# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Fe(Me2SiC6H4SiMe2)(MeSi(H) #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C22 H32 Fe O2 Si4' _chemical_formula_moiety 'C22 H32 Fe O2 Si4' _chemical_formula_weight 496.68 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 1/2+X,1/2-Y,+Z 4 -X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 17.122(3) _cell_length_b 16.141(2) _cell_length_c 9.4508(12) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2611.9(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6814 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 27.47 _cell_measurement_temperature 123 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048.00 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.977 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 123 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 20986 _diffrn_reflns_av_R_equivalents 0.1369 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5780 _reflns_number_gt 5362 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1434 _refine_ls_number_restraints 1 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5780 _refine_ls_number_parameters 262 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0667P)^2^+1.7618P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.780 _refine_diff_density_min -0.690 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2613 Friedel Pairs' _refine_ls_abs_structure_Flack -0.03(3) 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.3463 0.8444 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.0817 0.0704 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.75557(3) 0.96929(3) 0.38970(7) 0.01765(13) Uani 1.0 4 d . . . Si1 Si 0.81740(6) 0.87067(6) 0.54196(11) 0.0228(3) Uani 1.0 4 d . . . Si2 Si 0.88121(6) 0.98314(7) 0.27388(11) 0.0244(3) Uani 1.0 4 d . . . Si3 Si 0.64484(6) 1.00156(7) 0.24194(12) 0.0241(3) Uani 1.0 4 d . . . Si4 Si 0.73414(6) 1.10301(6) 0.49963(11) 0.0202(2) Uani 1.0 4 d . . . O1 O 0.63024(17) 0.93012(19) 0.5877(4) 0.0354(7) Uani 1.0 4 d . . . O2 O 0.7564(2) 0.8249(3) 0.2045(4) 0.0413(9) Uani 1.0 4 d . . . C1 C 0.6794(2) 0.9468(3) 0.5090(5) 0.0246(8) Uani 1.0 4 d . . . C2 C 0.7569(2) 0.8833(3) 0.2753(5) 0.0268(9) Uani 1.0 4 d . . . C3 C 0.9161(3) 0.8501(3) 0.4624(5) 0.0252(8) Uani 1.0 4 d . . . C4 C 0.9638(3) 0.7873(3) 0.5187(5) 0.0359(10) Uani 1.0 4 d . . . C5 C 1.0366(3) 0.7708(3) 0.4613(6) 0.0397(11) Uani 1.0 4 d . . . C6 C 1.0619(3) 0.8152(3) 0.3449(6) 0.0405(11) Uani 1.0 4 d . . . C7 C 1.0165(3) 0.8778(3) 0.2879(5) 0.0335(10) Uani 1.0 4 d . . . C8 C 0.9422(2) 0.8955(3) 0.3450(5) 0.0253(8) Uani 1.0 4 d . . . C9 C 0.8291(3) 0.9034(3) 0.7307(5) 0.0331(9) Uani 1.0 4 d . . . C10 C 0.7632(3) 0.7694(3) 0.5512(6) 0.0340(10) Uani 1.0 4 d . . . C11 C 0.9403(3) 1.0788(3) 0.3062(6) 0.0393(12) Uani 1.0 4 d . . . C12 C 0.8765(3) 0.9743(4) 0.0771(5) 0.0464(13) Uani 1.0 4 d . . . C13 C 0.5959(2) 1.0917(3) 0.3293(5) 0.0239(8) Uani 1.0 4 d . . . C14 C 0.5206(3) 1.1157(3) 0.2889(5) 0.0331(9) Uani 1.0 4 d . . . C15 C 0.4830(3) 1.1811(3) 0.3562(5) 0.0372(11) Uani 1.0 4 d . . . C16 C 0.5200(3) 1.2233(3) 0.4661(6) 0.0361(10) Uani 1.0 4 d . . . C17 C 0.5941(3) 1.2006(3) 0.5066(5) 0.0321(9) Uani 1.0 4 d . . . C18 C 0.6331(2) 1.1344(3) 0.4409(4) 0.0230(8) Uani 1.0 4 d . . . C19 C 0.5731(3) 0.9149(3) 0.2328(6) 0.0381(10) Uani 1.0 4 d . . . C20 C 0.6683(3) 1.0268(3) 0.0530(5) 0.0355(10) Uani 1.0 4 d . . . C21 C 0.7343(3) 1.0998(3) 0.6973(5) 0.0297(9) Uani 1.0 4 d . . . C22 C 0.7999(3) 1.1908(3) 0.4490(5) 0.0303(9) Uani 1.0 4 d . . . H1 H 0.9458 0.7557 0.5970 0.0430 Uiso 1.0 4 calc R . . H2 H 1.0689 0.7292 0.5017 0.0477 Uiso 1.0 4 calc R . . H3 H 1.1111 0.8026 0.3035 0.0486 Uiso 1.0 4 calc R . . H4 H 1.0354 0.9090 0.2098 0.0402 Uiso 1.0 4 calc R . . H5 H 0.8582 0.9557 0.7346 0.0397 Uiso 1.0 4 calc R . . H6 H 0.8578 0.8606 0.7828 0.0397 Uiso 1.0 4 calc R . . H7 H 0.7775 0.9111 0.7735 0.0397 Uiso 1.0 4 calc R . . H8 H 0.7928 0.7300 0.6092 0.0408 Uiso 1.0 4 calc R . . H9 H 0.7569 0.7469 0.4555 0.0408 Uiso 1.0 4 calc R . . H10 H 0.7117 0.7784 0.5936 0.0408 Uiso 1.0 4 calc R . . H11 H 0.9951 1.0679 0.2829 0.0471 Uiso 1.0 4 calc R . . H12 H 0.9361 1.0946 0.4060 0.0471 Uiso 1.0 4 calc R . . H13 H 0.9206 1.1239 0.2467 0.0471 Uiso 1.0 4 calc R . . H14 H 0.8534 0.9208 0.0512 0.0557 Uiso 1.0 4 calc R . . H15 H 0.9293 0.9782 0.0377 0.0557 Uiso 1.0 4 calc R . . H16 H 0.8442 1.0193 0.0390 0.0557 Uiso 1.0 4 calc R . . H17 H 0.4948 1.0870 0.2145 0.0397 Uiso 1.0 4 calc R . . H18 H 0.4320 1.1971 0.3273 0.0446 Uiso 1.0 4 calc R . . H19 H 0.4941 1.2676 0.5128 0.0433 Uiso 1.0 4 calc R . . H20 H 0.6194 1.2302 0.5804 0.0385 Uiso 1.0 4 calc R . . H21 H 0.5977 0.8667 0.1881 0.0457 Uiso 1.0 4 calc R . . H22 H 0.5278 0.9322 0.1768 0.0457 Uiso 1.0 4 calc R . . H23 H 0.5562 0.9002 0.3286 0.0457 Uiso 1.0 4 calc R . . H24 H 0.7062 1.0722 0.0499 0.0426 Uiso 1.0 4 calc R . . H25 H 0.6204 1.0435 0.0038 0.0426 Uiso 1.0 4 calc R . . H26 H 0.6904 0.9779 0.0067 0.0426 Uiso 1.0 4 calc R . . H27 H 0.7174 1.1536 0.7344 0.0357 Uiso 1.0 4 calc R . . H28 H 0.7872 1.0877 0.7311 0.0357 Uiso 1.0 4 calc R . . H29 H 0.6985 1.0566 0.7299 0.0357 Uiso 1.0 4 calc R . . H30 H 0.8015 1.1957 0.3456 0.0363 Uiso 1.0 4 calc R . . H31 H 0.8527 1.1802 0.4849 0.0363 Uiso 1.0 4 calc R . . H32 H 0.7800 1.2424 0.4898 0.0363 Uiso 1.0 4 calc R . . 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 Fe1 0.0208(3) 0.0156(3) 0.0165(3) 0.00005(17) -0.0001(2) -0.0018(2) Si1 0.0260(5) 0.0215(5) 0.0209(5) 0.0018(4) -0.0011(4) 0.0019(4) Si2 0.0236(5) 0.0269(5) 0.0226(6) 0.0021(4) 0.0043(4) 0.0001(4) Si3 0.0256(5) 0.0230(5) 0.0238(5) -0.0010(4) -0.0058(4) -0.0029(4) Si4 0.0207(5) 0.0191(5) 0.0209(5) -0.0012(4) -0.0002(4) -0.0046(4) O1 0.0313(15) 0.0362(17) 0.0386(18) -0.0082(13) 0.0102(13) 0.0040(14) O2 0.057(2) 0.0293(18) 0.038(2) 0.0071(14) -0.0072(14) -0.0168(15) C1 0.0248(18) 0.0189(17) 0.030(2) -0.0011(14) -0.0045(16) -0.0033(15) C2 0.0273(18) 0.027(3) 0.026(2) 0.0018(15) -0.0008(15) -0.0018(17) C3 0.0245(17) 0.0221(18) 0.029(2) 0.0032(15) -0.0037(15) -0.0039(15) C4 0.038(3) 0.029(2) 0.040(3) 0.0093(18) -0.0039(19) 0.0014(18) C5 0.032(2) 0.032(3) 0.056(3) 0.0094(19) -0.005(2) -0.004(2) C6 0.030(2) 0.032(3) 0.060(3) 0.0069(18) 0.002(2) -0.010(2) C7 0.0265(19) 0.031(2) 0.043(3) 0.0042(17) 0.0071(17) -0.0079(19) C8 0.0239(17) 0.0254(19) 0.0267(19) 0.0014(15) -0.0017(14) -0.0048(15) C9 0.036(2) 0.044(3) 0.0189(19) 0.0047(19) -0.0019(17) 0.0017(17) C10 0.041(3) 0.023(2) 0.039(3) -0.0037(17) -0.0005(19) 0.0079(19) C11 0.0243(19) 0.029(3) 0.065(4) 0.0006(17) 0.014(2) 0.006(2) C12 0.044(3) 0.072(4) 0.024(3) 0.011(3) 0.011(2) 0.003(3) C13 0.0213(17) 0.0242(19) 0.0262(18) -0.0012(15) -0.0037(15) 0.0041(15) C14 0.0241(19) 0.036(3) 0.039(3) 0.0037(17) -0.0064(17) 0.0017(19) C15 0.0237(18) 0.044(3) 0.044(3) 0.0148(18) 0.0011(17) 0.010(2) C16 0.036(3) 0.029(2) 0.043(3) 0.0088(18) 0.0099(19) 0.0043(19) C17 0.033(2) 0.0248(19) 0.039(3) 0.0038(16) 0.0054(18) 0.0003(17) C18 0.0234(17) 0.0201(18) 0.0256(18) -0.0019(14) 0.0022(14) 0.0025(14) C19 0.033(2) 0.034(3) 0.048(3) -0.0078(18) -0.013(2) -0.003(2) C20 0.048(3) 0.038(3) 0.021(2) 0.004(2) -0.0048(19) -0.0013(17) C21 0.035(2) 0.032(3) 0.022(2) 0.0014(17) -0.0006(16) -0.0075(16) C22 0.0263(18) 0.0248(19) 0.040(3) -0.0048(16) 0.0045(16) -0.0070(17) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe1 Si1 2.3928(12) yes . . Fe1 Si2 2.4240(12) yes . . Fe1 Si3 2.4116(13) yes . . Fe1 Si4 2.4233(12) yes . . Fe1 C1 1.762(4) yes . . Fe1 C2 1.760(5) yes . . Si1 C3 1.879(4) yes . . Si1 C9 1.871(5) yes . . Si1 C10 1.882(5) yes . . Si2 C8 1.882(4) yes . . Si2 C11 1.870(5) yes . . Si2 C12 1.867(5) yes . . Si3 C13 1.871(4) yes . . Si3 C19 1.864(5) yes . . Si3 C20 1.875(5) yes . . Si4 C18 1.887(4) yes . . Si4 C21 1.868(5) yes . . Si4 C22 1.872(4) yes . . O1 C1 1.155(5) yes . . O2 C2 1.156(6) yes . . C3 C4 1.406(6) yes . . C3 C8 1.403(6) yes . . C4 C5 1.385(7) yes . . C5 C6 1.383(8) yes . . C6 C7 1.384(7) yes . . C7 C8 1.411(6) yes . . C13 C14 1.400(6) yes . . C13 C18 1.412(6) yes . . C14 C15 1.391(7) yes . . C15 C16 1.393(7) yes . . C16 C17 1.376(6) yes . . C17 C18 1.404(6) yes . . C4 H1 0.950 no . . C5 H2 0.950 no . . C6 H3 0.950 no . . C7 H4 0.950 no . . C9 H5 0.980 no . . C9 H6 0.980 no . . C9 H7 0.980 no . . C10 H8 0.980 no . . C10 H9 0.980 no . . C10 H10 0.980 no . . C11 H11 0.980 no . . C11 H12 0.980 no . . C11 H13 0.980 no . . C12 H14 0.980 no . . C12 H15 0.980 no . . C12 H16 0.980 no . . C14 H17 0.950 no . . C15 H18 0.950 no . . C16 H19 0.950 no . . C17 H20 0.950 no . . C19 H21 0.980 no . . C19 H22 0.980 no . . C19 H23 0.980 no . . C20 H24 0.980 no . . C20 H25 0.980 no . . C20 H26 0.980 no . . C21 H27 0.980 no . . C21 H28 0.980 no . . C21 H29 0.980 no . . C22 H30 0.980 no . . C22 H31 0.980 no . . C22 H32 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Si1 Fe1 Si2 86.58(4) yes . . . Si1 Fe1 Si3 147.11(5) yes . . . Si1 Fe1 Si4 113.68(5) yes . . . Si1 Fe1 C1 78.80(13) yes . . . Si1 Fe1 C2 80.75(15) yes . . . Si2 Fe1 Si3 114.60(5) yes . . . Si2 Fe1 Si4 104.23(4) yes . . . Si2 Fe1 C1 164.79(13) yes . . . Si2 Fe1 C2 77.54(13) yes . . . Si3 Fe1 Si4 86.38(4) yes . . . Si3 Fe1 C1 80.38(13) yes . . . Si3 Fe1 C2 79.88(14) yes . . . Si4 Fe1 C1 78.30(13) yes . . . Si4 Fe1 C2 165.45(15) yes . . . C1 Fe1 C2 103.87(18) yes . . . Fe1 Si1 C3 105.95(13) yes . . . Fe1 Si1 C9 115.65(15) yes . . . Fe1 Si1 C10 112.81(16) yes . . . C3 Si1 C9 109.56(19) yes . . . C3 Si1 C10 107.98(19) yes . . . C9 Si1 C10 104.7(3) yes . . . Fe1 Si2 C8 105.17(13) yes . . . Fe1 Si2 C11 118.83(16) yes . . . Fe1 Si2 C12 113.84(17) yes . . . C8 Si2 C11 105.16(19) yes . . . C8 Si2 C12 108.8(3) yes . . . C11 Si2 C12 104.4(3) yes . . . Fe1 Si3 C13 105.35(13) yes . . . Fe1 Si3 C19 112.50(16) yes . . . Fe1 Si3 C20 115.48(16) yes . . . C13 Si3 C19 108.01(19) yes . . . C13 Si3 C20 110.3(2) yes . . . C19 Si3 C20 105.1(3) yes . . . Fe1 Si4 C18 104.60(13) yes . . . Fe1 Si4 C21 113.82(15) yes . . . Fe1 Si4 C22 118.25(14) yes . . . C18 Si4 C21 107.63(18) yes . . . C18 Si4 C22 105.86(18) yes . . . C21 Si4 C22 106.0(2) yes . . . Fe1 C1 O1 178.3(4) yes . . . Fe1 C2 O2 177.2(4) yes . . . Si1 C3 C4 119.9(3) yes . . . Si1 C3 C8 120.7(3) yes . . . C4 C3 C8 119.4(4) yes . . . C3 C4 C5 120.9(5) yes . . . C4 C5 C6 119.6(5) yes . . . C5 C6 C7 120.8(5) yes . . . C6 C7 C8 120.4(5) yes . . . Si2 C8 C3 119.9(3) yes . . . Si2 C8 C7 121.1(3) yes . . . C3 C8 C7 118.9(4) yes . . . Si3 C13 C14 120.5(3) yes . . . Si3 C13 C18 120.5(3) yes . . . C14 C13 C18 118.9(4) yes . . . C13 C14 C15 120.8(4) yes . . . C14 C15 C16 120.1(4) yes . . . C15 C16 C17 119.8(5) yes . . . C16 C17 C18 121.2(4) yes . . . Si4 C18 C13 120.1(3) yes . . . Si4 C18 C17 120.7(3) yes . . . C13 C18 C17 119.2(4) yes . . . C3 C4 H1 119.579 no . . . C5 C4 H1 119.568 no . . . C4 C5 H2 120.193 no . . . C6 C5 H2 120.202 no . . . C5 C6 H3 119.606 no . . . C7 C6 H3 119.611 no . . . C6 C7 H4 119.812 no . . . C8 C7 H4 119.803 no . . . Si1 C9 H5 109.470 no . . . Si1 C9 H6 109.474 no . . . Si1 C9 H7 109.472 no . . . H5 C9 H6 109.469 no . . . H5 C9 H7 109.465 no . . . H6 C9 H7 109.478 no . . . Si1 C10 H8 109.474 no . . . Si1 C10 H9 109.474 no . . . Si1 C10 H10 109.465 no . . . H8 C10 H9 109.472 no . . . H8 C10 H10 109.472 no . . . H9 C10 H10 109.470 no . . . Si2 C11 H11 109.478 no . . . Si2 C11 H12 109.473 no . . . Si2 C11 H13 109.478 no . . . H11 C11 H12 109.467 no . . . H11 C11 H13 109.468 no . . . H12 C11 H13 109.463 no . . . Si2 C12 H14 109.471 no . . . Si2 C12 H15 109.477 no . . . Si2 C12 H16 109.469 no . . . H14 C12 H15 109.468 no . . . H14 C12 H16 109.464 no . . . H15 C12 H16 109.479 no . . . C13 C14 H17 119.601 no . . . C15 C14 H17 119.609 no . . . C14 C15 H18 119.956 no . . . C16 C15 H18 119.978 no . . . C15 C16 H19 120.082 no . . . C17 C16 H19 120.095 no . . . C16 C17 H20 119.422 no . . . C18 C17 H20 119.412 no . . . Si3 C19 H21 109.479 no . . . Si3 C19 H22 109.477 no . . . Si3 C19 H23 109.472 no . . . H21 C19 H22 109.468 no . . . H21 C19 H23 109.473 no . . . H22 C19 H23 109.459 no . . . Si3 C20 H24 109.472 no . . . Si3 C20 H25 109.467 no . . . Si3 C20 H26 109.473 no . . . H24 C20 H25 109.471 no . . . H24 C20 H26 109.475 no . . . H25 C20 H26 109.470 no . . . Si4 C21 H27 109.473 no . . . Si4 C21 H28 109.469 no . . . Si4 C21 H29 109.467 no . . . H27 C21 H28 109.474 no . . . H27 C21 H29 109.475 no . . . H28 C21 H29 109.470 no . . . Si4 C22 H30 109.470 no . . . Si4 C22 H31 109.471 no . . . Si4 C22 H32 109.460 no . . . H30 C22 H31 109.478 no . . . H30 C22 H32 109.474 no . . . H31 C22 H32 109.474 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Si1 Fe1 Si2 C8 11.35(5) no . . . . Si1 Fe1 Si2 C11 -105.95(6) no . . . . Si1 Fe1 Si2 C12 130.39(6) no . . . . Si2 Fe1 Si1 C3 -9.69(5) no . . . . Si2 Fe1 Si1 C9 111.88(6) no . . . . Si2 Fe1 Si1 C10 -127.63(6) no . . . . Si1 Fe1 Si3 C13 115.81(8) no . . . . Si1 Fe1 Si3 C19 -1.62(12) no . . . . Si1 Fe1 Si3 C20 -122.23(8) no . . . . Si3 Fe1 Si1 C3 122.80(8) no . . . . Si3 Fe1 Si1 C9 -115.63(8) no . . . . Si3 Fe1 Si1 C10 4.87(11) no . . . . Si1 Fe1 Si4 C18 -138.14(5) no . . . . Si1 Fe1 Si4 C21 -20.94(7) no . . . . Si1 Fe1 Si4 C22 104.43(6) no . . . . Si4 Fe1 Si1 C3 -113.74(5) no . . . . Si4 Fe1 Si1 C9 7.83(7) no . . . . Si4 Fe1 Si1 C10 128.33(5) no . . . . C1 Fe1 Si1 C3 174.48(14) no . . . . C1 Fe1 Si1 C9 -63.95(14) no . . . . C1 Fe1 Si1 C10 56.55(14) no . . . . C2 Fe1 Si1 C3 68.23(14) no . . . . C2 Fe1 Si1 C9 -170.20(14) no . . . . C2 Fe1 Si1 C10 -49.71(14) no . . . . Si2 Fe1 Si3 C13 -118.24(6) no . . . . Si2 Fe1 Si3 C19 124.33(6) no . . . . Si2 Fe1 Si3 C20 3.72(8) no . . . . Si3 Fe1 Si2 C8 -142.52(5) no . . . . Si3 Fe1 Si2 C11 100.18(7) no . . . . Si3 Fe1 Si2 C12 -23.48(8) no . . . . Si2 Fe1 Si4 C18 129.34(5) no . . . . Si2 Fe1 Si4 C21 -113.46(6) no . . . . Si2 Fe1 Si4 C22 11.91(7) no . . . . Si4 Fe1 Si2 C8 124.93(5) no . . . . Si4 Fe1 Si2 C11 7.63(7) no . . . . Si4 Fe1 Si2 C12 -116.03(6) no . . . . C2 Fe1 Si2 C8 -69.92(15) no . . . . C2 Fe1 Si2 C11 172.78(16) no . . . . C2 Fe1 Si2 C12 49.12(16) no . . . . Si3 Fe1 Si4 C18 14.86(5) no . . . . Si3 Fe1 Si4 C21 132.07(6) no . . . . Si3 Fe1 Si4 C22 -102.56(6) no . . . . Si4 Fe1 Si3 C13 -14.24(5) no . . . . Si4 Fe1 Si3 C19 -131.67(6) no . . . . Si4 Fe1 Si3 C20 107.72(6) no . . . . C1 Fe1 Si3 C13 64.50(13) no . . . . C1 Fe1 Si3 C19 -52.93(14) no . . . . C1 Fe1 Si3 C20 -173.55(14) no . . . . C2 Fe1 Si3 C13 170.59(15) no . . . . C2 Fe1 Si3 C19 53.16(15) no . . . . C2 Fe1 Si3 C20 -67.45(15) no . . . . C1 Fe1 Si4 C18 -66.05(14) no . . . . C1 Fe1 Si4 C21 51.15(14) no . . . . C1 Fe1 Si4 C22 176.52(14) no . . . . Fe1 Si1 C3 C4 -172.8(3) no . . . . Fe1 Si1 C3 C8 5.7(3) no . . . . C9 Si1 C3 C4 61.8(4) no . . . . C9 Si1 C3 C8 -119.7(3) no . . . . C10 Si1 C3 C4 -51.7(4) no . . . . C10 Si1 C3 C8 126.8(3) no . . . . Fe1 Si2 C8 C3 -12.0(3) no . . . . Fe1 Si2 C8 C7 172.1(3) no . . . . C11 Si2 C8 C3 114.3(3) no . . . . C11 Si2 C8 C7 -61.7(4) no . . . . C12 Si2 C8 C3 -134.3(3) no . . . . C12 Si2 C8 C7 49.7(4) no . . . . Fe1 Si3 C13 C14 -166.5(3) no . . . . Fe1 Si3 C13 C18 10.9(3) no . . . . C19 Si3 C13 C14 -46.0(4) no . . . . C19 Si3 C13 C18 131.3(3) no . . . . C20 Si3 C13 C14 68.3(4) no . . . . C20 Si3 C13 C18 -114.4(3) no . . . . Fe1 Si4 C18 C13 -13.6(3) no . . . . Fe1 Si4 C18 C17 166.9(3) no . . . . C21 Si4 C18 C13 -135.0(3) no . . . . C21 Si4 C18 C17 45.5(4) no . . . . C22 Si4 C18 C13 112.0(3) no . . . . C22 Si4 C18 C17 -67.5(3) no . . . . Si1 C3 C4 C5 179.7(3) no . . . . Si1 C3 C8 Si2 4.4(5) no . . . . Si1 C3 C8 C7 -179.6(3) no . . . . C4 C3 C8 Si2 -177.1(3) no . . . . C4 C3 C8 C7 -1.1(6) no . . . . C8 C3 C4 C5 1.2(6) no . . . . C3 C4 C5 C6 -1.7(7) no . . . . C4 C5 C6 C7 2.2(7) no . . . . C5 C6 C7 C8 -2.1(7) no . . . . C6 C7 C8 Si2 177.5(4) no . . . . C6 C7 C8 C3 1.5(6) no . . . . Si3 C13 C14 C15 178.1(3) no . . . . Si3 C13 C18 Si4 1.9(5) no . . . . Si3 C13 C18 C17 -178.5(3) no . . . . C14 C13 C18 Si4 179.3(3) no . . . . C14 C13 C18 C17 -1.1(6) no . . . . C18 C13 C14 C15 0.7(6) no . . . . C13 C14 C15 C16 -0.5(7) no . . . . C14 C15 C16 C17 0.7(7) no . . . . C15 C16 C17 C18 -1.2(7) no . . . . C16 C17 C18 Si4 -179.1(4) no . . . . C16 C17 C18 C13 1.4(6) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Si1 O1 3.373(4) no . . Si1 O2 3.437(4) no . . Si2 O2 3.394(4) no . . Si3 O1 3.474(4) no . . Si3 O2 3.450(4) no . . Si4 O1 3.412(4) no . . O1 C10 3.469(6) no . . O1 C18 3.577(5) no . . O1 C19 3.502(6) no . . O1 C21 3.428(6) no . . O2 C10 3.399(7) no . . O2 C12 3.390(7) no . . O2 C19 3.468(6) no . . C1 C9 3.384(6) no . . C1 C10 3.228(6) no . . C1 C13 3.225(6) no . . C1 C18 3.196(6) no . . C1 C19 3.223(7) no . . C1 C21 3.186(6) no . . C2 C3 3.294(6) no . . C2 C8 3.247(6) no . . C2 C10 3.192(7) no . . C2 C12 3.141(7) no . . C2 C19 3.212(6) no . . C2 C20 3.475(7) no . . C3 C6 2.790(6) no . . C4 C7 2.776(7) no . . C4 C9 3.584(7) no . . C4 C10 3.460(7) no . . C5 C8 2.806(6) no . . C7 C11 3.501(6) no . . C7 C12 3.485(7) no . . C9 C21 3.576(7) no . . C11 C22 3.296(6) no . . C13 C16 2.806(6) no . . C14 C17 2.775(7) no . . C14 C19 3.406(7) no . . C15 C18 2.796(6) no . . C17 C21 3.414(6) no . . C17 C22 3.569(6) no . . O1 C14 3.291(6) no . 4_675 O2 C22 3.384(6) no . 2_644 C9 C12 3.561(7) no . 1_556 C12 C9 3.561(7) no . 1_554 C14 O1 3.291(6) no . 4_674 C22 O2 3.384(6) no . 2_655 Si1 H1 2.9239 no . . Si2 H4 2.9615 no . . Si3 H17 2.9271 no . . Si4 H12 3.5717 no . . Si4 H20 2.9422 no . . O1 H7 3.0880 no . . O1 H10 2.8182 no . . O1 H23 2.7991 no . . O1 H29 2.7084 no . . O2 H9 2.6867 no . . O2 H14 2.6936 no . . O2 H21 2.8037 no . . O2 H26 3.2956 no . . C1 H7 3.0669 no . . C1 H9 3.5256 no . . C1 H10 2.8863 no . . C1 H21 3.5812 no . . C1 H23 2.8140 no . . C1 H29 2.7577 no . . C2 H9 2.7840 no . . C2 H10 3.5373 no . . C2 H14 2.7544 no . . C2 H16 3.4698 no . . C2 H21 2.8599 no . . C2 H23 3.4832 no . . C2 H26 3.1730 no . . C3 H2 3.2851 no . . C3 H4 3.2821 no . . C3 H5 3.2407 no . . C3 H6 3.1927 no . . C3 H8 3.1843 no . . C3 H9 3.1960 no . . C4 H3 3.2488 no . . C4 H6 3.3055 no . . C4 H8 3.1872 no . . C5 H4 3.2590 no . . C6 H1 3.2482 no . . C7 H2 3.2615 no . . C7 H11 3.0908 no . . C7 H15 3.2322 no . . C8 H1 3.2815 no . . C8 H3 3.2809 no . . C8 H11 2.9841 no . . C8 H12 3.2666 no . . C8 H14 3.1924 no . . C8 H15 3.2042 no . . C9 H1 3.3573 no . . C9 H8 3.0876 no . . C9 H10 3.1292 no . . C9 H28 3.0594 no . . C9 H29 3.3337 no . . C10 H1 3.1649 no . . C10 H6 3.0953 no . . C10 H7 3.1163 no . . C11 H4 3.3158 no . . C11 H15 3.0187 no . . C11 H16 3.1629 no . . C11 H30 3.0569 no . . C11 H31 2.7898 no . . C12 H4 3.1769 no . . C12 H11 3.1925 no . . C12 H13 2.9948 no . . C12 H24 3.3262 no . . C12 H26 3.2548 no . . C13 H18 3.2818 no . . C13 H20 3.2856 no . . C13 H22 3.1728 no . . C13 H23 3.1646 no . . C13 H24 3.2614 no . . C13 H25 3.2003 no . . C14 H19 3.2697 no . . C14 H22 3.1489 no . . C14 H23 3.5516 no . . C14 H25 3.3970 no . . C15 H20 3.2520 no . . C16 H17 3.2670 no . . C17 H18 3.2529 no . . C17 H27 3.1092 no . . C17 H32 3.2568 no . . C18 H17 3.2811 no . . C18 H19 3.2778 no . . C18 H27 3.1426 no . . C18 H29 3.2081 no . . C18 H30 3.1801 no . . C18 H32 3.0952 no . . C19 H17 3.0899 no . . C19 H25 3.1069 no . . C19 H26 3.1039 no . . C20 H16 3.0180 no . . C20 H17 3.4776 no . . C20 H21 3.1261 no . . C20 H22 3.0806 no . . C21 H5 3.1680 no . . C21 H7 3.2163 no . . C21 H20 3.0854 no . . C21 H31 3.1327 no . . C21 H32 3.1230 no . . C22 H12 2.8302 no . . C22 H13 3.0150 no . . C22 H20 3.3911 no . . C22 H27 3.1037 no . . C22 H28 3.1509 no . . H1 H2 2.3320 no . . H1 H6 2.8671 no . . H1 H8 2.6556 no . . H1 H9 3.5036 no . . H2 H3 2.3300 no . . H3 H4 2.3259 no . . H4 H11 2.7448 no . . H4 H14 3.4636 no . . H4 H15 2.6827 no . . H5 H28 2.4531 no . . H5 H29 3.1831 no . . H6 H8 2.8927 no . . H6 H10 3.3487 no . . H7 H8 3.3199 no . . H7 H10 2.9581 no . . H7 H28 2.8826 no . . H7 H29 2.7407 no . . H11 H15 2.9560 no . . H11 H16 3.5500 no . . H11 H31 3.5886 no . . H12 H30 2.8800 no . . H12 H31 2.1222 no . . H13 H15 3.0748 no . . H13 H16 2.9005 no . . H13 H30 2.5247 no . . H13 H31 2.6923 no . . H14 H24 3.5105 no . . H14 H26 2.9682 no . . H16 H24 2.5152 no . . H16 H26 2.7340 no . . H17 H18 2.3348 no . . H17 H22 2.5871 no . . H17 H23 3.3702 no . . H17 H25 3.0140 no . . H18 H19 2.3443 no . . H19 H20 2.3191 no . . H20 H27 2.5424 no . . H20 H29 3.4183 no . . H20 H32 2.8859 no . . H21 H25 3.3670 no . . H21 H26 2.9467 no . . H22 H25 2.9023 no . . H22 H26 3.2994 no . . H27 H31 3.3323 no . . H27 H32 2.9235 no . . H28 H31 2.9831 no . . H28 H32 3.3848 no . . O1 H2 2.8944 no . 3_465 O1 H17 2.4695 no . 4_675 O1 H18 3.2374 no . 4_675 O2 H3 3.3620 no . 3_465 O2 H20 2.8697 no . 2_644 O2 H27 2.8160 no . 2_644 O2 H32 2.5053 no . 2_644 C1 H2 3.4134 no . 3_465 C2 H32 3.5843 no . 2_644 C4 H11 3.4924 no . 4_775 C4 H13 3.2585 no . 4_775 C5 H10 3.3435 no . 3_565 C5 H13 3.2716 no . 4_775 C5 H21 3.5609 no . 3_565 C5 H23 3.0500 no . 3_565 C6 H19 3.3703 no . 2_644 C6 H21 3.3446 no . 3_565 C6 H23 3.4817 no . 3_565 C6 H28 3.2075 no . 4_774 C7 H5 3.4769 no . 4_774 C7 H15 3.4411 no . 4_775 C7 H19 3.1553 no . 2_644 C7 H28 3.4491 no . 4_774 C8 H15 3.5087 no . 4_775 C9 H11 3.0852 no . 4_775 C9 H14 3.0703 no . 1_556 C9 H15 3.5800 no . 1_556 C9 H16 3.4722 no . 1_556 C10 H2 3.3588 no . 3_465 C10 H24 3.2246 no . 2_645 C10 H27 3.5445 no . 2_644 C10 H30 3.2227 no . 2_645 C11 H5 3.5601 no . 4_774 C11 H15 3.2583 no . 4_775 C11 H19 3.2883 no . 3_575 C12 H5 3.2656 no . 1_554 C12 H6 3.3477 no . 1_554 C12 H7 3.4843 no . 1_554 C13 H1 3.5123 no . 2_654 C13 H8 3.5978 no . 2_654 C14 H1 2.9536 no . 2_654 C15 H1 2.9892 no . 2_654 C15 H2 3.5526 no . 2_654 C15 H13 3.4808 no . 3_475 C15 H21 3.5128 no . 4_675 C15 H22 3.5440 no . 4_675 C15 H31 3.3861 no . 3_475 C16 H1 3.5748 no . 2_654 C16 H6 3.5066 no . 2_654 C16 H12 3.3201 no . 3_475 C16 H21 3.2511 no . 4_675 C16 H22 3.3062 no . 4_675 C16 H31 3.2658 no . 3_475 C17 H6 3.4390 no . 2_654 C17 H22 3.3961 no . 4_675 C19 H2 3.4454 no . 3_465 C20 H8 3.3894 no . 2_654 C20 H29 3.1343 no . 1_554 C21 H3 3.2397 no . 4_775 C21 H9 3.4080 no . 2_655 C21 H24 3.3968 no . 1_556 C22 H18 3.1158 no . 3_575 C22 H19 3.4447 no . 3_575 H1 C13 3.5123 no . 2_645 H1 C14 2.9536 no . 2_645 H1 C15 2.9892 no . 2_645 H1 C16 3.5748 no . 2_645 H1 H11 3.4947 no . 4_775 H1 H13 3.3174 no . 4_775 H1 H17 3.1114 no . 2_645 H1 H18 3.1634 no . 2_645 H2 O1 2.8944 no . 3_565 H2 C1 3.4134 no . 3_565 H2 C10 3.3588 no . 3_565 H2 C15 3.5526 no . 2_645 H2 C19 3.4454 no . 3_565 H2 H9 3.2703 no . 3_565 H2 H10 2.5964 no . 3_565 H2 H13 3.3192 no . 4_775 H2 H17 3.2416 no . 2_645 H2 H18 3.1212 no . 2_645 H2 H21 3.3790 no . 3_565 H2 H23 2.6620 no . 3_565 H3 O2 3.3620 no . 3_565 H3 C21 3.2397 no . 4_774 H3 H9 2.9892 no . 3_565 H3 H10 3.4915 no . 3_565 H3 H19 3.3331 no . 2_644 H3 H21 2.9506 no . 3_565 H3 H23 3.4140 no . 3_565 H3 H27 3.0900 no . 4_774 H3 H28 2.5767 no . 4_774 H3 H31 3.0870 no . 4_774 H3 H32 3.5778 no . 4_774 H4 H5 2.8548 no . 4_774 H4 H12 2.9129 no . 4_774 H4 H19 2.9885 no . 2_644 H4 H28 3.0440 no . 4_774 H4 H31 3.2034 no . 4_774 H5 C7 3.4769 no . 4_775 H5 C11 3.5601 no . 4_775 H5 C12 3.2656 no . 1_556 H5 H4 2.8548 no . 4_775 H5 H11 2.5814 no . 4_775 H5 H14 3.0453 no . 1_556 H5 H15 3.1335 no . 1_556 H5 H16 3.0642 no . 1_556 H6 C12 3.3477 no . 1_556 H6 C16 3.5066 no . 2_645 H6 C17 3.4390 no . 2_645 H6 H11 2.7711 no . 4_775 H6 H14 2.7177 no . 1_556 H6 H15 3.3023 no . 1_556 H6 H16 3.5324 no . 1_556 H6 H20 3.5349 no . 2_645 H7 C12 3.4843 no . 1_556 H7 H14 2.9323 no . 1_556 H7 H16 3.2631 no . 1_556 H7 H26 2.8700 no . 1_556 H7 H32 3.5435 no . 2_645 H8 C13 3.5978 no . 2_645 H8 C20 3.3894 no . 2_645 H8 H24 2.6082 no . 2_645 H8 H25 3.5019 no . 2_645 H8 H30 2.8122 no . 2_645 H9 C21 3.4080 no . 2_644 H9 H2 3.2703 no . 3_465 H9 H3 2.9892 no . 3_465 H9 H24 3.0232 no . 2_645 H9 H27 2.6129 no . 2_644 H9 H28 3.4168 no . 2_644 H10 C5 3.3435 no . 3_465 H10 H2 2.5964 no . 3_465 H10 H3 3.4915 no . 3_465 H10 H18 3.3295 no . 4_675 H10 H30 2.7400 no . 2_645 H11 C4 3.4924 no . 4_774 H11 C9 3.0852 no . 4_774 H11 H1 3.4947 no . 4_774 H11 H5 2.5814 no . 4_774 H11 H6 2.7711 no . 4_774 H11 H15 2.8330 no . 4_775 H11 H19 3.4315 no . 3_575 H12 C16 3.3201 no . 3_575 H12 H4 2.9129 no . 4_775 H12 H15 2.8708 no . 4_775 H12 H18 3.4436 no . 3_575 H12 H19 2.6366 no . 3_575 H13 C4 3.2585 no . 4_774 H13 C5 3.2716 no . 4_774 H13 C15 3.4808 no . 3_575 H13 H1 3.3174 no . 4_774 H13 H2 3.3192 no . 4_774 H13 H18 2.9946 no . 3_575 H13 H19 3.3134 no . 3_575 H14 C9 3.0703 no . 1_554 H14 H5 3.0453 no . 1_554 H14 H6 2.7177 no . 1_554 H14 H7 2.9323 no . 1_554 H14 H20 3.1244 no . 2_644 H15 C7 3.4411 no . 4_774 H15 C8 3.5087 no . 4_774 H15 C9 3.5800 no . 1_554 H15 C11 3.2583 no . 4_774 H15 H5 3.1335 no . 1_554 H15 H6 3.3023 no . 1_554 H15 H11 2.8330 no . 4_774 H15 H12 2.8708 no . 4_774 H16 C9 3.4722 no . 1_554 H16 H5 3.0642 no . 1_554 H16 H6 3.5324 no . 1_554 H16 H7 3.2631 no . 1_554 H16 H28 3.2622 no . 1_554 H17 O1 2.4695 no . 4_674 H17 H1 3.1114 no . 2_654 H17 H2 3.2416 no . 2_654 H18 O1 3.2374 no . 4_674 H18 C22 3.1158 no . 3_475 H18 H1 3.1634 no . 2_654 H18 H2 3.1212 no . 2_654 H18 H10 3.3295 no . 4_674 H18 H12 3.4436 no . 3_475 H18 H13 2.9946 no . 3_475 H18 H21 3.5979 no . 4_675 H18 H30 2.8302 no . 3_475 H18 H31 2.8259 no . 3_475 H18 H32 3.1758 no . 3_475 H19 C6 3.3703 no . 2_655 H19 C7 3.1553 no . 2_655 H19 C11 3.2883 no . 3_475 H19 C22 3.4447 no . 3_475 H19 H3 3.3331 no . 2_655 H19 H4 2.9885 no . 2_655 H19 H11 3.4315 no . 3_475 H19 H12 2.6366 no . 3_475 H19 H13 3.3134 no . 3_475 H19 H21 3.1475 no . 4_675 H19 H22 3.5966 no . 4_675 H19 H31 2.5774 no . 3_475 H20 O2 2.8697 no . 2_655 H20 H6 3.5349 no . 2_654 H20 H14 3.1244 no . 2_655 H21 C5 3.5609 no . 3_465 H21 C6 3.3446 no . 3_465 H21 C15 3.5128 no . 4_674 H21 C16 3.2511 no . 4_674 H21 H2 3.3790 no . 3_465 H21 H3 2.9506 no . 3_465 H21 H18 3.5979 no . 4_674 H21 H19 3.1475 no . 4_674 H21 H32 3.4531 no . 2_644 H22 C15 3.5440 no . 4_674 H22 C16 3.3062 no . 4_674 H22 C17 3.3961 no . 4_674 H22 H19 3.5966 no . 4_674 H23 C5 3.0500 no . 3_465 H23 C6 3.4817 no . 3_465 H23 H2 2.6620 no . 3_465 H23 H3 3.4140 no . 3_465 H23 H25 3.5650 no . 4_675 H24 C10 3.2246 no . 2_654 H24 C21 3.3968 no . 1_554 H24 H8 2.6082 no . 2_654 H24 H9 3.0232 no . 2_654 H24 H27 3.2637 no . 1_554 H24 H28 3.3264 no . 1_554 H24 H29 3.0376 no . 1_554 H25 H8 3.5019 no . 2_654 H25 H23 3.5650 no . 4_674 H25 H27 3.5209 no . 1_554 H25 H29 2.9206 no . 1_554 H26 H7 2.8700 no . 1_554 H26 H28 3.5598 no . 1_554 H26 H29 2.9110 no . 1_554 H27 O2 2.8160 no . 2_655 H27 C10 3.5445 no . 2_655 H27 H3 3.0900 no . 4_775 H27 H9 2.6129 no . 2_655 H27 H24 3.2637 no . 1_556 H27 H25 3.5209 no . 1_556 H28 C6 3.2075 no . 4_775 H28 C7 3.4491 no . 4_775 H28 H3 2.5767 no . 4_775 H28 H4 3.0440 no . 4_775 H28 H9 3.4168 no . 2_655 H28 H16 3.2622 no . 1_556 H28 H24 3.3264 no . 1_556 H28 H26 3.5598 no . 1_556 H29 C20 3.1343 no . 1_556 H29 H24 3.0376 no . 1_556 H29 H25 2.9206 no . 1_556 H29 H26 2.9110 no . 1_556 H30 C10 3.2227 no . 2_654 H30 H8 2.8122 no . 2_654 H30 H10 2.7400 no . 2_654 H30 H18 2.8302 no . 3_575 H31 C15 3.3861 no . 3_575 H31 C16 3.2658 no . 3_575 H31 H3 3.0870 no . 4_775 H31 H4 3.2034 no . 4_775 H31 H18 2.8259 no . 3_575 H31 H19 2.5774 no . 3_575 H32 O2 2.5053 no . 2_655 H32 C2 3.5843 no . 2_655 H32 H3 3.5778 no . 4_775 H32 H7 3.5435 no . 2_654 H32 H18 3.1758 no . 3_575 H32 H21 3.4531 no . 2_655 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 947204' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Fe(Si)2(S-S)(CO)2 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C17 H28 Fe O2 S2 Si2' _chemical_formula_moiety 'C17 H28 Fe O2 S2 Si2' _chemical_formula_weight 440.54 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 +X,-Y,1/2+Z 3 1/2+X,1/2+Y,+Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 16.522(4) _cell_length_b 9.0451(18) _cell_length_c 15.932(4) _cell_angle_alpha 90.0000 _cell_angle_beta 116.341(3) _cell_angle_gamma 90.0000 _cell_volume 2133.7(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3567 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 123 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.090 _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928.00 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.912 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 123 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 8514 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4220 _reflns_number_gt 4037 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0652 _refine_ls_number_restraints 2 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4220 _refine_ls_number_parameters 217 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.7093P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.410 _refine_diff_density_min -0.220 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1777 Friedel Pairs' _refine_ls_abs_structure_Flack -0.006(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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.3463 0.8444 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.0817 0.0704 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.06046(2) 1.03949(4) 0.14362(2) 0.01755(8) Uani 1.0 4 d . . . S1 S 0.18103(4) 1.19654(7) 0.20856(4) 0.02590(14) Uani 1.0 4 d . . . S2 S -0.03816(4) 1.17740(6) 0.17634(4) 0.02152(13) Uani 1.0 4 d . . . Si1 Si 0.15255(4) 0.88442(8) 0.10564(4) 0.02172(14) Uani 1.0 4 d . . . Si2 Si -0.05648(4) 0.86872(7) 0.06884(5) 0.02066(14) Uani 1.0 4 d . . . O1 O 0.11204(14) 0.8274(2) 0.29773(13) 0.0318(5) Uani 1.0 4 d . . . O2 O -0.00144(16) 1.1274(3) -0.05207(13) 0.0371(5) Uani 1.0 4 d . . . C1 C 0.09180(16) 0.9139(3) 0.23731(17) 0.0217(5) Uani 1.0 4 d . . . C2 C 0.02401(18) 1.0968(3) 0.02665(17) 0.0248(6) Uani 1.0 4 d . . . C3 C 0.08043(16) 0.7227(3) 0.03655(15) 0.0192(5) Uani 1.0 4 d . . . C4 C 0.11524(18) 0.6114(3) -0.00042(16) 0.0233(5) Uani 1.0 4 d . . . C5 C 0.06080(19) 0.4962(3) -0.05334(17) 0.0281(6) Uani 1.0 4 d . . . C6 C -0.0293(2) 0.4912(3) -0.07037(18) 0.0272(6) Uani 1.0 4 d . . . C7 C -0.06405(18) 0.5999(3) -0.03385(17) 0.0239(5) Uani 1.0 4 d . . . C8 C -0.01002(17) 0.7165(3) 0.02063(16) 0.0200(5) Uani 1.0 4 d . . . C9 C 0.25443(19) 0.8036(4) 0.2080(2) 0.0402(8) Uani 1.0 4 d . . . C10 C 0.2037(3) 0.9709(4) 0.0326(3) 0.0399(8) Uani 1.0 4 d . . . C11 C -0.1032(2) 0.7841(4) 0.1465(3) 0.0378(7) Uani 1.0 4 d . . . C12 C -0.1614(2) 0.9411(4) -0.0337(3) 0.0389(7) Uani 1.0 4 d . . . C13 C 0.23779(19) 1.1784(4) 0.33430(18) 0.0325(6) Uani 1.0 4 d . . . C14 C 0.1467(2) 1.3892(3) 0.19878(19) 0.0346(7) Uani 1.0 4 d . . . C15 C 0.0789(3) 1.4290(3) 0.2359(2) 0.0357(7) Uani 1.0 4 d . . . C16 C -0.0179(2) 1.3746(3) 0.1766(2) 0.0346(7) Uani 1.0 4 d . . . C17 C -0.01664(18) 1.1496(3) 0.29701(17) 0.0241(5) Uani 1.0 4 d . . . H1 H 0.1767 0.6152 0.0110 0.0279 Uiso 1.0 4 calc R . . H2 H 0.0849 0.4215 -0.0777 0.0337 Uiso 1.0 4 calc R . . H3 H -0.0671 0.4134 -0.1070 0.0327 Uiso 1.0 4 calc R . . H4 H -0.1257 0.5953 -0.0460 0.0286 Uiso 1.0 4 calc R . . H5 H 0.2905 0.8837 0.2490 0.0483 Uiso 1.0 4 calc R . . H6 H 0.2913 0.7484 0.1846 0.0483 Uiso 1.0 4 calc R . . H7 H 0.2342 0.7369 0.2434 0.0483 Uiso 1.0 4 calc R . . H8 H 0.2489 1.0443 0.0702 0.0479 Uiso 1.0 4 calc R . . H9 H 0.1562 1.0193 -0.0221 0.0479 Uiso 1.0 4 calc R . . H10 H 0.2326 0.8941 0.0118 0.0479 Uiso 1.0 4 calc R . . H11 H -0.1558 0.7230 0.1085 0.0453 Uiso 1.0 4 calc R . . H12 H -0.1212 0.8628 0.1770 0.0453 Uiso 1.0 4 calc R . . H13 H -0.0568 0.7224 0.1943 0.0453 Uiso 1.0 4 calc R . . H14 H -0.1806 1.0335 -0.0158 0.0467 Uiso 1.0 4 calc R . . H15 H -0.2099 0.8678 -0.0515 0.0467 Uiso 1.0 4 calc R . . H16 H -0.1481 0.9593 -0.0870 0.0467 Uiso 1.0 4 calc R . . H17 H 0.2550 1.0750 0.3510 0.0390 Uiso 1.0 4 calc R . . H18 H 0.1972 1.2100 0.3607 0.0390 Uiso 1.0 4 calc R . . H19 H 0.2920 1.2405 0.3595 0.0390 Uiso 1.0 4 calc R . . H20 H 0.2015 1.4501 0.2325 0.0415 Uiso 1.0 4 calc R . . H21 H 0.1205 1.4175 0.1319 0.0415 Uiso 1.0 4 calc R . . H22 H 0.0775 1.5380 0.2412 0.0428 Uiso 1.0 4 calc R . . H23 H 0.1006 1.3877 0.2998 0.0428 Uiso 1.0 4 calc R . . H24 H -0.0366 1.4060 0.1111 0.0416 Uiso 1.0 4 calc R . . H25 H -0.0579 1.4257 0.1987 0.0416 Uiso 1.0 4 calc R . . H26 H -0.0334 1.0484 0.3050 0.0289 Uiso 1.0 4 calc R . . H27 H -0.0526 1.2199 0.3132 0.0289 Uiso 1.0 4 calc R . . H28 H 0.0477 1.1653 0.3381 0.0289 Uiso 1.0 4 calc R . . 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 Fe1 0.02145(16) 0.01663(14) 0.01618(15) -0.00175(12) 0.00981(13) -0.00189(12) S1 0.0313(4) 0.0266(4) 0.0243(3) -0.0119(3) 0.0164(3) -0.0085(3) S2 0.0269(4) 0.0196(3) 0.0177(3) 0.0052(3) 0.0096(3) 0.0006(3) Si1 0.0185(4) 0.0284(4) 0.0198(4) -0.0028(3) 0.0100(3) -0.0076(3) Si2 0.0176(4) 0.0199(4) 0.0234(4) -0.0010(3) 0.0081(3) -0.0036(3) O1 0.0398(12) 0.0262(10) 0.0303(11) 0.0074(9) 0.0163(10) 0.0089(8) O2 0.0600(15) 0.0297(11) 0.0226(10) 0.0027(9) 0.0193(10) 0.0007(8) C1 0.0195(12) 0.0231(13) 0.0227(12) 0.0012(10) 0.0096(11) -0.0048(10) C2 0.0328(15) 0.0203(12) 0.0248(14) -0.0032(11) 0.0159(13) -0.0051(11) C3 0.0249(13) 0.0186(11) 0.0135(11) 0.0015(10) 0.0080(10) 0.0017(9) C4 0.0312(14) 0.0226(13) 0.0186(12) 0.0028(10) 0.0134(11) 0.0025(10) C5 0.0477(17) 0.0191(12) 0.0203(13) 0.0069(12) 0.0175(13) 0.0023(10) C6 0.0406(16) 0.0165(11) 0.0235(13) -0.0036(11) 0.0131(12) -0.0011(10) C7 0.0273(14) 0.0212(12) 0.0204(12) -0.0044(10) 0.0083(11) 0.0011(10) C8 0.0266(13) 0.0162(11) 0.0145(11) -0.0003(10) 0.0068(11) 0.0013(9) C9 0.0225(14) 0.061(2) 0.0305(16) 0.0107(14) 0.0062(13) -0.0144(14) C10 0.0427(18) 0.0491(19) 0.0410(17) -0.0229(15) 0.0304(16) -0.0228(14) C11 0.0350(16) 0.0404(16) 0.0466(18) -0.0157(13) 0.0259(15) -0.0147(14) C12 0.0231(15) 0.0375(16) 0.0435(18) 0.0061(12) 0.0033(14) -0.0100(14) C13 0.0289(15) 0.0332(15) 0.0265(14) -0.0043(12) 0.0043(12) -0.0051(11) C14 0.054(2) 0.0247(14) 0.0270(14) -0.0136(13) 0.0199(14) -0.0010(11) C15 0.059(2) 0.0178(13) 0.0325(15) -0.0019(13) 0.0227(15) -0.0020(11) C16 0.053(2) 0.0198(13) 0.0328(15) 0.0100(12) 0.0206(14) 0.0057(11) C17 0.0298(14) 0.0255(13) 0.0197(12) 0.0057(11) 0.0133(11) 0.0027(10) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe1 S1 2.2864(8) yes . . Fe1 S2 2.2883(9) yes . . Fe1 Si1 2.3378(9) yes . . Fe1 Si2 2.3442(8) yes . . Fe1 C1 1.761(3) yes . . Fe1 C2 1.763(3) yes . . S1 C13 1.803(3) yes . . S1 C14 1.818(3) yes . . S2 C16 1.814(3) yes . . S2 C17 1.811(3) yes . . Si1 C3 1.900(3) yes . . Si1 C9 1.895(3) yes . . Si1 C10 1.885(5) yes . . Si2 C8 1.897(3) yes . . Si2 C11 1.887(4) yes . . Si2 C12 1.895(3) yes . . O1 C1 1.169(4) yes . . O2 C2 1.165(4) yes . . C3 C4 1.411(4) yes . . C3 C8 1.402(4) yes . . C4 C5 1.390(4) yes . . C5 C6 1.390(5) yes . . C6 C7 1.390(5) yes . . C7 C8 1.406(4) yes . . C14 C15 1.524(6) yes . . C15 C16 1.533(5) yes . . C4 H1 0.950 no . . C5 H2 0.950 no . . C6 H3 0.950 no . . C7 H4 0.950 no . . C9 H5 0.980 no . . C9 H6 0.980 no . . C9 H7 0.980 no . . C10 H8 0.980 no . . C10 H9 0.980 no . . C10 H10 0.980 no . . C11 H11 0.980 no . . C11 H12 0.980 no . . C11 H13 0.980 no . . C12 H14 0.980 no . . C12 H15 0.980 no . . C12 H16 0.980 no . . C13 H17 0.980 no . . C13 H18 0.980 no . . C13 H19 0.980 no . . C14 H20 0.990 no . . C14 H21 0.990 no . . C15 H22 0.990 no . . C15 H23 0.990 no . . C16 H24 0.990 no . . C16 H25 0.990 no . . C17 H26 0.980 no . . C17 H27 0.980 no . . C17 H28 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 S1 Fe1 S2 97.11(3) yes . . . S1 Fe1 Si1 87.33(4) yes . . . S1 Fe1 Si2 174.54(4) yes . . . S1 Fe1 C1 98.49(8) yes . . . S1 Fe1 C2 96.67(9) yes . . . S2 Fe1 Si1 175.55(3) yes . . . S2 Fe1 Si2 88.02(3) yes . . . S2 Fe1 C1 97.46(11) yes . . . S2 Fe1 C2 97.86(10) yes . . . Si1 Fe1 Si2 87.56(4) yes . . . Si1 Fe1 C1 81.49(10) yes . . . Si1 Fe1 C2 81.90(10) yes . . . Si2 Fe1 C1 82.64(8) yes . . . Si2 Fe1 C2 80.71(9) yes . . . C1 Fe1 C2 156.89(12) yes . . . Fe1 S1 C13 111.44(11) yes . . . Fe1 S1 C14 112.36(10) yes . . . C13 S1 C14 99.84(14) yes . . . Fe1 S2 C16 112.78(13) yes . . . Fe1 S2 C17 109.99(10) yes . . . C16 S2 C17 100.66(14) yes . . . Fe1 Si1 C3 107.41(10) yes . . . Fe1 Si1 C9 116.12(12) yes . . . Fe1 Si1 C10 115.62(11) yes . . . C3 Si1 C9 106.90(12) yes . . . C3 Si1 C10 107.44(13) yes . . . C9 Si1 C10 102.77(15) yes . . . Fe1 Si2 C8 107.08(9) yes . . . Fe1 Si2 C11 114.77(10) yes . . . Fe1 Si2 C12 116.31(10) yes . . . C8 Si2 C11 109.13(14) yes . . . C8 Si2 C12 106.33(13) yes . . . C11 Si2 C12 102.80(15) yes . . . Fe1 C1 O1 178.1(3) yes . . . Fe1 C2 O2 176.6(3) yes . . . Si1 C3 C4 121.6(2) yes . . . Si1 C3 C8 118.66(19) yes . . . C4 C3 C8 119.7(2) yes . . . C3 C4 C5 120.9(3) yes . . . C4 C5 C6 119.4(3) yes . . . C5 C6 C7 120.1(3) yes . . . C6 C7 C8 121.5(3) yes . . . Si2 C8 C3 119.26(17) yes . . . Si2 C8 C7 122.3(3) yes . . . C3 C8 C7 118.4(3) yes . . . S1 C14 C15 116.7(3) yes . . . C14 C15 C16 115.5(3) yes . . . S2 C16 C15 117.26(19) yes . . . C3 C4 H1 119.531 no . . . C5 C4 H1 119.544 no . . . C4 C5 H2 120.286 no . . . C6 C5 H2 120.296 no . . . C5 C6 H3 119.976 no . . . C7 C6 H3 119.963 no . . . C6 C7 H4 119.253 no . . . C8 C7 H4 119.258 no . . . Si1 C9 H5 109.472 no . . . Si1 C9 H6 109.476 no . . . Si1 C9 H7 109.475 no . . . H5 C9 H6 109.467 no . . . H5 C9 H7 109.468 no . . . H6 C9 H7 109.469 no . . . Si1 C10 H8 109.463 no . . . Si1 C10 H9 109.472 no . . . Si1 C10 H10 109.474 no . . . H8 C10 H9 109.474 no . . . H8 C10 H10 109.475 no . . . H9 C10 H10 109.470 no . . . Si2 C11 H11 109.476 no . . . Si2 C11 H12 109.468 no . . . Si2 C11 H13 109.472 no . . . H11 C11 H12 109.468 no . . . H11 C11 H13 109.473 no . . . H12 C11 H13 109.470 no . . . Si2 C12 H14 109.478 no . . . Si2 C12 H15 109.471 no . . . Si2 C12 H16 109.473 no . . . H14 C12 H15 109.469 no . . . H14 C12 H16 109.467 no . . . H15 C12 H16 109.469 no . . . S1 C13 H17 109.464 no . . . S1 C13 H18 109.472 no . . . S1 C13 H19 109.469 no . . . H17 C13 H18 109.474 no . . . H17 C13 H19 109.471 no . . . H18 C13 H19 109.476 no . . . S1 C14 H20 108.125 no . . . S1 C14 H21 108.130 no . . . C15 C14 H20 108.126 no . . . C15 C14 H21 108.128 no . . . H20 C14 H21 107.315 no . . . C14 C15 H22 108.408 no . . . C14 C15 H23 108.410 no . . . C16 C15 H22 108.402 no . . . C16 C15 H23 108.401 no . . . H22 C15 H23 107.464 no . . . S2 C16 H24 107.985 no . . . S2 C16 H25 107.980 no . . . C15 C16 H24 107.996 no . . . C15 C16 H25 107.984 no . . . H24 C16 H25 107.236 no . . . S2 C17 H26 109.474 no . . . S2 C17 H27 109.475 no . . . S2 C17 H28 109.483 no . . . H26 C17 H27 109.467 no . . . H26 C17 H28 109.464 no . . . H27 C17 H28 109.466 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 S1 Fe1 S2 C16 31.21(4) no . . . . S1 Fe1 S2 C17 -80.27(4) no . . . . S2 Fe1 S1 C13 78.96(4) no . . . . S2 Fe1 S1 C14 -32.15(4) no . . . . S1 Fe1 Si1 C3 -176.38(3) no . . . . S1 Fe1 Si1 C9 64.08(4) no . . . . S1 Fe1 Si1 C10 -56.46(3) no . . . . Si1 Fe1 S1 C13 -100.70(4) no . . . . Si1 Fe1 S1 C14 148.19(4) no . . . . C1 Fe1 S1 C13 -19.72(11) no . . . . C1 Fe1 S1 C14 -130.82(11) no . . . . C2 Fe1 S1 C13 177.78(10) no . . . . C2 Fe1 S1 C14 66.67(11) no . . . . S2 Fe1 Si2 C8 178.69(4) no . . . . S2 Fe1 Si2 C11 -60.03(4) no . . . . S2 Fe1 Si2 C12 59.99(5) no . . . . Si2 Fe1 S2 C16 -146.90(3) no . . . . Si2 Fe1 S2 C17 101.62(4) no . . . . C1 Fe1 S2 C16 130.79(8) no . . . . C1 Fe1 S2 C17 19.31(8) no . . . . C2 Fe1 S2 C16 -66.57(9) no . . . . C2 Fe1 S2 C17 -178.05(9) no . . . . Si1 Fe1 Si2 C8 -1.80(4) no . . . . Si1 Fe1 Si2 C11 119.49(4) no . . . . Si1 Fe1 Si2 C12 -120.49(5) no . . . . Si2 Fe1 Si1 C3 1.70(4) no . . . . Si2 Fe1 Si1 C9 -117.84(4) no . . . . Si2 Fe1 Si1 C10 121.62(4) no . . . . C1 Fe1 Si1 C3 84.62(8) no . . . . C1 Fe1 Si1 C9 -34.92(8) no . . . . C1 Fe1 Si1 C10 -155.46(8) no . . . . C2 Fe1 Si1 C3 -79.25(9) no . . . . C2 Fe1 Si1 C9 161.21(10) no . . . . C2 Fe1 Si1 C10 40.67(9) no . . . . C1 Fe1 Si2 C8 -83.53(11) no . . . . C1 Fe1 Si2 C11 37.75(11) no . . . . C1 Fe1 Si2 C12 157.78(11) no . . . . C2 Fe1 Si2 C8 80.39(11) no . . . . C2 Fe1 Si2 C11 -158.33(11) no . . . . C2 Fe1 Si2 C12 -38.31(11) no . . . . Fe1 S1 C14 C15 53.54(17) no . . . . C13 S1 C14 C15 -64.66(19) no . . . . Fe1 S2 C16 C15 -51.0(3) no . . . . C17 S2 C16 C15 66.1(3) no . . . . Fe1 Si1 C3 C4 177.35(13) no . . . . Fe1 Si1 C3 C8 -1.26(17) no . . . . C9 Si1 C3 C4 -57.4(3) no . . . . C9 Si1 C3 C8 124.01(18) no . . . . C10 Si1 C3 C4 52.36(19) no . . . . C10 Si1 C3 C8 -126.25(18) no . . . . Fe1 Si2 C8 C3 1.63(18) no . . . . Fe1 Si2 C8 C7 -175.90(15) no . . . . C11 Si2 C8 C3 -123.15(18) no . . . . C11 Si2 C8 C7 59.3(2) no . . . . C12 Si2 C8 C3 126.60(18) no . . . . C12 Si2 C8 C7 -50.9(3) no . . . . Si1 C3 C4 C5 -177.95(15) no . . . . Si1 C3 C8 Si2 -0.3(3) no . . . . Si1 C3 C8 C7 177.38(14) no . . . . C4 C3 C8 Si2 -178.89(18) no . . . . C4 C3 C8 C7 -1.3(4) no . . . . C8 C3 C4 C5 0.6(4) no . . . . C3 C4 C5 C6 0.3(4) no . . . . C4 C5 C6 C7 -0.6(4) no . . . . C5 C6 C7 C8 0.0(4) no . . . . C6 C7 C8 Si2 178.5(2) no . . . . C6 C7 C8 C3 1.0(4) no . . . . S1 C14 C15 C16 -72.1(3) no . . . . C14 C15 C16 S2 70.8(4) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S1 C16 3.489(4) no . . S2 C14 3.486(4) no . . Si1 O1 3.449(3) no . . Si1 O2 3.456(2) no . . Si2 O1 3.4900(19) no . . Si2 O2 3.401(3) no . . O1 C9 3.257(5) no . . O1 C11 3.317(4) no . . O2 C10 3.354(5) no . . O2 C12 3.255(5) no . . C1 C3 3.567(4) no . . C1 C8 3.575(4) no . . C1 C9 3.090(5) no . . C1 C11 3.117(4) no . . C1 C13 3.259(4) no . . C1 C17 3.189(5) no . . C2 C3 3.495(4) no . . C2 C8 3.479(4) no . . C2 C10 3.141(5) no . . C2 C12 3.111(5) no . . C3 C6 2.798(4) no . . C4 C7 2.769(5) no . . C4 C9 3.544(4) no . . C4 C10 3.508(4) no . . C5 C8 2.820(5) no . . C7 C12 3.480(5) no . . C13 C15 3.292(4) no . . C15 C17 3.345(5) no . . O2 C5 3.494(4) no . 1_565 O2 C6 3.318(4) no . 1_565 O2 C17 3.403(4) no . 2_574 C4 C14 3.594(4) no . 1_545 C5 O2 3.494(4) no . 1_545 C5 C15 3.565(5) no . 2_574 C6 O2 3.318(4) no . 1_545 C14 C4 3.594(4) no . 1_565 C15 C5 3.565(5) no . 2_575 C17 O2 3.403(4) no . 2_575 Fe1 H17 3.4535 no . . Fe1 H18 3.5371 no . . Fe1 H21 3.5882 no . . Fe1 H26 3.5434 no . . Fe1 H28 3.3947 no . . S1 H5 3.2652 no . . S1 H8 3.1950 no . . S1 H23 2.9293 no . . S2 H12 3.1616 no . . S2 H14 3.1955 no . . S2 H23 2.9567 no . . Si1 H1 2.9825 no . . Si2 H4 2.9859 no . . O1 H5 3.4042 no . . O1 H7 2.6538 no . . O1 H12 3.4749 no . . O1 H13 2.7051 no . . O1 H17 3.0884 no . . O1 H26 3.1670 no . . O1 H28 3.3904 no . . O2 H9 2.6201 no . . O2 H14 3.3656 no . . O2 H16 2.7011 no . . C1 H5 3.2164 no . . C1 H7 2.8118 no . . C1 H12 3.2438 no . . C1 H13 2.8290 no . . C1 H17 2.8880 no . . C1 H18 3.3210 no . . C1 H26 2.9829 no . . C1 H28 3.0528 no . . C2 H8 3.4965 no . . C2 H9 2.7152 no . . C2 H14 3.1904 no . . C2 H16 2.8881 no . . C2 H21 3.3758 no . . C2 H24 3.4393 no . . C3 H2 3.2949 no . . C3 H4 3.2684 no . . C3 H6 3.2342 no . . C3 H7 3.1470 no . . C3 H9 3.2676 no . . C3 H10 3.1237 no . . C4 H3 3.2599 no . . C4 H6 3.3280 no . . C4 H10 3.1623 no . . C5 H4 3.2610 no . . C6 H1 3.2573 no . . C7 H2 3.2674 no . . C7 H11 3.4262 no . . C7 H15 3.3403 no . . C7 H16 3.4885 no . . C8 H1 3.2869 no . . C8 H3 3.2923 no . . C8 H11 3.2807 no . . C8 H13 3.1854 no . . C8 H15 3.2762 no . . C8 H16 3.0814 no . . C9 H1 3.2903 no . . C9 H8 3.0649 no . . C9 H10 3.0934 no . . C9 H17 3.3457 no . . C10 H1 3.2450 no . . C10 H5 3.1897 no . . C10 H6 2.9831 no . . C11 H4 3.3829 no . . C11 H14 3.2372 no . . C11 H15 2.9487 no . . C11 H26 3.2925 no . . C12 H4 3.2048 no . . C12 H11 2.9747 no . . C12 H12 3.1995 no . . C13 H5 3.2811 no . . C13 H20 2.8577 no . . C13 H23 2.8134 no . . C13 H28 3.1711 no . . C14 H18 2.8412 no . . C14 H19 2.9455 no . . C14 H24 2.7176 no . . C14 H25 3.3950 no . . C15 H18 2.8726 no . . C15 H27 3.4908 no . . C15 H28 3.0586 no . . C16 H20 3.3961 no . . C16 H21 2.7076 no . . C16 H27 2.8511 no . . C16 H28 2.9842 no . . C17 H12 3.2310 no . . C17 H18 3.2595 no . . C17 H23 2.8843 no . . C17 H25 2.8650 no . . H1 H2 2.3377 no . . H1 H6 2.8347 no . . H1 H7 3.5641 no . . H1 H10 2.6837 no . . H2 H3 2.3442 no . . H3 H4 2.3286 no . . H4 H11 2.9547 no . . H4 H15 2.8125 no . . H4 H16 3.3452 no . . H5 H8 2.9934 no . . H5 H10 3.4629 no . . H5 H17 2.6122 no . . H6 H8 3.1378 no . . H6 H10 2.8082 no . . H7 H17 3.4469 no . . H11 H14 3.3557 no . . H11 H15 2.6436 no . . H12 H14 3.1802 no . . H12 H15 3.2661 no . . H12 H26 2.5411 no . . H13 H26 3.3694 no . . H17 H28 3.4387 no . . H18 H20 3.0048 no . . H18 H23 2.1674 no . . H18 H28 2.3674 no . . H19 H20 2.6908 no . . H19 H23 3.1636 no . . H20 H22 2.2570 no . . H20 H23 2.4147 no . . H20 H24 3.5519 no . . H21 H22 2.4117 no . . H21 H23 2.8486 no . . H21 H24 2.4674 no . . H21 H25 3.5504 no . . H22 H24 2.4097 no . . H22 H25 2.2698 no . . H23 H24 2.8556 no . . H23 H25 2.4138 no . . H23 H27 3.0391 no . . H23 H28 2.3794 no . . H25 H27 2.5806 no . . H25 H28 3.1759 no . . S2 H6 2.9499 no . 3_455 O1 H2 3.1619 no . 2_565 O1 H9 2.9726 no . 2_575 O1 H15 3.3566 no . 4_565 O1 H22 2.7447 no . 1_545 O2 H2 3.1304 no . 1_565 O2 H3 2.7921 no . 1_565 O2 H19 3.2848 no . 4_474 O2 H26 2.6320 no . 2_574 O2 H28 3.4617 no . 2_574 C1 H9 3.5452 no . 2_575 C1 H22 3.4113 no . 1_545 C2 H3 3.4869 no . 1_565 C2 H26 3.4823 no . 2_574 C3 H21 3.0771 no . 1_545 C3 H27 3.2890 no . 2_574 C3 H28 3.1298 no . 2_574 C4 H14 3.5600 no . 3_545 C4 H18 3.4632 no . 2_574 C4 H21 2.7133 no . 1_545 C4 H23 3.0837 no . 2_574 C4 H27 3.3947 no . 2_574 C4 H28 3.0654 no . 2_574 C5 H21 2.7574 no . 1_545 C5 H22 3.4197 no . 2_574 C5 H23 2.8945 no . 2_574 C5 H27 3.3297 no . 2_574 C5 H28 3.4759 no . 2_574 C6 H5 3.2901 no . 4_464 C6 H17 3.2655 no . 4_464 C6 H19 3.3808 no . 4_464 C6 H21 3.1420 no . 1_545 C6 H24 3.0456 no . 1_545 C6 H25 3.5749 no . 2_574 C6 H27 3.1273 no . 2_574 C7 H5 3.2233 no . 4_464 C7 H17 3.1522 no . 4_464 C7 H21 3.4412 no . 1_545 C7 H24 2.7722 no . 1_545 C7 H27 3.0060 no . 2_574 C8 H21 3.4222 no . 1_545 C8 H22 3.5407 no . 1_545 C8 H24 3.2743 no . 1_545 C8 H27 3.1112 no . 2_574 C9 H20 3.3826 no . 1_545 C9 H25 3.3565 no . 3_545 C9 H27 2.9678 no . 3_545 C10 H11 3.0917 no . 3_555 C10 H17 3.3829 no . 2_574 C10 H18 3.1502 no . 2_574 C10 H28 3.2673 no . 2_574 C11 H8 3.0846 no . 3_445 C11 H22 3.4857 no . 1_545 C11 H25 3.3475 no . 1_545 C12 H1 3.4395 no . 3_455 C12 H7 3.5689 no . 4_464 C12 H19 3.2585 no . 4_474 C12 H20 3.5336 no . 4_474 C13 H3 3.0460 no . 4_565 C13 H4 3.3220 no . 4_565 C13 H10 2.9417 no . 2_575 C13 H14 3.3838 no . 4_575 C14 H7 3.4026 no . 1_565 C15 H2 3.2243 no . 2_575 C15 H13 3.3443 no . 1_565 C16 H6 3.4082 no . 3_455 C16 H13 3.2478 no . 1_565 C17 H6 3.0058 no . 3_455 C17 H9 3.3894 no . 2_575 C17 H16 3.5593 no . 2_575 H1 C12 3.4395 no . 3_545 H1 H14 2.6802 no . 3_545 H1 H15 3.3409 no . 3_545 H1 H18 3.0105 no . 2_574 H1 H21 3.0592 no . 1_545 H1 H23 3.0254 no . 2_574 H1 H28 3.2961 no . 2_574 H2 O1 3.1619 no . 2_564 H2 O2 3.1304 no . 1_545 H2 C15 3.2243 no . 2_574 H2 H13 3.5821 no . 2_564 H2 H15 3.2619 no . 3_545 H2 H21 3.1228 no . 1_545 H2 H22 2.8579 no . 2_574 H2 H23 2.7030 no . 2_574 H2 H25 3.5652 no . 2_574 H3 O2 2.7921 no . 1_545 H3 C2 3.4869 no . 1_545 H3 C13 3.0460 no . 4_464 H3 H5 3.0622 no . 4_464 H3 H13 3.4709 no . 2_564 H3 H17 2.7105 no . 4_464 H3 H19 2.5566 no . 4_464 H3 H24 3.2826 no . 1_545 H3 H25 3.4846 no . 2_574 H3 H27 3.5976 no . 2_574 H4 C13 3.3220 no . 4_464 H4 H5 2.9343 no . 4_464 H4 H7 3.4677 no . 4_464 H4 H8 3.3662 no . 3_445 H4 H10 3.3993 no . 3_445 H4 H17 2.4653 no . 4_464 H4 H19 3.3948 no . 4_464 H4 H24 2.8449 no . 1_545 H4 H27 3.4190 no . 2_574 H5 C6 3.2901 no . 4_565 H5 C7 3.2233 no . 4_565 H5 H3 3.0622 no . 4_565 H5 H4 2.9343 no . 4_565 H5 H25 2.9734 no . 3_545 H5 H27 2.7584 no . 3_545 H6 S2 2.9499 no . 3_545 H6 C16 3.4082 no . 3_545 H6 C17 3.0058 no . 3_545 H6 H20 3.3263 no . 1_545 H6 H25 2.8877 no . 3_545 H6 H26 3.2267 no . 3_545 H6 H27 2.4964 no . 3_545 H7 C12 3.5689 no . 4_565 H7 C14 3.4026 no . 1_545 H7 H4 3.4677 no . 4_565 H7 H15 3.1225 no . 4_565 H7 H16 3.0937 no . 4_565 H7 H20 2.6401 no . 1_545 H7 H21 3.4746 no . 1_545 H7 H22 3.1398 no . 1_545 H7 H27 3.1927 no . 3_545 H8 C11 3.0846 no . 3_555 H8 H4 3.3662 no . 3_555 H8 H11 2.1470 no . 3_555 H8 H12 3.5435 no . 3_555 H8 H13 3.3432 no . 3_555 H8 H24 3.5359 no . 3_545 H8 H25 3.1198 no . 3_545 H9 O1 2.9726 no . 2_574 H9 C1 3.5452 no . 2_574 H9 C17 3.3894 no . 2_574 H9 H11 3.4112 no . 3_555 H9 H17 3.2263 no . 2_574 H9 H18 3.0593 no . 2_574 H9 H26 3.1808 no . 2_574 H9 H28 2.7232 no . 2_574 H10 C13 2.9417 no . 2_574 H10 H4 3.3993 no . 3_555 H10 H11 3.4791 no . 3_555 H10 H17 2.7617 no . 2_574 H10 H18 2.4026 no . 2_574 H10 H19 3.2331 no . 2_574 H10 H24 3.4217 no . 3_545 H10 H25 3.4329 no . 3_545 H10 H28 3.1269 no . 2_574 H11 C10 3.0917 no . 3_445 H11 H8 2.1470 no . 3_445 H11 H9 3.4112 no . 3_445 H11 H10 3.4791 no . 3_445 H11 H24 3.4696 no . 1_545 H11 H25 3.1391 no . 1_545 H12 H8 3.5435 no . 3_445 H12 H20 3.5050 no . 3_445 H13 C15 3.3443 no . 1_545 H13 C16 3.2478 no . 1_545 H13 H2 3.5821 no . 2_565 H13 H3 3.4709 no . 2_565 H13 H8 3.3432 no . 3_445 H13 H22 2.6066 no . 1_545 H13 H24 3.2325 no . 1_545 H13 H25 2.6847 no . 1_545 H14 C4 3.5600 no . 3_455 H14 C13 3.3838 no . 4_474 H14 H1 2.6802 no . 3_455 H14 H18 3.1316 no . 4_474 H14 H19 2.7438 no . 4_474 H14 H23 3.5753 no . 4_474 H15 O1 3.3566 no . 4_464 H15 H1 3.3409 no . 3_455 H15 H2 3.2619 no . 3_455 H15 H7 3.1225 no . 4_464 H15 H20 3.4976 no . 4_474 H16 C17 3.5593 no . 2_574 H16 H7 3.0937 no . 4_464 H16 H19 2.8858 no . 4_474 H16 H20 2.9629 no . 4_474 H16 H26 3.0755 no . 2_574 H16 H27 3.1425 no . 2_574 H17 C6 3.2655 no . 4_565 H17 C7 3.1522 no . 4_565 H17 C10 3.3829 no . 2_575 H17 H3 2.7105 no . 4_565 H17 H4 2.4653 no . 4_565 H17 H9 3.2263 no . 2_575 H17 H10 2.7617 no . 2_575 H18 C4 3.4632 no . 2_575 H18 C10 3.1502 no . 2_575 H18 H1 3.0105 no . 2_575 H18 H9 3.0593 no . 2_575 H18 H10 2.4026 no . 2_575 H18 H14 3.1316 no . 4_575 H19 O2 3.2848 no . 4_575 H19 C6 3.3808 no . 4_565 H19 C12 3.2585 no . 4_575 H19 H3 2.5566 no . 4_565 H19 H4 3.3948 no . 4_565 H19 H10 3.2331 no . 2_575 H19 H14 2.7438 no . 4_575 H19 H16 2.8858 no . 4_575 H20 C9 3.3826 no . 1_565 H20 C12 3.5336 no . 4_575 H20 H6 3.3263 no . 1_565 H20 H7 2.6401 no . 1_565 H20 H12 3.5050 no . 3_555 H20 H15 3.4976 no . 4_575 H20 H16 2.9629 no . 4_575 H21 C3 3.0771 no . 1_565 H21 C4 2.7133 no . 1_565 H21 C5 2.7574 no . 1_565 H21 C6 3.1420 no . 1_565 H21 C7 3.4412 no . 1_565 H21 C8 3.4222 no . 1_565 H21 H1 3.0592 no . 1_565 H21 H2 3.1228 no . 1_565 H21 H7 3.4746 no . 1_565 H22 O1 2.7447 no . 1_565 H22 C1 3.4113 no . 1_565 H22 C5 3.4197 no . 2_575 H22 C8 3.5407 no . 1_565 H22 C11 3.4857 no . 1_565 H22 H2 2.8579 no . 2_575 H22 H7 3.1398 no . 1_565 H22 H13 2.6066 no . 1_565 H23 C4 3.0837 no . 2_575 H23 C5 2.8945 no . 2_575 H23 H1 3.0254 no . 2_575 H23 H2 2.7030 no . 2_575 H23 H14 3.5753 no . 4_575 H24 C6 3.0456 no . 1_565 H24 C7 2.7722 no . 1_565 H24 C8 3.2743 no . 1_565 H24 H3 3.2826 no . 1_565 H24 H4 2.8449 no . 1_565 H24 H8 3.5359 no . 3_455 H24 H10 3.4217 no . 3_455 H24 H11 3.4696 no . 1_565 H24 H13 3.2325 no . 1_565 H25 C6 3.5749 no . 2_575 H25 C9 3.3565 no . 3_455 H25 C11 3.3475 no . 1_565 H25 H2 3.5652 no . 2_575 H25 H3 3.4846 no . 2_575 H25 H5 2.9734 no . 3_455 H25 H6 2.8877 no . 3_455 H25 H8 3.1198 no . 3_455 H25 H10 3.4329 no . 3_455 H25 H11 3.1391 no . 1_565 H25 H13 2.6847 no . 1_565 H26 O2 2.6320 no . 2_575 H26 C2 3.4823 no . 2_575 H26 H6 3.2267 no . 3_455 H26 H9 3.1808 no . 2_575 H26 H16 3.0755 no . 2_575 H27 C3 3.2890 no . 2_575 H27 C4 3.3947 no . 2_575 H27 C5 3.3297 no . 2_575 H27 C6 3.1273 no . 2_575 H27 C7 3.0060 no . 2_575 H27 C8 3.1112 no . 2_575 H27 C9 2.9678 no . 3_455 H27 H3 3.5976 no . 2_575 H27 H4 3.4190 no . 2_575 H27 H5 2.7584 no . 3_455 H27 H6 2.4964 no . 3_455 H27 H7 3.1927 no . 3_455 H27 H16 3.1425 no . 2_575 H28 O2 3.4617 no . 2_575 H28 C3 3.1298 no . 2_575 H28 C4 3.0654 no . 2_575 H28 C5 3.4759 no . 2_575 H28 C10 3.2673 no . 2_575 H28 H1 3.2961 no . 2_575 H28 H9 2.7232 no . 2_575 H28 H10 3.1269 no . 2_575 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 947205'