# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ligand_H4L _database_code_depnum_ccdc_archive 'CCDC 855119' #TrackingRef 'H4L.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H12 N2 O4' _chemical_formula_sum 'C14 H12 N2 O4' _chemical_formula_weight 272.26 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.3000(10) _cell_length_b 6.2890(10) _cell_length_c 12.1960(10) _cell_angle_alpha 90.00(5) _cell_angle_beta 104.58(5) _cell_angle_gamma 90.00(5) _cell_volume 616.11(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1375 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 284 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2453 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1416 _reflns_number_gt 953 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0646P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.028(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1416 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 O1 O 0.26040(13) 0.15907(17) 0.57451(9) 0.0327(3) Uani 1 1 d . . . O2 O -0.11627(14) 0.32494(18) 0.29396(10) 0.0378(4) Uani 1 1 d . . . N1 N 0.00303(16) 0.0914(2) 0.46939(10) 0.0262(4) Uani 1 1 d . . . C1 C 0.01739(18) 0.4562(3) 0.32845(12) 0.0261(4) Uani 1 1 d . . . C2 C 0.03211(19) 0.6410(3) 0.26851(12) 0.0301(4) Uani 1 1 d . . . H2A H -0.0517 0.6757 0.2022 0.036 Uiso 1 1 calc . . . C3 C 0.1669(2) 0.7734(3) 0.30459(13) 0.0314(4) Uani 1 1 d . . . H3 H 0.1758 0.8986 0.2629 0.038 Uiso 1 1 calc . . . C4 C 0.2902(2) 0.7250(3) 0.40164(14) 0.0320(4) Uani 1 1 d . . . H4 H 0.3833 0.8166 0.4264 0.038 Uiso 1 1 calc . . . C5 C 0.27638(18) 0.5431(3) 0.46168(12) 0.0281(4) Uani 1 1 d . . . H5 H 0.3604 0.5108 0.5283 0.034 Uiso 1 1 calc . . . C6 C 0.14090(17) 0.4049(2) 0.42642(11) 0.0233(4) Uani 1 1 d . . . C7 C 0.14022(18) 0.2110(2) 0.49578(12) 0.0247(4) Uani 1 1 d . . . H1 H -0.167(3) 0.342(3) 0.218(2) 0.066(7) Uiso 1 1 d . . . H2 H -0.091(2) 0.117(3) 0.4054(15) 0.050(6) 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 O1 0.0289(6) 0.0379(7) 0.0261(6) 0.0038(5) -0.0025(5) 0.0017(5) O2 0.0324(7) 0.0448(8) 0.0288(7) 0.0106(5) -0.0065(5) -0.0130(5) N1 0.0259(7) 0.0254(8) 0.0254(7) 0.0063(5) 0.0033(6) -0.0002(6) C1 0.0227(8) 0.0303(9) 0.0245(8) -0.0011(6) 0.0042(6) -0.0016(7) C2 0.0296(9) 0.0330(10) 0.0272(8) 0.0062(7) 0.0063(6) 0.0028(7) C3 0.0375(10) 0.0262(9) 0.0340(9) 0.0032(7) 0.0155(7) 0.0000(7) C4 0.0302(9) 0.0292(9) 0.0384(9) -0.0047(7) 0.0121(7) -0.0053(7) C5 0.0255(8) 0.0317(9) 0.0267(8) -0.0041(7) 0.0056(6) -0.0002(7) C6 0.0234(8) 0.0245(9) 0.0231(8) -0.0013(6) 0.0077(6) 0.0008(6) C7 0.0243(8) 0.0278(9) 0.0216(8) -0.0026(6) 0.0052(6) 0.0021(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 O1 C7 1.2415(18) . ? O2 C1 1.3617(19) . ? O2 H1 0.92(2) . ? N1 C7 1.335(2) . ? N1 N1 1.378(2) 3_556 ? N1 H2 0.969(18) . ? C1 C2 1.395(2) . ? C1 C6 1.402(2) . ? C2 C3 1.375(2) . ? C2 H2A 0.9500 . ? C3 C4 1.390(2) . ? C3 H3 0.9500 . ? C4 C5 1.379(2) . ? C4 H4 0.9500 . ? C5 C6 1.401(2) . ? C5 H5 0.9500 . ? C6 C7 1.485(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 C1 O2 H1 111.9(13) . . ? C7 N1 N1 118.98(15) . 3_556 ? C7 N1 H2 124.5(11) . . ? N1 N1 H2 116.3(11) 3_556 . ? O2 C1 C2 121.02(13) . . ? O2 C1 C6 119.19(14) . . ? C2 C1 C6 119.79(14) . . ? C3 C2 C1 120.56(14) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C2 C3 C4 120.34(15) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.51(15) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.31(14) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.49(14) . . ? C5 C6 C7 116.91(13) . . ? C1 C6 C7 124.59(14) . . ? O1 C7 N1 120.60(14) . . ? O1 C7 C6 122.61(14) . . ? N1 C7 C6 116.79(12) . . ? 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 O2 C1 C2 C3 179.47(14) . . . . ? C6 C1 C2 C3 0.1(2) . . . . ? C1 C2 C3 C4 -0.2(3) . . . . ? C2 C3 C4 C5 0.0(3) . . . . ? C3 C4 C5 C6 0.4(2) . . . . ? C4 C5 C6 C1 -0.6(2) . . . . ? C4 C5 C6 C7 178.63(13) . . . . ? O2 C1 C6 C5 -179.10(13) . . . . ? C2 C1 C6 C5 0.3(2) . . . . ? O2 C1 C6 C7 1.8(2) . . . . ? C2 C1 C6 C7 -178.82(14) . . . . ? N1 N1 C7 O1 -0.3(3) 3_556 . . . ? N1 N1 C7 C6 179.38(15) 3_556 . . . ? C5 C6 C7 O1 -7.3(2) . . . . ? C1 C6 C7 O1 171.80(15) . . . . ? C5 C6 C7 N1 173.02(14) . . . . ? C1 C6 C7 N1 -7.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.205 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.048 data_complex_FE2_L9 _database_code_depnum_ccdc_archive 'CCDC 893268' #TrackingRef 'C1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 Cl2 Fe2 N6 O8' _chemical_formula_sum 'C26 H36 Cl2 Fe2 N6 O8' _chemical_formula_weight 743.21 _chemical_absolute_configuration ? 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1661(10) _cell_length_b 9.4408(10) _cell_length_c 21.396(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3265.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18818 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20823 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3749 _reflns_number_gt 2386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0920P)^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 SHELXL _refine_ls_extinction_coef 0.0084(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3749 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1629 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Fe Fe -0.05547(3) 0.63442(6) 0.41353(2) 0.0259(2) Uani 1 1 d . . . Cl Cl 0.07527(5) 0.71686(11) 0.37929(4) 0.0345(3) Uani 1 1 d . . . O1 O 0.03892(14) 0.2652(3) 0.50366(11) 0.0293(6) Uani 1 1 d . . . O2 O -0.06613(14) 0.4936(3) 0.35072(11) 0.0296(6) Uani 1 1 d . . . O3 O -0.11958(14) 0.7840(3) 0.36529(11) 0.0316(6) Uani 1 1 d . . . O4 O -0.17704(14) 0.5947(3) 0.44677(12) 0.0377(7) Uani 1 1 d . . . N1 N -0.01033(16) 0.4783(3) 0.46969(12) 0.0237(7) Uani 1 1 d . . . N2 N -0.17956(18) 0.8637(3) 0.27665(14) 0.0348(8) Uani 1 1 d . . . N3 N -0.27078(16) 0.5009(4) 0.51389(14) 0.0336(8) Uani 1 1 d . . . C1 C -0.0445(2) 0.3569(4) 0.34747(16) 0.0262(8) Uani 1 1 d . . . C2 C -0.0556(2) 0.2866(4) 0.29081(16) 0.0295(8) Uani 1 1 d . . . H2 H -0.0776 0.3373 0.2563 0.035 Uiso 1 1 calc R . . C3 C -0.0357(2) 0.1457(4) 0.28341(17) 0.0315(9) Uani 1 1 d . . . H3 H -0.0438 0.1014 0.2440 0.038 Uiso 1 1 calc R . . C4 C -0.0038(2) 0.0678(4) 0.33294(16) 0.0302(8) Uani 1 1 d . . . H4 H 0.0102 -0.0292 0.3280 0.036 Uiso 1 1 calc R . . C5 C 0.0072(2) 0.1359(4) 0.39016(17) 0.0269(8) Uani 1 1 d . . . H5 H 0.0276 0.0832 0.4247 0.032 Uiso 1 1 calc R . . C6 C -0.01127(19) 0.2803(4) 0.39819(16) 0.0237(8) Uani 1 1 d . . . C7 C 0.00617(19) 0.3429(4) 0.45997(15) 0.0247(8) Uani 1 1 d . . . C8 C -0.1300(2) 0.7785(4) 0.30734(18) 0.0329(9) Uani 1 1 d . . . H8 H -0.1005 0.7088 0.2844 0.039 Uiso 1 1 calc R . . C9 C -0.2283(2) 0.9720(5) 0.30819(19) 0.0464(11) Uani 1 1 d . . . H9A H -0.2216 0.9622 0.3535 0.070 Uiso 1 1 calc . . . H9B H -0.2868 0.9606 0.2972 0.070 Uiso 1 1 calc . . . H9C H -0.2093 1.0660 0.2951 0.070 Uiso 1 1 calc . . . C10 C -0.1856(3) 0.8553(5) 0.2081(2) 0.0563(13) Uani 1 1 d . . . H10A H -0.1412 0.7946 0.1920 0.085 Uiso 1 1 calc . . . H10B H -0.1801 0.9504 0.1902 0.085 Uiso 1 1 calc . . . H10C H -0.2393 0.8153 0.1964 0.085 Uiso 1 1 calc . . . C11 C -0.1950(2) 0.5210(4) 0.49337(17) 0.0337(9) Uani 1 1 d . . . H11 H -0.1510 0.4767 0.5154 0.040 Uiso 1 1 calc R . . C12 C -0.3420(2) 0.5639(5) 0.48270(18) 0.0427(10) Uani 1 1 d . . . H12A H -0.3229 0.6309 0.4508 0.064 Uiso 1 1 calc . . . H12B H -0.3761 0.6140 0.5135 0.064 Uiso 1 1 calc . . . H12C H -0.3749 0.4893 0.4629 0.064 Uiso 1 1 calc . . . C13 C -0.2867(2) 0.4100(6) 0.5671(2) 0.0530(13) Uani 1 1 d . . . H13A H -0.2344 0.3708 0.5825 0.080 Uiso 1 1 calc . . . H13B H -0.3235 0.3326 0.5545 0.080 Uiso 1 1 calc . . . H13C H -0.3131 0.4653 0.6004 0.080 Uiso 1 1 calc . . . 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 Fe 0.0285(3) 0.0268(3) 0.0222(3) 0.0032(2) -0.00263(19) 0.0023(2) Cl 0.0309(5) 0.0406(6) 0.0322(5) 0.0070(4) -0.0012(4) -0.0027(4) O1 0.0339(13) 0.0247(14) 0.0293(14) 0.0011(11) -0.0026(11) 0.0047(11) O2 0.0396(14) 0.0280(15) 0.0212(13) 0.0000(11) -0.0066(10) 0.0023(11) O3 0.0321(13) 0.0334(16) 0.0294(14) 0.0051(12) -0.0027(10) 0.0040(11) O4 0.0313(14) 0.0461(18) 0.0357(15) 0.0113(13) -0.0011(11) 0.0000(12) N1 0.0271(14) 0.0249(17) 0.0192(14) 0.0013(12) -0.0016(11) 0.0007(12) N2 0.0332(17) 0.041(2) 0.0300(17) 0.0081(15) -0.0031(13) 0.0043(14) N3 0.0244(15) 0.044(2) 0.0320(17) 0.0050(15) -0.0016(12) -0.0031(13) C1 0.0246(18) 0.028(2) 0.0257(19) 0.0026(16) 0.0022(14) -0.0034(15) C2 0.0321(18) 0.032(2) 0.0239(19) 0.0041(17) -0.0025(14) -0.0025(16) C3 0.0355(19) 0.035(2) 0.0242(19) -0.0051(17) 0.0017(16) -0.0052(17) C4 0.0309(18) 0.029(2) 0.030(2) -0.0062(18) 0.0022(15) -0.0031(16) C5 0.0256(18) 0.030(2) 0.0251(18) 0.0052(16) 0.0006(14) -0.0003(15) C6 0.0221(16) 0.025(2) 0.0235(18) -0.0008(15) 0.0011(13) -0.0029(15) C7 0.0195(16) 0.033(2) 0.0216(18) 0.0042(16) 0.0019(13) -0.0005(14) C8 0.0286(18) 0.033(2) 0.037(2) 0.0092(18) -0.0010(16) 0.0020(16) C9 0.040(2) 0.048(3) 0.052(3) 0.009(2) -0.0032(19) 0.017(2) C10 0.062(3) 0.071(4) 0.036(2) 0.012(2) -0.012(2) 0.009(2) C11 0.0283(18) 0.041(3) 0.032(2) 0.0001(18) -0.0047(15) 0.0006(17) C12 0.0258(18) 0.056(3) 0.046(2) 0.005(2) 0.0001(17) 0.0098(19) C13 0.032(2) 0.076(4) 0.051(3) 0.024(3) -0.0005(19) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O2 1.898(3) . ? Fe O1 2.027(2) 5_566 ? Fe O3 2.033(2) . ? Fe N1 2.037(3) . ? Fe O4 2.124(2) . ? Fe Cl 2.3684(10) . ? O1 C7 1.301(4) . ? O1 Fe 2.027(2) 5_566 ? O2 C1 1.339(4) . ? O3 C8 1.252(4) . ? O4 C11 1.250(4) . ? N1 C7 1.322(4) . ? N1 N1 1.401(5) 5_566 ? N2 C8 1.312(5) . ? N2 C9 1.456(5) . ? N2 C10 1.472(5) . ? N3 C11 1.315(5) . ? N3 C13 1.449(5) . ? N3 C12 1.458(4) . ? C1 C2 1.394(5) . ? C1 C6 1.411(5) . ? C2 C3 1.377(5) . ? C2 H2 0.9500 . ? C3 C4 1.389(5) . ? C3 H3 0.9500 . ? C4 C5 1.394(5) . ? C4 H4 0.9500 . ? C5 C6 1.406(5) . ? C5 H5 0.9500 . ? C6 C7 1.475(5) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe O1 163.38(11) . 5_566 ? O2 Fe O3 94.64(10) . . ? O1 Fe O3 100.74(10) 5_566 . ? O2 Fe N1 86.75(11) . . ? O1 Fe N1 77.02(10) 5_566 . ? O3 Fe N1 169.97(10) . . ? O2 Fe O4 91.68(10) . . ? O1 Fe O4 84.96(10) 5_566 . ? O3 Fe O4 79.70(10) . . ? N1 Fe O4 90.34(10) . . ? O2 Fe Cl 95.29(8) . . ? O1 Fe Cl 89.94(7) 5_566 . ? O3 Fe Cl 93.99(7) . . ? N1 Fe Cl 95.77(8) . . ? O4 Fe Cl 170.97(8) . . ? C7 O1 Fe 114.7(2) . 5_566 ? C1 O2 Fe 133.5(2) . . ? C8 O3 Fe 122.8(3) . . ? C11 O4 Fe 125.5(2) . . ? C7 N1 N1 112.4(3) . 5_566 ? C7 N1 Fe 132.8(2) . . ? N1 N1 Fe 114.8(3) 5_566 . ? C8 N2 C9 121.9(3) . . ? C8 N2 C10 120.4(3) . . ? C9 N2 C10 117.7(3) . . ? C11 N3 C13 120.9(3) . . ? C11 N3 C12 121.6(3) . . ? C13 N3 C12 117.4(3) . . ? O2 C1 C2 118.1(3) . . ? O2 C1 C6 123.6(3) . . ? C2 C1 C6 118.3(3) . . ? C3 C2 C1 122.0(3) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 118.3(3) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C4 C5 C6 121.8(3) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 119.0(3) . . ? C5 C6 C7 117.2(3) . . ? C1 C6 C7 123.8(3) . . ? O1 C7 N1 121.0(3) . . ? O1 C7 C6 119.7(3) . . ? N1 C7 C6 119.3(3) . . ? O3 C8 N2 123.5(4) . . ? O3 C8 H8 118.2 . . ? N2 C8 H8 118.2 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O4 C11 N3 124.3(3) . . ? O4 C11 H11 117.9 . . ? N3 C11 H11 117.9 . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Fe O2 C1 -17.5(5) 5_566 . . . ? O3 Fe O2 C1 -175.2(3) . . . . ? N1 Fe O2 C1 -5.2(3) . . . . ? O4 Fe O2 C1 -95.4(3) . . . . ? Cl Fe O2 C1 90.3(3) . . . . ? O2 Fe O3 C8 -20.1(3) . . . . ? O1 Fe O3 C8 166.2(3) 5_566 . . . ? N1 Fe O3 C8 -117.7(6) . . . . ? O4 Fe O3 C8 -111.0(3) . . . . ? Cl Fe O3 C8 75.5(3) . . . . ? O2 Fe O4 C11 99.7(3) . . . . ? O1 Fe O4 C11 -64.0(3) 5_566 . . . ? O3 Fe O4 C11 -165.9(3) . . . . ? N1 Fe O4 C11 12.9(3) . . . . ? O2 Fe N1 C7 3.4(3) . . . . ? O1 Fe N1 C7 179.8(3) 5_566 . . . ? O3 Fe N1 C7 101.6(7) . . . . ? O4 Fe N1 C7 95.0(3) . . . . ? Cl Fe N1 C7 -91.6(3) . . . . ? O2 Fe N1 N1 -179.1(3) . . . 5_566 ? O1 Fe N1 N1 -2.7(3) 5_566 . . 5_566 ? O3 Fe N1 N1 -80.9(7) . . . 5_566 ? O4 Fe N1 N1 -87.5(3) . . . 5_566 ? Cl Fe N1 N1 85.9(3) . . . 5_566 ? Fe O2 C1 C2 -174.5(2) . . . . ? Fe O2 C1 C6 5.6(5) . . . . ? O2 C1 C2 C3 -179.5(3) . . . . ? C6 C1 C2 C3 0.4(5) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C3 C4 C5 C6 -1.6(5) . . . . ? C4 C5 C6 C1 2.3(5) . . . . ? C4 C5 C6 C7 -177.3(3) . . . . ? O2 C1 C6 C5 178.2(3) . . . . ? C2 C1 C6 C5 -1.7(5) . . . . ? O2 C1 C6 C7 -2.2(5) . . . . ? C2 C1 C6 C7 177.9(3) . . . . ? Fe O1 C7 N1 3.2(4) 5_566 . . . ? Fe O1 C7 C6 -178.1(2) 5_566 . . . ? N1 N1 C7 O1 -0.8(5) 5_566 . . . ? Fe N1 C7 O1 176.8(2) . . . . ? N1 N1 C7 C6 -179.5(3) 5_566 . . . ? Fe N1 C7 C6 -1.9(5) . . . . ? C5 C6 C7 O1 1.4(5) . . . . ? C1 C6 C7 O1 -178.2(3) . . . . ? C5 C6 C7 N1 -179.9(3) . . . . ? C1 C6 C7 N1 0.5(5) . . . . ? Fe O3 C8 N2 171.2(3) . . . . ? C9 N2 C8 O3 -1.1(6) . . . . ? C10 N2 C8 O3 177.0(4) . . . . ? Fe O4 C11 N3 178.3(3) . . . . ? C13 N3 C11 O4 177.9(4) . . . . ? C12 N3 C11 O4 0.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.994 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.229 data_feii_dmf _database_code_depnum_ccdc_archive 'CCDC 893269' #TrackingRef 'C2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(Fe C18 H42 N6 O6), 4(Fe Cl4)' _chemical_formula_sum 'C72 H168 Cl16 Fe8 N24 O24' _chemical_formula_weight 2768.30 _chemical_absolute_configuration ? 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' O O 0.0106 0.0060 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.223(7) _cell_length_b 18.6840(10) _cell_length_c 20.178(2) _cell_angle_alpha 114.76(5) _cell_angle_beta 92.29(5) _cell_angle_gamma 91.81(5) _cell_volume 3150(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10078 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 25.68 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.300 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13910 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.68 _reflns_number_total 10078 _reflns_number_gt 6838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. ; # start Validation Reply Form _vrf_REFLT03_I ; PROBLEM: Reflection count < 85% complete (theta max?) RESPONSE: small and unstable single crystal ; _vrf_PLAT029_I ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.841 RESPONSE: small and unstable single crystal ; _vrf_PLAT412_I ; PROBLEM: Short Intra XH3 .. XHn H1A .. H2A .. 1.52 Ang. RESPONSE: due to the disorders on DMF molecules on Fe1 ; _vrf_PLAT413_I ; PROBLEM: Short Inter XH3 .. XHn H4B .. H8B .. 1.84 Ang. RESPONSE: due to the disorders on DMF molecules on Fe1 ; # end Validation Reply Form _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^)+(0.0513P)^2^+2.4540P] 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 10078 _refine_ls_number_parameters 644 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.002 _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 0.0000 0.5000 0.0000 0.0264(2) Uani 1 2 d S . . Fe2 Fe 1.0000 0.0000 0.0000 0.0286(2) Uani 1 2 d S . . Fe3 Fe 0.94739(6) 0.24193(3) 0.49291(3) 0.02834(17) Uani 1 1 d . . . Fe4 Fe 0.51289(6) 0.37749(4) 0.26096(3) 0.03296(17) Uani 1 1 d . . . Fe5 Fe 0.45996(6) -0.15525(4) 0.23549(3) 0.03151(17) Uani 1 1 d . . . Cl1 Cl 0.67356(13) 0.46659(7) 0.24661(7) 0.0490(3) Uani 1 1 d . . . Cl2 Cl 0.36903(13) 0.45064(8) 0.35550(7) 0.0545(4) Uani 1 1 d . . . Cl3 Cl 0.35298(13) 0.30879(7) 0.16098(7) 0.0476(3) Uani 1 1 d . . . Cl4 Cl 0.64776(13) 0.28548(7) 0.28249(8) 0.0551(4) Uani 1 1 d . . . Cl5 Cl 0.45304(15) -0.17089(8) 0.34394(7) 0.0558(4) Uani 1 1 d . . . Cl6 Cl 0.36796(15) -0.26408(7) 0.13391(8) 0.0586(4) Uani 1 1 d . . . Cl7 Cl 0.32064(14) -0.05220(7) 0.24316(8) 0.0565(4) Uani 1 1 d . . . Cl8 Cl 0.69664(13) -0.13589(10) 0.21286(8) 0.0678(4) Uani 1 1 d . . . O1A O 0.0141(7) 0.6014(4) 0.1046(4) 0.0357(11) Uiso 0.50 1 d P A 1 C1A C 0.0111(10) 0.6433(6) 0.1512(5) 0.0314(15) Uiso 0.50 1 d P A 1 H1A H 0.0916 0.6773 0.1533 0.038 Uiso 0.50 1 calc P B 1 O1B O -0.0509(7) 0.5704(4) 0.1091(4) 0.0357(11) Uiso 0.50 1 d P A 2 C1B C -0.0589(10) 0.6090(6) 0.1484(5) 0.0314(15) Uiso 0.50 1 d P A 2 H1B H -0.1565 0.5956 0.1540 0.038 Uiso 0.50 1 calc P C 2 O2A O -0.0610(7) 0.4297(4) 0.0547(4) 0.0380(11) Uiso 0.50 1 d P A 3 C4A C -0.0541(10) 0.3904(6) 0.0708(5) 0.0376(17) Uiso 0.50 1 d P A 3 H4A H 0.0456 0.3889 0.0837 0.045 Uiso 0.50 1 calc P D 3 O2B O -0.1012(7) 0.4031(4) 0.0123(4) 0.0380(11) Uiso 0.50 1 d P A 4 C4B C -0.1357(10) 0.3778(6) 0.0410(6) 0.0376(17) Uiso 0.50 1 d P A 4 H4B H -0.2363 0.3874 0.0414 0.045 Uiso 0.50 1 calc P E 4 O3 O 0.2074(3) 0.47396(18) 0.02615(18) 0.0462(9) Uani 1 1 d . A . O4 O 1.1105(3) 0.07578(17) 0.09974(16) 0.0375(8) Uani 1 1 d . . . O5 O 0.9673(3) -0.08201(18) 0.04242(17) 0.0402(8) Uani 1 1 d . . . O6 O 0.7931(3) 0.05094(18) 0.03117(16) 0.0388(8) Uani 1 1 d . . . O7 O 0.9171(3) 0.33454(18) 0.59442(17) 0.0416(8) Uani 1 1 d . . . O8 O 0.9711(3) 0.15407(17) 0.38689(16) 0.0377(8) Uani 1 1 d . . . O9 O 0.7173(3) 0.21786(17) 0.47033(16) 0.0336(7) Uani 1 1 d . . . O10 O 1.1722(3) 0.25914(19) 0.51602(18) 0.0416(8) Uani 1 1 d . . . O11 O 0.9519(3) 0.32610(16) 0.44722(16) 0.0333(7) Uani 1 1 d . . . O12 O 0.9434(3) 0.16042(17) 0.54249(16) 0.0370(8) Uani 1 1 d . . . N1 N -0.0451(4) 0.6805(2) 0.2158(2) 0.0446(11) Uani 1 1 d . . . N2 N -0.1267(4) 0.3346(2) 0.0834(2) 0.0413(10) Uani 1 1 d . . . N3 N 0.4366(4) 0.5012(2) 0.0767(2) 0.0351(9) Uani 1 1 d . A . N4 N 1.1421(4) 0.1766(2) 0.21160(19) 0.0363(9) Uani 1 1 d . . . N5 N 0.9018(4) -0.1964(2) 0.04848(19) 0.0333(9) Uani 1 1 d . . . N6 N 0.5858(4) 0.0922(2) -0.0031(2) 0.0397(10) Uani 1 1 d . . . N7 N 0.8055(4) 0.3951(2) 0.7002(2) 0.0389(10) Uani 1 1 d . . . N8 N 0.8767(4) 0.0841(2) 0.2710(2) 0.0348(9) Uani 1 1 d . . . N9 N 0.5306(4) 0.1264(2) 0.4371(2) 0.0343(9) Uani 1 1 d . . . N10 N 1.3799(4) 0.3262(2) 0.5165(2) 0.0376(10) Uani 1 1 d . . . N11 N 0.8735(4) 0.43542(19) 0.43728(19) 0.0293(8) Uani 1 1 d . . . N12 N 1.0458(4) 0.0780(2) 0.5849(2) 0.0338(9) Uani 1 1 d . . . C2 C 0.0359(6) 0.7541(4) 0.2505(3) 0.0636(16) Uani 1 1 d . A . H2A H 0.1093 0.7576 0.2180 0.095 Uiso 1 1 calc . . . H2B H 0.0840 0.7580 0.2962 0.095 Uiso 1 1 calc . . . H2C H -0.0297 0.7973 0.2612 0.095 Uiso 1 1 calc . . . C3 C -0.1623(6) 0.6687(4) 0.2558(4) 0.0681(17) Uani 1 1 d . A . H3A H -0.2404 0.7034 0.2565 0.102 Uiso 1 1 calc . . . H3B H -0.1267 0.6811 0.3060 0.102 Uiso 1 1 calc . . . H3C H -0.1997 0.6135 0.2320 0.102 Uiso 1 1 calc . . . C5 C -0.2481(6) 0.2804(4) 0.0525(4) 0.084(2) Uani 1 1 d . A . H5A H -0.3281 0.2966 0.0853 0.126 Uiso 1 1 calc . . . H5B H -0.2210 0.2275 0.0455 0.126 Uiso 1 1 calc . . . H5C H -0.2792 0.2795 0.0051 0.126 Uiso 1 1 calc . . . C6 C -0.0502(7) 0.3333(4) 0.1464(3) 0.0759(19) Uani 1 1 d . A . H6A H 0.0335 0.3713 0.1612 0.114 Uiso 1 1 calc . . . H6B H -0.0166 0.2803 0.1342 0.114 Uiso 1 1 calc . . . H6C H -0.1155 0.3474 0.1866 0.114 Uiso 1 1 calc . . . C7 C 0.3094(5) 0.5216(3) 0.0597(2) 0.0357(11) Uani 1 1 d . . . H7 H 0.2954 0.5761 0.0742 0.043 Uiso 1 1 calc . . . C8 C 0.4674(5) 0.4188(3) 0.0554(3) 0.0612(17) Uani 1 1 d . . . H8A H 0.4413 0.4032 0.0943 0.092 Uiso 1 1 calc . . . H8B H 0.5712 0.4121 0.0475 0.092 Uiso 1 1 calc . . . H8C H 0.4105 0.3858 0.0102 0.092 Uiso 1 1 calc . . . C9 C 0.5511(5) 0.5590(3) 0.1187(3) 0.0457(13) Uani 1 1 d . . . H9A H 0.5181 0.6122 0.1308 0.069 Uiso 1 1 calc . . . H9B H 0.6371 0.5508 0.0899 0.069 Uiso 1 1 calc . . . H9C H 0.5757 0.5533 0.1639 0.069 Uiso 1 1 calc . . . C10 C 1.0677(5) 0.1358(3) 0.1501(3) 0.0348(11) Uani 1 1 d . . . H10 H 0.9748 0.1530 0.1432 0.042 Uiso 1 1 calc . . . C11 C 1.0888(6) 0.2491(3) 0.2671(3) 0.0527(14) Uani 1 1 d . . . H11A H 0.9917 0.2576 0.2511 0.079 Uiso 1 1 calc . . . H11B H 1.1551 0.2939 0.2739 0.079 Uiso 1 1 calc . . . H11C H 1.0838 0.2441 0.3134 0.079 Uiso 1 1 calc . . . C12 C 1.2859(5) 0.1542(3) 0.2263(3) 0.0521(14) Uani 1 1 d . . . H12A H 1.3112 0.1065 0.1843 0.078 Uiso 1 1 calc . . . H12B H 1.2853 0.1436 0.2699 0.078 Uiso 1 1 calc . . . H12C H 1.3577 0.1972 0.2344 0.078 Uiso 1 1 calc . . . C13 C 0.8882(5) -0.1436(3) 0.0226(2) 0.0353(11) Uani 1 1 d . . . H13 H 0.8129 -0.1526 -0.0140 0.042 Uiso 1 1 calc . . . C14 C 0.7967(5) -0.2631(3) 0.0285(3) 0.0464(13) Uani 1 1 d . . . H14A H 0.7362 -0.2547 0.0697 0.070 Uiso 1 1 calc . . . H14B H 0.8483 -0.3117 0.0163 0.070 Uiso 1 1 calc . . . H14C H 0.7350 -0.2678 -0.0140 0.070 Uiso 1 1 calc . . . C15 C 1.0140(5) -0.1853(3) 0.1057(3) 0.0431(12) Uani 1 1 d . . . H15A H 1.0801 -0.1405 0.1123 0.065 Uiso 1 1 calc . . . H15B H 1.0687 -0.2331 0.0914 0.065 Uiso 1 1 calc . . . H15C H 0.9683 -0.1750 0.1516 0.065 Uiso 1 1 calc . . . C16 C 0.7142(5) 0.0614(3) -0.0151(3) 0.0370(11) Uani 1 1 d . . . H16 H 0.7488 0.0461 -0.0626 0.044 Uiso 1 1 calc . . . C17 C 0.4999(5) 0.1021(3) -0.0602(3) 0.0591(16) Uani 1 1 d . . . H17A H 0.5525 0.0830 -0.1051 0.089 Uiso 1 1 calc . . . H17B H 0.4824 0.1582 -0.0447 0.089 Uiso 1 1 calc . . . H17C H 0.4067 0.0720 -0.0692 0.089 Uiso 1 1 calc . . . C18 C 0.5256(5) 0.1168(3) 0.0686(3) 0.0527(14) Uani 1 1 d . . . H18A H 0.5952 0.1077 0.1019 0.079 Uiso 1 1 calc . . . H18B H 0.4346 0.0861 0.0638 0.079 Uiso 1 1 calc . . . H18C H 0.5068 0.1731 0.0882 0.079 Uiso 1 1 calc . . . C19 C 0.8224(5) 0.3360(3) 0.6366(3) 0.0381(11) Uani 1 1 d . . . H19 H 0.7569 0.2911 0.6220 0.046 Uiso 1 1 calc . . . C20 C 0.8995(6) 0.4658(3) 0.7283(3) 0.0567(15) Uani 1 1 d . . . H20A H 0.9880 0.4559 0.7012 0.085 Uiso 1 1 calc . . . H20B H 0.9252 0.4812 0.7802 0.085 Uiso 1 1 calc . . . H20C H 0.8491 0.5084 0.7225 0.085 Uiso 1 1 calc . . . C21 C 0.6848(6) 0.3924(3) 0.7440(3) 0.0580(15) Uani 1 1 d . . . H21A H 0.6268 0.3427 0.7183 0.087 Uiso 1 1 calc . . . H21B H 0.6236 0.4369 0.7518 0.087 Uiso 1 1 calc . . . H21C H 0.7230 0.3959 0.7913 0.087 Uiso 1 1 calc . . . C22 C 0.8799(5) 0.1435(3) 0.3353(3) 0.0341(11) Uani 1 1 d . . . H22 H 0.8082 0.1813 0.3437 0.041 Uiso 1 1 calc . . . C23 C 0.9844(5) 0.0239(3) 0.2518(3) 0.0412(12) Uani 1 1 d . . . H23A H 1.0654 0.0420 0.2889 0.062 Uiso 1 1 calc . . . H23B H 1.0207 0.0148 0.2040 0.062 Uiso 1 1 calc . . . H23C H 0.9394 -0.0253 0.2495 0.062 Uiso 1 1 calc . . . C24 C 0.7585(6) 0.0721(3) 0.2169(3) 0.0498(14) Uani 1 1 d . . . H24A H 0.6919 0.0289 0.2141 0.075 Uiso 1 1 calc . . . H24B H 0.7981 0.0589 0.1691 0.075 Uiso 1 1 calc . . . H24C H 0.7057 0.1206 0.2311 0.075 Uiso 1 1 calc . . . C25 C 0.6430(5) 0.1664(3) 0.4791(2) 0.0334(11) Uani 1 1 d . . . H25 H 0.6700 0.1553 0.5196 0.040 Uiso 1 1 calc . . . C26 C 0.4819(5) 0.1385(3) 0.3732(3) 0.0556(15) Uani 1 1 d . . . H26A H 0.5306 0.1866 0.3747 0.083 Uiso 1 1 calc . . . H26B H 0.3765 0.1438 0.3730 0.083 Uiso 1 1 calc . . . H26C H 0.5057 0.0932 0.3287 0.083 Uiso 1 1 calc . . . C27 C 0.4479(6) 0.0676(3) 0.4513(3) 0.0598(15) Uani 1 1 d . . . H27A H 0.4636 0.0150 0.4134 0.090 Uiso 1 1 calc . . . H27B H 0.3444 0.0777 0.4509 0.090 Uiso 1 1 calc . . . H27C H 0.4799 0.0703 0.4992 0.090 Uiso 1 1 calc . . . C28 C 1.2543(5) 0.2894(3) 0.4869(3) 0.0372(12) Uani 1 1 d . . . H28 H 1.2245 0.2858 0.4400 0.045 Uiso 1 1 calc . . . C29 C 1.4747(5) 0.3581(3) 0.4777(3) 0.0607(16) Uani 1 1 d . . . H29A H 1.4261 0.3501 0.4308 0.091 Uiso 1 1 calc . . . H29B H 1.5658 0.3308 0.4688 0.091 Uiso 1 1 calc . . . H29C H 1.4956 0.4146 0.5073 0.091 Uiso 1 1 calc . . . C30 C 1.4270(5) 0.3364(3) 0.5892(3) 0.0585(15) Uani 1 1 d . . . H30A H 1.3442 0.3496 0.6204 0.088 Uiso 1 1 calc . . . H30B H 1.5026 0.3792 0.6096 0.088 Uiso 1 1 calc . . . H30C H 1.4661 0.2873 0.5870 0.088 Uiso 1 1 calc . . . C31 C 0.8724(4) 0.3834(3) 0.4651(2) 0.0306(10) Uani 1 1 d . . . H31 H 0.8060 0.3898 0.5018 0.037 Uiso 1 1 calc . . . C32 C 0.7703(5) 0.4974(3) 0.4574(3) 0.0440(13) Uani 1 1 d . . . H32A H 0.7127 0.4961 0.4967 0.066 Uiso 1 1 calc . . . H32B H 0.7056 0.4890 0.4147 0.066 Uiso 1 1 calc . . . H32C H 0.8231 0.5489 0.4742 0.066 Uiso 1 1 calc . . . C33 C 0.9688(5) 0.4296(3) 0.3804(3) 0.0410(12) Uani 1 1 d . . . H33A H 1.0482 0.3958 0.3800 0.062 Uiso 1 1 calc . . . H33B H 1.0090 0.4824 0.3896 0.062 Uiso 1 1 calc . . . H33C H 0.9139 0.4068 0.3329 0.062 Uiso 1 1 calc . . . C34 C 1.0508(5) 0.1303(3) 0.5572(2) 0.0321(10) Uani 1 1 d . . . H34 H 1.1436 0.1463 0.5478 0.039 Uiso 1 1 calc . . . C35 C 1.1772(5) 0.0435(3) 0.5994(3) 0.0495(14) Uani 1 1 d . . . H35A H 1.2600 0.0593 0.5786 0.074 Uiso 1 1 calc . . . H35B H 1.1633 -0.0142 0.5769 0.074 Uiso 1 1 calc . . . H35C H 1.1961 0.0623 0.6523 0.074 Uiso 1 1 calc . . . C36 C 0.9085(5) 0.0521(3) 0.6034(3) 0.0459(13) Uani 1 1 d . . . H36A H 0.9056 0.0726 0.6567 0.069 Uiso 1 1 calc . . . H36B H 0.9000 -0.0057 0.5819 0.069 Uiso 1 1 calc . . . H36C H 0.8276 0.0719 0.5841 0.069 Uiso 1 1 calc . . . 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 0.0305(5) 0.0234(5) 0.0250(5) 0.0102(4) -0.0011(4) 0.0002(4) Fe2 0.0350(5) 0.0242(5) 0.0279(5) 0.0122(4) -0.0017(4) 0.0041(4) Fe3 0.0289(3) 0.0294(4) 0.0283(4) 0.0140(3) -0.0007(3) -0.0005(3) Fe4 0.0334(4) 0.0337(4) 0.0335(4) 0.0159(3) -0.0001(3) 0.0038(3) Fe5 0.0307(3) 0.0295(4) 0.0346(4) 0.0140(3) -0.0004(3) 0.0007(3) Cl1 0.0497(7) 0.0474(8) 0.0583(9) 0.0312(7) 0.0008(6) -0.0050(6) Cl2 0.0488(7) 0.0671(9) 0.0445(8) 0.0189(7) 0.0119(6) 0.0131(7) Cl3 0.0506(7) 0.0526(8) 0.0398(8) 0.0214(6) -0.0100(6) -0.0050(6) Cl4 0.0496(8) 0.0442(8) 0.0786(10) 0.0340(7) -0.0125(7) 0.0059(6) Cl5 0.0655(8) 0.0645(9) 0.0473(8) 0.0342(7) 0.0002(7) -0.0069(7) Cl6 0.0646(9) 0.0330(7) 0.0618(10) 0.0066(7) -0.0222(7) -0.0046(6) Cl7 0.0657(9) 0.0415(8) 0.0581(9) 0.0156(7) 0.0011(7) 0.0234(7) Cl8 0.0372(7) 0.0994(12) 0.0563(10) 0.0233(9) 0.0039(6) -0.0134(7) O3 0.0359(18) 0.0353(19) 0.056(2) 0.0103(17) -0.0154(16) -0.0001(16) O4 0.0464(19) 0.0304(18) 0.0293(19) 0.0069(15) -0.0058(14) 0.0047(15) O5 0.0447(19) 0.038(2) 0.046(2) 0.0270(17) -0.0065(16) -0.0050(16) O6 0.0384(17) 0.047(2) 0.0324(19) 0.0172(16) -0.0005(14) 0.0118(15) O7 0.0459(19) 0.043(2) 0.034(2) 0.0135(16) 0.0030(16) 0.0020(16) O8 0.0421(18) 0.0378(19) 0.0331(19) 0.0145(16) 0.0013(15) 0.0079(15) O9 0.0316(16) 0.0358(18) 0.038(2) 0.0210(16) -0.0021(14) -0.0042(15) O10 0.0295(17) 0.052(2) 0.055(2) 0.0359(19) -0.0020(15) -0.0064(16) O11 0.0352(17) 0.0307(17) 0.0364(19) 0.0167(15) 0.0001(14) 0.0046(15) O12 0.0347(17) 0.0414(19) 0.043(2) 0.0265(17) -0.0012(14) 0.0014(15) N1 0.053(3) 0.044(3) 0.027(2) 0.005(2) -0.002(2) 0.018(2) N2 0.056(3) 0.035(2) 0.042(3) 0.024(2) 0.014(2) 0.007(2) N3 0.032(2) 0.039(2) 0.037(2) 0.0202(19) -0.0065(17) -0.0011(18) N4 0.052(2) 0.033(2) 0.024(2) 0.0124(18) -0.0002(18) -0.0055(19) N5 0.042(2) 0.030(2) 0.031(2) 0.0152(18) -0.0009(17) 0.0028(18) N6 0.036(2) 0.044(2) 0.041(3) 0.020(2) 0.0033(18) 0.012(2) N7 0.057(3) 0.037(2) 0.022(2) 0.0100(19) 0.0021(19) 0.010(2) N8 0.046(2) 0.029(2) 0.029(2) 0.0105(18) 0.0031(18) 0.0059(18) N9 0.035(2) 0.036(2) 0.032(2) 0.0154(19) -0.0071(17) -0.0083(18) N10 0.026(2) 0.035(2) 0.054(3) 0.022(2) -0.0024(19) 0.0004(18) N11 0.032(2) 0.027(2) 0.029(2) 0.0118(17) 0.0034(16) 0.0036(17) N12 0.032(2) 0.035(2) 0.038(2) 0.0202(19) -0.0038(17) 0.0007(18) C2 0.060(4) 0.075(4) 0.077(4) 0.055(4) -0.010(3) -0.006(3) C3 0.051(3) 0.075(4) 0.082(5) 0.038(4) -0.004(3) -0.005(3) C5 0.058(4) 0.083(5) 0.082(5) 0.007(4) -0.008(3) 0.000(4) C6 0.078(4) 0.079(4) 0.062(4) 0.021(4) -0.011(3) 0.020(4) C7 0.043(3) 0.032(3) 0.031(3) 0.013(2) 0.000(2) 0.009(2) C8 0.047(3) 0.047(3) 0.105(5) 0.049(3) -0.013(3) 0.002(3) C9 0.037(3) 0.053(3) 0.045(3) 0.019(3) -0.007(2) -0.002(2) C10 0.040(3) 0.035(3) 0.033(3) 0.018(2) -0.001(2) -0.002(2) C11 0.076(4) 0.041(3) 0.028(3) 0.002(2) 0.009(3) -0.008(3) C12 0.053(3) 0.057(3) 0.044(3) 0.021(3) -0.019(2) -0.005(3) C13 0.036(3) 0.038(3) 0.036(3) 0.020(2) -0.001(2) 0.007(2) C14 0.060(3) 0.035(3) 0.044(3) 0.018(3) -0.003(3) -0.009(3) C15 0.052(3) 0.041(3) 0.042(3) 0.024(3) -0.007(2) 0.008(2) C16 0.039(3) 0.035(3) 0.035(3) 0.013(2) 0.001(2) 0.004(2) C17 0.048(3) 0.076(4) 0.062(4) 0.037(3) -0.005(3) 0.022(3) C18 0.044(3) 0.064(4) 0.053(4) 0.025(3) 0.010(3) 0.014(3) C19 0.045(3) 0.040(3) 0.034(3) 0.020(2) -0.002(2) 0.006(2) C20 0.082(4) 0.044(3) 0.041(3) 0.016(3) -0.006(3) 0.001(3) C21 0.063(4) 0.071(4) 0.041(3) 0.023(3) 0.011(3) 0.013(3) C22 0.041(3) 0.030(3) 0.036(3) 0.017(2) 0.009(2) 0.009(2) C23 0.050(3) 0.038(3) 0.040(3) 0.020(2) 0.010(2) 0.012(2) C24 0.061(3) 0.048(3) 0.035(3) 0.012(3) -0.006(2) 0.008(3) C25 0.034(3) 0.039(3) 0.032(3) 0.019(2) 0.002(2) 0.008(2) C26 0.050(3) 0.070(4) 0.050(4) 0.031(3) -0.017(3) -0.016(3) C27 0.061(3) 0.061(4) 0.063(4) 0.034(3) -0.009(3) -0.026(3) C28 0.033(3) 0.041(3) 0.041(3) 0.020(2) 0.000(2) 0.012(2) C29 0.039(3) 0.061(4) 0.101(5) 0.052(4) 0.015(3) 0.007(3) C30 0.041(3) 0.063(4) 0.061(4) 0.017(3) -0.012(3) 0.001(3) C31 0.027(2) 0.037(3) 0.029(3) 0.015(2) 0.0005(19) -0.003(2) C32 0.045(3) 0.044(3) 0.046(3) 0.021(3) 0.005(2) 0.017(2) C33 0.054(3) 0.039(3) 0.035(3) 0.019(2) 0.012(2) 0.011(2) C34 0.035(3) 0.030(3) 0.031(3) 0.014(2) -0.004(2) -0.005(2) C35 0.048(3) 0.050(3) 0.058(4) 0.031(3) -0.007(3) 0.007(3) C36 0.044(3) 0.050(3) 0.057(4) 0.036(3) 0.000(2) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O3 2.090(3) 2_565 ? Fe1 O3 2.090(3) . ? Fe1 O2A 2.116(7) 2_565 ? Fe1 O2A 2.116(7) . ? Fe1 O2B 2.120(7) 2_565 ? Fe1 O2B 2.120(7) . ? Fe1 O1B 2.120(7) . ? Fe1 O1B 2.120(7) 2_565 ? Fe1 O1A 2.162(7) . ? Fe1 O1A 2.162(7) 2_565 ? Fe2 O5 2.064(3) 2_755 ? Fe2 O5 2.064(3) . ? Fe2 O4 2.110(3) . ? Fe2 O4 2.110(3) 2_755 ? Fe2 O6 2.157(3) 2_755 ? Fe2 O6 2.157(3) . ? Fe3 O10 2.091(3) . ? Fe3 O7 2.092(3) . ? Fe3 O8 2.107(3) . ? Fe3 O11 2.130(3) . ? Fe3 O12 2.144(3) . ? Fe3 O9 2.146(3) . ? Fe4 Cl1 2.3094(18) . ? Fe4 Cl3 2.317(2) . ? Fe4 Cl2 2.324(2) . ? Fe4 Cl4 2.3257(16) . ? Fe5 Cl8 2.296(2) . ? Fe5 Cl7 2.3034(17) . ? Fe5 Cl6 2.306(2) . ? Fe5 Cl5 2.3290(15) . ? O1A C1A 0.940(9) . ? C1A N1 1.329(10) . ? C1A H1A 0.9500 . ? O1B C1B 0.827(9) . ? C1B N1 1.450(11) . ? C1B H1B 0.9500 . ? O2A C4A 0.920(10) . ? C4A N2 1.340(11) . ? C4A H4A 0.9500 . ? O2B C4B 0.947(10) . ? C4B N2 1.402(11) . ? C4B H4B 0.9500 . ? O3 C7 1.235(5) . ? O4 C10 1.246(5) . ? O5 C13 1.246(5) . ? O6 C16 1.245(5) . ? O7 C19 1.237(5) . ? O8 C22 1.256(5) . ? O9 C25 1.239(5) . ? O10 C28 1.235(5) . ? O11 C31 1.250(5) . ? O12 C34 1.240(5) . ? N1 C2 1.423(7) . ? N1 C3 1.440(7) . ? N2 C5 1.419(7) . ? N2 C6 1.438(7) . ? N3 C7 1.320(5) . ? N3 C9 1.446(6) . ? N3 C8 1.456(6) . ? N4 C10 1.303(5) . ? N4 C12 1.460(6) . ? N4 C11 1.464(6) . ? N5 C13 1.304(5) . ? N5 C14 1.458(6) . ? N5 C15 1.461(5) . ? N6 C16 1.319(5) . ? N6 C17 1.451(6) . ? N6 C18 1.461(6) . ? N7 C19 1.315(6) . ? N7 C20 1.443(7) . ? N7 C21 1.461(6) . ? N8 C22 1.306(5) . ? N8 C24 1.455(6) . ? N8 C23 1.462(5) . ? N9 C25 1.304(6) . ? N9 C27 1.449(6) . ? N9 C26 1.458(6) . ? N10 C28 1.311(6) . ? N10 C30 1.446(6) . ? N10 C29 1.465(6) . ? N11 C31 1.310(5) . ? N11 C33 1.444(6) . ? N11 C32 1.456(5) . ? N12 C34 1.314(5) . ? N12 C36 1.459(6) . ? N12 C35 1.467(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Fe1 O3 180.00(19) 2_565 . ? O3 Fe1 O2A 81.44(19) 2_565 2_565 ? O3 Fe1 O2A 98.6(2) . 2_565 ? O3 Fe1 O2A 98.6(2) 2_565 . ? O3 Fe1 O2A 81.44(19) . . ? O2A Fe1 O2A 180.000(1) 2_565 . ? O3 Fe1 O2B 92.95(19) 2_565 2_565 ? O3 Fe1 O2B 87.05(19) . 2_565 ? O2A Fe1 O2B 23.2(2) 2_565 2_565 ? O2A Fe1 O2B 156.8(2) . 2_565 ? O3 Fe1 O2B 87.05(19) 2_565 . ? O3 Fe1 O2B 92.95(19) . . ? O2A Fe1 O2B 156.8(2) 2_565 . ? O2A Fe1 O2B 23.2(2) . . ? O2B Fe1 O2B 180.0(4) 2_565 . ? O3 Fe1 O1B 84.00(19) 2_565 . ? O3 Fe1 O1B 96.00(19) . . ? O2A Fe1 O1B 111.5(3) 2_565 . ? O2A Fe1 O1B 68.5(3) . . ? O2B Fe1 O1B 93.0(3) 2_565 . ? O2B Fe1 O1B 87.0(3) . . ? O3 Fe1 O1B 96.00(19) 2_565 2_565 ? O3 Fe1 O1B 84.00(19) . 2_565 ? O2A Fe1 O1B 68.5(3) 2_565 2_565 ? O2A Fe1 O1B 111.5(3) . 2_565 ? O2B Fe1 O1B 87.0(3) 2_565 2_565 ? O2B Fe1 O1B 93.0(3) . 2_565 ? O1B Fe1 O1B 180.0(2) . 2_565 ? O3 Fe1 O1A 92.23(18) 2_565 . ? O3 Fe1 O1A 87.77(18) . . ? O2A Fe1 O1A 91.6(3) 2_565 . ? O2A Fe1 O1A 88.4(3) . . ? O2B Fe1 O1A 71.1(3) 2_565 . ? O2B Fe1 O1A 108.9(3) . . ? O1B Fe1 O1A 23.0(2) . . ? O1B Fe1 O1A 157.0(2) 2_565 . ? O3 Fe1 O1A 87.77(18) 2_565 2_565 ? O3 Fe1 O1A 92.23(18) . 2_565 ? O2A Fe1 O1A 88.4(3) 2_565 2_565 ? O2A Fe1 O1A 91.6(3) . 2_565 ? O2B Fe1 O1A 108.9(3) 2_565 2_565 ? O2B Fe1 O1A 71.1(3) . 2_565 ? O1B Fe1 O1A 157.0(2) . 2_565 ? O1B Fe1 O1A 23.0(2) 2_565 2_565 ? O1A Fe1 O1A 180.0(6) . 2_565 ? O5 Fe2 O5 180.00(11) 2_755 . ? O5 Fe2 O4 91.08(12) 2_755 . ? O5 Fe2 O4 88.92(12) . . ? O5 Fe2 O4 88.92(12) 2_755 2_755 ? O5 Fe2 O4 91.08(12) . 2_755 ? O4 Fe2 O4 180.0(3) . 2_755 ? O5 Fe2 O6 93.77(12) 2_755 2_755 ? O5 Fe2 O6 86.23(12) . 2_755 ? O4 Fe2 O6 85.92(13) . 2_755 ? O4 Fe2 O6 94.08(13) 2_755 2_755 ? O5 Fe2 O6 86.23(12) 2_755 . ? O5 Fe2 O6 93.77(12) . . ? O4 Fe2 O6 94.08(13) . . ? O4 Fe2 O6 85.92(13) 2_755 . ? O6 Fe2 O6 180.0(3) 2_755 . ? O10 Fe3 O7 89.44(14) . . ? O10 Fe3 O8 92.40(14) . . ? O7 Fe3 O8 175.57(11) . . ? O10 Fe3 O11 90.63(12) . . ? O7 Fe3 O11 88.22(12) . . ? O8 Fe3 O11 87.73(12) . . ? O10 Fe3 O12 88.97(12) . . ? O7 Fe3 O12 89.90(12) . . ? O8 Fe3 O12 94.16(12) . . ? O11 Fe3 O12 178.08(11) . . ? O10 Fe3 O9 176.49(12) . . ? O7 Fe3 O9 91.55(14) . . ? O8 Fe3 O9 86.86(13) . . ? O11 Fe3 O9 92.76(12) . . ? O12 Fe3 O9 87.67(12) . . ? Cl1 Fe4 Cl3 114.83(7) . . ? Cl1 Fe4 Cl2 106.56(7) . . ? Cl3 Fe4 Cl2 105.63(7) . . ? Cl1 Fe4 Cl4 107.91(7) . . ? Cl3 Fe4 Cl4 107.58(7) . . ? Cl2 Fe4 Cl4 114.54(7) . . ? Cl8 Fe5 Cl7 112.10(8) . . ? Cl8 Fe5 Cl6 105.53(8) . . ? Cl7 Fe5 Cl6 106.28(7) . . ? Cl8 Fe5 Cl5 109.70(7) . . ? Cl7 Fe5 Cl5 109.41(7) . . ? Cl6 Fe5 Cl5 113.80(6) . . ? C1A O1A Fe1 173.8(9) . . ? O1A C1A N1 153.4(12) . . ? O1A C1A H1A 103.3 . . ? N1 C1A H1A 103.3 . . ? C1B O1B Fe1 161.6(11) . . ? O1B C1B N1 169.2(13) . . ? O1B C1B H1B 95.4 . . ? N1 C1B H1B 95.4 . . ? C4A O2A Fe1 157.3(8) . . ? O2A C4A N2 145.7(11) . . ? O2A C4A H4A 107.1 . . ? N2 C4A H4A 107.1 . . ? C4B O2B Fe1 152.3(9) . . ? O2B C4B N2 156.7(10) . . ? O2B C4B H4B 101.7 . . ? N2 C4B H4B 101.7 . . ? C7 O3 Fe1 127.0(3) . . ? C10 O4 Fe2 129.0(3) . . ? C13 O5 Fe2 133.4(3) . . ? C16 O6 Fe2 118.7(3) . . ? C19 O7 Fe3 126.1(3) . . ? C22 O8 Fe3 121.1(3) . . ? C25 O9 Fe3 126.6(3) . . ? C28 O10 Fe3 123.8(3) . . ? C31 O11 Fe3 124.4(3) . . ? C34 O12 Fe3 125.6(3) . . ? C1A N1 C2 105.7(6) . . ? C1A N1 C3 138.6(6) . . ? C2 N1 C3 115.7(4) . . ? C1A N1 C1B 36.5(5) . . ? C2 N1 C1B 142.1(6) . . ? C3 N1 C1B 102.1(6) . . ? C4A N2 C4B 38.4(5) . . ? C4A N2 C5 138.3(6) . . ? C4B N2 C5 100.4(6) . . ? C4A N2 C6 104.6(6) . . ? C4B N2 C6 142.2(6) . . ? C5 N2 C6 117.1(5) . . ? C7 N3 C9 122.2(4) . . ? C7 N3 C8 121.4(4) . . ? C9 N3 C8 116.4(4) . . ? C10 N4 C12 121.1(4) . . ? C10 N4 C11 121.6(4) . . ? C12 N4 C11 117.2(4) . . ? C13 N5 C14 121.8(4) . . ? C13 N5 C15 120.4(4) . . ? C14 N5 C15 117.4(4) . . ? C16 N6 C17 121.4(4) . . ? C16 N6 C18 120.5(4) . . ? C17 N6 C18 118.0(4) . . ? C19 N7 C20 122.3(4) . . ? C19 N7 C21 120.4(4) . . ? C20 N7 C21 117.3(4) . . ? C22 N8 C24 120.8(4) . . ? C22 N8 C23 122.1(4) . . ? C24 N8 C23 117.0(4) . . ? C25 N9 C27 122.0(4) . . ? C25 N9 C26 121.5(4) . . ? C27 N9 C26 116.4(4) . . ? C28 N10 C30 119.9(4) . . ? C28 N10 C29 121.6(4) . . ? C30 N10 C29 118.5(4) . . ? C31 N11 C33 121.3(3) . . ? C31 N11 C32 121.7(4) . . ? C33 N11 C32 116.7(3) . . ? C34 N12 C36 121.3(4) . . ? C34 N12 C35 121.9(4) . . ? C36 N12 C35 116.7(4) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 N3 124.0(4) . . ? O3 C7 H7 118.0 . . ? N3 C7 H7 118.0 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 N4 124.3(4) . . ? O4 C10 H10 117.8 . . ? N4 C10 H10 117.8 . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 N5 124.5(4) . . ? O5 C13 H13 117.7 . . ? N5 C13 H13 117.7 . . ? N5 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 H15A 109.5 . . ? N5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O6 C16 N6 124.7(4) . . ? O6 C16 H16 117.6 . . ? N6 C16 H16 117.6 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N6 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O7 C19 N7 125.0(5) . . ? O7 C19 H19 117.5 . . ? N7 C19 H19 117.5 . . ? N7 C20 H20A 109.5 . . ? N7 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N7 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N7 C21 H21A 109.5 . . ? N7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O8 C22 N8 124.5(4) . . ? O8 C22 H22 117.8 . . ? N8 C22 H22 117.8 . . ? N8 C23 H23A 109.5 . . ? N8 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N8 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N8 C24 H24A 109.5 . . ? N8 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N8 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O9 C25 N9 125.2(4) . . ? O9 C25 H25 117.4 . . ? N9 C25 H25 117.4 . . ? N9 C26 H26A 109.5 . . ? N9 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N9 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N9 C27 H27A 109.5 . . ? N9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O10 C28 N10 124.4(4) . . ? O10 C28 H28 117.8 . . ? N10 C28 H28 117.8 . . ? N10 C29 H29A 109.5 . . ? N10 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N10 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N10 C30 H30A 109.5 . . ? N10 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N10 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O11 C31 N11 125.1(4) . . ? O11 C31 H31 117.5 . . ? N11 C31 H31 117.5 . . ? N11 C32 H32A 109.5 . . ? N11 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N11 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N11 C33 H33A 109.5 . . ? N11 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N11 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O12 C34 N12 124.8(4) . . ? O12 C34 H34 117.6 . . ? N12 C34 H34 117.6 . . ? N12 C35 H35A 109.5 . . ? N12 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N12 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N12 C36 H36A 109.5 . . ? N12 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N12 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Fe1 O1A C1A 57(7) 2_565 . . . ? O3 Fe1 O1A C1A -123(7) . . . . ? O2A Fe1 O1A C1A 139(7) 2_565 . . . ? O2A Fe1 O1A C1A -41(7) . . . . ? O2B Fe1 O1A C1A 150(7) 2_565 . . . ? O2B Fe1 O1A C1A -30(7) . . . . ? O1B Fe1 O1A C1A -12(7) . . . . ? O1B Fe1 O1A C1A 168(7) 2_565 . . . ? O1A Fe1 O1A C1A -57(100) 2_565 . . . ? Fe1 O1A C1A N1 3(9) . . . . ? O3 Fe1 O1B C1B -90(3) 2_565 . . . ? O3 Fe1 O1B C1B 90(3) . . . . ? O2A Fe1 O1B C1B -11(3) 2_565 . . . ? O2A Fe1 O1B C1B 169(3) . . . . ? O2B Fe1 O1B C1B 3(3) 2_565 . . . ? O2B Fe1 O1B C1B -177(3) . . . . ? O1B Fe1 O1B C1B 153(100) 2_565 . . . ? O1A Fe1 O1B C1B 21(3) . . . . ? O1A Fe1 O1B C1B -159(3) 2_565 . . . ? Fe1 O1B C1B N1 -45(8) . . . . ? O3 Fe1 O2A C4A 150(2) 2_565 . . . ? O3 Fe1 O2A C4A -30(2) . . . . ? O2A Fe1 O2A C4A -143(100) 2_565 . . . ? O2B Fe1 O2A C4A -91(2) 2_565 . . . ? O2B Fe1 O2A C4A 89(2) . . . . ? O1B Fe1 O2A C4A -130(2) . . . . ? O1B Fe1 O2A C4A 50(2) 2_565 . . . ? O1A Fe1 O2A C4A -118(2) . . . . ? O1A Fe1 O2A C4A 62(2) 2_565 . . . ? Fe1 O2A C4A N2 -141.1(16) . . . . ? O3 Fe1 O2B C4B -104.3(17) 2_565 . . . ? O3 Fe1 O2B C4B 75.7(17) . . . . ? O2A Fe1 O2B C4B -164.4(15) 2_565 . . . ? O2A Fe1 O2B C4B 15.6(15) . . . . ? O2B Fe1 O2B C4B -79(100) 2_565 . . . ? O1B Fe1 O2B C4B -20.2(16) . . . . ? O1B Fe1 O2B C4B 159.8(16) 2_565 . . . ? O1A Fe1 O2B C4B -13.0(17) . . . . ? O1A Fe1 O2B C4B 167.0(17) 2_565 . . . ? Fe1 O2B C4B N2 -82(3) . . . . ? O3 Fe1 O3 C7 111(100) 2_565 . . . ? O2A Fe1 O3 C7 54.6(4) 2_565 . . . ? O2A Fe1 O3 C7 -125.4(4) . . . . ? O2B Fe1 O3 C7 34.5(4) 2_565 . . . ? O2B Fe1 O3 C7 -145.5(4) . . . . ? O1B Fe1 O3 C7 -58.2(4) . . . . ? O1B Fe1 O3 C7 121.8(4) 2_565 . . . ? O1A Fe1 O3 C7 -36.7(4) . . . . ? O1A Fe1 O3 C7 143.3(4) 2_565 . . . ? O5 Fe2 O4 C10 75.7(4) 2_755 . . . ? O5 Fe2 O4 C10 -104.3(4) . . . . ? O4 Fe2 O4 C10 -111(100) 2_755 . . . ? O6 Fe2 O4 C10 169.4(4) 2_755 . . . ? O6 Fe2 O4 C10 -10.6(4) . . . . ? O5 Fe2 O5 C13 141(100) 2_755 . . . ? O4 Fe2 O5 C13 167.0(4) . . . . ? O4 Fe2 O5 C13 -13.0(4) 2_755 . . . ? O6 Fe2 O5 C13 -107.0(4) 2_755 . . . ? O6 Fe2 O5 C13 73.0(4) . . . . ? O5 Fe2 O6 C16 48.6(3) 2_755 . . . ? O5 Fe2 O6 C16 -131.4(3) . . . . ? O4 Fe2 O6 C16 139.4(3) . . . . ? O4 Fe2 O6 C16 -40.6(3) 2_755 . . . ? O6 Fe2 O6 C16 -69(100) 2_755 . . . ? O10 Fe3 O7 C19 -139.4(4) . . . . ? O8 Fe3 O7 C19 106.1(16) . . . . ? O11 Fe3 O7 C19 129.9(4) . . . . ? O12 Fe3 O7 C19 -50.4(4) . . . . ? O9 Fe3 O7 C19 37.2(4) . . . . ? O10 Fe3 O8 C22 -149.5(3) . . . . ? O7 Fe3 O8 C22 -35.1(18) . . . . ? O11 Fe3 O8 C22 -59.0(3) . . . . ? O12 Fe3 O8 C22 121.4(3) . . . . ? O9 Fe3 O8 C22 33.9(3) . . . . ? O10 Fe3 O9 C25 8(2) . . . . ? O7 Fe3 O9 C25 -97.9(4) . . . . ? O8 Fe3 O9 C25 86.3(4) . . . . ? O11 Fe3 O9 C25 173.9(3) . . . . ? O12 Fe3 O9 C25 -8.0(4) . . . . ? O7 Fe3 O10 C28 -106.6(4) . . . . ? O8 Fe3 O10 C28 69.3(4) . . . . ? O11 Fe3 O10 C28 -18.4(4) . . . . ? O12 Fe3 O10 C28 163.5(4) . . . . ? O9 Fe3 O10 C28 147.0(19) . . . . ? O10 Fe3 O11 C31 -128.0(3) . . . . ? O7 Fe3 O11 C31 -38.6(3) . . . . ? O8 Fe3 O11 C31 139.6(3) . . . . ? O12 Fe3 O11 C31 -50(3) . . . . ? O9 Fe3 O11 C31 52.9(3) . . . . ? O10 Fe3 O12 C34 -14.7(3) . . . . ? O7 Fe3 O12 C34 -104.1(4) . . . . ? O8 Fe3 O12 C34 77.7(4) . . . . ? O11 Fe3 O12 C34 -93(3) . . . . ? O9 Fe3 O12 C34 164.3(3) . . . . ? O1A C1A N1 C2 -175(2) . . . . ? O1A C1A N1 C3 2(3) . . . . ? O1A C1A N1 C1B 3.4(17) . . . . ? O1B C1B N1 C1A 20(6) . . . . ? O1B C1B N1 C2 23(7) . . . . ? O1B C1B N1 C3 -161(6) . . . . ? O2A C4A N2 C4B 24.4(16) . . . . ? O2A C4A N2 C5 35(2) . . . . ? O2A C4A N2 C6 -146.0(19) . . . . ? O2B C4B N2 C4A 39(3) . . . . ? O2B C4B N2 C5 -134(3) . . . . ? O2B C4B N2 C6 54(3) . . . . ? Fe1 O3 C7 N3 177.6(3) . . . . ? C9 N3 C7 O3 -177.4(4) . . . . ? C8 N3 C7 O3 1.0(7) . . . . ? Fe2 O4 C10 N4 176.3(3) . . . . ? C12 N4 C10 O4 0.1(7) . . . . ? C11 N4 C10 O4 176.8(4) . . . . ? Fe2 O5 C13 N5 166.1(3) . . . . ? C14 N5 C13 O5 173.6(4) . . . . ? C15 N5 C13 O5 1.1(7) . . . . ? Fe2 O6 C16 N6 -179.7(3) . . . . ? C17 N6 C16 O6 -179.7(5) . . . . ? C18 N6 C16 O6 -0.2(7) . . . . ? Fe3 O7 C19 N7 -179.9(3) . . . . ? C20 N7 C19 O7 -0.7(7) . . . . ? C21 N7 C19 O7 176.6(4) . . . . ? Fe3 O8 C22 N8 -170.6(3) . . . . ? C24 N8 C22 O8 173.8(4) . . . . ? C23 N8 C22 O8 -1.9(7) . . . . ? Fe3 O9 C25 N9 -144.9(3) . . . . ? C27 N9 C25 O9 -179.3(4) . . . . ? C26 N9 C25 O9 0.8(7) . . . . ? Fe3 O10 C28 N10 154.4(3) . . . . ? C30 N10 C28 O10 -2.8(7) . . . . ? C29 N10 C28 O10 177.6(4) . . . . ? Fe3 O11 C31 N11 -179.7(3) . . . . ? C33 N11 C31 O11 1.1(7) . . . . ? C32 N11 C31 O11 175.6(4) . . . . ? Fe3 O12 C34 N12 -177.1(3) . . . . ? C36 N12 C34 O12 -2.1(7) . . . . ? C35 N12 C34 O12 178.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.841 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.841 _refine_diff_density_max 0.770 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.084