#------------------------------------------------------------------------------ #$Date: 2021-10-29 02:40:48 +0300 (Fri, 29 Oct 2021) $ #$Revision: 270122 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708625.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_7708625 loop_ _publ_author_name 'Erb, William' 'Roisnel, Thierry' _publ_section_title ; The chemistry of ferrocenesulfonyl fluoride revealed ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03492H _journal_year 2021 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C13 H16 F Fe I O2 S Si' _chemical_formula_sum 'C13 H16 F Fe I O2 S Si' _chemical_formula_weight 466.16 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_update_record ; 2021-10-12 deposited with the CCDC. 2021-10-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.517(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.4866(5) _cell_length_b 16.5058(8) _cell_length_c 12.0171(6) _cell_measurement_reflns_used 5921 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30.3023 _cell_measurement_theta_min 2.4334 _cell_measurement_wavelength 0.710730 _cell_volume 1660.16(15) _computing_cell_refinement 'Bruker APEX2 (Bruker, 2014)' _computing_data_collection 'Bruker APEX2 (Bruker, 2014)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2014)' _computing_molecular_graphics ; 'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)' ; _computing_publication_material 'CRYSCALC (T. Roisnel, local program, 2020)' _computing_structure_refinement 'SHELXL-2018_3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018_2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.33 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.839 _diffrn_measurement_device_type 'APEXII Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_orient_matrix_UB_11 0.0879624 _diffrn_orient_matrix_UB_12 0.0028919 _diffrn_orient_matrix_UB_13 -0.0459031 _diffrn_orient_matrix_UB_21 -0.0807911 _diffrn_orient_matrix_UB_22 0.0007436 _diffrn_orient_matrix_UB_23 -0.0707312 _diffrn_orient_matrix_UB_31 -0.0032110 _diffrn_orient_matrix_UB_32 0.0605110 _diffrn_orient_matrix_UB_33 0.0030630 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_unetI/netI 0.0358 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11593 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.766 _diffrn_reflns_theta_min 2.468 _exptl_absorpt_coefficient_mu 2.973 _exptl_absorpt_correction_T_max 0.207 _exptl_absorpt_correction_T_min 0.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.865 _exptl_crystal_description prism _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.620 _exptl_crystal_size_mid 0.570 _exptl_crystal_size_min 0.530 _refine_diff_density_max 0.694 _refine_diff_density_min -1.403 _refine_diff_density_rms 0.132 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 184 _refine_ls_number_reflns 4356 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0313 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.9741P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.0723 _reflns_number_gt 3691 _reflns_number_total 4356 _reflns_threshold_expression >2sigma(I) _cod_data_source_file d1dt03492h2.cif _cod_data_source_block WE12671 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7708625 _shelx_res_file ; TITL WE12671 [Space group= P2(1)/n] job.res created by SHELXL-2018/3 at 14:54:49 on 11-Jan-2021 CELL 0.71073 8.4866 16.5058 12.0171 90.000 99.517 90.000 ZERR 4.00 0.0005 0.0008 0.0006 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H F FE I O S SI UNIT 52 64 4 4 4 8 4 4 MERG 2 OMIT -1 0 1 OMIT 2 0 0 FMAP 2 PLAN 20 SIZE 0.53 0.57 0.62 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.031200 0.974100 FVAR 0.33162 FE1 4 0.695942 0.808841 0.412593 11.00000 0.01300 0.01829 = 0.01102 -0.00191 0.00058 -0.00020 I1 5 0.301492 0.907734 0.316060 11.00000 0.02376 0.02662 = 0.03838 0.00100 0.00744 0.01114 S1 7 0.385342 0.699740 0.444300 11.00000 0.02036 0.03225 = 0.02036 0.00256 0.00800 -0.00355 SI1 8 0.715392 0.596682 0.331079 11.00000 0.01853 0.01687 = 0.02430 -0.00178 -0.00016 0.00221 C1 1 0.755160 0.797794 0.583541 11.00000 0.08274 0.05155 = 0.01305 0.00536 -0.01475 -0.04007 AFIX 43 H1 2 0.711116 0.759329 0.628570 11.00000 -1.20000 AFIX 0 C2 1 0.891468 0.787030 0.534567 11.00000 0.05248 0.04499 = 0.04210 -0.01582 -0.03248 0.01857 AFIX 43 H2 2 0.956481 0.739862 0.540777 11.00000 -1.20000 AFIX 0 C3 1 0.916239 0.856117 0.475694 11.00000 0.01968 0.07942 = 0.03182 -0.02405 0.00461 -0.01665 AFIX 43 H3 2 1.000964 0.864471 0.434248 11.00000 -1.20000 AFIX 0 C4 1 0.795884 0.912032 0.487014 11.00000 0.04974 0.02587 = 0.02705 -0.00299 -0.01049 -0.01371 AFIX 43 H4 2 0.784584 0.964798 0.455118 11.00000 -1.20000 AFIX 0 C5 1 0.694240 0.875559 0.554630 11.00000 0.02853 0.06310 = 0.02565 -0.03072 0.00475 -0.00832 AFIX 43 H5 2 0.601951 0.899200 0.576465 11.00000 -1.20000 AFIX 0 C6 1 0.700115 0.764479 0.251978 11.00000 0.01672 0.02023 = 0.01261 -0.00278 0.00377 -0.00036 AFIX 43 H6 2 0.790570 0.757220 0.215839 11.00000 -1.20000 AFIX 0 C7 1 0.607810 0.836361 0.247194 11.00000 0.02096 0.01713 = 0.01419 0.00044 0.00185 -0.00203 AFIX 43 H7 2 0.626116 0.884503 0.207924 11.00000 -1.20000 AFIX 0 C8 1 0.483622 0.824123 0.310979 11.00000 0.01399 0.01882 = 0.01526 -0.00303 -0.00016 0.00299 C9 1 0.501740 0.742814 0.355880 11.00000 0.01309 0.01974 = 0.01175 -0.00213 0.00263 -0.00087 C10 1 0.637944 0.704338 0.318905 11.00000 0.01443 0.01908 = 0.01524 -0.00440 0.00092 -0.00048 O11 6 0.313700 0.758559 0.505189 11.00000 0.04843 0.04884 = 0.04141 0.00345 0.03477 0.00621 F12 3 0.244715 0.665286 0.355943 11.00000 0.03139 0.08936 = 0.03928 0.00389 0.00245 -0.03477 O13 6 0.459997 0.630649 0.499102 11.00000 0.04524 0.03746 = 0.04113 0.01717 0.01817 0.00157 C14 1 0.545847 0.526856 0.276781 11.00000 0.02931 0.01979 = 0.03865 -0.00090 0.00118 -0.00412 AFIX 137 H14A 2 0.492038 0.545945 0.202982 11.00000 -1.50000 H14B 2 0.469607 0.526059 0.329763 11.00000 -1.50000 H14C 2 0.587260 0.472060 0.269213 11.00000 -1.50000 AFIX 0 C15 1 0.810161 0.567125 0.476019 11.00000 0.04715 0.03539 = 0.03652 0.00147 -0.01424 0.01323 AFIX 137 H15A 2 0.827973 0.508446 0.478949 11.00000 -1.50000 H15B 2 0.739782 0.582132 0.529629 11.00000 -1.50000 H15C 2 0.912692 0.595213 0.495890 11.00000 -1.50000 AFIX 0 C16 1 0.867442 0.592565 0.235370 11.00000 0.02970 0.02731 = 0.05102 -0.00871 0.01505 0.00439 AFIX 137 H16A 2 0.953269 0.631249 0.261328 11.00000 -1.50000 H16B 2 0.816904 0.606528 0.158451 11.00000 -1.50000 H16C 2 0.911993 0.537755 0.236077 11.00000 -1.50000 AFIX 0 HKLF 4 REM WE12671 [Space group= P2(1)/n] REM wR2 = 0.0723, GooF = S = 1.080, Restrained GooF = 1.080 for all data REM R1 = 0.0313 for 3691 Fo > 4sig(Fo) and 0.0404 for all 4356 data REM 184 parameters refined using 0 restraints END WGHT 0.0309 0.8968 REM Highest difference peak 0.694, deepest hole -1.403, 1-sigma level 0.132 Q1 1 0.3435 0.9117 0.3789 11.00000 0.05 0.69 Q2 1 0.2241 0.8893 0.3376 11.00000 0.05 0.64 Q3 1 0.2063 0.8407 0.3779 11.00000 0.05 0.41 Q4 1 0.4548 0.7234 0.4023 11.00000 0.05 0.39 Q5 1 0.7036 0.4649 0.1818 11.00000 0.05 0.39 Q6 1 0.3458 0.5588 0.2980 11.00000 0.05 0.39 Q7 1 0.6582 0.6530 0.3334 11.00000 0.05 0.38 Q8 1 0.7021 0.9241 0.6719 11.00000 0.05 0.38 Q9 1 0.7191 0.9527 0.7166 11.00000 0.05 0.37 Q10 1 0.4133 0.5504 0.2610 11.00000 0.05 0.37 Q11 1 0.2740 0.5539 0.2636 11.00000 0.05 0.36 Q12 1 0.7817 0.7952 0.6223 11.00000 0.05 0.36 Q13 1 0.3939 0.8231 0.5660 11.00000 0.05 0.36 Q14 1 0.8356 0.7717 0.1725 11.00000 0.05 0.36 Q15 1 0.1968 0.7814 0.5531 11.00000 0.05 0.36 Q16 1 0.2968 0.8153 0.5908 11.00000 0.05 0.35 Q17 1 1.0697 0.5902 0.2564 11.00000 0.05 0.35 Q18 1 0.3400 0.8386 0.5343 11.00000 0.05 0.34 Q19 1 0.7005 0.8293 0.5585 11.00000 0.05 0.34 Q20 1 0.7329 0.6239 0.0867 11.00000 0.05 0.34 ; _shelx_res_checksum 57766 loop_ _space_group_symop_operation_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' 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 0.69594(4) 0.80884(2) 0.41259(3) 0.01426(9) Uani 1 1 d . . . . . I1 I 0.30149(2) 0.90773(2) 0.31606(2) 0.02933(7) Uani 1 1 d . . . . . S1 S 0.38534(8) 0.69974(4) 0.44430(6) 0.02380(15) Uani 1 1 d . . . . . Si1 Si 0.71539(9) 0.59668(4) 0.33108(7) 0.02032(16) Uani 1 1 d . . . . . C1 C 0.7552(5) 0.7978(2) 0.5835(3) 0.0517(12) Uani 1 1 d . . . . . H1 H 0.711116 0.759329 0.628570 0.062 Uiso 1 1 calc R U . . . C2 C 0.8915(5) 0.7870(2) 0.5346(3) 0.0511(11) Uani 1 1 d . . . . . H2 H 0.956481 0.739862 0.540777 0.061 Uiso 1 1 calc R U . . . C3 C 0.9162(4) 0.8561(3) 0.4757(3) 0.0436(9) Uani 1 1 d . . . . . H3 H 1.000964 0.864471 0.434248 0.052 Uiso 1 1 calc R U . . . C4 C 0.7959(4) 0.91203(18) 0.4870(3) 0.0361(8) Uani 1 1 d . . . . . H4 H 0.784584 0.964798 0.455118 0.043 Uiso 1 1 calc R U . . . C5 C 0.6942(4) 0.8756(2) 0.5546(3) 0.0391(8) Uani 1 1 d . . . . . H5 H 0.601951 0.899200 0.576465 0.047 Uiso 1 1 calc R U . . . C6 C 0.7001(3) 0.76448(15) 0.2520(2) 0.0164(5) Uani 1 1 d . . . . . H6 H 0.790570 0.757220 0.215839 0.020 Uiso 1 1 calc R U . . . C7 C 0.6078(3) 0.83636(15) 0.2472(2) 0.0175(5) Uani 1 1 d . . . . . H7 H 0.626116 0.884503 0.207924 0.021 Uiso 1 1 calc R U . . . C8 C 0.4836(3) 0.82412(15) 0.3110(2) 0.0163(5) Uani 1 1 d . . . . . C9 C 0.5017(3) 0.74281(15) 0.3559(2) 0.0148(5) Uani 1 1 d . . . . . C10 C 0.6379(3) 0.70434(15) 0.3189(2) 0.0164(5) Uani 1 1 d . . . . . O11 O 0.3137(3) 0.75856(15) 0.5052(2) 0.0431(6) Uani 1 1 d . . . . . F12 F 0.2447(2) 0.66529(15) 0.35594(17) 0.0537(6) Uani 1 1 d . . . . . O13 O 0.4600(3) 0.63065(14) 0.4991(2) 0.0400(6) Uani 1 1 d . . . . . C14 C 0.5458(4) 0.52686(17) 0.2768(3) 0.0298(7) Uani 1 1 d . . . . . H14A H 0.492038 0.545945 0.202982 0.045 Uiso 1 1 calc R U . . . H14B H 0.469607 0.526059 0.329763 0.045 Uiso 1 1 calc R U . . . H14C H 0.587260 0.472060 0.269213 0.045 Uiso 1 1 calc R U . . . C15 C 0.8102(4) 0.5671(2) 0.4760(3) 0.0421(9) Uani 1 1 d . . . . . H15A H 0.827973 0.508446 0.478949 0.063 Uiso 1 1 calc R U . . . H15B H 0.739782 0.582132 0.529629 0.063 Uiso 1 1 calc R U . . . H15C H 0.912692 0.595213 0.495890 0.063 Uiso 1 1 calc R U . . . C16 C 0.8674(4) 0.59256(18) 0.2354(3) 0.0351(8) Uani 1 1 d . . . . . H16A H 0.953269 0.631249 0.261328 0.053 Uiso 1 1 calc R U . . . H16B H 0.816904 0.606528 0.158451 0.053 Uiso 1 1 calc R U . . . H16C H 0.911993 0.537755 0.236077 0.053 Uiso 1 1 calc R U . . . 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 0.01300(17) 0.01829(18) 0.01102(17) -0.00191(14) 0.00058(13) -0.00020(13) I1 0.02376(10) 0.02662(11) 0.03838(13) 0.00100(8) 0.00744(8) 0.01114(7) S1 0.0204(3) 0.0323(4) 0.0204(3) 0.0026(3) 0.0080(3) -0.0036(3) Si1 0.0185(4) 0.0169(3) 0.0243(4) -0.0018(3) -0.0002(3) 0.0022(3) C1 0.083(3) 0.052(2) 0.0131(15) 0.0054(15) -0.0147(17) -0.040(2) C2 0.052(2) 0.045(2) 0.042(2) -0.0158(18) -0.0325(18) 0.0186(18) C3 0.0197(15) 0.079(3) 0.0318(18) -0.0241(19) 0.0046(13) -0.0167(16) C4 0.050(2) 0.0259(15) 0.0270(17) -0.0030(13) -0.0105(14) -0.0137(14) C5 0.0285(16) 0.063(2) 0.0257(16) -0.0307(17) 0.0048(12) -0.0083(15) C6 0.0167(12) 0.0202(12) 0.0126(12) -0.0028(10) 0.0038(9) -0.0004(9) C7 0.0210(12) 0.0171(12) 0.0142(12) 0.0004(10) 0.0018(10) -0.0020(9) C8 0.0140(11) 0.0188(12) 0.0153(12) -0.0030(10) -0.0002(9) 0.0030(9) C9 0.0131(11) 0.0197(12) 0.0118(11) -0.0021(10) 0.0026(9) -0.0009(9) C10 0.0144(11) 0.0191(12) 0.0152(12) -0.0044(10) 0.0009(9) -0.0005(9) O11 0.0484(15) 0.0488(14) 0.0414(14) 0.0034(12) 0.0348(12) 0.0062(11) F12 0.0314(11) 0.0894(17) 0.0393(12) 0.0039(12) 0.0025(9) -0.0348(11) O13 0.0452(14) 0.0375(13) 0.0411(14) 0.0172(11) 0.0182(11) 0.0016(10) C14 0.0293(15) 0.0198(13) 0.0386(18) -0.0009(13) 0.0012(13) -0.0041(11) C15 0.047(2) 0.0354(17) 0.0365(19) 0.0015(16) -0.0142(16) 0.0132(15) C16 0.0297(16) 0.0273(15) 0.051(2) -0.0087(15) 0.0150(15) 0.0044(12) 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' I I -0.4742 1.8119 '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' Si Si 0.0817 0.0704 '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 C9 Fe1 C8 42.16(10) . . ? C9 Fe1 C5 117.48(12) . . ? C8 Fe1 C5 108.10(12) . . ? C9 Fe1 C1 110.27(13) . . ? C8 Fe1 C1 131.82(16) . . ? C5 Fe1 C1 40.37(16) . . ? C9 Fe1 C4 149.69(13) . . ? C8 Fe1 C4 115.17(12) . . ? C5 Fe1 C4 40.59(14) . . ? C1 Fe1 C4 67.56(14) . . ? C9 Fe1 C3 169.31(14) . . ? C8 Fe1 C3 147.54(14) . . ? C5 Fe1 C3 67.44(14) . . ? C1 Fe1 C3 66.69(15) . . ? C4 Fe1 C3 39.99(15) . . ? C9 Fe1 C7 69.09(10) . . ? C8 Fe1 C7 40.68(10) . . ? C5 Fe1 C7 129.80(13) . . ? C1 Fe1 C7 169.38(16) . . ? C4 Fe1 C7 107.31(12) . . ? C3 Fe1 C7 115.91(13) . . ? C9 Fe1 C2 132.08(14) . . ? C8 Fe1 C2 171.01(17) . . ? C5 Fe1 C2 67.25(15) . . ? C1 Fe1 C2 39.76(17) . . ? C4 Fe1 C2 66.80(14) . . ? C3 Fe1 C2 39.15(16) . . ? C7 Fe1 C2 148.19(16) . . ? C9 Fe1 C6 68.26(10) . . ? C8 Fe1 C6 68.37(10) . . ? C5 Fe1 C6 167.91(13) . . ? C1 Fe1 C6 150.19(15) . . ? C4 Fe1 C6 129.31(13) . . ? C3 Fe1 C6 108.91(12) . . ? C7 Fe1 C6 40.19(10) . . ? C2 Fe1 C6 117.81(14) . . ? C9 Fe1 C10 41.70(10) . . ? C8 Fe1 C10 70.58(10) . . ? C5 Fe1 C10 150.70(13) . . ? C1 Fe1 C10 117.97(13) . . ? C4 Fe1 C10 167.31(14) . . ? C3 Fe1 C10 129.55(13) . . ? C7 Fe1 C10 69.09(10) . . ? C2 Fe1 C10 109.42(12) . . ? C6 Fe1 C10 40.43(10) . . ? O11 S1 O13 120.76(15) . . ? O11 S1 F12 104.81(15) . . ? O13 S1 F12 104.80(14) . . ? O11 S1 C9 112.11(13) . . ? O13 S1 C9 111.25(13) . . ? F12 S1 C9 100.50(11) . . ? C15 Si1 C16 109.37(17) . . ? C15 Si1 C14 110.68(16) . . ? C16 Si1 C14 109.40(15) . . ? C15 Si1 C10 114.20(14) . . ? C16 Si1 C10 104.67(13) . . ? C14 Si1 C10 108.28(12) . . ? C2 C1 C5 108.0(3) . . ? C2 C1 Fe1 70.7(2) . . ? C5 C1 Fe1 69.53(18) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Fe1 C1 H1 125.3 . . ? C3 C2 C1 108.6(3) . . ? C3 C2 Fe1 70.26(18) . . ? C1 C2 Fe1 69.53(19) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Fe1 C2 H2 126.1 . . ? C2 C3 C4 108.7(3) . . ? C2 C3 Fe1 70.59(19) . . ? C4 C3 Fe1 69.62(17) . . ? C2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? Fe1 C3 H3 125.7 . . ? C3 C4 C5 107.4(3) . . ? C3 C4 Fe1 70.39(18) . . ? C5 C4 Fe1 69.38(17) . . ? C3 C4 H4 126.3 . . ? C5 C4 H4 126.3 . . ? Fe1 C4 H4 125.5 . . ? C1 C5 C4 107.2(3) . . ? C1 C5 Fe1 70.10(19) . . ? C4 C5 Fe1 70.03(17) . . ? C1 C5 H5 126.4 . . ? C4 C5 H5 126.4 . . ? Fe1 C5 H5 125.1 . . ? C7 C6 C10 110.5(2) . . ? C7 C6 Fe1 69.35(14) . . ? C10 C6 Fe1 69.93(14) . . ? C7 C6 H6 124.7 . . ? C10 C6 H6 124.7 . . ? Fe1 C6 H6 127.6 . . ? C6 C7 C8 108.3(2) . . ? C6 C7 Fe1 70.46(14) . . ? C8 C7 Fe1 68.26(14) . . ? C6 C7 H7 125.8 . . ? C8 C7 H7 125.8 . . ? Fe1 C7 H7 127.0 . . ? C7 C8 C9 107.0(2) . . ? C7 C8 Fe1 71.07(14) . . ? C9 C8 Fe1 68.21(13) . . ? C7 C8 I1 122.97(18) . . ? C9 C8 I1 129.70(19) . . ? Fe1 C8 I1 131.18(12) . . ? C8 C9 C10 109.5(2) . . ? C8 C9 S1 125.3(2) . . ? C10 C9 S1 125.18(19) . . ? C8 C9 Fe1 69.63(14) . . ? C10 C9 Fe1 71.91(13) . . ? S1 C9 Fe1 122.69(13) . . ? C6 C10 C9 104.8(2) . . ? C6 C10 Si1 122.61(19) . . ? C9 C10 Si1 132.17(19) . . ? C6 C10 Fe1 69.63(14) . . ? C9 C10 Fe1 66.39(13) . . ? Si1 C10 Fe1 133.70(13) . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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 C9 1.999(2) . ? Fe1 C8 2.018(2) . ? Fe1 C5 2.033(3) . ? Fe1 C1 2.041(3) . ? Fe1 C4 2.042(3) . ? Fe1 C3 2.052(3) . ? Fe1 C7 2.055(3) . ? Fe1 C2 2.056(3) . ? Fe1 C6 2.070(3) . ? Fe1 C10 2.074(2) . ? I1 C8 2.081(2) . ? S1 O11 1.412(2) . ? S1 O13 1.413(2) . ? S1 F12 1.5672(19) . ? S1 C9 1.720(3) . ? Si1 C15 1.859(3) . ? Si1 C16 1.866(4) . ? Si1 C14 1.875(3) . ? Si1 C10 1.892(3) . ? C1 C2 1.393(6) . ? C1 C5 1.406(6) . ? C1 H1 0.9500 . ? C2 C3 1.376(6) . ? C2 H2 0.9500 . ? C3 C4 1.400(5) . ? C3 H3 0.9500 . ? C4 C5 1.414(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.418(3) . ? C6 C10 1.432(4) . ? C6 H6 0.9500 . ? C7 C8 1.416(4) . ? C7 H7 0.9500 . ? C8 C9 1.445(3) . ? C9 C10 1.451(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 C5 C1 C2 C3 -0.2(4) . . . . ? Fe1 C1 C2 C3 59.6(2) . . . . ? C5 C1 C2 Fe1 -59.8(2) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? Fe1 C2 C3 C4 59.4(2) . . . . ? C1 C2 C3 Fe1 -59.1(2) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? Fe1 C3 C4 C5 59.8(2) . . . . ? C2 C3 C4 Fe1 -60.0(2) . . . . ? C2 C1 C5 C4 0.0(3) . . . . ? Fe1 C1 C5 C4 -60.5(2) . . . . ? C2 C1 C5 Fe1 60.5(2) . . . . ? C3 C4 C5 C1 0.1(3) . . . . ? Fe1 C4 C5 C1 60.5(2) . . . . ? C3 C4 C5 Fe1 -60.4(2) . . . . ? C10 C6 C7 C8 -0.1(3) . . . . ? Fe1 C6 C7 C8 -57.89(17) . . . . ? C10 C6 C7 Fe1 57.82(17) . . . . ? C6 C7 C8 C9 0.2(3) . . . . ? Fe1 C7 C8 C9 -59.01(16) . . . . ? C6 C7 C8 Fe1 59.25(17) . . . . ? C6 C7 C8 I1 -173.37(16) . . . . ? Fe1 C7 C8 I1 127.38(17) . . . . ? C7 C8 C9 C10 -0.3(3) . . . . ? Fe1 C8 C9 C10 -61.16(16) . . . . ? I1 C8 C9 C10 172.71(17) . . . . ? C7 C8 C9 S1 177.13(18) . . . . ? Fe1 C8 C9 S1 116.29(19) . . . . ? I1 C8 C9 S1 -9.8(3) . . . . ? C7 C8 C9 Fe1 60.84(16) . . . . ? I1 C8 C9 Fe1 -126.1(2) . . . . ? O11 S1 C9 C8 -24.0(3) . . . . ? O13 S1 C9 C8 -162.6(2) . . . . ? F12 S1 C9 C8 86.9(2) . . . . ? O11 S1 C9 C10 153.1(2) . . . . ? O13 S1 C9 C10 14.5(3) . . . . ? F12 S1 C9 C10 -96.0(2) . . . . ? O11 S1 C9 Fe1 63.0(2) . . . . ? O13 S1 C9 Fe1 -75.57(19) . . . . ? F12 S1 C9 Fe1 173.90(16) . . . . ? C7 C6 C10 C9 -0.1(3) . . . . ? Fe1 C6 C10 C9 57.35(15) . . . . ? C7 C6 C10 Si1 172.93(17) . . . . ? Fe1 C6 C10 Si1 -129.60(17) . . . . ? C7 C6 C10 Fe1 -57.48(17) . . . . ? C8 C9 C10 C6 0.3(3) . . . . ? S1 C9 C10 C6 -177.18(18) . . . . ? Fe1 C9 C10 C6 -59.48(16) . . . . ? C8 C9 C10 Si1 -171.83(19) . . . . ? S1 C9 C10 Si1 10.7(3) . . . . ? Fe1 C9 C10 Si1 128.4(2) . . . . ? C8 C9 C10 Fe1 59.75(16) . . . . ? S1 C9 C10 Fe1 -117.71(19) . . . . ? C15 Si1 C10 C6 116.7(2) . . . . ? C16 Si1 C10 C6 -2.9(2) . . . . ? C14 Si1 C10 C6 -119.6(2) . . . . ? C15 Si1 C10 C9 -72.4(3) . . . . ? C16 Si1 C10 C9 168.0(2) . . . . ? C14 Si1 C10 C9 51.4(3) . . . . ? C15 Si1 C10 Fe1 24.4(3) . . . . ? C16 Si1 C10 Fe1 -95.2(2) . . . . ? C14 Si1 C10 Fe1 148.16(19) . . . . ?