# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hongjie Zhang' _publ_contact_author_email hongjie@ciac.jl.cn _publ_author_name 'Hongjie Zhang' data_1 _database_code_depnum_ccdc_archive 'CCDC 870230' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H30 Mn N4 O8' _chemical_formula_weight 845.70 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number No.14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7092(5) _cell_length_b 25.9916(12) _cell_length_c 13.7412(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.5580(10) _cell_angle_gamma 90.00 _cell_volume 3812.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9295 _exptl_absorpt_correction_T_max 0.9484 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21115 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.07 _reflns_number_total 7544 _reflns_number_gt 4375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1099P)^2^+0.3613P] 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 7544 _refine_ls_number_parameters 556 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.2055 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 C13 C 0.8948(5) 0.48171(16) 0.6755(4) 0.0498(12) Uani 1 1 d . . . C14 C 0.9484(5) 0.43374(18) 0.6612(4) 0.0570(13) Uani 1 1 d . . . H14 H 0.9410 0.4178 0.5988 0.068 Uiso 1 1 calc R . . C15 C 1.0149(5) 0.40916(17) 0.7429(4) 0.0572(14) Uani 1 1 d . . . H15 H 1.0586 0.3779 0.7337 0.069 Uiso 1 1 calc R . . C16 C 1.0162(5) 0.43072(18) 0.8355(4) 0.0553(13) Uani 1 1 d . . . C17 C 0.9616(5) 0.47800(18) 0.8474(4) 0.0613(14) Uani 1 1 d . . . H17 H 0.9652 0.4933 0.9103 0.074 Uiso 1 1 calc R . . C18 C 0.9014(5) 0.50347(18) 0.7683(3) 0.0578(14) Uani 1 1 d . . . H18 H 0.8643 0.5361 0.7776 0.069 Uiso 1 1 calc R . . C19 C 1.0772(6) 0.40363(18) 0.9237(4) 0.0591(14) Uani 1 1 d . . . C20 C 0.7473(4) 0.64487(15) 0.5064(3) 0.0362(10) Uani 1 1 d . . . C21 C 0.7271(4) 0.66859(15) 0.4166(3) 0.0433(11) Uani 1 1 d . . . H21 H 0.7191 0.6486 0.3585 0.052 Uiso 1 1 calc R . . C22 C 0.7188(5) 0.72133(16) 0.4119(3) 0.0458(11) Uani 1 1 d . . . H22 H 0.7044 0.7370 0.3496 0.055 Uiso 1 1 calc R . . C23 C 0.7478(4) 0.72892(15) 0.5770(3) 0.0395(10) Uani 1 1 d . . . H23 H 0.7549 0.7499 0.6338 0.047 Uiso 1 1 calc R . . C24 C 0.7566(4) 0.67622(15) 0.5884(3) 0.0419(11) Uani 1 1 d . . . H24 H 0.7690 0.6616 0.6518 0.050 Uiso 1 1 calc R . . C33 C -0.2002(4) 0.17269(15) 0.4770(3) 0.0433(11) Uani 1 1 d . . . H33 H -0.1615 0.1518 0.4313 0.052 Uiso 1 1 calc R . . C34 C -0.2652(4) 0.15025(15) 0.5492(3) 0.0421(11) Uani 1 1 d . . . C35 C -0.3197(4) 0.18183(15) 0.6136(3) 0.0434(11) Uani 1 1 d . . . H35 H -0.3663 0.1674 0.6630 0.052 Uiso 1 1 calc R . . C36 C -0.3068(4) 0.23497(15) 0.6069(3) 0.0371(10) Uani 1 1 d . . . C37 C -0.3645(4) 0.27052(14) 0.6762(3) 0.0371(10) Uani 1 1 d . . . C38 C -0.4106(5) 0.25225(16) 0.7600(4) 0.0502(12) Uani 1 1 d . . . H38 H -0.4020 0.2167 0.7752 0.060 Uiso 1 1 calc R . . C39 C -0.4687(4) 0.28393(16) 0.8224(3) 0.0469(11) Uani 1 1 d . . . H39 H -0.4995 0.2700 0.8798 0.056 Uiso 1 1 calc R . . C40 C -0.4827(4) 0.33558(15) 0.8026(3) 0.0414(10) Uani 1 1 d . . . C41 C -0.4313(6) 0.35453(17) 0.7208(4) 0.0642(16) Uani 1 1 d . . . H41 H -0.4368 0.3903 0.7073 0.077 Uiso 1 1 calc R . . C42 C -0.3723(5) 0.32303(16) 0.6584(4) 0.0594(15) Uani 1 1 d . . . H42 H -0.3370 0.3372 0.6031 0.071 Uiso 1 1 calc R . . C43 C -0.5555(5) 0.36831(17) 0.8674(4) 0.0537(13) Uani 1 1 d . . . C44 C -0.2774(4) 0.09330(15) 0.5599(4) 0.0450(11) Uani 1 1 d . . . C45 C -0.2666(5) 0.07198(17) 0.6531(4) 0.0596(14) Uani 1 1 d . . . H45 H -0.2462 0.0931 0.7085 0.072 Uiso 1 1 calc R . . C46 C -0.2858(6) 0.01999(19) 0.6642(4) 0.0691(17) Uani 1 1 d . . . H46 H -0.2790 0.0053 0.7277 0.083 Uiso 1 1 calc R . . C47 C -0.3156(6) 0.00862(19) 0.4988(4) 0.0752(18) Uani 1 1 d . . . H47 H -0.3302 -0.0138 0.4445 0.090 Uiso 1 1 calc R . . C48 C -0.2968(6) 0.06062(18) 0.4830(4) 0.0672(16) Uani 1 1 d . . . H48 H -0.2976 0.0734 0.4182 0.081 Uiso 1 1 calc R . . N1 N 0.7298(3) 0.75173(12) 0.4907(2) 0.0355(8) Uani 1 1 d . . . N3 N -0.3137(4) -0.00996(15) 0.5866(4) 0.0652(13) Uani 1 1 d D . . N4 N -0.2444(3) 0.25687(12) 0.5369(3) 0.0396(8) Uani 1 1 d . . . O5 O 1.0529(4) 0.42385(14) 1.0063(3) 0.0780(12) Uani 1 1 d . . . O6 O 1.1393(3) 0.36561(14) 0.9120(3) 0.0669(10) Uani 1 1 d . . . O7 O -0.5843(3) 0.34993(11) 0.9468(2) 0.0505(8) Uani 1 1 d . . . O8 O -0.5858(4) 0.41247(12) 0.8363(3) 0.0867(14) Uani 1 1 d . . . H4A H 0.033(7) 0.397(2) 0.106(3) 0.130 Uiso 1 1 d D . . H3A H -0.338(7) -0.0436(12) 0.575(5) 0.130 Uiso 1 1 d D . . C1 C 0.3708(4) 0.38021(15) 0.1867(3) 0.0376(10) Uani 1 1 d . . . C2 C 0.4418(4) 0.41079(15) 0.2654(3) 0.0360(9) Uani 1 1 d . . . C3 C 0.5250(4) 0.38835(15) 0.3353(3) 0.0418(11) Uani 1 1 d . . . H3 H 0.5305 0.3519 0.3394 0.050 Uiso 1 1 calc R . . C4 C 0.6002(4) 0.41825(15) 0.3993(3) 0.0415(10) Uani 1 1 d . . . H4 H 0.6582 0.4021 0.4455 0.050 Uiso 1 1 calc R . . C5 C 0.5917(4) 0.47140(14) 0.3969(3) 0.0343(9) Uani 1 1 d . . . C6 C 0.5018(5) 0.49324(16) 0.3319(4) 0.0538(13) Uani 1 1 d . . . H6 H 0.4898 0.5295 0.3323 0.065 Uiso 1 1 calc R . . C7 C 0.4291(5) 0.46330(16) 0.2665(4) 0.0545(13) Uani 1 1 d . . . H7 H 0.3693 0.4793 0.2216 0.065 Uiso 1 1 calc R . . C8 C 0.6771(4) 0.50390(14) 0.4617(3) 0.0362(10) Uani 1 1 d . . . C9 C 0.6759(4) 0.55724(14) 0.4514(3) 0.0384(10) Uani 1 1 d . . . H9 H 0.6240 0.5729 0.4005 0.046 Uiso 1 1 calc R . . C10 C 0.7506(4) 0.58747(15) 0.5156(3) 0.0384(10) Uani 1 1 d . . . C11 C 0.8242(4) 0.56274(15) 0.5882(3) 0.0447(11) Uani 1 1 d . . . H11 H 0.8761 0.5821 0.6340 0.054 Uiso 1 1 calc R . . C12 C 0.8221(4) 0.50888(15) 0.5939(3) 0.0437(11) Uani 1 1 d . . . C25 C 0.0378(4) 0.33439(16) 0.1677(3) 0.0422(11) Uani 1 1 d . . . C26 C -0.0201(4) 0.30717(16) 0.2471(3) 0.0408(10) Uani 1 1 d . . . C27 C -0.0757(5) 0.33349(16) 0.3202(4) 0.0516(12) Uani 1 1 d . . . H27 H -0.0773 0.3700 0.3194 0.062 Uiso 1 1 calc R . . C28 C -0.1283(5) 0.30742(16) 0.3934(4) 0.0494(12) Uani 1 1 d . . . H28 H -0.1655 0.3261 0.4430 0.059 Uiso 1 1 calc R . . C29 C -0.1279(4) 0.25338(16) 0.3958(3) 0.0419(10) Uani 1 1 d . . . C30 C -0.0701(4) 0.22774(17) 0.3231(3) 0.0477(12) Uani 1 1 d . . . H30 H -0.0668 0.1912 0.3242 0.057 Uiso 1 1 calc R . . C31 C -0.0176(4) 0.25394(16) 0.2495(3) 0.0448(11) Uani 1 1 d . . . H31 H 0.0206 0.2354 0.2002 0.054 Uiso 1 1 calc R . . C32 C -0.1918(4) 0.22599(15) 0.4721(3) 0.0387(10) Uani 1 1 d . . . N2 N 0.7507(3) 0.47997(12) 0.5303(3) 0.0405(9) Uani 1 1 d . . . O1 O 0.3025(3) 0.40405(11) 0.1233(2) 0.0506(8) Uani 1 1 d . . . O2 O 0.3815(3) 0.33265(10) 0.1842(2) 0.0498(8) Uani 1 1 d . . . O3 O 0.0999(3) 0.31152(11) 0.1102(2) 0.0512(8) Uani 1 1 d . . . O4 O 0.0163(3) 0.38334(12) 0.1633(2) 0.0557(9) Uani 1 1 d D . . Mn1 Mn 0.26072(6) 0.33729(2) 0.02941(5) 0.0354(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C13 0.058(3) 0.033(2) 0.055(3) 0.010(2) -0.015(2) -0.005(2) C14 0.066(3) 0.045(3) 0.059(3) 0.014(2) 0.001(3) 0.008(2) C15 0.067(3) 0.036(3) 0.069(4) 0.019(3) 0.012(3) 0.013(2) C16 0.053(3) 0.049(3) 0.061(3) 0.013(3) -0.013(2) -0.008(2) C17 0.082(4) 0.045(3) 0.053(3) 0.006(2) -0.020(3) -0.004(3) C18 0.076(4) 0.046(3) 0.047(3) 0.004(2) -0.023(3) -0.002(2) C19 0.084(4) 0.034(3) 0.057(3) 0.010(2) -0.003(3) -0.011(3) C20 0.040(2) 0.027(2) 0.039(2) 0.0018(18) -0.0131(19) -0.0033(17) C21 0.063(3) 0.030(2) 0.035(3) -0.0001(19) -0.008(2) -0.004(2) C22 0.066(3) 0.033(2) 0.036(3) 0.007(2) -0.012(2) -0.006(2) C23 0.054(3) 0.032(2) 0.032(2) -0.0023(19) -0.003(2) -0.0070(19) C24 0.061(3) 0.028(2) 0.034(3) 0.0049(18) -0.013(2) -0.0017(19) C33 0.040(2) 0.035(2) 0.055(3) -0.008(2) 0.004(2) 0.0051(19) C34 0.038(3) 0.029(2) 0.060(3) -0.006(2) 0.010(2) -0.0033(18) C35 0.039(2) 0.029(2) 0.063(3) -0.006(2) 0.014(2) -0.0008(19) C36 0.031(2) 0.029(2) 0.052(3) -0.0057(19) 0.0022(19) 0.0028(17) C37 0.039(2) 0.026(2) 0.046(3) -0.0020(19) 0.004(2) 0.0035(17) C38 0.061(3) 0.026(2) 0.066(3) -0.002(2) 0.021(3) -0.004(2) C39 0.055(3) 0.033(2) 0.054(3) 0.000(2) 0.016(2) 0.000(2) C40 0.051(3) 0.031(2) 0.043(3) 0.001(2) 0.004(2) 0.0063(19) C41 0.106(5) 0.026(2) 0.066(3) 0.014(2) 0.040(3) 0.023(3) C42 0.095(4) 0.033(2) 0.054(3) 0.011(2) 0.034(3) 0.014(3) C43 0.067(3) 0.035(3) 0.062(3) 0.006(2) 0.020(3) 0.009(2) C44 0.044(3) 0.028(2) 0.066(3) -0.010(2) 0.022(2) -0.0037(19) C45 0.077(4) 0.033(2) 0.072(4) -0.008(2) 0.026(3) -0.014(2) C46 0.092(4) 0.043(3) 0.078(4) -0.007(3) 0.042(3) -0.014(3) C47 0.128(6) 0.037(3) 0.062(4) -0.020(3) 0.016(4) -0.016(3) C48 0.106(5) 0.038(3) 0.059(3) -0.007(2) 0.019(3) -0.003(3) N1 0.047(2) 0.0284(17) 0.0304(19) 0.0010(15) -0.0041(15) -0.0044(15) N3 0.076(3) 0.036(2) 0.089(4) -0.016(2) 0.040(3) -0.016(2) N4 0.042(2) 0.0316(18) 0.046(2) -0.0044(16) 0.0048(17) -0.0007(15) O5 0.118(3) 0.058(2) 0.055(2) 0.0136(19) -0.016(2) -0.006(2) O6 0.061(2) 0.063(2) 0.075(3) 0.019(2) -0.0078(19) 0.0063(19) O7 0.056(2) 0.0510(19) 0.0465(19) 0.0067(16) 0.0149(16) 0.0119(15) O8 0.137(4) 0.0363(19) 0.096(3) 0.0185(19) 0.065(3) 0.036(2) C1 0.046(3) 0.031(2) 0.036(2) -0.0034(19) 0.005(2) 0.0025(19) C2 0.041(2) 0.030(2) 0.037(2) -0.0046(18) -0.0005(19) -0.0048(18) C3 0.064(3) 0.0195(19) 0.042(3) -0.0036(18) -0.001(2) 0.0034(19) C4 0.059(3) 0.028(2) 0.036(2) -0.0034(19) -0.005(2) 0.004(2) C5 0.049(3) 0.0230(19) 0.030(2) -0.0011(16) -0.0036(19) -0.0005(17) C6 0.068(3) 0.022(2) 0.067(3) -0.001(2) -0.021(3) 0.000(2) C7 0.064(3) 0.031(2) 0.063(3) 0.005(2) -0.025(3) 0.004(2) C8 0.051(3) 0.026(2) 0.030(2) -0.0007(17) -0.0046(19) 0.0009(18) C9 0.054(3) 0.029(2) 0.030(2) 0.0025(18) -0.011(2) 0.0023(19) C10 0.049(3) 0.028(2) 0.036(2) 0.0023(18) -0.0107(19) -0.0020(18) C11 0.061(3) 0.029(2) 0.041(3) 0.0030(19) -0.018(2) -0.003(2) C12 0.058(3) 0.029(2) 0.042(3) 0.0068(19) -0.012(2) 0.005(2) C25 0.039(2) 0.031(2) 0.055(3) -0.003(2) -0.006(2) -0.0035(19) C26 0.040(3) 0.038(2) 0.045(3) 0.000(2) 0.006(2) -0.0021(19) C27 0.065(3) 0.028(2) 0.063(3) -0.005(2) 0.013(3) -0.005(2) C28 0.058(3) 0.037(2) 0.056(3) -0.006(2) 0.022(2) -0.002(2) C29 0.044(3) 0.037(2) 0.045(3) -0.001(2) 0.005(2) 0.0011(19) C30 0.057(3) 0.034(2) 0.054(3) -0.002(2) 0.014(2) 0.000(2) C31 0.048(3) 0.038(2) 0.050(3) -0.008(2) 0.007(2) -0.001(2) C32 0.036(2) 0.034(2) 0.046(3) -0.001(2) 0.0031(19) -0.0015(18) N2 0.058(2) 0.0227(16) 0.039(2) -0.0013(15) -0.0076(17) 0.0043(16) O1 0.061(2) 0.0364(17) 0.052(2) -0.0016(15) -0.0114(16) -0.0019(15) O2 0.065(2) 0.0339(17) 0.0487(19) -0.0099(14) -0.0087(16) 0.0013(14) O3 0.054(2) 0.0386(17) 0.063(2) -0.0033(16) 0.0161(17) -0.0028(15) O4 0.071(2) 0.0392(19) 0.059(2) 0.0026(16) 0.0171(18) -0.0026(16) Mn1 0.0431(4) 0.0258(3) 0.0365(4) -0.0031(3) -0.0024(3) 0.0042(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C13 C18 1.392(6) . ? C13 C14 1.393(6) . ? C13 C12 1.491(6) . ? C14 C15 1.431(7) . ? C14 H14 0.9500 . ? C15 C16 1.390(7) . ? C15 H15 0.9500 . ? C16 C17 1.376(7) . ? C16 C19 1.506(7) . ? C17 C18 1.387(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O6 1.209(6) . ? C19 O5 1.295(6) . ? C20 C21 1.381(6) . ? C20 C24 1.387(6) . ? C20 C10 1.498(5) . ? C21 C22 1.375(6) . ? C21 H21 0.9500 . ? C22 N1 1.338(5) . ? C22 H22 0.9500 . ? C23 N1 1.326(5) . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C33 C34 1.385(6) . ? C33 C32 1.390(6) . ? C33 H33 0.9500 . ? C34 C35 1.371(6) . ? C34 C44 1.494(6) . ? C35 C36 1.392(5) . ? C35 H35 0.9500 . ? C36 N4 1.342(5) . ? C36 C37 1.495(6) . ? C37 C38 1.373(6) . ? C37 C42 1.388(6) . ? C38 C39 1.373(6) . ? C38 H38 0.9500 . ? C39 C40 1.376(5) . ? C39 H39 0.9500 . ? C40 C41 1.381(6) . ? C40 C43 1.494(6) . ? C41 C42 1.375(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 O7 1.252(5) . ? C43 O8 1.258(5) . ? C44 C48 1.359(6) . ? C44 C45 1.392(7) . ? C45 C46 1.377(6) . ? C45 H45 0.9500 . ? C46 N3 1.335(7) . ? C46 H46 0.9500 . ? C47 N3 1.298(7) . ? C47 C48 1.386(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? N1 Mn1 2.244(3) 2_655 ? N3 H3A 0.92(2) . ? N4 C32 1.354(5) . ? O6 Mn1 2.122(3) 1_656 ? O7 Mn1 2.110(3) 1_456 ? C1 O2 1.242(4) . ? C1 O1 1.256(5) . ? C1 C2 1.499(6) . ? C1 Mn1 2.628(4) . ? C2 C7 1.372(6) . ? C2 C3 1.386(6) . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.382(6) . ? C5 C8 1.487(5) . ? C6 C7 1.381(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 N2 1.334(5) . ? C8 C9 1.394(5) . ? C9 C10 1.387(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C11 C12 1.403(5) . ? C11 H11 0.9500 . ? C12 N2 1.344(5) . ? C25 O3 1.226(5) . ? C25 O4 1.293(5) . ? C25 C26 1.478(6) . ? C26 C31 1.384(6) . ? C26 C27 1.388(6) . ? C27 C28 1.371(6) . ? C27 H27 0.9500 . ? C28 C29 1.405(6) . ? C28 H28 0.9500 . ? C29 C30 1.386(6) . ? C29 C32 1.480(6) . ? C30 C31 1.376(6) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? O1 Mn1 2.187(3) . ? O2 Mn1 2.403(3) . ? O3 Mn1 2.225(3) . ? O4 H4A 0.90(2) . ? Mn1 O7 2.110(3) 1_654 ? Mn1 O6 2.122(3) 1_454 ? Mn1 N1 2.244(3) 2_645 ? 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 C18 C13 C14 120.1(4) . . ? C18 C13 C12 118.8(4) . . ? C14 C13 C12 121.0(4) . . ? C13 C14 C15 118.3(5) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 120.4(4) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.7(5) . . ? C17 C16 C19 118.9(5) . . ? C15 C16 C19 121.4(5) . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 120.7(5) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? O6 C19 O5 126.8(5) . . ? O6 C19 C16 118.9(5) . . ? O5 C19 C16 114.3(5) . . ? C21 C20 C24 117.4(4) . . ? C21 C20 C10 121.4(4) . . ? C24 C20 C10 121.1(4) . . ? C22 C21 C20 119.5(4) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? N1 C22 C21 123.3(4) . . ? N1 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? N1 C23 C24 123.3(4) . . ? N1 C23 H23 118.4 . . ? C24 C23 H23 118.4 . . ? C23 C24 C20 119.4(4) . . ? C23 C24 H24 120.3 . . ? C20 C24 H24 120.3 . . ? C34 C33 C32 119.5(4) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 118.3(4) . . ? C35 C34 C44 119.0(4) . . ? C33 C34 C44 122.7(4) . . ? C34 C35 C36 120.1(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? N4 C36 C35 121.7(4) . . ? N4 C36 C37 116.7(3) . . ? C35 C36 C37 121.5(4) . . ? C38 C37 C42 117.9(4) . . ? C38 C37 C36 121.0(4) . . ? C42 C37 C36 121.2(4) . . ? C37 C38 C39 121.8(4) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C38 C39 C40 120.6(4) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C41 117.7(4) . . ? C39 C40 C43 119.5(4) . . ? C41 C40 C43 122.8(4) . . ? C42 C41 C40 121.9(4) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C41 C42 C37 120.0(4) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? O7 C43 O8 124.7(4) . . ? O7 C43 C40 118.6(4) . . ? O8 C43 C40 116.7(4) . . ? C48 C44 C45 117.6(4) . . ? C48 C44 C34 123.5(5) . . ? C45 C44 C34 118.9(4) . . ? C46 C45 C44 119.4(5) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? N3 C46 C45 120.6(5) . . ? N3 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? N3 C47 C48 121.1(5) . . ? N3 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C44 C48 C47 120.2(5) . . ? C44 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C23 N1 C22 117.2(3) . . ? C23 N1 Mn1 123.3(3) . 2_655 ? C22 N1 Mn1 119.2(3) . 2_655 ? C47 N3 C46 120.8(4) . . ? C47 N3 H3A 102(4) . . ? C46 N3 H3A 137(4) . . ? C36 N4 C32 118.5(3) . . ? C19 O6 Mn1 119.5(4) . 1_656 ? C43 O7 Mn1 141.9(3) . 1_456 ? O2 C1 O1 121.4(4) . . ? O2 C1 C2 120.4(4) . . ? O1 C1 C2 118.2(4) . . ? O2 C1 Mn1 65.8(2) . . ? O1 C1 Mn1 55.9(2) . . ? C2 C1 Mn1 170.8(3) . . ? C7 C2 C3 118.0(4) . . ? C7 C2 C1 119.4(4) . . ? C3 C2 C1 122.5(4) . . ? C4 C3 C2 120.9(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.8(4) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 117.8(4) . . ? C6 C5 C8 121.1(3) . . ? C4 C5 C8 121.1(4) . . ? C7 C6 C5 121.1(4) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C2 C7 C6 121.1(4) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? N2 C8 C9 122.4(4) . . ? N2 C8 C5 117.3(3) . . ? C9 C8 C5 120.3(4) . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 117.6(4) . . ? C11 C10 C20 122.3(4) . . ? C9 C10 C20 120.1(4) . . ? C10 C11 C12 119.7(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? N2 C12 C11 122.2(4) . . ? N2 C12 C13 117.4(4) . . ? C11 C12 C13 120.3(4) . . ? O3 C25 O4 123.4(4) . . ? O3 C25 C26 121.6(4) . . ? O4 C25 C26 114.9(4) . . ? C31 C26 C27 118.9(4) . . ? C31 C26 C25 119.2(4) . . ? C27 C26 C25 121.9(4) . . ? C28 C27 C26 120.8(4) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.7(4) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 117.7(4) . . ? C30 C29 C32 122.5(4) . . ? C28 C29 C32 119.8(4) . . ? C31 C30 C29 121.6(4) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 C26 120.2(4) . . ? C30 C31 H31 119.9 . . ? C26 C31 H31 119.9 . . ? N4 C32 C33 121.8(4) . . ? N4 C32 C29 114.9(3) . . ? C33 C32 C29 123.3(4) . . ? C8 N2 C12 118.2(3) . . ? C1 O1 Mn1 95.7(2) . . ? C1 O2 Mn1 86.0(3) . . ? C25 O3 Mn1 131.0(3) . . ? C25 O4 H4A 113(5) . . ? O7 Mn1 O6 89.86(13) 1_654 1_454 ? O7 Mn1 O1 93.50(13) 1_654 . ? O6 Mn1 O1 104.93(13) 1_454 . ? O7 Mn1 O3 171.33(11) 1_654 . ? O6 Mn1 O3 91.84(13) 1_454 . ? O1 Mn1 O3 94.27(12) . . ? O7 Mn1 N1 92.44(12) 1_654 2_645 ? O6 Mn1 N1 106.33(14) 1_454 2_645 ? O1 Mn1 N1 148.17(12) . 2_645 ? O3 Mn1 N1 78.92(12) . 2_645 ? O7 Mn1 O2 95.33(12) 1_654 . ? O6 Mn1 O2 160.85(13) 1_454 . ? O1 Mn1 O2 56.43(10) . . ? O3 Mn1 O2 85.79(12) . . ? N1 Mn1 O2 91.88(11) 2_645 . ? O7 Mn1 C1 93.19(13) 1_654 . ? O6 Mn1 C1 133.33(14) 1_454 . ? O1 Mn1 C1 28.41(11) . . ? O3 Mn1 C1 91.82(13) . . ? N1 Mn1 C1 120.02(12) 2_645 . ? O2 Mn1 C1 28.14(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 C18 C13 C14 C15 -3.1(7) . . . . ? C12 C13 C14 C15 -178.8(4) . . . . ? C13 C14 C15 C16 5.6(7) . . . . ? C14 C15 C16 C17 -5.2(8) . . . . ? C14 C15 C16 C19 175.3(5) . . . . ? C15 C16 C17 C18 2.4(8) . . . . ? C19 C16 C17 C18 -178.2(5) . . . . ? C16 C17 C18 C13 0.1(8) . . . . ? C14 C13 C18 C17 0.3(8) . . . . ? C12 C13 C18 C17 176.1(5) . . . . ? C17 C16 C19 O6 -170.3(5) . . . . ? C15 C16 C19 O6 9.2(8) . . . . ? C17 C16 C19 O5 11.6(7) . . . . ? C15 C16 C19 O5 -168.9(5) . . . . ? C24 C20 C21 C22 0.8(7) . . . . ? C10 C20 C21 C22 176.9(4) . . . . ? C20 C21 C22 N1 0.3(7) . . . . ? N1 C23 C24 C20 0.4(7) . . . . ? C21 C20 C24 C23 -1.1(6) . . . . ? C10 C20 C24 C23 -177.3(4) . . . . ? C32 C33 C34 C35 0.1(7) . . . . ? C32 C33 C34 C44 -179.4(4) . . . . ? C33 C34 C35 C36 -1.3(7) . . . . ? C44 C34 C35 C36 178.2(4) . . . . ? C34 C35 C36 N4 1.7(7) . . . . ? C34 C35 C36 C37 -179.8(4) . . . . ? N4 C36 C37 C38 -168.3(4) . . . . ? C35 C36 C37 C38 13.1(7) . . . . ? N4 C36 C37 C42 11.1(6) . . . . ? C35 C36 C37 C42 -167.5(5) . . . . ? C42 C37 C38 C39 3.3(7) . . . . ? C36 C37 C38 C39 -177.2(4) . . . . ? C37 C38 C39 C40 0.0(8) . . . . ? C38 C39 C40 C41 -3.0(7) . . . . ? C38 C39 C40 C43 175.0(5) . . . . ? C39 C40 C41 C42 2.6(8) . . . . ? C43 C40 C41 C42 -175.3(5) . . . . ? C40 C41 C42 C37 0.7(9) . . . . ? C38 C37 C42 C41 -3.7(8) . . . . ? C36 C37 C42 C41 176.9(5) . . . . ? C39 C40 C43 O7 11.6(7) . . . . ? C41 C40 C43 O7 -170.5(5) . . . . ? C39 C40 C43 O8 -166.8(5) . . . . ? C41 C40 C43 O8 11.0(8) . . . . ? C35 C34 C44 C48 140.4(5) . . . . ? C33 C34 C44 C48 -40.1(7) . . . . ? C35 C34 C44 C45 -40.5(6) . . . . ? C33 C34 C44 C45 138.9(5) . . . . ? C48 C44 C45 C46 -5.1(7) . . . . ? C34 C44 C45 C46 175.8(5) . . . . ? C44 C45 C46 N3 0.4(8) . . . . ? C45 C44 C48 C47 5.3(8) . . . . ? C34 C44 C48 C47 -175.6(5) . . . . ? N3 C47 C48 C44 -0.8(10) . . . . ? C24 C23 N1 C22 0.6(6) . . . . ? C24 C23 N1 Mn1 -172.1(3) . . . 2_655 ? C21 C22 N1 C23 -1.0(7) . . . . ? C21 C22 N1 Mn1 172.0(4) . . . 2_655 ? C48 C47 N3 C46 -4.2(10) . . . . ? C45 C46 N3 C47 4.3(9) . . . . ? C35 C36 N4 C32 -0.8(6) . . . . ? C37 C36 N4 C32 -179.4(4) . . . . ? O5 C19 O6 Mn1 -16.8(8) . . . 1_656 ? C16 C19 O6 Mn1 165.3(3) . . . 1_656 ? O8 C43 O7 Mn1 51.4(9) . . . 1_456 ? C40 C43 O7 Mn1 -126.9(4) . . . 1_456 ? O2 C1 C2 C7 179.7(4) . . . . ? O1 C1 C2 C7 0.7(6) . . . . ? Mn1 C1 C2 C7 49(2) . . . . ? O2 C1 C2 C3 2.7(7) . . . . ? O1 C1 C2 C3 -176.3(4) . . . . ? Mn1 C1 C2 C3 -127.6(18) . . . . ? C7 C2 C3 C4 -5.0(7) . . . . ? C1 C2 C3 C4 172.0(4) . . . . ? C2 C3 C4 C5 1.8(7) . . . . ? C3 C4 C5 C6 3.1(7) . . . . ? C3 C4 C5 C8 -176.5(4) . . . . ? C4 C5 C6 C7 -4.8(7) . . . . ? C8 C5 C6 C7 174.9(5) . . . . ? C3 C2 C7 C6 3.4(7) . . . . ? C1 C2 C7 C6 -173.7(5) . . . . ? C5 C6 C7 C2 1.5(8) . . . . ? C6 C5 C8 N2 172.0(4) . . . . ? C4 C5 C8 N2 -8.3(6) . . . . ? C6 C5 C8 C9 -6.2(6) . . . . ? C4 C5 C8 C9 173.5(4) . . . . ? N2 C8 C9 C10 -1.8(7) . . . . ? C5 C8 C9 C10 176.3(4) . . . . ? C8 C9 C10 C11 0.0(7) . . . . ? C8 C9 C10 C20 -178.5(4) . . . . ? C21 C20 C10 C11 148.5(5) . . . . ? C24 C20 C10 C11 -35.5(7) . . . . ? C21 C20 C10 C9 -33.1(6) . . . . ? C24 C20 C10 C9 142.9(4) . . . . ? C9 C10 C11 C12 0.6(7) . . . . ? C20 C10 C11 C12 179.1(4) . . . . ? C10 C11 C12 N2 0.4(7) . . . . ? C10 C11 C12 C13 -176.1(5) . . . . ? C18 C13 C12 N2 -138.9(5) . . . . ? C14 C13 C12 N2 36.8(7) . . . . ? C18 C13 C12 C11 37.8(7) . . . . ? C14 C13 C12 C11 -146.4(5) . . . . ? O3 C25 C26 C31 -8.2(7) . . . . ? O4 C25 C26 C31 171.0(4) . . . . ? O3 C25 C26 C27 171.0(4) . . . . ? O4 C25 C26 C27 -9.9(6) . . . . ? C31 C26 C27 C28 -0.5(7) . . . . ? C25 C26 C27 C28 -179.7(4) . . . . ? C26 C27 C28 C29 -0.4(8) . . . . ? C27 C28 C29 C30 1.4(7) . . . . ? C27 C28 C29 C32 -176.4(5) . . . . ? C28 C29 C30 C31 -1.6(7) . . . . ? C32 C29 C30 C31 176.1(4) . . . . ? C29 C30 C31 C26 0.7(7) . . . . ? C27 C26 C31 C30 0.4(7) . . . . ? C25 C26 C31 C30 179.6(4) . . . . ? C36 N4 C32 C33 -0.5(6) . . . . ? C36 N4 C32 C29 178.4(4) . . . . ? C34 C33 C32 N4 0.8(7) . . . . ? C34 C33 C32 C29 -178.0(4) . . . . ? C30 C29 C32 N4 -179.3(4) . . . . ? C28 C29 C32 N4 -1.7(6) . . . . ? C30 C29 C32 C33 -0.5(7) . . . . ? C28 C29 C32 C33 177.2(4) . . . . ? C9 C8 N2 C12 2.8(6) . . . . ? C5 C8 N2 C12 -175.4(4) . . . . ? C11 C12 N2 C8 -2.1(7) . . . . ? C13 C12 N2 C8 174.5(4) . . . . ? O2 C1 O1 Mn1 -7.3(5) . . . . ? C2 C1 O1 Mn1 171.7(3) . . . . ? O1 C1 O2 Mn1 6.6(4) . . . . ? C2 C1 O2 Mn1 -172.3(4) . . . . ? O4 C25 O3 Mn1 31.1(7) . . . . ? C26 C25 O3 Mn1 -149.8(3) . . . . ? C1 O1 Mn1 O7 -90.2(3) . . . 1_654 ? C1 O1 Mn1 O6 179.0(3) . . . 1_454 ? C1 O1 Mn1 O3 85.9(3) . . . . ? C1 O1 Mn1 N1 10.1(4) . . . 2_645 ? C1 O1 Mn1 O2 3.8(2) . . . . ? C25 O3 Mn1 O7 171.1(7) . . . 1_654 ? C25 O3 Mn1 O6 -87.6(4) . . . 1_454 ? C25 O3 Mn1 O1 17.5(4) . . . . ? C25 O3 Mn1 N1 166.1(4) . . . 2_645 ? C25 O3 Mn1 O2 73.3(4) . . . . ? C25 O3 Mn1 C1 45.8(4) . . . . ? C1 O2 Mn1 O7 86.8(3) . . . 1_654 ? C1 O2 Mn1 O6 -18.4(5) . . . 1_454 ? C1 O2 Mn1 O1 -3.9(2) . . . . ? C1 O2 Mn1 O3 -101.8(3) . . . . ? C1 O2 Mn1 N1 179.4(3) . . . 2_645 ? O2 C1 Mn1 O7 -95.3(3) . . . 1_654 ? O1 C1 Mn1 O7 91.5(3) . . . 1_654 ? C2 C1 Mn1 O7 38.5(19) . . . 1_654 ? O2 C1 Mn1 O6 171.8(2) . . . 1_454 ? O1 C1 Mn1 O6 -1.4(3) . . . 1_454 ? C2 C1 Mn1 O6 -54(2) . . . 1_454 ? O2 C1 Mn1 O1 173.2(4) . . . . ? C2 C1 Mn1 O1 -52.9(18) . . . . ? O2 C1 Mn1 O3 77.6(3) . . . . ? O1 C1 Mn1 O3 -95.6(3) . . . . ? C2 C1 Mn1 O3 -148.5(19) . . . . ? O2 C1 Mn1 N1 -0.7(3) . . . 2_645 ? O1 C1 Mn1 N1 -173.9(2) . . . 2_645 ? C2 C1 Mn1 N1 133.2(19) . . . 2_645 ? O1 C1 Mn1 O2 -173.2(4) . . . . ? C2 C1 Mn1 O2 134(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A O5 0.90(2) 1.57(2) 2.461(5) 175(8) 1_454 N3 H3A O8 0.92(2) 1.90(6) 2.555(5) 126(6) 2_446 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.944 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.076 #===END #========================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 870231' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H58 Co4 N8 O17' _chemical_formula_weight 1831.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number No.15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.1065(17) _cell_length_b 12.8792(8) _cell_length_c 23.3705(14) _cell_angle_alpha 90.00 _cell_angle_beta 109.4170(10) _cell_angle_gamma 90.00 _cell_volume 7694.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3736 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.8358 _exptl_absorpt_correction_T_max 0.8731 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20540 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.04 _reflns_number_total 7588 _reflns_number_gt 5223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1471P)^2^+119.3092P] 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 7588 _refine_ls_number_parameters 531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1377 _refine_ls_R_factor_gt 0.1041 _refine_ls_wR_factor_ref 0.3142 _refine_ls_wR_factor_gt 0.2918 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 C13 C 0.2253(3) 1.1467(7) -0.0859(4) 0.0368(19) Uani 1 1 d . . . C14 C 0.1800(3) 1.1084(7) -0.1269(4) 0.049(2) Uani 1 1 d . . . H14 H 0.1691 1.0400 -0.1217 0.059 Uiso 1 1 calc R . . C15 C 0.1500(3) 1.1667(7) -0.1755(4) 0.047(2) Uani 1 1 d . . . H15 H 0.1180 1.1402 -0.2023 0.057 Uiso 1 1 calc R . . C16 C 0.1673(3) 1.2652(6) -0.1847(4) 0.0339(18) Uani 1 1 d . . . C17 C 0.2123(3) 1.3057(7) -0.1423(4) 0.0398(19) Uani 1 1 d . . . H17 H 0.2234 1.3740 -0.1473 0.048 Uiso 1 1 calc R . . C18 C 0.2401(3) 1.2481(7) -0.0939(4) 0.042(2) Uani 1 1 d . . . H18 H 0.2704 1.2771 -0.0649 0.050 Uiso 1 1 calc R . . C19 C 0.1377(3) 1.3286(7) -0.2388(4) 0.0385(19) Uani 1 1 d . . . C20 C 0.3970(4) 1.0550(10) 0.0678(5) 0.0601(11) Uani 1 1 d . . . C21 C 0.4334(4) 1.0226(10) 0.0409(5) 0.0601(11) Uani 1 1 d . . . H21 H 0.4218 0.9922 0.0017 0.072 Uiso 1 1 calc R . . C22 C 0.4860(4) 1.0350(9) 0.0716(5) 0.0601(11) Uani 1 1 d . . . H22 H 0.5103 1.0134 0.0525 0.072 Uiso 1 1 calc R . . C23 C 0.4720(4) 1.1066(10) 0.1497(5) 0.0601(11) Uani 1 1 d . . . H23 H 0.4850 1.1416 0.1875 0.072 Uiso 1 1 calc R . . C24 C 0.4176(4) 1.0930(9) 0.1236(5) 0.0601(11) Uani 1 1 d . . . H24 H 0.3954 1.1112 0.1460 0.072 Uiso 1 1 calc R . . C37 C 0.0326(3) -0.1597(7) -0.1522(4) 0.0358(18) Uani 1 1 d . . . C38 C 0.0803(3) -0.1379(7) -0.1602(4) 0.044(2) Uani 1 1 d . . . H38 H 0.0958 -0.0712 -0.1502 0.052 Uiso 1 1 calc R . . C39 C 0.1053(3) -0.2148(8) -0.1830(4) 0.041(2) Uani 1 1 d . . . H39 H 0.1378 -0.1995 -0.1883 0.049 Uiso 1 1 calc R . . C40 C 0.0837(3) -0.3129(7) -0.1979(4) 0.0394(19) Uani 1 1 d . . . C41 C 0.0382(3) -0.3350(7) -0.1864(4) 0.043(2) Uani 1 1 d . . . H41 H 0.0241 -0.4032 -0.1935 0.052 Uiso 1 1 calc R . . C42 C 0.0128(3) -0.2604(7) -0.1646(4) 0.0381(19) Uani 1 1 d . . . H42 H -0.0189 -0.2776 -0.1579 0.046 Uiso 1 1 calc R . . C43 C 0.1054(3) -0.3909(7) -0.2322(4) 0.0360(18) Uani 1 1 d . . . C44 C -0.1372(3) 0.0208(6) -0.1803(3) 0.0290(16) Uani 1 1 d . . . C45 C -0.1612(3) 0.1156(6) -0.1848(4) 0.0379(19) Uani 1 1 d . . . H45 H -0.1415 0.1751 -0.1666 0.045 Uiso 1 1 calc R . . C46 C -0.2140(3) 0.1243(7) -0.2157(4) 0.040(2) Uani 1 1 d . . . H46 H -0.2298 0.1907 -0.2183 0.048 Uiso 1 1 calc R . . C47 C -0.2207(3) -0.0500(6) -0.2362(4) 0.0339(17) Uani 1 1 d . . . H47 H -0.2415 -0.1085 -0.2539 0.041 Uiso 1 1 calc R . . C48 C -0.1690(3) -0.0653(6) -0.2059(4) 0.0331(17) Uani 1 1 d . . . H48 H -0.1545 -0.1331 -0.2019 0.040 Uiso 1 1 calc R . . N1 N 0.5039(3) 1.0750(8) 0.1257(4) 0.0601(11) Uani 1 1 d . . . N3 N -0.2441(2) 0.0436(5) -0.2425(3) 0.0293(14) Uani 1 1 d . . . O2 O 0.1106(2) 0.6320(5) 0.1120(3) 0.0420(14) Uani 1 1 d . . . O1W O 0.0000 1.163(6) -0.2500 0.50(4) Uiso 1 2 d S . . O3 O 0.0916(2) 1.3065(5) -0.2679(3) 0.0444(15) Uani 1 1 d . . . O4 O 0.1620(2) 1.4044(5) -0.2538(3) 0.0437(14) Uani 1 1 d . . . O7 O 0.0748(2) -0.4638(5) -0.2601(3) 0.0434(14) Uani 1 1 d . . . O8 O 0.1497(2) -0.3723(5) -0.2350(3) 0.0404(14) Uani 1 1 d . . . C1 C 0.1578(3) 0.6160(6) 0.1143(4) 0.0318(17) Uani 1 1 d . . . C2 C 0.1829(3) 0.6947(6) 0.0847(3) 0.0280(16) Uani 1 1 d . . . C3 C 0.1539(3) 0.7696(7) 0.0448(4) 0.0367(19) Uani 1 1 d . . . H3 H 0.1168 0.7670 0.0309 0.044 Uiso 1 1 calc R . . C4 C 0.1795(3) 0.8486(7) 0.0251(4) 0.0368(19) Uani 1 1 d . . . H4 H 0.1596 0.8991 -0.0026 0.044 Uiso 1 1 calc R . . C5 C 0.2347(3) 0.8545(6) 0.0457(3) 0.0307(16) Uani 1 1 d . . . C6 C 0.2625(3) 0.7763(7) 0.0830(4) 0.039(2) Uani 1 1 d . . . H6 H 0.2996 0.7767 0.0953 0.047 Uiso 1 1 calc R . . C7 C 0.2373(3) 0.6964(7) 0.1032(4) 0.0365(19) Uani 1 1 d . . . H7 H 0.2572 0.6438 0.1293 0.044 Uiso 1 1 calc R . . C8 C 0.2626(3) 0.9412(6) 0.0279(4) 0.0331(17) Uani 1 1 d . . . C9 C 0.3163(3) 0.9585(7) 0.0580(4) 0.0365(19) Uani 1 1 d . . . H9 H 0.3353 0.9165 0.0915 0.044 Uiso 1 1 calc R . . C10 C 0.3409(3) 1.0377(6) 0.0381(4) 0.0331(17) Uani 1 1 d . . . C11 C 0.3112(3) 1.0976(7) -0.0102(4) 0.040(2) Uani 1 1 d . . . H11 H 0.3273 1.1505 -0.0261 0.049 Uiso 1 1 calc R . . C12 C 0.2579(3) 1.0804(7) -0.0354(3) 0.0336(18) Uani 1 1 d . . . C25 C 0.1179(3) 0.3353(6) 0.1209(3) 0.0278(16) Uani 1 1 d . . . C26 C 0.0882(3) 0.2645(6) 0.0703(3) 0.0314(17) Uani 1 1 d . . . C27 C 0.1119(3) 0.1791(6) 0.0547(4) 0.0383(19) Uani 1 1 d . . . H27 H 0.1474 0.1639 0.0770 0.046 Uiso 1 1 calc R . . C28 C 0.0843(3) 0.1150(7) 0.0069(4) 0.043(2) Uani 1 1 d . . . H28 H 0.1014 0.0578 -0.0042 0.051 Uiso 1 1 calc R . . C29 C 0.0314(3) 0.1348(6) -0.0251(3) 0.0326(17) Uani 1 1 d . . . C30 C 0.0089(3) 0.2208(8) -0.0089(4) 0.047(2) Uani 1 1 d . . . H30 H -0.0266 0.2366 -0.0311 0.057 Uiso 1 1 calc R . . C31 C 0.0361(3) 0.2853(7) 0.0384(4) 0.043(2) Uani 1 1 d . . . H31 H 0.0193 0.3432 0.0490 0.052 Uiso 1 1 calc R . . C32 C 0.0015(3) 0.0647(6) -0.0754(4) 0.0334(17) Uani 1 1 d . . . C33 C -0.0525(3) 0.0768(6) -0.1033(4) 0.0330(17) Uani 1 1 d . . . H33 H -0.0704 0.1318 -0.0915 0.040 Uiso 1 1 calc R . . C34 C -0.0798(3) 0.0076(6) -0.1485(3) 0.0303(16) Uani 1 1 d . . . C35 C -0.0510(3) -0.0700(6) -0.1636(4) 0.0324(17) Uani 1 1 d . . . H35 H -0.0681 -0.1187 -0.1944 0.039 Uiso 1 1 calc R . . C36 C 0.0024(3) -0.0776(6) -0.1344(4) 0.0325(17) Uani 1 1 d . . . N2 N 0.2343(2) 1.0035(5) -0.0174(3) 0.0338(15) Uani 1 1 d . . . N4 N 0.0290(2) -0.0107(5) -0.0905(3) 0.0332(15) Uani 1 1 d . . . O1 O 0.1865(2) 0.5441(4) 0.1429(2) 0.0329(12) Uani 1 1 d . . . O5 O 0.1651(2) 0.3175(4) 0.1499(2) 0.0343(12) Uani 1 1 d . . . O6 O 0.0941(2) 0.4126(4) 0.1321(3) 0.0381(13) Uani 1 1 d . . . Co1 Co 0.17771(4) 0.44374(8) 0.20576(5) 0.0322(3) Uani 1 1 d . . . Co2 Co 0.08325(4) 0.56450(9) 0.17551(5) 0.0364(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C13 0.022(4) 0.047(5) 0.040(4) 0.016(4) 0.009(3) 0.005(3) C14 0.031(4) 0.049(5) 0.057(6) 0.029(5) 0.001(4) -0.006(4) C15 0.033(5) 0.047(5) 0.048(5) 0.012(4) -0.005(4) -0.003(4) C16 0.027(4) 0.038(4) 0.039(4) 0.010(3) 0.013(3) 0.006(3) C17 0.038(5) 0.034(4) 0.053(5) 0.009(4) 0.021(4) 0.001(4) C18 0.036(5) 0.049(5) 0.044(5) 0.008(4) 0.017(4) -0.004(4) C19 0.037(5) 0.043(5) 0.038(4) 0.001(4) 0.016(4) 0.011(4) C20 0.0297(19) 0.090(3) 0.056(2) -0.012(2) 0.0092(17) 0.0018(19) C21 0.0297(19) 0.090(3) 0.056(2) -0.012(2) 0.0092(17) 0.0018(19) C22 0.0297(19) 0.090(3) 0.056(2) -0.012(2) 0.0092(17) 0.0018(19) C23 0.0297(19) 0.090(3) 0.056(2) -0.012(2) 0.0092(17) 0.0018(19) C24 0.0297(19) 0.090(3) 0.056(2) -0.012(2) 0.0092(17) 0.0018(19) C37 0.019(4) 0.051(5) 0.036(4) -0.005(4) 0.007(3) 0.002(3) C38 0.028(4) 0.051(5) 0.047(5) -0.003(4) 0.007(4) -0.007(4) C39 0.016(4) 0.070(6) 0.036(4) 0.006(4) 0.008(3) 0.013(4) C40 0.026(4) 0.051(5) 0.040(5) 0.005(4) 0.009(3) 0.008(4) C41 0.041(5) 0.045(5) 0.051(5) 0.004(4) 0.023(4) 0.007(4) C42 0.028(4) 0.044(5) 0.045(5) -0.005(4) 0.015(3) -0.003(3) C43 0.026(4) 0.041(5) 0.042(4) 0.009(4) 0.012(3) 0.009(3) C44 0.019(3) 0.035(4) 0.031(4) -0.010(3) 0.006(3) -0.004(3) C45 0.034(4) 0.034(4) 0.040(4) -0.009(4) 0.005(3) -0.002(3) C46 0.034(4) 0.032(4) 0.047(5) -0.007(4) 0.005(4) 0.005(3) C47 0.023(4) 0.032(4) 0.043(4) -0.006(3) 0.006(3) -0.005(3) C48 0.027(4) 0.022(4) 0.047(5) -0.005(3) 0.008(3) 0.005(3) N1 0.0297(19) 0.090(3) 0.056(2) -0.012(2) 0.0092(17) 0.0018(19) N3 0.024(3) 0.029(3) 0.031(3) -0.004(3) 0.003(3) 0.004(3) O2 0.026(3) 0.041(3) 0.059(4) 0.012(3) 0.013(3) -0.004(2) O3 0.037(3) 0.051(4) 0.039(3) 0.013(3) 0.004(3) 0.012(3) O4 0.046(4) 0.041(3) 0.046(3) 0.013(3) 0.018(3) 0.007(3) O7 0.032(3) 0.043(3) 0.054(4) -0.006(3) 0.013(3) 0.003(3) O8 0.025(3) 0.057(4) 0.038(3) -0.007(3) 0.008(2) 0.006(3) C1 0.028(4) 0.031(4) 0.037(4) -0.008(3) 0.010(3) -0.009(3) C2 0.024(4) 0.029(4) 0.033(4) 0.000(3) 0.011(3) -0.002(3) C3 0.019(4) 0.047(5) 0.042(4) 0.005(4) 0.008(3) 0.002(3) C4 0.019(4) 0.042(5) 0.047(5) 0.014(4) 0.008(3) 0.010(3) C5 0.020(3) 0.038(4) 0.034(4) 0.009(3) 0.007(3) -0.002(3) C6 0.015(3) 0.049(5) 0.051(5) 0.018(4) 0.007(3) -0.003(3) C7 0.022(4) 0.041(5) 0.045(5) 0.015(4) 0.009(3) -0.001(3) C8 0.018(3) 0.039(4) 0.039(4) 0.009(4) 0.006(3) 0.001(3) C9 0.023(4) 0.048(5) 0.037(4) 0.013(4) 0.007(3) -0.001(3) C10 0.021(4) 0.042(5) 0.034(4) 0.008(3) 0.006(3) -0.003(3) C11 0.028(4) 0.054(5) 0.040(4) 0.020(4) 0.013(3) -0.007(4) C12 0.028(4) 0.044(5) 0.028(4) 0.011(3) 0.008(3) 0.004(3) C25 0.026(4) 0.029(4) 0.027(4) -0.003(3) 0.007(3) -0.012(3) C26 0.031(4) 0.032(4) 0.029(4) -0.004(3) 0.007(3) -0.015(3) C27 0.025(4) 0.037(4) 0.043(5) -0.004(4) -0.001(3) -0.001(3) C28 0.041(5) 0.035(4) 0.045(5) -0.009(4) 0.005(4) 0.003(4) C29 0.026(4) 0.039(4) 0.033(4) -0.006(3) 0.010(3) -0.008(3) C30 0.022(4) 0.062(6) 0.048(5) -0.024(4) -0.001(4) -0.010(4) C31 0.026(4) 0.052(5) 0.050(5) -0.021(4) 0.011(4) -0.006(4) C32 0.024(4) 0.039(4) 0.035(4) -0.006(3) 0.006(3) -0.010(3) C33 0.023(4) 0.033(4) 0.042(4) -0.011(3) 0.009(3) -0.006(3) C34 0.026(4) 0.032(4) 0.030(4) 0.000(3) 0.005(3) -0.006(3) C35 0.027(4) 0.032(4) 0.037(4) -0.008(3) 0.009(3) -0.007(3) C36 0.026(4) 0.036(4) 0.035(4) -0.007(3) 0.010(3) -0.004(3) N2 0.022(3) 0.040(4) 0.038(4) 0.011(3) 0.007(3) -0.004(3) N4 0.018(3) 0.041(4) 0.040(4) -0.008(3) 0.007(3) -0.006(3) O1 0.028(3) 0.035(3) 0.033(3) 0.006(2) 0.007(2) -0.008(2) O5 0.024(3) 0.034(3) 0.041(3) -0.008(2) 0.006(2) -0.006(2) O6 0.032(3) 0.038(3) 0.038(3) -0.007(3) 0.005(2) -0.010(2) Co1 0.0255(6) 0.0330(6) 0.0340(6) 0.0020(4) 0.0046(4) -0.0099(4) Co2 0.0272(6) 0.0406(7) 0.0387(6) 0.0009(5) 0.0075(5) -0.0057(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C13 C14 1.373(12) . ? C13 C18 1.398(12) . ? C13 C12 1.486(10) . ? C14 C15 1.379(11) . ? C14 H14 0.9500 . ? C15 C16 1.393(12) . ? C15 H15 0.9500 . ? C16 C17 1.391(12) . ? C16 C19 1.495(11) . ? C17 C18 1.353(12) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O3 1.241(10) . ? C19 O4 1.290(10) . ? C19 Co2 2.474(8) 6_575 ? C20 C24 1.329(14) . ? C20 C21 1.398(14) . ? C20 C10 1.463(12) . ? C21 C22 1.377(13) . ? C21 H21 0.9500 . ? C22 N1 1.301(13) . ? C22 H22 0.9500 . ? C23 N1 1.244(13) . ? C23 C24 1.406(13) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C37 C38 1.394(11) . ? C37 C42 1.397(12) . ? C37 C36 1.479(11) . ? C38 C39 1.402(12) . ? C38 H38 0.9500 . ? C39 C40 1.388(13) . ? C39 H39 0.9500 . ? C40 C41 1.379(12) . ? C40 C43 1.519(12) . ? C41 C42 1.374(12) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 O8 1.245(9) . ? C43 O7 1.279(10) . ? C44 C45 1.371(11) . ? C44 C48 1.411(10) . ? C44 C34 1.495(10) . ? C45 C46 1.376(11) . ? C45 H45 0.9500 . ? C46 N3 1.340(10) . ? C46 H46 0.9500 . ? C47 N3 1.348(10) . ? C47 C48 1.357(10) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? N1 Co2 2.082(8) 3 ? N3 Co1 2.068(6) 8_455 ? O2 C1 1.278(9) . ? O2 Co2 2.060(6) . ? O3 Co2 2.088(6) 6_575 ? O4 Co2 2.258(6) 6_575 ? O4 Co1 2.273(6) 6_575 ? O7 Co2 2.056(6) 6 ? O8 Co1 2.011(6) 6 ? C1 O1 1.249(9) . ? C1 C2 1.511(10) . ? C2 C3 1.390(11) . ? C2 C7 1.392(10) . ? C3 C4 1.392(12) . ? C3 H3 0.9500 . ? C4 C5 1.414(10) . ? C4 H4 0.9500 . ? C5 C6 1.381(11) . ? C5 C8 1.482(11) . ? C6 C7 1.402(11) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 N2 1.347(10) . ? C8 C9 1.408(10) . ? C9 C10 1.382(11) . ? C9 H9 0.9500 . ? C10 C11 1.383(11) . ? C11 C12 1.385(11) . ? C11 H11 0.9500 . ? C12 N2 1.320(10) . ? C25 O5 1.253(9) . ? C25 O6 1.261(9) . ? C25 C26 1.497(10) . ? C26 C27 1.383(12) . ? C26 C31 1.386(11) . ? C27 C28 1.391(11) . ? C27 H27 0.9500 . ? C28 C29 1.404(11) . ? C28 H28 0.9500 . ? C29 C30 1.377(12) . ? C29 C32 1.489(10) . ? C30 C31 1.384(11) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 N4 1.341(10) . ? C32 C33 1.399(11) . ? C33 C34 1.392(10) . ? C33 H33 0.9500 . ? C34 C35 1.385(11) . ? C35 C36 1.383(11) . ? C35 H35 0.9500 . ? C36 N4 1.351(10) . ? O1 Co1 2.030(5) . ? O5 Co1 2.041(5) . ? O6 Co2 2.267(6) . ? O6 Co1 2.381(5) . ? Co1 O8 2.011(6) 6_556 ? Co1 N3 2.068(6) 8_556 ? Co1 O4 2.273(6) 6_576 ? Co1 Co2 2.8760(16) . ? Co2 O7 2.056(6) 6_556 ? Co2 N1 2.082(8) 3_445 ? Co2 O3 2.088(6) 6_576 ? Co2 O4 2.258(6) 6_576 ? Co2 C19 2.474(8) 6_576 ? 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 C14 C13 C18 118.2(8) . . ? C14 C13 C12 120.3(8) . . ? C18 C13 C12 121.4(8) . . ? C13 C14 C15 121.6(8) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C16 119.1(8) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 119.4(7) . . ? C17 C16 C19 119.6(7) . . ? C15 C16 C19 120.9(8) . . ? C18 C17 C16 120.2(8) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C13 121.3(8) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? O3 C19 O4 122.4(8) . . ? O3 C19 C16 119.9(8) . . ? O4 C19 C16 117.7(7) . . ? O3 C19 Co2 57.5(4) . 6_575 ? O4 C19 Co2 65.1(4) . 6_575 ? C16 C19 Co2 175.4(6) . 6_575 ? C24 C20 C21 114.9(9) . . ? C24 C20 C10 123.7(9) . . ? C21 C20 C10 121.2(9) . . ? C22 C21 C20 119.7(10) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? N1 C22 C21 122.6(10) . . ? N1 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? N1 C23 C24 123.3(10) . . ? N1 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C20 C24 C23 120.7(10) . . ? C20 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C38 C37 C42 118.0(8) . . ? C38 C37 C36 121.2(8) . . ? C42 C37 C36 120.7(7) . . ? C37 C38 C39 119.7(8) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C40 C39 C38 121.5(8) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C41 C40 C39 118.0(8) . . ? C41 C40 C43 119.8(8) . . ? C39 C40 C43 121.9(8) . . ? C42 C41 C40 121.3(9) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C41 C42 C37 121.3(8) . . ? C41 C42 H42 119.3 . . ? C37 C42 H42 119.3 . . ? O8 C43 O7 125.9(8) . . ? O8 C43 C40 116.7(8) . . ? O7 C43 C40 117.0(7) . . ? C45 C44 C48 117.4(7) . . ? C45 C44 C34 122.0(7) . . ? C48 C44 C34 120.6(7) . . ? C44 C45 C46 119.8(7) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? N3 C46 C45 123.2(7) . . ? N3 C46 H46 118.4 . . ? C45 C46 H46 118.4 . . ? N3 C47 C48 123.6(7) . . ? N3 C47 H47 118.2 . . ? C48 C47 H47 118.2 . . ? C47 C48 C44 119.1(7) . . ? C47 C48 H48 120.5 . . ? C44 C48 H48 120.5 . . ? C23 N1 C22 118.5(9) . . ? C23 N1 Co2 120.9(7) . 3 ? C22 N1 Co2 119.9(7) . 3 ? C46 N3 C47 116.8(6) . . ? C46 N3 Co1 124.0(5) . 8_455 ? C47 N3 Co1 119.2(5) . 8_455 ? C1 O2 Co2 119.7(5) . . ? C19 O3 Co2 92.4(5) . 6_575 ? C19 O4 Co2 83.7(5) . 6_575 ? C19 O4 Co1 161.4(6) . 6_575 ? Co2 O4 Co1 78.81(18) 6_575 6_575 ? C43 O7 Co2 128.7(5) . 6 ? C43 O8 Co1 122.6(6) . 6 ? O1 C1 O2 125.4(7) . . ? O1 C1 C2 116.5(7) . . ? O2 C1 C2 118.0(7) . . ? C3 C2 C7 120.1(7) . . ? C3 C2 C1 122.2(7) . . ? C7 C2 C1 117.4(7) . . ? C2 C3 C4 119.8(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 121.0(7) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 118.0(7) . . ? C6 C5 C8 120.3(6) . . ? C4 C5 C8 121.7(7) . . ? C5 C6 C7 121.6(7) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C2 C7 C6 119.4(7) . . ? C2 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? N2 C8 C9 121.4(7) . . ? N2 C8 C5 117.4(6) . . ? C9 C8 C5 121.2(7) . . ? C10 C9 C8 119.0(7) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 118.1(7) . . ? C9 C10 C20 119.7(8) . . ? C11 C10 C20 122.3(8) . . ? C10 C11 C12 120.0(7) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? N2 C12 C11 122.1(7) . . ? N2 C12 C13 117.4(7) . . ? C11 C12 C13 120.4(7) . . ? O5 C25 O6 122.1(6) . . ? O5 C25 C26 120.0(7) . . ? O6 C25 C26 117.9(7) . . ? C27 C26 C31 119.4(7) . . ? C27 C26 C25 121.2(7) . . ? C31 C26 C25 119.4(7) . . ? C26 C27 C28 120.8(7) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C29 120.1(8) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 117.9(7) . . ? C30 C29 C32 122.0(7) . . ? C28 C29 C32 120.1(7) . . ? C29 C30 C31 122.3(8) . . ? C29 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? C30 C31 C26 119.5(8) . . ? C30 C31 H31 120.3 . . ? C26 C31 H31 120.3 . . ? N4 C32 C33 122.9(7) . . ? N4 C32 C29 116.3(7) . . ? C33 C32 C29 120.7(7) . . ? C34 C33 C32 119.5(7) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C35 C34 C33 116.9(7) . . ? C35 C34 C44 122.6(7) . . ? C33 C34 C44 120.4(7) . . ? C36 C35 C34 120.8(7) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? N4 C36 C35 122.4(7) . . ? N4 C36 C37 117.7(7) . . ? C35 C36 C37 119.9(7) . . ? C12 N2 C8 119.3(6) . . ? C32 N4 C36 117.4(6) . . ? C1 O1 Co1 131.0(5) . . ? C25 O5 Co1 97.2(5) . . ? C25 O6 Co2 157.8(5) . . ? C25 O6 Co1 81.6(4) . . ? Co2 O6 Co1 76.42(16) . . ? O8 Co1 O1 162.2(2) 6_556 . ? O8 Co1 O5 93.1(2) 6_556 . ? O1 Co1 O5 94.6(2) . . ? O8 Co1 N3 100.5(2) 6_556 8_556 ? O1 Co1 N3 91.7(2) . 8_556 ? O5 Co1 N3 111.0(2) . 8_556 ? O8 Co1 O4 86.6(2) 6_556 6_576 ? O1 Co1 O4 80.6(2) . 6_576 ? O5 Co1 O4 159.4(2) . 6_576 ? N3 Co1 O4 89.2(2) 8_556 6_576 ? O8 Co1 O6 86.2(2) 6_556 . ? O1 Co1 O6 84.0(2) . . ? O5 Co1 O6 59.1(2) . . ? N3 Co1 O6 168.7(2) 8_556 . ? O4 Co1 O6 100.4(2) 6_576 . ? O8 Co1 Co2 84.67(17) 6_556 . ? O1 Co1 Co2 77.66(16) . . ? O5 Co1 Co2 109.08(15) . . ? N3 Co1 Co2 139.18(18) 8_556 . ? O4 Co1 Co2 50.36(16) 6_576 . ? O6 Co1 Co2 50.01(14) . . ? O7 Co2 O2 161.4(2) 6_556 . ? O7 Co2 N1 96.0(3) 6_556 3_445 ? O2 Co2 N1 97.1(3) . 3_445 ? O7 Co2 O3 93.1(2) 6_556 6_576 ? O2 Co2 O3 97.5(3) . 6_576 ? N1 Co2 O3 100.2(3) 3_445 6_576 ? O7 Co2 O4 83.4(2) 6_556 6_576 ? O2 Co2 O4 88.4(2) . 6_576 ? N1 Co2 O4 161.2(3) 3_445 6_576 ? O3 Co2 O4 61.2(2) 6_576 6_576 ? O7 Co2 O6 81.1(2) 6_556 . ? O2 Co2 O6 84.9(2) . . ? N1 Co2 O6 94.0(3) 3_445 . ? O3 Co2 O6 165.2(2) 6_576 . ? O4 Co2 O6 104.4(2) 6_576 . ? O7 Co2 C19 86.5(3) 6_556 6_576 ? O2 Co2 C19 95.0(3) . 6_576 ? N1 Co2 C19 130.1(3) 3_445 6_576 ? O3 Co2 C19 30.1(3) 6_576 6_576 ? O4 Co2 C19 31.2(2) 6_576 6_576 ? O6 Co2 C19 135.3(3) . 6_576 ? O7 Co2 Co1 77.61(17) 6_556 . ? O2 Co2 Co1 84.30(16) . . ? N1 Co2 Co1 147.4(3) 3_445 . ? O3 Co2 Co1 111.99(17) 6_576 . ? O4 Co2 Co1 50.83(15) 6_576 . ? O6 Co2 Co1 53.57(14) . . ? C19 Co2 Co1 81.9(2) 6_576 . ? 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 C18 C13 C14 C15 1.0(15) . . . . ? C12 C13 C14 C15 -177.6(9) . . . . ? C13 C14 C15 C16 3.0(16) . . . . ? C14 C15 C16 C17 -4.9(14) . . . . ? C14 C15 C16 C19 176.4(9) . . . . ? C15 C16 C17 C18 2.8(13) . . . . ? C19 C16 C17 C18 -178.4(8) . . . . ? C16 C17 C18 C13 1.2(13) . . . . ? C14 C13 C18 C17 -3.2(14) . . . . ? C12 C13 C18 C17 175.4(8) . . . . ? C17 C16 C19 O3 -161.3(8) . . . . ? C15 C16 C19 O3 17.4(12) . . . . ? C17 C16 C19 O4 19.7(11) . . . . ? C15 C16 C19 O4 -161.6(8) . . . . ? C17 C16 C19 Co2 -107(8) . . . 6_575 ? C15 C16 C19 Co2 71(8) . . . 6_575 ? C24 C20 C21 C22 -2.3(18) . . . . ? C10 C20 C21 C22 -176.4(11) . . . . ? C20 C21 C22 N1 1(2) . . . . ? C21 C20 C24 C23 5.3(18) . . . . ? C10 C20 C24 C23 179.2(11) . . . . ? N1 C23 C24 C20 -8(2) . . . . ? C42 C37 C38 C39 3.2(12) . . . . ? C36 C37 C38 C39 -173.5(8) . . . . ? C37 C38 C39 C40 0.0(13) . . . . ? C38 C39 C40 C41 -3.8(12) . . . . ? C38 C39 C40 C43 169.7(8) . . . . ? C39 C40 C41 C42 4.5(13) . . . . ? C43 C40 C41 C42 -169.2(8) . . . . ? C40 C41 C42 C37 -1.3(14) . . . . ? C38 C37 C42 C41 -2.6(13) . . . . ? C36 C37 C42 C41 174.2(8) . . . . ? C41 C40 C43 O8 -171.7(8) . . . . ? C39 C40 C43 O8 14.9(12) . . . . ? C41 C40 C43 O7 14.6(12) . . . . ? C39 C40 C43 O7 -158.8(7) . . . . ? C48 C44 C45 C46 -2.8(12) . . . . ? C34 C44 C45 C46 178.4(8) . . . . ? C44 C45 C46 N3 -0.1(14) . . . . ? N3 C47 C48 C44 -1.4(13) . . . . ? C45 C44 C48 C47 3.5(12) . . . . ? C34 C44 C48 C47 -177.8(7) . . . . ? C24 C23 N1 C22 5.8(19) . . . . ? C24 C23 N1 Co2 -164.7(9) . . . 3 ? C21 C22 N1 C23 -2.6(19) . . . . ? C21 C22 N1 Co2 168.0(9) . . . 3 ? C45 C46 N3 C47 2.2(13) . . . . ? C45 C46 N3 Co1 -175.6(7) . . . 8_455 ? C48 C47 N3 C46 -1.5(12) . . . . ? C48 C47 N3 Co1 176.4(7) . . . 8_455 ? O4 C19 O3 Co2 -5.4(8) . . . 6_575 ? C16 C19 O3 Co2 175.6(7) . . . 6_575 ? O3 C19 O4 Co2 5.0(8) . . . 6_575 ? C16 C19 O4 Co2 -176.0(7) . . . 6_575 ? O3 C19 O4 Co1 25(2) . . . 6_575 ? C16 C19 O4 Co1 -156.3(14) . . . 6_575 ? Co2 C19 O4 Co1 19.7(17) 6_575 . . 6_575 ? O8 C43 O7 Co2 -6.9(12) . . . 6 ? C40 C43 O7 Co2 166.1(5) . . . 6 ? O7 C43 O8 Co1 8.7(12) . . . 6 ? C40 C43 O8 Co1 -164.3(5) . . . 6 ? Co2 O2 C1 O1 17.7(10) . . . . ? Co2 O2 C1 C2 -157.0(5) . . . . ? O1 C1 C2 C3 170.7(7) . . . . ? O2 C1 C2 C3 -14.1(11) . . . . ? O1 C1 C2 C7 -15.3(10) . . . . ? O2 C1 C2 C7 159.9(8) . . . . ? C7 C2 C3 C4 -2.4(12) . . . . ? C1 C2 C3 C4 171.5(7) . . . . ? C2 C3 C4 C5 -0.8(13) . . . . ? C3 C4 C5 C6 3.8(13) . . . . ? C3 C4 C5 C8 -176.6(8) . . . . ? C4 C5 C6 C7 -3.9(13) . . . . ? C8 C5 C6 C7 176.5(8) . . . . ? C3 C2 C7 C6 2.4(13) . . . . ? C1 C2 C7 C6 -171.8(8) . . . . ? C5 C6 C7 C2 0.9(14) . . . . ? C6 C5 C8 N2 167.3(8) . . . . ? C4 C5 C8 N2 -12.3(12) . . . . ? C6 C5 C8 C9 -13.7(13) . . . . ? C4 C5 C8 C9 166.7(8) . . . . ? N2 C8 C9 C10 -3.8(13) . . . . ? C5 C8 C9 C10 177.3(8) . . . . ? C8 C9 C10 C11 1.1(13) . . . . ? C8 C9 C10 C20 -178.4(8) . . . . ? C24 C20 C10 C9 -70.6(15) . . . . ? C21 C20 C10 C9 103.0(13) . . . . ? C24 C20 C10 C11 109.9(14) . . . . ? C21 C20 C10 C11 -76.5(14) . . . . ? C9 C10 C11 C12 2.8(13) . . . . ? C20 C10 C11 C12 -177.7(9) . . . . ? C10 C11 C12 N2 -4.4(14) . . . . ? C10 C11 C12 C13 177.9(8) . . . . ? C14 C13 C12 N2 -24.9(12) . . . . ? C18 C13 C12 N2 156.5(8) . . . . ? C14 C13 C12 C11 152.9(9) . . . . ? C18 C13 C12 C11 -25.7(13) . . . . ? O5 C25 C26 C27 0.0(11) . . . . ? O6 C25 C26 C27 179.1(7) . . . . ? O5 C25 C26 C31 -179.8(8) . . . . ? O6 C25 C26 C31 -0.7(11) . . . . ? C31 C26 C27 C28 1.1(13) . . . . ? C25 C26 C27 C28 -178.6(8) . . . . ? C26 C27 C28 C29 -2.0(14) . . . . ? C27 C28 C29 C30 2.4(13) . . . . ? C27 C28 C29 C32 -178.5(8) . . . . ? C28 C29 C30 C31 -2.2(14) . . . . ? C32 C29 C30 C31 178.8(9) . . . . ? C29 C30 C31 C26 1.3(15) . . . . ? C27 C26 C31 C30 -0.8(13) . . . . ? C25 C26 C31 C30 179.0(8) . . . . ? C30 C29 C32 N4 173.9(8) . . . . ? C28 C29 C32 N4 -5.1(12) . . . . ? C30 C29 C32 C33 -7.9(13) . . . . ? C28 C29 C32 C33 173.1(8) . . . . ? N4 C32 C33 C34 0.7(13) . . . . ? C29 C32 C33 C34 -177.4(7) . . . . ? C32 C33 C34 C35 -0.6(12) . . . . ? C32 C33 C34 C44 -178.2(7) . . . . ? C45 C44 C34 C35 -152.1(8) . . . . ? C48 C44 C34 C35 29.2(12) . . . . ? C45 C44 C34 C33 25.4(12) . . . . ? C48 C44 C34 C33 -153.4(8) . . . . ? C33 C34 C35 C36 0.4(12) . . . . ? C44 C34 C35 C36 177.9(7) . . . . ? C34 C35 C36 N4 -0.3(13) . . . . ? C34 C35 C36 C37 -178.6(7) . . . . ? C38 C37 C36 N4 -43.3(12) . . . . ? C42 C37 C36 N4 140.1(8) . . . . ? C38 C37 C36 C35 135.2(8) . . . . ? C42 C37 C36 C35 -41.4(12) . . . . ? C11 C12 N2 C8 1.8(13) . . . . ? C13 C12 N2 C8 179.5(8) . . . . ? C9 C8 N2 C12 2.3(12) . . . . ? C5 C8 N2 C12 -178.7(7) . . . . ? C33 C32 N4 C36 -0.6(12) . . . . ? C29 C32 N4 C36 177.6(7) . . . . ? C35 C36 N4 C32 0.4(12) . . . . ? C37 C36 N4 C32 178.8(7) . . . . ? O2 C1 O1 Co1 -11.9(11) . . . . ? C2 C1 O1 Co1 162.8(5) . . . . ? O6 C25 O5 Co1 -0.9(8) . . . . ? C26 C25 O5 Co1 178.2(6) . . . . ? O5 C25 O6 Co2 7.6(19) . . . . ? C26 C25 O6 Co2 -171.5(10) . . . . ? O5 C25 O6 Co1 0.8(7) . . . . ? C26 C25 O6 Co1 -178.3(6) . . . . ? C1 O1 Co1 O8 -5.5(12) . . . 6_556 ? C1 O1 Co1 O5 109.8(6) . . . . ? C1 O1 Co1 N3 -139.0(7) . . . 8_556 ? C1 O1 Co1 O4 -50.1(6) . . . 6_576 ? C1 O1 Co1 O6 51.5(6) . . . . ? C1 O1 Co1 Co2 1.2(6) . . . . ? C25 O5 Co1 O8 84.1(5) . . . 6_556 ? C25 O5 Co1 O1 -79.8(5) . . . . ? C25 O5 Co1 N3 -173.4(4) . . . 8_556 ? C25 O5 Co1 O4 -4.6(9) . . . 6_576 ? C25 O5 Co1 O6 0.5(4) . . . . ? C25 O5 Co1 Co2 -1.3(5) . . . . ? C25 O6 Co1 O8 -96.4(4) . . . 6_556 ? Co2 O6 Co1 O8 86.2(2) . . . 6_556 ? C25 O6 Co1 O1 98.5(4) . . . . ? Co2 O6 Co1 O1 -78.9(2) . . . . ? C25 O6 Co1 O5 -0.5(4) . . . . ? Co2 O6 Co1 O5 -177.8(3) . . . . ? C25 O6 Co1 N3 30.1(13) . . . 8_556 ? Co2 O6 Co1 N3 -147.3(11) . . . 8_556 ? C25 O6 Co1 O4 177.7(4) . . . 6_576 ? Co2 O6 Co1 O4 0.4(2) . . . 6_576 ? C25 O6 Co1 Co2 177.4(5) . . . . ? C1 O2 Co2 O7 -25.0(11) . . . 6_556 ? C1 O2 Co2 N1 -159.4(6) . . . 3_445 ? C1 O2 Co2 O3 99.3(6) . . . 6_576 ? C1 O2 Co2 O4 38.6(6) . . . 6_576 ? C1 O2 Co2 O6 -66.0(6) . . . . ? C1 O2 Co2 C19 69.2(6) . . . 6_576 ? C1 O2 Co2 Co1 -12.1(6) . . . . ? C25 O6 Co2 O7 -88.0(14) . . . 6_556 ? Co1 O6 Co2 O7 -81.1(2) . . . 6_556 ? C25 O6 Co2 O2 79.8(14) . . . . ? Co1 O6 Co2 O2 86.69(19) . . . . ? C25 O6 Co2 N1 176.5(14) . . . 3_445 ? Co1 O6 Co2 N1 -176.6(3) . . . 3_445 ? C25 O6 Co2 O3 -20(2) . . . 6_576 ? Co1 O6 Co2 O3 -13.5(10) . . . 6_576 ? C25 O6 Co2 O4 -7.3(14) . . . 6_576 ? Co1 O6 Co2 O4 -0.4(2) . . . 6_576 ? C25 O6 Co2 C19 -12.2(15) . . . 6_576 ? Co1 O6 Co2 C19 -5.3(4) . . . 6_576 ? C25 O6 Co2 Co1 -6.9(13) . . . . ? O8 Co1 Co2 O7 -1.5(2) 6_556 . . 6_556 ? O1 Co1 Co2 O7 -179.4(2) . . . 6_556 ? O5 Co1 Co2 O7 90.0(2) . . . 6_556 ? N3 Co1 Co2 O7 -101.3(3) 8_556 . . 6_556 ? O4 Co1 Co2 O7 -91.5(3) 6_576 . . 6_556 ? O6 Co1 Co2 O7 88.0(3) . . . 6_556 ? O8 Co1 Co2 O2 -177.3(2) 6_556 . . . ? O1 Co1 Co2 O2 4.7(2) . . . . ? O5 Co1 Co2 O2 -85.9(2) . . . . ? N3 Co1 Co2 O2 82.8(3) 8_556 . . . ? O4 Co1 Co2 O2 92.6(3) 6_576 . . . ? O6 Co1 Co2 O2 -87.8(3) . . . . ? O8 Co1 Co2 N1 -83.1(5) 6_556 . . 3_445 ? O1 Co1 Co2 N1 98.9(5) . . . 3_445 ? O5 Co1 Co2 N1 8.3(5) . . . 3_445 ? N3 Co1 Co2 N1 177.0(6) 8_556 . . 3_445 ? O4 Co1 Co2 N1 -173.2(5) 6_576 . . 3_445 ? O6 Co1 Co2 N1 6.4(5) . . . 3_445 ? O8 Co1 Co2 O3 86.8(3) 6_556 . . 6_576 ? O1 Co1 Co2 O3 -91.1(2) . . . 6_576 ? O5 Co1 Co2 O3 178.3(3) . . . 6_576 ? N3 Co1 Co2 O3 -13.0(3) 8_556 . . 6_576 ? O4 Co1 Co2 O3 -3.2(3) 6_576 . . 6_576 ? O6 Co1 Co2 O3 176.3(3) . . . 6_576 ? O8 Co1 Co2 O4 90.0(3) 6_556 . . 6_576 ? O1 Co1 Co2 O4 -87.9(3) . . . 6_576 ? O5 Co1 Co2 O4 -178.5(3) . . . 6_576 ? N3 Co1 Co2 O4 -9.8(3) 8_556 . . 6_576 ? O6 Co1 Co2 O4 179.5(3) . . . 6_576 ? O8 Co1 Co2 O6 -89.5(3) 6_556 . . . ? O1 Co1 Co2 O6 92.6(2) . . . . ? O5 Co1 Co2 O6 2.0(2) . . . . ? N3 Co1 Co2 O6 170.7(3) 8_556 . . . ? O4 Co1 Co2 O6 -179.5(3) 6_576 . . . ? O8 Co1 Co2 C19 86.8(3) 6_556 . . 6_576 ? O1 Co1 Co2 C19 -91.2(2) . . . 6_576 ? O5 Co1 Co2 C19 178.2(3) . . . 6_576 ? N3 Co1 Co2 C19 -13.1(3) 8_556 . . 6_576 ? O4 Co1 Co2 C19 -3.3(3) 6_576 . . 6_576 ? O6 Co1 Co2 C19 176.2(3) . . . 6_576 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.745 _refine_diff_density_min -1.536 _refine_diff_density_rms 0.158 #===END #========================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 870232' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H62 N8 Ni O14' _chemical_formula_weight 1177.89 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number No.14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.5082(4) _cell_length_b 17.6296(9) _cell_length_c 21.3793(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.2160(10) _cell_angle_gamma 90.00 _cell_volume 2818.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9060 _exptl_absorpt_correction_T_max 0.9283 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15579 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.10 _reflns_number_total 5598 _reflns_number_gt 3822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0662P)^2^+1.3029P] 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 5598 _refine_ls_number_parameters 385 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 C19 C 0.5475(4) 1.01454(16) -0.35948(14) 0.0289(7) Uani 1 1 d . . . C20 C 0.2174(4) 0.75857(15) -0.02404(13) 0.0255(6) Uani 1 1 d . . . C21 C 0.2916(4) 0.69790(17) -0.05459(14) 0.0311(7) Uani 1 1 d . . . H21 H 0.3800 0.7066 -0.0829 0.037 Uiso 1 1 calc R . . C22 C 0.2350(4) 0.62497(16) -0.04326(14) 0.0310(7) Uani 1 1 d . . . H22 H 0.2869 0.5843 -0.0644 0.037 Uiso 1 1 calc R . . C23 C 0.0482(4) 0.66696(16) 0.02763(14) 0.0289(7) Uani 1 1 d . . . H23 H -0.0353 0.6564 0.0573 0.035 Uiso 1 1 calc R . . C24 C 0.0977(4) 0.74091(16) 0.01968(13) 0.0276(6) Uani 1 1 d . . . H24 H 0.0503 0.7799 0.0439 0.033 Uiso 1 1 calc R . . C25 C 0.3356(6) 0.6416(3) 0.1750(2) 0.0789(15) Uani 1 1 d . . . H25A H 0.3032 0.6798 0.2053 0.118 Uiso 1 1 calc R . . H25B H 0.3901 0.5978 0.1975 0.118 Uiso 1 1 calc R . . H25C H 0.2280 0.6253 0.1491 0.118 Uiso 1 1 calc R . . C26 C 0.5034(6) 0.7535(2) 0.1426(2) 0.0722(13) Uani 1 1 d . . . H26A H 0.4443 0.7739 0.1780 0.108 Uiso 1 1 calc R . . H26B H 0.4610 0.7807 0.1041 0.108 Uiso 1 1 calc R . . H26C H 0.6331 0.7599 0.1507 0.108 Uiso 1 1 calc R . . C27 C 0.5264(5) 0.6332(2) 0.09036(17) 0.0455(9) Uani 1 1 d . . . H27 H 0.4878 0.5820 0.0859 0.055 Uiso 1 1 calc R . . C28 C 1.0251(11) 1.2246(3) -0.2432(3) 0.128(3) Uani 1 1 d . . . H28A H 1.0608 1.2392 -0.2845 0.192 Uiso 1 1 calc R . . H28B H 1.1026 1.2501 -0.2103 0.192 Uiso 1 1 calc R . . H28C H 0.9006 1.2396 -0.2400 0.192 Uiso 1 1 calc R . . C29 C 1.1002(7) 1.1030(3) -0.2882(2) 0.0865(16) Uani 1 1 d . . . H29A H 1.1233 1.1385 -0.3218 0.130 Uiso 1 1 calc R . . H29B H 1.0070 1.0670 -0.3037 0.130 Uiso 1 1 calc R . . H29C H 1.2102 1.0753 -0.2747 0.130 Uiso 1 1 calc R . . C30 C 1.0005(7) 1.1124(3) -0.1843(2) 0.0747(14) Uani 1 1 d . . . H30 H 1.0234 1.0596 -0.1801 0.090 Uiso 1 1 calc R . . N2 N 0.1115(3) 0.60855(13) -0.00427(11) 0.0279(6) Uani 1 1 d . . . N3 N 0.4618(4) 0.67391(17) 0.13516(14) 0.0476(8) Uani 1 1 d . . . N4 N 1.0417(4) 1.14463(17) -0.23571(14) 0.0489(8) Uani 1 1 d . . . O1W O 0.2583(3) 0.45804(13) 0.02073(11) 0.0354(5) Uani 1 1 d . . . O2 O 0.6724(3) 1.06188(12) -0.36053(10) 0.0386(5) Uani 1 1 d . . . O1 O 0.4692(3) 0.98235(11) -0.40659(9) 0.0308(5) Uani 1 1 d . . . O5 O 0.6320(3) 0.65620(14) 0.05418(12) 0.0521(7) Uani 1 1 d . . . O6 O 0.9351(5) 1.14367(18) -0.14097(14) 0.0859(11) Uani 1 1 d . . . H1B H 0.288(8) 0.426(3) 0.005(3) 0.129 Uiso 1 1 d . . . H1A H 0.256(8) 0.444(3) 0.057(3) 0.129 Uiso 1 1 d . . . H1O H 0.184(7) 1.3409(18) 0.126(3) 0.129 Uiso 1 1 d D . . C1 C 0.1528(4) 1.23468(18) 0.13466(15) 0.0367(8) Uani 1 1 d . . . C2 C 0.1917(4) 1.16667(17) 0.09741(14) 0.0306(7) Uani 1 1 d . . . C3 C 0.1417(4) 1.09556(17) 0.11715(14) 0.0309(7) Uani 1 1 d . . . H3 H 0.0902 1.0902 0.1559 0.037 Uiso 1 1 calc R . . C4 C 0.1666(4) 1.03231(17) 0.08056(13) 0.0296(7) Uani 1 1 d . . . H4 H 0.1326 0.9838 0.0946 0.036 Uiso 1 1 calc R . . C5 C 0.2409(4) 1.03882(16) 0.02346(13) 0.0254(6) Uani 1 1 d . . . C6 C 0.2899(4) 1.11088(16) 0.00406(14) 0.0297(7) Uani 1 1 d . . . H6 H 0.3398 1.1165 -0.0349 0.036 Uiso 1 1 calc R . . C7 C 0.2671(4) 1.17368(17) 0.04045(15) 0.0314(7) Uani 1 1 d . . . H7 H 0.3029 1.2222 0.0268 0.038 Uiso 1 1 calc R . . C8 C 0.2648(4) 0.97247(16) -0.01798(13) 0.0256(6) Uani 1 1 d . . . C9 C 0.2370(4) 0.89795(16) 0.00162(13) 0.0266(6) Uani 1 1 d . . . H9 H 0.2063 0.8879 0.0430 0.032 Uiso 1 1 calc R . . C10 C 0.2553(4) 0.83866(16) -0.04058(13) 0.0253(6) Uani 1 1 d . . . C11 C 0.3025(4) 0.85664(16) -0.10015(13) 0.0273(6) Uani 1 1 d . . . H11 H 0.3162 0.8177 -0.1300 0.033 Uiso 1 1 calc R . . C12 C 0.3295(4) 0.93172(15) -0.11572(13) 0.0251(6) Uani 1 1 d . . . C13 C 0.3806(4) 0.95357(16) -0.17868(13) 0.0263(6) Uani 1 1 d . . . C14 C 0.3263(4) 0.91094(16) -0.23200(13) 0.0298(7) Uani 1 1 d . . . H14 H 0.2522 0.8678 -0.2283 0.036 Uiso 1 1 calc R . . C15 C 0.3790(4) 0.93082(16) -0.29025(13) 0.0309(7) Uani 1 1 d . . . H15 H 0.3404 0.9013 -0.3261 0.037 Uiso 1 1 calc R . . C16 C 0.4882(4) 0.99375(16) -0.29654(13) 0.0265(6) Uani 1 1 d . . . C17 C 0.5403(4) 1.03687(17) -0.24346(13) 0.0308(7) Uani 1 1 d . . . H17 H 0.6142 1.0801 -0.2471 0.037 Uiso 1 1 calc R . . C18 C 0.4861(4) 1.01773(16) -0.18578(14) 0.0310(7) Uani 1 1 d . . . H18 H 0.5210 1.0485 -0.1503 0.037 Uiso 1 1 calc R . . N1 N 0.3115(3) 0.98922(13) -0.07524(11) 0.0258(5) Uani 1 1 d . . . O3 O 0.2300(4) 1.29676(13) 0.11417(12) 0.0522(7) Uani 1 1 d D . . O4 O 0.0591(4) 1.23486(13) 0.17796(11) 0.0521(7) Uani 1 1 d . . . Ni1 Ni 0.0000 0.5000 0.0000 0.02664(17) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C19 0.0419(18) 0.0208(16) 0.0248(16) 0.0038(12) 0.0084(13) 0.0050(13) C20 0.0347(16) 0.0211(15) 0.0203(14) -0.0002(11) 0.0013(12) -0.0011(12) C21 0.0412(19) 0.0272(16) 0.0265(16) 0.0020(12) 0.0117(14) 0.0005(14) C22 0.0439(19) 0.0237(16) 0.0269(16) -0.0022(12) 0.0107(14) 0.0019(14) C23 0.0404(18) 0.0226(15) 0.0249(15) 0.0005(12) 0.0097(13) -0.0015(13) C24 0.0379(17) 0.0210(15) 0.0248(15) -0.0009(11) 0.0074(13) 0.0022(13) C25 0.066(3) 0.112(4) 0.063(3) -0.018(3) 0.023(2) -0.027(3) C26 0.088(3) 0.053(3) 0.077(3) -0.016(2) 0.018(3) 0.002(2) C27 0.049(2) 0.042(2) 0.044(2) -0.0048(16) -0.0009(18) 0.0036(17) C28 0.231(8) 0.053(3) 0.096(4) 0.023(3) -0.001(5) -0.005(4) C29 0.087(4) 0.122(5) 0.053(3) 0.010(3) 0.021(2) 0.044(3) C30 0.110(4) 0.053(3) 0.067(3) 0.012(2) 0.040(3) 0.008(3) N2 0.0416(15) 0.0218(13) 0.0215(12) 0.0000(10) 0.0095(11) 0.0004(11) N3 0.0451(18) 0.054(2) 0.0448(18) -0.0101(14) 0.0114(14) -0.0016(15) N4 0.058(2) 0.0453(18) 0.0455(18) 0.0092(14) 0.0162(15) 0.0089(15) O1W 0.0455(14) 0.0307(13) 0.0315(12) 0.0003(10) 0.0118(11) 0.0020(11) O2 0.0572(15) 0.0309(12) 0.0292(12) 0.0009(9) 0.0117(10) -0.0118(11) O1 0.0493(13) 0.0237(11) 0.0202(11) -0.0010(8) 0.0074(9) -0.0003(9) O5 0.0528(16) 0.0559(17) 0.0498(16) -0.0040(12) 0.0164(13) 0.0112(13) O6 0.141(3) 0.070(2) 0.0541(19) -0.0101(15) 0.049(2) 0.007(2) C1 0.045(2) 0.0313(18) 0.0338(18) -0.0019(14) 0.0015(15) 0.0041(15) C2 0.0313(17) 0.0296(17) 0.0301(17) -0.0040(13) -0.0014(13) 0.0025(13) C3 0.0382(18) 0.0305(17) 0.0251(16) -0.0004(12) 0.0083(13) 0.0034(14) C4 0.0416(18) 0.0233(15) 0.0242(15) 0.0003(12) 0.0041(13) 0.0001(13) C5 0.0260(15) 0.0242(15) 0.0259(15) 0.0002(12) 0.0009(12) -0.0003(12) C6 0.0346(17) 0.0259(16) 0.0296(16) 0.0006(12) 0.0082(13) 0.0000(13) C7 0.0344(17) 0.0247(16) 0.0357(17) -0.0006(13) 0.0056(14) -0.0004(13) C8 0.0286(16) 0.0252(15) 0.0230(15) 0.0003(11) 0.0031(12) -0.0001(12) C9 0.0359(17) 0.0238(15) 0.0209(15) 0.0007(11) 0.0068(13) -0.0010(13) C10 0.0282(15) 0.0254(15) 0.0227(15) 0.0021(11) 0.0044(12) -0.0001(12) C11 0.0371(17) 0.0245(15) 0.0208(14) -0.0003(12) 0.0059(12) 0.0006(13) C12 0.0291(16) 0.0242(15) 0.0222(14) 0.0009(11) 0.0040(12) -0.0014(12) C13 0.0344(17) 0.0241(15) 0.0205(15) 0.0029(11) 0.0036(12) 0.0020(13) C14 0.0413(18) 0.0234(16) 0.0254(16) -0.0006(12) 0.0064(13) -0.0058(13) C15 0.0450(19) 0.0257(16) 0.0225(15) -0.0015(12) 0.0053(13) -0.0025(13) C16 0.0370(17) 0.0228(15) 0.0202(14) 0.0036(11) 0.0060(12) 0.0026(13) C17 0.0415(18) 0.0258(16) 0.0258(16) 0.0026(12) 0.0067(13) -0.0049(14) C18 0.0440(18) 0.0274(17) 0.0216(15) -0.0038(12) 0.0035(13) -0.0066(13) N1 0.0315(13) 0.0243(13) 0.0218(12) 0.0010(10) 0.0041(10) -0.0005(10) O3 0.0714(18) 0.0310(14) 0.0568(16) -0.0075(12) 0.0203(14) -0.0010(13) O4 0.0738(18) 0.0417(15) 0.0431(15) -0.0092(11) 0.0176(13) 0.0042(13) Ni1 0.0424(3) 0.0195(3) 0.0193(3) -0.0002(2) 0.0096(2) -0.0007(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 C19 O1 1.255(4) . ? C19 O2 1.257(4) . ? C19 C16 1.501(4) . ? C20 C24 1.390(4) . ? C20 C21 1.395(4) . ? C20 C10 1.489(4) . ? C21 C22 1.382(4) . ? C21 H21 0.9500 . ? C22 N2 1.334(4) . ? C22 H22 0.9500 . ? C23 N2 1.345(3) . ? C23 C24 1.370(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 N3 1.447(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 N3 1.443(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O5 1.226(4) . ? C27 N3 1.324(4) . ? C27 H27 0.9500 . ? C28 N4 1.423(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N4 1.442(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 O6 1.218(5) . ? C30 N4 1.299(5) . ? C30 H30 0.9500 . ? N2 Ni1 2.094(2) . ? O1W Ni1 2.086(2) . ? O1W H1B 0.70(6) . ? O1W H1A 0.81(6) . ? O1 Ni1 2.0548(19) 2_554 ? C1 O4 1.212(4) . ? C1 O3 1.331(4) . ? C1 C2 1.483(4) . ? C2 C3 1.385(4) . ? C2 C7 1.394(4) . ? C3 C4 1.385(4) . ? C3 H3 0.9500 . ? C4 C5 1.392(4) . ? C4 H4 0.9500 . ? C5 C6 1.396(4) . ? C5 C8 1.488(4) . ? C6 C7 1.373(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 N1 1.337(3) . ? C8 C9 1.400(4) . ? C9 C10 1.396(4) . ? C9 H9 0.9500 . ? C10 C11 1.390(4) . ? C11 C12 1.384(4) . ? C11 H11 0.9500 . ? C12 N1 1.348(3) . ? C12 C13 1.483(4) . ? C13 C14 1.395(4) . ? C13 C18 1.397(4) . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.393(4) . ? C15 H15 0.9500 . ? C16 C17 1.392(4) . ? C17 C18 1.375(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O3 H1O 0.894(19) . ? Ni1 O1 2.0548(19) 4_576 ? Ni1 O1 2.0548(19) 2_544 ? Ni1 O1W 2.086(2) 3_565 ? Ni1 N2 2.094(2) 3_565 ? 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 O1 C19 O2 125.6(3) . . ? O1 C19 C16 117.0(3) . . ? O2 C19 C16 117.4(3) . . ? C24 C20 C21 117.0(3) . . ? C24 C20 C10 121.4(2) . . ? C21 C20 C10 121.5(3) . . ? C22 C21 C20 119.3(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? N2 C22 C21 123.6(3) . . ? N2 C22 H22 118.2 . . ? C21 C22 H22 118.2 . . ? N2 C23 C24 123.6(3) . . ? N2 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C20 119.7(3) . . ? C23 C24 H24 120.1 . . ? C20 C24 H24 120.1 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O5 C27 N3 125.2(4) . . ? O5 C27 H27 117.4 . . ? N3 C27 H27 117.4 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O6 C30 N4 126.1(4) . . ? O6 C30 H30 116.9 . . ? N4 C30 H30 116.9 . . ? C22 N2 C23 116.6(2) . . ? C22 N2 Ni1 121.94(19) . . ? C23 N2 Ni1 121.09(19) . . ? C27 N3 C26 121.2(3) . . ? C27 N3 C25 121.0(4) . . ? C26 N3 C25 117.7(3) . . ? C30 N4 C28 120.2(4) . . ? C30 N4 C29 123.3(4) . . ? C28 N4 C29 116.5(4) . . ? Ni1 O1W H1B 120(5) . . ? Ni1 O1W H1A 102(4) . . ? H1B O1W H1A 105(6) . . ? C19 O1 Ni1 128.75(19) . 2_554 ? O4 C1 O3 123.3(3) . . ? O4 C1 C2 124.6(3) . . ? O3 C1 C2 112.0(3) . . ? C3 C2 C7 119.3(3) . . ? C3 C2 C1 119.7(3) . . ? C7 C2 C1 120.8(3) . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 118.2(3) . . ? C4 C5 C8 122.5(3) . . ? C6 C5 C8 119.3(3) . . ? C7 C6 C5 121.1(3) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C2 120.3(3) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? N1 C8 C9 122.7(3) . . ? N1 C8 C5 115.3(2) . . ? C9 C8 C5 122.0(3) . . ? C10 C9 C8 118.9(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 118.0(3) . . ? C11 C10 C20 120.3(3) . . ? C9 C10 C20 121.7(3) . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? N1 C12 C11 122.6(3) . . ? N1 C12 C13 115.9(2) . . ? C11 C12 C13 121.5(2) . . ? C14 C13 C18 118.3(3) . . ? C14 C13 C12 121.4(3) . . ? C18 C13 C12 120.3(3) . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.5(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 118.7(3) . . ? C17 C16 C19 120.9(3) . . ? C15 C16 C19 120.4(3) . . ? C18 C17 C16 120.9(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C13 120.9(3) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? C8 N1 C12 118.2(2) . . ? C1 O3 H1O 116(4) . . ? O1 Ni1 O1 180.0 4_576 2_544 ? O1 Ni1 O1W 88.19(9) 4_576 3_565 ? O1 Ni1 O1W 91.81(9) 2_544 3_565 ? O1 Ni1 O1W 91.81(9) 4_576 . ? O1 Ni1 O1W 88.19(9) 2_544 . ? O1W Ni1 O1W 180.00(11) 3_565 . ? O1 Ni1 N2 89.12(8) 4_576 . ? O1 Ni1 N2 90.88(8) 2_544 . ? O1W Ni1 N2 91.97(9) 3_565 . ? O1W Ni1 N2 88.03(9) . . ? O1 Ni1 N2 90.88(8) 4_576 3_565 ? O1 Ni1 N2 89.12(8) 2_544 3_565 ? O1W Ni1 N2 88.03(9) 3_565 3_565 ? O1W Ni1 N2 91.97(9) . 3_565 ? N2 Ni1 N2 180.0 . 3_565 ? 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 C24 C20 C21 C22 4.1(4) . . . . ? C10 C20 C21 C22 -171.9(3) . . . . ? C20 C21 C22 N2 0.1(5) . . . . ? N2 C23 C24 C20 1.0(5) . . . . ? C21 C20 C24 C23 -4.6(4) . . . . ? C10 C20 C24 C23 171.4(3) . . . . ? C21 C22 N2 C23 -3.7(4) . . . . ? C21 C22 N2 Ni1 169.6(2) . . . . ? C24 C23 N2 C22 3.2(4) . . . . ? C24 C23 N2 Ni1 -170.2(2) . . . . ? O5 C27 N3 C26 4.3(6) . . . . ? O5 C27 N3 C25 179.2(4) . . . . ? O6 C30 N4 C28 5.2(8) . . . . ? O6 C30 N4 C29 -172.9(5) . . . . ? O2 C19 O1 Ni1 -5.1(4) . . . 2_554 ? C16 C19 O1 Ni1 175.79(17) . . . 2_554 ? O4 C1 C2 C3 -9.8(5) . . . . ? O3 C1 C2 C3 171.6(3) . . . . ? O4 C1 C2 C7 165.8(3) . . . . ? O3 C1 C2 C7 -12.8(4) . . . . ? C7 C2 C3 C4 0.0(5) . . . . ? C1 C2 C3 C4 175.7(3) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C3 C4 C5 C8 -178.2(3) . . . . ? C4 C5 C6 C7 0.5(4) . . . . ? C8 C5 C6 C7 178.9(3) . . . . ? C5 C6 C7 C2 -0.9(5) . . . . ? C3 C2 C7 C6 0.6(5) . . . . ? C1 C2 C7 C6 -175.0(3) . . . . ? C4 C5 C8 N1 170.0(3) . . . . ? C6 C5 C8 N1 -8.3(4) . . . . ? C4 C5 C8 C9 -8.9(4) . . . . ? C6 C5 C8 C9 172.8(3) . . . . ? N1 C8 C9 C10 -1.3(4) . . . . ? C5 C8 C9 C10 177.6(3) . . . . ? C8 C9 C10 C11 0.8(4) . . . . ? C8 C9 C10 C20 -176.4(3) . . . . ? C24 C20 C10 C11 -150.2(3) . . . . ? C21 C20 C10 C11 25.6(4) . . . . ? C24 C20 C10 C9 26.9(4) . . . . ? C21 C20 C10 C9 -157.3(3) . . . . ? C9 C10 C11 C12 -0.1(4) . . . . ? C20 C10 C11 C12 177.1(3) . . . . ? C10 C11 C12 N1 -0.2(5) . . . . ? C10 C11 C12 C13 179.8(3) . . . . ? N1 C12 C13 C14 -149.8(3) . . . . ? C11 C12 C13 C14 30.2(4) . . . . ? N1 C12 C13 C18 30.6(4) . . . . ? C11 C12 C13 C18 -149.4(3) . . . . ? C18 C13 C14 C15 1.4(5) . . . . ? C12 C13 C14 C15 -178.2(3) . . . . ? C13 C14 C15 C16 0.3(5) . . . . ? C14 C15 C16 C17 -1.2(4) . . . . ? C14 C15 C16 C19 179.1(3) . . . . ? O1 C19 C16 C17 -166.9(3) . . . . ? O2 C19 C16 C17 14.0(4) . . . . ? O1 C19 C16 C15 12.9(4) . . . . ? O2 C19 C16 C15 -166.3(3) . . . . ? C15 C16 C17 C18 0.4(5) . . . . ? C19 C16 C17 C18 -179.9(3) . . . . ? C16 C17 C18 C13 1.4(5) . . . . ? C14 C13 C18 C17 -2.2(5) . . . . ? C12 C13 C18 C17 177.4(3) . . . . ? C9 C8 N1 C12 1.0(4) . . . . ? C5 C8 N1 C12 -177.9(2) . . . . ? C11 C12 N1 C8 -0.3(4) . . . . ? C13 C12 N1 C8 179.7(2) . . . . ? C22 N2 Ni1 O1 149.2(2) . . . 4_576 ? C23 N2 Ni1 O1 -37.8(2) . . . 4_576 ? C22 N2 Ni1 O1 -30.8(2) . . . 2_544 ? C23 N2 Ni1 O1 142.2(2) . . . 2_544 ? C22 N2 Ni1 O1W -122.7(2) . . . 3_565 ? C23 N2 Ni1 O1W 50.4(2) . . . 3_565 ? C22 N2 Ni1 O1W 57.3(2) . . . . ? C23 N2 Ni1 O1W -129.6(2) . . . . ? C22 N2 Ni1 N2 -1(61) . . . 3_565 ? C23 N2 Ni1 N2 172(61) . . . 3_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1B O5 0.70(6) 2.05(6) 2.746(3) 171(7) 3_665 O1W H1A O2 0.81(6) 1.93(6) 2.698(3) 158(6) 4_576 O3 H1O O2 0.894(19) 1.74(3) 2.595(3) 158(5) 4_586 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.412 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.064 #===END #========================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 870233' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H58 Cu4 N8 O17' _chemical_formula_weight 1849.66 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number No.15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.2171(19) _cell_length_b 13.4833(9) _cell_length_c 22.4964(16) _cell_angle_alpha 90.00 _cell_angle_beta 108.1840(10) _cell_angle_gamma 90.00 _cell_volume 7555.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3768 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.7624 _exptl_absorpt_correction_T_max 0.8137 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20600 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.04 _reflns_number_total 7453 _reflns_number_gt 4595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1174P)^2^+40.7170P] 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 7453 _refine_ls_number_parameters 534 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1236 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2370 _refine_ls_wR_factor_gt 0.2038 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 C9 C 0.3104(3) 0.0874(5) 0.4929(3) 0.0336(16) Uani 1 1 d . . . H9 H 0.3258 0.1431 0.4791 0.040 Uiso 1 1 calc R . . C10 C 0.3423(3) 0.0241(5) 0.5366(3) 0.0303(15) Uani 1 1 d . . . C11 C 0.3178(3) -0.0571(5) 0.5557(3) 0.0325(15) Uani 1 1 d . . . H11 H 0.3385 -0.1023 0.5860 0.039 Uiso 1 1 calc R . . C12 C 0.2627(3) -0.0704(5) 0.5296(3) 0.0304(15) Uani 1 1 d . . . C13 C 0.2348(3) -0.1542(5) 0.5489(3) 0.0311(15) Uani 1 1 d . . . C14 C 0.1787(3) -0.1608(5) 0.5288(3) 0.0333(15) Uani 1 1 d . . . H14 H 0.1578 -0.1123 0.5011 0.040 Uiso 1 1 calc R . . C15 C 0.1534(3) -0.2380(5) 0.5493(3) 0.0306(15) Uani 1 1 d . . . H15 H 0.1153 -0.2413 0.5359 0.037 Uiso 1 1 calc R . . C16 C 0.1827(2) -0.3099(4) 0.5887(3) 0.0259(13) Uani 1 1 d . . . C17 C 0.2387(3) -0.3061(5) 0.6062(3) 0.0362(16) Uani 1 1 d . . . H17 H 0.2595 -0.3566 0.6320 0.043 Uiso 1 1 calc R . . C18 C 0.2633(3) -0.2304(5) 0.5863(3) 0.0409(18) Uani 1 1 d . . . H18 H 0.3015 -0.2294 0.5984 0.049 Uiso 1 1 calc R . . C19 C 0.1568(3) -0.3865(5) 0.6184(3) 0.0270(14) Uani 1 1 d . . . C20 C 0.4010(3) 0.0399(8) 0.5657(5) 0.0665(11) Uani 1 1 d . . . C21 C 0.4395(3) -0.0096(7) 0.5506(4) 0.0665(11) Uani 1 1 d . . . H21 H 0.4299 -0.0553 0.5168 0.080 Uiso 1 1 calc R . . C22 C 0.4927(3) 0.0052(7) 0.5833(4) 0.0665(11) Uani 1 1 d . . . H22 H 0.5188 -0.0308 0.5709 0.080 Uiso 1 1 calc R . . C23 C 0.4732(3) 0.1161(7) 0.6411(4) 0.0665(11) Uani 1 1 d . . . H23 H 0.4844 0.1633 0.6740 0.080 Uiso 1 1 calc R . . C24 C 0.4186(3) 0.1097(7) 0.6099(4) 0.0665(11) Uani 1 1 d . . . H24 H 0.3941 0.1539 0.6195 0.080 Uiso 1 1 calc R . . C25 C 0.1046(3) 0.6089(5) 0.2657(3) 0.0283(14) Uani 1 1 d . . . C26 C 0.0828(2) 0.6850(5) 0.3002(3) 0.0288(14) Uani 1 1 d . . . C27 C 0.1047(2) 0.7797(5) 0.3118(3) 0.0299(14) Uani 1 1 d . . . H27 H 0.1378 0.7935 0.3045 0.036 Uiso 1 1 calc R . . C28 C 0.0790(3) 0.8537(5) 0.3338(3) 0.0348(16) Uani 1 1 d . . . H28 H 0.0943 0.9183 0.3409 0.042 Uiso 1 1 calc R . . C29 C 0.0309(3) 0.8344(5) 0.3456(3) 0.0322(15) Uani 1 1 d . . . C30 C 0.0107(3) 0.7397(5) 0.3370(3) 0.0316(15) Uani 1 1 d . . . H30 H -0.0215 0.7251 0.3464 0.038 Uiso 1 1 calc R . . C31 C 0.0365(3) 0.6648(5) 0.3148(3) 0.0308(15) Uani 1 1 d . . . H31 H 0.0221 0.5995 0.3097 0.037 Uiso 1 1 calc R . . C32 C 0.0001(3) 0.9166(5) 0.3626(3) 0.0301(15) Uani 1 1 d . . . C33 C -0.0548(3) 0.9250(4) 0.3353(3) 0.0309(15) Uani 1 1 d . . . H33 H -0.0738 0.8760 0.3065 0.037 Uiso 1 1 calc R . . C34 C -0.0822(3) 1.0047(5) 0.3496(3) 0.0304(15) Uani 1 1 d . . . C35 C -0.0524(3) 1.0729(5) 0.3922(3) 0.0303(15) Uani 1 1 d . . . H35 H -0.0695 1.1290 0.4032 0.036 Uiso 1 1 calc R . . C36 C 0.0023(3) 1.0599(5) 0.4190(3) 0.0314(15) Uani 1 1 d . . . C37 C 0.0350(3) 1.1282(5) 0.4679(3) 0.0304(15) Uani 1 1 d . . . C38 C 0.0141(3) 1.2156(6) 0.4831(4) 0.0456(19) Uani 1 1 d . . . H38 H -0.0217 1.2343 0.4608 0.055 Uiso 1 1 calc R . . C39 C 0.0451(3) 1.2758(5) 0.5309(4) 0.0431(18) Uani 1 1 d . . . H39 H 0.0304 1.3359 0.5404 0.052 Uiso 1 1 calc R . . C40 C 0.0973(3) 1.2496(5) 0.5650(3) 0.0297(15) Uani 1 1 d . . . C41 C 0.1184(3) 1.1650(5) 0.5486(3) 0.0391(17) Uani 1 1 d . . . H41 H 0.1544 1.1471 0.5705 0.047 Uiso 1 1 calc R . . C42 C 0.0880(3) 1.1049(5) 0.5007(3) 0.0382(17) Uani 1 1 d . . . H42 H 0.1037 1.0467 0.4901 0.046 Uiso 1 1 calc R . . C43 C 0.1301(3) 1.3134(5) 0.6181(3) 0.0313(15) Uani 1 1 d . . . C44 C -0.1409(3) 1.0184(5) 0.3188(3) 0.0293(14) Uani 1 1 d . . . C45 C -0.1648(3) 1.1109(5) 0.3074(3) 0.0347(16) Uani 1 1 d . . . H45 H -0.1437 1.1687 0.3214 0.042 Uiso 1 1 calc R . . C46 C -0.2182(3) 1.1197(5) 0.2763(3) 0.0343(16) Uani 1 1 d . . . H46 H -0.2334 1.1843 0.2698 0.041 Uiso 1 1 calc R . . C47 C -0.2279(3) 0.9515(5) 0.2667(3) 0.0335(15) Uani 1 1 d . . . H47 H -0.2503 0.8949 0.2537 0.040 Uiso 1 1 calc R . . C48 C -0.1744(3) 0.9367(4) 0.2969(3) 0.0320(15) Uani 1 1 d . . . H48 H -0.1601 0.8714 0.3030 0.038 Uiso 1 1 calc R . . N1 N 0.5091(3) 0.0651(6) 0.6299(4) 0.0665(11) Uani 1 1 d . . . N2 N 0.2319(2) -0.0076(4) 0.4875(2) 0.0298(12) Uani 1 1 d . . . N3 N -0.2505(2) 1.0419(4) 0.2544(3) 0.0300(12) Uani 1 1 d . . . N4 N 0.0287(2) 0.9838(4) 0.4039(3) 0.0319(13) Uani 1 1 d . . . O1W O 0.0000 0.1373(11) 0.2500 0.142(5) Uani 1 2 d S . . O5 O 0.10933(17) -0.3729(3) 0.6172(2) 0.0308(10) Uani 1 1 d . . . O6 O 0.18690(17) -0.4579(3) 0.6442(2) 0.0299(10) Uani 1 1 d . . . O7 O 0.10919(17) 1.3916(3) 0.6297(2) 0.0321(10) Uani 1 1 d . . . O8 O 0.17645(19) 1.2883(4) 0.6479(2) 0.0427(12) Uani 1 1 d . . . C1 C 0.1252(3) 0.3079(5) 0.2665(3) 0.0371(16) Uani 1 1 d . . . C2 C 0.1578(3) 0.2474(5) 0.3215(3) 0.0352(16) Uani 1 1 d . . . C3 C 0.1410(3) 0.1553(5) 0.3326(4) 0.0441(18) Uani 1 1 d . . . H3 H 0.1076 0.1305 0.3065 0.053 Uiso 1 1 calc R . . C4 C 0.1721(3) 0.0976(6) 0.3814(4) 0.048(2) Uani 1 1 d . . . H4 H 0.1604 0.0332 0.3884 0.058 Uiso 1 1 calc R . . C5 C 0.2205(3) 0.1342(5) 0.4203(3) 0.0338(16) Uani 1 1 d . . . C6 C 0.2349(3) 0.2310(5) 0.4116(3) 0.0364(16) Uani 1 1 d . . . H6 H 0.2661 0.2588 0.4406 0.044 Uiso 1 1 calc R . . C7 C 0.2052(3) 0.2874(5) 0.3621(3) 0.0388(17) Uani 1 1 d . . . H7 H 0.2165 0.3523 0.3556 0.047 Uiso 1 1 calc R . . C8 C 0.2556(3) 0.0701(5) 0.4689(3) 0.0314(15) Uani 1 1 d . . . O1 O 0.14793(19) 0.3809(3) 0.2504(2) 0.0375(11) Uani 1 1 d . . . O2 O 0.07775(19) 0.2851(4) 0.2390(2) 0.0453(13) Uani 1 1 d . . . O3 O 0.07419(17) 0.5376(3) 0.2407(2) 0.0304(10) Uani 1 1 d . . . O4 O 0.15057(17) 0.6252(3) 0.2615(2) 0.0332(11) Uani 1 1 d . . . Cu1 Cu 0.17457(3) 0.56076(5) 0.19815(4) 0.0267(2) Uani 1 1 d . . . Cu2 Cu 0.08435(3) 0.43035(6) 0.18398(4) 0.0323(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C9 0.030(4) 0.040(4) 0.027(4) 0.007(3) 0.005(3) -0.011(3) C10 0.026(3) 0.036(3) 0.027(4) 0.004(3) 0.006(3) -0.010(3) C11 0.024(3) 0.038(4) 0.032(4) 0.014(3) 0.003(3) -0.004(3) C12 0.023(3) 0.034(4) 0.031(4) 0.007(3) 0.004(3) -0.008(3) C13 0.029(4) 0.031(3) 0.033(4) 0.005(3) 0.010(3) -0.006(3) C14 0.028(4) 0.033(4) 0.038(4) 0.011(3) 0.009(3) 0.004(3) C15 0.018(3) 0.036(4) 0.036(4) 0.003(3) 0.006(3) 0.001(3) C16 0.024(3) 0.024(3) 0.030(4) 0.000(3) 0.009(3) -0.008(3) C17 0.031(4) 0.034(4) 0.040(4) 0.013(3) 0.005(3) -0.003(3) C18 0.017(3) 0.049(4) 0.049(5) 0.016(4) 0.000(3) -0.001(3) C19 0.027(3) 0.028(3) 0.024(3) -0.006(3) 0.006(3) -0.012(3) C20 0.0289(17) 0.088(3) 0.074(3) -0.041(2) 0.0031(17) 0.0001(16) C21 0.0289(17) 0.088(3) 0.074(3) -0.041(2) 0.0031(17) 0.0001(16) C22 0.0289(17) 0.088(3) 0.074(3) -0.041(2) 0.0031(17) 0.0001(16) C23 0.0289(17) 0.088(3) 0.074(3) -0.041(2) 0.0031(17) 0.0001(16) C24 0.0289(17) 0.088(3) 0.074(3) -0.041(2) 0.0031(17) 0.0001(16) C25 0.024(3) 0.038(4) 0.022(3) 0.008(3) 0.006(3) 0.010(3) C26 0.023(3) 0.031(3) 0.031(4) 0.000(3) 0.006(3) 0.008(3) C27 0.015(3) 0.046(4) 0.029(4) 0.000(3) 0.007(3) 0.001(3) C28 0.028(4) 0.033(4) 0.041(4) 0.000(3) 0.008(3) 0.001(3) C29 0.025(3) 0.047(4) 0.023(3) -0.009(3) 0.004(3) 0.005(3) C30 0.027(3) 0.039(4) 0.030(4) -0.009(3) 0.011(3) 0.002(3) C31 0.027(3) 0.035(4) 0.031(4) -0.001(3) 0.010(3) 0.002(3) C32 0.026(3) 0.034(3) 0.030(4) -0.011(3) 0.008(3) -0.002(3) C33 0.031(4) 0.022(3) 0.035(4) -0.011(3) 0.005(3) -0.003(3) C34 0.023(3) 0.033(3) 0.032(4) -0.004(3) 0.004(3) -0.001(3) C35 0.029(4) 0.027(3) 0.034(4) -0.008(3) 0.009(3) -0.001(3) C36 0.030(4) 0.035(4) 0.027(4) -0.006(3) 0.005(3) -0.009(3) C37 0.027(3) 0.033(3) 0.029(4) -0.010(3) 0.005(3) -0.006(3) C38 0.028(4) 0.047(4) 0.054(5) -0.022(4) 0.001(3) 0.000(3) C39 0.042(4) 0.036(4) 0.053(5) -0.018(3) 0.018(4) -0.006(3) C40 0.024(3) 0.037(4) 0.029(4) -0.003(3) 0.010(3) -0.013(3) C41 0.030(4) 0.041(4) 0.044(4) -0.010(3) 0.007(3) -0.004(3) C42 0.034(4) 0.033(4) 0.046(4) -0.011(3) 0.010(3) -0.002(3) C43 0.027(4) 0.031(3) 0.040(4) -0.002(3) 0.016(3) -0.008(3) C44 0.029(3) 0.032(3) 0.025(3) -0.004(3) 0.006(3) -0.001(3) C45 0.034(4) 0.027(3) 0.041(4) -0.005(3) 0.009(3) -0.003(3) C46 0.034(4) 0.021(3) 0.045(4) -0.006(3) 0.008(3) 0.004(3) C47 0.028(4) 0.027(3) 0.040(4) -0.002(3) 0.003(3) -0.001(3) C48 0.030(4) 0.022(3) 0.037(4) 0.001(3) 0.000(3) 0.005(3) N1 0.0289(17) 0.088(3) 0.074(3) -0.041(2) 0.0031(17) 0.0001(16) N2 0.022(3) 0.032(3) 0.033(3) 0.007(2) 0.005(2) -0.003(2) N3 0.027(3) 0.029(3) 0.033(3) -0.004(2) 0.007(2) 0.008(2) N4 0.027(3) 0.032(3) 0.036(3) -0.007(2) 0.009(3) 0.001(2) O1W 0.090(10) 0.119(11) 0.216(16) 0.000 0.047(10) 0.000 O5 0.022(2) 0.035(2) 0.039(3) 0.005(2) 0.014(2) -0.0051(19) O6 0.025(2) 0.033(2) 0.031(2) 0.0060(19) 0.007(2) -0.0080(19) O7 0.028(2) 0.032(2) 0.035(3) -0.004(2) 0.007(2) -0.005(2) O8 0.026(3) 0.044(3) 0.051(3) -0.013(2) 0.000(2) -0.001(2) C1 0.029(4) 0.040(4) 0.043(4) 0.007(3) 0.013(3) 0.004(3) C2 0.025(3) 0.045(4) 0.031(4) 0.008(3) 0.004(3) 0.006(3) C3 0.036(4) 0.044(4) 0.044(5) 0.007(3) 0.000(3) -0.006(3) C4 0.037(4) 0.045(4) 0.050(5) 0.014(4) -0.004(4) -0.011(4) C5 0.022(3) 0.043(4) 0.033(4) 0.011(3) 0.004(3) -0.005(3) C6 0.031(4) 0.043(4) 0.032(4) 0.011(3) 0.006(3) -0.002(3) C7 0.033(4) 0.035(4) 0.048(4) 0.008(3) 0.013(3) 0.002(3) C8 0.025(3) 0.039(4) 0.027(4) 0.008(3) 0.003(3) -0.004(3) O1 0.033(3) 0.036(3) 0.040(3) 0.010(2) 0.007(2) 0.005(2) O2 0.027(3) 0.053(3) 0.047(3) 0.018(2) -0.002(2) 0.002(2) O3 0.029(2) 0.032(2) 0.033(3) -0.0052(19) 0.014(2) 0.004(2) O4 0.023(2) 0.046(3) 0.031(3) -0.006(2) 0.009(2) 0.006(2) Cu1 0.0200(4) 0.0260(4) 0.0327(5) -0.0028(3) 0.0063(3) 0.0041(3) Cu2 0.0220(4) 0.0388(5) 0.0338(5) -0.0038(3) 0.0055(4) 0.0053(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C10 1.371(9) . ? C9 C8 1.386(9) . ? C9 H9 0.9500 . ? C10 C11 1.402(9) . ? C10 C20 1.489(10) . ? C11 C12 1.390(9) . ? C11 H11 0.9500 . ? C12 N2 1.337(8) . ? C12 C13 1.482(8) . ? C13 C18 1.390(9) . ? C13 C14 1.402(9) . ? C14 C15 1.388(9) . ? C14 H14 0.9500 . ? C15 C16 1.374(9) . ? C15 H15 0.9500 . ? C16 C17 1.398(9) . ? C16 C19 1.502(8) . ? C17 C18 1.356(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O5 1.251(7) . ? C19 O6 1.264(8) . ? C20 C21 1.340(11) . ? C20 C24 1.341(11) . ? C21 C22 1.373(11) . ? C21 H21 0.9500 . ? C22 N1 1.286(10) . ? C22 H22 0.9500 . ? C23 N1 1.253(10) . ? C23 C24 1.387(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 O4 1.258(7) . ? C25 O3 1.263(8) . ? C25 C26 1.504(9) . ? C26 C31 1.380(9) . ? C26 C27 1.391(9) . ? C27 C28 1.380(9) . ? C27 H27 0.9500 . ? C28 C29 1.393(9) . ? C28 H28 0.9500 . ? C29 C30 1.372(9) . ? C29 C32 1.491(9) . ? C30 C31 1.392(9) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 N4 1.346(8) . ? C32 C33 1.382(9) . ? C33 C34 1.386(9) . ? C33 H33 0.9500 . ? C34 C35 1.382(9) . ? C34 C44 1.488(9) . ? C35 C36 1.382(9) . ? C35 H35 0.9500 . ? C36 N4 1.341(8) . ? C36 C37 1.484(8) . ? C37 C38 1.387(9) . ? C37 C42 1.391(9) . ? C38 C39 1.390(9) . ? C38 H38 0.9500 . ? C39 C40 1.390(10) . ? C39 H39 0.9500 . ? C40 C41 1.366(9) . ? C40 C43 1.505(9) . ? C41 C42 1.384(9) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 O8 1.239(8) . ? C43 O7 1.251(8) . ? C43 Cu1 2.484(6) 6_576 ? C44 C45 1.383(9) . ? C44 C48 1.399(9) . ? C45 C46 1.363(9) . ? C45 H45 0.9500 . ? C46 N3 1.342(8) . ? C46 H46 0.9500 . ? C47 N3 1.346(8) . ? C47 C48 1.370(9) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? N1 Cu2 1.969(7) 8_556 ? N2 C8 1.351(8) . ? N3 Cu1 1.993(5) 3_455 ? O5 Cu2 1.975(4) 6_556 ? O6 Cu1 1.936(4) 6_556 ? O7 Cu1 2.019(4) 6_576 ? O8 Cu1 2.336(5) 6_576 ? C1 O2 1.244(8) . ? C1 O1 1.260(8) . ? C1 C2 1.505(9) . ? C1 Cu2 2.465(7) . ? C2 C3 1.367(10) . ? C2 C7 1.401(10) . ? C3 C4 1.385(10) . ? C3 H3 0.9500 . ? C4 C5 1.388(9) . ? C4 H4 0.9500 . ? C5 C6 1.388(9) . ? C5 C8 1.471(9) . ? C6 C7 1.372(9) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? O1 Cu2 1.976(4) . ? O2 Cu2 2.352(5) . ? O3 Cu2 2.000(4) . ? O4 Cu1 1.935(4) . ? Cu1 O6 1.936(4) 6 ? Cu1 N3 1.993(5) 3_545 ? Cu1 O7 2.019(4) 6_575 ? Cu1 O8 2.336(5) 6_575 ? Cu1 C43 2.484(6) 6_575 ? Cu1 Cu2 2.8840(11) . ? Cu2 N1 1.969(7) 8_455 ? Cu2 O5 1.975(4) 6 ? 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 C10 C9 C8 120.0(6) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 118.0(6) . . ? C9 C10 C20 122.8(7) . . ? C11 C10 C20 119.1(7) . . ? C12 C11 C10 119.1(6) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? N2 C12 C11 122.4(6) . . ? N2 C12 C13 116.4(6) . . ? C11 C12 C13 121.1(6) . . ? C18 C13 C14 117.4(6) . . ? C18 C13 C12 121.3(6) . . ? C14 C13 C12 121.2(6) . . ? C15 C14 C13 120.2(6) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 121.0(6) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 118.8(6) . . ? C15 C16 C19 122.3(6) . . ? C17 C16 C19 118.7(6) . . ? C18 C17 C16 120.1(6) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C13 122.3(6) . . ? C17 C18 H18 118.8 . . ? C13 C18 H18 118.8 . . ? O5 C19 O6 126.6(6) . . ? O5 C19 C16 118.3(6) . . ? O6 C19 C16 115.1(5) . . ? C21 C20 C24 115.1(8) . . ? C21 C20 C10 125.2(8) . . ? C24 C20 C10 119.7(8) . . ? C20 C21 C22 120.8(8) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? N1 C22 C21 123.6(8) . . ? N1 C22 H22 118.2 . . ? C21 C22 H22 118.2 . . ? N1 C23 C24 125.8(8) . . ? N1 C23 H23 117.1 . . ? C24 C23 H23 117.1 . . ? C20 C24 C23 118.8(8) . . ? C20 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? O4 C25 O3 125.8(6) . . ? O4 C25 C26 116.6(6) . . ? O3 C25 C26 117.5(6) . . ? C31 C26 C27 118.7(6) . . ? C31 C26 C25 119.5(6) . . ? C27 C26 C25 121.4(6) . . ? C28 C27 C26 120.8(6) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.3(6) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 118.8(6) . . ? C30 C29 C32 120.7(6) . . ? C28 C29 C32 120.4(6) . . ? C29 C30 C31 121.0(6) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C26 C31 C30 120.3(6) . . ? C26 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? N4 C32 C33 122.1(6) . . ? N4 C32 C29 116.6(6) . . ? C33 C32 C29 121.2(6) . . ? C32 C33 C34 120.3(6) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 117.1(6) . . ? C35 C34 C44 121.3(6) . . ? C33 C34 C44 121.6(6) . . ? C36 C35 C34 120.2(6) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? N4 C36 C35 122.3(6) . . ? N4 C36 C37 115.9(6) . . ? C35 C36 C37 121.7(6) . . ? C38 C37 C42 117.9(6) . . ? C38 C37 C36 121.8(6) . . ? C42 C37 C36 120.3(6) . . ? C37 C38 C39 120.4(7) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C40 121.0(7) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C41 C40 C39 118.4(6) . . ? C41 C40 C43 120.9(6) . . ? C39 C40 C43 120.7(6) . . ? C40 C41 C42 121.1(7) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C41 C42 C37 121.2(6) . . ? C41 C42 H42 119.4 . . ? C37 C42 H42 119.4 . . ? O8 C43 O7 122.5(6) . . ? O8 C43 C40 119.6(6) . . ? O7 C43 C40 118.0(6) . . ? O8 C43 Cu1 68.6(4) . 6_576 ? O7 C43 Cu1 53.9(3) . 6_576 ? C40 C43 Cu1 171.4(5) . 6_576 ? C45 C44 C48 116.6(6) . . ? C45 C44 C34 122.7(6) . . ? C48 C44 C34 120.6(6) . . ? C46 C45 C44 120.5(6) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? N3 C46 C45 123.5(6) . . ? N3 C46 H46 118.3 . . ? C45 C46 H46 118.3 . . ? N3 C47 C48 123.4(6) . . ? N3 C47 H47 118.3 . . ? C48 C47 H47 118.3 . . ? C47 C48 C44 119.6(6) . . ? C47 C48 H48 120.2 . . ? C44 C48 H48 120.2 . . ? C23 N1 C22 115.3(7) . . ? C23 N1 Cu2 122.0(6) . 8_556 ? C22 N1 Cu2 122.6(6) . 8_556 ? C12 N2 C8 118.3(5) . . ? C46 N3 C47 116.5(6) . . ? C46 N3 Cu1 121.2(4) . 3_455 ? C47 N3 Cu1 122.0(4) . 3_455 ? C36 N4 C32 118.0(6) . . ? C19 O5 Cu2 119.3(4) . 6_556 ? C19 O6 Cu1 129.1(4) . 6_556 ? C43 O7 Cu1 96.0(4) . 6_576 ? C43 O8 Cu1 81.8(4) . 6_576 ? O2 C1 O1 122.7(6) . . ? O2 C1 C2 119.8(6) . . ? O1 C1 C2 117.5(6) . . ? O2 C1 Cu2 70.0(4) . . ? O1 C1 Cu2 52.7(3) . . ? C2 C1 Cu2 169.6(5) . . ? C3 C2 C7 120.1(6) . . ? C3 C2 C1 120.8(6) . . ? C7 C2 C1 119.2(6) . . ? C2 C3 C4 120.8(7) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 119.7(7) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 118.7(6) . . ? C4 C5 C8 119.7(6) . . ? C6 C5 C8 121.5(6) . . ? C7 C6 C5 121.7(7) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C2 118.6(7) . . ? C6 C7 H7 120.7 . . ? C2 C7 H7 120.7 . . ? N2 C8 C9 122.1(6) . . ? N2 C8 C5 116.4(6) . . ? C9 C8 C5 121.5(6) . . ? C1 O1 Cu2 96.8(4) . . ? C1 O2 Cu2 80.1(4) . . ? C25 O3 Cu2 130.1(4) . . ? C25 O4 Cu1 121.1(4) . . ? O4 Cu1 O6 160.1(2) . 6 ? O4 Cu1 N3 94.1(2) . 3_545 ? O6 Cu1 N3 89.00(19) 6 3_545 ? O4 Cu1 O7 91.46(18) . 6_575 ? O6 Cu1 O7 91.02(18) 6 6_575 ? N3 Cu1 O7 163.5(2) 3_545 6_575 ? O4 Cu1 O8 91.51(19) . 6_575 ? O6 Cu1 O8 106.73(19) 6 6_575 ? N3 Cu1 O8 104.7(2) 3_545 6_575 ? O7 Cu1 O8 59.63(17) 6_575 6_575 ? O4 Cu1 C43 92.3(2) . 6_575 ? O6 Cu1 C43 99.6(2) 6 6_575 ? N3 Cu1 C43 134.0(2) 3_545 6_575 ? O7 Cu1 C43 30.06(19) 6_575 6_575 ? O8 Cu1 C43 29.59(18) 6_575 6_575 ? O4 Cu1 Cu2 84.89(14) . . ? O6 Cu1 Cu2 77.62(14) 6 . ? N3 Cu1 Cu2 127.16(16) 3_545 . ? O7 Cu1 Cu2 68.79(13) 6_575 . ? O8 Cu1 Cu2 128.18(12) 6_575 . ? C43 Cu1 Cu2 98.78(16) 6_575 . ? N1 Cu2 O5 92.8(3) 8_455 6 ? N1 Cu2 O1 157.5(2) 8_455 . ? O5 Cu2 O1 92.39(19) 6 . ? N1 Cu2 O3 93.7(3) 8_455 . ? O5 Cu2 O3 155.57(19) 6 . ? O1 Cu2 O3 90.58(19) . . ? N1 Cu2 O2 97.3(2) 8_455 . ? O5 Cu2 O2 99.81(19) 6 . ? O1 Cu2 O2 60.27(18) . . ? O3 Cu2 O2 102.70(19) . . ? N1 Cu2 C1 127.0(3) 8_455 . ? O5 Cu2 C1 98.1(2) 6 . ? O1 Cu2 C1 30.5(2) . . ? O3 Cu2 C1 96.7(2) . . ? O2 Cu2 C1 29.81(19) . . ? N1 Cu2 Cu1 132.7(2) 8_455 . ? O5 Cu2 Cu1 82.42(13) 6 . ? O1 Cu2 Cu1 69.68(14) . . ? O3 Cu2 Cu1 75.91(13) . . ? O2 Cu2 Cu1 129.94(12) . . ? C1 Cu2 Cu1 100.14(17) . . ? 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 C8 C9 C10 C11 0.0(10) . . . . ? C8 C9 C10 C20 -178.1(7) . . . . ? C9 C10 C11 C12 0.3(10) . . . . ? C20 C10 C11 C12 178.5(7) . . . . ? C10 C11 C12 N2 -1.1(11) . . . . ? C10 C11 C12 C13 -179.1(6) . . . . ? N2 C12 C13 C18 172.1(7) . . . . ? C11 C12 C13 C18 -9.8(11) . . . . ? N2 C12 C13 C14 -6.4(10) . . . . ? C11 C12 C13 C14 171.7(7) . . . . ? C18 C13 C14 C15 3.8(10) . . . . ? C12 C13 C14 C15 -177.7(6) . . . . ? C13 C14 C15 C16 -0.9(10) . . . . ? C14 C15 C16 C17 -2.3(10) . . . . ? C14 C15 C16 C19 171.7(6) . . . . ? C15 C16 C17 C18 2.5(10) . . . . ? C19 C16 C17 C18 -171.7(7) . . . . ? C16 C17 C18 C13 0.5(12) . . . . ? C14 C13 C18 C17 -3.6(11) . . . . ? C12 C13 C18 C17 177.8(7) . . . . ? C15 C16 C19 O5 -14.2(9) . . . . ? C17 C16 C19 O5 159.8(6) . . . . ? C15 C16 C19 O6 167.8(6) . . . . ? C17 C16 C19 O6 -18.2(8) . . . . ? C9 C10 C20 C21 -103.0(12) . . . . ? C11 C10 C20 C21 78.9(13) . . . . ? C9 C10 C20 C24 75.6(13) . . . . ? C11 C10 C20 C24 -102.5(11) . . . . ? C24 C20 C21 C22 6.2(17) . . . . ? C10 C20 C21 C22 -175.1(10) . . . . ? C20 C21 C22 N1 0.6(18) . . . . ? C21 C20 C24 C23 -8.1(17) . . . . ? C10 C20 C24 C23 173.1(9) . . . . ? N1 C23 C24 C20 3.9(19) . . . . ? O4 C25 C26 C31 -170.2(6) . . . . ? O3 C25 C26 C31 13.7(9) . . . . ? O4 C25 C26 C27 16.9(9) . . . . ? O3 C25 C26 C27 -159.1(6) . . . . ? C31 C26 C27 C28 -4.0(10) . . . . ? C25 C26 C27 C28 168.9(6) . . . . ? C26 C27 C28 C29 0.9(10) . . . . ? C27 C28 C29 C30 2.3(10) . . . . ? C27 C28 C29 C32 -173.3(6) . . . . ? C28 C29 C30 C31 -2.3(10) . . . . ? C32 C29 C30 C31 173.3(6) . . . . ? C27 C26 C31 C30 3.9(9) . . . . ? C25 C26 C31 C30 -169.1(6) . . . . ? C29 C30 C31 C26 -0.8(10) . . . . ? C30 C29 C32 N4 141.6(7) . . . . ? C28 C29 C32 N4 -42.9(9) . . . . ? C30 C29 C32 C33 -41.0(10) . . . . ? C28 C29 C32 C33 134.5(7) . . . . ? N4 C32 C33 C34 0.4(11) . . . . ? C29 C32 C33 C34 -176.9(6) . . . . ? C32 C33 C34 C35 -0.7(10) . . . . ? C32 C33 C34 C44 177.2(6) . . . . ? C33 C34 C35 C36 -0.5(10) . . . . ? C44 C34 C35 C36 -178.4(6) . . . . ? C34 C35 C36 N4 2.0(11) . . . . ? C34 C35 C36 C37 -176.2(6) . . . . ? N4 C36 C37 C38 172.9(7) . . . . ? C35 C36 C37 C38 -8.8(11) . . . . ? N4 C36 C37 C42 -8.2(10) . . . . ? C35 C36 C37 C42 170.1(7) . . . . ? C42 C37 C38 C39 -1.6(11) . . . . ? C36 C37 C38 C39 177.3(7) . . . . ? C37 C38 C39 C40 -0.9(12) . . . . ? C38 C39 C40 C41 2.8(11) . . . . ? C38 C39 C40 C43 -177.9(7) . . . . ? C39 C40 C41 C42 -2.1(11) . . . . ? C43 C40 C41 C42 178.5(6) . . . . ? C40 C41 C42 C37 -0.4(11) . . . . ? C38 C37 C42 C41 2.3(11) . . . . ? C36 C37 C42 C41 -176.6(7) . . . . ? C41 C40 C43 O8 -0.9(10) . . . . ? C39 C40 C43 O8 179.8(7) . . . . ? C41 C40 C43 O7 177.9(6) . . . . ? C39 C40 C43 O7 -1.5(9) . . . . ? C41 C40 C43 Cu1 158(3) . . . 6_576 ? C39 C40 C43 Cu1 -21(3) . . . 6_576 ? C35 C34 C44 C45 29.4(10) . . . . ? C33 C34 C44 C45 -148.4(7) . . . . ? C35 C34 C44 C48 -154.0(7) . . . . ? C33 C34 C44 C48 28.2(10) . . . . ? C48 C44 C45 C46 0.0(10) . . . . ? C34 C44 C45 C46 176.7(7) . . . . ? C44 C45 C46 N3 -0.9(11) . . . . ? N3 C47 C48 C44 2.5(11) . . . . ? C45 C44 C48 C47 -0.7(10) . . . . ? C34 C44 C48 C47 -177.6(6) . . . . ? C24 C23 N1 C22 3.0(17) . . . . ? C24 C23 N1 Cu2 -172.6(9) . . . 8_556 ? C21 C22 N1 C23 -5.2(17) . . . . ? C21 C22 N1 Cu2 170.3(9) . . . 8_556 ? C11 C12 N2 C8 1.5(10) . . . . ? C13 C12 N2 C8 179.6(6) . . . . ? C45 C46 N3 C47 2.5(10) . . . . ? C45 C46 N3 Cu1 -170.4(5) . . . 3_455 ? C48 C47 N3 C46 -3.3(10) . . . . ? C48 C47 N3 Cu1 169.5(5) . . . 3_455 ? C35 C36 N4 C32 -2.3(10) . . . . ? C37 C36 N4 C32 176.0(6) . . . . ? C33 C32 N4 C36 1.1(10) . . . . ? C29 C32 N4 C36 178.5(6) . . . . ? O6 C19 O5 Cu2 25.5(8) . . . 6_556 ? C16 C19 O5 Cu2 -152.2(4) . . . 6_556 ? O5 C19 O6 Cu1 -8.2(9) . . . 6_556 ? C16 C19 O6 Cu1 169.6(4) . . . 6_556 ? O8 C43 O7 Cu1 2.3(7) . . . 6_576 ? C40 C43 O7 Cu1 -176.4(5) . . . 6_576 ? O7 C43 O8 Cu1 -2.0(6) . . . 6_576 ? C40 C43 O8 Cu1 176.7(6) . . . 6_576 ? O2 C1 C2 C3 15.8(11) . . . . ? O1 C1 C2 C3 -164.4(7) . . . . ? Cu2 C1 C2 C3 177(2) . . . . ? O2 C1 C2 C7 -162.8(7) . . . . ? O1 C1 C2 C7 16.9(10) . . . . ? Cu2 C1 C2 C7 -2(3) . . . . ? C7 C2 C3 C4 -4.4(12) . . . . ? C1 C2 C3 C4 177.0(7) . . . . ? C2 C3 C4 C5 1.1(13) . . . . ? C3 C4 C5 C6 4.3(12) . . . . ? C3 C4 C5 C8 -175.1(7) . . . . ? C4 C5 C6 C7 -6.5(11) . . . . ? C8 C5 C6 C7 172.9(7) . . . . ? C5 C6 C7 C2 3.2(11) . . . . ? C3 C2 C7 C6 2.2(11) . . . . ? C1 C2 C7 C6 -179.1(7) . . . . ? C12 N2 C8 C9 -1.3(10) . . . . ? C12 N2 C8 C5 176.9(6) . . . . ? C10 C9 C8 N2 0.5(11) . . . . ? C10 C9 C8 C5 -177.6(6) . . . . ? C4 C5 C8 N2 -21.9(10) . . . . ? C6 C5 C8 N2 158.8(7) . . . . ? C4 C5 C8 C9 156.4(7) . . . . ? C6 C5 C8 C9 -23.0(11) . . . . ? O2 C1 O1 Cu2 3.9(8) . . . . ? C2 C1 O1 Cu2 -175.9(5) . . . . ? O1 C1 O2 Cu2 -3.3(7) . . . . ? C2 C1 O2 Cu2 176.5(6) . . . . ? O4 C25 O3 Cu2 -2.9(9) . . . . ? C26 C25 O3 Cu2 172.8(4) . . . . ? O3 C25 O4 Cu1 15.8(9) . . . . ? C26 C25 O4 Cu1 -159.9(4) . . . . ? C25 O4 Cu1 O6 -43.3(8) . . . 6 ? C25 O4 Cu1 N3 -141.7(5) . . . 3_545 ? C25 O4 Cu1 O7 53.8(5) . . . 6_575 ? C25 O4 Cu1 O8 113.4(5) . . . 6_575 ? C25 O4 Cu1 C43 83.9(5) . . . 6_575 ? C25 O4 Cu1 Cu2 -14.8(5) . . . . ? C1 O1 Cu2 N1 1.3(10) . . . 8_455 ? C1 O1 Cu2 O5 -101.9(4) . . . 6 ? C1 O1 Cu2 O3 102.3(4) . . . . ? C1 O1 Cu2 O2 -2.0(4) . . . . ? C1 O1 Cu2 Cu1 177.1(4) . . . . ? C25 O3 Cu2 N1 -139.6(6) . . . 8_455 ? C25 O3 Cu2 O5 -34.6(8) . . . 6 ? C25 O3 Cu2 O1 62.5(5) . . . . ? C25 O3 Cu2 O2 122.1(5) . . . . ? C25 O3 Cu2 C1 92.4(5) . . . . ? C25 O3 Cu2 Cu1 -6.4(5) . . . . ? C1 O2 Cu2 N1 -176.7(5) . . . 8_455 ? C1 O2 Cu2 O5 89.2(4) . . . 6 ? C1 O2 Cu2 O1 2.0(4) . . . . ? C1 O2 Cu2 O3 -81.3(4) . . . . ? C1 O2 Cu2 Cu1 0.9(5) . . . . ? O2 C1 Cu2 N1 4.1(6) . . . 8_455 ? O1 C1 Cu2 N1 -179.4(5) . . . 8_455 ? C2 C1 Cu2 N1 -159(3) . . . 8_455 ? O2 C1 Cu2 O5 -95.6(4) . . . 6 ? O1 C1 Cu2 O5 80.9(4) . . . 6 ? C2 C1 Cu2 O5 102(3) . . . 6 ? O2 C1 Cu2 O1 -176.5(7) . . . . ? C2 C1 Cu2 O1 21(3) . . . . ? O2 C1 Cu2 O3 103.9(4) . . . . ? O1 C1 Cu2 O3 -79.6(4) . . . . ? C2 C1 Cu2 O3 -59(3) . . . . ? O1 C1 Cu2 O2 176.5(7) . . . . ? C2 C1 Cu2 O2 -163(3) . . . . ? O2 C1 Cu2 Cu1 -179.3(4) . . . . ? O1 C1 Cu2 Cu1 -2.8(4) . . . . ? C2 C1 Cu2 Cu1 18(3) . . . . ? O4 Cu1 Cu2 N1 90.6(4) . . . 8_455 ? O6 Cu1 Cu2 N1 -98.9(4) 6 . . 8_455 ? N3 Cu1 Cu2 N1 -178.1(4) 3_545 . . 8_455 ? O7 Cu1 Cu2 N1 -2.9(4) 6_575 . . 8_455 ? O8 Cu1 Cu2 N1 2.7(4) 6_575 . . 8_455 ? C43 Cu1 Cu2 N1 -0.9(4) 6_575 . . 8_455 ? O4 Cu1 Cu2 O5 177.41(18) . . . 6 ? O6 Cu1 Cu2 O5 -12.17(18) 6 . . 6 ? N3 Cu1 Cu2 O5 -91.3(2) 3_545 . . 6 ? O7 Cu1 Cu2 O5 83.84(19) 6_575 . . 6 ? O8 Cu1 Cu2 O5 89.5(2) 6_575 . . 6 ? C43 Cu1 Cu2 O5 85.8(2) 6_575 . . 6 ? O4 Cu1 Cu2 O1 -87.2(2) . . . . ? O6 Cu1 Cu2 O1 83.2(2) 6 . . . ? N3 Cu1 Cu2 O1 4.1(2) 3_545 . . . ? O7 Cu1 Cu2 O1 179.2(2) 6_575 . . . ? O8 Cu1 Cu2 O1 -175.1(2) 6_575 . . . ? C43 Cu1 Cu2 O1 -178.8(2) 6_575 . . . ? O4 Cu1 Cu2 O3 8.78(19) . . . . ? O6 Cu1 Cu2 O3 179.20(18) 6 . . . ? N3 Cu1 Cu2 O3 100.1(2) 3_545 . . . ? O7 Cu1 Cu2 O3 -84.79(19) 6_575 . . . ? O8 Cu1 Cu2 O3 -79.1(2) 6_575 . . . ? C43 Cu1 Cu2 O3 -82.8(2) 6_575 . . . ? O4 Cu1 Cu2 O2 -86.1(2) . . . . ? O6 Cu1 Cu2 O2 84.3(2) 6 . . . ? N3 Cu1 Cu2 O2 5.2(3) 3_545 . . . ? O7 Cu1 Cu2 O2 -179.7(2) 6_575 . . . ? O8 Cu1 Cu2 O2 -174.0(2) 6_575 . . . ? C43 Cu1 Cu2 O2 -177.7(2) 6_575 . . . ? O4 Cu1 Cu2 C1 -85.7(2) . . . . ? O6 Cu1 Cu2 C1 84.7(2) 6 . . . ? N3 Cu1 Cu2 C1 5.6(3) 3_545 . . . ? O7 Cu1 Cu2 C1 -179.2(2) 6_575 . . . ? O8 Cu1 Cu2 C1 -173.6(2) 6_575 . . . ? C43 Cu1 Cu2 C1 -177.2(2) 6_575 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.272 _refine_diff_density_min -1.457 _refine_diff_density_rms 0.138 #===END #========================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 870234' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H30 N4 O8 Zn' _chemical_formula_weight 856.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number No.2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5827(7) _cell_length_b 12.3343(7) _cell_length_c 14.7367(8) _cell_angle_alpha 66.6880(10) _cell_angle_beta 78.4610(10) _cell_angle_gamma 89.6640(10) _cell_volume 1888.10(19) _cell_formula_units_Z 2 _cell_measurement_temperature 179(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.341 _exptl_absorpt_correction_T_max 0.595 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 179(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10520 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.08 _reflns_number_total 7366 _reflns_number_gt 5500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0692P)^2^+2.2561P] 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 7366 _refine_ls_number_parameters 556 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 C21 C 1.2947(3) 1.0740(3) 0.3689(3) 0.0238(8) Uani 1 1 d . . . C22 C 1.2269(4) 1.0303(4) 0.3211(3) 0.0381(10) Uani 1 1 d . . . H22 H 1.2424 1.0610 0.2493 0.046 Uiso 1 1 calc R . . C24 C 1.3984(3) 1.1637(3) 0.3063(3) 0.0289(9) Uani 1 1 d . . . C42 C 0.0811(3) 1.1004(3) 0.0232(3) 0.0232(8) Uani 1 1 d . . . C43 C 0.0434(4) 1.0388(3) 0.1279(3) 0.0303(9) Uani 1 1 d . . . H43 H 0.0911 0.9818 0.1643 0.036 Uiso 1 1 calc R . . C44 C -0.0623(4) 1.0593(3) 0.1794(3) 0.0304(9) Uani 1 1 d . . . H44 H -0.0872 1.0152 0.2503 0.036 Uiso 1 1 calc R . . C45 C -0.1320(3) 1.1441(3) 0.1281(3) 0.0227(8) Uani 1 1 d . . . C46 C -0.0969(3) 1.2043(3) 0.0247(3) 0.0268(8) Uani 1 1 d . . . H46 H -0.1447 1.2615 -0.0112 0.032 Uiso 1 1 calc R . . C47 C 0.0075(3) 1.1821(3) -0.0271(3) 0.0277(8) Uani 1 1 d . . . H47 H 0.0295 1.2233 -0.0986 0.033 Uiso 1 1 calc R . . C48 C -0.2425(3) 1.1694(3) 0.1876(3) 0.0258(8) Uani 1 1 d . . . O3 O 1.4658(2) 1.1895(2) 0.35499(19) 0.0321(6) Uani 1 1 d . . . O4 O 1.4173(3) 1.2042(3) 0.2145(2) 0.0628(11) Uani 1 1 d . . . O7 O -0.2820(2) 1.1022(3) 0.2757(2) 0.0358(7) Uani 1 1 d . . . O8 O -0.2882(2) 1.2662(2) 0.14244(19) 0.0308(6) Uani 1 1 d . . . H1A H 0.757(4) 0.488(4) 1.0853(15) 0.046 Uiso 1 1 d D . . H2A H 0.500(4) 1.330(4) -0.5603(15) 0.046 Uiso 1 1 d D . . C1 C 0.7760(3) 0.4105(3) 0.2989(3) 0.0268(8) Uani 1 1 d . . . C2 C 0.8167(3) 0.4638(3) 0.3641(3) 0.0241(8) Uani 1 1 d . . . C3 C 0.7797(3) 0.4134(3) 0.4687(3) 0.0260(8) Uani 1 1 d . . . H3 H 0.7327 0.3401 0.5010 0.031 Uiso 1 1 calc R . . C4 C 0.8113(3) 0.4698(3) 0.5263(3) 0.0281(9) Uani 1 1 d . . . H4 H 0.7869 0.4332 0.5979 0.034 Uiso 1 1 calc R . . C5 C 0.8775(3) 0.5784(3) 0.4816(3) 0.0245(8) Uani 1 1 d . . . C6 C 0.9181(3) 0.6265(3) 0.3770(3) 0.0293(9) Uani 1 1 d . . . H6 H 0.9660 0.6993 0.3446 0.035 Uiso 1 1 calc R . . C7 C 0.8888(3) 0.5685(3) 0.3199(3) 0.0275(8) Uani 1 1 d . . . H7 H 0.9189 0.6014 0.2488 0.033 Uiso 1 1 calc R . . C8 C 0.9076(3) 0.6425(3) 0.5423(3) 0.0253(8) Uani 1 1 d . . . C9 C 0.8607(3) 0.6023(3) 0.6459(3) 0.0280(9) Uani 1 1 d . . . H9 H 0.8053 0.5349 0.6796 0.034 Uiso 1 1 calc R . . C10 C 0.8968(3) 0.6629(3) 0.6995(3) 0.0256(8) Uani 1 1 d . . . C11 C 0.9778(3) 0.7613(3) 0.6460(3) 0.0244(8) Uani 1 1 d . . . H11 H 1.0043 0.8044 0.6801 0.029 Uiso 1 1 calc R . . C12 C 1.0198(3) 0.7962(3) 0.5431(3) 0.0234(8) Uani 1 1 d . . . C13 C 0.8546(3) 0.6176(3) 0.8109(3) 0.0269(8) Uani 1 1 d . . . C14 C 0.7474(4) 0.5504(4) 0.8604(3) 0.0346(10) Uani 1 1 d . . . H14 H 0.6956 0.5384 0.8222 0.042 Uiso 1 1 calc R . . C15 C 0.7158(4) 0.5014(4) 0.9641(3) 0.0349(10) Uani 1 1 d . . . H15 H 0.6432 0.4541 0.9973 0.042 Uiso 1 1 calc R . . C16 C 0.8876(4) 0.5856(4) 0.9739(3) 0.0418(11) Uani 1 1 d . . . H16 H 0.9349 0.5995 1.0146 0.050 Uiso 1 1 calc R . . C17 C 0.9257(4) 0.6339(4) 0.8710(3) 0.0402(11) Uani 1 1 d . . . H17 H 1.0002 0.6784 0.8407 0.048 Uiso 1 1 calc R . . C18 C 1.1120(3) 0.8962(3) 0.4831(3) 0.0228(8) Uani 1 1 d . . . C19 C 1.1785(3) 0.9422(3) 0.5301(3) 0.0301(9) Uani 1 1 d . . . H19 H 1.1618 0.9133 0.6018 0.036 Uiso 1 1 calc R . . C20 C 1.2691(3) 1.0300(3) 0.4733(3) 0.0297(9) Uani 1 1 d . . . H20 H 1.3142 1.0603 0.5066 0.036 Uiso 1 1 calc R . . C23 C 1.1370(4) 0.9422(4) 0.3778(3) 0.0341(10) Uani 1 1 d . . . H23 H 1.0916 0.9126 0.3444 0.041 Uiso 1 1 calc R . . C25 C 0.5099(3) 0.5104(3) 0.2335(3) 0.0246(8) Uani 1 1 d . . . C26 C 0.4748(3) 0.6306(3) 0.1700(3) 0.0238(8) Uani 1 1 d . . . C27 C 0.4016(3) 0.6942(3) 0.2129(3) 0.0278(8) Uani 1 1 d . . . H27 H 0.3792 0.6661 0.2845 0.033 Uiso 1 1 calc R . . C28 C 0.3603(3) 0.7983(3) 0.1534(3) 0.0271(8) Uani 1 1 d . . . H28 H 0.3079 0.8395 0.1843 0.032 Uiso 1 1 calc R . . C29 C 0.3952(3) 0.8431(3) 0.0479(2) 0.0214(7) Uani 1 1 d . . . C30 C 0.4716(4) 0.7817(3) 0.0050(3) 0.0321(9) Uani 1 1 d . . . H30 H 0.4976 0.8118 -0.0664 0.038 Uiso 1 1 calc R . . C31 C 0.5106(4) 0.6765(3) 0.0654(3) 0.0316(9) Uani 1 1 d . . . H31 H 0.5628 0.6351 0.0346 0.038 Uiso 1 1 calc R . . C32 C 0.3456(3) 0.9509(3) -0.0174(2) 0.0206(7) Uani 1 1 d . . . C33 C 0.1939(3) 1.0745(3) -0.0297(3) 0.0221(8) Uani 1 1 d . . . C34 C 0.2408(3) 1.1394(3) -0.1326(3) 0.0241(8) Uani 1 1 d . . . H34 H 0.2023 1.2048 -0.1707 0.029 Uiso 1 1 calc R . . C35 C 0.3444(3) 1.1075(3) -0.1788(2) 0.0223(8) Uani 1 1 d . . . C36 C 0.3971(3) 1.0116(3) -0.1201(3) 0.0229(8) Uani 1 1 d . . . H36 H 0.4677 0.9873 -0.1492 0.027 Uiso 1 1 calc R . . C37 C 0.3946(3) 1.1735(3) -0.2889(3) 0.0225(8) Uani 1 1 d . . . C38 C 0.3764(3) 1.2920(3) -0.3376(3) 0.0280(8) Uani 1 1 d . . . H38 H 0.3349 1.3330 -0.3002 0.034 Uiso 1 1 calc R . . C39 C 0.4185(4) 1.3500(3) -0.4400(3) 0.0305(9) Uani 1 1 d . . . H39 H 0.4043 1.4306 -0.4737 0.037 Uiso 1 1 calc R . . C40 C 0.5027(4) 1.1817(3) -0.4481(3) 0.0310(9) Uani 1 1 d . . . H40 H 0.5489 1.1448 -0.4870 0.037 Uiso 1 1 calc R . . C41 C 0.4605(4) 1.1192(3) -0.3464(3) 0.0283(9) Uani 1 1 d . . . H41 H 0.4762 1.0386 -0.3151 0.034 Uiso 1 1 calc R . . N1 N 0.9851(3) 0.7377(3) 0.4916(2) 0.0241(7) Uani 1 1 d . . . N2 N 0.7859(3) 0.5198(3) 1.0179(2) 0.0354(8) Uani 1 1 d D . . N3 N 0.2469(3) 0.9831(3) 0.0266(2) 0.0229(7) Uani 1 1 d . . . N4 N 0.4793(3) 1.2938(3) -0.4925(2) 0.0288(7) Uani 1 1 d D . . O1 O 0.7000(2) 0.3223(2) 0.34263(18) 0.0246(6) Uani 1 1 d . . . O2 O 0.8159(3) 0.4596(3) 0.2062(2) 0.0462(8) Uani 1 1 d . . . O5 O 0.5582(2) 0.4503(2) 0.18474(19) 0.0292(6) Uani 1 1 d . . . O6 O 0.4879(3) 0.4779(2) 0.32608(19) 0.0379(7) Uani 1 1 d . . . Zn1 Zn 0.60369(4) 0.28726(4) 0.25592(3) 0.02418(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C21 0.024(2) 0.0210(18) 0.0233(18) -0.0075(15) -0.0012(15) -0.0006(15) C22 0.046(3) 0.045(2) 0.0189(19) -0.0101(18) -0.0018(18) -0.012(2) C24 0.027(2) 0.028(2) 0.030(2) -0.0150(17) 0.0052(16) -0.0035(16) C42 0.024(2) 0.0241(18) 0.0208(18) -0.0099(15) -0.0015(15) -0.0002(15) C43 0.033(2) 0.034(2) 0.0206(18) -0.0077(16) -0.0064(16) 0.0102(18) C44 0.032(2) 0.037(2) 0.0200(18) -0.0121(16) -0.0009(16) 0.0042(18) C45 0.0218(19) 0.0266(19) 0.0229(18) -0.0152(15) -0.0008(15) 0.0011(15) C46 0.026(2) 0.0258(19) 0.0257(19) -0.0086(16) -0.0040(16) 0.0044(16) C47 0.030(2) 0.031(2) 0.0182(18) -0.0071(15) -0.0024(15) 0.0040(17) C48 0.025(2) 0.034(2) 0.0248(19) -0.0192(17) -0.0036(16) 0.0005(17) O3 0.0283(15) 0.0337(15) 0.0283(14) -0.0089(12) -0.0002(12) -0.0095(12) O4 0.074(2) 0.079(3) 0.0221(16) -0.0172(16) 0.0126(16) -0.049(2) O7 0.0331(16) 0.0459(17) 0.0241(14) -0.0131(13) 0.0012(12) 0.0061(13) O8 0.0287(15) 0.0345(15) 0.0299(14) -0.0161(12) -0.0015(12) 0.0097(12) C1 0.028(2) 0.033(2) 0.0212(19) -0.0128(16) -0.0065(16) 0.0022(17) C2 0.024(2) 0.0284(19) 0.0226(18) -0.0124(15) -0.0065(15) 0.0007(16) C3 0.027(2) 0.0263(19) 0.0237(18) -0.0099(15) -0.0040(16) -0.0036(16) C4 0.033(2) 0.033(2) 0.0158(17) -0.0090(15) -0.0026(16) -0.0073(17) C5 0.024(2) 0.0301(19) 0.0216(18) -0.0125(15) -0.0051(15) -0.0011(16) C6 0.031(2) 0.031(2) 0.0216(18) -0.0076(16) -0.0035(16) -0.0104(17) C7 0.029(2) 0.035(2) 0.0173(17) -0.0100(16) -0.0028(15) -0.0029(17) C8 0.026(2) 0.0267(19) 0.0213(18) -0.0083(15) -0.0048(15) -0.0032(16) C9 0.030(2) 0.031(2) 0.0215(18) -0.0100(16) -0.0011(16) -0.0106(17) C10 0.024(2) 0.032(2) 0.0200(18) -0.0102(15) -0.0019(15) -0.0046(16) C11 0.029(2) 0.0273(19) 0.0185(17) -0.0113(15) -0.0030(15) -0.0030(16) C12 0.025(2) 0.0244(18) 0.0205(17) -0.0085(15) -0.0051(15) 0.0013(15) C13 0.033(2) 0.0262(19) 0.0197(18) -0.0099(15) -0.0003(16) -0.0071(16) C14 0.038(2) 0.042(2) 0.0214(19) -0.0127(17) -0.0009(17) -0.0108(19) C15 0.035(2) 0.039(2) 0.028(2) -0.0143(18) 0.0012(18) -0.0090(19) C16 0.054(3) 0.049(3) 0.023(2) -0.0152(19) -0.0056(19) -0.017(2) C17 0.046(3) 0.046(3) 0.023(2) -0.0126(18) 0.0012(19) -0.022(2) C18 0.0217(19) 0.0256(18) 0.0191(17) -0.0082(14) -0.0014(14) -0.0006(15) C19 0.035(2) 0.035(2) 0.0155(17) -0.0070(16) -0.0016(16) -0.0079(18) C20 0.030(2) 0.032(2) 0.028(2) -0.0141(17) -0.0037(17) -0.0086(17) C23 0.040(2) 0.039(2) 0.0209(19) -0.0101(17) -0.0051(17) -0.0148(19) C25 0.0218(19) 0.0247(19) 0.0210(18) -0.0039(15) -0.0016(15) -0.0042(15) C26 0.0218(19) 0.0254(19) 0.0216(18) -0.0063(15) -0.0059(15) -0.0001(15) C27 0.029(2) 0.034(2) 0.0114(16) -0.0030(15) 0.0012(15) -0.0006(17) C28 0.026(2) 0.0259(19) 0.0210(18) -0.0045(15) 0.0020(15) 0.0048(16) C29 0.0229(19) 0.0234(18) 0.0145(16) -0.0044(14) -0.0032(14) 0.0008(15) C30 0.041(2) 0.033(2) 0.0146(17) -0.0038(16) -0.0019(16) 0.0138(18) C31 0.037(2) 0.031(2) 0.0205(19) -0.0071(16) 0.0009(17) 0.0098(18) C32 0.0235(19) 0.0218(17) 0.0156(16) -0.0062(14) -0.0048(14) 0.0022(15) C33 0.0230(19) 0.0221(18) 0.0199(17) -0.0093(14) 0.0003(15) 0.0000(15) C34 0.026(2) 0.0222(18) 0.0216(18) -0.0063(15) -0.0050(15) 0.0058(15) C35 0.026(2) 0.0218(18) 0.0170(17) -0.0061(14) -0.0040(15) 0.0020(15) C36 0.0203(19) 0.0257(18) 0.0180(17) -0.0061(14) 0.0003(14) 0.0040(15) C37 0.0208(19) 0.0250(18) 0.0181(17) -0.0054(14) -0.0033(14) 0.0021(15) C38 0.029(2) 0.028(2) 0.0232(19) -0.0066(16) -0.0034(16) 0.0066(16) C39 0.034(2) 0.0241(19) 0.0245(19) -0.0014(16) -0.0051(17) 0.0043(17) C40 0.037(2) 0.032(2) 0.0208(19) -0.0096(16) -0.0019(17) 0.0060(18) C41 0.037(2) 0.0233(19) 0.0205(18) -0.0058(15) -0.0041(16) 0.0068(17) N1 0.0247(17) 0.0275(16) 0.0198(15) -0.0093(13) -0.0043(13) -0.0032(13) N2 0.049(2) 0.0343(19) 0.0185(16) -0.0108(14) 0.0044(15) -0.0111(17) N3 0.0243(17) 0.0222(15) 0.0190(15) -0.0065(12) -0.0015(13) 0.0020(13) N4 0.0355(19) 0.0296(17) 0.0131(14) -0.0016(13) -0.0019(14) 0.0027(15) O1 0.0295(14) 0.0212(13) 0.0238(13) -0.0095(10) -0.0066(11) -0.0016(11) O2 0.0488(19) 0.068(2) 0.0193(14) -0.0187(14) 0.0024(13) -0.0263(16) O5 0.0374(16) 0.0233(13) 0.0257(14) -0.0080(11) -0.0083(12) 0.0079(12) O6 0.0524(19) 0.0320(15) 0.0200(14) -0.0031(12) -0.0035(13) 0.0124(14) Zn1 0.0261(3) 0.0248(2) 0.0192(2) -0.00830(17) -0.00073(17) -0.00139(17) _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 C21 C20 1.381(5) . ? C21 C22 1.390(5) . ? C21 C24 1.510(5) . ? C22 C23 1.382(5) . ? C22 H22 0.9500 . ? C24 O4 1.215(5) . ? C24 O3 1.278(5) . ? C42 C47 1.394(5) . ? C42 C43 1.397(5) . ? C42 C33 1.484(5) . ? C43 C44 1.384(5) . ? C43 H43 0.9500 . ? C44 C45 1.388(5) . ? C44 H44 0.9500 . ? C45 C46 1.378(5) . ? C45 C48 1.505(5) . ? C46 C47 1.384(5) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 O7 1.224(4) . ? C48 O8 1.286(5) . ? C48 Zn1 2.591(4) 1_465 ? O3 Zn1 1.958(3) 1_665 ? O8 Zn1 1.984(3) 1_465 ? C1 O2 1.242(4) . ? C1 O1 1.266(4) . ? C1 C2 1.506(5) . ? C2 C7 1.385(5) . ? C2 C3 1.387(5) . ? C3 C4 1.390(5) . ? C3 H3 0.9500 . ? C4 C5 1.389(5) . ? C4 H4 0.9500 . ? C5 C6 1.392(5) . ? C5 C8 1.494(5) . ? C6 C7 1.389(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 N1 1.340(4) . ? C8 C9 1.395(5) . ? C9 C10 1.400(5) . ? C9 H9 0.9500 . ? C10 C11 1.392(5) . ? C10 C13 1.484(5) . ? C11 C12 1.383(5) . ? C11 H11 0.9500 . ? C12 N1 1.348(4) . ? C12 C18 1.490(5) . ? C13 C14 1.390(5) . ? C13 C17 1.392(5) . ? C14 C15 1.372(5) . ? C14 H14 0.9500 . ? C15 N2 1.320(5) . ? C15 H15 0.9500 . ? C16 N2 1.325(5) . ? C16 C17 1.368(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.388(5) . ? C18 C23 1.392(5) . ? C19 C20 1.385(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C23 H23 0.9500 . ? C25 O6 1.232(4) . ? C25 O5 1.279(4) . ? C25 C26 1.512(5) . ? C26 C27 1.380(5) . ? C26 C31 1.388(5) . ? C27 C28 1.384(5) . ? C27 H27 0.9500 . ? C28 C29 1.399(5) . ? C28 H28 0.9500 . ? C29 C30 1.379(5) . ? C29 C32 1.491(5) . ? C30 C31 1.385(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 N3 1.337(4) . ? C32 C36 1.397(5) . ? C33 N3 1.339(5) . ? C33 C34 1.396(5) . ? C34 C35 1.392(5) . ? C34 H34 0.9500 . ? C35 C36 1.383(5) . ? C35 C37 1.489(5) . ? C36 H36 0.9500 . ? C37 C38 1.386(5) . ? C37 C41 1.391(5) . ? C38 C39 1.372(5) . ? C38 H38 0.9500 . ? C39 N4 1.331(5) . ? C39 H39 0.9500 . ? C40 N4 1.329(5) . ? C40 C41 1.370(5) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? N2 H1A 0.902(19) . ? N4 H2A 0.899(19) . ? O1 Zn1 2.019(2) . ? O5 Zn1 1.990(2) . ? Zn1 O3 1.958(3) 1_445 ? Zn1 O8 1.984(3) 1_645 ? Zn1 C48 2.591(4) 1_645 ? 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 C20 C21 C22 119.0(3) . . ? C20 C21 C24 121.4(3) . . ? C22 C21 C24 119.5(3) . . ? C23 C22 C21 120.1(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? O4 C24 O3 123.0(4) . . ? O4 C24 C21 120.5(4) . . ? O3 C24 C21 116.5(3) . . ? C47 C42 C43 117.4(3) . . ? C47 C42 C33 122.9(3) . . ? C43 C42 C33 119.7(3) . . ? C44 C43 C42 121.2(4) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 120.4(3) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C46 C45 C44 119.1(3) . . ? C46 C45 C48 122.0(3) . . ? C44 C45 C48 118.9(3) . . ? C45 C46 C47 120.5(3) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C46 C47 C42 121.4(3) . . ? C46 C47 H47 119.3 . . ? C42 C47 H47 119.3 . . ? O7 C48 O8 122.9(4) . . ? O7 C48 C45 120.4(3) . . ? O8 C48 C45 116.6(3) . . ? O7 C48 Zn1 75.6(2) . 1_465 ? O8 C48 Zn1 48.29(17) . 1_465 ? C45 C48 Zn1 159.8(3) . 1_465 ? C24 O3 Zn1 107.5(2) . 1_665 ? C48 O8 Zn1 102.8(2) . 1_465 ? O2 C1 O1 125.4(3) . . ? O2 C1 C2 117.3(3) . . ? O1 C1 C2 117.2(3) . . ? C7 C2 C3 118.3(3) . . ? C7 C2 C1 120.0(3) . . ? C3 C2 C1 121.6(3) . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 121.5(3) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 118.0(3) . . ? C4 C5 C8 122.1(3) . . ? C6 C5 C8 120.0(3) . . ? C7 C6 C5 120.3(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C2 C7 C6 121.5(3) . . ? C2 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? N1 C8 C9 122.6(3) . . ? N1 C8 C5 115.7(3) . . ? C9 C8 C5 121.6(3) . . ? C8 C9 C10 118.9(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 117.9(3) . . ? C11 C10 C13 121.8(3) . . ? C9 C10 C13 120.1(3) . . ? C12 C11 C10 119.7(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? N1 C12 C11 122.3(3) . . ? N1 C12 C18 115.5(3) . . ? C11 C12 C18 122.1(3) . . ? C14 C13 C17 117.1(3) . . ? C14 C13 C10 122.1(3) . . ? C17 C13 C10 120.7(3) . . ? C15 C14 C13 120.5(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? N2 C15 C14 120.2(4) . . ? N2 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? N2 C16 C17 121.1(4) . . ? N2 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C13 119.6(4) . . ? C16 C17 H17 120.2 . . ? C13 C17 H17 120.2 . . ? C19 C18 C23 118.3(3) . . ? C19 C18 C12 121.2(3) . . ? C23 C18 C12 120.4(3) . . ? C20 C19 C18 120.5(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 120.8(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C23 C18 121.2(3) . . ? C22 C23 H23 119.4 . . ? C18 C23 H23 119.4 . . ? O6 C25 O5 125.8(3) . . ? O6 C25 C26 118.3(3) . . ? O5 C25 C26 115.8(3) . . ? C27 C26 C31 118.2(3) . . ? C27 C26 C25 121.7(3) . . ? C31 C26 C25 120.0(3) . . ? C26 C27 C28 121.1(3) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C29 120.3(4) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 118.6(3) . . ? C30 C29 C32 120.4(3) . . ? C28 C29 C32 120.9(3) . . ? C29 C30 C31 120.5(3) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C26 121.2(4) . . ? C30 C31 H31 119.4 . . ? C26 C31 H31 119.4 . . ? N3 C32 C36 122.0(3) . . ? N3 C32 C29 116.4(3) . . ? C36 C32 C29 121.5(3) . . ? N3 C33 C34 121.8(3) . . ? N3 C33 C42 115.9(3) . . ? C34 C33 C42 122.3(3) . . ? C35 C34 C33 119.5(3) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C36 C35 C34 118.1(3) . . ? C36 C35 C37 121.4(3) . . ? C34 C35 C37 120.5(3) . . ? C35 C36 C32 119.4(3) . . ? C35 C36 H36 120.3 . . ? C32 C36 H36 120.3 . . ? C38 C37 C41 117.8(3) . . ? C38 C37 C35 120.6(3) . . ? C41 C37 C35 121.6(3) . . ? C39 C38 C37 119.8(4) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? N4 C39 C38 120.4(3) . . ? N4 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? N4 C40 C41 120.1(4) . . ? N4 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C37 120.1(3) . . ? C40 C41 H41 120.0 . . ? C37 C41 H41 120.0 . . ? C8 N1 C12 118.6(3) . . ? C15 N2 C16 121.4(3) . . ? C15 N2 H1A 115(3) . . ? C16 N2 H1A 124(3) . . ? C32 N3 C33 119.1(3) . . ? C40 N4 C39 121.7(3) . . ? C40 N4 H2A 118(3) . . ? C39 N4 H2A 120(3) . . ? C1 O1 Zn1 116.9(2) . . ? C25 O5 Zn1 121.5(2) . . ? O3 Zn1 O8 131.75(11) 1_445 1_645 ? O3 Zn1 O5 109.28(11) 1_445 . ? O8 Zn1 O5 100.54(11) 1_645 . ? O3 Zn1 O1 103.04(10) 1_445 . ? O8 Zn1 O1 109.27(11) 1_645 . ? O5 Zn1 O1 98.28(10) . . ? O3 Zn1 C48 114.19(12) 1_445 1_645 ? O8 Zn1 C48 28.95(11) 1_645 1_645 ? O5 Zn1 C48 129.01(11) . 1_645 ? O1 Zn1 C48 96.68(11) . 1_645 ? 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 C20 C21 C22 C23 -1.4(6) . . . . ? C24 C21 C22 C23 175.5(4) . . . . ? C20 C21 C24 O4 -177.6(4) . . . . ? C22 C21 C24 O4 5.6(6) . . . . ? C20 C21 C24 O3 5.1(6) . . . . ? C22 C21 C24 O3 -171.6(4) . . . . ? C47 C42 C43 C44 -0.8(6) . . . . ? C33 C42 C43 C44 -178.9(3) . . . . ? C42 C43 C44 C45 -1.5(6) . . . . ? C43 C44 C45 C46 2.4(6) . . . . ? C43 C44 C45 C48 -176.2(3) . . . . ? C44 C45 C46 C47 -1.0(5) . . . . ? C48 C45 C46 C47 177.5(3) . . . . ? C45 C46 C47 C42 -1.3(6) . . . . ? C43 C42 C47 C46 2.2(6) . . . . ? C33 C42 C47 C46 -179.8(3) . . . . ? C46 C45 C48 O7 167.9(3) . . . . ? C44 C45 C48 O7 -13.6(5) . . . . ? C46 C45 C48 O8 -15.1(5) . . . . ? C44 C45 C48 O8 163.4(3) . . . . ? C46 C45 C48 Zn1 -52.6(9) . . . 1_465 ? C44 C45 C48 Zn1 125.9(7) . . . 1_465 ? O4 C24 O3 Zn1 -5.6(5) . . . 1_665 ? C21 C24 O3 Zn1 171.5(3) . . . 1_665 ? O7 C48 O8 Zn1 13.3(4) . . . 1_465 ? C45 C48 O8 Zn1 -163.7(2) . . . 1_465 ? O2 C1 C2 C7 4.7(6) . . . . ? O1 C1 C2 C7 -172.4(4) . . . . ? O2 C1 C2 C3 -178.2(4) . . . . ? O1 C1 C2 C3 4.8(6) . . . . ? C7 C2 C3 C4 2.3(6) . . . . ? C1 C2 C3 C4 -174.9(4) . . . . ? C2 C3 C4 C5 1.6(6) . . . . ? C3 C4 C5 C6 -3.9(6) . . . . ? C3 C4 C5 C8 177.3(4) . . . . ? C4 C5 C6 C7 2.3(6) . . . . ? C8 C5 C6 C7 -178.8(4) . . . . ? C3 C2 C7 C6 -3.9(6) . . . . ? C1 C2 C7 C6 173.3(4) . . . . ? C5 C6 C7 C2 1.6(6) . . . . ? C4 C5 C8 N1 171.2(4) . . . . ? C6 C5 C8 N1 -7.7(5) . . . . ? C4 C5 C8 C9 -6.5(6) . . . . ? C6 C5 C8 C9 174.6(4) . . . . ? N1 C8 C9 C10 -0.6(6) . . . . ? C5 C8 C9 C10 176.9(4) . . . . ? C8 C9 C10 C11 0.3(6) . . . . ? C8 C9 C10 C13 -176.0(4) . . . . ? C9 C10 C11 C12 0.1(6) . . . . ? C13 C10 C11 C12 176.3(4) . . . . ? C10 C11 C12 N1 -0.2(6) . . . . ? C10 C11 C12 C18 -176.2(3) . . . . ? C11 C10 C13 C14 156.5(4) . . . . ? C9 C10 C13 C14 -27.5(6) . . . . ? C11 C10 C13 C17 -28.2(6) . . . . ? C9 C10 C13 C17 147.9(4) . . . . ? C17 C13 C14 C15 -1.2(6) . . . . ? C10 C13 C14 C15 174.4(4) . . . . ? C13 C14 C15 N2 1.5(7) . . . . ? N2 C16 C17 C13 2.4(7) . . . . ? C14 C13 C17 C16 -0.8(7) . . . . ? C10 C13 C17 C16 -176.3(4) . . . . ? N1 C12 C18 C19 -162.0(4) . . . . ? C11 C12 C18 C19 14.3(6) . . . . ? N1 C12 C18 C23 15.1(5) . . . . ? C11 C12 C18 C23 -168.6(4) . . . . ? C23 C18 C19 C20 -1.4(6) . . . . ? C12 C18 C19 C20 175.8(4) . . . . ? C22 C21 C20 C19 1.0(6) . . . . ? C24 C21 C20 C19 -175.8(4) . . . . ? C18 C19 C20 C21 0.4(6) . . . . ? C21 C22 C23 C18 0.4(7) . . . . ? C19 C18 C23 C22 1.0(6) . . . . ? C12 C18 C23 C22 -176.2(4) . . . . ? O6 C25 C26 C27 -11.6(5) . . . . ? O5 C25 C26 C27 166.9(3) . . . . ? O6 C25 C26 C31 172.2(4) . . . . ? O5 C25 C26 C31 -9.4(5) . . . . ? C31 C26 C27 C28 3.0(6) . . . . ? C25 C26 C27 C28 -173.3(3) . . . . ? C26 C27 C28 C29 -2.0(6) . . . . ? C27 C28 C29 C30 -0.2(6) . . . . ? C27 C28 C29 C32 176.1(3) . . . . ? C28 C29 C30 C31 1.4(6) . . . . ? C32 C29 C30 C31 -175.0(4) . . . . ? C29 C30 C31 C26 -0.4(6) . . . . ? C27 C26 C31 C30 -1.8(6) . . . . ? C25 C26 C31 C30 174.6(4) . . . . ? C30 C29 C32 N3 159.5(3) . . . . ? C28 C29 C32 N3 -16.8(5) . . . . ? C30 C29 C32 C36 -17.9(5) . . . . ? C28 C29 C32 C36 165.8(3) . . . . ? C47 C42 C33 N3 -171.4(3) . . . . ? C43 C42 C33 N3 6.6(5) . . . . ? C47 C42 C33 C34 7.1(5) . . . . ? C43 C42 C33 C34 -174.9(3) . . . . ? N3 C33 C34 C35 1.1(5) . . . . ? C42 C33 C34 C35 -177.3(3) . . . . ? C33 C34 C35 C36 0.0(5) . . . . ? C33 C34 C35 C37 178.6(3) . . . . ? C34 C35 C36 C32 -0.2(5) . . . . ? C37 C35 C36 C32 -178.8(3) . . . . ? N3 C32 C36 C35 -0.6(5) . . . . ? C29 C32 C36 C35 176.6(3) . . . . ? C36 C35 C37 C38 -152.5(4) . . . . ? C34 C35 C37 C38 28.9(5) . . . . ? C36 C35 C37 C41 27.7(5) . . . . ? C34 C35 C37 C41 -150.9(4) . . . . ? C41 C37 C38 C39 2.9(5) . . . . ? C35 C37 C38 C39 -176.9(3) . . . . ? C37 C38 C39 N4 -1.7(6) . . . . ? N4 C40 C41 C37 -1.1(6) . . . . ? C38 C37 C41 C40 -1.5(6) . . . . ? C35 C37 C41 C40 178.3(4) . . . . ? C9 C8 N1 C12 0.6(6) . . . . ? C5 C8 N1 C12 -177.1(3) . . . . ? C11 C12 N1 C8 -0.2(5) . . . . ? C18 C12 N1 C8 176.1(3) . . . . ? C14 C15 N2 C16 0.2(7) . . . . ? C17 C16 N2 C15 -2.2(7) . . . . ? C36 C32 N3 C33 1.7(5) . . . . ? C29 C32 N3 C33 -175.7(3) . . . . ? C34 C33 N3 C32 -1.9(5) . . . . ? C42 C33 N3 C32 176.6(3) . . . . ? C41 C40 N4 C39 2.5(6) . . . . ? C38 C39 N4 C40 -1.1(6) . . . . ? O2 C1 O1 Zn1 -17.9(5) . . . . ? C2 C1 O1 Zn1 158.8(3) . . . . ? O6 C25 O5 Zn1 1.2(5) . . . . ? C26 C25 O5 Zn1 -177.2(2) . . . . ? C25 O5 Zn1 O3 54.5(3) . . . 1_445 ? C25 O5 Zn1 O8 -164.0(3) . . . 1_645 ? C25 O5 Zn1 O1 -52.5(3) . . . . ? C25 O5 Zn1 C48 -158.1(2) . . . 1_645 ? C1 O1 Zn1 O3 -160.0(3) . . . 1_445 ? C1 O1 Zn1 O8 56.4(3) . . . 1_645 ? C1 O1 Zn1 O5 -47.9(3) . . . . ? C1 O1 Zn1 C48 83.2(3) . . . 1_645 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1A O2 0.902(19) 1.94(3) 2.669(4) 137(4) 1_556 N2 H1A O5 0.902(19) 2.41(4) 3.083(4) 132(4) 1_556 N4 H2A O6 0.899(19) 1.95(3) 2.721(4) 142(4) 1_564 N4 H2A O1 0.899(19) 2.49(4) 3.068(4) 123(3) 1_564 N4 H2A O3 0.899(19) 2.58(4) 3.028(4) 111(3) 1_454 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.269 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.086 #===END #========================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 870235' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Cd N4 O8' _chemical_formula_weight 689.00 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number No.15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.3743(6) _cell_length_b 25.3285(11) _cell_length_c 11.2832(5) _cell_angle_alpha 90.00 _cell_angle_beta 130.1990(10) _cell_angle_gamma 90.00 _cell_volume 3356.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.615 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9233 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.06 _reflns_number_total 3312 _reflns_number_gt 3061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0784P)^2^+8.1380P] 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 3312 _refine_ls_number_parameters 187 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6340(3) 0.40918(15) 1.0414(4) 0.0294(7) Uani 1 1 d . . . C2 C 0.7060(3) 0.43709(14) 1.1950(4) 0.0282(7) Uani 1 1 d . . . C3 C 0.6666(3) 0.48286(15) 1.2135(4) 0.0362(9) Uani 1 1 d . . . H3 H 0.5923 0.4954 1.1305 0.043 Uiso 1 1 calc R . . C4 C 0.7351(3) 0.51053(15) 1.3529(4) 0.0360(9) Uani 1 1 d . . . H4 H 0.7063 0.5412 1.3654 0.043 Uiso 1 1 calc R . . C5 C 0.8449(3) 0.49370(13) 1.4736(4) 0.0292(7) Uani 1 1 d . . . C6 C 0.8825(3) 0.44676(15) 1.4555(4) 0.0364(9) Uani 1 1 d . . . H6 H 0.9564 0.4338 1.5387 0.044 Uiso 1 1 calc R . . C7 C 0.8133(3) 0.41895(15) 1.3178(4) 0.0355(8) Uani 1 1 d . . . H7 H 0.8400 0.3869 1.3076 0.043 Uiso 1 1 calc R . . C8 C 0.9227(3) 0.52471(14) 1.6187(4) 0.0291(8) Uani 1 1 d . . . C9 C 0.9178(3) 0.58006(14) 1.6159(4) 0.0298(8) Uani 1 1 d . . . H9 H 0.8588 0.5982 1.5233 0.036 Uiso 1 1 calc R . . C10 C 1.0000 0.60768(19) 1.7500 0.0288(10) Uani 1 2 d S . . C11 C 1.0000 0.66649(18) 1.7500 0.0282(10) Uani 1 2 d S . . C12 C 1.1012(3) 0.69501(14) 1.8321(4) 0.0351(9) Uani 1 1 d . . . H12 H 1.1723 0.6772 1.8900 0.042 Uiso 1 1 calc R . . C13 C 1.0970(3) 0.74916(15) 1.8281(5) 0.0358(9) Uani 1 1 d . . . H13 H 1.1666 0.7681 1.8838 0.043 Uiso 1 1 calc R . . N1 N 1.0000 0.77665(16) 1.7500 0.0293(9) Uani 1 2 d S . . N2 N 1.0000 0.49757(16) 1.7500 0.0293(9) Uani 1 2 d S . . O1 O 0.5504(3) 0.43239(11) 0.9254(3) 0.0462(8) Uani 1 1 d . . . O2 O 0.6595(3) 0.36326(12) 1.0332(4) 0.0514(9) Uani 1 1 d . . . Cd1 Cd 0.5000 0.367201(12) 0.7500 0.02344(15) Uani 1 2 d S . . O3 O 0.3444(3) 0.35518(14) 0.7506(4) 0.0521(8) Uiso 1 1 d . . . N3 N 0.2470(11) 0.3643(5) 0.8239(16) 0.086(4) Uiso 0.50 1 d PD . . C14' C 0.3712(11) 0.3636(5) 0.8824(17) 0.065(3) Uiso 0.50 1 d PD . . N3' N 0.3195(13) 0.3779(6) 0.9308(17) 0.102(4) Uiso 0.50 1 d PD . . C14 C 0.3281(11) 0.3754(5) 0.8194(15) 0.056(3) Uiso 0.50 1 d P . . C15 C 0.2151(17) 0.4005(8) 0.896(2) 0.114(6) Uiso 0.50 1 d PD . . C16' C 0.1961(17) 0.3949(11) 0.804(3) 0.144(8) Uiso 0.50 1 d PD . . C15' C 0.383(2) 0.3926(10) 1.098(2) 0.143(7) Uiso 0.50 1 d PD . . C16 C 0.1532(14) 0.3280(6) 0.7141(19) 0.100(5) Uiso 0.50 1 d PD . . O1W O 0.165(2) 0.2369(10) 0.715(3) 0.249(11) Uiso 0.50 1 d P . . O1W' O -0.058(3) 0.2567(15) 0.568(5) 0.355(18) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0263(17) 0.0324(19) 0.0228(16) -0.0079(14) 0.0129(15) -0.0045(14) C2 0.0284(18) 0.0265(17) 0.0201(16) -0.0037(13) 0.0113(15) -0.0029(14) C3 0.0282(18) 0.0303(19) 0.0228(17) -0.0030(14) 0.0041(15) 0.0054(15) C4 0.033(2) 0.0262(18) 0.0254(18) -0.0042(14) 0.0084(16) 0.0066(15) C5 0.0317(18) 0.0219(16) 0.0186(16) -0.0009(13) 0.0092(15) 0.0004(14) C6 0.0287(19) 0.0315(19) 0.0233(17) -0.0028(15) 0.0051(15) 0.0072(15) C7 0.034(2) 0.0294(18) 0.0278(18) -0.0066(15) 0.0126(16) 0.0051(15) C8 0.0305(19) 0.0223(17) 0.0186(17) 0.0014(13) 0.0087(16) 0.0006(13) C9 0.0334(19) 0.0201(16) 0.0190(16) 0.0015(12) 0.0091(15) 0.0007(13) C10 0.030(3) 0.019(2) 0.023(2) 0.000 0.011(2) 0.000 C11 0.030(3) 0.016(2) 0.020(2) 0.000 0.008(2) 0.000 C12 0.0238(18) 0.0244(18) 0.0311(19) 0.0005(14) 0.0060(16) 0.0025(14) C13 0.0217(17) 0.0247(18) 0.037(2) -0.0003(15) 0.0077(16) -0.0005(14) N1 0.023(2) 0.0193(19) 0.025(2) 0.000 0.0068(18) 0.000 N2 0.031(2) 0.0200(19) 0.019(2) 0.000 0.0077(18) 0.000 O1 0.0464(17) 0.0383(16) 0.0201(13) -0.0061(11) 0.0062(13) 0.0039(13) O2 0.0352(16) 0.0500(19) 0.0340(17) -0.0204(13) 0.0065(14) 0.0091(13) Cd1 0.0244(2) 0.0183(2) 0.0171(2) 0.000 0.00862(17) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.241(5) . ? C1 O2 1.250(4) . ? C1 C2 1.500(5) . ? C1 Cd1 2.728(3) . ? C2 C7 1.379(5) . ? C2 C3 1.386(5) . ? C3 C4 1.391(5) . ? C3 H3 0.9500 . ? C4 C5 1.386(5) . ? C4 H4 0.9500 . ? C5 C6 1.393(5) . ? C5 C8 1.483(5) . ? C6 C7 1.381(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 N2 1.344(4) . ? C8 C9 1.403(5) . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C9 1.381(4) 2_758 ? C10 C11 1.490(7) . ? C11 C12 1.393(4) . ? C11 C12 1.393(4) 2_758 ? C12 C13 1.372(5) . ? C12 H12 0.9500 . ? C13 N1 1.338(4) . ? C13 H13 0.9500 . ? N1 C13 1.338(4) 2_758 ? N1 Cd1 2.293(4) 3_556 ? N2 C8 1.344(4) 2_758 ? O1 Cd1 2.295(3) . ? O2 Cd1 2.474(3) . ? Cd1 N1 2.293(4) 3_444 ? Cd1 O1 2.295(3) 2_656 ? Cd1 O3 2.417(3) . ? Cd1 O3 2.417(3) 2_656 ? Cd1 O2 2.474(3) 2_656 ? Cd1 C1 2.728(3) 2_656 ? O3 C14 1.085(12) . ? O3 C14' 1.279(14) . ? N3 C16' 1.02(2) . ? N3 N3' 1.039(17) . ? N3 C14 1.310(17) . ? N3 C16 1.469(15) . ? N3 C15 1.505(16) . ? N3 C14' 1.566(14) . ? C14' C14 0.652(15) . ? C14' N3' 1.273(14) . ? N3' C14 1.347(18) . ? N3' C15 1.50(2) . ? N3' C15' 1.511(16) . ? N3' C16' 1.525(17) . ? C14 C16' 1.99(3) . ? C15 C16' 0.89(3) . ? C16' C16 1.87(3) . ? 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 O1 C1 O2 121.6(3) . . ? O1 C1 C2 119.0(3) . . ? O2 C1 C2 119.4(3) . . ? O1 C1 Cd1 56.70(18) . . ? O2 C1 Cd1 65.0(2) . . ? C2 C1 Cd1 174.8(3) . . ? C7 C2 C3 118.9(3) . . ? C7 C2 C1 121.1(3) . . ? C3 C2 C1 120.0(3) . . ? C2 C3 C4 120.4(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 118.4(3) . . ? C4 C5 C8 121.7(3) . . ? C6 C5 C8 119.9(3) . . ? C7 C6 C5 120.6(3) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C2 C7 C6 120.9(3) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? N2 C8 C9 122.2(3) . . ? N2 C8 C5 117.1(3) . . ? C9 C8 C5 120.7(3) . . ? C10 C9 C8 118.9(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C9 119.1(4) . 2_758 ? C9 C10 C11 120.4(2) . . ? C9 C10 C11 120.4(2) 2_758 . ? C12 C11 C12 117.5(4) . 2_758 ? C12 C11 C10 121.2(2) . . ? C12 C11 C10 121.2(2) 2_758 . ? C13 C12 C11 119.2(3) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? N1 C13 C12 123.4(4) . . ? N1 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? C13 N1 C13 117.2(4) . 2_758 ? C13 N1 Cd1 121.4(2) . 3_556 ? C13 N1 Cd1 121.4(2) 2_758 3_556 ? C8 N2 C8 118.5(4) 2_758 . ? C1 O1 Cd1 96.4(2) . . ? C1 O2 Cd1 87.8(2) . . ? N1 Cd1 O1 136.02(7) 3_444 . ? N1 Cd1 O1 136.02(7) 3_444 2_656 ? O1 Cd1 O1 87.95(15) . 2_656 ? N1 Cd1 O3 82.76(8) 3_444 . ? O1 Cd1 O3 82.62(12) . . ? O1 Cd1 O3 108.04(12) 2_656 . ? N1 Cd1 O3 82.76(8) 3_444 2_656 ? O1 Cd1 O3 108.04(12) . 2_656 ? O1 Cd1 O3 82.62(12) 2_656 2_656 ? O3 Cd1 O3 165.53(17) . 2_656 ? N1 Cd1 O2 87.69(7) 3_444 2_656 ? O1 Cd1 O2 130.13(11) . 2_656 ? O1 Cd1 O2 54.10(9) 2_656 2_656 ? O3 Cd1 O2 80.84(12) . 2_656 ? O3 Cd1 O2 98.57(13) 2_656 2_656 ? N1 Cd1 O2 87.69(7) 3_444 . ? O1 Cd1 O2 54.10(9) . . ? O1 Cd1 O2 130.13(11) 2_656 . ? O3 Cd1 O2 98.57(13) . . ? O3 Cd1 O2 80.84(12) 2_656 . ? O2 Cd1 O2 175.37(14) 2_656 . ? N1 Cd1 C1 112.94(8) 3_444 . ? O1 Cd1 C1 26.87(11) . . ? O1 Cd1 C1 109.33(10) 2_656 . ? O3 Cd1 C1 91.38(11) . . ? O3 Cd1 C1 94.25(11) 2_656 . ? O2 Cd1 C1 156.99(12) 2_656 . ? O2 Cd1 C1 27.26(10) . . ? N1 Cd1 C1 112.94(8) 3_444 2_656 ? O1 Cd1 C1 109.33(10) . 2_656 ? O1 Cd1 C1 26.87(11) 2_656 2_656 ? O3 Cd1 C1 94.25(11) . 2_656 ? O3 Cd1 C1 91.38(11) 2_656 2_656 ? O2 Cd1 C1 27.26(10) 2_656 2_656 ? O2 Cd1 C1 156.99(12) . 2_656 ? C1 Cd1 C1 134.12(16) . 2_656 ? C14 O3 C14' 30.6(7) . . ? C14 O3 Cd1 129.0(7) . . ? C14' O3 Cd1 114.0(6) . . ? C16' N3 N3' 95.6(17) . . ? C16' N3 C14 116(2) . . ? N3' N3 C14 68.9(11) . . ? C16' N3 C16 95.4(19) . . ? N3' N3 C16 157.1(17) . . ? C14 N3 C16 122.9(13) . . ? C16' N3 C15 35.0(15) . . ? N3' N3 C15 69.4(12) . . ? C14 N3 C15 122.8(12) . . ? C16 N3 C15 110.7(13) . . ? C16' N3 C14' 131.1(19) . . ? N3' N3 C14' 54.0(9) . . ? C14 N3 C14' 24.2(7) . . ? C16 N3 C14' 127.9(12) . . ? C15 N3 C14' 120.9(12) . . ? C14 C14' N3' 82.0(17) . . ? C14 C14' O3 58.0(16) . . ? N3' C14' O3 136.4(13) . . ? C14 C14' N3 55.3(15) . . ? N3' C14' N3 41.4(8) . . ? O3 C14' N3 97.0(10) . . ? N3 N3' C14' 84.6(12) . . ? N3 N3' C14 65.1(12) . . ? C14' N3' C14 28.6(7) . . ? N3 N3' C15 70.1(12) . . ? C14' N3' C15 149.0(16) . . ? C14 N3' C15 120.6(15) . . ? N3 N3' C15' 151.2(18) . . ? C14' N3' C15' 121.9(16) . . ? C14 N3' C15' 143.7(16) . . ? C15 N3' C15' 87.1(14) . . ? N3 N3' C16' 41.7(12) . . ? C14' N3' C16' 115.0(16) . . ? C14 N3' C16' 87.3(15) . . ? C15 N3' C16' 34.2(11) . . ? C15' N3' C16' 120.7(17) . . ? C14' C14 O3 91.4(18) . . ? C14' C14 N3 100.5(18) . . ? O3 C14 N3 126.3(12) . . ? C14' C14 N3' 69.3(16) . . ? O3 C14 N3' 153.7(13) . . ? N3 C14 N3' 46.0(9) . . ? C14' C14 C16' 118.0(18) . . ? O3 C14 C16' 138.6(12) . . ? N3 C14 C16' 27.3(10) . . ? N3' C14 C16' 50.1(9) . . ? C16' C15 N3' 74.5(17) . . ? C16' C15 N3 41.1(17) . . ? N3' C15 N3 40.5(8) . . ? C15 C16' N3 104(3) . . ? C15 C16' N3' 71.3(18) . . ? N3 C16' N3' 42.7(11) . . ? C15 C16' C16 121(3) . . ? N3 C16' C16 51.6(16) . . ? N3' C16' C16 92.5(16) . . ? C15 C16' C14 113(2) . . ? N3 C16' C14 36.2(13) . . ? N3' C16' C14 42.6(9) . . ? C16 C16' C14 78.6(12) . . ? N3 C16 C16' 33.0(8) . . ? 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 O1 C1 C2 C7 -164.1(4) . . . . ? O2 C1 C2 C7 15.7(6) . . . . ? Cd1 C1 C2 C7 -130(3) . . . . ? O1 C1 C2 C3 13.7(6) . . . . ? O2 C1 C2 C3 -166.4(4) . . . . ? Cd1 C1 C2 C3 48(3) . . . . ? C7 C2 C3 C4 1.2(6) . . . . ? C1 C2 C3 C4 -176.7(4) . . . . ? C2 C3 C4 C5 2.0(7) . . . . ? C3 C4 C5 C6 -3.9(6) . . . . ? C3 C4 C5 C8 175.2(4) . . . . ? C4 C5 C6 C7 2.7(6) . . . . ? C8 C5 C6 C7 -176.4(4) . . . . ? C3 C2 C7 C6 -2.4(6) . . . . ? C1 C2 C7 C6 175.5(4) . . . . ? C5 C6 C7 C2 0.4(7) . . . . ? C4 C5 C8 N2 149.2(4) . . . . ? C6 C5 C8 N2 -31.7(5) . . . . ? C4 C5 C8 C9 -33.3(6) . . . . ? C6 C5 C8 C9 145.8(4) . . . . ? N2 C8 C9 C10 4.8(5) . . . . ? C5 C8 C9 C10 -172.6(3) . . . . ? C8 C9 C10 C9 -2.3(3) . . . 2_758 ? C8 C9 C10 C11 177.7(3) . . . . ? C9 C10 C11 C12 -140.4(3) . . . . ? C9 C10 C11 C12 39.6(3) 2_758 . . . ? C9 C10 C11 C12 39.6(3) . . . 2_758 ? C9 C10 C11 C12 -140.4(3) 2_758 . . 2_758 ? C12 C11 C12 C13 -0.3(3) 2_758 . . . ? C10 C11 C12 C13 179.7(3) . . . . ? C11 C12 C13 N1 0.6(6) . . . . ? C12 C13 N1 C13 -0.3(3) . . . 2_758 ? C12 C13 N1 Cd1 179.7(3) . . . 3_556 ? C9 C8 N2 C8 -2.4(3) . . . 2_758 ? C5 C8 N2 C8 175.1(4) . . . 2_758 ? O2 C1 O1 Cd1 -3.4(4) . . . . ? C2 C1 O1 Cd1 176.5(3) . . . . ? O1 C1 O2 Cd1 3.1(4) . . . . ? C2 C1 O2 Cd1 -176.7(3) . . . . ? C1 O1 Cd1 N1 36.5(3) . . . 3_444 ? C1 O1 Cd1 O1 -143.5(3) . . . 2_656 ? C1 O1 Cd1 O3 108.0(3) . . . . ? C1 O1 Cd1 O3 -61.9(3) . . . 2_656 ? C1 O1 Cd1 O2 179.4(2) . . . 2_656 ? C1 O1 Cd1 O2 1.8(2) . . . . ? C1 O1 Cd1 C1 -160.04(19) . . . 2_656 ? C1 O2 Cd1 N1 -158.5(3) . . . 3_444 ? C1 O2 Cd1 O1 -1.8(2) . . . . ? C1 O2 Cd1 O1 46.3(3) . . . 2_656 ? C1 O2 Cd1 O3 -76.2(3) . . . . ? C1 O2 Cd1 O3 118.5(3) . . . 2_656 ? C1 O2 Cd1 O2 -158.5(3) . . . 2_656 ? C1 O2 Cd1 C1 47.0(5) . . . 2_656 ? O1 C1 Cd1 N1 -153.3(2) . . . 3_444 ? O2 C1 Cd1 N1 23.5(3) . . . 3_444 ? C2 C1 Cd1 N1 170(3) . . . 3_444 ? O2 C1 Cd1 O1 176.8(4) . . . . ? C2 C1 Cd1 O1 -36(3) . . . . ? O1 C1 Cd1 O1 39.1(3) . . . 2_656 ? O2 C1 Cd1 O1 -144.1(3) . . . 2_656 ? C2 C1 Cd1 O1 3(3) . . . 2_656 ? O1 C1 Cd1 O3 -70.6(3) . . . . ? O2 C1 Cd1 O3 106.2(3) . . . . ? C2 C1 Cd1 O3 -107(3) . . . . ? O1 C1 Cd1 O3 122.7(3) . . . 2_656 ? O2 C1 Cd1 O3 -60.5(3) . . . 2_656 ? C2 C1 Cd1 O3 86(3) . . . 2_656 ? O1 C1 Cd1 O2 -1.1(4) . . . 2_656 ? O2 C1 Cd1 O2 175.66(13) . . . 2_656 ? C2 C1 Cd1 O2 -37(3) . . . 2_656 ? O1 C1 Cd1 O2 -176.8(4) . . . . ? C2 C1 Cd1 O2 147(3) . . . . ? O1 C1 Cd1 C1 26.7(2) . . . 2_656 ? O2 C1 Cd1 C1 -156.5(3) . . . 2_656 ? C2 C1 Cd1 C1 -10(3) . . . 2_656 ? N1 Cd1 O3 C14 135.5(9) 3_444 . . . ? O1 Cd1 O3 C14 -2.9(9) . . . . ? O1 Cd1 O3 C14 -88.3(9) 2_656 . . . ? O3 Cd1 O3 C14 135.5(9) 2_656 . . . ? O2 Cd1 O3 C14 -135.7(9) 2_656 . . . ? O2 Cd1 O3 C14 49.0(9) . . . . ? C1 Cd1 O3 C14 22.6(9) . . . . ? C1 Cd1 O3 C14 -111.9(9) 2_656 . . . ? N1 Cd1 O3 C14' 103.9(7) 3_444 . . . ? O1 Cd1 O3 C14' -34.5(7) . . . . ? O1 Cd1 O3 C14' -119.9(7) 2_656 . . . ? O3 Cd1 O3 C14' 103.9(7) 2_656 . . . ? O2 Cd1 O3 C14' -167.3(7) 2_656 . . . ? O2 Cd1 O3 C14' 17.3(7) . . . . ? C1 Cd1 O3 C14' -9.1(7) . . . . ? C1 Cd1 O3 C14' -143.5(7) 2_656 . . . ? Cd1 O3 C14' C14 126.9(17) . . . . ? C14 O3 C14' N3' 26.7(16) . . . . ? Cd1 O3 C14' N3' 153.6(15) . . . . ? C14 O3 C14' N3 41.2(15) . . . . ? Cd1 O3 C14' N3 168.1(5) . . . . ? C16' N3 C14' C14 -60(3) . . . . ? N3' N3 C14' C14 -122(2) . . . . ? C16 N3 C14' C14 87(2) . . . . ? C15 N3 C14' C14 -102(2) . . . . ? C16' N3 C14' N3' 62(3) . . . . ? C14 N3 C14' N3' 122(2) . . . . ? C16 N3 C14' N3' -151(2) . . . . ? C15 N3 C14' N3' 20.0(16) . . . . ? C16' N3 C14' O3 -103(3) . . . . ? N3' N3 C14' O3 -164.8(15) . . . . ? C14 N3 C14' O3 -42.8(17) . . . . ? C16 N3 C14' O3 43.9(17) . . . . ? C15 N3 C14' O3 -144.8(14) . . . . ? C16' N3 N3' C14' -138(2) . . . . ? C14 N3 N3' C14' -21.9(9) . . . . ? C16 N3 N3' C14' 104(4) . . . . ? C15 N3 N3' C14' -161.7(14) . . . . ? C16' N3 N3' C14 -116(2) . . . . ? C16 N3 N3' C14 125(4) . . . . ? C15 N3 N3' C14 -139.9(13) . . . . ? C14' N3 N3' C14 21.9(9) . . . . ? C16' N3 N3' C15 24(2) . . . . ? C14 N3 N3' C15 139.9(13) . . . . ? C16 N3 N3' C15 -95(4) . . . . ? C14' N3 N3' C15 161.7(14) . . . . ? C16' N3 N3' C15' 63(4) . . . . ? C16 N3 N3' C15' -55(6) . . . . ? C15 N3 N3' C15' 40(4) . . . . ? C14' N3 N3' C15' -159(4) . . . . ? C14 N3 N3' C16' 116(2) . . . . ? C16 N3 N3' C16' -118(4) . . . . ? C15 N3 N3' C16' -24(2) . . . . ? C14' N3 N3' C16' 138(2) . . . . ? C14 C14' N3' N3 45(2) . . . . ? O3 C14' N3' N3 22(2) . . . . ? O3 C14' N3' C14 -22.6(14) . . . . ? N3 C14' N3' C14 -45(2) . . . . ? C14 C14' N3' C15 10(4) . . . . ? O3 C14' N3' C15 -13(4) . . . . ? N3 C14' N3' C15 -35(2) . . . . ? C14 C14' N3' C15' -147(2) . . . . ? O3 C14' N3' C15' -169.9(16) . . . . ? N3 C14' N3' C15' 168(2) . . . . ? C14 C14' N3' C16' 15(2) . . . . ? O3 C14' N3' C16' -7(3) . . . . ? N3 C14' N3' C16' -29.4(14) . . . . ? N3' C14' C14 O3 -161.8(10) . . . . ? N3 C14' C14 O3 -127.3(14) . . . . ? N3' C14' C14 N3 -34.5(13) . . . . ? O3 C14' C14 N3 127.3(14) . . . . ? O3 C14' C14 N3' 161.8(10) . . . . ? N3 C14' C14 N3' 34.5(13) . . . . ? N3' C14' C14 C16' -12.1(19) . . . . ? O3 C14' C14 C16' 150(2) . . . . ? N3 C14' C14 C16' 22.4(12) . . . . ? Cd1 O3 C14 C14' -70.1(19) . . . . ? C14' O3 C14 N3 -104(2) . . . . ? Cd1 O3 C14 N3 -174.2(10) . . . . ? C14' O3 C14 N3' -41(3) . . . . ? Cd1 O3 C14 N3' -112(3) . . . . ? C14' O3 C14 C16' -138(3) . . . . ? Cd1 O3 C14 C16' 152.4(14) . . . . ? C16' N3 C14 C14' 133(3) . . . . ? N3' N3 C14 C14' 47(2) . . . . ? C16 N3 C14 C14' -110(2) . . . . ? C15 N3 C14 C14' 93(2) . . . . ? C16' N3 C14 O3 -127(2) . . . . ? N3' N3 C14 O3 146.9(17) . . . . ? C16 N3 C14 O3 -11(2) . . . . ? C15 N3 C14 O3 -167.3(15) . . . . ? C14' N3 C14 O3 100(2) . . . . ? C16' N3 C14 N3' 86(2) . . . . ? C16 N3 C14 N3' -158(2) . . . . ? C15 N3 C14 N3' 45.8(16) . . . . ? C14' N3 C14 N3' -47(2) . . . . ? N3' N3 C14 C16' -86(2) . . . . ? C16 N3 C14 C16' 117(3) . . . . ? C15 N3 C14 C16' -39.8(17) . . . . ? C14' N3 C14 C16' -133(3) . . . . ? N3 N3' C14 C14' -129(2) . . . . ? C15 N3' C14 C14' -174(2) . . . . ? C15' N3' C14 C14' 51(3) . . . . ? C16' N3' C14 C14' -166(2) . . . . ? N3 N3' C14 O3 -84(3) . . . . ? C14' N3' C14 O3 45(3) . . . . ? C15 N3' C14 O3 -129(3) . . . . ? C15' N3' C14 O3 96(4) . . . . ? C16' N3' C14 O3 -121(3) . . . . ? C14' N3' C14 N3 129(2) . . . . ? C15 N3' C14 N3 -44.7(14) . . . . ? C15' N3' C14 N3 -180(3) . . . . ? C16' N3' C14 N3 -36.7(13) . . . . ? N3 N3' C14 C16' 36.7(13) . . . . ? C14' N3' C14 C16' 166(2) . . . . ? C15 N3' C14 C16' -8.1(17) . . . . ? C15' N3' C14 C16' -143(3) . . . . ? N3 N3' C15 C16' -28(3) . . . . ? C14' N3' C15 C16' 9(4) . . . . ? C14 N3' C15 C16' 14(3) . . . . ? C15' N3' C15 C16' 170(3) . . . . ? C14' N3' C15 N3 37(3) . . . . ? C14 N3' C15 N3 42.8(13) . . . . ? C15' N3' C15 N3 -162.0(19) . . . . ? C16' N3' C15 N3 28(3) . . . . ? N3' N3 C15 C16' 136(4) . . . . ? C14 N3 C15 C16' 90(3) . . . . ? C16 N3 C15 C16' -69(3) . . . . ? C14' N3 C15 C16' 119(3) . . . . ? C16' N3 C15 N3' -136(4) . . . . ? C14 N3 C15 N3' -45.6(15) . . . . ? C16 N3 C15 N3' 155.5(18) . . . . ? C14' N3 C15 N3' -17.2(14) . . . . ? N3' C15 C16' N3 28(2) . . . . ? N3 C15 C16' N3' -28(2) . . . . ? N3' C15 C16' C16 81(2) . . . . ? N3 C15 C16' C16 53(2) . . . . ? N3' C15 C16' C14 -9.1(19) . . . . ? N3 C15 C16' C14 -37.0(13) . . . . ? N3' N3 C16' C15 -41(3) . . . . ? C14 N3 C16' C15 -110(3) . . . . ? C16 N3 C16' C15 119(3) . . . . ? C14' N3 C16' C15 -87(4) . . . . ? C14 N3 C16' N3' -69.2(16) . . . . ? C16 N3 C16' N3' 159.8(18) . . . . ? C15 N3 C16' N3' 41(3) . . . . ? C14' N3 C16' N3' -45.8(18) . . . . ? N3' N3 C16' C16 -159.8(18) . . . . ? C14 N3 C16' C16 131(2) . . . . ? C15 N3 C16' C16 -119(3) . . . . ? C14' N3 C16' C16 154(3) . . . . ? N3' N3 C16' C14 69.2(15) . . . . ? C16 N3 C16' C14 -131(2) . . . . ? C15 N3 C16' C14 110(3) . . . . ? C14' N3 C16' C14 23.4(12) . . . . ? N3 N3' C16' C15 138(4) . . . . ? C14' N3' C16' C15 -175(2) . . . . ? C14 N3' C16' C15 -168(3) . . . . ? C15' N3' C16' C15 -12(3) . . . . ? C14' N3' C16' N3 47(2) . . . . ? C14 N3' C16' N3 54.5(18) . . . . ? C15 N3' C16' N3 -138(4) . . . . ? C15' N3' C16' N3 -150(2) . . . . ? N3 N3' C16' C16 15.7(14) . . . . ? C14' N3' C16' C16 62.9(18) . . . . ? C14 N3' C16' C16 70.2(13) . . . . ? C15 N3' C16' C16 -122(3) . . . . ? C15' N3' C16' C16 -134.2(18) . . . . ? N3 N3' C16' C14 -54.5(18) . . . . ? C14' N3' C16' C14 -7.3(11) . . . . ? C15 N3' C16' C14 168(3) . . . . ? C15' N3' C16' C14 156(2) . . . . ? C14' C14 C16' C15 28(4) . . . . ? O3 C14 C16' C15 158(3) . . . . ? N3 C14 C16' C15 82(3) . . . . ? N3' C14 C16' C15 13(3) . . . . ? C14' C14 C16' N3 -55(3) . . . . ? O3 C14 C16' N3 76(3) . . . . ? N3' C14 C16' N3 -69(2) . . . . ? C14' C14 C16' N3' 15(2) . . . . ? O3 C14 C16' N3' 145.0(19) . . . . ? N3 C14 C16' N3' 69(2) . . . . ? C14' C14 C16' C16 -92(2) . . . . ? O3 C14 C16' C16 39(2) . . . . ? N3 C14 C16' C16 -37.1(19) . . . . ? N3' C14 C16' C16 -106.5(15) . . . . ? N3' N3 C16 C16' 118(4) . . . . ? C14 N3 C16 C16' -126(3) . . . . ? C15 N3 C16 C16' 32.4(17) . . . . ? C14' N3 C16 C16' -156(3) . . . . ? C15 C16' C16 N3 -83(3) . . . . ? N3' C16' C16 N3 -13.5(13) . . . . ? C14 C16' C16 N3 27.0(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.285 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.129 #===END