# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_Fe3CrEt _database_code_depnum_ccdc_archive 'CCDC 904914' #TrackingRef 'Fe3CrEt_19-08-2012_Pasquale1.cif' _audit_creation_date 2012-01-17T09:40:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(m4-2-(oxymethyl)-2-ethylpropane-1,3-diolato)-hexakis(dipivaloylmethanato)-chromium(III)-tri-iron(III) dimethoxyethane solvate ; _chemical_name_common 'iron and chromium etyl alkoxide' _chemical_formula_moiety 'C78 H136 Cr Fe3 O18' _chemical_formula_sum 'C78 H136 Cr Fe3 O18' _chemical_formula_weight 1581.42 _chemical_melting_point none #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c:h _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 16.4250(5) _cell_length_b 16.4250(5) _cell_length_c 58.768(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 13730.5(8) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4579 _cell_measurement_theta_min 2.689 _cell_measurement_theta_max 19.0585 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour green-red _exptl_crystal_size_max 0.443 _exptl_crystal_size_mid 0.371 _exptl_crystal_size_min 0.196 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5100 _exptl_special_details ; XPREP (Bruker, 2006) was used to perform the Gaussian absorption correction based on the face-indexed crystal size ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details XPREP _exptl_absorpt_correction_T_min 0.9189 _exptl_absorpt_correction_T_max 0.9935 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean none _diffrn_measurement_device_type 'X8 APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_unetI/netI 0.0306 _diffrn_reflns_number 56495 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -67 _diffrn_reflns_limit_l_max 74 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.82 _diffrn_reflns_theta_full 26.82 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 3222 _reflns_number_gt 1459 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER APEX-II' _computing_cell_refinement 'BRUKER SANT' _computing_data_reduction 'BRUKER SOFTWARE' _computing_structure_solution 'SHELXL97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0861P)^2^+22.9064P] 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 none _refine_ls_number_reflns 3222 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.066 _refine_ls_wR_factor_ref 0.2245 _refine_ls_wR_factor_gt 0.1704 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.281 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.044 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.48259(6) 0.14926(6) 0.0833 0.0928(4) Uani 1 2 d S . . Cr Cr 0.6667 0.3333 0.0833 0.0815(5) Uani 1 6 d S . . O3 O 0.5556(2) 0.2614(2) 0.06445(4) 0.0880(9) Uani 1 1 d . . . O1 O 0.4073(3) 0.1949(2) 0.10004(5) 0.1062(10) Uani 1 1 d . . . O2 O 0.3771(3) 0.0936(3) 0.06120(6) 0.1103(11) Uani 1 1 d . . . C13 C 0.6667 0.3333 0.03252(12) 0.094(2) Uani 1 3 d S . . C12 C 0.5667(4) 0.2676(4) 0.04030(7) 0.1110(17) Uani 1 1 d . . . H12A H 0.5261 0.2889 0.0339 0.133 Uiso 1 1 calc R . . H12B H 0.5463 0.2053 0.0343 0.133 Uiso 1 1 calc R . . C5 C 0.3225(5) 0.1719(4) 0.09781(9) 0.1118(16) Uani 1 1 d . . . C7 C 0.2962(5) 0.0831(4) 0.06214(10) 0.1151(17) Uani 1 1 d . . . C4 C 0.2838(5) 0.2077(6) 0.11663(11) 0.133(2) Uani 1 1 d . . . C11 C 0.2329(5) 0.0268(6) 0.04163(13) 0.142(2) Uani 1 1 d . . . C6 C 0.2660(5) 0.1178(5) 0.07953(11) 0.135(2) Uani 1 1 d . . . H6 H 0.2039 0.1047 0.0792 0.162 Uiso 1 1 calc R . . C3 C 0.1842(6) 0.1864(7) 0.11220(17) 0.203(4) Uani 1 1 d . . . H3A H 0.1823 0.2157 0.0982 0.305 Uiso 1 1 calc R . . H3B H 0.1638 0.2102 0.1245 0.305 Uiso 1 1 calc R . . H3C H 0.1434 0.1196 0.111 0.305 Uiso 1 1 calc R . . C1 C 0.2901(8) 0.1643(9) 0.13822(12) 0.256(6) Uani 1 1 d . . . H1A H 0.2681 0.1865 0.1506 0.384 Uiso 1 1 calc R . . H1B H 0.3543 0.181 0.1409 0.384 Uiso 1 1 calc R . . H1C H 0.2519 0.0971 0.1371 0.384 Uiso 1 1 calc R . . C9 C 0.1486(9) 0.0395(10) 0.0395(2) 0.327(9) Uani 1 1 d . . . H9A H 0.1692 0.1048 0.0371 0.491 Uiso 1 1 calc R . . H9B H 0.112 0.0183 0.0532 0.491 Uiso 1 1 calc R . . H9C H 0.111 0.0035 0.0268 0.491 Uiso 1 1 calc R . . C2 C 0.3476(7) 0.3156(7) 0.11754(18) 0.236(5) Uani 1 1 d . . . H2A H 0.3425 0.3425 0.1035 0.353 Uiso 1 1 calc R . . H2B H 0.4117 0.331 0.1198 0.353 Uiso 1 1 calc R . . H2C H 0.3284 0.3403 0.1299 0.353 Uiso 1 1 calc R . . C10 C 0.2860(8) 0.0656(8) 0.02030(14) 0.265(6) Uani 1 1 d . . . H10A H 0.302 0.1302 0.0187 0.398 Uiso 1 1 calc R . . H10B H 0.2481 0.0301 0.0076 0.398 Uiso 1 1 calc R . . H10C H 0.3425 0.0619 0.0207 0.398 Uiso 1 1 calc R . . C8 C 0.2048(10) -0.0713(7) 0.0449(2) 0.332(10) Uani 1 1 d . . . H8A H 0.1699 -0.0936 0.0588 0.498 Uiso 1 1 calc R . . H8B H 0.2598 -0.0776 0.0456 0.498 Uiso 1 1 calc R . . H8C H 0.1663 -0.1075 0.0323 0.498 Uiso 1 1 calc R . . C14 C 0.6667 0.3333 0.0056 0.143(4) Uani 1 3 d S . . H14A H 0.6447 0.2688 0.0011 0.171 Uiso 0.33 1 calc PR . . H14B H 0.618 0.347 0.0011 0.171 Uiso 0.33 1 calc PR . . C15 C 0.7285 0.3777 -0.0055 0.211(18) Uani 0.33 1 d P . . H15A H 0.7101 0.3645 -0.0212 0.316 Uiso 0.33 1 calc PR . . H15B H 0.7777 0.3639 -0.0025 0.316 Uiso 0.33 1 calc PR . . H15C H 0.7507 0.4429 -0.0025 0.316 Uiso 0.33 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0939(6) 0.0939(6) 0.0899(6) -0.0041(2) 0.0041(2) 0.0462(6) Cr 0.0881(8) 0.0881(8) 0.0681(9) 0 0 0.0441(4) O3 0.092(2) 0.098(2) 0.0723(15) -0.0021(14) -0.0054(14) 0.0463(17) O1 0.098(3) 0.116(3) 0.110(2) -0.0081(19) 0.004(2) 0.057(2) O2 0.092(2) 0.121(3) 0.115(2) -0.021(2) -0.0094(19) 0.052(2) C13 0.109(4) 0.109(4) 0.063(4) 0 0 0.0546(19) C12 0.127(4) 0.129(4) 0.075(3) -0.002(3) -0.013(3) 0.063(4) C5 0.128(5) 0.115(4) 0.108(4) 0.011(3) 0.019(4) 0.073(4) C7 0.115(5) 0.097(4) 0.122(4) 0.003(3) -0.007(4) 0.044(4) C4 0.133(5) 0.171(6) 0.127(5) 0.005(4) 0.026(4) 0.100(5) C11 0.109(5) 0.147(6) 0.147(6) -0.037(4) -0.038(4) 0.047(4) C6 0.119(5) 0.166(6) 0.136(5) -0.017(4) 0.000(4) 0.083(5) C3 0.172(8) 0.279(12) 0.198(8) -0.038(7) 0.019(6) 0.143(8) C1 0.335(14) 0.469(19) 0.116(5) 0.044(8) 0.047(7) 0.314(15) C9 0.231(12) 0.50(2) 0.318(14) -0.224(15) -0.163(11) 0.231(15) C2 0.203(9) 0.202(10) 0.291(11) -0.099(9) 0.035(8) 0.093(8) C10 0.224(11) 0.334(15) 0.122(6) -0.022(7) -0.024(7) 0.052(9) C8 0.43(2) 0.114(7) 0.380(17) -0.074(9) -0.257(16) 0.086(9) C14 0.179(7) 0.179(7) 0.070(5) 0 0 0.089(3) C15 0.20(2) 0.42(6) 0.100(10) 0.09(2) 0.073(12) 0.22(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O3 1.963(3) 18_544 ? Fe O3 1.963(3) . ? Fe O2 1.986(4) 18_544 ? Fe O2 1.986(4) . ? Fe O1 1.996(3) . ? Fe O1 1.996(3) 18_544 ? Cr O3 1.949(3) 16_554 ? Cr O3 1.949(3) 18_544 ? Cr O3 1.949(3) 17_654 ? Cr O3 1.949(3) 2_655 ? Cr O3 1.949(3) . ? Cr O3 1.949(3) 3_665 ? O3 C12 1.428(5) . ? O1 C5 1.254(6) . ? O2 C7 1.253(7) . ? C13 C12 1.515(6) 2_655 ? C13 C12 1.515(6) . ? C13 C12 1.515(6) 3_665 ? C13 C14 1.582(7) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C5 C6 1.407(8) . ? C5 C4 1.532(7) . ? C7 C6 1.378(8) . ? C7 C11 1.559(8) . ? C4 C1 1.484(9) . ? C4 C3 1.515(9) . ? C4 C2 1.544(10) . ? C11 C8 1.450(11) . ? C11 C10 1.478(10) . ? C11 C9 1.504(13) . ? C6 H6 0.93 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C14 C15 1.1178 . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Fe O3 78.46(16) 18_544 . ? O3 Fe O2 92.58(13) 18_544 18_544 ? O3 Fe O2 170.93(14) . 18_544 ? O3 Fe O2 170.93(14) 18_544 . ? O3 Fe O2 92.58(13) . . ? O2 Fe O2 96.4(2) 18_544 . ? O3 Fe O1 93.51(13) 18_544 . ? O3 Fe O1 97.36(14) . . ? O2 Fe O1 84.47(15) 18_544 . ? O2 Fe O1 86.19(15) . . ? O3 Fe O1 97.36(14) 18_544 18_544 ? O3 Fe O1 93.50(13) . 18_544 ? O2 Fe O1 86.19(15) 18_544 18_544 ? O2 Fe O1 84.46(15) . 18_544 ? O1 Fe O1 166.0(2) . 18_544 ? O3 Cr O3 90.81(11) 16_554 18_544 ? O3 Cr O3 90.80(11) 16_554 17_654 ? O3 Cr O3 90.80(11) 18_544 17_654 ? O3 Cr O3 164.14(18) 16_554 2_655 ? O3 Cr O3 101.46(17) 18_544 2_655 ? O3 Cr O3 79.12(17) 17_654 2_655 ? O3 Cr O3 101.46(17) 16_554 . ? O3 Cr O3 79.13(17) 18_544 . ? O3 Cr O3 164.14(18) 17_654 . ? O3 Cr O3 90.80(11) 2_655 . ? O3 Cr O3 79.13(17) 16_554 3_665 ? O3 Cr O3 164.14(18) 18_544 3_665 ? O3 Cr O3 101.46(17) 17_654 3_665 ? O3 Cr O3 90.80(11) 2_655 3_665 ? O3 Cr O3 90.80(11) . 3_665 ? C12 O3 Cr 118.3(3) . . ? C12 O3 Fe 128.7(3) . . ? Cr O3 Fe 101.20(12) . . ? C5 O1 Fe 129.7(4) . . ? C7 O2 Fe 130.9(4) . . ? C12 C13 C12 111.3(3) 2_655 . ? C12 C13 C12 111.3(3) 2_655 3_665 ? C12 C13 C12 111.3(3) . 3_665 ? C12 C13 C14 107.5(3) 2_655 . ? C12 C13 C14 107.6(3) . . ? C12 C13 C14 107.6(3) 3_665 . ? O3 C12 C13 113.9(4) . . ? O3 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? O3 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O1 C5 C6 123.6(5) . . ? O1 C5 C4 114.9(6) . . ? C6 C5 C4 121.6(6) . . ? O2 C7 C6 123.6(6) . . ? O2 C7 C11 113.3(6) . . ? C6 C7 C11 123.1(7) . . ? C1 C4 C3 111.2(7) . . ? C1 C4 C5 106.9(6) . . ? C3 C4 C5 113.3(7) . . ? C1 C4 C2 110.6(9) . . ? C3 C4 C2 107.8(7) . . ? C5 C4 C2 107.0(6) . . ? C8 C11 C10 112.4(10) . . ? C8 C11 C9 111.2(9) . . ? C10 C11 C9 104.8(9) . . ? C8 C11 C7 107.7(6) . . ? C10 C11 C7 109.0(6) . . ? C9 C11 C7 111.8(7) . . ? C7 C6 C5 124.5(6) . . ? C7 C6 H6 117.8 . . ? C5 C6 H6 117.8 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C11 C9 H9A 109.5 . . ? C11 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C11 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 C8 H8A 109.5 . . ? C11 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C11 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C15 C14 C13 125.8110(10) . . ? C15 C14 H14A 105.9 . . ? C13 C14 H14A 105.9 . . ? C15 C14 H14B 105.9 . . ? C13 C14 H14B 105.9 . . ? H14A C14 H14B 106.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cr O3 C12 125.2(4) 16_554 . . . ? O3 Cr O3 C12 -146.2(4) 18_544 . . . ? O3 Cr O3 C12 -94.8(3) 17_654 . . . ? O3 Cr O3 C12 -44.6(3) 2_655 . . . ? O3 Cr O3 C12 46.2(3) 3_665 . . . ? O3 Cr O3 Fe -88.60(12) 16_554 . . . ? O3 Cr O3 Fe 0 18_544 . . . ? O3 Cr O3 Fe 51.41(10) 17_654 . . . ? O3 Cr O3 Fe 101.52(19) 2_655 . . . ? O3 Cr O3 Fe -167.67(15) 3_665 . . . ? O3 Fe O3 C12 141.1(4) 18_544 . . . ? O2 Fe O3 C12 132.1(9) 18_544 . . . ? O2 Fe O3 C12 -40.3(4) . . . . ? O1 Fe O3 C12 -126.8(4) . . . . ? O1 Fe O3 C12 44.3(4) 18_544 . . . ? O3 Fe O3 Cr 0 18_544 . . . ? O2 Fe O3 Cr -9.0(9) 18_544 . . . ? O2 Fe O3 Cr 178.58(15) . . . . ? O1 Fe O3 Cr 92.09(15) . . . . ? O1 Fe O3 Cr -96.81(15) 18_544 . . . ? O3 Fe O1 C5 -175.5(5) 18_544 . . . ? O3 Fe O1 C5 105.7(5) . . . . ? O2 Fe O1 C5 -83.2(5) 18_544 . . . ? O2 Fe O1 C5 13.6(5) . . . . ? O1 Fe O1 C5 -34.7(5) 18_544 . . . ? O3 Fe O2 C7 -99.1(10) 18_544 . . . ? O3 Fe O2 C7 -107.9(5) . . . . ? O2 Fe O2 C7 73.3(5) 18_544 . . . ? O1 Fe O2 C7 -10.7(5) . . . . ? O1 Fe O2 C7 158.8(5) 18_544 . . . ? Cr O3 C12 C13 -1.4(5) . . . . ? Fe O3 C12 C13 -137.0(3) . . . . ? C12 C13 C12 O3 63.2(5) 2_655 . . . ? C12 C13 C12 O3 -61.6(5) 3_665 . . . ? C14 C13 C12 O3 -179.2(3) . . . . ? Fe O1 C5 C6 -11.5(8) . . . . ? Fe O1 C5 C4 168.9(4) . . . . ? Fe O2 C7 C6 5.5(9) . . . . ? Fe O2 C7 C11 -174.6(4) . . . . ? O1 C5 C4 C1 -62.5(9) . . . . ? C6 C5 C4 C1 117.8(8) . . . . ? O1 C5 C4 C3 174.6(6) . . . . ? C6 C5 C4 C3 -5.1(9) . . . . ? O1 C5 C4 C2 55.9(8) . . . . ? C6 C5 C4 C2 -123.8(8) . . . . ? O2 C7 C11 C8 74.3(10) . . . . ? C6 C7 C11 C8 -105.8(10) . . . . ? O2 C7 C11 C10 -47.9(9) . . . . ? C6 C7 C11 C10 132.0(8) . . . . ? O2 C7 C11 C9 -163.2(9) . . . . ? C6 C7 C11 C9 16.7(11) . . . . ? O2 C7 C6 C5 2.4(10) . . . . ? C11 C7 C6 C5 -177.5(6) . . . . ? O1 C5 C6 C7 0.7(10) . . . . ? C4 C5 C6 C7 -179.6(6) . . . . ? C12 C13 C14 C15 -63.9(2) 2_655 . . . ? C12 C13 C14 C15 176.2(2) . . . . ? C12 C13 C14 C15 56.1(2) 3_665 . . . ? data_Fe3CrPh _database_code_depnum_ccdc_archive 'CCDC 904915' #TrackingRef 'PhFeCr_19-08-2012_Pasquale1.cif' _audit_creation_date 2012-08-13T11:36:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(m4-2-(oxymethyl)-2-phenylpropane-1,3-diolato)-hexakis(dipivaloylmethanato)-chromium(III)-tri-iron(III) dimethoxyethane solvate ; _chemical_name_common 'iron and chromium phenyl alkoxide' _chemical_formula_moiety 'C90 H146 Cr Fe3 O20' _chemical_formula_sum 'C90 H146 Cr Fe3 O20' _chemical_formula_weight 1767.62 _chemical_melting_point none #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.6204(7) _cell_length_b 22.0622(7) _cell_length_c 24.7198(9) _cell_angle_alpha 90 _cell_angle_beta 107.964(2) _cell_angle_gamma 90 _cell_volume 10178.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.492 _cell_measurement_theta_max 26.7735 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description tabular _exptl_crystal_colour brown _exptl_crystal_size_max 0.554 _exptl_crystal_size_mid 0.207 _exptl_crystal_size_min 0.128 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_special_details ; XPREP (Bruker, 2006) was used to perform the Gaussian absorption correction based on the face-indexed crystal size ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.583 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details XPREP _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_T_max 0.942 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean none _diffrn_measurement_device_type 'X8 APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_number 73182 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.8 _diffrn_reflns_theta_full 26.8 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 10712 _reflns_number_gt 6747 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER APEX-II' _computing_cell_refinement 'BRUKER SANT' _computing_data_reduction 'BRUKER SOFTWARE' _computing_structure_solution 'SHELXL97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1319P)^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 none _refine_ls_number_reflns 10712 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.2188 _refine_ls_wR_factor_gt 0.1958 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.095 _refine_ls_shift/su_mean 0.019 _refine_diff_density_max 0.77 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.075 # 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 0.000 0.170 0.250 357 43 ' ' 2 0.000 0.830 0.750 357 43 ' ' 3 0.500 0.330 0.750 357 43 ' ' 4 0.500 0.670 0.250 357 43 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.5 0.09678(3) 0.25 0.0522(2) Uani 1 2 d S . . Cr Cr 0.5 0.23357(3) 0.25 0.0437(2) Uani 1 2 d S . . Fe2 Fe 0.50211(2) 0.30082(2) 0.357038(19) 0.04770(18) Uani 1 1 d . . . O8 O 0.56048(12) 0.16593(10) 0.28716(10) 0.0501(6) Uani 1 1 d . . . O3 O 0.44716(13) 0.37303(11) 0.31876(10) 0.0573(6) Uani 1 1 d . . . O7 O 0.56086(11) 0.28911(10) 0.30581(9) 0.0462(5) Uani 1 1 d . . . O5 O 0.43460(14) 0.29992(12) 0.40315(11) 0.0652(7) Uani 1 1 d . . . O9 O 0.44080(12) 0.24454(10) 0.29994(9) 0.0474(5) Uani 1 1 d . . . O6 O 0.55670(13) 0.23802(12) 0.41058(10) 0.0596(6) Uani 1 1 d . . . O4 O 0.57074(13) 0.36041(12) 0.40606(11) 0.0644(7) Uani 1 1 d . . . O2 O 0.55982(13) 0.08675(11) 0.19742(11) 0.0599(6) Uani 1 1 d . . . O1 O 0.43633(14) 0.03465(12) 0.20042(12) 0.0661(7) Uani 1 1 d . . . C35 C 0.66156(18) 0.23397(16) 0.28859(14) 0.0495(8) Uani 1 1 d . . . C38 C 0.74402(19) 0.23667(18) 0.30670(15) 0.0576(9) Uani 1 1 d . . . C16 C 0.4517(2) 0.42790(18) 0.33478(16) 0.0600(9) Uani 1 1 d . . . C7 C 0.5611(2) 0.04432(18) 0.16418(17) 0.0616(10) Uani 1 1 d . . . C5 C 0.4498(2) -0.00237(18) 0.16622(17) 0.0658(10) Uani 1 1 d . . . C36 C 0.36545(18) 0.24600(18) 0.27635(14) 0.0542(9) Uani 1 1 d . . . H36A H 0.3483 0.2854 0.2838 0.065 Uiso 1 1 calc R . . H36B H 0.3449 0.2158 0.2953 0.065 Uiso 1 1 calc R . . C27 C 0.5483(2) 0.21685(16) 0.45470(15) 0.0562(9) Uani 1 1 d . . . C37 C 0.63699(18) 0.28397(17) 0.32121(16) 0.0544(9) Uani 1 1 d . . . H37A H 0.6559 0.2757 0.3616 0.065 Uiso 1 1 calc R . . H37B H 0.6567 0.3224 0.314 0.065 Uiso 1 1 calc R . . C12 C 0.3901(2) 0.46773(19) 0.2993(2) 0.0738(12) Uani 1 1 d . . . C18 C 0.5635(2) 0.41607(19) 0.41379(18) 0.0661(10) Uani 1 1 d . . . C34 C 0.63657(19) 0.17162(16) 0.30200(16) 0.0557(9) Uani 1 1 d . . . H34A H 0.6545 0.141 0.2817 0.067 Uiso 1 1 calc R . . H34B H 0.6573 0.1638 0.3424 0.067 Uiso 1 1 calc R . . C23 C 0.6080(2) 0.17310(19) 0.48755(17) 0.0691(11) Uani 1 1 d . . . C29 C 0.4380(2) 0.2706(2) 0.44848(19) 0.0737(11) Uani 1 1 d . . . C1 C 0.3914(3) -0.0528(2) 0.1446(2) 0.0932(16) Uani 1 1 d . . . C6 C 0.5094(2) -0.0007(2) 0.14912(19) 0.0759(12) Uani 1 1 d . . . H6 H 0.5158 -0.0318 0.1258 0.091 Uiso 1 1 calc R . . C8 C 0.6230(3) 0.0441(2) 0.1398(2) 0.0857(14) Uani 1 1 d . . . C28 C 0.4901(3) 0.2306(2) 0.4731(2) 0.0887(15) Uani 1 1 d . . . H28 H 0.4869 0.2105 0.5053 0.106 Uiso 1 1 calc R . . C43 C 0.7875(2) 0.1896(2) 0.3352(2) 0.0801(13) Uani 1 1 d . . . H43 H 0.7668 0.1545 0.3438 0.096 Uiso 1 1 calc R . . C17 C 0.5060(2) 0.44952(19) 0.3804(2) 0.0800(13) Uani 1 1 d . . . H17 H 0.5039 0.4902 0.3897 0.096 Uiso 1 1 calc R . . C39 C 0.7785(2) 0.2876(2) 0.2966(2) 0.0789(12) Uani 1 1 d . . . H39 H 0.7513 0.3206 0.2789 0.095 Uiso 1 1 calc R . . C30 C 0.3760(4) 0.2826(3) 0.4711(3) 0.129(3) Uani 1 1 d . . . C42 C 0.8614(3) 0.1944(3) 0.3509(2) 0.0961(16) Uani 1 1 d . . . H42 H 0.8893 0.1623 0.3701 0.115 Uiso 1 1 calc R . . C19 C 0.6245(3) 0.4449(2) 0.4609(2) 0.0959(17) Uani 1 1 d . . . C40 C 0.8528(3) 0.2913(3) 0.3119(2) 0.0948(16) Uani 1 1 d . . . H40 H 0.8742 0.3261 0.3035 0.114 Uiso 1 1 calc R . . C41 C 0.8942(3) 0.2446(3) 0.3391(2) 0.0967(17) Uani 1 1 d . . . H41 H 0.9439 0.2468 0.3493 0.116 Uiso 1 1 calc R . . C15 C 0.3873(4) 0.4638(3) 0.2382(2) 0.131(2) Uani 1 1 d . . . H15A H 0.3489 0.4886 0.2155 0.197 Uiso 1 1 calc R . . H15B H 0.3794 0.4225 0.2256 0.197 Uiso 1 1 calc R . . H15C H 0.4319 0.4777 0.2342 0.197 Uiso 1 1 calc R . . C4 C 0.4057(5) -0.0907(5) 0.1011(5) 0.293(8) Uani 1 1 d . . . H4A H 0.4132 -0.0654 0.0718 0.44 Uiso 1 1 calc R . . H4B H 0.3655 -0.1169 0.0849 0.44 Uiso 1 1 calc R . . H4C H 0.4478 -0.1146 0.1179 0.44 Uiso 1 1 calc R . . C3 C 0.3811(5) -0.0839(3) 0.1944(3) 0.174(4) Uani 1 1 d . . . H3A H 0.3708 -0.0545 0.2194 0.262 Uiso 1 1 calc R . . H3B H 0.424 -0.1055 0.2142 0.262 Uiso 1 1 calc R . . H3C H 0.3419 -0.1118 0.1819 0.262 Uiso 1 1 calc R . . C14 C 0.3955(4) 0.5326(3) 0.3202(3) 0.169(4) Uani 1 1 d . . . H14A H 0.3973 0.5331 0.3594 0.253 Uiso 1 1 calc R . . H14B H 0.3544 0.5549 0.298 0.253 Uiso 1 1 calc R . . H14C H 0.4382 0.5508 0.3164 0.253 Uiso 1 1 calc R . . C13 C 0.3212(3) 0.4397(4) 0.3030(3) 0.165(3) Uani 1 1 d . . . H13A H 0.3201 0.442 0.3415 0.247 Uiso 1 1 calc R . . H13B H 0.3188 0.3981 0.2914 0.247 Uiso 1 1 calc R . . H13C H 0.281 0.4614 0.2786 0.247 Uiso 1 1 calc R . . C24 C 0.6097(4) 0.1215(3) 0.4488(2) 0.127(2) Uani 1 1 d . . . H24A H 0.5636 0.1021 0.4368 0.191 Uiso 1 1 calc R . . H24B H 0.6455 0.0928 0.4685 0.191 Uiso 1 1 calc R . . H24C H 0.6209 0.1365 0.4161 0.191 Uiso 1 1 calc R . . C22 C 0.6432(4) 0.4044(4) 0.5116(3) 0.169(3) Uani 1 1 d . . . H22A H 0.6562 0.3652 0.5012 0.254 Uiso 1 1 calc R . . H22B H 0.6026 0.4006 0.5253 0.254 Uiso 1 1 calc R . . H22C H 0.6828 0.4214 0.5409 0.254 Uiso 1 1 calc R . . C26 C 0.5895(4) 0.1424(3) 0.5388(3) 0.155(3) Uani 1 1 d . . . H26A H 0.5468 0.1185 0.5246 0.232 Uiso 1 1 calc R . . H26B H 0.582 0.1731 0.5638 0.232 Uiso 1 1 calc R . . H26C H 0.6285 0.1167 0.5592 0.232 Uiso 1 1 calc R . . C20 C 0.6095(5) 0.5040(4) 0.4761(5) 0.309(10) Uani 1 1 d . . . H20A H 0.5976 0.5296 0.443 0.463 Uiso 1 1 calc R . . H20B H 0.6509 0.52 0.5043 0.463 Uiso 1 1 calc R . . H20C H 0.5699 0.5027 0.4911 0.463 Uiso 1 1 calc R . . C2 C 0.3197(4) -0.0201(4) 0.1154(4) 0.192(4) Uani 1 1 d . . . H2A H 0.3084 0.0065 0.1422 0.289 Uiso 1 1 calc R . . H2B H 0.2822 -0.0495 0.1022 0.289 Uiso 1 1 calc R . . H2C H 0.324 0.0031 0.0838 0.289 Uiso 1 1 calc R . . C11 C 0.6006(5) 0.0542(9) 0.0817(5) 0.412(14) Uani 1 1 d . . . H11A H 0.5603 0.0286 0.0639 0.618 Uiso 1 1 calc R . . H11B H 0.639 0.0451 0.0666 0.618 Uiso 1 1 calc R . . H11C H 0.5869 0.0959 0.0743 0.618 Uiso 1 1 calc R . . C31 C 0.3651(6) 0.2387(5) 0.5093(6) 0.265(7) Uani 1 1 d . . . H31A H 0.4103 0.2279 0.5361 0.398 Uiso 1 1 calc R . . H31B H 0.3431 0.2034 0.4885 0.398 Uiso 1 1 calc R . . H31C H 0.3344 0.2551 0.5293 0.398 Uiso 1 1 calc R . . C25 C 0.6740(3) 0.2089(3) 0.5096(4) 0.173(4) Uani 1 1 d . . . H25A H 0.6663 0.2406 0.5338 0.259 Uiso 1 1 calc R . . H25B H 0.6865 0.2265 0.4784 0.259 Uiso 1 1 calc R . . H25C H 0.7121 0.1831 0.5311 0.259 Uiso 1 1 calc R . . C21 C 0.6898(3) 0.4437(4) 0.4374(4) 0.179(4) Uani 1 1 d . . . H21A H 0.6966 0.4032 0.4258 0.268 Uiso 1 1 calc R . . H21B H 0.7321 0.4566 0.4666 0.268 Uiso 1 1 calc R . . H21C H 0.6808 0.4705 0.4053 0.268 Uiso 1 1 calc R . . C10 C 0.6606(4) -0.0192(5) 0.1521(4) 0.202(4) Uani 1 1 d . . . H10A H 0.6278 -0.0501 0.1326 0.303 Uiso 1 1 calc R . . H10B H 0.6752 -0.0269 0.1923 0.303 Uiso 1 1 calc R . . H10C H 0.7019 -0.0193 0.1391 0.303 Uiso 1 1 calc R . . C32 C 0.3960(11) 0.3373(7) 0.5045(10) 0.428(16) Uani 1 1 d . . . H32A H 0.4379 0.3297 0.5363 0.642 Uiso 1 1 calc R . . H32B H 0.3573 0.3498 0.5181 0.642 Uiso 1 1 calc R . . H32C H 0.4061 0.3689 0.4813 0.642 Uiso 1 1 calc R . . C9 C 0.6828(5) 0.0809(5) 0.1737(5) 0.290(8) Uani 1 1 d . . . H9A H 0.721 0.0798 0.157 0.435 Uiso 1 1 calc R . . H9B H 0.6997 0.0651 0.2117 0.435 Uiso 1 1 calc R . . H9C H 0.6672 0.122 0.1747 0.435 Uiso 1 1 calc R . . C33 C 0.3146(6) 0.3047(9) 0.4284(6) 0.386(14) Uani 1 1 d . . . H33A H 0.3289 0.3352 0.4064 0.579 Uiso 1 1 calc R . . H33B H 0.2817 0.322 0.446 0.579 Uiso 1 1 calc R . . H33C H 0.2916 0.2719 0.404 0.579 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 0.0583(4) 0.0413(4) 0.0662(5) 0 0.0328(3) 0 Cr 0.0501(4) 0.0401(4) 0.0447(4) 0 0.0205(3) 0 Fe2 0.0500(3) 0.0511(3) 0.0427(3) 0.0014(2) 0.0152(2) 0.0124(2) O8 0.0544(14) 0.0456(13) 0.0543(13) 0.0041(10) 0.0228(11) 0.0060(10) O3 0.0581(14) 0.0517(15) 0.0577(14) -0.0011(12) 0.0115(11) 0.0129(12) O7 0.0474(12) 0.0468(13) 0.0467(12) -0.0025(10) 0.0178(10) 0.0049(10) O5 0.0657(16) 0.0817(19) 0.0543(14) 0.0069(14) 0.0277(12) 0.0241(14) O9 0.0498(13) 0.0494(13) 0.0461(12) 0.0018(10) 0.0194(10) 0.0036(10) O6 0.0597(15) 0.0692(17) 0.0532(14) 0.0157(12) 0.0225(11) 0.0208(13) O4 0.0597(15) 0.0604(17) 0.0640(16) -0.0106(13) 0.0056(12) 0.0127(13) O2 0.0638(15) 0.0539(15) 0.0729(16) -0.0079(13) 0.0372(13) -0.0068(12) O1 0.0661(16) 0.0529(15) 0.0886(19) -0.0146(14) 0.0376(14) -0.0103(13) C35 0.0487(18) 0.051(2) 0.0518(18) -0.0003(16) 0.0199(14) 0.0044(15) C38 0.053(2) 0.063(2) 0.059(2) -0.0062(18) 0.0221(16) 0.0058(18) C16 0.058(2) 0.057(2) 0.067(2) -0.0033(19) 0.0227(18) 0.0126(18) C7 0.065(2) 0.057(2) 0.068(2) -0.0087(19) 0.0289(19) 0.0050(19) C5 0.076(3) 0.052(2) 0.069(2) -0.0040(19) 0.021(2) -0.0093(19) C36 0.0496(19) 0.062(2) 0.058(2) 0.0023(17) 0.0256(16) -0.0042(17) C27 0.066(2) 0.053(2) 0.0475(19) 0.0024(16) 0.0141(17) 0.0040(17) C37 0.051(2) 0.053(2) 0.060(2) -0.0088(17) 0.0201(16) -0.0021(16) C12 0.073(3) 0.053(2) 0.092(3) 0.009(2) 0.020(2) 0.019(2) C18 0.058(2) 0.063(3) 0.078(3) -0.014(2) 0.0211(19) 0.0071(19) C34 0.053(2) 0.052(2) 0.060(2) 0.0021(17) 0.0155(16) 0.0043(16) C23 0.080(3) 0.060(3) 0.062(2) 0.015(2) 0.015(2) 0.015(2) C29 0.079(3) 0.074(3) 0.082(3) 0.005(2) 0.045(2) 0.010(2) C1 0.105(4) 0.080(3) 0.096(3) -0.026(3) 0.034(3) -0.039(3) C6 0.080(3) 0.070(3) 0.089(3) -0.028(2) 0.042(2) -0.007(2) C8 0.081(3) 0.096(4) 0.095(3) -0.022(3) 0.050(3) 0.001(3) C28 0.116(4) 0.084(3) 0.088(3) 0.033(3) 0.063(3) 0.034(3) C43 0.063(3) 0.070(3) 0.101(3) 0.001(2) 0.016(2) 0.007(2) C17 0.071(3) 0.053(3) 0.106(3) -0.015(2) 0.013(2) 0.010(2) C39 0.058(2) 0.082(3) 0.093(3) 0.010(2) 0.018(2) -0.005(2) C30 0.160(6) 0.120(5) 0.162(6) 0.051(4) 0.133(5) 0.068(4) C42 0.060(3) 0.096(4) 0.122(4) -0.005(3) 0.012(3) 0.021(3) C19 0.081(3) 0.080(3) 0.106(4) -0.034(3) 0.000(3) 0.004(3) C40 0.066(3) 0.123(5) 0.099(4) -0.003(3) 0.031(3) -0.019(3) C41 0.056(3) 0.121(5) 0.109(4) -0.024(3) 0.019(3) 0.013(3) C15 0.161(6) 0.128(5) 0.089(4) 0.031(4) 0.017(4) 0.066(4) C4 0.245(10) 0.311(13) 0.413(16) -0.300(13) 0.231(11) -0.215(10) C3 0.228(9) 0.127(6) 0.160(7) 0.011(5) 0.048(6) -0.108(6) C14 0.180(7) 0.088(4) 0.188(7) -0.021(4) -0.016(6) 0.080(5) C13 0.077(4) 0.205(8) 0.221(8) 0.099(7) 0.057(5) 0.073(5) C24 0.164(6) 0.111(5) 0.103(4) 0.016(4) 0.036(4) 0.073(4) C22 0.189(8) 0.193(8) 0.091(4) -0.034(5) -0.008(5) -0.053(6) C26 0.200(7) 0.164(6) 0.110(5) 0.083(5) 0.064(5) 0.079(6) C20 0.184(9) 0.205(10) 0.377(17) -0.192(11) -0.148(10) 0.077(7) C2 0.103(5) 0.175(7) 0.238(10) 0.054(7) -0.038(6) -0.057(5) C11 0.128(7) 0.93(4) 0.223(11) 0.332(18) 0.125(8) 0.156(14) C31 0.262(11) 0.234(11) 0.428(17) 0.170(12) 0.296(13) 0.126(10) C25 0.084(4) 0.122(5) 0.242(9) 0.058(5) -0.053(5) -0.005(4) C21 0.084(4) 0.251(10) 0.179(7) -0.013(7) 0.008(5) -0.053(5) C10 0.114(6) 0.314(13) 0.203(9) 0.014(9) 0.085(6) 0.073(7) C32 0.46(3) 0.346(19) 0.67(4) -0.29(2) 0.46(3) -0.080(19) C9 0.192(8) 0.337(13) 0.445(17) -0.299(13) 0.251(11) -0.176(9) C33 0.185(10) 0.72(3) 0.345(17) 0.35(2) 0.210(12) 0.267(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O8 1.977(2) . ? Fe1 O8 1.977(2) 2_655 ? Fe1 O1 1.999(3) . ? Fe1 O1 1.999(3) 2_655 ? Fe1 O2 2.014(2) 2_655 ? Fe1 O2 2.014(2) . ? Cr O8 1.951(2) 2_655 ? Cr O8 1.951(2) . ? Cr O7 1.953(2) . ? Cr O7 1.953(2) 2_655 ? Cr O9 1.953(2) . ? Cr O9 1.953(2) 2_655 ? Fe2 O7 1.975(2) . ? Fe2 O9 1.983(2) . ? Fe2 O6 1.986(2) . ? Fe2 O3 1.991(2) . ? Fe2 O5 1.996(3) . ? Fe2 O4 2.001(3) . ? O8 C34 1.429(4) . ? O3 C16 1.268(4) . ? O7 C37 1.428(4) . ? O5 C29 1.278(5) . ? O9 C36 1.413(4) . ? O6 C27 1.243(4) . ? O4 C18 1.258(4) . ? O2 C7 1.251(4) . ? O1 C5 1.261(5) . ? C35 C37 1.529(5) . ? C35 C34 1.531(5) . ? C35 C38 1.541(5) . ? C35 C36 1.550(5) 2_655 ? C38 C39 1.373(5) . ? C38 C43 1.390(5) . ? C16 C17 1.375(6) . ? C16 C12 1.533(5) . ? C7 C6 1.387(5) . ? C7 C8 1.513(6) . ? C5 C6 1.360(6) . ? C5 C1 1.568(6) . ? C36 C35 1.550(5) 2_655 ? C36 H36A 0.97 . ? C36 H36B 0.97 . ? C27 C28 1.386(6) . ? C27 C23 1.542(5) . ? C37 H37A 0.97 . ? C37 H37B 0.97 . ? C12 C15 1.497(7) . ? C12 C13 1.516(8) . ? C12 C14 1.514(7) . ? C18 C17 1.388(5) . ? C18 C19 1.528(6) . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C23 C25 1.470(7) . ? C23 C24 1.495(7) . ? C23 C26 1.575(7) . ? C29 C28 1.344(6) . ? C29 C30 1.512(6) . ? C1 C4 1.457(8) . ? C1 C3 1.475(8) . ? C1 C2 1.547(9) . ? C6 H6 0.93 . ? C8 C11 1.384(10) . ? C8 C9 1.461(9) . ? C8 C10 1.564(10) . ? C28 H28 0.93 . ? C43 C42 1.383(6) . ? C43 H43 0.93 . ? C17 H17 0.93 . ? C39 C40 1.391(6) . ? C39 H39 0.93 . ? C30 C33 1.421(12) . ? C30 C31 1.413(9) . ? C30 C32 1.448(14) . ? C42 C41 1.358(7) . ? C42 H42 0.93 . ? C19 C20 1.412(9) . ? C19 C22 1.490(9) . ? C19 C21 1.564(9) . ? C40 C41 1.355(7) . ? C40 H40 0.93 . ? C41 H41 0.93 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C33 H33A 0.96 . ? C33 H33B 0.96 . ? C33 H33C 0.96 . ? 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 O8 Fe1 O8 78.96(13) . 2_655 ? O8 Fe1 O1 170.44(11) . . ? O8 Fe1 O1 94.14(10) 2_655 . ? O8 Fe1 O1 94.14(10) . 2_655 ? O8 Fe1 O1 170.44(11) 2_655 2_655 ? O1 Fe1 O1 93.43(16) . 2_655 ? O8 Fe1 O2 99.83(10) . 2_655 ? O8 Fe1 O2 89.93(10) 2_655 2_655 ? O1 Fe1 O2 86.68(11) . 2_655 ? O1 Fe1 O2 84.68(10) 2_655 2_655 ? O8 Fe1 O2 89.93(10) . . ? O8 Fe1 O2 99.83(10) 2_655 . ? O1 Fe1 O2 84.68(10) . . ? O1 Fe1 O2 86.68(11) 2_655 . ? O2 Fe1 O2 167.39(14) 2_655 . ? O8 Cr O8 80.21(14) 2_655 . ? O8 Cr O7 164.37(9) 2_655 . ? O8 Cr O7 89.81(9) . . ? O8 Cr O7 89.81(9) 2_655 2_655 ? O8 Cr O7 164.37(9) . 2_655 ? O7 Cr O7 102.28(13) . 2_655 ? O8 Cr O9 89.91(9) 2_655 . ? O8 Cr O9 101.02(10) . . ? O7 Cr O9 80.16(9) . . ? O7 Cr O9 90.89(9) 2_655 . ? O8 Cr O9 101.02(10) 2_655 2_655 ? O8 Cr O9 89.91(9) . 2_655 ? O7 Cr O9 90.89(9) . 2_655 ? O7 Cr O9 80.16(9) 2_655 2_655 ? O9 Cr O9 165.77(13) . 2_655 ? O7 Fe2 O9 78.91(9) . . ? O7 Fe2 O6 91.98(9) . . ? O9 Fe2 O6 96.98(10) . . ? O7 Fe2 O3 97.90(10) . . ? O9 Fe2 O3 92.41(9) . . ? O6 Fe2 O3 167.52(10) . . ? O7 Fe2 O5 170.46(10) . . ? O9 Fe2 O5 92.10(10) . . ? O6 Fe2 O5 85.92(10) . . ? O3 Fe2 O5 85.52(10) . . ? O7 Fe2 O4 93.29(10) . . ? O9 Fe2 O4 171.69(10) . . ? O6 Fe2 O4 86.04(11) . . ? O3 Fe2 O4 85.80(10) . . ? O5 Fe2 O4 95.84(11) . . ? C34 O8 Cr 119.3(2) . . ? C34 O8 Fe1 128.1(2) . . ? Cr O8 Fe1 100.41(11) . . ? C16 O3 Fe2 129.7(2) . . ? C37 O7 Cr 120.00(19) . . ? C37 O7 Fe2 127.5(2) . . ? Cr O7 Fe2 100.62(10) . . ? C29 O5 Fe2 129.8(3) . . ? C36 O9 Cr 119.51(19) . . ? C36 O9 Fe2 127.4(2) . . ? Cr O9 Fe2 100.31(10) . . ? C27 O6 Fe2 131.0(2) . . ? C18 O4 Fe2 130.3(2) . . ? C7 O2 Fe1 129.8(2) . . ? C5 O1 Fe1 129.4(3) . . ? C37 C35 C34 111.1(3) . . ? C37 C35 C38 107.0(3) . . ? C34 C35 C38 110.5(3) . . ? C37 C35 C36 111.1(3) . 2_655 ? C34 C35 C36 110.4(3) . 2_655 ? C38 C35 C36 106.7(3) . 2_655 ? C39 C38 C43 116.3(4) . . ? C39 C38 C35 120.7(3) . . ? C43 C38 C35 123.0(4) . . ? O3 C16 C17 123.3(3) . . ? O3 C16 C12 113.6(3) . . ? C17 C16 C12 123.0(4) . . ? O2 C7 C6 123.4(4) . . ? O2 C7 C8 116.5(4) . . ? C6 C7 C8 120.1(4) . . ? O1 C5 C6 124.7(4) . . ? O1 C5 C1 113.9(4) . . ? C6 C5 C1 121.5(4) . . ? O9 C36 C35 113.8(3) . 2_655 ? O9 C36 H36A 108.8 . . ? C35 C36 H36A 108.8 2_655 . ? O9 C36 H36B 108.8 . . ? C35 C36 H36B 108.8 2_655 . ? H36A C36 H36B 107.7 . . ? O6 C27 C28 123.4(4) . . ? O6 C27 C23 114.3(3) . . ? C28 C27 C23 122.2(4) . . ? O7 C37 C35 113.0(3) . . ? O7 C37 H37A 109 . . ? C35 C37 H37A 109 . . ? O7 C37 H37B 109 . . ? C35 C37 H37B 109 . . ? H37A C37 H37B 107.8 . . ? C15 C12 C13 106.4(5) . . ? C15 C12 C14 112.1(5) . . ? C13 C12 C14 109.5(6) . . ? C15 C12 C16 108.8(4) . . ? C13 C12 C16 107.0(4) . . ? C14 C12 C16 112.8(4) . . ? O4 C18 C17 122.6(4) . . ? O4 C18 C19 115.1(4) . . ? C17 C18 C19 122.3(4) . . ? O8 C34 C35 113.7(3) . . ? O8 C34 H34A 108.8 . . ? C35 C34 H34A 108.8 . . ? O8 C34 H34B 108.8 . . ? C35 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C25 C23 C24 117.2(6) . . ? C25 C23 C27 107.3(4) . . ? C24 C23 C27 107.6(3) . . ? C25 C23 C26 109.1(6) . . ? C24 C23 C26 104.1(5) . . ? C27 C23 C26 111.5(4) . . ? O5 C29 C28 123.8(4) . . ? O5 C29 C30 113.9(4) . . ? C28 C29 C30 122.3(4) . . ? C4 C1 C3 117.1(7) . . ? C4 C1 C2 106.1(7) . . ? C3 C1 C2 105.5(6) . . ? C4 C1 C5 111.8(5) . . ? C3 C1 C5 108.6(4) . . ? C2 C1 C5 107.0(4) . . ? C5 C6 C7 124.4(4) . . ? C5 C6 H6 117.8 . . ? C7 C6 H6 117.8 . . ? C11 C8 C9 116.6(9) . . ? C11 C8 C7 112.1(5) . . ? C9 C8 C7 111.7(4) . . ? C11 C8 C10 109.1(9) . . ? C9 C8 C10 97.8(7) . . ? C7 C8 C10 108.3(5) . . ? C29 C28 C27 125.7(4) . . ? C29 C28 H28 117.2 . . ? C27 C28 H28 117.2 . . ? C42 C43 C38 120.8(5) . . ? C42 C43 H43 119.6 . . ? C38 C43 H43 119.6 . . ? C16 C17 C18 125.8(4) . . ? C16 C17 H17 117.1 . . ? C18 C17 H17 117.1 . . ? C38 C39 C40 122.2(4) . . ? C38 C39 H39 118.9 . . ? C40 C39 H39 118.9 . . ? C33 C30 C31 117.6(9) . . ? C33 C30 C32 99.0(11) . . ? C31 C30 C32 105.1(12) . . ? C33 C30 C29 112.3(6) . . ? C31 C30 C29 115.6(5) . . ? C32 C30 C29 104.4(7) . . ? C41 C42 C43 121.7(5) . . ? C41 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? C20 C19 C22 110.4(8) . . ? C20 C19 C18 114.2(5) . . ? C22 C19 C18 108.9(5) . . ? C20 C19 C21 112.1(8) . . ? C22 C19 C21 106.6(6) . . ? C18 C19 C21 104.4(5) . . ? C41 C40 C39 120.5(5) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 118.4(5) . . ? C40 C41 H41 120.8 . . ? C42 C41 H41 120.8 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.4 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C23 C25 H25A 109.4 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C8 C10 H10A 109.4 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C30 C33 H33A 109.4 . . ? C30 C33 H33B 109.4 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 Cr O8 C34 145.4(3) 2_655 . . . ? O7 Cr O8 C34 -46.7(2) . . . . ? O7 Cr O8 C34 94.3(4) 2_655 . . . ? O9 Cr O8 C34 -126.7(2) . . . . ? O9 Cr O8 C34 44.2(2) 2_655 . . . ? O8 Cr O8 Fe1 0 2_655 . . . ? O7 Cr O8 Fe1 167.91(10) . . . . ? O7 Cr O8 Fe1 -51.0(4) 2_655 . . . ? O9 Cr O8 Fe1 87.98(11) . . . . ? O9 Cr O8 Fe1 -101.20(10) 2_655 . . . ? O8 Fe1 O8 C34 -140.9(3) 2_655 . . . ? O1 Fe1 O8 C34 -96.5(6) . . . . ? O1 Fe1 O8 C34 45.8(3) 2_655 . . . ? O2 Fe1 O8 C34 131.1(3) 2_655 . . . ? O2 Fe1 O8 C34 -40.9(3) . . . . ? O8 Fe1 O8 Cr 0 2_655 . . . ? O1 Fe1 O8 Cr 44.4(6) . . . . ? O1 Fe1 O8 Cr -173.31(11) 2_655 . . . ? O2 Fe1 O8 Cr -87.99(11) 2_655 . . . ? O2 Fe1 O8 Cr 100.03(11) . . . . ? O7 Fe2 O3 C16 -108.2(3) . . . . ? O9 Fe2 O3 C16 172.7(3) . . . . ? O6 Fe2 O3 C16 33.9(7) . . . . ? O5 Fe2 O3 C16 80.7(3) . . . . ? O4 Fe2 O3 C16 -15.5(3) . . . . ? O8 Cr O7 C37 94.4(4) 2_655 . . . ? O8 Cr O7 C37 44.4(2) . . . . ? O7 Cr O7 C37 -125.7(3) 2_655 . . . ? O9 Cr O7 C37 145.6(2) . . . . ? O9 Cr O7 C37 -45.5(2) 2_655 . . . ? O8 Cr O7 Fe2 -51.1(4) 2_655 . . . ? O8 Cr O7 Fe2 -101.11(10) . . . . ? O7 Cr O7 Fe2 88.87(9) 2_655 . . . ? O9 Cr O7 Fe2 0.11(9) . . . . ? O9 Cr O7 Fe2 168.98(10) 2_655 . . . ? O9 Fe2 O7 C37 -141.9(3) . . . . ? O6 Fe2 O7 C37 -45.1(3) . . . . ? O3 Fe2 O7 C37 127.2(3) . . . . ? O5 Fe2 O7 C37 -122.3(6) . . . . ? O4 Fe2 O7 C37 41.0(3) . . . . ? O9 Fe2 O7 Cr -0.11(9) . . . . ? O6 Fe2 O7 Cr 96.62(11) . . . . ? O3 Fe2 O7 Cr -91.02(10) . . . . ? O5 Fe2 O7 Cr 19.5(6) . . . . ? O4 Fe2 O7 Cr -177.24(10) . . . . ? O7 Fe2 O5 C29 81.2(7) . . . . ? O9 Fe2 O5 C29 100.5(4) . . . . ? O6 Fe2 O5 C29 3.6(4) . . . . ? O3 Fe2 O5 C29 -167.3(4) . . . . ? O4 Fe2 O5 C29 -82.0(4) . . . . ? O8 Cr O9 C36 -47.9(2) 2_655 . . . ? O8 Cr O9 C36 -127.9(2) . . . . ? O7 Cr O9 C36 144.2(2) . . . . ? O7 Cr O9 C36 41.9(2) 2_655 . . . ? O9 Cr O9 C36 92.5(2) 2_655 . . . ? O8 Cr O9 Fe2 167.77(10) 2_655 . . . ? O8 Cr O9 Fe2 87.76(11) . . . . ? O7 Cr O9 Fe2 -0.11(9) . . . . ? O7 Cr O9 Fe2 -102.42(10) 2_655 . . . ? O9 Cr O9 Fe2 -51.79(7) 2_655 . . . ? O7 Fe2 O9 C36 -140.2(3) . . . . ? O6 Fe2 O9 C36 129.2(2) . . . . ? O3 Fe2 O9 C36 -42.6(3) . . . . ? O5 Fe2 O9 C36 43.0(3) . . . . ? O4 Fe2 O9 C36 -120.0(7) . . . . ? O7 Fe2 O9 Cr 0.11(9) . . . . ? O6 Fe2 O9 Cr -90.55(10) . . . . ? O3 Fe2 O9 Cr 97.69(11) . . . . ? O5 Fe2 O9 Cr -176.70(10) . . . . ? O4 Fe2 O9 Cr 20.3(7) . . . . ? O7 Fe2 O6 C27 -176.3(3) . . . . ? O9 Fe2 O6 C27 -97.2(3) . . . . ? O3 Fe2 O6 C27 41.3(7) . . . . ? O5 Fe2 O6 C27 -5.6(3) . . . . ? O4 Fe2 O6 C27 90.6(3) . . . . ? O7 Fe2 O4 C18 113.5(4) . . . . ? O9 Fe2 O4 C18 93.7(7) . . . . ? O6 Fe2 O4 C18 -154.7(4) . . . . ? O3 Fe2 O4 C18 15.8(4) . . . . ? O5 Fe2 O4 C18 -69.2(4) . . . . ? O8 Fe1 O2 C7 168.4(3) . . . . ? O8 Fe1 O2 C7 -112.9(3) 2_655 . . . ? O1 Fe1 O2 C7 -19.6(3) . . . . ? O1 Fe1 O2 C7 74.2(3) 2_655 . . . ? O2 Fe1 O2 C7 27.4(3) 2_655 . . . ? O8 Fe1 O1 C5 74.5(7) . . . . ? O8 Fe1 O1 C5 118.1(3) 2_655 . . . ? O1 Fe1 O1 C5 -67.8(3) 2_655 . . . ? O2 Fe1 O1 C5 -152.3(3) 2_655 . . . ? O2 Fe1 O1 C5 18.5(3) . . . . ? C37 C35 C38 C39 -61.7(5) . . . . ? C34 C35 C38 C39 177.3(4) . . . . ? C36 C35 C38 C39 57.3(5) 2_655 . . . ? C37 C35 C38 C43 116.4(4) . . . . ? C34 C35 C38 C43 -4.7(5) . . . . ? C36 C35 C38 C43 -124.7(4) 2_655 . . . ? Fe2 O3 C16 C17 10.3(6) . . . . ? Fe2 O3 C16 C12 -168.4(3) . . . . ? Fe1 O2 C7 C6 13.1(6) . . . . ? Fe1 O2 C7 C8 -167.4(3) . . . . ? Fe1 O1 C5 C6 -11.4(6) . . . . ? Fe1 O1 C5 C1 167.9(3) . . . . ? Cr O9 C36 C35 3.9(4) . . . 2_655 ? Fe2 O9 C36 C35 137.7(2) . . . 2_655 ? Fe2 O6 C27 C28 6.7(6) . . . . ? Fe2 O6 C27 C23 -173.7(2) . . . . ? Cr O7 C37 C35 1.8(4) . . . . ? Fe2 O7 C37 C35 137.2(2) . . . . ? C34 C35 C37 O7 -63.0(4) . . . . ? C38 C35 C37 O7 176.4(3) . . . . ? C36 C35 C37 O7 60.3(4) 2_655 . . . ? O3 C16 C12 C15 -56.7(5) . . . . ? C17 C16 C12 C15 124.6(5) . . . . ? O3 C16 C12 C13 57.9(6) . . . . ? C17 C16 C12 C13 -120.8(6) . . . . ? O3 C16 C12 C14 178.3(5) . . . . ? C17 C16 C12 C14 -0.4(7) . . . . ? Fe2 O4 C18 C17 -10.7(6) . . . . ? Fe2 O4 C18 C19 171.9(3) . . . . ? Cr O8 C34 C35 2.8(4) . . . . ? Fe1 O8 C34 C35 137.5(2) . . . . ? C37 C35 C34 O8 60.5(4) . . . . ? C38 C35 C34 O8 179.1(3) . . . . ? C36 C35 C34 O8 -63.2(4) 2_655 . . . ? O6 C27 C23 C25 67.1(6) . . . . ? C28 C27 C23 C25 -113.4(6) . . . . ? O6 C27 C23 C24 -59.9(5) . . . . ? C28 C27 C23 C24 119.7(5) . . . . ? O6 C27 C23 C26 -173.4(4) . . . . ? C28 C27 C23 C26 6.1(6) . . . . ? Fe2 O5 C29 C28 -2.9(7) . . . . ? Fe2 O5 C29 C30 179.6(4) . . . . ? O1 C5 C1 C4 174.3(7) . . . . ? C6 C5 C1 C4 -6.4(9) . . . . ? O1 C5 C1 C3 -54.9(7) . . . . ? C6 C5 C1 C3 124.3(6) . . . . ? O1 C5 C1 C2 58.6(6) . . . . ? C6 C5 C1 C2 -122.1(6) . . . . ? O1 C5 C6 C7 -4.3(7) . . . . ? C1 C5 C6 C7 176.5(4) . . . . ? O2 C7 C6 C5 3.4(7) . . . . ? C8 C7 C6 C5 -176.1(5) . . . . ? O2 C7 C8 C11 -113.3(10) . . . . ? C6 C7 C8 C11 66.2(11) . . . . ? O2 C7 C8 C9 19.7(8) . . . . ? C6 C7 C8 C9 -160.8(7) . . . . ? O2 C7 C8 C10 126.3(5) . . . . ? C6 C7 C8 C10 -54.2(6) . . . . ? O5 C29 C28 C27 2.2(9) . . . . ? C30 C29 C28 C27 179.5(6) . . . . ? O6 C27 C28 C29 -4.1(8) . . . . ? C23 C27 C28 C29 176.4(5) . . . . ? C39 C38 C43 C42 -1.4(7) . . . . ? C35 C38 C43 C42 -179.6(4) . . . . ? O3 C16 C17 C18 2.2(8) . . . . ? C12 C16 C17 C18 -179.3(4) . . . . ? O4 C18 C17 C16 -1.9(8) . . . . ? C19 C18 C17 C16 175.2(5) . . . . ? C43 C38 C39 C40 2.4(7) . . . . ? C35 C38 C39 C40 -179.4(4) . . . . ? O5 C29 C30 C33 22.2(13) . . . . ? C28 C29 C30 C33 -155.3(11) . . . . ? O5 C29 C30 C31 161.0(8) . . . . ? C28 C29 C30 C31 -16.5(11) . . . . ? O5 C29 C30 C32 -84.0(13) . . . . ? C28 C29 C30 C32 98.4(13) . . . . ? C38 C43 C42 C41 -0.3(8) . . . . ? O4 C18 C19 C20 -168.9(9) . . . . ? C17 C18 C19 C20 13.8(11) . . . . ? O4 C18 C19 C22 -45.1(7) . . . . ? C17 C18 C19 C22 137.6(6) . . . . ? O4 C18 C19 C21 68.4(6) . . . . ? C17 C18 C19 C21 -108.9(6) . . . . ? C38 C39 C40 C41 -1.7(8) . . . . ? C39 C40 C41 C42 -0.1(8) . . . . ? C43 C42 C41 C40 1.1(9) . . . . ?