#------------------------------------------------------------------------------ #$Date: 2021-10-29 02:40:48 +0300 (Fri, 29 Oct 2021) $ #$Revision: 270122 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708622.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_7708622 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 H17 F Fe O2 S Si' _chemical_formula_sum 'C13 H17 F Fe O2 S Si' _chemical_formula_weight 340.26 _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 110.418(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.0861(5) _cell_length_b 13.3795(6) _cell_length_c 12.8394(7) _cell_measurement_reflns_used 2537 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.1983 _cell_measurement_theta_min 2.8355 _cell_measurement_wavelength 0.710730 _cell_volume 1462.79(13) _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 0.999 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'APEXII Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_orient_matrix_UB_11 0.0536813 _diffrn_orient_matrix_UB_12 0.0309878 _diffrn_orient_matrix_UB_13 -0.0480320 _diffrn_orient_matrix_UB_21 0.1034913 _diffrn_orient_matrix_UB_22 -0.0068458 _diffrn_orient_matrix_UB_23 0.0616650 _diffrn_orient_matrix_UB_31 0.0141124 _diffrn_orient_matrix_UB_32 -0.0676696 _diffrn_orient_matrix_UB_33 -0.0282336 _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 0.0447 _diffrn_reflns_av_unetI/netI 0.0538 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 9844 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.490 _diffrn_reflns_theta_min 2.835 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_T_max 0.797 _exptl_absorpt_correction_T_min 0.723 _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 1.545 _exptl_crystal_description prism _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.374 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.083 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 175 _refine_ls_number_reflns 3333 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0372 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.0716P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.0887 _reflns_number_gt 2688 _reflns_number_total 3333 _reflns_threshold_expression >2sigma(I) _cod_data_source_file d1dt03492h2.cif _cod_data_source_block WE12631 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7708622 _shelx_res_file ; TITL WE12631 [Space group= P2(1)/n] job.res created by SHELXL-2018/3 at 15:27:59 on 11-Jan-2021 CELL 0.71073 9.0861 13.3795 12.8394 90.000 110.418 90.000 ZERR 4.00 0.0005 0.0006 0.0007 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H F FE O S SI UNIT 52 68 4 4 8 4 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.18 0.26 0.40 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.040200 0.071600 FVAR 0.50857 FE1 4 0.547243 0.348955 0.233574 11.00000 0.01605 0.01510 = 0.01633 0.00181 0.00605 0.00074 S1 6 0.476976 0.108567 0.210822 11.00000 0.02840 0.01713 = 0.02927 -0.00167 0.00899 0.00168 SI1 7 0.357972 0.262894 0.417930 11.00000 0.01780 0.02385 = 0.01773 0.00123 0.00694 -0.00138 C1 1 0.485373 0.371059 0.066593 11.00000 0.04122 0.03144 = 0.01686 0.00377 0.00819 0.00492 AFIX 43 H1 2 0.511464 0.328524 0.016373 11.00000 -1.20000 AFIX 0 C2 1 0.575644 0.451903 0.124986 11.00000 0.03243 0.02908 = 0.02901 0.01464 0.01243 -0.00046 AFIX 43 H2 2 0.673294 0.473620 0.121375 11.00000 -1.20000 AFIX 0 C3 1 0.494888 0.495020 0.190017 11.00000 0.04848 0.01703 = 0.02684 0.00510 0.00703 0.00422 AFIX 43 H3 2 0.528622 0.551078 0.237864 11.00000 -1.20000 AFIX 0 C4 1 0.355245 0.440190 0.171432 11.00000 0.03166 0.03459 = 0.03625 0.01875 0.01715 0.01911 AFIX 43 H4 2 0.278638 0.452791 0.204682 11.00000 -1.20000 AFIX 0 C5 1 0.349528 0.363913 0.095312 11.00000 0.02395 0.02817 = 0.03017 0.00988 -0.00273 -0.00109 AFIX 43 H5 2 0.268261 0.315787 0.067860 11.00000 -1.20000 AFIX 0 C6 1 0.649246 0.342574 0.403589 11.00000 0.02043 0.02270 = 0.01686 0.00009 0.00190 -0.00160 AFIX 43 H6 2 0.652979 0.393989 0.455481 11.00000 -1.20000 AFIX 0 C7 1 0.765000 0.327258 0.354270 11.00000 0.01458 0.02860 = 0.02927 0.00565 0.00365 -0.00189 AFIX 43 H7 2 0.856823 0.366484 0.367185 11.00000 -1.20000 AFIX 0 C8 1 0.720624 0.243974 0.282873 11.00000 0.01495 0.02541 = 0.03139 0.00595 0.00923 0.00568 AFIX 43 H8 2 0.776300 0.216785 0.239100 11.00000 -1.20000 AFIX 0 C9 1 0.574866 0.208174 0.289131 11.00000 0.01761 0.01367 = 0.02007 0.00340 0.00544 0.00240 C10 1 0.525991 0.270129 0.364659 11.00000 0.01714 0.01795 = 0.01530 0.00345 0.00263 0.00062 O11 5 0.535578 0.086726 0.124718 11.00000 0.06180 0.04138 = 0.05183 -0.02317 0.03614 -0.00980 F12 3 0.538438 0.021189 0.296915 11.00000 0.04818 0.01741 = 0.06049 0.01269 0.00420 0.00369 O13 5 0.313685 0.110055 0.190013 11.00000 0.02691 0.02730 = 0.03879 -0.00603 0.00713 -0.00334 C14 1 0.383236 0.145872 0.501062 11.00000 0.02911 0.03983 = 0.03288 0.01106 0.01046 -0.00581 AFIX 137 H14A 2 0.490219 0.143105 0.555462 11.00000 -1.50000 H14B 2 0.365099 0.087928 0.451470 11.00000 -1.50000 H14C 2 0.307676 0.145041 0.539974 11.00000 -1.50000 AFIX 0 C15 1 0.158798 0.266524 0.308230 11.00000 0.01744 0.03576 = 0.03032 0.00266 0.00790 -0.00027 AFIX 137 H15A 2 0.152998 0.216828 0.250859 11.00000 -1.50000 H15B 2 0.139463 0.333243 0.274689 11.00000 -1.50000 H15C 2 0.079341 0.251407 0.341536 11.00000 -1.50000 AFIX 0 C16 1 0.376954 0.374888 0.508397 11.00000 0.03784 0.03987 = 0.03329 -0.01147 0.01960 -0.00462 AFIX 137 H16A 2 0.293132 0.374171 0.539999 11.00000 -1.50000 H16B 2 0.368454 0.435668 0.464077 11.00000 -1.50000 H16C 2 0.479241 0.373623 0.568609 11.00000 -1.50000 AFIX 0 HKLF 4 REM WE12631 [Space group= P2(1)/n] REM wR2 = 0.0887, GooF = S = 1.014, Restrained GooF = 1.014 for all data REM R1 = 0.0372 for 2688 Fo > 4sig(Fo) and 0.0508 for all 3333 data REM 175 parameters refined using 0 restraints END WGHT 0.0384 0.0538 REM Highest difference peak 0.374, deepest hole -0.382, 1-sigma level 0.083 Q1 1 0.4400 0.2697 0.3830 11.00000 0.05 0.37 Q2 1 0.2638 0.2659 0.3596 11.00000 0.05 0.34 Q3 1 0.2936 0.0930 0.4772 11.00000 0.05 0.32 Q4 1 0.2956 0.1097 0.2447 11.00000 0.05 0.30 Q5 1 0.9142 0.2645 0.2039 11.00000 0.05 0.30 Q6 1 0.1592 0.3818 0.1310 11.00000 0.05 0.29 Q7 1 0.3337 0.3508 0.6573 11.00000 0.05 0.29 Q8 1 0.5900 0.2489 -0.0023 11.00000 0.05 0.29 Q9 1 0.5516 0.2335 0.3459 11.00000 0.05 0.28 Q10 1 0.6868 0.4686 0.0820 11.00000 0.05 0.28 Q11 1 0.5369 0.1602 0.2582 11.00000 0.05 0.27 Q12 1 0.5965 0.2941 0.4028 11.00000 0.05 0.27 Q13 1 0.7798 0.2650 0.3248 11.00000 0.05 0.27 Q14 1 0.5461 0.0630 0.3531 11.00000 0.05 0.27 Q15 1 0.3799 0.1034 0.2057 11.00000 0.05 0.26 Q16 1 0.2735 0.5812 0.2017 11.00000 0.05 0.26 Q17 1 0.1028 0.2870 0.3160 11.00000 0.05 0.26 Q18 1 0.1284 0.2860 0.2392 11.00000 0.05 0.26 Q19 1 0.2198 0.4237 0.4338 11.00000 0.05 0.26 Q20 1 0.4266 0.1164 0.4800 11.00000 0.05 0.26 ; _shelx_res_checksum 13217 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 0.54724(4) 0.34895(2) 0.23357(3) 0.01572(11) Uani 1 1 d . . . . . S1 S 0.47698(7) 0.10857(4) 0.21082(6) 0.02522(16) Uani 1 1 d . . . . . Si1 Si 0.35797(8) 0.26289(5) 0.41793(6) 0.01960(16) Uani 1 1 d . . . . . C1 C 0.4854(3) 0.37106(19) 0.0666(2) 0.0304(6) Uani 1 1 d . . . . . H1 H 0.511464 0.328524 0.016373 0.036 Uiso 1 1 calc R U . . . C2 C 0.5756(3) 0.45190(18) 0.1250(2) 0.0297(6) Uani 1 1 d . . . . . H2 H 0.673294 0.473620 0.121375 0.036 Uiso 1 1 calc R U . . . C3 C 0.4949(3) 0.49502(18) 0.1900(2) 0.0324(7) Uani 1 1 d . . . . . H3 H 0.528622 0.551078 0.237864 0.039 Uiso 1 1 calc R U . . . C4 C 0.3552(3) 0.44019(19) 0.1714(2) 0.0328(7) Uani 1 1 d . . . . . H4 H 0.278638 0.452791 0.204682 0.039 Uiso 1 1 calc R U . . . C5 C 0.3495(3) 0.36391(18) 0.0953(2) 0.0306(6) Uani 1 1 d . . . . . H5 H 0.268261 0.315787 0.067860 0.037 Uiso 1 1 calc R U . . . C6 C 0.6492(3) 0.34257(17) 0.4036(2) 0.0212(5) Uani 1 1 d . . . . . H6 H 0.652979 0.393989 0.455481 0.025 Uiso 1 1 calc R U . . . C7 C 0.7650(3) 0.32726(19) 0.3543(2) 0.0252(6) Uani 1 1 d . . . . . H7 H 0.856823 0.366484 0.367185 0.030 Uiso 1 1 calc R U . . . C8 C 0.7206(3) 0.24397(17) 0.2829(2) 0.0236(6) Uani 1 1 d . . . . . H8 H 0.776300 0.216785 0.239100 0.028 Uiso 1 1 calc R U . . . C9 C 0.5749(3) 0.20817(16) 0.28913(19) 0.0174(5) Uani 1 1 d . . . . . C10 C 0.5260(3) 0.27013(16) 0.36466(19) 0.0176(5) Uani 1 1 d . . . . . O11 O 0.5356(2) 0.08673(14) 0.12472(18) 0.0474(6) Uani 1 1 d . . . . . F12 F 0.53844(19) 0.02119(10) 0.29692(14) 0.0459(5) Uani 1 1 d . . . . . O13 O 0.3137(2) 0.11005(13) 0.19001(16) 0.0321(4) Uani 1 1 d . . . . . C14 C 0.3832(3) 0.14587(19) 0.5011(2) 0.0340(7) Uani 1 1 d . . . . . H14A H 0.490219 0.143105 0.555462 0.051 Uiso 1 1 calc R U . . . H14B H 0.365099 0.087928 0.451470 0.051 Uiso 1 1 calc R U . . . H14C H 0.307676 0.145041 0.539974 0.051 Uiso 1 1 calc R U . . . C15 C 0.1588(3) 0.26652(19) 0.3082(2) 0.0280(6) Uani 1 1 d . . . . . H15A H 0.152998 0.216828 0.250859 0.042 Uiso 1 1 calc R U . . . H15B H 0.139463 0.333243 0.274689 0.042 Uiso 1 1 calc R U . . . H15C H 0.079341 0.251407 0.341536 0.042 Uiso 1 1 calc R U . . . C16 C 0.3770(3) 0.3749(2) 0.5084(2) 0.0351(7) Uani 1 1 d . . . . . H16A H 0.293132 0.374171 0.539999 0.053 Uiso 1 1 calc R U . . . H16B H 0.368454 0.435668 0.464077 0.053 Uiso 1 1 calc R U . . . H16C H 0.479241 0.373623 0.568609 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 0.01605(18) 0.01510(19) 0.01633(19) 0.00181(13) 0.00605(14) 0.00074(12) S1 0.0284(4) 0.0171(3) 0.0293(4) -0.0017(3) 0.0090(3) 0.0017(3) Si1 0.0178(3) 0.0239(4) 0.0177(3) 0.0012(3) 0.0069(3) -0.0014(3) C1 0.0412(17) 0.0314(14) 0.0169(13) 0.0038(11) 0.0082(12) 0.0049(12) C2 0.0324(15) 0.0291(14) 0.0290(15) 0.0146(12) 0.0124(12) -0.0005(11) C3 0.0485(18) 0.0170(13) 0.0268(15) 0.0051(11) 0.0070(13) 0.0042(12) C4 0.0317(15) 0.0346(15) 0.0362(16) 0.0188(13) 0.0171(13) 0.0191(12) C5 0.0239(14) 0.0282(14) 0.0302(15) 0.0099(12) -0.0027(12) -0.0011(11) C6 0.0204(12) 0.0227(12) 0.0169(12) 0.0001(10) 0.0019(10) -0.0016(10) C7 0.0146(12) 0.0286(13) 0.0293(14) 0.0057(11) 0.0036(11) -0.0019(10) C8 0.0150(11) 0.0254(13) 0.0314(15) 0.0059(11) 0.0092(11) 0.0057(10) C9 0.0176(11) 0.0137(11) 0.0201(12) 0.0034(9) 0.0054(10) 0.0024(9) C10 0.0171(11) 0.0180(11) 0.0153(12) 0.0035(10) 0.0026(9) 0.0006(9) O11 0.0618(14) 0.0414(12) 0.0518(14) -0.0232(11) 0.0361(12) -0.0098(10) F12 0.0482(10) 0.0174(8) 0.0605(12) 0.0127(8) 0.0042(9) 0.0037(7) O13 0.0269(10) 0.0273(9) 0.0388(12) -0.0060(8) 0.0071(9) -0.0033(8) C14 0.0291(15) 0.0398(16) 0.0329(16) 0.0111(13) 0.0105(13) -0.0058(12) C15 0.0174(12) 0.0358(14) 0.0303(15) 0.0027(12) 0.0079(11) -0.0003(11) C16 0.0378(16) 0.0399(16) 0.0333(16) -0.0115(13) 0.0196(14) -0.0046(13) 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' 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 C1 117.78(10) . . ? C9 Fe1 C8 41.67(9) . . ? C1 Fe1 C8 109.02(11) . . ? C9 Fe1 C2 148.26(10) . . ? C1 Fe1 C2 40.32(10) . . ? C8 Fe1 C2 114.15(10) . . ? C9 Fe1 C3 170.96(10) . . ? C1 Fe1 C3 67.73(11) . . ? C8 Fe1 C3 145.56(10) . . ? C2 Fe1 C3 40.50(10) . . ? C9 Fe1 C5 111.37(10) . . ? C1 Fe1 C5 40.34(10) . . ? C8 Fe1 C5 133.27(11) . . ? C2 Fe1 C5 67.87(10) . . ? C3 Fe1 C5 67.61(10) . . ? C9 Fe1 C10 42.17(9) . . ? C1 Fe1 C10 150.07(10) . . ? C8 Fe1 C10 71.03(9) . . ? C2 Fe1 C10 168.14(10) . . ? C3 Fe1 C10 129.56(10) . . ? C5 Fe1 C10 117.14(10) . . ? C9 Fe1 C6 68.14(9) . . ? C1 Fe1 C6 168.49(10) . . ? C8 Fe1 C6 68.18(10) . . ? C2 Fe1 C6 129.55(10) . . ? C3 Fe1 C6 107.84(10) . . ? C5 Fe1 C6 149.25(11) . . ? C10 Fe1 C6 40.85(8) . . ? C9 Fe1 C4 133.17(10) . . ? C1 Fe1 C4 67.62(11) . . ? C8 Fe1 C4 172.58(11) . . ? C2 Fe1 C4 67.98(10) . . ? C3 Fe1 C4 40.37(10) . . ? C5 Fe1 C4 40.01(10) . . ? C10 Fe1 C4 108.34(10) . . ? C6 Fe1 C4 116.47(10) . . ? C9 Fe1 C7 68.37(9) . . ? C1 Fe1 C7 130.55(10) . . ? C8 Fe1 C7 40.17(10) . . ? C2 Fe1 C7 106.95(10) . . ? C3 Fe1 C7 114.25(11) . . ? C5 Fe1 C7 170.31(10) . . ? C10 Fe1 C7 69.62(9) . . ? C6 Fe1 C7 40.31(9) . . ? C4 Fe1 C7 147.03(11) . . ? O13 S1 O11 120.78(13) . . ? O13 S1 F12 103.62(11) . . ? O11 S1 F12 104.93(11) . . ? O13 S1 C9 113.24(11) . . ? O11 S1 C9 110.99(12) . . ? F12 S1 C9 100.43(10) . . ? C14 Si1 C15 110.33(12) . . ? C14 Si1 C16 110.60(13) . . ? C15 Si1 C16 107.67(13) . . ? C14 Si1 C10 107.35(11) . . ? C15 Si1 C10 114.88(11) . . ? C16 Si1 C10 105.93(11) . . ? C2 C1 C5 108.3(2) . . ? C2 C1 Fe1 69.84(14) . . ? C5 C1 Fe1 70.15(15) . . ? C2 C1 H1 125.8 . . ? C5 C1 H1 125.8 . . ? Fe1 C1 H1 125.7 . . ? C1 C2 C3 107.6(2) . . ? C1 C2 Fe1 69.84(14) . . ? C3 C2 Fe1 69.88(14) . . ? C1 C2 H2 126.2 . . ? C3 C2 H2 126.2 . . ? Fe1 C2 H2 125.7 . . ? C2 C3 C4 108.0(2) . . ? C2 C3 Fe1 69.62(14) . . ? C4 C3 Fe1 70.06(14) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? Fe1 C3 H3 125.9 . . ? C5 C4 C3 108.0(2) . . ? C5 C4 Fe1 69.95(14) . . ? C3 C4 Fe1 69.57(14) . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Fe1 C4 H4 126.0 . . ? C4 C5 C1 108.1(2) . . ? C4 C5 Fe1 70.05(15) . . ? C1 C5 Fe1 69.51(14) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe1 C5 H5 126.1 . . ? C7 C6 C10 110.9(2) . . ? C7 C6 Fe1 70.23(14) . . ? C10 C6 Fe1 69.48(13) . . ? C7 C6 H6 124.5 . . ? C10 C6 H6 124.5 . . ? Fe1 C6 H6 127.4 . . ? C8 C7 C6 108.4(2) . . ? C8 C7 Fe1 68.97(13) . . ? C6 C7 Fe1 69.46(13) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? Fe1 C7 H7 127.4 . . ? C7 C8 C9 106.7(2) . . ? C7 C8 Fe1 70.86(14) . . ? C9 C8 Fe1 67.65(12) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? Fe1 C8 H8 126.4 . . ? C8 C9 C10 110.4(2) . . ? C8 C9 S1 121.65(18) . . ? C10 C9 S1 127.91(17) . . ? C8 C9 Fe1 70.69(13) . . ? C10 C9 Fe1 70.86(12) . . ? S1 C9 Fe1 123.16(13) . . ? C6 C10 C9 103.6(2) . . ? C6 C10 Si1 122.88(17) . . ? C9 C10 Si1 133.39(17) . . ? C6 C10 Fe1 69.67(13) . . ? C9 C10 Fe1 66.98(13) . . ? Si1 C10 Fe1 130.21(12) . . ? 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 C1 2.039(3) . ? Fe1 C8 2.039(2) . ? Fe1 C2 2.039(2) . ? Fe1 C3 2.043(2) . ? Fe1 C5 2.048(3) . ? Fe1 C10 2.052(2) . ? Fe1 C6 2.054(2) . ? Fe1 C4 2.049(2) . ? Fe1 C7 2.064(2) . ? S1 O13 1.4130(18) . ? S1 O11 1.415(2) . ? S1 F12 1.5716(16) . ? S1 C9 1.719(2) . ? Si1 C14 1.863(2) . ? Si1 C15 1.866(3) . ? Si1 C16 1.867(3) . ? Si1 C10 1.881(2) . ? C1 C2 1.406(4) . ? C1 C5 1.409(4) . ? C1 H1 0.9500 . ? C2 C3 1.413(4) . ? C2 H2 0.9500 . ? C3 C4 1.412(4) . ? C3 H3 0.9500 . ? C4 C5 1.401(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.419(3) . ? C6 C10 1.433(3) . ? C6 H6 0.9500 . ? C7 C8 1.409(3) . ? C7 H7 0.9500 . ? C8 C9 1.437(3) . ? C8 H8 0.9500 . ? C9 C10 1.458(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 -0.1(3) . . . . ? Fe1 C1 C2 C3 -59.93(17) . . . . ? C5 C1 C2 Fe1 59.84(17) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? Fe1 C2 C3 C4 -59.77(18) . . . . ? C1 C2 C3 Fe1 59.91(17) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? Fe1 C3 C4 C5 -59.63(17) . . . . ? C2 C3 C4 Fe1 59.50(18) . . . . ? C3 C4 C5 C1 0.1(3) . . . . ? Fe1 C4 C5 C1 -59.32(17) . . . . ? C3 C4 C5 Fe1 59.39(17) . . . . ? C2 C1 C5 C4 0.0(3) . . . . ? Fe1 C1 C5 C4 59.65(17) . . . . ? C2 C1 C5 Fe1 -59.65(17) . . . . ? C10 C6 C7 C8 -0.5(3) . . . . ? Fe1 C6 C7 C8 -58.08(17) . . . . ? C10 C6 C7 Fe1 57.56(16) . . . . ? C6 C7 C8 C9 0.0(3) . . . . ? Fe1 C7 C8 C9 -58.37(15) . . . . ? C6 C7 C8 Fe1 58.39(17) . . . . ? C7 C8 C9 C10 0.5(3) . . . . ? Fe1 C8 C9 C10 -59.94(16) . . . . ? C7 C8 C9 S1 178.13(17) . . . . ? Fe1 C8 C9 S1 117.70(17) . . . . ? C7 C8 C9 Fe1 60.43(16) . . . . ? O13 S1 C9 C8 -154.38(18) . . . . ? O11 S1 C9 C8 -14.8(2) . . . . ? F12 S1 C9 C8 95.8(2) . . . . ? O13 S1 C9 C10 22.8(2) . . . . ? O11 S1 C9 C10 162.4(2) . . . . ? F12 S1 C9 C10 -87.0(2) . . . . ? O13 S1 C9 Fe1 -67.89(17) . . . . ? O11 S1 C9 Fe1 71.69(17) . . . . ? F12 S1 C9 Fe1 -177.75(13) . . . . ? C7 C6 C10 C9 0.8(3) . . . . ? Fe1 C6 C10 C9 58.78(14) . . . . ? C7 C6 C10 Si1 176.54(16) . . . . ? Fe1 C6 C10 Si1 -125.47(16) . . . . ? C7 C6 C10 Fe1 -57.99(17) . . . . ? C8 C9 C10 C6 -0.8(2) . . . . ? S1 C9 C10 C6 -178.23(17) . . . . ? Fe1 C9 C10 C6 -60.62(15) . . . . ? C8 C9 C10 Si1 -175.86(18) . . . . ? S1 C9 C10 Si1 6.7(3) . . . . ? Fe1 C9 C10 Si1 124.3(2) . . . . ? C8 C9 C10 Fe1 59.84(16) . . . . ? S1 C9 C10 Fe1 -117.62(19) . . . . ? C14 Si1 C10 C6 -110.6(2) . . . . ? C15 Si1 C10 C6 126.34(19) . . . . ? C16 Si1 C10 C6 7.6(2) . . . . ? C14 Si1 C10 C9 63.7(2) . . . . ? C15 Si1 C10 C9 -59.4(3) . . . . ? C16 Si1 C10 C9 -178.1(2) . . . . ? C14 Si1 C10 Fe1 159.16(15) . . . . ? C15 Si1 C10 Fe1 36.06(19) . . . . ? C16 Si1 C10 Fe1 -82.64(17) . . . . ?