# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Christophe Bucher' _publ_contact_author_email christophe.bucher@ujf-grenoble.fr loop_ _publ_author_name C.H.Devillers A.Milet J.-C.Moutet J.Pecaut G.Royal ; E.Saint-Aman ; C.Bucher data_2Zn _database_code_depnum_ccdc_archive 'CCDC 893172' #TrackingRef '- 2Zn_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H42 Fe N4 S2 Zn' _chemical_formula_weight 932.26 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' S S 0.1246 0.1234 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.426(16) _cell_length_b 10.100(5) _cell_length_c 32.153(15) _cell_angle_alpha 90.00 _cell_angle_beta 112.358(8) _cell_angle_gamma 90.00 _cell_volume 10339(8) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5950 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 23.32 _exptl_crystal_description 'long block' _exptl_crystal_colour dark _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3856 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7820 _exptl_absorpt_correction_T_max 0.9188 _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 15373 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 23.32 _reflns_number_total 7295 _reflns_number_gt 5950 _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^)+(0.0425P)^2^+59.5665P] 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 7295 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1682 _refine_ls_wR_factor_gt 0.1578 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.36913(2) 0.49267(7) 0.35819(2) 0.0548(2) Uani 1 1 d . . . Fe Fe 0.18191(3) 0.57388(8) 0.19698(3) 0.0528(3) Uani 1 1 d . A . S1 S 0.10652(5) 0.22671(17) 0.10278(5) 0.0718(5) Uani 1 1 d . . . S2 S 0.06595(7) 0.4250(3) 0.14094(9) 0.1118(8) Uani 1 1 d . . . N1 N 0.31264(15) 0.4922(5) 0.36574(14) 0.0530(12) Uani 1 1 d . . . N2 N 0.33846(14) 0.5596(5) 0.29361(14) 0.0498(11) Uani 1 1 d . . . N3 N 0.42144(15) 0.4533(5) 0.34418(16) 0.0579(13) Uani 1 1 d . . . N4 N 0.39545(15) 0.3896(5) 0.41761(15) 0.0556(13) Uani 1 1 d . . . C1 C 0.30718(19) 0.4673(6) 0.40508(18) 0.0572(15) Uani 1 1 d . . . C2 C 0.2649(2) 0.4975(7) 0.3997(2) 0.0705(18) Uani 1 1 d . . . H2 H 0.2534 0.4893 0.4215 0.085 Uiso 1 1 calc R . . C3 C 0.2450(2) 0.5399(7) 0.3572(2) 0.0649(17) Uani 1 1 d . . . H3 H 0.2171 0.5669 0.3443 0.078 Uiso 1 1 calc R . . C4 C 0.27415(18) 0.5363(5) 0.33515(18) 0.0518(14) Uani 1 1 d . . . C5 C 0.26619(17) 0.5802(5) 0.29133(17) 0.0449(13) Uani 1 1 d . . . C6 C 0.29724(17) 0.5996(5) 0.27369(16) 0.0443(13) Uani 1 1 d . . . C7 C 0.29187(19) 0.6645(6) 0.23186(19) 0.0551(15) Uani 1 1 d . . . H7 H 0.2671 0.7021 0.2119 0.066 Uiso 1 1 calc R . . C8 C 0.32871(19) 0.6614(6) 0.22669(18) 0.0569(15) Uani 1 1 d . . . H8 H 0.3343 0.6968 0.2028 0.068 Uiso 1 1 calc R . . C9 C 0.35798(18) 0.5932(6) 0.26495(17) 0.0530(15) Uani 1 1 d . . . C10 C 0.3992(2) 0.5608(7) 0.2702(2) 0.0681(18) Uani 1 1 d . . . C11 C 0.4284(2) 0.4925(7) 0.3072(2) 0.0678(18) Uani 1 1 d . . . C12 C 0.4696(2) 0.4519(10) 0.3111(3) 0.098(3) Uani 1 1 d . . . H12 H 0.4818 0.4660 0.2902 0.117 Uiso 1 1 calc R . . C13 C 0.4871(2) 0.3897(9) 0.3507(3) 0.093(3) Uani 1 1 d . . . H13 H 0.5138 0.3525 0.3621 0.112 Uiso 1 1 calc R . . C14 C 0.45788(19) 0.3903(7) 0.3721(2) 0.0651(17) Uani 1 1 d . . . C15 C 0.4646(2) 0.3374(6) 0.4144(2) 0.0651(18) Uani 1 1 d . . . C16 C 0.4357(2) 0.3382(6) 0.4351(2) 0.0632(17) Uani 1 1 d . . . C17 C 0.4431(2) 0.2905(7) 0.4793(2) 0.077(2) Uani 1 1 d . . . H17 H 0.4678 0.2516 0.4988 0.093 Uiso 1 1 calc R . . C18 C 0.4085(2) 0.3112(7) 0.4882(2) 0.074(2) Uani 1 1 d . . . H18 H 0.4048 0.2889 0.5145 0.088 Uiso 1 1 calc R . . C19 C 0.3777(2) 0.3749(6) 0.44889(19) 0.0615(17) Uani 1 1 d . . . C20 C 0.3378(2) 0.4137(6) 0.44425(18) 0.0616(16) Uani 1 1 d . . . C21 C 0.22094(17) 0.6103(5) 0.26368(17) 0.0483(14) Uani 1 1 d . . . C22 C 0.18694(18) 0.5248(6) 0.26032(18) 0.0548(15) Uani 1 1 d . . . H22 H 0.1898 0.4346 0.2723 0.066 Uiso 1 1 calc R . . C23 C 0.1492(2) 0.5893(7) 0.2375(2) 0.0675(18) Uani 1 1 d . . . H23 H 0.1211 0.5531 0.2312 0.081 Uiso 1 1 calc R . . C24 C 0.1581(2) 0.7178(7) 0.2261(2) 0.0716(19) Uani 1 1 d . . . H24 H 0.1375 0.7858 0.2102 0.086 Uiso 1 1 calc R . . C25 C 0.2026(2) 0.7303(6) 0.24179(18) 0.0568(15) Uani 1 1 d . . . H25 H 0.2179 0.8082 0.2381 0.068 Uiso 1 1 calc R . . C26 C 0.19193(19) 0.4085(6) 0.16482(19) 0.0613(16) Uani 1 1 d . A . H26 H 0.2041 0.3244 0.1791 0.074 Uiso 1 1 calc R . . C27 C 0.14868(18) 0.4434(6) 0.14824(18) 0.0566(15) Uani 1 1 d . . . C28 C 0.1446(2) 0.5719(6) 0.1294(2) 0.074(2) Uani 1 1 d . A . H28 H 0.1183 0.6210 0.1147 0.089 Uiso 1 1 calc R . . C29 C 0.1854(3) 0.6163(7) 0.1362(2) 0.078(2) Uani 1 1 d . . . H29 H 0.1923 0.7030 0.1272 0.094 Uiso 1 1 calc R A . C30 C 0.2143(2) 0.5176(7) 0.1576(2) 0.0720(19) Uani 1 1 d . A . H30 H 0.2448 0.5227 0.1660 0.086 Uiso 1 1 calc R . . C31 C 0.11539(19) 0.3484(6) 0.1484(2) 0.0662(17) Uani 1 1 d . A . H31 H 0.1256 0.3011 0.1772 0.079 Uiso 1 1 calc R . . C32A C 0.0359(4) 0.2847(18) 0.1163(8) 0.118(8) Uani 0.65(2) 1 d P A -1 H32A H 0.0386 0.2198 0.1395 0.142 Uiso 0.65(2) 1 calc PR A -1 H32B H 0.0066 0.3095 0.1022 0.142 Uiso 0.65(2) 1 calc PR A -1 C32B C 0.0346(6) 0.353(3) 0.0837(9) 0.083(10) Uani 0.35(2) 1 d P A -2 H32C H 0.0050 0.3487 0.0790 0.100 Uiso 0.35(2) 1 calc PR A -2 H32D H 0.0376 0.4071 0.0603 0.100 Uiso 0.35(2) 1 calc PR A -2 C33 C 0.0499(2) 0.2256(10) 0.0823(3) 0.109(3) Uani 1 1 d . . . H33A H 0.0384 0.2756 0.0546 0.131 Uiso 1 1 calc R A . H33B H 0.0396 0.1353 0.0762 0.131 Uiso 1 1 calc R . . C41 C 0.4121(2) 0.5976(11) 0.2325(2) 0.097(3) Uani 1 1 d . . . C42 C 0.4023(4) 0.5184(14) 0.1953(3) 0.151(5) Uani 1 1 d . . . H42 H 0.3893 0.4372 0.1945 0.181 Uiso 1 1 calc R . . C43 C 0.4120(5) 0.560(2) 0.1574(4) 0.196(9) Uani 1 1 d . . . H43 H 0.4060 0.5072 0.1321 0.235 Uiso 1 1 calc R . . C44 C 0.4307(6) 0.684(4) 0.1605(8) 0.239(16) Uani 1 1 d . . . C45 C 0.4407(6) 0.747(3) 0.1951(6) 0.253(13) Uani 1 1 d . . . H45 H 0.4565 0.8234 0.1972 0.303 Uiso 1 1 calc R . . C46 C 0.4308(4) 0.7154(16) 0.2324(4) 0.168(6) Uani 1 1 d . . . H46 H 0.4370 0.7738 0.2564 0.201 Uiso 1 1 calc R . . C47 C 0.4380(5) 0.712(3) 0.1157(5) 0.381(19) Uani 1 1 d . . . H47A H 0.4230 0.7911 0.1017 0.572 Uiso 1 1 calc R . . H47B H 0.4279 0.6388 0.0956 0.572 Uiso 1 1 calc R . . H47C H 0.4674 0.7246 0.1225 0.572 Uiso 1 1 calc R . . C51 C 0.5071(2) 0.2765(7) 0.4396(2) 0.075(2) Uani 1 1 d . . . C52 C 0.5122(3) 0.1425(9) 0.4437(4) 0.160(5) Uani 1 1 d . . . H52 H 0.4891 0.0869 0.4315 0.192 Uiso 1 1 calc R . . C53 C 0.5519(3) 0.0890(10) 0.4659(4) 0.159(5) Uani 1 1 d . . . H53 H 0.5548 -0.0026 0.4671 0.191 Uiso 1 1 calc R . . C54 C 0.5863(3) 0.1631(10) 0.4858(3) 0.100(3) Uani 1 1 d . . . C55 C 0.5801(2) 0.2948(9) 0.4838(3) 0.099(3) Uani 1 1 d . . . H55 H 0.6030 0.3497 0.4981 0.119 Uiso 1 1 calc R . . C56 C 0.5414(2) 0.3521(8) 0.4614(3) 0.085(2) Uani 1 1 d . . . H56 H 0.5388 0.4437 0.4611 0.102 Uiso 1 1 calc R . . C57 C 0.6298(3) 0.1031(11) 0.5098(3) 0.136(4) Uani 1 1 d . . . H57A H 0.6271 0.0104 0.5147 0.204 Uiso 1 1 calc R . . H57B H 0.6435 0.1466 0.5382 0.204 Uiso 1 1 calc R . . H57C H 0.6461 0.1147 0.4917 0.204 Uiso 1 1 calc R . . C61 C 0.3254(2) 0.3922(8) 0.4834(2) 0.0724(19) Uani 1 1 d . . . C62 C 0.3178(2) 0.2644(9) 0.4963(3) 0.091(2) Uani 1 1 d . . . H62 H 0.3204 0.1910 0.4801 0.109 Uiso 1 1 calc R . . C63 C 0.3066(3) 0.2475(12) 0.5327(3) 0.117(3) Uani 1 1 d . . . H63 H 0.3017 0.1623 0.5405 0.140 Uiso 1 1 calc R . . C64 C 0.3025(3) 0.3507(16) 0.5574(3) 0.126(4) Uani 1 1 d . . . C65 C 0.3081(3) 0.4765(14) 0.5448(3) 0.132(4) Uani 1 1 d . . . H65 H 0.3041 0.5489 0.5605 0.158 Uiso 1 1 calc R . . C66 C 0.3201(3) 0.4965(10) 0.5078(3) 0.106(3) Uani 1 1 d . . . H66 H 0.3245 0.5822 0.4999 0.128 Uiso 1 1 calc R . . C67 C 0.2897(4) 0.3302(16) 0.5985(3) 0.192(7) Uani 1 1 d . . . H67A H 0.2647 0.2774 0.5896 0.288 Uiso 1 1 calc R . . H67B H 0.2846 0.4147 0.6091 0.288 Uiso 1 1 calc R . . H67C H 0.3120 0.2858 0.6221 0.288 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 Zn 0.0534(4) 0.0556(4) 0.0442(4) 0.0013(3) 0.0058(3) 0.0049(3) Fe 0.0529(5) 0.0436(5) 0.0485(5) 0.0030(4) 0.0043(4) 0.0005(4) S1 0.0706(11) 0.0592(10) 0.0566(9) 0.0026(8) -0.0085(8) -0.0127(9) S2 0.0650(12) 0.1084(18) 0.141(2) -0.0160(16) 0.0157(13) 0.0082(12) N1 0.062(3) 0.046(3) 0.043(3) 0.002(2) 0.011(2) 0.001(2) N2 0.047(3) 0.051(3) 0.040(2) -0.003(2) 0.004(2) 0.001(2) N3 0.052(3) 0.064(3) 0.051(3) -0.011(2) 0.012(2) -0.002(2) N4 0.057(3) 0.044(3) 0.049(3) 0.001(2) 0.000(2) 0.004(2) C1 0.063(4) 0.057(4) 0.046(3) 0.001(3) 0.014(3) -0.001(3) C2 0.074(4) 0.089(5) 0.054(4) 0.011(4) 0.030(3) 0.007(4) C3 0.062(4) 0.076(5) 0.054(4) 0.004(3) 0.019(3) 0.010(3) C4 0.056(3) 0.045(3) 0.048(3) 0.001(3) 0.011(3) 0.003(3) C5 0.055(3) 0.031(3) 0.041(3) 0.001(2) 0.010(3) -0.002(3) C6 0.057(3) 0.030(3) 0.037(3) -0.004(2) 0.008(3) -0.002(3) C7 0.056(4) 0.047(3) 0.053(3) -0.002(3) 0.009(3) -0.007(3) C8 0.064(4) 0.060(4) 0.045(3) -0.001(3) 0.018(3) -0.005(3) C9 0.059(4) 0.056(4) 0.040(3) -0.005(3) 0.015(3) -0.004(3) C10 0.060(4) 0.089(5) 0.052(4) -0.007(3) 0.018(3) -0.003(4) C11 0.055(4) 0.083(5) 0.058(4) -0.013(4) 0.013(3) 0.000(4) C12 0.067(5) 0.149(8) 0.077(5) -0.008(5) 0.026(4) 0.014(5) C13 0.067(5) 0.121(7) 0.074(5) -0.003(5) 0.007(4) 0.028(5) C14 0.048(4) 0.077(5) 0.063(4) -0.012(3) 0.013(3) 0.011(3) C15 0.055(4) 0.052(4) 0.063(4) -0.006(3) -0.006(3) 0.003(3) C16 0.061(4) 0.044(4) 0.061(4) -0.004(3) -0.003(3) 0.001(3) C17 0.072(5) 0.070(5) 0.059(4) 0.019(3) -0.011(4) 0.000(4) C18 0.067(5) 0.079(5) 0.054(4) 0.022(3) 0.001(3) -0.007(4) C19 0.075(4) 0.053(4) 0.040(3) 0.004(3) 0.004(3) -0.007(3) C20 0.069(4) 0.058(4) 0.045(3) 0.002(3) 0.007(3) -0.004(3) C21 0.049(3) 0.041(3) 0.045(3) -0.001(2) 0.007(3) 0.000(3) C22 0.060(4) 0.048(4) 0.053(3) 0.003(3) 0.017(3) -0.001(3) C23 0.058(4) 0.066(5) 0.066(4) 0.004(3) 0.010(3) 0.001(3) C24 0.069(4) 0.065(5) 0.070(4) 0.005(3) 0.014(4) 0.027(4) C25 0.073(4) 0.035(3) 0.053(3) 0.000(3) 0.014(3) 0.004(3) C26 0.068(4) 0.045(4) 0.055(3) -0.006(3) 0.006(3) 0.000(3) C27 0.056(4) 0.052(4) 0.042(3) -0.001(3) -0.003(3) -0.002(3) C28 0.096(5) 0.047(4) 0.056(4) 0.016(3) 0.002(4) 0.006(4) C29 0.115(6) 0.062(5) 0.050(4) -0.004(3) 0.023(4) -0.032(5) C30 0.074(4) 0.077(5) 0.063(4) -0.014(4) 0.023(4) -0.022(4) C31 0.056(4) 0.058(4) 0.065(4) 0.007(3) 0.000(3) 0.000(3) C32A 0.045(7) 0.113(13) 0.155(18) 0.032(12) -0.010(8) -0.001(7) C32B 0.061(13) 0.079(19) 0.078(17) -0.005(13) -0.008(11) 0.000(12) C33 0.064(5) 0.091(7) 0.113(7) 0.012(6) -0.034(5) -0.010(5) C41 0.061(5) 0.164(9) 0.060(4) 0.013(5) 0.015(4) 0.010(5) C42 0.151(10) 0.237(15) 0.072(6) -0.011(8) 0.051(6) 0.029(9) C43 0.146(13) 0.37(3) 0.066(7) -0.013(12) 0.033(8) 0.088(15) C44 0.124(14) 0.45(5) 0.163(17) 0.13(3) 0.077(15) 0.043(19) C45 0.200(18) 0.41(4) 0.174(16) 0.11(2) 0.100(16) -0.051(19) C46 0.157(11) 0.236(16) 0.123(9) 0.042(10) 0.067(8) -0.060(11) C47 0.253(19) 0.77(6) 0.191(15) 0.24(2) 0.166(15) 0.13(3) C51 0.061(4) 0.064(5) 0.073(4) -0.005(4) -0.004(3) 0.014(4) C52 0.098(7) 0.073(6) 0.212(11) -0.042(7) -0.050(7) 0.027(5) C53 0.124(9) 0.074(6) 0.196(11) -0.035(7) -0.031(8) 0.044(6) C54 0.068(5) 0.102(7) 0.101(6) -0.007(5) -0.001(4) 0.032(5) C55 0.054(4) 0.092(7) 0.118(7) 0.008(5) -0.005(4) 0.001(4) C56 0.057(4) 0.064(5) 0.106(6) 0.007(4) 0.001(4) 0.003(4) C57 0.090(6) 0.139(9) 0.146(8) 0.009(7) 0.007(6) 0.058(6) C61 0.072(4) 0.091(6) 0.042(3) 0.008(4) 0.009(3) -0.008(4) C62 0.093(6) 0.100(6) 0.074(5) 0.018(5) 0.024(4) -0.007(5) C63 0.116(8) 0.136(9) 0.092(7) 0.039(7) 0.031(6) -0.021(7) C64 0.115(8) 0.194(13) 0.061(5) 0.005(7) 0.024(5) -0.057(8) C65 0.148(9) 0.176(12) 0.081(6) -0.037(7) 0.055(6) -0.047(8) C66 0.137(8) 0.120(7) 0.071(5) -0.013(5) 0.050(5) -0.032(6) C67 0.210(13) 0.303(19) 0.082(7) -0.006(9) 0.077(8) -0.093(13) _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 Zn N1 2.049(5) . ? Zn N2 2.053(4) . ? Zn N3 2.054(5) . ? Zn N4 2.059(5) . ? Zn S1 2.658(2) 4 ? Fe C23 2.027(7) . ? Fe C27 2.034(6) . ? Fe C22 2.038(6) . ? Fe C29 2.048(6) . ? Fe C28 2.060(6) . ? Fe C24 2.060(7) . ? Fe C30 2.061(7) . ? Fe C26 2.062(6) . ? Fe C25 2.073(6) . ? Fe C21 2.085(5) . ? S1 C33 1.806(8) . ? S1 C31 1.848(7) . ? S1 Zn 2.658(2) 4_545 ? S2 C32A 1.755(16) . ? S2 C31 1.801(7) . ? S2 C32B 1.89(2) . ? N1 C1 1.371(7) . ? N1 C4 1.389(7) . ? N2 C9 1.373(7) . ? N2 C6 1.377(7) . ? N3 C11 1.360(8) . ? N3 C14 1.388(8) . ? N4 C19 1.369(8) . ? N4 C16 1.382(8) . ? C1 C20 1.408(8) . ? C1 C2 1.431(9) . ? C2 C3 1.347(8) . ? C3 C4 1.433(8) . ? C4 C5 1.401(7) . ? C5 C6 1.402(8) . ? C5 C21 1.502(7) . ? C6 C7 1.444(7) . ? C7 C8 1.341(8) . ? C8 C9 1.435(8) . ? C9 C10 1.404(8) . ? C10 C11 1.411(9) . ? C10 C41 1.486(10) . ? C11 C12 1.433(9) . ? C12 C13 1.338(10) . ? C13 C14 1.418(10) . ? C14 C15 1.397(9) . ? C15 C16 1.392(9) . ? C15 C51 1.509(8) . ? C16 C17 1.431(9) . ? C17 C18 1.342(9) . ? C18 C19 1.454(8) . ? C19 C20 1.379(9) . ? C20 C61 1.491(9) . ? C21 C25 1.423(8) . ? C21 C22 1.425(8) . ? C22 C23 1.388(8) . ? C23 C24 1.414(9) . ? C24 C25 1.423(9) . ? C26 C30 1.414(9) . ? C26 C27 1.422(8) . ? C27 C28 1.416(8) . ? C27 C31 1.496(9) . ? C28 C29 1.411(10) . ? C29 C30 1.391(10) . ? C32A C33 1.48(2) . ? C32B C33 1.39(3) . ? C41 C46 1.354(15) . ? C41 C42 1.371(13) . ? C42 C43 1.445(18) . ? C43 C44 1.40(3) . ? C44 C45 1.21(3) . ? C44 C47 1.58(2) . ? C45 C46 1.402(17) . ? C51 C56 1.355(9) . ? C51 C52 1.365(11) . ? C52 C53 1.388(12) . ? C53 C54 1.338(13) . ? C54 C55 1.345(11) . ? C54 C57 1.527(10) . ? C55 C56 1.378(9) . ? C61 C66 1.367(11) . ? C61 C62 1.410(10) . ? C62 C63 1.373(11) . ? C63 C64 1.350(15) . ? C64 C65 1.370(15) . ? C64 C67 1.557(12) . ? C65 C66 1.413(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn N2 88.54(18) . . ? N1 Zn N3 167.38(19) . . ? N2 Zn N3 89.91(19) . . ? N1 Zn N4 89.50(19) . . ? N2 Zn N4 168.67(19) . . ? N3 Zn N4 89.6(2) . . ? N1 Zn S1 95.12(14) . 4 ? N2 Zn S1 97.65(14) . 4 ? N3 Zn S1 97.50(14) . 4 ? N4 Zn S1 93.63(14) . 4 ? C23 Fe C27 104.9(3) . . ? C23 Fe C22 39.9(2) . . ? C27 Fe C22 114.9(2) . . ? C23 Fe C29 147.7(3) . . ? C27 Fe C29 67.7(3) . . ? C22 Fe C29 172.1(3) . . ? C23 Fe C28 113.7(3) . . ? C27 Fe C28 40.4(2) . . ? C22 Fe C28 146.4(3) . . ? C29 Fe C28 40.2(3) . . ? C23 Fe C24 40.5(3) . . ? C27 Fe C24 127.1(3) . . ? C22 Fe C24 67.3(3) . . ? C29 Fe C24 117.6(3) . . ? C28 Fe C24 106.8(3) . . ? C23 Fe C30 168.4(3) . . ? C27 Fe C30 68.0(3) . . ? C22 Fe C30 133.4(3) . . ? C29 Fe C30 39.6(3) . . ? C28 Fe C30 67.4(3) . . ? C24 Fe C30 151.1(3) . . ? C23 Fe C26 128.7(3) . . ? C27 Fe C26 40.6(2) . . ? C22 Fe C26 109.7(2) . . ? C29 Fe C26 67.0(3) . . ? C28 Fe C26 67.6(3) . . ? C24 Fe C26 166.2(3) . . ? C30 Fe C26 40.1(2) . . ? C23 Fe C25 67.8(3) . . ? C27 Fe C25 166.6(2) . . ? C22 Fe C25 67.3(2) . . ? C29 Fe C25 112.0(3) . . ? C28 Fe C25 130.7(2) . . ? C24 Fe C25 40.3(2) . . ? C30 Fe C25 121.0(3) . . ? C26 Fe C25 152.6(2) . . ? C23 Fe C21 67.9(2) . . ? C27 Fe C21 149.3(2) . . ? C22 Fe C21 40.4(2) . . ? C29 Fe C21 134.1(3) . . ? C28 Fe C21 170.2(2) . . ? C24 Fe C21 67.7(2) . . ? C30 Fe C21 113.2(3) . . ? C26 Fe C21 119.6(2) . . ? C25 Fe C21 40.0(2) . . ? C33 S1 C31 97.0(4) . . ? C33 S1 Zn 105.6(3) . 4_545 ? C31 S1 Zn 106.8(2) . 4_545 ? C32A S2 C31 94.5(6) . . ? C32A S2 C32B 39.5(8) . . ? C31 S2 C32B 97.1(7) . . ? C1 N1 C4 106.5(5) . . ? C1 N1 Zn 125.4(4) . . ? C4 N1 Zn 127.4(4) . . ? C9 N2 C6 107.2(4) . . ? C9 N2 Zn 124.4(4) . . ? C6 N2 Zn 127.6(4) . . ? C11 N3 C14 106.4(5) . . ? C11 N3 Zn 126.7(4) . . ? C14 N3 Zn 126.8(4) . . ? C19 N4 C16 108.6(5) . . ? C19 N4 Zn 125.1(4) . . ? C16 N4 Zn 125.9(4) . . ? N1 C1 C20 125.2(6) . . ? N1 C1 C2 109.9(5) . . ? C20 C1 C2 124.8(6) . . ? C3 C2 C1 107.0(6) . . ? C2 C3 C4 108.1(6) . . ? N1 C4 C5 125.6(5) . . ? N1 C4 C3 108.5(5) . . ? C5 C4 C3 125.7(5) . . ? C4 C5 C6 124.3(5) . . ? C4 C5 C21 114.9(5) . . ? C6 C5 C21 120.7(5) . . ? N2 C6 C5 125.5(5) . . ? N2 C6 C7 108.1(5) . . ? C5 C6 C7 126.4(5) . . ? C8 C7 C6 108.2(5) . . ? C7 C8 C9 107.1(5) . . ? N2 C9 C10 126.3(5) . . ? N2 C9 C8 109.3(5) . . ? C10 C9 C8 124.3(5) . . ? C9 C10 C11 125.4(6) . . ? C9 C10 C41 116.4(6) . . ? C11 C10 C41 118.1(6) . . ? N3 C11 C10 125.0(6) . . ? N3 C11 C12 109.7(6) . . ? C10 C11 C12 125.3(7) . . ? C13 C12 C11 107.0(7) . . ? C12 C13 C14 108.3(7) . . ? N3 C14 C15 125.4(6) . . ? N3 C14 C13 108.7(6) . . ? C15 C14 C13 125.9(6) . . ? C16 C15 C14 125.4(6) . . ? C16 C15 C51 118.1(6) . . ? C14 C15 C51 116.5(6) . . ? N4 C16 C15 126.7(6) . . ? N4 C16 C17 107.6(6) . . ? C15 C16 C17 125.7(6) . . ? C18 C17 C16 108.7(6) . . ? C17 C18 C19 107.3(6) . . ? N4 C19 C20 126.4(5) . . ? N4 C19 C18 107.7(6) . . ? C20 C19 C18 125.9(6) . . ? C19 C20 C1 125.6(6) . . ? C19 C20 C61 117.4(5) . . ? C1 C20 C61 116.9(6) . . ? C25 C21 C22 106.3(5) . . ? C25 C21 C5 129.1(5) . . ? C22 C21 C5 124.0(5) . . ? C25 C21 Fe 69.5(3) . . ? C22 C21 Fe 68.0(3) . . ? C5 C21 Fe 133.7(4) . . ? C23 C22 C21 109.4(5) . . ? C23 C22 Fe 69.6(4) . . ? C21 C22 Fe 71.6(3) . . ? C22 C23 C24 108.4(6) . . ? C22 C23 Fe 70.5(4) . . ? C24 C23 Fe 71.0(4) . . ? C23 C24 C25 107.5(5) . . ? C23 C24 Fe 68.5(4) . . ? C25 C24 Fe 70.4(3) . . ? C24 C25 C21 108.4(5) . . ? C24 C25 Fe 69.4(4) . . ? C21 C25 Fe 70.4(3) . . ? C30 C26 C27 107.6(6) . . ? C30 C26 Fe 69.9(4) . . ? C27 C26 Fe 68.6(3) . . ? C28 C27 C26 107.9(6) . . ? C28 C27 C31 129.6(6) . . ? C26 C27 C31 122.3(5) . . ? C28 C27 Fe 70.8(4) . . ? C26 C27 Fe 70.7(3) . . ? C31 C27 Fe 128.3(4) . . ? C29 C28 C27 107.1(6) . . ? C29 C28 Fe 69.4(4) . . ? C27 C28 Fe 68.8(3) . . ? C30 C29 C28 109.4(6) . . ? C30 C29 Fe 70.7(4) . . ? C28 C29 Fe 70.4(4) . . ? C29 C30 C26 107.9(6) . . ? C29 C30 Fe 69.7(4) . . ? C26 C30 Fe 70.0(4) . . ? C27 C31 S2 114.2(5) . . ? C27 C31 S1 108.6(5) . . ? S2 C31 S1 108.5(3) . . ? C33 C32A S2 111.1(12) . . ? C33 C32B S2 107.8(15) . . ? C32B C33 C32A 51.0(12) . . ? C32B C33 S1 110.6(10) . . ? C32A C33 S1 109.7(7) . . ? C46 C41 C42 118.0(10) . . ? C46 C41 C10 120.8(9) . . ? C42 C41 C10 121.0(10) . . ? C41 C42 C43 120.5(14) . . ? C44 C43 C42 116.8(17) . . ? C45 C44 C43 120(2) . . ? C45 C44 C47 131(3) . . ? C43 C44 C47 109(2) . . ? C44 C45 C46 126(3) . . ? C41 C46 C45 118.3(16) . . ? C56 C51 C52 117.0(7) . . ? C56 C51 C15 121.6(6) . . ? C52 C51 C15 121.3(7) . . ? C51 C52 C53 120.0(9) . . ? C54 C53 C52 123.1(9) . . ? C53 C54 C55 115.9(7) . . ? C53 C54 C57 122.6(9) . . ? C55 C54 C57 121.5(9) . . ? C54 C55 C56 122.9(8) . . ? C51 C56 C55 120.8(7) . . ? C66 C61 C62 117.1(7) . . ? C66 C61 C20 121.0(7) . . ? C62 C61 C20 121.8(7) . . ? C63 C62 C61 120.6(9) . . ? C64 C63 C62 122.1(10) . . ? C63 C64 C65 118.9(9) . . ? C63 C64 C67 121.6(12) . . ? C65 C64 C67 119.5(13) . . ? C64 C65 C66 120.1(11) . . ? C61 C66 C65 121.2(9) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.856 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.076 # Attachment '- 8Zn_revised.cif' data_8Zn _database_code_depnum_ccdc_archive 'CCDC 893173' #TrackingRef '- 8Zn_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H48 Fe2 N4 O4 Zn' _chemical_formula_weight 1042.07 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.236(2) _cell_length_b 12.414(4) _cell_length_c 12.620(4) _cell_angle_alpha 67.731(5) _cell_angle_beta 72.240(5) _cell_angle_gamma 76.832(5) _cell_volume 1127.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3967 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 26.37 _exptl_crystal_description needle _exptl_crystal_colour dark _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details SADABS _exptl_special_details ; 3582 Reflections employed for parameter determination Rint decreases from 2.09 to 1.34 using Sadabs absorption correction ; _diffrn_ambient_temperature 223(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 6557 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4461 _reflns_number_gt 3967 _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^)+(0.0445P)^2^+1.5379P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4461 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 Zn Zn 0.0000 1.0000 0.0000 0.02685(14) Uani 1 2 d S . . Fe Fe 0.72450(5) 0.77907(4) -0.25174(4) 0.02789(13) Uani 1 1 d . . . N1 N 0.1263(3) 1.0612(2) -0.17384(19) 0.0226(5) Uani 1 1 d . . . N2 N 0.2319(3) 0.9155(2) 0.03815(19) 0.0227(5) Uani 1 1 d . . . C1 C 0.0544(4) 1.1447(2) -0.2618(2) 0.0229(5) Uani 1 1 d . . . C2 C 0.1883(4) 1.1853(2) -0.3659(2) 0.0265(6) Uani 1 1 d . . . H2 H 0.168(4) 1.244(3) -0.435(3) 0.029(8) Uiso 1 1 d . . . C3 C 0.3385(4) 1.1252(3) -0.3420(2) 0.0272(6) Uani 1 1 d . . . H3 H 0.442(5) 1.133(3) -0.387(3) 0.036(9) Uiso 1 1 d . . . C4 C 0.3001(3) 1.0454(2) -0.2218(2) 0.0233(6) Uani 1 1 d . . . C5 C 0.4234(3) 0.9660(2) -0.1628(2) 0.0228(5) Uani 1 1 d . . . C6 C 0.3907(3) 0.9100(2) -0.0395(2) 0.0233(6) Uani 1 1 d . . . C7 C 0.5144(4) 0.8357(3) 0.0262(3) 0.0289(6) Uani 1 1 d . . . H7 H 0.626(5) 0.819(3) -0.006(3) 0.032(9) Uiso 1 1 d . . . C8 C 0.4303(4) 0.7967(3) 0.1404(3) 0.0283(6) Uani 1 1 d . . . H8 H 0.469(5) 0.749(3) 0.203(3) 0.044(10) Uiso 1 1 d . . . C9 C 0.2521(3) 0.8439(2) 0.1485(2) 0.0228(5) Uani 1 1 d . . . C10 C 0.5946(4) 0.9413(2) -0.2398(2) 0.0243(6) Uani 1 1 d . . . C11 C 0.6216(4) 0.9325(3) -0.3546(3) 0.0277(6) Uani 1 1 d . . . H11 H 0.533(5) 0.936(3) -0.385(3) 0.034(9) Uiso 1 1 d . . . C12 C 0.8010(4) 0.9128(3) -0.4036(3) 0.0325(7) Uani 1 1 d . . . H12 H 0.852(5) 0.903(3) -0.478(3) 0.038(9) Uiso 1 1 d . . . C13 C 0.8871(4) 0.9057(3) -0.3188(3) 0.0306(6) Uani 1 1 d . . . H13 H 1.005(5) 0.890(3) -0.329(3) 0.038(9) Uiso 1 1 d . . . C14 C 0.7618(4) 0.9234(2) -0.2194(3) 0.0266(6) Uani 1 1 d . . . H14 H 0.787(4) 0.929(3) -0.155(3) 0.029(8) Uiso 1 1 d . . . C15 C 0.5710(4) 0.6492(3) -0.1628(3) 0.0389(8) Uani 1 1 d . . . C16 C 0.6468(4) 0.6506(3) -0.2816(3) 0.0395(8) Uani 1 1 d . . . H16 H 0.585(5) 0.661(3) -0.342(3) 0.041(10) Uiso 1 1 d . . . C17 C 0.8272(5) 0.6302(3) -0.2961(4) 0.0426(8) Uani 1 1 d . . . H17 H 0.910(6) 0.626(4) -0.365(4) 0.057(12) Uiso 1 1 d . . . C18 C 0.8634(5) 0.6182(3) -0.1892(4) 0.0454(9) Uani 1 1 d . . . H18 H 0.971(6) 0.612(4) -0.176(4) 0.063(13) Uiso 1 1 d . . . C19 C 0.7070(5) 0.6297(3) -0.1062(3) 0.0421(8) Uani 1 1 d . . . H19 H 0.695(5) 0.621(3) -0.028(4) 0.046(11) Uiso 1 1 d . . . C20 C 0.3886(5) 0.6802(3) -0.1118(4) 0.0501(9) Uani 1 1 d . . . H20 H 0.358(6) 0.686(4) -0.028(4) 0.062(12) Uiso 1 1 d . . . C21 C 0.1209(4) 0.8152(2) 0.2521(2) 0.0225(5) Uani 1 1 d . . . C22 C 0.1731(3) 0.7309(2) 0.3618(2) 0.0230(6) Uani 1 1 d . . . C23 C 0.1802(5) 0.6112(3) 0.3899(3) 0.0376(7) Uani 1 1 d . . . H23 H 0.157(5) 0.586(3) 0.342(4) 0.051(11) Uiso 1 1 d . . . C24 C 0.2291(5) 0.5330(3) 0.4905(3) 0.0398(8) Uani 1 1 d . . . H24 H 0.233(5) 0.457(4) 0.508(3) 0.049(11) Uiso 1 1 d . . . C25 C 0.2715(4) 0.5716(3) 0.5665(3) 0.0318(7) Uani 1 1 d . . . C26 C 0.2630(4) 0.6915(3) 0.5393(3) 0.0347(7) Uani 1 1 d . . . H26 H 0.282(4) 0.714(3) 0.587(3) 0.027(9) Uiso 1 1 d . . . C27 C 0.2142(4) 0.7701(3) 0.4385(3) 0.0299(6) Uani 1 1 d . . . H27 H 0.206(4) 0.849(3) 0.421(3) 0.035(9) Uiso 1 1 d . . . C28 C 0.3228(6) 0.4858(4) 0.6768(4) 0.0494(10) Uani 1 1 d . . . H28A H 0.294(8) 0.510(5) 0.734(6) 0.09(2) Uiso 1 1 d . . . H28B H 0.425(9) 0.483(5) 0.673(5) 0.10(2) Uiso 1 1 d . . . H28C H 0.289(8) 0.425(5) 0.696(5) 0.10(2) Uiso 1 1 d . . . C31 C -0.0440(6) 0.7107(4) 0.0706(4) 0.0435(8) Uani 1 1 d . . . H31A H 0.052(6) 0.683(4) 0.103(4) 0.058(12) Uiso 1 1 d . . . H31B H -0.056(5) 0.656(3) 0.050(3) 0.034(9) Uiso 1 1 d . . . H31C H -0.131(6) 0.728(4) 0.123(4) 0.066(15) Uiso 1 1 d . . . O1 O 0.2732(3) 0.7039(3) -0.1618(3) 0.0616(8) Uani 1 1 d . . . O2 O -0.0174(3) 0.8142(2) -0.0265(2) 0.0416(6) Uani 1 1 d . . . H2O H 0.081(7) 0.787(5) -0.085(5) 0.100(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0192(2) 0.0370(3) 0.0158(2) -0.00143(19) -0.00584(17) 0.00182(18) Fe 0.0239(2) 0.0272(2) 0.0313(2) -0.01258(18) -0.00358(17) -0.00001(16) N1 0.0232(11) 0.0248(12) 0.0164(11) -0.0051(9) -0.0066(9) 0.0028(9) N2 0.0224(11) 0.0245(11) 0.0179(11) -0.0056(9) -0.0065(9) 0.0029(9) C1 0.0268(14) 0.0232(13) 0.0174(13) -0.0069(10) -0.0066(11) 0.0010(11) C2 0.0317(15) 0.0237(14) 0.0187(13) -0.0035(11) -0.0060(11) 0.0001(11) C3 0.0240(15) 0.0304(15) 0.0202(14) -0.0050(12) -0.0024(11) -0.0003(12) C4 0.0241(14) 0.0239(13) 0.0204(13) -0.0079(11) -0.0045(10) -0.0005(11) C5 0.0216(13) 0.0239(13) 0.0215(13) -0.0086(11) -0.0047(10) 0.0011(10) C6 0.0236(13) 0.0228(13) 0.0215(13) -0.0077(11) -0.0067(11) 0.0028(10) C7 0.0227(15) 0.0340(16) 0.0247(14) -0.0091(12) -0.0068(12) 0.0068(12) C8 0.0278(15) 0.0286(15) 0.0236(14) -0.0044(12) -0.0112(12) 0.0047(12) C9 0.0240(14) 0.0224(13) 0.0202(13) -0.0057(11) -0.0091(11) 0.0031(10) C10 0.0248(14) 0.0235(13) 0.0219(13) -0.0070(11) -0.0054(11) 0.0008(11) C11 0.0268(15) 0.0291(15) 0.0259(14) -0.0100(12) -0.0068(12) 0.0009(12) C12 0.0346(16) 0.0323(16) 0.0254(15) -0.0114(13) 0.0022(13) -0.0037(13) C13 0.0228(15) 0.0275(15) 0.0355(16) -0.0080(13) -0.0031(12) -0.0013(12) C14 0.0251(14) 0.0265(14) 0.0283(15) -0.0095(12) -0.0069(12) -0.0022(11) C15 0.0361(18) 0.0314(16) 0.047(2) -0.0166(15) -0.0010(15) -0.0065(13) C16 0.0341(17) 0.0371(18) 0.053(2) -0.0255(16) -0.0021(15) -0.0082(14) C17 0.0380(19) 0.0342(18) 0.056(2) -0.0264(17) -0.0008(17) -0.0007(14) C18 0.0373(19) 0.0290(17) 0.064(2) -0.0130(16) -0.0140(17) 0.0056(14) C19 0.048(2) 0.0301(17) 0.040(2) -0.0063(15) -0.0079(16) -0.0037(15) C20 0.041(2) 0.051(2) 0.058(2) -0.0277(19) 0.0063(18) -0.0140(17) C21 0.0261(14) 0.0213(13) 0.0184(13) -0.0051(10) -0.0082(10) 0.0013(10) C22 0.0201(13) 0.0245(13) 0.0193(13) -0.0043(11) -0.0057(10) 0.0029(10) C23 0.054(2) 0.0282(16) 0.0345(17) -0.0103(14) -0.0207(16) 0.0009(14) C24 0.053(2) 0.0211(16) 0.0381(18) -0.0021(14) -0.0154(16) 0.0018(14) C25 0.0200(14) 0.0369(17) 0.0230(14) 0.0032(12) -0.0042(11) 0.0011(12) C26 0.0381(18) 0.0409(18) 0.0256(16) -0.0046(14) -0.0153(13) -0.0067(14) C27 0.0343(16) 0.0252(15) 0.0283(15) -0.0023(12) -0.0139(13) -0.0034(12) C28 0.045(2) 0.051(3) 0.031(2) 0.0100(18) -0.0147(17) -0.0003(19) C31 0.044(2) 0.040(2) 0.047(2) -0.0092(17) -0.0146(18) -0.0104(17) O1 0.0308(14) 0.094(2) 0.071(2) -0.0459(18) -0.0012(13) -0.0115(14) O2 0.0362(13) 0.0463(14) 0.0371(13) -0.0108(11) -0.0094(10) -0.0001(11) _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 Zn N1 2.044(2) 2_575 ? Zn N1 2.044(2) . ? Zn N2 2.060(2) . ? Zn N2 2.060(2) 2_575 ? Fe C11 2.023(3) . ? Fe C15 2.037(3) . ? Fe C12 2.038(3) . ? Fe C16 2.040(3) . ? Fe C19 2.053(4) . ? Fe C17 2.056(3) . ? Fe C13 2.059(3) . ? Fe C18 2.058(3) . ? Fe C14 2.086(3) . ? Fe C10 2.092(3) . ? N1 C4 1.374(4) . ? N1 C1 1.381(3) . ? N2 C9 1.376(3) . ? N2 C6 1.379(4) . ? C1 C21 1.399(4) 2_575 ? C1 C2 1.437(4) . ? C2 C3 1.346(4) . ? C2 H2 0.93(3) . ? C3 C4 1.447(4) . ? C3 H3 0.87(4) . ? C4 C5 1.416(4) . ? C5 C6 1.410(4) . ? C5 C10 1.490(4) . ? C6 C7 1.444(4) . ? C7 C8 1.344(4) . ? C7 H7 0.89(4) . ? C8 C9 1.439(4) . ? C8 H8 0.88(4) . ? C9 C21 1.401(4) . ? C10 C14 1.430(4) . ? C10 C11 1.440(4) . ? C11 C12 1.420(4) . ? C11 H11 0.91(3) . ? C12 C13 1.421(5) . ? C12 H12 0.95(4) . ? C13 C14 1.415(4) . ? C13 H13 0.92(4) . ? C14 H14 0.92(3) . ? C15 C16 1.433(5) . ? C15 C19 1.435(5) . ? C15 C20 1.467(5) . ? C16 C17 1.415(5) . ? C16 H16 0.99(4) . ? C17 C18 1.415(6) . ? C17 H17 0.94(4) . ? C18 C19 1.408(5) . ? C18 H18 0.92(5) . ? C19 H19 0.92(4) . ? C20 O1 1.219(5) . ? C20 H20 1.03(4) . ? C21 C1 1.399(4) 2_575 ? C21 C22 1.502(4) . ? C22 C23 1.383(4) . ? C22 C27 1.386(4) . ? C23 C24 1.384(5) . ? C23 H23 0.86(4) . ? C24 C25 1.379(5) . ? C24 H24 0.88(4) . ? C25 C26 1.385(5) . ? C25 C28 1.510(4) . ? C26 C27 1.387(4) . ? C26 H26 0.81(3) . ? C27 H27 0.91(4) . ? C28 H28A 0.83(6) . ? C28 H28B 0.83(6) . ? C28 H28C 0.79(6) . ? C31 O2 1.404(4) . ? C31 H31A 0.94(5) . ? C31 H31B 0.86(4) . ? C31 H31C 0.86(5) . ? O2 H2O 1.00(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn N1 180.0 2_575 . ? N1 Zn N2 91.38(9) 2_575 . ? N1 Zn N2 88.62(9) . . ? N1 Zn N2 88.62(9) 2_575 2_575 ? N1 Zn N2 91.38(9) . 2_575 ? N2 Zn N2 180.00(15) . 2_575 ? C11 Fe C15 117.14(14) . . ? C11 Fe C12 40.94(12) . . ? C15 Fe C12 147.51(14) . . ? C11 Fe C16 105.65(14) . . ? C15 Fe C16 41.14(14) . . ? C12 Fe C16 112.29(14) . . ? C11 Fe C19 152.37(14) . . ? C15 Fe C19 41.07(15) . . ? C12 Fe C19 166.68(14) . . ? C16 Fe C19 69.11(16) . . ? C11 Fe C17 126.46(15) . . ? C15 Fe C17 68.08(14) . . ? C12 Fe C17 104.08(14) . . ? C16 Fe C17 40.43(14) . . ? C19 Fe C17 67.94(16) . . ? C11 Fe C13 68.30(12) . . ? C15 Fe C13 171.79(14) . . ? C12 Fe C13 40.58(13) . . ? C16 Fe C13 145.52(13) . . ? C19 Fe C13 131.55(14) . . ? C17 Fe C13 114.38(14) . . ? C11 Fe C18 164.96(14) . . ? C15 Fe C18 68.01(15) . . ? C12 Fe C18 127.12(14) . . ? C16 Fe C18 68.27(16) . . ? C19 Fe C18 40.07(15) . . ? C17 Fe C18 40.25(16) . . ? C13 Fe C18 108.41(14) . . ? C11 Fe C14 67.77(12) . . ? C15 Fe C14 134.64(13) . . ? C12 Fe C14 67.71(12) . . ? C16 Fe C14 170.48(13) . . ? C19 Fe C14 113.25(14) . . ? C17 Fe C14 149.02(13) . . ? C13 Fe C14 39.92(12) . . ? C18 Fe C14 119.82(14) . . ? C11 Fe C10 40.92(11) . . ? C15 Fe C10 111.65(12) . . ? C12 Fe C10 68.65(12) . . ? C16 Fe C10 130.56(13) . . ? C19 Fe C10 121.26(13) . . ? C17 Fe C10 166.68(14) . . ? C13 Fe C10 67.91(12) . . ? C18 Fe C10 152.93(14) . . ? C14 Fe C10 40.03(11) . . ? C4 N1 C1 106.7(2) . . ? C4 N1 Zn 127.46(18) . . ? C1 N1 Zn 124.84(18) . . ? C9 N2 C6 106.9(2) . . ? C9 N2 Zn 124.73(18) . . ? C6 N2 Zn 128.09(18) . . ? N1 C1 C21 125.9(2) . 2_575 ? N1 C1 C2 109.3(2) . . ? C21 C1 C2 124.8(2) 2_575 . ? C3 C2 C1 107.5(2) . . ? C3 C2 H2 129(2) . . ? C1 C2 H2 123(2) . . ? C2 C3 C4 107.4(3) . . ? C2 C3 H3 128(2) . . ? C4 C3 H3 124(2) . . ? N1 C4 C5 125.8(2) . . ? N1 C4 C3 109.1(2) . . ? C5 C4 C3 125.1(2) . . ? C6 C5 C4 123.9(2) . . ? C6 C5 C10 120.3(2) . . ? C4 C5 C10 115.9(2) . . ? N2 C6 C5 124.9(2) . . ? N2 C6 C7 108.7(2) . . ? C5 C6 C7 126.3(3) . . ? C8 C7 C6 107.6(3) . . ? C8 C7 H7 128(2) . . ? C6 C7 H7 124(2) . . ? C7 C8 C9 107.6(3) . . ? C7 C8 H8 130(2) . . ? C9 C8 H8 122(2) . . ? N2 C9 C21 126.3(2) . . ? N2 C9 C8 109.1(2) . . ? C21 C9 C8 124.5(2) . . ? C14 C10 C11 106.0(2) . . ? C14 C10 C5 129.2(3) . . ? C11 C10 C5 124.8(3) . . ? C14 C10 Fe 69.79(16) . . ? C11 C10 Fe 66.97(16) . . ? C5 C10 Fe 128.23(19) . . ? C12 C11 C10 109.1(3) . . ? C12 C11 Fe 70.12(17) . . ? C10 C11 Fe 72.11(16) . . ? C12 C11 H11 129(2) . . ? C10 C11 H11 122(2) . . ? Fe C11 H11 122(2) . . ? C11 C12 C13 107.5(3) . . ? C11 C12 Fe 68.94(17) . . ? C13 C12 Fe 70.49(18) . . ? C11 C12 H12 125(2) . . ? C13 C12 H12 127(2) . . ? Fe C12 H12 124(2) . . ? C14 C13 C12 108.3(3) . . ? C14 C13 Fe 71.09(17) . . ? C12 C13 Fe 68.93(18) . . ? C14 C13 H13 128(2) . . ? C12 C13 H13 123(2) . . ? Fe C13 H13 124(2) . . ? C13 C14 C10 109.1(3) . . ? C13 C14 Fe 69.00(17) . . ? C10 C14 Fe 70.18(16) . . ? C13 C14 H14 124(2) . . ? C10 C14 H14 126(2) . . ? Fe C14 H14 131(2) . . ? C16 C15 C19 108.1(3) . . ? C16 C15 C20 126.5(4) . . ? C19 C15 C20 124.7(3) . . ? C16 C15 Fe 69.55(19) . . ? C19 C15 Fe 70.05(19) . . ? C20 C15 Fe 119.0(2) . . ? C17 C16 C15 107.1(3) . . ? C17 C16 Fe 70.38(19) . . ? C15 C16 Fe 69.30(19) . . ? C17 C16 H16 126(2) . . ? C15 C16 H16 127(2) . . ? Fe C16 H16 127(2) . . ? C18 C17 C16 108.7(3) . . ? C18 C17 Fe 70.0(2) . . ? C16 C17 Fe 69.20(19) . . ? C18 C17 H17 125(3) . . ? C16 C17 H17 127(3) . . ? Fe C17 H17 126(3) . . ? C19 C18 C17 108.8(3) . . ? C19 C18 Fe 69.7(2) . . ? C17 C18 Fe 69.8(2) . . ? C19 C18 H18 124(3) . . ? C17 C18 H18 127(3) . . ? Fe C18 H18 122(3) . . ? C18 C19 C15 107.3(3) . . ? C18 C19 Fe 70.2(2) . . ? C15 C19 Fe 68.9(2) . . ? C18 C19 H19 126(2) . . ? C15 C19 H19 126(2) . . ? Fe C19 H19 129(2) . . ? O1 C20 C15 125.3(4) . . ? O1 C20 H20 118(2) . . ? C15 C20 H20 116(2) . . ? C1 C21 C9 126.0(2) 2_575 . ? C1 C21 C22 117.2(2) 2_575 . ? C9 C21 C22 116.8(2) . . ? C23 C22 C27 117.8(3) . . ? C23 C22 C21 120.8(3) . . ? C27 C22 C21 121.4(3) . . ? C22 C23 C24 121.1(3) . . ? C22 C23 H23 118(3) . . ? C24 C23 H23 121(3) . . ? C25 C24 C23 121.2(3) . . ? C25 C24 H24 118(3) . . ? C23 C24 H24 120(3) . . ? C24 C25 C26 117.9(3) . . ? C24 C25 C28 120.9(4) . . ? C26 C25 C28 121.2(4) . . ? C25 C26 C27 121.0(3) . . ? C25 C26 H26 118(2) . . ? C27 C26 H26 121(2) . . ? C22 C27 C26 121.0(3) . . ? C22 C27 H27 117(2) . . ? C26 C27 H27 122(2) . . ? C25 C28 H28A 115(4) . . ? C25 C28 H28B 112(4) . . ? H28A C28 H28B 91(5) . . ? C25 C28 H28C 111(4) . . ? H28A C28 H28C 110(6) . . ? H28B C28 H28C 116(6) . . ? O2 C31 H31A 111(3) . . ? O2 C31 H31B 111(2) . . ? H31A C31 H31B 106(3) . . ? O2 C31 H31C 107(3) . . ? H31A C31 H31C 108(4) . . ? H31B C31 H31C 113(4) . . ? C31 O2 H2O 103(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2O O1 1.00(6) 1.90(6) 2.881(4) 166(5) . C14 H14 O2 0.92(3) 2.46(3) 3.185(4) 135(3) 1_655 _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.534 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.068 # Attachment '- 4Zn_revised.cif' data_4Zn _database_code_depnum_ccdc_archive 'CCDC 893174' #TrackingRef '- 4Zn_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H64 Fe2 N4 O2 S4 Zn' _chemical_formula_weight 1274.54 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' S S 0.1246 0.1234 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.415(6) _cell_length_b 12.697(4) _cell_length_c 24.742(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5785(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2042 _cell_measurement_theta_min 0.936 _cell_measurement_theta_max 0.989 _exptl_crystal_description needle _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8097 _exptl_absorpt_correction_T_max 0.9891 _exptl_absorpt_process_details Sadabs _exptl_special_details ; 2575 Reflections employed for parameter determination Rint decreases from 5.01 to 4.57 using Sadabs absorption correction ; _diffrn_ambient_temperature 223(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 12817 _diffrn_reflns_av_R_equivalents 0.1441 _diffrn_reflns_av_sigmaI/netI 0.2005 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4773 _reflns_number_gt 2042 _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. Restraints were introduced and yield to a convergent refinement : for distances in thf solvent molecule (dfix instructions), and for anisotropic displacement parameters of thf molecule and the dithiolanyl cycle (simu and isor instructions). ; _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^)+(0.0847P)^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 4773 _refine_ls_number_parameters 367 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.1892 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1876 _refine_ls_wR_factor_gt 0.1529 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 Zn Zn 0.5000 0.5000 0.5000 0.0298(4) Uani 1 2 d S . . Fe Fe 0.82514(6) 0.34210(10) 0.41399(5) 0.0335(4) Uani 1 1 d . . . S1 S 1.08261(15) 0.3615(3) 0.43144(16) 0.0995(14) Uani 1 1 d U . . S2 S 0.99472(12) 0.1722(2) 0.40790(10) 0.0489(7) Uani 1 1 d . . . N1 N 0.4796(3) 0.6152(5) 0.5558(2) 0.0208(17) Uani 1 1 d . . . N2 N 0.6082(3) 0.5047(5) 0.5175(2) 0.0205(16) Uani 1 1 d . . . C1 C 0.4144(4) 0.6613(7) 0.5664(3) 0.026(2) Uani 1 1 d . . . C2 C 0.4261(4) 0.7490(7) 0.6025(3) 0.034(2) Uani 1 1 d . . . H2A H 0.3900 0.7947 0.6157 0.040 Uiso 1 1 calc R . . C3 C 0.4965(5) 0.7541(7) 0.6137(3) 0.034(2) Uani 1 1 d . . . H3A H 0.5196 0.8038 0.6359 0.041 Uiso 1 1 calc R . . C4 C 0.5307(4) 0.6686(7) 0.5850(3) 0.025(2) Uani 1 1 d . . . C5 C 0.6044(4) 0.6430(6) 0.5870(3) 0.023(2) Uani 1 1 d . . . C6 C 0.6400(4) 0.5669(7) 0.5561(3) 0.022(2) Uani 1 1 d . . . C7 C 0.7165(4) 0.5439(7) 0.5577(3) 0.025(2) Uani 1 1 d . . . H7A H 0.7507 0.5755 0.5808 0.030 Uiso 1 1 calc R . . C8 C 0.7304(4) 0.4715(6) 0.5214(3) 0.027(2) Uani 1 1 d . . . H8A H 0.7763 0.4428 0.5135 0.032 Uiso 1 1 calc R . . C9 C 0.6629(4) 0.4437(6) 0.4959(3) 0.023(2) Uani 1 1 d . . . C10 C 0.6533(4) 0.3694(6) 0.4541(3) 0.021(2) Uani 1 1 d . . . C11 C 0.6506(4) 0.7017(7) 0.6287(3) 0.028(2) Uani 1 1 d . . . C12 C 0.6737(5) 0.8031(7) 0.6193(3) 0.035(2) Uani 1 1 d . . . H12A H 0.6596 0.8388 0.5877 0.042 Uiso 1 1 calc R . . C13 C 0.7184(5) 0.8527(8) 0.6574(4) 0.044(3) Uani 1 1 d . . . H13A H 0.7347 0.9215 0.6502 0.052 Uiso 1 1 calc R . . C14 C 0.7391(4) 0.8058(8) 0.7040(4) 0.036(2) Uani 1 1 d . . . C15 C 0.7160(5) 0.7061(8) 0.7124(4) 0.044(3) Uani 1 1 d . . . H15A H 0.7299 0.6711 0.7442 0.053 Uiso 1 1 calc R . . C16 C 0.6725(5) 0.6544(8) 0.6756(4) 0.042(2) Uani 1 1 d . . . H16A H 0.6576 0.5851 0.6830 0.050 Uiso 1 1 calc R . . C17 C 0.7890(5) 0.8627(9) 0.7440(4) 0.061(3) Uani 1 1 d . . . H17A H 0.7979 0.8176 0.7750 0.091 Uiso 1 1 calc R . . H17B H 0.7659 0.9273 0.7559 0.091 Uiso 1 1 calc R . . H17C H 0.8347 0.8791 0.7265 0.091 Uiso 1 1 calc R . . C21 C 0.7180(4) 0.3082(7) 0.4346(3) 0.030(2) Uani 1 1 d . . . C22 C 0.7671(4) 0.2482(6) 0.4669(4) 0.030(2) Uani 1 1 d . . . H22A H 0.7704 0.2502 0.5068 0.036 Uiso 1 1 calc R . . C23 C 0.8121(4) 0.1887(7) 0.4321(4) 0.038(3) Uani 1 1 d . . . H23A H 0.8510 0.1397 0.4436 0.046 Uiso 1 1 calc R . . C24 C 0.7906(5) 0.2083(8) 0.3784(4) 0.044(3) Uani 1 1 d . . . H24A H 0.8112 0.1754 0.3455 0.053 Uiso 1 1 calc R . . C25 C 0.7335(4) 0.2824(7) 0.3802(4) 0.038(3) Uani 1 1 d . . . H25A H 0.7083 0.3119 0.3483 0.046 Uiso 1 1 calc R . . C26 C 0.8468(5) 0.4989(8) 0.4194(5) 0.059(3) Uani 1 1 d . . . H26A H 0.8123 0.5537 0.4316 0.071 Uiso 1 1 calc R . . C27 C 0.8961(5) 0.4437(8) 0.4529(4) 0.044(3) Uani 1 1 d . . . H27A H 0.9019 0.4522 0.4925 0.053 Uiso 1 1 calc R . . C28 C 0.9341(5) 0.3712(7) 0.4192(4) 0.043(3) Uani 1 1 d . . . C29 C 0.9089(5) 0.3847(8) 0.3658(4) 0.050(3) Uani 1 1 d . . . H29A H 0.9263 0.3460 0.3336 0.060 Uiso 1 1 calc R . . C30 C 0.8557(6) 0.4645(9) 0.3663(5) 0.069(4) Uani 1 1 d . . . H30A H 0.8288 0.4911 0.3344 0.083 Uiso 1 1 calc R . . C31 C 0.9934(5) 0.3018(7) 0.4409(4) 0.047(3) Uani 1 1 d . . . H31A H 0.9853 0.2914 0.4801 0.057 Uiso 1 1 calc R . . C32 C 1.1104(7) 0.2848(11) 0.3836(6) 0.103(3) Uani 1 1 d U . . H32A H 1.0966 0.3178 0.3493 0.124 Uiso 1 1 calc R . . H32B H 1.1635 0.2845 0.3849 0.124 Uiso 1 1 calc R . . C33 C 1.0868(5) 0.1759(9) 0.3813(5) 0.069(3) Uani 1 1 d U . . H33A H 1.1189 0.1313 0.4031 0.082 Uiso 1 1 calc R . . H33B H 1.0877 0.1504 0.3439 0.082 Uiso 1 1 calc R . . O O -0.0272(7) 0.9954(15) 0.7323(8) 0.260(6) Uani 1 1 d DU . . C41 C 0.0136(12) 0.9313(17) 0.7684(9) 0.256(6) Uani 1 1 d DU . . H41A H 0.0211 0.9665 0.8032 0.307 Uiso 1 1 calc R . . H41B H -0.0102 0.8633 0.7745 0.307 Uiso 1 1 calc R . . C42 C 0.0795(11) 0.9191(16) 0.7401(10) 0.254(7) Uani 1 1 d DU . . H42A H 0.0733 0.8730 0.7087 0.304 Uiso 1 1 calc R . . H42B H 0.1174 0.8901 0.7635 0.304 Uiso 1 1 calc R . . C43 C 0.0967(9) 1.025(2) 0.7237(10) 0.252(7) Uani 1 1 d DU . . H43A H 0.1284 1.0593 0.7502 0.303 Uiso 1 1 calc R . . H43B H 0.1205 1.0256 0.6883 0.303 Uiso 1 1 calc R . . C44 C 0.0274(13) 1.0743(14) 0.7215(10) 0.254(6) Uani 1 1 d DU . . H44A H 0.0195 1.1052 0.6857 0.305 Uiso 1 1 calc R . . H44B H 0.0246 1.1306 0.7485 0.305 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 Zn 0.0173(6) 0.0382(9) 0.0338(8) -0.0138(8) 0.0001(7) -0.0017(7) Fe 0.0279(7) 0.0322(8) 0.0403(8) 0.0040(8) 0.0034(6) 0.0037(6) S1 0.0408(17) 0.099(3) 0.159(3) -0.068(3) 0.0175(19) -0.0146(17) S2 0.0322(13) 0.0517(18) 0.0629(18) -0.0120(15) 0.0011(13) 0.0073(13) N1 0.012(3) 0.029(4) 0.021(4) -0.006(4) 0.000(3) 0.001(3) N2 0.018(3) 0.026(4) 0.018(4) -0.009(4) -0.004(3) 0.002(3) C1 0.037(5) 0.020(5) 0.020(5) 0.000(5) -0.001(4) 0.000(4) C2 0.021(5) 0.035(6) 0.044(6) -0.017(5) -0.010(4) 0.008(4) C3 0.032(5) 0.037(6) 0.034(5) -0.014(5) -0.002(5) -0.005(5) C4 0.019(4) 0.028(5) 0.027(5) -0.002(5) 0.000(4) 0.001(4) C5 0.019(4) 0.026(6) 0.024(5) -0.006(5) -0.005(4) -0.007(4) C6 0.019(4) 0.024(5) 0.024(5) 0.002(5) 0.002(4) -0.003(4) C7 0.018(4) 0.028(5) 0.028(6) 0.000(5) -0.006(4) -0.004(4) C8 0.017(4) 0.029(6) 0.035(6) -0.004(5) -0.001(4) 0.004(4) C9 0.020(4) 0.022(5) 0.026(5) 0.006(5) 0.001(4) -0.004(4) C10 0.027(5) 0.022(5) 0.016(5) -0.007(4) -0.005(4) 0.000(4) C11 0.023(5) 0.030(6) 0.030(6) -0.006(5) 0.002(4) -0.003(4) C12 0.043(5) 0.044(7) 0.018(5) 0.001(5) -0.008(4) 0.000(5) C13 0.047(6) 0.049(7) 0.035(6) -0.010(6) 0.003(5) -0.027(5) C14 0.031(5) 0.055(7) 0.021(6) -0.009(6) -0.003(4) -0.011(5) C15 0.055(7) 0.052(7) 0.027(6) 0.005(6) -0.013(5) -0.013(6) C16 0.054(6) 0.037(6) 0.034(6) 0.012(6) -0.017(5) -0.012(5) C17 0.052(6) 0.095(9) 0.036(6) -0.011(6) 0.009(5) -0.036(6) C21 0.031(5) 0.027(6) 0.031(6) -0.012(5) -0.006(4) 0.003(4) C22 0.028(5) 0.022(5) 0.039(6) 0.000(5) -0.002(4) -0.003(4) C23 0.020(5) 0.029(6) 0.066(8) 0.004(5) -0.002(5) 0.004(4) C24 0.038(6) 0.055(7) 0.041(7) -0.018(6) 0.001(5) 0.004(5) C25 0.029(5) 0.049(7) 0.037(6) -0.008(5) 0.003(4) 0.008(5) C26 0.053(7) 0.032(7) 0.091(10) 0.027(8) 0.031(7) 0.008(5) C27 0.034(6) 0.037(7) 0.060(7) -0.002(6) 0.011(5) -0.012(5) C28 0.031(5) 0.038(7) 0.061(8) -0.017(6) 0.021(5) 0.001(5) C29 0.045(6) 0.062(8) 0.044(7) 0.013(6) 0.015(5) 0.007(5) C30 0.053(7) 0.076(10) 0.077(10) 0.043(8) 0.012(7) 0.006(7) C31 0.029(5) 0.060(7) 0.052(6) -0.027(6) 0.002(5) -0.001(5) C32 0.076(5) 0.102(6) 0.132(6) -0.027(6) 0.028(5) -0.012(5) C33 0.044(6) 0.076(7) 0.086(7) -0.005(7) 0.020(5) 0.004(6) O 0.259(8) 0.262(8) 0.259(8) 0.009(7) -0.006(6) 0.019(7) C41 0.262(9) 0.255(9) 0.251(9) 0.024(7) -0.001(7) 0.020(7) C42 0.246(9) 0.255(9) 0.260(9) 0.013(7) -0.006(7) 0.026(7) C43 0.243(9) 0.252(9) 0.261(8) 0.022(7) 0.003(7) 0.012(7) C44 0.253(9) 0.249(9) 0.261(8) 0.025(7) 0.004(7) 0.007(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 Zn N2 2.040(6) . ? Zn N2 2.040(6) 5_666 ? Zn N1 2.046(6) . ? Zn N1 2.046(6) 5_666 ? Fe C23 2.013(9) . ? Fe C24 2.017(9) . ? Fe C29 2.024(9) . ? Fe C25 2.029(9) . ? Fe C30 2.031(10) . ? Fe C26 2.035(10) . ? Fe C28 2.044(9) . ? Fe C22 2.068(8) . ? Fe C27 2.074(9) . ? Fe C21 2.083(8) . ? S1 C32 1.615(12) . ? S1 C31 1.823(9) . ? S2 C33 1.821(9) . ? S2 C31 1.837(9) . ? N1 C1 1.362(9) . ? N1 C4 1.367(9) . ? N2 C6 1.370(9) . ? N2 C9 1.378(9) . ? C1 C10 1.401(10) 5_666 ? C1 C2 1.443(11) . ? C2 C3 1.328(10) . ? C3 C4 1.441(11) . ? C4 C5 1.397(10) . ? C5 C6 1.395(10) . ? C5 C11 1.531(11) . ? C6 C7 1.439(10) . ? C7 C8 1.310(10) . ? C8 C9 1.439(10) . ? C9 C10 1.410(10) . ? C10 C1 1.401(10) 5_666 ? C10 C21 1.502(11) . ? C11 C16 1.369(11) . ? C11 C12 1.376(11) . ? C12 C13 1.400(11) . ? C13 C14 1.353(11) . ? C14 C15 1.351(12) . ? C14 C17 1.531(11) . ? C15 C16 1.378(11) . ? C21 C25 1.414(11) . ? C21 C22 1.426(11) . ? C22 C23 1.414(11) . ? C23 C24 1.409(12) . ? C24 C25 1.411(11) . ? C26 C30 1.394(14) . ? C26 C27 1.416(13) . ? C27 C28 1.427(12) . ? C28 C29 1.410(13) . ? C28 C31 1.503(13) . ? C29 C30 1.411(13) . ? C32 C33 1.451(14) . ? O C41 1.422(15) . ? O C44 1.444(15) . ? C41 C42 1.410(16) . ? C42 C43 1.437(16) . ? C43 C44 1.425(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn N2 180.000(1) . 5_666 ? N2 Zn N1 90.9(2) . . ? N2 Zn N1 89.1(2) 5_666 . ? N2 Zn N1 89.1(2) . 5_666 ? N2 Zn N1 90.9(2) 5_666 5_666 ? N1 Zn N1 180.000(1) . 5_666 ? C23 Fe C24 40.9(3) . . ? C23 Fe C29 118.7(4) . . ? C24 Fe C29 102.0(4) . . ? C23 Fe C25 68.3(4) . . ? C24 Fe C25 40.8(3) . . ? C29 Fe C25 119.4(4) . . ? C23 Fe C30 154.5(5) . . ? C24 Fe C30 118.6(5) . . ? C29 Fe C30 40.7(4) . . ? C25 Fe C30 106.1(4) . . ? C23 Fe C26 162.8(5) . . ? C24 Fe C26 156.2(5) . . ? C29 Fe C26 68.2(4) . . ? C25 Fe C26 123.8(4) . . ? C30 Fe C26 40.1(4) . . ? C23 Fe C28 106.1(4) . . ? C24 Fe C28 119.3(4) . . ? C29 Fe C28 40.6(4) . . ? C25 Fe C28 155.4(4) . . ? C30 Fe C28 68.1(4) . . ? C26 Fe C28 68.1(4) . . ? C23 Fe C22 40.5(3) . . ? C24 Fe C22 68.1(4) . . ? C29 Fe C22 157.1(4) . . ? C25 Fe C22 67.3(4) . . ? C30 Fe C22 162.2(4) . . ? C26 Fe C22 128.6(4) . . ? C28 Fe C22 124.9(4) . . ? C23 Fe C27 125.0(4) . . ? C24 Fe C27 157.8(4) . . ? C29 Fe C27 68.1(4) . . ? C25 Fe C27 161.4(4) . . ? C30 Fe C27 67.6(5) . . ? C26 Fe C27 40.3(4) . . ? C28 Fe C27 40.5(3) . . ? C22 Fe C27 113.0(4) . . ? C23 Fe C21 68.4(3) . . ? C24 Fe C21 68.5(3) . . ? C29 Fe C21 157.2(4) . . ? C25 Fe C21 40.2(3) . . ? C30 Fe C21 124.3(4) . . ? C26 Fe C21 111.8(4) . . ? C28 Fe C21 162.1(4) . . ? C22 Fe C21 40.2(3) . . ? C27 Fe C21 127.7(3) . . ? C32 S1 C31 97.4(5) . . ? C33 S2 C31 98.6(5) . . ? C1 N1 C4 107.0(6) . . ? C1 N1 Zn 126.8(5) . . ? C4 N1 Zn 125.8(5) . . ? C6 N2 C9 106.4(6) . . ? C6 N2 Zn 125.6(5) . . ? C9 N2 Zn 127.9(5) . . ? N1 C1 C10 126.5(8) . 5_666 ? N1 C1 C2 108.6(7) . . ? C10 C1 C2 124.9(7) 5_666 . ? C3 C2 C1 108.2(7) . . ? C2 C3 C4 106.7(8) . . ? N1 C4 C5 124.9(7) . . ? N1 C4 C3 109.4(7) . . ? C5 C4 C3 125.7(8) . . ? C6 C5 C4 126.8(7) . . ? C6 C5 C11 116.5(7) . . ? C4 C5 C11 116.7(7) . . ? N2 C6 C5 125.4(7) . . ? N2 C6 C7 108.7(7) . . ? C5 C6 C7 125.8(8) . . ? C8 C7 C6 108.3(7) . . ? C7 C8 C9 107.7(7) . . ? N2 C9 C10 124.7(7) . . ? N2 C9 C8 108.8(7) . . ? C10 C9 C8 126.4(7) . . ? C1 C10 C9 124.3(7) 5_666 . ? C1 C10 C21 116.4(7) 5_666 . ? C9 C10 C21 118.8(7) . . ? C16 C11 C12 117.5(8) . . ? C16 C11 C5 121.5(8) . . ? C12 C11 C5 121.0(8) . . ? C11 C12 C13 119.4(9) . . ? C14 C13 C12 122.7(9) . . ? C15 C14 C13 117.1(9) . . ? C15 C14 C17 122.1(9) . . ? C13 C14 C17 120.8(9) . . ? C14 C15 C16 121.8(9) . . ? C11 C16 C15 121.5(9) . . ? C25 C21 C22 106.3(8) . . ? C25 C21 C10 125.9(7) . . ? C22 C21 C10 126.8(8) . . ? C25 C21 Fe 67.9(5) . . ? C22 C21 Fe 69.3(5) . . ? C10 C21 Fe 136.3(6) . . ? C23 C22 C21 108.5(8) . . ? C23 C22 Fe 67.7(5) . . ? C21 C22 Fe 70.5(5) . . ? C24 C23 C22 108.3(8) . . ? C24 C23 Fe 69.7(5) . . ? C22 C23 Fe 71.8(5) . . ? C23 C24 C25 107.2(8) . . ? C23 C24 Fe 69.4(5) . . ? C25 C24 Fe 70.1(5) . . ? C24 C25 C21 109.7(9) . . ? C24 C25 Fe 69.1(5) . . ? C21 C25 Fe 72.0(5) . . ? C30 C26 C27 108.8(10) . . ? C30 C26 Fe 69.8(7) . . ? C27 C26 Fe 71.3(6) . . ? C26 C27 C28 106.9(9) . . ? C26 C27 Fe 68.4(6) . . ? C28 C27 Fe 68.6(5) . . ? C29 C28 C27 108.0(9) . . ? C29 C28 C31 130.2(9) . . ? C27 C28 C31 121.7(10) . . ? C29 C28 Fe 68.9(5) . . ? C27 C28 Fe 70.8(5) . . ? C31 C28 Fe 129.0(7) . . ? C28 C29 C30 107.9(10) . . ? C28 C29 Fe 70.5(5) . . ? C30 C29 Fe 69.9(6) . . ? C26 C30 C29 108.4(10) . . ? C26 C30 Fe 70.1(6) . . ? C29 C30 Fe 69.4(6) . . ? C28 C31 S1 111.4(7) . . ? C28 C31 S2 112.0(6) . . ? S1 C31 S2 107.6(5) . . ? C33 C32 S1 120.6(10) . . ? C32 C33 S2 106.7(8) . . ? C41 O C44 98.4(11) . . ? C42 C41 O 101.8(13) . . ? C41 C42 C43 103.2(13) . . ? C44 C43 C42 103.0(10) . . ? C43 C44 O 108.1(11) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.744 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.105 # Attachment '- 10Zn_revised.cif' data_10Zn _database_code_depnum_ccdc_archive 'CCDC 893175' #TrackingRef '- 10Zn_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H55.50 Fe4 N4 O2 Zn' _chemical_formula_weight 1213.40 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 58.224(18) _cell_length_b 7.400(2) _cell_length_c 27.891(9) _cell_angle_alpha 90.00 _cell_angle_beta 110.088(5) _cell_angle_gamma 90.00 _cell_volume 11286(6) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6518 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 23.30 _exptl_crystal_description needle _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4988 _exptl_absorpt_coefficient_mu 1.471 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6667 _exptl_absorpt_correction_T_max 0.8914 _exptl_absorpt_process_details sadabs _exptl_special_details ; 11964 Reflections employed for parameter determination Rint decreases from 7.73 to 5.34 using Sadabs absorption correction ; _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 22893 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 64 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 23.30 _reflns_number_total 8100 _reflns_number_gt 6518 _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. Restraints were introduced and yield to a convergent refinement : for distances in thf solvent molecules (dfix instructions, 1.5 for C C distances and 1.45 for O C distances), and for anisotropic displacement parameters of all thf molecules (simu, delu and isor instructions). anisotropic displacement parameters of C45 were also restaint with isor instruction ; _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^)+(0.0991P)^2^+288.0086P] 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 8100 _refine_ls_number_parameters 775 _refine_ls_number_restraints 285 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.1088 _refine_ls_wR_factor_ref 0.2887 _refine_ls_wR_factor_gt 0.2746 _refine_ls_goodness_of_fit_ref 1.296 _refine_ls_restrained_S_all 1.277 _refine_ls_shift/su_max 0.089 _refine_ls_shift/su_mean 0.004 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 Zn Zn 0.62710(2) 0.6043(2) 0.61336(5) 0.0298(4) Uani 1 1 d . . . Fe1 Fe 0.71564(3) 0.9282(2) 0.79019(7) 0.0312(5) Uani 1 1 d . A . Fe2 Fe 0.65420(3) 0.2778(3) 0.42547(7) 0.0358(5) Uani 1 1 d . A . Fe3 Fe 0.53197(3) 0.8891(2) 0.44137(7) 0.0353(5) Uani 1 1 d . A . Fe4 Fe 0.57468(3) 0.1520(2) 0.74948(7) 0.0360(5) Uani 1 1 d . A . N1 N 0.64138(16) 0.5507(14) 0.6895(3) 0.028(2) Uani 1 1 d . A . N2 N 0.66173(16) 0.5870(14) 0.6119(3) 0.028(2) Uani 1 1 d . A . N3 N 0.61350(16) 0.5862(14) 0.5354(3) 0.030(2) Uani 1 1 d . A . N4 N 0.59324(16) 0.5481(14) 0.6151(3) 0.030(2) Uani 1 1 d . A . C1 C 0.62843(19) 0.5031(15) 0.7210(4) 0.025(3) Uani 1 1 d . . . C2 C 0.6439(2) 0.5327(17) 0.7733(4) 0.031(3) Uani 1 1 d . A . H2A H 0.6398 0.5096 0.8021 0.038 Uiso 1 1 calc R . . C3 C 0.6652(2) 0.5996(18) 0.7727(4) 0.035(3) Uani 1 1 d . . . H3A H 0.6784 0.6353 0.8010 0.042 Uiso 1 1 calc R A . C4 C 0.66388(19) 0.6058(16) 0.7205(4) 0.028(3) Uani 1 1 d . A . C5 C 0.6836(2) 0.6482(16) 0.7030(4) 0.028(3) Uani 1 1 d . . . C6 C 0.6826(2) 0.6184(17) 0.6521(4) 0.031(3) Uani 1 1 d . A . C7 C 0.7035(2) 0.6053(19) 0.6356(4) 0.038(3) Uani 1 1 d . . . H7A H 0.7198 0.6213 0.6556 0.045 Uiso 1 1 calc R A . C8 C 0.6945(2) 0.565(2) 0.5849(5) 0.041(3) Uani 1 1 d . A . H8A H 0.7038 0.5460 0.5640 0.050 Uiso 1 1 calc R . . C9 C 0.6683(2) 0.5564(17) 0.5692(5) 0.033(3) Uani 1 1 d . . . C10 C 0.6522(2) 0.5306(17) 0.5190(4) 0.029(3) Uani 1 1 d . A . C11 C 0.6270(2) 0.5634(17) 0.5034(4) 0.032(3) Uani 1 1 d . . . C12 C 0.6106(2) 0.5873(18) 0.4520(5) 0.039(3) Uani 1 1 d . A . H12A H 0.6147 0.5782 0.4226 0.047 Uiso 1 1 calc R . . C13 C 0.5881(2) 0.6258(18) 0.4540(5) 0.039(3) Uani 1 1 d . . . H13A H 0.5741 0.6530 0.4264 0.047 Uiso 1 1 calc R A . C14 C 0.5899(2) 0.6167(17) 0.5057(4) 0.033(3) Uani 1 1 d . A . C15 C 0.5701(2) 0.6244(16) 0.5242(4) 0.029(3) Uani 1 1 d . . . C16 C 0.5721(2) 0.5675(16) 0.5746(4) 0.030(3) Uani 1 1 d . A . C17 C 0.5517(2) 0.5096(18) 0.5887(5) 0.037(3) Uani 1 1 d . . . H17A H 0.5353 0.5122 0.5683 0.044 Uiso 1 1 calc R A . C18 C 0.5612(2) 0.4509(18) 0.6373(5) 0.038(3) Uani 1 1 d . A . H18A H 0.5525 0.3999 0.6564 0.046 Uiso 1 1 calc R . . C19 C 0.5870(2) 0.4810(17) 0.6544(4) 0.030(3) Uani 1 1 d . . . C20 C 0.6037(2) 0.4530(15) 0.7046(4) 0.023(2) Uani 1 1 d . A . C21 C 0.7076(2) 0.7161(16) 0.7388(4) 0.026(3) Uani 1 1 d . A . C22 C 0.7217(2) 0.8509(18) 0.7251(5) 0.034(3) Uani 1 1 d . . . H22A H 0.7169 0.9179 0.6929 0.041 Uiso 1 1 calc R A . C23 C 0.7443(2) 0.8694(19) 0.7670(5) 0.040(3) Uani 1 1 d . A . H23A H 0.7577 0.9515 0.7684 0.048 Uiso 1 1 calc R . . C24 C 0.7439(2) 0.7506(19) 0.8053(5) 0.043(3) Uani 1 1 d . . . H24A H 0.7571 0.7379 0.8383 0.052 Uiso 1 1 calc R A . C25 C 0.7217(2) 0.6522(17) 0.7900(4) 0.033(3) Uani 1 1 d . A . H25A H 0.7167 0.5600 0.8098 0.040 Uiso 1 1 calc R . . C26 C 0.6847(3) 1.050(2) 0.7921(7) 0.064(5) Uani 1 1 d . . . H26A H 0.6680 1.0141 0.7722 0.077 Uiso 1 1 calc R A . C27 C 0.6992(3) 1.178(2) 0.7763(7) 0.064(5) Uani 1 1 d . A . H27A H 0.6942 1.2449 0.7440 0.076 Uiso 1 1 calc R . . C28 C 0.7221(3) 1.190(2) 0.8170(7) 0.064(5) Uani 1 1 d . . . H28A H 0.7360 1.2656 0.8175 0.077 Uiso 1 1 calc R A . C29 C 0.7213(4) 1.066(3) 0.8570(7) 0.074(5) Uani 1 1 d . A . H29A H 0.7345 1.0448 0.8896 0.089 Uiso 1 1 calc R . . C30 C 0.6983(3) 0.989(2) 0.8411(7) 0.064(5) Uani 1 1 d . A . H30A H 0.6926 0.9001 0.8605 0.077 Uiso 1 1 calc R . . C31 C 0.6637(2) 0.4783(17) 0.4806(4) 0.031(3) Uani 1 1 d . . . C32 C 0.6621(2) 0.5486(17) 0.4332(5) 0.038(3) Uani 1 1 d . A . H32A H 0.6509 0.6453 0.4153 0.045 Uiso 1 1 calc R . . C33 C 0.6783(3) 0.457(2) 0.4142(5) 0.053(4) Uani 1 1 d . . . H33A H 0.6808 0.4811 0.3817 0.064 Uiso 1 1 calc R A . C34 C 0.6907(3) 0.330(2) 0.4502(6) 0.057(4) Uani 1 1 d . A . H34A H 0.7033 0.2474 0.4470 0.069 Uiso 1 1 calc R . . C35 C 0.6820(2) 0.331(2) 0.4888(5) 0.044(3) Uani 1 1 d U A . H35A H 0.6876 0.2525 0.5190 0.053 Uiso 1 1 calc R . . C36 C 0.6216(3) 0.167(2) 0.4225(7) 0.061(4) Uani 1 1 d . . . H36A H 0.6116 0.2067 0.4424 0.073 Uiso 1 1 calc R A . C37 C 0.6200(3) 0.235(2) 0.3730(6) 0.058(4) Uani 1 1 d . A . H37A H 0.6086 0.3275 0.3530 0.069 Uiso 1 1 calc R . . C38 C 0.6376(3) 0.142(2) 0.3586(6) 0.059(4) Uani 1 1 d . . . H38A H 0.6409 0.1604 0.3268 0.070 Uiso 1 1 calc R A . C39 C 0.6498(3) 0.020(2) 0.3969(6) 0.055(4) Uani 1 1 d . A . H39A H 0.6631 -0.0597 0.3962 0.066 Uiso 1 1 calc R . . C40 C 0.6403(3) 0.032(2) 0.4378(7) 0.064(5) Uani 1 1 d . A . H40A H 0.6454 -0.0381 0.4695 0.077 Uiso 1 1 calc R . . C41 C 0.5450(2) 0.6712(16) 0.4900(4) 0.029(3) Uani 1 1 d . A . C42 C 0.5288(2) 0.7795(18) 0.5065(5) 0.040(3) Uani 1 1 d . . . H42A H 0.5329 0.8399 0.5397 0.048 Uiso 1 1 calc R A . C43 C 0.5054(2) 0.786(2) 0.4654(5) 0.048(4) Uani 1 1 d . A . H43A H 0.4908 0.8499 0.4661 0.057 Uiso 1 1 calc R . . C44 C 0.5072(2) 0.681(2) 0.4244(6) 0.050(4) Uani 1 1 d . . . H44A H 0.4941 0.6594 0.3916 0.060 Uiso 1 1 calc R A . C45 C 0.5317(2) 0.6093(14) 0.4402(5) 0.033(3) Uani 1 1 d U A . H45A H 0.5384 0.5337 0.4192 0.039 Uiso 1 1 calc R . . C46 C 0.5602(3) 1.050(2) 0.4403(7) 0.063(5) Uani 1 1 d . . . H46A H 0.5776 1.0306 0.4595 0.076 Uiso 1 1 calc R A . C47 C 0.5432(4) 1.149(2) 0.4577(7) 0.078(6) Uani 1 1 d . A . H47A H 0.5469 1.2104 0.4907 0.094 Uiso 1 1 calc R . . C48 C 0.5202(3) 1.147(2) 0.4169(11) 0.092(8) Uani 1 1 d . . . H48A H 0.5050 1.2044 0.4168 0.111 Uiso 1 1 calc R A . C49 C 0.5236(4) 1.050(3) 0.3775(8) 0.078(5) Uani 1 1 d . A . H49A H 0.5106 1.0241 0.3449 0.094 Uiso 1 1 calc R . . C50 C 0.5475(3) 0.992(2) 0.3903(7) 0.058(4) Uani 1 1 d . A . H50A H 0.5543 0.9217 0.3686 0.070 Uiso 1 1 calc R . . C51 C 0.5952(2) 0.3782(16) 0.7457(4) 0.029(3) Uani 1 1 d . . . C52 C 0.5739(2) 0.4305(17) 0.7571(5) 0.036(3) Uani 1 1 d . A . H52A H 0.5609 0.5117 0.7367 0.043 Uiso 1 1 calc R . . C53 C 0.5745(3) 0.3376(19) 0.8018(5) 0.049(4) Uani 1 1 d . . . H53A H 0.5622 0.3474 0.8187 0.059 Uiso 1 1 calc R A . C54 C 0.5962(2) 0.2375(17) 0.8195(4) 0.033(3) Uani 1 1 d . A . H54A H 0.6015 0.1635 0.8506 0.040 Uiso 1 1 calc R . . C55 C 0.6085(2) 0.2535(16) 0.7842(4) 0.033(3) Uani 1 1 d . A . H55A H 0.6239 0.1945 0.7867 0.039 Uiso 1 1 calc R . . C56 C 0.5661(4) 0.001(3) 0.6843(8) 0.087(7) Uani 1 1 d . . . H56A H 0.5709 0.0254 0.6545 0.104 Uiso 1 1 calc R A . C57 C 0.5444(4) 0.058(3) 0.6918(7) 0.079(6) Uani 1 1 d . A . H57A H 0.5316 0.1333 0.6682 0.095 Uiso 1 1 calc R . . C58 C 0.5444(4) -0.010(3) 0.7404(8) 0.093(7) Uani 1 1 d . . . H58A H 0.5318 0.0096 0.7556 0.111 Uiso 1 1 calc R A . C59 C 0.5658(4) -0.105(2) 0.7615(7) 0.066(5) Uani 1 1 d . A . H59A H 0.5708 -0.1656 0.7948 0.079 Uiso 1 1 calc R . . C60 C 0.5794(4) -0.104(2) 0.7283(9) 0.077(6) Uani 1 1 d . A . H60A H 0.5951 -0.1644 0.7342 0.093 Uiso 1 1 calc R . . O1 O 0.6252(4) 0.901(3) 0.6144(9) 0.055(5) Uani 0.50 1 d PU A 1 O61 O 0.6216(6) 0.946(5) 0.6316(11) 0.095(7) Uani 0.50 1 d PDU B 2 C61 C 0.6440(6) 1.046(6) 0.6483(13) 0.092(7) Uani 0.50 1 d PDU B 2 H61A H 0.6571 0.9758 0.6717 0.111 Uiso 0.50 1 calc PR B 2 H61B H 0.6422 1.1578 0.6649 0.111 Uiso 0.50 1 calc PR B 2 C62 C 0.6486(6) 1.083(6) 0.5996(12) 0.092(7) Uani 0.50 1 d PDU B 2 H62A H 0.6536 1.2070 0.5977 0.110 Uiso 0.50 1 calc PR B 2 H62B H 0.6607 1.0015 0.5950 0.110 Uiso 0.50 1 calc PR B 2 C63 C 0.6240(6) 1.047(6) 0.5624(13) 0.087(7) Uani 0.50 1 d PDU B 2 H63A H 0.6197 1.1412 0.5366 0.104 Uiso 0.50 1 calc PR B 2 H63B H 0.6241 0.9327 0.5454 0.104 Uiso 0.50 1 calc PR B 2 C64 C 0.6055(6) 1.041(6) 0.5874(13) 0.090(6) Uani 0.50 1 d PDU B 2 H64A H 0.6008 1.1595 0.5955 0.108 Uiso 0.50 1 calc PR B 2 H64B H 0.5911 0.9710 0.5684 0.108 Uiso 0.50 1 calc PR B 2 O2 O 0.7343(11) 0.776(9) 0.503(2) 0.107(11) Uani 0.25 1 d PU C 1 O71 O 0.7295(9) 0.972(8) 0.485(2) 0.099(10) Uani 0.25 1 d PDU D 2 C71 C 0.7539(11) 0.921(12) 0.517(3) 0.099(10) Uani 0.25 1 d PDU D 2 H71A H 0.7668 0.9635 0.5048 0.119 Uiso 0.25 1 calc PR D 2 H71B H 0.7559 0.7939 0.5258 0.119 Uiso 0.25 1 calc PR D 2 C72 C 0.7490(14) 1.040(11) 0.555(3) 0.097(11) Uani 0.25 1 d PDU D 2 H72A H 0.7631 1.0465 0.5865 0.116 Uiso 0.25 1 calc PR D 2 H72B H 0.7445 1.1612 0.5421 0.116 Uiso 0.25 1 calc PR D 2 C73 C 0.7281(13) 0.945(12) 0.563(3) 0.096(11) Uani 0.25 1 d PDU D 2 H73A H 0.7178 1.0276 0.5740 0.116 Uiso 0.25 1 calc PR D 2 H73B H 0.7335 0.8480 0.5882 0.116 Uiso 0.25 1 calc PR D 2 C74 C 0.7157(14) 0.876(11) 0.511(2) 0.097(10) Uani 0.25 1 d PDU D 2 H74A H 0.7173 0.7458 0.5086 0.116 Uiso 0.25 1 calc PR D 2 H74B H 0.6985 0.9082 0.4975 0.116 Uiso 0.25 1 calc PR D 2 O81 O 0.4949(9) 0.379(6) 0.7121(17) 0.147(10) Uani 0.50 1 d PDU E -1 C81 C 0.4984(17) 0.348(8) 0.7655(18) 0.146(11) Uani 0.50 1 d PDU E -1 H81A H 0.5138 0.2855 0.7822 0.176 Uiso 0.50 1 calc PR E -1 H81B H 0.4852 0.2750 0.7688 0.176 Uiso 0.50 1 calc PR E -1 C82 C 0.4987(12) 0.532(7) 0.789(2) 0.144(11) Uani 0.50 1 d PDU E -1 H82A H 0.4824 0.5650 0.7881 0.173 Uiso 0.50 1 calc PR E -1 H82B H 0.5097 0.5341 0.8239 0.173 Uiso 0.50 1 calc PR E -1 C83 C 0.5072(10) 0.659(7) 0.7566(19) 0.143(11) Uani 0.50 1 d PDU E -1 H83A H 0.5244 0.6456 0.7611 0.172 Uiso 0.50 1 calc PR E -1 H83B H 0.5033 0.7848 0.7604 0.172 Uiso 0.50 1 calc PR E -1 C84 C 0.4904(12) 0.573(6) 0.709(2) 0.147(11) Uani 0.50 1 d PDU E -1 H84A H 0.4735 0.5967 0.7052 0.176 Uiso 0.50 1 calc PR E -1 H84B H 0.4934 0.6219 0.6792 0.176 Uiso 0.50 1 calc PR E -1 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 Zn 0.0259(7) 0.0427(9) 0.0216(7) 0.0018(6) 0.0093(6) -0.0029(6) Fe1 0.0391(10) 0.0257(10) 0.0338(10) -0.0063(8) 0.0191(8) -0.0069(8) Fe2 0.0415(11) 0.0397(11) 0.0289(10) -0.0062(9) 0.0154(8) -0.0062(9) Fe3 0.0333(10) 0.0289(10) 0.0439(11) 0.0107(9) 0.0136(8) 0.0024(8) Fe4 0.0387(10) 0.0264(10) 0.0393(11) 0.0095(9) 0.0089(9) -0.0063(8) N1 0.027(5) 0.044(6) 0.014(5) 0.006(5) 0.007(4) -0.007(5) N2 0.021(5) 0.044(6) 0.021(5) -0.004(5) 0.008(4) 0.001(5) N3 0.025(5) 0.046(6) 0.017(5) 0.004(5) 0.006(4) 0.008(5) N4 0.025(5) 0.041(6) 0.023(5) 0.003(5) 0.005(4) -0.007(5) C1 0.023(6) 0.023(6) 0.036(7) 0.001(5) 0.016(5) -0.002(5) C2 0.035(7) 0.041(8) 0.015(6) 0.007(5) 0.006(5) -0.012(6) C3 0.037(7) 0.051(8) 0.017(6) -0.001(6) 0.010(5) -0.017(6) C4 0.023(6) 0.031(7) 0.026(6) -0.010(5) 0.004(5) -0.007(5) C5 0.034(6) 0.030(7) 0.020(6) -0.004(5) 0.012(5) -0.004(5) C6 0.027(6) 0.042(8) 0.028(7) -0.004(6) 0.014(5) 0.005(6) C7 0.024(6) 0.059(9) 0.027(7) -0.004(7) 0.006(5) -0.003(6) C8 0.028(7) 0.064(10) 0.037(8) -0.023(7) 0.017(6) -0.007(6) C9 0.036(7) 0.036(7) 0.029(7) -0.005(6) 0.015(6) -0.002(6) C10 0.025(6) 0.036(7) 0.028(7) -0.011(6) 0.012(5) -0.005(5) C11 0.042(7) 0.035(7) 0.020(6) -0.003(6) 0.014(6) -0.001(6) C12 0.043(7) 0.048(8) 0.023(7) -0.003(6) 0.008(6) 0.010(7) C13 0.034(7) 0.048(9) 0.035(7) -0.002(6) 0.010(6) 0.011(6) C14 0.040(7) 0.037(8) 0.019(6) 0.001(6) 0.006(5) 0.002(6) C15 0.025(6) 0.028(7) 0.032(7) 0.001(5) 0.007(5) -0.005(5) C16 0.029(6) 0.027(7) 0.033(7) 0.008(6) 0.010(6) -0.005(5) C17 0.019(6) 0.051(9) 0.034(7) 0.020(7) 0.000(5) 0.001(6) C18 0.030(7) 0.046(8) 0.040(8) 0.008(7) 0.012(6) -0.004(6) C19 0.026(6) 0.036(7) 0.032(7) 0.008(6) 0.012(5) -0.004(5) C20 0.031(6) 0.020(6) 0.021(6) 0.001(5) 0.012(5) 0.001(5) C21 0.024(6) 0.031(7) 0.024(6) -0.001(5) 0.010(5) -0.007(5) C22 0.036(7) 0.041(8) 0.025(6) -0.011(6) 0.011(6) -0.008(6) C23 0.033(7) 0.050(9) 0.043(8) -0.019(7) 0.021(6) -0.022(6) C24 0.031(7) 0.044(8) 0.047(8) -0.008(7) 0.004(6) -0.005(6) C25 0.033(7) 0.034(7) 0.022(6) -0.003(6) -0.005(5) -0.002(6) C26 0.056(10) 0.052(10) 0.094(14) -0.015(10) 0.040(10) 0.006(8) C27 0.080(12) 0.029(8) 0.088(13) -0.007(9) 0.037(11) 0.009(8) C28 0.066(11) 0.034(9) 0.100(14) -0.014(9) 0.038(11) -0.009(8) C29 0.094(14) 0.079(13) 0.061(11) -0.030(10) 0.043(10) -0.006(11) C30 0.093(13) 0.049(10) 0.080(13) -0.013(9) 0.068(11) 0.001(10) C31 0.035(7) 0.040(8) 0.018(6) 0.000(6) 0.009(5) 0.004(6) C32 0.044(8) 0.030(7) 0.040(8) -0.002(6) 0.016(6) -0.014(6) C33 0.044(8) 0.087(12) 0.037(8) -0.030(9) 0.027(7) -0.038(9) C34 0.036(8) 0.083(12) 0.049(9) -0.027(9) 0.010(7) 0.009(8) C35 0.028(6) 0.063(7) 0.032(6) 0.008(6) -0.003(5) -0.012(6) C36 0.053(9) 0.055(10) 0.086(13) -0.020(9) 0.041(9) -0.021(8) C37 0.044(9) 0.044(9) 0.072(11) -0.007(9) 0.003(8) -0.016(7) C38 0.074(11) 0.054(10) 0.052(10) -0.022(9) 0.026(9) -0.020(9) C39 0.077(11) 0.034(8) 0.053(10) -0.008(8) 0.022(9) 0.001(8) C40 0.091(13) 0.047(10) 0.076(12) -0.004(9) 0.055(11) -0.022(9) C41 0.024(6) 0.028(7) 0.033(7) 0.009(6) 0.006(5) -0.004(5) C42 0.036(7) 0.045(8) 0.039(8) 0.021(7) 0.014(6) 0.008(6) C43 0.038(8) 0.060(10) 0.055(9) 0.014(8) 0.028(7) 0.005(7) C44 0.023(7) 0.055(9) 0.056(9) 0.032(8) -0.006(6) 0.006(6) C45 0.037(6) 0.004(5) 0.042(6) 0.005(5) -0.005(5) 0.003(5) C46 0.050(9) 0.050(10) 0.085(13) 0.019(10) 0.018(9) -0.021(8) C47 0.15(2) 0.023(8) 0.081(13) -0.014(9) 0.061(14) -0.038(11) C48 0.049(10) 0.044(11) 0.19(3) 0.059(14) 0.045(14) 0.022(9) C49 0.091(15) 0.062(13) 0.076(13) 0.032(11) 0.023(11) 0.000(11) C50 0.069(11) 0.049(10) 0.068(11) 0.026(9) 0.038(9) 0.002(9) C51 0.033(6) 0.028(7) 0.028(6) 0.003(6) 0.012(5) -0.009(6) C52 0.029(6) 0.028(7) 0.057(9) -0.015(6) 0.025(6) -0.005(6) C53 0.067(10) 0.041(8) 0.058(9) -0.002(7) 0.045(8) -0.027(8) C54 0.048(8) 0.034(7) 0.010(6) 0.007(5) 0.001(5) 0.004(6) C55 0.036(7) 0.028(7) 0.033(7) 0.009(6) 0.008(6) -0.005(6) C56 0.121(18) 0.079(15) 0.069(13) -0.035(12) 0.043(13) -0.045(14) C57 0.074(12) 0.066(12) 0.069(12) 0.012(10) -0.012(10) -0.039(11) C58 0.067(12) 0.100(16) 0.099(16) 0.024(13) 0.013(11) -0.041(12) C59 0.089(13) 0.026(8) 0.057(11) 0.005(8) -0.009(10) -0.025(9) C60 0.076(12) 0.024(9) 0.105(16) -0.016(10) -0.002(12) 0.008(8) O1 0.082(11) 0.033(10) 0.072(11) -0.002(9) 0.055(9) -0.013(8) O61 0.101(9) 0.093(10) 0.090(9) 0.019(7) 0.031(7) 0.002(7) C61 0.097(9) 0.088(10) 0.086(8) 0.001(8) 0.023(6) 0.013(7) C62 0.092(8) 0.090(10) 0.095(10) 0.004(8) 0.033(7) 0.004(8) C63 0.094(9) 0.086(10) 0.081(8) 0.004(8) 0.032(6) -0.002(8) C64 0.092(8) 0.087(10) 0.088(9) 0.004(8) 0.027(6) -0.002(8) O2 0.107(14) 0.105(14) 0.105(14) 0.002(11) 0.031(11) -0.004(11) O71 0.100(12) 0.099(12) 0.097(11) 0.000(8) 0.034(7) 0.000(8) C71 0.098(11) 0.101(13) 0.099(12) 0.000(8) 0.034(7) -0.003(8) C72 0.095(13) 0.098(13) 0.097(12) 0.001(8) 0.033(8) -0.002(7) C73 0.095(13) 0.097(14) 0.096(12) 0.002(8) 0.032(8) -0.001(8) C74 0.097(12) 0.096(13) 0.097(12) 0.001(7) 0.032(8) -0.001(7) O81 0.152(13) 0.145(12) 0.144(12) -0.003(7) 0.050(9) 0.001(8) C81 0.148(14) 0.144(12) 0.146(13) 0.004(7) 0.050(9) -0.004(8) C82 0.145(14) 0.148(13) 0.143(12) 0.000(7) 0.053(9) -0.002(8) C83 0.145(14) 0.141(12) 0.145(13) 0.002(7) 0.050(8) 0.000(8) C84 0.149(14) 0.146(12) 0.143(12) 0.003(7) 0.049(8) 0.002(8) _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 Zn N4 2.031(9) . ? Zn N2 2.035(9) . ? Zn N1 2.036(9) . ? Zn N3 2.047(9) . ? Zn O1 2.20(2) . ? Fe1 C26 2.031(15) . ? Fe1 C23 2.032(12) . ? Fe1 C24 2.035(14) . ? Fe1 C22 2.046(11) . ? Fe1 C29 2.051(16) . ? Fe1 C27 2.057(15) . ? Fe1 C30 2.057(14) . ? Fe1 C28 2.062(16) . ? Fe1 C21 2.068(12) . ? Fe1 C25 2.073(13) . ? Fe2 C35 1.982(12) . ? Fe2 C34 2.034(14) . ? Fe2 C33 2.034(13) . ? Fe2 C36 2.043(14) . ? Fe2 C38 2.047(15) . ? Fe2 C39 2.048(14) . ? Fe2 C32 2.051(13) . ? Fe2 C37 2.052(14) . ? Fe2 C40 2.064(15) . ? Fe2 C31 2.070(12) . ? Fe3 C43 2.035(13) . ? Fe3 C47 2.035(15) . ? Fe3 C46 2.039(14) . ? Fe3 C42 2.054(12) . ? Fe3 C44 2.054(14) . ? Fe3 C49 2.059(17) . ? Fe3 C48 2.066(16) . ? Fe3 C45 2.071(11) . ? Fe3 C41 2.076(12) . ? Fe3 C50 2.078(14) . ? Fe4 C53 2.008(14) . ? Fe4 C55 2.017(12) . ? Fe4 C54 2.026(11) . ? Fe4 C60 2.030(16) . ? Fe4 C59 2.032(15) . ? Fe4 C56 2.045(17) . ? Fe4 C57 2.057(16) . ? Fe4 C58 2.073(17) . ? Fe4 C52 2.074(12) . ? Fe4 C51 2.081(11) . ? N1 C4 1.360(14) . ? N1 C1 1.386(13) . ? N2 C6 1.362(15) . ? N2 C9 1.390(14) . ? N3 C14 1.359(15) . ? N3 C11 1.385(14) . ? N4 C16 1.362(14) . ? N4 C19 1.363(14) . ? C1 C20 1.406(15) . ? C1 C2 1.443(16) . ? C2 C3 1.344(16) . ? C3 C4 1.433(15) . ? C4 C5 1.429(15) . ? C5 C6 1.418(15) . ? C5 C21 1.496(16) . ? C6 C7 1.446(16) . ? C7 C8 1.360(17) . ? C8 C9 1.439(16) . ? C9 C10 1.404(16) . ? C10 C11 1.403(16) . ? C10 C31 1.499(15) . ? C11 C12 1.434(17) . ? C12 C13 1.364(17) . ? C13 C14 1.411(16) . ? C14 C15 1.415(16) . ? C15 C16 1.432(16) . ? C15 C41 1.488(16) . ? C16 C17 1.436(16) . ? C17 C18 1.349(17) . ? C18 C19 1.430(16) . ? C19 C20 1.416(16) . ? C20 C51 1.501(15) . ? C21 C22 1.424(16) . ? C21 C25 1.459(16) . ? C22 C23 1.435(17) . ? C23 C24 1.388(19) . ? C24 C25 1.420(17) . ? C26 C30 1.40(2) . ? C26 C27 1.43(2) . ? C27 C28 1.43(2) . ? C28 C29 1.46(2) . ? C29 C30 1.39(2) . ? C31 C32 1.392(17) . ? C31 C35 1.485(19) . ? C32 C33 1.407(19) . ? C33 C34 1.38(2) . ? C34 C35 1.341(19) . ? C36 C40 1.43(2) . ? C36 C37 1.44(2) . ? C37 C38 1.40(2) . ? C38 C39 1.39(2) . ? C39 C40 1.43(2) . ? C41 C45 1.414(17) . ? C41 C42 1.426(17) . ? C42 C43 1.451(19) . ? C43 C44 1.41(2) . ? C44 C45 1.445(17) . ? C46 C50 1.40(2) . ? C46 C47 1.44(2) . ? C47 C48 1.43(3) . ? C48 C49 1.38(3) . ? C49 C50 1.38(2) . ? C51 C55 1.425(17) . ? C51 C52 1.435(16) . ? C52 C53 1.415(18) . ? C53 C54 1.401(19) . ? C54 C55 1.408(17) . ? C56 C57 1.41(3) . ? C56 C60 1.43(3) . ? C57 C58 1.45(3) . ? C58 C59 1.37(3) . ? C59 C60 1.41(3) . ? O61 C61 1.429(19) . ? O61 C64 1.449(19) . ? C61 C62 1.498(19) . ? C62 C63 1.477(19) . ? C63 C64 1.471(19) . ? O71 C74 1.44(2) . ? O71 C71 1.44(2) . ? C71 C72 1.49(2) . ? C72 C73 1.49(2) . ? C73 C74 1.49(2) . ? O81 C81 1.452(19) . ? O81 C84 1.45(2) . ? C81 C82 1.51(2) . ? C82 C83 1.50(2) . ? C83 C84 1.50(2) . ? 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 N4 Zn N2 164.6(4) . . ? N4 Zn N1 89.3(4) . . ? N2 Zn N1 87.5(4) . . ? N4 Zn N3 89.3(4) . . ? N2 Zn N3 89.9(3) . . ? N1 Zn N3 164.9(4) . . ? N4 Zn O1 98.6(6) . . ? N2 Zn O1 96.8(6) . . ? N1 Zn O1 100.7(7) . . ? N3 Zn O1 94.4(7) . . ? C26 Fe1 C23 159.3(7) . . ? C26 Fe1 C24 160.7(7) . . ? C23 Fe1 C24 39.9(5) . . ? C26 Fe1 C22 124.9(7) . . ? C23 Fe1 C22 41.2(5) . . ? C24 Fe1 C22 68.2(5) . . ? C26 Fe1 C29 67.8(8) . . ? C23 Fe1 C29 120.1(6) . . ? C24 Fe1 C29 105.5(7) . . ? C22 Fe1 C29 157.3(6) . . ? C26 Fe1 C27 41.0(6) . . ? C23 Fe1 C27 120.9(6) . . ? C24 Fe1 C27 155.7(6) . . ? C22 Fe1 C27 107.2(6) . . ? C29 Fe1 C27 69.1(8) . . ? C26 Fe1 C30 40.0(7) . . ? C23 Fe1 C30 156.7(7) . . ? C24 Fe1 C30 123.6(7) . . ? C22 Fe1 C30 161.7(7) . . ? C29 Fe1 C30 39.4(7) . . ? C27 Fe1 C30 68.0(7) . . ? C26 Fe1 C28 68.1(7) . . ? C23 Fe1 C28 104.4(6) . . ? C24 Fe1 C28 119.8(6) . . ? C22 Fe1 C28 121.2(6) . . ? C29 Fe1 C28 41.5(7) . . ? C27 Fe1 C28 40.6(6) . . ? C30 Fe1 C28 67.5(7) . . ? C26 Fe1 C21 111.4(6) . . ? C23 Fe1 C21 68.4(5) . . ? C24 Fe1 C21 68.1(5) . . ? C22 Fe1 C21 40.5(5) . . ? C29 Fe1 C21 159.4(7) . . ? C27 Fe1 C21 124.8(6) . . ? C30 Fe1 C21 126.6(6) . . ? C28 Fe1 C21 158.9(6) . . ? C26 Fe1 C25 126.2(6) . . ? C23 Fe1 C25 68.3(5) . . ? C24 Fe1 C25 40.4(5) . . ? C22 Fe1 C25 69.0(5) . . ? C29 Fe1 C25 121.3(7) . . ? C27 Fe1 C25 162.4(6) . . ? C30 Fe1 C25 110.0(6) . . ? C28 Fe1 C25 156.3(6) . . ? C21 Fe1 C25 41.3(4) . . ? C35 Fe2 C34 39.0(5) . . ? C35 Fe2 C33 67.3(6) . . ? C34 Fe2 C33 39.7(6) . . ? C35 Fe2 C36 125.3(6) . . ? C34 Fe2 C36 159.8(7) . . ? C33 Fe2 C36 159.6(7) . . ? C35 Fe2 C38 153.5(7) . . ? C34 Fe2 C38 120.9(6) . . ? C33 Fe2 C38 108.4(6) . . ? C36 Fe2 C38 67.9(6) . . ? C35 Fe2 C39 119.0(6) . . ? C34 Fe2 C39 106.5(7) . . ? C33 Fe2 C39 123.1(6) . . ? C36 Fe2 C39 67.7(7) . . ? C38 Fe2 C39 39.7(6) . . ? C35 Fe2 C32 68.2(6) . . ? C34 Fe2 C32 66.9(6) . . ? C33 Fe2 C32 40.3(6) . . ? C36 Fe2 C32 124.7(6) . . ? C38 Fe2 C32 126.5(6) . . ? C39 Fe2 C32 160.7(6) . . ? C35 Fe2 C37 164.1(6) . . ? C34 Fe2 C37 156.4(7) . . ? C33 Fe2 C37 122.9(7) . . ? C36 Fe2 C37 41.3(6) . . ? C38 Fe2 C37 40.0(6) . . ? C39 Fe2 C37 67.6(7) . . ? C32 Fe2 C37 110.7(6) . . ? C35 Fe2 C40 105.8(7) . . ? C34 Fe2 C40 122.3(8) . . ? C33 Fe2 C40 158.5(7) . . ? C36 Fe2 C40 40.7(7) . . ? C38 Fe2 C40 68.3(7) . . ? C39 Fe2 C40 40.8(6) . . ? C32 Fe2 C40 158.2(6) . . ? C37 Fe2 C40 69.1(7) . . ? C35 Fe2 C31 42.9(5) . . ? C34 Fe2 C31 68.3(5) . . ? C33 Fe2 C31 67.9(5) . . ? C36 Fe2 C31 109.1(6) . . ? C38 Fe2 C31 162.1(6) . . ? C39 Fe2 C31 157.2(6) . . ? C32 Fe2 C31 39.5(5) . . ? C37 Fe2 C31 126.0(6) . . ? C40 Fe2 C31 121.8(6) . . ? C43 Fe3 C47 120.3(7) . . ? C43 Fe3 C46 158.9(7) . . ? C47 Fe3 C46 41.5(7) . . ? C43 Fe3 C42 41.6(5) . . ? C47 Fe3 C42 107.2(7) . . ? C46 Fe3 C42 124.1(6) . . ? C43 Fe3 C44 40.5(6) . . ? C47 Fe3 C44 155.3(8) . . ? C46 Fe3 C44 160.5(7) . . ? C42 Fe3 C44 68.8(6) . . ? C43 Fe3 C49 121.4(7) . . ? C47 Fe3 C49 66.9(8) . . ? C46 Fe3 C49 66.5(7) . . ? C42 Fe3 C49 158.0(7) . . ? C44 Fe3 C49 107.2(7) . . ? C43 Fe3 C48 104.7(7) . . ? C47 Fe3 C48 40.8(8) . . ? C46 Fe3 C48 68.4(7) . . ? C42 Fe3 C48 122.5(8) . . ? C44 Fe3 C48 119.4(7) . . ? C49 Fe3 C48 39.2(8) . . ? C43 Fe3 C45 68.1(6) . . ? C47 Fe3 C45 161.8(8) . . ? C46 Fe3 C45 125.8(6) . . ? C42 Fe3 C45 67.5(6) . . ? C44 Fe3 C45 41.0(5) . . ? C49 Fe3 C45 124.5(7) . . ? C48 Fe3 C45 156.9(8) . . ? C43 Fe3 C41 68.9(5) . . ? C47 Fe3 C41 124.9(7) . . ? C46 Fe3 C41 110.4(6) . . ? C42 Fe3 C41 40.4(5) . . ? C44 Fe3 C41 68.7(5) . . ? C49 Fe3 C41 160.2(8) . . ? C48 Fe3 C41 160.0(9) . . ? C45 Fe3 C41 39.9(5) . . ? C43 Fe3 C50 157.4(6) . . ? C47 Fe3 C50 67.9(7) . . ? C46 Fe3 C50 39.8(6) . . ? C42 Fe3 C50 160.6(6) . . ? C44 Fe3 C50 123.8(7) . . ? C49 Fe3 C50 39.1(7) . . ? C48 Fe3 C50 66.9(8) . . ? C45 Fe3 C50 111.0(6) . . ? C41 Fe3 C50 125.9(6) . . ? C53 Fe4 C55 69.2(6) . . ? C53 Fe4 C54 40.6(6) . . ? C55 Fe4 C54 40.8(5) . . ? C53 Fe4 C60 152.2(8) . . ? C55 Fe4 C60 106.2(7) . . ? C54 Fe4 C60 118.1(7) . . ? C53 Fe4 C59 117.0(7) . . ? C55 Fe4 C59 122.2(6) . . ? C54 Fe4 C59 104.0(6) . . ? C60 Fe4 C59 40.7(8) . . ? C53 Fe4 C56 163.7(9) . . ? C55 Fe4 C56 122.0(7) . . ? C54 Fe4 C56 155.4(8) . . ? C60 Fe4 C56 41.2(8) . . ? C59 Fe4 C56 68.7(8) . . ? C53 Fe4 C57 125.6(8) . . ? C55 Fe4 C57 159.1(7) . . ? C54 Fe4 C57 160.0(7) . . ? C60 Fe4 C57 67.8(8) . . ? C59 Fe4 C57 67.3(7) . . ? C56 Fe4 C57 40.3(8) . . ? C53 Fe4 C58 105.5(8) . . ? C55 Fe4 C58 157.3(7) . . ? C54 Fe4 C58 121.1(7) . . ? C60 Fe4 C58 67.6(9) . . ? C59 Fe4 C58 39.0(7) . . ? C56 Fe4 C58 68.7(9) . . ? C57 Fe4 C58 41.0(7) . . ? C53 Fe4 C52 40.5(5) . . ? C55 Fe4 C52 68.4(5) . . ? C54 Fe4 C52 67.6(5) . . ? C60 Fe4 C52 165.1(8) . . ? C59 Fe4 C52 153.9(7) . . ? C56 Fe4 C52 128.8(8) . . ? C57 Fe4 C52 111.9(7) . . ? C58 Fe4 C52 122.7(8) . . ? C53 Fe4 C51 68.5(5) . . ? C55 Fe4 C51 40.7(5) . . ? C54 Fe4 C51 67.8(5) . . ? C60 Fe4 C51 126.7(7) . . ? C59 Fe4 C51 161.1(7) . . ? C56 Fe4 C51 111.4(7) . . ? C57 Fe4 C51 125.8(6) . . ? C58 Fe4 C51 159.8(7) . . ? C52 Fe4 C51 40.4(4) . . ? C4 N1 C1 106.8(9) . . ? C4 N1 Zn 124.3(7) . . ? C1 N1 Zn 126.5(7) . . ? C6 N2 C9 107.7(9) . . ? C6 N2 Zn 125.7(7) . . ? C9 N2 Zn 126.4(8) . . ? C14 N3 C11 107.8(9) . . ? C14 N3 Zn 125.3(7) . . ? C11 N3 Zn 126.4(8) . . ? C16 N4 C19 107.0(9) . . ? C16 N4 Zn 124.6(7) . . ? C19 N4 Zn 128.5(8) . . ? N1 C1 C20 125.6(10) . . ? N1 C1 C2 108.5(9) . . ? C20 C1 C2 125.7(10) . . ? C3 C2 C1 107.6(10) . . ? C2 C3 C4 107.2(10) . . ? N1 C4 C5 124.2(10) . . ? N1 C4 C3 109.9(9) . . ? C5 C4 C3 125.7(10) . . ? C6 C5 C4 123.0(10) . . ? C6 C5 C21 115.4(10) . . ? C4 C5 C21 121.5(9) . . ? N2 C6 C5 124.8(10) . . ? N2 C6 C7 109.7(10) . . ? C5 C6 C7 125.5(11) . . ? C8 C7 C6 106.3(10) . . ? C7 C8 C9 108.4(10) . . ? N2 C9 C10 126.2(10) . . ? N2 C9 C8 107.9(10) . . ? C10 C9 C8 125.9(10) . . ? C11 C10 C9 123.8(10) . . ? C11 C10 C31 120.1(10) . . ? C9 C10 C31 115.9(10) . . ? N3 C11 C10 125.8(11) . . ? N3 C11 C12 107.6(10) . . ? C10 C11 C12 126.6(11) . . ? C13 C12 C11 107.6(11) . . ? C12 C13 C14 107.3(11) . . ? N3 C14 C13 109.6(10) . . ? N3 C14 C15 124.3(10) . . ? C13 C14 C15 125.9(11) . . ? C14 C15 C16 123.0(10) . . ? C14 C15 C41 121.3(10) . . ? C16 C15 C41 115.3(10) . . ? N4 C16 C15 126.1(10) . . ? N4 C16 C17 109.7(10) . . ? C15 C16 C17 124.0(10) . . ? C18 C17 C16 106.4(10) . . ? C17 C18 C19 107.7(11) . . ? N4 C19 C20 124.6(10) . . ? N4 C19 C18 109.2(10) . . ? C20 C19 C18 126.2(10) . . ? C1 C20 C19 124.1(10) . . ? C1 C20 C51 114.6(10) . . ? C19 C20 C51 121.1(10) . . ? C22 C21 C25 107.9(10) . . ? C22 C21 C5 123.3(10) . . ? C25 C21 C5 128.6(10) . . ? C22 C21 Fe1 68.9(7) . . ? C25 C21 Fe1 69.5(7) . . ? C5 C21 Fe1 130.9(8) . . ? C21 C22 C23 107.5(11) . . ? C21 C22 Fe1 70.6(7) . . ? C23 C22 Fe1 68.9(7) . . ? C24 C23 C22 108.3(11) . . ? C24 C23 Fe1 70.2(7) . . ? C22 C23 Fe1 69.9(7) . . ? C23 C24 C25 110.3(12) . . ? C23 C24 Fe1 69.9(8) . . ? C25 C24 Fe1 71.2(7) . . ? C24 C25 C21 106.0(11) . . ? C24 C25 Fe1 68.4(8) . . ? C21 C25 Fe1 69.2(7) . . ? C30 C26 C27 108.8(16) . . ? C30 C26 Fe1 71.0(9) . . ? C27 C26 Fe1 70.5(9) . . ? C28 C27 C26 106.5(16) . . ? C28 C27 Fe1 69.9(9) . . ? C26 C27 Fe1 68.6(9) . . ? C27 C28 C29 107.7(15) . . ? C27 C28 Fe1 69.5(9) . . ? C29 C28 Fe1 68.8(9) . . ? C30 C29 C28 107.2(17) . . ? C30 C29 Fe1 70.5(9) . . ? C28 C29 Fe1 69.7(9) . . ? C29 C30 C26 109.8(16) . . ? C29 C30 Fe1 70.0(9) . . ? C26 C30 Fe1 69.0(8) . . ? C32 C31 C35 103.6(10) . . ? C32 C31 C10 132.9(12) . . ? C35 C31 C10 123.5(11) . . ? C32 C31 Fe2 69.5(7) . . ? C35 C31 Fe2 65.4(7) . . ? C10 C31 Fe2 130.1(9) . . ? C31 C32 C33 110.0(13) . . ? C31 C32 Fe2 71.0(7) . . ? C33 C32 Fe2 69.2(8) . . ? C34 C33 C32 107.7(12) . . ? C34 C33 Fe2 70.1(9) . . ? C32 C33 Fe2 70.5(7) . . ? C35 C34 C33 109.5(13) . . ? C35 C34 Fe2 68.4(8) . . ? C33 C34 Fe2 70.1(8) . . ? C34 C35 C31 109.0(13) . . ? C34 C35 Fe2 72.6(8) . . ? C31 C35 Fe2 71.7(7) . . ? C40 C36 C37 108.9(14) . . ? C40 C36 Fe2 70.5(8) . . ? C37 C36 Fe2 69.7(8) . . ? C38 C37 C36 106.7(15) . . ? C38 C37 Fe2 69.8(9) . . ? C36 C37 Fe2 69.0(8) . . ? C39 C38 C37 109.3(15) . . ? C39 C38 Fe2 70.2(9) . . ? C37 C38 Fe2 70.2(8) . . ? C38 C39 C40 109.5(15) . . ? C38 C39 Fe2 70.1(9) . . ? C40 C39 Fe2 70.2(8) . . ? C36 C40 C39 105.6(15) . . ? C36 C40 Fe2 68.9(9) . . ? C39 C40 Fe2 69.0(8) . . ? C45 C41 C42 107.6(10) . . ? C45 C41 C15 129.7(11) . . ? C42 C41 C15 122.4(11) . . ? C45 C41 Fe3 69.9(6) . . ? C42 C41 Fe3 69.0(7) . . ? C15 C41 Fe3 131.1(8) . . ? C41 C42 C43 107.9(12) . . ? C41 C42 Fe3 70.6(7) . . ? C43 C42 Fe3 68.5(7) . . ? C44 C43 C42 108.2(12) . . ? C44 C43 Fe3 70.5(8) . . ? C42 C43 Fe3 69.9(7) . . ? C43 C44 C45 107.1(12) . . ? C43 C44 Fe3 69.0(8) . . ? C45 C44 Fe3 70.1(7) . . ? C41 C45 C44 109.2(12) . . ? C41 C45 Fe3 70.3(7) . . ? C44 C45 Fe3 68.9(7) . . ? C50 C46 C47 107.6(15) . . ? C50 C46 Fe3 71.6(8) . . ? C47 C46 Fe3 69.1(8) . . ? C48 C47 C46 106.9(17) . . ? C48 C47 Fe3 70.8(10) . . ? C46 C47 Fe3 69.4(8) . . ? C49 C48 C47 106.8(17) . . ? C49 C48 Fe3 70.2(10) . . ? C47 C48 Fe3 68.5(9) . . ? C48 C49 C50 111.1(19) . . ? C48 C49 Fe3 70.6(11) . . ? C50 C49 Fe3 71.2(10) . . ? C49 C50 C46 107.6(17) . . ? C49 C50 Fe3 69.7(9) . . ? C46 C50 Fe3 68.6(8) . . ? C55 C51 C52 107.1(10) . . ? C55 C51 C20 125.5(10) . . ? C52 C51 C20 127.2(11) . . ? C55 C51 Fe4 67.3(6) . . ? C52 C51 Fe4 69.5(7) . . ? C20 C51 Fe4 132.8(8) . . ? C53 C52 C51 107.7(12) . . ? C53 C52 Fe4 67.2(8) . . ? C51 C52 Fe4 70.1(7) . . ? C54 C53 C52 108.1(11) . . ? C54 C53 Fe4 70.4(8) . . ? C52 C53 Fe4 72.2(8) . . ? C53 C54 C55 108.9(10) . . ? C53 C54 Fe4 69.0(7) . . ? C55 C54 Fe4 69.2(7) . . ? C54 C55 C51 107.9(11) . . ? C54 C55 Fe4 70.0(7) . . ? C51 C55 Fe4 72.1(7) . . ? C57 C56 C60 106.4(17) . . ? C57 C56 Fe4 70.3(10) . . ? C60 C56 Fe4 68.8(10) . . ? C56 C57 C58 108.7(18) . . ? C56 C57 Fe4 69.4(10) . . ? C58 C57 Fe4 70.1(10) . . ? C59 C58 C57 107.0(19) . . ? C59 C58 Fe4 68.9(10) . . ? C57 C58 Fe4 68.9(9) . . ? C58 C59 C60 110.1(17) . . ? C58 C59 Fe4 72.1(10) . . ? C60 C59 Fe4 69.6(9) . . ? C59 C60 C56 107.8(17) . . ? C59 C60 Fe4 69.7(10) . . ? C56 C60 Fe4 70.0(10) . . ? C61 O61 C64 106(3) . . ? O61 C61 C62 103(3) . . ? C63 C62 C61 100(3) . . ? C64 C63 C62 111(3) . . ? O61 C64 C63 93(3) . . ? C74 O71 C71 99(6) . . ? O71 C71 C72 84(5) . . ? C73 C72 C71 102(6) . . ? C72 C73 C74 99(6) . . ? O71 C74 C73 99(5) . . ? C81 O81 C84 100(5) . . ? O81 C81 C82 106(5) . . ? C83 C82 C81 105(5) . . ? C82 C83 C84 91(4) . . ? O81 C84 C83 108(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.294 _refine_diff_density_min -0.842 _refine_diff_density_rms 0.198