# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xiaohong Peng' _publ_contact_author_email nan-feiyan@163.com _publ_author_name 'Xiaohong Peng' #=================================END data_3 _database_code_depnum_ccdc_archive 'CCDC 727396' #TrackingRef '- crystal data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H66 N4 O9 Zn2' _chemical_formula_weight 997.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.739(2) _cell_length_b 10.4668(11) _cell_length_c 29.254(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.362(2) _cell_angle_gamma 90.00 _cell_volume 5057.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5570 _cell_measurement_theta_min 2.117 _cell_measurement_theta_max 23.889 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6387 _exptl_absorpt_correction_T_max 0.8018 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25503 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8913 _reflns_number_gt 5879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.0541P)^2^+1.7596P] 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 8913 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.05532(2) 0.19831(4) 0.357093(14) 0.03005(13) Uani 1 1 d . . . Zn2 Zn 0.07107(3) 0.26143(4) 0.563614(15) 0.03603(14) Uani 1 1 d . . . N1 N 0.05963(16) 0.3653(3) 0.32087(9) 0.0291(7) Uani 1 1 d . . . N2 N -0.01347(16) 0.4298(3) 0.30909(10) 0.0332(7) Uani 1 1 d . . . H2 H -0.0173 0.5005 0.2939 0.040 Uiso 1 1 calc R . . N3 N 0.05424(19) 0.4545(3) 0.56699(11) 0.0392(8) Uani 1 1 d . . . N4 N -0.02515(18) 0.4895(3) 0.56849(11) 0.0406(8) Uani 1 1 d . . . H4 H -0.0408 0.5678 0.5658 0.049 Uiso 1 1 calc R . . O1 O 0.17119(14) 0.1793(2) 0.35591(9) 0.0379(6) Uani 1 1 d . . . O2 O -0.06994(15) 0.2737(3) 0.34613(9) 0.0446(7) Uani 1 1 d . . . O3 O 0.05085(16) 0.2368(2) 0.42431(8) 0.0399(7) Uani 1 1 d . . . O4 O 0.03900(18) 0.2297(3) 0.49642(9) 0.0598(9) Uani 1 1 d . . . O5 O 0.02543(14) 0.0145(2) 0.35099(8) 0.0361(6) Uani 1 1 d . . . O6 O 0.02228(16) 0.0492(2) 0.27629(9) 0.0435(7) Uani 1 1 d . . . O7 O 0.18728(16) 0.2908(2) 0.57361(10) 0.0494(7) Uani 1 1 d . . . O8 O -0.05045(17) 0.2821(3) 0.57763(10) 0.0478(7) Uani 1 1 d . . . O9 O 0.07302(16) 0.0935(3) 0.59709(10) 0.0507(8) Uani 1 1 d . . . H9 H 0.0379 0.0718 0.6121 0.076 Uiso 1 1 d R . . C1 C 0.1217(2) 0.4144(4) 0.30656(12) 0.0334(9) Uani 1 1 d . . . H1 H 0.1141 0.4922 0.2911 0.040 Uiso 1 1 calc R . . C2 C 0.2008(2) 0.3606(4) 0.31216(12) 0.0308(9) Uani 1 1 d . . . C3 C 0.2212(2) 0.2423(4) 0.33522(12) 0.0325(9) Uani 1 1 d . . . C4 C 0.3017(2) 0.1939(4) 0.33496(12) 0.0341(9) Uani 1 1 d . . . C5 C 0.3552(2) 0.2688(4) 0.31645(13) 0.0413(10) Uani 1 1 d . . . H5 H 0.4074 0.2373 0.3174 0.050 Uiso 1 1 calc R . . C6 C 0.3380(2) 0.3890(4) 0.29617(13) 0.0385(10) Uani 1 1 d . . . C7 C 0.2603(2) 0.4310(4) 0.29381(13) 0.0380(10) Uani 1 1 d . . . H7 H 0.2458 0.5090 0.2796 0.046 Uiso 1 1 calc R . . C8 C 0.3236(2) 0.0595(4) 0.35420(15) 0.0472(11) Uani 1 1 d . . . C9 C 0.3242(3) 0.0578(5) 0.40672(15) 0.0685(15) Uani 1 1 d . . . H9A H 0.3637 0.1177 0.4214 0.103 Uiso 1 1 calc R . . H9B H 0.3378 -0.0264 0.4185 0.103 Uiso 1 1 calc R . . H9C H 0.2716 0.0810 0.4131 0.103 Uiso 1 1 calc R . . C10 C 0.2627(3) -0.0399(4) 0.33060(17) 0.0616(13) Uani 1 1 d . . . H10A H 0.2121 -0.0300 0.3416 0.092 Uiso 1 1 calc R . . H10B H 0.2835 -0.1243 0.3378 0.092 Uiso 1 1 calc R . . H10C H 0.2546 -0.0273 0.2977 0.092 Uiso 1 1 calc R . . C11 C 0.4076(3) 0.0170(5) 0.34518(18) 0.0761(16) Uani 1 1 d . . . H11A H 0.4095 0.0219 0.3126 0.114 Uiso 1 1 calc R . . H11B H 0.4175 -0.0694 0.3556 0.114 Uiso 1 1 calc R . . H11C H 0.4483 0.0719 0.3617 0.114 Uiso 1 1 calc R . . C12 C 0.4040(2) 0.4679(5) 0.27828(16) 0.0525(12) Uani 1 1 d . . . C13 C 0.4655(3) 0.5101(7) 0.3183(2) 0.112(3) Uani 1 1 d . . . H13A H 0.4805 0.4391 0.3387 0.168 Uiso 1 1 calc R . . H13B H 0.4430 0.5766 0.3349 0.168 Uiso 1 1 calc R . . H13C H 0.5126 0.5419 0.3071 0.168 Uiso 1 1 calc R . . C14 C 0.4462(4) 0.3888(7) 0.2470(2) 0.134(3) Uani 1 1 d . . . H14A H 0.4833 0.4415 0.2335 0.200 Uiso 1 1 calc R . . H14B H 0.4069 0.3530 0.2228 0.200 Uiso 1 1 calc R . . H14C H 0.4755 0.3211 0.2644 0.200 Uiso 1 1 calc R . . C15 C 0.3717(3) 0.5853(7) 0.2531(3) 0.149(4) Uani 1 1 d . . . H15A H 0.3412 0.6337 0.2722 0.223 Uiso 1 1 calc R . . H15B H 0.3373 0.5618 0.2248 0.223 Uiso 1 1 calc R . . H15C H 0.4159 0.6362 0.2461 0.223 Uiso 1 1 calc R . . C16 C -0.0781(2) 0.3738(4) 0.32312(13) 0.0333(9) Uani 1 1 d . . . C17 C -0.1567(2) 0.4399(4) 0.31143(12) 0.0341(9) Uani 1 1 d . . . C18 C -0.1639(2) 0.5649(4) 0.29609(14) 0.0461(11) Uani 1 1 d . . . H18 H -0.1177 0.6104 0.2923 0.055 Uiso 1 1 calc R . . C19 C -0.2382(3) 0.6230(4) 0.28632(15) 0.0538(12) Uani 1 1 d . . . H19 H -0.2424 0.7069 0.2757 0.065 Uiso 1 1 calc R . . C20 C -0.3065(3) 0.5563(5) 0.29231(16) 0.0587(13) Uani 1 1 d . . . H20 H -0.3569 0.5957 0.2861 0.070 Uiso 1 1 calc R . . C21 C -0.3008(3) 0.4324(5) 0.30738(18) 0.0673(15) Uani 1 1 d . . . H21 H -0.3473 0.3875 0.3111 0.081 Uiso 1 1 calc R . . C22 C -0.2254(2) 0.3737(5) 0.31717(16) 0.0565(13) Uani 1 1 d . . . H22 H -0.2215 0.2896 0.3276 0.068 Uiso 1 1 calc R . . C23 C 0.1066(2) 0.5425(4) 0.56395(14) 0.0429(10) Uani 1 1 d . . . H23 H 0.0887 0.6267 0.5621 0.052 Uiso 1 1 calc R . . C24 C 0.1908(2) 0.5196(4) 0.56323(14) 0.0400(10) Uani 1 1 d . . . C25 C 0.2279(2) 0.3954(4) 0.56833(14) 0.0407(10) Uani 1 1 d . . . C26 C 0.3127(2) 0.3891(4) 0.56785(13) 0.0390(10) Uani 1 1 d . . . C27 C 0.3545(3) 0.5003(4) 0.56311(14) 0.0465(11) Uani 1 1 d . . . H27 H 0.4099 0.4941 0.5632 0.056 Uiso 1 1 calc R . . C28 C 0.3199(3) 0.6212(4) 0.55816(14) 0.0453(11) Uani 1 1 d . . . C29 C 0.2383(3) 0.6278(4) 0.55848(14) 0.0482(11) Uani 1 1 d . . . H29 H 0.2133 0.7074 0.5554 0.058 Uiso 1 1 calc R . . C30 C 0.3577(2) 0.2605(4) 0.57255(15) 0.0433(10) Uani 1 1 d . . . C31 C 0.4466(3) 0.2729(5) 0.5680(2) 0.0777(17) Uani 1 1 d . . . H31A H 0.4716 0.1901 0.5709 0.117 Uiso 1 1 calc R . . H31B H 0.4733 0.3281 0.5919 0.117 Uiso 1 1 calc R . . H31C H 0.4510 0.3083 0.5382 0.117 Uiso 1 1 calc R . . C32 C 0.3184(3) 0.1678(4) 0.53504(16) 0.0668(14) Uani 1 1 d . . . H32A H 0.3252 0.1995 0.5051 0.100 Uiso 1 1 calc R . . H32B H 0.2617 0.1603 0.5365 0.100 Uiso 1 1 calc R . . H32C H 0.3436 0.0855 0.5400 0.100 Uiso 1 1 calc R . . C33 C 0.3544(3) 0.2039(4) 0.62022(15) 0.0592(13) Uani 1 1 d . . . H33A H 0.3780 0.1201 0.6222 0.089 Uiso 1 1 calc R . . H33B H 0.2990 0.1983 0.6249 0.089 Uiso 1 1 calc R . . H33C H 0.3841 0.2576 0.6436 0.089 Uiso 1 1 calc R . . C34 C 0.3695(3) 0.7426(4) 0.55343(17) 0.0574(13) Uani 1 1 d . . . C35 C 0.3702(3) 0.8257(5) 0.59558(18) 0.0783(16) Uani 1 1 d . . . H35A H 0.4036 0.8993 0.5933 0.117 Uiso 1 1 calc R . . H35B H 0.3915 0.7781 0.6229 0.117 Uiso 1 1 calc R . . H35C H 0.3160 0.8527 0.5974 0.117 Uiso 1 1 calc R . . C36 C 0.3326(4) 0.8153(5) 0.51042(19) 0.110(2) Uani 1 1 d . . . H36A H 0.2782 0.8395 0.5129 0.165 Uiso 1 1 calc R . . H36B H 0.3321 0.7620 0.4837 0.165 Uiso 1 1 calc R . . H36C H 0.3641 0.8906 0.5074 0.165 Uiso 1 1 calc R . . C37 C 0.4580(4) 0.7111(5) 0.5499(3) 0.120(3) Uani 1 1 d . . . H37A H 0.4866 0.7886 0.5457 0.180 Uiso 1 1 calc R . . H37B H 0.4596 0.6556 0.5239 0.180 Uiso 1 1 calc R . . H37C H 0.4831 0.6695 0.5778 0.180 Uiso 1 1 calc R . . C38 C -0.0758(2) 0.3947(4) 0.57428(13) 0.0390(10) Uani 1 1 d . . . C39 C -0.1607(2) 0.4273(4) 0.57735(13) 0.0373(9) Uani 1 1 d . . . C40 C -0.1967(3) 0.5389(4) 0.55984(15) 0.0513(12) Uani 1 1 d . . . H40 H -0.1676 0.5967 0.5448 0.062 Uiso 1 1 calc R . . C41 C -0.2760(3) 0.5657(5) 0.56444(17) 0.0600(13) Uani 1 1 d . . . H41 H -0.2999 0.6417 0.5528 0.072 Uiso 1 1 calc R . . C42 C -0.3192(3) 0.4810(5) 0.58604(17) 0.0608(13) Uani 1 1 d . . . H42 H -0.3724 0.4993 0.5892 0.073 Uiso 1 1 calc R . . C43 C -0.2843(3) 0.3690(5) 0.60312(17) 0.0623(13) Uani 1 1 d . . . H43 H -0.3139 0.3111 0.6177 0.075 Uiso 1 1 calc R . . C44 C -0.2056(3) 0.3417(4) 0.59882(15) 0.0541(12) Uani 1 1 d . . . H44 H -0.1824 0.2651 0.6104 0.065 Uiso 1 1 calc R . . C45 C 0.0626(2) 0.1802(4) 0.46216(13) 0.0332(9) Uani 1 1 d . . . C46 C 0.1033(3) 0.0538(4) 0.46624(15) 0.0575(13) Uani 1 1 d . . . H46A H 0.0784 -0.0009 0.4416 0.086 Uiso 1 1 calc R . . H46B H 0.0983 0.0161 0.4955 0.086 Uiso 1 1 calc R . . H46C H 0.1595 0.0645 0.4642 0.086 Uiso 1 1 calc R . . C47 C 0.0224(2) -0.0242(4) 0.30898(14) 0.0385(10) Uani 1 1 d . . . C48 C 0.0206(3) -0.1668(4) 0.30211(16) 0.0690(15) Uani 1 1 d . . . H48A H -0.0288 -0.1905 0.2824 0.103 Uiso 1 1 calc R . . H48B H 0.0234 -0.2084 0.3316 0.103 Uiso 1 1 calc R . . H48C H 0.0659 -0.1923 0.2880 0.103 Uiso 1 1 calc R . . C49 C 0.1413(3) 0.0089(4) 0.60723(17) 0.0603(13) Uani 1 1 d . . . H49A H 0.1809 0.0310 0.5877 0.072 Uiso 1 1 calc R . . H49B H 0.1235 -0.0780 0.5998 0.072 Uiso 1 1 calc R . . C50 C 0.1795(3) 0.0149(6) 0.65576(19) 0.0904(19) Uani 1 1 d . . . H50A H 0.1903 0.1024 0.6645 0.136 Uiso 1 1 calc R . . H50B H 0.2294 -0.0321 0.6598 0.136 Uiso 1 1 calc R . . H50C H 0.1439 -0.0215 0.6749 0.136 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0306(2) 0.0310(3) 0.0296(2) 0.0043(2) 0.00790(17) -0.0023(2) Zn2 0.0479(3) 0.0283(3) 0.0335(3) 0.0020(2) 0.0114(2) -0.0003(2) N1 0.0244(16) 0.0320(18) 0.0306(17) 0.0024(14) 0.0038(13) 0.0003(14) N2 0.0273(17) 0.0341(19) 0.0386(18) 0.0092(15) 0.0064(14) 0.0059(15) N3 0.046(2) 0.0293(19) 0.044(2) -0.0012(16) 0.0118(16) 0.0030(16) N4 0.0390(19) 0.034(2) 0.050(2) 0.0007(16) 0.0123(16) 0.0041(16) O1 0.0300(14) 0.0388(16) 0.0458(16) 0.0120(13) 0.0091(12) 0.0003(12) O2 0.0346(15) 0.0470(18) 0.0530(17) 0.0211(15) 0.0100(13) 0.0011(13) O3 0.0558(17) 0.0366(16) 0.0294(15) 0.0024(12) 0.0136(13) 0.0024(13) O4 0.075(2) 0.076(2) 0.0300(16) -0.0050(15) 0.0125(15) 0.0124(18) O5 0.0439(15) 0.0383(16) 0.0277(15) -0.0055(12) 0.0105(12) -0.0097(13) O6 0.0646(19) 0.0350(16) 0.0318(16) -0.0011(13) 0.0108(13) -0.0070(14) O7 0.0475(17) 0.0287(16) 0.073(2) 0.0079(15) 0.0145(15) -0.0048(14) O8 0.0570(18) 0.0311(17) 0.0591(19) 0.0050(14) 0.0206(15) 0.0049(14) O9 0.0452(17) 0.0466(18) 0.063(2) 0.0283(15) 0.0157(14) 0.0042(15) C1 0.034(2) 0.033(2) 0.033(2) 0.0061(18) 0.0035(17) -0.0052(18) C2 0.0247(19) 0.037(2) 0.030(2) 0.0025(18) 0.0030(15) -0.0020(17) C3 0.029(2) 0.037(2) 0.031(2) -0.0016(18) 0.0022(16) -0.0057(18) C4 0.026(2) 0.040(2) 0.035(2) 0.0033(19) 0.0040(16) 0.0006(18) C5 0.028(2) 0.054(3) 0.042(2) 0.000(2) 0.0053(18) -0.001(2) C6 0.028(2) 0.051(3) 0.038(2) -0.002(2) 0.0069(17) -0.0116(19) C7 0.035(2) 0.039(2) 0.039(2) 0.0057(19) 0.0047(18) -0.0081(19) C8 0.040(2) 0.050(3) 0.052(3) 0.012(2) 0.010(2) 0.011(2) C9 0.067(3) 0.082(4) 0.054(3) 0.024(3) 0.003(2) 0.016(3) C10 0.067(3) 0.042(3) 0.077(4) 0.010(3) 0.016(3) 0.005(3) C11 0.054(3) 0.076(4) 0.102(4) 0.026(3) 0.021(3) 0.028(3) C12 0.036(2) 0.067(3) 0.057(3) 0.010(2) 0.012(2) -0.019(2) C13 0.082(4) 0.163(7) 0.091(5) -0.011(4) 0.015(3) -0.082(4) C14 0.156(6) 0.135(6) 0.140(6) -0.045(5) 0.118(5) -0.066(5) C15 0.074(4) 0.160(7) 0.214(9) 0.118(7) 0.029(5) -0.031(5) C16 0.032(2) 0.038(2) 0.031(2) 0.0013(19) 0.0068(16) 0.0010(19) C17 0.028(2) 0.041(2) 0.034(2) 0.0045(18) 0.0077(16) 0.0028(18) C18 0.037(2) 0.045(3) 0.056(3) 0.004(2) 0.006(2) 0.004(2) C19 0.046(3) 0.050(3) 0.065(3) 0.005(2) 0.008(2) 0.012(2) C20 0.040(3) 0.071(4) 0.065(3) 0.000(3) 0.006(2) 0.020(3) C21 0.030(3) 0.084(4) 0.089(4) 0.017(3) 0.014(2) 0.003(3) C22 0.036(2) 0.062(3) 0.073(3) 0.025(3) 0.014(2) 0.006(2) C23 0.057(3) 0.024(2) 0.050(3) 0.0009(19) 0.015(2) 0.003(2) C24 0.050(3) 0.026(2) 0.046(3) 0.0012(19) 0.016(2) 0.000(2) C25 0.056(3) 0.025(2) 0.044(2) 0.0003(19) 0.014(2) -0.003(2) C26 0.050(3) 0.028(2) 0.041(2) -0.0014(18) 0.0164(19) -0.0016(19) C27 0.055(3) 0.030(2) 0.058(3) -0.004(2) 0.021(2) -0.005(2) C28 0.062(3) 0.028(2) 0.051(3) -0.004(2) 0.025(2) -0.008(2) C29 0.065(3) 0.024(2) 0.059(3) 0.000(2) 0.020(2) 0.002(2) C30 0.046(2) 0.032(2) 0.055(3) -0.003(2) 0.016(2) -0.002(2) C31 0.069(3) 0.052(3) 0.121(5) -0.001(3) 0.041(3) 0.009(3) C32 0.097(4) 0.038(3) 0.067(3) -0.004(2) 0.018(3) 0.009(3) C33 0.073(3) 0.045(3) 0.059(3) 0.009(2) 0.010(2) 0.008(3) C34 0.071(3) 0.032(2) 0.076(3) -0.001(2) 0.032(3) -0.012(2) C35 0.098(4) 0.048(3) 0.088(4) -0.010(3) 0.014(3) -0.025(3) C36 0.184(7) 0.065(4) 0.073(4) 0.017(3) -0.005(4) -0.062(4) C37 0.106(5) 0.059(4) 0.216(8) -0.002(5) 0.087(5) -0.029(4) C38 0.054(3) 0.032(2) 0.031(2) -0.0003(18) 0.0103(19) -0.001(2) C39 0.043(2) 0.036(2) 0.033(2) -0.0006(19) 0.0073(18) 0.002(2) C40 0.049(3) 0.043(3) 0.060(3) 0.009(2) 0.006(2) -0.002(2) C41 0.056(3) 0.048(3) 0.071(3) 0.008(3) -0.005(2) 0.014(3) C42 0.050(3) 0.066(3) 0.068(3) 0.003(3) 0.011(2) 0.012(3) C43 0.054(3) 0.060(3) 0.077(4) 0.013(3) 0.023(3) 0.001(3) C44 0.055(3) 0.046(3) 0.063(3) 0.010(2) 0.016(2) 0.006(2) C45 0.030(2) 0.038(2) 0.030(2) -0.0053(19) 0.0016(16) -0.0077(18) C46 0.070(3) 0.052(3) 0.044(3) 0.007(2) -0.009(2) 0.009(3) C47 0.035(2) 0.041(3) 0.038(3) -0.007(2) 0.0051(18) -0.0049(19) C48 0.122(5) 0.035(3) 0.048(3) -0.004(2) 0.007(3) -0.007(3) C49 0.052(3) 0.052(3) 0.079(4) 0.026(3) 0.020(3) 0.009(2) C50 0.064(4) 0.114(5) 0.089(4) 0.030(4) -0.002(3) -0.012(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 Zn1 O1 1.956(2) . ? Zn1 O5 1.989(2) . ? Zn1 O3 2.020(2) . ? Zn1 N1 2.051(3) . ? Zn1 O2 2.214(3) . ? Zn2 O7 1.944(3) . ? Zn2 O4 1.980(3) . ? Zn2 O9 2.010(3) . ? Zn2 N3 2.045(3) . ? Zn2 O8 2.150(3) . ? N1 C1 1.288(4) . ? N1 N2 1.391(4) . ? N2 C16 1.351(4) . ? N2 H2 0.8600 . ? N3 C23 1.285(5) . ? N3 N4 1.386(4) . ? N4 C38 1.333(5) . ? N4 H4 0.8600 . ? O1 C3 1.292(4) . ? O2 C16 1.241(4) . ? O3 C45 1.243(4) . ? O4 C45 1.248(4) . ? O5 C47 1.287(4) . ? O6 C47 1.226(4) . ? O7 C25 1.311(4) . ? O8 C38 1.251(4) . ? O9 C49 1.438(5) . ? O9 H9 0.8200 . ? C1 C2 1.425(5) . ? C1 H1 0.9300 . ? C2 C7 1.412(5) . ? C2 C3 1.424(5) . ? C3 C4 1.439(5) . ? C4 C5 1.367(5) . ? C4 C8 1.538(5) . ? C5 C6 1.401(5) . ? C5 H5 0.9300 . ? C6 C7 1.364(5) . ? C6 C12 1.538(5) . ? C7 H7 0.9300 . ? C8 C9 1.535(6) . ? C8 C10 1.538(6) . ? C8 C11 1.539(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C15 1.489(7) . ? C12 C14 1.494(7) . ? C12 C13 1.495(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.476(5) . ? C17 C22 1.377(5) . ? C17 C18 1.382(5) . ? C18 C19 1.372(5) . ? C18 H18 0.9300 . ? C19 C20 1.374(6) . ? C19 H19 0.9300 . ? C20 C21 1.368(7) . ? C20 H20 0.9300 . ? C21 C22 1.391(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.432(5) . ? C23 H23 0.9300 . ? C24 C29 1.403(5) . ? C24 C25 1.438(5) . ? C25 C26 1.423(5) . ? C26 C27 1.376(5) . ? C26 C30 1.539(5) . ? C27 C28 1.389(5) . ? C27 H27 0.9300 . ? C28 C29 1.369(5) . ? C28 C34 1.537(5) . ? C29 H29 0.9300 . ? C30 C31 1.520(6) . ? C30 C33 1.525(6) . ? C30 C32 1.530(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.507(6) . ? C34 C36 1.514(7) . ? C34 C37 1.538(7) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.479(5) . ? C39 C40 1.375(5) . ? C39 C44 1.384(5) . ? C40 C41 1.385(6) . ? C40 H40 0.9300 . ? C41 C42 1.362(6) . ? C41 H41 0.9300 . ? C42 C43 1.367(6) . ? C42 H42 0.9300 . ? C43 C44 1.373(6) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.483(5) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.506(6) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.461(7) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O5 97.79(10) . . ? O1 Zn1 O3 103.38(11) . . ? O5 Zn1 O3 103.40(10) . . ? O1 Zn1 N1 87.67(10) . . ? O5 Zn1 N1 143.84(11) . . ? O3 Zn1 N1 110.05(11) . . ? O1 Zn1 O2 162.22(10) . . ? O5 Zn1 O2 96.51(10) . . ? O3 Zn1 O2 83.44(10) . . ? N1 Zn1 O2 74.55(10) . . ? O7 Zn2 O4 106.20(12) . . ? O7 Zn2 O9 97.39(11) . . ? O4 Zn2 O9 108.50(13) . . ? O7 Zn2 N3 88.77(12) . . ? O4 Zn2 N3 101.34(13) . . ? O9 Zn2 N3 146.32(12) . . ? O7 Zn2 O8 155.49(12) . . ? O4 Zn2 O8 95.40(12) . . ? O9 Zn2 O8 86.31(10) . . ? N3 Zn2 O8 75.50(12) . . ? C1 N1 N2 116.7(3) . . ? C1 N1 Zn1 127.3(2) . . ? N2 N1 Zn1 116.0(2) . . ? C16 N2 N1 115.5(3) . . ? C16 N2 H2 122.3 . . ? N1 N2 H2 122.3 . . ? C23 N3 N4 118.8(3) . . ? C23 N3 Zn2 127.2(3) . . ? N4 N3 Zn2 113.8(2) . . ? C38 N4 N3 116.1(3) . . ? C38 N4 H4 122.0 . . ? N3 N4 H4 122.0 . . ? C3 O1 Zn1 132.6(2) . . ? C16 O2 Zn1 113.4(2) . . ? C45 O3 Zn1 138.3(3) . . ? C45 O4 Zn2 142.8(3) . . ? C47 O5 Zn1 111.1(2) . . ? C25 O7 Zn2 129.8(3) . . ? C38 O8 Zn2 113.5(3) . . ? C49 O9 Zn2 126.1(2) . . ? C49 O9 H9 109.4 . . ? Zn2 O9 H9 123.2 . . ? N1 C1 C2 126.1(3) . . ? N1 C1 H1 117.0 . . ? C2 C1 H1 117.0 . . ? C7 C2 C3 120.3(3) . . ? C7 C2 C1 116.7(3) . . ? C3 C2 C1 123.0(3) . . ? O1 C3 C2 122.8(3) . . ? O1 C3 C4 120.1(3) . . ? C2 C3 C4 117.1(3) . . ? C5 C4 C3 118.3(3) . . ? C5 C4 C8 122.5(3) . . ? C3 C4 C8 119.2(3) . . ? C4 C5 C6 125.4(4) . . ? C4 C5 H5 117.3 . . ? C6 C5 H5 117.3 . . ? C7 C6 C5 116.1(3) . . ? C7 C6 C12 122.9(4) . . ? C5 C6 C12 121.1(4) . . ? C6 C7 C2 122.5(4) . . ? C6 C7 H7 118.7 . . ? C2 C7 H7 118.7 . . ? C9 C8 C4 109.8(4) . . ? C9 C8 C10 109.8(4) . . ? C4 C8 C10 110.7(3) . . ? C9 C8 C11 108.1(4) . . ? C4 C8 C11 111.8(3) . . ? C10 C8 C11 106.5(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C14 108.9(5) . . ? C15 C12 C13 106.9(5) . . ? C14 C12 C13 108.1(5) . . ? C15 C12 C6 112.8(4) . . ? C14 C12 C6 110.4(4) . . ? C13 C12 C6 109.5(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 N2 120.5(3) . . ? O2 C16 C17 122.4(3) . . ? N2 C16 C17 117.0(3) . . ? C22 C17 C18 119.0(4) . . ? C22 C17 C16 117.8(4) . . ? C18 C17 C16 123.1(3) . . ? C19 C18 C17 121.0(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 119.5(4) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.9(4) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 C21 120.0(4) . . ? C17 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? N3 C23 C24 124.4(4) . . ? N3 C23 H23 117.8 . . ? C24 C23 H23 117.8 . . ? C29 C24 C23 116.2(4) . . ? C29 C24 C25 119.8(4) . . ? C23 C24 C25 124.0(4) . . ? O7 C25 C26 120.0(3) . . ? O7 C25 C24 122.9(4) . . ? C26 C25 C24 117.1(4) . . ? C27 C26 C25 119.0(4) . . ? C27 C26 C30 120.0(4) . . ? C25 C26 C30 121.0(3) . . ? C26 C27 C28 124.8(4) . . ? C26 C27 H27 117.6 . . ? C28 C27 H27 117.6 . . ? C29 C28 C27 116.4(4) . . ? C29 C28 C34 120.9(4) . . ? C27 C28 C34 122.7(4) . . ? C28 C29 C24 122.9(4) . . ? C28 C29 H29 118.6 . . ? C24 C29 H29 118.6 . . ? C31 C30 C33 107.2(4) . . ? C31 C30 C32 107.7(4) . . ? C33 C30 C32 109.5(4) . . ? C31 C30 C26 112.9(3) . . ? C33 C30 C26 109.3(3) . . ? C32 C30 C26 110.1(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C36 109.7(4) . . ? C35 C34 C28 109.6(4) . . ? C36 C34 C28 109.7(4) . . ? C35 C34 C37 107.4(5) . . ? C36 C34 C37 108.6(5) . . ? C28 C34 C37 111.7(4) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O8 C38 N4 119.8(4) . . ? O8 C38 C39 121.9(4) . . ? N4 C38 C39 118.2(4) . . ? C40 C39 C44 118.8(4) . . ? C40 C39 C38 122.7(4) . . ? C44 C39 C38 118.5(4) . . ? C39 C40 C41 120.3(4) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 120.2(4) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 120.0(4) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C44 120.3(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 120.4(4) . . ? C43 C44 H44 119.8 . . ? C39 C44 H44 119.8 . . ? O3 C45 O4 119.5(4) . . ? O3 C45 C46 120.1(3) . . ? O4 C45 C46 120.4(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O6 C47 O5 122.9(4) . . ? O6 C47 C48 121.3(4) . . ? O5 C47 C48 115.9(4) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O9 C49 C50 112.4(4) . . ? O9 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? O9 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn1 N1 C1 1.2(3) . . . . ? O5 Zn1 N1 C1 -98.8(3) . . . . ? O3 Zn1 N1 C1 104.6(3) . . . . ? O2 Zn1 N1 C1 -178.5(3) . . . . ? O1 Zn1 N1 N2 178.7(2) . . . . ? O5 Zn1 N1 N2 78.6(3) . . . . ? O3 Zn1 N1 N2 -77.9(2) . . . . ? O2 Zn1 N1 N2 -1.1(2) . . . . ? C1 N1 N2 C16 177.8(3) . . . . ? Zn1 N1 N2 C16 0.0(4) . . . . ? O7 Zn2 N3 C23 15.5(3) . . . . ? O4 Zn2 N3 C23 -90.8(3) . . . . ? O9 Zn2 N3 C23 117.0(3) . . . . ? O8 Zn2 N3 C23 176.5(4) . . . . ? O7 Zn2 N3 N4 -170.8(2) . . . . ? O4 Zn2 N3 N4 83.0(2) . . . . ? O9 Zn2 N3 N4 -69.2(3) . . . . ? O8 Zn2 N3 N4 -9.7(2) . . . . ? C23 N3 N4 C38 -176.3(3) . . . . ? Zn2 N3 N4 C38 9.3(4) . . . . ? O5 Zn1 O1 C3 137.0(3) . . . . ? O3 Zn1 O1 C3 -117.2(3) . . . . ? N1 Zn1 O1 C3 -7.1(3) . . . . ? O2 Zn1 O1 C3 -6.2(6) . . . . ? O1 Zn1 O2 C16 1.2(5) . . . . ? O5 Zn1 O2 C16 -142.1(3) . . . . ? O3 Zn1 O2 C16 115.1(3) . . . . ? N1 Zn1 O2 C16 2.1(3) . . . . ? O1 Zn1 O3 C45 -70.2(4) . . . . ? O5 Zn1 O3 C45 31.3(4) . . . . ? N1 Zn1 O3 C45 -162.6(3) . . . . ? O2 Zn1 O3 C45 126.5(4) . . . . ? O7 Zn2 O4 C45 34.9(5) . . . . ? O9 Zn2 O4 C45 -68.9(5) . . . . ? N3 Zn2 O4 C45 127.0(5) . . . . ? O8 Zn2 O4 C45 -156.8(5) . . . . ? O1 Zn1 O5 C47 -76.7(2) . . . . ? O3 Zn1 O5 C47 177.5(2) . . . . ? N1 Zn1 O5 C47 20.0(3) . . . . ? O2 Zn1 O5 C47 92.7(2) . . . . ? O4 Zn2 O7 C25 82.7(3) . . . . ? O9 Zn2 O7 C25 -165.5(3) . . . . ? N3 Zn2 O7 C25 -18.7(3) . . . . ? O8 Zn2 O7 C25 -68.1(4) . . . . ? O7 Zn2 O8 C38 61.4(4) . . . . ? O4 Zn2 O8 C38 -90.6(3) . . . . ? O9 Zn2 O8 C38 161.2(3) . . . . ? N3 Zn2 O8 C38 9.8(3) . . . . ? O7 Zn2 O9 C49 -20.4(3) . . . . ? O4 Zn2 O9 C49 89.4(3) . . . . ? N3 Zn2 O9 C49 -119.4(4) . . . . ? O8 Zn2 O9 C49 -176.1(3) . . . . ? N2 N1 C1 C2 -176.0(3) . . . . ? Zn1 N1 C1 C2 1.5(5) . . . . ? N1 C1 C2 C7 -179.8(3) . . . . ? N1 C1 C2 C3 -0.3(6) . . . . ? Zn1 O1 C3 C2 10.0(5) . . . . ? Zn1 O1 C3 C4 -170.2(2) . . . . ? C7 C2 C3 O1 174.2(3) . . . . ? C1 C2 C3 O1 -5.4(6) . . . . ? C7 C2 C3 C4 -5.6(5) . . . . ? C1 C2 C3 C4 174.9(3) . . . . ? O1 C3 C4 C5 -174.1(3) . . . . ? C2 C3 C4 C5 5.7(5) . . . . ? O1 C3 C4 C8 7.4(5) . . . . ? C2 C3 C4 C8 -172.8(3) . . . . ? C3 C4 C5 C6 -1.9(6) . . . . ? C8 C4 C5 C6 176.5(4) . . . . ? C4 C5 C6 C7 -2.2(6) . . . . ? C4 C5 C6 C12 177.3(4) . . . . ? C5 C6 C7 C2 2.3(6) . . . . ? C12 C6 C7 C2 -177.1(4) . . . . ? C3 C2 C7 C6 1.6(6) . . . . ? C1 C2 C7 C6 -178.8(3) . . . . ? C5 C4 C8 C9 114.0(4) . . . . ? C3 C4 C8 C9 -67.6(5) . . . . ? C5 C4 C8 C10 -124.7(4) . . . . ? C3 C4 C8 C10 53.7(5) . . . . ? C5 C4 C8 C11 -6.1(6) . . . . ? C3 C4 C8 C11 172.4(4) . . . . ? C7 C6 C12 C15 -7.3(7) . . . . ? C5 C6 C12 C15 173.3(5) . . . . ? C7 C6 C12 C14 -129.4(5) . . . . ? C5 C6 C12 C14 51.2(6) . . . . ? C7 C6 C12 C13 111.7(5) . . . . ? C5 C6 C12 C13 -67.7(6) . . . . ? Zn1 O2 C16 N2 -3.0(4) . . . . ? Zn1 O2 C16 C17 179.5(3) . . . . ? N1 N2 C16 O2 2.1(5) . . . . ? N1 N2 C16 C17 179.7(3) . . . . ? O2 C16 C17 C22 -14.9(6) . . . . ? N2 C16 C17 C22 167.6(4) . . . . ? O2 C16 C17 C18 163.8(4) . . . . ? N2 C16 C17 C18 -13.8(6) . . . . ? C22 C17 C18 C19 -0.4(6) . . . . ? C16 C17 C18 C19 -179.0(4) . . . . ? C17 C18 C19 C20 0.6(7) . . . . ? C18 C19 C20 C21 -0.8(7) . . . . ? C19 C20 C21 C22 0.7(8) . . . . ? C18 C17 C22 C21 0.3(6) . . . . ? C16 C17 C22 C21 178.9(4) . . . . ? C20 C21 C22 C17 -0.4(7) . . . . ? N4 N3 C23 C24 178.4(3) . . . . ? Zn2 N3 C23 C24 -8.1(6) . . . . ? N3 C23 C24 C29 178.3(4) . . . . ? N3 C23 C24 C25 -3.5(6) . . . . ? Zn2 O7 C25 C26 -166.3(3) . . . . ? Zn2 O7 C25 C24 14.3(6) . . . . ? C29 C24 C25 O7 178.9(4) . . . . ? C23 C24 C25 O7 0.8(6) . . . . ? C29 C24 C25 C26 -0.6(6) . . . . ? C23 C24 C25 C26 -178.7(4) . . . . ? O7 C25 C26 C27 -178.8(4) . . . . ? C24 C25 C26 C27 0.7(6) . . . . ? O7 C25 C26 C30 1.2(6) . . . . ? C24 C25 C26 C30 -179.3(4) . . . . ? C25 C26 C27 C28 -0.7(6) . . . . ? C30 C26 C27 C28 179.3(4) . . . . ? C26 C27 C28 C29 0.5(6) . . . . ? C26 C27 C28 C34 179.4(4) . . . . ? C27 C28 C29 C24 -0.4(6) . . . . ? C34 C28 C29 C24 -179.3(4) . . . . ? C23 C24 C29 C28 178.7(4) . . . . ? C25 C24 C29 C28 0.4(6) . . . . ? C27 C26 C30 C31 -3.9(6) . . . . ? C25 C26 C30 C31 176.1(4) . . . . ? C27 C26 C30 C33 115.4(4) . . . . ? C25 C26 C30 C33 -64.6(5) . . . . ? C27 C26 C30 C32 -124.3(4) . . . . ? C25 C26 C30 C32 55.7(5) . . . . ? C29 C28 C34 C35 65.7(6) . . . . ? C27 C28 C34 C35 -113.1(5) . . . . ? C29 C28 C34 C36 -54.8(6) . . . . ? C27 C28 C34 C36 126.3(5) . . . . ? C29 C28 C34 C37 -175.3(5) . . . . ? C27 C28 C34 C37 5.8(7) . . . . ? Zn2 O8 C38 N4 -8.1(4) . . . . ? Zn2 O8 C38 C39 173.0(3) . . . . ? N3 N4 C38 O8 -0.5(5) . . . . ? N3 N4 C38 C39 178.4(3) . . . . ? O8 C38 C39 C40 -159.0(4) . . . . ? N4 C38 C39 C40 22.1(6) . . . . ? O8 C38 C39 C44 21.1(6) . . . . ? N4 C38 C39 C44 -157.8(4) . . . . ? C44 C39 C40 C41 1.1(6) . . . . ? C38 C39 C40 C41 -178.8(4) . . . . ? C39 C40 C41 C42 -0.5(7) . . . . ? C40 C41 C42 C43 -0.2(7) . . . . ? C41 C42 C43 C44 0.3(8) . . . . ? C42 C43 C44 C39 0.3(7) . . . . ? C40 C39 C44 C43 -1.0(6) . . . . ? C38 C39 C44 C43 178.9(4) . . . . ? Zn1 O3 C45 O4 -166.5(3) . . . . ? Zn1 O3 C45 C46 12.5(6) . . . . ? Zn2 O4 C45 O3 -137.9(4) . . . . ? Zn2 O4 C45 C46 43.1(7) . . . . ? Zn1 O5 C47 O6 -13.2(5) . . . . ? Zn1 O5 C47 C48 165.6(3) . . . . ? Zn2 O9 C49 C50 104.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.471 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.069 data_1 _database_code_depnum_ccdc_archive 'CCDC 727397' #TrackingRef '- crystal data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H76 N4 O10 Zn2' _chemical_formula_weight 1047.9 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 7.7586(6) _cell_length_b 11.1224(15) _cell_length_c 17.327(2) _cell_angle_alpha 96.667(2) _cell_angle_beta 102.141(3) _cell_angle_gamma 95.722(2) _cell_volume 1440.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1623 _cell_measurement_theta_min 2.429 _cell_measurement_theta_max 25.161 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6910 _exptl_absorpt_correction_T_max 0.9088 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7433 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.1286 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6034 _reflns_number_gt 3569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.1070P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 6034 _refine_ls_number_parameters 629 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2072 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.96552(14) 0.71617(10) 0.26434(8) 0.0420(5) Uani 1 1 d . . . Zn2 Zn 1.09558(14) 0.27201(10) 0.51769(8) 0.0445(5) Uani 1 1 d . . . N1 N 1.0088(13) 0.4330(9) 0.3991(6) 0.041(2) Uani 1 1 d . . . H1 H 0.9940 0.4999 0.3796 0.049 Uiso 1 1 calc R . . N2 N 1.0000(15) 0.4258(11) 0.4775(7) 0.043(3) Uani 1 1 d . . . N3 N 0.9971(14) 0.9337(9) 0.3806(7) 0.046(3) Uani 1 1 d . . . H3 H 1.0035 1.0097 0.3988 0.056 Uiso 1 1 calc R . . N4 N 0.9113(13) 0.8869(10) 0.3034(7) 0.042(3) Uani 1 1 d . . . O1 O 1.0638(15) 0.2390(10) 0.3846(7) 0.062(3) Uani 1 1 d . . . O2 O 0.9700(13) 0.5473(8) 0.2782(6) 0.051(3) Uani 1 1 d . . . O3 O 0.9934(14) 0.3145(8) 0.6097(5) 0.060(3) Uani 1 1 d . . . O4 O 1.0605(14) 0.7465(9) 0.3946(6) 0.054(3) Uani 1 1 d . . . O5 O 1.0736(13) 1.0946(8) 0.5039(6) 0.054(3) Uani 1 1 d . . . O6 O 0.7559(12) 0.7136(8) 0.1775(5) 0.051(2) Uani 1 1 d . . . O7 O 1.1891(15) 0.7607(10) 0.2256(7) 0.082(3) Uani 1 1 d . A . H7 H 1.2799 0.7416 0.2524 0.123 Uiso 1 1 d R . . O8 O 1.3600(16) 0.3274(11) 0.5537(8) 0.093(4) Uani 1 1 d . B . H8 H 1.4208 0.2977 0.5249 0.140 Uiso 1 1 d R . . O9 O 0.4933(17) 0.6741(13) 0.2697(8) 0.102(4) Uani 1 1 d . C . H9 H 0.5633 0.6694 0.2403 0.152 Uiso 1 1 calc R . . O10 O 0.627(2) 0.2200(18) 0.5219(11) 0.146(6) Uani 1 1 d . D . H10 H 0.7243 0.2327 0.5532 0.220 Uiso 1 1 calc R . . C1 C 1.0399(18) 0.3376(11) 0.3550(9) 0.050(4) Uani 1 1 d . . . C2 C 1.0351(19) 0.3335(13) 0.2711(7) 0.059(4) Uani 1 1 d . . . C3 C 1.0198(19) 0.4537(12) 0.2359(9) 0.043(4) Uani 1 1 d . . . C4 C 1.042(2) 0.4526(15) 0.1579(9) 0.057(5) Uani 1 1 d . . . H4 H 1.0221 0.5206 0.1323 0.068 Uiso 1 1 calc R . . C5 C 1.091(3) 0.3544(18) 0.1193(12) 0.075(6) Uani 1 1 d . . . H5 H 1.1108 0.3593 0.0686 0.090 Uiso 1 1 calc R . . C6 C 1.113(3) 0.2488(15) 0.1496(11) 0.089(6) Uani 1 1 d . . . H6 H 1.1411 0.1814 0.1198 0.107 Uiso 1 1 calc R . . C7 C 1.094(2) 0.2453(13) 0.2269(9) 0.070(5) Uani 1 1 d . . . H7A H 1.1232 0.1767 0.2501 0.083 Uiso 1 1 calc R . . C8 C 0.9634(18) 0.5162(14) 0.5183(9) 0.045(4) Uani 1 1 d . . . H8A H 0.9414 0.5844 0.4932 0.054 Uiso 1 1 calc R . . C9 C 0.9524(19) 0.5240(13) 0.5999(8) 0.040(4) Uani 1 1 d . . . C10 C 0.9726(17) 0.4207(11) 0.6438(8) 0.045(3) Uani 1 1 d . . . C11 C 0.954(2) 0.4420(12) 0.7261(8) 0.056(4) Uani 1 1 d . . . C12 C 0.9350(19) 0.5559(12) 0.7582(8) 0.056(4) Uani 1 1 d . . . H12 H 0.9353 0.5686 0.8122 0.067 Uiso 1 1 calc R . . C13 C 0.9142(19) 0.6598(12) 0.7143(8) 0.052(3) Uani 1 1 d . . . C14 C 0.928(2) 0.6381(14) 0.6378(10) 0.051(4) Uani 1 1 d . . . H14 H 0.9212 0.7027 0.6081 0.061 Uiso 1 1 calc R . . C15 C 0.964(3) 0.3356(19) 0.7758(11) 0.095(6) Uani 1 1 d . . . C16 C 0.828(3) 0.231(2) 0.7374(14) 0.128(8) Uani 1 1 d . . . H16A H 0.7136 0.2592 0.7259 0.192 Uiso 1 1 calc R . . H16B H 0.8274 0.1710 0.7726 0.192 Uiso 1 1 calc R . . H16C H 0.8552 0.1964 0.6887 0.192 Uiso 1 1 calc R . . C17 C 1.148(3) 0.2952(19) 0.7844(11) 0.108(7) Uani 1 1 d . . . H17A H 1.1949 0.2863 0.8390 0.162 Uiso 1 1 calc R . . H17B H 1.2259 0.3554 0.7683 0.162 Uiso 1 1 calc R . . H17C H 1.1404 0.2185 0.7513 0.162 Uiso 1 1 calc R . . C18 C 0.950(3) 0.3790(19) 0.8624(11) 0.112(7) Uani 1 1 d . . . H18A H 0.8648 0.4363 0.8615 0.167 Uiso 1 1 calc R . . H18B H 1.0636 0.4176 0.8931 0.167 Uiso 1 1 calc R . . H18C H 0.9117 0.3101 0.8860 0.167 Uiso 1 1 calc R . . C19 C 0.891(2) 0.7811(15) 0.7573(10) 0.072(4) Uani 1 1 d . . . C20 C 0.736(3) 0.7690(17) 0.7979(11) 0.095(6) Uani 1 1 d . . . H20A H 0.6483 0.7032 0.7687 0.143 Uiso 1 1 calc R . . H20B H 0.6833 0.8436 0.7992 0.143 Uiso 1 1 calc R . . H20C H 0.7771 0.7525 0.8513 0.143 Uiso 1 1 calc R . . C21 C 1.063(3) 0.8299(17) 0.8146(11) 0.098(6) Uani 1 1 d . . . H21A H 1.0725 0.7907 0.8616 0.147 Uiso 1 1 calc R . . H21B H 1.0672 0.9163 0.8290 0.147 Uiso 1 1 calc R . . H21C H 1.1599 0.8140 0.7901 0.147 Uiso 1 1 calc R . . C22 C 0.853(2) 0.8761(15) 0.6981(10) 0.084(5) Uani 1 1 d . . . H22A H 0.9524 0.8892 0.6736 0.126 Uiso 1 1 calc R . . H22B H 0.8368 0.9519 0.7266 0.126 Uiso 1 1 calc R . . H22C H 0.7480 0.8457 0.6577 0.126 Uiso 1 1 calc R . . C23 C 1.070(2) 0.8535(16) 0.4257(10) 0.069(4) Uani 1 1 d . . . C24 C 1.146(2) 0.8870(13) 0.5094(9) 0.060(4) Uani 1 1 d . . . C25 C 1.165(2) 1.0193(15) 0.5450(10) 0.061(4) Uani 1 1 d . . . C26 C 1.254(2) 1.0526(16) 0.6226(10) 0.067(5) Uani 1 1 d . . . H26 H 1.2582 1.1322 0.6468 0.080 Uiso 1 1 calc R . . C27 C 1.337(2) 0.9717(18) 0.6648(11) 0.071(5) Uani 1 1 d . . . H27 H 1.3993 0.9979 0.7171 0.085 Uiso 1 1 calc R . . C28 C 1.333(2) 0.8528(16) 0.6330(10) 0.074(5) Uani 1 1 d . . . H28 H 1.3853 0.7979 0.6644 0.089 Uiso 1 1 calc R . . C29 C 1.253(2) 0.8158(15) 0.5556(10) 0.072(5) Uani 1 1 d . . . H29 H 1.2693 0.7397 0.5320 0.086 Uiso 1 1 calc R . . C30 C 0.8287(18) 0.9641(13) 0.2599(8) 0.041(3) Uani 1 1 d . . . H30 H 0.8286 1.0438 0.2832 0.049 Uiso 1 1 calc R . . C31 C 0.7410(16) 0.9280(13) 0.1788(8) 0.036(3) Uani 1 1 d . . . C32 C 0.7026(17) 0.8065(11) 0.1390(8) 0.045(3) Uani 1 1 d . . . C33 C 0.6023(17) 0.7829(11) 0.0591(7) 0.042(3) Uani 1 1 d . . . C34 C 0.5547(18) 0.8823(14) 0.0233(9) 0.058(4) Uani 1 1 d . . . H34 H 0.4914 0.8674 -0.0294 0.069 Uiso 1 1 calc R . . C35 C 0.593(2) 1.0045(13) 0.0596(9) 0.050(3) Uani 1 1 d . . . C36 C 0.6796(19) 1.0266(14) 0.1366(10) 0.050(4) Uani 1 1 d . . . H36 H 0.7002 1.1060 0.1632 0.060 Uiso 1 1 calc R . . C37 C 0.551(2) 0.6532(16) 0.0129(10) 0.078(5) Uani 1 1 d . . . C38 C 0.447(3) 0.5702(17) 0.0589(11) 0.099(6) Uani 1 1 d . . . H38A H 0.3598 0.6136 0.0779 0.148 Uiso 1 1 calc R . . H38B H 0.5285 0.5482 0.1033 0.148 Uiso 1 1 calc R . . H38C H 0.3890 0.4977 0.0238 0.148 Uiso 1 1 calc R . . C39 C 0.713(3) 0.5967(18) 0.0030(11) 0.097(6) Uani 1 1 d . . . H39A H 0.6781 0.5145 -0.0236 0.145 Uiso 1 1 calc R . . H39B H 0.7882 0.5961 0.0545 0.145 Uiso 1 1 calc R . . H39C H 0.7754 0.6431 -0.0281 0.145 Uiso 1 1 calc R . . C40 C 0.431(3) 0.6463(16) -0.0686(10) 0.096(6) Uani 1 1 d . . . H40A H 0.3227 0.6785 -0.0634 0.145 Uiso 1 1 calc R . . H40B H 0.4032 0.5627 -0.0933 0.145 Uiso 1 1 calc R . . H40C H 0.4894 0.6932 -0.1009 0.145 Uiso 1 1 calc R . . C41 C 0.543(3) 1.1071(15) 0.0108(10) 0.078(5) Uani 1 1 d . . . C42 C 0.650(3) 1.1145(18) -0.0487(12) 0.113(8) Uani 1 1 d . . . H42A H 0.6359 1.1883 -0.0717 0.170 Uiso 1 1 calc R . . H42B H 0.6123 1.0455 -0.0897 0.170 Uiso 1 1 calc R . . H42C H 0.7731 1.1145 -0.0238 0.170 Uiso 1 1 calc R . . C43 C 0.342(3) 1.0847(18) -0.0252(12) 0.115(8) Uani 1 1 d . . . H43A H 0.2967 1.1616 -0.0298 0.172 Uiso 1 1 calc R . . H43B H 0.2830 1.0412 0.0087 0.172 Uiso 1 1 calc R . . H43C H 0.3193 1.0374 -0.0771 0.172 Uiso 1 1 calc R . . C44 C 0.582(3) 1.2341(16) 0.0630(11) 0.106(7) Uani 1 1 d . . . H44A H 0.6981 1.2428 0.0973 0.159 Uiso 1 1 calc R . . H44B H 0.4947 1.2414 0.0948 0.159 Uiso 1 1 calc R . . H44C H 0.5762 1.2969 0.0292 0.159 Uiso 1 1 calc R . . C45 C 1.231(3) 0.8632(18) 0.1859(12) 0.091(6) Uani 1 1 d . . . H45A H 1.3576 0.8724 0.1878 0.109 Uiso 0.62(3) 1 calc PR A 1 H45B H 1.2059 0.9364 0.2155 0.109 Uiso 0.62(3) 1 calc PR A 1 H45C H 1.1214 0.8879 0.1577 0.109 Uiso 0.38(3) 1 d PR A 2 H45D H 1.2979 0.8388 0.1466 0.109 Uiso 0.38(3) 1 d PR A 2 C47 C 1.442(3) 0.4481(18) 0.5937(12) 0.094(6) Uani 1 1 d . . . H47C H 1.5502 0.4396 0.6312 0.113 Uiso 0.49(2) 1 calc PR B 1 H47D H 1.3619 0.4820 0.6241 0.113 Uiso 0.49(2) 1 calc PR B 1 H47A H 1.3789 0.5065 0.5651 0.113 Uiso 0.51(2) 1 d PR B 2 H47B H 1.5642 0.4606 0.5888 0.113 Uiso 0.51(2) 1 d PR B 2 C49 C 0.535(3) 0.597(2) 0.3295(14) 0.112(7) Uani 1 1 d . . . H49A H 0.6600 0.5881 0.3377 0.134 Uiso 0.47(3) 1 calc PR C 1 H49B H 0.4687 0.5167 0.3094 0.134 Uiso 0.47(3) 1 calc PR C 1 H49C H 0.4614 0.6130 0.3676 0.134 Uiso 0.53(3) 1 d PR C 2 H49D H 0.6569 0.6248 0.3571 0.134 Uiso 0.53(3) 1 d PR C 2 C51 C 0.602(4) 0.098(3) 0.480(2) 0.165(11) Uani 1 1 d . . . H51A H 0.5351 0.0458 0.5078 0.198 Uiso 0.62(3) 1 calc PR D 1 H51B H 0.7172 0.0706 0.4837 0.198 Uiso 0.62(3) 1 calc PR D 1 H51C H 0.7019 0.1028 0.4551 0.198 Uiso 0.38(3) 1 d PR D 2 H51D H 0.4948 0.0922 0.4386 0.198 Uiso 0.38(3) 1 d PR D 2 C46 C 1.132(4) 0.854(3) 0.099(2) 0.097(9) Uani 0.62(3) 1 d P A 1 H46A H 1.2000 0.8175 0.0651 0.146 Uiso 0.62(3) 1 calc PR A 1 H46B H 1.1137 0.9348 0.0869 0.146 Uiso 0.62(3) 1 calc PR A 1 H46C H 1.0186 0.8056 0.0915 0.146 Uiso 0.62(3) 1 calc PR A 1 C48 C 1.486(6) 0.538(4) 0.539(2) 0.100(9) Uani 0.49(2) 1 d P B 1 H48A H 1.5229 0.4959 0.4951 0.150 Uiso 0.49(2) 1 calc PR B 1 H48B H 1.5805 0.5995 0.5684 0.150 Uiso 0.49(2) 1 calc PR B 1 H48C H 1.3829 0.5762 0.5196 0.150 Uiso 0.49(2) 1 calc PR B 1 C50 C 0.495(6) 0.639(5) 0.410(3) 0.123(11) Uani 0.47(3) 1 d P C 1 H50A H 0.5872 0.6204 0.4521 0.184 Uiso 0.47(3) 1 calc PR C 1 H50B H 0.3829 0.5979 0.4136 0.184 Uiso 0.47(3) 1 calc PR C 1 H50C H 0.4912 0.7256 0.4162 0.184 Uiso 0.47(3) 1 calc PR C 1 C52 C 0.505(6) 0.082(4) 0.393(3) 0.156(15) Uani 0.62(3) 1 d P D 1 H52A H 0.3794 0.0651 0.3882 0.235 Uiso 0.62(3) 1 calc PR D 1 H52B H 0.5455 0.0159 0.3637 0.235 Uiso 0.62(3) 1 calc PR D 1 H52C H 0.5297 0.1559 0.3708 0.235 Uiso 0.62(3) 1 calc PR D 1 C46' C 1.329(7) 0.977(5) 0.241(3) 0.097(9) Uani 0.38(3) 1 d P A 2 H46D H 1.2480 1.0151 0.2685 0.146 Uiso 0.38(3) 1 calc PR A 2 H46E H 1.3764 1.0337 0.2109 0.146 Uiso 0.38(3) 1 calc PR A 2 H46F H 1.4245 0.9552 0.2800 0.146 Uiso 0.38(3) 1 calc PR A 2 C48' C 1.434(5) 0.475(4) 0.681(2) 0.100(9) Uani 0.51(2) 1 d P B 2 H48D H 1.3170 0.4472 0.6867 0.150 Uiso 0.51(2) 1 calc PR B 2 H48E H 1.4611 0.5610 0.6980 0.150 Uiso 0.51(2) 1 calc PR B 2 H48F H 1.5193 0.4329 0.7122 0.150 Uiso 0.51(2) 1 calc PR B 2 C50' C 0.543(6) 0.463(4) 0.300(3) 0.123(11) Uani 0.53(3) 1 d P C 2 H50D H 0.4341 0.4296 0.2629 0.184 Uiso 0.53(3) 1 calc PR C 2 H50E H 0.5616 0.4181 0.3441 0.184 Uiso 0.53(3) 1 calc PR C 2 H50F H 0.6404 0.4581 0.2735 0.184 Uiso 0.53(3) 1 calc PR C 2 C52' C 0.674(11) 0.001(8) 0.528(5) 0.156(15) Uani 0.38(3) 1 d P D 2 H52D H 0.6778 -0.0708 0.4928 0.235 Uiso 0.38(3) 1 calc PR D 2 H52E H 0.5985 -0.0178 0.5638 0.235 Uiso 0.38(3) 1 calc PR D 2 H52F H 0.7919 0.0314 0.5590 0.235 Uiso 0.38(3) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0461(11) 0.0306(10) 0.0531(12) 0.0113(8) 0.0138(9) 0.0111(9) Zn2 0.0537(12) 0.0291(10) 0.0525(12) 0.0093(8) 0.0116(9) 0.0098(9) N1 0.056(7) 0.032(6) 0.041(6) 0.010(5) 0.019(5) 0.010(5) N2 0.055(8) 0.034(7) 0.041(7) -0.002(5) 0.018(6) 0.002(6) N3 0.047(7) 0.039(6) 0.053(7) 0.005(6) 0.005(6) 0.015(6) N4 0.035(6) 0.036(6) 0.057(8) 0.013(6) 0.010(6) 0.011(5) O1 0.089(9) 0.043(7) 0.063(7) 0.021(5) 0.029(6) 0.013(6) O2 0.075(8) 0.029(5) 0.052(7) 0.002(4) 0.020(6) 0.012(5) O3 0.109(8) 0.027(5) 0.055(6) 0.015(4) 0.027(6) 0.023(5) O4 0.066(7) 0.034(6) 0.058(7) -0.001(5) 0.005(5) 0.014(5) O5 0.079(8) 0.024(5) 0.055(6) 0.018(4) -0.002(5) 0.012(5) O6 0.067(6) 0.035(5) 0.051(6) 0.012(4) 0.000(5) 0.025(5) O7 0.079(8) 0.070(8) 0.114(10) 0.035(7) 0.044(7) 0.011(7) O8 0.092(9) 0.073(9) 0.114(10) 0.010(8) 0.020(8) 0.013(7) O9 0.090(10) 0.110(12) 0.114(10) 0.045(9) 0.031(8) 0.009(8) O10 0.133(15) 0.146(18) 0.145(15) -0.019(13) 0.023(11) 0.011(13) C1 0.060(9) 0.024(7) 0.073(10) 0.013(7) 0.029(8) 0.010(7) C2 0.094(11) 0.082(10) 0.028(7) 0.028(7) 0.030(7) 0.083(9) C3 0.045(9) 0.025(7) 0.053(10) 0.003(6) 0.002(7) -0.004(7) C4 0.091(13) 0.043(9) 0.032(9) 0.011(7) 0.007(8) -0.003(9) C5 0.127(18) 0.051(12) 0.067(13) 0.020(10) 0.054(12) 0.018(11) C6 0.136(16) 0.053(11) 0.110(15) 0.011(10) 0.093(13) 0.031(11) C7 0.127(14) 0.042(9) 0.062(10) 0.025(7) 0.059(10) 0.018(9) C8 0.038(9) 0.037(9) 0.057(10) 0.002(7) 0.007(7) 0.009(7) C9 0.049(9) 0.039(8) 0.030(8) 0.004(6) 0.006(7) 0.005(7) C10 0.048(8) 0.024(7) 0.058(9) 0.003(6) 0.008(7) -0.002(6) C11 0.097(12) 0.034(8) 0.043(8) 0.003(6) 0.027(8) 0.015(8) C12 0.072(10) 0.046(9) 0.052(9) 0.004(7) 0.021(7) 0.012(8) C13 0.069(10) 0.035(8) 0.047(9) -0.005(6) 0.014(8) 0.002(7) C14 0.053(9) 0.031(9) 0.069(12) 0.007(8) 0.015(8) 0.010(7) C15 0.140(19) 0.087(15) 0.069(13) 0.025(11) 0.038(13) 0.026(15) C16 0.16(2) 0.111(19) 0.109(18) 0.026(15) 0.031(16) 0.006(18) C17 0.14(2) 0.092(16) 0.092(15) 0.018(11) 0.013(13) 0.045(14) C18 0.17(2) 0.100(16) 0.075(13) 0.033(11) 0.035(13) 0.017(15) C19 0.083(12) 0.059(11) 0.070(11) -0.002(8) 0.013(9) 0.022(9) C20 0.120(17) 0.069(13) 0.095(14) 0.000(10) 0.020(12) 0.032(12) C21 0.109(16) 0.070(13) 0.097(14) -0.016(10) -0.009(12) 0.025(12) C22 0.099(14) 0.059(11) 0.088(13) -0.001(9) 0.012(10) 0.023(10) C23 0.075(11) 0.062(11) 0.073(12) 0.015(9) 0.016(9) 0.023(10) C24 0.069(10) 0.056(10) 0.057(10) 0.003(7) 0.007(8) 0.043(8) C25 0.073(11) 0.050(10) 0.061(12) 0.012(8) 0.011(9) 0.026(9) C26 0.080(12) 0.055(11) 0.065(12) 0.011(8) 0.007(10) 0.025(10) C27 0.082(13) 0.060(12) 0.069(12) 0.007(9) 0.005(10) 0.025(10) C28 0.084(12) 0.062(12) 0.074(12) 0.010(9) 0.005(10) 0.025(10) C29 0.081(12) 0.060(10) 0.072(12) 0.011(9) 0.004(9) 0.026(9) C30 0.048(8) 0.031(7) 0.046(9) 0.002(6) 0.015(7) 0.006(6) C31 0.027(7) 0.044(8) 0.045(9) 0.013(6) 0.015(6) 0.022(6) C32 0.057(8) 0.021(6) 0.067(9) 0.011(6) 0.030(7) 0.010(6) C33 0.056(8) 0.039(8) 0.031(7) 0.001(5) 0.006(6) 0.015(6) C34 0.052(9) 0.066(10) 0.055(9) 0.023(8) 0.003(7) 0.008(8) C35 0.061(9) 0.039(8) 0.050(9) 0.011(7) 0.008(7) 0.007(7) C36 0.044(9) 0.029(8) 0.084(13) 0.022(8) 0.020(8) 0.009(7) C37 0.090(13) 0.072(12) 0.075(12) 0.011(9) 0.017(10) 0.021(11) C38 0.117(16) 0.078(14) 0.099(15) 0.016(11) 0.019(12) 0.006(12) C39 0.110(15) 0.084(14) 0.089(14) -0.013(10) 0.009(11) 0.040(12) C40 0.119(16) 0.077(13) 0.079(13) -0.001(10) -0.005(12) 0.020(12) C41 0.114(15) 0.054(11) 0.070(12) 0.032(9) 0.009(11) 0.029(10) C42 0.16(2) 0.085(15) 0.096(15) 0.053(13) 0.020(15) 0.014(14) C43 0.15(2) 0.079(14) 0.099(15) 0.031(11) -0.028(14) 0.024(14) C44 0.15(2) 0.054(11) 0.106(16) 0.030(11) -0.003(13) 0.023(12) C45 0.086(13) 0.087(15) 0.106(16) 0.010(12) 0.035(12) 0.016(11) C47 0.093(14) 0.083(15) 0.100(16) 0.005(12) 0.007(12) 0.020(12) C49 0.109(18) 0.110(19) 0.112(19) 0.015(15) 0.017(14) 0.010(15) C51 0.16(3) 0.16(3) 0.16(3) -0.02(2) 0.02(2) 0.00(2) C46 0.10(2) 0.09(2) 0.11(2) 0.013(16) 0.032(17) 0.013(16) C48 0.10(2) 0.09(2) 0.10(2) 0.007(17) 0.008(17) 0.022(17) C50 0.12(3) 0.12(3) 0.12(3) 0.01(2) 0.02(2) 0.01(2) C52 0.15(3) 0.15(4) 0.15(4) -0.01(3) 0.02(3) 0.00(3) C46' 0.10(2) 0.09(2) 0.11(2) 0.013(16) 0.032(17) 0.013(16) C48' 0.10(2) 0.09(2) 0.10(2) 0.007(17) 0.008(17) 0.022(17) C50' 0.12(3) 0.12(3) 0.12(3) 0.01(2) 0.02(2) 0.01(2) C52' 0.15(3) 0.15(4) 0.15(4) -0.01(3) 0.02(3) 0.00(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 Zn1 O2 1.924(9) . ? Zn1 O6 1.965(8) . ? Zn1 O7 2.025(10) . ? Zn1 N4 2.054(11) . ? Zn1 O4 2.197(10) . ? Zn2 O5 1.945(9) 1_545 ? Zn2 O3 1.955(9) . ? Zn2 O8 2.025(13) . ? Zn2 N2 2.067(12) . ? Zn2 O1 2.249(11) . ? N1 C1 1.308(16) . ? N1 N2 1.386(14) . ? N1 H1 0.8600 . ? N2 C8 1.252(18) . ? N3 C23 1.344(17) . ? N3 N4 1.378(15) . ? N3 H3 0.8600 . ? N4 C30 1.332(16) . ? O1 C1 1.278(15) . ? O2 C3 1.338(17) . ? O3 C10 1.299(15) . ? O4 C23 1.236(19) . ? O5 C25 1.327(17) . ? O5 Zn2 1.945(9) 1_565 ? O6 C32 1.347(13) . ? O7 C45 1.442(19) . ? O7 H7 0.8200 . ? O8 C47 1.45(2) . ? O8 H8 0.8200 . ? O9 C49 1.43(2) . ? O9 H9 0.8200 . ? O10 C51 1.43(3) . ? O10 H10 0.8200 . ? C1 C2 1.441(17) . ? C2 C7 1.348(18) . ? C2 C3 1.538(18) . ? C3 C4 1.40(2) . ? C4 C5 1.34(2) . ? C4 H4 0.9300 . ? C5 C6 1.35(2) . ? C5 H5 0.9300 . ? C6 C7 1.38(2) . ? C6 H6 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.43(2) . ? C8 H8A 0.9300 . ? C9 C14 1.41(2) . ? C9 C10 1.453(18) . ? C10 C11 1.459(17) . ? C11 C12 1.357(18) . ? C11 C15 1.54(2) . ? C12 C13 1.459(18) . ? C12 H12 0.9300 . ? C13 C14 1.349(19) . ? C13 C19 1.51(2) . ? C14 H14 0.9300 . ? C15 C16 1.48(3) . ? C15 C17 1.52(3) . ? C15 C18 1.55(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C21 1.50(2) . ? C19 C20 1.52(2) . ? C19 C22 1.56(2) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.43(2) . ? C24 C29 1.399(19) . ? C24 C25 1.51(2) . ? C25 C26 1.37(2) . ? C26 C27 1.35(2) . ? C26 H26 0.9300 . ? C27 C28 1.37(2) . ? C27 H27 0.9300 . ? C28 C29 1.35(2) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.418(19) . ? C30 H30 0.9300 . ? C31 C32 1.416(19) . ? C31 C36 1.452(18) . ? C32 C33 1.418(18) . ? C33 C34 1.374(17) . ? C33 C37 1.54(2) . ? C34 C35 1.40(2) . ? C34 H34 0.9300 . ? C35 C36 1.34(2) . ? C35 C41 1.530(18) . ? C36 H36 0.9300 . ? C37 C39 1.49(2) . ? C37 C40 1.51(2) . ? C37 C38 1.56(2) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.46(3) . ? C41 C43 1.54(3) . ? C41 C44 1.55(2) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.52(3) . ? C45 C46' 1.53(6) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C45 H45D 0.9700 . ? C47 C48' 1.52(4) . ? C47 C48 1.52(4) . ? C47 H47C 0.9700 . ? C47 H47D 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C49 C50 1.53(5) . ? C49 C50' 1.53(5) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C49 H49D 0.9700 . ? C51 C52' 1.52(8) . ? C51 C52 1.53(4) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C51 H51D 0.9700 . ? C46 H45C 1.0579 . ? C46 H45D 1.4130 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C48 H47A 1.0733 . ? C48 H47B 1.3816 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C50 H49C 0.7445 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C52 H51D 0.8130 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C46' H46D 0.9600 . ? C46' H46E 0.9600 . ? C46' H46F 0.9600 . ? C48' H48D 0.9600 . ? C48' H48E 0.9600 . ? C48' H48F 0.9600 . ? C50' H50D 0.9600 . ? C50' H50E 0.9600 . ? C50' H50F 0.9600 . ? C52' H52D 0.9600 . ? C52' H52E 0.9600 . ? C52' H52F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O6 103.8(4) . . ? O2 Zn1 O7 104.1(4) . . ? O6 Zn1 O7 109.6(4) . . ? O2 Zn1 N4 149.2(4) . . ? O6 Zn1 N4 85.0(4) . . ? O7 Zn1 N4 100.3(4) . . ? O2 Zn1 O4 83.2(4) . . ? O6 Zn1 O4 143.6(4) . . ? O7 Zn1 O4 102.8(5) . . ? N4 Zn1 O4 73.2(4) . . ? O5 Zn2 O3 104.2(4) 1_545 . ? O5 Zn2 O8 104.9(4) 1_545 . ? O3 Zn2 O8 106.5(5) . . ? O5 Zn2 N2 147.0(4) 1_545 . ? O3 Zn2 N2 85.6(4) . . ? O8 Zn2 N2 102.2(5) . . ? O5 Zn2 O1 81.7(4) 1_545 . ? O3 Zn2 O1 149.2(4) . . ? O8 Zn2 O1 100.9(5) . . ? N2 Zn2 O1 74.9(4) . . ? C1 N1 N2 119.6(10) . . ? C1 N1 H1 120.2 . . ? N2 N1 H1 120.2 . . ? C8 N2 N1 119.1(13) . . ? C8 N2 Zn2 127.4(11) . . ? N1 N2 Zn2 112.6(8) . . ? C23 N3 N4 115.9(12) . . ? C23 N3 H3 122.0 . . ? N4 N3 H3 122.0 . . ? C30 N4 N3 116.3(12) . . ? C30 N4 Zn1 127.7(10) . . ? N3 N4 Zn1 115.0(7) . . ? C1 O1 Zn2 110.4(10) . . ? C3 O2 Zn1 132.0(9) . . ? C10 O3 Zn2 129.9(8) . . ? C23 O4 Zn1 114.6(10) . . ? C25 O5 Zn2 130.9(10) . 1_565 ? C32 O6 Zn1 128.1(8) . . ? C45 O7 Zn1 128.1(10) . . ? C45 O7 H7 110.6 . . ? Zn1 O7 H7 114.6 . . ? C47 O8 Zn2 125.7(12) . . ? C47 O8 H8 111.2 . . ? Zn2 O8 H8 115.1 . . ? C49 O9 H9 109.5 . . ? C51 O10 H10 109.5 . . ? O1 C1 N1 119.9(13) . . ? O1 C1 C2 116.8(12) . . ? N1 C1 C2 123.2(11) . . ? C7 C2 C1 124.6(11) . . ? C7 C2 C3 115.2(11) . . ? C1 C2 C3 117.3(12) . . ? O2 C3 C4 124.5(13) . . ? O2 C3 C2 118.5(13) . . ? C4 C3 C2 116.6(13) . . ? C5 C4 C3 120.8(16) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 124.1(17) . . ? C4 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C5 C6 C7 117.3(16) . . ? C5 C6 H6 121.4 . . ? C7 C6 H6 121.4 . . ? C2 C7 C6 125.2(13) . . ? C2 C7 H7A 117.4 . . ? C6 C7 H7A 117.4 . . ? N2 C8 C9 125.8(15) . . ? N2 C8 H8A 117.1 . . ? C9 C8 H8A 117.1 . . ? C14 C9 C8 117.2(14) . . ? C14 C9 C10 120.7(14) . . ? C8 C9 C10 122.0(14) . . ? O3 C10 C9 121.6(12) . . ? O3 C10 C11 122.6(11) . . ? C9 C10 C11 115.6(12) . . ? C12 C11 C10 119.4(12) . . ? C12 C11 C15 121.5(13) . . ? C10 C11 C15 119.0(12) . . ? C11 C12 C13 125.0(13) . . ? C11 C12 H12 117.5 . . ? C13 C12 H12 117.5 . . ? C14 C13 C12 114.7(13) . . ? C14 C13 C19 125.8(13) . . ? C12 C13 C19 119.4(13) . . ? C13 C14 C9 124.3(14) . . ? C13 C14 H14 117.9 . . ? C9 C14 H14 117.9 . . ? C16 C15 C17 110(2) . . ? C16 C15 C11 111.2(18) . . ? C17 C15 C11 108.7(16) . . ? C16 C15 C18 111.6(17) . . ? C17 C15 C18 104.9(17) . . ? C11 C15 C18 110.7(16) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C13 107.7(13) . . ? C21 C19 C20 112.7(16) . . ? C13 C19 C20 111.4(14) . . ? C21 C19 C22 106.6(15) . . ? C13 C19 C22 111.0(13) . . ? C20 C19 C22 107.4(13) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O4 C23 N3 118.3(15) . . ? O4 C23 C24 119.9(13) . . ? N3 C23 C24 121.6(15) . . ? C29 C24 C23 123.7(14) . . ? C29 C24 C25 114.3(14) . . ? C23 C24 C25 118.9(13) . . ? O5 C25 C26 122.2(15) . . ? O5 C25 C24 118.4(15) . . ? C26 C25 C24 118.6(14) . . ? C27 C26 C25 121.1(18) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 122.1(19) . . ? C26 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C29 C28 C27 119.3(16) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C24 122.9(15) . . ? C28 C29 H29 118.5 . . ? C24 C29 H29 118.5 . . ? N4 C30 C31 121.6(13) . . ? N4 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C32 C31 C30 125.7(12) . . ? C32 C31 C36 119.4(14) . . ? C30 C31 C36 114.9(14) . . ? O6 C32 C31 120.3(13) . . ? O6 C32 C33 120.1(11) . . ? C31 C32 C33 119.6(11) . . ? C34 C33 C32 116.9(12) . . ? C34 C33 C37 120.6(13) . . ? C32 C33 C37 122.5(11) . . ? C33 C34 C35 125.6(13) . . ? C33 C34 H34 117.2 . . ? C35 C34 H34 117.2 . . ? C36 C35 C34 117.6(12) . . ? C36 C35 C41 122.3(14) . . ? C34 C35 C41 120.1(14) . . ? C35 C36 C31 120.8(15) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C39 C37 C40 108.0(16) . . ? C39 C37 C33 110.7(15) . . ? C40 C37 C33 114.4(13) . . ? C39 C37 C38 107.6(15) . . ? C40 C37 C38 105.3(16) . . ? C33 C37 C38 110.6(14) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C35 109.8(15) . . ? C42 C41 C43 113.5(16) . . ? C35 C41 C43 108.6(14) . . ? C42 C41 C44 105.9(17) . . ? C35 C41 C44 112.2(14) . . ? C43 C41 C44 106.8(16) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O7 C45 C46 115.4(19) . . ? O7 C45 C46' 115(3) . . ? C46 C45 C46' 128(3) . . ? O7 C45 H45A 108.4 . . ? C46 C45 H45A 108.4 . . ? C46' C45 H45A 67.9 . . ? O7 C45 H45B 108.4 . . ? C46 C45 H45B 108.4 . . ? C46' C45 H45B 40.1 . . ? H45A C45 H45B 107.5 . . ? O7 C45 H45C 109.1 . . ? C46 C45 H45C 43.6 . . ? C46' C45 H45C 105.2 . . ? H45A C45 H45C 140.9 . . ? H45B C45 H45C 70.4 . . ? O7 C45 H45D 109.6 . . ? C46 C45 H45D 64.7 . . ? C46' C45 H45D 110.4 . . ? H45A C45 H45D 48.3 . . ? H45B C45 H45D 140.1 . . ? H45C C45 H45D 107.5 . . ? O8 C47 C48' 115(2) . . ? O8 C47 C48 115(2) . . ? C48' C47 C48 128(3) . . ? O8 C47 H47C 108.5 . . ? C48' C47 H47C 65.4 . . ? C48 C47 H47C 108.5 . . ? O8 C47 H47D 108.4 . . ? C48' C47 H47D 42.6 . . ? C48 C47 H47D 108.5 . . ? H47C C47 H47D 107.5 . . ? O8 C47 H47A 106.8 . . ? C48' C47 H47A 108.0 . . ? C48 C47 H47A 44.8 . . ? H47C C47 H47A 143.2 . . ? H47D C47 H47A 70.4 . . ? O8 C47 H47B 109.4 . . ? C48' C47 H47B 109.6 . . ? C48 C47 H47B 63.1 . . ? H47C C47 H47B 50.1 . . ? H47D C47 H47B 140.8 . . ? H47A C47 H47B 107.4 . . ? O9 C49 C50 116(3) . . ? O9 C49 C50' 116(3) . . ? C50 C49 C50' 123(3) . . ? O9 C49 H49A 108.2 . . ? C50 C49 H49A 108.2 . . ? C50' C49 H49A 74.1 . . ? O9 C49 H49B 108.2 . . ? C50 C49 H49B 108.2 . . ? C50' C49 H49B 33.5 . . ? H49A C49 H49B 107.4 . . ? O9 C49 H49C 107.6 . . ? C50 C49 H49C 23.5 . . ? C50' C49 H49C 117.2 . . ? H49A C49 H49C 130.7 . . ? H49B C49 H49C 92.2 . . ? O9 C49 H49D 105.7 . . ? C50 C49 H49D 83.6 . . ? C50' C49 H49D 101.9 . . ? H49A C49 H49D 30.1 . . ? H49B C49 H49D 133.3 . . ? H49C C49 H49D 107.1 . . ? O10 C51 C52' 116(4) . . ? O10 C51 C52 116(3) . . ? C52' C51 C52 128(5) . . ? O10 C51 H51A 108.4 . . ? C52' C51 H51A 54.2 . . ? C52 C51 H51A 108.4 . . ? O10 C51 H51B 108.4 . . ? C52' C51 H51B 53.7 . . ? C52 C51 H51B 108.4 . . ? H51A C51 H51B 107.4 . . ? O10 C51 H51C 99.8 . . ? C52' C51 H51C 91.7 . . ? C52 C51 H51C 79.4 . . ? H51A C51 H51C 142.7 . . ? H51B C51 H51C 38.7 . . ? O10 C51 H51D 106.2 . . ? C52' C51 H51D 129.4 . . ? C52 C51 H51D 28.0 . . ? H51A C51 H51D 88.1 . . ? H51B C51 H51D 134.6 . . ? H51C C51 H51D 107.2 . . ? C45 C46 H45C 39.2 . . ? C45 C46 H45D 38.4 . . ? H45C C46 H45D 77.1 . . ? C45 C46 H46A 109.5 . . ? H45C C46 H46A 148.6 . . ? H45D C46 H46A 71.6 . . ? C45 C46 H46B 109.5 . . ? H45C C46 H46B 86.2 . . ? H45D C46 H46B 118.0 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H45C C46 H46C 89.3 . . ? H45D C46 H46C 129.1 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C47 C48 H47A 39.5 . . ? C47 C48 H47B 38.8 . . ? H47A C48 H47B 78.0 . . ? C47 C48 H48A 109.5 . . ? H47A C48 H48A 126.4 . . ? H47B C48 H48A 90.4 . . ? C47 C48 H48B 109.5 . . ? H47A C48 H48B 121.3 . . ? H47B C48 H48B 85.7 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H47A C48 H48C 70.0 . . ? H47B C48 H48C 148.0 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C49 C50 H49C 31.2 . . ? C49 C50 H50A 109.5 . . ? H49C C50 H50A 133.2 . . ? C49 C50 H50B 109.5 . . ? H49C C50 H50B 80.9 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H49C C50 H50C 109.2 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C51 C52 H51D 34.1 . . ? C51 C52 H52A 109.5 . . ? H51D C52 H52A 76.2 . . ? C51 C52 H52B 109.5 . . ? H51D C52 H52B 129.9 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H51D C52 H52C 115.1 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C45 C46' H46D 109.5 . . ? C45 C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? C45 C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? C47 C48' H48D 109.5 . . ? C47 C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? C47 C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? C49 C50' H50D 109.5 . . ? C49 C50' H50E 109.5 . . ? H50D C50' H50E 109.5 . . ? C49 C50' H50F 109.5 . . ? H50D C50' H50F 109.5 . . ? H50E C50' H50F 109.5 . . ? C51 C52' H52D 109.5 . . ? C51 C52' H52E 109.5 . . ? H52D C52' H52E 109.5 . . ? C51 C52' H52F 109.5 . . ? H52D C52' H52F 109.5 . . ? H52E C52' H52F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 N2 C8 -177.3(13) . . . . ? C1 N1 N2 Zn2 13.1(14) . . . . ? O5 Zn2 N2 C8 131.8(12) 1_545 . . . ? O3 Zn2 N2 C8 22.4(12) . . . . ? O8 Zn2 N2 C8 -83.5(13) . . . . ? O1 Zn2 N2 C8 178.3(13) . . . . ? O5 Zn2 N2 N1 -59.7(12) 1_545 . . . ? O3 Zn2 N2 N1 -169.0(8) . . . . ? O8 Zn2 N2 N1 85.1(8) . . . . ? O1 Zn2 N2 N1 -13.1(7) . . . . ? C23 N3 N4 C30 175.8(12) . . . . ? C23 N3 N4 Zn1 -14.8(14) . . . . ? O2 Zn1 N4 C30 -135.9(11) . . . . ? O6 Zn1 N4 C30 -27.1(11) . . . . ? O7 Zn1 N4 C30 82.0(11) . . . . ? O4 Zn1 N4 C30 -177.6(11) . . . . ? O2 Zn1 N4 N3 56.1(12) . . . . ? O6 Zn1 N4 N3 164.9(8) . . . . ? O7 Zn1 N4 N3 -86.0(9) . . . . ? O4 Zn1 N4 N3 14.4(8) . . . . ? O5 Zn2 O1 C1 169.6(10) 1_545 . . . ? O3 Zn2 O1 C1 65.8(12) . . . . ? O8 Zn2 O1 C1 -86.7(10) . . . . ? N2 Zn2 O1 C1 13.1(9) . . . . ? O6 Zn1 O2 C3 76.5(13) . . . . ? O7 Zn1 O2 C3 -38.3(13) . . . . ? N4 Zn1 O2 C3 -179.8(11) . . . . ? O4 Zn1 O2 C3 -139.8(13) . . . . ? O5 Zn2 O3 C10 -179.1(11) 1_545 . . . ? O8 Zn2 O3 C10 70.3(12) . . . . ? N2 Zn2 O3 C10 -31.1(12) . . . . ? O1 Zn2 O3 C10 -81.4(14) . . . . ? O2 Zn1 O4 C23 -173.6(12) . . . . ? O6 Zn1 O4 C23 -69.5(13) . . . . ? O7 Zn1 O4 C23 83.4(12) . . . . ? N4 Zn1 O4 C23 -13.7(11) . . . . ? O2 Zn1 O6 C32 -172.6(10) . . . . ? O7 Zn1 O6 C32 -61.8(11) . . . . ? N4 Zn1 O6 C32 37.4(10) . . . . ? O4 Zn1 O6 C32 90.0(11) . . . . ? O2 Zn1 O7 C45 161.9(15) . . . . ? O6 Zn1 O7 C45 51.3(16) . . . . ? N4 Zn1 O7 C45 -37.0(15) . . . . ? O4 Zn1 O7 C45 -112.0(15) . . . . ? O5 Zn2 O8 C47 -160.9(13) 1_545 . . . ? O3 Zn2 O8 C47 -50.8(14) . . . . ? N2 Zn2 O8 C47 38.1(14) . . . . ? O1 Zn2 O8 C47 114.9(14) . . . . ? Zn2 O1 C1 N1 -10.8(16) . . . . ? Zn2 O1 C1 C2 174.0(10) . . . . ? N2 N1 C1 O1 -0.8(19) . . . . ? N2 N1 C1 C2 174.1(12) . . . . ? O1 C1 C2 C7 -16(2) . . . . ? N1 C1 C2 C7 168.8(16) . . . . ? O1 C1 C2 C3 -175.8(13) . . . . ? N1 C1 C2 C3 9(2) . . . . ? Zn1 O2 C3 C4 -17(2) . . . . ? Zn1 O2 C3 C2 170.2(9) . . . . ? C7 C2 C3 O2 -177.1(14) . . . . ? C1 C2 C3 O2 -15.6(19) . . . . ? C7 C2 C3 C4 9(2) . . . . ? C1 C2 C3 C4 170.8(14) . . . . ? O2 C3 C4 C5 -179.5(16) . . . . ? C2 C3 C4 C5 -6(2) . . . . ? C3 C4 C5 C6 4(3) . . . . ? C4 C5 C6 C7 -4(3) . . . . ? C1 C2 C7 C6 -170.3(17) . . . . ? C3 C2 C7 C6 -10(3) . . . . ? C5 C6 C7 C2 8(3) . . . . ? N1 N2 C8 C9 -178.8(12) . . . . ? Zn2 N2 C8 C9 -11(2) . . . . ? N2 C8 C9 C14 173.4(15) . . . . ? N2 C8 C9 C10 -4(2) . . . . ? Zn2 O3 C10 C9 27.3(19) . . . . ? Zn2 O3 C10 C11 -157.6(10) . . . . ? C14 C9 C10 O3 179.3(13) . . . . ? C8 C9 C10 O3 -3(2) . . . . ? C14 C9 C10 C11 3.9(19) . . . . ? C8 C9 C10 C11 -178.7(13) . . . . ? O3 C10 C11 C12 179.2(14) . . . . ? C9 C10 C11 C12 -5.5(19) . . . . ? O3 C10 C11 C15 2(2) . . . . ? C9 C10 C11 C15 177.1(15) . . . . ? C10 C11 C12 C13 6(2) . . . . ? C15 C11 C12 C13 -176.4(16) . . . . ? C11 C12 C13 C14 -5(2) . . . . ? C11 C12 C13 C19 178.9(15) . . . . ? C12 C13 C14 C9 3(2) . . . . ? C19 C13 C14 C9 179.0(15) . . . . ? C8 C9 C14 C13 179.6(14) . . . . ? C10 C9 C14 C13 -3(2) . . . . ? C12 C11 C15 C16 125(2) . . . . ? C10 C11 C15 C16 -58(2) . . . . ? C12 C11 C15 C17 -114.5(19) . . . . ? C10 C11 C15 C17 63(2) . . . . ? C12 C11 C15 C18 0(3) . . . . ? C10 C11 C15 C18 177.5(16) . . . . ? C14 C13 C19 C21 -107.0(18) . . . . ? C12 C13 C19 C21 68.9(19) . . . . ? C14 C13 C19 C20 128.9(17) . . . . ? C12 C13 C19 C20 -55.1(19) . . . . ? C14 C13 C19 C22 9(2) . . . . ? C12 C13 C19 C22 -174.8(14) . . . . ? Zn1 O4 C23 N3 10.4(19) . . . . ? Zn1 O4 C23 C24 -174.3(11) . . . . ? N4 N3 C23 O4 2(2) . . . . ? N4 N3 C23 C24 -172.9(13) . . . . ? O4 C23 C24 C29 18(3) . . . . ? N3 C23 C24 C29 -167.1(15) . . . . ? O4 C23 C24 C25 176.5(15) . . . . ? N3 C23 C24 C25 -8(2) . . . . ? Zn2 O5 C25 C26 24(2) 1_565 . . . ? Zn2 O5 C25 C24 -166.3(10) 1_565 . . . ? C29 C24 C25 O5 177.5(14) . . . . ? C23 C24 C25 O5 17(2) . . . . ? C29 C24 C25 C26 -12(2) . . . . ? C23 C24 C25 C26 -173.0(16) . . . . ? O5 C25 C26 C27 175.7(16) . . . . ? C24 C25 C26 C27 6(3) . . . . ? C25 C26 C27 C28 -1(3) . . . . ? C26 C27 C28 C29 4(3) . . . . ? C27 C28 C29 C24 -12(3) . . . . ? C23 C24 C29 C28 175.1(17) . . . . ? C25 C24 C29 C28 15(2) . . . . ? N3 N4 C30 C31 177.8(11) . . . . ? Zn1 N4 C30 C31 10.0(18) . . . . ? N4 C30 C31 C32 12(2) . . . . ? N4 C30 C31 C36 -171.6(11) . . . . ? Zn1 O6 C32 C31 -30.1(16) . . . . ? Zn1 O6 C32 C33 152.2(9) . . . . ? C30 C31 C32 O6 -2.4(19) . . . . ? C36 C31 C32 O6 -178.9(11) . . . . ? C30 C31 C32 C33 175.4(12) . . . . ? C36 C31 C32 C33 -1.2(18) . . . . ? O6 C32 C33 C34 -179.1(11) . . . . ? C31 C32 C33 C34 3.1(18) . . . . ? O6 C32 C33 C37 0(2) . . . . ? C31 C32 C33 C37 -178.2(12) . . . . ? C32 C33 C34 C35 -2(2) . . . . ? C37 C33 C34 C35 179.7(14) . . . . ? C33 C34 C35 C36 -2(2) . . . . ? C33 C34 C35 C41 175.9(14) . . . . ? C34 C35 C36 C31 4(2) . . . . ? C41 C35 C36 C31 -173.8(13) . . . . ? C32 C31 C36 C35 -2.7(19) . . . . ? C30 C31 C36 C35 -179.6(13) . . . . ? C34 C33 C37 C39 115.8(16) . . . . ? C32 C33 C37 C39 -62.9(19) . . . . ? C34 C33 C37 C40 -6(2) . . . . ? C32 C33 C37 C40 174.9(14) . . . . ? C34 C33 C37 C38 -125.1(15) . . . . ? C32 C33 C37 C38 56.2(19) . . . . ? C36 C35 C41 C42 110.4(19) . . . . ? C34 C35 C41 C42 -68(2) . . . . ? C36 C35 C41 C43 -124.9(17) . . . . ? C34 C35 C41 C43 57(2) . . . . ? C36 C35 C41 C44 -7(2) . . . . ? C34 C35 C41 C44 174.9(15) . . . . ? Zn1 O7 C45 C46 -73(2) . . . . ? Zn1 O7 C45 C46' 91(3) . . . . ? Zn2 O8 C47 C48' 75(2) . . . . ? Zn2 O8 C47 C48 -93(2) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.544 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.105 #=================================END data_4 _database_code_depnum_ccdc_archive 'CCDC 727399' #TrackingRef '- crystal data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H140 Co3 N12 O14' _chemical_formula_weight 1935.05 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 Tetragonal _symmetry_space_group_name_H-M p43212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' _cell_length_a 16.175(2) _cell_length_b 16.175(2) _cell_length_c 41.560(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10873(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4116 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7904 _exptl_absorpt_correction_T_max 0.8246 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54507 _diffrn_reflns_av_R_equivalents 0.1518 _diffrn_reflns_av_sigmaI/netI 0.1108 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9576 _reflns_number_gt 5617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.1164P)^2^+0.8801P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 9576 _refine_ls_number_parameters 601 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1197 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.2132 _refine_ls_wR_factor_gt 0.1913 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _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 Co1 Co 0.88929(5) 0.12284(6) 0.13182(2) 0.0409(2) Uani 1 1 d . . . Co2 Co 0.19947(6) 0.19947(6) 0.0000 0.0522(4) Uani 1 2 d S . . N1 N 0.8801(3) 0.1638(3) 0.19620(12) 0.0417(13) Uani 1 1 d . . . N2 N 0.8356(3) 0.1259(3) 0.17187(12) 0.0399(13) Uani 1 1 d . . . N3 N 0.9207(4) 0.1911(4) 0.07221(13) 0.0477(15) Uani 1 1 d . . . N4 N 0.9460(4) 0.1294(4) 0.09296(12) 0.0432(14) Uani 1 1 d . . . N5 N 0.1066(4) 0.2774(4) 0.08907(14) 0.0610(18) Uani 1 1 d . . . N6 N 0.3985(5) 0.0865(5) 0.04768(17) 0.072(2) Uani 1 1 d . . . O1 O 0.9738(3) 0.1794(3) 0.15494(10) 0.0408(11) Uani 1 1 d . . . O2 O 0.8042(3) 0.0668(3) 0.11146(10) 0.0477(12) Uani 1 1 d . . . O3 O 0.8444(3) 0.2259(3) 0.11658(11) 0.0478(11) Uani 1 1 d . . . O4 O 0.9365(3) 0.0227(3) 0.14446(9) 0.0413(11) Uani 1 1 d . . . O5 O 0.1721(4) 0.2241(4) 0.04680(12) 0.0669(16) Uani 1 1 d . . . O6 O 0.2904(4) 0.1143(4) 0.01565(13) 0.0798(17) Uani 1 1 d . . . O7 O 0.1079(6) 0.1079(6) 0.0000 0.118(4) Uani 1 2 d SD . . H7 H 0.0624 0.1266 -0.0048 0.177 Uiso 0.50 1 d PRD . . O8 O 0.2888(3) 0.2888(3) 0.0000 0.0555(18) Uani 1 2 d S . . H8A H 0.3115 0.2964 -0.0182 0.067 Uiso 0.50 1 d PR . . H8B H 0.3249 0.2829 0.0146 0.067 Uiso 0.50 1 d PR . . C1 C 0.9524(4) 0.1844(4) 0.18526(14) 0.0373(15) Uani 1 1 d . . . C2 C 1.0166(4) 0.2127(4) 0.20782(14) 0.0397(16) Uani 1 1 d . . . C3 C 1.0060(5) 0.1967(6) 0.24084(17) 0.064(2) Uani 1 1 d . . . H3 H 0.9587 0.1708 0.2486 0.077 Uiso 1 1 calc R . . C4 C 1.0703(6) 0.2218(6) 0.26163(19) 0.074(3) Uani 1 1 d . . . H4 H 1.0652 0.2132 0.2837 0.089 Uiso 1 1 calc R . . C5 C 1.1417(5) 0.2595(5) 0.2495(2) 0.072(2) Uani 1 1 d . . . H5 H 1.1826 0.2768 0.2638 0.087 Uiso 1 1 calc R . . C6 C 1.1526(5) 0.2714(6) 0.2174(2) 0.072(3) Uani 1 1 d . . . H6 H 1.2018 0.2928 0.2094 0.087 Uiso 1 1 calc R . . C7 C 1.0892(4) 0.2509(5) 0.19713(17) 0.056(2) Uani 1 1 d . . . H7A H 1.0945 0.2628 0.1753 0.067 Uiso 1 1 calc R . . C8 C 0.7677(4) 0.0909(4) 0.17894(16) 0.0450(17) Uani 1 1 d . . . H8 H 0.7469 0.0997 0.1995 0.054 Uiso 1 1 calc R . . C9 C 0.7197(4) 0.0385(5) 0.15758(16) 0.0454(17) Uani 1 1 d . . . C10 C 0.7436(4) 0.0262(4) 0.12525(15) 0.0416(16) Uani 1 1 d . . . C11 C 0.6972(5) -0.0315(5) 0.1073(2) 0.059(2) Uani 1 1 d . . . C12 C 0.6312(5) -0.0704(5) 0.12273(19) 0.064(2) Uani 1 1 d . . . H12 H 0.6017 -0.1093 0.1109 0.076 Uiso 1 1 calc R . . C13 C 0.6053(5) -0.0564(5) 0.15405(19) 0.056(2) Uani 1 1 d . . . C14 C 0.6508(4) -0.0026(5) 0.17072(19) 0.0534(19) Uani 1 1 d . . . H14 H 0.6365 0.0082 0.1920 0.064 Uiso 1 1 calc R . . C15 C 0.7246(6) -0.0554(6) 0.07353(19) 0.072(3) Uani 1 1 d . . . C16 C 0.8110(7) -0.0893(7) 0.0739(2) 0.090(3) Uani 1 1 d . . . H16A H 0.8485 -0.0474 0.0812 0.135 Uiso 1 1 calc R . . H16B H 0.8261 -0.1064 0.0526 0.135 Uiso 1 1 calc R . . H16C H 0.8135 -0.1360 0.0882 0.135 Uiso 1 1 calc R . . C17 C 0.7188(8) 0.0234(8) 0.0517(2) 0.114(4) Uani 1 1 d . . . H17A H 0.7654 0.0586 0.0557 0.171 Uiso 1 1 calc R . . H17B H 0.6687 0.0528 0.0565 0.171 Uiso 1 1 calc R . . H17C H 0.7186 0.0070 0.0295 0.171 Uiso 1 1 calc R . . C18 C 0.6651(8) -0.1218(8) 0.0584(2) 0.116(5) Uani 1 1 d . . . H18A H 0.6719 -0.1224 0.0354 0.174 Uiso 1 1 calc R . . H18B H 0.6088 -0.1082 0.0636 0.174 Uiso 1 1 calc R . . H18C H 0.6782 -0.1754 0.0669 0.174 Uiso 1 1 calc R . . C19 C 0.5295(5) -0.0969(6) 0.1687(2) 0.068(2) Uani 1 1 d . . . C20 C 0.5502(9) -0.1303(12) 0.2004(4) 0.194(9) Uani 1 1 d . . . H20A H 0.5438 -0.0879 0.2163 0.291 Uiso 1 1 calc R . . H20B H 0.6064 -0.1494 0.2003 0.291 Uiso 1 1 calc R . . H20C H 0.5139 -0.1756 0.2053 0.291 Uiso 1 1 calc R . . C21 C 0.4979(9) -0.1671(10) 0.1487(3) 0.166(7) Uani 1 1 d . . . H21A H 0.4434 -0.1820 0.1558 0.249 Uiso 1 1 calc R . . H21B H 0.5342 -0.2137 0.1509 0.249 Uiso 1 1 calc R . . H21C H 0.4959 -0.1505 0.1265 0.249 Uiso 1 1 calc R . . C22 C 0.4581(8) -0.0404(10) 0.1698(4) 0.163(7) Uani 1 1 d . . . H22A H 0.4690 0.0035 0.1847 0.244 Uiso 1 1 calc R . . H22B H 0.4098 -0.0703 0.1765 0.244 Uiso 1 1 calc R . . H22C H 0.4488 -0.0176 0.1487 0.244 Uiso 1 1 calc R . . C23 C 0.8673(5) 0.2380(5) 0.08752(17) 0.0488(18) Uani 1 1 d . . . C24 C 0.8347(5) 0.3103(5) 0.06963(17) 0.0518(19) Uani 1 1 d . . . C25 C 0.8494(6) 0.3221(6) 0.0377(2) 0.077(3) Uani 1 1 d . . . H25 H 0.8828 0.2857 0.0263 0.093 Uiso 1 1 calc R . . C26 C 0.8140(7) 0.3887(8) 0.0230(2) 0.099(4) Uani 1 1 d . . . H26 H 0.8253 0.3982 0.0013 0.118 Uiso 1 1 calc R . . C27 C 0.7620(7) 0.4424(7) 0.0390(3) 0.097(3) Uani 1 1 d . . . H27 H 0.7367 0.4859 0.0282 0.116 Uiso 1 1 calc R . . C28 C 0.7489(6) 0.4312(6) 0.0696(2) 0.082(3) Uani 1 1 d . . . H28 H 0.7152 0.4676 0.0809 0.099 Uiso 1 1 calc R . . C29 C 0.7841(6) 0.3671(5) 0.0849(2) 0.074(2) Uani 1 1 d . . . H29 H 0.7740 0.3606 0.1068 0.088 Uiso 1 1 calc R . . C30 C 1.0078(5) 0.0830(4) 0.08434(17) 0.0507(19) Uani 1 1 d . . . H30 H 1.0324 0.0941 0.0646 0.061 Uiso 1 1 calc R . . C31 C 1.0407(4) 0.0168(4) 0.10268(15) 0.0411(16) Uani 1 1 d . . . C32 C 1.0020(4) -0.0099(4) 0.13244(14) 0.0447(15) Uani 1 1 d . . . C33 C 1.0399(4) -0.0778(4) 0.14853(16) 0.0457(18) Uani 1 1 d . . . C34 C 1.1101(5) -0.1135(5) 0.1352(2) 0.067(2) Uani 1 1 d . . . H34 H 1.1338 -0.1577 0.1461 0.081 Uiso 1 1 calc R . . C35 C 1.1476(5) -0.0879(5) 0.10663(18) 0.055(2) Uani 1 1 d . . . C36 C 1.1093(5) -0.0221(5) 0.09134(19) 0.058(2) Uani 1 1 d . . . H36 H 1.1320 -0.0034 0.0721 0.069 Uiso 1 1 calc R . . C37 C 1.0009(6) -0.1098(5) 0.17917(19) 0.069(2) Uani 1 1 d . . . C38 C 0.9121(6) -0.1428(6) 0.1716(2) 0.085(3) Uani 1 1 d . . . H38A H 0.8780 -0.0980 0.1644 0.127 Uiso 1 1 calc R . . H38B H 0.8887 -0.1664 0.1908 0.127 Uiso 1 1 calc R . . H38C H 0.9152 -0.1843 0.1552 0.127 Uiso 1 1 calc R . . C39 C 0.9974(6) -0.0430(6) 0.20496(19) 0.076(3) Uani 1 1 d . . . H39A H 1.0525 -0.0290 0.2116 0.115 Uiso 1 1 calc R . . H39B H 0.9667 -0.0630 0.2231 0.115 Uiso 1 1 calc R . . H39C H 0.9706 0.0053 0.1964 0.115 Uiso 1 1 calc R . . C40 C 1.0508(7) -0.1834(7) 0.1931(2) 0.106(4) Uani 1 1 d . . . H40A H 1.0544 -0.2264 0.1772 0.158 Uiso 1 1 calc R . . H40B H 1.0235 -0.2041 0.2119 0.158 Uiso 1 1 calc R . . H40C H 1.1054 -0.1651 0.1987 0.158 Uiso 1 1 calc R . . C41 C 1.2262(5) -0.1284(6) 0.0936(2) 0.073(3) Uani 1 1 d . . . C42 C 1.2958(7) -0.0667(9) 0.0948(4) 0.153(6) Uani 1 1 d . . . H42A H 1.3393 -0.0843 0.0807 0.229 Uiso 1 1 calc R . . H42B H 1.3165 -0.0630 0.1164 0.229 Uiso 1 1 calc R . . H42C H 1.2759 -0.0135 0.0881 0.229 Uiso 1 1 calc R . . C43 C 1.2472(9) -0.2058(9) 0.1091(4) 0.192(9) Uani 1 1 d . . . H43A H 1.2060 -0.2466 0.1041 0.289 Uiso 1 1 calc R . . H43B H 1.2494 -0.1979 0.1320 0.289 Uiso 1 1 calc R . . H43C H 1.3001 -0.2243 0.1016 0.289 Uiso 1 1 calc R . . C44 C 1.2221(9) -0.1475(11) 0.0589(3) 0.170(7) Uani 1 1 d . . . H44A H 1.2612 -0.1903 0.0539 0.256 Uiso 1 1 calc R . . H44B H 1.2351 -0.0988 0.0467 0.256 Uiso 1 1 calc R . . H44C H 1.1674 -0.1659 0.0535 0.256 Uiso 1 1 calc R . . C45 C 0.1202(6) 0.2659(5) 0.05825(17) 0.058(2) Uani 1 1 d . . . H45 H 0.0854 0.2935 0.0440 0.069 Uiso 1 1 calc R . . C46 C 0.1609(6) 0.2343(7) 0.11110(19) 0.086(3) Uani 1 1 d . . . H46A H 0.2083 0.2141 0.0996 0.128 Uiso 1 1 calc R . . H46B H 0.1319 0.1886 0.1206 0.128 Uiso 1 1 calc R . . H46C H 0.1786 0.2715 0.1277 0.128 Uiso 1 1 calc R . . C47 C 0.0445(5) 0.3321(5) 0.10292(18) 0.058(2) Uani 1 1 d . . . H47A H 0.0131 0.3575 0.0860 0.087 Uiso 1 1 calc R . . H47B H 0.0713 0.3742 0.1154 0.087 Uiso 1 1 calc R . . H47C H 0.0081 0.3007 0.1165 0.087 Uiso 1 1 calc R . . C48 C 0.3261(6) 0.1236(5) 0.04130(19) 0.067(2) Uani 1 1 d . . . H48 H 0.3024 0.1575 0.0569 0.081 Uiso 1 1 calc R . . C49 C 0.4383(9) 0.0358(11) 0.0227(3) 0.161(7) Uani 1 1 d . . . H49A H 0.4432 -0.0201 0.0302 0.241 Uiso 1 1 calc R . . H49B H 0.4923 0.0575 0.0182 0.241 Uiso 1 1 calc R . . H49C H 0.4054 0.0370 0.0035 0.241 Uiso 1 1 calc R . . C50 C 0.4361(7) 0.1002(7) 0.0784(2) 0.097(4) Uani 1 1 d . . . H50A H 0.4921 0.1184 0.0754 0.145 Uiso 1 1 calc R . . H50B H 0.4358 0.0497 0.0905 0.145 Uiso 1 1 calc R . . H50C H 0.4057 0.1418 0.0898 0.145 Uiso 1 1 calc R . . C51 C 0.1083(16) 0.0229(17) 0.0029(5) 0.117(9) Uani 0.50 1 d P . . H51A H 0.1319 0.0098 0.0237 0.141 Uiso 0.50 1 d PR . . H51B H 0.1457 0.0010 -0.0133 0.141 Uiso 0.50 1 d PR . . C52 C 0.0280(13) -0.0228(15) 0.0006(6) 0.108(10) Uani 0.50 1 d P . . H52A H 0.0093 -0.0390 0.0216 0.162 Uiso 0.50 1 d PR . . H52B H 0.0356 -0.0711 -0.0125 0.162 Uiso 0.50 1 d PR . . H52C H -0.0124 0.0126 -0.0092 0.162 Uiso 0.50 1 d PR . . 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 Co1 0.0437(6) 0.0449(6) 0.0342(4) -0.0021(4) 0.0020(4) -0.0001(4) Co2 0.0607(6) 0.0607(6) 0.0352(7) -0.0009(5) 0.0009(5) -0.0116(7) N1 0.041(3) 0.053(3) 0.031(3) -0.002(2) 0.001(3) 0.010(3) N2 0.038(3) 0.046(3) 0.037(3) 0.005(3) -0.002(2) 0.003(3) N3 0.057(4) 0.049(4) 0.037(3) 0.008(3) -0.006(3) 0.001(3) N4 0.051(4) 0.045(4) 0.033(3) -0.006(3) -0.012(3) -0.010(3) N5 0.053(4) 0.092(5) 0.038(4) 0.001(3) 0.001(3) -0.014(4) N6 0.079(6) 0.071(5) 0.065(5) 0.002(4) -0.003(4) -0.006(4) O1 0.044(3) 0.047(3) 0.031(2) -0.004(2) -0.001(2) -0.003(2) O2 0.054(3) 0.046(3) 0.043(3) -0.001(2) 0.004(2) -0.005(2) O3 0.052(3) 0.054(3) 0.038(3) 0.005(2) -0.003(2) -0.002(2) O4 0.041(3) 0.055(3) 0.028(2) -0.003(2) 0.005(2) 0.003(2) O5 0.068(4) 0.099(4) 0.034(3) -0.002(3) 0.005(3) 0.028(3) O6 0.104(5) 0.082(4) 0.053(3) 0.001(3) -0.011(3) 0.011(4) O7 0.151(6) 0.151(6) 0.052(6) 0.009(5) -0.009(5) -0.035(9) O8 0.065(3) 0.065(3) 0.035(3) -0.005(3) 0.005(3) -0.022(4) C1 0.048(4) 0.041(4) 0.023(3) -0.002(3) -0.002(3) 0.009(3) C2 0.046(4) 0.039(4) 0.034(4) -0.013(3) -0.006(3) 0.003(3) C3 0.050(5) 0.107(7) 0.035(4) 0.002(4) 0.007(3) -0.002(4) C4 0.069(6) 0.112(8) 0.042(5) -0.008(5) -0.009(4) 0.017(5) C5 0.047(5) 0.090(7) 0.079(6) -0.038(6) -0.006(5) -0.005(4) C6 0.053(5) 0.096(7) 0.068(6) -0.030(5) -0.009(4) -0.005(5) C7 0.048(5) 0.088(6) 0.031(4) 0.003(4) 0.009(3) 0.000(4) C8 0.053(5) 0.046(4) 0.036(4) -0.002(3) 0.006(3) -0.001(3) C9 0.035(4) 0.058(5) 0.043(4) 0.002(3) -0.005(3) 0.002(3) C10 0.051(4) 0.036(4) 0.037(4) 0.003(3) -0.007(3) 0.000(3) C11 0.050(5) 0.053(5) 0.072(5) 0.004(4) -0.011(4) -0.010(4) C12 0.065(5) 0.064(5) 0.062(5) 0.008(4) -0.015(4) -0.019(4) C13 0.045(5) 0.062(5) 0.062(5) 0.009(4) -0.004(4) -0.010(4) C14 0.043(4) 0.068(5) 0.049(4) 0.003(4) 0.012(4) 0.000(4) C15 0.085(7) 0.083(6) 0.049(5) -0.017(5) 0.004(5) -0.035(5) C16 0.100(8) 0.097(8) 0.073(6) -0.027(5) 0.010(6) -0.014(6) C17 0.138(10) 0.137(10) 0.068(7) 0.031(7) -0.034(7) -0.046(8) C18 0.172(12) 0.125(10) 0.050(5) -0.026(6) 0.012(6) -0.069(9) C19 0.059(5) 0.090(7) 0.055(5) 0.011(5) 0.007(4) -0.023(5) C20 0.123(12) 0.30(2) 0.162(14) 0.081(15) 0.010(10) -0.118(14) C21 0.140(13) 0.199(17) 0.159(13) -0.010(13) 0.052(10) -0.086(12) C22 0.090(10) 0.143(13) 0.255(19) 0.042(13) 0.045(11) 0.009(9) C23 0.052(5) 0.056(5) 0.038(4) 0.004(4) -0.017(4) -0.010(4) C24 0.055(5) 0.054(5) 0.046(4) 0.016(4) -0.011(4) -0.006(4) C25 0.098(7) 0.081(6) 0.053(5) 0.020(5) -0.013(5) 0.015(5) C26 0.119(9) 0.117(9) 0.060(6) 0.042(6) -0.017(6) 0.016(8) C27 0.107(9) 0.085(8) 0.098(8) 0.012(7) -0.026(7) 0.031(7) C28 0.099(8) 0.073(6) 0.076(7) 0.012(5) -0.016(6) 0.028(5) C29 0.076(6) 0.062(6) 0.082(6) 0.006(5) 0.000(5) 0.013(5) C30 0.066(5) 0.049(5) 0.037(4) -0.004(3) 0.003(4) 0.002(4) C31 0.048(4) 0.041(4) 0.035(4) -0.008(3) -0.001(3) 0.005(3) C32 0.044(4) 0.061(5) 0.029(3) -0.011(3) -0.005(3) 0.003(3) C33 0.050(4) 0.042(4) 0.046(4) -0.001(3) 0.003(3) 0.007(3) C34 0.082(6) 0.050(5) 0.071(5) 0.008(4) -0.001(5) 0.012(4) C35 0.042(4) 0.068(5) 0.053(5) -0.002(4) 0.006(4) -0.001(4) C36 0.063(5) 0.060(5) 0.050(5) -0.002(4) 0.020(4) -0.001(4) C37 0.089(6) 0.061(5) 0.056(5) 0.006(4) 0.023(5) 0.015(5) C38 0.101(8) 0.067(6) 0.088(7) -0.012(5) 0.015(6) -0.018(5) C39 0.103(7) 0.083(6) 0.044(5) 0.000(4) 0.009(4) 0.003(5) C40 0.130(10) 0.118(9) 0.069(6) 0.042(6) 0.047(6) 0.060(8) C41 0.060(6) 0.071(6) 0.088(7) 0.006(5) 0.004(5) 0.024(5) C42 0.055(7) 0.145(12) 0.259(19) -0.046(12) 0.027(9) 0.004(7) C43 0.152(13) 0.119(11) 0.31(2) 0.073(13) 0.144(14) 0.073(11) C44 0.134(12) 0.26(2) 0.117(10) -0.094(12) 0.011(9) 0.073(12) C45 0.077(6) 0.065(5) 0.031(4) 0.005(4) -0.009(4) -0.029(5) C46 0.066(6) 0.151(10) 0.040(5) -0.005(5) -0.004(4) 0.015(6) C47 0.064(5) 0.060(5) 0.050(5) -0.011(4) 0.012(4) -0.008(4) C48 0.095(7) 0.066(6) 0.041(5) 0.017(4) 0.002(5) -0.001(5) C49 0.124(11) 0.212(17) 0.146(12) -0.036(12) -0.027(10) 0.090(12) C50 0.098(8) 0.099(8) 0.092(7) 0.027(6) -0.044(6) -0.031(6) C51 0.15(2) 0.16(2) 0.046(11) 0.006(15) -0.015(14) -0.038(19) C52 0.119(19) 0.17(2) 0.033(7) 0.016(19) -0.014(16) -0.047(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 Co1 O2 1.853(5) . ? Co1 N4 1.860(6) . ? Co1 O4 1.866(5) . ? Co1 N2 1.878(5) . ? Co1 O1 1.905(4) . ? Co1 O3 1.925(5) . ? Co2 O5 2.034(5) 6 ? Co2 O5 2.034(5) . ? Co2 O8 2.043(6) . ? Co2 O7 2.095(13) . ? Co2 O6 2.118(6) . ? Co2 O6 2.118(6) 6 ? N1 C1 1.298(8) . ? N1 N2 1.384(7) . ? N2 C8 1.270(8) . ? N3 C23 1.314(9) . ? N3 N4 1.381(8) . ? N4 C30 1.301(9) . ? N5 C45 1.313(9) . ? N5 C46 1.448(11) . ? N5 C47 1.457(10) . ? N6 C48 1.343(11) . ? N6 C50 1.431(10) . ? N6 C49 1.469(14) . ? O1 C1 1.309(7) . ? O2 C10 1.312(8) . ? O3 C23 1.278(8) . ? O4 C32 1.284(8) . ? O5 C45 1.178(10) . ? O6 C48 1.221(9) . ? O7 C51 1.38(3) . ? O7 C51 1.38(3) 6 ? O7 H7 0.8204 . ? O8 H8A 0.8510 . ? O8 H8B 0.8489 . ? C1 C2 1.473(9) . ? C2 C7 1.398(10) . ? C2 C3 1.407(9) . ? C3 C4 1.413(11) . ? C3 H3 0.9300 . ? C4 C5 1.399(12) . ? C4 H4 0.9300 . ? C5 C6 1.363(12) . ? C5 H5 0.9300 . ? C6 C7 1.367(10) . ? C6 H6 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.452(10) . ? C8 H8 0.9300 . ? C9 C14 1.408(10) . ? C9 C10 1.412(9) . ? C10 C11 1.412(10) . ? C11 C12 1.396(11) . ? C11 C15 1.519(11) . ? C12 C13 1.386(11) . ? C12 H12 0.9300 . ? C13 C14 1.334(10) . ? C13 C19 1.517(10) . ? C14 H14 0.9300 . ? C15 C16 1.501(14) . ? C15 C17 1.567(14) . ? C15 C18 1.574(12) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.461(16) . ? C19 C22 1.474(16) . ? C19 C21 1.497(16) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.482(10) . ? C24 C25 1.360(10) . ? C24 C29 1.385(12) . ? C25 C26 1.366(13) . ? C25 H25 0.9300 . ? C26 C27 1.382(15) . ? C26 H26 0.9300 . ? C27 C28 1.301(13) . ? C27 H27 0.9300 . ? C28 C29 1.342(12) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.418(10) . ? C30 H30 0.9300 . ? C31 C36 1.360(10) . ? C31 C32 1.452(9) . ? C32 C33 1.424(10) . ? C33 C34 1.388(10) . ? C33 C37 1.513(10) . ? C34 C35 1.397(11) . ? C34 H34 0.9300 . ? C35 C36 1.384(11) . ? C35 C41 1.529(11) . ? C36 H36 0.9300 . ? C37 C39 1.524(11) . ? C37 C40 1.549(13) . ? C37 C38 1.564(13) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C43 1.450(15) . ? C41 C44 1.477(14) . ? C41 C42 1.505(15) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48 0.9300 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.50(3) . ? C51 C51 1.97(6) 6 ? C51 H51A 0.9700 . ? C51 H51B 0.9702 . ? C52 C52 1.16(5) 6 ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9599 . ? 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 O2 Co1 N4 89.9(2) . . ? O2 Co1 O4 90.5(2) . . ? N4 Co1 O4 95.3(2) . . ? O2 Co1 N2 94.3(2) . . ? N4 Co1 N2 174.8(2) . . ? O4 Co1 N2 87.9(2) . . ? O2 Co1 O1 176.87(19) . . ? N4 Co1 O1 93.2(2) . . ? O4 Co1 O1 88.89(19) . . ? N2 Co1 O1 82.7(2) . . ? O2 Co1 O3 89.6(2) . . ? N4 Co1 O3 81.4(2) . . ? O4 Co1 O3 176.69(19) . . ? N2 Co1 O3 95.4(2) . . ? O1 Co1 O3 91.20(19) . . ? O5 Co2 O5 178.2(4) 6 . ? O5 Co2 O8 90.91(19) 6 . ? O5 Co2 O8 90.91(19) . . ? O5 Co2 O7 89.09(19) 6 . ? O5 Co2 O7 89.09(19) . . ? O8 Co2 O7 180.000(1) . . ? O5 Co2 O6 90.9(2) 6 . ? O5 Co2 O6 89.1(2) . . ? O8 Co2 O6 88.22(19) . . ? O7 Co2 O6 91.78(19) . . ? O5 Co2 O6 89.1(2) 6 6 ? O5 Co2 O6 90.9(2) . 6 ? O8 Co2 O6 88.22(19) . 6 ? O7 Co2 O6 91.78(19) . 6 ? O6 Co2 O6 176.4(4) . 6 ? C1 N1 N2 109.0(5) . . ? C8 N2 N1 118.6(5) . . ? C8 N2 Co1 126.4(5) . . ? N1 N2 Co1 114.7(4) . . ? C23 N3 N4 108.1(6) . . ? C30 N4 N3 118.2(6) . . ? C30 N4 Co1 125.8(5) . . ? N3 N4 Co1 115.9(5) . . ? C45 N5 C46 116.5(8) . . ? C45 N5 C47 126.0(7) . . ? C46 N5 C47 117.4(6) . . ? C48 N6 C50 118.5(8) . . ? C48 N6 C49 119.5(8) . . ? C50 N6 C49 122.0(9) . . ? C1 O1 Co1 109.0(4) . . ? C10 O2 Co1 126.9(4) . . ? C23 O3 Co1 109.6(5) . . ? C32 O4 Co1 125.8(4) . . ? C45 O5 Co2 130.8(5) . . ? C48 O6 Co2 121.1(6) . . ? C51 O7 C51 91(2) . 6 ? C51 O7 Co2 134.5(12) . . ? C51 O7 Co2 134.5(12) 6 . ? C51 O7 H7 113.2 . . ? C51 O7 H7 23.6 6 . ? Co2 O7 H7 111.9 . . ? Co2 O8 H8A 114.0 . . ? Co2 O8 H8B 114.1 . . ? H8A O8 H8B 110.9 . . ? N1 C1 O1 124.1(6) . . ? N1 C1 C2 119.5(6) . . ? O1 C1 C2 116.4(6) . . ? C7 C2 C3 119.6(6) . . ? C7 C2 C1 121.8(6) . . ? C3 C2 C1 118.5(6) . . ? C2 C3 C4 117.0(7) . . ? C2 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? C5 C4 C3 120.9(8) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 121.4(8) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 118.2(8) . . ? C5 C6 H6 120.9 . . ? C7 C6 H6 120.9 . . ? C6 C7 C2 122.8(7) . . ? C6 C7 H7A 118.6 . . ? C2 C7 H7A 118.6 . . ? N2 C8 C9 125.5(6) . . ? N2 C8 H8 117.3 . . ? C9 C8 H8 117.3 . . ? C14 C9 C10 121.3(7) . . ? C14 C9 C8 117.5(6) . . ? C10 C9 C8 121.2(6) . . ? O2 C10 C9 123.4(6) . . ? O2 C10 C11 119.8(6) . . ? C9 C10 C11 116.9(7) . . ? C12 C11 C10 117.4(7) . . ? C12 C11 C15 122.3(7) . . ? C10 C11 C15 120.1(7) . . ? C13 C12 C11 126.2(7) . . ? C13 C12 H12 116.9 . . ? C11 C12 H12 116.9 . . ? C14 C13 C12 115.3(7) . . ? C14 C13 C19 121.3(7) . . ? C12 C13 C19 123.4(7) . . ? C13 C14 C9 123.0(7) . . ? C13 C14 H14 118.5 . . ? C9 C14 H14 118.5 . . ? C16 C15 C11 110.8(7) . . ? C16 C15 C17 111.1(9) . . ? C11 C15 C17 108.1(8) . . ? C16 C15 C18 108.9(9) . . ? C11 C15 C18 111.3(7) . . ? C17 C15 C18 106.6(8) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 112.4(12) . . ? C20 C19 C21 107.4(11) . . ? C22 C19 C21 102.7(11) . . ? C20 C19 C13 109.6(8) . . ? C22 C19 C13 112.2(9) . . ? C21 C19 C13 112.3(8) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 N3 124.0(7) . . ? O3 C23 C24 119.5(7) . . ? N3 C23 C24 116.5(6) . . ? C25 C24 C29 117.1(8) . . ? C25 C24 C23 122.5(8) . . ? C29 C24 C23 120.2(7) . . ? C24 C25 C26 118.4(10) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C25 C26 C27 122.2(9) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C28 C27 C26 118.9(10) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 120.1(10) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C24 123.1(9) . . ? C28 C29 H29 118.4 . . ? C24 C29 H29 118.4 . . ? N4 C30 C31 125.2(7) . . ? N4 C30 H30 117.4 . . ? C31 C30 H30 117.4 . . ? C36 C31 C30 118.0(7) . . ? C36 C31 C32 120.6(7) . . ? C30 C31 C32 121.3(6) . . ? O4 C32 C33 119.3(6) . . ? O4 C32 C31 124.4(6) . . ? C33 C32 C31 116.3(6) . . ? C34 C33 C32 119.1(7) . . ? C34 C33 C37 122.2(7) . . ? C32 C33 C37 118.7(6) . . ? C33 C34 C35 124.7(7) . . ? C33 C34 H34 117.6 . . ? C35 C34 H34 117.6 . . ? C36 C35 C34 115.1(7) . . ? C36 C35 C41 122.5(7) . . ? C34 C35 C41 122.3(7) . . ? C31 C36 C35 124.1(7) . . ? C31 C36 H36 117.9 . . ? C35 C36 H36 117.9 . . ? C33 C37 C39 111.4(7) . . ? C33 C37 C40 111.1(7) . . ? C39 C37 C40 107.6(7) . . ? C33 C37 C38 109.4(7) . . ? C39 C37 C38 110.3(7) . . ? C40 C37 C38 106.9(8) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C44 105.3(11) . . ? C43 C41 C42 112.5(11) . . ? C44 C41 C42 101.8(11) . . ? C43 C41 C35 114.1(8) . . ? C44 C41 C35 113.5(8) . . ? C42 C41 C35 109.1(8) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O5 C45 N5 126.5(8) . . ? O5 C45 H45 116.7 . . ? N5 C45 H45 116.7 . . ? N5 C46 H46A 109.5 . . ? N5 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N5 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N5 C47 H47A 109.5 . . ? N5 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O6 C48 N6 122.0(9) . . ? O6 C48 H48 119.0 . . ? N6 C48 H48 119.0 . . ? N6 C49 H49A 109.5 . . ? N6 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N6 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N6 C50 H50A 109.5 . . ? N6 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N6 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O7 C51 C52 119(2) . . ? O7 C51 C51 44.5(12) . 6 ? C52 C51 C51 74.3(14) . 6 ? O7 C51 H51A 107.2 . . ? C52 C51 H51A 106.9 . . ? C51 C51 H51A 122.4 6 . ? O7 C51 H51B 107.8 . . ? C52 C51 H51B 108.5 . . ? C51 C51 H51B 127.5 6 . ? H51A C51 H51B 107.2 . . ? C52 C52 C51 105.5(15) 6 . ? C52 C52 H52A 90.4 6 . ? C51 C52 H52A 110.5 . . ? C52 C52 H52B 130.0 6 . ? C51 C52 H52B 109.1 . . ? H52A C52 H52B 109.5 . . ? C52 C52 H52C 23.0 6 . ? C51 C52 H52C 108.9 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 N2 C8 170.4(6) . . . . ? C1 N1 N2 Co1 -3.7(6) . . . . ? O2 Co1 N2 C8 5.6(6) . . . . ? N4 Co1 N2 C8 148(3) . . . . ? O4 Co1 N2 C8 -84.7(6) . . . . ? O1 Co1 N2 C8 -173.8(6) . . . . ? O3 Co1 N2 C8 95.7(6) . . . . ? O2 Co1 N2 N1 179.2(4) . . . . ? N4 Co1 N2 N1 -38(3) . . . . ? O4 Co1 N2 N1 88.9(4) . . . . ? O1 Co1 N2 N1 -0.3(4) . . . . ? O3 Co1 N2 N1 -90.8(4) . . . . ? C23 N3 N4 C30 -170.2(6) . . . . ? C23 N3 N4 Co1 8.0(7) . . . . ? O2 Co1 N4 C30 -101.7(6) . . . . ? O4 Co1 N4 C30 -11.2(6) . . . . ? N2 Co1 N4 C30 116(3) . . . . ? O1 Co1 N4 C30 78.0(6) . . . . ? O3 Co1 N4 C30 168.7(6) . . . . ? O2 Co1 N4 N3 80.3(4) . . . . ? O4 Co1 N4 N3 170.8(4) . . . . ? N2 Co1 N4 N3 -62(3) . . . . ? O1 Co1 N4 N3 -100.0(4) . . . . ? O3 Co1 N4 N3 -9.3(4) . . . . ? O2 Co1 O1 C1 -6(4) . . . . ? N4 Co1 O1 C1 -179.0(4) . . . . ? O4 Co1 O1 C1 -83.8(4) . . . . ? N2 Co1 O1 C1 4.2(4) . . . . ? O3 Co1 O1 C1 99.5(4) . . . . ? N4 Co1 O2 C10 166.6(5) . . . . ? O4 Co1 O2 C10 71.3(5) . . . . ? N2 Co1 O2 C10 -16.6(5) . . . . ? O1 Co1 O2 C10 -7(4) . . . . ? O3 Co1 O2 C10 -112.0(5) . . . . ? O2 Co1 O3 C23 -81.5(4) . . . . ? N4 Co1 O3 C23 8.4(4) . . . . ? O4 Co1 O3 C23 10(4) . . . . ? N2 Co1 O3 C23 -175.7(4) . . . . ? O1 Co1 O3 C23 101.5(4) . . . . ? O2 Co1 O4 C32 106.4(5) . . . . ? N4 Co1 O4 C32 16.5(5) . . . . ? N2 Co1 O4 C32 -159.4(5) . . . . ? O1 Co1 O4 C32 -76.7(5) . . . . ? O3 Co1 O4 C32 15(4) . . . . ? O5 Co2 O5 C45 -83.4(8) 6 . . . ? O8 Co2 O5 C45 96.6(8) . . . . ? O7 Co2 O5 C45 -83.4(8) . . . . ? O6 Co2 O5 C45 -175.2(8) . . . . ? O6 Co2 O5 C45 8.4(8) 6 . . . ? O5 Co2 O6 C48 152.6(7) 6 . . . ? O5 Co2 O6 C48 -29.2(7) . . . . ? O8 Co2 O6 C48 61.7(7) . . . . ? O7 Co2 O6 C48 -118.3(7) . . . . ? O6 Co2 O6 C48 61.7(7) 6 . . . ? O5 Co2 O7 C51 79.9(12) 6 . . . ? O5 Co2 O7 C51 -100.1(12) . . . . ? O8 Co2 O7 C51 6.9(12) . . . . ? O6 Co2 O7 C51 -11.0(12) . . . . ? O6 Co2 O7 C51 169.0(12) 6 . . . ? O5 Co2 O7 C51 -100.1(12) 6 . . 6 ? O5 Co2 O7 C51 79.9(12) . . . 6 ? O8 Co2 O7 C51 -173.1(12) . . . 6 ? O6 Co2 O7 C51 169.0(12) . . . 6 ? O6 Co2 O7 C51 -11.0(12) 6 . . 6 ? N2 N1 C1 O1 8.3(8) . . . . ? N2 N1 C1 C2 -169.5(5) . . . . ? Co1 O1 C1 N1 -8.5(8) . . . . ? Co1 O1 C1 C2 169.3(4) . . . . ? N1 C1 C2 C7 -167.1(7) . . . . ? O1 C1 C2 C7 15.0(10) . . . . ? N1 C1 C2 C3 16.3(9) . . . . ? O1 C1 C2 C3 -161.7(6) . . . . ? C7 C2 C3 C4 0.8(11) . . . . ? C1 C2 C3 C4 177.6(7) . . . . ? C2 C3 C4 C5 -1.1(13) . . . . ? C3 C4 C5 C6 -1.7(14) . . . . ? C4 C5 C6 C7 4.6(14) . . . . ? C5 C6 C7 C2 -5.0(13) . . . . ? C3 C2 C7 C6 2.3(12) . . . . ? C1 C2 C7 C6 -174.4(7) . . . . ? N1 N2 C8 C9 -170.5(6) . . . . ? Co1 N2 C8 C9 2.8(10) . . . . ? N2 C8 C9 C14 172.8(7) . . . . ? N2 C8 C9 C10 -4.2(11) . . . . ? Co1 O2 C10 C9 19.3(9) . . . . ? Co1 O2 C10 C11 -162.5(5) . . . . ? C14 C9 C10 O2 175.8(6) . . . . ? C8 C9 C10 O2 -7.2(10) . . . . ? C14 C9 C10 C11 -2.5(10) . . . . ? C8 C9 C10 C11 174.5(7) . . . . ? O2 C10 C11 C12 -177.3(7) . . . . ? C9 C10 C11 C12 1.0(10) . . . . ? O2 C10 C11 C15 8.4(11) . . . . ? C9 C10 C11 C15 -173.2(7) . . . . ? C10 C11 C12 C13 1.5(13) . . . . ? C15 C11 C12 C13 175.6(9) . . . . ? C11 C12 C13 C14 -2.5(13) . . . . ? C11 C12 C13 C19 176.0(8) . . . . ? C12 C13 C14 C9 1.0(12) . . . . ? C19 C13 C14 C9 -177.6(7) . . . . ? C10 C9 C14 C13 1.5(11) . . . . ? C8 C9 C14 C13 -175.6(7) . . . . ? C12 C11 C15 C16 -116.5(9) . . . . ? C10 C11 C15 C16 57.5(10) . . . . ? C12 C11 C15 C17 121.6(9) . . . . ? C10 C11 C15 C17 -64.4(10) . . . . ? C12 C11 C15 C18 4.7(13) . . . . ? C10 C11 C15 C18 178.7(8) . . . . ? C14 C13 C19 C20 -49.1(14) . . . . ? C12 C13 C19 C20 132.6(12) . . . . ? C14 C13 C19 C22 76.6(12) . . . . ? C12 C13 C19 C22 -101.8(12) . . . . ? C14 C13 C19 C21 -168.3(10) . . . . ? C12 C13 C19 C21 13.3(14) . . . . ? Co1 O3 C23 N3 -6.9(8) . . . . ? Co1 O3 C23 C24 175.0(5) . . . . ? N4 N3 C23 O3 -0.3(9) . . . . ? N4 N3 C23 C24 177.8(6) . . . . ? O3 C23 C24 C25 -172.8(7) . . . . ? N3 C23 C24 C25 8.9(11) . . . . ? O3 C23 C24 C29 4.1(11) . . . . ? N3 C23 C24 C29 -174.1(7) . . . . ? C29 C24 C25 C26 0.3(13) . . . . ? C23 C24 C25 C26 177.3(9) . . . . ? C24 C25 C26 C27 -2.2(17) . . . . ? C25 C26 C27 C28 2.9(19) . . . . ? C26 C27 C28 C29 -1.6(18) . . . . ? C27 C28 C29 C24 -0.3(16) . . . . ? C25 C24 C29 C28 1.0(14) . . . . ? C23 C24 C29 C28 -176.1(8) . . . . ? N3 N4 C30 C31 -179.4(6) . . . . ? Co1 N4 C30 C31 2.7(10) . . . . ? N4 C30 C31 C36 -175.4(7) . . . . ? N4 C30 C31 C32 5.5(11) . . . . ? Co1 O4 C32 C33 167.7(5) . . . . ? Co1 O4 C32 C31 -13.3(9) . . . . ? C36 C31 C32 O4 -178.9(7) . . . . ? C30 C31 C32 O4 0.1(10) . . . . ? C36 C31 C32 C33 0.1(10) . . . . ? C30 C31 C32 C33 179.2(6) . . . . ? O4 C32 C33 C34 179.2(7) . . . . ? C31 C32 C33 C34 0.1(10) . . . . ? O4 C32 C33 C37 0.8(10) . . . . ? C31 C32 C33 C37 -178.3(7) . . . . ? C32 C33 C34 C35 0.0(12) . . . . ? C37 C33 C34 C35 178.4(8) . . . . ? C33 C34 C35 C36 -0.3(12) . . . . ? C33 C34 C35 C41 178.4(8) . . . . ? C30 C31 C36 C35 -179.6(7) . . . . ? C32 C31 C36 C35 -0.5(12) . . . . ? C34 C35 C36 C31 0.6(12) . . . . ? C41 C35 C36 C31 -178.2(8) . . . . ? C34 C33 C37 C39 121.6(9) . . . . ? C32 C33 C37 C39 -60.0(10) . . . . ? C34 C33 C37 C40 1.6(12) . . . . ? C32 C33 C37 C40 180.0(8) . . . . ? C34 C33 C37 C38 -116.2(8) . . . . ? C32 C33 C37 C38 62.2(9) . . . . ? C36 C35 C41 C43 -168.2(12) . . . . ? C34 C35 C41 C43 13.2(15) . . . . ? C36 C35 C41 C44 -47.6(14) . . . . ? C34 C35 C41 C44 133.8(11) . . . . ? C36 C35 C41 C42 65.1(12) . . . . ? C34 C35 C41 C42 -113.5(11) . . . . ? Co2 O5 C45 N5 179.2(6) . . . . ? C46 N5 C45 O5 0.0(12) . . . . ? C47 N5 C45 O5 177.1(8) . . . . ? Co2 O6 C48 N6 -160.4(6) . . . . ? C50 N6 C48 O6 -179.7(8) . . . . ? C49 N6 C48 O6 2.7(15) . . . . ? C51 O7 C51 C52 2.0(13) 6 . . . ? Co2 O7 C51 C52 -178.0(13) . . . . ? Co2 O7 C51 C51 180.0 . . . 6 ? O7 C51 C52 C52 -6(4) . . . 6 ? C51 C51 C52 C52 -5(3) 6 . . 6 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.822 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.088 #=================================END data_2 _database_code_depnum_ccdc_archive 'CCDC 727400' #TrackingRef '- crystal data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H32 Cu N2 O5' _chemical_formula_weight 480.05 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8520(8) _cell_length_b 9.5110(10) _cell_length_c 19.477(2) _cell_angle_alpha 99.223(2) _cell_angle_beta 93.968(2) _cell_angle_gamma 105.547(3) _cell_volume 1198.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2247 _cell_measurement_theta_min 2.315 _cell_measurement_theta_max 25.766 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 506 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6493 _exptl_absorpt_correction_T_max 0.7211 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6236 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4125 _reflns_number_gt 3029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.1032P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4125 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _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 Cu1 Cu 0.56979(8) 0.23803(5) 0.58054(3) 0.0347(2) Uani 1 1 d . . . N1 N 0.7496(5) 0.4942(4) 0.53011(17) 0.0312(8) Uani 1 1 d . . . N2 N 0.7092(5) 0.4432(4) 0.59193(17) 0.0303(8) Uani 1 1 d . . . O1 O 0.5930(4) 0.2483(3) 0.48197(14) 0.0358(7) Uani 1 1 d . . . O2 O 0.8351(5) 0.6838(3) 0.44983(16) 0.0460(8) Uani 1 1 d . . . H2 H 0.8148 0.6541 0.4867 0.069 Uiso 1 1 calc R . . O3 O 0.5809(5) 0.2386(3) 0.67597(14) 0.0415(8) Uani 1 1 d . . . O4 O 0.3695(4) 0.0382(3) 0.56057(15) 0.0385(7) Uani 1 1 d . . . H4A H 0.4310 -0.0282 0.5614 0.046 Uiso 1 1 d R . . H4B H 0.3039 0.0233 0.5202 0.046 Uiso 1 1 d R . . O5 O 0.8519(5) 0.0631(4) 0.56382(18) 0.0658(10) Uani 1 1 d . . . H5 H 0.9558 0.0964 0.5462 0.079 Uiso 1 1 d R . . C1 C 0.6844(6) 0.3835(4) 0.4762(2) 0.0298(9) Uani 1 1 d . . . C2 C 0.7158(6) 0.4192(4) 0.4059(2) 0.0311(9) Uani 1 1 d . . . C3 C 0.7883(6) 0.5661(5) 0.3959(2) 0.0326(9) Uani 1 1 d . . . C4 C 0.8103(7) 0.5955(5) 0.3289(2) 0.0419(11) Uani 1 1 d . . . H4 H 0.8571 0.6932 0.3225 0.050 Uiso 1 1 calc R . . C5 C 0.7639(7) 0.4818(5) 0.2721(2) 0.0473(12) Uani 1 1 d . . . H5A H 0.7803 0.5024 0.2274 0.057 Uiso 1 1 calc R . . C6 C 0.6933(8) 0.3379(5) 0.2811(2) 0.0492(12) Uani 1 1 d . . . H6 H 0.6609 0.2609 0.2425 0.059 Uiso 1 1 calc R . . C7 C 0.6701(7) 0.3070(5) 0.3473(2) 0.0427(11) Uani 1 1 d . . . H7 H 0.6227 0.2087 0.3527 0.051 Uiso 1 1 calc R . . C8 C 0.7658(6) 0.5368(4) 0.6503(2) 0.0326(9) Uani 1 1 d . . . H8 H 0.8313 0.6351 0.6485 0.039 Uiso 1 1 calc R . . C9 C 0.7342(6) 0.4991(4) 0.7176(2) 0.0332(9) Uani 1 1 d . . . C10 C 0.6451(6) 0.3527(4) 0.7277(2) 0.0323(9) Uani 1 1 d . . . C11 C 0.6218(7) 0.3281(5) 0.7972(2) 0.0380(10) Uani 1 1 d . . . C12 C 0.6921(7) 0.4498(5) 0.8516(2) 0.0463(12) Uani 1 1 d . . . H12 H 0.6772 0.4332 0.8970 0.056 Uiso 1 1 calc R . . C13 C 0.7835(7) 0.5955(5) 0.8432(2) 0.0441(11) Uani 1 1 d . . . C14 C 0.8027(7) 0.6178(5) 0.7763(2) 0.0383(10) Uani 1 1 d . . . H14 H 0.8621 0.7133 0.7688 0.046 Uiso 1 1 calc R . . C15 C 0.5296(8) 0.1714(5) 0.8111(2) 0.0492(13) Uani 1 1 d . . . C16 C 0.3119(8) 0.1077(6) 0.7735(3) 0.0655(16) Uani 1 1 d . . . H16A H 0.2306 0.1715 0.7896 0.098 Uiso 1 1 calc R . . H16B H 0.2535 0.0104 0.7834 0.098 Uiso 1 1 calc R . . H16C H 0.3151 0.1011 0.7239 0.098 Uiso 1 1 calc R . . C17 C 0.6601(10) 0.0725(6) 0.7851(3) 0.0718(17) Uani 1 1 d . . . H17A H 0.6663 0.0692 0.7358 0.108 Uiso 1 1 calc R . . H17B H 0.6013 -0.0260 0.7934 0.108 Uiso 1 1 calc R . . H17C H 0.7953 0.1116 0.8096 0.108 Uiso 1 1 calc R . . C18 C 0.5171(11) 0.1698(7) 0.8890(3) 0.083(2) Uani 1 1 d . . . H18A H 0.6516 0.2080 0.9141 0.124 Uiso 1 1 calc R . . H18B H 0.4585 0.0698 0.8954 0.124 Uiso 1 1 calc R . . H18C H 0.4333 0.2307 0.9064 0.124 Uiso 1 1 calc R . . C19 C 0.8530(10) 0.7204(6) 0.9071(3) 0.0649(16) Uani 1 1 d . . . C20 C 0.9253(18) 0.6764(8) 0.9687(4) 0.155(5) Uani 1 1 d . . . H20A H 0.8306 0.5863 0.9754 0.232 Uiso 1 1 calc R . . H20B H 0.9374 0.7532 1.0086 0.232 Uiso 1 1 calc R . . H20C H 1.0562 0.6601 0.9634 0.232 Uiso 1 1 calc R . . C21 C 0.6489(15) 0.7633(9) 0.9283(4) 0.135(4) Uani 1 1 d . . . H21A H 0.5617 0.6827 0.9455 0.202 Uiso 1 1 calc R . . H21B H 0.5783 0.7817 0.8879 0.202 Uiso 1 1 calc R . . H21C H 0.6859 0.8510 0.9641 0.202 Uiso 1 1 calc R . . C22 C 0.9772(15) 0.8614(7) 0.8903(4) 0.118(3) Uani 1 1 d . . . H22A H 1.0025 0.9389 0.9308 0.177 Uiso 1 1 calc R . . H22B H 0.9049 0.8872 0.8525 0.177 Uiso 1 1 calc R . . H22C H 1.1047 0.8494 0.8768 0.177 Uiso 1 1 calc R . . C23 C 0.8883(9) -0.0320(7) 0.6080(3) 0.0742(18) Uani 1 1 d . . . H23A H 1.0029 -0.0660 0.5950 0.111 Uiso 1 1 calc R . . H23B H 0.7699 -0.1157 0.6036 0.111 Uiso 1 1 calc R . . H23C H 0.9171 0.0204 0.6556 0.111 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0435(4) 0.0285(3) 0.0284(3) 0.0058(2) 0.0081(2) 0.0026(2) N1 0.035(2) 0.0314(18) 0.0263(18) 0.0089(15) 0.0057(15) 0.0057(15) N2 0.0329(19) 0.0293(18) 0.0284(19) 0.0077(15) 0.0066(15) 0.0059(15) O1 0.0461(18) 0.0260(15) 0.0308(16) 0.0069(12) 0.0075(13) 0.0010(13) O2 0.067(2) 0.0321(16) 0.0353(17) 0.0109(14) 0.0107(15) 0.0038(15) O3 0.061(2) 0.0302(16) 0.0283(16) 0.0061(13) 0.0075(14) 0.0034(15) O4 0.0424(18) 0.0360(16) 0.0338(16) 0.0064(13) 0.0034(13) 0.0060(14) O5 0.052(2) 0.078(3) 0.050(2) 0.0132(19) -0.0022(17) -0.0091(19) C1 0.028(2) 0.030(2) 0.032(2) 0.0075(18) 0.0019(17) 0.0078(18) C2 0.025(2) 0.037(2) 0.032(2) 0.0119(19) 0.0011(17) 0.0084(18) C3 0.028(2) 0.036(2) 0.032(2) 0.0069(18) 0.0001(18) 0.0085(18) C4 0.046(3) 0.041(3) 0.041(3) 0.018(2) 0.007(2) 0.010(2) C5 0.050(3) 0.060(3) 0.032(3) 0.016(2) 0.005(2) 0.011(2) C6 0.061(3) 0.051(3) 0.031(3) 0.002(2) 0.003(2) 0.011(3) C7 0.052(3) 0.035(2) 0.038(3) 0.008(2) 0.003(2) 0.007(2) C8 0.031(2) 0.028(2) 0.036(2) 0.0070(18) 0.0029(18) 0.0033(18) C9 0.034(2) 0.033(2) 0.031(2) 0.0054(18) 0.0027(18) 0.0059(18) C10 0.032(2) 0.033(2) 0.031(2) 0.0057(18) 0.0031(18) 0.0075(19) C11 0.041(3) 0.038(2) 0.031(2) 0.0081(19) 0.0031(19) 0.004(2) C12 0.058(3) 0.047(3) 0.028(2) 0.008(2) 0.007(2) 0.004(2) C13 0.053(3) 0.043(3) 0.031(2) 0.003(2) 0.001(2) 0.010(2) C14 0.041(3) 0.031(2) 0.038(3) 0.0050(19) 0.005(2) 0.0039(19) C15 0.062(3) 0.044(3) 0.032(3) 0.012(2) 0.001(2) -0.004(2) C16 0.061(4) 0.062(3) 0.062(4) 0.024(3) 0.006(3) -0.009(3) C17 0.095(5) 0.046(3) 0.077(4) 0.023(3) 0.000(3) 0.020(3) C18 0.120(6) 0.065(4) 0.046(3) 0.026(3) 0.005(3) -0.010(4) C19 0.103(5) 0.043(3) 0.034(3) -0.002(2) 0.003(3) 0.003(3) C20 0.280(13) 0.075(5) 0.077(5) -0.010(4) -0.089(7) 0.036(7) C21 0.164(9) 0.120(7) 0.092(6) -0.037(5) 0.036(6) 0.020(6) C22 0.188(9) 0.062(4) 0.062(4) -0.010(3) 0.005(5) -0.021(5) C23 0.054(4) 0.103(5) 0.056(4) 0.024(3) 0.004(3) 0.002(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 Cu1 O3 1.854(3) . ? Cu1 N2 1.898(3) . ? Cu1 O1 1.953(3) . ? Cu1 O4 1.984(3) . ? Cu1 O5 2.872(4) . ? N1 C1 1.319(5) . ? N1 N2 1.387(4) . ? N2 C8 1.290(5) . ? O1 C1 1.297(5) . ? O2 C3 1.357(5) . ? O2 H2 0.8200 . ? O3 C10 1.311(5) . ? O4 H4A 0.8500 . ? O4 H4B 0.8500 . ? O5 C23 1.401(6) . ? O5 H5 0.8200 . ? C1 C2 1.479(5) . ? C2 C7 1.386(6) . ? C2 C3 1.402(6) . ? C3 C4 1.389(6) . ? C4 C5 1.371(6) . ? C4 H4 0.9300 . ? C5 C6 1.367(6) . ? C5 H5A 0.9300 . ? C6 C7 1.378(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.428(6) . ? C8 H8 0.9300 . ? C9 C10 1.413(6) . ? C9 C14 1.426(6) . ? C10 C11 1.423(6) . ? C11 C12 1.390(6) . ? C11 C15 1.530(6) . ? C12 C13 1.400(6) . ? C12 H12 0.9300 . ? C13 C14 1.363(6) . ? C13 C19 1.525(7) . ? C14 H14 0.9300 . ? C15 C17 1.517(8) . ? C15 C18 1.528(7) . ? C15 C16 1.533(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.432(9) . ? C19 C22 1.482(8) . ? C19 C21 1.620(11) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 N2 94.10(13) . . ? O3 Cu1 O1 173.21(13) . . ? N2 Cu1 O1 81.78(12) . . ? O3 Cu1 O4 90.80(12) . . ? N2 Cu1 O4 166.71(13) . . ? O1 Cu1 O4 94.40(11) . . ? O3 Cu1 O5 92.01(12) . . ? N2 Cu1 O5 110.46(12) . . ? O1 Cu1 O5 84.44(11) . . ? O4 Cu1 O5 81.66(11) . . ? C1 N1 N2 110.0(3) . . ? C8 N2 N1 118.5(3) . . ? C8 N2 Cu1 126.6(3) . . ? N1 N2 Cu1 114.9(2) . . ? C1 O1 Cu1 109.6(2) . . ? C3 O2 H2 109.5 . . ? C10 O3 Cu1 128.2(3) . . ? Cu1 O4 H4A 110.0 . . ? Cu1 O4 H4B 109.9 . . ? H4A O4 H4B 108.5 . . ? C23 O5 Cu1 125.9(3) . . ? C23 O5 H5 109.5 . . ? Cu1 O5 H5 117.9 . . ? O1 C1 N1 123.6(4) . . ? O1 C1 C2 119.4(4) . . ? N1 C1 C2 117.0(4) . . ? C7 C2 C3 117.9(4) . . ? C7 C2 C1 120.5(4) . . ? C3 C2 C1 121.6(4) . . ? O2 C3 C4 117.6(4) . . ? O2 C3 C2 122.4(4) . . ? C4 C3 C2 120.0(4) . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.0(4) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 121.5(4) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? N2 C8 C9 124.2(4) . . ? N2 C8 H8 117.9 . . ? C9 C8 H8 117.9 . . ? C10 C9 C14 120.1(4) . . ? C10 C9 C8 123.4(4) . . ? C14 C9 C8 116.5(4) . . ? O3 C10 C9 123.1(4) . . ? O3 C10 C11 118.3(4) . . ? C9 C10 C11 118.6(4) . . ? C12 C11 C10 117.7(4) . . ? C12 C11 C15 121.6(4) . . ? C10 C11 C15 120.6(4) . . ? C11 C12 C13 125.0(4) . . ? C11 C12 H12 117.5 . . ? C13 C12 H12 117.5 . . ? C14 C13 C12 116.7(4) . . ? C14 C13 C19 123.2(4) . . ? C12 C13 C19 120.2(4) . . ? C13 C14 C9 121.9(4) . . ? C13 C14 H14 119.0 . . ? C9 C14 H14 119.0 . . ? C17 C15 C18 108.1(5) . . ? C17 C15 C11 109.6(4) . . ? C18 C15 C11 112.2(4) . . ? C17 C15 C16 109.9(5) . . ? C18 C15 C16 107.3(4) . . ? C11 C15 C16 109.8(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 116.7(7) . . ? C20 C19 C13 114.3(5) . . ? C22 C19 C13 113.0(5) . . ? C20 C19 C21 103.1(7) . . ? C22 C19 C21 101.8(6) . . ? C13 C19 C21 105.8(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 N2 C8 179.0(3) . . . . ? C1 N1 N2 Cu1 -1.8(4) . . . . ? O3 Cu1 N2 C8 -4.8(4) . . . . ? O1 Cu1 N2 C8 -179.4(4) . . . . ? O4 Cu1 N2 C8 106.6(6) . . . . ? O5 Cu1 N2 C8 -98.5(3) . . . . ? O3 Cu1 N2 N1 176.0(3) . . . . ? O1 Cu1 N2 N1 1.4(3) . . . . ? O4 Cu1 N2 N1 -72.6(6) . . . . ? O5 Cu1 N2 N1 82.3(3) . . . . ? O3 Cu1 O1 C1 -53.8(11) . . . . ? N2 Cu1 O1 C1 -0.8(3) . . . . ? O4 Cu1 O1 C1 166.4(3) . . . . ? O5 Cu1 O1 C1 -112.5(3) . . . . ? N2 Cu1 O3 C10 6.9(4) . . . . ? O1 Cu1 O3 C10 59.3(11) . . . . ? O4 Cu1 O3 C10 -160.8(4) . . . . ? O5 Cu1 O3 C10 117.5(4) . . . . ? O3 Cu1 O5 C23 24.2(4) . . . . ? N2 Cu1 O5 C23 119.3(4) . . . . ? O1 Cu1 O5 C23 -161.6(4) . . . . ? O4 Cu1 O5 C23 -66.3(4) . . . . ? Cu1 O1 C1 N1 0.0(5) . . . . ? Cu1 O1 C1 C2 -178.8(3) . . . . ? N2 N1 C1 O1 1.1(5) . . . . ? N2 N1 C1 C2 180.0(3) . . . . ? O1 C1 C2 C7 -7.5(6) . . . . ? N1 C1 C2 C7 173.6(4) . . . . ? O1 C1 C2 C3 171.2(4) . . . . ? N1 C1 C2 C3 -7.7(6) . . . . ? C7 C2 C3 O2 179.3(4) . . . . ? C1 C2 C3 O2 0.5(6) . . . . ? C7 C2 C3 C4 0.6(6) . . . . ? C1 C2 C3 C4 -178.2(4) . . . . ? O2 C3 C4 C5 -179.4(4) . . . . ? C2 C3 C4 C5 -0.7(7) . . . . ? C3 C4 C5 C6 0.6(7) . . . . ? C4 C5 C6 C7 -0.4(8) . . . . ? C5 C6 C7 C2 0.4(7) . . . . ? C3 C2 C7 C6 -0.5(7) . . . . ? C1 C2 C7 C6 178.4(4) . . . . ? N1 N2 C8 C9 -179.8(4) . . . . ? Cu1 N2 C8 C9 1.0(6) . . . . ? N2 C8 C9 C10 3.0(7) . . . . ? N2 C8 C9 C14 -178.5(4) . . . . ? Cu1 O3 C10 C9 -5.1(6) . . . . ? Cu1 O3 C10 C11 174.2(3) . . . . ? C14 C9 C10 O3 -179.4(4) . . . . ? C8 C9 C10 O3 -0.9(7) . . . . ? C14 C9 C10 C11 1.3(6) . . . . ? C8 C9 C10 C11 179.8(4) . . . . ? O3 C10 C11 C12 179.5(4) . . . . ? C9 C10 C11 C12 -1.2(6) . . . . ? O3 C10 C11 C15 1.7(6) . . . . ? C9 C10 C11 C15 -178.9(4) . . . . ? C10 C11 C12 C13 0.3(7) . . . . ? C15 C11 C12 C13 178.0(5) . . . . ? C11 C12 C13 C14 0.4(8) . . . . ? C11 C12 C13 C19 179.5(5) . . . . ? C12 C13 C14 C9 -0.3(7) . . . . ? C19 C13 C14 C9 -179.3(5) . . . . ? C10 C9 C14 C13 -0.6(7) . . . . ? C8 C9 C14 C13 -179.1(4) . . . . ? C12 C11 C15 C17 -117.3(5) . . . . ? C10 C11 C15 C17 60.4(6) . . . . ? C12 C11 C15 C18 2.7(7) . . . . ? C10 C11 C15 C18 -179.6(5) . . . . ? C12 C11 C15 C16 121.9(5) . . . . ? C10 C11 C15 C16 -60.4(6) . . . . ? C14 C13 C19 C20 -147.5(7) . . . . ? C12 C13 C19 C20 33.5(9) . . . . ? C14 C13 C19 C22 -10.9(9) . . . . ? C12 C13 C19 C22 170.2(6) . . . . ? C14 C13 C19 C21 99.7(6) . . . . ? C12 C13 C19 C21 -79.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.981 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.094 #=================================END data_5 _database_code_depnum_ccdc_archive 'CCDC 727401' #TrackingRef '- crystal data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H62 Cl Fe N4 O6' _chemical_formula_weight 858.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.801(11) _cell_length_b 13.610(12) _cell_length_c 14.805(13) _cell_angle_alpha 88.618(13) _cell_angle_beta 86.079(12) _cell_angle_gamma 88.823(12) _cell_volume 2371(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2908 _cell_measurement_theta_min 2.267 _cell_measurement_theta_max 22.489 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 914 _exptl_absorpt_coefficient_mu 0.423 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8559 _exptl_absorpt_correction_T_max 0.9630 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12409 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8212 _reflns_number_gt 4848 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. Two tert-butyl groups (C12 - C15 and C34 - C37) in the structure were both found to be disordered over two orientations. Their occupancies were freely refined against each other. Their occupancies were refined to be 84.9:15.1 for tert-butyl group C12 - C15 and 56.7:43.3 for tert-butyl group C34 - C37. Atoms C12/C12' and C34/C34' were fixed at the same position respectively, and the command EADP and EXYZ were used. All disordered parts were restrained using DFIX, SIMU and ISOR restraints. Uncoordinated methanol molecule (C46-O6) was also found to be disordered over two orientations. The occupancies were freely refined and the occupancies were refined to be 63.4:36.6. The disordered parts were restrained using SIMU and ISOR restraints. ; _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^)+(0.0264P)^2^+0.4595P] 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 8212 _refine_ls_number_parameters 616 _refine_ls_number_restraints 325 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.013 _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 Fe1 Fe 0.89378(4) 0.78106(3) 0.66946(3) 0.04276(15) Uani 1 1 d . . . Cl1 Cl 0.06941(9) 0.64212(7) 0.40140(8) 0.0915(4) Uani 1 1 d D . . N1 N 0.9301(2) 0.62918(18) 0.66256(18) 0.0451(7) Uani 1 1 d . . . N2 N 0.8793(2) 0.58419(19) 0.59374(18) 0.0538(7) Uani 1 1 d . . . H2 H 0.8842 0.5218 0.5860 0.065 Uiso 1 1 calc R . . N3 N 0.9023(2) 0.93671(17) 0.67242(16) 0.0410(6) Uani 1 1 d . . . N4 N 1.00241(19) 0.97206(17) 0.63013(16) 0.0439(6) Uani 1 1 d . . . H4 H 1.0212 1.0327 0.6319 0.053 Uiso 1 1 calc R . . O1 O 0.97035(17) 0.76883(14) 0.77703(14) 0.0483(6) Uani 1 1 d . . . O2 O 0.82005(18) 0.73433(15) 0.55364(14) 0.0532(6) Uani 1 1 d . . . O3 O 0.74560(16) 0.80453(14) 0.71870(14) 0.0484(6) Uani 1 1 d . . . O4 O 1.03368(17) 0.81742(16) 0.58785(15) 0.0580(6) Uani 1 1 d . . . O5 O 0.0346(2) 0.16615(17) 0.6639(2) 0.0866(9) Uani 1 1 d . . . H5 H 0.0035 0.2134 0.6397 0.130 Uiso 1 1 calc R . . C1 C 0.9948(3) 0.5743(2) 0.7107(2) 0.0505(9) Uani 1 1 d . . . H1 H 1.0065 0.5091 0.6944 0.061 Uiso 1 1 calc R . . C2 C 1.0493(2) 0.6072(2) 0.7868(2) 0.0455(8) Uani 1 1 d . . . C3 C 1.0335(2) 0.7037(2) 0.8187(2) 0.0431(8) Uani 1 1 d . . . C4 C 1.0839(2) 0.7282(2) 0.8993(2) 0.0449(8) Uani 1 1 d . . . C5 C 1.1473(3) 0.6564(2) 0.9408(2) 0.0517(9) Uani 1 1 d . A . H5A H 1.1812 0.6730 0.9930 0.062 Uiso 1 1 calc R . . C6 C 1.1647(3) 0.5599(2) 0.9101(2) 0.0510(9) Uani 1 1 d . . . C7 C 1.1152(3) 0.5379(2) 0.8326(2) 0.0524(9) Uani 1 1 d . A . H7 H 1.1254 0.4751 0.8096 0.063 Uiso 1 1 calc R . . C8 C 1.0649(3) 0.8313(2) 0.9379(2) 0.0526(9) Uani 1 1 d . . . C9 C 1.1060(3) 0.9097(2) 0.8686(2) 0.0667(11) Uani 1 1 d . . . H9A H 1.1861 0.9010 0.8547 0.100 Uiso 1 1 calc R . . H9B H 1.0909 0.9737 0.8932 0.100 Uiso 1 1 calc R . . H9C H 1.0666 0.9037 0.8144 0.100 Uiso 1 1 calc R . . C10 C 0.9377(3) 0.8473(3) 0.9637(2) 0.0747(12) Uani 1 1 d . . . H10A H 0.8956 0.8407 0.9110 0.112 Uiso 1 1 calc R . . H10B H 0.9250 0.9120 0.9873 0.112 Uiso 1 1 calc R . . H10C H 0.9129 0.7992 1.0089 0.112 Uiso 1 1 calc R . . C11 C 1.1298(4) 0.8438(3) 1.0227(3) 0.0925(14) Uani 1 1 d . . . H11A H 1.1034 0.7971 1.0686 0.139 Uiso 1 1 calc R . . H11B H 1.1171 0.9092 1.0446 0.139 Uiso 1 1 calc R . . H11C H 1.2095 0.8329 1.0081 0.139 Uiso 1 1 calc R . . C12 C 1.2318(3) 0.4853(3) 0.9643(3) 0.0608(10) Uani 0.849(10) 1 d PD A 1 C13 C 1.2450(7) 0.3863(4) 0.9162(5) 0.103(2) Uani 0.849(10) 1 d PDU A 1 H13A H 1.1712 0.3611 0.9074 0.155 Uiso 0.849(10) 1 calc PR A 1 H13B H 1.2858 0.3403 0.9527 0.155 Uiso 0.849(10) 1 calc PR A 1 H13C H 1.2861 0.3956 0.8585 0.155 Uiso 0.849(10) 1 calc PR A 1 C14 C 1.1642(5) 0.4627(5) 1.0537(4) 0.0820(19) Uani 0.849(10) 1 d PDU A 1 H14A H 1.1584 0.5207 1.0895 0.123 Uiso 0.849(10) 1 calc PR A 1 H14B H 1.2023 0.4112 1.0860 0.123 Uiso 0.849(10) 1 calc PR A 1 H14C H 1.0895 0.4420 1.0417 0.123 Uiso 0.849(10) 1 calc PR A 1 C15 C 1.3477(4) 0.5232(5) 0.9802(6) 0.097(2) Uani 0.849(10) 1 d PDU A 1 H15A H 1.3854 0.5431 0.9234 0.145 Uiso 0.849(10) 1 calc PR A 1 H15B H 1.3917 0.4721 1.0080 0.145 Uiso 0.849(10) 1 calc PR A 1 H15C H 1.3398 0.5784 1.0194 0.145 Uiso 0.849(10) 1 calc PR A 1 C12' C 1.2318(3) 0.4853(3) 0.9643(3) 0.0608(10) Uani 0.151(10) 1 d PD A 2 C15' C 1.3520(18) 0.479(3) 0.918(3) 0.090(8) Uani 0.151(10) 1 d PDU A 2 H15D H 1.3483 0.4563 0.8574 0.134 Uiso 0.151(10) 1 calc PR A 2 H15E H 1.3980 0.4346 0.9515 0.134 Uiso 0.151(10) 1 calc PR A 2 H15F H 1.3849 0.5433 0.9158 0.134 Uiso 0.151(10) 1 calc PR A 2 C14' C 1.205(4) 0.501(3) 1.0676(14) 0.104(9) Uani 0.151(10) 1 d PDU A 2 H14D H 1.2696 0.5270 1.0934 0.156 Uiso 0.151(10) 1 calc PR A 2 H14E H 1.1857 0.4389 1.0968 0.156 Uiso 0.151(10) 1 calc PR A 2 H14F H 1.1413 0.5459 1.0762 0.156 Uiso 0.151(10) 1 calc PR A 2 C13' C 1.187(3) 0.3821(17) 0.960(3) 0.103(9) Uani 0.151(10) 1 d PDU A 2 H13D H 1.1143 0.3785 0.9937 0.154 Uiso 0.151(10) 1 calc PR A 2 H13E H 1.2389 0.3361 0.9856 0.154 Uiso 0.151(10) 1 calc PR A 2 H13F H 1.1779 0.3662 0.8981 0.154 Uiso 0.151(10) 1 calc PR A 2 C16 C 0.8224(3) 0.6441(3) 0.5403(2) 0.0491(9) Uani 1 1 d . . . C17 C 0.7586(3) 0.6004(3) 0.4696(2) 0.0598(10) Uani 1 1 d . . . C18 C 0.7735(3) 0.5054(3) 0.4432(3) 0.0865(13) Uani 1 1 d . . . H18 H 0.8282 0.4657 0.4690 0.104 Uiso 1 1 calc R . . C19 C 0.7090(4) 0.4674(4) 0.3791(3) 0.0998(16) Uani 1 1 d . . . H19 H 0.7213 0.4029 0.3609 0.120 Uiso 1 1 calc R . . C20 C 0.6279(5) 0.5235(4) 0.3427(3) 0.1118(18) Uani 1 1 d . . . H20 H 0.5834 0.4974 0.3000 0.134 Uiso 1 1 calc R . . C21 C 0.6111(5) 0.6180(4) 0.3682(4) 0.149(3) Uani 1 1 d . . . H21 H 0.5545 0.6565 0.3434 0.179 Uiso 1 1 calc R . . C22 C 0.6774(4) 0.6570(3) 0.4304(3) 0.1086(17) Uani 1 1 d . . . H22 H 0.6670 0.7225 0.4461 0.130 Uiso 1 1 calc R . . C23 C 0.8341(2) 0.9978(2) 0.7144(2) 0.0445(8) Uani 1 1 d . . . H23 H 0.8571 1.0625 0.7179 0.053 Uiso 1 1 calc R . . C24 C 0.7267(2) 0.9733(2) 0.7553(2) 0.0420(8) Uani 1 1 d . . . C25 C 0.6822(2) 0.8778(2) 0.7511(2) 0.0409(8) Uani 1 1 d . . . C26 C 0.5672(3) 0.8626(2) 0.7791(2) 0.0459(8) Uani 1 1 d . . . C27 C 0.5052(3) 0.9415(2) 0.8143(2) 0.0518(9) Uani 1 1 d . B . H27 H 0.4295 0.9313 0.8332 0.062 Uiso 1 1 calc R . . C28 C 0.5478(3) 1.0357(2) 0.8236(2) 0.0503(9) Uani 1 1 d . . . C29 C 0.6580(3) 1.0499(2) 0.7925(2) 0.0502(9) Uani 1 1 d . B . H29 H 0.6885 1.1121 0.7959 0.060 Uiso 1 1 calc R . . C30 C 0.5146(3) 0.7620(2) 0.7670(2) 0.0560(9) Uani 1 1 d . . . C31 C 0.5755(3) 0.6830(3) 0.8214(3) 0.0768(12) Uani 1 1 d . . . H31A H 0.6541 0.6791 0.7999 0.115 Uiso 1 1 calc R . . H31B H 0.5410 0.6207 0.8142 0.115 Uiso 1 1 calc R . . H31C H 0.5699 0.6994 0.8843 0.115 Uiso 1 1 calc R . . C32 C 0.5228(3) 0.7372(3) 0.6666(2) 0.0741(12) Uani 1 1 d . . . H32A H 0.6012 0.7315 0.6451 0.111 Uiso 1 1 calc R . . H32B H 0.4861 0.7883 0.6328 0.111 Uiso 1 1 calc R . . H32C H 0.4860 0.6760 0.6587 0.111 Uiso 1 1 calc R . . C33 C 0.3884(3) 0.7613(3) 0.7997(3) 0.0825(13) Uani 1 1 d . . . H33A H 0.3586 0.6972 0.7915 0.124 Uiso 1 1 calc R . . H33B H 0.3474 0.8091 0.7653 0.124 Uiso 1 1 calc R . . H33C H 0.3802 0.7771 0.8627 0.124 Uiso 1 1 calc R . . C34 C 0.4709(3) 1.1201(3) 0.8592(3) 0.0644(10) Uani 0.567(13) 1 d PD B 1 C35 C 0.4401(10) 1.1839(8) 0.7804(6) 0.089(3) Uani 0.567(13) 1 d PDU B 1 H35A H 0.5082 1.2062 0.7476 0.133 Uiso 0.567(13) 1 calc PR B 1 H35B H 0.3959 1.2396 0.8019 0.133 Uiso 0.567(13) 1 calc PR B 1 H35C H 0.3967 1.1469 0.7411 0.133 Uiso 0.567(13) 1 calc PR B 1 C36 C 0.3659(9) 1.0870(9) 0.9136(9) 0.090(4) Uani 0.567(13) 1 d PDU B 1 H36A H 0.3270 1.1430 0.9403 0.135 Uiso 0.567(13) 1 calc PR B 1 H36B H 0.3867 1.0416 0.9605 0.135 Uiso 0.567(13) 1 calc PR B 1 H36C H 0.3167 1.0553 0.8747 0.135 Uiso 0.567(13) 1 calc PR B 1 C37 C 0.5377(7) 1.1844(7) 0.9245(8) 0.076(3) Uani 0.567(13) 1 d PDU B 1 H37A H 0.6058 1.2080 0.8927 0.115 Uiso 0.567(13) 1 calc PR B 1 H37B H 0.5572 1.1451 0.9761 0.115 Uiso 0.567(13) 1 calc PR B 1 H37C H 0.4908 1.2393 0.9443 0.115 Uiso 0.567(13) 1 calc PR B 1 C34' C 0.4709(3) 1.1201(3) 0.8592(3) 0.0644(10) Uani 0.433(13) 1 d PD B 2 C35' C 0.3771(12) 1.1360(11) 0.7883(8) 0.094(4) Uani 0.433(13) 1 d PDU B 2 H35D H 0.3251 1.1875 0.8082 0.140 Uiso 0.433(13) 1 calc PR B 2 H35E H 0.3364 1.0763 0.7834 0.140 Uiso 0.433(13) 1 calc PR B 2 H35F H 0.4130 1.1540 0.7302 0.140 Uiso 0.433(13) 1 calc PR B 2 C36' C 0.4028(14) 1.0885(13) 0.9484(9) 0.091(5) Uani 0.433(13) 1 d PDU B 2 H36D H 0.4546 1.0706 0.9935 0.136 Uiso 0.433(13) 1 calc PR B 2 H36E H 0.3569 1.0332 0.9373 0.136 Uiso 0.433(13) 1 calc PR B 2 H36F H 0.3547 1.1422 0.9694 0.136 Uiso 0.433(13) 1 calc PR B 2 C37' C 0.5295(10) 1.2159(8) 0.8638(13) 0.093(4) Uani 0.433(13) 1 d PDU B 2 H37D H 0.5934 1.2078 0.9002 0.139 Uiso 0.433(13) 1 calc PR B 2 H37E H 0.4775 1.2640 0.8903 0.139 Uiso 0.433(13) 1 calc PR B 2 H37F H 0.5551 1.2376 0.8038 0.139 Uiso 0.433(13) 1 calc PR B 2 C38 C 1.0668(3) 0.9045(2) 0.5867(2) 0.0434(8) Uani 1 1 d . . . C39 C 1.1750(3) 0.9304(2) 0.5384(2) 0.0450(8) Uani 1 1 d . . . C40 C 1.2162(3) 1.0247(2) 0.5313(2) 0.0555(9) Uani 1 1 d . . . H40 H 1.1749 1.0760 0.5589 0.067 Uiso 1 1 calc R . . C41 C 1.3177(3) 1.0432(3) 0.4838(2) 0.0654(10) Uani 1 1 d . . . H41 H 1.3449 1.1069 0.4796 0.078 Uiso 1 1 calc R . . C42 C 1.3788(3) 0.9686(3) 0.4427(2) 0.0642(10) Uani 1 1 d . . . H42 H 1.4477 0.9815 0.4108 0.077 Uiso 1 1 calc R . . C43 C 1.3390(3) 0.8745(3) 0.4485(2) 0.0700(11) Uani 1 1 d . . . H43 H 1.3807 0.8237 0.4205 0.084 Uiso 1 1 calc R . . C44 C 1.2371(3) 0.8557(3) 0.4960(2) 0.0612(10) Uani 1 1 d . . . H44 H 1.2099 0.7920 0.4996 0.073 Uiso 1 1 calc R . . C45 C 0.0885(5) 0.1970(4) 0.7370(4) 0.151(2) Uani 1 1 d . . . H45A H 0.1275 0.2569 0.7212 0.226 Uiso 1 1 calc R . . H45B H 0.1423 0.1474 0.7545 0.226 Uiso 1 1 calc R . . H45C H 0.0335 0.2084 0.7867 0.226 Uiso 1 1 calc R . . C46 C 0.3145(14) 0.5958(12) 0.2480(10) 0.147(5) Uani 0.634(18) 1 d PU C 1 H46A H 0.3706 0.6066 0.1988 0.221 Uiso 0.634(18) 1 calc PR C 1 H46B H 0.2427 0.5829 0.2243 0.221 Uiso 0.634(18) 1 calc PR C 1 H46C H 0.3374 0.5405 0.2843 0.221 Uiso 0.634(18) 1 calc PR C 1 O6 O 0.3042(8) 0.6793(6) 0.3012(8) 0.160(5) Uani 0.634(18) 1 d PU C 1 C46' C 0.335(3) 0.584(2) 0.292(2) 0.170(9) Uani 0.366(18) 1 d PU C 2 H46D H 0.4106 0.5812 0.2630 0.255 Uiso 0.366(18) 1 calc PR C 2 H46E H 0.3015 0.5207 0.2904 0.255 Uiso 0.366(18) 1 calc PR C 2 H46F H 0.3386 0.6035 0.3534 0.255 Uiso 0.366(18) 1 calc PR C 2 O6' O 0.2493(15) 0.6742(13) 0.2313(14) 0.172(8) Uani 0.366(18) 1 d PU C 2 H6 H 0.209(4) 0.696(4) 0.300(4) 0.207 Uiso 1 1 d 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 Fe1 0.0446(3) 0.0298(3) 0.0538(3) -0.0065(2) -0.0013(2) 0.00039(19) Cl1 0.0998(8) 0.0442(6) 0.1318(10) -0.0227(6) -0.0125(7) 0.0063(5) N1 0.0499(16) 0.0340(16) 0.0512(18) -0.0081(13) -0.0003(14) -0.0024(13) N2 0.073(2) 0.0318(16) 0.058(2) -0.0130(14) -0.0113(16) -0.0037(14) N3 0.0399(15) 0.0353(15) 0.0481(17) 0.0002(12) -0.0050(13) -0.0010(12) N4 0.0389(15) 0.0319(15) 0.0603(18) -0.0009(13) -0.0004(13) -0.0017(12) O1 0.0552(13) 0.0322(12) 0.0592(15) -0.0113(10) -0.0149(12) 0.0091(10) O2 0.0674(15) 0.0385(14) 0.0545(15) -0.0061(11) -0.0079(12) -0.0043(11) O3 0.0410(12) 0.0322(12) 0.0712(16) -0.0053(11) 0.0027(11) -0.0005(10) O4 0.0591(14) 0.0390(14) 0.0745(17) -0.0157(11) 0.0143(12) -0.0080(11) O5 0.092(2) 0.0401(16) 0.128(3) -0.0044(15) -0.0083(19) 0.0011(14) C1 0.056(2) 0.0309(19) 0.064(3) -0.0106(17) 0.0011(19) 0.0058(16) C2 0.0441(19) 0.037(2) 0.055(2) -0.0064(16) 0.0010(17) 0.0043(15) C3 0.0383(18) 0.038(2) 0.053(2) -0.0053(16) -0.0004(16) 0.0023(15) C4 0.0417(18) 0.041(2) 0.052(2) -0.0052(16) -0.0042(16) 0.0029(15) C5 0.048(2) 0.051(2) 0.057(2) -0.0016(18) -0.0073(17) 0.0007(17) C6 0.0416(19) 0.045(2) 0.065(3) 0.0054(18) 0.0013(18) 0.0085(16) C7 0.051(2) 0.037(2) 0.068(3) -0.0030(18) 0.0030(19) 0.0112(16) C8 0.060(2) 0.044(2) 0.055(2) -0.0113(17) -0.0126(18) 0.0063(17) C9 0.073(3) 0.043(2) 0.085(3) -0.014(2) -0.008(2) -0.0057(19) C10 0.074(3) 0.065(3) 0.083(3) -0.021(2) 0.009(2) 0.018(2) C11 0.128(4) 0.067(3) 0.087(3) -0.025(2) -0.041(3) 0.019(3) C12 0.050(2) 0.055(2) 0.076(3) 0.013(2) -0.001(2) 0.0125(18) C13 0.122(5) 0.076(4) 0.108(5) 0.015(3) -0.008(4) 0.051(3) C14 0.075(4) 0.082(4) 0.088(4) 0.033(3) -0.011(3) 0.005(3) C15 0.054(3) 0.099(4) 0.136(6) 0.049(4) -0.022(3) 0.008(3) C12' 0.050(2) 0.055(2) 0.076(3) 0.013(2) -0.001(2) 0.0125(18) C15' 0.074(10) 0.095(11) 0.100(11) 0.020(8) -0.017(8) 0.015(8) C14' 0.102(12) 0.104(12) 0.104(11) 0.013(9) -0.007(9) 0.017(9) C13' 0.102(11) 0.094(11) 0.112(11) 0.018(8) -0.015(9) 0.003(8) C16 0.055(2) 0.043(2) 0.050(2) -0.0088(18) 0.0012(18) -0.0094(17) C17 0.076(3) 0.050(2) 0.055(2) -0.0068(19) -0.007(2) -0.016(2) C18 0.091(3) 0.068(3) 0.105(4) -0.031(3) -0.033(3) -0.003(2) C19 0.117(4) 0.086(4) 0.102(4) -0.039(3) -0.028(3) -0.018(3) C20 0.160(5) 0.090(4) 0.094(4) -0.004(3) -0.063(4) -0.042(4) C21 0.235(7) 0.074(4) 0.157(5) -0.007(3) -0.141(5) -0.003(4) C22 0.169(5) 0.051(3) 0.116(4) -0.002(3) -0.080(4) -0.005(3) C23 0.0413(19) 0.0313(18) 0.062(2) -0.0058(16) -0.0062(16) -0.0023(15) C24 0.0391(18) 0.0363(19) 0.051(2) -0.0019(15) -0.0066(16) 0.0025(14) C25 0.0452(19) 0.0339(18) 0.044(2) -0.0005(15) -0.0080(16) 0.0031(15) C26 0.0393(19) 0.043(2) 0.055(2) 0.0047(16) 0.0001(16) 0.0010(15) C27 0.0405(19) 0.049(2) 0.064(2) 0.0039(18) 0.0026(17) 0.0009(16) C28 0.048(2) 0.041(2) 0.062(2) -0.0007(16) -0.0003(17) 0.0083(16) C29 0.048(2) 0.037(2) 0.066(2) -0.0059(16) -0.0029(18) 0.0010(16) C30 0.046(2) 0.044(2) 0.078(3) -0.0004(19) 0.0034(19) -0.0046(16) C31 0.079(3) 0.050(2) 0.099(3) 0.014(2) 0.005(2) -0.006(2) C32 0.068(3) 0.072(3) 0.083(3) -0.017(2) -0.001(2) -0.026(2) C33 0.059(2) 0.064(3) 0.123(4) -0.005(2) 0.016(2) -0.017(2) C34 0.054(2) 0.052(2) 0.084(3) -0.005(2) 0.011(2) 0.0147(19) C35 0.089(6) 0.073(6) 0.101(6) 0.003(4) 0.002(5) 0.038(5) C36 0.081(6) 0.077(5) 0.110(7) -0.017(6) 0.021(5) 0.013(5) C37 0.078(5) 0.061(5) 0.090(6) -0.033(4) 0.003(5) 0.015(4) C34' 0.054(2) 0.052(2) 0.084(3) -0.005(2) 0.011(2) 0.0147(19) C35' 0.082(7) 0.081(7) 0.116(7) 0.006(6) -0.008(6) 0.038(5) C36' 0.092(8) 0.086(7) 0.091(8) -0.017(6) 0.013(6) 0.030(6) C37' 0.091(6) 0.075(7) 0.111(8) -0.021(6) 0.006(6) 0.018(5) C38 0.0449(19) 0.041(2) 0.045(2) 0.0003(16) -0.0082(16) -0.0032(16) C39 0.0455(19) 0.043(2) 0.046(2) -0.0012(16) -0.0031(16) -0.0016(16) C40 0.053(2) 0.048(2) 0.065(3) -0.0035(18) 0.0015(18) -0.0039(17) C41 0.057(2) 0.066(3) 0.073(3) 0.000(2) 0.004(2) -0.017(2) C42 0.041(2) 0.079(3) 0.071(3) 0.003(2) 0.0025(18) -0.008(2) C43 0.058(2) 0.068(3) 0.081(3) -0.007(2) 0.016(2) 0.008(2) C44 0.058(2) 0.051(2) 0.074(3) -0.0039(19) 0.005(2) -0.0056(18) C45 0.200(6) 0.113(5) 0.147(6) -0.012(4) -0.055(5) -0.015(4) C46 0.150(8) 0.151(8) 0.140(8) -0.021(7) 0.003(7) -0.001(6) O6 0.152(6) 0.141(6) 0.187(8) -0.054(5) 0.029(5) -0.047(5) C46' 0.161(11) 0.170(12) 0.177(12) -0.001(9) -0.001(9) -0.010(9) O6' 0.165(10) 0.182(10) 0.164(10) 0.022(7) 0.019(7) -0.006(7) _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 Fe1 O3 1.872(2) . ? Fe1 O1 1.886(2) . ? Fe1 O4 2.040(2) . ? Fe1 O2 2.093(2) . ? Fe1 N1 2.106(3) . ? Fe1 N3 2.125(3) . ? N1 C1 1.295(4) . ? N1 N2 1.378(3) . ? N2 C16 1.327(4) . ? N2 H2 0.8600 . ? N3 C23 1.286(3) . ? N3 N4 1.388(3) . ? N4 C38 1.330(3) . ? N4 H4 0.8600 . ? O1 C3 1.315(4) . ? O2 C16 1.248(4) . ? O3 C25 1.315(3) . ? O4 C38 1.255(3) . ? O5 C45 1.372(5) . ? O5 H5 0.8200 . ? C1 C2 1.421(4) . ? C1 H1 0.9300 . ? C2 C7 1.403(4) . ? C2 C3 1.411(4) . ? C3 C4 1.419(4) . ? C4 C5 1.377(4) . ? C4 C8 1.534(4) . ? C5 C6 1.406(4) . ? C5 H5A 0.9300 . ? C6 C7 1.365(4) . ? C6 C12 1.523(5) . ? C7 H7 0.9300 . ? C8 C9 1.525(5) . ? C8 C11 1.528(4) . ? C8 C10 1.536(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C15 1.507(6) . ? C12 C14 1.526(6) . ? C12 C13 1.539(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15' H15D 0.9600 . ? C15' H15E 0.9600 . ? C15' H15F 0.9600 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C13' H13D 0.9600 . ? C13' H13E 0.9600 . ? C13' H13F 0.9600 . ? C16 C17 1.474(4) . ? C17 C18 1.364(5) . ? C17 C22 1.369(5) . ? C18 C19 1.373(5) . ? C18 H18 0.9300 . ? C19 C20 1.345(6) . ? C19 H19 0.9300 . ? C20 C21 1.357(6) . ? C20 H20 0.9300 . ? C21 C22 1.371(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.410(4) . ? C23 H23 0.9300 . ? C24 C29 1.407(4) . ? C24 C25 1.415(4) . ? C25 C26 1.410(4) . ? C26 C27 1.379(4) . ? C26 C30 1.533(4) . ? C27 C28 1.400(4) . ? C27 H27 0.9300 . ? C28 C29 1.366(4) . ? C28 C34 1.530(4) . ? C29 H29 0.9300 . ? C30 C31 1.526(5) . ? C30 C32 1.529(5) . ? C30 C33 1.535(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.498(8) . ? C34 C36 1.502(9) . ? C34 C37 1.580(8) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C35' H35D 0.9600 . ? C35' H35E 0.9600 . ? C35' H35F 0.9600 . ? C36' H36D 0.9600 . ? C36' H36E 0.9600 . ? C36' H36F 0.9600 . ? C37' H37D 0.9600 . ? C37' H37E 0.9600 . ? C37' H37F 0.9600 . ? C38 C39 1.465(4) . ? C39 C44 1.380(4) . ? C39 C40 1.381(4) . ? C40 C41 1.371(4) . ? C40 H40 0.9300 . ? C41 C42 1.364(5) . ? C41 H41 0.9300 . ? C42 C43 1.371(5) . ? C42 H42 0.9300 . ? C43 C44 1.377(4) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 O6 1.396(18) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? O6 H6 1.14(6) . ? C46' O6' 1.83(4) . ? C46' H46D 0.9600 . ? C46' H46E 0.9600 . ? C46' H46F 0.9600 . ? O6' H6 1.14(5) . ? 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 O3 Fe1 O1 99.72(10) . . ? O3 Fe1 O4 152.58(9) . . ? O1 Fe1 O4 95.70(11) . . ? O3 Fe1 O2 86.74(10) . . ? O1 Fe1 O2 157.13(9) . . ? O4 Fe1 O2 87.77(10) . . ? O3 Fe1 N1 110.95(9) . . ? O1 Fe1 N1 82.92(10) . . ? O4 Fe1 N1 93.29(9) . . ? O2 Fe1 N1 74.31(10) . . ? O3 Fe1 N3 82.86(9) . . ? O1 Fe1 N3 90.83(9) . . ? O4 Fe1 N3 74.34(9) . . ? O2 Fe1 N3 111.81(9) . . ? N1 Fe1 N3 165.58(10) . . ? C1 N1 N2 116.7(3) . . ? C1 N1 Fe1 129.7(2) . . ? N2 N1 Fe1 113.6(2) . . ? C16 N2 N1 115.2(3) . . ? C16 N2 H2 122.4 . . ? N1 N2 H2 122.4 . . ? C23 N3 N4 118.4(3) . . ? C23 N3 Fe1 128.7(2) . . ? N4 N3 Fe1 112.55(17) . . ? C38 N4 N3 114.5(2) . . ? C38 N4 H4 122.8 . . ? N3 N4 H4 122.8 . . ? C3 O1 Fe1 138.8(2) . . ? C16 O2 Fe1 116.8(2) . . ? C25 O3 Fe1 139.17(19) . . ? C38 O4 Fe1 118.7(2) . . ? C45 O5 H5 109.5 . . ? N1 C1 C2 124.2(3) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C7 C2 C3 120.8(3) . . ? C7 C2 C1 117.1(3) . . ? C3 C2 C1 122.1(3) . . ? O1 C3 C2 121.2(3) . . ? O1 C3 C4 120.4(3) . . ? C2 C3 C4 118.4(3) . . ? C5 C4 C3 117.7(3) . . ? C5 C4 C8 122.5(3) . . ? C3 C4 C8 119.8(3) . . ? C4 C5 C6 125.0(3) . . ? C4 C5 H5A 117.5 . . ? C6 C5 H5A 117.5 . . ? C7 C6 C5 116.3(3) . . ? C7 C6 C12 123.3(3) . . ? C5 C6 C12 120.3(3) . . ? C6 C7 C2 121.8(3) . . ? C6 C7 H7 119.1 . . ? C2 C7 H7 119.1 . . ? C9 C8 C11 107.5(3) . . ? C9 C8 C4 110.6(3) . . ? C11 C8 C4 111.6(3) . . ? C9 C8 C10 109.8(3) . . ? C11 C8 C10 108.3(3) . . ? C4 C8 C10 109.0(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C6 110.9(3) . . ? C15 C12 C14 111.1(4) . . ? C6 C12 C14 108.6(3) . . ? C15 C12 C13 109.4(4) . . ? C6 C12 C13 111.5(4) . . ? C14 C12 C13 105.2(4) . . ? H15D C15' H15E 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? H14D C14' H14E 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? H13D C13' H13E 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? O2 C16 N2 119.7(3) . . ? O2 C16 C17 122.1(3) . . ? N2 C16 C17 118.2(3) . . ? C18 C17 C22 118.1(4) . . ? C18 C17 C16 123.5(4) . . ? C22 C17 C16 118.3(4) . . ? C17 C18 C19 121.1(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 120.0(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 119.9(5) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 120.2(5) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C17 C22 C21 120.5(4) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? N3 C23 C24 124.4(3) . . ? N3 C23 H23 117.8 . . ? C24 C23 H23 117.8 . . ? C29 C24 C23 117.6(3) . . ? C29 C24 C25 119.8(3) . . ? C23 C24 C25 122.2(3) . . ? O3 C25 C26 119.9(3) . . ? O3 C25 C24 120.9(3) . . ? C26 C25 C24 119.2(3) . . ? C27 C26 C25 117.5(3) . . ? C27 C26 C30 122.6(3) . . ? C25 C26 C30 119.9(3) . . ? C26 C27 C28 124.9(3) . . ? C26 C27 H27 117.5 . . ? C28 C27 H27 117.5 . . ? C29 C28 C27 116.6(3) . . ? C29 C28 C34 122.0(3) . . ? C27 C28 C34 121.1(3) . . ? C28 C29 C24 121.9(3) . . ? C28 C29 H29 119.0 . . ? C24 C29 H29 119.0 . . ? C31 C30 C32 110.2(3) . . ? C31 C30 C26 110.3(3) . . ? C32 C30 C26 109.5(3) . . ? C31 C30 C33 107.6(3) . . ? C32 C30 C33 107.3(3) . . ? C26 C30 C33 111.8(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C36 110.6(6) . . ? C35 C34 C28 108.4(4) . . ? C36 C34 C28 114.0(6) . . ? C35 C34 C37 108.1(6) . . ? C36 C34 C37 106.0(6) . . ? C28 C34 C37 109.5(4) . . ? H35D C35' H35E 109.5 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? H36D C36' H36E 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? H37D C37' H37E 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? O4 C38 N4 118.9(3) . . ? O4 C38 C39 120.1(3) . . ? N4 C38 C39 121.0(3) . . ? C44 C39 C40 118.7(3) . . ? C44 C39 C38 117.3(3) . . ? C40 C39 C38 124.0(3) . . ? C41 C40 C39 120.4(3) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C42 C41 C40 120.3(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 120.2(3) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C42 C43 C44 119.7(3) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C39 120.7(3) . . ? C43 C44 H44 119.7 . . ? C39 C44 H44 119.7 . . ? O5 C45 H45A 109.5 . . ? O5 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O5 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 O6 H6 101(3) . . ? O6' C46' H46D 109.5 . . ? O6' C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? O6' C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? C46' O6' H6 87(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Fe1 N1 C1 -107.6(3) . . . . ? O1 Fe1 N1 C1 -9.8(3) . . . . ? O4 Fe1 N1 C1 85.5(3) . . . . ? O2 Fe1 N1 C1 172.3(3) . . . . ? N3 Fe1 N1 C1 55.1(6) . . . . ? O3 Fe1 N1 N2 75.1(2) . . . . ? O1 Fe1 N1 N2 172.8(2) . . . . ? O4 Fe1 N1 N2 -91.8(2) . . . . ? O2 Fe1 N1 N2 -5.09(18) . . . . ? N3 Fe1 N1 N2 -122.3(4) . . . . ? C1 N1 N2 C16 -173.8(3) . . . . ? Fe1 N1 N2 C16 3.9(3) . . . . ? O3 Fe1 N3 C23 14.0(3) . . . . ? O1 Fe1 N3 C23 -85.7(3) . . . . ? O4 Fe1 N3 C23 178.6(3) . . . . ? O2 Fe1 N3 C23 97.6(3) . . . . ? N1 Fe1 N3 C23 -149.7(4) . . . . ? O3 Fe1 N3 N4 -173.17(18) . . . . ? O1 Fe1 N3 N4 87.14(19) . . . . ? O4 Fe1 N3 N4 -8.55(17) . . . . ? O2 Fe1 N3 N4 -89.59(19) . . . . ? N1 Fe1 N3 N4 23.2(5) . . . . ? C23 N3 N4 C38 -178.6(3) . . . . ? Fe1 N3 N4 C38 7.8(3) . . . . ? O3 Fe1 O1 C3 121.4(3) . . . . ? O4 Fe1 O1 C3 -81.3(3) . . . . ? O2 Fe1 O1 C3 16.5(4) . . . . ? N1 Fe1 O1 C3 11.3(3) . . . . ? N3 Fe1 O1 C3 -155.7(3) . . . . ? O3 Fe1 O2 C16 -106.7(2) . . . . ? O1 Fe1 O2 C16 0.8(4) . . . . ? O4 Fe1 O2 C16 100.2(2) . . . . ? N1 Fe1 O2 C16 6.1(2) . . . . ? N3 Fe1 O2 C16 172.3(2) . . . . ? O1 Fe1 O3 C25 81.2(3) . . . . ? O4 Fe1 O3 C25 -42.1(4) . . . . ? O2 Fe1 O3 C25 -120.9(3) . . . . ? N1 Fe1 O3 C25 167.3(3) . . . . ? N3 Fe1 O3 C25 -8.4(3) . . . . ? O3 Fe1 O4 C38 43.9(3) . . . . ? O1 Fe1 O4 C38 -80.3(2) . . . . ? O2 Fe1 O4 C38 122.4(2) . . . . ? N1 Fe1 O4 C38 -163.5(2) . . . . ? N3 Fe1 O4 C38 9.0(2) . . . . ? N2 N1 C1 C2 -176.8(3) . . . . ? Fe1 N1 C1 C2 5.9(5) . . . . ? N1 C1 C2 C7 178.9(3) . . . . ? N1 C1 C2 C3 2.4(5) . . . . ? Fe1 O1 C3 C2 -7.6(5) . . . . ? Fe1 O1 C3 C4 174.8(2) . . . . ? C7 C2 C3 O1 -178.9(3) . . . . ? C1 C2 C3 O1 -2.6(5) . . . . ? C7 C2 C3 C4 -1.2(4) . . . . ? C1 C2 C3 C4 175.1(3) . . . . ? O1 C3 C4 C5 178.8(3) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? O1 C3 C4 C8 -0.1(4) . . . . ? C2 C3 C4 C8 -177.8(3) . . . . ? C3 C4 C5 C6 -0.9(5) . . . . ? C8 C4 C5 C6 177.9(3) . . . . ? C4 C5 C6 C7 0.8(5) . . . . ? C4 C5 C6 C12 -177.0(3) . . . . ? C5 C6 C7 C2 -0.8(5) . . . . ? C12 C6 C7 C2 176.9(3) . . . . ? C3 C2 C7 C6 1.1(5) . . . . ? C1 C2 C7 C6 -175.4(3) . . . . ? C5 C4 C8 C9 122.8(3) . . . . ? C3 C4 C8 C9 -58.3(4) . . . . ? C5 C4 C8 C11 3.2(4) . . . . ? C3 C4 C8 C11 -178.0(3) . . . . ? C5 C4 C8 C10 -116.3(3) . . . . ? C3 C4 C8 C10 62.5(4) . . . . ? C7 C6 C12 C15 127.1(5) . . . . ? C5 C6 C12 C15 -55.3(5) . . . . ? C7 C6 C12 C14 -110.5(5) . . . . ? C5 C6 C12 C14 67.1(5) . . . . ? C7 C6 C12 C13 5.0(6) . . . . ? C5 C6 C12 C13 -177.4(4) . . . . ? Fe1 O2 C16 N2 -6.3(4) . . . . ? Fe1 O2 C16 C17 170.5(2) . . . . ? N1 N2 C16 O2 1.5(4) . . . . ? N1 N2 C16 C17 -175.4(3) . . . . ? O2 C16 C17 C18 168.8(3) . . . . ? N2 C16 C17 C18 -14.4(5) . . . . ? O2 C16 C17 C22 -13.5(5) . . . . ? N2 C16 C17 C22 163.3(4) . . . . ? C22 C17 C18 C19 0.0(6) . . . . ? C16 C17 C18 C19 177.7(4) . . . . ? C17 C18 C19 C20 -1.4(7) . . . . ? C18 C19 C20 C21 1.0(9) . . . . ? C19 C20 C21 C22 0.7(9) . . . . ? C18 C17 C22 C21 1.7(7) . . . . ? C16 C17 C22 C21 -176.1(5) . . . . ? C20 C21 C22 C17 -2.1(9) . . . . ? N4 N3 C23 C24 175.9(3) . . . . ? Fe1 N3 C23 C24 -11.6(4) . . . . ? N3 C23 C24 C29 -175.1(3) . . . . ? N3 C23 C24 C25 -2.2(5) . . . . ? Fe1 O3 C25 C26 177.2(2) . . . . ? Fe1 O3 C25 C24 -0.4(5) . . . . ? C29 C24 C25 O3 -178.4(3) . . . . ? C23 C24 C25 O3 8.9(5) . . . . ? C29 C24 C25 C26 4.0(4) . . . . ? C23 C24 C25 C26 -168.7(3) . . . . ? O3 C25 C26 C27 178.7(3) . . . . ? C24 C25 C26 C27 -3.7(4) . . . . ? O3 C25 C26 C30 -3.2(4) . . . . ? C24 C25 C26 C30 174.5(3) . . . . ? C25 C26 C27 C28 0.6(5) . . . . ? C30 C26 C27 C28 -177.5(3) . . . . ? C26 C27 C28 C29 2.2(5) . . . . ? C26 C27 C28 C34 176.9(3) . . . . ? C27 C28 C29 C24 -1.9(5) . . . . ? C34 C28 C29 C24 -176.6(3) . . . . ? C23 C24 C29 C28 171.9(3) . . . . ? C25 C24 C29 C28 -1.2(5) . . . . ? C27 C26 C30 C31 -120.5(3) . . . . ? C25 C26 C30 C31 61.5(4) . . . . ? C27 C26 C30 C32 118.0(3) . . . . ? C25 C26 C30 C32 -60.0(4) . . . . ? C27 C26 C30 C33 -0.8(5) . . . . ? C25 C26 C30 C33 -178.8(3) . . . . ? C29 C28 C34 C35 72.6(7) . . . . ? C27 C28 C34 C35 -101.9(7) . . . . ? C29 C28 C34 C36 -163.8(7) . . . . ? C27 C28 C34 C36 21.8(8) . . . . ? C29 C28 C34 C37 -45.2(7) . . . . ? C27 C28 C34 C37 140.3(6) . . . . ? Fe1 O4 C38 N4 -7.8(4) . . . . ? Fe1 O4 C38 C39 172.0(2) . . . . ? N3 N4 C38 O4 -0.4(4) . . . . ? N3 N4 C38 C39 179.7(2) . . . . ? O4 C38 C39 C44 -0.5(4) . . . . ? N4 C38 C39 C44 179.3(3) . . . . ? O4 C38 C39 C40 177.9(3) . . . . ? N4 C38 C39 C40 -2.3(5) . . . . ? C44 C39 C40 C41 -0.7(5) . . . . ? C38 C39 C40 C41 -179.2(3) . . . . ? C39 C40 C41 C42 0.3(5) . . . . ? C40 C41 C42 C43 0.1(5) . . . . ? C41 C42 C43 C44 -0.1(6) . . . . ? C42 C43 C44 C39 -0.4(5) . . . . ? C40 C39 C44 C43 0.8(5) . . . . ? C38 C39 C44 C43 179.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.309 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.045 #=================================END