 0.8689(3) 0.79643(15) 0.27596(8) 0.0171(4) Uani 1 1 d . . . H3 H 0.9095 0.8730 0.2886 0.0193(19) Uiso 1 1 calc R . . C4 C 0.6953(3) 0.72211(14) 0.29511(8) 0.0146(4) Uani 1 1 d . . . C5 C 0.5449(3) 0.74990(15) 0.33205(8) 0.0147(4) Uani 1 1 d . . . C6 C 0.3584(3) 0.67791(15) 0.34410(8) 0.0140(4) Uani 1 1 d . . . C7 C 0.2067(3) 0.71129(15) 0.38246(8) 0.0173(4) Uani 1 1 d . . . H7 H 0.2157 0.7824 0.4026 0.0193(19) Uiso 1 1 calc R . . C8 C 0.0511(3) 0.62188(15) 0.38386(8) 0.0159(4) Uani 1 1 d . . . H8 H -0.0722 0.6177 0.4048 0.0193(19) Uiso 1 1 calc R . . C9 C 0.1084(3) 0.53297(15) 0.34704(8) 0.0138(4) Uani 1 1 d . . . C10 C -0.0137(3) 0.42474(15) 0.33942(8) 0.0141(4) Uani 1 1 d . . . C11 C 0.0277(3) 0.33790(15) 0.30144(8) 0.0133(4) Uani 1 1 d . . . C12 C -0.0783(3) 0.22470(15) 0.29722(8) 0.0167(4) Uani 1 1 d . . . H12 H -0.1976 0.1954 0.3174 0.0193(19) Uiso 1 1 calc R . . C13 C 0.0222(3) 0.16667(15) 0.25913(8) 0.0175(4) Uani 1 1 d . . . H13 H -0.0151 0.0896 0.2479 0.0193(19) Uiso 1 1 calc R . . C14 C 0.1940(3) 0.24180(15) 0.23895(8) 0.0146(4) Uani 1 1 d . . . C15 C 0.3452(3) 0.21329(14) 0.20211(8) 0.0139(4) Uani 1 1 d . . . C16 C 0.5303(3) 0.28546(14) 0.18895(8) 0.0136(4) Uani 1 1 d . . . C17 C 0.6793(3) 0.25349(15) 0.14925(8) 0.0168(4) Uani 1 1 d . . . H17 H 0.6716 0.1823 0.1293 0.0193(19) Uiso 1 1 calc R . . C18 C 0.8300(3) 0.34372(15) 0.14610(8) 0.0167(4) Uani 1 1 d . . . H18 H 0.9497 0.3488 0.1236 0.0193(19) Uiso 1 1 calc R . . C19 C 0.7747(3) 0.43217(15) 0.18376(8) 0.0137(4) Uani 1 1 d . . . C20 C 0.8960(3) 0.54085(15) 0.19149(8) 0.0132(4) Uani 1 1 d . . . C21 C 1.0702(3) 0.56915(14) 0.15212(8) 0.0129(4) Uani 1 1 d . . . C22 C 1.0235(3) 0.56027(14) 0.09231(8) 0.0147(4) Uani 1 1 d . . . H22 H 0.8825 0.5339 0.0773 0.0179(19) Uiso 1 1 calc R . . C23 C 1.1813(3) 0.58961(14) 0.05469(8) 0.0156(4) Uani 1 1 d . . . H23 H 1.1478 0.5831 0.0141 0.0179(19) Uiso 1 1 calc R . . C24 C 1.3889(3) 0.62870(14) 0.07640(8) 0.0135(4) Uani 1 1 d . . . C25 C 1.4367(3) 0.63782(15) 0.13583(8) 0.0153(4) Uani 1 1 d . . . H25 H 1.5778 0.6646 0.1508 0.0179(19) Uiso 1 1 calc R . . C26 C 1.2788(3) 0.60792(15) 0.17344(8) 0.0151(4) Uani 1 1 d . . . H26 H 1.3129 0.6139 0.2139 0.0179(19) Uiso 1 1 calc R . . C27 C -0.1914(3) 0.39756(14) 0.37783(8) 0.0140(4) Uani 1 1 d . . . C28 C -0.3968(3) 0.35392(15) 0.35554(8) 0.0173(4) Uani 1 1 d . . . H28 H -0.4266 0.3438 0.3147 0.0179(19) Uiso 1 1 calc R . . C29 C -0.5585(3) 0.32504(16) 0.39189(8) 0.0181(4) Uani 1 1 d . . . H29 H -0.6980 0.2942 0.3765 0.0179(19) Uiso 1 1 calc R . . C30 C -0.5109(3) 0.34237(15) 0.45140(8) 0.0160(4) Uani 1 1 d . . . C31 C -0.3105(3) 0.38642(15) 0.47527(8) 0.0173(4) Uani 1 1 d . . . H31 H -0.2827 0.3982 0.5162 0.0179(19) Uiso 1 1 calc R . . C32 C -0.1510(3) 0.41307(14) 0.43829(8) 0.0155(4) Uani 1 1 d . . . H32 H -0.0116 0.4424 0.4541 0.0179(19) Uiso 1 1 calc R . . C33 C 0.5869(3) 0.86623(15) 0.36018(8) 0.0170(4) Uani 1 1 d . . . C34 C 0.4594(3) 0.93548(16) 0.34648(9) 0.0233(5) Uani 1 1 d . . . H34 H 0.3467 0.9095 0.3179 0.036(2) Uiso 1 1 calc R . . C35 C 0.4950(3) 1.04244(17) 0.37411(10) 0.0304(5) Uani 1 1 d . . . H35 H 0.4051 1.0887 0.3651 0.036(2) Uiso 1 1 calc R . . C36 C 0.6620(4) 1.08154(17) 0.41493(10) 0.0306(5) Uani 1 1 d . . . H36 H 0.6867 1.1547 0.4338 0.036(2) Uiso 1 1 calc R . . C37 C 0.7922(4) 1.01397(17) 0.42812(10) 0.0317(5) Uani 1 1 d . . . H37 H 0.9076 1.0410 0.4557 0.036(2) Uiso 1 1 calc R . . C38 C 0.7546(3) 0.90634(16) 0.40103(9) 0.0241(5) Uani 1 1 d . . . H38 H 0.8440 0.8600 0.4105 0.036(2) Uiso 1 1 calc R . . C39 C 0.3025(3) 0.09702(15) 0.17482(8) 0.0168(4) Uani 1 1 d . . . C40 C 0.1261(3) 0.05430(16) 0.13690(9) 0.0245(5) Uani 1 1 d . . . H40 H 0.0325 0.0996 0.1292 0.036(2) Uiso 1 1 calc R . . C41 C 0.0855(4) -0.05313(18) 0.11044(10) 0.0323(5) Uani 1 1 d . . . H41 H -0.0352 -0.0813 0.0848 0.036(2) Uiso 1 1 calc R . . C42 C 0.2217(4) -0.11932(17) 0.12149(10) 0.0326(6) Uani 1 1 d . . . H42 H 0.1942 -0.1931 0.1034 0.036(2) Uiso 1 1 calc R . . C43 C 0.3975(4) -0.07854(17) 0.15879(10) 0.0318(5) Uani 1 1 d . . . H43 H 0.4911 -0.1241 0.1660 0.036(2) Uiso 1 1 calc R . . C44 C 0.4375(3) 0.02886(16) 0.18579(9) 0.0234(5) Uani 1 1 d . . . H44 H 0.5572 0.0561 0.2119 0.036(2) Uiso 1 1 calc R . . C45 C 1.5618(3) 0.66478(15) 0.03808(8) 0.0159(4) Uani 1 1 d . . . C46 C 1.6665(3) 0.66326(17) -0.05831(9) 0.0254(5) Uani 1 1 d . . . H46A H 1.6896 0.7426 -0.0593 0.031(3) Uiso 1 1 calc R . . H46B H 1.6211 0.6247 -0.0973 0.031(3) Uiso 1 1 calc R . . H46C H 1.7974 0.6453 -0.0453 0.031(3) Uiso 1 1 calc R . . H1 H 0.5991 0.5588 0.2729 0.042(7) Uiso 1 1 d R . . H4 H 0.2760 0.4102 0.2631 0.044(7) Uiso 1 1 d 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 O1 0.0175(7) 0.0311(8) 0.0239(8) 0.0046(6) 0.0049(6) -0.0023(6) O2 0.0213(7) 0.0254(8) 0.0153(7) 0.0039(6) 0.0073(6) 0.0036(6) O3 0.0350(9) 0.0454(10) 0.0214(8) 0.0097(7) 0.0144(7) 0.0143(8) O4 0.0170(8) 0.0446(10) 0.0420(10) 0.0148(8) 0.0095(7) -0.0004(7) N1 0.0142(8) 0.0121(8) 0.0137(8) 0.0005(6) 0.0029(6) 0.0015(6) N2 0.0125(8) 0.0135(8) 0.0125(7) 0.0022(6) 0.0018(6) 0.0017(6) N3 0.0142(8) 0.0123(8) 0.0146(8) 0.0006(6) 0.0018(6) 0.0018(6) N4 0.0137(8) 0.0106(8) 0.0149(8) 0.0004(6) 0.0018(6) -0.0005(6) N5 0.0196(9) 0.0217(9) 0.0285(10) 0.0104(7) 0.0103(7) 0.0098(7) C1 0.0134(9) 0.0145(9) 0.0131(9) 0.0027(7) 0.0015(7) 0.0015(7) C2 0.0145(9) 0.0148(10) 0.0192(10) 0.0018(7) 0.0034(8) -0.0007(8) C3 0.0167(10) 0.0140(9) 0.0187(10) 0.0003(7) 0.0016(8) 0.0005(8) C4 0.0153(9) 0.0122(9) 0.0151(9) 0.0010(7) -0.0006(7) 0.0010(7) C5 0.0155(9) 0.0140(9) 0.0148(9) 0.0020(7) 0.0015(7) 0.0037(7) C6 0.0167(10) 0.0135(9) 0.0124(9) 0.0023(7) 0.0023(7) 0.0045(7) C7 0.0219(10) 0.0143(9) 0.0171(9) 0.0022(7) 0.0064(8) 0.0066(8) C8 0.0175(10) 0.0148(9) 0.0171(9) 0.0038(7) 0.0070(8) 0.0055(8) C9 0.0144(9) 0.0150(9) 0.0128(9) 0.0024(7) 0.0019(7) 0.0045(7) C10 0.0130(9) 0.0167(10) 0.0134(9) 0.0044(7) 0.0016(7) 0.0039(7) C11 0.0102(9) 0.0156(9) 0.0135(9) 0.0020(7) 0.0013(7) 0.0017(7) C12 0.0131(9) 0.0173(10) 0.0185(10) 0.0028(8) 0.0032(7) 0.0003(8) C13 0.0156(10) 0.0143(9) 0.0202(10) -0.0006(7) 0.0036(8) -0.0009(8) C14 0.0134(9) 0.0147(9) 0.0148(9) 0.0012(7) 0.0006(7) 0.0012(7) C15 0.0139(9) 0.0130(9) 0.0144(9) 0.0019(7) 0.0011(7) 0.0024(7) C16 0.0135(9) 0.0135(9) 0.0135(9) 0.0018(7) 0.0023(7) 0.0023(7) C17 0.0182(10) 0.0130(9) 0.0195(10) -0.0001(7) 0.0052(8) 0.0046(8) C18 0.0174(10) 0.0164(10) 0.0173(10) 0.0018(7) 0.0072(8) 0.0051(8) C19 0.0143(9) 0.0157(9) 0.0120(9) 0.0020(7) 0.0021(7) 0.0047(7) C20 0.0109(9) 0.0166(9) 0.0125(9) 0.0020(7) 0.0022(7) 0.0033(7) C21 0.0150(9) 0.0103(9) 0.0138(9) 0.0021(7) 0.0037(7) 0.0032(7) C22 0.0124(9) 0.0122(9) 0.0177(9) -0.0014(7) -0.0001(7) 0.0008(7) C23 0.0189(10) 0.0135(9) 0.0131(9) -0.0002(7) 0.0007(7) 0.0017(8) C24 0.0140(9) 0.0107(9) 0.0167(9) 0.0022(7) 0.0040(7) 0.0038(7) C25 0.0126(9) 0.0137(9) 0.0190(10) 0.0018(7) 0.0009(7) 0.0018(7) C26 0.0144(9) 0.0165(10) 0.0137(9) 0.0024(7) -0.0001(7) 0.0022(7) C27 0.0147(9) 0.0118(9) 0.0162(9) 0.0021(7) 0.0045(7) 0.0038(7) C28 0.0146(10) 0.0211(10) 0.0164(9) 0.0030(8) 0.0013(7) 0.0038(8) C29 0.0116(9) 0.0223(10) 0.0212(10) 0.0052(8) 0.0008(8) 0.0045(8) C30 0.0150(9) 0.0147(9) 0.0209(10) 0.0060(8) 0.0080(8) 0.0056(8) C31 0.0229(10) 0.0140(9) 0.0151(9) 0.0008(7) 0.0039(8) 0.0045(8) C32 0.0156(10) 0.0123(9) 0.0171(9) 0.0013(7) 0.0014(7) -0.0002(7) C33 0.0200(10) 0.0133(9) 0.0170(9) 0.0017(7) 0.0076(8) 0.0016(8) C34 0.0192(10) 0.0159(10) 0.0343(12) 0.0041(9) 0.0049(9) 0.0024(8) C35 0.0276(12) 0.0153(11) 0.0503(15) 0.0066(10) 0.0096(11) 0.0074(9) C36 0.0400(14) 0.0125(10) 0.0369(13) -0.0040(9) 0.0119(11) 0.0032(9) C37 0.0416(14) 0.0202(11) 0.0281(12) -0.0053(9) -0.0015(10) 0.0005(10) C38 0.0285(12) 0.0161(10) 0.0256(11) -0.0020(8) 0.0003(9) 0.0032(9) C39 0.0168(10) 0.0128(9) 0.0193(10) 0.0004(7) 0.0072(8) -0.0001(7) C40 0.0255(11) 0.0182(10) 0.0266(11) -0.0029(8) 0.0016(9) 0.0011(9) C41 0.0334(13) 0.0254(12) 0.0313(12) -0.0063(9) 0.0034(10) -0.0030(10) C42 0.0439(14) 0.0114(10) 0.0369(13) -0.0056(9) 0.0161(11) -0.0033(10) C43 0.0357(13) 0.0147(11) 0.0465(14) 0.0035(10) 0.0133(11) 0.0076(10) C44 0.0227(11) 0.0146(10) 0.0320(12) 0.0026(8) 0.0061(9) 0.0017(8) C45 0.0163(10) 0.0129(9) 0.0191(10) 0.0034(7) 0.0044(8) 0.0036(8) C46 0.0262(12) 0.0321(12) 0.0219(11) 0.0119(9) 0.0115(9) 0.0091(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C45 1.205(2) . ? O2 C45 1.348(2) . ? O2 C46 1.447(2) . ? O3 N5 1.225(2) . ? O4 N5 1.228(2) . ? N1 C4 1.373(2) . ? N1 C1 1.374(2) . ? N1 H1 0.9050 . ? N2 C6 1.366(2) . ? N2 C9 1.371(2) . ? N3 C14 1.369(2) . ? N3 C11 1.372(2) . ? N3 H4 0.8987 . ? N4 C19 1.370(2) . ? N4 C16 1.372(2) . ? N5 C30 1.475(2) . ? C1 C20 1.401(2) . ? C1 C2 1.431(2) . ? C2 C3 1.364(3) . ? C2 H2 0.9500 . ? C3 C4 1.422(2) . ? C3 H3 0.9500 . ? C4 C5 1.401(2) . ? C5 C6 1.408(2) . ? C5 C33 1.495(2) . ? C6 C7 1.452(2) . ? C7 C8 1.346(3) . ? C7 H7 0.9500 . ? C8 C9 1.452(2) . ? C8 H8 0.9500 . ? C9 C10 1.408(2) . ? C10 C11 1.403(2) . ? C10 C27 1.492(2) . ? C11 C12 1.431(2) . ? C12 C13 1.359(3) . ? C12 H12 0.9500 . ? C13 C14 1.430(2) . ? C13 H13 0.9500 . ? C14 C15 1.407(3) . ? C15 C16 1.410(2) . ? C15 C39 1.489(2) . ? C16 C17 1.451(2) . ? C17 C18 1.341(3) . ? C17 H17 0.9500 . ? C18 C19 1.452(2) . ? C18 H18 0.9500 . ? C19 C20 1.411(2) . ? C20 C21 1.492(2) . ? C21 C26 1.398(2) . ? C21 C22 1.398(2) . ? C22 C23 1.388(2) . ? C22 H22 0.9500 . ? C23 C24 1.395(2) . ? C23 H23 0.9500 . ? C24 C25 1.391(3) . ? C24 C45 1.486(3) . ? C25 C26 1.390(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.393(3) . ? C27 C32 1.403(3) . ? C28 C29 1.386(3) . ? C28 H28 0.9500 . ? C29 C30 1.388(3) . ? C29 H29 0.9500 . ? C30 C31 1.377(3) . ? C31 C32 1.381(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.388(3) . ? C33 C38 1.392(3) . ? C34 C35 1.390(3) . ? C34 H34 0.9500 . ? C35 C36 1.387(3) . ? C35 H35 0.9500 . ? C36 C37 1.381(3) . ? C36 H36 0.9500 . ? C37 C38 1.392(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.397(3) . ? C39 C44 1.397(3) . ? C40 C41 1.384(3) . ? C40 H40 0.9500 . ? C41 C42 1.384(3) . ? C41 H41 0.9500 . ? C42 C43 1.382(3) . ? C42 H42 0.9500 . ? C43 C44 1.388(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? 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 C45 O2 C46 115.17(15) . . ? C4 N1 C1 109.93(15) . . ? C4 N1 H1 122.8 . . ? C1 N1 H1 127.3 . . ? C6 N2 C9 105.22(15) . . ? C14 N3 C11 109.78(15) . . ? C14 N3 H4 131.1 . . ? C11 N3 H4 119.1 . . ? C19 N4 C16 105.17(15) . . ? O3 N5 O4 124.14(17) . . ? O3 N5 C30 117.58(17) . . ? O4 N5 C30 118.28(17) . . ? N1 C1 C20 126.12(16) . . ? N1 C1 C2 107.05(15) . . ? C20 C1 C2 126.65(17) . . ? C3 C2 C1 107.57(16) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? C2 C3 C4 108.57(17) . . ? C2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? N1 C4 C5 126.82(17) . . ? N1 C4 C3 106.86(16) . . ? C5 C4 C3 126.18(17) . . ? C4 C5 C6 125.39(17) . . ? C4 C5 C33 116.63(16) . . ? C6 C5 C33 117.97(16) . . ? N2 C6 C5 126.00(16) . . ? N2 C6 C7 110.85(15) . . ? C5 C6 C7 123.14(16) . . ? C8 C7 C6 106.64(16) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? C7 C8 C9 106.53(16) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C10 126.21(16) . . ? N2 C9 C8 110.74(16) . . ? C10 C9 C8 123.04(16) . . ? C11 C10 C9 125.11(17) . . ? C11 C10 C27 116.97(16) . . ? C9 C10 C27 117.74(16) . . ? N3 C11 C10 125.98(16) . . ? N3 C11 C12 107.15(15) . . ? C10 C11 C12 126.63(17) . . ? C13 C12 C11 107.81(16) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 108.13(17) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? N3 C14 C15 126.99(17) . . ? N3 C14 C13 107.12(15) . . ? C15 C14 C13 125.76(17) . . ? C14 C15 C16 125.47(16) . . ? C14 C15 C39 116.33(16) . . ? C16 C15 C39 118.20(16) . . ? N4 C16 C15 125.66(16) . . ? N4 C16 C17 110.58(15) . . ? C15 C16 C17 123.73(16) . . ? C18 C17 C16 106.85(16) . . ? C18 C17 H17 126.6 . . ? C16 C17 H17 126.6 . . ? C17 C18 C19 106.68(16) . . ? C17 C18 H18 126.7 . . ? C19 C18 H18 126.7 . . ? N4 C19 C20 125.92(16) . . ? N4 C19 C18 110.73(16) . . ? C20 C19 C18 123.35(16) . . ? C1 C20 C19 125.23(16) . . ? C1 C20 C21 116.98(16) . . ? C19 C20 C21 117.64(15) . . ? C26 C21 C22 118.83(16) . . ? C26 C21 C20 121.88(16) . . ? C22 C21 C20 119.25(16) . . ? C23 C22 C21 120.69(17) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.08(17) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 119.62(16) . . ? C25 C24 C45 118.36(16) . . ? C23 C24 C45 121.99(17) . . ? C26 C25 C24 120.26(17) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C21 120.52(17) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 118.57(16) . . ? C28 C27 C10 122.05(16) . . ? C32 C27 C10 119.36(16) . . ? C29 C28 C27 121.18(17) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 118.13(17) . . ? C28 C29 H29 120.9 . . ? C30 C29 H29 120.9 . . ? C31 C30 C29 122.56(17) . . ? C31 C30 N5 118.39(17) . . ? C29 C30 N5 119.04(17) . . ? C30 C31 C32 118.43(17) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? C31 C32 C27 121.12(17) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? C34 C33 C38 118.99(18) . . ? C34 C33 C5 120.83(18) . . ? C38 C33 C5 120.18(17) . . ? C33 C34 C35 120.6(2) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 120.0(2) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 119.90(19) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 120.1(2) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 120.4(2) . . ? C37 C38 H38 119.8 . . ? C33 C38 H38 119.8 . . ? C40 C39 C44 118.61(18) . . ? C40 C39 C15 120.10(17) . . ? C44 C39 C15 121.28(17) . . ? C41 C40 C39 120.9(2) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C42 C41 C40 119.7(2) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C43 C42 C41 120.3(2) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.1(2) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 120.4(2) . . ? C43 C44 H44 119.8 . . ? C39 C44 H44 119.8 . . ? O1 C45 O2 123.29(17) . . ? O1 C45 C24 124.39(18) . . ? O2 C45 C24 112.32(16) . . ? O2 C46 H46A 109.5 . . ? O2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C20 -174.23(17) . . . . ? C4 N1 C1 C2 1.1(2) . . . . ? N1 C1 C2 C3 -0.2(2) . . . . ? C20 C1 C2 C3 175.06(18) . . . . ? C1 C2 C3 C4 -0.7(2) . . . . ? C1 N1 C4 C5 174.28(17) . . . . ? C1 N1 C4 C3 -1.5(2) . . . . ? C2 C3 C4 N1 1.3(2) . . . . ? C2 C3 C4 C5 -174.48(18) . . . . ? N1 C4 C5 C6 -4.5(3) . . . . ? C3 C4 C5 C6 170.54(18) . . . . ? N1 C4 C5 C33 176.22(17) . . . . ? C3 C4 C5 C33 -8.8(3) . . . . ? C9 N2 C6 C5 178.77(17) . . . . ? C9 N2 C6 C7 -0.8(2) . . . . ? C4 C5 C6 N2 1.0(3) . . . . ? C33 C5 C6 N2 -179.69(17) . . . . ? C4 C5 C6 C7 -179.50(18) . . . . ? C33 C5 C6 C7 -0.2(3) . . . . ? N2 C6 C7 C8 -0.1(2) . . . . ? C5 C6 C7 C8 -179.63(17) . . . . ? C6 C7 C8 C9 0.9(2) . . . . ? C6 N2 C9 C10 -177.65(17) . . . . ? C6 N2 C9 C8 1.3(2) . . . . ? C7 C8 C9 N2 -1.4(2) . . . . ? C7 C8 C9 C10 177.61(17) . . . . ? N2 C9 C10 C11 -5.6(3) . . . . ? C8 C9 C10 C11 175.52(17) . . . . ? N2 C9 C10 C27 169.36(17) . . . . ? C8 C9 C10 C27 -9.5(3) . . . . ? C14 N3 C11 C10 173.90(17) . . . . ? C14 N3 C11 C12 -0.7(2) . . . . ? C9 C10 C11 N3 -1.1(3) . . . . ? C27 C10 C11 N3 -176.13(16) . . . . ? C9 C10 C11 C12 172.46(17) . . . . ? C27 C10 C11 C12 -2.6(3) . . . . ? N3 C11 C12 C13 0.2(2) . . . . ? C10 C11 C12 C13 -174.39(18) . . . . ? C11 C12 C13 C14 0.4(2) . . . . ? C11 N3 C14 C15 -175.13(17) . . . . ? C11 N3 C14 C13 0.9(2) . . . . ? C12 C13 C14 N3 -0.8(2) . . . . ? C12 C13 C14 C15 175.31(18) . . . . ? N3 C14 C15 C16 5.0(3) . . . . ? C13 C14 C15 C16 -170.43(18) . . . . ? N3 C14 C15 C39 -174.55(17) . . . . ? C13 C14 C15 C39 10.1(3) . . . . ? C19 N4 C16 C15 -177.61(17) . . . . ? C19 N4 C16 C17 0.4(2) . . . . ? C14 C15 C16 N4 -0.3(3) . . . . ? C39 C15 C16 N4 179.20(17) . . . . ? C14 C15 C16 C17 -178.02(18) . . . . ? C39 C15 C16 C17 1.5(3) . . . . ? N4 C16 C17 C18 -0.1(2) . . . . ? C15 C16 C17 C18 177.88(18) . . . . ? C16 C17 C18 C19 -0.1(2) . . . . ? C16 N4 C19 C20 179.43(17) . . . . ? C16 N4 C19 C18 -0.5(2) . . . . ? C17 C18 C19 N4 0.4(2) . . . . ? C17 C18 C19 C20 -179.51(17) . . . . ? N1 C1 C20 C19 -0.5(3) . . . . ? C2 C1 C20 C19 -174.97(18) . . . . ? N1 C1 C20 C21 174.86(16) . . . . ? C2 C1 C20 C21 0.4(3) . . . . ? N4 C19 C20 C1 5.2(3) . . . . ? C18 C19 C20 C1 -174.91(17) . . . . ? N4 C19 C20 C21 -170.15(16) . . . . ? C18 C19 C20 C21 9.7(3) . . . . ? C1 C20 C21 C26 63.8(2) . . . . ? C19 C20 C21 C26 -120.43(19) . . . . ? C1 C20 C21 C22 -114.01(19) . . . . ? C19 C20 C21 C22 61.8(2) . . . . ? C26 C21 C22 C23 -0.1(3) . . . . ? C20 C21 C22 C23 177.75(16) . . . . ? C21 C22 C23 C24 -0.2(3) . . . . ? C22 C23 C24 C25 0.1(3) . . . . ? C22 C23 C24 C45 -177.80(16) . . . . ? C23 C24 C25 C26 0.2(3) . . . . ? C45 C24 C25 C26 178.19(16) . . . . ? C24 C25 C26 C21 -0.5(3) . . . . ? C22 C21 C26 C25 0.4(3) . . . . ? C20 C21 C26 C25 -177.38(16) . . . . ? C11 C10 C27 C28 -60.9(2) . . . . ? C9 C10 C27 C28 123.7(2) . . . . ? C11 C10 C27 C32 117.11(19) . . . . ? C9 C10 C27 C32 -58.3(2) . . . . ? C32 C27 C28 C29 -0.7(3) . . . . ? C10 C27 C28 C29 177.34(17) . . . . ? C27 C28 C29 C30 1.0(3) . . . . ? C28 C29 C30 C31 -0.3(3) . . . . ? C28 C29 C30 N5 -179.00(16) . . . . ? O3 N5 C30 C31 10.9(3) . . . . ? O4 N5 C30 C31 -168.83(17) . . . . ? O3 N5 C30 C29 -170.32(17) . . . . ? O4 N5 C30 C29 10.0(3) . . . . ? C29 C30 C31 C32 -0.7(3) . . . . ? N5 C30 C31 C32 178.01(16) . . . . ? C30 C31 C32 C27 1.0(3) . . . . ? C28 C27 C32 C31 -0.3(3) . . . . ? C10 C27 C32 C31 -178.43(17) . . . . ? C4 C5 C33 C34 113.7(2) . . . . ? C6 C5 C33 C34 -65.7(2) . . . . ? C4 C5 C33 C38 -66.8(2) . . . . ? C6 C5 C33 C38 113.8(2) . . . . ? C38 C33 C34 C35 -1.6(3) . . . . ? C5 C33 C34 C35 177.89(18) . . . . ? C33 C34 C35 C36 1.4(3) . . . . ? C34 C35 C36 C37 -0.2(3) . . . . ? C35 C36 C37 C38 -0.8(3) . . . . ? C36 C37 C38 C33 0.5(3) . . . . ? C34 C33 C38 C37 0.7(3) . . . . ? C5 C33 C38 C37 -178.83(18) . . . . ? C14 C15 C39 C40 62.6(2) . . . . ? C16 C15 C39 C40 -117.0(2) . . . . ? C14 C15 C39 C44 -118.2(2) . . . . ? C16 C15 C39 C44 62.3(2) . . . . ? C44 C39 C40 C41 -0.3(3) . . . . ? C15 C39 C40 C41 179.01(18) . . . . ? C39 C40 C41 C42 -0.2(3) . . . . ? C40 C41 C42 C43 0.0(3) . . . . ? C41 C42 C43 C44 0.6(3) . . . . ? C42 C43 C44 C39 -1.0(3) . . . . ? C40 C39 C44 C43 0.9(3) . . . . ? C15 C39 C44 C43 -178.42(18) . . . . ? C46 O2 C45 O1 -1.6(3) . . . . ? C46 O2 C45 C24 179.05(15) . . . . ? C25 C24 C45 O1 -13.3(3) . . . . ? C23 C24 C45 O1 164.64(19) . . . . ? C25 C24 C45 O2 165.97(16) . . . . ? C23 C24 C45 O2 -16.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.392 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.061 #===END data_ar221 _database_code_depnum_ccdc_archive 'CCDC 659520' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [5-(4-nitrophenyl)-15-(carbomethoxyphenyl)-10,20-bis(phenyl)porphyrinato] (tetrahydrofuran)zinc(II) ; _chemical_name_common ; (5-(4-nitrophenyl)-15-(carbomethoxyphenyl)-10,20- bis(phenyl)porphyrinato) (tetrahydrofuran)zinc(ii) ; _chemical_melting_point 205 _chemical_formula_moiety 'C50 H35.5 N5 O5 Zn, C2 H4 O0.5' _chemical_formula_sum 'C52 H39.50 N5 O5.50 Zn' _chemical_formula_weight 887.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 12.8840(8) _cell_length_b 31.4296(19) _cell_length_c 21.9485(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.6760(10) _cell_angle_gamma 90.00 _cell_volume 8703.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3684 _exptl_absorpt_coefficient_mu 0.621 _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 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart1000' _diffrn_measurement_method 'O-Scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 216499 _diffrn_reflns_av_R_equivalents 0.1374 _diffrn_reflns_av_sigmaI/netI 0.1351 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 32.20 _reflns_number_total 14625 _reflns_number_gt 7230 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1731P)^2^+27.9828P] 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 14625 _refine_ls_number_parameters 678 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2113 _refine_ls_R_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.3360 _refine_ls_wR_factor_gt 0.2344 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 0.62198(4) 0.122075(15) 0.31107(3) 0.02252(17) Uani 1 1 d . . . O1 O -0.0005(5) 0.0515(2) -0.0112(2) 0.0786(18) Uani 1 1 d . . . O2 O -0.0804(4) 0.0407(2) 0.0669(3) 0.0770(18) Uani 1 1 d . . . O3 O 1.2527(4) 0.23688(18) 0.5915(2) 0.0619(14) Uani 1 1 d . . . O4 O 1.1833(4) 0.2089(2) 0.6620(2) 0.0790(19) Uani 1 1 d . . . O5 O 0.7031(3) 0.11190(11) 0.23649(18) 0.0344(8) Uani 1 1 d . C . N1 N 0.4943(3) 0.15325(11) 0.25791(19) 0.0265(8) Uani 1 1 d . . . N2 N 0.6852(3) 0.18003(11) 0.3426(2) 0.0253(8) Uani 1 1 d . . . N3 N 0.7284(3) 0.09291(11) 0.38214(19) 0.0230(8) Uani 1 1 d . . . N4 N 0.5364(3) 0.06640(11) 0.29811(18) 0.0227(8) Uani 1 1 d . . . N5 N 1.1826(4) 0.21741(17) 0.6074(3) 0.0419(12) Uani 1 1 d . D . C1 C 0.4108(4) 0.13394(16) 0.2194(2) 0.0299(10) Uani 1 1 d . . . C2 C 0.3493(5) 0.16629(17) 0.1803(3) 0.0379(13) Uani 1 1 d . . . H2 H 0.2869 0.1616 0.1496 0.047(4) Uiso 1 1 calc R . . C3 C 0.3971(5) 0.20402(17) 0.1956(3) 0.0401(13) Uani 1 1 d . . . H3 H 0.3755 0.2308 0.1773 0.047(4) Uiso 1 1 calc R . . C4 C 0.4870(4) 0.19603(15) 0.2448(2) 0.0297(10) Uani 1 1 d . . . C5 C 0.5550(4) 0.22737(14) 0.2761(2) 0.0282(10) Uani 1 1 d . . . C6 C 0.6444(4) 0.21961(14) 0.3224(2) 0.0264(10) Uani 1 1 d . . . C7 C 0.7064(4) 0.25209(14) 0.3596(3) 0.0322(11) Uani 1 1 d . . . H7 H 0.6951 0.2819 0.3557 0.047(4) Uiso 1 1 calc R . . C8 C 0.7836(4) 0.23245(14) 0.4010(3) 0.0316(11) Uani 1 1 d . . . H8 H 0.8366 0.2457 0.4315 0.047(4) Uiso 1 1 calc R . . C9 C 0.7695(4) 0.18718(14) 0.3898(2) 0.0264(10) Uani 1 1 d . . . C10 C 0.8310(4) 0.15581(14) 0.4258(2) 0.0247(9) Uani 1 1 d . . . C11 C 0.8108(3) 0.11210(13) 0.4220(2) 0.0218(9) Uani 1 1 d . . . C12 C 0.8712(4) 0.07987(14) 0.4604(2) 0.0258(9) Uani 1 1 d . . . H12 H 0.9327 0.0845 0.4918 0.047(4) Uiso 1 1 calc R . . C13 C 0.8246(4) 0.04173(14) 0.4439(2) 0.0254(9) Uani 1 1 d . . . H13 H 0.8469 0.0148 0.4615 0.047(4) Uiso 1 1 calc R . . C14 C 0.7345(4) 0.05009(13) 0.3943(2) 0.0216(8) Uani 1 1 d . . . C15 C 0.6627(4) 0.01899(13) 0.3659(2) 0.0217(8) Uani 1 1 d . . . C16 C 0.5715(4) 0.02689(13) 0.3207(2) 0.0214(8) Uani 1 1 d . . . C17 C 0.5016(4) -0.00558(14) 0.2891(2) 0.0261(9) Uani 1 1 d . . . H17 H 0.5081 -0.0354 0.2959 0.047(4) Uiso 1 1 calc R . . C18 C 0.4248(4) 0.01455(14) 0.2477(2) 0.0271(10) Uani 1 1 d . . . H18 H 0.3672 0.0015 0.2201 0.047(4) Uiso 1 1 calc R . . C19 C 0.4470(4) 0.05945(14) 0.2534(2) 0.0228(9) Uani 1 1 d . . . C20 C 0.3862(4) 0.09077(15) 0.2170(2) 0.0250(9) Uani 1 1 d . . . C21 C 0.2881(4) 0.07697(15) 0.1729(2) 0.0299(10) Uani 1 1 d . . . C22 C 0.1988(4) 0.06585(19) 0.1943(2) 0.0366(12) Uani 1 1 d . . . H22 H 0.2012 0.0655 0.2379 0.047(4) Uiso 1 1 calc R . . C23 C 0.1046(5) 0.0550(2) 0.1535(3) 0.0457(14) Uani 1 1 d . . . H23 H 0.0439 0.0469 0.1692 0.047(4) Uiso 1 1 calc R . . C24 C 0.1008(4) 0.05602(19) 0.0904(3) 0.0404(14) Uani 1 1 d . . . C25 C 0.1903(6) 0.0661(3) 0.0684(3) 0.0561(18) Uani 1 1 d . . . H25 H 0.1882 0.0661 0.0249 0.047(4) Uiso 1 1 calc R . . C26 C 0.2831(6) 0.0761(3) 0.1091(3) 0.0541(18) Uani 1 1 d . . . H26 H 0.3447 0.0825 0.0933 0.047(4) Uiso 1 1 calc R . . C27 C 0.9249(4) 0.17086(14) 0.4725(2) 0.0269(10) Uani 1 1 d . D . C28 C 0.9299(4) 0.16384(15) 0.5360(3) 0.0310(10) Uani 1 1 d . . . H28 H 0.8750 0.1483 0.5489 0.047(4) Uiso 1 1 calc R . . C29 C 1.0127(4) 0.17910(16) 0.5797(3) 0.0331(11) Uani 1 1 d . D . H29 H 1.0152 0.1745 0.6228 0.047(4) Uiso 1 1 calc R . . C30 C 1.0926(4) 0.20136(16) 0.5601(3) 0.0316(11) Uani 1 1 d . . . C31 C 1.0906(4) 0.20821(16) 0.4979(3) 0.0328(11) Uani 1 1 d . D . H31 H 1.1466 0.2233 0.4852 0.047(4) Uiso 1 1 calc R . . C32 C 1.0064(4) 0.19297(15) 0.4541(2) 0.0285(10) Uani 1 1 d . . . H32 H 1.0043 0.1977 0.4111 0.047(4) Uiso 1 1 calc R D . C33 C 0.5271(5) 0.27274(14) 0.2595(3) 0.0339(12) Uani 1 1 d . . . C34 C 0.5878(4) 0.29779(16) 0.2291(3) 0.0356(12) Uani 1 1 d . B . H34 H 0.6491 0.2860 0.2178 0.047(4) Uiso 1 1 calc R . . C35 C 0.5617(4) 0.33996(15) 0.2144(3) 0.0338(11) Uani 1 1 d . . . H35 H 0.6104 0.3577 0.1991 0.047(4) Uiso 1 1 calc R A 1 C46 C -0.1807(11) 0.0369(4) 0.0196(7) 0.049(3) Uiso 0.50 1 d P . 1 C36 C 0.4669(6) 0.3560(2) 0.2219(4) 0.0345(15) Uani 0.75 1 d P B 1 H36 H 0.4483 0.3845 0.2100 0.047(4) Uiso 0.75 1 calc PR B 1 C37 C 0.3982(6) 0.3311(2) 0.2467(4) 0.0343(15) Uani 0.75 1 d P B 1 H37 H 0.3320 0.3423 0.2517 0.047(4) Uiso 0.75 1 calc PR B 1 C38 C 0.4254(5) 0.28939(19) 0.2643(3) 0.0298(14) Uani 0.75 1 d P B 1 H38 H 0.3764 0.2718 0.2796 0.047(4) Uiso 0.75 1 calc PR B 1 C51 C 0.7329(15) 0.0688(5) 0.1524(7) 0.046(3) Uani 0.50 1 d P C 1 H51A H 0.7938 0.0538 0.1410 0.064(9) Uiso 0.50 1 calc PR C 1 H51B H 0.6665 0.0543 0.1324 0.064(9) Uiso 0.50 1 calc PR C 1 C52 C 0.7313(14) 0.1146(6) 0.1341(7) 0.053(4) Uani 0.50 1 d P C 1 H52A H 0.8040 0.1257 0.1366 0.064(9) Uiso 0.50 1 calc PR C 1 H52B H 0.6899 0.1189 0.0913 0.064(9) Uiso 0.50 1 calc PR C 1 C46X C 1.2724(17) 0.1972(7) 0.7085(10) 0.032(4) Uiso 0.25 1 d P D 2 H46A H 1.3361 0.1970 0.6906 0.06(4) Uiso 0.25 1 calc PR D 2 H46B H 1.2611 0.1687 0.7243 0.06(4) Uiso 0.25 1 calc PR D 2 H46C H 1.2813 0.2177 0.7428 0.06(4) Uiso 0.25 1 calc PR D 2 C36X C 0.5069(18) 0.3613(7) 0.2537(11) 0.032(4) Uiso 0.25 1 d P B 2 H36X H 0.4929 0.3909 0.2480 0.047(4) Uiso 0.25 1 calc PR B 2 C37X C 0.4729(15) 0.3399(5) 0.3007(10) 0.026(4) Uani 0.25 1 d P B 2 H37X H 0.4348 0.3545 0.3272 0.047(4) Uiso 0.25 1 calc PR B 2 C38X C 0.4951(16) 0.2964(6) 0.3089(8) 0.026(4) Uani 0.25 1 d P B 2 H38X H 0.4892 0.2827 0.3466 0.047(4) Uiso 0.25 1 calc PR B 2 C51X C 0.687(3) 0.0562(9) 0.1699(17) 0.059(9) Uani 0.25 1 d P C 2 H51C H 0.6256 0.0390 0.1766 0.064(9) Uiso 0.25 1 calc PR C 2 H51D H 0.7312 0.0386 0.1478 0.064(9) Uiso 0.25 1 calc PR C 2 C52X C 0.650(3) 0.0969(9) 0.1335(13) 0.068(10) Uani 0.25 1 d P C 2 H52C H 0.5724 0.0962 0.1177 0.064(9) Uiso 0.25 1 calc PR C 2 H52D H 0.6853 0.0998 0.0977 0.064(9) Uiso 0.25 1 calc PR C 2 C46Y C -0.064(4) 0.0571(17) -0.067(2) 0.110(15) Uiso 0.25 1 d P E 3 H46D H -0.1240 0.0375 -0.0710 0.06(4) Uiso 0.25 1 calc PR E 3 H46E H -0.0242 0.0515 -0.0995 0.06(4) Uiso 0.25 1 calc PR E 3 H46F H -0.0899 0.0865 -0.0701 0.06(4) Uiso 0.25 1 calc PR E 3 C51Y C 0.804(3) 0.0784(9) 0.1735(15) 0.057(8) Uani 0.25 1 d P C 3 H51E H 0.8817 0.0770 0.1901 0.064(9) Uiso 0.25 1 calc PR C 3 H51F H 0.7852 0.0570 0.1401 0.064(9) Uiso 0.25 1 calc PR C 3 C52Y C 0.772(2) 0.1224(9) 0.1494(13) 0.035(6) Uiso 0.25 1 d P C 3 H52E H 0.7501 0.1220 0.1035 0.064(9) Uiso 0.25 1 calc PR C 3 H52F H 0.8323 0.1425 0.1610 0.064(9) Uiso 0.25 1 calc PR C 3 C39 C 0.6864(4) -0.02635(13) 0.3843(2) 0.0226(9) Uani 1 1 d . . . C40 C 0.6186(4) -0.04900(14) 0.4138(2) 0.0277(10) Uani 1 1 d . . . H40 H 0.5580 -0.0354 0.4234 0.047(4) Uiso 1 1 calc R . . C41 C 0.6388(4) -0.09167(14) 0.4295(3) 0.0323(11) Uani 1 1 d . . . H41 H 0.5924 -0.1070 0.4500 0.047(4) Uiso 1 1 calc R . . C42 C 0.7269(4) -0.11160(15) 0.4150(3) 0.0336(11) Uani 1 1 d . . . H42 H 0.7403 -0.1407 0.4252 0.047(4) Uiso 1 1 calc R . . C43 C 0.7949(4) -0.08914(16) 0.3858(3) 0.0333(11) Uani 1 1 d . . . H43 H 0.8554 -0.1028 0.3761 0.047(4) Uiso 1 1 calc R . . C44 C 0.7749(4) -0.04663(14) 0.3707(2) 0.0272(10) Uani 1 1 d . . . H44 H 0.8221 -0.0312 0.3508 0.047(4) Uiso 1 1 calc R . . C45 C 0.0006(5) 0.0485(2) 0.0443(3) 0.0512(17) Uani 1 1 d . . . C50 C 0.7439(6) 0.07083(18) 0.2246(3) 0.0440(14) Uani 1 1 d . . . H50A H 0.7024 0.0479 0.2392 0.064(9) Uiso 1 1 calc R C 1 H50B H 0.8191 0.0680 0.2458 0.064(9) Uiso 1 1 calc R C 1 C53 C 0.6804(6) 0.1352(2) 0.1796(3) 0.0463(15) Uani 1 1 d . . . H53A H 0.7067 0.1647 0.1868 0.064(9) Uiso 1 1 calc R C 1 H53B H 0.6028 0.1363 0.1638 0.064(9) Uiso 1 1 calc R C 1 O6 O 0.9164(9) 0.3194(4) 0.4671(5) 0.064(3) Uani 0.50 1 d P . . C63 C 1.0151(12) 0.3254(5) 0.4612(6) 0.055(4) Uani 0.50 1 d P G . H63A H 1.0243 0.3532 0.4416 0.064(9) Uiso 0.50 1 calc PR F 1 H63B H 1.0399 0.3023 0.4370 0.064(9) Uiso 0.50 1 calc PR F 1 C60 C 0.906(2) 0.3290(7) 0.5268(9) 0.045(5) Uani 0.30 1 d P G 1 H60A H 0.8465 0.3127 0.5374 0.064(9) Uiso 0.30 1 calc PR G 1 H60B H 0.8905 0.3597 0.5299 0.064(9) Uiso 0.30 1 calc PR G 1 C61 C 1.000(3) 0.3189(9) 0.5684(10) 0.057(7) Uani 0.30 1 d P G 1 H61A H 1.0125 0.3384 0.6046 0.064(9) Uiso 0.30 1 calc PR G 1 H61B H 0.9989 0.2892 0.5833 0.064(9) Uiso 0.30 1 calc PR G 1 C62 C 1.0737(19) 0.3243(5) 0.5325(13) 0.030(5) Uani 0.30 1 d P G 1 H62A H 1.1254 0.3006 0.5396 0.064(9) Uiso 0.30 1 calc PR G 1 H62B H 1.1126 0.3513 0.5437 0.064(9) Uiso 0.30 1 calc PR G 1 C60X C 0.952(4) 0.3080(9) 0.5344(18) 0.058(12) Uani 0.20 1 d P G 2 H60C H 0.9357 0.2777 0.5403 0.064(9) Uiso 0.20 1 calc PR G 2 H60D H 0.9117 0.3252 0.5595 0.064(9) Uiso 0.20 1 calc PR G 2 C61X C 1.073(4) 0.3157(17) 0.5582(18) 0.054(13) Uani 0.20 1 d P G 2 H61C H 1.0844 0.3396 0.5883 0.064(9) Uiso 0.20 1 calc PR G 2 H61D H 1.1067 0.2899 0.5795 0.064(9) Uiso 0.20 1 calc PR G 2 C62X C 1.111(3) 0.3238(10) 0.5148(16) 0.036(8) Uiso 0.20 1 d P G 2 H62C H 1.1618 0.3014 0.5080 0.064(9) Uiso 0.20 1 calc PR G 2 H62D H 1.1485 0.3516 0.5203 0.064(9) Uiso 0.20 1 calc PR G 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 Zn1 0.0267(3) 0.0134(2) 0.0262(3) 0.00189(19) 0.0022(2) 0.00047(19) O1 0.092(4) 0.079(4) 0.045(3) -0.016(3) -0.033(3) 0.015(3) O2 0.034(3) 0.124(5) 0.064(3) -0.034(3) -0.012(2) 0.002(3) O3 0.039(2) 0.086(4) 0.061(3) -0.034(3) 0.010(2) -0.034(2) O4 0.039(3) 0.158(6) 0.034(3) -0.007(3) -0.006(2) 0.005(3) O5 0.047(2) 0.0237(16) 0.035(2) 0.0059(14) 0.0155(17) 0.0083(15) N1 0.033(2) 0.0153(16) 0.028(2) 0.0013(14) -0.0010(17) 0.0030(15) N2 0.029(2) 0.0139(16) 0.032(2) 0.0018(15) 0.0048(17) -0.0018(14) N3 0.0243(19) 0.0150(15) 0.029(2) 0.0001(14) 0.0023(15) -0.0033(13) N4 0.0260(19) 0.0136(15) 0.027(2) 0.0008(14) 0.0024(15) 0.0003(13) N5 0.026(2) 0.049(3) 0.048(3) -0.014(2) 0.001(2) 0.003(2) C1 0.034(3) 0.023(2) 0.031(3) 0.0028(18) 0.001(2) 0.0084(19) C2 0.045(3) 0.031(3) 0.030(3) 0.012(2) -0.009(2) 0.012(2) C3 0.053(4) 0.028(2) 0.034(3) 0.009(2) -0.002(3) 0.012(2) C4 0.038(3) 0.020(2) 0.029(2) 0.0029(18) 0.003(2) 0.0041(19) C5 0.042(3) 0.0131(18) 0.031(2) 0.0063(17) 0.011(2) 0.0039(17) C6 0.031(2) 0.0148(18) 0.035(3) 0.0022(17) 0.009(2) -0.0011(16) C7 0.041(3) 0.0140(19) 0.041(3) -0.0008(18) 0.008(2) -0.0017(18) C8 0.032(3) 0.0169(19) 0.045(3) -0.0047(19) 0.007(2) -0.0036(18) C9 0.027(2) 0.0165(18) 0.036(3) 0.0006(17) 0.006(2) -0.0039(16) C10 0.026(2) 0.0175(19) 0.030(2) -0.0023(17) 0.0031(18) -0.0040(16) C11 0.021(2) 0.0175(18) 0.026(2) -0.0011(16) 0.0008(17) -0.0028(15) C12 0.022(2) 0.023(2) 0.030(2) 0.0008(18) -0.0016(18) -0.0008(16) C13 0.023(2) 0.0181(19) 0.032(2) 0.0009(17) -0.0005(19) 0.0010(16) C14 0.026(2) 0.0131(17) 0.025(2) 0.0005(15) 0.0039(17) 0.0009(15) C15 0.023(2) 0.0144(17) 0.027(2) 0.0008(15) 0.0015(17) 0.0001(15) C16 0.023(2) 0.0147(17) 0.025(2) 0.0022(15) 0.0015(17) 0.0018(15) C17 0.029(2) 0.0157(18) 0.032(2) -0.0029(17) 0.0006(19) -0.0007(16) C18 0.027(2) 0.020(2) 0.031(2) -0.0022(18) -0.0016(19) 0.0016(17) C19 0.023(2) 0.0187(18) 0.025(2) -0.0005(16) 0.0015(17) 0.0020(16) C20 0.027(2) 0.024(2) 0.022(2) -0.0017(17) 0.0019(18) 0.0002(17) C21 0.030(3) 0.026(2) 0.029(2) -0.0003(19) -0.004(2) 0.0049(19) C22 0.032(3) 0.050(3) 0.024(2) 0.000(2) -0.002(2) 0.000(2) C23 0.037(3) 0.061(4) 0.035(3) -0.001(3) -0.004(2) 0.001(3) C24 0.032(3) 0.042(3) 0.038(3) -0.010(2) -0.013(2) 0.011(2) C25 0.056(4) 0.085(5) 0.024(3) -0.008(3) 0.002(3) -0.006(4) C26 0.048(4) 0.084(5) 0.029(3) -0.007(3) 0.006(3) -0.010(3) C27 0.025(2) 0.020(2) 0.034(3) -0.0029(18) 0.0028(19) -0.0045(17) C28 0.031(3) 0.024(2) 0.039(3) -0.001(2) 0.009(2) -0.0015(18) C29 0.032(3) 0.029(2) 0.036(3) -0.003(2) 0.002(2) 0.005(2) C30 0.027(2) 0.029(2) 0.036(3) -0.005(2) 0.000(2) 0.0017(19) C31 0.029(3) 0.025(2) 0.044(3) -0.007(2) 0.007(2) -0.0019(19) C32 0.027(2) 0.026(2) 0.032(3) -0.0050(19) 0.004(2) -0.0039(18) C33 0.046(3) 0.0141(19) 0.044(3) 0.0076(19) 0.017(3) 0.0074(19) C34 0.034(3) 0.024(2) 0.054(3) 0.010(2) 0.023(3) 0.0071(19) C35 0.038(3) 0.020(2) 0.044(3) 0.007(2) 0.012(2) -0.0002(19) C36 0.044(4) 0.018(3) 0.040(4) 0.011(3) 0.004(3) 0.006(3) C37 0.028(3) 0.024(3) 0.049(4) 0.004(3) 0.000(3) 0.007(2) C38 0.026(3) 0.020(3) 0.043(4) 0.004(3) 0.006(3) 0.000(2) C51 0.061(11) 0.047(8) 0.034(7) -0.005(6) 0.019(7) 0.009(7) C52 0.048(9) 0.082(12) 0.031(7) 0.011(7) 0.011(7) 0.012(9) C37X 0.026(9) 0.016(7) 0.040(11) -0.002(7) 0.014(8) -0.002(6) C38X 0.035(10) 0.026(8) 0.016(8) 0.011(7) 0.005(7) -0.002(7) C51X 0.07(2) 0.032(13) 0.06(2) -0.005(13) -0.026(17) 0.008(13) C52X 0.10(3) 0.046(15) 0.035(14) 0.000(11) -0.028(16) 0.007(16) C51Y 0.10(3) 0.038(14) 0.045(16) 0.018(12) 0.036(18) 0.018(16) C39 0.027(2) 0.0118(16) 0.026(2) 0.0016(15) -0.0008(18) -0.0002(15) C40 0.029(2) 0.0174(19) 0.036(3) 0.0042(18) 0.006(2) 0.0010(17) C41 0.036(3) 0.018(2) 0.043(3) 0.005(2) 0.011(2) -0.0025(18) C42 0.043(3) 0.0146(19) 0.041(3) 0.0057(19) 0.004(2) 0.0054(18) C43 0.039(3) 0.024(2) 0.036(3) 0.001(2) 0.004(2) 0.009(2) C44 0.031(2) 0.0180(19) 0.031(2) 0.0014(17) 0.004(2) 0.0036(17) C45 0.040(3) 0.056(4) 0.047(4) -0.016(3) -0.016(3) 0.015(3) C50 0.061(4) 0.028(3) 0.048(3) 0.007(2) 0.022(3) 0.016(3) C53 0.066(4) 0.037(3) 0.039(3) 0.018(3) 0.018(3) 0.009(3) O6 0.072(7) 0.070(7) 0.050(6) -0.006(5) 0.011(5) -0.027(6) C63 0.071(10) 0.047(7) 0.046(7) 0.028(6) 0.007(7) 0.001(6) C60 0.070(15) 0.034(10) 0.034(10) 0.009(8) 0.017(10) 0.000(10) C61 0.10(2) 0.057(14) 0.015(9) 0.014(10) 0.021(12) 0.016(14) C62 0.033(11) 0.007(6) 0.050(15) 0.001(8) 0.010(12) 0.001(6) C60X 0.13(4) 0.014(12) 0.04(2) -0.006(12) 0.05(2) 0.019(17) C61X 0.04(2) 0.09(4) 0.025(18) -0.019(19) 0.010(18) -0.04(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 N2 2.057(4) . ? Zn1 N4 2.057(4) . ? Zn1 N1 2.062(4) . ? Zn1 N3 2.071(4) . ? Zn1 O5 2.137(4) . ? O1 C45 1.221(9) . ? O1 C46Y 1.33(5) . ? O2 C45 1.266(9) . ? O2 C46 1.488(14) . ? O3 N5 1.200(7) . ? O4 N5 1.227(7) . ? O4 C46X 1.42(2) . ? O5 C53 1.426(7) . ? O5 C50 1.438(6) . ? N1 C1 1.368(6) . ? N1 C4 1.374(6) . ? N2 C9 1.360(6) . ? N2 C6 1.388(6) . ? N3 C14 1.371(5) . ? N3 C11 1.371(6) . ? N4 C19 1.370(6) . ? N4 C16 1.380(5) . ? N5 C30 1.478(7) . ? C1 C20 1.392(7) . ? C1 C2 1.457(7) . ? C2 C3 1.347(8) . ? C2 H2 0.9500 . ? C3 C4 1.436(7) . ? C3 H3 0.9500 . ? C4 C5 1.402(7) . ? C5 C6 1.395(7) . ? C5 C33 1.497(6) . ? C6 C7 1.443(7) . ? C7 C8 1.353(7) . ? C7 H7 0.9500 . ? C8 C9 1.449(6) . ? C8 H8 0.9500 . ? C9 C10 1.403(7) . ? C10 C11 1.397(6) . ? C10 C27 1.496(7) . ? C11 C12 1.441(6) . ? C12 C13 1.356(6) . ? C12 H12 0.9500 . ? C13 C14 1.447(6) . ? C13 H13 0.9500 . ? C14 C15 1.402(6) . ? C15 C16 1.397(6) . ? C15 C39 1.496(6) . ? C16 C17 1.443(6) . ? C17 C18 1.358(7) . ? C17 H17 0.9500 . ? C18 C19 1.440(6) . ? C18 H18 0.9500 . ? C19 C20 1.403(6) . ? C20 C21 1.493(7) . ? C21 C22 1.373(8) . ? C21 C26 1.389(8) . ? C22 C23 1.398(8) . ? C22 H22 0.9500 . ? C23 C24 1.378(9) . ? C23 H23 0.9500 . ? C24 C25 1.374(10) . ? C24 C45 1.488(8) . ? C25 C26 1.375(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.385(7) . ? C27 C28 1.399(7) . ? C28 C29 1.370(7) . ? C28 H28 0.9500 . ? C29 C30 1.383(8) . ? C29 H29 0.9500 . ? C30 C31 1.378(8) . ? C31 C32 1.381(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.375(7) . ? C33 C38 1.434(8) . ? C33 C38X 1.44(2) . ? C34 C35 1.389(7) . ? C34 H34 0.9500 . ? C35 C36 1.362(9) . ? C35 C36X 1.39(2) . ? C35 H35 0.9500 . ? C46 C46 1.82(3) 2_455 ? C36 C37 1.375(10) . ? C36 H36 0.9500 . ? C37 C38 1.390(9) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C51 C52 1.49(2) . ? C51 C50 1.563(15) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.452(16) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C46X H46A 0.9800 . ? C46X H46B 0.9800 . ? C46X H46C 0.9800 . ? C36X C37X 1.38(3) . ? C36X H36X 0.9500 . ? C37X C38X 1.40(2) . ? C37X H37X 0.9500 . ? C38X H38X 0.9500 . ? C51X C50 1.35(3) . ? C51X C52X 1.53(4) . ? C51X H51C 0.9900 . ? C51X H51D 0.9900 . ? C52X C53 1.57(3) . ? C52X H52C 0.9900 . ? C52X H52D 0.9900 . ? C46Y H46D 0.9800 . ? C46Y H46E 0.9800 . ? C46Y H46F 0.9800 . ? C51Y C52Y 1.51(4) . ? C51Y C50 1.51(3) . ? C51Y H51E 0.9900 . ? C51Y H51F 0.9900 . ? C52Y C53 1.53(3) . ? C52Y H52E 0.9900 . ? C52Y H52F 0.9900 . ? C39 C40 1.385(7) . ? C39 C44 1.391(7) . ? C40 C41 1.396(6) . ? C40 H40 0.9500 . ? C41 C42 1.388(8) . ? C41 H41 0.9500 . ? C42 C43 1.380(8) . ? C42 H42 0.9500 . ? C43 C44 1.388(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? O6 C63 1.318(18) . ? O6 C60 1.38(2) . ? O6 C60X 1.50(4) . ? C63 C62X 1.53(3) . ? C63 C62 1.59(3) . ? C63 C60X 2.02(4) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C60 C61 1.40(4) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.36(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C60X C61X 1.56(7) . ? C60X H60C 0.9900 . ? C60X H60D 0.9900 . ? C61X C62X 1.19(5) . ? C61X H61C 0.9900 . ? C61X H61D 0.9900 . ? C62X H62C 0.9900 . ? C62X H62D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N4 164.64(16) . . ? N2 Zn1 N1 89.20(15) . . ? N4 Zn1 N1 88.95(15) . . ? N2 Zn1 N3 88.94(15) . . ? N4 Zn1 N3 89.00(15) . . ? N1 Zn1 N3 165.37(17) . . ? N2 Zn1 O5 99.71(16) . . ? N4 Zn1 O5 95.65(15) . . ? N1 Zn1 O5 95.50(16) . . ? N3 Zn1 O5 99.12(15) . . ? C45 O1 C46Y 143(2) . . ? C45 O2 C46 114.3(7) . . ? N5 O4 C46X 127.1(10) . . ? C53 O5 C50 108.6(4) . . ? C53 O5 Zn1 123.3(3) . . ? C50 O5 Zn1 121.8(3) . . ? C1 N1 C4 107.0(4) . . ? C1 N1 Zn1 125.2(3) . . ? C4 N1 Zn1 126.6(3) . . ? C9 N2 C6 106.7(4) . . ? C9 N2 Zn1 127.1(3) . . ? C6 N2 Zn1 126.0(3) . . ? C14 N3 C11 107.5(4) . . ? C14 N3 Zn1 125.7(3) . . ? C11 N3 Zn1 126.5(3) . . ? C19 N4 C16 106.3(4) . . ? C19 N4 Zn1 125.7(3) . . ? C16 N4 Zn1 126.0(3) . . ? O3 N5 O4 122.6(5) . . ? O3 N5 C30 120.0(5) . . ? O4 N5 C30 117.4(5) . . ? N1 C1 C20 126.9(4) . . ? N1 C1 C2 108.7(4) . . ? C20 C1 C2 124.5(5) . . ? C3 C2 C1 107.5(5) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? C2 C3 C4 107.0(4) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C5 125.1(5) . . ? N1 C4 C3 109.8(4) . . ? C5 C4 C3 125.0(4) . . ? C6 C5 C4 125.2(4) . . ? C6 C5 C33 117.7(4) . . ? C4 C5 C33 117.1(5) . . ? N2 C6 C5 126.4(4) . . ? N2 C6 C7 108.8(4) . . ? C5 C6 C7 124.7(4) . . ? C8 C7 C6 107.7(4) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? C7 C8 C9 106.5(4) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C10 125.8(4) . . ? N2 C9 C8 110.2(4) . . ? C10 C9 C8 123.9(5) . . ? C11 C10 C9 125.5(4) . . ? C11 C10 C27 117.8(4) . . ? C9 C10 C27 116.7(4) . . ? N3 C11 C10 125.5(4) . . ? N3 C11 C12 108.7(4) . . ? C10 C11 C12 125.8(4) . . ? C13 C12 C11 107.9(4) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? C12 C13 C14 106.5(4) . . ? C12 C13 H13 126.7 . . ? C14 C13 H13 126.7 . . ? N3 C14 C15 126.2(4) . . ? N3 C14 C13 109.3(4) . . ? C15 C14 C13 124.4(4) . . ? C16 C15 C14 125.2(4) . . ? C16 C15 C39 117.2(4) . . ? C14 C15 C39 117.6(4) . . ? N4 C16 C15 125.7(4) . . ? N4 C16 C17 109.6(4) . . ? C15 C16 C17 124.7(4) . . ? C18 C17 C16 107.0(4) . . ? C18 C17 H17 126.5 . . ? C16 C17 H17 126.5 . . ? C17 C18 C19 107.0(4) . . ? C17 C18 H18 126.5 . . ? C19 C18 H18 126.5 . . ? N4 C19 C20 125.9(4) . . ? N4 C19 C18 110.0(4) . . ? C20 C19 C18 124.0(4) . . ? C1 C20 C19 124.5(4) . . ? C1 C20 C21 117.6(4) . . ? C19 C20 C21 117.9(4) . . ? C22 C21 C26 118.0(5) . . ? C22 C21 C20 120.6(5) . . ? C26 C21 C20 121.4(5) . . ? C21 C22 C23 121.4(5) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 119.2(6) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 119.8(5) . . ? C25 C24 C45 118.3(6) . . ? C23 C24 C45 121.9(6) . . ? C24 C25 C26 120.4(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 121.1(6) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C32 C27 C28 119.0(4) . . ? C32 C27 C10 121.0(5) . . ? C28 C27 C10 120.0(4) . . ? C29 C28 C27 121.0(5) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C30 118.9(5) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? C31 C30 C29 121.4(5) . . ? C31 C30 N5 119.8(5) . . ? C29 C30 N5 118.8(5) . . ? C30 C31 C32 119.4(5) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C31 C32 C27 120.4(5) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C34 C33 C38 116.4(5) . . ? C34 C33 C38X 110.3(8) . . ? C38 C33 C38X 49.7(8) . . ? C34 C33 C5 122.1(5) . . ? C38 C33 C5 120.5(5) . . ? C38X C33 C5 113.6(8) . . ? C33 C34 C35 121.6(5) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C36 C35 C34 120.5(5) . . ? C36 C35 C36X 33.6(9) . . ? C34 C35 C36X 116.5(10) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C36X C35 H35 112.9 . . ? O2 C46 C46 163.9(14) . 2_455 ? C35 C36 C37 120.0(6) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C36 C37 C38 120.1(6) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C33 120.4(6) . . ? C37 C38 H38 119.8 . . ? C33 C38 H38 119.8 . . ? C52 C51 C50 103.1(11) . . ? C52 C51 H51A 111.1 . . ? C50 C51 H51A 111.1 . . ? C52 C51 H51B 111.1 . . ? C50 C51 H51B 111.1 . . ? H51A C51 H51B 109.1 . . ? C53 C52 C51 103.2(11) . . ? C53 C52 H52A 111.1 . . ? C51 C52 H52A 111.1 . . ? C53 C52 H52B 111.1 . . ? C51 C52 H52B 111.1 . . ? H52A C52 H52B 109.1 . . ? O4 C46X H46A 109.5 . . ? O4 C46X H46B 109.5 . . ? H46A C46X H46B 109.5 . . ? O4 C46X H46C 109.5 . . ? H46A C46X H46C 109.5 . . ? H46B C46X H46C 109.5 . . ? C37X C36X C35 120.5(18) . . ? C37X C36X H36X 119.8 . . ? C35 C36X H36X 119.8 . . ? C36X C37X C38X 119.0(18) . . ? C36X C37X H37X 120.5 . . ? C38X C37X H37X 120.5 . . ? C37X C38X C33 119.3(14) . . ? C37X C38X H38X 120.4 . . ? C33 C38X H38X 120.4 . . ? C50 C51X C52X 103(2) . . ? C50 C51X H51C 111.1 . . ? C52X C51X H51C 111.1 . . ? C50 C51X H51D 111.1 . . ? C52X C51X H51D 111.1 . . ? H51C C51X H51D 109.1 . . ? C51X C52X C53 107.1(19) . . ? C51X C52X H52C 110.3 . . ? C53 C52X H52C 110.3 . . ? C51X C52X H52D 110.3 . . ? C53 C52X H52D 110.3 . . ? H52C C52X H52D 108.5 . . ? O1 C46Y H46D 109.5 . . ? O1 C46Y H46E 109.5 . . ? O1 C46Y H46F 109.5 . . ? C52Y C51Y C50 105(2) . . ? C52Y C51Y H51E 110.7 . . ? C50 C51Y H51E 110.7 . . ? C52Y C51Y H51F 110.7 . . ? C50 C51Y H51F 110.7 . . ? H51E C51Y H51F 108.8 . . ? C51Y C52Y C53 106(2) . . ? C51Y C52Y H52E 110.6 . . ? C53 C52Y H52E 110.6 . . ? C51Y C52Y H52F 110.6 . . ? C53 C52Y H52F 110.6 . . ? H52E C52Y H52F 108.7 . . ? C40 C39 C44 119.2(4) . . ? C40 C39 C15 120.2(4) . . ? C44 C39 C15 120.6(4) . . ? C39 C40 C41 120.4(5) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 119.8(5) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C43 C42 C41 120.1(4) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 119.9(5) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C43 C44 C39 120.7(5) . . ? C43 C44 H44 119.7 . . ? C39 C44 H44 119.7 . . ? O1 C45 O2 124.2(6) . . ? O1 C45 C24 119.9(7) . . ? O2 C45 C24 115.9(6) . . ? C51X C50 O5 108.3(13) . . ? C51X C50 C51Y 70(2) . . ? O5 C50 C51Y 104.8(11) . . ? C51X C50 C51 33.6(17) . . ? O5 C50 C51 105.1(7) . . ? C51Y C50 C51 37.6(15) . . ? C51X C50 H50A 78.8 . . ? O5 C50 H50A 110.7 . . ? C51Y C50 H50A 138.7 . . ? C51 C50 H50A 110.7 . . ? C51X C50 H50B 133.7 . . ? O5 C50 H50B 110.7 . . ? C51Y C50 H50B 76.2 . . ? C51 C50 H50B 110.7 . . ? H50A C50 H50B 108.8 . . ? O5 C53 C52 109.4(7) . . ? O5 C53 C52Y 101.8(11) . . ? C52 C53 C52Y 23.8(10) . . ? O5 C53 C52X 98.7(11) . . ? C52 C53 C52X 46.0(17) . . ? C52Y C53 C52X 68.4(19) . . ? O5 C53 H53A 109.8 . . ? C52 C53 H53A 109.8 . . ? C52Y C53 H53A 92.6 . . ? C52X C53 H53A 148.7 . . ? O5 C53 H53B 109.8 . . ? C52 C53 H53B 109.8 . . ? C52Y C53 H53B 132.5 . . ? C52X C53 H53B 72.4 . . ? H53A C53 H53B 108.2 . . ? C63 O6 C60 110.1(14) . . ? C63 O6 C60X 91(2) . . ? C60 O6 C60X 35.3(14) . . ? O6 C63 C62X 124.6(17) . . ? O6 C63 C62 100.1(14) . . ? C62X C63 C62 25.0(12) . . ? O6 C63 C60X 47.9(16) . . ? C62X C63 C60X 77(2) . . ? C62 C63 C60X 53.1(17) . . ? O6 C63 H63A 111.8 . . ? C62X C63 H63A 102.4 . . ? C62 C63 H63A 111.8 . . ? C60X C63 H63A 133.4 . . ? O6 C63 H63B 111.8 . . ? C62X C63 H63B 95.2 . . ? C62 C63 H63B 111.8 . . ? C60X C63 H63B 117.0 . . ? H63A C63 H63B 109.5 . . ? O6 C60 C61 110(2) . . ? O6 C60 H60A 109.7 . . ? C61 C60 H60A 109.7 . . ? O6 C60 H60B 109.7 . . ? C61 C60 H60B 109.7 . . ? H60A C60 H60B 108.2 . . ? C62 C61 C60 101.9(18) . . ? C62 C61 H61A 111.4 . . ? C60 C61 H61A 111.4 . . ? C62 C61 H61B 111.4 . . ? C60 C61 H61B 111.4 . . ? H61A C61 H61B 109.3 . . ? C61 C62 C63 109(2) . . ? C61 C62 H62A 109.9 . . ? C63 C62 H62A 109.9 . . ? C61 C62 H62B 109.9 . . ? C63 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? O6 C60X C61X 112(3) . . ? O6 C60X C63 40.8(10) . . ? C61X C60X C63 72(2) . . ? O6 C60X H60C 109.2 . . ? C61X C60X H60C 109.2 . . ? C63 C60X H60C 119.6 . . ? O6 C60X H60D 109.2 . . ? C61X C60X H60D 109.2 . . ? C63 C60X H60D 129.5 . . ? H60C C60X H60D 107.9 . . ? C62X C61X C60X 108(4) . . ? C62X C61X H61C 110.0 . . ? C60X C61X H61C 110.0 . . ? C62X C61X H61D 110.0 . . ? C60X C61X H61D 110.0 . . ? H61C C61X H61D 108.4 . . ? C61X C62X C63 103(3) . . ? C61X C62X H62C 111.2 . . ? C63 C62X H62C 111.2 . . ? C61X C62X H62D 111.2 . . ? C63 C62X H62D 111.2 . . ? H62C C62X H62D 109.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zn1 O5 C53 -72.0(5) . . . . ? N4 Zn1 O5 C53 107.6(5) . . . . ? N1 Zn1 O5 C53 18.1(5) . . . . ? N3 Zn1 O5 C53 -162.5(5) . . . . ? N2 Zn1 O5 C50 139.1(4) . . . . ? N4 Zn1 O5 C50 -41.3(5) . . . . ? N1 Zn1 O5 C50 -130.8(4) . . . . ? N3 Zn1 O5 C50 48.6(5) . . . . ? N2 Zn1 N1 C1 179.1(4) . . . . ? N4 Zn1 N1 C1 -16.2(4) . . . . ? N3 Zn1 N1 C1 -98.2(7) . . . . ? O5 Zn1 N1 C1 79.4(4) . . . . ? N2 Zn1 N1 C4 13.2(4) . . . . ? N4 Zn1 N1 C4 177.9(4) . . . . ? N3 Zn1 N1 C4 95.9(7) . . . . ? O5 Zn1 N1 C4 -86.5(4) . . . . ? N4 Zn1 N2 C9 86.5(7) . . . . ? N1 Zn1 N2 C9 169.6(4) . . . . ? N3 Zn1 N2 C9 4.1(4) . . . . ? O5 Zn1 N2 C9 -94.9(4) . . . . ? N4 Zn1 N2 C6 -88.4(7) . . . . ? N1 Zn1 N2 C6 -5.3(4) . . . . ? N3 Zn1 N2 C6 -170.7(4) . . . . ? O5 Zn1 N2 C6 90.2(4) . . . . ? N2 Zn1 N3 C14 178.0(4) . . . . ? N4 Zn1 N3 C14 13.2(4) . . . . ? N1 Zn1 N3 C14 95.3(7) . . . . ? O5 Zn1 N3 C14 -82.3(4) . . . . ? N2 Zn1 N3 C11 -7.8(4) . . . . ? N4 Zn1 N3 C11 -172.6(4) . . . . ? N1 Zn1 N3 C11 -90.6(7) . . . . ? O5 Zn1 N3 C11 91.8(4) . . . . ? N2 Zn1 N4 C19 99.9(7) . . . . ? N1 Zn1 N4 C19 16.8(4) . . . . ? N3 Zn1 N4 C19 -177.7(4) . . . . ? O5 Zn1 N4 C19 -78.7(4) . . . . ? N2 Zn1 N4 C16 -98.1(7) . . . . ? N1 Zn1 N4 C16 178.8(4) . . . . ? N3 Zn1 N4 C16 -15.7(4) . . . . ? O5 Zn1 N4 C16 83.4(4) . . . . ? C46X O4 N5 O3 -37.9(15) . . . . ? C46X O4 N5 C30 140.0(12) . . . . ? C4 N1 C1 C20 -179.4(5) . . . . ? Zn1 N1 C1 C20 12.4(8) . . . . ? C4 N1 C1 C2 0.4(6) . . . . ? Zn1 N1 C1 C2 -167.9(4) . . . . ? N1 C1 C2 C3 0.5(7) . . . . ? C20 C1 C2 C3 -179.8(5) . . . . ? C1 C2 C3 C4 -1.1(7) . . . . ? C1 N1 C4 C5 176.9(5) . . . . ? Zn1 N1 C4 C5 -15.1(7) . . . . ? C1 N1 C4 C3 -1.0(6) . . . . ? Zn1 N1 C4 C3 167.0(4) . . . . ? C2 C3 C4 N1 1.3(7) . . . . ? C2 C3 C4 C5 -176.6(5) . . . . ? N1 C4 C5 C6 4.6(9) . . . . ? C3 C4 C5 C6 -177.7(5) . . . . ? N1 C4 C5 C33 -173.5(5) . . . . ? C3 C4 C5 C33 4.1(8) . . . . ? C9 N2 C6 C5 -177.5(5) . . . . ? Zn1 N2 C6 C5 -1.7(7) . . . . ? C9 N2 C6 C7 -0.6(5) . . . . ? Zn1 N2 C6 C7 175.2(3) . . . . ? C4 C5 C6 N2 4.3(8) . . . . ? C33 C5 C6 N2 -177.5(5) . . . . ? C4 C5 C6 C7 -172.1(5) . . . . ? C33 C5 C6 C7 6.1(8) . . . . ? N2 C6 C7 C8 0.5(6) . . . . ? C5 C6 C7 C8 177.5(5) . . . . ? C6 C7 C8 C9 -0.2(6) . . . . ? C6 N2 C9 C10 176.7(5) . . . . ? Zn1 N2 C9 C10 1.1(7) . . . . ? C6 N2 C9 C8 0.4(6) . . . . ? Zn1 N2 C9 C8 -175.2(3) . . . . ? C7 C8 C9 N2 -0.1(6) . . . . ? C7 C8 C9 C10 -176.5(5) . . . . ? N2 C9 C10 C11 -5.2(8) . . . . ? C8 C9 C10 C11 170.6(5) . . . . ? N2 C9 C10 C27 175.8(5) . . . . ? C8 C9 C10 C27 -8.3(7) . . . . ? C14 N3 C11 C10 -178.1(5) . . . . ? Zn1 N3 C11 C10 6.9(7) . . . . ? C14 N3 C11 C12 0.4(5) . . . . ? Zn1 N3 C11 C12 -174.6(3) . . . . ? C9 C10 C11 N3 0.9(8) . . . . ? C27 C10 C11 N3 179.8(4) . . . . ? C9 C10 C11 C12 -177.4(5) . . . . ? C27 C10 C11 C12 1.6(7) . . . . ? N3 C11 C12 C13 -0.5(6) . . . . ? C10 C11 C12 C13 178.0(5) . . . . ? C11 C12 C13 C14 0.4(6) . . . . ? C11 N3 C14 C15 177.1(5) . . . . ? Zn1 N3 C14 C15 -7.9(7) . . . . ? C11 N3 C14 C13 -0.2(5) . . . . ? Zn1 N3 C14 C13 174.9(3) . . . . ? C12 C13 C14 N3 -0.2(6) . . . . ? C12 C13 C14 C15 -177.4(5) . . . . ? N3 C14 C15 C16 -1.1(8) . . . . ? C13 C14 C15 C16 175.7(5) . . . . ? N3 C14 C15 C39 177.7(4) . . . . ? C13 C14 C15 C39 -5.5(7) . . . . ? C19 N4 C16 C15 178.0(5) . . . . ? Zn1 N4 C16 C15 13.1(7) . . . . ? C19 N4 C16 C17 -0.1(5) . . . . ? Zn1 N4 C16 C17 -164.9(3) . . . . ? C14 C15 C16 N4 -1.6(8) . . . . ? C39 C15 C16 N4 179.6(4) . . . . ? C14 C15 C16 C17 176.1(5) . . . . ? C39 C15 C16 C17 -2.7(7) . . . . ? N4 C16 C17 C18 0.0(6) . . . . ? C15 C16 C17 C18 -178.1(5) . . . . ? C16 C17 C18 C19 0.1(6) . . . . ? C16 N4 C19 C20 -178.4(5) . . . . ? Zn1 N4 C19 C20 -13.5(7) . . . . ? C16 N4 C19 C18 0.1(5) . . . . ? Zn1 N4 C19 C18 165.0(3) . . . . ? C17 C18 C19 N4 -0.1(6) . . . . ? C17 C18 C19 C20 178.4(5) . . . . ? N1 C1 C20 C19 -2.2(9) . . . . ? C2 C1 C20 C19 178.1(5) . . . . ? N1 C1 C20 C21 177.5(5) . . . . ? C2 C1 C20 C21 -2.2(8) . . . . ? N4 C19 C20 C1 2.7(8) . . . . ? C18 C19 C20 C1 -175.6(5) . . . . ? N4 C19 C20 C21 -177.0(4) . . . . ? C18 C19 C20 C21 4.7(7) . . . . ? C1 C20 C21 C22 -105.1(6) . . . . ? C19 C20 C21 C22 74.6(6) . . . . ? C1 C20 C21 C26 73.1(7) . . . . ? C19 C20 C21 C26 -107.2(6) . . . . ? C26 C21 C22 C23 -1.6(9) . . . . ? C20 C21 C22 C23 176.7(5) . . . . ? C21 C22 C23 C24 -1.0(10) . . . . ? C22 C23 C24 C25 2.6(10) . . . . ? C22 C23 C24 C45 -174.6(6) . . . . ? C23 C24 C25 C26 -1.6(11) . . . . ? C45 C24 C25 C26 175.7(7) . . . . ? C24 C25 C26 C21 -1.0(12) . . . . ? C22 C21 C26 C25 2.6(10) . . . . ? C20 C21 C26 C25 -175.6(6) . . . . ? C11 C10 C27 C32 120.0(5) . . . . ? C9 C10 C27 C32 -60.9(6) . . . . ? C11 C10 C27 C28 -62.0(6) . . . . ? C9 C10 C27 C28 117.1(5) . . . . ? C32 C27 C28 C29 1.1(7) . . . . ? C10 C27 C28 C29 -176.9(4) . . . . ? C27 C28 C29 C30 -0.6(8) . . . . ? C28 C29 C30 C31 -0.3(8) . . . . ? C28 C29 C30 N5 -179.3(5) . . . . ? O3 N5 C30 C31 1.1(8) . . . . ? O4 N5 C30 C31 -176.8(6) . . . . ? O3 N5 C30 C29 -179.8(5) . . . . ? O4 N5 C30 C29 2.3(8) . . . . ? C29 C30 C31 C32 0.8(8) . . . . ? N5 C30 C31 C32 179.8(5) . . . . ? C30 C31 C32 C27 -0.3(7) . . . . ? C28 C27 C32 C31 -0.6(7) . . . . ? C10 C27 C32 C31 177.4(4) . . . . ? C6 C5 C33 C34 69.7(7) . . . . ? C4 C5 C33 C34 -112.0(7) . . . . ? C6 C5 C33 C38 -122.2(6) . . . . ? C4 C5 C33 C38 56.1(7) . . . . ? C6 C5 C33 C38X -66.5(11) . . . . ? C4 C5 C33 C38X 111.9(10) . . . . ? C38 C33 C34 C35 12.0(9) . . . . ? C38X C33 C34 C35 -42.0(11) . . . . ? C5 C33 C34 C35 -179.4(5) . . . . ? C33 C34 C35 C36 -9.4(10) . . . . ? C33 C34 C35 C36X 28.7(14) . . . . ? C45 O2 C46 C46 -154(2) . . . 2_455 ? C34 C35 C36 C37 2.9(11) . . . . ? C36X C35 C36 C37 -90.0(19) . . . . ? C35 C36 C37 C38 0.2(12) . . . . ? C36 C37 C38 C33 2.9(11) . . . . ? C34 C33 C38 C37 -8.8(10) . . . . ? C38X C33 C38 C37 86.2(11) . . . . ? C5 C33 C38 C37 -177.5(6) . . . . ? C50 C51 C52 C53 -31.9(16) . . . . ? C36 C35 C36X C37X 100(3) . . . . ? C34 C35 C36X C37X -6(3) . . . . ? C35 C36X C37X C38X 1(3) . . . . ? C36X C37X C38X C33 -16(3) . . . . ? C34 C33 C38X C37X 35.1(19) . . . . ? C38 C33 C38X C37X -72.8(16) . . . . ? C5 C33 C38X C37X 176.3(14) . . . . ? C50 C51X C52X C53 -8(4) . . . . ? C50 C51Y C52Y C53 -10(3) . . . . ? C16 C15 C39 C40 -64.9(6) . . . . ? C14 C15 C39 C40 116.2(5) . . . . ? C16 C15 C39 C44 113.4(5) . . . . ? C14 C15 C39 C44 -65.5(6) . . . . ? C44 C39 C40 C41 -0.1(7) . . . . ? C15 C39 C40 C41 178.1(5) . . . . ? C39 C40 C41 C42 -0.5(8) . . . . ? C40 C41 C42 C43 0.7(8) . . . . ? C41 C42 C43 C44 -0.3(8) . . . . ? C42 C43 C44 C39 -0.3(8) . . . . ? C40 C39 C44 C43 0.5(7) . . . . ? C15 C39 C44 C43 -177.7(5) . . . . ? C46Y O1 C45 O2 17(4) . . . . ? C46Y O1 C45 C24 -160(4) . . . . ? C46 O2 C45 O1 -2.0(12) . . . . ? C46 O2 C45 C24 175.2(7) . . . . ? C25 C24 C45 O1 -0.5(10) . . . . ? C23 C24 C45 O1 176.8(7) . . . . ? C25 C24 C45 O2 -177.7(7) . . . . ? C23 C24 C45 O2 -0.5(10) . . . . ? C52X C51X C50 O5 28(3) . . . . ? C52X C51X C50 C51Y -72(3) . . . . ? C52X C51X C50 C51 -62(3) . . . . ? C53 O5 C50 C51X -41(2) . . . . ? Zn1 O5 C50 C51X 112(2) . . . . ? C53 O5 C50 C51Y 33.0(19) . . . . ? Zn1 O5 C50 C51Y -174.1(18) . . . . ? C53 O5 C50 C51 -6.0(10) . . . . ? Zn1 O5 C50 C51 146.9(8) . . . . ? C52Y C51Y C50 C51X 92(3) . . . . ? C52Y C51Y C50 O5 -13(3) . . . . ? C52Y C51Y C50 C51 83(3) . . . . ? C52 C51 C50 C51X 124(3) . . . . ? C52 C51 C50 O5 23.7(14) . . . . ? C52 C51 C50 C51Y -71(2) . . . . ? C50 O5 C53 C52 -15.0(11) . . . . ? Zn1 O5 C53 C52 -167.4(9) . . . . ? C50 O5 C53 C52Y -38.4(12) . . . . ? Zn1 O5 C53 C52Y 169.2(11) . . . . ? C50 O5 C53 C52X 31.2(18) . . . . ? Zn1 O5 C53 C52X -121.2(17) . . . . ? C51 C52 C53 O5 30.0(15) . . . . ? C51 C52 C53 C52Y 105(4) . . . . ? C51 C52 C53 C52X -53.2(18) . . . . ? C51Y C52Y C53 O5 29(2) . . . . ? C51Y C52Y C53 C52 -83(4) . . . . ? C51Y C52Y C53 C52X -66(2) . . . . ? C51X C52X C53 O5 -14(3) . . . . ? C51X C52X C53 C52 95(3) . . . . ? C51X C52X C53 C52Y 85(3) . . . . ? C60 O6 C63 C62X 25(2) . . . . ? C60X O6 C63 C62X -6(2) . . . . ? C60 O6 C63 C62 19.5(16) . . . . ? C60X O6 C63 C62 -11.1(15) . . . . ? C60 O6 C63 C60X 30.6(14) . . . . ? C63 O6 C60 C61 -33(2) . . . . ? C60X O6 C60 C61 29(3) . . . . ? O6 C60 C61 C62 29(3) . . . . ? C60 C61 C62 C63 -16(3) . . . . ? O6 C63 C62 C61 -1.4(19) . . . . ? C62X C63 C62 C61 -171(4) . . . . ? C60X C63 C62 C61 -11.7(18) . . . . ? C63 O6 C60X C61X 8(3) . . . . ? C60 O6 C60X C61X -116(4) . . . . ? C60 O6 C60X C63 -124(3) . . . . ? C62X C63 C60X O6 175(2) . . . . ? C62 C63 C60X O6 166.3(18) . . . . ? O6 C63 C60X C61X -172(3) . . . . ? C62X C63 C60X C61X 3(3) . . . . ? C62 C63 C60X C61X -6(2) . . . . ? O6 C60X C61X C62X -9(5) . . . . ? C63 C60X C61X C62X -3(4) . . . . ? C60X C61X C62X C63 4(5) . . . . ? O6 C63 C62X C61X 1(4) . . . . ? C62 C63 C62X C61X 13(3) . . . . ? C60X C63 C62X C61X -3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 32.20 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.902 _refine_diff_density_min -1.538 _refine_diff_density_rms 0.156 #===END data_cu92 _database_code_depnum_ccdc_archive 'CCDC 659521' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [5-(4-nitrophenyl)-15-(carbomethoxyphenyl)-10,20-bis(phenyl)porphyrinato] copper(II) ; _chemical_name_common ; (5-(4-nitrophenyl)-15-(carbomethoxyphenyl)-10,20- bis(phenyl)porphyrinato) copper(ii) ; _chemical_melting_point 205 _chemical_formula_moiety 'C46 H29 Cu N5 O4, 0.125(C8 O2)' _chemical_formula_sum 'C47 H29 Cu N5 O4.25' _chemical_formula_weight 795.29 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' Cu Cu 0.3201 1.2651 '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' _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 10.0786(8) _cell_length_b 12.1933(10) _cell_length_c 16.6574(13) _cell_angle_alpha 68.8270(10) _cell_angle_beta 75.0110(10) _cell_angle_gamma 82.700(2) _cell_volume 1842.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_absorpt_coefficient_mu 0.648 _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 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart1000' _diffrn_measurement_method 'O-Scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7266 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.02 _reflns_number_total 7261 _reflns_number_gt 4846 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1185P)^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 7261 _refine_ls_number_parameters 509 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.2065 _refine_ls_wR_factor_gt 0.1886 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.07015(5) 0.14674(5) 0.04577(3) 0.0164(2) Uani 1 1 d . . . O1 O 0.2905(5) 0.0639(5) -0.5450(3) 0.0577(13) Uani 1 1 d . . . O2 O 0.4710(5) 0.1622(5) -0.5572(3) 0.0658(15) Uani 1 1 d . . . O3 O -0.1086(8) 0.3273(6) 0.5925(4) 0.104(2) Uani 1 1 d . . . O4 O 0.0939(8) 0.3920(5) 0.5343(4) 0.085(2) Uani 1 1 d . . . N1 N 0.0157(4) 0.2321(3) -0.0682(2) 0.0177(8) Uani 1 1 d . . . N2 N -0.0471(4) 0.2602(3) 0.0977(2) 0.0177(8) Uani 1 1 d . . . N3 N 0.1404(4) 0.0716(3) 0.1561(2) 0.0177(8) Uani 1 1 d . . . N4 N 0.1883(4) 0.0332(3) -0.0063(2) 0.0157(8) Uani 1 1 d . . . N5 N -0.0036(9) 0.3437(5) 0.5348(4) 0.069(2) Uani 1 1 d . . . C1 C 0.0703(4) 0.2146(4) -0.1484(3) 0.0188(10) Uani 1 1 d . . . C2 C 0.0240(5) 0.3073(4) -0.2182(3) 0.0247(11) Uani 1 1 d . . . H2 H 0.0495 0.3169 -0.2793 0.034(3) Uiso 1 1 calc R . . C3 C -0.0624(5) 0.3779(4) -0.1811(3) 0.0229(10) Uani 1 1 d . . . H3 H -0.1108 0.4461 -0.2112 0.034(3) Uiso 1 1 calc R . . C4 C -0.0685(4) 0.3323(4) -0.0880(3) 0.0181(9) Uani 1 1 d . . . C5 C -0.1468(4) 0.3846(4) -0.0278(3) 0.0181(10) Uani 1 1 d . . . C6 C -0.1350(4) 0.3490(4) 0.0591(3) 0.0190(10) Uani 1 1 d . . . C7 C -0.2041(5) 0.4063(4) 0.1209(3) 0.0229(10) Uani 1 1 d . . . H7 H -0.2727 0.4677 0.1118 0.034(3) Uiso 1 1 calc R . . C8 C -0.1541(5) 0.3575(5) 0.1942(3) 0.0255(11) Uani 1 1 d . . . H8 H -0.1787 0.3799 0.2453 0.034(3) Uiso 1 1 calc R . . C9 C -0.0569(5) 0.2654(4) 0.1806(3) 0.0198(10) Uani 1 1 d . . . C10 C 0.0227(5) 0.1999(4) 0.2394(3) 0.0205(10) Uani 1 1 d . . . C11 C 0.1154(5) 0.1101(4) 0.2272(3) 0.0225(10) Uani 1 1 d . . . C12 C 0.1967(5) 0.0417(4) 0.2873(3) 0.0246(11) Uani 1 1 d . . . H12 H 0.1995 0.0518 0.3408 0.034(3) Uiso 1 1 calc R . . C13 C 0.2688(5) -0.0395(4) 0.2551(3) 0.0241(11) Uani 1 1 d . . . H13 H 0.3317 -0.0976 0.2816 0.034(3) Uiso 1 1 calc R . . C14 C 0.2337(4) -0.0226(4) 0.1735(3) 0.0197(10) Uani 1 1 d . . . C15 C 0.2889(4) -0.0897(4) 0.1193(3) 0.0173(9) Uani 1 1 d . . . C16 C 0.2636(4) -0.0626(4) 0.0352(3) 0.0161(9) Uani 1 1 d . . . C17 C 0.3230(5) -0.1280(4) -0.0230(3) 0.0181(9) Uani 1 1 d . . . H17 H 0.3769 -0.1993 -0.0092 0.034(3) Uiso 1 1 calc R . . C18 C 0.2878(5) -0.0696(4) -0.1004(3) 0.0212(10) Uani 1 1 d . . . H18 H 0.3124 -0.0916 -0.1516 0.034(3) Uiso 1 1 calc R . . C19 C 0.2059(4) 0.0325(4) -0.0910(3) 0.0182(10) Uani 1 1 d . . . C20 C 0.1580(5) 0.1187(4) -0.1583(3) 0.0203(10) Uani 1 1 d . . . C21 C 0.2090(5) 0.1157(4) -0.2508(3) 0.0200(10) Uani 1 1 d . . . C22 C 0.3470(5) 0.1300(5) -0.2921(3) 0.0324(13) Uani 1 1 d . . . H22 H 0.4084 0.1409 -0.2611 0.034(3) Uiso 1 1 calc R . . C23 C 0.3976(5) 0.1289(6) -0.3772(4) 0.0387(14) Uani 1 1 d . . . H23 H 0.4920 0.1412 -0.4052 0.034(3) Uiso 1 1 calc R . . C24 C 0.3085(5) 0.1095(5) -0.4211(3) 0.0293(12) Uani 1 1 d . . . C25 C 0.1711(5) 0.0927(4) -0.3811(3) 0.0265(11) Uani 1 1 d . . . H25 H 0.1108 0.0782 -0.4113 0.034(3) Uiso 1 1 calc R . . C26 C 0.1210(5) 0.0970(4) -0.2956(3) 0.0238(10) Uani 1 1 d . . . H26 H 0.0260 0.0870 -0.2683 0.034(3) Uiso 1 1 calc R . . C27 C 0.0156(5) 0.2342(4) 0.3184(3) 0.0226(10) Uani 1 1 d . . . C28 C 0.1148(6) 0.3040(5) 0.3158(3) 0.0290(11) Uani 1 1 d . . . H28 H 0.1880 0.3280 0.2649 0.034(3) Uiso 1 1 calc R . . C29 C 0.1088(7) 0.3395(5) 0.3869(4) 0.0404(14) Uani 1 1 d . . . H29 H 0.1773 0.3876 0.3852 0.034(3) Uiso 1 1 calc R . . C30 C 0.0031(7) 0.3044(5) 0.4590(4) 0.0406(15) Uani 1 1 d . . . C31 C -0.0948(8) 0.2330(6) 0.4658(4) 0.0499(17) Uani 1 1 d . . . H31 H -0.1654 0.2072 0.5182 0.034(3) Uiso 1 1 calc R . . C32 C -0.0891(6) 0.1981(5) 0.3936(4) 0.0407(14) Uani 1 1 d . . . H32 H -0.1576 0.1493 0.3963 0.034(3) Uiso 1 1 calc R . . C33 C -0.2448(4) 0.4848(4) -0.0602(3) 0.0182(10) Uani 1 1 d . . . C34 C -0.2390(5) 0.5934(4) -0.0527(3) 0.0227(10) Uani 1 1 d . . . H34 H -0.1701 0.6059 -0.0276 0.034(3) Uiso 1 1 calc R . . C35 C -0.3319(5) 0.6837(4) -0.0809(3) 0.0247(11) Uani 1 1 d . . . H35 H -0.3283 0.7569 -0.0736 0.034(3) Uiso 1 1 calc R . . C36 C -0.4302(5) 0.6682(4) -0.1198(3) 0.0257(11) Uani 1 1 d . . . H36 H -0.4943 0.7303 -0.1393 0.034(3) Uiso 1 1 calc R . . C37 C -0.4342(5) 0.5617(4) -0.1301(3) 0.0230(10) Uani 1 1 d . . . H37 H -0.4997 0.5514 -0.1586 0.034(3) Uiso 1 1 calc R . . C38 C -0.3446(4) 0.4698(4) -0.0997(3) 0.0203(10) Uani 1 1 d . . . H38 H -0.3508 0.3961 -0.1055 0.034(3) Uiso 1 1 calc R . . C39 C 0.3844(5) -0.1914(4) 0.1520(3) 0.0197(10) Uani 1 1 d . . . C40 C 0.3383(5) -0.2820(4) 0.2307(3) 0.0239(11) Uani 1 1 d . . . H40 H 0.2451 -0.2812 0.2621 0.034(3) Uiso 1 1 calc R . . C41 C 0.4281(6) -0.3739(5) 0.2638(4) 0.0302(12) Uani 1 1 d . . . H41 H 0.3965 -0.4351 0.3182 0.034(3) Uiso 1 1 calc R . . C42 C 0.5633(5) -0.3766(5) 0.2177(4) 0.0306(12) Uani 1 1 d . . . H42 H 0.6245 -0.4396 0.2403 0.034(3) Uiso 1 1 calc R . . C43 C 0.6090(5) -0.2874(5) 0.1388(3) 0.0264(11) Uani 1 1 d . . . H43 H 0.7013 -0.2897 0.1064 0.034(3) Uiso 1 1 calc R . . C44 C 0.5206(5) -0.1947(4) 0.1067(3) 0.0216(10) Uani 1 1 d . . . H44 H 0.5534 -0.1326 0.0531 0.034(3) Uiso 1 1 calc R . . C45 C 0.3546(6) 0.1081(6) -0.5130(4) 0.0395(14) Uani 1 1 d . . . C46 C 0.5116(9) 0.1792(7) -0.6546(4) 0.083(3) Uani 1 1 d . . . H46A H 0.4941 0.1076 -0.6633 0.125 Uiso 1 1 calc R . . H46B H 0.6096 0.1956 -0.6771 0.125 Uiso 1 1 calc R . . H46C H 0.4576 0.2455 -0.6865 0.125 Uiso 1 1 calc R . . O90 O 0.3976(12) -0.5319(8) 0.5251(4) 0.068(6) Uiso 0.25 1 d PRD . . C92 C 0.4289(11) -0.4006(10) 0.5535(4) 0.072(5) Uiso 0.25 1 d PRD . . C91 C 0.3491(11) -0.4330(9) 0.6168(4) 0.072(5) Uiso 0.25 1 d PRD . . C90 C 0.2876(13) -0.5239(8) 0.6019(4) 0.072(5) Uiso 0.25 1 d PRD . . C93 C 0.4923(11) -0.4654(9) 0.5114(4) 0.072(5) Uiso 0.25 1 d PRD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0166(3) 0.0226(3) 0.0142(3) -0.0106(2) -0.0048(2) -0.0004(2) O1 0.064(3) 0.090(4) 0.039(3) -0.043(3) -0.019(2) 0.006(3) O2 0.062(3) 0.118(5) 0.025(2) -0.038(3) 0.005(2) -0.019(3) O3 0.177(7) 0.099(5) 0.026(3) -0.035(3) 0.020(4) -0.016(5) O4 0.173(7) 0.053(3) 0.063(4) -0.035(3) -0.066(4) 0.005(4) N1 0.0179(18) 0.024(2) 0.018(2) -0.0133(17) -0.0070(15) 0.0014(16) N2 0.0167(18) 0.024(2) 0.016(2) -0.0103(17) -0.0072(15) 0.0002(16) N3 0.0194(19) 0.023(2) 0.016(2) -0.0130(17) -0.0046(15) 0.0003(16) N4 0.0178(18) 0.020(2) 0.0118(19) -0.0080(16) -0.0029(15) -0.0033(15) N5 0.140(7) 0.042(4) 0.032(3) -0.021(3) -0.026(4) 0.008(4) C1 0.016(2) 0.029(3) 0.016(2) -0.013(2) -0.0044(18) -0.0026(19) C2 0.026(2) 0.034(3) 0.017(2) -0.012(2) -0.007(2) 0.003(2) C3 0.022(2) 0.026(3) 0.025(3) -0.010(2) -0.012(2) 0.004(2) C4 0.017(2) 0.023(2) 0.019(2) -0.010(2) -0.0071(18) -0.0022(18) C5 0.015(2) 0.022(2) 0.022(2) -0.012(2) -0.0067(18) -0.0013(18) C6 0.012(2) 0.027(3) 0.022(2) -0.013(2) -0.0029(18) -0.0009(18) C7 0.021(2) 0.029(3) 0.021(3) -0.013(2) -0.0046(19) 0.005(2) C8 0.029(3) 0.036(3) 0.015(2) -0.015(2) -0.004(2) 0.002(2) C9 0.020(2) 0.027(3) 0.016(2) -0.012(2) -0.0021(18) -0.0005(19) C10 0.025(2) 0.024(3) 0.015(2) -0.011(2) -0.0026(19) -0.0025(19) C11 0.028(2) 0.028(3) 0.018(2) -0.014(2) -0.006(2) -0.003(2) C12 0.028(3) 0.030(3) 0.023(3) -0.015(2) -0.011(2) 0.001(2) C13 0.025(2) 0.031(3) 0.023(3) -0.014(2) -0.013(2) 0.003(2) C14 0.017(2) 0.026(3) 0.018(2) -0.009(2) -0.0044(18) -0.0020(19) C15 0.015(2) 0.024(2) 0.016(2) -0.0091(19) -0.0032(17) -0.0033(18) C16 0.015(2) 0.018(2) 0.018(2) -0.0088(19) -0.0023(18) -0.0026(17) C17 0.022(2) 0.018(2) 0.019(2) -0.0108(19) -0.0060(19) 0.0000(18) C18 0.022(2) 0.025(3) 0.021(3) -0.014(2) -0.0043(19) -0.0010(19) C19 0.015(2) 0.025(3) 0.017(2) -0.010(2) -0.0018(18) -0.0043(18) C20 0.018(2) 0.032(3) 0.016(2) -0.015(2) -0.0021(18) -0.003(2) C21 0.025(2) 0.022(2) 0.016(2) -0.011(2) -0.0070(19) 0.0042(19) C22 0.023(2) 0.056(4) 0.026(3) -0.022(3) -0.007(2) 0.000(2) C23 0.023(3) 0.070(4) 0.028(3) -0.024(3) -0.004(2) 0.002(3) C24 0.038(3) 0.034(3) 0.020(3) -0.015(2) -0.010(2) 0.010(2) C25 0.038(3) 0.030(3) 0.021(3) -0.015(2) -0.014(2) 0.003(2) C26 0.028(2) 0.026(3) 0.022(3) -0.013(2) -0.009(2) 0.000(2) C27 0.029(3) 0.027(3) 0.016(2) -0.013(2) -0.008(2) 0.007(2) C28 0.037(3) 0.029(3) 0.025(3) -0.014(2) -0.009(2) -0.001(2) C29 0.064(4) 0.028(3) 0.041(4) -0.017(3) -0.027(3) 0.000(3) C30 0.078(4) 0.031(3) 0.019(3) -0.015(2) -0.016(3) 0.011(3) C31 0.079(5) 0.046(4) 0.020(3) -0.018(3) 0.006(3) -0.005(3) C32 0.050(4) 0.045(4) 0.030(3) -0.021(3) 0.003(3) -0.010(3) C33 0.018(2) 0.024(2) 0.014(2) -0.0101(19) -0.0012(18) -0.0001(18) C34 0.019(2) 0.027(3) 0.023(3) -0.011(2) -0.0012(19) -0.007(2) C35 0.032(3) 0.018(2) 0.023(3) -0.009(2) 0.001(2) -0.005(2) C36 0.028(3) 0.026(3) 0.021(3) -0.011(2) -0.002(2) 0.007(2) C37 0.022(2) 0.029(3) 0.022(3) -0.012(2) -0.006(2) 0.001(2) C38 0.020(2) 0.026(3) 0.017(2) -0.010(2) -0.0028(18) -0.0022(19) C39 0.021(2) 0.024(3) 0.021(2) -0.014(2) -0.0089(19) 0.0008(19) C40 0.024(2) 0.031(3) 0.022(3) -0.014(2) -0.008(2) -0.002(2) C41 0.044(3) 0.027(3) 0.026(3) -0.012(2) -0.016(2) 0.002(2) C42 0.034(3) 0.027(3) 0.041(3) -0.018(3) -0.022(2) 0.010(2) C43 0.020(2) 0.036(3) 0.033(3) -0.022(2) -0.010(2) 0.003(2) C44 0.025(2) 0.025(3) 0.024(3) -0.017(2) -0.009(2) -0.001(2) C45 0.041(3) 0.056(4) 0.023(3) -0.021(3) -0.007(3) 0.015(3) C46 0.096(6) 0.113(7) 0.025(4) -0.015(4) -0.004(4) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.989(4) . ? Cu1 N2 1.995(4) . ? Cu1 N4 2.001(4) . ? Cu1 N3 2.002(4) . ? O1 C45 1.210(7) . ? O2 C45 1.323(8) . ? O2 C46 1.508(7) . ? O3 N5 1.213(9) . ? O4 N5 1.206(9) . ? N1 C4 1.383(6) . ? N1 C1 1.388(6) . ? N2 C9 1.383(6) . ? N2 C6 1.385(6) . ? N3 C11 1.380(6) . ? N3 C14 1.383(6) . ? N4 C16 1.371(6) . ? N4 C19 1.379(6) . ? N5 C30 1.488(8) . ? C1 C20 1.406(6) . ? C1 C2 1.430(7) . ? C2 C3 1.340(7) . ? C2 H2 0.9500 . ? C3 C4 1.434(7) . ? C3 H3 0.9500 . ? C4 C5 1.400(6) . ? C5 C6 1.386(6) . ? C5 C33 1.500(6) . ? C6 C7 1.434(6) . ? C7 C8 1.347(7) . ? C7 H7 0.9500 . ? C8 C9 1.436(6) . ? C8 H8 0.9500 . ? C9 C10 1.385(6) . ? C10 C11 1.384(7) . ? C10 C27 1.501(6) . ? C11 C12 1.420(7) . ? C12 C13 1.340(7) . ? C12 H12 0.9500 . ? C13 C14 1.429(6) . ? C13 H13 0.9500 . ? C14 C15 1.398(6) . ? C15 C16 1.402(6) . ? C15 C39 1.497(6) . ? C16 C17 1.439(6) . ? C17 C18 1.343(6) . ? C17 H17 0.9500 . ? C18 C19 1.438(6) . ? C18 H18 0.9500 . ? C19 C20 1.377(7) . ? C20 C21 1.505(6) . ? C21 C26 1.384(6) . ? C21 C22 1.385(7) . ? C22 C23 1.382(7) . ? C22 H22 0.9500 . ? C23 C24 1.384(7) . ? C23 H23 0.9500 . ? C24 C25 1.379(7) . ? C24 C45 1.486(7) . ? C25 C26 1.399(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.375(7) . ? C27 C32 1.384(7) . ? C28 C29 1.386(7) . ? C28 H28 0.9500 . ? C29 C30 1.357(9) . ? C29 H29 0.9500 . ? C30 C31 1.354(9) . ? C31 C32 1.399(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.385(7) . ? C33 C38 1.397(6) . ? C34 C35 1.380(7) . ? C34 H34 0.9500 . ? C35 C36 1.380(7) . ? C35 H35 0.9500 . ? C36 C37 1.377(7) . ? C36 H36 0.9500 . ? C37 C38 1.377(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.387(7) . ? C39 C44 1.389(6) . ? C40 C41 1.391(7) . ? C40 H40 0.9500 . ? C41 C42 1.383(8) . ? C41 H41 0.9500 . ? C42 C43 1.381(8) . ? C42 H42 0.9500 . ? C43 C44 1.381(7) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? O90 C93 1.12(2) 2_646 ? O90 C93 1.2535 . ? O90 C90 1.4847 . ? O90 C92 1.908(2) . ? C92 C91 1.1206 . ? C92 C93 1.2511 . ? C92 C90 2.0029(12) . ? C91 C90 1.4576(14) . ? C93 C93 1.02(2) 2_646 ? C93 O90 1.122(18) 2_646 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N2 89.61(15) . . ? N1 Cu1 N4 90.46(15) . . ? N2 Cu1 N4 179.78(15) . . ? N1 Cu1 N3 174.32(15) . . ? N2 Cu1 N3 90.33(15) . . ? N4 Cu1 N3 89.57(15) . . ? C45 O2 C46 115.7(6) . . ? C4 N1 C1 105.0(4) . . ? C4 N1 Cu1 127.3(3) . . ? C1 N1 Cu1 127.0(3) . . ? C9 N2 C6 106.0(4) . . ? C9 N2 Cu1 126.4(3) . . ? C6 N2 Cu1 127.6(3) . . ? C11 N3 C14 105.5(4) . . ? C11 N3 Cu1 126.8(3) . . ? C14 N3 Cu1 127.4(3) . . ? C16 N4 C19 105.7(4) . . ? C16 N4 Cu1 127.6(3) . . ? C19 N4 Cu1 126.7(3) . . ? O4 N5 O3 124.0(7) . . ? O4 N5 C30 118.2(7) . . ? O3 N5 C30 117.8(8) . . ? N1 C1 C20 124.2(4) . . ? N1 C1 C2 110.3(4) . . ? C20 C1 C2 125.5(4) . . ? C3 C2 C1 107.1(4) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 107.8(4) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? N1 C4 C5 126.1(4) . . ? N1 C4 C3 109.8(4) . . ? C5 C4 C3 124.0(4) . . ? C6 C5 C4 122.6(4) . . ? C6 C5 C33 119.4(4) . . ? C4 C5 C33 118.0(4) . . ? N2 C6 C5 125.9(4) . . ? N2 C6 C7 109.3(4) . . ? C5 C6 C7 124.6(4) . . ? C8 C7 C6 107.8(4) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? C7 C8 C9 107.2(4) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N2 C9 C10 126.0(4) . . ? N2 C9 C8 109.6(4) . . ? C10 C9 C8 124.2(4) . . ? C11 C10 C9 124.5(4) . . ? C11 C10 C27 117.6(4) . . ? C9 C10 C27 117.8(4) . . ? N3 C11 C10 125.3(4) . . ? N3 C11 C12 109.8(4) . . ? C10 C11 C12 124.9(4) . . ? C13 C12 C11 107.8(4) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 107.3(4) . . ? C12 C13 H13 126.3 . . ? C14 C13 H13 126.3 . . ? N3 C14 C15 125.8(4) . . ? N3 C14 C13 109.5(4) . . ? C15 C14 C13 124.7(4) . . ? C14 C15 C16 123.1(4) . . ? C14 C15 C39 117.5(4) . . ? C16 C15 C39 119.4(4) . . ? N4 C16 C15 125.8(4) . . ? N4 C16 C17 110.0(4) . . ? C15 C16 C17 124.0(4) . . ? C18 C17 C16 107.2(4) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 107.1(4) . . ? C17 C18 H18 126.4 . . ? C19 C18 H18 126.4 . . ? C20 C19 N4 125.6(4) . . ? C20 C19 C18 124.5(4) . . ? N4 C19 C18 109.9(4) . . ? C19 C20 C1 124.9(4) . . ? C19 C20 C21 118.3(4) . . ? C1 C20 C21 116.7(4) . . ? C26 C21 C22 118.7(4) . . ? C26 C21 C20 121.4(4) . . ? C22 C21 C20 119.9(4) . . ? C23 C22 C21 121.7(5) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 119.0(5) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 120.6(5) . . ? C25 C24 C45 117.1(5) . . ? C23 C24 C45 122.2(5) . . ? C24 C25 C26 119.6(5) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C21 C26 C25 120.4(5) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C32 119.1(5) . . ? C28 C27 C10 119.4(4) . . ? C32 C27 C10 121.5(5) . . ? C27 C28 C29 120.6(5) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 118.8(6) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C31 C30 C29 122.9(5) . . ? C31 C30 N5 118.5(6) . . ? C29 C30 N5 118.6(6) . . ? C30 C31 C32 118.1(6) . . ? C30 C31 H31 120.9 . . ? C32 C31 H31 120.9 . . ? C27 C32 C31 120.5(6) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C38 118.3(4) . . ? C34 C33 C5 121.7(4) . . ? C38 C33 C5 120.0(4) . . ? C35 C34 C33 121.0(4) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 120.3(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C37 C36 C35 119.2(4) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C38 C37 C36 121.0(4) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C33 120.2(4) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? C40 C39 C44 119.0(4) . . ? C40 C39 C15 119.8(4) . . ? C44 C39 C15 121.1(4) . . ? C39 C40 C41 120.1(5) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 120.2(5) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 119.7(5) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.1(5) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 120.7(5) . . ? C43 C44 H44 119.6 . . ? C39 C44 H44 119.6 . . ? O1 C45 O2 123.2(5) . . ? O1 C45 C24 123.2(6) . . ? O2 C45 C24 113.5(5) . . ? O2 C46 H46A 109.5 . . ? O2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C93 O90 C93 50.7(12) 2_646 . ? C93 O90 C90 153.3(9) 2_646 . ? C93 O90 C90 109.6 . . ? C93 O90 C92 91.0(12) 2_646 . ? C93 O90 C92 40.3 . . ? C90 O90 C92 71.1 . . ? C91 C92 C93 123.44(8) . . ? C91 C92 O90 89.0 . . ? C93 C92 O90 40.43(5) . . ? C91 C92 C90 45.6 . . ? C93 C92 C90 83.69(11) . . ? O90 C92 C90 44.54(5) . . ? C92 C91 C90 101.1 . . ? C91 C90 O90 96.5 . . ? C91 C90 C92 33.3 . . ? O90 C90 C92 64.33(5) . . ? C93 C93 O90 71.3(9) 2_646 2_646 ? C93 C93 C92 157.1(13) 2_646 . ? O90 C93 C92 131.4(13) 2_646 . ? C93 C93 O90 58.0(14) 2_646 . ? O90 C93 O90 129.3(13) 2_646 . ? C92 C93 O90 99.24(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 N1 C4 2.0(4) . . . . ? N4 Cu1 N1 C4 -177.8(4) . . . . ? N3 Cu1 N1 C4 -87.5(15) . . . . ? N2 Cu1 N1 C1 171.4(4) . . . . ? N4 Cu1 N1 C1 -8.4(4) . . . . ? N3 Cu1 N1 C1 81.9(16) . . . . ? N1 Cu1 N2 C9 -174.5(4) . . . . ? N4 Cu1 N2 C9 -64(47) . . . . ? N3 Cu1 N2 C9 -0.2(4) . . . . ? N1 Cu1 N2 C6 5.8(4) . . . . ? N4 Cu1 N2 C6 116(47) . . . . ? N3 Cu1 N2 C6 -179.9(4) . . . . ? N1 Cu1 N3 C11 82.6(15) . . . . ? N2 Cu1 N3 C11 -6.9(4) . . . . ? N4 Cu1 N3 C11 172.9(4) . . . . ? N1 Cu1 N3 C14 -90.9(15) . . . . ? N2 Cu1 N3 C14 179.6(4) . . . . ? N4 Cu1 N3 C14 -0.6(4) . . . . ? N1 Cu1 N4 C16 -177.8(4) . . . . ? N2 Cu1 N4 C16 72(47) . . . . ? N3 Cu1 N4 C16 7.9(4) . . . . ? N1 Cu1 N4 C19 -0.9(4) . . . . ? N2 Cu1 N4 C19 -111(47) . . . . ? N3 Cu1 N4 C19 -175.2(4) . . . . ? C4 N1 C1 C20 -177.3(4) . . . . ? Cu1 N1 C1 C20 11.5(6) . . . . ? C4 N1 C1 C2 2.5(5) . . . . ? Cu1 N1 C1 C2 -168.8(3) . . . . ? N1 C1 C2 C3 -2.5(5) . . . . ? C20 C1 C2 C3 177.2(5) . . . . ? C1 C2 C3 C4 1.5(5) . . . . ? C1 N1 C4 C5 179.7(4) . . . . ? Cu1 N1 C4 C5 -9.1(7) . . . . ? C1 N1 C4 C3 -1.5(5) . . . . ? Cu1 N1 C4 C3 169.7(3) . . . . ? C2 C3 C4 N1 0.0(5) . . . . ? C2 C3 C4 C5 178.8(4) . . . . ? N1 C4 C5 C6 8.5(7) . . . . ? C3 C4 C5 C6 -170.1(4) . . . . ? N1 C4 C5 C33 -172.8(4) . . . . ? C3 C4 C5 C33 8.6(7) . . . . ? C9 N2 C6 C5 172.4(4) . . . . ? Cu1 N2 C6 C5 -7.8(7) . . . . ? C9 N2 C6 C7 -2.4(5) . . . . ? Cu1 N2 C6 C7 177.4(3) . . . . ? C4 C5 C6 N2 0.3(7) . . . . ? C33 C5 C6 N2 -178.4(4) . . . . ? C4 C5 C6 C7 174.4(4) . . . . ? C33 C5 C6 C7 -4.3(7) . . . . ? N2 C6 C7 C8 3.0(5) . . . . ? C5 C6 C7 C8 -171.9(5) . . . . ? C6 C7 C8 C9 -2.3(6) . . . . ? C6 N2 C9 C10 -173.6(5) . . . . ? Cu1 N2 C9 C10 6.6(7) . . . . ? C6 N2 C9 C8 1.0(5) . . . . ? Cu1 N2 C9 C8 -178.8(3) . . . . ? C7 C8 C9 N2 0.9(6) . . . . ? C7 C8 C9 C10 175.6(5) . . . . ? N2 C9 C10 C11 -6.9(8) . . . . ? C8 C9 C10 C11 179.2(5) . . . . ? N2 C9 C10 C27 168.4(4) . . . . ? C8 C9 C10 C27 -5.4(7) . . . . ? C14 N3 C11 C10 -176.8(5) . . . . ? Cu1 N3 C11 C10 8.6(7) . . . . ? C14 N3 C11 C12 1.8(5) . . . . ? Cu1 N3 C11 C12 -172.9(3) . . . . ? C9 C10 C11 N3 -1.1(8) . . . . ? C27 C10 C11 N3 -176.5(4) . . . . ? C9 C10 C11 C12 -179.4(5) . . . . ? C27 C10 C11 C12 5.2(7) . . . . ? N3 C11 C12 C13 -1.3(6) . . . . ? C10 C11 C12 C13 177.3(5) . . . . ? C11 C12 C13 C14 0.2(6) . . . . ? C11 N3 C14 C15 179.9(4) . . . . ? Cu1 N3 C14 C15 -5.5(7) . . . . ? C11 N3 C14 C13 -1.6(5) . . . . ? Cu1 N3 C14 C13 173.0(3) . . . . ? C12 C13 C14 N3 0.9(6) . . . . ? C12 C13 C14 C15 179.3(5) . . . . ? N3 C14 C15 C16 5.4(7) . . . . ? C13 C14 C15 C16 -172.8(4) . . . . ? N3 C14 C15 C39 -177.6(4) . . . . ? C13 C14 C15 C39 4.2(7) . . . . ? C19 N4 C16 C15 172.3(4) . . . . ? Cu1 N4 C16 C15 -10.3(6) . . . . ? C19 N4 C16 C17 -3.3(5) . . . . ? Cu1 N4 C16 C17 174.1(3) . . . . ? C14 C15 C16 N4 2.8(7) . . . . ? C39 C15 C16 N4 -174.1(4) . . . . ? C14 C15 C16 C17 177.8(4) . . . . ? C39 C15 C16 C17 0.9(7) . . . . ? N4 C16 C17 C18 2.2(5) . . . . ? C15 C16 C17 C18 -173.5(4) . . . . ? C16 C17 C18 C19 -0.2(5) . . . . ? C16 N4 C19 C20 -174.1(4) . . . . ? Cu1 N4 C19 C20 8.4(6) . . . . ? C16 N4 C19 C18 3.2(5) . . . . ? Cu1 N4 C19 C18 -174.3(3) . . . . ? C17 C18 C19 C20 175.5(4) . . . . ? C17 C18 C19 N4 -1.9(5) . . . . ? N4 C19 C20 C1 -7.6(7) . . . . ? C18 C19 C20 C1 175.5(4) . . . . ? N4 C19 C20 C21 168.5(4) . . . . ? C18 C19 C20 C21 -8.5(7) . . . . ? N1 C1 C20 C19 -2.9(7) . . . . ? C2 C1 C20 C19 177.5(5) . . . . ? N1 C1 C20 C21 -179.0(4) . . . . ? C2 C1 C20 C21 1.3(7) . . . . ? C19 C20 C21 C26 115.2(5) . . . . ? C1 C20 C21 C26 -68.4(6) . . . . ? C19 C20 C21 C22 -63.8(6) . . . . ? C1 C20 C21 C22 112.6(5) . . . . ? C26 C21 C22 C23 1.6(8) . . . . ? C20 C21 C22 C23 -179.3(5) . . . . ? C21 C22 C23 C24 -1.9(9) . . . . ? C22 C23 C24 C25 0.6(9) . . . . ? C22 C23 C24 C45 179.4(6) . . . . ? C23 C24 C25 C26 1.0(8) . . . . ? C45 C24 C25 C26 -177.9(5) . . . . ? C22 C21 C26 C25 0.0(7) . . . . ? C20 C21 C26 C25 -179.0(5) . . . . ? C24 C25 C26 C21 -1.3(7) . . . . ? C11 C10 C27 C28 78.4(6) . . . . ? C9 C10 C27 C28 -97.3(6) . . . . ? C11 C10 C27 C32 -102.2(6) . . . . ? C9 C10 C27 C32 82.1(6) . . . . ? C32 C27 C28 C29 -1.1(8) . . . . ? C10 C27 C28 C29 178.3(5) . . . . ? C27 C28 C29 C30 -0.1(8) . . . . ? C28 C29 C30 C31 2.1(9) . . . . ? C28 C29 C30 N5 -179.4(5) . . . . ? O4 N5 C30 C31 168.9(6) . . . . ? O3 N5 C30 C31 -12.6(9) . . . . ? O4 N5 C30 C29 -9.6(9) . . . . ? O3 N5 C30 C29 168.8(6) . . . . ? C29 C30 C31 C32 -2.6(10) . . . . ? N5 C30 C31 C32 178.9(6) . . . . ? C28 C27 C32 C31 0.5(9) . . . . ? C10 C27 C32 C31 -178.9(5) . . . . ? C30 C31 C32 C27 1.3(10) . . . . ? C6 C5 C33 C34 54.6(6) . . . . ? C4 C5 C33 C34 -124.2(5) . . . . ? C6 C5 C33 C38 -125.7(5) . . . . ? C4 C5 C33 C38 55.5(6) . . . . ? C38 C33 C34 C35 1.9(7) . . . . ? C5 C33 C34 C35 -178.4(4) . . . . ? C33 C34 C35 C36 -1.9(7) . . . . ? C34 C35 C36 C37 0.0(7) . . . . ? C35 C36 C37 C38 2.0(7) . . . . ? C36 C37 C38 C33 -2.1(7) . . . . ? C34 C33 C38 C37 0.1(7) . . . . ? C5 C33 C38 C37 -179.6(4) . . . . ? C14 C15 C39 C40 60.2(6) . . . . ? C16 C15 C39 C40 -122.8(5) . . . . ? C14 C15 C39 C44 -117.3(5) . . . . ? C16 C15 C39 C44 59.8(6) . . . . ? C44 C39 C40 C41 0.6(7) . . . . ? C15 C39 C40 C41 -176.9(4) . . . . ? C39 C40 C41 C42 -1.1(7) . . . . ? C40 C41 C42 C43 0.2(8) . . . . ? C41 C42 C43 C44 1.1(7) . . . . ? C42 C43 C44 C39 -1.6(7) . . . . ? C40 C39 C44 C43 0.7(7) . . . . ? C15 C39 C44 C43 178.2(4) . . . . ? C46 O2 C45 O1 7.3(9) . . . . ? C46 O2 C45 C24 -171.3(5) . . . . ? C25 C24 C45 O1 -20.0(8) . . . . ? C23 C24 C45 O1 161.1(6) . . . . ? C25 C24 C45 O2 158.6(5) . . . . ? C23 C24 C45 O2 -20.3(8) . . . . ? C93 O90 C92 C91 -148.3(7) 2_646 . . . ? C93 O90 C92 C91 -150.5 . . . . ? C90 O90 C92 C91 11.4 . . . . ? C93 O90 C92 C93 2.2(7) 2_646 . . . ? C90 O90 C92 C93 162.0 . . . . ? C93 O90 C92 C90 -159.8(7) 2_646 . . . ? C93 O90 C92 C90 -162.0 . . . . ? C93 C92 C91 C90 -33.7 . . . . ? O90 C92 C91 C90 -11.2 . . . . ? C92 C91 C90 O90 14.6 . . . . ? C93 O90 C90 C91 41(2) 2_646 . . . ? C93 O90 C90 C91 3.4 . . . . ? C92 O90 C90 C91 -8.8 . . . . ? C93 O90 C90 C92 50(2) 2_646 . . . ? C93 O90 C90 C92 12.3 . . . . ? C93 C92 C90 C91 152.2 . . . . ? O90 C92 C90 C91 163.9 . . . . ? C91 C92 C90 O90 -163.9 . . . . ? C93 C92 C90 O90 -11.6 . . . . ? C91 C92 C93 C93 29.9(19) . . . 2_646 ? O90 C92 C93 C93 -6.2(19) . . . 2_646 ? C90 C92 C93 C93 6.4(19) . . . 2_646 ? C91 C92 C93 O90 -141.0(9) . . . 2_646 ? O90 C92 C93 O90 -177.1(9) . . . 2_646 ? C90 C92 C93 O90 -164.5(9) . . . 2_646 ? C91 C92 C93 O90 36.1 . . . . ? C90 C92 C93 O90 12.6 . . . . ? C90 O90 C93 C93 159.1(9) . . . 2_646 ? C92 O90 C93 C93 177.1(9) . . . 2_646 ? C93 O90 C93 O90 0.0(3) 2_646 . . 2_646 ? C90 O90 C93 O90 159.1(9) . . . 2_646 ? C92 O90 C93 O90 177.1(9) . . . 2_646 ? C93 O90 C93 C92 -177.1(9) 2_646 . . . ? C90 O90 C93 C92 -18.1 . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.391 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.120 #===END