#------------------------------------------------------------------------------ #$Date: 2021-10-07 02:12:10 +0300 (Thu, 07 Oct 2021) $ #$Revision: 269806 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708521.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7708521 loop_ _publ_author_name 'Casper, Larissa Alina' 'Ebel, Viktoria' 'Linseis, Michael' 'Winter, Rainer' _publ_section_title ; Five Shades of Green: Substituent Influence on the (Spectro-) Electrochemical Properties of Diferrocenylphenyl Methylium Dyes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03009D _journal_year 2021 _chemical_formula_moiety 'C29 H22 F6 Fe2 O' _chemical_formula_sum 'C29 H22 F6 Fe2 O' _chemical_formula_weight 612.16 _space_group_crystal_system orthorhombic _space_group_IT_number 43 _space_group_name_Hall 'F 2 -2d' _space_group_name_H-M_alt 'F d d 2' _atom_sites_solution_hydrogens geom _audit_creation_date 2021-03-26 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _audit_update_record ; 2021-07-09 deposited with the CCDC. 2021-10-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 15.9862(5) _cell_length_b 40.2342(8) _cell_length_c 14.6279(3) _cell_measurement_reflns_used 20105 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.15 _cell_measurement_theta_min 2.42 _cell_volume 9408.5(4) _computing_cell_refinement ; X-Area Recipe 1.33.0.0 (STOE, 2015) ; _computing_data_collection ; X-Area WinXpose 2.0.22.0 (STOE, 2016) ; _computing_data_reduction ; X-Area Integrate 1.74.2.0 (STOE, 2018) X-Area LANA 1.75.3.0 (STOE, 2018) ; _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean 6.67 _diffrn_detector_type 'STOE Imaging Plate' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_details ; 185 frames, detector distance = 100 mm ; _diffrn_measurement_device '2-circle diffractometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method, \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_unetI/netI 0.0276 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 52 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 9610 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.576 _diffrn_reflns_theta_min 2.422 _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_T_max 0.3406 _exptl_absorpt_correction_T_min 0.2202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; STOE LANA, absorption correction by scaling of reflection intensities. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different absorption corrections on the model structure of tetrakis(\m~2~-acetato)- diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140. Afterwards a spherical absorption correction was performed within STOE LANA. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cube _exptl_crystal_F_000 4960 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.467 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.266 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.056 _refine_ls_abs_structure_details ; Flack x determined using 2366 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.000 _refine_ls_extinction_coef 0.00010(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 346 _refine_ls_number_reflns 5389 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0238 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+10.6031P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.0589 _reflns_Friedel_coverage 0.925 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.992 _reflns_number_gt 5092 _reflns_number_total 5389 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03009d2.cif _cod_data_source_block lc51b _cod_database_code 7708521 _shelx_shelxl_version_number 2018/3 _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_max 0.780 _shelx_estimated_absorpt_t_min 0.508 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.500(15) 0.500(15) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H) groups 3.a Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C25(H25), C27(H27) 3.b Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL lc51b_a.res in Fdd2 lc51b.res created by SHELXL-2018/3 at 14:30:33 on 26-Mar-2021 REM Old TITL lc51b_a.res in Fdd2 REM SHELXT solution in Fdd2: R1 0.064, Rweak 0.018, Alpha 0.001 REM 1.520 for 129 systematic absences, Orientation as input REM Flack x = 0.132 ( 0.009 ) from 1669 Parsons' quotients REM Formula found by SHELXT: C28 F7 Fe1 CELL 0.71073 15.9862 40.2342 14.6279 90 90 90 ZERR 16 0.0005 0.0008 0.0003 0 0 0 LATT -4 SYMM -X,-Y,+Z SYMM 0.25+X,0.25-Y,0.25+Z SYMM 0.25-X,0.25+Y,0.25+Z SFAC C H F Fe O UNIT 464 352 96 32 16 L.S. 10 PLAN 5 SIZE 0.2 0.467 0.6 TEMP -173.15 CONF BOND list 4 fmap 2 acta MORE -1 BOND $H TWIN -1 0 0 0 1 0 0 0 -1 2 REM REM REM WGHT 0.032300 10.603101 EXTI 0.000096 BASF 0.50000 FVAR 0.29451 FE1 4 0.574891 0.427784 0.302682 11.00000 0.01872 0.01913 = 0.01611 -0.00181 -0.00091 -0.00116 FE2 4 0.825732 0.515515 0.454239 11.00000 0.01433 0.01895 = 0.01753 0.00074 0.00154 -0.00197 F1 3 0.705685 0.352472 0.655954 11.00000 0.04020 0.02232 = 0.03156 -0.00250 -0.00681 0.01221 F2 3 0.650481 0.364502 0.784634 11.00000 0.03598 0.04622 = 0.03094 0.02090 0.00733 0.01236 F3 3 0.762774 0.389058 0.741495 11.00000 0.02617 0.02825 = 0.04994 0.00429 -0.02038 0.00107 F4 3 0.368480 0.433755 0.599639 11.00000 0.01500 0.08210 = 0.03084 -0.00082 -0.00288 0.00192 F5 3 0.406223 0.470241 0.694228 11.00000 0.03181 0.03791 = 0.08478 -0.02058 0.01913 0.00736 F6 3 0.392342 0.419750 0.737583 11.00000 0.02244 0.07346 = 0.04464 0.03390 0.01729 0.01349 O1 5 0.616546 0.496122 0.461725 11.00000 0.01615 0.01512 = 0.02496 0.00250 0.00232 0.00189 AFIX 147 H1 2 0.647566 0.511949 0.445809 11.00000 -1.50000 AFIX 0 C1 1 0.665939 0.466696 0.473134 11.00000 0.01336 0.01732 = 0.01690 -0.00051 0.00104 -0.00004 C2 1 0.667214 0.446562 0.386087 11.00000 0.01282 0.02041 = 0.01527 -0.00216 -0.00053 0.00042 C3 1 0.673418 0.410907 0.378629 11.00000 0.02290 0.02248 = 0.02008 -0.00071 -0.00136 0.00483 AFIX 43 H3 2 0.670466 0.395478 0.427685 11.00000 -1.20000 AFIX 0 C4 1 0.684755 0.402967 0.284617 11.00000 0.02684 0.02730 = 0.02422 -0.00763 -0.00037 0.00987 AFIX 43 H4 2 0.690947 0.381240 0.260112 11.00000 -1.20000 AFIX 0 C5 1 0.685245 0.432817 0.233948 11.00000 0.02060 0.03497 = 0.01653 -0.00528 0.00085 0.00308 AFIX 43 H5 2 0.691740 0.434598 0.169579 11.00000 -1.20000 AFIX 0 C6 1 0.674325 0.459856 0.295875 11.00000 0.01689 0.02499 = 0.01792 0.00029 0.00143 -0.00090 AFIX 43 H6 2 0.672158 0.482726 0.279902 11.00000 -1.20000 AFIX 0 C7 1 0.461375 0.427269 0.368211 11.00000 0.02068 0.05973 = 0.02647 -0.01206 0.00127 -0.00774 AFIX 43 H7 2 0.452214 0.430206 0.431869 11.00000 -1.20000 AFIX 0 C8 1 0.474865 0.396795 0.323373 11.00000 0.03220 0.03380 = 0.02677 0.00423 -0.00149 -0.01291 AFIX 43 H8 2 0.476767 0.375544 0.351604 11.00000 -1.20000 AFIX 0 C9 1 0.485071 0.403256 0.229299 11.00000 0.03182 0.03259 = 0.02349 -0.00462 -0.00452 -0.01008 AFIX 43 H9 2 0.494839 0.387109 0.183132 11.00000 -1.20000 AFIX 0 C10 1 0.478313 0.437595 0.215727 11.00000 0.02161 0.03970 = 0.03385 0.01170 -0.00915 -0.00661 AFIX 43 H10 2 0.482681 0.448734 0.158663 11.00000 -1.20000 AFIX 0 C11 1 0.463891 0.452892 0.301284 11.00000 0.01510 0.02972 = 0.07273 -0.00910 -0.00774 0.00079 AFIX 43 H11 2 0.457128 0.476019 0.312085 11.00000 -1.20000 AFIX 0 C12 1 0.754841 0.476243 0.498886 11.00000 0.01578 0.01512 = 0.01730 0.00119 -0.00021 -0.00054 C13 1 0.776803 0.497084 0.574310 11.00000 0.01560 0.02324 = 0.01611 0.00008 0.00192 -0.00333 AFIX 43 H13 2 0.738828 0.508072 0.614085 11.00000 -1.20000 AFIX 0 C14 1 0.865849 0.498453 0.579253 11.00000 0.01904 0.02408 = 0.01840 0.00194 -0.00051 -0.00378 AFIX 43 H14 2 0.897670 0.510689 0.622564 11.00000 -1.20000 AFIX 0 C15 1 0.898753 0.478172 0.507556 11.00000 0.01333 0.02851 = 0.02279 0.00435 0.00085 0.00150 AFIX 43 H15 2 0.956341 0.474424 0.495286 11.00000 -1.20000 AFIX 0 C16 1 0.830411 0.464556 0.457699 11.00000 0.01691 0.01853 = 0.02098 0.00198 0.00185 0.00121 AFIX 43 H16 2 0.834319 0.450248 0.406213 11.00000 -1.20000 AFIX 0 C17 1 0.761534 0.544245 0.360982 11.00000 0.01963 0.02445 = 0.03038 0.00933 0.00112 -0.00228 AFIX 43 H17 2 0.706082 0.540694 0.339772 11.00000 -1.20000 AFIX 0 C18 1 0.784657 0.563533 0.437318 11.00000 0.03730 0.01617 = 0.03519 0.00361 0.01121 -0.00015 AFIX 43 H18 2 0.747452 0.575114 0.476687 11.00000 -1.20000 AFIX 0 C19 1 0.872951 0.562674 0.445227 11.00000 0.03683 0.02842 = 0.02989 0.00359 -0.00174 -0.01571 AFIX 43 H19 2 0.905425 0.573634 0.490498 11.00000 -1.20000 AFIX 0 C20 1 0.904125 0.542508 0.373399 11.00000 0.02137 0.03744 = 0.02842 0.01048 0.00261 -0.00542 AFIX 43 H20 2 0.961292 0.537529 0.362127 11.00000 -1.20000 AFIX 0 C21 1 0.835145 0.531086 0.321397 11.00000 0.02708 0.02684 = 0.01913 0.00571 0.00085 0.00050 AFIX 43 H21 2 0.837839 0.517076 0.269204 11.00000 -1.20000 AFIX 0 C22 1 0.627579 0.446837 0.551175 11.00000 0.01848 0.01547 = 0.01331 -0.00190 -0.00093 0.00003 C23 1 0.674244 0.422903 0.597597 11.00000 0.01250 0.01999 = 0.01865 -0.00257 -0.00118 -0.00007 AFIX 43 H23 2 0.731315 0.419495 0.582110 11.00000 -1.20000 AFIX 0 C24 1 0.637799 0.404053 0.666235 11.00000 0.01720 0.01580 = 0.01593 -0.00081 -0.00275 0.00068 C25 1 0.554890 0.408813 0.691365 11.00000 0.01763 0.01965 = 0.01527 -0.00019 0.00017 -0.00168 AFIX 43 H25 2 0.530146 0.395892 0.738520 11.00000 -1.20000 AFIX 0 C26 1 0.509393 0.432879 0.645831 11.00000 0.01366 0.01976 = 0.01690 -0.00193 0.00180 0.00036 C27 1 0.544764 0.451846 0.576031 11.00000 0.01507 0.01689 = 0.01621 0.00080 -0.00113 0.00114 AFIX 43 H27 2 0.512188 0.468185 0.545520 11.00000 -1.20000 AFIX 0 C28 1 0.688907 0.377841 0.712258 11.00000 0.01999 0.02394 = 0.01955 0.00105 -0.00287 0.00062 C29 1 0.420135 0.439009 0.670244 11.00000 0.01859 0.02554 = 0.01918 0.00219 0.00185 0.00195 HKLF 4 REM lc51b_a.res in Fdd2 REM wR2 = 0.0589, GooF = S = 1.024, Restrained GooF = 1.024 for all data REM R1 = 0.0238 for 5092 Fo > 4sig(Fo) and 0.0264 for all 5389 data REM 346 parameters refined using 1 restraints END WGHT 0.0323 10.5992 REM Highest difference peak 0.266, deepest hole -0.368, 1-sigma level 0.056 Q1 1 0.8231 0.4943 0.4620 11.00000 0.05 0.27 Q2 1 0.5757 0.4055 0.3006 11.00000 0.05 0.25 Q3 1 0.8613 0.5421 0.4620 11.00000 0.05 0.25 Q4 1 0.4682 0.4215 0.2221 11.00000 0.05 0.25 Q5 1 0.6483 0.4072 0.6155 11.00000 0.05 0.24 ; _shelx_res_checksum 10491 _shelx_hkl_file ; 20 -12 2 31.59 40.49 -2 -20 -12 -2 31.59 40.49 1 20 -10 2 405.23 40.85 -2 -20 -10 -2 405.23 40.85 1 20 -8 4 1245.60 47.21 -2 -20 -8 -4 1245.60 47.21 1 20 -8 2 65.00 34.93 -2 -20 -8 -2 65.00 34.93 1 20 -6 4 19.34 34.75 -2 -20 -6 -4 19.34 34.75 1 20 -6 2 1344.35 42.64 -2 -20 -6 -2 1344.35 42.64 1 20 -4 4 993.84 38.19 -2 -20 -4 -4 993.84 38.19 1 20 -4 2 47.73 31.51 -2 -20 -4 -2 47.73 31.51 1 20 -2 4 154.74 40.53 -2 -20 -2 -4 154.74 40.53 1 20 -2 2 834.84 40.84 -2 -20 -2 -2 834.84 40.84 1 20 0 4 125.18 45.10 -2 -20 0 -4 125.18 45.10 1 19 -19 3 1009.04 45.20 -2 -19 -19 -3 1009.04 45.20 1 19 -19 1 933.39 39.76 -2 -19 -19 -1 933.39 39.76 1 19 -17 3 1255.56 39.32 -2 -19 -17 -3 1255.56 39.32 1 19 -17 1 97.96 33.25 -2 -19 -17 -1 97.96 33.25 1 19 -15 5 816.92 31.03 -2 -19 -15 -5 816.92 31.03 1 19 -15 3 754.99 32.44 -2 -19 -15 -3 754.99 32.44 1 19 -15 1 272.76 37.89 -2 -19 -15 -1 272.76 37.89 1 19 -13 5 235.87 29.04 -2 -19 -13 -5 235.87 29.04 1 19 -13 3 222.82 29.33 -2 -19 -13 -3 222.82 29.33 1 19 -13 1 1640.96 87.81 -2 -19 -13 -1 1640.96 87.81 1 19 -11 5 75.96 27.33 -2 -19 -11 -5 75.96 27.33 1 19 -11 3 207.22 32.97 -2 -19 -11 -3 207.22 32.97 1 19 -11 1 289.04 36.54 -2 -19 -11 -1 289.04 36.54 1 19 -9 5 75.07 27.40 -2 -19 -9 -5 75.07 27.40 1 19 -9 3 91.75 24.90 -2 -19 -9 -3 91.75 24.90 1 19 -9 1 340.07 35.25 -2 -19 -9 -1 340.07 35.25 1 19 -7 7 270.43 28.44 -2 -19 -7 -7 270.43 28.44 1 19 -7 5 53.62 29.97 -2 -19 -7 -5 53.62 29.97 1 19 -7 3 1450.09 48.19 -2 -19 -7 -3 1450.09 48.19 1 19 -7 1 1124.18 54.93 -2 -19 -7 -1 1124.18 54.93 1 19 -5 7 356.88 27.16 -2 -19 -5 -7 356.88 27.16 1 19 -5 5 595.41 27.92 -2 -19 -5 -5 595.41 27.92 1 19 -5 3 161.75 29.46 -2 -19 -5 -3 161.75 29.46 1 19 -5 1 918.09 60.64 -2 -19 -5 -1 918.09 60.64 1 19 -3 7 42.12 27.30 -2 -19 -3 -7 42.12 27.30 1 19 -3 5 163.46 31.86 -2 -19 -3 -5 163.46 31.86 1 19 -3 3 406.38 37.90 -2 -19 -3 -3 406.38 37.90 1 19 -3 1 510.31 29.26 -2 -19 -3 -1 510.31 29.26 1 19 -1 7 48.15 31.61 -2 -19 -1 -7 48.15 31.61 1 19 -1 5 199.37 30.23 -2 -19 -1 -5 199.37 30.23 1 19 -1 3 2353.83 60.18 -2 -19 -1 -3 2353.83 60.18 1 19 -1 1 543.73 33.31 -2 -19 -1 -1 543.73 33.31 1 18 -24 2 280.05 29.42 -2 -18 -24 -2 280.05 29.42 1 18 -22 4 54.24 26.69 -2 -18 -22 -4 54.24 26.69 1 18 -22 2 1672.86 50.12 -2 -18 -22 -2 1672.86 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1452.35 46.04 -2 18 12 4 1452.35 46.04 1 -18 12 -6 399.67 32.13 -2 18 12 6 399.67 32.13 1 -18 12 -8 252.10 41.27 -2 18 12 8 252.10 41.27 1 -18 14 0 254.25 37.71 -2 18 14 0 254.25 37.71 1 -18 14 -2 614.50 31.34 -2 18 14 2 614.50 31.34 1 -18 14 -4 329.62 34.81 -2 18 14 4 329.62 34.81 1 -18 14 -6 634.12 34.55 -2 18 14 6 634.12 34.55 1 -18 16 0 2613.49 75.58 -2 18 16 0 2613.49 75.58 1 -18 16 -2 211.88 31.68 -2 18 16 2 211.88 31.68 1 -18 16 -4 257.34 33.85 -2 18 16 4 257.34 33.85 1 -18 16 -6 7.26 30.99 -2 18 16 6 7.26 30.99 1 -18 18 0 112.24 24.83 -2 18 18 0 112.24 24.83 1 -18 18 -2 338.22 29.28 -2 18 18 2 338.22 29.28 1 -18 18 -4 54.96 33.78 -2 18 18 4 54.96 33.78 1 -18 18 -6 890.33 40.08 -2 18 18 6 890.33 40.08 1 -18 20 0 782.79 29.43 -2 18 20 0 782.79 29.43 1 -18 20 -2 194.27 38.07 -2 18 20 2 194.27 38.07 1 -18 20 -4 431.01 36.56 -2 18 20 4 431.01 36.56 1 -18 20 -6 23.36 51.37 -2 18 20 6 23.36 51.37 1 -18 22 0 361.98 29.88 -2 18 22 0 361.98 29.88 1 -18 22 -2 1622.69 115.97 -2 18 22 2 1622.69 115.97 1 -18 22 -4 40.85 34.21 -2 18 22 4 40.85 34.21 1 -18 24 0 84.86 25.89 -2 18 24 0 84.86 25.89 1 -18 24 -2 338.07 46.58 -2 18 24 2 338.07 46.58 1 -18 26 0 62.58 49.77 -2 18 26 0 62.58 49.77 1 -19 1 -1 579.11 30.57 -2 19 1 1 579.11 30.57 1 -19 1 -3 2326.10 101.49 -2 19 1 3 2326.10 101.49 1 -19 1 -5 130.09 33.54 -2 19 1 5 130.09 33.54 1 -19 1 -7 48.69 34.82 -2 19 1 7 48.69 34.82 1 -19 3 -1 504.94 35.71 -2 19 3 1 504.94 35.71 1 -19 3 -3 424.47 30.27 -2 19 3 3 424.47 30.27 1 -19 3 -5 164.59 31.72 -2 19 3 5 164.59 31.72 1 -19 3 -7 32.86 32.38 -2 19 3 7 32.86 32.38 1 -19 5 -1 949.07 36.24 -2 19 5 1 949.07 36.24 1 -19 5 -3 278.48 36.29 -2 19 5 3 278.48 36.29 1 -19 5 -5 597.01 38.49 -2 19 5 5 597.01 38.49 1 -19 5 -7 374.13 64.23 -2 19 5 7 374.13 64.23 1 -19 7 -1 1128.74 42.99 -2 19 7 1 1128.74 42.99 1 -19 7 -3 1405.82 32.74 -2 19 7 3 1405.82 32.74 1 -19 7 -5 59.82 31.70 -2 19 7 5 59.82 31.70 1 -19 7 -7 273.10 36.57 -2 19 7 7 273.10 36.57 1 -19 9 -1 381.22 37.19 -2 19 9 1 381.22 37.19 1 -19 9 -3 35.96 32.91 -2 19 9 3 35.96 32.91 1 -19 9 -5 32.29 32.78 -2 19 9 5 32.29 32.78 1 -19 11 -1 313.07 34.55 -2 19 11 1 313.07 34.55 1 -19 11 -3 151.04 37.60 -2 19 11 3 151.04 37.60 1 -19 11 -5 91.65 36.71 -2 19 11 5 91.65 36.71 1 -19 13 -1 1675.67 35.99 -2 19 13 1 1675.67 35.99 1 -19 13 -3 269.83 60.12 -2 19 13 3 269.83 60.12 1 -19 13 -5 285.26 30.93 -2 19 13 5 285.26 30.93 1 -19 15 -1 244.92 34.37 -2 19 15 1 244.92 34.37 1 -19 15 -3 769.23 33.64 -2 19 15 3 769.23 33.64 1 -19 15 -5 859.39 36.63 -2 19 15 5 859.39 36.63 1 -19 17 -1 45.63 33.54 -2 19 17 1 45.63 33.54 1 -19 17 -3 1229.14 39.39 -2 19 17 3 1229.14 39.39 1 -19 19 -1 914.97 42.84 -2 19 19 1 914.97 42.84 1 -19 19 -3 972.72 36.81 -2 19 19 3 972.72 36.81 1 -20 0 0 5306.72 187.22 -2 20 0 0 5306.72 187.22 1 -20 0 -4 202.48 47.12 -2 20 0 4 202.48 47.12 1 -20 2 0 41.41 43.67 -2 20 2 0 41.41 43.67 1 -20 2 -2 800.53 42.34 -2 20 2 2 800.53 42.34 1 -20 2 -4 131.48 36.09 -2 20 2 4 131.48 36.09 1 -20 4 0 766.41 38.48 -2 20 4 0 766.41 38.48 1 -20 4 -2 56.95 31.05 -2 20 4 2 56.95 31.05 1 -20 4 -4 1066.16 43.00 -2 20 4 4 1066.16 43.00 1 -20 6 0 246.87 32.46 -2 20 6 0 246.87 32.46 1 -20 6 -2 1441.25 42.62 -2 20 6 2 1441.25 42.62 1 -20 6 -4 19.79 31.55 -2 20 6 4 19.79 31.55 1 -20 8 0 317.95 36.19 -2 20 8 0 317.95 36.19 1 -20 8 -2 80.61 34.50 -2 20 8 2 80.61 34.50 1 -20 8 -4 1216.85 40.52 -2 20 8 4 1216.85 40.52 1 -20 10 0 52.82 32.11 -2 20 10 0 52.82 32.11 1 -20 10 -2 340.73 34.96 -2 20 10 2 340.73 34.96 1 -20 12 0 1179.21 73.17 -2 20 12 0 1179.21 73.17 1 -20 12 -2 13.95 35.24 -2 20 12 2 13.95 35.24 1 -20 14 0 -30.80 78.91 -2 20 14 0 -30.80 78.91 1 0 0 0 REM TWIN -1 0 0 0 1 0 0 0 -1 ; _shelx_hkl_checksum 4094 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.57489(3) 0.42778(2) 0.30268(2) 0.01799(10) Uani 1 1 d . . . . . Fe2 Fe 0.82573(2) 0.51551(2) 0.45424(3) 0.01694(10) Uani 1 1 d . . . . . F1 F 0.70569(13) 0.35247(5) 0.65595(13) 0.0314(4) Uani 1 1 d . . . . . F2 F 0.65048(14) 0.36450(6) 0.78463(14) 0.0377(5) Uani 1 1 d . . . . . F3 F 0.76277(12) 0.38906(5) 0.74149(15) 0.0348(5) Uani 1 1 d . . . . . F4 F 0.36848(12) 0.43376(7) 0.59964(14) 0.0426(6) Uani 1 1 d . . . . . F5 F 0.40622(14) 0.47024(6) 0.6942(2) 0.0515(7) Uani 1 1 d . . . . . F6 F 0.39234(13) 0.41975(7) 0.73758(15) 0.0468(6) Uani 1 1 d . . . . . O1 O 0.61655(12) 0.49612(5) 0.46173(15) 0.0187(4) Uani 1 1 d . . . . . H1 H 0.647566 0.511949 0.445809 0.028 Uiso 1 1 calc R U . . . C1 C 0.66594(16) 0.46670(7) 0.47313(18) 0.0159(5) Uani 1 1 d . . . . . C2 C 0.66721(17) 0.44656(7) 0.38609(19) 0.0162(5) Uani 1 1 d . . . . . C3 C 0.67342(18) 0.41091(8) 0.3786(2) 0.0218(6) Uani 1 1 d . . . . . H3 H 0.670466 0.395478 0.427685 0.026 Uiso 1 1 calc R U . . . C4 C 0.6848(2) 0.40297(8) 0.2846(2) 0.0261(7) Uani 1 1 d . . . . . H4 H 0.690947 0.381240 0.260112 0.031 Uiso 1 1 calc R U . . . C5 C 0.68525(19) 0.43282(9) 0.2339(2) 0.0240(6) Uani 1 1 d . . . . . H5 H 0.691740 0.434598 0.169579 0.029 Uiso 1 1 calc R U . . . C6 C 0.67432(17) 0.45986(8) 0.2959(2) 0.0199(5) Uani 1 1 d . . . . . H6 H 0.672158 0.482726 0.279902 0.024 Uiso 1 1 calc R U . . . C7 C 0.4614(2) 0.42727(11) 0.3682(2) 0.0356(8) Uani 1 1 d . . . . . H7 H 0.452214 0.430206 0.431869 0.043 Uiso 1 1 calc R U . . . C8 C 0.4749(2) 0.39680(9) 0.3234(2) 0.0309(7) Uani 1 1 d . . . . . H8 H 0.476767 0.375544 0.351604 0.037 Uiso 1 1 calc R U . . . C9 C 0.4851(2) 0.40326(9) 0.2293(2) 0.0293(7) Uani 1 1 d . . . . . H9 H 0.494839 0.387109 0.183132 0.035 Uiso 1 1 calc R U . . . C10 C 0.4783(2) 0.43759(9) 0.2157(3) 0.0317(7) Uani 1 1 d . . . . . H10 H 0.482681 0.448734 0.158663 0.038 Uiso 1 1 calc R U . . . C11 C 0.4639(2) 0.45289(8) 0.3013(3) 0.0392(9) Uani 1 1 d . . . . . H11 H 0.457128 0.476019 0.312085 0.047 Uiso 1 1 calc R U . . . C12 C 0.75484(17) 0.47624(7) 0.49889(18) 0.0161(5) Uani 1 1 d . . . . . C13 C 0.77680(17) 0.49708(7) 0.57431(19) 0.0183(5) Uani 1 1 d . . . . . H13 H 0.738828 0.508072 0.614085 0.022 Uiso 1 1 calc R U . . . C14 C 0.86585(18) 0.49845(7) 0.57925(19) 0.0205(6) Uani 1 1 d . . . . . H14 H 0.897670 0.510689 0.622564 0.025 Uiso 1 1 calc R U . . . C15 C 0.89875(18) 0.47817(8) 0.5076(2) 0.0215(6) Uani 1 1 d . . . . . H15 H 0.956341 0.474424 0.495286 0.026 Uiso 1 1 calc R U . . . C16 C 0.83041(17) 0.46456(7) 0.4577(2) 0.0188(5) Uani 1 1 d . . . . . H16 H 0.834319 0.450248 0.406213 0.023 Uiso 1 1 calc R U . . . C17 C 0.76153(19) 0.54424(8) 0.3610(2) 0.0248(6) Uani 1 1 d . . . . . H17 H 0.706082 0.540694 0.339772 0.030 Uiso 1 1 calc R U . . . C18 C 0.7847(2) 0.56353(7) 0.4373(2) 0.0296(7) Uani 1 1 d . . . . . H18 H 0.747452 0.575114 0.476687 0.035 Uiso 1 1 calc R U . . . C19 C 0.8730(2) 0.56267(8) 0.4452(2) 0.0317(7) Uani 1 1 d . . . . . H19 H 0.905425 0.573634 0.490498 0.038 Uiso 1 1 calc R U . . . C20 C 0.9041(2) 0.54251(9) 0.3734(2) 0.0291(7) Uani 1 1 d . . . . . H20 H 0.961292 0.537529 0.362127 0.035 Uiso 1 1 calc R U . . . C21 C 0.8351(2) 0.53109(8) 0.3214(2) 0.0243(6) Uani 1 1 d . . . . . H21 H 0.837839 0.517076 0.269204 0.029 Uiso 1 1 calc R U . . . C22 C 0.62758(17) 0.44684(6) 0.55117(18) 0.0158(5) Uani 1 1 d . . . . . C23 C 0.67424(17) 0.42290(7) 0.59760(19) 0.0170(5) Uani 1 1 d . . . . . H23 H 0.731315 0.419495 0.582110 0.020 Uiso 1 1 calc R U . . . C24 C 0.63780(17) 0.40405(7) 0.66624(18) 0.0163(5) Uani 1 1 d . . . . . C25 C 0.55489(17) 0.40881(7) 0.69137(18) 0.0175(5) Uani 1 1 d . . . . . H25 H 0.530146 0.395892 0.738520 0.021 Uiso 1 1 calc R U . . . C26 C 0.50939(17) 0.43288(7) 0.64583(18) 0.0168(5) Uani 1 1 d . . . . . C27 C 0.54476(17) 0.45185(7) 0.57603(18) 0.0161(5) Uani 1 1 d . . . . . H27 H 0.512188 0.468185 0.545520 0.019 Uiso 1 1 calc R U . . . C28 C 0.68891(18) 0.37784(7) 0.7123(2) 0.0212(6) Uani 1 1 d . . . . . C29 C 0.42014(18) 0.43901(8) 0.6702(2) 0.0211(6) Uani 1 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 Fe1 0.01872(19) 0.01913(19) 0.01611(17) -0.00181(15) -0.00091(16) -0.00116(15) Fe2 0.01433(17) 0.01895(19) 0.01753(18) 0.00074(15) 0.00154(16) -0.00197(14) F1 0.0402(11) 0.0223(9) 0.0316(9) -0.0025(8) -0.0068(9) 0.0122(8) F2 0.0360(11) 0.0462(12) 0.0309(10) 0.0209(9) 0.0073(8) 0.0124(9) F3 0.0262(10) 0.0282(10) 0.0499(11) 0.0043(9) -0.0204(9) 0.0011(8) F4 0.0150(9) 0.0821(17) 0.0308(10) -0.0008(11) -0.0029(8) 0.0019(9) F5 0.0318(11) 0.0379(12) 0.0848(19) -0.0206(13) 0.0191(13) 0.0074(9) F6 0.0224(9) 0.0735(15) 0.0446(13) 0.0339(12) 0.0173(9) 0.0135(11) O1 0.0161(9) 0.0151(9) 0.0250(10) 0.0025(8) 0.0023(8) 0.0019(7) C1 0.0134(12) 0.0173(12) 0.0169(12) -0.0005(10) 0.0010(9) 0.0000(9) C2 0.0128(12) 0.0204(13) 0.0153(12) -0.0022(11) -0.0005(9) 0.0004(10) C3 0.0229(14) 0.0225(14) 0.0201(13) -0.0007(11) -0.0014(11) 0.0048(11) C4 0.0268(15) 0.0273(15) 0.0242(15) -0.0076(12) -0.0004(12) 0.0099(13) C5 0.0206(15) 0.0350(16) 0.0165(13) -0.0053(12) 0.0008(11) 0.0031(12) C6 0.0169(13) 0.0250(13) 0.0179(13) 0.0003(11) 0.0014(11) -0.0009(10) C7 0.0207(16) 0.060(2) 0.0265(16) -0.0121(15) 0.0013(13) -0.0077(15) C8 0.0322(17) 0.0338(17) 0.0268(15) 0.0042(13) -0.0015(13) -0.0129(14) C9 0.0318(17) 0.0326(17) 0.0235(15) -0.0046(13) -0.0045(12) -0.0101(14) C10 0.0216(15) 0.0397(18) 0.0338(17) 0.0117(15) -0.0092(13) -0.0066(13) C11 0.0151(14) 0.0297(17) 0.073(3) -0.0091(19) -0.0077(17) 0.0008(12) C12 0.0158(12) 0.0151(12) 0.0173(12) 0.0012(10) -0.0002(10) -0.0005(9) C13 0.0156(12) 0.0232(13) 0.0161(11) 0.0001(11) 0.0019(10) -0.0033(10) C14 0.0190(13) 0.0241(14) 0.0184(12) 0.0019(11) -0.0005(11) -0.0038(11) C15 0.0133(12) 0.0285(15) 0.0228(14) 0.0043(12) 0.0008(11) 0.0015(11) C16 0.0169(12) 0.0185(12) 0.0210(12) 0.0020(12) 0.0019(11) 0.0012(10) C17 0.0196(14) 0.0244(15) 0.0304(15) 0.0093(12) 0.0011(12) -0.0023(11) C18 0.0373(18) 0.0162(13) 0.0352(17) 0.0036(12) 0.0112(14) -0.0002(12) C19 0.0368(17) 0.0284(15) 0.0299(15) 0.0036(14) -0.0017(14) -0.0157(13) C20 0.0214(14) 0.0374(18) 0.0284(16) 0.0105(14) 0.0026(12) -0.0054(13) C21 0.0271(15) 0.0268(15) 0.0191(13) 0.0057(12) 0.0009(11) 0.0005(12) C22 0.0185(12) 0.0155(11) 0.0133(11) -0.0019(10) -0.0009(10) 0.0000(10) C23 0.0125(12) 0.0200(12) 0.0186(12) -0.0026(11) -0.0012(10) -0.0001(9) C24 0.0172(13) 0.0158(12) 0.0159(11) -0.0008(10) -0.0027(10) 0.0007(10) C25 0.0176(12) 0.0197(12) 0.0153(11) -0.0002(10) 0.0002(10) -0.0017(10) C26 0.0137(12) 0.0198(13) 0.0169(12) -0.0019(10) 0.0018(10) 0.0004(10) C27 0.0151(12) 0.0169(12) 0.0162(11) 0.0008(10) -0.0011(10) 0.0011(10) C28 0.0200(13) 0.0239(14) 0.0195(13) 0.0011(11) -0.0029(11) 0.0006(11) C29 0.0186(13) 0.0255(14) 0.0192(12) 0.0022(11) 0.0019(10) 0.0019(11) 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' F F 0.0171 0.0103 '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' 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 C3 Fe1 C2 41.16(12) . . ? C3 Fe1 C6 68.77(12) . . ? C3 Fe1 C7 115.10(14) . . ? C3 Fe1 C8 108.59(14) . . ? C3 Fe1 C9 131.74(13) . . ? C4 Fe1 C2 68.82(12) . . ? C4 Fe1 C3 40.83(12) . . ? C4 Fe1 C5 40.49(13) . . ? C4 Fe1 C6 68.52(13) . . ? C4 Fe1 C7 144.86(16) . . ? C4 Fe1 C8 113.17(15) . . ? C4 Fe1 C9 107.48(14) . . ? C4 Fe1 C10 131.81(14) . . ? C4 Fe1 C11 171.97(16) . . ? C5 Fe1 C2 68.64(11) . . ? C5 Fe1 C3 68.56(12) . . ? C5 Fe1 C6 40.82(12) . . ? C5 Fe1 C7 174.57(16) . . ? C5 Fe1 C8 143.84(14) . . ? C5 Fe1 C9 113.33(13) . . ? C5 Fe1 C11 134.21(15) . . ? C6 Fe1 C2 40.69(11) . . ? C6 Fe1 C7 135.62(14) . . ? C6 Fe1 C8 174.19(13) . . ? C7 Fe1 C2 111.15(12) . . ? C8 Fe1 C2 134.02(12) . . ? C8 Fe1 C7 40.12(15) . . ? C9 Fe1 C2 172.27(13) . . ? C9 Fe1 C6 145.31(12) . . ? C9 Fe1 C7 67.65(14) . . ? C9 Fe1 C8 40.26(13) . . ? C10 Fe1 C2 147.31(13) . . ? C10 Fe1 C3 170.78(14) . . ? C10 Fe1 C5 109.15(14) . . ? C10 Fe1 C6 115.79(13) . . ? C10 Fe1 C7 67.90(15) . . ? C10 Fe1 C8 67.62(14) . . ? C10 Fe1 C9 40.08(14) . . ? C10 Fe1 C11 40.53(17) . . ? C11 Fe1 C2 116.58(13) . . ? C11 Fe1 C3 147.10(15) . . ? C11 Fe1 C6 111.22(13) . . ? C11 Fe1 C7 40.65(17) . . ? C11 Fe1 C8 67.95(15) . . ? C11 Fe1 C9 67.89(15) . . ? C12 Fe2 C13 40.69(11) . . ? C12 Fe2 C14 68.40(11) . . ? C12 Fe2 C15 68.29(11) . . ? C12 Fe2 C16 40.77(11) . . ? C12 Fe2 C17 111.56(11) . . ? C12 Fe2 C18 125.86(12) . . ? C13 Fe2 C17 125.22(12) . . ? C14 Fe2 C13 40.55(11) . . ? C14 Fe2 C15 40.67(12) . . ? C14 Fe2 C17 158.60(12) . . ? C15 Fe2 C13 68.24(12) . . ? C15 Fe2 C17 160.60(13) . . ? C16 Fe2 C13 68.49(12) . . ? C16 Fe2 C14 68.48(12) . . ? C16 Fe2 C15 40.54(11) . . ? C16 Fe2 C17 126.48(12) . . ? C16 Fe2 C18 162.48(13) . . ? C18 Fe2 C13 108.64(12) . . ? C18 Fe2 C14 121.37(13) . . ? C18 Fe2 C15 156.03(14) . . ? C18 Fe2 C17 40.03(14) . . ? C19 Fe2 C12 159.81(13) . . ? C19 Fe2 C13 121.91(13) . . ? C19 Fe2 C14 104.59(13) . . ? C19 Fe2 C15 119.51(13) . . ? C19 Fe2 C16 156.13(14) . . ? C19 Fe2 C17 67.74(13) . . ? C19 Fe2 C18 40.41(14) . . ? C19 Fe2 C21 68.16(14) . . ? C20 Fe2 C12 159.32(13) . . ? C20 Fe2 C13 156.97(13) . . ? C20 Fe2 C14 120.17(13) . . ? C20 Fe2 C15 105.10(13) . . ? C20 Fe2 C16 121.64(14) . . ? C20 Fe2 C17 67.86(13) . . ? C20 Fe2 C18 68.00(14) . . ? C20 Fe2 C19 40.64(15) . . ? C20 Fe2 C21 40.58(13) . . ? C21 Fe2 C12 125.35(12) . . ? C21 Fe2 C13 161.27(12) . . ? C21 Fe2 C14 157.45(13) . . ? C21 Fe2 C15 122.81(13) . . ? C21 Fe2 C16 109.05(13) . . ? C21 Fe2 C17 40.27(12) . . ? C21 Fe2 C18 67.76(13) . . ? C1 O1 H1 109.5 . . ? O1 C1 C2 110.6(2) . . ? O1 C1 C12 109.6(2) . . ? O1 C1 C22 107.4(2) . . ? C2 C1 C12 109.4(2) . . ? C2 C1 C22 110.9(2) . . ? C12 C1 C22 108.9(2) . . ? C1 C2 Fe1 133.42(19) . . ? C3 C2 Fe1 68.86(16) . . ? C3 C2 C1 126.8(3) . . ? C6 C2 Fe1 69.33(16) . . ? C6 C2 C1 125.4(3) . . ? C6 C2 C3 107.3(2) . . ? Fe1 C3 H3 126.1 . . ? C2 C3 Fe1 69.98(16) . . ? C2 C3 H3 126.1 . . ? C4 C3 Fe1 69.36(17) . . ? C4 C3 C2 107.8(3) . . ? C4 C3 H3 126.1 . . ? Fe1 C4 H4 126.1 . . ? C3 C4 Fe1 69.82(17) . . ? C3 C4 H4 125.8 . . ? C5 C4 Fe1 69.87(18) . . ? C5 C4 C3 108.5(3) . . ? C5 C4 H4 125.8 . . ? Fe1 C5 H5 126.2 . . ? C4 C5 Fe1 69.64(19) . . ? C4 C5 H5 125.8 . . ? C4 C5 C6 108.4(3) . . ? C6 C5 Fe1 69.94(16) . . ? C6 C5 H5 125.8 . . ? Fe1 C6 H6 126.4 . . ? C2 C6 Fe1 69.98(16) . . ? C2 C6 H6 125.9 . . ? C5 C6 Fe1 69.25(17) . . ? C5 C6 C2 108.1(3) . . ? C5 C6 H6 125.9 . . ? Fe1 C7 H7 126.4 . . ? C8 C7 Fe1 69.9(2) . . ? C8 C7 H7 126.1 . . ? C8 C7 C11 107.8(3) . . ? C11 C7 Fe1 69.3(2) . . ? C11 C7 H7 126.1 . . ? Fe1 C8 H8 125.9 . . ? C7 C8 Fe1 70.03(19) . . ? C7 C8 H8 125.9 . . ? C7 C8 C9 108.2(3) . . ? C9 C8 Fe1 69.73(19) . . ? C9 C8 H8 125.9 . . ? Fe1 C9 H9 126.0 . . ? C8 C9 Fe1 70.01(19) . . ? C8 C9 H9 125.9 . . ? C10 C9 Fe1 69.67(18) . . ? C10 C9 C8 108.1(3) . . ? C10 C9 H9 125.9 . . ? Fe1 C10 H10 125.7 . . ? C9 C10 Fe1 70.25(19) . . ? C9 C10 H10 125.8 . . ? C9 C10 C11 108.5(3) . . ? C11 C10 Fe1 69.85(19) . . ? C11 C10 H10 125.8 . . ? Fe1 C11 H11 125.6 . . ? C7 C11 Fe1 70.1(2) . . ? C7 C11 H11 126.3 . . ? C10 C11 Fe1 69.62(19) . . ? C10 C11 C7 107.4(3) . . ? C10 C11 H11 126.3 . . ? C1 C12 Fe2 129.23(19) . . ? C13 C12 Fe2 70.01(15) . . ? C13 C12 C1 124.7(2) . . ? C16 C12 Fe2 69.65(15) . . ? C16 C12 C1 127.1(2) . . ? C16 C12 C13 108.1(2) . . ? Fe2 C13 H13 126.7 . . ? C12 C13 Fe2 69.30(15) . . ? C12 C13 H13 126.1 . . ? C14 C13 Fe2 69.54(16) . . ? C14 C13 C12 107.9(3) . . ? C14 C13 H13 126.1 . . ? Fe2 C14 H14 126.0 . . ? C13 C14 Fe2 69.91(16) . . ? C13 C14 H14 126.0 . . ? C13 C14 C15 107.9(3) . . ? C15 C14 Fe2 69.68(17) . . ? C15 C14 H14 126.0 . . ? Fe2 C15 H15 126.5 . . ? C14 C15 Fe2 69.65(17) . . ? C14 C15 H15 125.9 . . ? C16 C15 Fe2 69.58(16) . . ? C16 C15 C14 108.3(3) . . ? C16 C15 H15 125.9 . . ? Fe2 C16 H16 126.0 . . ? C12 C16 Fe2 69.57(15) . . ? C12 C16 H16 126.1 . . ? C15 C16 Fe2 69.88(16) . . ? C15 C16 C12 107.8(3) . . ? C15 C16 H16 126.1 . . ? Fe2 C17 H17 126.6 . . ? C18 C17 Fe2 69.75(18) . . ? C18 C17 H17 125.9 . . ? C18 C17 C21 108.2(3) . . ? C21 C17 Fe2 69.32(17) . . ? C21 C17 H17 125.9 . . ? Fe2 C18 H18 126.0 . . ? C17 C18 Fe2 70.22(18) . . ? C17 C18 H18 125.9 . . ? C17 C18 C19 108.2(3) . . ? C19 C18 Fe2 69.45(19) . . ? C19 C18 H18 125.9 . . ? Fe2 C19 H19 126.0 . . ? C18 C19 Fe2 70.14(18) . . ? C18 C19 H19 126.2 . . ? C18 C19 C20 107.7(3) . . ? C20 C19 Fe2 69.32(19) . . ? C20 C19 H19 126.2 . . ? Fe2 C20 H20 125.5 . . ? C19 C20 Fe2 70.04(18) . . ? C19 C20 H20 126.0 . . ? C21 C20 Fe2 70.11(18) . . ? C21 C20 C19 108.1(3) . . ? C21 C20 H20 126.0 . . ? Fe2 C21 H21 125.8 . . ? C17 C21 Fe2 70.41(17) . . ? C17 C21 C20 107.8(3) . . ? C17 C21 H21 126.1 . . ? C20 C21 Fe2 69.31(18) . . ? C20 C21 H21 126.1 . . ? C23 C22 C1 120.8(2) . . ? C27 C22 C1 120.3(2) . . ? C27 C22 C23 118.9(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 C22 120.4(2) . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 121.1(3) . . ? C23 C24 C28 118.8(2) . . ? C25 C24 C28 120.0(3) . . ? C24 C25 H25 120.9 . . ? C26 C25 C24 118.1(3) . . ? C26 C25 H25 120.9 . . ? C25 C26 C27 121.5(3) . . ? C25 C26 C29 120.3(3) . . ? C27 C26 C29 118.2(3) . . ? C22 C27 C26 119.9(2) . . ? C22 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? F1 C28 C24 111.7(2) . . ? F2 C28 F1 105.9(2) . . ? F2 C28 C24 112.9(2) . . ? F3 C28 F1 106.1(2) . . ? F3 C28 F2 106.8(2) . . ? F3 C28 C24 112.9(2) . . ? F4 C29 C26 112.3(2) . . ? F5 C29 F4 104.5(3) . . ? F5 C29 F6 107.5(3) . . ? F5 C29 C26 112.4(3) . . ? F6 C29 F4 105.9(3) . . ? F6 C29 C26 113.6(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 2.059(3) . ? Fe1 C3 2.044(3) . ? Fe1 C4 2.038(3) . ? Fe1 C5 2.041(3) . ? Fe1 C6 2.050(3) . ? Fe1 C7 2.052(3) . ? Fe1 C8 2.050(3) . ? Fe1 C9 2.046(3) . ? Fe1 C10 2.039(3) . ? Fe1 C11 2.042(3) . ? Fe2 C12 2.051(3) . ? Fe2 C13 2.061(3) . ? Fe2 C14 2.056(3) . ? Fe2 C15 2.056(3) . ? Fe2 C16 2.052(3) . ? Fe2 C17 2.062(3) . ? Fe2 C18 2.055(3) . ? Fe2 C19 2.046(3) . ? Fe2 C20 2.037(3) . ? Fe2 C21 2.047(3) . ? F1 C28 1.339(4) . ? F2 C28 1.337(4) . ? F3 C28 1.335(3) . ? F4 C29 1.339(4) . ? F5 C29 1.323(4) . ? F6 C29 1.330(4) . ? O1 H1 0.8400 . ? O1 C1 1.433(3) . ? C1 C2 1.509(4) . ? C1 C12 1.520(4) . ? C1 C22 1.522(4) . ? C2 C3 1.442(4) . ? C2 C6 1.428(4) . ? C3 H3 0.9500 . ? C3 C4 1.423(4) . ? C4 H4 0.9500 . ? C4 C5 1.411(4) . ? C5 H5 0.9500 . ? C5 C6 1.426(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C7 C8 1.407(5) . ? C7 C11 1.422(6) . ? C8 H8 0.9500 . ? C8 C9 1.410(5) . ? C9 H9 0.9500 . ? C9 C10 1.400(5) . ? C10 H10 0.9500 . ? C10 C11 1.414(6) . ? C11 H11 0.9500 . ? C12 C13 1.430(4) . ? C12 C16 1.430(4) . ? C13 H13 0.9500 . ? C13 C14 1.426(4) . ? C14 H14 0.9500 . ? C14 C15 1.429(4) . ? C15 H15 0.9500 . ? C15 C16 1.423(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C17 C18 1.409(5) . ? C17 C21 1.414(4) . ? C18 H18 0.9500 . ? C18 C19 1.417(5) . ? C19 H19 0.9500 . ? C19 C20 1.418(5) . ? C20 H20 0.9500 . ? C20 C21 1.416(5) . ? C21 H21 0.9500 . ? C22 C23 1.395(4) . ? C22 C27 1.388(4) . ? C23 H23 0.9500 . ? C23 C24 1.387(4) . ? C24 C25 1.389(4) . ? C24 C28 1.494(4) . ? C25 H25 0.9500 . ? C25 C26 1.382(4) . ? C26 C27 1.395(4) . ? C26 C29 1.491(4) . ? C27 H27 0.9500 . ? 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 Fe1 C2 C3 C4 59.3(2) . . . . ? Fe1 C2 C6 C5 -58.9(2) . . . . ? Fe1 C3 C4 C5 59.4(2) . . . . ? Fe1 C4 C5 C6 59.4(2) . . . . ? Fe1 C5 C6 C2 59.4(2) . . . . ? Fe1 C7 C8 C9 -59.5(2) . . . . ? Fe1 C7 C11 C10 59.9(2) . . . . ? Fe1 C8 C9 C10 -59.5(2) . . . . ? Fe1 C9 C10 C11 -59.6(2) . . . . ? Fe1 C10 C11 C7 -60.2(2) . . . . ? Fe2 C12 C13 C14 -59.04(19) . . . . ? Fe2 C12 C16 C15 59.7(2) . . . . ? Fe2 C13 C14 C15 -59.5(2) . . . . ? Fe2 C14 C15 C16 -59.1(2) . . . . ? Fe2 C15 C16 C12 -59.45(19) . . . . ? Fe2 C17 C18 C19 59.3(2) . . . . ? Fe2 C17 C21 C20 -59.4(2) . . . . ? Fe2 C18 C19 C20 59.4(2) . . . . ? Fe2 C19 C20 C21 60.1(2) . . . . ? Fe2 C20 C21 C17 60.1(2) . . . . ? O1 C1 C2 Fe1 -53.6(3) . . . . ? O1 C1 C2 C3 -148.6(3) . . . . ? O1 C1 C2 C6 40.8(3) . . . . ? O1 C1 C12 Fe2 -37.2(3) . . . . ? O1 C1 C12 C13 54.4(3) . . . . ? O1 C1 C12 C16 -130.3(3) . . . . ? O1 C1 C22 C23 -159.7(2) . . . . ? O1 C1 C22 C27 21.6(3) . . . . ? C1 C2 C3 Fe1 129.1(3) . . . . ? C1 C2 C3 C4 -171.6(3) . . . . ? C1 C2 C6 Fe1 -129.3(3) . . . . ? C1 C2 C6 C5 171.8(3) . . . . ? C1 C12 C13 Fe2 -124.5(3) . . . . ? C1 C12 C13 C14 176.4(2) . . . . ? C1 C12 C16 Fe2 124.4(3) . . . . ? C1 C12 C16 C15 -175.9(3) . . . . ? C1 C22 C23 C24 -177.5(2) . . . . ? C1 C22 C27 C26 178.1(2) . . . . ? C2 C1 C12 Fe2 84.3(3) . . . . ? C2 C1 C12 C13 175.9(3) . . . . ? C2 C1 C12 C16 -8.8(4) . . . . ? C2 C1 C22 C23 79.3(3) . . . . ? C2 C1 C22 C27 -99.4(3) . . . . ? C2 C3 C4 Fe1 -59.7(2) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C3 C2 C6 Fe1 58.59(19) . . . . ? C3 C2 C6 C5 -0.3(3) . . . . ? C3 C4 C5 Fe1 -59.3(2) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C4 C5 C6 Fe1 -59.2(2) . . . . ? C4 C5 C6 C2 0.2(3) . . . . ? C6 C2 C3 Fe1 -58.89(19) . . . . ? C6 C2 C3 C4 0.4(3) . . . . ? C7 C8 C9 Fe1 59.7(2) . . . . ? C7 C8 C9 C10 0.2(4) . . . . ? C8 C7 C11 Fe1 -59.4(2) . . . . ? C8 C7 C11 C10 0.5(4) . . . . ? C8 C9 C10 Fe1 59.7(2) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C9 C10 C11 Fe1 59.9(2) . . . . ? C9 C10 C11 C7 -0.3(4) . . . . ? C11 C7 C8 Fe1 59.1(2) . . . . ? C11 C7 C8 C9 -0.4(4) . . . . ? C12 C1 C2 Fe1 -174.5(2) . . . . ? C12 C1 C2 C3 90.5(3) . . . . ? C12 C1 C2 C6 -80.1(3) . . . . ? C12 C1 C22 C23 -41.1(3) . . . . ? C12 C1 C22 C27 140.2(2) . . . . ? C12 C13 C14 Fe2 58.89(19) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? C13 C12 C16 Fe2 -59.69(19) . . . . ? C13 C12 C16 C15 0.0(3) . . . . ? C13 C14 C15 Fe2 59.7(2) . . . . ? C13 C14 C15 C16 0.6(3) . . . . ? C14 C15 C16 Fe2 59.1(2) . . . . ? C14 C15 C16 C12 -0.4(3) . . . . ? C16 C12 C13 Fe2 59.46(19) . . . . ? C16 C12 C13 C14 0.4(3) . . . . ? C17 C18 C19 Fe2 -59.7(2) . . . . ? C17 C18 C19 C20 -0.4(4) . . . . ? C18 C17 C21 Fe2 59.1(2) . . . . ? C18 C17 C21 C20 -0.3(3) . . . . ? C18 C19 C20 Fe2 -59.9(2) . . . . ? C18 C19 C20 C21 0.1(4) . . . . ? C19 C20 C21 Fe2 -60.0(2) . . . . ? C19 C20 C21 C17 0.1(4) . . . . ? C21 C17 C18 Fe2 -58.8(2) . . . . ? C21 C17 C18 C19 0.4(4) . . . . ? C22 C1 C2 Fe1 65.5(3) . . . . ? C22 C1 C2 C3 -29.6(4) . . . . ? C22 C1 C2 C6 159.8(3) . . . . ? C22 C1 C12 Fe2 -154.4(2) . . . . ? C22 C1 C12 C13 -62.8(3) . . . . ? C22 C1 C12 C16 112.5(3) . . . . ? C22 C23 C24 C25 -1.0(4) . . . . ? C22 C23 C24 C28 177.9(3) . . . . ? C23 C22 C27 C26 -0.6(4) . . . . ? C23 C24 C25 C26 0.2(4) . . . . ? C23 C24 C28 F1 -69.0(3) . . . . ? C23 C24 C28 F2 171.8(3) . . . . ? C23 C24 C28 F3 50.5(4) . . . . ? C24 C25 C26 C27 0.5(4) . . . . ? C24 C25 C26 C29 -179.9(3) . . . . ? C25 C24 C28 F1 109.9(3) . . . . ? C25 C24 C28 F2 -9.3(4) . . . . ? C25 C24 C28 F3 -130.5(3) . . . . ? C25 C26 C27 C22 -0.3(4) . . . . ? C25 C26 C29 F4 -119.6(3) . . . . ? C25 C26 C29 F5 122.9(3) . . . . ? C25 C26 C29 F6 0.5(4) . . . . ? C27 C22 C23 C24 1.2(4) . . . . ? C27 C26 C29 F4 60.0(4) . . . . ? C27 C26 C29 F5 -57.5(4) . . . . ? C27 C26 C29 F6 -179.9(3) . . . . ? C28 C24 C25 C26 -178.7(3) . . . . ? C29 C26 C27 C22 -179.9(2) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.500(15) 2 0.500(15)