#------------------------------------------------------------------------------ #$Date: 2024-12-07 19:07:00 +0200 (Sat, 07 Dec 2024) $ #$Revision: 296763 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/26/2312653.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2312653 loop_ _publ_author_name 'Blockhaus, Tobias' 'Sünkel, Karlheinz' _publ_section_title ; Molecular and crystal structures of six poly(arylsulfinyl)- and poly(arylsulfanyl)ferrocenes. ; _journal_coeditor_code UX3008 _journal_issue 'Pt 11' _journal_name_full 'Acta crystallographica. Section C, Structural chemistry' _journal_page_first 716 _journal_page_last 727 _journal_paper_doi 10.1107/S2053229624009318 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '[Fe (C5 H5) (C19 H17 O2 S2)]' _chemical_formula_moiety 'C24 H22 Fe O2 S2' _chemical_formula_sum 'C24 H22 Fe O2 S2' _chemical_formula_weight 462.38 _chemical_name_systematic ; 1,2-Bis[(4-methylbenzene)sulfinyl]ferrocene ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 109.4670(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.8964(2) _cell_length_b 12.9064(3) _cell_length_c 11.0124(3) _cell_measurement_reflns_used 6560 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 27.4727 _cell_measurement_theta_min 4.9918 _cell_volume 1058.16(5) _computing_cell_refinement ; APEX2 (Bruker, 2011) ; _computing_data_collection ; APEX2 (Bruker, 2011) ; _computing_data_reduction ; SAINT (Bruker, 2011) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2020) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 297(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method 'mix of omega and phi scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_unetI/netI 0.0403 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 11282 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.490 _diffrn_reflns_theta_min 3.157 _diffrn_source 'rotating anode generator' _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 480 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.408 _refine_diff_density_min -0.342 _refine_ls_abs_structure_details ; Flack x determined using 1876 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.014(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 4815 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.154 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0337 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.2017P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.0844 _reflns_number_gt 4393 _reflns_number_total 4815 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ux3008.cif _cod_data_source_block comp_2a _cod_depositor_comments 'Adding full bibliography for 2312653--2312658.cif.' _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2312653 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.938 _shelx_estimated_absorpt_t_max 0.964 _shelx_hkl_file ; -1 0 0 0.07 0.28 -1 0 0 -0.07 0.26 2 0 0 9851.31 417.88 3 0 0 4559.89 227.88 -4 0 0 244.87 11.16 -4 0 0 243.91 11.35 4 0 0 239.83 11.19 4 0 0 234.29 11.04 -5 0 0 1538.35 63.16 -5 0 0 1599.44 63.03 5 0 0 1545.39 63.04 5 0 0 1576.80 63.76 6 0 0 154.62 9.17 -6 0 0 162.33 9.02 -6 0 0 169.62 9.46 7 0 0 129.42 8.54 -7 0 0 131.96 8.43 8 0 0 18.88 3.95 -8 0 0 18.48 3.88 9 0 0 69.69 6.85 -1 -1 0 2670.63 129.57 1 -1 0 2790.29 122.39 2 -1 0 805.86 32.76 2 1 0 816.64 32.72 2 1 0 837.11 32.78 3 -1 0 933.90 37.86 -3 -1 0 927.32 37.86 -3 -1 0 914.61 37.82 3 -1 0 900.87 37.47 -3 1 0 982.31 37.63 3 1 0 949.81 37.81 -3 1 0 963.80 37.92 3 1 0 950.41 37.83 3 1 0 929.47 37.77 4 -1 0 144.71 7.28 4 -1 0 147.01 6.95 -4 -1 0 147.16 7.31 -4 -1 0 140.36 7.27 4 1 0 129.12 7.05 -4 1 0 131.53 7.20 -4 1 0 133.86 6.93 4 1 0 123.48 7.00 4 1 0 125.85 6.99 5 -1 0 124.09 6.64 -5 -1 0 116.23 7.03 5 -1 0 116.07 6.89 -5 1 0 126.63 6.90 5 1 0 122.69 6.97 5 1 0 127.21 6.98 5 1 0 121.93 7.04 -5 1 0 112.48 7.13 6 -1 0 274.35 13.77 -6 -1 0 289.12 14.33 -6 1 0 297.20 14.57 6 1 0 312.85 14.54 -6 1 0 297.70 15.03 -7 -1 0 90.58 6.68 7 1 0 85.96 6.63 -7 1 0 89.14 6.40 -7 1 0 87.93 6.92 8 -1 0 192.95 12.00 -8 1 0 199.50 12.10 -8 1 0 212.26 11.53 8 1 0 207.65 11.92 -9 -1 0 14.78 3.69 9 -1 0 9.87 3.53 -9 1 0 5.47 3.14 9 1 0 11.62 3.59 0 -2 0 3300.83 152.70 0 2 0 3591.61 155.25 -1 2 0 261.80 10.29 -2 -2 0 202.90 8.92 2 -2 0 201.94 8.85 2 -2 0 197.23 8.29 -2 -2 0 200.91 8.70 2 2 0 191.48 8.65 -2 2 0 199.41 8.31 -2 2 0 200.99 8.88 2 2 0 200.88 8.89 3 -2 0 479.01 20.22 -3 -2 0 466.28 20.25 3 -2 0 467.17 19.61 3 2 0 474.52 20.11 -3 2 0 492.07 19.71 3 2 0 483.73 20.06 3 2 0 494.69 20.28 -3 2 0 494.43 20.29 4 -2 0 305.28 13.88 -4 -2 0 290.51 14.47 4 -2 0 305.59 14.46 4 2 0 340.66 14.48 4 2 0 329.67 14.61 -4 2 0 335.47 14.66 -4 2 0 337.64 14.07 4 2 0 344.81 14.53 5 -2 0 315.73 16.16 -5 -2 0 321.34 16.29 5 -2 0 340.82 15.68 -5 2 0 387.81 15.98 -5 2 0 387.68 17.71 5 2 0 373.33 16.36 5 2 0 387.75 16.55 5 2 0 363.55 16.35 6 -2 0 127.20 7.56 -6 -2 0 135.21 8.46 -6 2 0 149.95 8.73 6 2 0 147.40 8.40 -6 2 0 151.38 8.10 -7 -2 0 15.91 3.54 -7 2 0 14.05 3.50 -7 2 0 18.93 3.41 7 2 0 17.41 3.57 -8 -2 0 24.79 4.53 8 2 0 18.37 3.85 -8 2 0 26.50 5.42 -8 2 0 23.67 3.83 9 -2 0 17.25 4.38 -9 -2 0 20.52 4.51 -9 2 0 16.84 3.57 9 2 0 19.11 4.39 0 -3 0 0.62 0.49 0 -3 0 0.69 0.69 0 3 0 1.30 0.55 1 -3 0 273.57 11.32 -1 -3 0 277.00 11.20 -1 -3 0 276.60 11.34 -1 3 0 255.95 11.27 1 3 0 272.38 11.68 1 3 0 258.68 11.15 2 -3 0 512.50 20.34 -2 -3 0 490.62 20.37 -2 -3 0 511.52 20.14 2 -3 0 493.12 19.44 2 3 0 475.03 20.06 2 3 0 476.40 20.31 -2 3 0 479.30 19.45 -2 3 0 494.35 20.33 -3 -3 0 903.57 35.27 -3 -3 0 927.45 35.68 3 -3 0 895.76 35.46 3 -3 0 901.13 34.59 3 3 0 854.83 35.17 3 3 0 873.65 35.30 -3 3 0 827.06 34.55 3 3 0 836.39 35.42 -3 3 0 821.16 35.38 -4 -3 0 263.33 12.03 4 -3 0 259.24 11.93 4 -3 0 259.70 10.98 -4 3 0 243.53 10.96 4 3 0 243.60 11.52 -4 3 0 237.39 11.76 4 3 0 239.82 11.56 5 -3 0 70.35 4.37 -5 -3 0 67.87 5.05 5 3 0 70.70 5.00 5 3 0 79.65 5.07 -5 3 0 71.64 4.52 -5 3 0 72.07 5.30 6 -3 0 9.18 2.11 -6 -3 0 7.69 2.76 -6 3 0 7.37 2.05 6 3 0 8.54 2.48 -6 3 0 7.88 2.58 -7 -3 0 119.32 8.36 -7 3 0 126.35 8.69 7 3 0 129.74 8.28 -7 3 0 135.84 7.79 -8 -3 0 9.58 3.60 8 3 0 10.71 3.41 -8 3 0 10.00 4.13 -8 3 0 13.89 3.19 9 -3 0 42.79 6.24 -9 -3 0 44.00 6.24 -9 3 0 44.52 6.38 -9 3 0 39.58 4.82 9 3 0 37.59 5.57 0 -4 0 6616.86 294.68 0 4 0 6489.52 294.29 -1 -4 0 77.71 3.84 1 -4 0 81.12 2.97 -1 -4 0 80.94 3.82 1 4 0 60.71 3.60 1 4 0 62.26 3.67 -1 4 0 59.40 3.73 2 -4 0 21.63 1.21 -2 -4 0 24.88 2.07 2 -4 0 24.02 2.27 -2 -4 0 21.15 2.27 -2 4 0 25.77 1.24 2 4 0 28.74 2.20 2 4 0 22.48 2.27 -2 4 0 25.89 2.40 -3 -4 0 20.28 2.09 3 -4 0 15.42 1.41 -3 -4 0 17.71 2.42 3 -4 0 22.06 2.45 -3 4 0 17.06 1.47 -3 4 0 16.03 2.41 3 4 0 18.25 2.14 3 4 0 19.78 2.56 4 -4 0 953.46 38.19 -4 -4 0 933.69 39.53 4 -4 0 962.30 39.40 -4 4 0 953.96 38.24 4 4 0 967.42 39.51 4 4 0 963.48 39.21 -4 4 0 964.95 39.46 4 4 0 966.47 39.11 -5 -4 0 267.93 12.81 5 -4 0 261.93 11.34 -5 4 0 242.92 11.31 -5 4 0 249.45 12.61 5 4 0 248.08 12.26 5 4 0 246.19 12.12 -6 -4 0 85.18 6.36 6 -4 0 81.70 4.91 6 4 0 77.02 5.67 -6 4 0 75.61 6.04 -6 4 0 66.54 4.77 -7 -4 0 9.47 3.14 7 -4 0 11.22 2.28 -7 4 0 5.06 2.92 7 4 0 5.17 2.56 -7 4 0 7.07 2.44 -8 -4 0 12.00 3.51 8 4 0 12.81 3.52 -8 4 0 11.33 3.68 -8 4 0 22.23 3.47 -9 -4 0 7.33 3.11 -9 4 0 7.12 3.63 -9 4 0 4.82 2.43 9 4 0 6.37 3.58 0 5 0 8.40 1.42 1 -5 0 408.09 16.32 1 -5 0 410.07 15.27 -1 -5 0 435.90 16.23 -1 -5 0 416.63 16.24 1 5 0 346.49 16.02 1 5 0 358.89 16.06 -1 5 0 349.64 15.24 -1 5 0 364.06 16.25 2 -5 0 664.74 26.64 -2 -5 0 637.23 26.65 -2 -5 0 651.87 26.37 -2 5 0 637.77 26.66 2 5 0 635.53 26.34 2 5 0 646.15 26.64 3 -5 0 1854.03 73.56 -3 -5 0 1872.53 73.27 3 5 0 1873.69 73.71 -3 5 0 1790.71 73.59 -4 -5 0 381.32 16.58 -4 -5 0 373.04 16.99 4 -5 0 362.34 16.69 4 5 0 361.70 16.47 -4 5 0 379.32 16.91 4 5 0 362.86 16.34 4 5 0 360.33 16.79 -4 5 0 381.52 15.30 -5 -5 0 135.18 8.26 5 -5 0 136.79 6.67 -5 5 0 140.19 6.72 -5 5 0 136.89 8.20 5 5 0 139.78 7.81 -6 -5 0 131.69 8.36 6 -5 0 125.20 6.38 6 5 0 113.38 7.40 -6 5 0 118.44 8.03 -6 5 0 116.31 6.44 -7 -5 0 41.01 5.12 7 -5 0 40.93 3.66 7 5 0 50.43 5.24 -7 5 0 52.21 4.10 -7 5 0 47.14 5.39 -8 -5 0 94.27 7.67 -8 5 0 76.53 5.66 -8 5 0 71.28 7.23 8 5 0 83.84 6.89 -9 -5 0 17.32 4.46 9 5 0 29.35 4.94 -9 5 0 32.94 3.88 -9 5 0 27.89 5.45 0 -6 0 8200.46 379.11 0 6 0 8182.20 379.59 -1 -6 0 1760.49 123.46 1 -6 0 1909.30 120.69 1 6 0 1981.32 130.06 2 -6 0 870.35 34.40 -2 -6 0 861.58 34.10 -2 -6 0 821.64 34.31 2 6 0 842.10 34.33 2 6 0 816.55 34.04 -2 6 0 826.14 34.38 -3 -6 0 768.79 30.75 3 -6 0 731.55 30.97 -3 -6 0 767.04 31.22 -3 6 0 743.04 31.13 3 6 0 749.66 31.12 3 6 0 708.29 30.55 4 -6 0 200.72 8.96 -4 -6 0 209.73 10.99 -4 -6 0 203.34 10.38 -4 6 0 228.23 9.05 4 6 0 225.27 10.61 -4 6 0 233.28 11.20 -5 -6 0 641.07 27.51 5 -6 0 637.97 25.17 -5 6 0 597.75 27.18 5 6 0 616.98 26.67 -5 6 0 613.39 25.16 6 -6 0 123.40 6.35 -6 -6 0 129.92 8.58 6 6 0 129.03 7.82 -6 6 0 121.73 6.40 -6 6 0 122.29 8.37 7 -6 0 65.53 4.41 -7 -6 0 70.65 6.14 7 6 0 58.09 5.52 -7 6 0 60.89 4.38 -7 6 0 61.37 6.09 -8 -6 0 2.16 2.74 8 -6 0 1.85 2.04 8 6 0 8.63 3.94 -8 6 0 0.21 2.46 -9 -6 0 24.49 5.24 -9 6 0 20.12 4.92 -9 6 0 31.66 3.68 9 6 0 32.83 5.13 0 -7 0 5.50 1.61 0 7 0 5.72 1.25 0 7 0 7.79 1.80 1 -7 0 1004.54 41.61 -1 -7 0 994.20 41.35 1 -7 0 1003.70 40.42 -1 -7 0 1020.19 41.48 1 7 0 1036.36 41.40 -1 7 0 1032.53 40.44 -1 7 0 1072.59 41.80 1 7 0 1073.75 41.61 -2 -7 0 365.12 16.37 2 -7 0 361.28 17.23 -2 -7 0 350.86 16.53 2 7 0 397.64 16.72 -2 7 0 411.56 16.96 2 7 0 389.25 16.46 -3 -7 0 981.43 41.37 3 -7 0 964.38 41.18 -3 -7 0 1010.31 40.95 -3 7 0 1026.21 41.49 3 7 0 1028.20 40.95 3 7 0 1019.36 41.41 -4 -7 0 58.54 5.14 -4 -7 0 57.58 4.50 -4 7 0 81.76 5.64 4 7 0 81.41 5.04 -5 -7 0 308.28 15.31 5 -7 0 306.87 12.53 -5 7 0 288.66 14.89 5 7 0 312.16 14.54 6 -7 0 180.56 8.31 -6 -7 0 170.78 10.84 -6 7 0 185.94 10.94 -6 7 0 181.19 8.29 6 7 0 198.50 10.34 7 -7 0 1.63 1.47 -7 -7 0 7.26 3.95 -7 7 0 3.85 1.39 7 7 0 3.49 2.47 -7 7 0 0.89 2.88 -8 -7 0 166.82 11.75 -8 7 0 186.39 9.17 8 7 0 198.46 11.77 -8 7 0 190.10 12.01 0 -8 0 2573.87 165.76 0 8 0 2449.44 164.78 1 -8 0 571.16 23.11 -1 -8 0 576.69 24.05 -1 -8 0 580.89 24.24 1 -8 0 556.24 24.98 -1 8 0 571.09 23.06 -1 8 0 593.18 24.54 1 8 0 599.53 24.34 1 8 0 572.33 24.01 2 -8 0 33.02 3.11 -2 -8 0 29.61 3.16 -2 -8 0 23.78 2.63 2 8 0 25.61 3.17 -2 8 0 24.07 3.24 2 8 0 26.98 2.99 -3 -8 0 82.38 5.34 -3 8 0 88.41 5.99 3 8 0 98.98 5.96 3 8 0 89.95 5.54 -4 -8 0 46.86 4.09 -4 -8 0 43.55 4.53 4 8 0 66.72 5.56 -5 -8 0 345.15 17.83 5 8 0 382.32 17.20 -5 8 0 380.62 18.00 6 -8 0 52.76 2.89 -6 -8 0 59.99 6.04 -6 8 0 62.67 5.93 6 8 0 74.21 5.80 -7 -8 0 39.31 5.59 7 -8 0 34.63 2.66 -7 8 0 36.91 2.55 -7 8 0 43.04 5.97 7 8 0 36.85 4.85 -8 -8 0 4.20 3.37 -8 8 0 10.86 1.75 -8 8 0 7.98 3.53 8 8 0 7.57 3.14 0 -9 0 3.24 1.57 0 -9 0 5.80 1.36 0 9 0 1.83 1.20 0 9 0 5.91 1.89 -1 -9 0 160.05 8.14 1 -9 0 156.23 7.15 1 -9 0 158.94 8.46 -1 -9 0 162.35 8.40 -1 9 0 164.33 7.17 1 9 0 174.31 8.53 1 9 0 161.54 8.11 -1 9 0 173.60 8.75 -2 -9 0 206.71 9.75 -2 -9 0 189.15 9.34 -2 9 0 172.47 9.62 2 9 0 183.25 9.44 2 9 0 181.13 9.42 -3 -9 0 12.79 2.33 -3 -9 0 12.42 2.69 -3 9 0 6.74 2.37 3 9 0 4.29 1.95 -4 -9 0 5.87 2.63 4 9 0 6.90 2.57 -4 9 0 8.91 2.86 -5 -9 0 114.66 8.19 -5 9 0 122.37 8.27 5 9 0 118.15 7.47 -6 -9 0 29.24 4.97 6 9 0 34.33 4.23 -6 9 0 33.58 5.20 -7 -9 0 75.03 7.36 7 9 0 87.36 7.10 -7 9 0 82.85 7.54 -8 -9 0 17.21 4.30 -8 9 0 17.00 4.45 8 9 0 12.66 3.84 0 -10 0 36.06 3.33 0 10 0 25.61 2.55 0 10 0 25.56 3.86 -1 -10 0 391.93 16.62 1 -10 0 379.76 15.46 -1 -10 0 371.74 16.87 1 10 0 375.81 16.99 -1 10 0 371.30 17.17 1 10 0 361.66 16.49 -2 -10 0 7.48 2.01 -2 -10 0 9.17 2.26 2 10 0 5.39 2.15 -2 10 0 3.62 2.13 -3 -10 0 37.85 4.37 3 10 0 43.84 4.17 -3 10 0 40.73 4.45 -4 -10 0 263.73 13.74 4 10 0 263.42 13.08 -4 10 0 264.17 13.78 -5 -10 0 121.42 8.70 -5 10 0 131.48 8.85 5 10 0 127.18 7.93 -6 -10 0 55.22 6.03 -6 10 0 58.48 6.10 6 10 0 52.45 5.24 -7 -10 0 4.82 3.21 7 10 0 6.19 3.39 -7 10 0 4.81 3.34 1 -11 0 100.09 4.76 -1 -11 0 107.64 6.07 1 11 0 97.05 6.49 -1 11 0 86.57 6.30 -1 11 0 90.04 4.69 -2 -11 0 448.30 20.01 2 11 0 452.01 20.16 -2 11 0 440.87 20.46 -3 -11 0 187.62 10.13 3 11 0 166.92 9.62 -3 11 0 172.71 10.23 -4 -11 0 108.72 7.85 4 11 0 120.67 7.69 -4 11 0 113.62 8.02 -5 -11 0 50.95 5.78 5 11 0 54.25 5.37 -5 11 0 58.34 5.93 -6 -11 0 24.31 4.78 6 11 0 19.58 3.80 -6 11 0 24.68 4.78 -7 -11 0 71.68 7.28 7 11 0 64.41 6.48 -7 11 0 62.23 6.99 0 -12 0 220.13 9.62 0 12 0 196.71 10.69 0 12 0 186.09 9.40 1 -12 0 118.53 5.70 -1 -12 0 116.72 6.93 1 12 0 118.79 6.84 -1 12 0 121.56 5.73 1 12 0 131.60 7.88 -1 12 0 117.21 7.65 -2 -12 0 88.86 6.30 -2 12 0 93.93 6.77 2 12 0 91.61 6.40 -3 -12 0 35.46 4.76 3 12 0 36.68 4.47 -3 12 0 29.18 4.47 -4 -12 0 179.10 10.82 -4 12 0 181.98 10.89 4 12 0 171.39 10.18 -5 -12 0 165.05 11.74 5 12 0 143.73 9.20 -5 12 0 155.68 10.30 -6 -12 0 42.52 6.13 6 12 0 37.55 5.06 -6 12 0 34.79 5.43 0 13 0 8.28 1.90 0 13 0 16.17 3.20 1 -13 0 99.09 4.81 -1 -13 0 96.05 6.02 -1 13 0 92.14 7.10 1 13 0 108.34 7.01 1 13 0 87.15 6.04 -1 13 0 93.28 4.82 -2 -13 0 190.32 10.76 2 13 0 210.47 11.31 -2 13 0 214.62 11.65 -3 -13 0 333.23 15.89 -3 13 0 319.17 16.31 3 13 0 295.59 15.42 -4 -13 0 66.55 6.45 4 13 0 75.04 6.34 -4 13 0 64.55 6.65 -5 -13 0 32.50 5.21 -5 13 0 36.07 5.60 5 13 0 37.18 5.16 -6 -13 0 25.81 4.88 -6 13 0 26.15 5.06 6 13 0 22.95 4.40 0 -14 0 252.00 11.85 0 14 0 246.34 11.80 0 14 0 279.69 13.76 -1 -14 0 10.74 2.46 1 -14 0 7.10 1.26 1 14 0 13.34 3.28 -1 14 0 11.11 3.23 -1 14 0 13.57 2.26 -2 -14 0 60.04 5.13 2 14 0 59.40 5.59 -2 14 0 64.51 5.96 -3 -14 0 31.62 4.70 3 14 0 36.24 4.92 -3 14 0 39.22 5.66 -4 14 0 2.64 2.78 4 14 0 3.75 2.56 -5 -14 0 51.32 6.67 5 14 0 41.31 6.54 -5 14 0 47.89 6.58 0 15 0 1.00 1.76 0 15 0 15.98 3.54 -1 -15 0 10.19 2.62 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4.41 -1 8 12 19.87 4.48 -1 8 12 16.80 4.21 -3 -9 12 12.74 4.33 -3 9 12 19.41 4.18 -3 9 12 21.19 4.71 -2 9 12 23.72 4.76 -7 0 13 0.84 3.73 -6 0 13 75.62 7.91 -6 0 13 77.68 4.70 -5 0 13 44.76 6.25 -5 0 13 49.69 3.68 -4 0 13 92.67 5.57 4 0 -13 86.66 5.70 -4 0 13 87.06 7.91 -3 0 13 0.61 2.59 -3 0 13 -0.39 1.75 -2 0 13 0.09 2.74 -2 0 13 3.59 2.25 -1 0 13 78.99 7.82 -1 0 13 75.26 6.19 0 0 13 7.95 3.83 0 0 13 11.17 3.26 -7 -1 13 23.34 5.59 -7 1 13 24.76 5.45 -7 1 13 33.12 3.23 -6 -1 13 5.78 1.11 -6 -1 13 7.85 3.70 -6 1 13 7.68 3.53 -6 1 13 6.73 2.04 -5 -1 13 4.20 3.14 -5 -1 13 3.19 1.16 -5 1 13 -0.95 2.59 -5 1 13 2.49 1.74 -4 -1 13 8.06 1.74 -4 -1 13 6.97 3.69 -4 -1 13 9.34 1.68 -4 1 13 9.18 3.73 -4 1 13 10.21 2.44 -3 -1 13 39.77 3.30 -3 -1 13 33.57 5.73 -3 -1 13 33.35 3.43 -3 1 13 53.68 6.88 -3 1 13 43.83 4.34 -2 -1 13 11.94 4.11 -2 -1 13 12.75 2.63 -2 1 13 16.25 4.41 -2 1 13 14.61 3.13 -1 -1 13 20.16 3.39 -1 -1 13 25.96 5.52 -1 1 13 23.26 3.88 -1 1 13 24.08 4.95 0 -1 13 3.56 3.53 0 -1 13 4.89 2.70 0 1 13 3.80 2.74 0 1 13 13.89 4.63 -6 -2 13 9.89 4.16 -6 2 13 13.72 2.57 -6 2 13 15.69 4.25 -5 -2 13 -5.10 2.53 -5 2 13 0.22 2.83 -5 2 13 2.14 1.89 -4 -2 13 8.28 1.30 -4 -2 13 6.75 1.19 -4 -2 13 4.78 3.45 -4 2 13 5.14 2.30 -4 2 13 4.49 3.14 -3 -2 13 0.83 2.81 -3 -2 13 2.81 1.43 -3 -2 13 6.00 1.34 -3 2 13 0.18 2.76 -3 2 13 3.13 2.39 -2 -2 13 3.22 3.34 -2 -2 13 4.44 1.95 -2 2 13 4.70 2.64 -2 2 13 8.23 3.61 -1 -2 13 6.72 2.45 -1 -2 13 9.40 3.71 -1 2 13 9.55 3.82 -1 2 13 11.98 3.39 0 -2 13 5.88 2.70 0 -2 13 6.54 3.92 0 2 13 5.02 3.44 -6 -3 13 0.67 3.39 -6 3 13 6.26 2.21 -6 3 13 -4.49 2.92 -5 -3 13 -1.88 2.67 -5 3 13 2.66 2.13 -5 3 13 4.56 3.18 -4 -3 13 -2.46 2.78 -4 3 13 1.93 2.18 -4 3 13 0.74 2.84 -3 -3 13 -0.64 0.81 -3 -3 13 0.68 0.90 -3 -3 13 -4.63 2.32 -3 3 13 -0.21 2.68 -3 3 13 0.48 2.21 -2 -3 13 6.37 3.37 -2 -3 13 2.06 1.59 -2 3 13 3.46 2.60 -2 3 13 7.54 3.44 -1 -3 13 3.57 3.28 -1 -3 13 2.90 2.02 -1 3 13 5.84 3.11 -1 3 13 11.51 3.94 0 -3 13 -1.48 3.03 0 -3 13 0.97 2.13 0 3 13 8.13 4.05 0 3 13 3.33 2.74 -6 -4 13 5.16 3.54 -6 4 13 1.60 3.18 -6 4 13 5.31 2.31 -5 -4 13 6.58 4.07 -5 4 13 13.06 3.79 -5 4 13 8.24 2.76 -4 -4 13 8.37 3.71 -4 4 13 7.68 2.88 -4 4 13 11.50 4.01 -3 -4 13 -0.96 3.14 -3 4 13 1.28 2.71 -3 4 13 -0.65 2.54 -2 -4 13 17.68 4.69 -2 -4 13 10.61 1.78 -2 4 13 14.66 4.38 -2 4 13 17.73 3.65 -1 -4 13 2.44 3.31 -1 4 13 0.89 2.84 -1 4 13 -1.72 2.14 0 -4 13 13.42 4.43 0 -4 13 11.73 2.89 0 4 13 11.32 4.14 0 4 13 8.32 3.53 -5 -5 13 3.07 3.66 -5 5 13 5.07 2.75 -5 5 13 1.81 3.01 -4 -5 13 6.14 3.83 -4 5 13 8.53 3.77 -4 5 13 6.66 3.10 -3 -5 13 29.26 5.31 -3 5 13 30.20 4.56 -3 5 13 31.03 5.38 -2 -5 13 11.66 1.49 -2 -5 13 16.37 4.40 -2 5 13 11.99 4.08 -2 5 13 10.70 3.48 -1 -5 13 6.48 2.00 -1 -5 13 10.00 4.23 -1 5 13 12.06 4.27 -1 5 13 14.67 4.06 -5 -6 13 20.62 5.23 -5 6 13 24.78 4.33 -5 6 13 21.85 4.59 -4 -6 13 64.79 7.43 -4 6 13 56.73 6.41 -4 6 13 61.97 6.00 -3 -6 13 -0.58 3.20 -3 6 13 2.11 2.56 -3 6 13 0.56 2.73 -2 -6 13 -3.61 2.78 -2 6 13 3.14 3.16 -2 6 13 4.62 3.22 -5 0 14 19.87 4.90 -5 0 14 31.38 2.85 -4 0 14 26.27 4.50 -4 0 14 30.08 5.45 -3 0 14 104.61 6.69 -3 0 14 110.41 9.46 -2 0 14 13.39 3.15 -2 0 14 20.76 4.88 -5 -1 14 5.82 4.05 -5 -1 14 9.48 1.96 -5 1 14 5.37 1.84 -5 1 14 2.21 3.23 -4 -1 14 7.99 3.92 -4 -1 14 9.05 1.71 -4 1 14 14.82 2.79 -4 1 14 10.69 4.04 -3 -1 14 1.10 3.43 -3 1 14 4.33 2.41 -3 1 14 7.39 3.67 -2 -1 14 1.74 2.07 -2 -1 14 6.50 4.14 -2 1 14 6.92 3.66 -2 1 14 2.02 2.29 -4 -2 14 -2.28 2.86 -4 2 14 -0.02 3.06 -4 2 14 3.65 2.35 -3 -2 14 8.16 1.74 -3 -2 14 7.67 4.05 -3 2 14 7.59 4.03 -3 2 14 7.04 2.84 -2 -2 14 9.88 2.41 -2 -2 14 11.07 4.41 -2 2 14 7.48 3.85 -2 2 14 11.81 3.44 -4 -3 14 -2.83 2.88 -4 3 14 3.77 3.62 -4 3 14 2.22 2.22 -3 -3 14 -3.64 2.85 -3 3 14 -0.49 2.28 -3 3 14 2.43 3.23 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6791 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71077 7.894 12.907 11.014 89.998 109.471 90.002 ) _computing_structure_solution 'SHELXT2014 (Sheldrick, 2015a)' ; _shelx_hkl_checksum 49224 _shelx_res_file ; TITL shelxt_a.res in P2(1) shelx.res created by SHELXL-2018/3 at 09:46:08 on 04-Feb-2024 CELL 0.71073 7.8964 12.9064 11.0124 90.000 109.467 90.000 ZERR 2.00 0.0002 0.0003 0.0003 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H FE O S UNIT 48 44 2 4 4 MERG 2 OMIT -1 0 1 OMIT 0 -1 1 OMIT 1 0 0 OMIT 0 1 1 OMIT 1 2 0 SIZE 0.07 0.05 0.04 TEMP 24 FMAP 2 PLAN 5 ACTA CONF BOND $H SIMU 0.001 C6 C10 C9 C10 LIST 4 L.S. 64 WGHT 0.032000 0.201700 FVAR 0.89003 C1 1 0.734025 0.390239 0.173126 11.00000 0.03149 0.03082 = 0.04516 -0.00170 0.01324 -0.00581 C2 1 0.586505 0.399946 0.223115 11.00000 0.04416 0.02945 = 0.04993 0.00170 0.02158 -0.00079 C3 1 0.424085 0.375882 0.120841 11.00000 0.03465 0.04113 = 0.06844 0.00286 0.01785 0.00119 AFIX 43 H3 2 0.309241 0.375323 0.126613 11.00000 -1.20000 AFIX 0 C4 1 0.468154 0.353229 0.010125 11.00000 0.04123 0.04605 = 0.04917 -0.00037 0.00340 -0.00275 AFIX 43 H4 2 0.387042 0.335938 -0.070202 11.00000 -1.20000 AFIX 0 C5 1 0.656655 0.361148 0.041392 11.00000 0.04521 0.04271 = 0.04552 -0.00534 0.01859 -0.00540 AFIX 43 H5 2 0.719835 0.349264 -0.015019 11.00000 -1.20000 AFIX 0 C6 1 0.616696 0.155869 0.306666 11.00000 0.08371 0.03741 = 0.11357 0.01332 0.01852 -0.00128 AFIX 43 H6 2 0.616680 0.175080 0.388056 11.00000 -1.20000 AFIX 0 C7 1 0.468034 0.131996 0.201979 11.00000 0.08035 0.04666 = 0.11122 0.00613 0.02996 -0.02148 AFIX 43 H7 2 0.350270 0.131767 0.202000 11.00000 -1.20000 AFIX 0 C8 1 0.519827 0.108384 0.096686 11.00000 0.08484 0.03746 = 0.10738 -0.01422 0.02238 -0.01596 AFIX 43 H8 2 0.443710 0.090050 0.015076 11.00000 -1.20000 AFIX 0 C9 1 0.705351 0.116945 0.134596 11.00000 0.08090 0.03808 = 0.11853 0.00605 0.02323 0.00506 AFIX 43 H9 2 0.776227 0.105979 0.083190 11.00000 -1.20000 AFIX 0 C10 1 0.767309 0.145897 0.268018 11.00000 0.08196 0.03736 = 0.11754 0.01083 0.01670 0.00207 AFIX 43 H10 2 0.886184 0.156157 0.319415 11.00000 -1.20000 AFIX 0 C11 1 0.986188 0.538690 0.229716 11.00000 0.03536 0.04161 = 0.05188 -0.00276 0.00904 -0.00892 C12 1 1.026819 0.601168 0.337204 11.00000 0.07890 0.05214 = 0.04553 -0.00491 0.01225 -0.01920 AFIX 43 H12 2 1.044430 0.572275 0.417855 11.00000 -1.20000 AFIX 0 C13 1 1.041185 0.706910 0.324306 11.00000 0.09312 0.04887 = 0.05896 -0.01457 0.01939 -0.02085 AFIX 43 H13 2 1.066819 0.748998 0.396752 11.00000 -1.20000 AFIX 0 C14 1 1.018179 0.751306 0.205779 11.00000 0.05179 0.04547 = 0.06192 0.00005 0.01428 -0.01086 C15 1 0.980451 0.687317 0.099784 11.00000 0.06498 0.05184 = 0.05122 0.00210 0.01711 -0.01034 AFIX 43 H15 2 0.965955 0.715920 0.019430 11.00000 -1.20000 AFIX 0 C16 1 0.963728 0.581001 0.110872 11.00000 0.05456 0.04988 = 0.04630 -0.00792 0.00970 -0.00966 AFIX 43 H16 2 0.937554 0.538774 0.038515 11.00000 -1.20000 AFIX 0 C17 1 1.032314 0.866689 0.193244 11.00000 0.08233 0.04963 = 0.08016 -0.00459 0.02559 -0.01432 AFIX 137 H17A 2 0.987817 0.885622 0.103857 11.00000 -1.50000 H17B 2 1.155708 0.887402 0.229871 11.00000 -1.50000 H17C 2 0.962445 0.900734 0.237998 11.00000 -1.50000 AFIX 0 C21 1 0.599338 0.562208 0.381603 11.00000 0.06033 0.03750 = 0.04379 0.00028 0.02423 0.00215 C22 1 0.708095 0.611039 0.489702 11.00000 0.10223 0.04703 = 0.04826 0.00296 0.00509 0.01264 AFIX 43 H22 2 0.777193 0.572577 0.560229 11.00000 -1.20000 AFIX 0 C23 1 0.714388 0.717707 0.493197 11.00000 0.10075 0.05459 = 0.06176 -0.01132 0.00365 -0.00098 AFIX 43 H23 2 0.785744 0.750675 0.567797 11.00000 -1.20000 AFIX 0 C24 1 0.618620 0.776153 0.390024 11.00000 0.08239 0.03943 = 0.06304 0.00135 0.03987 0.00685 C25 1 0.503816 0.726147 0.285640 11.00000 0.08877 0.05430 = 0.06211 0.01440 0.01754 0.01959 AFIX 43 H25 2 0.431880 0.764802 0.216351 11.00000 -1.20000 AFIX 0 C26 1 0.492338 0.619299 0.280852 11.00000 0.06831 0.05145 = 0.05924 0.00280 0.00677 0.01044 AFIX 43 H26 2 0.412284 0.586525 0.209497 11.00000 -1.20000 AFIX 0 C27 1 0.639431 0.894081 0.390251 11.00000 0.14916 0.04256 = 0.10309 0.00536 0.07441 0.00503 AFIX 137 H27A 2 0.681413 0.918813 0.477443 11.00000 -1.50000 H27B 2 0.525421 0.925180 0.344837 11.00000 -1.50000 H27C 2 0.724509 0.912206 0.348615 11.00000 -1.50000 AFIX 0 FE1 3 0.598638 0.255104 0.158720 11.00000 0.04166 0.02846 = 0.05870 -0.00265 0.01363 -0.00473 O1 4 1.048155 0.347634 0.164830 11.00000 0.04406 0.06072 = 0.12089 -0.02050 0.03691 -0.00156 O2 4 0.768205 0.390570 0.471479 11.00000 0.16653 0.05437 = 0.04954 0.00937 0.00856 0.03591 S1 5 0.966716 0.401949 0.252310 11.00000 0.03592 0.03947 = 0.06248 -0.00143 0.00729 -0.00404 S2 5 0.591711 0.423106 0.381458 11.00000 0.10461 0.03802 = 0.05654 0.00528 0.04552 0.00126 HKLF 4 REM shelxt_a.res in P2(1) REM wR2 = 0.0844, GooF = S = 1.142, Restrained GooF = 1.154 for all data REM R1 = 0.0337 for 4393 Fo > 4sig(Fo) and 0.0383 for all 4815 data REM 264 parameters refined using 13 restraints END WGHT 0.0377 0.2824 REM Highest difference peak 0.408, deepest hole -0.342, 1-sigma level 0.045 Q1 1 0.8048 0.1398 0.2088 11.00000 0.05 0.41 Q2 1 0.7014 0.4318 0.4271 11.00000 0.05 0.30 Q3 1 0.7336 0.1611 0.3050 11.00000 0.05 0.29 Q4 1 0.7066 0.2526 0.1435 11.00000 0.05 0.28 Q5 1 0.6702 0.1233 0.0784 11.00000 0.05 0.20 ; _shelx_res_checksum 74148 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.7340(4) 0.3902(3) 0.1731(3) 0.0357(7) Uani d 1 . . C C2 0.5865(5) 0.3999(3) 0.2231(4) 0.0397(7) Uani d 1 . . C C3 0.4241(5) 0.3759(3) 0.1208(4) 0.0479(9) Uani d 1 . . H H3 0.309241 0.375323 0.126613 0.057 Uiso calc 1 . . C C4 0.4682(5) 0.3532(3) 0.0101(4) 0.0484(9) Uani d 1 . . H H4 0.387042 0.335938 -0.070202 0.058 Uiso calc 1 . . C C5 0.6567(5) 0.3611(3) 0.0414(4) 0.0436(8) Uani d 1 . . H H5 0.719835 0.349264 -0.015019 0.052 Uiso calc 1 . . C C6 0.6167(8) 0.1559(4) 0.3067(7) 0.0818(11) Uani d 1 . . H H6 0.616680 0.175080 0.388056 0.098 Uiso calc 1 . . C C7 0.4680(8) 0.1320(4) 0.2020(7) 0.0799(16) Uani d 1 . . H H7 0.350270 0.131767 0.202000 0.096 Uiso calc 1 . . C C8 0.5198(8) 0.1084(4) 0.0967(7) 0.0790(16) Uani d 1 . . H H8 0.443710 0.090050 0.015076 0.095 Uiso calc 1 . . C C9 0.7054(8) 0.1169(4) 0.1346(7) 0.0817(12) Uani d 1 . . H H9 0.776227 0.105979 0.083190 0.098 Uiso calc 1 . . C C10 0.7673(8) 0.1459(4) 0.2680(7) 0.0831(11) Uani d 1 . . H H10 0.886184 0.156157 0.319415 0.100 Uiso calc 1 . . C C11 0.9862(5) 0.5387(3) 0.2297(4) 0.0443(8) Uani d 1 . . C C12 1.0268(7) 0.6012(4) 0.3372(4) 0.0610(11) Uani d 1 . . H H12 1.044430 0.572275 0.417855 0.073 Uiso calc 1 . . C C13 1.0412(8) 0.7069(4) 0.3243(5) 0.0685(13) Uani d 1 . . H H13 1.066819 0.748998 0.396752 0.082 Uiso calc 1 . . C C14 1.0182(5) 0.7513(4) 0.2058(4) 0.0542(9) Uani d 1 . . C C15 0.9805(7) 0.6873(3) 0.0998(4) 0.0566(11) Uani d 1 . . H H15 0.965955 0.715920 0.019430 0.068 Uiso calc 1 . . C C16 0.9637(6) 0.5810(3) 0.1109(4) 0.0520(10) Uani d 1 . . H H16 0.937554 0.538774 0.038515 0.062 Uiso calc 1 . . C C17 1.0323(8) 0.8667(4) 0.1932(5) 0.0711(13) Uani d 1 . . H H17A 0.987817 0.885622 0.103857 0.107 Uiso calc 1 . . H H17B 1.155708 0.887402 0.229871 0.107 Uiso calc 1 . . H H17C 0.962445 0.900734 0.237998 0.107 Uiso calc 1 . . C C21 0.5993(6) 0.5622(3) 0.3816(4) 0.0455(9) Uani d 1 . . C C22 0.7081(8) 0.6110(4) 0.4897(5) 0.0708(14) Uani d 1 . . H H22 0.777193 0.572577 0.560229 0.085 Uiso calc 1 . . C C23 0.7144(9) 0.7177(4) 0.4932(5) 0.0782(15) Uani d 1 . . H H23 0.785744 0.750675 0.567797 0.094 Uiso calc 1 . . C C24 0.6186(7) 0.7762(3) 0.3900(4) 0.0577(11) Uani d 1 . . C C25 0.5038(7) 0.7261(4) 0.2856(5) 0.0703(13) Uani d 1 . . H H25 0.431880 0.764802 0.216351 0.084 Uiso calc 1 . . C C26 0.4923(7) 0.6193(4) 0.2809(5) 0.0633(12) Uani d 1 . . H H26 0.412284 0.586525 0.209497 0.076 Uiso calc 1 . . C C27 0.6394(10) 0.8941(4) 0.3903(6) 0.0902(19) Uani d 1 . . H H27A 0.681413 0.918813 0.477443 0.135 Uiso calc 1 . . H H27B 0.525421 0.925180 0.344837 0.135 Uiso calc 1 . . H H27C 0.724509 0.912206 0.348615 0.135 Uiso calc 1 . . Fe Fe1 0.59864(6) 0.25510(3) 0.15872(5) 0.04371(15) Uani d 1 . . O O1 1.0482(4) 0.3476(3) 0.1648(4) 0.0729(10) Uani d 1 . . O O2 0.7682(7) 0.3906(3) 0.4715(3) 0.0970(14) Uani d 1 . . S S1 0.96672(12) 0.40195(7) 0.25231(10) 0.0482(2) Uani d 1 . . S S2 0.59171(19) 0.42311(8) 0.38146(11) 0.0617(3) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0315(16) 0.0308(16) 0.0452(18) -0.0058(13) 0.0132(14) -0.0017(14) C2 0.0442(18) 0.0295(16) 0.0499(19) -0.0008(15) 0.0216(16) 0.0017(15) C3 0.0346(18) 0.041(2) 0.068(3) 0.0012(15) 0.0178(18) 0.0029(18) C4 0.041(2) 0.046(2) 0.049(2) -0.0028(16) 0.0034(17) -0.0004(17) C5 0.0452(19) 0.0427(19) 0.0455(19) -0.0054(15) 0.0186(16) -0.0053(16) C6 0.084(2) 0.0374(16) 0.114(3) -0.0013(17) 0.019(2) 0.0133(18) C7 0.080(4) 0.047(3) 0.111(5) -0.021(3) 0.030(3) 0.006(3) C8 0.085(4) 0.037(2) 0.107(5) -0.016(3) 0.022(3) -0.014(3) C9 0.081(2) 0.0381(16) 0.119(3) 0.0051(17) 0.023(2) 0.0060(18) C10 0.082(2) 0.0374(15) 0.118(3) 0.0021(16) 0.017(2) 0.0108(17) C11 0.0354(18) 0.0416(19) 0.052(2) -0.0089(15) 0.0090(16) -0.0028(16) C12 0.079(3) 0.052(2) 0.046(2) -0.019(2) 0.012(2) -0.0049(19) C13 0.093(4) 0.049(2) 0.059(3) -0.021(2) 0.019(3) -0.015(2) C14 0.052(2) 0.045(2) 0.062(2) -0.011(2) 0.0143(17) 0.000(2) C15 0.065(3) 0.052(2) 0.051(2) -0.010(2) 0.017(2) 0.0021(18) C16 0.055(2) 0.050(2) 0.046(2) -0.0097(18) 0.0097(18) -0.0079(16) C17 0.082(3) 0.050(3) 0.080(3) -0.014(2) 0.026(3) -0.005(2) C21 0.060(2) 0.0375(18) 0.044(2) 0.0022(17) 0.0242(18) 0.0003(15) C22 0.102(4) 0.047(2) 0.048(2) 0.013(3) 0.005(2) 0.003(2) C23 0.101(4) 0.055(3) 0.062(3) -0.001(3) 0.004(3) -0.011(2) C24 0.082(3) 0.039(2) 0.063(3) 0.0069(19) 0.040(2) 0.0013(18) C25 0.089(4) 0.054(3) 0.062(3) 0.020(2) 0.018(3) 0.014(2) C26 0.068(3) 0.051(2) 0.059(3) 0.010(2) 0.007(2) 0.003(2) C27 0.149(6) 0.043(3) 0.103(4) 0.005(3) 0.074(4) 0.005(3) Fe1 0.0417(3) 0.0285(2) 0.0587(3) -0.0047(2) 0.0136(2) -0.0026(2) O1 0.0441(16) 0.061(2) 0.121(3) -0.0016(15) 0.0369(18) -0.0205(19) O2 0.167(4) 0.0544(19) 0.0495(18) 0.036(2) 0.009(2) 0.0094(15) S1 0.0359(4) 0.0395(5) 0.0625(6) -0.0040(4) 0.0073(4) -0.0014(4) S2 0.1046(9) 0.0380(5) 0.0565(6) 0.0013(5) 0.0455(6) 0.0053(4) 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' Fe Fe 0.3463 0.8444 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C5 C1 C2 . . 106.5(3) ? C5 C1 S1 . . 123.4(3) ? C2 C1 S1 . . 130.0(3) ? C5 C1 Fe1 . . 69.9(2) ? C2 C1 Fe1 . . 68.54(19) ? S1 C1 Fe1 . . 123.39(19) ? C3 C2 C1 . . 107.8(3) ? C3 C2 S2 . . 122.5(3) ? C1 C2 S2 . . 129.5(3) ? C3 C2 Fe1 . . 69.9(2) ? C1 C2 Fe1 . . 69.36(19) ? S2 C2 Fe1 . . 121.32(19) ? C4 C3 C2 . . 108.2(3) ? C4 C3 Fe1 . . 70.8(2) ? C2 C3 Fe1 . . 68.6(2) ? C4 C3 H3 . . 125.9 ? C2 C3 H3 . . 125.9 ? Fe1 C3 H3 . . 126.2 ? C3 C4 C5 . . 108.6(3) ? C3 C4 Fe1 . . 68.9(2) ? C5 C4 Fe1 . . 69.1(2) ? C3 C4 H4 . . 125.7 ? C5 C4 H4 . . 125.7 ? Fe1 C4 H4 . . 127.8 ? C1 C5 C4 . . 109.0(3) ? C1 C5 Fe1 . . 69.0(2) ? C4 C5 Fe1 . . 70.4(2) ? C1 C5 H5 . . 125.5 ? C4 C5 H5 . . 125.5 ? Fe1 C5 H5 . . 126.7 ? C7 C6 C10 . . 107.4(6) ? C7 C6 Fe1 . . 70.1(3) ? C10 C6 Fe1 . . 69.8(4) ? C7 C6 H6 . . 126.3 ? C10 C6 H6 . . 126.3 ? Fe1 C6 H6 . . 125.4 ? C6 C7 C8 . . 110.0(6) ? C6 C7 Fe1 . . 70.4(3) ? C8 C7 Fe1 . . 70.2(3) ? C6 C7 H7 . . 125.0 ? C8 C7 H7 . . 125.0 ? Fe1 C7 H7 . . 126.0 ? C7 C8 C9 . . 107.9(6) ? C7 C8 Fe1 . . 70.0(3) ? C9 C8 Fe1 . . 69.6(3) ? C7 C8 H8 . . 126.1 ? C9 C8 H8 . . 126.1 ? Fe1 C8 H8 . . 125.9 ? C8 C9 C10 . . 107.1(6) ? C8 C9 Fe1 . . 70.5(3) ? C10 C9 Fe1 . . 69.6(3) ? C8 C9 H9 . . 126.4 ? C10 C9 H9 . . 126.4 ? Fe1 C9 H9 . . 125.1 ? C6 C10 C9 . . 107.6(6) ? C6 C10 Fe1 . . 70.1(3) ? C9 C10 Fe1 . . 69.0(3) ? C6 C10 H10 . . 126.2 ? C9 C10 H10 . . 126.2 ? Fe1 C10 H10 . . 126.2 ? C16 C11 C12 . . 120.3(4) ? C16 C11 S1 . . 122.2(3) ? C12 C11 S1 . . 117.5(3) ? C11 C12 C13 . . 119.6(4) ? C11 C12 H12 . . 120.2 ? C13 C12 H12 . . 120.2 ? C14 C13 C12 . . 121.2(4) ? C14 C13 H13 . . 119.4 ? C12 C13 H13 . . 119.4 ? C13 C14 C15 . . 118.3(4) ? C13 C14 C17 . . 120.5(4) ? C15 C14 C17 . . 121.2(4) ? C14 C15 C16 . . 121.2(4) ? C14 C15 H15 . . 119.4 ? C16 C15 H15 . . 119.4 ? C11 C16 C15 . . 119.4(4) ? C11 C16 H16 . . 120.3 ? C15 C16 H16 . . 120.3 ? C14 C17 H17A . . 109.5 ? C14 C17 H17B . . 109.5 ? H17A C17 H17B . . 109.5 ? C14 C17 H17C . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? C26 C21 C22 . . 119.9(4) ? C26 C21 S2 . . 121.8(3) ? C22 C21 S2 . . 118.2(3) ? C21 C22 C23 . . 119.4(4) ? C21 C22 H22 . . 120.3 ? C23 C22 H22 . . 120.3 ? C24 C23 C22 . . 121.7(5) ? C24 C23 H23 . . 119.2 ? C22 C23 H23 . . 119.2 ? C25 C24 C23 . . 117.9(4) ? C25 C24 C27 . . 120.8(5) ? C23 C24 C27 . . 121.3(5) ? C24 C25 C26 . . 121.4(4) ? C24 C25 H25 . . 119.3 ? C26 C25 H25 . . 119.3 ? C21 C26 C25 . . 119.5(4) ? C21 C26 H26 . . 120.2 ? C25 C26 H26 . . 120.2 ? C24 C27 H27A . . 109.5 ? C24 C27 H27B . . 109.5 ? H27A C27 H27B . . 109.5 ? C24 C27 H27C . . 109.5 ? H27A C27 H27C . . 109.5 ? H27B C27 H27C . . 109.5 ? C2 Fe1 C1 . . 42.10(14) ? C2 Fe1 C9 . . 159.0(2) ? C1 Fe1 C9 . . 122.44(18) ? C2 Fe1 C3 . . 41.45(15) ? C1 Fe1 C3 . . 70.07(15) ? C9 Fe1 C3 . . 158.7(2) ? C2 Fe1 C10 . . 122.2(2) ? C1 Fe1 C10 . . 109.03(19) ? C9 Fe1 C10 . . 41.4(3) ? C3 Fe1 C10 . . 156.8(2) ? C2 Fe1 C7 . . 123.7(2) ? C1 Fe1 C7 . . 161.8(2) ? C9 Fe1 C7 . . 67.0(3) ? C3 Fe1 C7 . . 106.6(2) ? C10 Fe1 C7 . . 66.7(2) ? C2 Fe1 C5 . . 69.30(14) ? C1 Fe1 C5 . . 41.06(14) ? C9 Fe1 C5 . . 108.5(2) ? C3 Fe1 C5 . . 68.56(16) ? C10 Fe1 C5 . . 126.8(2) ? C7 Fe1 C5 . . 155.8(2) ? C2 Fe1 C6 . . 107.5(2) ? C1 Fe1 C6 . . 125.7(2) ? C9 Fe1 C6 . . 68.3(3) ? C3 Fe1 C6 . . 120.5(2) ? C10 Fe1 C6 . . 40.1(3) ? C7 Fe1 C6 . . 39.5(2) ? C5 Fe1 C6 . . 163.4(2) ? C2 Fe1 C8 . . 159.3(2) ? C1 Fe1 C8 . . 157.1(2) ? C9 Fe1 C8 . . 39.9(2) ? C3 Fe1 C8 . . 122.3(2) ? C10 Fe1 C8 . . 67.8(2) ? C7 Fe1 C8 . . 39.8(3) ? C5 Fe1 C8 . . 121.3(2) ? C6 Fe1 C8 . . 67.5(3) ? C2 Fe1 C4 . . 68.77(16) ? C1 Fe1 C4 . . 69.07(15) ? C9 Fe1 C4 . . 123.9(2) ? C3 Fe1 C4 . . 40.26(17) ? C10 Fe1 C4 . . 162.5(2) ? C7 Fe1 C4 . . 120.6(2) ? C5 Fe1 C4 . . 40.48(15) ? C6 Fe1 C4 . . 155.0(2) ? C8 Fe1 C4 . . 106.8(2) ? O1 S1 C1 . . 104.03(18) ? O1 S1 C11 . . 107.2(2) ? C1 S1 C11 . . 98.01(17) ? O2 S2 C2 . . 108.8(2) ? O2 S2 C21 . . 105.1(2) ? C2 S2 C21 . . 99.25(17) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C5 . 1.424(5) ? C1 C2 . 1.450(5) ? C1 S1 . 1.758(3) ? C1 Fe1 . 2.024(3) ? C2 C3 . 1.431(5) ? C2 S2 . 1.756(4) ? C2 Fe1 . 2.013(3) ? C3 C4 . 1.406(6) ? C3 Fe1 . 2.030(4) ? C3 H3 . 0.9300 ? C4 C5 . 1.415(5) ? C4 Fe1 . 2.054(4) ? C4 H4 . 0.9300 ? C5 Fe1 . 2.036(4) ? C5 H5 . 0.9300 ? C6 C7 . 1.378(8) ? C6 C10 . 1.396(9) ? C6 Fe1 . 2.040(6) ? C6 H6 . 0.9300 ? C7 C8 . 1.386(9) ? C7 Fe1 . 2.035(5) ? C7 H7 . 0.9300 ? C8 C9 . 1.387(9) ? C8 Fe1 . 2.039(5) ? C8 H8 . 0.9300 ? C9 C10 . 1.435(10) ? C9 Fe1 . 2.027(6) ? C9 H9 . 0.9300 ? C10 Fe1 . 2.035(5) ? C10 H10 . 0.9300 ? C11 C16 . 1.374(6) ? C11 C12 . 1.379(6) ? C11 S1 . 1.796(4) ? C12 C13 . 1.381(7) ? C12 H12 . 0.9300 ? C13 C14 . 1.381(7) ? C13 H13 . 0.9300 ? C14 C15 . 1.379(6) ? C14 C17 . 1.503(7) ? C15 C16 . 1.388(6) ? C15 H15 . 0.9300 ? C16 H16 . 0.9300 ? C17 H17A . 0.9600 ? C17 H17B . 0.9600 ? C17 H17C . 0.9600 ? C21 C26 . 1.365(6) ? C21 C22 . 1.368(6) ? C21 S2 . 1.796(4) ? C22 C23 . 1.378(7) ? C22 H22 . 0.9300 ? C23 C24 . 1.363(7) ? C23 H23 . 0.9300 ? C24 C25 . 1.366(7) ? C24 C27 . 1.531(6) ? C25 C26 . 1.382(7) ? C25 H25 . 0.9300 ? C26 H26 . 0.9300 ? C27 H27A . 0.9600 ? C27 H27B . 0.9600 ? C27 H27C . 0.9600 ? O1 S1 . 1.499(4) ? O2 S2 . 1.477(4) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C5 C1 C2 C3 . . . . 0.4(4) ? S1 C1 C2 C3 . . . . -175.8(3) ? Fe1 C1 C2 C3 . . . . -59.6(3) ? C5 C1 C2 S2 . . . . 174.1(3) ? S1 C1 C2 S2 . . . . -2.1(5) ? Fe1 C1 C2 S2 . . . . 114.2(3) ? C5 C1 C2 Fe1 . . . . 60.0(2) ? S1 C1 C2 Fe1 . . . . -116.2(3) ? C1 C2 C3 C4 . . . . -0.8(4) ? S2 C2 C3 C4 . . . . -175.0(3) ? Fe1 C2 C3 C4 . . . . -60.0(3) ? C1 C2 C3 Fe1 . . . . 59.2(2) ? S2 C2 C3 Fe1 . . . . -115.0(3) ? C2 C3 C4 C5 . . . . 0.8(5) ? Fe1 C3 C4 C5 . . . . -57.8(3) ? C2 C3 C4 Fe1 . . . . 58.7(3) ? C2 C1 C5 C4 . . . . 0.1(4) ? S1 C1 C5 C4 . . . . 176.7(3) ? Fe1 C1 C5 C4 . . . . 59.2(3) ? C2 C1 C5 Fe1 . . . . -59.1(2) ? S1 C1 C5 Fe1 . . . . 117.4(3) ? C3 C4 C5 C1 . . . . -0.6(5) ? Fe1 C4 C5 C1 . . . . -58.3(3) ? C3 C4 C5 Fe1 . . . . 57.7(3) ? C10 C6 C7 C8 . . . . -0.8(6) ? Fe1 C6 C7 C8 . . . . 59.2(4) ? C10 C6 C7 Fe1 . . . . -60.1(4) ? C6 C7 C8 C9 . . . . 0.2(6) ? Fe1 C7 C8 C9 . . . . 59.5(4) ? C6 C7 C8 Fe1 . . . . -59.3(4) ? C7 C8 C9 C10 . . . . 0.5(6) ? Fe1 C8 C9 C10 . . . . 60.3(4) ? C7 C8 C9 Fe1 . . . . -59.7(4) ? C7 C6 C10 C9 . . . . 1.1(6) ? Fe1 C6 C10 C9 . . . . -59.1(4) ? C7 C6 C10 Fe1 . . . . 60.2(4) ? C8 C9 C10 C6 . . . . -1.0(6) ? Fe1 C9 C10 C6 . . . . 59.8(3) ? C8 C9 C10 Fe1 . . . . -60.8(4) ? C16 C11 C12 C13 . . . . 1.3(7) ? S1 C11 C12 C13 . . . . -179.3(4) ? C11 C12 C13 C14 . . . . -1.0(8) ? C12 C13 C14 C15 . . . . -0.1(8) ? C12 C13 C14 C17 . . . . 179.3(5) ? C13 C14 C15 C16 . . . . 0.7(7) ? C17 C14 C15 C16 . . . . -178.7(4) ? C12 C11 C16 C15 . . . . -0.7(7) ? S1 C11 C16 C15 . . . . 180.0(3) ? C14 C15 C16 C11 . . . . -0.4(7) ? C26 C21 C22 C23 . . . . -3.0(8) ? S2 C21 C22 C23 . . . . -179.0(5) ? C21 C22 C23 C24 . . . . -1.9(10) ? C22 C23 C24 C25 . . . . 5.2(9) ? C22 C23 C24 C27 . . . . -174.4(5) ? C23 C24 C25 C26 . . . . -3.9(8) ? C27 C24 C25 C26 . . . . 175.8(5) ? C22 C21 C26 C25 . . . . 4.3(8) ? S2 C21 C26 C25 . . . . -179.8(4) ? C24 C25 C26 C21 . . . . -0.8(8) ? C5 C1 S1 O1 . . . . -15.3(4) ? C2 C1 S1 O1 . . . . 160.3(3) ? Fe1 C1 S1 O1 . . . . 71.4(3) ? C5 C1 S1 C11 . . . . 94.8(3) ? C2 C1 S1 C11 . . . . -89.6(4) ? Fe1 C1 S1 C11 . . . . -178.5(2) ? C16 C11 S1 O1 . . . . 38.0(4) ? C12 C11 S1 O1 . . . . -141.4(4) ? C16 C11 S1 C1 . . . . -69.4(4) ? C12 C11 S1 C1 . . . . 111.2(4) ? C3 C2 S2 O2 . . . . 150.0(3) ? C1 C2 S2 O2 . . . . -23.0(4) ? Fe1 C2 S2 O2 . . . . 65.1(3) ? C3 C2 S2 C21 . . . . -100.5(3) ? C1 C2 S2 C21 . . . . 86.5(4) ? Fe1 C2 S2 C21 . . . . 174.6(2) ? C26 C21 S2 O2 . . . . 156.5(4) ? C22 C21 S2 O2 . . . . -27.6(5) ? C26 C21 S2 C2 . . . . 44.0(4) ? C22 C21 S2 C2 . . . . -140.1(4) ?