# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1186 data_zulfin8 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H12 Fe2 O6 Te2' _chemical_formula_weight 715.2 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.863(2) _cell_length_b 7.245(2) _cell_length_c 14.380(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.49(2) _cell_angle_gamma 90.00 _cell_volume 1090.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5937 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 25.2 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_method ? _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 3.985 _exptl_absorpt_correction_type ; Specific absorption corrections not applied. Averaging of symmetry equivalent reflections for small near equi-dimensional crystal will minimize absorption effects. ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKa _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku area detector diffractometer' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5937 #all data with I > 1sigma(I) _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.21 _reflns_number_total 1888 _reflns_number_observed 1781 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ; Unit cell dimensions were obtained by post refinement of the full data set. ; _computing_data_reduction ? _computing_structure_solution 'TEXSAN (see reference 11)' _computing_structure_refinement 'SHELXL-93 (see reference 12)' _computing_molecular_graphics 'ORTEP (see reference 13)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^. Weighted R-factors, wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[s^2^(Fo^2^)+( 0.0232P)^2^+4.8089P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1888 #all data with I > 1sigma(I) _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 #all data with I > 1sigma(I) _refine_ls_R_factor_obs 0.0533 #all data with I > 2sigma(I) _refine_ls_wR_factor_all 0.1060 _refine_ls_wR_factor_obs 0.1042 _refine_ls_goodness_of_fit_all 1.256 _refine_ls_goodness_of_fit_obs 1.274 _refine_ls_restrained_S_all 1.256 _refine_ls_restrained_S_obs 1.274 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Te1 Te 0.46030(5) 0.22868(7) -0.01185(4) 0.0500(2) Uani 1 d . . Fe1 Fe 0.32196(10) -0.0643(2) -0.02825(8) 0.0472(3) Uani 1 d . . O1 O 0.0982(6) 0.1474(11) -0.0162(5) 0.079(2) Uani 1 d . . O2 O 0.2696(7) -0.0445(12) -0.2396(5) 0.095(2) Uani 1 d . . O3 O 0.1987(6) -0.4255(10) -0.0377(5) 0.084(2) Uani 1 d . . C1 C 0.4210(9) 0.2825(13) 0.1237(7) 0.066(2) Uani 1 d . . H1A H 0.4901(9) 0.3543(13) 0.1643(7) 0.079 Uiso 1 calc R . H1B H 0.3429(9) 0.3538(13) 0.1133(7) 0.079 Uiso 1 calc R . C2 C 0.4069(7) 0.1019(13) 0.1736(6) 0.054(2) Uani 1 d . . C3 C 0.4358(8) 0.1002(16) 0.2748(7) 0.068(3) Uani 1 d . . H3 H 0.4661(8) 0.2070(16) 0.3092(7) 0.081 Uiso 1 calc R . C4 C 0.4199(9) -0.0559(17) 0.3233(7) 0.077(3) Uani 1 d . . H4 H 0.4389(9) -0.0546(17) 0.3903(7) 0.093 Uiso 1 calc R . C5 C 0.3763(10) -0.2136(16) 0.2738(8) 0.076(3) Uani 1 d . . H5 H 0.3656(10) -0.3205(16) 0.3066(8) 0.091 Uiso 1 calc R . C6 C 0.3482(9) -0.2127(13) 0.1737(7) 0.065(2) Uani 1 d . . H6 H 0.3168(9) -0.3204(13) 0.1407(7) 0.078 Uiso 1 calc R . C7 C 0.3646(7) -0.0583(11) 0.1203(6) 0.048(2) Uani 1 d . . C8 C 0.1865(8) 0.0662(13) -0.0231(6) 0.056(2) Uani 1 d . . C9 C 0.2946(8) -0.0530(13) -0.1577(7) 0.062(2) Uani 1 d . . C10 C 0.2468(8) -0.2832(13) -0.0332(7) 0.060(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0507(3) 0.0444(3) 0.0563(4) 0.0013(2) 0.0167(2) -0.0046(2) Fe1 0.0438(6) 0.0517(7) 0.0451(6) -0.0005(5) 0.0103(5) -0.0070(5) O1 0.061(4) 0.091(5) 0.086(5) 0.006(4) 0.019(4) 0.009(4) O2 0.097(5) 0.136(7) 0.047(4) 0.003(4) 0.010(4) -0.003(5) O3 0.075(4) 0.074(5) 0.093(5) 0.004(4) 0.005(4) -0.029(4) C1 0.071(6) 0.070(6) 0.060(6) -0.020(5) 0.022(5) -0.011(5) C2 0.044(4) 0.069(6) 0.056(5) -0.008(4) 0.023(4) 0.000(4) C3 0.052(5) 0.099(8) 0.056(6) -0.020(5) 0.022(4) -0.008(5) C4 0.067(6) 0.118(9) 0.049(6) 0.005(6) 0.017(5) 0.003(6) C5 0.071(6) 0.099(8) 0.064(6) 0.023(6) 0.030(5) 0.002(6) C6 0.071(6) 0.070(6) 0.056(6) 0.003(4) 0.020(5) -0.003(5) C7 0.042(4) 0.056(5) 0.048(5) 0.005(4) 0.015(4) -0.003(4) C8 0.050(5) 0.067(5) 0.050(5) 0.008(4) 0.010(4) -0.008(4) C9 0.060(5) 0.069(6) 0.053(6) -0.001(4) 0.009(4) -0.005(5) C10 0.049(5) 0.069(6) 0.059(6) 0.002(4) 0.009(4) -0.011(4) _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 Te1 C1 2.139(9) . ? Te1 Fe1 2.5723(13) 3_655 ? Te1 Fe1 2.5750(13) . ? Fe1 C8 1.767(10) . ? Fe1 C10 1.777(9) . ? Fe1 C9 1.806(10) . ? Fe1 C7 2.062(8) . ? Fe1 Te1 2.5723(13) 3_655 ? O1 C8 1.152(10) . ? O2 C9 1.138(10) . ? O3 C10 1.149(10) . ? C1 C2 1.520(13) . ? C2 C7 1.400(11) . ? C2 C3 1.404(12) . ? C3 C4 1.364(14) . ? C4 C5 1.363(14) . ? C5 C6 1.389(13) . ? C6 C7 1.395(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te1 Fe1 106.0(3) . 3_655 ? C1 Te1 Fe1 88.9(2) . . ? Fe1 Te1 Fe1 96.78(4) 3_655 . ? C8 Fe1 C10 95.8(4) . . ? C8 Fe1 C9 96.3(4) . . ? C10 Fe1 C9 93.0(4) . . ? C8 Fe1 C7 84.5(3) . . ? C10 Fe1 C7 92.0(4) . . ? C9 Fe1 C7 174.9(4) . . ? C8 Fe1 Te1 164.7(3) . 3_655 ? C10 Fe1 Te1 88.9(3) . 3_655 ? C9 Fe1 Te1 98.1(3) . 3_655 ? C7 Fe1 Te1 80.7(2) . 3_655 ? C8 Fe1 Te1 91.6(3) . . ? C10 Fe1 Te1 172.0(3) . . ? C9 Fe1 Te1 89.3(3) . . ? C7 Fe1 Te1 85.6(2) . . ? Te1 Fe1 Te1 83.22(4) 3_655 . ? C2 C1 Te1 110.1(6) . . ? C7 C2 C3 120.7(9) . . ? C7 C2 C1 121.0(8) . . ? C3 C2 C1 118.3(8) . . ? C4 C3 C2 120.9(10) . . ? C5 C4 C3 120.1(10) . . ? C4 C5 C6 119.1(10) . . ? C5 C6 C7 123.3(10) . . ? C6 C7 C2 115.8(8) . . ? C6 C7 Fe1 121.8(7) . . ? C2 C7 Fe1 122.3(6) . . ? O1 C8 Fe1 177.1(8) . . ? O2 C9 Fe1 175.8(9) . . ? O3 C10 Fe1 178.9(9) . . ? _refine_diff_density_max 0.515 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.119 #=END data_zulfi925a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H6 O2' _chemical_formula_weight 134.13 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.760(2) _cell_length_b 10.799(3) _cell_length_c 8.234(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.88(2) _cell_angle_gamma 90.00 _cell_volume 635.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2740 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 25.2 _exptl_crystal_description ? _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method ? _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKa _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku area detector diffractometer' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2740 #all data with I > 1sigma(I) _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.24 _reflns_number_total 966 _reflns_number_observed 772 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ; Unit cell dimensions were obtained by post refinement of the full data set. ; _computing_data_reduction ? _computing_structure_solution 'Texsan (see reference 11)' _computing_structure_refinement 'SHELXL-93 (see reference 12)' _computing_molecular_graphics 'ORTEP (see reference 13)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^. Weighted R-factors, wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[s^2^(Fo^2^)+( 0.1280P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 966 #all data with I > 1sigma(I) _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0986 #all data with I > 1sigma(I) _refine_ls_R_factor_obs 0.0739 #all data with I > 2sigma(I) _refine_ls_wR_factor_all 0.2246 _refine_ls_wR_factor_obs 0.1944 _refine_ls_goodness_of_fit_all 1.193 _refine_ls_goodness_of_fit_obs 1.161 _refine_ls_restrained_S_all 1.193 _refine_ls_restrained_S_obs 1.161 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1 O 0.6238(3) 0.0925(2) 0.7126(3) 0.0630(9) Uani 1 d . . O2 O 0.6745(4) 0.2535(3) 0.8957(5) 0.0857(11) Uani 1 d . . C1 C 0.7321(5) 0.0095(4) 0.6496(5) 0.0592(10) Uani 1 d . . H1A H 0.6979(5) 0.0194(4) 0.5238(5) 0.071 Uiso 1 calc R . H1B H 0.7129(5) -0.0761(4) 0.6738(5) 0.071 Uiso 1 calc R . C2 C 0.9299(4) 0.0477(3) 0.7500(4) 0.0495(9) Uani 1 d . . C3 C 1.0960(5) 0.0028(4) 0.7469(5) 0.0594(10) Uani 1 d . . H3 H 1.0965(5) -0.0635(4) 0.6751(5) 0.071 Uiso 1 calc R . C4 C 1.2596(5) 0.0591(4) 0.8528(5) 0.0639(11) Uani 1 d . . H4 H 1.3727(5) 0.0317(4) 0.8516(5) 0.077 Uiso 1 calc R . C5 C 1.2576(5) 0.1574(4) 0.9627(5) 0.0691(12) Uani 1 d . . H5 H 1.3703(5) 0.1935(4) 1.0347(5) 0.083 Uiso 1 calc R . C6 C 1.0947(5) 0.2016(4) 0.9671(5) 0.0625(11) Uani 1 d . . H6 H 1.0942(5) 0.2666(4) 1.0410(5) 0.075 Uiso 1 calc R . C7 C 0.9298(4) 0.1455(3) 0.8569(4) 0.0510(9) Uani 1 d . . C8 C 0.7370(5) 0.1741(4) 0.8306(5) 0.0602(10) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0425(14) 0.064(2) 0.074(2) -0.0041(13) 0.0128(12) -0.0042(11) O2 0.074(2) 0.078(2) 0.108(3) -0.023(2) 0.038(2) 0.008(2) C1 0.050(2) 0.055(2) 0.065(2) -0.004(2) 0.014(2) -0.003(2) C2 0.043(2) 0.048(2) 0.052(2) 0.007(2) 0.0121(14) -0.0004(15) C3 0.053(2) 0.055(2) 0.066(2) 0.006(2) 0.017(2) 0.004(2) C4 0.044(2) 0.073(3) 0.074(2) 0.015(2) 0.022(2) 0.009(2) C5 0.043(2) 0.074(3) 0.073(2) 0.014(2) 0.003(2) -0.010(2) C6 0.053(2) 0.057(2) 0.065(2) -0.003(2) 0.009(2) -0.003(2) C7 0.045(2) 0.046(2) 0.053(2) 0.0033(15) 0.0100(15) 0.0001(14) C8 0.055(2) 0.055(2) 0.066(2) 0.001(2) 0.018(2) -0.003(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 O1 C8 1.352(4) . ? O1 C1 1.455(4) . ? O2 C8 1.208(4) . ? C1 C2 1.491(5) . ? C2 C7 1.374(5) . ? C2 C3 1.386(5) . ? C3 C4 1.371(5) . ? C4 C5 1.399(6) . ? C5 C6 1.365(5) . ? C6 C7 1.388(5) . ? C7 C8 1.459(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 C8 O1 C1 110.7(3) . . ? O1 C1 C2 104.2(3) . . ? C7 C2 C3 120.8(3) . . ? C7 C2 C1 108.1(3) . . ? C3 C2 C1 131.1(4) . . ? C4 C3 C2 118.1(4) . . ? C3 C4 C5 120.5(4) . . ? C6 C5 C4 121.7(3) . . ? C5 C6 C7 117.3(4) . . ? C2 C7 C6 121.6(3) . . ? C2 C7 C8 108.9(3) . . ? C6 C7 C8 129.5(4) . . ? O2 C8 O1 121.4(4) . . ? O2 C8 C7 130.5(4) . . ? O1 C8 C7 108.1(3) . . ? _refine_diff_density_max 0.395 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.125 #=END data_zuln155 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H6 Fe2 O6 Se' _chemical_formula_weight 448.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.479(2) _cell_length_b 15.339(3) _cell_length_c 10.637(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.730(10) _cell_angle_gamma 90.00 _cell_volume 1532.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8792 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.2 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method ? _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 4.290 _exptl_absorpt_correction_type ; Specific absorption corrections not applied. Averaging of symmetry equivalent reflections for small near equi-dimensional crystal will minimize absorption effects. ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKa _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku area detector diffractometer' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8792 #all data with I > 1sigma(I) _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.24 _reflns_number_total 2680 _reflns_number_observed 2190 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ; Unit cell dimensions were obtained by post refinement of the full data set. ; _computing_data_reduction ? _computing_structure_solution 'Texsan (see reference 11)' _computing_structure_refinement 'SHELXL-93 (see reference 12' _computing_molecular_graphics 'ORTEP (see reference 13)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^. Weighted R-factors, wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[s^2^(Fo^2^)+( 0.0790P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2680 #all data with I > 1sigma(I) _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 #all data with I > 1sigma(I) _refine_ls_R_factor_obs 0.0564 #all data with I > 2sigma(I) _refine_ls_wR_factor_all 0.1422 _refine_ls_wR_factor_obs 0.1307 _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.086 _refine_ls_restrained_S_all 1.061 _refine_ls_restrained_S_obs 1.086 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Se1 Se 0.69254(7) 0.01134(3) 0.74955(6) 0.0722(3) Uani 1 d . . Fe1 Fe 0.65620(8) 0.14097(4) 0.85792(7) 0.0572(3) Uani 1 d . . Fe2 Fe 0.67680(8) 0.14187(4) 0.62779(6) 0.0555(3) Uani 1 d . . O1 O 0.5620(6) 0.3204(3) 0.8806(5) 0.104(2) Uani 1 d . . O2 O 0.3813(6) 0.0730(4) 0.9149(5) 0.130(2) Uani 1 d . . O3 O 0.8211(6) 0.1133(4) 1.1082(4) 0.109(2) Uani 1 d . . O4 O 0.6388(6) 0.3230(3) 0.5448(4) 0.100(2) Uani 1 d . . O5 O 0.3718(6) 0.1182(4) 0.5618(5) 0.1039(15) Uani 1 d . . O6 O 0.7835(6) 0.0681(3) 0.4032(4) 0.103(2) Uani 1 d . . C1 C 0.9017(7) 0.0179(3) 0.7716(6) 0.075(2) Uani 1 d . . H1A H 0.9415(7) -0.0030(3) 0.8549(6) 0.090 Uiso 1 calc R . H1B H 0.9399(7) -0.0168(3) 0.7078(6) 0.090 Uiso 1 calc R . C2 C 0.9350(6) 0.1116(3) 0.7571(4) 0.0577(12) Uani 1 d . . C3 C 1.0662(7) 0.1347(4) 0.7219(5) 0.076(2) Uani 1 d . . H3 H 1.1270(7) 0.0912(4) 0.7003(5) 0.091 Uiso 1 calc R . C4 C 1.1071(7) 0.2190(4) 0.7185(6) 0.079(2) Uani 1 d . . H4 H 1.1959(7) 0.2329(4) 0.6962(6) 0.095 Uiso 1 calc R . C5 C 1.0176(6) 0.2842(4) 0.7480(5) 0.0702(15) Uani 1 d . . H5 H 1.0458(6) 0.3422(4) 0.7459(5) 0.084 Uiso 1 calc R . C6 C 0.8868(6) 0.2635(3) 0.7805(4) 0.0589(12) Uani 1 d . . H6 H 0.8272(6) 0.3086(3) 0.7988(4) 0.071 Uiso 1 calc R . C7 C 0.8381(5) 0.1770(3) 0.7875(4) 0.0527(11) Uani 1 d . . C8 C 0.6005(6) 0.2505(4) 0.8718(5) 0.0701(14) Uani 1 d . . C9 C 0.4896(7) 0.0997(4) 0.8914(6) 0.083(2) Uani 1 d . . C10 C 0.7544(6) 0.1236(4) 1.0109(5) 0.0723(15) Uani 1 d . . C11 C 0.6565(6) 0.2529(4) 0.5768(5) 0.0686(14) Uani 1 d . . C12 C 0.4923(7) 0.1274(4) 0.5885(5) 0.0713(15) Uani 1 d . . C13 C 0.7434(7) 0.0978(4) 0.4906(5) 0.0709(15) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0896(5) 0.0397(3) 0.0880(4) 0.0060(2) 0.0148(3) -0.0015(2) Fe1 0.0664(5) 0.0532(4) 0.0533(4) 0.0108(3) 0.0132(3) 0.0118(3) Fe2 0.0709(5) 0.0454(4) 0.0496(4) -0.0006(3) 0.0066(3) -0.0032(3) O1 0.141(5) 0.075(3) 0.103(3) 0.010(3) 0.038(3) 0.048(3) O2 0.082(4) 0.152(5) 0.160(5) 0.063(4) 0.035(3) 0.005(3) O3 0.113(4) 0.146(4) 0.065(3) 0.019(3) 0.000(2) 0.042(3) O4 0.151(4) 0.056(2) 0.084(3) 0.012(2) -0.020(3) -0.002(3) O5 0.079(3) 0.130(4) 0.101(3) 0.009(3) 0.007(3) -0.013(3) O6 0.130(4) 0.103(3) 0.083(3) -0.019(3) 0.040(3) 0.002(3) C1 0.083(4) 0.055(3) 0.089(4) 0.007(3) 0.020(3) 0.026(3) C2 0.063(3) 0.051(3) 0.059(3) 0.002(2) 0.006(2) 0.011(2) C3 0.071(4) 0.077(4) 0.082(4) -0.007(3) 0.017(3) 0.016(3) C4 0.070(4) 0.090(5) 0.079(4) 0.004(3) 0.017(3) -0.005(3) C5 0.076(4) 0.065(3) 0.067(3) 0.002(3) 0.001(3) -0.011(3) C6 0.071(3) 0.045(3) 0.058(3) 0.000(2) -0.004(2) 0.004(2) C7 0.060(3) 0.044(2) 0.053(2) 0.002(2) 0.003(2) 0.012(2) C8 0.086(4) 0.071(3) 0.056(3) 0.007(3) 0.021(3) 0.022(3) C9 0.079(4) 0.093(4) 0.077(4) 0.030(3) 0.013(3) 0.017(4) C10 0.074(4) 0.078(4) 0.068(3) 0.012(3) 0.019(3) 0.024(3) C11 0.094(4) 0.056(3) 0.051(3) -0.001(2) -0.008(3) -0.006(3) C12 0.076(4) 0.077(4) 0.063(3) 0.003(3) 0.016(3) -0.009(3) C13 0.082(4) 0.064(3) 0.068(3) -0.008(3) 0.016(3) -0.007(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 Se1 C1 1.967(6) . ? Se1 Fe1 2.3469(9) . ? Se1 Fe2 2.3782(9) . ? Fe1 C8 1.774(6) . ? Fe1 C9 1.781(7) . ? Fe1 C10 1.783(6) . ? Fe1 C7 2.046(5) . ? Fe1 Fe2 2.4817(11) . ? Fe2 C12 1.757(7) . ? Fe2 C11 1.789(5) . ? Fe2 C13 1.798(6) . ? Fe2 C7 2.194(5) . ? O1 C8 1.140(6) . ? O2 C9 1.164(7) . ? O3 C10 1.148(6) . ? O4 C11 1.134(6) . ? O5 C12 1.148(7) . ? O6 C13 1.144(6) . ? C1 C2 1.485(7) . ? C2 C3 1.392(8) . ? C2 C7 1.426(6) . ? C3 C4 1.352(8) . ? C4 C5 1.374(8) . ? C5 C6 1.368(7) . ? C6 C7 1.410(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 Fe1 96.3(2) . . ? C1 Se1 Fe2 90.6(2) . . ? Fe1 Se1 Fe2 63.36(3) . . ? C8 Fe1 C9 92.2(3) . . ? C8 Fe1 C10 101.0(3) . . ? C9 Fe1 C10 97.6(3) . . ? C8 Fe1 C7 92.9(2) . . ? C9 Fe1 C7 169.3(2) . . ? C10 Fe1 C7 90.7(2) . . ? C8 Fe1 Se1 155.3(2) . . ? C9 Fe1 Se1 89.4(2) . . ? C10 Fe1 Se1 103.2(2) . . ? C7 Fe1 Se1 82.08(13) . . ? C8 Fe1 Fe2 98.1(2) . . ? C9 Fe1 Fe2 112.9(2) . . ? C10 Fe1 Fe2 143.2(2) . . ? C7 Fe1 Fe2 57.00(13) . . ? Se1 Fe1 Fe2 58.93(3) . . ? C12 Fe2 C11 89.2(3) . . ? C12 Fe2 C13 101.9(3) . . ? C11 Fe2 C13 98.5(3) . . ? C12 Fe2 C7 141.5(2) . . ? C11 Fe2 C7 92.1(2) . . ? C13 Fe2 C7 115.9(2) . . ? C12 Fe2 Se1 90.6(2) . . ? C11 Fe2 Se1 164.2(2) . . ? C13 Fe2 Se1 97.0(2) . . ? C7 Fe2 Se1 78.39(13) . . ? C12 Fe2 Fe1 91.5(2) . . ? C11 Fe2 Fe1 106.5(2) . . ? C13 Fe2 Fe1 151.8(2) . . ? C7 Fe2 Fe1 51.45(13) . . ? Se1 Fe2 Fe1 57.70(3) . . ? C2 C1 Se1 105.2(3) . . ? C3 C2 C7 120.6(5) . . ? C3 C2 C1 119.0(5) . . ? C7 C2 C1 120.3(5) . . ? C4 C3 C2 121.4(5) . . ? C3 C4 C5 120.1(6) . . ? C6 C5 C4 119.8(5) . . ? C5 C6 C7 123.1(5) . . ? C6 C7 C2 115.1(5) . . ? C6 C7 Fe1 124.8(4) . . ? C2 C7 Fe1 119.6(4) . . ? C6 C7 Fe2 112.9(3) . . ? C2 C7 Fe2 93.2(3) . . ? Fe1 C7 Fe2 71.5(2) . . ? O1 C8 Fe1 178.7(6) . . ? O2 C9 Fe1 179.1(6) . . ? O3 C10 Fe1 178.0(6) . . ? O4 C11 Fe2 177.7(6) . . ? O5 C12 Fe2 179.4(5) . . ? O6 C13 Fe2 178.3(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 C1 Se1 Fe1 C8 110.9(5) . . . . ? Fe2 Se1 Fe1 C8 23.4(5) . . . . ? C1 Se1 Fe1 C9 -155.1(2) . . . . ? Fe2 Se1 Fe1 C9 117.4(2) . . . . ? C1 Se1 Fe1 C10 -57.5(3) . . . . ? Fe2 Se1 Fe1 C10 -144.9(2) . . . . ? C1 Se1 Fe1 C7 31.4(2) . . . . ? Fe2 Se1 Fe1 C7 -56.08(13) . . . . ? C1 Se1 Fe1 Fe2 87.5(2) . . . . ? Fe2 Se1 Fe1 Fe2 0.0 . . . . ? C1 Se1 Fe2 C12 171.8(2) . . . . ? Fe1 Se1 Fe2 C12 -91.4(2) . . . . ? C1 Se1 Fe2 C11 -99.2(7) . . . . ? Fe1 Se1 Fe2 C11 -2.4(7) . . . . ? C1 Se1 Fe2 C13 69.7(3) . . . . ? Fe1 Se1 Fe2 C13 166.5(2) . . . . ? C1 Se1 Fe2 C7 -45.3(2) . . . . ? Fe1 Se1 Fe2 C7 51.48(13) . . . . ? C1 Se1 Fe2 Fe1 -96.8(2) . . . . ? Fe1 Se1 Fe2 Fe1 0.0 . . . . ? C8 Fe1 Fe2 C12 -80.6(3) . . . . ? C9 Fe1 Fe2 C12 15.3(3) . . . . ? C10 Fe1 Fe2 C12 158.7(4) . . . . ? C7 Fe1 Fe2 C12 -168.7(2) . . . . ? Se1 Fe1 Fe2 C12 89.8(2) . . . . ? C8 Fe1 Fe2 C11 9.0(3) . . . . ? C9 Fe1 Fe2 C11 104.8(3) . . . . ? C10 Fe1 Fe2 C11 -111.7(4) . . . . ? C7 Fe1 Fe2 C11 -79.2(2) . . . . ? Se1 Fe1 Fe2 C11 179.3(2) . . . . ? C8 Fe1 Fe2 C13 160.4(5) . . . . ? C9 Fe1 Fe2 C13 -103.8(5) . . . . ? C10 Fe1 Fe2 C13 39.7(5) . . . . ? C7 Fe1 Fe2 C13 72.2(4) . . . . ? Se1 Fe1 Fe2 C13 -29.3(4) . . . . ? C8 Fe1 Fe2 C7 88.2(3) . . . . ? C9 Fe1 Fe2 C7 -176.0(3) . . . . ? C10 Fe1 Fe2 C7 -32.6(4) . . . . ? C7 Fe1 Fe2 C7 0.0 . . . . ? Se1 Fe1 Fe2 C7 -101.5(2) . . . . ? C8 Fe1 Fe2 Se1 -170.3(2) . . . . ? C9 Fe1 Fe2 Se1 -74.5(2) . . . . ? C10 Fe1 Fe2 Se1 68.9(3) . . . . ? C7 Fe1 Fe2 Se1 101.5(2) . . . . ? Se1 Fe1 Fe2 Se1 0.0 . . . . ? Fe1 Se1 C1 C2 -38.5(4) . . . . ? Fe2 Se1 C1 C2 24.8(4) . . . . ? Se1 C1 C2 C3 -156.9(4) . . . . ? Se1 C1 C2 C7 27.5(6) . . . . ? C7 C2 C3 C4 1.6(9) . . . . ? C1 C2 C3 C4 -173.9(5) . . . . ? C2 C3 C4 C5 -1.1(9) . . . . ? C3 C4 C5 C6 -0.2(8) . . . . ? C4 C5 C6 C7 1.0(8) . . . . ? C5 C6 C7 C2 -0.5(7) . . . . ? C5 C6 C7 Fe1 171.4(4) . . . . ? C5 C6 C7 Fe2 -105.8(5) . . . . ? C3 C2 C7 C6 -0.8(7) . . . . ? C1 C2 C7 C6 174.7(5) . . . . ? C3 C2 C7 Fe1 -173.2(4) . . . . ? C1 C2 C7 Fe1 2.4(6) . . . . ? C3 C2 C7 Fe2 116.3(5) . . . . ? C1 C2 C7 Fe2 -68.2(5) . . . . ? C8 Fe1 C7 C6 7.7(4) . . . . ? C9 Fe1 C7 C6 125.7(12) . . . . ? C10 Fe1 C7 C6 -93.3(4) . . . . ? Se1 Fe1 C7 C6 163.4(4) . . . . ? Fe2 Fe1 C7 C6 105.5(4) . . . . ? C8 Fe1 C7 C2 179.3(4) . . . . ? C9 Fe1 C7 C2 -62.8(13) . . . . ? C10 Fe1 C7 C2 78.2(4) . . . . ? Se1 Fe1 C7 C2 -25.0(3) . . . . ? Fe2 Fe1 C7 C2 -82.9(4) . . . . ? C8 Fe1 C7 Fe2 -97.8(2) . . . . ? C9 Fe1 C7 Fe2 20.2(13) . . . . ? C10 Fe1 C7 Fe2 161.2(2) . . . . ? Se1 Fe1 C7 Fe2 57.94(8) . . . . ? Fe2 Fe1 C7 Fe2 0.0 . . . . ? C12 Fe2 C7 C6 -102.6(5) . . . . ? C11 Fe2 C7 C6 -11.3(4) . . . . ? C13 Fe2 C7 C6 89.2(4) . . . . ? Se1 Fe2 C7 C6 -178.6(4) . . . . ? Fe1 Fe2 C7 C6 -120.8(4) . . . . ? C12 Fe2 C7 C2 138.5(4) . . . . ? C11 Fe2 C7 C2 -130.2(4) . . . . ? C13 Fe2 C7 C2 -29.8(4) . . . . ? Se1 Fe2 C7 C2 62.5(3) . . . . ? Fe1 Fe2 C7 C2 120.2(3) . . . . ? C12 Fe2 C7 Fe1 18.3(4) . . . . ? C11 Fe2 C7 Fe1 109.6(2) . . . . ? C13 Fe2 C7 Fe1 -150.0(2) . . . . ? Se1 Fe2 C7 Fe1 -57.74(9) . . . . ? Fe1 Fe2 C7 Fe1 0.0 . . . . ? C9 Fe1 C8 O1 -15.2(208) . . . . ? C10 Fe1 C8 O1 -113.4(208) . . . . ? C7 Fe1 C8 O1 155.3(208) . . . . ? Se1 Fe1 C8 O1 78.2(208) . . . . ? Fe2 Fe1 C8 O1 98.3(208) . . . . ? C8 Fe1 C9 O2 -76.1(382) . . . . ? C10 Fe1 C9 O2 25.2(382) . . . . ? C7 Fe1 C9 O2 165.8(373) . . . . ? Se1 Fe1 C9 O2 128.5(382) . . . . ? Fe2 Fe1 C9 O2 -175.9(1000) . . . . ? C8 Fe1 C10 O3 -89.1(166) . . . . ? C9 Fe1 C10 O3 177.1(1000) . . . . ? C7 Fe1 C10 O3 3.9(166) . . . . ? Se1 Fe1 C10 O3 86.0(166) . . . . ? Fe2 Fe1 C10 O3 30.8(168) . . . . ? C12 Fe2 C11 O4 16.7(117) . . . . ? C13 Fe2 C11 O4 118.6(117) . . . . ? C7 Fe2 C11 O4 -124.9(117) . . . . ? Se1 Fe2 C11 O4 -72.5(118) . . . . ? Fe1 Fe2 C11 O4 -74.6(117) . . . . ? C11 Fe2 C12 O5 50.4(590) . . . . ? C13 Fe2 C12 O5 -48.1(590) . . . . ? C7 Fe2 C12 O5 142.7(588) . . . . ? Se1 Fe2 C12 O5 -145.4(590) . . . . ? Fe1 Fe2 C12 O5 156.9(1000) . . . . ? C12 Fe2 C13 O6 -39.0(190) . . . . ? C11 Fe2 C13 O6 -130.0(190) . . . . ? C7 Fe2 C13 O6 133.5(189) . . . . ? Se1 Fe2 C13 O6 53.1(190) . . . . ? Fe1 Fe2 C13 O6 77.7(191) . . . . ? _refine_diff_density_max 0.804 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.114 #=END data_zuln188 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15 H6 Fe3 O8 Se' _chemical_formula_weight 560.71 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2640(10) _cell_length_b 15.591(2) _cell_length_c 13.628(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.340(10) _cell_angle_gamma 90.00 _cell_volume 1741.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10382 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.2 _exptl_crystal_description ? _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.139 _exptl_crystal_density_method ? _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 4.597 _exptl_absorpt_correction_type ; Specific absorption corrections not applied. Averaging of symmetry equivalent reflections for small near equi-dimensional crystal will minimize absorption effects. ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKa _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku area detector diffractometer' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10382 #all data with I > 1sigma(I) _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.22 _reflns_number_total 2899 _reflns_number_observed 2733 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ; Unit cell dimensions were obtained by post refinement of the full data set. ; _computing_data_reduction ? _computing_structure_solution 'Texsan (see reference 11)' _computing_structure_refinement 'SHELXL-93 (see reference 12)' _computing_molecular_graphics 'ORTEP (see reference 13)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^. Weighted R-factors, wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[s^2^(Fo^2^)+( 0.0564P)^2^+0.8212P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2899 #all data with I > 1sigma(I) _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 #all data with I > 1sigma(I) _refine_ls_R_factor_obs 0.0366 #all data with I > 2sigma(I) _refine_ls_wR_factor_all 0.1009 _refine_ls_wR_factor_obs 0.0985 _refine_ls_goodness_of_fit_all 1.166 _refine_ls_goodness_of_fit_obs 1.175 _refine_ls_restrained_S_all 1.166 _refine_ls_restrained_S_obs 1.175 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Se1 Se 0.08467(5) 0.17030(3) 0.74522(3) 0.0434(2) Uani 1 d . . Fe1 Fe -0.02340(7) 0.18367(3) 0.89624(4) 0.0389(2) Uani 1 d . . Fe2 Fe -0.02395(7) 0.30816(3) 0.77472(4) 0.0375(2) Uani 1 d . . Fe3 Fe 0.26402(7) 0.38754(3) 0.86821(4) 0.0378(2) Uani 1 d . . O1 O 0.1686(5) 0.0558(2) 1.0162(3) 0.0835(12) Uani 1 d . . O2 O -0.3051(6) 0.0757(3) 0.8204(3) 0.0927(13) Uani 1 d . . O3 O -0.1989(4) 0.2539(2) 1.0503(3) 0.0660(9) Uani 1 d . . O4 O -0.3493(4) 0.2562(3) 0.6885(3) 0.0687(9) Uani 1 d . . O5 O -0.1942(4) 0.4357(2) 0.8793(3) 0.0724(10) Uani 1 d . . O6 O 0.0425(6) 0.4030(4) 0.5984(3) 0.105(2) Uani 1 d . . O7 O 0.1197(5) 0.5577(2) 0.8694(3) 0.0676(9) Uani 1 d . . O8 O 0.4113(6) 0.4304(3) 0.6915(3) 0.0889(13) Uani 1 d . . C1 C 0.3102(5) 0.1881(3) 0.8020(3) 0.0436(9) Uani 1 d . . H1A H 0.3573(5) 0.1347(3) 0.8286(3) 0.052 Uiso 1 calc R . H1B H 0.3740(5) 0.2084(3) 0.7516(3) 0.052 Uiso 1 calc R . C2 C 0.3111(5) 0.2528(2) 0.8819(3) 0.0378(8) Uani 1 d . . C3 C 0.4537(5) 0.2987(3) 0.9130(3) 0.0431(9) Uani 1 d . . H3 H 0.5486(5) 0.2852(3) 0.8864(3) 0.052 Uiso 1 calc R . C4 C 0.4575(5) 0.3652(3) 0.9838(3) 0.0477(9) Uani 1 d . . H4 H 0.5516(5) 0.3970(3) 1.0022(3) 0.057 Uiso 1 calc R . C5 C 0.3141(5) 0.3810(3) 1.0252(3) 0.0447(9) Uani 1 d . . H5 H 0.3139(5) 0.4225(3) 1.0742(3) 0.054 Uiso 1 calc R . C6 C 0.1718(5) 0.3358(2) 0.9941(3) 0.0399(9) Uani 1 d . . H6 H 0.0780(5) 0.3507(2) 1.0213(3) 0.048 Uiso 1 calc R . C7 C 0.1602(5) 0.2676(2) 0.9230(3) 0.0374(8) Uani 1 d . . C8 C 0.0922(6) 0.1036(3) 0.9692(3) 0.0510(10) Uani 1 d . . C9 C -0.1966(7) 0.1176(3) 0.8496(4) 0.0594(12) Uani 1 d . . C10 C -0.1297(5) 0.2269(3) 0.9895(3) 0.0470(9) Uani 1 d . . C11 C -0.2186(5) 0.2743(3) 0.7221(3) 0.0456(9) Uani 1 d . . C12 C -0.1210(6) 0.3874(3) 0.8388(3) 0.0508(10) Uani 1 d . . C13 C 0.0230(6) 0.3671(4) 0.6691(4) 0.0618(12) Uani 1 d . . C14 C 0.1764(6) 0.4908(3) 0.8679(3) 0.0478(10) Uani 1 d . . C15 C 0.3495(6) 0.4125(3) 0.7597(3) 0.0551(11) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0453(3) 0.0485(3) 0.0361(2) -0.0105(2) 0.0039(2) 0.0047(2) Fe1 0.0407(4) 0.0401(3) 0.0361(3) 0.0026(2) 0.0064(2) -0.0010(2) Fe2 0.0385(4) 0.0438(3) 0.0304(3) 0.0007(2) 0.0052(2) 0.0048(2) Fe3 0.0435(4) 0.0385(3) 0.0321(3) 0.0018(2) 0.0079(2) -0.0018(2) O1 0.080(3) 0.065(2) 0.100(3) 0.034(2) -0.007(2) 0.006(2) O2 0.085(3) 0.080(3) 0.106(3) 0.005(2) -0.013(2) -0.033(2) O3 0.055(2) 0.093(3) 0.054(2) -0.004(2) 0.022(2) 0.002(2) O4 0.050(2) 0.094(3) 0.060(2) -0.021(2) 0.003(2) 0.000(2) O5 0.065(2) 0.065(2) 0.090(3) -0.019(2) 0.020(2) 0.014(2) O6 0.094(3) 0.150(4) 0.075(3) 0.063(3) 0.026(2) 0.015(3) O7 0.089(3) 0.041(2) 0.076(2) 0.007(2) 0.023(2) 0.008(2) O8 0.119(4) 0.089(3) 0.069(2) 0.019(2) 0.053(2) -0.001(2) C1 0.038(2) 0.051(2) 0.042(2) -0.007(2) 0.009(2) 0.007(2) C2 0.039(2) 0.040(2) 0.035(2) 0.0038(15) 0.009(2) 0.004(2) C3 0.031(2) 0.058(2) 0.039(2) -0.001(2) -0.002(2) 0.003(2) C4 0.051(3) 0.050(2) 0.041(2) 0.000(2) 0.000(2) -0.004(2) C5 0.054(3) 0.047(2) 0.031(2) -0.005(2) -0.004(2) 0.001(2) C6 0.054(3) 0.040(2) 0.027(2) 0.0015(14) 0.011(2) 0.003(2) C7 0.048(2) 0.035(2) 0.030(2) 0.0028(14) 0.008(2) 0.000(2) C8 0.054(3) 0.045(2) 0.054(2) 0.006(2) 0.006(2) -0.006(2) C9 0.064(3) 0.056(3) 0.057(3) 0.006(2) 0.005(2) -0.004(2) C10 0.047(2) 0.052(2) 0.043(2) 0.006(2) 0.008(2) -0.004(2) C11 0.041(3) 0.060(3) 0.035(2) -0.007(2) 0.005(2) 0.006(2) C12 0.056(3) 0.046(2) 0.050(2) -0.001(2) 0.006(2) 0.002(2) C13 0.049(3) 0.083(3) 0.055(3) 0.019(2) 0.009(2) 0.013(2) C14 0.056(3) 0.047(2) 0.042(2) 0.005(2) 0.011(2) -0.004(2) C15 0.066(3) 0.053(2) 0.049(2) 0.002(2) 0.018(2) 0.003(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 Se1 C1 1.945(4) . ? Se1 Fe1 2.3551(7) . ? Se1 Fe2 2.3831(7) . ? Fe1 C10 1.769(4) . ? Fe1 C8 1.794(5) . ? Fe1 C9 1.811(5) . ? Fe1 C7 2.001(4) . ? Fe1 Fe2 2.5511(8) . ? Fe2 C11 1.757(5) . ? Fe2 C12 1.764(4) . ? Fe2 C13 1.791(5) . ? Fe2 C7 2.452(4) . ? Fe2 Fe3 2.8362(9) . ? Fe3 C15 1.762(4) . ? Fe3 C14 1.765(5) . ? Fe3 C3 2.122(4) . ? Fe3 C6 2.124(4) . ? Fe3 C4 2.125(4) . ? Fe3 C5 2.129(4) . ? Fe3 C2 2.140(4) . ? Fe3 C7 2.226(4) . ? O1 C8 1.123(6) . ? O2 C9 1.139(6) . ? O3 C10 1.145(5) . ? O4 C11 1.153(5) . ? O5 C12 1.151(5) . ? O6 C13 1.143(6) . ? O7 C14 1.145(5) . ? O8 C15 1.150(6) . ? C1 C2 1.484(5) . ? C2 C3 1.397(6) . ? C2 C7 1.449(5) . ? C3 C4 1.413(6) . ? C4 C5 1.398(6) . ? C5 C6 1.390(6) . ? C6 C7 1.434(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 C1 Se1 Fe1 95.23(12) . . ? C1 Se1 Fe2 99.61(11) . . ? Fe1 Se1 Fe2 65.15(2) . . ? C10 Fe1 C8 98.3(2) . . ? C10 Fe1 C9 91.5(2) . . ? C8 Fe1 C9 98.0(2) . . ? C10 Fe1 C7 93.1(2) . . ? C8 Fe1 C7 90.9(2) . . ? C9 Fe1 C7 169.2(2) . . ? C10 Fe1 Se1 160.16(14) . . ? C8 Fe1 Se1 100.84(15) . . ? C9 Fe1 Se1 90.8(2) . . ? C7 Fe1 Se1 81.57(10) . . ? C10 Fe1 Fe2 102.53(14) . . ? C8 Fe1 Fe2 147.78(15) . . ? C9 Fe1 Fe2 105.6(2) . . ? C7 Fe1 Fe2 63.84(10) . . ? Se1 Fe1 Fe2 57.96(2) . . ? C11 Fe2 C12 87.8(2) . . ? C11 Fe2 C13 96.2(2) . . ? C12 Fe2 C13 101.4(2) . . ? C11 Fe2 Se1 90.30(14) . . ? C12 Fe2 Se1 156.96(15) . . ? C13 Fe2 Se1 101.7(2) . . ? C11 Fe2 C7 134.3(2) . . ? C12 Fe2 C7 92.7(2) . . ? C13 Fe2 C7 128.2(2) . . ? Se1 Fe2 C7 72.47(9) . . ? C11 Fe2 Fe1 87.82(14) . . ? C12 Fe2 Fe1 100.07(15) . . ? C13 Fe2 Fe1 158.3(2) . . ? Se1 Fe2 Fe1 56.90(2) . . ? C7 Fe2 Fe1 47.11(9) . . ? C11 Fe2 Fe3 170.59(14) . . ? C12 Fe2 Fe3 83.1(2) . . ? C13 Fe2 Fe3 83.2(2) . . ? Se1 Fe2 Fe3 99.02(2) . . ? C7 Fe2 Fe3 49.12(9) . . ? Fe1 Fe2 Fe3 96.23(3) . . ? C15 Fe3 C14 90.3(2) . . ? C15 Fe3 C3 91.4(2) . . ? C14 Fe3 C3 152.1(2) . . ? C15 Fe3 C6 170.4(2) . . ? C14 Fe3 C6 99.1(2) . . ? C3 Fe3 C6 81.2(2) . . ? C15 Fe3 C4 108.3(2) . . ? C14 Fe3 C4 114.9(2) . . ? C3 Fe3 C4 38.9(2) . . ? C6 Fe3 C4 69.6(2) . . ? C15 Fe3 C5 143.8(2) . . ? C14 Fe3 C5 94.2(2) . . ? C3 Fe3 C5 68.8(2) . . ? C6 Fe3 C5 38.2(2) . . ? C4 Fe3 C5 38.4(2) . . ? C15 Fe3 C2 101.7(2) . . ? C14 Fe3 C2 164.9(2) . . ? C3 Fe3 C2 38.3(2) . . ? C6 Fe3 C2 68.69(14) . . ? C4 Fe3 C2 70.3(2) . . ? C5 Fe3 C2 81.71(15) . . ? C15 Fe3 C7 132.9(2) . . ? C14 Fe3 C7 126.3(2) . . ? C3 Fe3 C7 69.96(15) . . ? C6 Fe3 C7 38.42(14) . . ? C4 Fe3 C7 84.2(2) . . ? C5 Fe3 C7 69.93(15) . . ? C2 Fe3 C7 38.70(13) . . ? C15 Fe3 Fe2 97.1(2) . . ? C14 Fe3 Fe2 94.38(15) . . ? C3 Fe3 Fe2 113.02(11) . . ? C6 Fe3 Fe2 80.22(12) . . ? C4 Fe3 Fe2 140.35(12) . . ? C5 Fe3 Fe2 118.35(12) . . ? C2 Fe3 Fe2 75.14(11) . . ? C7 Fe3 Fe2 56.41(10) . . ? C2 C1 Se1 107.7(3) . . ? C3 C2 C7 122.4(3) . . ? C3 C2 C1 119.7(3) . . ? C7 C2 C1 117.9(3) . . ? C3 C2 Fe3 70.2(2) . . ? C7 C2 Fe3 73.9(2) . . ? C1 C2 Fe3 128.3(3) . . ? C2 C3 C4 121.8(4) . . ? C2 C3 Fe3 71.6(2) . . ? C4 C3 Fe3 70.7(2) . . ? C5 C4 C3 117.3(4) . . ? C5 C4 Fe3 71.0(2) . . ? C3 C4 Fe3 70.4(2) . . ? C6 C5 C4 121.0(4) . . ? C6 C5 Fe3 70.7(2) . . ? C4 C5 Fe3 70.7(2) . . ? C5 C6 C7 124.3(4) . . ? C5 C6 Fe3 71.1(2) . . ? C7 C6 Fe3 74.6(2) . . ? C6 C7 C2 113.1(3) . . ? C6 C7 Fe1 126.2(3) . . ? C2 C7 Fe1 119.7(3) . . ? C6 C7 Fe3 67.0(2) . . ? C2 C7 Fe3 67.5(2) . . ? Fe1 C7 Fe3 143.5(2) . . ? C6 C7 Fe2 110.3(3) . . ? C2 C7 Fe2 101.4(2) . . ? Fe1 C7 Fe2 69.05(12) . . ? Fe3 C7 Fe2 74.47(11) . . ? O1 C8 Fe1 177.4(4) . . ? O2 C9 Fe1 179.6(5) . . ? O3 C10 Fe1 179.2(4) . . ? O4 C11 Fe2 176.6(4) . . ? O5 C12 Fe2 175.1(4) . . ? O6 C13 Fe2 175.1(5) . . ? O7 C14 Fe3 178.8(4) . . ? O8 C15 Fe3 176.9(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 C1 Se1 Fe1 C10 109.5(4) . . . . ? Fe2 Se1 Fe1 C10 11.3(4) . . . . ? C1 Se1 Fe1 C8 -55.5(2) . . . . ? Fe2 Se1 Fe1 C8 -153.68(15) . . . . ? C1 Se1 Fe1 C9 -153.8(2) . . . . ? Fe2 Se1 Fe1 C9 108.0(2) . . . . ? C1 Se1 Fe1 C7 33.8(2) . . . . ? Fe2 Se1 Fe1 C7 -64.34(11) . . . . ? C1 Se1 Fe1 Fe2 98.18(12) . . . . ? Fe2 Se1 Fe1 Fe2 0.0 . . . . ? C1 Se1 Fe2 C11 -178.5(2) . . . . ? Fe1 Se1 Fe2 C11 -87.20(13) . . . . ? C1 Se1 Fe2 C12 -93.4(4) . . . . ? Fe1 Se1 Fe2 C12 -2.1(4) . . . . ? C1 Se1 Fe2 C13 85.1(2) . . . . ? Fe1 Se1 Fe2 C13 176.4(2) . . . . ? C1 Se1 Fe2 C7 -41.6(2) . . . . ? Fe1 Se1 Fe2 C7 49.75(9) . . . . ? C1 Se1 Fe2 Fe1 -91.34(12) . . . . ? Fe1 Se1 Fe2 Fe1 0.0 . . . . ? C1 Se1 Fe2 Fe3 0.25(12) . . . . ? Fe1 Se1 Fe2 Fe3 91.59(3) . . . . ? C10 Fe1 Fe2 C11 -84.3(2) . . . . ? C8 Fe1 Fe2 C11 146.5(3) . . . . ? C9 Fe1 Fe2 C11 10.8(2) . . . . ? C7 Fe1 Fe2 C11 -171.6(2) . . . . ? Se1 Fe1 Fe2 C11 91.79(13) . . . . ? C10 Fe1 Fe2 C12 3.1(2) . . . . ? C8 Fe1 Fe2 C12 -126.1(3) . . . . ? C9 Fe1 Fe2 C12 98.2(2) . . . . ? C7 Fe1 Fe2 C12 -84.2(2) . . . . ? Se1 Fe1 Fe2 C12 179.2(2) . . . . ? C10 Fe1 Fe2 C13 174.4(5) . . . . ? C8 Fe1 Fe2 C13 45.3(6) . . . . ? C9 Fe1 Fe2 C13 -90.4(5) . . . . ? C7 Fe1 Fe2 C13 87.1(5) . . . . ? Se1 Fe1 Fe2 C13 -9.5(5) . . . . ? C10 Fe1 Fe2 Se1 -176.08(15) . . . . ? C8 Fe1 Fe2 Se1 54.8(3) . . . . ? C9 Fe1 Fe2 Se1 -80.9(2) . . . . ? C7 Fe1 Fe2 Se1 96.59(12) . . . . ? Se1 Fe1 Fe2 Se1 0.0 . . . . ? C10 Fe1 Fe2 C7 87.3(2) . . . . ? C8 Fe1 Fe2 C7 -41.8(3) . . . . ? C9 Fe1 Fe2 C7 -177.5(2) . . . . ? C7 Fe1 Fe2 C7 0.0 . . . . ? Se1 Fe1 Fe2 C7 -96.59(12) . . . . ? C10 Fe1 Fe2 Fe3 87.20(15) . . . . ? C8 Fe1 Fe2 Fe3 -42.0(3) . . . . ? C9 Fe1 Fe2 Fe3 -177.7(2) . . . . ? C7 Fe1 Fe2 Fe3 -0.13(12) . . . . ? Se1 Fe1 Fe2 Fe3 -96.73(2) . . . . ? C11 Fe2 Fe3 C15 -106.9(8) . . . . ? C12 Fe2 Fe3 C15 -122.6(2) . . . . ? C13 Fe2 Fe3 C15 -20.3(2) . . . . ? Se1 Fe2 Fe3 C15 80.5(2) . . . . ? C7 Fe2 Fe3 C15 137.8(2) . . . . ? Fe1 Fe2 Fe3 C15 137.9(2) . . . . ? C11 Fe2 Fe3 C14 -16.1(8) . . . . ? C12 Fe2 Fe3 C14 -31.8(2) . . . . ? C13 Fe2 Fe3 C14 70.5(2) . . . . ? Se1 Fe2 Fe3 C14 171.34(13) . . . . ? C7 Fe2 Fe3 C14 -131.4(2) . . . . ? Fe1 Fe2 Fe3 C14 -131.27(13) . . . . ? C11 Fe2 Fe3 C3 158.5(8) . . . . ? C12 Fe2 Fe3 C3 142.8(2) . . . . ? C13 Fe2 Fe3 C3 -114.9(2) . . . . ? Se1 Fe2 Fe3 C3 -14.07(12) . . . . ? C7 Fe2 Fe3 C3 43.2(2) . . . . ? Fe1 Fe2 Fe3 C3 43.32(12) . . . . ? C11 Fe2 Fe3 C6 82.4(8) . . . . ? C12 Fe2 Fe3 C6 66.7(2) . . . . ? C13 Fe2 Fe3 C6 169.1(2) . . . . ? Se1 Fe2 Fe3 C6 -90.12(11) . . . . ? C7 Fe2 Fe3 C6 -32.9(2) . . . . ? Fe1 Fe2 Fe3 C6 -32.73(11) . . . . ? C11 Fe2 Fe3 C4 122.9(8) . . . . ? C12 Fe2 Fe3 C4 107.1(2) . . . . ? C13 Fe2 Fe3 C4 -150.5(2) . . . . ? Se1 Fe2 Fe3 C4 -49.7(2) . . . . ? C7 Fe2 Fe3 C4 7.6(2) . . . . ? Fe1 Fe2 Fe3 C4 7.7(2) . . . . ? C11 Fe2 Fe3 C5 81.0(8) . . . . ? C12 Fe2 Fe3 C5 65.3(2) . . . . ? C13 Fe2 Fe3 C5 167.7(2) . . . . ? Se1 Fe2 Fe3 C5 -91.52(13) . . . . ? C7 Fe2 Fe3 C5 -34.3(2) . . . . ? Fe1 Fe2 Fe3 C5 -34.14(13) . . . . ? C11 Fe2 Fe3 C2 152.8(8) . . . . ? C12 Fe2 Fe3 C2 137.1(2) . . . . ? C13 Fe2 Fe3 C2 -120.5(2) . . . . ? Se1 Fe2 Fe3 C2 -19.74(10) . . . . ? C7 Fe2 Fe3 C2 37.52(15) . . . . ? Fe1 Fe2 Fe3 C2 37.65(10) . . . . ? C11 Fe2 Fe3 C7 115.3(8) . . . . ? C12 Fe2 Fe3 C7 99.6(2) . . . . ? C13 Fe2 Fe3 C7 -158.1(2) . . . . ? Se1 Fe2 Fe3 C7 -57.26(11) . . . . ? C7 Fe2 Fe3 C7 0.0 . . . . ? Fe1 Fe2 Fe3 C7 0.13(11) . . . . ? Fe1 Se1 C1 C2 -36.5(3) . . . . ? Fe2 Se1 C1 C2 29.1(3) . . . . ? Se1 C1 C2 C3 -158.8(3) . . . . ? Se1 C1 C2 C7 19.4(4) . . . . ? Se1 C1 C2 Fe3 -71.5(4) . . . . ? C15 Fe3 C2 C3 77.3(3) . . . . ? C14 Fe3 C2 C3 -141.2(6) . . . . ? C3 Fe3 C2 C3 0.0 . . . . ? C6 Fe3 C2 C3 -103.3(3) . . . . ? C4 Fe3 C2 C3 -28.2(2) . . . . ? C5 Fe3 C2 C3 -66.1(2) . . . . ? C7 Fe3 C2 C3 -134.2(3) . . . . ? Fe2 Fe3 C2 C3 171.6(2) . . . . ? C15 Fe3 C2 C7 -148.5(3) . . . . ? C14 Fe3 C2 C7 -7.0(7) . . . . ? C3 Fe3 C2 C7 134.2(3) . . . . ? C6 Fe3 C2 C7 30.9(2) . . . . ? C4 Fe3 C2 C7 106.0(2) . . . . ? C5 Fe3 C2 C7 68.1(2) . . . . ? C7 Fe3 C2 C7 0.000(1) . . . . ? Fe2 Fe3 C2 C7 -54.2(2) . . . . ? C15 Fe3 C2 C1 -35.5(4) . . . . ? C14 Fe3 C2 C1 106.1(7) . . . . ? C3 Fe3 C2 C1 -112.7(4) . . . . ? C6 Fe3 C2 C1 143.9(4) . . . . ? C4 Fe3 C2 C1 -140.9(4) . . . . ? C5 Fe3 C2 C1 -178.8(4) . . . . ? C7 Fe3 C2 C1 113.1(4) . . . . ? Fe2 Fe3 C2 C1 58.8(3) . . . . ? C7 C2 C3 C4 -2.7(6) . . . . ? C1 C2 C3 C4 175.5(4) . . . . ? Fe3 C2 C3 C4 51.9(4) . . . . ? C7 C2 C3 Fe3 -54.6(3) . . . . ? C1 C2 C3 Fe3 123.5(3) . . . . ? Fe3 C2 C3 Fe3 0.0 . . . . ? C15 Fe3 C3 C2 -107.2(3) . . . . ? C14 Fe3 C3 C2 159.5(3) . . . . ? C6 Fe3 C3 C2 66.5(2) . . . . ? C4 Fe3 C3 C2 134.8(3) . . . . ? C5 Fe3 C3 C2 104.0(2) . . . . ? C2 Fe3 C3 C2 0.0 . . . . ? C7 Fe3 C3 C2 28.5(2) . . . . ? Fe2 Fe3 C3 C2 -8.9(2) . . . . ? C15 Fe3 C3 C4 118.0(3) . . . . ? C14 Fe3 C3 C4 24.7(5) . . . . ? C6 Fe3 C3 C4 -68.3(3) . . . . ? C4 Fe3 C3 C4 0.000(3) . . . . ? C5 Fe3 C3 C4 -30.8(2) . . . . ? C2 Fe3 C3 C4 -134.8(3) . . . . ? C7 Fe3 C3 C4 -106.3(3) . . . . ? Fe2 Fe3 C3 C4 -143.7(2) . . . . ? C2 C3 C4 C5 2.7(6) . . . . ? Fe3 C3 C4 C5 55.0(3) . . . . ? C2 C3 C4 Fe3 -52.3(4) . . . . ? Fe3 C3 C4 Fe3 0.000(2) . . . . ? C15 Fe3 C4 C5 162.0(3) . . . . ? C14 Fe3 C4 C5 62.8(3) . . . . ? C3 Fe3 C4 C5 -129.7(4) . . . . ? C6 Fe3 C4 C5 -28.0(2) . . . . ? C5 Fe3 C4 C5 0.000(3) . . . . ? C2 Fe3 C4 C5 -101.8(3) . . . . ? C7 Fe3 C4 C5 -64.7(3) . . . . ? Fe2 Fe3 C4 C5 -71.0(3) . . . . ? C15 Fe3 C4 C3 -68.4(3) . . . . ? C14 Fe3 C4 C3 -167.5(3) . . . . ? C3 Fe3 C4 C3 0.000(3) . . . . ? C6 Fe3 C4 C3 101.6(3) . . . . ? C5 Fe3 C4 C3 129.7(4) . . . . ? C2 Fe3 C4 C3 27.8(2) . . . . ? C7 Fe3 C4 C3 65.0(2) . . . . ? Fe2 Fe3 C4 C3 58.6(3) . . . . ? C3 C4 C5 C6 -3.0(6) . . . . ? Fe3 C4 C5 C6 51.8(3) . . . . ? C3 C4 C5 Fe3 -54.7(3) . . . . ? Fe3 C4 C5 Fe3 0.000(2) . . . . ? C15 Fe3 C5 C6 -164.3(3) . . . . ? C14 Fe3 C5 C6 99.5(3) . . . . ? C3 Fe3 C5 C6 -103.3(3) . . . . ? C6 Fe3 C5 C6 0.0 . . . . ? C4 Fe3 C5 C6 -134.5(4) . . . . ? C2 Fe3 C5 C6 -65.9(2) . . . . ? C7 Fe3 C5 C6 -27.7(2) . . . . ? Fe2 Fe3 C5 C6 2.2(3) . . . . ? C15 Fe3 C5 C4 -29.8(4) . . . . ? C14 Fe3 C5 C4 -126.0(3) . . . . ? C3 Fe3 C5 C4 31.2(2) . . . . ? C6 Fe3 C5 C4 134.5(4) . . . . ? C4 Fe3 C5 C4 0.000(3) . . . . ? C2 Fe3 C5 C4 68.6(3) . . . . ? C7 Fe3 C5 C4 106.8(3) . . . . ? Fe2 Fe3 C5 C4 136.7(2) . . . . ? C4 C5 C6 C7 3.4(6) . . . . ? Fe3 C5 C6 C7 55.1(3) . . . . ? C4 C5 C6 Fe3 -51.7(4) . . . . ? Fe3 C5 C6 Fe3 0.0 . . . . ? C15 Fe3 C6 C5 107.7(12) . . . . ? C14 Fe3 C6 C5 -85.1(3) . . . . ? C3 Fe3 C6 C5 66.7(2) . . . . ? C4 Fe3 C6 C5 28.2(2) . . . . ? C5 Fe3 C6 C5 0.0 . . . . ? C2 Fe3 C6 C5 104.2(3) . . . . ? C7 Fe3 C6 C5 135.3(4) . . . . ? Fe2 Fe3 C6 C5 -178.0(2) . . . . ? C15 Fe3 C6 C7 -27.6(13) . . . . ? C14 Fe3 C6 C7 139.6(3) . . . . ? C3 Fe3 C6 C7 -68.7(2) . . . . ? C4 Fe3 C6 C7 -107.1(3) . . . . ? C5 Fe3 C6 C7 -135.3(4) . . . . ? C2 Fe3 C6 C7 -31.1(2) . . . . ? C7 Fe3 C6 C7 0.000(2) . . . . ? Fe2 Fe3 C6 C7 46.7(2) . . . . ? C5 C6 C7 C2 -3.0(5) . . . . ? Fe3 C6 C7 C2 50.6(3) . . . . ? C5 C6 C7 Fe1 165.9(3) . . . . ? Fe3 C6 C7 Fe1 -140.5(3) . . . . ? C5 C6 C7 Fe3 -53.6(3) . . . . ? Fe3 C6 C7 Fe3 0.000(1) . . . . ? C5 C6 C7 Fe2 -115.7(4) . . . . ? Fe3 C6 C7 Fe2 -62.1(2) . . . . ? C3 C2 C7 C6 2.6(5) . . . . ? C1 C2 C7 C6 -175.5(3) . . . . ? Fe3 C2 C7 C6 -50.3(3) . . . . ? C3 C2 C7 Fe1 -167.1(3) . . . . ? C1 C2 C7 Fe1 14.7(4) . . . . ? Fe3 C2 C7 Fe1 139.9(2) . . . . ? C3 C2 C7 Fe3 53.0(3) . . . . ? C1 C2 C7 Fe3 -125.2(3) . . . . ? Fe3 C2 C7 Fe3 0.000(1) . . . . ? C3 C2 C7 Fe2 120.7(3) . . . . ? C1 C2 C7 Fe2 -57.5(3) . . . . ? Fe3 C2 C7 Fe2 67.72(14) . . . . ? C10 Fe1 C7 C6 -2.1(3) . . . . ? C8 Fe1 C7 C6 -100.5(3) . . . . ? C9 Fe1 C7 C6 113.1(10) . . . . ? Se1 Fe1 C7 C6 158.7(3) . . . . ? Fe2 Fe1 C7 C6 100.4(3) . . . . ? C10 Fe1 C7 C2 166.2(3) . . . . ? C8 Fe1 C7 C2 67.8(3) . . . . ? C9 Fe1 C7 C2 -78.6(11) . . . . ? Se1 Fe1 C7 C2 -33.1(3) . . . . ? Fe2 Fe1 C7 C2 -91.4(3) . . . . ? C10 Fe1 C7 Fe3 -102.1(3) . . . . ? C8 Fe1 C7 Fe3 159.5(3) . . . . ? C9 Fe1 C7 Fe3 13.1(12) . . . . ? Se1 Fe1 C7 Fe3 58.6(3) . . . . ? Fe2 Fe1 C7 Fe3 0.3(2) . . . . ? C10 Fe1 C7 Fe2 -102.42(15) . . . . ? C8 Fe1 C7 Fe2 159.2(2) . . . . ? C9 Fe1 C7 Fe2 12.8(11) . . . . ? Se1 Fe1 C7 Fe2 58.35(5) . . . . ? Fe2 Fe1 C7 Fe2 0.0 . . . . ? C15 Fe3 C7 C6 173.9(3) . . . . ? C14 Fe3 C7 C6 -52.6(3) . . . . ? C3 Fe3 C7 C6 101.5(3) . . . . ? C6 Fe3 C7 C6 0.000(2) . . . . ? C4 Fe3 C7 C6 64.2(2) . . . . ? C5 Fe3 C7 C6 27.5(2) . . . . ? C2 Fe3 C7 C6 129.7(3) . . . . ? Fe2 Fe3 C7 C6 -120.6(3) . . . . ? C15 Fe3 C7 C2 44.2(3) . . . . ? C14 Fe3 C7 C2 177.7(2) . . . . ? C3 Fe3 C7 C2 -28.2(2) . . . . ? C6 Fe3 C7 C2 -129.7(3) . . . . ? C4 Fe3 C7 C2 -65.5(2) . . . . ? C5 Fe3 C7 C2 -102.1(2) . . . . ? C2 Fe3 C7 C2 0.000(1) . . . . ? Fe2 Fe3 C7 C2 109.7(2) . . . . ? C15 Fe3 C7 Fe1 -65.7(4) . . . . ? C14 Fe3 C7 Fe1 67.8(4) . . . . ? C3 Fe3 C7 Fe1 -138.2(3) . . . . ? C6 Fe3 C7 Fe1 120.3(4) . . . . ? C4 Fe3 C7 Fe1 -175.4(3) . . . . ? C5 Fe3 C7 Fe1 147.9(4) . . . . ? C2 Fe3 C7 Fe1 -110.0(4) . . . . ? Fe2 Fe3 C7 Fe1 -0.3(2) . . . . ? C15 Fe3 C7 Fe2 -65.5(3) . . . . ? C14 Fe3 C7 Fe2 68.1(2) . . . . ? C3 Fe3 C7 Fe2 -137.90(15) . . . . ? C6 Fe3 C7 Fe2 120.6(3) . . . . ? C4 Fe3 C7 Fe2 -175.15(14) . . . . ? C5 Fe3 C7 Fe2 148.2(2) . . . . ? C2 Fe3 C7 Fe2 -109.7(2) . . . . ? Fe2 Fe3 C7 Fe2 0.0 . . . . ? C11 Fe2 C7 C6 -110.5(3) . . . . ? C12 Fe2 C7 C6 -20.9(3) . . . . ? C13 Fe2 C7 C6 85.8(4) . . . . ? Se1 Fe2 C7 C6 177.0(3) . . . . ? Fe1 Fe2 C7 C6 -122.2(3) . . . . ? Fe3 Fe2 C7 C6 57.6(2) . . . . ? C11 Fe2 C7 C2 129.4(3) . . . . ? C12 Fe2 C7 C2 -141.0(3) . . . . ? C13 Fe2 C7 C2 -34.3(4) . . . . ? Se1 Fe2 C7 C2 56.9(2) . . . . ? Fe1 Fe2 C7 C2 117.7(3) . . . . ? Fe3 Fe2 C7 C2 -62.5(2) . . . . ? C11 Fe2 C7 Fe1 11.7(2) . . . . ? C12 Fe2 C7 Fe1 101.3(2) . . . . ? C13 Fe2 C7 Fe1 -152.0(2) . . . . ? Se1 Fe2 C7 Fe1 -60.77(7) . . . . ? Fe1 Fe2 C7 Fe1 0.0 . . . . ? Fe3 Fe2 C7 Fe1 179.8(2) . . . . ? C11 Fe2 C7 Fe3 -168.1(2) . . . . ? C12 Fe2 C7 Fe3 -78.5(2) . . . . ? C13 Fe2 C7 Fe3 28.2(3) . . . . ? Se1 Fe2 C7 Fe3 119.40(9) . . . . ? Fe1 Fe2 C7 Fe3 -179.8(2) . . . . ? Fe3 Fe2 C7 Fe3 0.0 . . . . ? C10 Fe1 C8 O1 -79.4(102) . . . . ? C9 Fe1 C8 O1 -172.1(102) . . . . ? C7 Fe1 C8 O1 13.9(102) . . . . ? Se1 Fe1 C8 O1 95.5(102) . . . . ? Fe2 Fe1 C8 O1 50.7(103) . . . . ? C10 Fe1 C9 O2 -126.0(717) . . . . ? C8 Fe1 C9 O2 -27.3(717) . . . . ? C7 Fe1 C9 O2 118.7(712) . . . . ? Se1 Fe1 C9 O2 73.8(717) . . . . ? Fe2 Fe1 C9 O2 130.6(716) . . . . ? C8 Fe1 C10 O3 -45.4(297) . . . . ? C9 Fe1 C10 O3 53.0(297) . . . . ? C7 Fe1 C10 O3 -136.8(297) . . . . ? Se1 Fe1 C10 O3 149.5(294) . . . . ? Fe2 Fe1 C10 O3 159.3(297) . . . . ? C12 Fe2 C11 O4 23.4(63) . . . . ? C13 Fe2 C11 O4 -77.8(63) . . . . ? Se1 Fe2 C11 O4 -179.6(1000) . . . . ? C7 Fe2 C11 O4 115.0(63) . . . . ? Fe1 Fe2 C11 O4 123.6(63) . . . . ? Fe3 Fe2 C11 O4 7.8(70) . . . . ? C11 Fe2 C12 O5 18.9(51) . . . . ? C13 Fe2 C12 O5 114.7(51) . . . . ? Se1 Fe2 C12 O5 -66.8(52) . . . . ? C7 Fe2 C12 O5 -115.4(51) . . . . ? Fe1 Fe2 C12 O5 -68.5(51) . . . . ? Fe3 Fe2 C12 O5 -163.7(51) . . . . ? C11 Fe2 C13 O6 -1.2(61) . . . . ? C12 Fe2 C13 O6 -90.2(61) . . . . ? Se1 Fe2 C13 O6 90.4(61) . . . . ? C7 Fe2 C13 O6 167.2(60) . . . . ? Fe1 Fe2 C13 O6 98.5(60) . . . . ? Fe3 Fe2 C13 O6 -171.8(61) . . . . ? C15 Fe3 C14 O7 -149.2(204) . . . . ? C3 Fe3 C14 O7 -55.6(205) . . . . ? C6 Fe3 C14 O7 32.9(204) . . . . ? C4 Fe3 C14 O7 -38.8(205) . . . . ? C5 Fe3 C14 O7 -5.2(204) . . . . ? C2 Fe3 C14 O7 68.3(206) . . . . ? C7 Fe3 C14 O7 62.9(205) . . . . ? Fe2 Fe3 C14 O7 113.7(204) . . . . ? C14 Fe3 C15 O8 86.4(84) . . . . ? C3 Fe3 C15 O8 -65.7(84) . . . . ? C6 Fe3 C15 O8 -106.2(82) . . . . ? C4 Fe3 C15 O8 -30.0(84) . . . . ? C5 Fe3 C15 O8 -11.0(85) . . . . ? C2 Fe3 C15 O8 -102.9(84) . . . . ? C7 Fe3 C15 O8 -129.3(83) . . . . ? Fe2 Fe3 C15 O8 -179.1(1000) . . . . ? _refine_diff_density_max 0.498 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.101