# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; Dr. Guoping Yong Department of Chemistry, University of Science and Technology of China, Hefei, 230026, China, ; _publ_contact_author_email gpyong@ustc.edu.cn _publ_contact_author_name 'Dr. Guoping Yong' loop_ _publ_author_name 'Guoping Yong' 'Yingzhou Li' 'Yiman Zhang' 'Wenlong She' data_1 _database_code_depnum_ccdc_archive 'CCDC 828174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H40 Cd3 N16 O8' _chemical_formula_weight 1498.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(2)/nbc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x, -y+1/2, -z' '-x+1/2, y, -z' '-y+1/2, -x+1/2, -z+1/2' 'y, x, -z+1/2' 'y, -x+1/2, z+1/2' '-y+1/2, x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x, y-1/2, z' 'x-1/2, -y, z' 'y-1/2, x-1/2, z-1/2' '-y, -x, z-1/2' '-y, x-1/2, -z-1/2' 'y-1/2, -x, -z-1/2' _cell_length_a 16.3292(4) _cell_length_b 16.3292(4) _cell_length_c 19.9708(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5325.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 1.268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.776 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24533 _diffrn_reflns_av_R_equivalents 0.1222 _diffrn_reflns_av_sigmaI/netI 0.0979 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2357 _reflns_number_gt 1006 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2357 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0308 _refine_ls_wR_factor_gt 0.0276 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _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 Cd1 Cd 0.10449(3) -0.2500 0.5000 0.04606(14) Uani 1 2 d S . . Cd2 Cd 0.2500 -0.2500 0.2500 0.04053(18) Uani 1 4 d S . . C1 C 0.0863(3) -0.4241(4) 0.5670(2) 0.0430(14) Uani 1 1 d . . . C2 C 0.0531(3) -0.3931(3) 0.6262(2) 0.0602(18) Uani 1 1 d . . . H2A H 0.0538 -0.3370 0.6343 0.072 Uiso 1 1 calc R . . C3 C 0.0201(4) -0.4440(4) 0.6716(3) 0.062(2) Uani 1 1 d . . . H3A H -0.0027 -0.4233 0.7108 0.075 Uiso 1 1 calc R . . C4 C 0.0202(4) -0.5273(4) 0.6598(3) 0.068(2) Uani 1 1 d . . . H4A H -0.0028 -0.5622 0.6914 0.081 Uiso 1 1 calc R . . C5 C 0.0529(3) -0.5590(3) 0.6037(3) 0.0608(18) Uani 1 1 d . . . H5A H 0.0528 -0.6152 0.5963 0.073 Uiso 1 1 calc R . . C6 C 0.1195(3) -0.5219(3) 0.4968(4) 0.0530(13) Uani 1 1 d . . . H6A H 0.1269 -0.5728 0.4769 0.064 Uiso 1 1 calc R . . C7 C 0.1402(3) -0.4470(3) 0.4702(2) 0.0412(16) Uani 1 1 d . . . C8 C 0.1751(3) -0.4245(3) 0.4060(2) 0.0402(15) Uani 1 1 d . . . C9 C 0.2156(3) -0.5613(4) 0.3589(2) 0.065(2) Uani 1 1 d . . . H9A H 0.2008 -0.5913 0.3965 0.078 Uiso 1 1 calc R . . C10 C 0.2469(6) -0.6009(3) 0.3048(2) 0.0759(15) Uani 1 1 d . . . H10A H 0.2543 -0.6574 0.3056 0.091 Uiso 1 1 calc R . . C11 C 0.2678(5) -0.5561(3) 0.2484(2) 0.065(2) Uani 1 1 d . . . H11A H 0.2867 -0.5829 0.2104 0.079 Uiso 1 1 calc R . . C12 C 0.2609(5) -0.4739(3) 0.2482(2) 0.0496(15) Uani 1 1 d . . . H12A H 0.2778 -0.4441 0.2110 0.059 Uiso 1 1 calc R . . C13 C 0.2286(3) -0.4339(3) 0.3032(2) 0.0363(17) Uani 1 1 d . . . C14 C 0.1793(3) -0.3469(3) 0.3757(3) 0.0386(13) Uani 1 1 d . . . C15 C -0.0676(5) -0.2500 0.5000 0.062(2) Uani 1 2 d S . . C16 C -0.1627(4) -0.2500 0.5000 0.0588(19) Uani 1 2 d S . . C17 C -0.2082(3) -0.2493(7) 0.5596(2) 0.0595(16) Uani 1 1 d . . . H17A H -0.170(2) -0.255(5) 0.5990(14) 0.077(15) Uiso 1 1 d . . . N1 N 0.1179(2) -0.3854(2) 0.5144(2) 0.0416(12) Uani 1 1 d . . . N2 N 0.0861(3) -0.5070(3) 0.55797(19) 0.0484(12) Uani 1 1 d . . . N3 N 0.2148(2) -0.3546(3) 0.31221(17) 0.0394(11) Uani 1 1 d . . . N4 N 0.2057(2) -0.4793(3) 0.35900(19) 0.0439(13) Uani 1 1 d . . . O1 O 0.1557(2) -0.27737(18) 0.39718(13) 0.0527(11) Uani 1 1 d . . . O2 O -0.0350(2) -0.2459(5) 0.55384(14) 0.0942(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0603(4) 0.0399(3) 0.0380(3) 0.0009(6) 0.000 0.000 Cd2 0.0462(3) 0.0462(3) 0.0291(3) 0.000 0.000 0.000 C1 0.053(5) 0.044(5) 0.031(3) -0.004(3) 0.007(3) -0.001(3) C2 0.096(5) 0.041(4) 0.043(4) 0.000(3) 0.024(3) -0.004(3) C3 0.101(6) 0.042(5) 0.044(4) 0.004(4) 0.019(4) 0.006(4) C4 0.116(7) 0.054(6) 0.034(4) 0.014(3) 0.008(4) -0.021(5) C5 0.102(6) 0.043(4) 0.037(4) 0.012(3) 0.010(4) 0.004(3) C6 0.081(4) 0.044(4) 0.033(3) -0.010(5) 0.017(6) 0.006(3) C7 0.059(4) 0.036(4) 0.029(3) 0.002(3) 0.004(3) -0.004(3) C8 0.057(4) 0.027(4) 0.036(4) -0.002(3) -0.003(3) -0.001(3) C9 0.089(6) 0.041(5) 0.065(4) 0.006(3) 0.028(3) 0.004(3) C10 0.116(5) 0.043(4) 0.068(3) -0.005(3) 0.037(7) 0.014(7) C11 0.088(7) 0.060(4) 0.048(3) -0.009(3) 0.027(4) -0.011(4) C12 0.061(4) 0.049(3) 0.039(3) 0.005(3) 0.008(4) -0.013(5) C13 0.042(5) 0.041(4) 0.027(3) 0.001(3) 0.002(3) 0.002(3) C14 0.037(3) 0.043(4) 0.036(3) 0.004(4) 0.001(2) 0.002(3) C15 0.070(7) 0.037(5) 0.081(7) 0.002(13) 0.000 0.000 C16 0.067(6) 0.040(4) 0.070(6) -0.007(11) 0.000 0.000 C17 0.065(4) 0.053(3) 0.061(3) -0.005(9) -0.007(3) 0.007(9) N1 0.054(3) 0.042(3) 0.028(3) 0.003(2) 0.007(2) -0.006(2) N2 0.071(4) 0.046(3) 0.028(3) 0.004(3) 0.010(3) 0.007(3) N3 0.038(3) 0.050(3) 0.030(2) -0.004(2) 0.0021(19) 0.006(2) N4 0.058(3) 0.037(3) 0.036(3) -0.002(3) 0.004(2) 0.001(2) O1 0.070(3) 0.041(3) 0.047(2) 0.0026(18) 0.0197(17) 0.0059(19) O2 0.080(3) 0.087(3) 0.116(3) -0.009(6) -0.028(2) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.241(4) 3_546 ? Cd1 N1 2.241(4) . ? Cd1 O1 2.262(3) 3_546 ? Cd1 O1 2.262(3) . ? Cd1 O2 2.520(4) 3_546 ? Cd1 O2 2.520(4) . ? Cd2 N3 2.189(4) 2_545 ? Cd2 N3 2.189(4) 16_656 ? Cd2 N3 2.189(4) . ? Cd2 N3 2.189(4) 15_556 ? C1 N1 1.329(5) . ? C1 N2 1.366(5) . ? C1 C2 1.396(5) . ? C2 C3 1.343(6) . ? C2 H2A 0.9300 . ? C3 C4 1.380(6) . ? C3 H3A 0.9300 . ? C4 C5 1.346(6) . ? C4 H4A 0.9300 . ? C5 N2 1.359(5) . ? C5 H5A 0.9300 . ? C6 N2 1.360(7) . ? C6 C7 1.376(5) . ? C6 H6A 0.9300 . ? C7 N1 1.387(5) . ? C7 C8 1.451(6) . ? C8 N4 1.389(5) . ? C8 C14 1.405(6) . ? C9 N4 1.348(5) . ? C9 C10 1.359(6) . ? C9 H9A 0.9300 . ? C10 C11 1.385(6) . ? C10 H10A 0.9300 . ? C11 C12 1.346(5) . ? C11 H11A 0.9300 . ? C12 C13 1.382(6) . ? C12 H12A 0.9300 . ? C13 N3 1.326(5) . ? C13 N4 1.390(5) . ? C14 O1 1.274(5) . ? C14 N3 1.400(5) . ? C15 O2 1.202(4) . ? C15 O2 1.202(4) 3_546 ? C15 C16 1.552(8) . ? C16 C17 1.403(5) . ? C16 C17 1.403(5) 3_546 ? C17 C17 1.365(9) 2_445 ? C17 H17A 1.01(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 168.76(19) 3_546 . ? N1 Cd1 O1 83.42(13) 3_546 3_546 ? N1 Cd1 O1 92.41(12) . 3_546 ? N1 Cd1 O1 92.41(12) 3_546 . ? N1 Cd1 O1 83.42(13) . . ? O1 Cd1 O1 136.59(17) 3_546 . ? N1 Cd1 O2 93.4(2) 3_546 3_546 ? N1 Cd1 O2 96.7(2) . 3_546 ? O1 Cd1 O2 136.62(11) 3_546 3_546 ? O1 Cd1 O2 86.66(11) . 3_546 ? N1 Cd1 O2 96.7(2) 3_546 . ? N1 Cd1 O2 93.4(2) . . ? O1 Cd1 O2 86.66(11) 3_546 . ? O1 Cd1 O2 136.62(11) . . ? O2 Cd1 O2 50.61(13) 3_546 . ? N3 Cd2 N3 108.79(10) 2_545 16_656 ? N3 Cd2 N3 110.8(2) 2_545 . ? N3 Cd2 N3 108.79(10) 16_656 . ? N3 Cd2 N3 108.79(10) 2_545 15_556 ? N3 Cd2 N3 110.8(2) 16_656 15_556 ? N3 Cd2 N3 108.79(10) . 15_556 ? N1 C1 N2 111.6(5) . . ? N1 C1 C2 130.4(5) . . ? N2 C1 C2 118.0(5) . . ? C3 C2 C1 120.2(5) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 119.6(6) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 121.5(6) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 N2 118.5(6) . . ? C4 C5 H5A 120.7 . . ? N2 C5 H5A 120.7 . . ? N2 C6 C7 106.7(5) . . ? N2 C6 H6A 126.6 . . ? C7 C6 H6A 126.6 . . ? C6 C7 N1 109.4(5) . . ? C6 C7 C8 131.5(5) . . ? N1 C7 C8 118.9(5) . . ? N4 C8 C14 105.9(4) . . ? N4 C8 C7 125.1(5) . . ? C14 C8 C7 128.8(5) . . ? N4 C9 C10 121.3(5) . . ? N4 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C9 C10 C11 119.2(5) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C12 C11 C10 120.6(5) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? N3 C13 C12 129.4(5) . . ? N3 C13 N4 111.5(4) . . ? C12 C13 N4 119.1(5) . . ? O1 C14 N3 120.7(5) . . ? O1 C14 C8 130.1(5) . . ? N3 C14 C8 109.2(4) . . ? O2 C15 O2 127.4(9) . 3_546 ? O2 C15 C16 116.3(4) . . ? O2 C15 C16 116.3(4) 3_546 . ? C17 C16 C17 116.0(7) . 3_546 ? C17 C16 C15 122.0(3) . . ? C17 C16 C15 122.0(3) 3_546 . ? C17 C17 C16 122.0(3) 2_445 . ? C17 C17 H17A 128(2) 2_445 . ? C16 C17 H17A 110(2) . . ? C1 N1 C7 105.1(4) . . ? C1 N1 Cd1 122.1(4) . . ? C7 N1 Cd1 131.2(3) . . ? C5 N2 C6 130.7(5) . . ? C5 N2 C1 122.1(5) . . ? C6 N2 C1 107.1(4) . . ? C13 N3 C14 106.3(4) . . ? C13 N3 Cd2 129.8(3) . . ? C14 N3 Cd2 123.6(3) . . ? C9 N4 C8 133.2(5) . . ? C9 N4 C13 119.7(4) . . ? C8 N4 C13 107.1(5) . . ? C14 O1 Cd1 126.4(3) . . ? C15 O2 Cd1 91.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 176.3(6) . . . . ? N2 C1 C2 C3 -1.8(8) . . . . ? C1 C2 C3 C4 0.9(9) . . . . ? C2 C3 C4 C5 0.1(10) . . . . ? C3 C4 C5 N2 -0.2(10) . . . . ? N2 C6 C7 N1 -1.3(6) . . . . ? N2 C6 C7 C8 -177.6(5) . . . . ? C6 C7 C8 N4 -9.0(9) . . . . ? N1 C7 C8 N4 175.0(4) . . . . ? C6 C7 C8 C14 165.2(5) . . . . ? N1 C7 C8 C14 -10.8(8) . . . . ? N4 C9 C10 C11 -1.0(12) . . . . ? C9 C10 C11 C12 3.1(13) . . . . ? C10 C11 C12 C13 -3.5(13) . . . . ? C11 C12 C13 N3 -178.0(6) . . . . ? C11 C12 C13 N4 1.7(10) . . . . ? N4 C8 C14 O1 176.9(5) . . . . ? C7 C8 C14 O1 1.8(9) . . . . ? N4 C8 C14 N3 -2.2(5) . . . . ? C7 C8 C14 N3 -177.2(5) . . . . ? O2 C15 C16 C17 -3.0(7) . . . . ? O2 C15 C16 C17 177.0(7) 3_546 . . . ? O2 C15 C16 C17 177.0(7) . . . 3_546 ? O2 C15 C16 C17 -3.0(7) 3_546 . . 3_546 ? C17 C16 C17 C17 1.1(12) 3_546 . . 2_445 ? C15 C16 C17 C17 -178.9(12) . . . 2_445 ? N2 C1 N1 C7 -1.0(6) . . . . ? C2 C1 N1 C7 -179.3(5) . . . . ? N2 C1 N1 Cd1 166.4(3) . . . . ? C2 C1 N1 Cd1 -11.8(8) . . . . ? C6 C7 N1 C1 1.4(6) . . . . ? C8 C7 N1 C1 178.2(5) . . . . ? C6 C7 N1 Cd1 -164.4(3) . . . . ? C8 C7 N1 Cd1 12.4(7) . . . . ? N1 Cd1 N1 C1 121.5(4) 3_546 . . . ? O1 Cd1 N1 C1 53.6(4) 3_546 . . . ? O1 Cd1 N1 C1 -169.7(4) . . . . ? O2 Cd1 N1 C1 -83.9(4) 3_546 . . . ? O2 Cd1 N1 C1 -33.2(4) . . . . ? N1 Cd1 N1 C7 -74.7(4) 3_546 . . . ? O1 Cd1 N1 C7 -142.6(4) 3_546 . . . ? O1 Cd1 N1 C7 -5.9(4) . . . . ? O2 Cd1 N1 C7 79.9(4) 3_546 . . . ? O2 Cd1 N1 C7 130.6(4) . . . . ? C4 C5 N2 C6 -176.9(6) . . . . ? C4 C5 N2 C1 -0.8(8) . . . . ? C7 C6 N2 C5 177.2(5) . . . . ? C7 C6 N2 C1 0.6(6) . . . . ? N1 C1 N2 C5 -176.7(5) . . . . ? C2 C1 N2 C5 1.8(8) . . . . ? N1 C1 N2 C6 0.3(6) . . . . ? C2 C1 N2 C6 178.7(4) . . . . ? C12 C13 N3 C14 178.2(6) . . . . ? N4 C13 N3 C14 -1.5(5) . . . . ? C12 C13 N3 Cd2 -8.5(9) . . . . ? N4 C13 N3 Cd2 171.8(3) . . . . ? O1 C14 N3 C13 -176.9(5) . . . . ? C8 C14 N3 C13 2.3(5) . . . . ? O1 C14 N3 Cd2 9.3(6) . . . . ? C8 C14 N3 Cd2 -171.6(3) . . . . ? N3 Cd2 N3 C13 -142.0(4) 2_545 . . . ? N3 Cd2 N3 C13 98.4(5) 16_656 . . . ? N3 Cd2 N3 C13 -22.4(4) 15_556 . . . ? N3 Cd2 N3 C14 30.3(3) 2_545 . . . ? N3 Cd2 N3 C14 -89.3(3) 16_656 . . . ? N3 Cd2 N3 C14 149.9(3) 15_556 . . . ? C10 C9 N4 C8 179.3(6) . . . . ? C10 C9 N4 C13 -0.8(8) . . . . ? C14 C8 N4 C9 -178.8(5) . . . . ? C7 C8 N4 C9 -3.6(8) . . . . ? C14 C8 N4 C13 1.2(5) . . . . ? C7 C8 N4 C13 176.5(5) . . . . ? N3 C13 N4 C9 -179.8(4) . . . . ? C12 C13 N4 C9 0.5(7) . . . . ? N3 C13 N4 C8 0.2(5) . . . . ? C12 C13 N4 C8 -179.6(5) . . . . ? N3 C14 O1 Cd1 -175.9(3) . . . . ? C8 C14 O1 Cd1 5.2(8) . . . . ? N1 Cd1 O1 C14 166.6(4) 3_546 . . . ? N1 Cd1 O1 C14 -2.9(4) . . . . ? O1 Cd1 O1 C14 83.6(4) 3_546 . . . ? O2 Cd1 O1 C14 -100.1(5) 3_546 . . . ? O2 Cd1 O1 C14 -90.9(5) . . . . ? O2 C15 O2 Cd1 0.000(1) 3_546 . . . ? C16 C15 O2 Cd1 180.0 . . . . ? N1 Cd1 O2 C15 88.9(4) 3_546 . . . ? N1 Cd1 O2 C15 -95.9(4) . . . . ? O1 Cd1 O2 C15 171.9(4) 3_546 . . . ? O1 Cd1 O2 C15 -11.9(6) . . . . ? O2 Cd1 O2 C15 0.0 3_546 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.042 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.070 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 828175' #TrackingRef '- Compd1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H40 Fe3 N16 O8' _chemical_formula_weight 1328.67 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(2)/nbc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x, -y+1/2, -z' '-x+1/2, y, -z' '-y+1/2, -x+1/2, -z+1/2' 'y, x, -z+1/2' 'y, -x+1/2, z+1/2' '-y+1/2, x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x, y-1/2, z' 'x-1/2, -y, z' 'y-1/2, x-1/2, z-1/2' '-y, -x, z-1/2' '-y, x-1/2, -z-1/2' 'y-1/2, -x, -z-1/2' _cell_length_a 16.172(5) _cell_length_b 16.172(5) _cell_length_c 19.553(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 5114(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10849 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.19 _reflns_number_total 2044 _reflns_number_gt 923 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0952P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2044 _refine_ls_number_parameters 207 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 0.807 _refine_ls_restrained_S_all 0.807 _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 Fe1 Fe 0.60965(9) 0.2500 0.5000 0.0680(5) Uani 1 2 d S . . Fe2 Fe 0.7500 0.2500 0.2500 0.0564(5) Uani 1 4 d S . . C1 C 0.5766(4) 0.4166(4) 0.5683(2) 0.0560(18) Uani 1 1 d . . . C2 C 0.5348(4) 0.3839(5) 0.6237(3) 0.073(2) Uani 1 1 d . . . H2A H 0.5307 0.3270 0.6297 0.088 Uiso 1 1 calc R . . C3 C 0.4999(5) 0.4369(5) 0.6694(3) 0.076(2) Uani 1 1 d . . . H3A H 0.4722 0.4157 0.7072 0.091 Uiso 1 1 calc R . . C4 C 0.5047(4) 0.5213(4) 0.6607(3) 0.068(2) Uani 1 1 d . . . H4A H 0.4800 0.5560 0.6927 0.081 Uiso 1 1 calc R . . C5 C 0.5446(4) 0.5543(4) 0.6071(3) 0.070(2) Uani 1 1 d . . . H5A H 0.5471 0.6113 0.6011 0.084 Uiso 1 1 calc R . . C6 C 0.6228(4) 0.5177(4) 0.5008(3) 0.0567(16) Uani 1 1 d . . . H6A H 0.6351 0.5694 0.4827 0.068 Uiso 1 1 calc R . . C7 C 0.6418(4) 0.4429(4) 0.4735(3) 0.0530(17) Uani 1 1 d . . . C8 C 0.6800(4) 0.4189(4) 0.4095(3) 0.0527(17) Uani 1 1 d . . . C9 C 0.7247(4) 0.5564(4) 0.3614(3) 0.067(2) Uani 1 1 d . . . H9A H 0.7106 0.5873 0.3998 0.081 Uiso 1 1 calc R . . C10 C 0.7553(5) 0.5945(4) 0.3060(3) 0.0702(19) Uani 1 1 d . . . H10A H 0.7619 0.6516 0.3063 0.084 Uiso 1 1 calc R . . C11 C 0.7772(4) 0.5502(4) 0.2485(3) 0.066(2) Uani 1 1 d . . . H11A H 0.7975 0.5778 0.2103 0.079 Uiso 1 1 calc R . . C12 C 0.7693(4) 0.4672(4) 0.2474(3) 0.0596(19) Uani 1 1 d . . . H12A H 0.7852 0.4376 0.2088 0.072 Uiso 1 1 calc R . . C13 C 0.7372(4) 0.4257(4) 0.3043(2) 0.0510(17) Uani 1 1 d . . . C14 C 0.6835(4) 0.3395(4) 0.3806(3) 0.0531(17) Uani 1 1 d . . . C15 C 0.4328(10) 0.2500 0.5000 0.170(10) Uani 1 2 d SD . . C16 C 0.3368(6) 0.2500 0.5000 0.076(3) Uani 1 2 d SD . . C17 C 0.2907(4) 0.2507(6) 0.4393(3) 0.078(2) Uani 1 1 d . . . H17A H 0.3185 0.2523 0.3977 0.117 Uiso 1 1 calc R . . N1 N 0.6131(3) 0.3808(3) 0.5155(2) 0.0586(14) Uani 1 1 d . . . N2 N 0.5820(3) 0.5011(4) 0.5606(2) 0.0576(15) Uani 1 1 d . . . N3 N 0.7188(3) 0.3464(3) 0.3149(2) 0.0505(13) Uani 1 1 d . . . N4 N 0.7140(3) 0.4726(3) 0.3617(2) 0.0513(14) Uani 1 1 d . . . O1 O 0.6571(3) 0.2709(3) 0.40435(18) 0.0585(12) Uani 1 1 d . . . O2 O 0.4664(5) 0.2677(6) 0.4494(8) 0.254(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0913(11) 0.0682(10) 0.0444(6) -0.0005(7) 0.000 0.000 Fe2 0.0641(8) 0.0641(8) 0.0409(8) 0.000 0.000 0.000 C1 0.077(5) 0.060(5) 0.031(3) -0.001(3) 0.001(3) 0.007(4) C2 0.097(6) 0.076(5) 0.046(3) -0.005(4) 0.012(4) -0.003(5) C3 0.090(6) 0.096(6) 0.041(3) -0.005(4) 0.013(4) 0.009(5) C4 0.097(6) 0.065(5) 0.042(4) -0.010(3) 0.005(4) 0.010(6) C5 0.089(6) 0.072(5) 0.049(4) -0.019(4) 0.002(4) 0.001(4) C6 0.078(5) 0.056(4) 0.036(3) -0.003(3) 0.002(4) -0.005(4) C7 0.061(4) 0.059(5) 0.040(3) -0.001(3) -0.001(3) -0.006(4) C8 0.062(5) 0.057(4) 0.040(3) 0.001(3) 0.000(3) -0.004(4) C9 0.093(6) 0.061(5) 0.048(4) -0.008(3) 0.007(3) -0.001(4) C10 0.093(5) 0.063(4) 0.056(3) -0.001(3) 0.013(4) -0.006(5) C11 0.087(6) 0.074(5) 0.038(3) 0.013(3) 0.006(3) -0.005(4) C12 0.068(5) 0.072(5) 0.039(3) -0.002(3) 0.005(3) 0.002(4) C13 0.059(5) 0.063(4) 0.031(3) -0.001(3) -0.003(3) 0.003(4) C14 0.056(4) 0.066(5) 0.038(3) -0.005(3) -0.001(3) 0.003(4) C15 0.13(2) 0.038(9) 0.34(4) -0.024(18) 0.000 0.000 C16 0.068(7) 0.055(6) 0.107(8) 0.010(8) 0.000 0.000 C17 0.095(6) 0.063(4) 0.075(4) 0.002(5) 0.014(4) -0.001(7) N1 0.079(4) 0.059(3) 0.038(3) 0.000(2) 0.002(2) 0.007(3) N2 0.074(4) 0.060(4) 0.038(3) -0.007(3) -0.002(3) 0.008(3) N3 0.058(3) 0.055(3) 0.038(2) -0.004(2) 0.003(2) -0.001(3) N4 0.064(3) 0.055(4) 0.035(2) -0.006(2) 0.001(2) 0.000(3) O1 0.075(3) 0.058(3) 0.042(2) -0.003(2) 0.016(2) -0.011(3) O2 0.119(6) 0.070(7) 0.57(3) -0.012(9) 0.158(9) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 2.050(4) 3_556 ? Fe1 O1 2.050(4) . ? Fe1 N1 2.137(5) 3_556 ? Fe1 N1 2.137(5) . ? Fe2 N3 2.072(5) 15_656 ? Fe2 N3 2.072(5) . ? Fe2 N3 2.072(5) 16_666 ? Fe2 N3 2.072(5) 2_655 ? C1 N1 1.323(7) . ? C1 N2 1.378(8) . ? C1 C2 1.383(8) . ? C2 C3 1.360(8) . ? C3 C4 1.377(9) . ? C4 C5 1.343(8) . ? C5 N2 1.390(7) . ? C6 C7 1.358(8) . ? C6 N2 1.369(7) . ? C7 N1 1.378(7) . ? C7 C8 1.447(8) . ? C8 N4 1.390(7) . ? C8 C14 1.405(8) . ? C9 C10 1.341(8) . ? C9 N4 1.367(8) . ? C10 C11 1.378(8) . ? C11 C12 1.348(9) . ? C12 C13 1.400(8) . ? C13 N3 1.333(7) . ? C13 N4 1.405(7) . ? C14 O1 1.276(7) . ? C14 N3 1.410(7) . ? C15 O2 1.164(11) 3_556 ? C15 O2 1.164(11) . ? C15 C16 1.552(16) . ? C16 C17 1.402(8) . ? C16 C17 1.402(8) 3_556 ? C17 C17 1.317(13) 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 O1 Fe1 O1 136.0(3) 3_556 . ? O1 Fe1 N1 87.50(16) 3_556 3_556 ? O1 Fe1 N1 91.37(16) . 3_556 ? O1 Fe1 N1 91.37(16) 3_556 . ? O1 Fe1 N1 87.50(16) . . ? N1 Fe1 N1 177.0(3) 3_556 . ? N3 Fe2 N3 112.02(14) 15_656 . ? N3 Fe2 N3 104.5(3) 15_656 16_666 ? N3 Fe2 N3 112.02(14) . 16_666 ? N3 Fe2 N3 112.02(14) 15_656 2_655 ? N3 Fe2 N3 104.5(3) . 2_655 ? N3 Fe2 N3 112.02(14) 16_666 2_655 ? N1 C1 N2 108.7(5) . . ? N1 C1 C2 131.5(7) . . ? N2 C1 C2 119.8(6) . . ? C3 C2 C1 118.4(7) . . ? C2 C3 C4 121.4(7) . . ? C5 C4 C3 121.2(6) . . ? C4 C5 N2 118.2(6) . . ? C7 C6 N2 105.7(5) . . ? C6 C7 N1 109.8(5) . . ? C6 C7 C8 132.5(6) . . ? N1 C7 C8 117.6(6) . . ? N4 C8 C14 106.5(5) . . ? N4 C8 C7 125.7(6) . . ? C14 C8 C7 127.6(6) . . ? C10 C9 N4 120.3(6) . . ? C9 C10 C11 121.0(6) . . ? C12 C11 C10 120.4(6) . . ? C11 C12 C13 119.9(6) . . ? N3 C13 C12 131.9(5) . . ? N3 C13 N4 109.7(5) . . ? C12 C13 N4 118.4(6) . . ? O1 C14 C8 129.4(5) . . ? O1 C14 N3 122.4(5) . . ? C8 C14 N3 108.2(5) . . ? O2 C15 O2 124(2) 3_556 . ? O2 C15 C16 117.9(11) 3_556 . ? O2 C15 C16 117.9(11) . . ? C17 C16 C17 115.8(9) . 3_556 ? C17 C16 C15 122.1(5) . . ? C17 C16 C15 122.1(5) 3_556 . ? C17 C17 C16 122.1(5) 2 . ? C1 N1 C7 107.2(5) . . ? C1 N1 Fe1 122.2(4) . . ? C7 N1 Fe1 130.2(4) . . ? C6 N2 C1 108.5(5) . . ? C6 N2 C5 130.3(6) . . ? C1 N2 C5 121.0(5) . . ? C13 N3 C14 107.9(5) . . ? C13 N3 Fe2 125.1(4) . . ? C14 N3 Fe2 126.7(4) . . ? C9 N4 C8 132.2(5) . . ? C9 N4 C13 119.9(5) . . ? C8 N4 C13 107.8(5) . . ? C14 O1 Fe1 127.0(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.19 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.416 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.066 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 828176' #TrackingRef '- Compd1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 Fe3 N8 O9' _chemical_formula_weight 882.20 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.046(4) _cell_length_b 14.024(3) _cell_length_c 13.553(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.20(3) _cell_angle_gamma 90.00 _cell_volume 3429.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.549 _exptl_absorpt_correction_T_max 0.663 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13183 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0985 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 23.25 _reflns_number_total 4896 _reflns_number_gt 2980 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4896 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1396 _refine_ls_R_factor_gt 0.1036 _refine_ls_wR_factor_ref 0.3076 _refine_ls_wR_factor_gt 0.2898 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Fe1 Fe 0.29605(8) 0.56932(11) 0.64003(10) 0.0283(5) Uani 1 1 d . . . Fe2 Fe 0.19239(8) 0.64309(11) 0.46804(11) 0.0321(5) Uani 1 1 d . . . Fe3 Fe 0.24179(12) 0.65276(14) 0.87368(15) 0.0581(7) Uani 1 1 d . . . C1 C 0.4572(6) 0.4847(9) 0.6560(8) 0.036(3) Uani 1 1 d . . . C2 C 0.4394(8) 0.3991(10) 0.7007(9) 0.050(3) Uani 1 1 d . . . H2A H 0.3901 0.3855 0.7147 0.060 Uiso 1 1 calc R . . C3 C 0.4906(9) 0.3370(10) 0.7237(10) 0.061(4) Uani 1 1 d . . . H3A H 0.4771 0.2786 0.7507 0.073 Uiso 1 1 calc R . . C4 C 0.5658(10) 0.3576(12) 0.7080(10) 0.072(5) Uani 1 1 d . . . H4A H 0.6025 0.3148 0.7273 0.086 Uiso 1 1 calc R . . C5 C 0.5834(8) 0.4402(13) 0.6648(10) 0.070(5) Uani 1 1 d . . . H5A H 0.6327 0.4551 0.6528 0.084 Uiso 1 1 calc R . . C6 C 0.5320(7) 0.5899(10) 0.5914(9) 0.051(4) Uani 1 1 d . . . H6A H 0.5746 0.6209 0.5701 0.061 Uiso 1 1 calc R . . C7 C 0.4611(6) 0.6226(9) 0.5820(8) 0.034(3) Uani 1 1 d . . . C8 C 0.4301(6) 0.7042(8) 0.5337(8) 0.036(3) Uani 1 1 d . . . C9 C 0.5416(7) 0.8067(12) 0.4994(10) 0.063(4) Uani 1 1 d . . . H9A H 0.5746 0.7714 0.5374 0.076 Uiso 1 1 calc R . . C10 C 0.5654(9) 0.8823(13) 0.4497(11) 0.077(5) Uani 1 1 d . . . H10A H 0.6152 0.8990 0.4526 0.092 Uiso 1 1 calc R . . C11 C 0.5167(9) 0.9366(12) 0.3935(11) 0.081(6) Uani 1 1 d . . . H11A H 0.5345 0.9883 0.3578 0.097 Uiso 1 1 calc R . . C12 C 0.4429(9) 0.9146(11) 0.3902(10) 0.065(4) Uani 1 1 d . . . H12A H 0.4103 0.9520 0.3536 0.078 Uiso 1 1 calc R . . C13 C 0.4174(7) 0.8364(9) 0.4415(8) 0.037(3) Uani 1 1 d . . . C14 C 0.3573(6) 0.7174(9) 0.5036(7) 0.033(3) Uani 1 1 d . . . C15 C 0.0335(6) 0.6288(9) 0.3812(9) 0.041(3) Uani 1 1 d . . . C16 C 0.0544(7) 0.6376(11) 0.2840(9) 0.060(4) Uani 1 1 d . . . H16A H 0.1040 0.6451 0.2670 0.072 Uiso 1 1 calc R . . C17 C -0.0014(8) 0.6350(11) 0.2110(11) 0.065(4) Uani 1 1 d . . . H17A H 0.0105 0.6437 0.1449 0.078 Uiso 1 1 calc R . . C18 C -0.0739(7) 0.6192(11) 0.2391(10) 0.056(4) Uani 1 1 d . . . H18A H -0.1100 0.6129 0.1903 0.067 Uiso 1 1 calc R . . C19 C -0.0943(7) 0.6128(10) 0.3332(10) 0.053(4) Uani 1 1 d . . . H19A H -0.1438 0.6053 0.3502 0.063 Uiso 1 1 calc R . . C20 C -0.0437(7) 0.6113(10) 0.5077(9) 0.045(3) Uani 1 1 d . . . H20A H -0.0864 0.6034 0.5452 0.054 Uiso 1 1 calc R . . C21 C 0.0254(6) 0.6190(9) 0.5418(8) 0.036(3) Uani 1 1 d . . . C22 C 0.0552(6) 0.6190(9) 0.6432(8) 0.037(3) Uani 1 1 d . . . C23 C -0.0644(7) 0.6153(11) 0.7429(11) 0.060(4) Uani 1 1 d . . . H23A H -0.0968 0.6128 0.6894 0.073 Uiso 1 1 calc R . . C24 C -0.0908(8) 0.6183(13) 0.8373(10) 0.073(5) Uani 1 1 d . . . H24A H -0.1412 0.6265 0.8486 0.088 Uiso 1 1 calc R . . C25 C -0.0426(8) 0.6093(14) 0.9156(10) 0.077(5) Uani 1 1 d . . . H25A H -0.0618 0.6026 0.9787 0.092 Uiso 1 1 calc R . . C26 C 0.0306(8) 0.6098(12) 0.9042(9) 0.067(4) Uani 1 1 d . . . H26A H 0.0613 0.6066 0.9594 0.080 Uiso 1 1 calc R . . C27 C 0.0632(7) 0.6153(10) 0.8064(9) 0.048(3) Uani 1 1 d . . . C28 C 0.1263(6) 0.6153(9) 0.6733(9) 0.039(3) Uani 1 1 d . . . C29 C 0.2645(7) 0.0504(9) 0.3349(10) 0.044(3) Uani 1 1 d . . . C30 C 0.2577(6) 0.1510(8) 0.3677(8) 0.036(3) Uani 1 1 d . . . C31 C 0.2632(7) 0.2258(9) 0.3024(8) 0.045(3) Uani 1 1 d . . . H31A H 0.2705 0.2127 0.2359 0.054 Uiso 1 1 calc R . . C32 C 0.2585(7) 0.3174(9) 0.3316(8) 0.040(3) Uani 1 1 d . . . H32A H 0.2611 0.3659 0.2850 0.048 Uiso 1 1 calc R . . C33 C 0.2499(6) 0.3396(8) 0.4284(8) 0.039(3) Uani 1 1 d . . . C34 C 0.2441(7) 0.2640(9) 0.4968(8) 0.047(3) Uani 1 1 d . . . H34A H 0.2382 0.2777 0.5634 0.057 Uiso 1 1 calc R . . C35 C 0.2471(7) 0.1719(8) 0.4672(9) 0.046(3) Uani 1 1 d . . . H35A H 0.2420 0.1229 0.5129 0.055 Uiso 1 1 calc R . . C36 C 0.2479(6) 0.4410(8) 0.4659(9) 0.036(3) Uani 1 1 d . . . N1 N 0.4145(5) 0.5556(7) 0.6263(7) 0.038(2) Uani 1 1 d . . . N2 N 0.5291(5) 0.5023(8) 0.6382(7) 0.047(3) Uani 1 1 d . . . N3 N 0.3499(5) 0.7993(7) 0.4496(6) 0.041(2) Uani 1 1 d . . . N4 N 0.4688(6) 0.7805(8) 0.4948(7) 0.046(3) Uani 1 1 d . . . N5 N 0.0740(5) 0.6303(7) 0.4633(7) 0.041(3) Uani 1 1 d . . . N6 N -0.0399(5) 0.6174(7) 0.4052(7) 0.044(3) Uani 1 1 d . . . N7 N 0.1320(5) 0.6142(8) 0.7774(7) 0.043(3) Uani 1 1 d . . . N8 N 0.0128(5) 0.6161(8) 0.7283(7) 0.046(3) Uani 1 1 d . . . O1 O 0.3036(4) 0.6592(5) 0.5203(5) 0.0363(19) Uani 1 1 d . . . O2 O 0.1845(4) 0.6060(6) 0.6182(5) 0.041(2) Uani 1 1 d . . . O3 O 0.2584(6) -0.0119(6) 0.4013(8) 0.071(3) Uani 1 1 d . . . O4 O 0.2763(5) 0.0342(6) 0.2458(7) 0.058(2) Uani 1 1 d . . . O5 O 0.2826(5) 0.4515(6) 0.5484(6) 0.055(2) Uani 1 1 d . . . O6 O 0.2150(5) 0.5017(6) 0.4205(6) 0.044(2) Uani 1 1 d . . . O7 O 0.2964(5) 0.6831(7) 0.7423(6) 0.060(3) Uani 1 1 d . . . O8 O 0.1846(4) 0.7916(6) 0.4840(6) 0.051(2) Uani 1 1 d . . . H8A H 0.1594 0.8247 0.5330 0.076 Uiso 1 1 calc R . . O9 O 0.2305(5) 0.6837(7) 0.3081(8) 0.077(3) Uani 1 1 d . . . H9B H 0.2525 0.7348 0.3096 0.115 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 Fe1 0.0348(9) 0.0251(10) 0.0251(8) 0.0016(7) -0.0058(6) 0.0013(7) Fe2 0.0324(9) 0.0324(11) 0.0314(9) -0.0020(7) -0.0072(7) 0.0017(7) Fe3 0.0769(15) 0.0437(14) 0.0536(13) -0.0134(9) -0.0109(10) 0.0146(10) C1 0.038(7) 0.037(8) 0.034(6) -0.004(6) 0.000(5) 0.011(6) C2 0.056(8) 0.048(9) 0.047(8) 0.005(7) -0.004(6) 0.021(7) C3 0.079(11) 0.047(10) 0.057(9) 0.003(7) 0.000(8) 0.025(8) C4 0.099(14) 0.072(12) 0.046(8) 0.008(8) 0.000(8) 0.061(10) C5 0.053(9) 0.105(15) 0.051(9) -0.009(9) 0.006(7) 0.036(9) C6 0.041(8) 0.072(11) 0.039(7) 0.009(7) -0.006(6) -0.008(7) C7 0.028(6) 0.042(8) 0.031(6) 0.000(5) -0.003(5) 0.000(5) C8 0.038(7) 0.038(8) 0.033(6) 0.003(6) -0.002(5) -0.001(6) C9 0.045(8) 0.093(12) 0.052(8) 0.015(8) -0.011(6) -0.029(8) C10 0.067(10) 0.104(14) 0.058(9) 0.028(10) -0.012(8) -0.041(10) C11 0.074(11) 0.104(15) 0.063(10) 0.045(10) -0.014(8) -0.045(10) C12 0.085(12) 0.063(11) 0.046(8) 0.022(7) -0.014(7) -0.025(8) C13 0.051(8) 0.040(8) 0.020(6) 0.008(5) -0.016(5) -0.013(6) C14 0.040(7) 0.046(8) 0.013(5) -0.008(5) -0.005(4) -0.007(6) C15 0.030(7) 0.043(8) 0.050(8) 0.006(6) -0.017(6) -0.003(6) C16 0.037(7) 0.102(13) 0.040(8) 0.006(7) -0.009(6) -0.017(7) C17 0.058(10) 0.084(12) 0.053(9) -0.001(8) -0.020(7) -0.007(8) C18 0.044(8) 0.079(11) 0.045(8) 0.005(7) -0.026(6) -0.007(7) C19 0.038(7) 0.058(9) 0.062(9) -0.009(7) -0.021(6) -0.009(7) C20 0.038(7) 0.057(9) 0.039(7) -0.002(6) -0.005(5) -0.006(6) C21 0.038(7) 0.036(7) 0.033(6) 0.000(5) 0.002(5) 0.005(5) C22 0.035(7) 0.043(8) 0.031(6) 0.007(6) -0.003(5) -0.003(6) C23 0.045(8) 0.068(10) 0.069(10) 0.006(8) -0.001(7) 0.000(7) C24 0.047(9) 0.133(15) 0.040(8) 0.008(9) 0.012(7) -0.012(9) C25 0.061(10) 0.125(15) 0.044(9) -0.002(9) 0.020(8) -0.014(10) C26 0.073(11) 0.099(13) 0.027(7) -0.002(7) -0.002(7) -0.017(9) C27 0.051(8) 0.048(9) 0.045(8) 0.005(6) -0.009(6) 0.005(7) C28 0.033(7) 0.038(7) 0.047(7) -0.001(6) 0.004(6) 0.006(6) C29 0.044(7) 0.029(8) 0.059(9) 0.007(7) -0.019(6) 0.000(6) C30 0.039(7) 0.030(7) 0.040(7) -0.007(6) -0.006(5) 0.003(5) C31 0.066(8) 0.043(9) 0.026(6) -0.009(6) -0.009(6) 0.008(6) C32 0.057(8) 0.026(7) 0.037(7) 0.005(6) -0.001(6) 0.003(6) C33 0.038(7) 0.040(8) 0.041(7) -0.010(6) -0.010(5) 0.003(5) C34 0.079(9) 0.036(8) 0.026(6) -0.016(6) 0.004(6) -0.002(7) C35 0.076(10) 0.024(7) 0.038(7) 0.007(6) 0.007(6) -0.007(6) C36 0.040(7) 0.023(7) 0.045(7) -0.013(6) 0.000(6) 0.000(6) N1 0.038(6) 0.039(6) 0.036(5) -0.001(5) -0.007(4) 0.002(5) N2 0.039(6) 0.071(8) 0.029(5) -0.002(6) -0.007(4) 0.025(6) N3 0.052(7) 0.044(7) 0.028(5) 0.010(5) -0.012(4) -0.005(5) N4 0.053(7) 0.051(7) 0.034(5) 0.004(5) -0.003(5) -0.019(5) N5 0.034(5) 0.054(7) 0.035(5) 0.001(5) -0.012(4) 0.000(5) N6 0.043(6) 0.040(6) 0.048(6) -0.004(5) -0.013(5) -0.002(5) N7 0.040(6) 0.050(7) 0.040(6) 0.015(5) -0.003(5) -0.006(5) N8 0.048(7) 0.051(7) 0.038(6) 0.003(5) -0.003(5) 0.003(5) O1 0.040(5) 0.033(5) 0.036(4) 0.009(4) -0.009(3) -0.007(4) O2 0.036(5) 0.050(5) 0.038(4) 0.006(4) -0.006(4) -0.002(4) O3 0.112(9) 0.025(6) 0.075(7) -0.009(5) -0.022(6) 0.001(5) O4 0.063(6) 0.039(6) 0.073(7) -0.030(5) 0.003(5) 0.002(5) O5 0.077(6) 0.032(5) 0.055(6) -0.022(4) -0.034(5) 0.013(4) O6 0.054(5) 0.030(5) 0.048(5) -0.008(4) -0.019(4) 0.004(4) O7 0.063(6) 0.088(7) 0.028(4) 0.004(5) -0.020(4) -0.039(5) O8 0.049(5) 0.047(6) 0.055(5) 0.022(4) -0.003(4) 0.008(4) O9 0.067(7) 0.046(6) 0.117(9) 0.025(6) -0.028(6) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 2.059(7) . ? Fe1 O4 2.072(9) 4_566 ? Fe1 O5 2.080(8) . ? Fe1 O2 2.098(7) . ? Fe1 O7 2.114(10) . ? Fe1 N1 2.155(9) . ? Fe2 O8 2.099(9) . ? Fe2 O2 2.106(7) . ? Fe2 O6 2.124(8) . ? Fe2 O1 2.139(7) . ? Fe2 N5 2.145(9) . ? Fe2 O9 2.347(11) . ? Fe3 O8 1.979(8) 4_576 ? Fe3 O3 2.033(9) 4_566 ? Fe3 O7 2.082(8) . ? Fe3 N3 2.303(10) 4_576 ? Fe3 N7 2.430(10) . ? C1 N1 1.319(14) . ? C1 N2 1.343(15) . ? C1 C2 1.384(18) . ? C2 C3 1.306(17) . ? C3 C4 1.40(2) . ? C4 C5 1.34(2) . ? C5 N2 1.359(17) . ? C6 C7 1.364(16) . ? C6 N2 1.383(16) . ? C7 N1 1.397(14) . ? C7 C8 1.431(16) . ? C8 N4 1.384(14) . ? C8 C14 1.388(15) . ? C9 C10 1.33(2) . ? C9 N4 1.364(15) . ? C10 C11 1.39(2) . ? C11 C12 1.37(2) . ? C12 C13 1.378(17) . ? C13 N3 1.329(14) . ? C13 N4 1.412(15) . ? C14 O1 1.287(13) . ? C14 N3 1.368(14) . ? C15 N5 1.330(14) . ? C15 N6 1.373(14) . ? C15 C16 1.377(18) . ? C16 C17 1.409(17) . ? C17 C18 1.382(18) . ? C18 C19 1.332(18) . ? C19 N6 1.383(14) . ? C20 C21 1.333(16) . ? C20 N6 1.395(15) . ? C21 N5 1.390(14) . ? C21 C22 1.474(16) . ? C22 C28 1.346(16) . ? C22 N8 1.388(14) . ? C23 C24 1.368(19) . ? C23 N8 1.408(16) . ? C24 C25 1.376(19) . ? C25 C26 1.331(19) . ? C26 C27 1.454(18) . ? C27 N7 1.304(15) . ? C27 N8 1.393(15) . ? C28 O2 1.297(13) . ? C28 N7 1.414(15) . ? C29 O4 1.249(15) . ? C29 O3 1.259(15) . ? C29 C30 1.483(16) . ? C30 C31 1.377(16) . ? C30 C35 1.394(16) . ? C31 C32 1.347(17) . ? C32 C33 1.358(16) . ? C33 C34 1.412(16) . ? C33 C36 1.511(15) . ? C34 C35 1.353(16) . ? C36 O6 1.206(13) . ? C36 O5 1.288(14) . ? N3 Fe3 2.303(10) 4_575 ? O3 Fe3 2.033(9) 4_565 ? O4 Fe1 2.072(9) 4_565 ? O8 Fe3 1.979(8) 4_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O4 170.4(3) . 4_566 ? O1 Fe1 O5 91.4(3) . . ? O4 Fe1 O5 80.6(4) 4_566 . ? O1 Fe1 O2 78.8(3) . . ? O4 Fe1 O2 95.8(3) 4_566 . ? O5 Fe1 O2 90.1(3) . . ? O1 Fe1 O7 93.1(3) . . ? O4 Fe1 O7 94.3(4) 4_566 . ? O5 Fe1 O7 172.3(4) . . ? O2 Fe1 O7 84.7(3) . . ? O1 Fe1 N1 85.3(3) . . ? O4 Fe1 N1 99.8(4) 4_566 . ? O5 Fe1 N1 89.5(4) . . ? O2 Fe1 N1 164.0(3) . . ? O7 Fe1 N1 97.1(3) . . ? O8 Fe2 O2 98.1(3) . . ? O8 Fe2 O6 166.0(3) . . ? O2 Fe2 O6 94.4(3) . . ? O8 Fe2 O1 85.6(3) . . ? O2 Fe2 O1 76.8(3) . . ? O6 Fe2 O1 91.0(3) . . ? O8 Fe2 N5 91.1(4) . . ? O2 Fe2 N5 86.4(3) . . ? O6 Fe2 N5 96.0(4) . . ? O1 Fe2 N5 162.3(3) . . ? O8 Fe2 O9 82.8(4) . . ? O2 Fe2 O9 166.8(3) . . ? O6 Fe2 O9 83.6(3) . . ? O1 Fe2 O9 90.1(3) . . ? N5 Fe2 O9 106.7(3) . . ? O8 Fe3 O3 108.7(4) 4_576 4_566 ? O8 Fe3 O7 144.6(4) 4_576 . ? O3 Fe3 O7 106.6(4) 4_566 . ? O8 Fe3 N3 89.5(3) 4_576 4_576 ? O3 Fe3 N3 94.4(4) 4_566 4_576 ? O7 Fe3 N3 85.4(3) . 4_576 ? O8 Fe3 N7 93.8(3) 4_576 . ? O3 Fe3 N7 90.1(4) 4_566 . ? O7 Fe3 N7 88.5(3) . . ? N3 Fe3 N7 173.2(3) 4_576 . ? N1 C1 N2 111.7(11) . . ? N1 C1 C2 130.6(11) . . ? N2 C1 C2 117.6(11) . . ? C3 C2 C1 121.2(14) . . ? C2 C3 C4 120.7(15) . . ? C5 C4 C3 118.3(13) . . ? C4 C5 N2 120.0(15) . . ? C7 C6 N2 107.7(11) . . ? C6 C7 N1 107.4(11) . . ? C6 C7 C8 132.6(11) . . ? N1 C7 C8 119.9(10) . . ? N4 C8 C14 105.3(10) . . ? N4 C8 C7 126.6(10) . . ? C14 C8 C7 127.6(11) . . ? C10 C9 N4 120.3(14) . . ? C9 C10 C11 120.7(14) . . ? C12 C11 C10 120.6(13) . . ? C11 C12 C13 119.3(14) . . ? N3 C13 C12 131.4(12) . . ? N3 C13 N4 110.0(10) . . ? C12 C13 N4 118.7(12) . . ? O1 C14 N3 123.8(10) . . ? O1 C14 C8 125.1(11) . . ? N3 C14 C8 111.1(10) . . ? N5 C15 N6 109.3(11) . . ? N5 C15 C16 130.3(11) . . ? N6 C15 C16 120.4(10) . . ? C15 C16 C17 118.1(12) . . ? C18 C17 C16 119.1(13) . . ? C19 C18 C17 122.6(12) . . ? C18 C19 N6 118.4(12) . . ? C21 C20 N6 106.9(10) . . ? C20 C21 N5 109.6(10) . . ? C20 C21 C22 131.3(11) . . ? N5 C21 C22 119.0(10) . . ? C28 C22 N8 105.9(10) . . ? C28 C22 C21 128.8(11) . . ? N8 C22 C21 125.1(10) . . ? C24 C23 N8 118.6(13) . . ? C23 C24 C25 119.8(13) . . ? C26 C25 C24 122.5(13) . . ? C25 C26 C27 120.7(13) . . ? N7 C27 N8 113.0(11) . . ? N7 C27 C26 131.5(12) . . ? N8 C27 C26 115.4(12) . . ? O2 C28 C22 127.1(11) . . ? O2 C28 N7 121.1(10) . . ? C22 C28 N7 111.6(10) . . ? O4 C29 O3 125.4(12) . . ? O4 C29 C30 118.5(11) . . ? O3 C29 C30 116.0(12) . . ? C31 C30 C35 118.2(10) . . ? C31 C30 C29 121.8(11) . . ? C35 C30 C29 120.1(11) . . ? C32 C31 C30 122.3(11) . . ? C31 C32 C33 120.7(11) . . ? C32 C33 C34 118.1(11) . . ? C32 C33 C36 122.9(11) . . ? C34 C33 C36 119.0(10) . . ? C35 C34 C33 121.3(10) . . ? C34 C35 C30 119.5(11) . . ? O6 C36 O5 126.8(10) . . ? O6 C36 C33 120.3(10) . . ? O5 C36 C33 112.8(10) . . ? C1 N1 C7 106.6(9) . . ? C1 N1 Fe1 128.3(8) . . ? C7 N1 Fe1 125.1(7) . . ? C1 N2 C5 122.1(13) . . ? C1 N2 C6 106.5(9) . . ? C5 N2 C6 131.5(13) . . ? C13 N3 C14 106.6(9) . . ? C13 N3 Fe3 128.6(8) . 4_575 ? C14 N3 Fe3 124.3(7) . 4_575 ? C9 N4 C8 132.7(12) . . ? C9 N4 C13 120.3(11) . . ? C8 N4 C13 107.0(9) . . ? C15 N5 C21 107.0(9) . . ? C15 N5 Fe2 124.9(8) . . ? C21 N5 Fe2 128.1(7) . . ? C15 N6 C19 121.4(11) . . ? C15 N6 C20 107.1(9) . . ? C19 N6 C20 131.5(11) . . ? C27 N7 C28 103.6(10) . . ? C27 N7 Fe3 127.7(8) . . ? C28 N7 Fe3 126.1(7) . . ? C22 N8 C27 105.7(10) . . ? C22 N8 C23 131.7(11) . . ? C27 N8 C23 122.5(11) . . ? C14 O1 Fe1 125.4(6) . . ? C14 O1 Fe2 135.6(7) . . ? Fe1 O1 Fe2 97.6(3) . . ? C28 O2 Fe1 136.3(7) . . ? C28 O2 Fe2 126.1(7) . . ? Fe1 O2 Fe2 97.4(3) . . ? C29 O3 Fe3 123.8(9) . 4_565 ? C29 O4 Fe1 145.9(9) . 4_565 ? C36 O5 Fe1 131.6(8) . . ? C36 O6 Fe2 126.8(7) . . ? Fe3 O7 Fe1 114.0(4) . . ? Fe3 O8 Fe2 106.2(4) 4_575 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.892 _refine_diff_density_min -1.255 _refine_diff_density_rms 0.201 #===END