#------------------------------------------------------------------------------ #$Date: 2013-12-28 09:07:06 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91932 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/50/27/1502740.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1502740 loop_ _publ_author_name 'Farrugia, Louis J.' 'Senn, Hans Martin' _publ_section_title ; Metal-metal and metal-ligand bonding at a QTAIM catastrophe: a combined experimental and theoretical charge density study on the alkylidyne cluster Fe3(\m-H)(\m-COMe)(CO)10. ; _journal_issue 51 _journal_name_full 'The journal of physical chemistry. A' _journal_page_first 13418 _journal_page_last 13433 _journal_volume 114 _journal_year 2010 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C12 H4 Fe3 O11' _chemical_formula_sum 'C12 H4 Fe3 O11' _chemical_formula_weight 491.7 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_creation_date '30-Sep-09 T18:02:13-00:00' _audit_creation_method 'XD routine XDCIF' _cell_angle_alpha 90 _cell_angle_beta 103.9270(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.46720(10) _cell_length_b 16.4731(2) _cell_length_c 13.74140(10) _cell_measurement_reflns_used 84907 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 55.734 _cell_measurement_theta_min 2 _cell_measurement_wavelength 0.71073 _cell_volume 1640.61(3) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _diffrn_ambient_temperature 173(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_UB_11 -0.835814E-1 _diffrn_orient_matrix_UB_12 0.27222E-2 _diffrn_orient_matrix_UB_13 0.468772E-1 _diffrn_orient_matrix_UB_21 0.875286E-1 _diffrn_orient_matrix_UB_22 -0.349279E-1 _diffrn_orient_matrix_UB_23 0.490164E-1 _diffrn_orient_matrix_UB_31 0.662568E-1 _diffrn_orient_matrix_UB_32 0.495755E-1 _diffrn_orient_matrix_UB_33 0.319599E-1 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 131757 _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _diffrn_reflns_theta_full 50.04 _diffrn_reflns_theta_max 50.04 _diffrn_reflns_theta_min 2.47 _diffrn_source 'Enraf Nonius FR590' _exptl_absorpt_coefficient_mu 2.674 _exptl_absorpt_correction_T_max 0.636 _exptl_absorpt_correction_T_min 0.433 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst. (1965), 18, 1035-1038 ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 968 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.405 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.412 _refine_ls_matrix_type full _refine_ls_number_parameters 721 _refine_ls_number_reflns 14316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.035 _refine_ls_R_factor_gt 0.02 _refine_ls_shift/su_max 0.00004 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; calc w1 = 1/[s^2^(Fo)] ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.016 _reflns_number_gt 14317 _reflns_number_total 17081 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file jp1098624_si_002.cif _[local]_cod_data_source_block multipole _cod_database_code 1502740 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_local_axes_atom_label _atom_local_axes_atom0 _atom_local_axes_ax1 _atom_local_axes_atom1 _atom_local_axes_atom2 _atom_local_axes_ax2 FE(1) C(14) Z FE(1) C(12) Y FE(2) C(21) Z FE(2) C(22) Y FE(3) C(31) Z FE(3) C(32) Y O(1) C(1) Z O(1) C(2) Y O(11) C(11) Z O(11) H(2C) Y O(12) C(12) Z O(12) H(1) Y O(13) C(13) Z O(13) FE(1) Y O(14) C(14) Z O(14) FE(1) Y O(21) C(21) Z O(21) FE(2) Y O(22) C(22) Z O(22) FE(2) Y O(23) C(23) Z O(23) FE(2) Y O(31) C(31) Z O(31) FE(3) Y O(32) C(32) Z O(32) FE(3) Y O(33) C(33) Z O(33) FE(3) Y C(1) O(1) Z C(1) FE(3) Y C(2) O(1) Z C(2) H(2A) Y C(11) O(11) Z C(11) FE(1) Y C(12) O(12) Z C(12) FE(1) Y C(13) O(13) Z C(13) FE(1) Y C(14) O(14) Z C(14) FE(1) Y C(21) O(21) Z C(21) FE(2) Y C(22) O(22) Z C(22) FE(2) Y C(23) O(23) Z C(23) FE(2) Y C(31) O(31) Z C(31) FE(3) Y C(32) O(32) Z C(32) FE(3) Y C(33) O(33) Z C(33) FE(3) Y H(1) FE(2) Z H(1) FE(3) Y H(2A) C(2) Z H(2A) H(2B) Y H(2B) C(2) Z H(2B) H(2C) Y H(2C) C(2) Z H(2C) H(2B) Y loop_ _atom_rho_multipole_atom_label _atom_rho_multipole_coeff_Pv _atom_rho_multipole_coeff_P00 _atom_rho_multipole_coeff_P11 _atom_rho_multipole_coeff_P1-1 _atom_rho_multipole_coeff_P10 _atom_rho_multipole_coeff_P20 _atom_rho_multipole_coeff_P21 _atom_rho_multipole_coeff_P2-1 _atom_rho_multipole_coeff_P22 _atom_rho_multipole_coeff_P2-2 _atom_rho_multipole_coeff_P30 _atom_rho_multipole_coeff_P31 _atom_rho_multipole_coeff_P3-1 _atom_rho_multipole_coeff_P32 _atom_rho_multipole_coeff_P3-2 _atom_rho_multipole_coeff_P33 _atom_rho_multipole_coeff_P3-3 _atom_rho_multipole_coeff_P40 _atom_rho_multipole_coeff_P41 _atom_rho_multipole_coeff_P4-1 _atom_rho_multipole_coeff_P42 _atom_rho_multipole_coeff_P4-2 _atom_rho_multipole_coeff_P43 _atom_rho_multipole_coeff_P4-3 _atom_rho_multipole_coeff_P44 _atom_rho_multipole_coeff_P4-4 _atom_rho_multipole_kappa _atom_rho_multipole_kappa_prime0 _atom_rho_multipole_kappa_prime1 _atom_rho_multipole_kappa_prime2 _atom_rho_multipole_kappa_prime3 _atom_rho_multipole_kappa_prime4 Fe(1) 5.429(17) 0 -0.058(10) -0.089(10) -0.110(11) -0.003(14) 0.042(12) -0.011(12) 0.130(13) -0.035(13) -0.044(10) -0.037(9) -0.035(9) 0.002(8) -0.016(9) 0.017(8) 0.027(8) -0.135(15) -0.058(13) 0.056(13) -0.053(13) -0.014(14) 0.035(12) -0.007(13) -0.164(11) 0.058(11) 1.01239 1.075384 1.075384 1.075384 1.075384 1.075384 Fe(2) 5.418(16) 0 -0.014(10) -0.015(10) 0.027(10) 0.059(13) 0.002(12) 0.034(12) 0.015(12) -0.011(12) 0.010(8) 0.005(8) 0.024(8) 0.002(8) -0.022(8) -0.020(8) -0.010(8) -0.247(13) 0.028(12) -0.036(12) -0.048(12) 0.020(12) -0.025(12) -0.053(12) -0.190(11) -0.091(11) 1.01239 1.075384 1.075384 1.075384 1.075384 1.075384 Fe(3) 5.408(16) 0 -0.014(10) -0.036(10) 0.070(10) 0.053(13) 0.005(12) 0.004(13) -0.021(12) -0.011(12) 0.047(9) -0.024(8) 0.000(9) -0.003(8) 0.005(8) 0.022(8) 0.002(8) -0.226(14) -0.035(13) -0.023(13) -0.052(13) 0.014(13) 0.005(12) -0.025(12) -0.184(11) 0.040(11) 1.01239 1.075384 1.075384 1.075384 1.075384 1.075384 O(1) 5.99(2) 0 0.018(14) -0.083(15) 0.009(13) 0.056(14) 0.020(14) 0.058(14) 0.033(15) 0.030(15) 0.052(10) -0.009(9) -0.003(10) 0.056(10) 0.015(10) -0.002(10) -0.030(10) 0.016(13) -0.019(11) -0.011(12) 0.009(12) -0.007(12) -0.014(12) -0.002(12) -0.016(12) 0.039(12) 0.996583 1.020057 1.020057 1.020057 1.020057 1.020057 O(11) 5.81(3) 0 -0.029(16) 0.013(16) -0.066(17) 0.066(18) -0.004(16) -0.005(16) -0.005(16) -0.010(16) 0.004(12) -0.006(11) -0.006(12) -0.019(11) -0.018(11) -0.040(11) -0.041(11) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 O(12) 5.97(3) 0 -0.048(16) -0.027(14) 0.027(17) 0.120(17) 0.040(16) -0.001(15) -0.016(15) 0.026(15) 0.028(11) 0.008(11) 0.003(10) 0.005(11) 0.004(11) -0.027(10) -0.006(10) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 O(13) 5.99(4) 0 0.07(2) -0.02(3) 0.10(2) 0.17(2) -0.02(2) 0.01(2) 0.06(3) 0.02(3) -0.050(15) -0.035(13) 0.022(15) -0.037(15) 0.064(15) 0.079(16) -0.013(16) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 O(14) 6.01(4) 0 -0.09(2) 0.032(19) 0.12(2) 0.15(2) -0.01(2) 0.02(2) 0.01(2) 0.10(2) 0.022(16) 0.053(15) -0.001(13) 0.039(15) -0.015(15) -0.028(13) -0.003(13) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 O(21) 5.90(2) 0 0.001(14) 0.019(13) -0.014(16) 0.150(16) 0.006(15) 0.021(14) -0.030(14) 0.014(14) 0.031(11) -0.005(10) -0.003(10) -0.011(10) -0.004(10) 0.028(10) 0.029(10) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 O(22) 5.94(3) 0 0.012(17) 0.043(18) -0.086(18) 0.113(19) -0.010(17) 0.009(18) 0.005(18) 0.000(18) 0.022(13) -0.023(12) 0.011(12) 0.020(12) -0.011(12) -0.011(12) 0.026(12) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 O(23) 5.95(3) 0 0.028(15) 0.006(15) 0.017(16) 0.121(17) -0.018(16) 0.002(15) -0.009(16) -0.005(15) 0.022(11) -0.023(11) 0.022(11) -0.014(11) 0.016(11) -0.023(10) -0.012(10) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 O(31) 6.05(4) 0 0.02(2) -0.01(2) 0.07(2) 0.14(2) 0.04(2) 0.05(2) 0.04(2) -0.03(2) 0.001(15) 0.024(14) -0.013(15) -0.012(14) 0.033(14) 0.025(14) 0.079(14) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 O(32) 5.93(3) 0 -0.04(2) 0.051(17) 0.046(19) 0.14(2) -0.02(2) -0.039(17) -0.04(2) -0.01(2) -0.002(14) 0.015(13) -0.040(12) 0.017(13) -0.012(13) -0.038(13) 0.079(13) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 O(33) 5.91(3) 0 -0.028(18) 0.02(2) -0.014(19) 0.08(2) 0.000(18) -0.038(19) -0.04(2) 0.00(2) -0.080(13) 0.015(12) -0.040(13) -0.055(13) 0.117(13) -0.048(14) -0.073(13) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294 1.007294 C(1) 4.48(2) 0 0.035(16) 0.030(16) -0.24(2) 0.20(2) -0.053(16) 0.029(17) -0.284(15) -0.146(15) 0.30(3) -0.01(2) 0.05(2) 0.165(19) 0.066(19) -0.112(17) -0.010(17) -0.09(3) 0.01(3) -0.02(3) 0.00(3) 0.05(3) -0.09(2) 0.04(2) 0.01(2) 0.03(2) 0.963612 0.733485 0.733485 0.733485 0.733485 0.733485 C(2) 4.14(6) 0 -0.053(14) -0.054(14) -0.145(18) -0.181(18) 0.030(16) -0.045(15) 0.033(15) -0.005(14) 0.50(2) -0.001(19) -0.047(17) -0.051(17) 0.069(16) 0.011(18) -0.216(18) 0.21(2) 0.03(2) 0.04(2) 0.07(2) -0.03(2) -0.06(2) 0.16(2) -0.047(19) 0.054(18) 0.990068 0.87519 0.87519 0.87519 0.87519 0.87519 C(11) 4.18(3) 0 -0.042(13) -0.054(13) 0.08(2) 0.52(2) -0.021(15) -0.020(15) 0.006(12) 0.014(13) 0.15(2) 0.039(17) -0.006(17) 0.008(14) -0.002(15) 0.013(13) 0.021(13) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 C(12) 4.13(3) 0 -0.060(14) 0.019(13) -0.11(2) 0.48(2) -0.017(15) -0.062(15) 0.021(12) -0.007(13) 0.07(2) 0.017(17) -0.005(18) 0.014(14) -0.032(16) 0.000(13) 0.025(14) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 C(13) 4.21(3) 0 -0.058(14) -0.013(15) -0.07(3) 0.40(2) -0.012(16) -0.060(18) -0.008(14) -0.017(14) 0.01(2) 0.011(18) -0.015(19) 0.000(16) 0.063(16) 0.015(15) -0.035(15) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 C(14) 4.09(4) 0 -0.004(15) 0.003(14) -0.15(3) 0.45(2) 0.024(17) 0.009(16) 0.009(14) -0.038(15) 0.03(2) 0.00(2) 0.015(19) -0.022(17) 0.009(17) 0.015(14) 0.014(13) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 C(21) 4.01(3) 0 -0.012(12) 0.004(12) -0.05(2) 0.510(19) -0.002(14) -0.041(14) -0.008(12) 0.021(12) 0.07(2) 0.006(16) -0.047(17) 0.014(14) -0.021(14) -0.012(13) -0.002(13) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 C(22) 4.32(3) 0 -0.070(13) -0.027(14) 0.01(2) 0.51(2) -0.013(15) -0.003(15) -0.036(13) 0.005(13) 0.11(2) -0.005(18) -0.021(18) -0.018(15) 0.016(15) 0.006(14) 0.004(14) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 C(23) 4.22(3) 0 -0.022(13) -0.052(13) -0.06(2) 0.44(2) -0.019(14) -0.018(14) 0.010(12) 0.034(12) 0.09(2) -0.035(17) 0.030(18) -0.011(15) -0.016(14) -0.038(13) 0.045(13) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 C(31) 4.27(3) 0 0.034(14) 0.017(15) -0.08(3) 0.41(2) 0.049(16) -0.013(17) 0.040(13) 0.011(13) 0.04(2) 0.027(19) 0.05(2) -0.023(16) 0.024(16) 0.027(14) -0.025(14) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 C(32) 4.00(3) 0 0.024(14) 0.017(12) -0.11(2) 0.45(2) -0.017(16) 0.026(15) 0.007(14) -0.021(13) 0.07(2) -0.001(19) 0.034(17) 0.057(15) -0.022(15) 0.000(13) 0.000(14) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 C(33) 4.19(3) 0 -0.006(14) 0.057(14) 0.05(2) 0.50(2) 0.038(15) 0.043(16) -0.016(14) 0.012(13) 0.11(2) -0.029(17) 0.037(18) 0.051(15) 0.057(16) 0.060(14) -0.006(15) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585 0.884585 H(1) 1.296(16) 0 -0.04(4) 0.05(4) -0.01(4) 0.04(2) -0.085(19) -0.053(19) -0.01(2) 0.011(19) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.012809 1.012809 1.012809 1.012809 1.012809 1.012809 H(2A) 0.916(19) 0 0.012(12) 0.058(12) 0.156(12) 0.032(17) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.158107 1.158107 1.158107 1.158107 1.158107 1.158107 H(2B) 0.916(19) 0 0.012(12) 0.058(12) 0.156(12) 0.032(17) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.158107 1.158107 1.158107 1.158107 1.158107 1.158107 H(2C) 0.916(19) 0 0.012(12) 0.058(12) 0.156(12) 0.032(17) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.158107 1.158107 1.158107 1.158107 1.158107 1.158107 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 Fe(1) Fe 0.334365(16) 0.060764(8) 0.188579(9) 0.013 Uani 1 4 Fe(2) Fe 0.174446(14) 0.056401(7) 0.340676(8) 0.011 Uani 1 4 Fe(3) Fe 0.331354(16) 0.190514(7) 0.305413(9) 0.013 Uani 1 4 O(1) O -0.06991(8) 0.17003(4) 0.21520(5) 0.018 Uani 1 4 O(11) O -0.01607(10) 0.08612(6) 0.03426(6) 0.025 Uani 1 4 O(12) O 0.66434(9) 0.03262(5) 0.35272(6) 0.023 Uani 1 4 O(13) O 0.56577(14) 0.10887(11) 0.05138(8) 0.041 Uani 1 4 O(14) O 0.31932(18) -0.11716(6) 0.16657(8) 0.037 Uani 1 4 O(21) O 0.01848(9) 0.09985(4) 0.51081(5) 0.02 Uani 1 4 O(22) O -0.12469(11) -0.04365(6) 0.22279(7) 0.028 Uani 1 4 O(23) O 0.38893(10) -0.08665(4) 0.43805(6) 0.023 Uani 1 4 O(31) O 0.19716(19) 0.31426(7) 0.42422(8) 0.038 Uani 1 4 O(32) O 0.34868(13) 0.28957(6) 0.13032(7) 0.032 Uani 1 4 O(33) O 0.72867(12) 0.21534(6) 0.40801(9) 0.034 Uani 1 4 C(1) C 0.09540(5) 0.14793(2) 0.26279(3) 0.014 Uani 1 4 C(2) C -0.09857(8) 0.24783(4) 0.16372(5) 0.026 Uani 1 4 C(11) C 0.11743(6) 0.07884(3) 0.09496(4) 0.017 Uani 1 4 C(12) C 0.53295(6) 0.04847(3) 0.29245(4) 0.018 Uani 1 4 C(13) C 0.47455(7) 0.09168(4) 0.10442(4) 0.024 Uani 1 4 C(14) C 0.32140(8) -0.04770(4) 0.17195(4) 0.022 Uani 1 4 C(21) C 0.07573(6) 0.08187(3) 0.44384(3) 0.014 Uani 1 4 C(22) C -0.00836(6) -0.00501(3) 0.27000(4) 0.017 Uani 1 4 C(23) C 0.31186(6) -0.02990(3) 0.40271(3) 0.015 Uani 1 4 C(31) C 0.25367(8) 0.26688(3) 0.37854(4) 0.021 Uani 1 4 C(32) C 0.33952(7) 0.25044(3) 0.19820(4) 0.02 Uani 1 4 C(33) C 0.57822(7) 0.20385(3) 0.36742(4) 0.021 Uani 1 4 H(1) H 0.338(3) 0.1178(14) 0.3917(15) 0.029 Uani 1 4 H(2A) H -0.247749 0.256184 0.144954 0.073 Uani 1 4 H(2B) H -0.035424 0.295676 0.215494 0.077 Uani 1 4 H(2C) H -0.038602 0.245887 0.098855 0.073 Uani 1 4 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(1) 0.01398(4) 0.01543(4) 0.01081(4) -0.00090(3) 0.00379(3) -0.00115(3) Fe(2) 0.01133(3) 0.01089(3) 0.01096(3) 0.00117(3) 0.00306(3) -0.00006(3) Fe(3) 0.01423(4) 0.01089(3) 0.01162(3) 0.00110(3) 0.00095(3) -0.00157(3) O(1) 0.01355(19) 0.0183(2) 0.0192(2) 0.00342(18) -0.00021(16) 0.00255(17) O(11) 0.0214(2) 0.0320(3) 0.0187(2) -0.0011(2) -0.0021(2) 0.0020(2) O(12) 0.0134(2) 0.0339(3) 0.0206(2) -0.0010(2) 0.00149(18) 0.0035(2) O(13) 0.0285(4) 0.0724(7) 0.0260(4) 0.0091(5) 0.0162(3) -0.0069(4) O(14) 0.0576(5) 0.0165(3) 0.0325(4) -0.0048(3) 0.0015(4) 0.0067(3) O(21) 0.0220(2) 0.0235(2) 0.0168(2) -0.0013(2) 0.00985(18) 0.0006(2) O(22) 0.0220(3) 0.0306(3) 0.0319(3) -0.0137(3) 0.0060(2) -0.0112(3) O(23) 0.0253(3) 0.0184(2) 0.0235(3) 0.0063(2) 0.0038(2) 0.0075(2) O(31) 0.0596(5) 0.0269(4) 0.0253(4) -0.0096(3) 0.0065(4) 0.0136(4) O(32) 0.0360(4) 0.0326(4) 0.0260(3) 0.0161(3) 0.0070(3) -0.0057(3) O(33) 0.0205(3) 0.0251(3) 0.0457(4) 0.0088(3) -0.0109(3) -0.0067(2) C(1) 0.01392(13) 0.01352(14) 0.01299(14) 0.00169(11) 0.00089(10) 0.00006(11) C(2) 0.0239(2) 0.0202(2) 0.0279(3) 0.00639(19) -0.00351(18) 0.00436(17) C(11) 0.01729(16) 0.01870(18) 0.01398(16) -0.00093(14) 0.00209(13) -0.00080(14) C(12) 0.01401(15) 0.0254(2) 0.01511(17) -0.00106(15) 0.00313(13) -0.00024(14) C(13) 0.01996(18) 0.0369(3) 0.0172(2) 0.0029(2) 0.00789(16) -0.00293(19) C(14) 0.0281(2) 0.0166(2) 0.01842(19) -0.00255(15) 0.00212(16) 0.00344(16) C(21) 0.01479(14) 0.01563(16) 0.01329(15) 0.00098(12) 0.00510(12) 0.00037(12) C(22) 0.01553(16) 0.01656(17) 0.01887(18) -0.00303(14) 0.00436(13) -0.00351(13) C(23) 0.01621(15) 0.01415(16) 0.01584(16) 0.00256(13) 0.00397(12) 0.00212(13) C(31) 0.0305(2) 0.01544(18) 0.01609(18) -0.00279(15) 0.00119(16) 0.00225(16) C(32) 0.02145(18) 0.0199(2) 0.01824(19) 0.00696(16) 0.00320(15) -0.00321(15) C(33) 0.01741(18) 0.01723(18) 0.0253(2) 0.00487(16) -0.00294(16) -0.00449(14) H(1) 0.028735 0.028553 0.026133 0.003508 0.00044 -0.003055 H(2A) 0.041416 0.119068 0.056726 0.010302 0.006826 0.020402 H(2B) 0.051128 0.058025 0.103633 -0.028121 -0.014104 0.008969 H(2C) 0.047273 0.115415 0.056276 0.019426 0.013011 0.018912 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 2 1 0.1 0 -2 -1 0.1 0 0 -1 0.13 0 0 1 0.09 0 1 -1 0.17 0 -2 1 0.09 1 0 0 0.19 -1 0 0 0.2 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(11) FE(1) C(12) 172.54(2) 1_555 1_555 1_555 yes C(11) FE(1) C(13) 93.16(2) 1_555 1_555 1_555 yes C(11) FE(1) C(14) 93.48(2) 1_555 1_555 1_555 yes C(12) FE(1) C(13) 92.60(2) 1_555 1_555 1_555 yes C(12) FE(1) C(14) 89.88(2) 1_555 1_555 1_555 yes C(13) FE(1) C(14) 102.70(3) 1_555 1_555 1_555 yes C(1) FE(2) C(21) 97.528(19) 1_555 1_555 1_555 yes C(1) FE(2) C(22) 92.92(2) 1_555 1_555 1_555 yes C(1) FE(2) C(23) 163.257(19) 1_555 1_555 1_555 yes C(1) FE(2) H(1) 81.0(8) 1_555 1_555 1_555 yes C(21) FE(2) C(22) 98.98(2) 1_555 1_555 1_555 yes C(21) FE(2) C(23) 95.96(2) 1_555 1_555 1_555 yes C(21) FE(2) H(1) 85.5(7) 1_555 1_555 1_555 yes C(22) FE(2) C(23) 94.73(2) 1_555 1_555 1_555 yes C(22) FE(2) H(1) 172.9(7) 1_555 1_555 1_555 yes C(23) FE(2) H(1) 90.2(8) 1_555 1_555 1_555 yes C(1) FE(3) C(31) 91.80(2) 1_555 1_555 1_555 yes C(1) FE(3) C(32) 99.61(2) 1_555 1_555 1_555 yes C(1) FE(3) C(33) 163.01(2) 1_555 1_555 1_555 yes C(1) FE(3) H(1) 79.5(7) 1_555 1_555 1_555 yes C(31) FE(3) C(32) 98.89(3) 1_555 1_555 1_555 yes C(31) FE(3) C(33) 94.57(3) 1_555 1_555 1_555 yes C(31) FE(3) H(1) 93.6(8) 1_555 1_555 1_555 yes C(32) FE(3) C(33) 94.95(2) 1_555 1_555 1_555 yes C(32) FE(3) H(1) 167.5(8) 1_555 1_555 1_555 yes C(33) FE(3) H(1) 84.4(7) 1_555 1_555 1_555 yes C(1) O(1) C(2) 120.09(5) 1_555 1_555 1_555 yes FE(2) C(1) FE(3) 88.802(17) 1_555 1_555 1_555 yes FE(2) C(1) O(1) 130.28(4) 1_555 1_555 1_555 yes FE(3) C(1) O(1) 140.02(4) 1_555 1_555 1_555 yes O(1) C(2) H(2A) 104.0 1_555 1_555 1_555 yes O(1) C(2) H(2B) 109.0 1_555 1_555 1_555 yes O(1) C(2) H(2C) 109.0 1_555 1_555 1_555 yes H(2A) C(2) H(2B) 109.0 1_555 1_555 1_555 yes H(2A) C(2) H(2C) 114.0 1_555 1_555 1_555 yes H(2B) C(2) H(2C) 111.0 1_555 1_555 1_555 yes FE(1) C(11) O(11) 176.21(6) 1_555 1_555 1_555 yes FE(1) C(12) O(12) 171.85(6) 1_555 1_555 1_555 yes FE(1) C(13) O(13) 177.84(10) 1_555 1_555 1_555 yes FE(1) C(14) O(14) 176.23(7) 1_555 1_555 1_555 yes FE(2) C(21) O(21) 177.47(5) 1_555 1_555 1_555 yes FE(2) C(22) O(22) 178.46(7) 1_555 1_555 1_555 yes FE(2) C(23) O(23) 175.76(6) 1_555 1_555 1_555 yes FE(3) C(31) O(31) 177.24(9) 1_555 1_555 1_555 yes FE(3) C(32) O(32) 178.46(6) 1_555 1_555 1_555 yes FE(3) C(33) O(33) 176.70(8) 1_555 1_555 1_555 yes FE(2) H(1) FE(3) 104.5(11) 1_555 1_555 1_555 yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag FE(1) FE(2) 2.64590(16) 1_555 1_555 yes FE(1) FE(3) 2.67653(17) 1_555 1_555 yes FE(2) FE(3) 2.60033(15) 1_555 1_555 yes FE(1) C(11) 1.8342(5) 1_555 1_555 yes FE(1) C(12) 1.8051(5) 1_555 1_555 yes FE(1) C(13) 1.8097(6) 1_555 1_555 yes FE(1) C(14) 1.8009(6) 1_555 1_555 yes FE(2) C(1) 1.8610(4) 1_555 1_555 yes FE(2) C(21) 1.7978(5) 1_555 1_555 yes FE(2) C(22) 1.7865(5) 1_555 1_555 yes FE(2) C(23) 1.8383(5) 1_555 1_555 yes FE(2) H(1) 1.61(2) 1_555 1_555 yes FE(3) C(1) 1.8555(4) 1_555 1_555 yes FE(3) C(31) 1.7915(6) 1_555 1_555 yes FE(3) C(32) 1.7866(5) 1_555 1_555 yes FE(3) C(33) 1.8483(5) 1_555 1_555 yes FE(3) H(1) 1.68(2) 1_555 1_555 yes O(1) C(1) 1.3021(6) 1_555 1_555 yes O(1) C(2) 1.4546(8) 1_555 1_555 yes O(11) C(11) 1.1418(8) 1_555 1_555 yes O(12) C(12) 1.1513(8) 1_555 1_555 yes O(13) C(13) 1.1465(9) 1_555 1_555 yes O(14) C(14) 1.1466(10) 1_555 1_555 yes O(21) C(21) 1.1431(7) 1_555 1_555 yes O(22) C(22) 1.1443(8) 1_555 1_555 yes O(23) C(23) 1.1431(7) 1_555 1_555 yes O(31) C(31) 1.1440(10) 1_555 1_555 yes O(32) C(32) 1.1493(9) 1_555 1_555 yes O(33) C(33) 1.1434(8) 1_555 1_555 yes C(2) H(2A) 1.090 1_555 1_555 yes C(2) H(2B) 1.090 1_555 1_555 yes C(2) H(2C) 1.090 1_555 1_555 yes _journal_paper_doi 10.1021/jp1098624