# Electronic Supplementary Material (ESI) for Chemical Communications # 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_7mz6fecl2 _database_code_depnum_ccdc_archive 'CCDC 896157' #TrackingRef 'Fe3_IL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H11 N2 O2, Cl4 Fe' _chemical_formula_sum 'C7 H11 Cl4 Fe N2 O2' _chemical_formula_weight 352.83 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 6.3649(5) _cell_length_b 14.6411(11) _cell_length_c 15.9618(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.004(9) _cell_angle_gamma 90.00 _cell_volume 1460.12(19) _cell_formula_units_Z 4 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 25.58 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 1.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.407 _exptl_absorpt_correction_T_max 0.491 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(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 'Stoe IPDS' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11346 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.93 _reflns_number_total 2832 _reflns_number_gt 2457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_cell_refinement 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_data_reduction 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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^)+(0.0582P)^2^+0.4389P] 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 2832 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.38045(5) 0.30389(2) 0.34667(2) 0.03173(12) Uani 1 1 d . . . Cl1 Cl 0.21824(11) 0.31584(5) 0.21197(4) 0.04832(18) Uani 1 1 d . . . Cl2 Cl 0.25380(10) 0.19013(4) 0.41370(4) 0.04435(17) Uani 1 1 d . . . Cl3 Cl 0.33913(11) 0.43230(4) 0.41427(4) 0.04549(17) Uani 1 1 d . . . Cl4 Cl 0.72816(10) 0.28552(5) 0.35164(5) 0.04940(18) Uani 1 1 d . . . C7 C 0.6996(5) 0.0079(2) 0.42467(19) 0.0597(8) Uani 1 1 d . . . H7A H 0.7223 -0.0167 0.4814 0.089 Uiso 1 1 calc R . . H7B H 0.7171 0.0730 0.4275 0.089 Uiso 1 1 calc R . . H7C H 0.8016 -0.0181 0.3943 0.089 Uiso 1 1 calc R . . O1 O 0.4828(3) -0.01422(14) 0.38018(12) 0.0517(5) Uani 1 1 d . . . O2 O 0.5309(3) 0.07371(14) 0.26840(12) 0.0494(4) Uani 1 1 d . . . C1 C 0.4206(4) 0.02537(17) 0.30346(16) 0.0418(5) Uani 1 1 d . . . C2 C 0.1924(5) -0.00157(19) 0.26569(18) 0.0499(6) Uani 1 1 d . . . H2A H 0.1908 -0.0638 0.2448 0.060 Uiso 1 1 calc R . . H2B H 0.1075 0.0003 0.3101 0.060 Uiso 1 1 calc R . . N1 N 0.0950(3) 0.05850(15) 0.19573(14) 0.0436(5) Uani 1 1 d . . . C3 C -0.0704(4) 0.11402(19) 0.19795(17) 0.0450(6) Uani 1 1 d . . . H3A H -0.1370 0.1222 0.2444 0.054 Uiso 1 1 calc R . . N2 N -0.1246(3) 0.15584(18) 0.12274(14) 0.0464(5) Uani 1 1 d . . . C4 C 0.0130(4) 0.1261(2) 0.07014(18) 0.0508(6) Uani 1 1 d . . . H4A H 0.0114 0.1447 0.0143 0.061 Uiso 1 1 calc R . . C5 C 0.1494(4) 0.0652(2) 0.11543(17) 0.0485(6) Uani 1 1 d . . . H5A H 0.2586 0.0338 0.0966 0.058 Uiso 1 1 calc R . . C6 C -0.3005(5) 0.2217(3) 0.1004(2) 0.0671(9) Uani 1 1 d . . . H6A H -0.2468 0.2771 0.0802 0.101 Uiso 1 1 calc R . . H6B H -0.3606 0.2345 0.1499 0.101 Uiso 1 1 calc R . . H6C H -0.4090 0.1964 0.0564 0.101 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 0.02951(19) 0.03008(19) 0.03584(19) -0.00039(12) 0.00681(13) 0.00048(12) Cl1 0.0530(4) 0.0503(4) 0.0380(3) 0.0007(2) -0.0006(3) -0.0058(3) Cl2 0.0462(3) 0.0352(3) 0.0551(4) 0.0087(2) 0.0183(3) 0.0021(2) Cl3 0.0566(4) 0.0335(3) 0.0481(3) -0.0060(2) 0.0144(3) 0.0022(3) Cl4 0.0306(3) 0.0542(4) 0.0644(4) -0.0028(3) 0.0117(3) 0.0020(3) C7 0.0658(18) 0.0655(19) 0.0496(15) 0.0088(14) 0.0158(14) 0.0152(16) O1 0.0644(12) 0.0453(10) 0.0515(10) 0.0098(8) 0.0266(9) 0.0075(9) O2 0.0499(10) 0.0580(12) 0.0436(9) 0.0026(8) 0.0175(8) -0.0103(9) C1 0.0537(14) 0.0331(11) 0.0446(13) -0.0013(10) 0.0241(11) -0.0010(11) C2 0.0559(16) 0.0407(14) 0.0580(16) -0.0020(12) 0.0235(13) -0.0139(12) N1 0.0422(11) 0.0449(12) 0.0475(12) -0.0101(9) 0.0182(9) -0.0114(9) C3 0.0390(13) 0.0541(15) 0.0454(13) -0.0173(12) 0.0168(10) -0.0121(11) N2 0.0344(10) 0.0595(14) 0.0456(12) -0.0177(10) 0.0083(9) -0.0075(10) C4 0.0477(14) 0.0650(18) 0.0434(13) -0.0130(12) 0.0178(11) -0.0079(13) C5 0.0472(14) 0.0559(16) 0.0479(14) -0.0132(12) 0.0228(11) -0.0059(12) C6 0.0464(16) 0.093(3) 0.0591(18) -0.0125(17) 0.0032(14) 0.0110(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Cl1 2.2073(7) . ? Fe1 Cl3 2.2083(7) . ? Fe1 Cl2 2.2130(7) . ? Fe1 Cl4 2.2158(7) . ? C7 O1 1.462(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? O1 C1 1.344(3) . ? O2 C1 1.207(3) . ? C1 C2 1.515(4) . ? C2 N1 1.463(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N1 C3 1.336(3) . ? N1 C5 1.393(3) . ? C3 N2 1.333(4) . ? C3 H3A 0.9300 . ? N2 C4 1.393(3) . ? N2 C6 1.469(4) . ? C4 C5 1.354(4) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Fe1 Cl3 109.35(3) . . ? Cl1 Fe1 Cl2 112.63(3) . . ? Cl3 Fe1 Cl2 108.43(3) . . ? Cl1 Fe1 Cl4 108.83(3) . . ? Cl3 Fe1 Cl4 107.28(3) . . ? Cl2 Fe1 Cl4 110.17(3) . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 O1 C7 115.7(2) . . ? O2 C1 O1 125.4(3) . . ? O2 C1 C2 124.5(2) . . ? O1 C1 C2 110.1(2) . . ? N1 C2 C1 112.4(2) . . ? N1 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C3 N1 C5 108.5(2) . . ? C3 N1 C2 124.5(2) . . ? C5 N1 C2 126.9(2) . . ? N2 C3 N1 109.0(2) . . ? N2 C3 H3A 125.5 . . ? N1 C3 H3A 125.5 . . ? C3 N2 C4 108.4(2) . . ? C3 N2 C6 125.1(2) . . ? C4 N2 C6 126.6(3) . . ? C5 C4 N2 107.3(2) . . ? C5 C4 H4A 126.4 . . ? N2 C4 H4A 126.4 . . ? C4 C5 N1 106.9(2) . . ? C4 C5 H5A 126.5 . . ? N1 C5 H5A 126.5 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.228 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.076 data_fe37s _database_code_depnum_ccdc_archive 'CCDC 896158' #TrackingRef 'Fe3_IL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H64 Cl28 Fe10 N12 O21, 7(Cl4 Fe), 5(H2 O)' _chemical_formula_sum 'C36 H64 Cl28 Fe10 N12 O21' _chemical_formula_weight 2552.09 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 12.6816(9) _cell_length_b 26.2169(14) _cell_length_c 15.5404(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.243(5) _cell_angle_gamma 90.00 _cell_volume 4878.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31601 _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 26.36 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 2.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.571 _exptl_absorpt_correction_T_max 0.640 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67061 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9461 _reflns_number_gt 6622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. One FeCl4 anion (Fe(8)) was disordered either side of the mirror plane, with the two mirror-related components overlapping. The half-occupancy anion was refined with similarity restraints applied both to the Fe-Cl and Cl..Cl distances, and to the anisotropic thermal parameters (DELU) of the five atoms. It proved not possible to refine the hydrogen atoms of the aquo ligands. Lattice waters were disordered between the (FeCl4)- anions, and proved difficult to model in the presence of the heavy atoms of the anions. They were handled using SQUEEZE: ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.099 0.250 0.113 79 23 '2 H2O (= 20 e)' 2 -0.100 0.750 0.887 78 23 '2 H2O (= 20 e)' 3 0.237 0.624 0.027 79 15 '1.5 H2O (= 15 e)' 4 0.237 0.876 0.027 79 15 '1.5 H2O (= 15 e)' 5 0.762 0.124 0.973 78 15 '1.5 H2O (= 15 e)' 6 0.763 0.376 0.973 79 15 '1.5 H2O (= 15 e)' _platon_squeeze_details ; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _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^)+(0.1173P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9461 _refine_ls_number_parameters 511 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1726 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.44009(8) 0.2500 0.19156(7) 0.0383(2) Uani 1 2 d S . . Fe2 Fe 0.67141(8) 0.2500 0.36962(7) 0.0376(2) Uani 1 2 d S . . Fe3 Fe 0.68962(10) 0.2500 0.16292(8) 0.0458(3) Uani 1 2 d S . . O1 O 0.6008(4) 0.2500 0.2418(3) 0.0408(11) Uani 1 2 d S . . O2 O 0.4200(3) 0.30488(14) 0.2754(3) 0.0440(8) Uani 1 1 d . . . O3 O 0.5755(3) 0.30507(13) 0.3975(2) 0.0409(8) Uani 1 1 d . . . C1 C 0.4806(4) 0.32128(17) 0.3507(4) 0.0372(11) Uani 1 1 d . . . C2 C 0.4304(4) 0.36516(19) 0.3884(4) 0.0431(12) Uani 1 1 d . . . H2A H 0.4110 0.3931 0.3430 0.052 Uiso 1 1 calc R . . H2B H 0.3602 0.3533 0.3967 0.052 Uiso 1 1 calc R . . N1 N 0.5028(4) 0.38532(15) 0.4741(3) 0.0424(10) Uani 1 1 d . . . C3 C 0.5148(5) 0.3687(2) 0.5567(4) 0.0489(13) Uani 1 1 d . . . H3A H 0.4752 0.3406 0.5699 0.059 Uiso 1 1 calc R . . N2 N 0.5887(4) 0.39601(17) 0.6181(3) 0.0482(11) Uani 1 1 d . . . C4 C 0.6227(8) 0.4339(3) 0.5725(5) 0.087(3) Uani 1 1 d . . . H4A H 0.6751 0.4600 0.5993 0.104 Uiso 1 1 calc R . . C5 C 0.5689(8) 0.4274(3) 0.4833(5) 0.082(2) Uani 1 1 d . . . H5A H 0.5755 0.4482 0.4353 0.099 Uiso 1 1 calc R . . C6 C 0.6225(6) 0.3905(3) 0.7177(4) 0.0618(16) Uani 1 1 d . . . H6A H 0.5731 0.3660 0.7331 0.093 Uiso 1 1 calc R . . H6B H 0.6173 0.4236 0.7452 0.093 Uiso 1 1 calc R . . H6C H 0.6997 0.3782 0.7412 0.093 Uiso 1 1 calc R . . O4 O 0.7824(3) 0.30615(14) 0.3718(3) 0.0458(8) Uani 1 1 d . . . O5 O 0.7949(3) 0.30477(16) 0.2314(3) 0.0571(10) Uani 1 1 d . . . C7 C 0.8150(5) 0.3234(2) 0.3086(5) 0.0510(14) Uani 1 1 d . . . C8 C 0.8850(6) 0.3712(2) 0.3247(5) 0.0632(17) Uani 1 1 d . . . H8A H 0.9531 0.3643 0.3088 0.076 Uiso 1 1 calc R . . H8B H 0.8423 0.3982 0.2834 0.076 Uiso 1 1 calc R . . N3 N 0.9178(4) 0.38979(17) 0.4177(4) 0.0520(12) Uani 1 1 d . . . C9 C 1.0015(6) 0.3739(3) 0.4837(6) 0.0693(19) Uani 1 1 d . . . H9A H 1.0508 0.3477 0.4784 0.083 Uiso 1 1 calc R . . N4 N 1.0111(4) 0.3984(2) 0.5602(4) 0.0668(15) Uani 1 1 d . . . C10 C 0.9305(9) 0.4329(4) 0.5396(7) 0.115(4) Uani 1 1 d . . . H10A H 0.9160 0.4570 0.5801 0.138 Uiso 1 1 calc R . . C11 C 0.8738(10) 0.4274(5) 0.4516(7) 0.135(5) Uani 1 1 d . . . H11A H 0.8114 0.4474 0.4179 0.161 Uiso 1 1 calc R . . C12 C 1.0960(7) 0.3906(5) 0.6512(8) 0.120(4) Uani 1 1 d . . . H12A H 1.0994 0.3543 0.6672 0.181 Uiso 1 1 calc R . . H12B H 1.0757 0.4105 0.6967 0.181 Uiso 1 1 calc R . . H12C H 1.1692 0.4018 0.6498 0.181 Uiso 1 1 calc R . . O6 O 0.6023(4) 0.30546(16) 0.0825(3) 0.0557(10) Uani 1 1 d . . . O7 O 0.4321(3) 0.30503(15) 0.0980(3) 0.0493(9) Uani 1 1 d . . . C13 C 0.5043(5) 0.3217(2) 0.0658(4) 0.0511(13) Uani 1 1 d . . . C14 C 0.4752(6) 0.3662(3) 0.0011(5) 0.0609(16) Uani 1 1 d . . . H14A H 0.5226 0.3956 0.0298 0.073 Uiso 1 1 calc R . . H14B H 0.4924 0.3572 -0.0547 0.073 Uiso 1 1 calc R . . N5 N 0.3582(5) 0.3811(2) -0.0244(4) 0.0594(13) Uani 1 1 d . . . C15 C 0.3211(6) 0.4218(3) 0.0065(4) 0.0647(17) Uani 1 1 d . . . H15A H 0.3663 0.4457 0.0485 0.078 Uiso 1 1 calc R . . N6 N 0.2117(5) 0.4241(3) -0.0301(4) 0.0726(16) Uani 1 1 d . . . C16 C 0.1787(7) 0.3829(4) -0.0892(6) 0.089(2) Uani 1 1 d . . . H16A H 0.1042 0.3748 -0.1254 0.107 Uiso 1 1 calc R . . C17 C 0.2694(7) 0.3568(3) -0.0862(6) 0.083(2) Uani 1 1 d . . . H17A H 0.2724 0.3270 -0.1202 0.100 Uiso 1 1 calc R . . C18 C 0.1396(7) 0.4646(4) -0.0163(6) 0.093(3) Uani 1 1 d . . . H18A H 0.1854 0.4905 0.0248 0.140 Uiso 1 1 calc R . . H18B H 0.0864 0.4502 0.0107 0.140 Uiso 1 1 calc R . . H18C H 0.0987 0.4803 -0.0750 0.140 Uiso 1 1 calc R . . O8 O 0.2695(5) 0.2500 0.1373(4) 0.0551(14) Uani 1 2 d S . . O9 O 0.7489(5) 0.2500 0.5104(4) 0.0580(14) Uani 1 2 d S . . O10 O 0.7816(5) 0.2500 0.0752(4) 0.0641(16) Uani 1 2 d S . . Fe4 Fe 0.14178(7) 0.46939(3) 0.25193(6) 0.0479(2) Uani 1 1 d . . . Cl41 Cl 0.30135(13) 0.46313(7) 0.22630(12) 0.0656(4) Uani 1 1 d . . . Cl42 Cl 0.09043(14) 0.54957(6) 0.22828(15) 0.0715(5) Uani 1 1 d . . . Cl43 Cl 0.01379(15) 0.42118(6) 0.15910(12) 0.0662(4) Uani 1 1 d . . . Cl44 Cl 0.17072(17) 0.45076(6) 0.39538(12) 0.0680(4) Uani 1 1 d . . . Fe5 Fe 0.62154(8) 0.49314(3) 0.22989(6) 0.0554(2) Uani 1 1 d . . . Cl51 Cl 0.58352(14) 0.41168(5) 0.23967(12) 0.0603(4) Uani 1 1 d . . . Cl52 Cl 0.63647(15) 0.53083(6) 0.35921(12) 0.0635(4) Uani 1 1 d . . . Cl53 Cl 0.78276(18) 0.49690(7) 0.20747(17) 0.0872(6) Uani 1 1 d . . . Cl54 Cl 0.49139(18) 0.52927(7) 0.11654(12) 0.0741(5) Uani 1 1 d . . . Fe6 Fe 0.57189(13) 0.7500 0.26671(11) 0.0661(4) Uani 1 2 d S . . Cl61 Cl 0.65799(18) 0.67913(6) 0.31861(16) 0.0813(6) Uani 1 1 d . . . Cl62 Cl 0.4117(2) 0.7500 0.2940(3) 0.0862(8) Uani 1 2 d S . . Cl63 Cl 0.5429(4) 0.7500 0.1197(2) 0.1152(13) Uani 1 2 d S . . Fe7 Fe 0.81470(11) 0.7500 0.59751(14) 0.0771(5) Uani 1 2 d SD . . Cl71 Cl 0.85676(16) 0.68191(7) 0.6823(2) 0.1038(8) Uani 1 1 d D A . Cl72 Cl 0.63590(17) 0.7500 0.52439(15) 0.0532(5) Uani 1 2 d SD A . Cl73 Cl 0.9347(6) 0.7500 0.5375(8) 0.107(3) Uani 0.50 2 d SPD A 1 Cl74 Cl 0.8970(6) 0.7500 0.4855(4) 0.0707(18) Uani 0.50 2 d SPD A 2 Fe8 Fe 0.95145(17) 0.26280(9) 0.76222(17) 0.0847(10) Uani 0.50 1 d PDU B -3 Cl81 Cl 0.8693(8) 0.1905(3) 0.7284(12) 0.288(9) Uani 0.50 1 d PDU B -3 Cl82 Cl 0.8650(6) 0.32056(19) 0.6728(4) 0.103(2) Uani 0.50 1 d PDU B -3 Cl83 Cl 1.1230(3) 0.2569(7) 0.7704(4) 0.121(4) Uani 0.50 1 d PDU B -3 Cl84 Cl 0.9449(9) 0.2893(5) 0.8933(5) 0.285(8) Uani 0.50 1 d PDU B -3 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 0.0443(5) 0.0392(5) 0.0361(6) 0.000 0.0196(5) 0.000 Fe2 0.0393(5) 0.0375(5) 0.0417(6) 0.000 0.0210(5) 0.000 Fe3 0.0537(6) 0.0474(6) 0.0477(6) 0.000 0.0323(5) 0.000 O1 0.050(3) 0.033(2) 0.047(3) 0.000 0.024(2) 0.000 O2 0.047(2) 0.0431(18) 0.046(2) 0.0000(16) 0.0217(18) 0.0020(15) O3 0.0421(19) 0.0425(18) 0.043(2) -0.0024(15) 0.0198(16) 0.0006(15) C1 0.043(3) 0.032(2) 0.045(3) -0.002(2) 0.025(2) -0.001(2) C2 0.050(3) 0.039(3) 0.047(3) -0.001(2) 0.024(3) 0.005(2) N1 0.053(2) 0.034(2) 0.048(3) -0.0060(18) 0.027(2) -0.0056(18) C3 0.056(3) 0.046(3) 0.048(3) -0.002(2) 0.022(3) -0.014(2) N2 0.059(3) 0.043(2) 0.051(3) -0.009(2) 0.029(2) -0.006(2) C4 0.120(6) 0.083(5) 0.069(5) -0.019(4) 0.047(5) -0.062(5) C5 0.129(7) 0.067(4) 0.060(4) -0.011(3) 0.045(5) -0.052(4) C6 0.077(4) 0.061(4) 0.047(4) -0.011(3) 0.021(3) -0.018(3) O4 0.0436(19) 0.0449(19) 0.056(2) -0.0045(17) 0.0253(18) -0.0031(15) O5 0.060(2) 0.066(2) 0.058(3) -0.011(2) 0.036(2) -0.0113(19) C7 0.046(3) 0.045(3) 0.073(4) 0.001(3) 0.035(3) 0.001(2) C8 0.072(4) 0.051(3) 0.086(5) -0.007(3) 0.053(4) -0.015(3) N3 0.047(3) 0.039(2) 0.078(4) -0.008(2) 0.033(3) -0.006(2) C9 0.063(4) 0.057(4) 0.098(6) -0.023(4) 0.041(4) 0.007(3) N4 0.047(3) 0.064(3) 0.090(4) -0.019(3) 0.023(3) -0.003(2) C10 0.144(9) 0.103(7) 0.095(7) -0.023(5) 0.034(7) 0.066(7) C11 0.149(9) 0.160(10) 0.083(7) -0.018(6) 0.022(6) 0.110(8) C12 0.059(5) 0.166(11) 0.116(8) -0.031(8) 0.001(5) 0.006(6) O6 0.065(3) 0.060(2) 0.055(2) 0.0090(19) 0.037(2) 0.0037(19) O7 0.055(2) 0.050(2) 0.046(2) 0.0077(17) 0.0211(18) 0.0014(17) C13 0.064(4) 0.047(3) 0.048(3) 0.003(2) 0.026(3) 0.000(3) C14 0.068(4) 0.064(4) 0.061(4) 0.017(3) 0.036(3) 0.010(3) N5 0.068(3) 0.058(3) 0.057(3) 0.015(2) 0.025(3) 0.004(3) C15 0.069(4) 0.082(5) 0.045(4) 0.018(3) 0.021(3) 0.007(3) N6 0.073(4) 0.091(4) 0.058(3) 0.026(3) 0.027(3) 0.023(3) C16 0.080(5) 0.091(6) 0.081(6) 0.015(5) 0.005(4) 0.002(5) C17 0.090(6) 0.072(5) 0.077(5) 0.007(4) 0.011(5) 0.014(4) C18 0.089(5) 0.135(8) 0.061(5) 0.025(5) 0.033(4) 0.047(5) O8 0.051(3) 0.062(3) 0.054(4) 0.000 0.019(3) 0.000 O9 0.053(3) 0.071(4) 0.050(3) 0.000 0.016(3) 0.000 O10 0.075(4) 0.073(4) 0.065(4) 0.000 0.051(3) 0.000 Fe4 0.0516(4) 0.0426(4) 0.0526(5) 0.0063(3) 0.0215(4) -0.0001(3) Cl41 0.0567(8) 0.0817(11) 0.0642(10) 0.0156(8) 0.0277(8) 0.0148(7) Cl42 0.0615(9) 0.0460(8) 0.1033(14) 0.0121(8) 0.0222(9) 0.0062(7) Cl43 0.0704(10) 0.0615(9) 0.0639(10) 0.0040(7) 0.0185(8) -0.0114(7) Cl44 0.1004(13) 0.0569(8) 0.0556(9) -0.0001(7) 0.0376(9) -0.0068(8) Fe5 0.0732(6) 0.0439(4) 0.0654(6) 0.0066(4) 0.0446(5) -0.0005(4) Cl51 0.0716(9) 0.0443(7) 0.0800(11) 0.0038(7) 0.0454(9) -0.0006(6) Cl52 0.0833(11) 0.0517(8) 0.0635(10) 0.0032(7) 0.0349(9) 0.0028(7) Cl53 0.0931(13) 0.0697(11) 0.1309(18) 0.0122(11) 0.0804(14) -0.0023(9) Cl54 0.1029(13) 0.0639(9) 0.0623(10) 0.0191(8) 0.0365(10) -0.0027(9) Fe6 0.0908(10) 0.0483(7) 0.0747(9) 0.000 0.0484(8) 0.000 Cl61 0.0980(13) 0.0519(9) 0.1209(17) 0.0080(9) 0.0726(13) 0.0101(8) Cl62 0.0735(16) 0.0655(15) 0.130(3) 0.000 0.0479(17) 0.000 Cl63 0.181(4) 0.100(2) 0.073(2) 0.000 0.054(2) 0.000 Fe7 0.0475(7) 0.0389(6) 0.1488(16) 0.000 0.0375(9) 0.000 Cl71 0.0592(10) 0.0605(10) 0.170(2) 0.0207(12) 0.0083(13) 0.0078(8) Cl72 0.0561(11) 0.0475(10) 0.0642(13) 0.000 0.0309(10) 0.000 Cl73 0.048(4) 0.065(3) 0.219(11) 0.000 0.061(6) 0.000 Cl74 0.057(4) 0.095(4) 0.072(4) 0.000 0.037(3) 0.000 Fe8 0.0589(10) 0.089(3) 0.0999(15) 0.0284(13) 0.0175(10) -0.0051(10) Cl81 0.106(6) 0.066(4) 0.70(3) 0.028(8) 0.139(12) -0.006(3) Cl82 0.079(3) 0.048(2) 0.143(4) -0.043(2) -0.014(3) 0.004(2) Cl83 0.0666(18) 0.119(10) 0.170(4) 0.028(7) 0.029(2) -0.009(4) Cl84 0.209(9) 0.56(3) 0.110(5) 0.012(8) 0.094(6) -0.032(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.927(5) . ? Fe1 O2 2.013(4) . ? Fe1 O2 2.013(4) 4_565 ? Fe1 O7 2.027(4) . ? Fe1 O7 2.027(4) 4_565 ? Fe1 O8 2.047(6) . ? Fe2 O1 1.891(5) . ? Fe2 O3 2.025(3) . ? Fe2 O3 2.025(3) 4_565 ? Fe2 O4 2.029(4) . ? Fe2 O4 2.029(4) 4_565 ? Fe2 O9 2.082(6) . ? Fe3 O1 1.919(5) . ? Fe3 O6 1.998(4) 4_565 ? Fe3 O6 1.998(4) . ? Fe3 O5 2.010(4) . ? Fe3 O5 2.010(4) 4_565 ? Fe3 O10 2.066(5) . ? O2 C1 1.246(6) . ? O3 C1 1.257(6) . ? C1 C2 1.522(6) . ? C2 N1 1.446(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 C3 1.315(7) . ? N1 C5 1.363(7) . ? C3 N2 1.309(7) . ? C3 H3A 0.9500 . ? N2 C4 1.370(8) . ? N2 C6 1.471(8) . ? C4 C5 1.339(11) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O4 C7 1.268(7) . ? O5 C7 1.242(7) . ? C7 C8 1.509(8) . ? C8 N3 1.451(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N3 C9 1.279(9) . ? N3 C11 1.325(9) . ? C9 N4 1.321(9) . ? C9 H9A 0.9500 . ? N4 C10 1.324(10) . ? N4 C12 1.482(12) . ? C10 C11 1.327(13) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O6 C13 1.256(7) . ? O7 C13 1.257(7) . ? C13 C14 1.505(8) . ? C14 N5 1.458(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? N5 C15 1.318(9) . ? N5 C17 1.373(10) . ? C15 N6 1.316(9) . ? C15 H15A 0.9500 . ? N6 C16 1.391(11) . ? N6 C18 1.463(10) . ? C16 C17 1.326(12) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Fe4 Cl43 2.1839(19) . ? Fe4 Cl44 2.1917(18) . ? Fe4 Cl41 2.1936(17) . ? Fe4 Cl42 2.1955(17) . ? Fe5 Cl53 2.1865(19) . ? Fe5 Cl52 2.1910(19) . ? Fe5 Cl54 2.193(2) . ? Fe5 Cl51 2.2056(16) . ? Fe6 Cl61 2.171(2) . ? Fe6 Cl61 2.171(2) 4_575 ? Fe6 Cl63 2.191(4) . ? Fe6 Cl62 2.207(3) . ? Fe7 Cl73 2.030(8) . ? Fe7 Cl72 2.176(3) . ? Fe7 Cl71 2.178(2) 4_575 ? Fe7 Cl71 2.178(2) . ? Fe7 Cl74 2.305(6) . ? Fe8 Cl82 2.103(6) . ? Fe8 Cl83 2.142(5) . ? Fe8 Cl81 2.144(8) . ? Fe8 Cl84 2.179(8) . ? 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 O2 94.59(15) . . ? O1 Fe1 O2 94.58(15) . 4_565 ? O2 Fe1 O2 91.2(2) . 4_565 ? O1 Fe1 O7 94.98(15) . . ? O2 Fe1 O7 88.21(15) . . ? O2 Fe1 O7 170.43(16) 4_565 . ? O1 Fe1 O7 94.98(15) . 4_565 ? O2 Fe1 O7 170.43(16) . 4_565 ? O2 Fe1 O7 88.21(15) 4_565 4_565 ? O7 Fe1 O7 90.7(2) . 4_565 ? O1 Fe1 O8 179.6(2) . . ? O2 Fe1 O8 85.68(16) . . ? O2 Fe1 O8 85.68(16) 4_565 . ? O7 Fe1 O8 84.75(16) . . ? O7 Fe1 O8 84.75(16) 4_565 . ? O1 Fe2 O3 96.60(15) . . ? O1 Fe2 O3 96.60(15) . 4_565 ? O3 Fe2 O3 90.95(19) . 4_565 ? O1 Fe2 O4 95.94(15) . . ? O3 Fe2 O4 86.64(14) . . ? O3 Fe2 O4 167.42(16) 4_565 . ? O1 Fe2 O4 95.94(15) . 4_565 ? O3 Fe2 O4 167.42(16) . 4_565 ? O3 Fe2 O4 86.63(14) 4_565 4_565 ? O4 Fe2 O4 93.0(2) . 4_565 ? O1 Fe2 O9 179.9(2) . . ? O3 Fe2 O9 83.33(15) . . ? O3 Fe2 O9 83.33(15) 4_565 . ? O4 Fe2 O9 84.13(16) . . ? O4 Fe2 O9 84.13(16) 4_565 . ? O1 Fe3 O6 94.50(15) . 4_565 ? O1 Fe3 O6 94.50(15) . . ? O6 Fe3 O6 93.4(3) 4_565 . ? O1 Fe3 O5 95.12(16) . . ? O6 Fe3 O5 170.32(15) 4_565 . ? O6 Fe3 O5 86.89(19) . . ? O1 Fe3 O5 95.12(16) . 4_565 ? O6 Fe3 O5 86.89(19) 4_565 4_565 ? O6 Fe3 O5 170.32(15) . 4_565 ? O5 Fe3 O5 91.2(3) . 4_565 ? O1 Fe3 O10 178.6(3) . . ? O6 Fe3 O10 84.53(17) 4_565 . ? O6 Fe3 O10 84.52(17) . . ? O5 Fe3 O10 85.87(18) . . ? O5 Fe3 O10 85.88(18) 4_565 . ? Fe2 O1 Fe3 119.8(3) . . ? Fe2 O1 Fe1 119.8(2) . . ? Fe3 O1 Fe1 120.4(3) . . ? C1 O2 Fe1 133.2(3) . . ? C1 O3 Fe2 130.2(3) . . ? O2 C1 O3 127.1(4) . . ? O2 C1 C2 114.6(4) . . ? O3 C1 C2 118.3(5) . . ? N1 C2 C1 114.3(4) . . ? N1 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C3 N1 C5 107.3(5) . . ? C3 N1 C2 127.7(4) . . ? C5 N1 C2 125.0(5) . . ? N2 C3 N1 110.7(5) . . ? N2 C3 H3A 124.6 . . ? N1 C3 H3A 124.6 . . ? C3 N2 C4 106.9(5) . . ? C3 N2 C6 127.2(5) . . ? C4 N2 C6 125.7(5) . . ? C5 C4 N2 107.7(6) . . ? C5 C4 H4A 126.2 . . ? N2 C4 H4A 126.2 . . ? C4 C5 N1 107.2(6) . . ? C4 C5 H5A 126.4 . . ? N1 C5 H5A 126.4 . . ? 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 . . ? C7 O4 Fe2 130.3(4) . . ? C7 O5 Fe3 132.9(4) . . ? O5 C7 O4 126.4(5) . . ? O5 C7 C8 114.1(5) . . ? O4 C7 C8 119.4(6) . . ? N3 C8 C7 113.9(5) . . ? N3 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? N3 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C9 N3 C11 105.7(7) . . ? C9 N3 C8 125.4(5) . . ? C11 N3 C8 128.7(7) . . ? N3 C9 N4 111.7(6) . . ? N3 C9 H9A 124.2 . . ? N4 C9 H9A 124.2 . . ? C9 N4 C10 106.3(7) . . ? C9 N4 C12 127.9(7) . . ? C10 N4 C12 125.9(8) . . ? N4 C10 C11 106.7(7) . . ? N4 C10 H10A 126.6 . . ? C11 C10 H10A 126.6 . . ? N3 C11 C10 109.5(8) . . ? N3 C11 H11A 125.2 . . ? C10 C11 H11A 125.2 . . ? 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 . . ? C13 O6 Fe3 133.0(4) . . ? C13 O7 Fe1 131.4(4) . . ? O6 C13 O7 127.0(5) . . ? O6 C13 C14 114.0(5) . . ? O7 C13 C14 119.0(5) . . ? N5 C14 C13 113.1(5) . . ? N5 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? N5 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C15 N5 C17 108.8(6) . . ? C15 N5 C14 124.9(6) . . ? C17 N5 C14 126.3(6) . . ? N6 C15 N5 109.4(7) . . ? N6 C15 H15A 125.3 . . ? N5 C15 H15A 125.3 . . ? C15 N6 C16 107.2(7) . . ? C15 N6 C18 126.2(8) . . ? C16 N6 C18 126.5(7) . . ? C17 C16 N6 107.9(8) . . ? C17 C16 H16A 126.0 . . ? N6 C16 H16A 126.0 . . ? C16 C17 N5 106.7(8) . . ? C16 C17 H17A 126.7 . . ? N5 C17 H17A 126.7 . . ? 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 . . ? Cl43 Fe4 Cl44 112.45(7) . . ? Cl43 Fe4 Cl41 111.47(8) . . ? Cl44 Fe4 Cl41 108.23(8) . . ? Cl43 Fe4 Cl42 109.18(8) . . ? Cl44 Fe4 Cl42 108.94(8) . . ? Cl41 Fe4 Cl42 106.36(7) . . ? Cl53 Fe5 Cl52 108.85(9) . . ? Cl53 Fe5 Cl54 110.38(9) . . ? Cl52 Fe5 Cl54 110.90(8) . . ? Cl53 Fe5 Cl51 106.97(7) . . ? Cl52 Fe5 Cl51 109.16(7) . . ? Cl54 Fe5 Cl51 110.48(8) . . ? Cl61 Fe6 Cl61 117.68(15) . 4_575 ? Cl61 Fe6 Cl63 106.16(9) . . ? Cl61 Fe6 Cl63 106.16(9) 4_575 . ? Cl61 Fe6 Cl62 108.09(7) . . ? Cl61 Fe6 Cl62 108.09(7) 4_575 . ? Cl63 Fe6 Cl62 110.58(18) . . ? Cl73 Fe7 Cl72 124.8(3) . . ? Cl73 Fe7 Cl71 101.92(19) . 4_575 ? Cl72 Fe7 Cl71 108.74(7) . 4_575 ? Cl73 Fe7 Cl71 101.92(19) . . ? Cl72 Fe7 Cl71 108.74(7) . . ? Cl71 Fe7 Cl71 110.08(17) 4_575 . ? Cl72 Fe7 Cl74 105.0(2) . . ? Cl71 Fe7 Cl74 112.03(12) 4_575 . ? Cl71 Fe7 Cl74 112.03(12) . . ? Cl82 Fe8 Cl83 112.9(4) . . ? Cl82 Fe8 Cl81 111.7(3) . . ? Cl83 Fe8 Cl81 110.6(5) . . ? Cl82 Fe8 Cl84 102.5(4) . . ? Cl83 Fe8 Cl84 108.6(3) . . ? Cl81 Fe8 Cl84 110.3(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.013 _refine_diff_density_min -1.880 _refine_diff_density_rms 0.119 data_6feclmeth5 _database_code_depnum_ccdc_archive 'CCDC 896159' #TrackingRef 'Fe3_IL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H60 Fe3 N12 O16, 7(Cl4 Fe), H2 O, 2(C H4 O)' _chemical_formula_sum 'C41 H70 Cl28 Fe10 N12 O19' _chemical_formula_weight 2586.19 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' 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' _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 12.7495(4) _cell_length_b 15.5320(5) _cell_length_c 26.1211(7) _cell_angle_alpha 90.846(2) _cell_angle_beta 91.244(2) _cell_angle_gamma 108.346(2) _cell_volume 4907.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 95831 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 26.34 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 2.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_T_max 0.610 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61617 _diffrn_reflns_av_R_equivalents 0.1154 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.43 _reflns_number_total 17953 _reflns_number_gt 14338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The crystal structure is closely related to the monoclinic P21/m structure of the previous complex (fe37s), and is derived from it by a slight change of the angles alpha and gamma from 90 degrees, followed by the necessary axis permutation to give the conventional triclinic cell. The unit cell contents of the present structure also approximate to that of fe37s, and the resulting pseudo-symmetry hampered refinement. Not unexpectedly, this pseudo-symmetry also resulted in pseudo-merohedral twinning by 180 degree rotation about the triclinic c-axis (corresponds to monoclinic b in fe37s). This was not noticeable during data collection (ca. 14% for the minor domain), so that a datafile in HKLF 5 format was created using the TWINROTMAT option within PLATON (Spek, A.L. (2003), J.Appl. Cryst. 36, 7-13). Refinement was then relatively straightforward. One of the (FeCl4)- anions was disordered: the Fe of the minor component refined to a site occupancy of 0.16. The chlorines of this minor component were then further disordered, and could not be refined satisfactorily. One MeOH ligand, and the lattice water to which it hydrogen bonds, were twofold disordered either side of the pseudo-mirror plane. ; _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^)+(0.1381P)^2^+2.2130P] 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 17953 _refine_ls_number_parameters 980 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2169 _refine_ls_wR_factor_gt 0.2023 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.44097(5) 0.19547(5) 0.25078(3) 0.04876(18) Uani 1 1 d . B . Fe2 Fe 0.66888(5) 0.37134(5) 0.25606(3) 0.04776(18) Uani 1 1 d . . . Fe3 Fe 0.68795(6) 0.16493(5) 0.25558(3) 0.05139(19) Uani 1 1 d . . . O1 O 0.5997(3) 0.2450(2) 0.25431(13) 0.0497(7) Uani 1 1 d . . . O2 O 0.4174(3) 0.2779(2) 0.30660(14) 0.0549(8) Uani 1 1 d . . . O3 O 0.5710(3) 0.3975(2) 0.30991(13) 0.0531(8) Uani 1 1 d . . . C1 C 0.4778(4) 0.3528(3) 0.32446(19) 0.0505(11) Uani 1 1 d . . . C2 C 0.4276(5) 0.3910(4) 0.3679(2) 0.0572(12) Uani 1 1 d . . . H2A H 0.3592 0.3992 0.3555 0.069 Uiso 1 1 calc R . . H2B H 0.4095 0.3471 0.3950 0.069 Uiso 1 1 calc R . . N1 N 0.4984(4) 0.4761(3) 0.38905(16) 0.0554(10) Uani 1 1 d . . . C3 C 0.5067(5) 0.5583(4) 0.3725(2) 0.0595(13) Uani 1 1 d . . . H3A H 0.4651 0.5710 0.3457 0.071 Uiso 1 1 calc R . . N2 N 0.5838(4) 0.6193(3) 0.40025(18) 0.0625(11) Uani 1 1 d . . . C4 C 0.6265(7) 0.5749(5) 0.4359(3) 0.087(2) Uani 1 1 d . . . H4A H 0.6821 0.6012 0.4603 0.104 Uiso 1 1 calc R . . C5 C 0.5728(7) 0.4859(5) 0.4289(3) 0.085(2) Uani 1 1 d . . . H5A H 0.5843 0.4392 0.4478 0.102 Uiso 1 1 calc R . . C6 C 0.6166(6) 0.7177(4) 0.3941(3) 0.0740(16) Uani 1 1 d . . . H6A H 0.5756 0.7313 0.3658 0.111 Uiso 1 1 calc R . . H6B H 0.6942 0.7404 0.3876 0.111 Uiso 1 1 calc R . . H6C H 0.6016 0.7458 0.4248 0.111 Uiso 1 1 calc R . . O4 O 0.4232(3) 0.2801(2) 0.19618(14) 0.0561(8) Uani 1 1 d . . . O5 O 0.5761(3) 0.4021(2) 0.19963(13) 0.0531(8) Uani 1 1 d . . . C7 C 0.4830(4) 0.3559(3) 0.18182(18) 0.0491(11) Uani 1 1 d . . . C8 C 0.4307(4) 0.3925(4) 0.1376(2) 0.0549(11) Uani 1 1 d . . . H8A H 0.4099 0.3468 0.1102 0.066 Uiso 1 1 calc R . . H8B H 0.3638 0.4026 0.1492 0.066 Uiso 1 1 calc R . . N3 N 0.5026(4) 0.4766(3) 0.11705(16) 0.0540(10) Uani 1 1 d . . . C9 C 0.5221(5) 0.5599(4) 0.1365(2) 0.0617(13) Uani 1 1 d . . . H9A H 0.4928 0.5745 0.1665 0.074 Uiso 1 1 calc R . . N4 N 0.5895(4) 0.6186(3) 0.10655(18) 0.0623(11) Uani 1 1 d . . . C10 C 0.6104(6) 0.5704(5) 0.0654(3) 0.0768(17) Uani 1 1 d . . . H10A H 0.6536 0.5949 0.0377 0.092 Uiso 1 1 calc R . . C11 C 0.5584(6) 0.4832(5) 0.0723(2) 0.0719(16) Uani 1 1 d . . . H11A H 0.5595 0.4354 0.0507 0.086 Uiso 1 1 calc R . . C12 C 0.6266(6) 0.7165(4) 0.1128(3) 0.0775(17) Uani 1 1 d . . . H12A H 0.5977 0.7332 0.1437 0.116 Uiso 1 1 calc R . . H12B H 0.6007 0.7427 0.0840 0.116 Uiso 1 1 calc R . . H12C H 0.7059 0.7384 0.1147 0.116 Uiso 1 1 calc R . . O6 O 0.7800(3) 0.3717(2) 0.31291(14) 0.0561(8) Uani 1 1 d . . . O7 O 0.7866(3) 0.2285(3) 0.31478(16) 0.0650(10) Uani 1 1 d . . . C13 C 0.8119(4) 0.3092(4) 0.3316(2) 0.0542(11) Uani 1 1 d . . . C14 C 0.8863(5) 0.3296(4) 0.3785(2) 0.0586(12) Uani 1 1 d . . . H14A H 0.8467 0.2952 0.4067 0.070 Uiso 1 1 calc R . . H14B H 0.9497 0.3095 0.3723 0.070 Uiso 1 1 calc R . . N5 N 0.9249(4) 0.4249(3) 0.39328(16) 0.0573(10) Uani 1 1 d . . . C15 C 0.9974(5) 0.4881(4) 0.3695(2) 0.0655(14) Uani 1 1 d . . . H15A H 1.0333 0.4790 0.3403 0.079 Uiso 1 1 calc R . . N6 N 1.0128(4) 0.5675(4) 0.39277(19) 0.0664(12) Uani 1 1 d . . . C16 C 0.9480(7) 0.5526(6) 0.4331(3) 0.087(2) Uani 1 1 d . . . H16A H 0.9418 0.5966 0.4563 0.105 Uiso 1 1 calc R . . C17 C 0.8935(7) 0.4640(5) 0.4348(3) 0.0838(19) Uani 1 1 d . . . H17A H 0.8439 0.4347 0.4594 0.101 Uiso 1 1 calc R . . C18 C 1.0891(7) 0.6560(6) 0.3753(4) 0.101(2) Uani 1 1 d . . . H18A H 1.1240 0.6460 0.3446 0.152 Uiso 1 1 calc R . . H18B H 1.1444 0.6818 0.4015 0.152 Uiso 1 1 calc R . . H18C H 1.0477 0.6968 0.3685 0.152 Uiso 1 1 calc R . . O8 O 0.7783(3) 0.3731(2) 0.20098(14) 0.0558(8) Uani 1 1 d . . . O9 O 0.7970(3) 0.2353(3) 0.20536(16) 0.0644(10) Uani 1 1 d . . . C19 C 0.8122(4) 0.3109(4) 0.1851(2) 0.0576(12) Uani 1 1 d . . . C20 C 0.8766(5) 0.3215(4) 0.1371(2) 0.0636(13) Uani 1 1 d . . . H20A H 0.9432 0.3057 0.1439 0.076 Uiso 1 1 calc R . . H20B H 0.8329 0.2791 0.1112 0.076 Uiso 1 1 calc R . . N7 N 0.9074(4) 0.4125(4) 0.11675(17) 0.0608(11) Uani 1 1 d . . . C21 C 1.0042(5) 0.4738(5) 0.1213(2) 0.0735(17) Uani 1 1 d . . . H21A H 1.0655 0.4653 0.1378 0.088 Uiso 1 1 calc R . . N8 N 1.0033(4) 0.5491(4) 0.0995(2) 0.0725(13) Uani 1 1 d . . . C22 C 0.8982(7) 0.5350(6) 0.0806(4) 0.107(3) Uani 1 1 d . . . H22A H 0.8735 0.5765 0.0626 0.128 Uiso 1 1 calc R . . C23 C 0.8371(7) 0.4507(6) 0.0925(4) 0.106(3) Uani 1 1 d . . . H23A H 0.7619 0.4236 0.0857 0.128 Uiso 1 1 calc R . . C24 C 1.0969(7) 0.6338(7) 0.0973(5) 0.117(3) Uani 1 1 d . . . H24A H 1.1608 0.6257 0.1141 0.175 Uiso 1 1 calc R . . H24B H 1.0781 0.6820 0.1142 0.175 Uiso 1 1 calc R . . H24C H 1.1128 0.6488 0.0621 0.175 Uiso 1 1 calc R . . O10 O 0.5986(3) 0.0838(3) 0.30786(15) 0.0629(9) Uani 1 1 d . . . O11 O 0.4307(3) 0.1019(2) 0.30524(14) 0.0578(8) Uani 1 1 d . . . C25 C 0.5014(4) 0.0680(3) 0.3229(2) 0.0551(11) Uani 1 1 d . . . C26 C 0.4715(5) 0.0019(4) 0.3655(2) 0.0646(14) Uani 1 1 d . . . H26A H 0.4860 -0.0534 0.3550 0.077 Uiso 1 1 calc R . . H26B H 0.5192 0.0272 0.3951 0.077 Uiso 1 1 calc R . . N9 N 0.3573(4) -0.0210(3) 0.3807(2) 0.0634(11) Uani 1 1 d . . . C27 C 0.3230(5) 0.0087(4) 0.4224(3) 0.0657(14) Uani 1 1 d . . . H27A H 0.3680 0.0486 0.4467 0.079 Uiso 1 1 calc R . . N10 N 0.2139(4) -0.0274(4) 0.4244(2) 0.0742(14) Uani 1 1 d . . . C28 C 0.1787(6) -0.0818(5) 0.3815(4) 0.090(2) Uani 1 1 d . . . H28A H 0.1059 -0.1155 0.3732 0.108 Uiso 1 1 calc R . . C29 C 0.2672(6) -0.0783(5) 0.3533(3) 0.0824(18) Uani 1 1 d . . . H29A H 0.2677 -0.1079 0.3222 0.099 Uiso 1 1 calc R . . C30 C 0.1470(8) -0.0151(6) 0.4664(4) 0.109(3) Uani 1 1 d . . . H30A H 0.0706 -0.0471 0.4586 0.163 Uiso 1 1 calc R . . H30B H 0.1566 0.0484 0.4713 0.163 Uiso 1 1 calc R . . H30C H 0.1696 -0.0383 0.4971 0.163 Uiso 1 1 calc R . . O12 O 0.6061(3) 0.0897(3) 0.19597(15) 0.0632(9) Uani 1 1 d . . . O13 O 0.4350(3) 0.1027(2) 0.19484(15) 0.0582(8) Uani 1 1 d . . . C31 C 0.5092(5) 0.0728(3) 0.1785(2) 0.0557(12) Uani 1 1 d . . . C32 C 0.4844(5) 0.0099(4) 0.1315(2) 0.0652(14) Uani 1 1 d . . . H32A H 0.5291 0.0408 0.1036 0.078 Uiso 1 1 calc R . . H32B H 0.5057 -0.0433 0.1391 0.078 Uiso 1 1 calc R . . N11 N 0.3690(4) -0.0189(3) 0.11487(18) 0.0613(11) Uani 1 1 d . . . C33 C 0.3273(5) 0.0158(4) 0.0762(2) 0.0665(14) Uani 1 1 d . . . H33A H 0.3666 0.0634 0.0560 0.080 Uiso 1 1 calc R . . N12 N 0.2203(5) -0.0290(4) 0.0714(2) 0.0719(13) Uani 1 1 d . . . C34 C 0.1930(7) -0.0919(6) 0.1087(3) 0.088(2) Uani 1 1 d . . . H34A H 0.1227 -0.1314 0.1145 0.106 Uiso 1 1 calc R . . C35 C 0.2859(6) -0.0866(5) 0.1358(3) 0.0788(17) Uani 1 1 d . . . H35A H 0.2923 -0.1221 0.1634 0.095 Uiso 1 1 calc R . . C36 C 0.1435(7) -0.0144(5) 0.0318(4) 0.097(3) Uani 1 1 d . . . H36A H 0.1825 0.0344 0.0104 0.146 Uiso 1 1 calc R . . H36B H 0.0844 0.0006 0.0480 0.146 Uiso 1 1 calc R . . H36C H 0.1135 -0.0688 0.0113 0.146 Uiso 1 1 calc R . . O14 O 0.2730(3) 0.1433(3) 0.24708(16) 0.0651(9) Uani 1 1 d . . . H141 H 0.2400 0.1312 0.2145 0.078 Uiso 0.59 1 calc PR A 1 H142 H 0.2340 0.1357 0.2772 0.078 Uiso 0.41 1 d PR A 2 C37A C 0.1984(12) 0.1226(10) 0.2908(5) 0.092(3) Uiso 0.59 1 d P B 1 H37A H 0.1231 0.0997 0.2784 0.139 Uiso 0.59 1 calc PR B 1 H37B H 0.2084 0.1769 0.3111 0.139 Uiso 0.59 1 calc PR B 1 H37C H 0.2150 0.0778 0.3116 0.139 Uiso 0.59 1 calc PR B 1 C37B C 0.202(3) 0.116(2) 0.1984(11) 0.129(8) Uiso 0.41 1 d P B 2 H37D H 0.1257 0.0947 0.2070 0.193 Uiso 0.41 1 calc PR B 2 H37E H 0.2215 0.0694 0.1805 0.193 Uiso 0.41 1 calc PR B 2 H37F H 0.2149 0.1682 0.1770 0.193 Uiso 0.41 1 calc PR B 2 O15 O 0.7459(3) 0.5108(3) 0.26094(16) 0.0656(9) Uani 1 1 d . . . H151 H 0.7669 0.5398 0.2301 0.079 Uiso 1 1 calc R . . C38 C 0.7707(8) 0.5680(6) 0.3066(4) 0.101(2) Uani 1 1 d . . . H38A H 0.8067 0.6297 0.2974 0.152 Uiso 1 1 calc R . . H38B H 0.8186 0.5483 0.3292 0.152 Uiso 1 1 calc R . . H38C H 0.7034 0.5640 0.3236 0.152 Uiso 1 1 calc R . . O16 O 0.7781(3) 0.0760(3) 0.25591(16) 0.0703(10) Uani 1 1 d . . . H161 H 0.7408 0.0139 0.2550 0.084 Uiso 1 1 calc R . . C39 C 0.9015(3) 0.1080(3) 0.25749(16) 0.198(8) Uani 1 1 d R . . H39A H 0.9281 0.0567 0.2573 0.297 Uiso 1 1 calc R . . H39B H 0.9279 0.1440 0.2881 0.297 Uiso 1 1 calc R . . H39C H 0.9279 0.1441 0.2281 0.297 Uiso 1 1 calc R . . Fe4 Fe 0.14039(6) 0.24661(6) 0.46866(3) 0.0590(2) Uani 1 1 d . . . Cl41 Cl 0.30069(13) 0.22419(11) 0.46160(7) 0.0745(4) Uani 1 1 d . . . Cl42 Cl 0.16164(14) 0.38945(10) 0.45354(6) 0.0720(4) Uani 1 1 d . . . Cl43 Cl 0.09331(14) 0.22071(14) 0.54884(6) 0.0816(4) Uani 1 1 d . . . Cl44 Cl 0.01540(15) 0.15521(12) 0.41782(8) 0.0840(5) Uani 1 1 d . . . Fe5 Fe 0.14409(7) 0.25634(6) 0.02805(3) 0.0614(2) Uani 1 1 d . . . Cl51 Cl 0.30387(13) 0.23140(13) 0.03455(7) 0.0801(4) Uani 1 1 d . . . Cl52 Cl 0.08760(14) 0.22777(15) -0.05215(6) 0.0828(4) Uani 1 1 d . . . Cl53 Cl 0.02329(14) 0.16784(12) 0.07777(6) 0.0768(4) Uani 1 1 d . . . Cl54 Cl 0.1769(2) 0.40062(13) 0.04560(8) 0.0995(6) Uani 1 1 d . . . Fe6 Fe 0.63158(7) 0.23601(6) 0.49602(3) 0.0619(2) Uani 1 1 d . . . Cl61 Cl 0.59012(13) 0.24470(12) 0.41456(6) 0.0713(4) Uani 1 1 d . . . Cl62 Cl 0.64576(16) 0.36536(11) 0.53458(6) 0.0783(4) Uani 1 1 d . . . Cl63 Cl 0.50495(15) 0.12225(11) 0.52996(7) 0.0786(4) Uani 1 1 d . . . Cl64 Cl 0.79434(16) 0.21652(16) 0.50182(7) 0.0922(6) Uani 1 1 d . . . Fe7 Fe 0.62203(7) 0.23320(6) 0.00839(3) 0.0627(2) Uani 1 1 d . . . Cl71 Cl 0.58209(12) 0.24555(11) 0.08950(5) 0.0664(3) Uani 1 1 d . . . Cl72 Cl 0.63084(14) 0.35912(12) -0.03030(6) 0.0738(4) Uani 1 1 d . . . Cl73 Cl 0.49510(17) 0.11813(13) -0.02863(7) 0.0874(5) Uani 1 1 d . . . Cl74 Cl 0.78328(16) 0.21205(16) 0.00804(7) 0.0915(6) Uani 1 1 d . . . Fe8 Fe 0.43351(7) 0.74314(6) 0.24980(3) 0.0649(2) Uani 1 1 d . . . Cl81 Cl 0.34663(15) 0.68433(13) 0.17874(6) 0.0802(4) Uani 1 1 d . . . Cl82 Cl 0.34787(16) 0.69874(14) 0.32062(6) 0.0835(5) Uani 1 1 d . . . Cl83 Cl 0.59051(16) 0.71235(18) 0.25438(7) 0.0955(6) Uani 1 1 d . . . Cl84 Cl 0.4617(2) 0.88923(13) 0.24627(9) 0.1088(7) Uani 1 1 d . . . Fe9 Fe 0.18657(7) 0.41349(7) 0.24965(3) 0.0664(2) Uani 1 1 d . . . Cl91 Cl 0.36490(12) 0.48309(10) 0.25344(5) 0.0645(3) Uani 1 1 d . . . Cl92 Cl 0.14845(14) 0.32330(14) 0.18209(7) 0.0833(5) Uani 1 1 d . . . Cl93 Cl 0.13941(15) 0.33539(15) 0.31875(7) 0.0879(5) Uani 1 1 d . . . Cl94 Cl 0.09162(18) 0.50904(17) 0.24406(7) 0.0997(6) Uani 1 1 d . . . Fe10 Fe 0.95794(11) 0.79239(10) 0.22870(5) 0.0802(3) Uani 0.84 1 d P C 1 Cl11 Cl 1.12477(19) 0.7830(2) 0.23867(11) 0.1030(7) Uani 0.84 1 d P C 1 Cl12 Cl 0.8559(2) 0.66879(17) 0.18779(8) 0.0951(7) Uani 0.84 1 d P C 1 Cl13 Cl 0.9003(2) 0.81014(19) 0.30659(9) 0.0940(6) Uani 0.84 1 d P C 1 Cl14 Cl 0.9548(3) 0.9057(2) 0.18172(13) 0.1204(9) Uani 0.84 1 d P C 1 Fe11 Fe 0.9519(6) 0.7574(6) 0.2471(3) 0.0802(3) Uani 0.16 1 d P D 2 O41A O 0.1611(11) 0.0959(10) 0.1610(5) 0.138(4) Uiso 0.65 1 d P E 1 O41B O 0.1542(18) 0.1069(16) 0.3253(8) 0.123(6) Uiso 0.35 1 d P F 2 O42 O 0.7314(11) -0.0617(7) 0.3218(4) 0.186(4) Uani 1 1 d DU . . C42 C 0.7677(15) -0.0288(14) 0.3774(6) 0.180(6) Uani 1 1 d DU . . O43 O 0.745(2) -0.043(2) 0.1709(10) 0.387(14) Uiso 1 1 d D . . C43 C 0.764(3) -0.005(2) 0.1157(11) 0.283(13) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0479(4) 0.0437(4) 0.0636(4) 0.0044(3) -0.0021(3) 0.0273(3) Fe2 0.0459(3) 0.0456(4) 0.0611(4) 0.0055(3) -0.0014(3) 0.0278(3) Fe3 0.0508(4) 0.0474(4) 0.0672(4) 0.0050(3) -0.0016(3) 0.0316(3) O1 0.0491(17) 0.0456(17) 0.0643(19) 0.0044(14) -0.0007(14) 0.0291(14) O2 0.0538(19) 0.049(2) 0.069(2) 0.0020(16) 0.0037(15) 0.0273(16) O3 0.0539(19) 0.0505(19) 0.065(2) 0.0042(15) 0.0031(15) 0.0308(16) C1 0.052(3) 0.053(3) 0.058(3) 0.008(2) -0.001(2) 0.033(2) C2 0.059(3) 0.058(3) 0.065(3) 0.004(2) 0.004(2) 0.034(2) N1 0.064(2) 0.056(2) 0.061(2) -0.0028(19) -0.0056(19) 0.039(2) C3 0.064(3) 0.060(3) 0.067(3) 0.003(2) -0.006(2) 0.037(3) N2 0.070(3) 0.060(3) 0.069(3) -0.006(2) -0.013(2) 0.038(2) C4 0.101(5) 0.072(4) 0.097(5) -0.014(3) -0.047(4) 0.046(4) C5 0.115(6) 0.069(4) 0.085(4) -0.003(3) -0.038(4) 0.051(4) C6 0.085(4) 0.055(3) 0.086(4) -0.007(3) -0.017(3) 0.031(3) O4 0.0528(18) 0.052(2) 0.072(2) 0.0090(16) -0.0066(16) 0.0290(16) O5 0.0528(19) 0.0507(19) 0.065(2) 0.0092(15) -0.0027(15) 0.0294(16) C7 0.049(3) 0.052(3) 0.057(3) 0.005(2) 0.000(2) 0.032(2) C8 0.052(3) 0.057(3) 0.065(3) 0.009(2) -0.005(2) 0.031(2) N3 0.058(2) 0.057(3) 0.062(2) 0.0095(19) 0.0026(18) 0.039(2) C9 0.066(3) 0.058(3) 0.070(3) 0.012(3) 0.009(3) 0.032(3) N4 0.066(3) 0.067(3) 0.068(3) 0.017(2) 0.006(2) 0.040(2) C10 0.084(4) 0.081(4) 0.079(4) 0.016(3) 0.019(3) 0.045(4) C11 0.093(4) 0.071(4) 0.069(3) 0.011(3) 0.014(3) 0.051(4) C12 0.082(4) 0.061(4) 0.093(4) 0.011(3) 0.004(3) 0.027(3) O6 0.0532(19) 0.055(2) 0.069(2) 0.0050(16) -0.0055(15) 0.0297(16) O7 0.063(2) 0.060(2) 0.084(2) -0.0001(19) -0.0135(18) 0.0383(19) C13 0.052(3) 0.058(3) 0.064(3) 0.004(2) -0.001(2) 0.033(2) C14 0.056(3) 0.059(3) 0.069(3) 0.001(2) -0.009(2) 0.032(2) N5 0.055(2) 0.071(3) 0.057(2) 0.002(2) -0.0039(18) 0.037(2) C15 0.062(3) 0.069(4) 0.073(3) -0.003(3) 0.006(3) 0.031(3) N6 0.064(3) 0.066(3) 0.075(3) -0.004(2) 0.000(2) 0.029(2) C16 0.100(5) 0.087(5) 0.080(4) -0.011(4) 0.015(4) 0.037(4) C17 0.102(5) 0.077(5) 0.077(4) -0.005(3) 0.027(4) 0.035(4) C18 0.078(5) 0.078(5) 0.142(7) -0.005(5) 0.016(5) 0.016(4) O8 0.0507(18) 0.054(2) 0.070(2) 0.0095(16) 0.0060(15) 0.0269(16) O9 0.060(2) 0.064(2) 0.085(2) 0.0139(19) 0.0117(18) 0.0408(18) C19 0.051(3) 0.063(3) 0.071(3) 0.003(2) -0.005(2) 0.035(2) C20 0.072(3) 0.063(3) 0.070(3) 0.006(3) 0.005(3) 0.041(3) N7 0.056(3) 0.075(3) 0.063(3) 0.010(2) 0.0026(19) 0.038(2) C21 0.058(3) 0.096(5) 0.077(4) 0.023(3) -0.002(3) 0.038(3) N8 0.054(3) 0.080(3) 0.088(3) 0.025(3) 0.005(2) 0.026(2) C22 0.092(5) 0.086(5) 0.133(7) 0.038(5) -0.045(5) 0.017(4) C23 0.083(5) 0.091(6) 0.148(7) 0.024(5) -0.046(5) 0.034(4) C24 0.074(5) 0.095(6) 0.178(9) 0.046(6) 0.008(5) 0.020(4) O10 0.065(2) 0.059(2) 0.079(2) 0.0129(18) 0.0022(18) 0.0387(18) O11 0.058(2) 0.0495(19) 0.076(2) 0.0110(16) 0.0011(16) 0.0307(16) C25 0.061(3) 0.043(3) 0.068(3) 0.009(2) 0.001(2) 0.026(2) C26 0.063(3) 0.059(3) 0.081(4) 0.021(3) 0.005(3) 0.032(3) N9 0.062(3) 0.056(3) 0.081(3) 0.020(2) 0.005(2) 0.029(2) C27 0.063(3) 0.053(3) 0.089(4) 0.018(3) 0.005(3) 0.028(3) N10 0.068(3) 0.054(3) 0.110(4) 0.023(3) 0.017(3) 0.032(2) C28 0.061(4) 0.070(4) 0.136(7) 0.020(4) -0.007(4) 0.017(3) C29 0.083(5) 0.067(4) 0.092(5) 0.003(3) -0.006(4) 0.018(3) C30 0.107(6) 0.071(5) 0.170(8) 0.037(5) 0.059(6) 0.054(4) O12 0.065(2) 0.060(2) 0.076(2) -0.0068(18) -0.0093(18) 0.0380(19) O13 0.059(2) 0.052(2) 0.074(2) -0.0005(16) -0.0027(16) 0.0322(17) C31 0.066(3) 0.045(3) 0.066(3) 0.004(2) 0.002(2) 0.032(2) C32 0.072(4) 0.062(3) 0.071(3) -0.007(3) -0.008(3) 0.035(3) N11 0.063(3) 0.057(3) 0.069(3) -0.003(2) -0.006(2) 0.028(2) C33 0.072(4) 0.060(3) 0.078(4) 0.003(3) -0.003(3) 0.035(3) N12 0.077(3) 0.061(3) 0.088(3) -0.007(3) -0.015(3) 0.038(3) C34 0.078(4) 0.079(5) 0.101(5) 0.009(4) -0.011(4) 0.017(4) C35 0.074(4) 0.080(4) 0.078(4) 0.009(3) -0.007(3) 0.018(3) C36 0.091(5) 0.073(4) 0.136(7) -0.010(4) -0.046(5) 0.042(4) O14 0.0499(19) 0.066(2) 0.083(2) 0.0041(19) -0.0051(17) 0.0237(17) O15 0.067(2) 0.048(2) 0.084(3) 0.0046(18) 0.0003(19) 0.0215(17) C38 0.104(6) 0.085(5) 0.120(6) 0.000(5) -0.007(5) 0.037(5) O16 0.072(2) 0.062(2) 0.095(3) 0.006(2) -0.001(2) 0.047(2) C39 0.116(9) 0.222(16) 0.30(2) -0.091(15) -0.056(11) 0.121(11) Fe4 0.0582(4) 0.0573(4) 0.0698(5) 0.0097(3) -0.0020(3) 0.0300(4) Cl41 0.0632(8) 0.0713(9) 0.1016(11) 0.0172(8) 0.0119(7) 0.0380(7) Cl42 0.0911(10) 0.0582(8) 0.0776(9) 0.0047(6) -0.0073(7) 0.0395(7) Cl43 0.0717(9) 0.1013(12) 0.0778(9) 0.0230(8) 0.0094(7) 0.0343(9) Cl44 0.0820(10) 0.0680(9) 0.1018(12) 0.0056(8) -0.0239(9) 0.0247(8) Fe5 0.0652(5) 0.0592(5) 0.0687(5) 0.0025(4) -0.0025(4) 0.0324(4) Cl51 0.0654(8) 0.0798(10) 0.1021(11) -0.0003(8) -0.0137(8) 0.0341(8) Cl52 0.0734(9) 0.1053(13) 0.0711(9) 0.0019(8) -0.0076(7) 0.0306(9) Cl53 0.0748(9) 0.0771(10) 0.0809(9) 0.0034(7) 0.0067(7) 0.0270(8) Cl54 0.1542(19) 0.0635(10) 0.0948(12) 0.0063(8) 0.0161(12) 0.0534(11) Fe6 0.0696(5) 0.0641(5) 0.0672(5) 0.0125(4) 0.0011(4) 0.0422(4) Cl61 0.0801(9) 0.0846(10) 0.0662(8) 0.0102(7) -0.0004(6) 0.0499(8) Cl62 0.0997(12) 0.0662(9) 0.0795(9) 0.0062(7) 0.0024(8) 0.0408(8) Cl63 0.0910(10) 0.0659(9) 0.0872(10) 0.0211(7) -0.0012(8) 0.0359(8) Cl64 0.0849(11) 0.1230(15) 0.0965(11) 0.0253(10) 0.0019(9) 0.0713(11) Fe7 0.0696(5) 0.0667(5) 0.0667(5) 0.0013(4) 0.0030(4) 0.0425(4) Cl71 0.0695(8) 0.0751(9) 0.0672(8) 0.0037(6) 0.0045(6) 0.0408(7) Cl72 0.0867(10) 0.0731(9) 0.0748(9) 0.0077(7) 0.0027(7) 0.0441(8) Cl73 0.0984(12) 0.0751(10) 0.0921(11) -0.0171(8) 0.0079(9) 0.0329(9) Cl74 0.0881(11) 0.1256(16) 0.0905(11) 0.0048(10) 0.0070(9) 0.0757(12) Fe8 0.0723(5) 0.0642(5) 0.0693(5) 0.0061(4) -0.0035(4) 0.0377(4) Cl81 0.0894(11) 0.0855(11) 0.0802(9) -0.0053(8) -0.0153(8) 0.0499(9) Cl82 0.0881(11) 0.1043(13) 0.0792(9) 0.0179(9) 0.0108(8) 0.0590(10) Cl83 0.0744(10) 0.1427(18) 0.0863(11) 0.0058(11) -0.0012(8) 0.0585(11) Cl84 0.156(2) 0.0581(9) 0.1096(14) 0.0070(9) -0.0200(13) 0.0306(11) Fe9 0.0618(5) 0.0859(6) 0.0640(5) 0.0026(4) 0.0015(4) 0.0412(4) Cl91 0.0664(8) 0.0631(8) 0.0727(8) 0.0039(6) -0.0003(6) 0.0330(6) Cl92 0.0660(9) 0.1062(13) 0.0842(10) -0.0163(9) -0.0087(7) 0.0377(9) Cl93 0.0747(10) 0.1145(14) 0.0821(10) 0.0214(9) 0.0113(8) 0.0392(10) Cl94 0.1099(14) 0.1335(17) 0.0924(11) 0.0085(11) 0.0088(10) 0.0900(14) Fe10 0.0759(7) 0.0866(9) 0.0802(8) 0.0149(6) 0.0045(6) 0.0280(6) Cl11 0.0717(12) 0.130(2) 0.1176(18) 0.0046(15) 0.0008(11) 0.0463(13) Cl12 0.1072(16) 0.0882(14) 0.0750(12) 0.0149(10) -0.0025(11) 0.0092(12) Cl13 0.0899(14) 0.1051(17) 0.0941(14) 0.0003(12) 0.0052(11) 0.0409(13) Cl14 0.142(2) 0.1014(19) 0.138(2) 0.0181(16) 0.0035(18) 0.0659(19) Fe11 0.0759(7) 0.0866(9) 0.0802(8) 0.0149(6) 0.0045(6) 0.0280(6) O42 0.247(12) 0.124(7) 0.216(9) 0.012(6) -0.051(9) 0.105(8) C42 0.159(13) 0.218(18) 0.178(10) 0.040(11) -0.021(10) 0.084(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.925(3) . ? Fe1 O4 2.010(3) . ? Fe1 O2 2.016(4) . ? Fe1 O13 2.020(4) . ? Fe1 O11 2.026(4) . ? Fe1 O14 2.036(4) . ? Fe2 O1 1.880(3) . ? Fe2 O3 2.020(3) . ? Fe2 O8 2.020(3) . ? Fe2 O5 2.025(3) . ? Fe2 O6 2.029(3) . ? Fe2 O15 2.079(4) . ? Fe3 O1 1.923(3) . ? Fe3 O10 1.991(4) . ? Fe3 O12 1.997(4) . ? Fe3 O9 2.003(4) . ? Fe3 O7 2.009(4) . ? Fe3 O16 2.056(3) . ? O2 C1 1.252(6) . ? O3 C1 1.244(6) . ? C1 C2 1.516(7) . ? C2 N1 1.440(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N1 C3 1.327(7) . ? N1 C5 1.367(8) . ? C3 N2 1.324(8) . ? C3 H3A 0.9300 . ? N2 C4 1.369(8) . ? N2 C6 1.464(8) . ? C4 C5 1.343(11) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? O4 C7 1.253(6) . ? O5 C7 1.252(6) . ? C7 C8 1.525(6) . ? C8 N3 1.457(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N3 C9 1.329(8) . ? N3 C11 1.371(7) . ? C9 N4 1.318(8) . ? C9 H9A 0.9300 . ? N4 C10 1.378(8) . ? N4 C12 1.449(8) . ? C10 C11 1.324(10) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? O6 C13 1.265(6) . ? O7 C13 1.261(7) . ? C13 C14 1.501(7) . ? C14 N5 1.448(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? N5 C15 1.294(8) . ? N5 C17 1.363(8) . ? C15 N6 1.324(8) . ? C15 H15A 0.9300 . ? N6 C16 1.332(9) . ? N6 C18 1.496(10) . ? C16 C17 1.334(11) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? O8 C19 1.246(6) . ? O9 C19 1.255(7) . ? C19 C20 1.496(8) . ? C20 N7 1.454(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? N7 C21 1.302(9) . ? N7 C23 1.370(8) . ? C21 N8 1.312(8) . ? C21 H21A 0.9300 . ? N8 C22 1.368(9) . ? N8 C24 1.475(10) . ? C22 C23 1.341(12) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? O10 C25 1.257(7) . ? O11 C25 1.261(6) . ? C25 C26 1.499(7) . ? C26 N9 1.452(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? N9 C27 1.312(8) . ? N9 C29 1.386(9) . ? C27 N10 1.328(8) . ? C27 H27A 0.9300 . ? N10 C28 1.373(11) . ? N10 C30 1.451(10) . ? C28 C29 1.346(11) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? O12 C31 1.253(7) . ? O13 C31 1.258(6) . ? C31 C32 1.521(8) . ? C32 N11 1.451(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? N11 C33 1.329(7) . ? N11 C35 1.367(9) . ? C33 N12 1.325(9) . ? C33 H33A 0.9300 . ? N12 C34 1.362(10) . ? N12 C36 1.477(8) . ? C34 C35 1.345(10) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? O14 C37A 1.477(15) . ? O14 C37B 1.52(3) . ? O14 H141 0.9300 . ? O14 H142 0.9299 . ? C37A H142 0.5703 . ? C37A H37A 0.9600 . ? C37A H37B 0.9600 . ? C37A H37C 0.9600 . ? C37B H37D 0.9600 . ? C37B H37E 0.9600 . ? C37B H37F 0.9600 . ? O15 C38 1.445(10) . ? O15 H151 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? O16 C39 1.4934 . ? O16 H161 0.9300 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? Fe4 Cl44 2.179(2) . ? Fe4 Cl41 2.1896(15) . ? Fe4 Cl42 2.1918(16) . ? Fe4 Cl43 2.1991(18) . ? Fe5 Cl53 2.1805(19) . ? Fe5 Cl54 2.186(2) . ? Fe5 Cl52 2.1933(18) . ? Fe5 Cl51 2.1938(17) . ? Fe6 Cl62 2.1880(19) . ? Fe6 Cl64 2.1917(17) . ? Fe6 Cl63 2.197(2) . ? Fe6 Cl61 2.1976(16) . ? Fe7 Cl74 2.1819(17) . ? Fe7 Cl72 2.1871(18) . ? Fe7 Cl73 2.193(2) . ? Fe7 Cl71 2.2093(16) . ? Fe8 Cl81 2.1749(19) . ? Fe8 Cl82 2.1774(19) . ? Fe8 Cl84 2.187(2) . ? Fe8 Cl83 2.2007(18) . ? Fe9 Cl93 2.178(2) . ? Fe9 Cl92 2.1848(19) . ? Fe9 Cl91 2.1880(17) . ? Fe9 Cl94 2.1953(18) . ? Fe10 Cl14 2.170(3) . ? Fe10 Cl11 2.188(2) . ? Fe10 Cl12 2.197(3) . ? Fe10 Cl13 2.220(3) . ? O42 C42 1.544(17) . ? O43 C43 1.56(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 O4 94.18(14) . . ? O1 Fe1 O2 94.62(14) . . ? O4 Fe1 O2 91.63(15) . . ? O1 Fe1 O13 95.61(14) . . ? O4 Fe1 O13 88.22(15) . . ? O2 Fe1 O13 169.75(15) . . ? O1 Fe1 O11 95.46(14) . . ? O4 Fe1 O11 170.36(15) . . ? O2 Fe1 O11 87.41(15) . . ? O13 Fe1 O11 91.02(15) . . ? O1 Fe1 O14 179.89(18) . . ? O4 Fe1 O14 85.76(16) . . ? O2 Fe1 O14 85.28(16) . . ? O13 Fe1 O14 84.49(16) . . ? O11 Fe1 O14 84.59(16) . . ? O1 Fe2 O3 95.32(15) . . ? O1 Fe2 O8 96.33(15) . . ? O3 Fe2 O8 168.22(15) . . ? O1 Fe2 O5 97.46(14) . . ? O3 Fe2 O5 90.97(14) . . ? O8 Fe2 O5 85.77(14) . . ? O1 Fe2 O6 95.71(14) . . ? O3 Fe2 O6 88.14(14) . . ? O8 Fe2 O6 92.46(14) . . ? O5 Fe2 O6 166.82(15) . . ? O1 Fe2 O15 177.87(16) . . ? O3 Fe2 O15 83.32(16) . . ? O8 Fe2 O15 85.08(16) . . ? O5 Fe2 O15 84.22(15) . . ? O6 Fe2 O15 82.62(16) . . ? O1 Fe3 O10 94.84(14) . . ? O1 Fe3 O12 93.62(14) . . ? O10 Fe3 O12 94.49(18) . . ? O1 Fe3 O9 94.82(14) . . ? O10 Fe3 O9 170.10(14) . . ? O12 Fe3 O9 87.06(18) . . ? O1 Fe3 O7 95.50(14) . . ? O10 Fe3 O7 85.74(18) . . ? O12 Fe3 O7 170.82(14) . . ? O9 Fe3 O7 91.17(18) . . ? O1 Fe3 O16 178.13(17) . . ? O10 Fe3 O16 84.43(16) . . ? O12 Fe3 O16 84.72(16) . . ? O9 Fe3 O16 85.98(16) . . ? O7 Fe3 O16 86.17(16) . . ? Fe2 O1 Fe3 119.80(17) . . ? Fe2 O1 Fe1 120.37(15) . . ? Fe3 O1 Fe1 119.83(17) . . ? C1 O2 Fe1 131.8(3) . . ? C1 O3 Fe2 131.7(3) . . ? O3 C1 O2 127.1(5) . . ? O3 C1 C2 118.6(5) . . ? O2 C1 C2 114.3(5) . . ? N1 C2 C1 114.1(5) . . ? N1 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C3 N1 C5 107.8(5) . . ? C3 N1 C2 126.7(4) . . ? C5 N1 C2 125.4(5) . . ? N2 C3 N1 109.0(5) . . ? N2 C3 H3A 125.5 . . ? N1 C3 H3A 125.5 . . ? C3 N2 C4 108.5(5) . . ? C3 N2 C6 125.6(5) . . ? C4 N2 C6 125.9(5) . . ? C5 C4 N2 106.8(5) . . ? C5 C4 H4A 126.6 . . ? N2 C4 H4A 126.6 . . ? C4 C5 N1 107.9(5) . . ? C4 C5 H5A 126.1 . . ? N1 C5 H5A 126.1 . . ? 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 . . ? C7 O4 Fe1 133.5(3) . . ? C7 O5 Fe2 129.0(3) . . ? O5 C7 O4 127.7(4) . . ? O5 C7 C8 119.4(5) . . ? O4 C7 C8 112.9(4) . . ? N3 C8 C7 114.0(4) . . ? N3 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? N3 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C9 N3 C11 108.0(5) . . ? C9 N3 C8 127.0(4) . . ? C11 N3 C8 125.0(5) . . ? N4 C9 N3 109.2(5) . . ? N4 C9 H9A 125.4 . . ? N3 C9 H9A 125.4 . . ? C9 N4 C10 107.4(5) . . ? C9 N4 C12 126.6(5) . . ? C10 N4 C12 125.8(5) . . ? C11 C10 N4 108.1(6) . . ? C11 C10 H10A 126.0 . . ? N4 C10 H10A 126.0 . . ? C10 C11 N3 107.3(6) . . ? C10 C11 H11A 126.4 . . ? N3 C11 H11A 126.4 . . ? 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 . . ? C13 O6 Fe2 132.1(4) . . ? C13 O7 Fe3 131.2(3) . . ? O7 C13 O6 126.3(5) . . ? O7 C13 C14 114.8(4) . . ? O6 C13 C14 118.9(5) . . ? N5 C14 C13 113.6(4) . . ? N5 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? N5 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C15 N5 C17 107.8(6) . . ? C15 N5 C14 125.6(5) . . ? C17 N5 C14 126.6(6) . . ? N5 C15 N6 110.1(5) . . ? N5 C15 H15A 125.0 . . ? N6 C15 H15A 125.0 . . ? C15 N6 C16 107.1(6) . . ? C15 N6 C18 124.8(6) . . ? C16 N6 C18 128.1(6) . . ? N6 C16 C17 108.6(6) . . ? N6 C16 H16A 125.7 . . ? C17 C16 H16A 125.7 . . ? C16 C17 N5 106.4(6) . . ? C16 C17 H17A 126.8 . . ? N5 C17 H17A 126.8 . . ? 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 . . ? C19 O8 Fe2 129.5(4) . . ? C19 O9 Fe3 133.2(3) . . ? O8 C19 O9 126.2(5) . . ? O8 C19 C20 120.5(5) . . ? O9 C19 C20 113.3(4) . . ? N7 C20 C19 114.0(5) . . ? N7 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? N7 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C21 N7 C23 108.0(6) . . ? C21 N7 C20 126.2(5) . . ? C23 N7 C20 125.7(6) . . ? N7 C21 N8 110.6(5) . . ? N7 C21 H21A 124.7 . . ? N8 C21 H21A 124.7 . . ? C21 N8 C22 107.0(6) . . ? C21 N8 C24 126.5(6) . . ? C22 N8 C24 126.5(6) . . ? C23 C22 N8 107.9(6) . . ? C23 C22 H22A 126.1 . . ? N8 C22 H22A 126.1 . . ? C22 C23 N7 106.4(7) . . ? C22 C23 H23A 126.8 . . ? N7 C23 H23A 126.8 . . ? 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 . . ? C25 O10 Fe3 133.9(3) . . ? C25 O11 Fe1 131.4(4) . . ? O10 C25 O11 126.0(5) . . ? O10 C25 C26 114.3(4) . . ? O11 C25 C26 119.7(5) . . ? N9 C26 C25 114.3(4) . . ? N9 C26 H26A 108.7 . . ? C25 C26 H26A 108.7 . . ? N9 C26 H26B 108.7 . . ? C25 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C27 N9 C29 109.3(6) . . ? C27 N9 C26 125.5(6) . . ? C29 N9 C26 125.2(6) . . ? N9 C27 N10 109.2(6) . . ? N9 C27 H27A 125.4 . . ? N10 C27 H27A 125.4 . . ? C27 N10 C28 107.4(6) . . ? C27 N10 C30 125.3(7) . . ? C28 N10 C30 127.2(7) . . ? C29 C28 N10 108.6(6) . . ? C29 C28 H28A 125.7 . . ? N10 C28 H28A 125.7 . . ? C28 C29 N9 105.4(7) . . ? C28 C29 H29A 127.3 . . ? N9 C29 H29A 127.3 . . ? 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 . . ? C31 O12 Fe3 132.8(3) . . ? C31 O13 Fe1 130.4(4) . . ? O12 C31 O13 127.6(5) . . ? O12 C31 C32 113.3(4) . . ? O13 C31 C32 119.1(5) . . ? N11 C32 C31 113.6(5) . . ? N11 C32 H32A 108.8 . . ? C31 C32 H32A 108.8 . . ? N11 C32 H32B 108.8 . . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C33 N11 C35 108.9(5) . . ? C33 N11 C32 125.3(5) . . ? C35 N11 C32 125.8(5) . . ? N12 C33 N11 108.3(6) . . ? N12 C33 H33A 125.8 . . ? N11 C33 H33A 125.8 . . ? C33 N12 C34 108.4(5) . . ? C33 N12 C36 126.0(6) . . ? C34 N12 C36 125.6(7) . . ? C35 C34 N12 107.9(7) . . ? C35 C34 H34A 126.1 . . ? N12 C34 H34A 126.1 . . ? C34 C35 N11 106.5(6) . . ? C34 C35 H35A 126.8 . . ? N11 C35 H35A 126.8 . . ? 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 . . ? C37A O14 C37B 107.6(13) . . ? C37A O14 Fe1 126.6(6) . . ? C37B O14 Fe1 125.7(12) . . ? C37A O14 H141 116.7 . . ? C37B O14 H141 9.2 . . ? Fe1 O14 H141 116.7 . . ? C37A O14 H142 7.8 . . ? C37B O14 H142 115.0 . . ? Fe1 O14 H142 119.2 . . ? H141 O14 H142 124.0 . . ? O14 C37A H142 12.8 . . ? O14 C37A H37A 109.5 . . ? H142 C37A H37A 121.3 . . ? O14 C37A H37B 109.5 . . ? H142 C37A H37B 99.2 . . ? H37A C37A H37B 109.5 . . ? O14 C37A H37C 109.5 . . ? H142 C37A H37C 107.1 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? O14 C37B H37D 109.5 . . ? O14 C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? O14 C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C38 O15 Fe2 127.5(5) . . ? C38 O15 H151 116.2 . . ? Fe2 O15 H151 116.2 . . ? O15 C38 H38A 109.5 . . ? O15 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O15 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C39 O16 Fe3 121.93(13) . . ? C39 O16 H161 119.0 . . ? Fe3 O16 H161 119.0 . . ? O16 C39 H39A 109.5 . . ? O16 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O16 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Cl44 Fe4 Cl41 111.36(8) . . ? Cl44 Fe4 Cl42 112.06(7) . . ? Cl41 Fe4 Cl42 108.48(7) . . ? Cl44 Fe4 Cl43 109.92(8) . . ? Cl41 Fe4 Cl43 106.48(7) . . ? Cl42 Fe4 Cl43 108.34(8) . . ? Cl53 Fe5 Cl54 113.38(8) . . ? Cl53 Fe5 Cl52 109.70(8) . . ? Cl54 Fe5 Cl52 109.38(9) . . ? Cl53 Fe5 Cl51 111.22(7) . . ? Cl54 Fe5 Cl51 106.35(9) . . ? Cl52 Fe5 Cl51 106.54(7) . . ? Cl62 Fe6 Cl64 107.24(9) . . ? Cl62 Fe6 Cl63 111.93(8) . . ? Cl64 Fe6 Cl63 110.77(8) . . ? Cl62 Fe6 Cl61 108.94(7) . . ? Cl64 Fe6 Cl61 108.28(7) . . ? Cl63 Fe6 Cl61 109.59(8) . . ? Cl74 Fe7 Cl72 109.79(8) . . ? Cl74 Fe7 Cl73 110.86(8) . . ? Cl72 Fe7 Cl73 110.41(8) . . ? Cl74 Fe7 Cl71 106.76(7) . . ? Cl72 Fe7 Cl71 109.23(6) . . ? Cl73 Fe7 Cl71 109.71(8) . . ? Cl81 Fe8 Cl82 116.89(9) . . ? Cl81 Fe8 Cl84 106.26(8) . . ? Cl82 Fe8 Cl84 106.46(9) . . ? Cl81 Fe8 Cl83 108.54(8) . . ? Cl82 Fe8 Cl83 107.33(7) . . ? Cl84 Fe8 Cl83 111.39(11) . . ? Cl93 Fe9 Cl92 110.20(9) . . ? Cl93 Fe9 Cl91 108.88(7) . . ? Cl92 Fe9 Cl91 108.39(7) . . ? Cl93 Fe9 Cl94 108.46(8) . . ? Cl92 Fe9 Cl94 108.87(8) . . ? Cl91 Fe9 Cl94 112.04(9) . . ? Cl14 Fe10 Cl11 112.21(14) . . ? Cl14 Fe10 Cl12 106.58(13) . . ? Cl11 Fe10 Cl12 107.92(13) . . ? Cl14 Fe10 Cl13 109.87(13) . . ? Cl11 Fe10 Cl13 106.47(11) . . ? Cl12 Fe10 Cl13 113.89(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H141 O41A 0.93 1.68 2.604(14) 169.6 . O14 H142 O41B 0.93 1.61 2.53(2) 170.6 . O15 H151 Cl12 0.93 2.28 3.118(5) 149.1 . O16 H161 O42 0.93 2.10 2.691(11) 120.1 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.020 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.133 data_13acpyw _database_code_depnum_ccdc_archive 'CCDC 896160' #TrackingRef 'Fe3_IL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C36 H54 Fe3 N12 O16), 3(Cl4 Fe), 4(Cl), 7(H2 O)' _chemical_formula_sum 'C36 H68 Cl16 Fe6 N12 O23' _chemical_formula_weight 1939.32 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' 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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P -6 2 c' _symmetry_space_group_name_Hall 'P -6c -2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z+1/2' '-y, x-y, -z+1/2' '-x+y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' _cell_length_a 13.3201(6) _cell_length_b 13.3201(6) _cell_length_c 24.7380(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3801.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.56 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Stoe IPDS' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29754 _diffrn_reflns_av_R_equivalents 0.0869 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.09 _reflns_number_total 2588 _reflns_number_gt 2153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_cell_refinement 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_data_reduction 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. Geometrical restraints were applied to positions of water H atoms. A chloride anion and a lattice water were 50:50 disordered; a similarity restraint was applied to the anisotropic thermal parameters of the closely separated atoms ; _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^)+(0.0783P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 2588 _refine_ls_number_parameters 171 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.068 _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 0.09987(7) 0.16432(7) 0.2500 0.0258(2) Uani 1 2 d S . . O1 O 0.0000 0.0000 0.2500 0.0272(15) Uani 1 6 d S . . O2 O 0.2048(3) 0.1634(3) 0.30759(16) 0.0352(8) Uani 1 1 d . . . O3 O 0.1857(3) -0.0132(3) 0.30776(15) 0.0341(8) Uani 1 1 d . . . C1 C 0.2282(4) 0.0883(4) 0.3237(2) 0.0297(10) Uani 1 1 d . . . C2 C 0.3191(5) 0.1305(5) 0.3670(2) 0.0431(13) Uani 1 1 d . . . H2A H 0.3881 0.1984 0.3537 0.052 Uiso 1 1 calc R . . H2B H 0.2913 0.1545 0.3979 0.052 Uiso 1 1 calc R . . N1 N 0.3507(4) 0.0465(4) 0.38492(19) 0.0427(11) Uani 1 1 d . . . C3 C 0.4416(5) 0.0431(5) 0.3677(3) 0.0452(14) Uani 1 1 d . . . H3A H 0.4944 0.0930 0.3422 0.054 Uiso 1 1 calc R . . N2 N 0.4464(4) -0.0435(4) 0.3924(2) 0.0483(13) Uani 1 1 d . . . C4 C 0.3534(7) -0.0980(7) 0.4256(3) 0.0658(19) Uani 1 1 d . . . H4A H 0.3347 -0.1618 0.4474 0.079 Uiso 1 1 calc R . . C5 C 0.2930(7) -0.0413(7) 0.4208(3) 0.0665(19) Uani 1 1 d . . . H5A H 0.2247 -0.0591 0.4388 0.080 Uiso 1 1 calc R . . C6 C 0.5391(7) -0.0717(7) 0.3858(4) 0.072(2) Uani 1 1 d . . . H6A H 0.5944 -0.0201 0.3598 0.108 Uiso 1 1 calc R . . H6B H 0.5064 -0.1502 0.3734 0.108 Uiso 1 1 calc R . . H6C H 0.5770 -0.0633 0.4199 0.108 Uiso 1 1 calc R . . O4 O 0.2112(4) 0.3397(4) 0.2500 0.0463(14) Uani 1 2 d SD . . H41 H 0.288(5) 0.367(9) 0.256(10) 0.069 Uiso 0.50 1 d PD . . H42 H 0.187(9) 0.392(7) 0.2500 0.069 Uiso 1 2 d SD . . O5 O 0.1667(7) 0.5086(7) 0.2500 0.098(4) Uani 1 2 d SD . . H51 H 0.097(8) 0.510(15) 0.2500 0.147 Uiso 1 2 d SD . . H52 H 0.208(13) 0.554(18) 0.280(6) 0.147 Uiso 0.50 1 d PD A -1 O6 O 0.4299(8) 0.1645(7) 0.2500 0.074(2) Uani 1 2 d SD . . H61 H 0.477(7) 0.230(5) 0.2787(10) 0.112 Uiso 1 1 d D . . Fe2 Fe 0.6667 0.3333 0.44040(5) 0.0421(3) Uani 1 3 d S . . Cl1 Cl 0.6667 0.3333 0.35269(10) 0.0528(6) Uani 1 3 d S . . Cl2 Cl 0.50470(13) 0.31716(14) 0.47034(6) 0.0543(4) Uani 1 1 d . . . Fe3 Fe 0.0000 0.0000 0.5000 0.0484(5) Uani 1 6 d S . . Cl3 Cl 0.0000 0.0000 0.40595(19) 0.0585(13) Uani 0.50 3 d SP . . Cl4 Cl 0.1624(7) 0.1594(6) 0.5134(3) 0.102(3) Uani 0.50 1 d P . . Cl11 Cl 0.4696(2) 0.4145(2) 0.2500 0.0659(7) Uani 1 2 d S . . Cl12 Cl 0.3333 0.6667 0.3425(6) 0.088(4) Uani 0.50 3 d SPU B 1 O12 O 0.3333 0.6667 0.324(2) 0.095(6) Uani 0.50 3 d SPU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0218(4) 0.0219(4) 0.0332(5) 0.000 0.000 0.0107(4) O1 0.026(2) 0.026(2) 0.029(4) 0.000 0.000 0.0131(11) O2 0.0329(18) 0.0260(16) 0.046(2) -0.0038(15) -0.0057(14) 0.0143(15) O3 0.0336(17) 0.0289(17) 0.040(2) -0.0015(15) -0.0058(15) 0.0158(14) C1 0.030(2) 0.030(2) 0.032(3) 0.0018(19) -0.0001(19) 0.0163(19) C2 0.056(3) 0.041(3) 0.043(3) -0.012(2) -0.018(3) 0.032(3) N1 0.050(3) 0.044(2) 0.035(3) -0.005(2) -0.017(2) 0.024(2) C3 0.049(3) 0.039(3) 0.053(4) 0.007(3) -0.008(3) 0.026(3) N2 0.055(3) 0.044(3) 0.052(3) -0.002(2) -0.014(2) 0.028(2) C4 0.069(4) 0.067(4) 0.064(5) 0.021(4) -0.007(4) 0.036(4) C5 0.066(4) 0.087(5) 0.051(4) 0.019(4) -0.001(3) 0.042(4) C6 0.079(5) 0.078(5) 0.081(6) 0.007(4) -0.010(4) 0.056(4) O4 0.028(2) 0.027(2) 0.075(4) 0.000 0.000 0.007(2) O5 0.067(5) 0.054(5) 0.181(12) 0.000 0.000 0.036(4) O6 0.092(6) 0.073(5) 0.069(5) 0.000 0.000 0.050(5) Fe2 0.0468(5) 0.0468(5) 0.0329(7) 0.000 0.000 0.0234(2) Cl1 0.0610(9) 0.0610(9) 0.0365(12) 0.000 0.000 0.0305(5) Cl2 0.0488(8) 0.0719(10) 0.0446(8) -0.0095(7) -0.0033(6) 0.0320(8) Fe3 0.0457(7) 0.0457(7) 0.0536(12) 0.000 0.000 0.0229(3) Cl3 0.075(2) 0.075(2) 0.026(2) 0.000 0.000 0.0373(11) Cl4 0.071(4) 0.071(4) 0.152(10) -0.049(5) -0.043(5) 0.0276(17) Cl11 0.0429(11) 0.0493(12) 0.100(2) 0.000 0.000 0.0187(9) Cl12 0.075(2) 0.075(2) 0.115(11) 0.000 0.000 0.0373(12) O12 0.082(5) 0.082(5) 0.120(15) 0.000 0.000 0.041(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 Fe1 O1 1.9101(8) . ? Fe1 O2 2.000(4) . ? Fe1 O2 2.000(4) 4 ? Fe1 O3 2.029(3) 5 ? Fe1 O3 2.029(3) 2 ? Fe1 O4 2.048(5) . ? O1 Fe1 1.9101(8) 2 ? O1 Fe1 1.9101(8) 3 ? O2 C1 1.253(6) . ? O3 C1 1.241(6) . ? O3 Fe1 2.029(3) 3 ? C1 C2 1.499(7) . ? C2 N1 1.449(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N1 C3 1.305(8) . ? N1 C5 1.359(9) . ? C3 N2 1.336(7) . ? C3 H3A 0.9300 . ? N2 C4 1.355(10) . ? N2 C6 1.469(9) . ? C4 C5 1.356(10) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? O4 H41 0.90(4) . ? O4 H42 0.90(4) . ? O5 H51 0.94(4) . ? O5 H52 0.95(4) . ? O6 H61 1.06(4) 4 ? O6 H61 1.06(4) . ? Fe2 Cl1 2.170(3) . ? Fe2 Cl2 2.1874(16) 3_665 ? Fe2 Cl2 2.1874(15) 2_655 ? Fe2 Cl2 2.1874(16) . ? Fe3 Cl4 2.169(4) . ? Fe3 Cl4 2.169(4) 2 ? Fe3 Cl4 2.169(4) 3 ? Fe3 Cl3 2.327(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 94.68(10) . . ? O1 Fe1 O2 94.68(10) . 4 ? O2 Fe1 O2 90.9(2) . 4 ? O1 Fe1 O3 96.36(10) . 5 ? O2 Fe1 O3 168.94(14) . 5 ? O2 Fe1 O3 88.75(14) 4 5 ? O1 Fe1 O3 96.36(10) . 2 ? O2 Fe1 O3 88.75(14) . 2 ? O2 Fe1 O3 168.94(14) 4 2 ? O3 Fe1 O3 89.5(2) 5 2 ? O1 Fe1 O4 178.25(16) . . ? O2 Fe1 O4 84.10(15) . . ? O2 Fe1 O4 84.10(15) 4 . ? O3 Fe1 O4 84.87(15) 5 . ? O3 Fe1 O4 84.87(15) 2 . ? Fe1 O1 Fe1 120.0 2 3 ? Fe1 O1 Fe1 120.0 2 . ? Fe1 O1 Fe1 120.0 3 . ? C1 O2 Fe1 133.2(3) . . ? C1 O3 Fe1 130.1(3) . 3 ? O3 C1 O2 127.5(5) . . ? O3 C1 C2 118.6(4) . . ? O2 C1 C2 113.9(4) . . ? N1 C2 C1 114.9(4) . . ? N1 C2 H2A 108.5 . . ? C1 C2 H2A 108.5 . . ? N1 C2 H2B 108.5 . . ? C1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C3 N1 C5 108.6(5) . . ? C3 N1 C2 124.0(5) . . ? C5 N1 C2 127.4(6) . . ? N1 C3 N2 109.0(6) . . ? N1 C3 H3A 125.5 . . ? N2 C3 H3A 125.5 . . ? C3 N2 C4 108.3(5) . . ? C3 N2 C6 125.4(6) . . ? C4 N2 C6 126.2(6) . . ? N2 C4 C5 106.6(6) . . ? N2 C4 H4A 126.7 . . ? C5 C4 H4A 126.7 . . ? C4 C5 N1 107.4(7) . . ? C4 C5 H5A 126.3 . . ? N1 C5 H5A 126.3 . . ? 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 . . ? Fe1 O4 H41 119(7) . . ? Fe1 O4 H42 123(7) . . ? H41 O4 H42 117(10) . . ? H51 O5 H52 105(6) . . ? H61 O6 H61 85(5) 4 . ? Cl1 Fe2 Cl2 109.79(5) . 3_665 ? Cl1 Fe2 Cl2 109.79(5) . 2_655 ? Cl2 Fe2 Cl2 109.15(5) 3_665 2_655 ? Cl1 Fe2 Cl2 109.79(5) . . ? Cl2 Fe2 Cl2 109.15(5) 3_665 . ? Cl2 Fe2 Cl2 109.15(5) 2_655 . ? Cl4 Fe3 Cl4 117.71(11) . 2 ? Cl4 Fe3 Cl4 117.71(11) . 3 ? Cl4 Fe3 Cl4 117.71(11) 2 3 ? Cl4 Fe3 Cl3 98.8(2) . . ? Cl4 Fe3 Cl3 98.8(2) 2 . ? Cl4 Fe3 Cl3 98.8(2) 3 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H41 Cl11 0.90(4) 2.18(6) 3.067(6) 166(20) . O4 H42 O5 0.90(4) 1.71(4) 2.596(9) 170(11) . O5 H51 Cl11 0.94(4) 2.18(4) 3.111(9) 175(15) 3_565 O5 H52 Cl12 0.95(4) 2.21(5) 3.150(12) 170(15) . O6 H61 Cl1 1.06(4) 2.85(6) 3.790(7) 148(7) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.289 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.094 data_19tfsaa _database_code_depnum_ccdc_archive 'CCDC 896161' #TrackingRef 'Fe3_IL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H54 Fe3 N19 O37, 7(C2 F6 N O6 S2), 2.43(H2 O)' _chemical_formula_sum 'C50 H58.86 F42 Fe3 N19 O46.43 S14' _chemical_formula_weight 3083.29 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14.9606(4) _cell_length_b 15.5623(4) _cell_length_c 27.4325(9) _cell_angle_alpha 93.562(2) _cell_angle_beta 101.381(2) _cell_angle_gamma 115.135(2) _cell_volume 5591.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 22508 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 26.36 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3087 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.917 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37919 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.73 _reflns_number_total 20945 _reflns_number_gt 13084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. O-H bond lengths were restrained to 0.92(4) Ang. Three of the (TFSA)- anions were extensively disordered. Refinement (with disordered partial-occupancy atoms isotropic) was successful with S-N, S-O, S-C and C-F bond lengths restrained to common values, as were S..S and F..F 1-3 distances where necessary. A (partial occupancy) lattice water, O(63B), was only consistent with the minor component of one of the TFSA anions; no corresponding major component appeared to be present, resulting in the total of 2.43 lattice waters per formula unit. ; _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^)+(0.0948P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20945 _refine_ls_number_parameters 1724 _refine_ls_number_restraints 147 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.19551(4) 0.21290(4) 0.25741(2) 0.02211(14) Uani 1 1 d . . . Fe2 Fe 0.08140(4) 0.35086(4) 0.22538(2) 0.02177(14) Uani 1 1 d . . . Fe3 Fe 0.33270(4) 0.44322(4) 0.25309(2) 0.02246(15) Uani 1 1 d . . . O1 O 0.2026(2) 0.33528(19) 0.24503(11) 0.0226(6) Uani 1 1 d . . . O2 O 0.0995(2) 0.1894(2) 0.30340(11) 0.0277(7) Uani 1 1 d . . . O3 O 0.0158(2) 0.2740(2) 0.27582(12) 0.0312(7) Uani 1 1 d . . . C1 C 0.0371(3) 0.2232(3) 0.30488(16) 0.0238(9) Uani 1 1 d . . . C2 C -0.0189(4) 0.2034(3) 0.34646(18) 0.0326(11) Uani 1 1 d . . . H2A H 0.0019 0.2651 0.3683 0.039 Uiso 1 1 calc R . . H2B H -0.0929 0.1763 0.3311 0.039 Uiso 1 1 calc R . . N1 N -0.0002(3) 0.1374(3) 0.37764(14) 0.0284(8) Uani 1 1 d . . . C3 C -0.0623(4) 0.0450(3) 0.37438(18) 0.0339(11) Uani 1 1 d . . . H3A H -0.1262 0.0100 0.3506 0.041 Uiso 1 1 calc R . . N2 N -0.0211(3) 0.0095(3) 0.40934(16) 0.0383(10) Uani 1 1 d . . . C4 C 0.0702(4) 0.0798(5) 0.4356(2) 0.0496(14) Uani 1 1 d . . . H4A H 0.1161 0.0735 0.4628 0.059 Uiso 1 1 calc R . . C5 C 0.0838(4) 0.1600(4) 0.41625(19) 0.0424(12) Uani 1 1 d . . . H5A H 0.1411 0.2213 0.4273 0.051 Uiso 1 1 calc R . . C6 C -0.0694(5) -0.0913(4) 0.4190(3) 0.0616(18) Uani 1 1 d . . . H6A H -0.1360 -0.1270 0.3951 0.092 Uiso 1 1 calc R . . H6B H -0.0781 -0.0910 0.4535 0.092 Uiso 1 1 calc R . . H6C H -0.0257 -0.1222 0.4149 0.092 Uiso 1 1 calc R . . O4 O 0.0792(2) 0.1384(2) 0.19694(12) 0.0322(7) Uani 1 1 d . . . O5 O 0.0133(2) 0.2369(2) 0.16979(13) 0.0358(8) Uani 1 1 d . . . C7 C 0.0206(3) 0.1595(3) 0.16670(18) 0.0316(10) Uani 1 1 d . . . C8 C -0.0514(5) 0.0851(4) 0.1202(2) 0.0496(14) Uani 1 1 d . . . H8A H -0.1228 0.0667 0.1214 0.060 Uiso 1 1 calc R . . H8B H -0.0405 0.1142 0.0895 0.060 Uiso 1 1 calc R . . N3 N -0.0346(3) -0.0006(3) 0.11748(15) 0.0343(9) Uani 1 1 d . . . C9 C 0.0160(4) -0.0204(3) 0.08818(18) 0.0340(11) Uani 1 1 d . . . H9A H 0.0453 0.0175 0.0645 0.041 Uiso 1 1 calc R . . N4 N 0.0198(3) -0.1017(3) 0.09685(14) 0.0333(9) Uani 1 1 d . . . C10 C -0.0304(4) -0.1344(4) 0.1335(2) 0.0424(12) Uani 1 1 d . . . H10A H -0.0396 -0.1915 0.1471 0.051 Uiso 1 1 calc R . . C11 C -0.0639(4) -0.0722(4) 0.1468(2) 0.0429(13) Uani 1 1 d . . . H11A H -0.1009 -0.0761 0.1717 0.051 Uiso 1 1 calc R . . C12 C 0.0661(4) -0.1496(4) 0.0698(2) 0.0478(14) Uani 1 1 d . . . H12A H 0.0972 -0.1102 0.0457 0.072 Uiso 1 1 calc R . . H12B H 0.0135 -0.2128 0.0517 0.072 Uiso 1 1 calc R . . H12C H 0.1185 -0.1578 0.0940 0.072 Uiso 1 1 calc R . . O6 O 0.1258(2) 0.4671(2) 0.27779(12) 0.0296(7) Uani 1 1 d . . . O7 O 0.2934(2) 0.5369(2) 0.28567(13) 0.0323(7) Uani 1 1 d . . . C13 C 0.2147(3) 0.5310(3) 0.29684(16) 0.0232(9) Uani 1 1 d . . . C14 C 0.2264(4) 0.6076(3) 0.33727(18) 0.0322(10) Uani 1 1 d . . . H14A H 0.1799 0.6356 0.3244 0.039 Uiso 1 1 calc R . . H14B H 0.2062 0.5778 0.3667 0.039 Uiso 1 1 calc R . . N5 N 0.3303(3) 0.6843(3) 0.35356(15) 0.0337(9) Uani 1 1 d . . . C15 C 0.3625(4) 0.7682(3) 0.3376(2) 0.0424(13) Uani 1 1 d . . . H15A H 0.3210 0.7898 0.3161 0.051 Uiso 1 1 calc R . . N6 N 0.4615(4) 0.8170(3) 0.35644(18) 0.0552(13) Uani 1 1 d . . . C16 C 0.4941(5) 0.7636(4) 0.3853(2) 0.0605(17) Uani 1 1 d . . . H16A H 0.5621 0.7823 0.4038 0.073 Uiso 1 1 calc R . . C17 C 0.4126(4) 0.6789(4) 0.3829(2) 0.0527(15) Uani 1 1 d . . . H17A H 0.4123 0.6260 0.3985 0.063 Uiso 1 1 calc R . . C18 C 0.5270(6) 0.9132(5) 0.3464(3) 0.096(3) Uani 1 1 d . . . H18A H 0.4850 0.9361 0.3242 0.144 Uiso 1 1 calc R . . H18B H 0.5781 0.9089 0.3302 0.144 Uiso 1 1 calc R . . H18C H 0.5614 0.9582 0.3783 0.144 Uiso 1 1 calc R . . O8 O 0.1274(2) 0.4330(2) 0.17312(12) 0.0318(7) Uani 1 1 d . . . O9 O 0.2949(2) 0.4818(2) 0.18633(13) 0.0367(8) Uani 1 1 d . . . C19 C 0.2111(4) 0.4721(3) 0.16171(17) 0.0276(10) Uani 1 1 d . . . C20 C 0.2051(4) 0.5066(4) 0.11166(18) 0.0390(12) Uani 1 1 d . . . H20A H 0.1728 0.4501 0.0844 0.047 Uiso 1 1 calc R . . H20B H 0.1607 0.5394 0.1087 0.047 Uiso 1 1 calc R . . N7 N 0.3036(3) 0.5723(3) 0.10422(15) 0.0342(9) Uani 1 1 d . . . C21 C 0.3263(3) 0.6582(3) 0.09171(16) 0.0307(10) Uani 1 1 d . . . H21A H 0.2822 0.6882 0.0879 0.037 Uiso 1 1 calc R . . N8 N 0.4191(3) 0.6959(3) 0.08528(17) 0.0461(12) Uani 1 1 d . . . C22 C 0.4554(6) 0.6307(7) 0.0929(4) 0.105(4) Uani 1 1 d . . . H22A H 0.5204 0.6381 0.0900 0.126 Uiso 1 1 calc R . . C23 C 0.3847(6) 0.5543(6) 0.1051(4) 0.099(3) Uani 1 1 d . . . H23A H 0.3901 0.4978 0.1129 0.119 Uiso 1 1 calc R . . C24 C 0.4720(5) 0.7915(5) 0.0705(3) 0.072(2) Uani 1 1 d . . . H24A H 0.4283 0.8242 0.0680 0.108 Uiso 1 1 calc R . . H24B H 0.4868 0.7831 0.0378 0.108 Uiso 1 1 calc R . . H24C H 0.5359 0.8304 0.0960 0.108 Uiso 1 1 calc R . . O10 O 0.3904(2) 0.4290(2) 0.32284(11) 0.0318(7) Uani 1 1 d . . . O11 O 0.3085(2) 0.2703(2) 0.32092(12) 0.0331(7) Uani 1 1 d . . . C25 C 0.3686(3) 0.3543(3) 0.34260(17) 0.0273(10) Uani 1 1 d . . . C26 C 0.4163(5) 0.3713(4) 0.39808(19) 0.0422(13) Uani 1 1 d . . . H26A H 0.4871 0.4227 0.4051 0.051 Uiso 1 1 calc R . . H26B H 0.3784 0.3946 0.4167 0.051 Uiso 1 1 calc R . . N9 N 0.4181(3) 0.2863(3) 0.41722(14) 0.0336(9) Uani 1 1 d . . . C27 C 0.5004(4) 0.2878(4) 0.44659(18) 0.0369(11) Uani 1 1 d . . . H27A H 0.5657 0.3417 0.4566 0.044 Uiso 1 1 calc R . . N10 N 0.4769(4) 0.2020(3) 0.45973(17) 0.0449(11) Uani 1 1 d . . . C28 C 0.3763(5) 0.1432(4) 0.4377(2) 0.0570(16) Uani 1 1 d . . . H28A H 0.3400 0.0773 0.4402 0.068 Uiso 1 1 calc R . . C29 C 0.3383(4) 0.1958(4) 0.4117(2) 0.0508(15) Uani 1 1 d . . . H29A H 0.2699 0.1747 0.3932 0.061 Uiso 1 1 calc R . . C30 C 0.5509(6) 0.1752(6) 0.4905(3) 0.076(2) Uani 1 1 d . . . H30A H 0.5162 0.1078 0.4948 0.114 Uiso 1 1 calc R . . H30B H 0.5805 0.2165 0.5236 0.114 Uiso 1 1 calc R . . H30C H 0.6051 0.1835 0.4735 0.114 Uiso 1 1 calc R . . O12 O 0.3944(2) 0.3701(2) 0.22011(12) 0.0305(7) Uani 1 1 d . . . O13 O 0.2924(2) 0.2137(2) 0.21616(13) 0.0344(8) Uani 1 1 d . . . C31 C 0.3662(3) 0.2823(3) 0.20749(17) 0.0285(10) Uani 1 1 d . . . C32 C 0.4259(4) 0.2522(3) 0.1767(2) 0.0366(12) Uani 1 1 d . . . H32A H 0.4561 0.2156 0.1964 0.044 Uiso 1 1 calc R . . H32B H 0.3779 0.2085 0.1455 0.044 Uiso 1 1 calc R . . N11 N 0.5063(3) 0.3319(3) 0.16303(14) 0.0271(8) Uani 1 1 d . . . C33 C 0.6045(4) 0.3705(4) 0.18644(18) 0.0349(11) Uani 1 1 d . . . H33A H 0.6337 0.3500 0.2145 0.042 Uiso 1 1 calc R . . N12 N 0.6546(3) 0.4420(3) 0.16419(16) 0.0372(10) Uani 1 1 d . . . C34 C 0.5863(4) 0.4490(4) 0.1252(2) 0.0407(12) Uani 1 1 d . . . H34A H 0.6018 0.4945 0.1028 0.049 Uiso 1 1 calc R . . C35 C 0.4949(4) 0.3808(4) 0.12434(19) 0.0367(11) Uani 1 1 d . . . H35A H 0.4328 0.3680 0.1012 0.044 Uiso 1 1 calc R . . C36 C 0.7662(4) 0.4958(5) 0.1755(3) 0.073(2) Uani 1 1 d . . . H36A H 0.7967 0.4763 0.2051 0.109 Uiso 1 1 calc R . . H36B H 0.7863 0.5649 0.1824 0.109 Uiso 1 1 calc R . . H36C H 0.7900 0.4821 0.1465 0.109 Uiso 1 1 calc R . . O14 O 0.1913(3) 0.0853(2) 0.27080(13) 0.0331(7) Uani 1 1 d D . . H141 H 0.212(4) 0.055(4) 0.253(2) 0.050 Uiso 1 1 d D . . H142 H 0.149(4) 0.045(4) 0.287(2) 0.050 Uiso 1 1 d D . . O15 O -0.0552(2) 0.3579(2) 0.20194(12) 0.0283(7) Uani 1 1 d D . . H151 H -0.099(4) 0.321(3) 0.1740(15) 0.042 Uiso 1 1 d D . . H152 H -0.092(4) 0.352(4) 0.2233(18) 0.042 Uiso 1 1 d D . . O16 O 0.4695(2) 0.5606(2) 0.26133(15) 0.0389(8) Uani 1 1 d D . . H161 H 0.465(5) 0.612(3) 0.252(2) 0.058 Uiso 1 1 d D . . H162 H 0.528(3) 0.571(4) 0.2832(19) 0.058 Uiso 1 1 d D . . O61 O 0.4466(3) 0.7162(3) 0.2438(2) 0.0766(16) Uani 1 1 d D . . H611 H 0.383(4) 0.714(6) 0.230(3) 0.115 Uiso 1 1 d D . . H612 H 0.487(6) 0.769(4) 0.234(3) 0.115 Uiso 1 1 d D . . O62 O 0.0785(5) -0.0362(4) 0.3192(3) 0.100(2) Uani 1 1 d D . . H621 H 0.105(8) -0.075(7) 0.332(4) 0.149 Uiso 1 1 d D . . H622 H 0.012(3) -0.065(8) 0.315(4) 0.149 Uiso 1 1 d D . . O63B O 0.6181(8) 0.5243(8) 0.3117(4) 0.067(3) Uiso 0.43 1 d P A 2 S1 S 0.27489(10) -0.09471(9) 0.21112(5) 0.0383(3) Uani 1 1 d . . . N21 N 0.1809(3) -0.1874(3) 0.17951(17) 0.0415(10) Uani 1 1 d . . . S2 S 0.15739(10) -0.29383(9) 0.18517(6) 0.0429(3) Uani 1 1 d . . . O22 O 0.2488(4) -0.0165(3) 0.20808(18) 0.0635(12) Uani 1 1 d . . . O23 O 0.3252(4) -0.1048(3) 0.25838(14) 0.0657(13) Uani 1 1 d . . . O24 O 0.2352(3) -0.3097(3) 0.21567(19) 0.0635(12) Uani 1 1 d . . . O25 O 0.1050(4) -0.3524(3) 0.13681(19) 0.0851(16) Uani 1 1 d . . . C41 C 0.3665(4) -0.0680(4) 0.1721(2) 0.0453(13) Uani 1 1 d . . . F1 F 0.4526(3) 0.0054(3) 0.19517(16) 0.0814(13) Uani 1 1 d . . . F2 F 0.3317(3) -0.0493(3) 0.12850(14) 0.0718(11) Uani 1 1 d . . . F3 F 0.3836(3) -0.1437(3) 0.16311(17) 0.0760(12) Uani 1 1 d . . . C42 C 0.0598(5) -0.3249(5) 0.2203(3) 0.0632(19) Uani 1 1 d . . . F4 F 0.0272(3) -0.4154(3) 0.2266(2) 0.0982(17) Uani 1 1 d . . . F5 F -0.0184(3) -0.3135(3) 0.1960(2) 0.0941(16) Uani 1 1 d . . . F6 F 0.0979(4) -0.2698(4) 0.26535(19) 0.1004(16) Uani 1 1 d . . . S3 S 0.20634(10) 0.19744(11) 0.02418(5) 0.0515(4) Uani 1 1 d . . . N26 N 0.2139(4) 0.2435(4) -0.02464(17) 0.0529(13) Uani 1 1 d . . . S4 S 0.29652(11) 0.34537(12) -0.02826(6) 0.0570(4) Uani 1 1 d . . . O27 O 0.2540(3) 0.2607(3) 0.07104(15) 0.0603(12) Uani 1 1 d . . . O28 O 0.1033(3) 0.1255(3) 0.01748(16) 0.0762(16) Uani 1 1 d . . . O29 O 0.3779(3) 0.3936(4) 0.0144(2) 0.0886(18) Uani 1 1 d . . . O30 O 0.3207(4) 0.3425(4) -0.0762(2) 0.0873(18) Uani 1 1 d . . . C43 C 0.2769(7) 0.1290(6) 0.0209(3) 0.081(2) Uani 1 1 d . . . F7 F 0.2743(4) 0.0817(3) 0.0607(2) 0.117(2) Uani 1 1 d . . . F8 F 0.2402(5) 0.0662(4) -0.0196(2) 0.134(2) Uani 1 1 d . . . F9 F 0.3742(4) 0.1857(4) 0.0245(2) 0.1061(16) Uani 1 1 d . . . C44 C 0.2204(5) 0.4116(5) -0.0361(2) 0.0561(16) Uani 1 1 d . . . F10 F 0.1477(3) 0.3758(3) -0.07744(15) 0.0781(11) Uani 1 1 d . . . F11 F 0.1790(4) 0.4080(4) 0.00256(16) 0.0922(14) Uani 1 1 d . . . F12 F 0.2790(4) 0.5028(3) -0.03731(18) 0.0865(13) Uani 1 1 d . . . S5 S 0.78578(10) 0.33128(10) 0.30479(5) 0.0399(3) Uani 1 1 d . . . N31 N 0.6777(3) 0.3267(3) 0.29924(15) 0.0350(9) Uani 1 1 d . . . S6 S 0.61192(9) 0.29512(9) 0.33900(5) 0.0371(3) Uani 1 1 d . . . O32 O 0.8097(3) 0.2707(4) 0.33543(19) 0.0735(14) Uani 1 1 d . . . O33 O 0.8022(3) 0.3320(3) 0.25534(14) 0.0567(11) Uani 1 1 d . . . O34 O 0.6659(3) 0.3037(3) 0.38939(14) 0.0602(12) Uani 1 1 d . . . O35 O 0.5403(3) 0.3326(3) 0.33101(18) 0.0608(12) Uani 1 1 d . . . C45 C 0.8738(5) 0.4546(6) 0.3362(2) 0.067(2) Uani 1 1 d . . . F13 F 0.9683(3) 0.4676(4) 0.33853(18) 0.1022(17) Uani 1 1 d . . . F14 F 0.8554(4) 0.5171(3) 0.3095(2) 0.1058(16) Uani 1 1 d . . . F15 F 0.8650(3) 0.4718(4) 0.38087(17) 0.116(2) Uani 1 1 d . . . C46 C 0.5342(5) 0.1660(4) 0.3173(2) 0.0528(15) Uani 1 1 d . . . F16 F 0.4705(3) 0.1503(3) 0.27307(15) 0.0878(13) Uani 1 1 d . . . F17 F 0.4786(3) 0.1286(3) 0.34959(17) 0.0838(13) Uani 1 1 d . . . F18 F 0.5891(3) 0.1214(3) 0.31318(17) 0.0756(11) Uani 1 1 d . . . S7 S 0.80854(11) 0.23787(10) 0.01493(5) 0.0423(3) Uani 1 1 d . . . N36 N 0.7199(3) 0.2434(3) 0.03540(17) 0.0434(10) Uani 1 1 d . . . S8 S 0.70133(11) 0.22292(12) 0.08867(6) 0.0544(4) Uani 1 1 d . . . O37 O 0.7789(3) 0.2234(3) -0.03891(14) 0.0563(10) Uani 1 1 d . . . O38 O 0.8544(4) 0.1825(4) 0.03793(16) 0.0674(13) Uani 1 1 d . . . O39 O 0.7831(3) 0.2180(4) 0.12498(15) 0.0711(14) Uani 1 1 d . . . O40 O 0.6517(5) 0.2758(4) 0.1036(2) 0.103(2) Uani 1 1 d . . . C47 C 0.9063(5) 0.3633(6) 0.0308(3) 0.0691(19) Uani 1 1 d . . . F19 F 0.8732(4) 0.4197(3) 0.0080(2) 0.0939(14) Uani 1 1 d . . . F20 F 0.9330(4) 0.3925(4) 0.08018(19) 0.1051(17) Uani 1 1 d . . . F21 F 0.9874(3) 0.3694(4) 0.0167(2) 0.1165(19) Uani 1 1 d . . . C48 C 0.6026(5) 0.1000(6) 0.0744(2) 0.0642(19) Uani 1 1 d . . . F22 F 0.6351(4) 0.0395(3) 0.05801(19) 0.0941(14) Uani 1 1 d . . . F23 F 0.5230(3) 0.0907(3) 0.03940(17) 0.0922(14) Uani 1 1 d . . . F24 F 0.5712(4) 0.0726(4) 0.11565(19) 0.120(2) Uani 1 1 d . . . S9 S 0.76141(10) 0.05264(10) 0.48346(5) 0.0433(3) Uani 1 1 d D . . O42A O 0.6549(5) 0.0230(6) 0.4798(3) 0.0468(18) Uani 0.52 1 d PD B 1 O43A O 0.7916(8) -0.0184(6) 0.4692(3) 0.061(2) Uani 0.52 1 d PD B 1 N41A N 0.8263(7) 0.0958(6) 0.5426(3) 0.044(2) Uani 0.52 1 d PD B 1 O42B O 0.6726(9) -0.0327(7) 0.4568(4) 0.086(4) Uani 0.48 1 d PD B 2 O43B O 0.8556(7) 0.0495(8) 0.4889(3) 0.056(2) Uani 0.48 1 d PD B 2 N41B N 0.7381(7) 0.1081(7) 0.5218(3) 0.046(2) Uani 0.48 1 d PD B 2 S10 S 0.80481(11) 0.15386(12) 0.57987(5) 0.0495(4) Uani 1 1 d D . . O44A O 0.8007(7) 0.1261(7) 0.6281(3) 0.068(2) Uani 0.52 1 d PD B 1 O45A O 0.7378(6) 0.1983(7) 0.5637(3) 0.064(2) Uani 0.52 1 d PD B 1 C49A C 0.8042(8) 0.1451(7) 0.4497(4) 0.043(3) Uiso 0.52 1 d PD B 1 F25A F 0.7648(6) 0.1138(6) 0.4014(3) 0.070(2) Uiso 0.52 1 d PD B 1 F26A F 0.7858(5) 0.2177(5) 0.4605(2) 0.0590(16) Uiso 0.52 1 d PD B 1 F27A F 0.9036(5) 0.1823(5) 0.4548(2) 0.0584(16) Uiso 0.52 1 d PD B 1 C50A C 0.9337(11) 0.2646(10) 0.5982(6) 0.079(5) Uiso 0.52 1 d PD B 1 F28A F 0.9554(7) 0.3021(7) 0.5586(3) 0.086(3) Uiso 0.52 1 d PD B 1 F29A F 0.9292(7) 0.3321(6) 0.6293(3) 0.081(2) Uiso 0.52 1 d PD B 1 F30A F 1.0051(7) 0.2449(6) 0.6223(3) 0.087(2) Uiso 0.52 1 d PD B 1 O44B O 0.8495(7) 0.0875(6) 0.5959(3) 0.053(2) Uani 0.48 1 d PD B 2 O45B O 0.7393(9) 0.1634(10) 0.6062(4) 0.087(3) Uani 0.48 1 d PD B 2 C49B C 0.7692(9) 0.1325(8) 0.4330(5) 0.044(3) Uiso 0.48 1 d PD B 2 F25B F 0.7705(6) 0.0867(6) 0.3903(3) 0.056(2) Uiso 0.48 1 d PD B 2 F26B F 0.6872(6) 0.1467(6) 0.4217(3) 0.077(2) Uiso 0.48 1 d PD B 2 F27B F 0.8526(7) 0.2144(7) 0.4460(3) 0.086(3) Uiso 0.48 1 d PD B 2 C50B C 0.9062(11) 0.2632(10) 0.5819(6) 0.070(5) Uiso 0.48 1 d PD B 2 F28B F 0.8701(11) 0.3213(10) 0.5623(5) 0.142(5) Uiso 0.48 1 d PD B 2 F29B F 0.9698(7) 0.2569(7) 0.5555(3) 0.078(2) Uiso 0.48 1 d PD B 2 F30B F 0.9558(12) 0.2975(12) 0.6306(6) 0.144(5) Uiso 0.48 1 d PD B 2 S11 S 0.75540(13) 0.53410(13) 0.53681(7) 0.0630(5) Uani 1 1 d D . . S12 S 0.66688(14) 0.61840(16) 0.46810(7) 0.0758(5) Uani 1 1 d D . . N46A N 0.6833(6) 0.5336(5) 0.4827(3) 0.051(2) Uani 0.57 1 d PD C 1 O47A O 0.7092(9) 0.4315(7) 0.5399(5) 0.075(4) Uani 0.57 1 d PD C 1 O48A O 0.7763(7) 0.5996(7) 0.5742(3) 0.073(3) Uani 0.57 1 d PD C 1 O49A O 0.5649(11) 0.6020(15) 0.4521(9) 0.113(8) Uani 0.57 1 d PD C 1 O50A O 0.7329(10) 0.7112(6) 0.4997(4) 0.128(5) Uani 0.57 1 d PD C 1 N46B N 0.7412(12) 0.6212(8) 0.5184(4) 0.103(6) Uani 0.43 1 d PD C 2 O47B O 0.6809(11) 0.4473(8) 0.5290(7) 0.066(4) Uani 0.43 1 d PD C 2 O48B O 0.7994(9) 0.5757(8) 0.5963(4) 0.062(3) Uani 0.43 1 d PD C 2 O49B O 0.5747(12) 0.610(2) 0.4719(10) 0.094(8) Uani 0.43 1 d PD C 2 O50B O 0.6466(10) 0.5207(8) 0.4339(4) 0.111(6) Uani 0.43 1 d PD C 2 C51 C 0.8717(5) 0.5460(5) 0.5220(2) 0.073(2) Uani 1 1 d D C . F31A F 0.8552(8) 0.4851(7) 0.4814(3) 0.100(3) Uiso 0.57 1 d PD C 1 F32A F 0.9312(7) 0.5387(7) 0.5580(3) 0.092(2) Uiso 0.57 1 d PD C 1 F33A F 0.9192(6) 0.6413(5) 0.5130(3) 0.088(2) Uiso 0.57 1 d PD C 1 F31B F 0.8621(8) 0.5281(8) 0.4760(4) 0.081(3) Uiso 0.43 1 d PD C 2 F32B F 0.8900(9) 0.4755(8) 0.5486(4) 0.094(3) Uiso 0.43 1 d PD C 2 F33B F 0.9543(10) 0.6249(9) 0.5444(5) 0.115(4) Uiso 0.43 1 d PD C 2 C52A C 0.7066(8) 0.6303(8) 0.4089(4) 0.066(3) Uiso 0.57 1 d PD C 1 F34A F 0.7984(6) 0.6501(5) 0.4115(3) 0.0781(19) Uiso 0.57 1 d PD C 1 F35A F 0.6936(15) 0.6955(13) 0.3835(9) 0.269(13) Uiso 0.57 1 d PD C 1 F36A F 0.6502(7) 0.5527(6) 0.3749(3) 0.107(3) Uiso 0.57 1 d PD C 1 C52B C 0.7393(15) 0.7118(14) 0.4423(7) 0.155(11) Uiso 0.43 1 d PD C 2 F34B F 0.8227(9) 0.7054(9) 0.4437(4) 0.101(3) Uiso 0.43 1 d PD C 2 F35B F 0.7427(10) 0.7787(10) 0.4740(5) 0.122(4) Uiso 0.43 1 d PD C 2 F36B F 0.6928(7) 0.7092(7) 0.3956(4) 0.065(3) Uiso 0.43 1 d PD C 2 S13A S 0.69268(18) 0.92086(19) 0.19843(10) 0.0486(5) Uani 0.57 1 d PD D 1 N51A N 0.7792(8) 0.8974(8) 0.2302(6) 0.053(4) Uani 0.57 1 d PD D 1 S14A S 0.7590(2) 0.8189(2) 0.26572(10) 0.0526(5) Uani 0.57 1 d PD D 1 O52A O 0.5918(10) 0.864(3) 0.2040(13) 0.058(6) Uani 0.57 1 d PD D 1 O53A O 0.7115(6) 0.9421(7) 0.1505(3) 0.057(2) Uani 0.57 1 d PD D 1 O54A O 0.8543(9) 0.8418(10) 0.2986(5) 0.089(4) Uani 0.57 1 d PD D 1 O55A O 0.6771(7) 0.8020(7) 0.2891(3) 0.073(2) Uani 0.57 1 d PD D 1 C53A C 0.7323(7) 1.0388(7) 0.2351(4) 0.053(3) Uiso 0.57 1 d PD D 1 F37A F 0.6685(6) 1.0752(5) 0.2155(3) 0.0685(19) Uiso 0.57 1 d PD D 1 F38A F 0.8242(5) 1.1006(5) 0.2321(2) 0.0653(17) Uiso 0.57 1 d PD D 1 F39A F 0.7297(5) 1.0296(5) 0.2837(3) 0.0703(18) Uiso 0.57 1 d PD D 1 C54A C 0.7261(10) 0.7090(9) 0.2276(5) 0.079(4) Uiso 0.57 1 d PD D 1 F40A F 0.7141(8) 0.6388(7) 0.2566(4) 0.103(3) Uiso 0.57 1 d PD D 1 F41A F 0.6370(7) 0.6784(7) 0.1937(3) 0.105(3) Uiso 0.57 1 d PD D 1 F42A F 0.7943(8) 0.7130(9) 0.2033(4) 0.121(4) Uiso 0.57 1 d PD D 1 S13B S 0.6979(2) 0.9219(3) 0.23869(13) 0.0486(5) Uani 0.43 1 d PD E 2 N51B N 0.7427(14) 0.8555(13) 0.2170(6) 0.062(5) Uani 0.43 1 d PD E 2 S14B S 0.8147(3) 0.8160(3) 0.24513(14) 0.0526(5) Uani 0.43 1 d PD E 2 O52B O 0.7278(8) 0.9563(11) 0.2901(4) 0.091(4) Uani 0.43 1 d PD E 2 O53B O 0.5915(14) 0.880(4) 0.2148(18) 0.083(16) Uani 0.43 1 d PD E 2 O54B O 0.8858(12) 0.8832(11) 0.2885(6) 0.086(5) Uani 0.43 1 d PD E 2 O55B O 0.8517(16) 0.7763(13) 0.2109(6) 0.123(7) Uani 0.43 1 d PD E 2 C53B C 0.7494(9) 1.0218(8) 0.2067(4) 0.046(3) Uiso 0.43 1 d PD E 2 F37B F 0.7266(7) 0.9991(7) 0.1587(3) 0.063(3) Uiso 0.43 1 d PD E 2 F38B F 0.8508(8) 1.0624(8) 0.2226(4) 0.093(3) Uiso 0.43 1 d PD E 2 F39B F 0.7199(10) 1.0866(9) 0.2170(5) 0.101(4) Uiso 0.43 1 d PD E 2 C54B C 0.7388(11) 0.7149(11) 0.2690(6) 0.081(5) Uiso 0.43 1 d PD E 2 F40B F 0.6870(8) 0.7339(8) 0.2975(4) 0.093(3) Uiso 0.43 1 d PD E 2 F41B F 0.7987(9) 0.6800(9) 0.2948(4) 0.107(4) Uiso 0.43 1 d PD E 2 F42B F 0.6716(9) 0.6424(8) 0.2287(4) 0.096(3) Uiso 0.43 1 d PD E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0184(3) 0.0203(3) 0.0339(3) 0.0089(2) 0.0113(3) 0.0118(2) Fe2 0.0172(3) 0.0198(3) 0.0323(3) 0.0084(2) 0.0085(2) 0.0104(2) Fe3 0.0169(3) 0.0200(3) 0.0344(3) 0.0080(2) 0.0106(2) 0.0095(2) O1 0.0179(14) 0.0221(14) 0.0330(16) 0.0079(12) 0.0097(12) 0.0117(12) O2 0.0275(16) 0.0299(16) 0.0363(17) 0.0131(13) 0.0173(14) 0.0175(14) O3 0.0236(15) 0.0331(17) 0.0470(19) 0.0200(15) 0.0152(14) 0.0173(14) C1 0.017(2) 0.022(2) 0.032(2) 0.0054(18) 0.0085(17) 0.0073(18) C2 0.031(2) 0.039(3) 0.042(3) 0.016(2) 0.019(2) 0.024(2) N1 0.0253(19) 0.038(2) 0.031(2) 0.0117(17) 0.0124(16) 0.0197(17) C3 0.029(2) 0.039(3) 0.041(3) 0.015(2) 0.016(2) 0.018(2) N2 0.045(3) 0.050(3) 0.041(2) 0.025(2) 0.023(2) 0.034(2) C4 0.048(3) 0.079(4) 0.036(3) 0.024(3) 0.010(3) 0.039(3) C5 0.031(3) 0.056(3) 0.038(3) 0.006(2) 0.005(2) 0.018(2) C6 0.080(4) 0.060(4) 0.083(5) 0.047(4) 0.049(4) 0.049(4) O4 0.0316(17) 0.0245(16) 0.0391(18) 0.0028(14) 0.0014(14) 0.0147(14) O5 0.0335(18) 0.0285(17) 0.047(2) -0.0009(15) 0.0021(15) 0.0200(15) C7 0.026(2) 0.029(2) 0.040(3) 0.003(2) 0.009(2) 0.013(2) C8 0.054(3) 0.034(3) 0.053(3) -0.010(2) -0.017(3) 0.028(3) N3 0.038(2) 0.028(2) 0.035(2) -0.0008(17) 0.0014(18) 0.0179(18) C9 0.034(3) 0.033(3) 0.030(2) 0.005(2) 0.002(2) 0.013(2) N4 0.034(2) 0.041(2) 0.027(2) 0.0026(17) 0.0056(17) 0.0204(19) C10 0.051(3) 0.035(3) 0.047(3) 0.014(2) 0.019(3) 0.020(2) C11 0.053(3) 0.035(3) 0.047(3) 0.006(2) 0.021(3) 0.022(3) C12 0.052(3) 0.064(4) 0.042(3) 0.001(3) 0.009(3) 0.042(3) O6 0.0245(16) 0.0266(16) 0.0417(18) 0.0052(14) 0.0115(14) 0.0137(14) O7 0.0266(16) 0.0202(15) 0.054(2) 0.0012(14) 0.0178(15) 0.0109(13) C13 0.023(2) 0.022(2) 0.029(2) 0.0102(17) 0.0081(18) 0.0124(18) C14 0.032(2) 0.029(2) 0.038(3) 0.006(2) 0.014(2) 0.014(2) N5 0.038(2) 0.027(2) 0.034(2) 0.0010(17) 0.0132(18) 0.0115(18) C15 0.048(3) 0.027(3) 0.042(3) 0.003(2) 0.006(2) 0.009(2) N6 0.056(3) 0.032(2) 0.050(3) 0.006(2) 0.003(2) 0.000(2) C16 0.043(3) 0.051(4) 0.063(4) 0.008(3) -0.003(3) 0.006(3) C17 0.044(3) 0.045(3) 0.060(4) 0.009(3) -0.003(3) 0.017(3) C18 0.081(5) 0.043(4) 0.108(6) 0.023(4) 0.004(5) -0.017(4) O8 0.0249(16) 0.0353(18) 0.0398(18) 0.0160(15) 0.0121(14) 0.0145(14) O9 0.0289(17) 0.0434(19) 0.046(2) 0.0241(16) 0.0171(15) 0.0182(15) C19 0.035(3) 0.026(2) 0.030(2) 0.0087(19) 0.014(2) 0.018(2) C20 0.042(3) 0.037(3) 0.032(3) 0.011(2) 0.014(2) 0.009(2) N7 0.043(2) 0.040(2) 0.037(2) 0.0155(18) 0.0243(19) 0.028(2) C21 0.030(2) 0.037(3) 0.026(2) 0.0089(19) 0.0063(19) 0.015(2) N8 0.033(2) 0.061(3) 0.048(3) 0.029(2) 0.019(2) 0.018(2) C22 0.079(5) 0.168(9) 0.152(8) 0.120(7) 0.089(6) 0.094(6) C23 0.107(6) 0.129(7) 0.167(8) 0.111(7) 0.114(7) 0.103(6) C24 0.055(4) 0.067(4) 0.073(4) 0.032(4) 0.019(3) 0.003(3) O10 0.0332(17) 0.0291(17) 0.0331(17) 0.0074(14) 0.0061(14) 0.0144(14) O11 0.0249(16) 0.0274(17) 0.0448(19) 0.0093(15) 0.0007(14) 0.0125(14) C25 0.022(2) 0.034(3) 0.037(3) 0.008(2) 0.0112(19) 0.021(2) C26 0.065(4) 0.039(3) 0.035(3) 0.009(2) 0.016(3) 0.033(3) N9 0.036(2) 0.041(2) 0.033(2) 0.0132(18) 0.0155(18) 0.0222(19) C27 0.032(3) 0.051(3) 0.034(3) 0.010(2) 0.012(2) 0.023(2) N10 0.048(3) 0.060(3) 0.050(3) 0.025(2) 0.023(2) 0.039(2) C28 0.051(4) 0.052(4) 0.074(4) 0.038(3) 0.027(3) 0.020(3) C29 0.029(3) 0.055(3) 0.064(4) 0.031(3) 0.017(3) 0.010(3) C30 0.085(5) 0.104(6) 0.078(5) 0.046(4) 0.025(4) 0.072(5) O12 0.0250(16) 0.0303(18) 0.0436(19) 0.0055(14) 0.0176(14) 0.0152(14) O13 0.0344(18) 0.0296(17) 0.054(2) 0.0160(15) 0.0286(16) 0.0195(15) C31 0.029(2) 0.034(3) 0.034(2) 0.010(2) 0.015(2) 0.021(2) C32 0.038(3) 0.030(2) 0.058(3) 0.013(2) 0.029(2) 0.021(2) N11 0.0234(19) 0.033(2) 0.034(2) 0.0092(16) 0.0133(16) 0.0181(17) C33 0.035(3) 0.045(3) 0.031(3) 0.011(2) 0.007(2) 0.024(2) N12 0.024(2) 0.040(2) 0.046(2) 0.0127(19) 0.0104(18) 0.0111(18) C34 0.038(3) 0.047(3) 0.047(3) 0.024(2) 0.019(2) 0.021(2) C35 0.030(3) 0.047(3) 0.039(3) 0.015(2) 0.007(2) 0.022(2) C36 0.029(3) 0.070(4) 0.096(5) 0.019(4) 0.007(3) 0.004(3) O14 0.0367(18) 0.0264(17) 0.050(2) 0.0156(15) 0.0207(16) 0.0212(15) O15 0.0232(16) 0.0323(17) 0.0332(18) 0.0081(14) 0.0090(13) 0.0147(14) O16 0.0226(16) 0.0326(18) 0.064(2) 0.0175(17) 0.0134(16) 0.0120(15) O61 0.041(2) 0.043(2) 0.158(5) 0.048(3) 0.037(3) 0.021(2) O62 0.122(5) 0.101(4) 0.141(5) 0.091(4) 0.093(5) 0.074(4) S1 0.0461(7) 0.0300(6) 0.0426(7) 0.0060(5) 0.0184(6) 0.0173(6) N21 0.034(2) 0.033(2) 0.057(3) 0.014(2) 0.008(2) 0.0150(19) S2 0.0352(7) 0.0316(7) 0.0606(9) 0.0071(6) 0.0087(6) 0.0152(6) O22 0.084(3) 0.043(2) 0.092(3) 0.020(2) 0.052(3) 0.041(2) O23 0.078(3) 0.048(2) 0.039(2) 0.0070(18) 0.000(2) 0.005(2) O24 0.030(2) 0.039(2) 0.121(4) 0.024(2) 0.005(2) 0.0191(17) O25 0.106(4) 0.053(3) 0.069(3) -0.010(2) 0.008(3) 0.019(3) C41 0.039(3) 0.041(3) 0.051(3) -0.003(3) 0.013(3) 0.014(3) F1 0.047(2) 0.069(2) 0.087(3) -0.019(2) 0.022(2) -0.0107(19) F2 0.072(2) 0.088(3) 0.057(2) 0.025(2) 0.0299(19) 0.029(2) F3 0.057(2) 0.072(2) 0.111(3) -0.006(2) 0.032(2) 0.039(2) C42 0.044(3) 0.052(4) 0.105(6) 0.044(4) 0.026(4) 0.025(3) F4 0.060(2) 0.070(3) 0.182(5) 0.085(3) 0.043(3) 0.031(2) F5 0.039(2) 0.088(3) 0.178(5) 0.079(3) 0.037(3) 0.038(2) F6 0.121(4) 0.114(4) 0.088(3) 0.035(3) 0.063(3) 0.055(3) S3 0.0357(7) 0.0577(9) 0.0430(8) 0.0246(7) 0.0000(6) 0.0061(6) N26 0.041(3) 0.065(3) 0.044(3) 0.030(2) 0.010(2) 0.014(2) S4 0.0400(8) 0.0680(10) 0.0733(10) 0.0418(9) 0.0254(8) 0.0248(7) O27 0.040(2) 0.077(3) 0.045(2) 0.014(2) 0.0029(18) 0.012(2) O28 0.041(2) 0.084(3) 0.058(3) 0.041(2) -0.007(2) -0.010(2) O29 0.045(3) 0.078(3) 0.109(4) 0.047(3) -0.004(3) 0.002(2) O30 0.104(4) 0.101(4) 0.124(4) 0.076(3) 0.097(4) 0.071(3) C43 0.080(6) 0.067(5) 0.081(5) 0.013(4) -0.008(4) 0.030(4) F7 0.133(4) 0.085(3) 0.111(4) 0.045(3) -0.021(3) 0.045(3) F8 0.179(6) 0.106(4) 0.110(4) -0.018(3) -0.020(4) 0.086(4) F9 0.079(3) 0.114(4) 0.142(5) 0.020(3) 0.018(3) 0.062(3) C44 0.060(4) 0.074(4) 0.048(4) 0.018(3) 0.030(3) 0.034(3) F10 0.078(3) 0.108(3) 0.063(2) 0.022(2) 0.005(2) 0.060(3) F11 0.104(3) 0.125(4) 0.082(3) 0.021(3) 0.063(3) 0.065(3) F12 0.108(3) 0.064(3) 0.104(3) 0.028(2) 0.047(3) 0.043(2) S5 0.0357(7) 0.0637(9) 0.0381(7) 0.0139(6) 0.0168(5) 0.0347(6) N31 0.029(2) 0.051(3) 0.038(2) 0.0131(19) 0.0123(18) 0.0279(19) S6 0.0309(6) 0.0468(7) 0.0412(7) 0.0035(6) 0.0146(5) 0.0224(6) O32 0.063(3) 0.118(4) 0.091(3) 0.058(3) 0.038(3) 0.074(3) O33 0.049(2) 0.087(3) 0.043(2) 0.008(2) 0.0259(19) 0.032(2) O34 0.049(2) 0.094(3) 0.033(2) -0.001(2) 0.0156(18) 0.027(2) O35 0.040(2) 0.061(3) 0.104(3) 0.016(2) 0.034(2) 0.035(2) C45 0.036(3) 0.097(6) 0.050(4) -0.008(4) 0.010(3) 0.016(3) F13 0.0317(19) 0.147(4) 0.099(3) -0.011(3) 0.016(2) 0.018(2) F14 0.091(3) 0.065(3) 0.134(4) 0.011(3) 0.014(3) 0.016(3) F15 0.067(3) 0.153(5) 0.074(3) -0.049(3) 0.019(2) 0.009(3) C46 0.061(4) 0.047(3) 0.051(4) 0.013(3) 0.020(3) 0.022(3) F16 0.087(3) 0.070(3) 0.066(3) -0.006(2) -0.016(2) 0.015(2) F17 0.083(3) 0.069(3) 0.095(3) 0.021(2) 0.055(3) 0.015(2) F18 0.097(3) 0.052(2) 0.103(3) 0.023(2) 0.047(3) 0.046(2) S7 0.0478(8) 0.0540(8) 0.0436(7) 0.0153(6) 0.0177(6) 0.0359(7) N36 0.037(2) 0.050(3) 0.049(3) 0.007(2) 0.013(2) 0.025(2) S8 0.0419(8) 0.0676(10) 0.0460(8) -0.0089(7) 0.0151(7) 0.0181(7) O37 0.075(3) 0.075(3) 0.041(2) 0.015(2) 0.019(2) 0.050(2) O38 0.087(3) 0.097(3) 0.064(3) 0.037(3) 0.029(2) 0.075(3) O39 0.046(2) 0.103(4) 0.036(2) -0.003(2) 0.0014(19) 0.013(2) O40 0.110(5) 0.103(4) 0.116(5) -0.015(3) 0.057(4) 0.057(4) C47 0.041(3) 0.084(5) 0.080(5) 0.015(4) 0.022(3) 0.022(4) F19 0.089(3) 0.058(2) 0.130(4) 0.034(3) 0.026(3) 0.026(2) F20 0.077(3) 0.095(3) 0.087(3) -0.016(3) 0.002(2) -0.002(3) F21 0.050(2) 0.144(5) 0.153(5) 0.039(4) 0.048(3) 0.029(3) C48 0.041(3) 0.084(5) 0.055(4) 0.017(4) 0.006(3) 0.017(3) F22 0.088(3) 0.066(3) 0.113(4) 0.019(3) 0.007(3) 0.028(3) F23 0.048(2) 0.097(3) 0.095(3) 0.020(3) -0.009(2) 0.011(2) F24 0.069(3) 0.168(5) 0.093(3) 0.059(3) 0.029(3) 0.015(3) S9 0.0396(7) 0.0418(7) 0.0520(8) 0.0117(6) 0.0103(6) 0.0214(6) O42A 0.027(4) 0.053(5) 0.058(5) 0.017(4) 0.010(3) 0.014(3) O43A 0.074(6) 0.051(5) 0.063(6) 0.006(4) 0.012(5) 0.037(5) N41A 0.046(5) 0.049(5) 0.049(5) 0.005(4) 0.007(4) 0.034(4) O42B 0.088(8) 0.055(6) 0.056(6) 0.015(5) -0.005(6) -0.012(6) O43B 0.067(6) 0.095(7) 0.038(5) 0.015(5) 0.015(4) 0.065(6) N41B 0.045(5) 0.070(7) 0.036(5) 0.006(5) 0.008(4) 0.040(5) S10 0.0463(8) 0.0788(10) 0.0399(7) 0.0202(7) 0.0168(6) 0.0389(8) O44A 0.088(6) 0.091(6) 0.034(4) 0.027(4) 0.022(4) 0.043(6) O45A 0.063(5) 0.111(7) 0.052(5) 0.013(5) 0.015(4) 0.071(5) O44B 0.065(5) 0.067(5) 0.040(4) 0.019(4) 0.011(4) 0.040(5) O45B 0.096(8) 0.148(11) 0.062(7) 0.016(7) 0.039(6) 0.089(8) S11 0.0536(9) 0.0661(11) 0.0785(12) 0.0302(10) 0.0272(9) 0.0281(9) S12 0.0616(11) 0.1083(16) 0.0527(10) -0.0084(10) -0.0062(8) 0.0452(11) N46A 0.049(5) 0.052(5) 0.047(5) 0.005(4) -0.003(4) 0.025(4) O47A 0.048(7) 0.080(7) 0.079(7) 0.039(6) 0.000(5) 0.017(5) O48A 0.070(6) 0.107(8) 0.047(6) 0.012(5) 0.010(5) 0.047(6) O49A 0.058(8) 0.096(11) 0.17(2) -0.011(11) -0.018(9) 0.041(7) O50A 0.194(13) 0.066(6) 0.092(7) -0.033(6) -0.048(8) 0.069(8) N46B 0.137(14) 0.042(7) 0.065(9) -0.015(6) -0.063(9) 0.021(8) O47B 0.050(9) 0.052(7) 0.079(11) 0.010(7) -0.006(7) 0.015(6) O48B 0.082(9) 0.069(7) 0.060(8) 0.024(6) 0.026(7) 0.051(6) O49B 0.033(8) 0.138(17) 0.108(16) -0.017(11) 0.014(8) 0.041(10) O50B 0.117(11) 0.064(7) 0.066(8) 0.002(6) -0.038(7) -0.012(7) C51 0.062(4) 0.097(6) 0.048(4) -0.006(4) -0.003(3) 0.032(4) S13A 0.0321(9) 0.0641(13) 0.0491(11) 0.0222(11) 0.0122(9) 0.0185(9) N51A 0.025(5) 0.061(7) 0.070(9) 0.022(6) 0.012(5) 0.015(5) S14A 0.0538(13) 0.0579(12) 0.0549(13) 0.0191(10) 0.0165(10) 0.0306(11) O52A 0.031(7) 0.041(8) 0.085(8) 0.031(8) 0.009(5) 0.002(5) O53A 0.059(5) 0.069(6) 0.037(4) 0.011(4) 0.015(3) 0.020(4) O54A 0.069(8) 0.102(10) 0.083(7) 0.034(7) -0.010(6) 0.036(7) O55A 0.091(6) 0.098(6) 0.065(5) 0.044(5) 0.046(5) 0.059(5) S13B 0.0321(9) 0.0641(13) 0.0491(11) 0.0222(11) 0.0122(9) 0.0185(9) N51B 0.074(13) 0.103(15) 0.053(10) 0.036(11) 0.031(10) 0.070(12) S14B 0.0538(13) 0.0579(12) 0.0549(13) 0.0191(10) 0.0165(10) 0.0306(11) O52B 0.050(6) 0.137(12) 0.067(8) 0.025(8) 0.015(6) 0.023(7) O53B 0.031(10) 0.07(2) 0.15(3) 0.04(2) 0.020(11) 0.016(10) O54B 0.069(10) 0.075(11) 0.120(14) 0.024(9) 0.028(9) 0.034(8) O55B 0.192(17) 0.136(14) 0.169(15) 0.089(12) 0.148(15) 0.140(14) _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 1.918(3) . ? Fe1 O13 2.004(3) . ? Fe1 O4 2.008(3) . ? Fe1 O11 2.013(3) . ? Fe1 O14 2.019(3) . ? Fe1 O2 2.028(3) . ? Fe2 O1 1.908(3) . ? Fe2 O5 2.006(3) . ? Fe2 O8 2.008(3) . ? Fe2 O3 2.013(3) . ? Fe2 O6 2.014(3) . ? Fe2 O15 2.069(3) . ? Fe3 O1 1.915(3) . ? Fe3 O10 2.005(3) . ? Fe3 O7 2.011(3) . ? Fe3 O9 2.012(3) . ? Fe3 O12 2.015(3) . ? Fe3 O16 2.041(3) . ? O2 C1 1.256(5) . ? O3 C1 1.247(5) . ? C1 C2 1.516(6) . ? C2 N1 1.457(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 C3 1.326(6) . ? N1 C5 1.370(6) . ? C3 N2 1.314(6) . ? C3 H3A 0.9500 . ? N2 C4 1.351(7) . ? N2 C6 1.490(7) . ? C4 C5 1.338(8) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O4 C7 1.247(6) . ? O5 C7 1.254(6) . ? C7 C8 1.530(7) . ? C8 N3 1.458(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N3 C9 1.313(6) . ? N3 C11 1.385(6) . ? C9 N4 1.324(6) . ? C9 H9A 0.9500 . ? N4 C10 1.368(6) . ? N4 C12 1.469(6) . ? C10 C11 1.327(7) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O6 C13 1.251(5) . ? O7 C13 1.242(5) . ? C13 C14 1.505(6) . ? C14 N5 1.456(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? N5 C15 1.323(6) . ? N5 C17 1.370(7) . ? C15 N6 1.315(7) . ? C15 H15A 0.9500 . ? N6 C16 1.353(8) . ? N6 C18 1.478(7) . ? C16 C17 1.350(8) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O8 C19 1.251(5) . ? O9 C19 1.242(6) . ? C19 C20 1.506(6) . ? C20 N7 1.456(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N7 C21 1.318(6) . ? N7 C23 1.353(8) . ? C21 N8 1.312(6) . ? C21 H21A 0.9500 . ? N8 C22 1.349(9) . ? N8 C24 1.485(7) . ? C22 C23 1.328(10) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O10 C25 1.256(5) . ? O11 C25 1.251(5) . ? C25 C26 1.502(7) . ? C26 N9 1.461(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N9 C27 1.322(6) . ? N9 C29 1.381(6) . ? C27 N10 1.323(7) . ? C27 H27A 0.9500 . ? N10 C28 1.368(8) . ? N10 C30 1.476(8) . ? C28 C29 1.345(8) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? O12 C31 1.248(5) . ? O13 C31 1.246(5) . ? C31 C32 1.528(6) . ? C32 N11 1.447(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? N11 C33 1.327(6) . ? N11 C35 1.369(6) . ? C33 N12 1.314(6) . ? C33 H33A 0.9500 . ? N12 C34 1.370(7) . ? N12 C36 1.470(7) . ? C34 C35 1.322(7) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O14 H141 0.84(4) . ? O14 H142 0.88(3) . ? O15 H151 0.88(3) . ? O15 H152 0.86(3) . ? O16 H161 0.87(4) . ? O16 H162 0.91(4) . ? O61 H611 0.93(4) . ? O61 H612 0.89(3) . ? O62 H621 0.91(4) . ? O62 H622 0.89(4) . ? S1 O23 1.418(4) . ? S1 O22 1.430(4) . ? S1 N21 1.565(4) . ? S1 C41 1.829(5) . ? N21 S2 1.566(4) . ? S2 O24 1.415(4) . ? S2 O25 1.427(5) . ? S2 C42 1.817(7) . ? C41 F1 1.305(6) . ? C41 F2 1.308(7) . ? C41 F3 1.326(7) . ? C42 F5 1.316(7) . ? C42 F4 1.315(7) . ? C42 F6 1.329(9) . ? S3 O27 1.420(4) . ? S3 O28 1.436(4) . ? S3 N26 1.559(4) . ? S3 C43 1.800(9) . ? N26 S4 1.567(5) . ? S4 O29 1.402(5) . ? S4 O30 1.433(5) . ? S4 C44 1.826(7) . ? C43 F8 1.287(9) . ? C43 F9 1.321(9) . ? C43 F7 1.351(9) . ? C44 F10 1.304(7) . ? C44 F11 1.322(6) . ? C44 F12 1.321(7) . ? S5 O32 1.411(4) . ? S5 O33 1.425(4) . ? S5 N31 1.564(4) . ? S5 C45 1.833(7) . ? N31 S6 1.574(4) . ? S6 O35 1.411(4) . ? S6 O34 1.423(4) . ? S6 C46 1.826(6) . ? C45 F15 1.282(7) . ? C45 F13 1.328(7) . ? C45 F14 1.339(9) . ? C46 F18 1.298(7) . ? C46 F16 1.323(7) . ? C46 F17 1.325(6) . ? S7 O38 1.418(4) . ? S7 O37 1.430(4) . ? S7 N36 1.570(4) . ? S7 C47 1.833(7) . ? N36 S8 1.567(5) . ? S8 O40 1.412(5) . ? S8 O39 1.450(5) . ? S8 C48 1.809(7) . ? C47 F19 1.311(9) . ? C47 F21 1.314(8) . ? C47 F20 1.324(8) . ? C48 F23 1.321(8) . ? C48 F22 1.321(9) . ? C48 F24 1.336(7) . ? S9 O43B 1.410(8) . ? S9 O43A 1.421(8) . ? S9 O42A 1.438(7) . ? S9 O42B 1.436(9) . ? S9 N41B 1.503(8) . ? S9 N41A 1.648(8) . ? S9 C49A 1.718(10) . ? S9 C49B 1.904(11) . ? N41A S10 1.492(8) . ? N41B S10 1.633(8) . ? S10 O45B 1.376(8) . ? S10 O44A 1.421(7) . ? S10 O45A 1.460(7) . ? S10 O44B 1.495(8) . ? S10 C50B 1.721(13) . ? S10 C50A 1.905(14) . ? C49A F26A 1.301(11) . ? C49A F25A 1.307(12) . ? C49A F27A 1.320(12) . ? C50A F28A 1.297(14) . ? C50A F30A 1.302(15) . ? C50A F29A 1.345(15) . ? C49B F27B 1.313(12) . ? C49B F26B 1.319(12) . ? C49B F25B 1.342(13) . ? C50B F28B 1.326(15) . ? C50B F29B 1.335(14) . ? C50B F30B 1.343(16) . ? S11 O48A 1.288(8) . ? S11 O47B 1.305(11) . ? S11 O47A 1.462(9) . ? S11 N46B 1.557(10) . ? S11 O48B 1.612(10) . ? S11 N46A 1.651(7) . ? S11 C51 1.799(7) . ? S12 O49B 1.355(13) . ? S12 O49A 1.405(11) . ? S12 O50A 1.452(8) . ? S12 N46A 1.505(7) . ? S12 N46B 1.577(9) . ? S12 O50B 1.614(11) . ? S12 C52B 1.697(18) . ? S12 C52A 1.830(11) . ? C51 F32A 1.238(9) . ? C51 F31B 1.243(10) . ? C51 F33B 1.315(12) . ? C51 F31A 1.329(10) . ? C51 F33A 1.409(10) . ? C51 F32B 1.445(11) . ? C52A F34A 1.259(11) . ? C52A F36A 1.312(12) . ? C52A F35A 1.325(16) . ? C52B F34B 1.285(17) . ? C52B F35B 1.292(17) . ? C52B F36B 1.322(17) . ? S13A O52A 1.434(15) . ? S13A O53A 1.429(7) . ? S13A N51A 1.601(11) . ? S13A C53A 1.828(10) . ? N51A S14A 1.575(12) . ? S14A O55A 1.427(8) . ? S14A O54A 1.413(11) . ? S14A C54A 1.767(12) . ? C53A F38A 1.324(10) . ? C53A F37A 1.348(12) . ? C53A F39A 1.356(11) . ? C54A F42A 1.308(13) . ? C54A F41A 1.336(13) . ? C54A F40A 1.361(13) . ? S13B O52B 1.388(11) . ? S13B O53B 1.429(19) . ? S13B N51B 1.593(14) . ? S13B C53B 1.790(11) . ? N51B S14B 1.558(13) . ? S14B O55B 1.412(10) . ? S14B O54B 1.428(15) . ? S14B C54B 1.759(14) . ? C53B F37B 1.277(12) . ? C53B F39B 1.298(14) . ? C53B F38B 1.334(13) . ? C54B F40B 1.307(14) . ? C54B F41B 1.345(15) . ? C54B F42B 1.396(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O13 95.35(12) . . ? O1 Fe1 O4 94.14(12) . . ? O13 Fe1 O4 89.04(14) . . ? O1 Fe1 O11 93.41(13) . . ? O13 Fe1 O11 91.84(14) . . ? O4 Fe1 O11 172.29(12) . . ? O1 Fe1 O14 178.80(13) . . ? O13 Fe1 O14 83.85(13) . . ? O4 Fe1 O14 86.76(14) . . ? O11 Fe1 O14 85.72(14) . . ? O1 Fe1 O2 95.56(12) . . ? O13 Fe1 O2 168.96(12) . . ? O4 Fe1 O2 91.84(13) . . ? O11 Fe1 O2 85.85(13) . . ? O14 Fe1 O2 85.20(12) . . ? O1 Fe2 O5 94.31(13) . . ? O1 Fe2 O8 95.57(12) . . ? O5 Fe2 O8 87.55(13) . . ? O1 Fe2 O3 93.78(12) . . ? O5 Fe2 O3 93.19(14) . . ? O8 Fe2 O3 170.54(13) . . ? O1 Fe2 O6 96.07(13) . . ? O5 Fe2 O6 169.61(13) . . ? O8 Fe2 O6 92.01(13) . . ? O3 Fe2 O6 85.56(13) . . ? O1 Fe2 O15 176.10(13) . . ? O5 Fe2 O15 82.10(13) . . ? O8 Fe2 O15 85.83(12) . . ? O3 Fe2 O15 84.93(12) . . ? O6 Fe2 O15 87.51(13) . . ? O1 Fe3 O10 94.93(12) . . ? O1 Fe3 O7 94.24(12) . . ? O10 Fe3 O7 87.19(14) . . ? O1 Fe3 O9 94.76(13) . . ? O10 Fe3 O9 169.73(13) . . ? O7 Fe3 O9 88.72(14) . . ? O1 Fe3 O12 95.74(12) . . ? O10 Fe3 O12 93.54(13) . . ? O7 Fe3 O12 169.90(12) . . ? O9 Fe3 O12 88.85(14) . . ? O1 Fe3 O16 178.48(14) . . ? O10 Fe3 O16 85.89(14) . . ? O7 Fe3 O16 84.53(13) . . ? O9 Fe3 O16 84.35(14) . . ? O12 Fe3 O16 85.47(14) . . ? Fe2 O1 Fe3 119.69(14) . . ? Fe2 O1 Fe1 120.70(14) . . ? Fe3 O1 Fe1 119.61(15) . . ? C1 O2 Fe1 128.3(3) . . ? C1 O3 Fe2 134.6(3) . . ? O3 C1 O2 127.1(4) . . ? O3 C1 C2 114.3(4) . . ? O2 C1 C2 118.6(4) . . ? N1 C2 C1 113.9(4) . . ? N1 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C3 N1 C5 107.6(4) . . ? C3 N1 C2 126.1(4) . . ? C5 N1 C2 126.3(4) . . ? N2 C3 N1 108.9(4) . . ? N2 C3 H3A 125.6 . . ? N1 C3 H3A 125.6 . . ? C3 N2 C4 108.9(4) . . ? C3 N2 C6 125.0(5) . . ? C4 N2 C6 126.0(5) . . ? C5 C4 N2 107.3(5) . . ? C5 C4 H4A 126.4 . . ? N2 C4 H4A 126.4 . . ? C4 C5 N1 107.3(5) . . ? C4 C5 H5A 126.3 . . ? N1 C5 H5A 126.3 . . ? 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 . . ? C7 O4 Fe1 133.9(3) . . ? C7 O5 Fe2 129.7(3) . . ? O4 C7 O5 127.0(4) . . ? O4 C7 C8 118.5(4) . . ? O5 C7 C8 114.5(4) . . ? N3 C8 C7 111.5(4) . . ? N3 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N3 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C9 N3 C11 108.0(4) . . ? C9 N3 C8 125.3(4) . . ? C11 N3 C8 126.6(5) . . ? N3 C9 N4 109.2(4) . . ? N3 C9 H9A 125.4 . . ? N4 C9 H9A 125.4 . . ? C9 N4 C10 108.0(4) . . ? C9 N4 C12 125.3(4) . . ? C10 N4 C12 126.6(4) . . ? C11 C10 N4 107.8(4) . . ? C11 C10 H10A 126.1 . . ? N4 C10 H10A 126.1 . . ? C10 C11 N3 107.0(4) . . ? C10 C11 H11A 126.5 . . ? N3 C11 H11A 126.5 . . ? 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 . . ? C13 O6 Fe2 127.6(3) . . ? C13 O7 Fe3 134.8(3) . . ? O7 C13 O6 126.4(4) . . ? O7 C13 C14 117.3(4) . . ? O6 C13 C14 116.4(4) . . ? N5 C14 C13 112.7(4) . . ? N5 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? N5 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C15 N5 C17 108.4(4) . . ? C15 N5 C14 124.6(5) . . ? C17 N5 C14 126.6(4) . . ? N6 C15 N5 108.8(5) . . ? N6 C15 H15A 125.6 . . ? N5 C15 H15A 125.6 . . ? C15 N6 C16 108.8(5) . . ? C15 N6 C18 125.7(6) . . ? C16 N6 C18 125.5(6) . . ? C17 C16 N6 107.5(5) . . ? C17 C16 H16A 126.3 . . ? N6 C16 H16A 126.3 . . ? C16 C17 N5 106.5(5) . . ? C16 C17 H17A 126.8 . . ? N5 C17 H17A 126.8 . . ? 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 . . ? C19 O8 Fe2 132.8(3) . . ? C19 O9 Fe3 130.4(3) . . ? O9 C19 O8 126.9(4) . . ? O9 C19 C20 118.7(4) . . ? O8 C19 C20 114.4(4) . . ? N7 C20 C19 114.0(4) . . ? N7 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? N7 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C21 N7 C23 107.8(5) . . ? C21 N7 C20 125.2(4) . . ? C23 N7 C20 126.9(5) . . ? N8 C21 N7 109.5(5) . . ? N8 C21 H21A 125.3 . . ? N7 C21 H21A 125.3 . . ? C21 N8 C22 107.4(5) . . ? C21 N8 C24 125.8(5) . . ? C22 N8 C24 126.8(5) . . ? C23 C22 N8 108.4(6) . . ? C23 C22 H22A 125.8 . . ? N8 C22 H22A 125.8 . . ? C22 C23 N7 107.0(6) . . ? C22 C23 H23A 126.5 . . ? N7 C23 H23A 126.5 . . ? 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 . . ? C25 O10 Fe3 129.0(3) . . ? C25 O11 Fe1 134.4(3) . . ? O11 C25 O10 126.1(4) . . ? O11 C25 C26 118.9(4) . . ? O10 C25 C26 115.0(4) . . ? N9 C26 C25 114.2(4) . . ? N9 C26 H26A 108.7 . . ? C25 C26 H26A 108.7 . . ? N9 C26 H26B 108.7 . . ? C25 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C27 N9 C29 108.4(4) . . ? C27 N9 C26 122.9(4) . . ? C29 N9 C26 128.5(5) . . ? N10 C27 N9 108.8(5) . . ? N10 C27 H27A 125.6 . . ? N9 C27 H27A 125.6 . . ? C27 N10 C28 108.7(5) . . ? C27 N10 C30 124.2(5) . . ? C28 N10 C30 127.0(5) . . ? C29 C28 N10 107.4(5) . . ? C29 C28 H28A 126.3 . . ? N10 C28 H28A 126.3 . . ? C28 C29 N9 106.7(5) . . ? C28 C29 H29A 126.7 . . ? N9 C29 H29A 126.7 . . ? 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 . . ? C31 O12 Fe3 132.4(3) . . ? C31 O13 Fe1 130.2(3) . . ? O13 C31 O12 127.8(4) . . ? O13 C31 C32 114.0(4) . . ? O12 C31 C32 118.2(4) . . ? N11 C32 C31 114.0(4) . . ? N11 C32 H32A 108.8 . . ? C31 C32 H32A 108.8 . . ? N11 C32 H32B 108.8 . . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C33 N11 C35 108.2(4) . . ? C33 N11 C32 125.4(4) . . ? C35 N11 C32 126.4(4) . . ? N12 C33 N11 108.5(4) . . ? N12 C33 H33A 125.8 . . ? N11 C33 H33A 125.8 . . ? C33 N12 C34 108.5(4) . . ? C33 N12 C36 124.8(5) . . ? C34 N12 C36 126.3(4) . . ? C35 C34 N12 107.5(4) . . ? C35 C34 H34A 126.2 . . ? N12 C34 H34A 126.2 . . ? C34 C35 N11 107.4(4) . . ? C34 C35 H35A 126.3 . . ? N11 C35 H35A 126.3 . . ? 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 . . ? Fe1 O14 H141 122(4) . . ? Fe1 O14 H142 125(4) . . ? H141 O14 H142 109(5) . . ? Fe2 O15 H151 120(4) . . ? Fe2 O15 H152 118(4) . . ? H151 O15 H152 104(5) . . ? Fe3 O16 H161 115(4) . . ? Fe3 O16 H162 125(4) . . ? H161 O16 H162 116(6) . . ? H611 O61 H612 101(8) . . ? H621 O62 H622 110(10) . . ? O23 S1 O22 119.3(3) . . ? O23 S1 N21 116.6(2) . . ? O22 S1 N21 107.6(3) . . ? O23 S1 C41 105.6(3) . . ? O22 S1 C41 102.3(3) . . ? N21 S1 C41 103.0(2) . . ? S1 N21 S2 126.3(3) . . ? O24 S2 O25 118.6(3) . . ? O24 S2 N21 117.5(2) . . ? O25 S2 N21 108.1(3) . . ? O24 S2 C42 104.1(3) . . ? O25 S2 C42 104.2(4) . . ? N21 S2 C42 101.8(3) . . ? F1 C41 F2 109.1(5) . . ? F1 C41 F3 108.8(5) . . ? F2 C41 F3 107.5(5) . . ? F1 C41 S1 110.4(4) . . ? F2 C41 S1 111.5(4) . . ? F3 C41 S1 109.6(4) . . ? F5 C42 F4 108.2(5) . . ? F5 C42 F6 109.1(6) . . ? F4 C42 F6 108.5(6) . . ? F5 C42 S2 110.9(5) . . ? F4 C42 S2 110.1(5) . . ? F6 C42 S2 110.0(4) . . ? O27 S3 O28 117.4(3) . . ? O27 S3 N26 117.3(3) . . ? O28 S3 N26 108.1(2) . . ? O27 S3 C43 105.8(3) . . ? O28 S3 C43 103.9(4) . . ? N26 S3 C43 102.3(4) . . ? S3 N26 S4 125.6(3) . . ? O29 S4 O30 117.4(3) . . ? O29 S4 N26 116.9(3) . . ? O30 S4 N26 109.3(3) . . ? O29 S4 C44 107.8(4) . . ? O30 S4 C44 102.2(3) . . ? N26 S4 C44 100.7(3) . . ? F8 C43 F9 109.4(8) . . ? F8 C43 F7 107.9(7) . . ? F9 C43 F7 106.2(7) . . ? F8 C43 S3 112.6(6) . . ? F9 C43 S3 111.4(6) . . ? F7 C43 S3 109.1(7) . . ? F10 C44 F11 108.6(5) . . ? F10 C44 F12 108.8(5) . . ? F11 C44 F12 108.2(5) . . ? F10 C44 S4 111.6(5) . . ? F11 C44 S4 109.5(5) . . ? F12 C44 S4 110.0(4) . . ? O32 S5 O33 119.5(3) . . ? O32 S5 N31 117.1(2) . . ? O33 S5 N31 105.8(2) . . ? O32 S5 C45 105.9(4) . . ? O33 S5 C45 102.4(3) . . ? N31 S5 C45 104.2(3) . . ? S5 N31 S6 124.9(3) . . ? O35 S6 O34 118.2(3) . . ? O35 S6 N31 108.1(2) . . ? O34 S6 N31 116.5(2) . . ? O35 S6 C46 103.5(3) . . ? O34 S6 C46 105.3(3) . . ? N31 S6 C46 103.2(2) . . ? F15 C45 F13 109.2(6) . . ? F15 C45 F14 108.0(7) . . ? F13 C45 F14 109.2(6) . . ? F15 C45 S5 112.5(5) . . ? F13 C45 S5 108.3(6) . . ? F14 C45 S5 109.7(5) . . ? F18 C46 F16 108.6(5) . . ? F18 C46 F17 108.7(5) . . ? F16 C46 F17 107.4(5) . . ? F18 C46 S6 112.2(4) . . ? F16 C46 S6 110.3(4) . . ? F17 C46 S6 109.5(4) . . ? O38 S7 O37 118.0(3) . . ? O38 S7 N36 117.4(2) . . ? O37 S7 N36 108.0(3) . . ? O38 S7 C47 106.3(3) . . ? O37 S7 C47 102.7(3) . . ? N36 S7 C47 102.0(3) . . ? S8 N36 S7 124.9(3) . . ? O40 S8 O39 119.8(4) . . ? O40 S8 N36 108.7(3) . . ? O39 S8 N36 116.8(2) . . ? O40 S8 C48 103.4(4) . . ? O39 S8 C48 103.3(3) . . ? N36 S8 C48 102.0(3) . . ? F19 C47 F21 109.3(6) . . ? F19 C47 F20 109.3(7) . . ? F21 C47 F20 108.1(6) . . ? F19 C47 S7 110.9(5) . . ? F21 C47 S7 108.8(6) . . ? F20 C47 S7 110.4(5) . . ? F23 C48 F22 107.8(6) . . ? F23 C48 F24 108.1(5) . . ? F22 C48 F24 107.5(7) . . ? F23 C48 S8 111.2(5) . . ? F22 C48 S8 112.0(4) . . ? F24 C48 S8 110.2(5) . . ? O43A S9 O42A 118.1(5) . . ? O43B S9 O42B 116.3(8) . . ? O43B S9 N41B 124.1(5) . . ? O42B S9 N41B 112.1(7) . . ? O43A S9 N41A 103.7(5) . . ? O42A S9 N41A 109.6(5) . . ? O43A S9 C49A 109.5(5) . . ? O42A S9 C49A 108.6(5) . . ? N41A S9 C49A 106.9(5) . . ? O43B S9 C49B 100.2(5) . . ? O42B S9 C49B 99.0(5) . . ? N41B S9 C49B 98.2(5) . . ? S10 N41A S9 126.0(5) . . ? S9 N41B S10 126.3(6) . . ? O44A S10 O45A 112.7(5) . . ? O44A S10 N41A 118.0(5) . . ? O45A S10 N41A 121.2(5) . . ? O45B S10 O44B 116.9(6) . . ? O45B S10 N41B 106.3(6) . . ? O44B S10 N41B 105.5(5) . . ? O45B S10 C50B 111.4(7) . . ? O44B S10 C50B 106.2(7) . . ? N41B S10 C50B 110.3(6) . . ? O44A S10 C50A 99.0(6) . . ? O45A S10 C50A 100.5(6) . . ? N41A S10 C50A 99.1(5) . . ? F26A C49A F25A 106.7(9) . . ? F26A C49A F27A 105.5(8) . . ? F25A C49A F27A 104.5(8) . . ? F26A C49A S9 116.3(7) . . ? F25A C49A S9 110.6(8) . . ? F27A C49A S9 112.4(8) . . ? F28A C50A F30A 112.0(11) . . ? F28A C50A F29A 106.4(11) . . ? F30A C50A F29A 107.0(12) . . ? F28A C50A S10 110.1(11) . . ? F30A C50A S10 111.7(9) . . ? F29A C50A S10 109.5(9) . . ? F27B C49B F26B 111.3(9) . . ? F27B C49B F25B 107.8(9) . . ? F26B C49B F25B 105.4(10) . . ? F27B C49B S9 111.8(9) . . ? F26B C49B S9 111.3(7) . . ? F25B C49B S9 108.8(7) . . ? F28B C50B F29B 107.7(13) . . ? F28B C50B F30B 110.9(15) . . ? F29B C50B F30B 110.0(14) . . ? F28B C50B S10 108.3(12) . . ? F29B C50B S10 112.9(10) . . ? F30B C50B S10 107.0(11) . . ? O48A S11 O47A 122.6(7) . . ? O47B S11 N46B 123.1(8) . . ? O47B S11 O48B 110.6(9) . . ? N46B S11 O48B 98.9(5) . . ? O48A S11 N46A 117.9(5) . . ? O47A S11 N46A 100.3(5) . . ? O48A S11 C51 109.5(5) . . ? O47B S11 C51 117.0(9) . . ? O47A S11 C51 99.3(7) . . ? N46B S11 C51 104.5(7) . . ? O48B S11 C51 98.7(5) . . ? N46A S11 C51 104.5(4) . . ? O49A S12 O50A 113.5(9) . . ? O49A S12 N46A 116.1(9) . . ? O50A S12 N46A 117.2(5) . . ? O49B S12 N46B 116.3(12) . . ? O49B S12 O50B 106.9(11) . . ? N46B S12 O50B 102.6(6) . . ? O49B S12 C52B 117.9(16) . . ? N46B S12 C52B 104.6(9) . . ? O50B S12 C52B 107.2(8) . . ? O49A S12 C52A 101.6(11) . . ? O50A S12 C52A 104.0(7) . . ? N46A S12 C52A 101.3(5) . . ? S12 N46A S11 124.8(5) . . ? S11 N46B S12 126.4(7) . . ? F31B C51 F33B 113.1(9) . . ? F32A C51 F31A 110.3(8) . . ? F32A C51 F33A 106.5(7) . . ? F31A C51 F33A 109.7(7) . . ? F31B C51 F32B 112.0(8) . . ? F33B C51 F32B 100.7(8) . . ? F32A C51 S11 112.7(6) . . ? F31B C51 S11 112.6(7) . . ? F33B C51 S11 116.0(8) . . ? F31A C51 S11 112.6(6) . . ? F33A C51 S11 104.7(6) . . ? F32B C51 S11 101.1(6) . . ? F34A C52A F36A 107.5(10) . . ? F34A C52A F35A 102.8(11) . . ? F36A C52A F35A 99.7(11) . . ? F34A C52A S12 116.6(9) . . ? F36A C52A S12 111.7(8) . . ? F35A C52A S12 116.8(14) . . ? F34B C52B F35B 117.6(16) . . ? F34B C52B F36B 110.9(14) . . ? F35B C52B F36B 113.0(15) . . ? F34B C52B S12 106.3(13) . . ? F35B C52B S12 96.0(13) . . ? F36B C52B S12 111.8(13) . . ? O52A S13A O53A 121.7(13) . . ? O52A S13A N51A 115.2(11) . . ? O53A S13A N51A 110.5(7) . . ? O52A S13A C53A 104.1(19) . . ? O53A S13A C53A 103.8(5) . . ? N51A S13A C53A 97.4(6) . . ? S14A N51A S13A 124.3(7) . . ? O55A S14A O54A 115.9(7) . . ? O55A S14A N51A 116.0(6) . . ? O54A S14A N51A 106.3(6) . . ? O55A S14A C54A 106.1(6) . . ? O54A S14A C54A 104.9(8) . . ? N51A S14A C54A 106.7(7) . . ? F38A C53A F37A 106.2(8) . . ? F38A C53A F39A 111.0(8) . . ? F37A C53A F39A 109.6(8) . . ? F38A C53A S13A 111.1(7) . . ? F37A C53A S13A 109.3(7) . . ? F39A C53A S13A 109.6(7) . . ? F42A C54A F41A 107.7(10) . . ? F42A C54A F40A 107.5(11) . . ? F41A C54A F40A 105.9(10) . . ? F42A C54A S14A 113.5(10) . . ? F41A C54A S14A 111.8(9) . . ? F40A C54A S14A 110.0(9) . . ? O52B S13B O53B 118(2) . . ? O52B S13B N51B 119.0(9) . . ? O53B S13B N51B 108(3) . . ? O52B S13B C53B 108.2(7) . . ? O53B S13B C53B 102.3(18) . . ? N51B S13B C53B 99.3(8) . . ? S14B N51B S13B 130.1(12) . . ? O55B S14B O54B 118.7(12) . . ? O55B S14B N51B 111.0(10) . . ? O54B S14B N51B 111.0(10) . . ? O55B S14B C54B 102.7(9) . . ? O54B S14B C54B 105.2(8) . . ? N51B S14B C54B 107.2(9) . . ? F37B C53B F39B 107.7(10) . . ? F37B C53B F38B 107.6(10) . . ? F39B C53B F38B 107.6(10) . . ? F37B C53B S13B 114.1(9) . . ? F39B C53B S13B 111.4(10) . . ? F38B C53B S13B 108.2(9) . . ? F40B C54B F41B 110.3(12) . . ? F40B C54B F42B 109.2(12) . . ? F41B C54B F42B 106.2(12) . . ? F40B C54B S14B 112.8(11) . . ? F41B C54B S14B 109.0(11) . . ? F42B C54B S14B 109.0(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H141 O22 0.84(4) 1.92(4) 2.759(5) 176(6) . O14 H142 O62 0.88(3) 1.70(4) 2.583(5) 174(6) . O15 H151 O39 0.88(3) 1.97(4) 2.827(5) 164(5) 1_455 O15 H152 O33 0.86(3) 1.88(4) 2.728(4) 166(5) 1_455 O16 H161 O61 0.87(4) 1.78(4) 2.646(5) 169(6) . O16 H162 O63B 0.91(4) 1.85(5) 2.667(12) 150(6) . O61 H611 O24 0.93(4) 2.04(4) 2.945(6) 166(8) 1_565 O61 H612 O52A 0.89(3) 2.00(3) 2.87(2) 164(8) . O61 H612 O53B 0.89(3) 1.96(5) 2.84(4) 172(9) . O62 H621 O44A 0.91(4) 2.07(5) 2.946(11) 164(10) 2_656 O62 H622 O54B 0.89(4) 1.68(5) 2.537(17) 163(12) 1_445 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.205 _refine_diff_density_min -1.035 _refine_diff_density_rms 0.094 data_rfe3pymaa _database_code_depnum_ccdc_archive 'CCDC 896162' #TrackingRef 'Fe3_IL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 Fe3 N6 O16, 6(Cl4 Fe), Cl, 4(H2 O)' _chemical_formula_sum 'C48 H68 Cl25 Fe9 N6 O20' _chemical_formula_weight 2437.98 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 24.8363(12) _cell_length_b 13.7847(7) _cell_length_c 27.4404(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9394.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27410 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 25.95 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4868 _exptl_absorpt_coefficient_mu 2.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.390 _exptl_absorpt_correction_T_max 0.464 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82847 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8600 _reflns_number_gt 6026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The Fe and two Cl atoms of a (FeCl4)- anion were twofold disordered, while three Cl atoms of another anion were similarly disordered. Within each anion, similarity restraints were applied to Fe-Cl distances. Geometrical restraints were applied to O-H bonds. ; _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^)+(0.1404P)^2^+6.4189P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8600 _refine_ls_number_parameters 527 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.2165 _refine_ls_wR_factor_gt 0.1977 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.074 _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 0.5000 0.23004(9) 0.2500 0.0260(3) Uani 1 2 d S . . Fe2 Fe 0.52548(3) 0.02340(6) 0.30566(3) 0.0276(2) Uani 1 1 d . . . O1 O 0.5000 0.0916(4) 0.2500 0.0280(13) Uani 1 2 d S . . O2 O 0.46016(18) 0.2395(3) 0.31407(16) 0.0317(10) Uani 1 1 d . . . O3 O 0.48294(19) 0.1027(3) 0.35393(17) 0.0349(10) Uani 1 1 d . . . C1 C 0.4567(2) 0.1807(5) 0.3496(2) 0.0302(14) Uani 1 1 d . . . C2 C 0.4183(3) 0.2030(6) 0.3902(3) 0.0406(16) Uani 1 1 d . . . H2A H 0.4393 0.2124 0.4205 0.049 Uiso 1 1 calc R . . H2B H 0.3947 0.1459 0.3952 0.049 Uiso 1 1 calc R . . C3 C 0.3831(3) 0.2911(6) 0.3825(4) 0.053(2) Uani 1 1 d . . . H3A H 0.3697 0.2910 0.3485 0.063 Uiso 1 1 calc R . . H3B H 0.3514 0.2866 0.4044 0.063 Uiso 1 1 calc R . . N1 N 0.4114(3) 0.3838(5) 0.3919(3) 0.0525(17) Uani 1 1 d . . . C4 C 0.4255(4) 0.4412(6) 0.3541(4) 0.060(2) Uani 1 1 d . . . H4A H 0.4181 0.4213 0.3216 0.072 Uiso 1 1 calc R . . C5 C 0.4505(5) 0.5286(7) 0.3627(5) 0.074(3) Uani 1 1 d . . . H5A H 0.4612 0.5685 0.3362 0.089 Uiso 1 1 calc R . . C6 C 0.4600(5) 0.5581(7) 0.4101(5) 0.085(4) Uani 1 1 d . . . H6A H 0.4766 0.6189 0.4166 0.102 Uiso 1 1 calc R . . C7 C 0.4449(5) 0.4972(8) 0.4482(4) 0.076(3) Uani 1 1 d . . . H7A H 0.4508 0.5157 0.4811 0.092 Uiso 1 1 calc R . . C8 C 0.4216(4) 0.4111(7) 0.4375(4) 0.063(2) Uani 1 1 d . . . H8A H 0.4123 0.3686 0.4634 0.075 Uiso 1 1 calc R . . O4 O 0.57135(18) 0.2470(3) 0.28204(17) 0.0332(10) Uani 1 1 d . . . O5 O 0.59183(18) 0.1035(3) 0.31636(17) 0.0318(10) Uani 1 1 d . . . C9 C 0.6028(2) 0.1910(5) 0.3052(2) 0.0296(13) Uani 1 1 d . . . C10 C 0.6561(3) 0.2293(5) 0.3215(3) 0.0337(14) Uani 1 1 d . . . H10A H 0.6853 0.1928 0.3052 0.040 Uiso 1 1 calc R . . H10B H 0.6599 0.2197 0.3571 0.040 Uiso 1 1 calc R . . C11 C 0.6615(3) 0.3373(6) 0.3096(3) 0.0483(19) Uani 1 1 d . . . H11A H 0.6640 0.3456 0.2738 0.058 Uiso 1 1 calc R . . H11B H 0.6289 0.3719 0.3210 0.058 Uiso 1 1 calc R . . N2 N 0.7094(2) 0.3804(4) 0.3328(3) 0.0435(15) Uani 1 1 d . . . C12 C 0.7070(4) 0.4038(6) 0.3804(4) 0.055(2) Uani 1 1 d . . . H12A H 0.6754 0.3911 0.3988 0.066 Uiso 1 1 calc R . . C13 C 0.7512(4) 0.4466(7) 0.4022(4) 0.072(3) Uani 1 1 d . . . H13A H 0.7506 0.4631 0.4358 0.087 Uiso 1 1 calc R . . C14 C 0.7962(4) 0.4650(8) 0.3744(5) 0.080(3) Uani 1 1 d . . . H14A H 0.8264 0.4962 0.3888 0.096 Uiso 1 1 calc R . . C15 C 0.7980(4) 0.4401(8) 0.3283(5) 0.069(3) Uani 1 1 d . . . H15A H 0.8299 0.4514 0.3099 0.083 Uiso 1 1 calc R . . C16 C 0.7541(3) 0.3975(7) 0.3063(4) 0.056(2) Uani 1 1 d . . . H16A H 0.7553 0.3805 0.2727 0.067 Uiso 1 1 calc R . . O6 O 0.46548(18) -0.0761(3) 0.30495(17) 0.0350(10) Uani 1 1 d . . . O7 O 0.42755(18) -0.0710(3) 0.23059(18) 0.0352(10) Uani 1 1 d . . . C17 C 0.4311(3) -0.1017(4) 0.2743(3) 0.0362(16) Uani 1 1 d . . . C18 C 0.3889(3) -0.1773(5) 0.2889(3) 0.0438(17) Uani 1 1 d . . . H18A H 0.3528 -0.1473 0.2869 0.053 Uiso 1 1 calc R . . H18B H 0.3901 -0.2314 0.2652 0.053 Uiso 1 1 calc R . . C19 C 0.3965(3) -0.2180(6) 0.3394(4) 0.054(2) Uani 1 1 d . . . H19A H 0.3744 -0.2774 0.3428 0.065 Uiso 1 1 calc R . . H19B H 0.4347 -0.2365 0.3437 0.065 Uiso 1 1 calc R . . N3 N 0.3813(3) -0.1487(5) 0.3778(3) 0.0533(18) Uani 1 1 d . . . C20 C 0.4183(4) -0.1002(8) 0.4037(3) 0.060(3) Uani 1 1 d . . . H20A H 0.4555 -0.1112 0.3979 0.073 Uiso 1 1 calc R . . C21 C 0.4025(5) -0.0347(9) 0.4385(4) 0.074(3) Uani 1 1 d . . . H21A H 0.4288 -0.0001 0.4566 0.089 Uiso 1 1 calc R . . C22 C 0.3482(6) -0.0187(10) 0.4475(4) 0.084(4) Uani 1 1 d . . . H22A H 0.3369 0.0268 0.4714 0.100 Uiso 1 1 calc R . . C23 C 0.3115(5) -0.0707(10) 0.4209(4) 0.079(3) Uani 1 1 d . . . H23A H 0.2741 -0.0623 0.4266 0.095 Uiso 1 1 calc R . . C24 C 0.3282(4) -0.1332(8) 0.3869(4) 0.067(3) Uani 1 1 d . . . H24A H 0.3022 -0.1680 0.3685 0.081 Uiso 1 1 calc R . . O8 O 0.5000 0.3796(5) 0.2500 0.0369(15) Uani 1 2 d SD . . H8 H 0.470(2) 0.409(6) 0.241(3) 0.044 Uiso 1 1 d D . . O9 O 0.5497(2) -0.0541(4) 0.3666(2) 0.0424(12) Uani 1 1 d D . . H91 H 0.566(3) -0.025(6) 0.392(2) 0.051 Uiso 1 1 d D . . H92 H 0.549(4) -0.119(3) 0.372(3) 0.051 Uiso 1 1 d D . . Cl11 Cl 0.5000 0.6863(2) 0.2500 0.0689(9) Uani 1 2 d S . . Fe3 Fe 0.57518(5) 0.24172(8) 0.46648(4) 0.0442(3) Uani 1 1 d . . . Cl31 Cl 0.60209(10) 0.09846(16) 0.44175(7) 0.0577(6) Uani 1 1 d . . . Cl32 Cl 0.55469(9) 0.33114(15) 0.40257(8) 0.0530(5) Uani 1 1 d . . . Cl33 Cl 0.50297(11) 0.2277(2) 0.51125(9) 0.0752(7) Uani 1 1 d . . . Cl34 Cl 0.63918(13) 0.3079(2) 0.50867(13) 0.0881(9) Uani 1 1 d . . . Fe4A Fe 0.2572(3) 0.0879(5) 0.3238(3) 0.0480(13) Uani 0.53 1 d PD A 1 Fe4B Fe 0.2526(4) 0.0828(7) 0.3110(3) 0.059(2) Uani 0.47 1 d PD A 2 Cl41 Cl 0.34051(9) 0.07083(18) 0.30028(9) 0.0608(6) Uani 1 1 d D . . Cl42 Cl 0.21553(11) -0.0563(3) 0.31866(11) 0.0846(9) Uani 1 1 d D . . Cl43 Cl 0.2564(3) 0.1561(5) 0.3957(2) 0.0585(14) Uani 0.53 1 d PD A 1 Cl44 Cl 0.2262(3) 0.1942(5) 0.2700(2) 0.0720(16) Uani 0.53 1 d PD A 1 Cl45 Cl 0.2349(5) 0.1511(9) 0.3806(3) 0.104(4) Uani 0.47 1 d PD A 2 Cl46 Cl 0.2087(3) 0.1525(6) 0.2514(3) 0.079(2) Uani 0.47 1 d PD A 2 Fe5 Fe 0.66735(6) 0.68236(12) 0.44325(6) 0.0683(4) Uani 1 1 d D . . Cl51 Cl 0.59923(12) 0.58624(19) 0.42120(13) 0.0818(8) Uani 1 1 d D B . Cl52 Cl 0.62931(19) 0.8297(3) 0.4534(2) 0.0585(11) Uiso 0.53 1 d PD B 1 Cl53 Cl 0.7129(2) 0.6940(4) 0.3735(2) 0.0670(12) Uiso 0.53 1 d PD B 1 Cl54 Cl 0.7101(3) 0.6351(6) 0.5046(3) 0.0992(19) Uiso 0.53 1 d PD B 1 Cl55 Cl 0.6372(2) 0.8130(4) 0.4731(3) 0.0698(15) Uiso 0.47 1 d PD B 2 Cl56 Cl 0.7302(2) 0.6912(4) 0.3914(2) 0.0567(12) Uiso 0.47 1 d PD B 2 Cl57 Cl 0.6968(4) 0.5853(7) 0.5050(3) 0.107(2) Uiso 0.47 1 d PD B 2 O11 O 0.5383(3) 0.7565(5) 0.3559(3) 0.074(2) Uani 1 1 d D . . H111 H 0.544(4) 0.748(9) 0.3218(15) 0.089 Uiso 1 1 d D . . H112 H 0.567(3) 0.723(8) 0.369(3) 0.089 Uiso 1 1 d D . . O12A O 0.4224(5) 0.5144(8) 0.2418(4) 0.063(3) Uiso 0.59 1 d P C 1 O12B O 0.4355(6) 0.5067(12) 0.2012(6) 0.062(4) Uiso 0.41 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0259(6) 0.0179(6) 0.0342(6) 0.000 -0.0023(5) 0.000 Fe2 0.0242(4) 0.0211(4) 0.0373(5) 0.0037(4) -0.0035(4) 0.0000(3) O1 0.021(3) 0.024(3) 0.040(3) 0.000 0.000(2) 0.000 O2 0.034(2) 0.025(2) 0.036(2) -0.0004(19) -0.0007(18) 0.0033(18) O3 0.035(2) 0.031(2) 0.039(3) 0.004(2) -0.0053(19) 0.0051(19) C1 0.025(3) 0.032(4) 0.033(3) -0.003(3) 0.002(2) 0.000(3) C2 0.037(4) 0.039(4) 0.045(4) -0.007(3) 0.008(3) 0.002(3) C3 0.040(4) 0.047(5) 0.071(5) -0.008(4) 0.014(4) 0.006(4) N1 0.050(4) 0.041(4) 0.066(4) -0.010(3) 0.015(3) 0.015(3) C4 0.069(6) 0.038(4) 0.073(6) 0.001(4) 0.001(5) 0.018(4) C5 0.087(7) 0.036(5) 0.100(8) 0.004(5) -0.006(6) 0.006(5) C6 0.089(8) 0.033(5) 0.133(11) -0.024(6) 0.004(7) 0.012(5) C7 0.091(8) 0.056(6) 0.082(7) -0.022(5) 0.011(6) 0.005(6) C8 0.072(6) 0.045(5) 0.071(6) -0.016(4) 0.019(5) 0.001(4) O4 0.031(2) 0.023(2) 0.045(3) 0.0006(19) -0.004(2) -0.0014(18) O5 0.029(2) 0.026(2) 0.041(3) 0.0004(19) -0.0026(19) -0.0023(18) C9 0.027(3) 0.027(3) 0.035(3) -0.001(3) 0.001(3) -0.002(3) C10 0.026(3) 0.028(3) 0.047(4) 0.000(3) -0.008(3) -0.003(3) C11 0.039(4) 0.035(4) 0.071(5) 0.012(4) -0.017(4) -0.012(3) N2 0.030(3) 0.031(3) 0.069(4) 0.002(3) -0.009(3) -0.009(2) C12 0.051(5) 0.040(4) 0.074(6) -0.007(4) 0.002(4) -0.002(4) C13 0.080(7) 0.051(5) 0.086(7) -0.024(5) -0.028(6) 0.000(5) C14 0.044(5) 0.054(6) 0.142(11) -0.015(6) -0.020(6) -0.023(4) C15 0.041(5) 0.061(6) 0.105(8) 0.003(6) 0.004(5) -0.016(4) C16 0.039(4) 0.060(5) 0.069(5) 0.002(4) 0.004(4) -0.017(4) O6 0.031(2) 0.031(2) 0.043(3) 0.006(2) -0.005(2) -0.0045(19) O7 0.029(2) 0.028(2) 0.048(3) 0.001(2) -0.007(2) -0.0033(19) C17 0.028(3) 0.015(3) 0.066(5) -0.001(3) -0.004(3) -0.002(2) C18 0.030(4) 0.033(4) 0.068(5) 0.008(3) -0.001(3) -0.011(3) C19 0.034(4) 0.042(4) 0.087(6) 0.027(4) 0.000(4) -0.005(3) N3 0.043(4) 0.049(4) 0.067(4) 0.029(4) 0.003(3) -0.008(3) C20 0.054(5) 0.075(6) 0.051(5) 0.028(5) -0.004(4) -0.023(5) C21 0.090(8) 0.083(8) 0.049(5) 0.024(5) -0.005(5) -0.027(6) C22 0.108(10) 0.087(8) 0.056(6) 0.030(6) 0.016(6) 0.006(7) C23 0.065(6) 0.098(9) 0.074(7) 0.034(7) 0.018(6) 0.022(6) C24 0.046(5) 0.078(7) 0.078(7) 0.038(6) 0.003(5) 0.000(5) O8 0.037(4) 0.024(3) 0.051(4) 0.000 -0.006(3) 0.000 O9 0.042(3) 0.032(3) 0.053(3) 0.009(2) -0.013(2) -0.001(2) Cl11 0.071(2) 0.0302(14) 0.106(3) 0.000 0.0033(19) 0.000 Fe3 0.0455(6) 0.0434(6) 0.0438(6) -0.0093(5) -0.0017(5) 0.0059(5) Cl31 0.0810(15) 0.0474(11) 0.0445(10) -0.0095(8) -0.0038(10) 0.0186(10) Cl32 0.0552(11) 0.0441(11) 0.0597(12) 0.0035(9) -0.0006(9) 0.0052(9) Cl33 0.0628(14) 0.107(2) 0.0558(13) 0.0065(13) 0.0157(11) 0.0232(14) Cl34 0.0870(19) 0.0698(17) 0.107(2) -0.0234(16) -0.0436(17) -0.0020(14) Fe4A 0.0484(19) 0.044(2) 0.052(4) 0.016(2) 0.0228(19) 0.0186(14) Fe4B 0.066(3) 0.061(3) 0.051(4) 0.012(2) 0.027(3) 0.031(2) Cl41 0.0486(11) 0.0569(13) 0.0771(14) -0.0037(11) 0.0172(10) -0.0041(9) Cl42 0.0640(15) 0.107(2) 0.0823(17) 0.0252(16) -0.0059(13) -0.0362(15) Cl43 0.070(4) 0.047(2) 0.059(3) 0.000(2) 0.021(3) 0.015(3) Cl44 0.062(3) 0.079(4) 0.075(4) 0.024(3) 0.012(3) 0.038(3) Cl45 0.130(9) 0.109(7) 0.073(6) -0.008(5) 0.009(5) 0.074(7) Cl46 0.068(4) 0.097(6) 0.072(4) 0.024(4) 0.007(3) 0.038(4) Fe5 0.0517(8) 0.0743(10) 0.0789(10) 0.0025(8) 0.0194(7) 0.0038(7) Cl51 0.0774(17) 0.0521(14) 0.116(2) 0.0042(14) 0.0048(16) -0.0032(12) O11 0.081(5) 0.044(4) 0.098(5) 0.021(4) -0.038(4) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.908(6) . ? Fe1 O4 1.992(4) . ? Fe1 O4 1.992(4) 3_655 ? Fe1 O2 2.022(4) . ? Fe1 O2 2.022(4) 3_655 ? Fe1 O8 2.062(7) . ? Fe2 O1 1.902(3) . ? Fe2 O5 2.006(4) . ? Fe2 O7 2.011(5) 3_655 ? Fe2 O3 2.016(5) . ? Fe2 O6 2.025(5) . ? Fe2 O9 2.073(5) . ? O1 Fe2 1.902(3) 3_655 ? O2 C1 1.271(8) . ? O3 C1 1.263(8) . ? C1 C2 1.498(9) . ? C2 C3 1.512(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.482(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N1 C8 1.329(12) . ? N1 C4 1.353(12) . ? C4 C5 1.375(14) . ? C4 H4A 0.9500 . ? C5 C6 1.384(17) . ? C5 H5A 0.9500 . ? C6 C7 1.393(17) . ? C6 H6A 0.9500 . ? C7 C8 1.352(15) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? O4 C9 1.268(8) . ? O5 C9 1.274(8) . ? C9 C10 1.494(8) . ? C10 C11 1.530(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N2 1.475(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N2 C16 1.346(11) . ? N2 C12 1.349(12) . ? C12 C13 1.383(13) . ? C12 H12A 0.9500 . ? C13 C14 1.376(16) . ? C13 H13A 0.9500 . ? C14 C15 1.312(16) . ? C14 H14A 0.9500 . ? C15 C16 1.378(13) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? O6 C17 1.249(8) . ? O7 C17 1.274(9) . ? O7 Fe2 2.011(5) 3_655 ? C17 C18 1.532(9) . ? C18 C19 1.505(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N3 1.472(13) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? N3 C20 1.341(12) . ? N3 C24 1.358(12) . ? C20 C21 1.373(16) . ? C20 H20A 0.9500 . ? C21 C22 1.387(17) . ? C21 H21A 0.9500 . ? C22 C23 1.372(18) . ? C22 H22A 0.9500 . ? C23 C24 1.336(17) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? O8 H8 0.89(4) 3_655 ? O8 H8 0.89(4) . ? O9 H91 0.90(4) . ? O9 H92 0.91(4) . ? Fe3 Cl34 2.167(3) . ? Fe3 Cl33 2.182(3) . ? Fe3 Cl31 2.193(2) . ? Fe3 Cl32 2.203(2) . ? Fe4A Cl41 2.180(7) . ? Fe4A Cl43 2.185(9) . ? Fe4A Cl44 2.218(8) . ? Fe4A Cl42 2.245(8) . ? Fe4B Cl42 2.138(10) . ? Fe4B Cl45 2.175(10) . ? Fe4B Cl46 2.188(10) . ? Fe4B Cl41 2.208(9) . ? Fe5 Cl54 2.093(7) . ? Fe5 Cl56 2.116(5) . ? Fe5 Cl55 2.115(6) . ? Fe5 Cl53 2.228(5) . ? Fe5 Cl51 2.233(3) . ? Fe5 Cl52 2.257(5) . ? Fe5 Cl57 2.280(8) . ? O11 H111 0.95(4) . ? O11 H112 0.93(4) . ? 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 96.75(13) . . ? O1 Fe1 O4 96.75(13) . 3_655 ? O4 Fe1 O4 166.5(3) . 3_655 ? O1 Fe1 O2 93.70(13) . . ? O4 Fe1 O2 92.52(19) . . ? O4 Fe1 O2 86.61(18) 3_655 . ? O1 Fe1 O2 93.70(13) . 3_655 ? O4 Fe1 O2 86.61(18) . 3_655 ? O4 Fe1 O2 92.52(19) 3_655 3_655 ? O2 Fe1 O2 172.6(3) . 3_655 ? O1 Fe1 O8 180.000(1) . . ? O4 Fe1 O8 83.25(13) . . ? O4 Fe1 O8 83.25(13) 3_655 . ? O2 Fe1 O8 86.30(13) . . ? O2 Fe1 O8 86.30(13) 3_655 . ? O1 Fe2 O5 96.82(18) . . ? O1 Fe2 O7 96.63(18) . 3_655 ? O5 Fe2 O7 87.26(19) . 3_655 ? O1 Fe2 O3 94.90(17) . . ? O5 Fe2 O3 92.05(19) . . ? O7 Fe2 O3 168.45(19) 3_655 . ? O1 Fe2 O6 94.72(18) . . ? O5 Fe2 O6 168.23(19) . . ? O7 Fe2 O6 89.1(2) 3_655 . ? O3 Fe2 O6 89.3(2) . . ? O1 Fe2 O9 177.27(17) . . ? O5 Fe2 O9 85.8(2) . . ? O7 Fe2 O9 84.1(2) 3_655 . ? O3 Fe2 O9 84.4(2) . . ? O6 Fe2 O9 82.7(2) . . ? Fe2 O1 Fe2 120.8(3) 3_655 . ? Fe2 O1 Fe1 119.62(16) 3_655 . ? Fe2 O1 Fe1 119.62(16) . . ? C1 O2 Fe1 131.3(4) . . ? C1 O3 Fe2 132.1(4) . . ? O3 C1 O2 125.4(6) . . ? O3 C1 C2 115.7(6) . . ? O2 C1 C2 118.9(6) . . ? C1 C2 C3 115.4(7) . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? C3 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? N1 C3 C2 113.2(7) . . ? N1 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? N1 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.8 . . ? C8 N1 C4 120.5(8) . . ? C8 N1 C3 120.0(8) . . ? C4 N1 C3 119.6(8) . . ? N1 C4 C5 119.8(10) . . ? N1 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 119.8(11) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C5 C6 C7 118.9(10) . . ? C5 C6 H6A 120.6 . . ? C7 C6 H6A 120.6 . . ? C8 C7 C6 118.7(11) . . ? C8 C7 H7A 120.7 . . ? C6 C7 H7A 120.7 . . ? N1 C8 C7 122.4(10) . . ? N1 C8 H8A 118.8 . . ? C7 C8 H8A 118.8 . . ? C9 O4 Fe1 134.2(4) . . ? C9 O5 Fe2 131.4(4) . . ? O4 C9 O5 124.4(6) . . ? O4 C9 C10 118.7(6) . . ? O5 C9 C10 116.8(6) . . ? C9 C10 C11 110.9(6) . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C10 111.7(6) . . ? N2 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C16 N2 C12 121.2(7) . . ? C16 N2 C11 120.2(8) . . ? C12 N2 C11 118.6(7) . . ? N2 C12 C13 119.1(9) . . ? N2 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 118.9(10) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C15 C14 C13 121.0(9) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? C14 C15 C16 120.4(9) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? N2 C16 C15 119.4(9) . . ? N2 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C17 O6 Fe2 134.4(5) . . ? C17 O7 Fe2 129.8(4) . 3_655 ? O6 C17 O7 126.0(6) . . ? O6 C17 C18 118.8(7) . . ? O7 C17 C18 115.1(6) . . ? C19 C18 C17 114.2(6) . . ? C19 C18 H18A 108.7 . . ? C17 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? N3 C19 C18 112.6(7) . . ? N3 C19 H19A 109.1 . . ? C18 C19 H19A 109.1 . . ? N3 C19 H19B 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C20 N3 C24 119.3(10) . . ? C20 N3 C19 121.8(8) . . ? C24 N3 C19 118.9(8) . . ? N3 C20 C21 120.0(10) . . ? N3 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 C22 120.5(11) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C23 C22 C21 117.9(12) . . ? C23 C22 H22A 121.1 . . ? C21 C22 H22A 121.1 . . ? C24 C23 C22 120.2(11) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 N3 122.1(11) . . ? C23 C24 H24A 119.0 . . ? N3 C24 H24A 119.0 . . ? H8 O8 Fe1 117(6) 3_655 . ? H8 O8 H8 125(10) 3_655 . ? Fe1 O8 H8 117(6) . . ? Fe2 O9 H91 122(6) . . ? Fe2 O9 H92 130(6) . . ? H91 O9 H92 108(8) . . ? Cl34 Fe3 Cl33 109.83(14) . . ? Cl34 Fe3 Cl31 108.70(12) . . ? Cl33 Fe3 Cl31 110.19(12) . . ? Cl34 Fe3 Cl32 111.05(12) . . ? Cl33 Fe3 Cl32 107.93(10) . . ? Cl31 Fe3 Cl32 109.14(9) . . ? Cl41 Fe4A Cl43 108.8(4) . . ? Cl41 Fe4A Cl44 101.7(3) . . ? Cl43 Fe4A Cl44 108.3(4) . . ? Cl41 Fe4A Cl42 108.9(3) . . ? Cl43 Fe4A Cl42 115.7(3) . . ? Cl44 Fe4A Cl42 112.5(4) . . ? Cl42 Fe4B Cl45 102.4(5) . . ? Cl42 Fe4B Cl46 104.6(5) . . ? Cl45 Fe4B Cl46 111.4(5) . . ? Cl42 Fe4B Cl41 111.8(4) . . ? Cl45 Fe4B Cl41 110.5(5) . . ? Cl46 Fe4B Cl41 115.2(4) . . ? Cl56 Fe5 Cl55 118.2(2) . . ? Cl54 Fe5 Cl53 117.1(3) . . ? Cl54 Fe5 Cl51 114.7(3) . . ? Cl56 Fe5 Cl51 114.23(19) . . ? Cl55 Fe5 Cl51 110.01(19) . . ? Cl53 Fe5 Cl51 101.25(18) . . ? Cl54 Fe5 Cl52 113.1(3) . . ? Cl53 Fe5 Cl52 104.7(2) . . ? Cl51 Fe5 Cl52 104.50(15) . . ? Cl56 Fe5 Cl57 107.3(3) . . ? Cl55 Fe5 Cl57 109.0(3) . . ? Cl51 Fe5 Cl57 95.5(3) . . ? H111 O11 H112 101(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8 O12A 0.89(4) 1.87(5) 2.685(12) 152(8) . O8 H8 O12B 0.89(4) 1.93(6) 2.725(17) 149(8) . O9 H91 Cl31 0.90(4) 2.36(5) 3.220(6) 159(8) . O9 H92 O11 0.91(4) 1.80(5) 2.642(9) 154(8) 1_545 O11 H111 Cl11 0.95(4) 2.41(8) 3.208(8) 141(9) . O11 H112 Cl51 0.93(4) 2.50(7) 3.317(7) 147(10) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.949 _refine_diff_density_min -1.420 _refine_diff_density_rms 0.150