Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 2004-03-06 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? _publ_contact_author_name 'Hiroyuki Kawaguchi' _publ_contact_author_address ; Coordination Chemistry Laboratories Institute for Molecular Science Myodaiji Okazaki 444-8585 JAPAN ; _publ_contact_author_email hkawa@ims.ac.jp _publ_contact_author_fax +81-564-55-5245 _publ_contact_author_phone +81-564-55-7290 _publ_section_title ; Synthesis and structural characterization of silanethiolato complexes having tert-butyldimethylsilyl and trimethylsilyl groups ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; loop_ _publ_author_name 'Hiroyuki Kawaguchi' 'Takashi Komuro' 'Tsukasa Matsuo' 'Kazuyuki Tatsumi' #============================================================================== data_[Li(tmeda)(SSiMe2tBu)]2 _database_code_depnum_ccdc_archive 'CCDC 227191' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H62 Li2 N4 S2 Si2 ' _chemical_formula_moiety '[Li(tmeda)(SSiMe2tBu)]2' _chemical_formula_weight 540.95 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c 21 ' _symmetry_space_group_name_Hall 'C 2c -2' _symmetry_Int_Tables_number 36 loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z -x,y,z -x+1/2,y+1/2,z x,-y,z+1/2 x+1/2,-y+1/2,z+1/2 -x,-y,z+1/2 -x+1/2,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 16.9833(7) _cell_length_b 15.8113(4) _cell_length_c 13.6271(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3659.3(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6663 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 0.982 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200.00 _exptl_absorpt_coefficient_mu 0.227 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.32 _diffrn_reflns_number 33628 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9906 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9889 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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 4451 _reflns_number_gt 3525 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1680 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4290 _refine_ls_number_parameters 209 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0039Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.08 _refine_diff_density_min -0.46 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 0 Friedel Pairs' _refine_ls_abs_structure_Flack 0.07(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Li Li 0.000 0.000 ; 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 S(1) S -0.39853(4) -0.84971(4) -0.10223(10) 0.0517(2) Uani 1.00 1 d . . . Si(1) Si -0.27691(4) -0.84044(5) -0.11606(9) 0.0506(2) Uani 1.00 1 d . . . N(1) N -0.5000 -1.0439(2) -0.2395(2) 0.0514(9) Uani 1.00 1 d . . . N(2) N -0.5000 -0.8926(2) -0.3588(2) 0.0551(10) Uani 1.00 1 d . . . N(3) N -0.5000 -0.6285(2) -0.1616(3) 0.0506(9) Uani 1.00 1 d . . . N(4) N -0.5000 -0.6685(2) 0.0491(3) 0.0520(9) Uani 1.00 1 d . . . C(1) C -0.2400(3) -0.8932(5) -0.2296(3) 0.105(2) Uani 1.00 1 d . . . C(2) C -0.2422(2) -0.7267(3) -0.1179(6) 0.118(2) Uani 1.00 1 d . . . C(3) C -0.2258(2) -0.8912(2) -0.0069(2) 0.0569(8) Uani 1.00 1 d . . . C(4) C -0.1362(2) -0.8803(3) -0.0156(4) 0.0824(12) Uani 1.00 1 d . . . C(5) C -0.2547(3) -0.8512(4) 0.0879(3) 0.097(2) Uani 1.00 1 d . . . C(6) C -0.2466(3) -0.9861(3) -0.0085(4) 0.0822(12) Uani 1.00 1 d . . . C(7) C -0.4300(3) -1.0850(3) -0.2004(4) 0.0822(13) Uani 1.00 1 d . . . C(8) C -0.5178(6) -1.0465(4) -0.3457(3) 0.061(3) Uani 0.50 1 d P . . C(9) C -0.4728(4) -0.9752(4) -0.3960(4) 0.067(2) Uani 0.50 1 d P . . C(10) C -0.5692(4) -0.8487(5) -0.3918(4) 0.135(3) Uani 1.00 1 d . . . C(11) C -0.5693(4) -0.6156(4) -0.2188(6) 0.128(2) Uani 1.00 1 d . . . C(12) C -0.4773(4) -0.5686(4) -0.0839(6) 0.070(2) Uani 0.50 1 d P . . C(13) C -0.5199(4) -0.5841(4) 0.0107(5) 0.064(2) Uani 0.50 1 d P . . C(14) C -0.4324(3) -0.6831(4) 0.1089(4) 0.104(2) Uani 1.00 1 d . . . Li(1) Li -0.5000 -0.9122(4) -0.2045(4) 0.044(2) Uani 1.00 1 d . . . Li(2) Li -0.5000 -0.7460(4) -0.0789(4) 0.047(2) Uani 1.00 1 d . . . H(1) H -0.1835 -0.8857 -0.2348 0.127 Uiso 1.00 1 c . . . H(2) H -0.2654 -0.8691 -0.2869 0.127 Uiso 1.00 1 c . . . H(3) H -0.2521 -0.9530 -0.2256 0.127 Uiso 1.00 1 c . . . H(4) H -0.2567 -0.6986 -0.0573 0.141 Uiso 1.00 1 c . . . H(5) H -0.2667 -0.6979 -0.1728 0.141 Uiso 1.00 1 c . . . H(6) H -0.1854 -0.7253 -0.1256 0.141 Uiso 1.00 1 c . . . H(7) H -0.1228 -0.8206 -0.0151 0.099 Uiso 1.00 1 c . . . H(8) H -0.1182 -0.9055 -0.0765 0.099 Uiso 1.00 1 c . . . H(9) H -0.1108 -0.9082 0.0393 0.099 Uiso 1.00 1 c . . . H(10) H -0.3114 -0.8579 0.0928 0.116 Uiso 1.00 1 c . . . H(11) H -0.2416 -0.7915 0.0886 0.116 Uiso 1.00 1 c . . . H(12) H -0.2296 -0.8791 0.1430 0.116 Uiso 1.00 1 c . . . H(13) H -0.2207 -1.0136 0.0463 0.099 Uiso 1.00 1 c . . . H(14) H -0.2285 -1.0110 -0.0695 0.099 Uiso 1.00 1 c . . . H(15) H -0.3031 -0.9934 -0.0029 0.098 Uiso 1.00 1 c . . . H(16) H -0.4278 -1.0771 -0.1298 0.099 Uiso 1.00 1 c . . . H(17) H -0.3834 -1.0606 -0.2302 0.099 Uiso 1.00 1 c . . . H(18) H -0.4323 -1.1449 -0.2151 0.099 Uiso 1.00 1 c . . . H(19) H -0.6152 -0.8834 -0.3796 0.162 Uiso 1.00 1 c . . . H(20) H -0.5647 -0.8375 -0.4616 0.162 Uiso 1.00 1 c . . . H(21) H -0.5743 -0.7956 -0.3567 0.162 Uiso 1.00 1 c . . . H(22) H -0.6152 -0.6139 -0.1766 0.153 Uiso 1.00 1 c . . . H(23) H -0.5743 -0.6621 -0.2648 0.153 Uiso 1.00 1 c . . . H(24) H -0.5651 -0.5628 -0.2547 0.153 Uiso 1.00 1 c . . . H(25) H -0.4359 -0.6486 0.1676 0.125 Uiso 1.00 1 c . . . H(26) H -0.3855 -0.6679 0.0723 0.125 Uiso 1.00 1 c . . . H(27) H -0.4298 -0.7423 0.1272 0.125 Uiso 1.00 1 c . . . 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 S(1) 0.0330(3) 0.0593(4) 0.0627(4) 0.0024(2) -0.0026(3) -0.0182(3) Si(1) 0.0352(3) 0.0633(4) 0.0531(4) -0.0023(3) 0.0021(3) 0.0054(4) N(1) 0.070(2) 0.046(2) 0.038(1) 0.0000 0.0000 -0.0031(13) N(2) 0.078(3) 0.047(2) 0.040(2) 0.0000 0.0000 -0.0057(13) N(3) 0.051(2) 0.045(2) 0.055(2) 0.0000 0.0000 -0.000(1) N(4) 0.053(2) 0.049(2) 0.055(2) 0.0000 0.0000 -0.011(1) C(1) 0.063(3) 0.190(6) 0.063(2) 0.014(3) 0.015(2) -0.019(3) C(2) 0.066(2) 0.072(2) 0.215(7) -0.017(2) -0.004(4) 0.055(4) C(3) 0.048(2) 0.063(2) 0.060(2) 0.0108(12) -0.0038(13) -0.0037(13) C(4) 0.050(2) 0.091(3) 0.106(3) 0.015(2) -0.023(2) -0.021(2) C(5) 0.085(3) 0.150(5) 0.056(2) 0.039(3) -0.015(2) -0.025(2) C(6) 0.078(2) 0.066(2) 0.102(3) 0.014(2) 0.010(2) 0.021(2) C(7) 0.084(3) 0.075(2) 0.088(3) 0.014(2) -0.008(2) -0.014(2) C(8) 0.096(11) 0.052(3) 0.035(2) -0.004(3) -0.006(3) -0.009(2) C(9) 0.100(7) 0.059(3) 0.043(3) -0.002(3) 0.024(3) -0.000(2) C(10) 0.133(6) 0.212(9) 0.060(2) 0.080(5) -0.011(3) 0.003(3) C(11) 0.115(4) 0.100(4) 0.168(6) -0.024(3) -0.071(4) 0.054(4) C(12) 0.077(6) 0.048(3) 0.084(4) -0.012(3) -0.006(3) -0.007(3) C(13) 0.069(7) 0.047(3) 0.077(4) 0.007(3) -0.011(3) -0.015(2) C(14) 0.079(3) 0.122(4) 0.111(4) 0.020(3) -0.034(3) -0.049(3) Li(1) 0.045(3) 0.044(3) 0.042(3) 0.0000 0.0000 -0.001(2) Li(2) 0.060(4) 0.034(3) 0.048(3) 0.0000 0.0000 -0.004(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; 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 S(1) Si(1) 2.079(1) yes . . S(1) Li(1) 2.426(4) yes . . S(1) Li(2) 2.400(4) yes . . Si(1) C(1) 1.866(5) yes . . Si(1) C(2) 1.893(4) yes . . Si(1) C(3) 1.901(3) yes . . N(1) C(7) 1.456(5) yes . . N(1) C(8) 1.479(6) yes . . N(1) Li(1) 2.137(7) yes . . N(2) C(9) 1.475(7) yes . . N(2) C(10) 1.437(7) yes . . N(2) Li(1) 2.125(7) yes . . N(3) C(11) 1.426(7) yes . . N(3) C(12) 1.472(7) yes . . N(3) Li(2) 2.173(7) yes . . N(4) C(13) 1.472(7) yes . . N(4) C(14) 1.427(6) yes . . N(4) Li(2) 2.132(7) yes . . C(3) C(4) 1.536(5) yes . . C(3) C(5) 1.519(6) yes . . C(3) C(6) 1.541(5) yes . . C(8) C(9) 1.52(1) yes . . C(12) C(13) 1.50(1) yes . . 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 Si(1) S(1) Li(1) 133.0(1) yes . . . Si(1) S(1) Li(2) 132.6(1) yes . . . Li(1) S(1) Li(2) 81.0(2) yes . . . C(1) Si(1) C(2) 108.0(3) yes . . . C(1) Si(1) C(3) 107.9(2) yes . . . C(1) Si(1) S(1) 112.2(2) yes . . . C(2) Si(1) C(3) 105.6(2) yes . . . C(2) Si(1) S(1) 112.2(1) yes . . . C(3) Si(1) S(1) 110.7(1) yes . . . C(7) N(1) C(8) 120.9(4) yes . . . C(7) N(1) Li(1) 110.7(2) yes . . . C(8) N(1) Li(1) 104.2(3) yes . . . C(9) N(2) C(10) 125.2(4) yes . . . C(9) N(2) Li(1) 102.2(3) yes . . . C(10) N(2) Li(1) 112.3(3) yes . . . C(11) N(3) C(12) 121.2(4) yes . . . C(11) N(3) Li(2) 113.9(3) yes . . . C(12) N(3) Li(2) 100.2(3) yes . . . C(13) N(4) C(14) 122.3(4) yes . . . C(13) N(4) Li(2) 103.3(4) yes . . . C(14) N(4) Li(2) 112.0(3) yes . . . C(4) C(3) C(5) 109.9(3) yes . . . C(4) C(3) C(6) 109.6(3) yes . . . C(4) C(3) Si(1) 110.1(3) yes . . . C(5) C(3) C(6) 110.1(3) yes . . . C(5) C(3) Si(1) 110.0(3) yes . . . C(6) C(3) Si(1) 107.2(2) yes . . . C(9) C(8) N(1) 108.5(5) yes . . . N(2) C(9) C(8) 110.1(5) yes . . . C(13) C(12) N(3) 112.8(5) yes . . . N(4) C(13) C(12) 110.0(5) yes . . . S(1) Li(1) N(1) 121.7(2) yes . . . S(1) Li(1) N(2) 120.6(2) yes . . . N(1) Li(1) N(2) 85.5(2) yes . . . S(1) Li(2) N(3) 121.0(2) yes . . . S(1) Li(2) N(4) 120.1(2) yes . . . N(3) Li(2) N(4) 86.2(2) yes . . . S(1) Li(1) S(1) 41.72(9) yes . . 65502 S(1) Li(2) S(1) 41.15(9) yes . . 65502 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 Li(1) S(1) Si(1) C(1) -1.4(2) yes . . . . Li(1) S(1) Si(1) C(2) 120.4(3) yes . . . . Li(1) S(1) Si(1) C(3) -121.9(1) yes . . . . Li(2) S(1) Si(1) C(1) -126.0(2) yes . . . . Li(2) S(1) Si(1) C(2) -4.3(3) yes . . . . Li(2) S(1) Si(1) C(3) 113.5(1) yes . . . . Si(1) S(1) Li(1) N(1) 60.2(3) yes . . . . Si(1) S(1) Li(1) N(2) -44.7(4) yes . . . . Li(2) S(1) Li(1) N(1) -157.6(3) yes . . . . Li(2) S(1) Li(1) N(2) 97.5(3) yes . . . . Si(1) S(1) Li(2) N(3) 43.6(4) yes . . . . Si(1) S(1) Li(2) N(4) -61.3(3) yes . . . . Li(1) S(1) Li(2) N(3) -98.9(3) yes . . . . Li(1) S(1) Li(2) N(4) 156.2(3) yes . . . . S(1) Si(1) C(3) C(4) -177.3(2) yes . . . . S(1) Si(1) C(3) C(5) -56.1(3) yes . . . . S(1) Si(1) C(3) C(6) 63.5(2) yes . . . . C(1) Si(1) C(3) C(4) 59.6(3) yes . . . . C(1) Si(1) C(3) C(5) -179.2(3) yes . . . . C(1) Si(1) C(3) C(6) -59.6(2) yes . . . . C(2) Si(1) C(3) C(4) -55.7(3) yes . . . . C(2) Si(1) C(3) C(5) 65.5(3) yes . . . . C(2) Si(1) C(3) C(6) -174.9(2) yes . . . . C(7) N(1) C(8) C(9) -84.6(6) yes . . . . Li(1) N(1) C(8) C(9) 40.6(6) yes . . . . C(7) N(1) Li(1) S(1) -4.2(3) yes . . . . C(7) N(1) Li(1) N(2) 119.2(2) yes . . . . C(8) N(1) Li(1) S(1) -135.6(2) yes . . . . C(8) N(1) Li(1) N(2) -12.16(4) yes . . . . C(10) N(2) C(9) C(8) -81.8(6) yes . . . . Li(1) N(2) C(9) C(8) 47.1(5) yes . . . . C(9) N(2) Li(1) S(1) 105.7(3) yes . . . . C(9) N(2) Li(1) N(1) -18.65(7) yes . . . . C(10) N(2) Li(1) S(1) -117.7(2) yes . . . . C(10) N(2) Li(1) N(1) 117.9(2) yes . . . . C(11) N(3) C(12) C(13) 82.3(6) yes . . . . Li(2) N(3) C(12) C(13) -43.8(5) yes . . . . C(11) N(3) Li(2) S(1) 121.4(2) yes . . . . C(11) N(3) Li(2) N(4) -115.5(2) yes . . . . C(12) N(3) Li(2) S(1) -107.7(2) yes . . . . C(12) N(3) Li(2) N(4) 15.40(5) yes . . . . C(14) N(4) C(13) C(12) 86.2(6) yes . . . . Li(2) N(4) C(13) C(12) -41.1(5) yes . . . . C(13) N(4) Li(2) S(1) 137.6(2) yes . . . . C(13) N(4) Li(2) N(3) 13.68(5) yes . . . . C(14) N(4) Li(2) S(1) 4.1(4) yes . . . . C(14) N(4) Li(2) N(3) -119.9(2) yes . . . . N(1) C(8) C(9) N(2) -62.9(8) yes . . . . N(3) C(12) C(13) N(4) 62.5(7) yes . . . . 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 S(1) S(1) 3.447(1) yes . 45502 S(1) C(1) 3.276(5) yes . 55501 S(1) C(2) 3.298(4) yes . 55501 S(1) C(3) 3.275(3) yes . 55501 S(1) Li(1) 2.426(4) yes . 55501 S(1) Li(2) 2.400(4) yes . 55501 Si(1) C(2) 1.893(4) yes . 55501 Si(1) C(3) 1.901(3) yes . 55501 Si(1) C(4) 2.826(4) yes . 55501 Si(1) C(5) 2.810(4) yes . 55501 Si(1) C(6) 2.777(4) yes . 55501 N(1) N(2) 2.892(5) yes . 55501 N(1) C(9) 2.437(7) yes . 55501 N(1) C(9) 2.437(7) yes . 45502 N(1) Li(1) 2.137(7) yes . 55501 N(2) N(1) 2.892(5) yes . 55501 N(2) C(8) 2.458(7) yes . 55501 N(2) C(8) 2.458(7) yes . 45502 N(2) Li(1) 2.125(7) yes . 55501 N(3) N(4) 2.940(5) yes . 55501 N(3) C(13) 2.475(8) yes . 55501 N(3) C(13) 2.475(8) yes . 45502 N(3) Li(2) 2.173(7) yes . 55501 N(4) N(3) 2.940(5) yes . 55501 N(4) C(12) 2.434(8) yes . 55501 N(4) C(12) 2.434(8) yes . 45502 N(4) Li(2) 2.132(7) yes . 55501 C(1) S(1) 3.276(5) yes . 55501 C(1) C(2) 3.041(9) yes . 55501 C(1) C(3) 3.045(5) yes . 55501 C(1) C(4) 3.414(6) yes . 55501 C(1) C(6) 3.354(7) yes . 55501 C(2) S(1) 3.298(4) yes . 55501 C(2) Si(1) 1.893(4) yes . 55501 C(2) C(1) 3.041(9) yes . 55501 C(2) C(3) 3.023(6) yes . 55501 C(2) C(4) 3.330(7) yes . 55501 C(2) C(5) 3.434(8) yes . 55501 C(3) S(1) 3.275(3) yes . 55501 C(3) Si(1) 1.901(3) yes . 55501 C(3) C(1) 3.045(5) yes . 55501 C(3) C(2) 3.023(6) yes . 55501 C(3) C(6) 1.541(5) yes . 55501 C(4) Si(1) 2.826(4) yes . 55501 C(4) C(1) 3.414(6) yes . 55501 C(4) C(2) 3.330(7) yes . 55501 C(4) C(5) 2.501(6) yes . 55501 C(4) C(6) 2.515(6) yes . 55501 C(5) Si(1) 2.810(4) yes . 55501 C(5) C(2) 3.434(8) yes . 55501 C(5) C(4) 2.501(6) yes . 55501 C(5) C(6) 2.508(7) yes . 55501 C(6) Si(1) 2.777(4) yes . 55501 C(6) C(1) 3.354(7) yes . 55501 C(6) C(3) 1.541(5) yes . 55501 C(6) C(4) 2.515(6) yes . 55501 C(6) C(5) 2.508(7) yes . 55501 C(7) C(7) 2.378(6) yes . 45502 C(7) C(8) 2.553(8) yes . 55501 C(7) C(8) 2.254(8) yes . 45502 C(7) C(9) 3.264(8) yes . 55501 C(7) Li(1) 2.981(7) yes . 55501 C(8) N(2) 2.458(7) yes . 55501 C(8) C(7) 2.553(8) yes . 55501 C(8) C(7) 2.254(8) yes . 45502 C(8) C(10) 3.31(1) yes . 55501 C(8) Li(1) 2.882(8) yes . 55501 C(9) N(1) 2.437(7) yes . 55501 C(9) C(7) 3.264(8) yes . 55501 C(9) C(10) 2.59(1) yes . 55501 C(9) C(10) 2.13(1) yes . 45502 C(9) Li(1) 2.832(8) yes . 55501 C(10) C(8) 3.31(1) yes . 55501 C(10) C(9) 2.59(1) yes . 55501 C(10) C(9) 2.13(1) yes . 45502 C(10) C(10) 2.35(1) yes . 45502 C(10) Li(1) 2.983(8) yes . 55501 C(11) C(11) 2.35(1) yes . 45502 C(11) C(12) 2.52(1) yes . 55501 C(11) C(12) 2.14(1) yes . 45502 C(11) C(13) 3.28(1) yes . 55501 C(11) Li(2) 3.044(9) yes . 55501 C(12) N(4) 2.434(8) yes . 55501 C(12) C(11) 2.52(1) yes . 55501 C(12) C(11) 2.14(1) yes . 45502 C(12) C(14) 3.280(9) yes . 55501 C(12) Li(2) 2.831(8) yes . 55501 C(13) N(3) 2.475(8) yes . 55501 C(13) C(11) 3.28(1) yes . 55501 C(13) C(14) 2.540(8) yes . 55501 C(13) C(14) 2.213(9) yes . 45502 C(13) Li(2) 2.856(8) yes . 55501 C(14) C(12) 3.280(9) yes . 55501 C(14) C(13) 2.540(8) yes . 55501 C(14) C(13) 2.213(9) yes . 45502 C(14) C(14) 2.295(7) yes . 45502 C(14) Li(2) 2.976(8) yes . 55501 Li(1) S(1) 2.426(4) yes . 55501 Li(1) S(1) 2.426(4) yes . 45502 Li(1) N(1) 2.137(7) yes . 55501 Li(1) N(2) 2.125(7) yes . 55501 Li(1) C(7) 2.981(7) yes . 55501 Li(1) C(7) 2.981(7) yes . 45502 Li(1) C(8) 2.882(8) yes . 55501 Li(1) C(8) 2.882(8) yes . 45502 Li(1) C(9) 2.832(8) yes . 55501 Li(1) C(9) 2.832(8) yes . 45502 Li(1) C(10) 2.983(8) yes . 55501 Li(1) C(10) 2.983(8) yes . 45502 Li(1) Li(2) 3.136(8) yes . 55501 Li(2) S(1) 2.400(4) yes . 55501 Li(2) S(1) 2.400(4) yes . 45502 Li(2) N(3) 2.173(7) yes . 55501 Li(2) N(4) 2.132(7) yes . 55501 Li(2) C(11) 3.044(9) yes . 55501 Li(2) C(11) 3.044(9) yes . 45502 Li(2) C(12) 2.831(8) yes . 55501 Li(2) C(12) 2.831(8) yes . 45502 Li(2) C(13) 2.856(8) yes . 55501 Li(2) C(13) 2.856(8) yes . 45502 Li(2) C(14) 2.976(8) yes . 55501 Li(2) C(14) 2.976(8) yes . 45502 Li(2) Li(1) 3.136(8) yes . 55501 S(1) S(1) 30.520(1) yes . 65502 #============================================================================== # 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 #============================================================================== #===END #============================================================================== data_Co(SSiMe2tBu)2(tmeda) _database_code_depnum_ccdc_archive 'CCDC 227192' _audit_creation_date 2004-03-06 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C18 H46 Co N2 S2 Si2 ' _chemical_formula_moiety Co(SSiMe2tBu)2(tmeda) _chemical_formula_weight 469.80 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall 'P 21/B 2/C 21/N ' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y,z+1/2 -x,y,-z+1/2 -x+1/2,-y+1/2,z+1/2 x+1/2,y+1/2,-z+1/2 #------------------------------------------------------------------------------ _cell_length_a 12.856(7) _cell_length_b 10.124(5) _cell_length_c 21.322(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2775.2(24) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8520 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 223.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020.00 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.958 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 42844 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9920 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9909 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -100.0 sigma(F^2^). 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 3579 _reflns_number_gt 2606 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1760 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3162 _refine_ls_number_parameters 137 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0040Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.81 _refine_diff_density_min -0.41 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Co Co 0.349 0.972 ; 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 Co(1) Co 0.5000 0.95868(5) 0.2500 0.0349(2) Uani 1.00 1 d . . . S(1) S 0.36967(6) 0.85670(9) 0.19736(4) 0.0473(2) Uani 1.00 1 d . . . Si(1) Si 0.42995(7) 0.71992(9) 0.13152(4) 0.0433(3) Uani 1.00 1 d . . . N(1) N 0.5754(2) 1.1139(3) 0.20005(13) 0.0499(8) Uani 1.00 1 d . . . C(1) C 0.4174(5) 0.5477(4) 0.1628(2) 0.082(2) Uani 1.00 1 d . . . C(2) C 0.5705(3) 0.7472(5) 0.1137(3) 0.080(2) Uani 1.00 1 d . . . C(3) C 0.3512(3) 0.7339(3) 0.0567(2) 0.0447(8) Uani 1.00 1 d . . . C(4) C 0.3831(4) 0.6239(4) 0.0104(2) 0.0641(12) Uani 1.00 1 d . . . C(5) C 0.3705(4) 0.8680(4) 0.0255(2) 0.0673(12) Uani 1.00 1 d . . . C(6) C 0.2352(3) 0.7216(5) 0.0724(2) 0.0681(13) Uani 1.00 1 d . . . C(7) C 0.5291(4) 1.1292(5) 0.1368(2) 0.0687(13) Uani 1.00 1 d . . . C(8) C 0.6889(4) 1.0974(5) 0.1928(3) 0.086(2) Uani 1.00 1 d . . . C(9) C 0.5544(4) 1.2337(4) 0.2386(2) 0.071(1) Uani 1.00 1 d . . . H(1) H 0.3450 0.5294 0.1723 0.099 Uiso 1.00 1 c . . . H(2) H 0.4420 0.4856 0.1315 0.099 Uiso 1.00 1 c . . . H(3) H 0.4587 0.5388 0.2006 0.099 Uiso 1.00 1 c . . . H(4) H 0.6112 0.7363 0.1517 0.097 Uiso 1.00 1 c . . . H(5) H 0.5934 0.6838 0.0825 0.097 Uiso 1.00 1 c . . . H(6) H 0.5798 0.8360 0.0976 0.097 Uiso 1.00 1 c . . . H(7) H 0.3716 0.5384 0.0297 0.077 Uiso 1.00 1 c . . . H(8) H 0.3411 0.6311 -0.0272 0.077 Uiso 1.00 1 c . . . H(9) H 0.4560 0.6330 -0.0005 0.077 Uiso 1.00 1 c . . . H(10) H 0.4432 0.8760 0.0141 0.081 Uiso 1.00 1 c . . . H(11) H 0.3278 0.8741 -0.0119 0.081 Uiso 1.00 1 c . . . H(12) H 0.3519 0.9385 0.0542 0.081 Uiso 1.00 1 c . . . H(13) H 0.2146 0.7926 0.1004 0.082 Uiso 1.00 1 c . . . H(14) H 0.1946 0.7263 0.0342 0.082 Uiso 1.00 1 c . . . H(15) H 0.2232 0.6373 0.0928 0.082 Uiso 1.00 1 c . . . H(16) H 0.5594 1.2052 0.1160 0.082 Uiso 1.00 1 c . . . H(17) H 0.5425 1.0504 0.1122 0.082 Uiso 1.00 1 c . . . H(18) H 0.4546 1.1418 0.1410 0.082 Uiso 1.00 1 c . . . H(19) H 0.7212 1.0875 0.2337 0.103 Uiso 1.00 1 c . . . H(20) H 0.7020 1.0190 0.1679 0.104 Uiso 1.00 1 c . . . H(21) H 0.7180 1.1739 0.1718 0.103 Uiso 1.00 1 c . . . H(22) H 0.6004 1.2330 0.2747 0.085 Uiso 1.00 1 c . . . H(23) H 0.5674 1.3121 0.2137 0.085 Uiso 1.00 1 c . . . 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 Co(1) 0.0359(3) 0.0338(3) 0.0352(3) 0.0000 -0.0010(2) 0.0000 S(1) 0.0410(4) 0.0535(5) 0.0474(5) -0.0037(4) 0.0016(3) -0.0162(4) Si(1) 0.0437(5) 0.0408(5) 0.0454(5) 0.0051(4) -0.0009(4) -0.0059(4) N(1) 0.054(2) 0.046(2) 0.050(2) -0.0114(13) -0.0048(13) 0.0118(12) C(1) 0.128(5) 0.047(2) 0.071(3) 0.016(2) -0.010(3) 0.005(2) C(2) 0.044(2) 0.101(4) 0.097(3) 0.014(2) 0.002(2) -0.034(3) C(3) 0.051(2) 0.040(2) 0.043(2) 0.004(1) 0.001(1) -0.0105(13) C(4) 0.082(3) 0.057(2) 0.054(2) 0.013(2) 0.001(2) -0.020(2) C(5) 0.098(3) 0.053(2) 0.051(2) 0.010(2) 0.003(2) 0.003(2) C(6) 0.052(2) 0.084(3) 0.068(3) 0.002(2) -0.009(2) -0.030(2) C(7) 0.090(3) 0.068(3) 0.048(2) -0.015(2) -0.005(2) 0.018(2) C(8) 0.058(3) 0.094(4) 0.106(4) -0.024(2) 0.005(3) 0.041(3) C(9) 0.101(4) 0.040(2) 0.071(3) -0.018(2) -0.008(3) 0.006(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; 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 Co(1) S(1) 2.2656(9) yes . . Co(1) N(1) 2.131(3) yes . . S(1) Si(1) 2.119(1) yes . . Si(1) C(1) 1.874(4) yes . . Si(1) C(2) 1.867(4) yes . . Si(1) C(3) 1.895(3) yes . . N(1) C(7) 1.482(5) yes . . N(1) C(8) 1.477(6) yes . . N(1) C(9) 1.490(5) yes . . C(3) C(4) 1.544(5) yes . . C(3) C(5) 1.532(5) yes . . C(3) C(6) 1.533(5) yes . . 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 S(1) Co(1) N(1) 115.14(8) yes . . . Si(1) S(1) Co(1) 110.83(4) yes . . . C(1) Si(1) C(2) 107.1(3) yes . . . C(1) Si(1) C(3) 108.8(2) yes . . . C(1) Si(1) S(1) 109.9(2) yes . . . C(2) Si(1) C(3) 109.6(2) yes . . . C(2) Si(1) S(1) 113.1(2) yes . . . C(3) Si(1) S(1) 108.3(1) yes . . . C(7) N(1) C(8) 108.3(3) yes . . . C(7) N(1) C(9) 110.1(3) yes . . . C(7) N(1) Co(1) 110.4(2) yes . . . C(8) N(1) C(9) 109.2(3) yes . . . C(8) N(1) Co(1) 114.7(3) yes . . . C(9) N(1) Co(1) 104.0(2) yes . . . C(4) C(3) C(5) 108.6(3) yes . . . C(4) C(3) C(6) 109.9(3) yes . . . C(4) C(3) Si(1) 110.0(2) yes . . . C(5) C(3) C(6) 108.9(3) yes . . . C(5) C(3) Si(1) 110.2(2) yes . . . C(6) C(3) Si(1) 109.2(2) yes . . . S(1) Co(1) S(1) 125.78(4) yes . . 65507 N(1) Co(1) N(1) 85.0(1) yes . . 65507 S(1) Co(1) N(1) 104.30(8) yes . . 65507 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 N(1) Co(1) S(1) Si(1) 78.63(5) yes . . . . S(1) Co(1) N(1) C(7) -0.5(3) yes . . . . S(1) Co(1) N(1) C(8) -123.2(3) yes . . . . S(1) Co(1) N(1) C(9) 117.6(2) yes . . . . Co(1) S(1) Si(1) C(1) 102.5(2) yes . . . . Co(1) S(1) Si(1) C(2) -17.1(2) yes . . . . Co(1) S(1) Si(1) C(3) -138.7(1) yes . . . . S(1) Si(1) C(3) C(4) -172.8(2) yes . . . . S(1) Si(1) C(3) C(5) 67.5(3) yes . . . . S(1) Si(1) C(3) C(6) -52.1(3) yes . . . . C(1) Si(1) C(3) C(4) -53.3(3) yes . . . . C(1) Si(1) C(3) C(5) -173.0(2) yes . . . . C(1) Si(1) C(3) C(6) 67.4(3) yes . . . . C(2) Si(1) C(3) C(4) 63.5(2) yes . . . . C(2) Si(1) C(3) C(5) -56.2(3) yes . . . . C(2) Si(1) C(3) C(6) -175.8(2) yes . . . . 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 Co(1) S(1) 2.2656(9) yes . 55501 Co(1) S(1) 2.2656(9) yes . 65507 Co(1) N(1) 2.131(3) yes . 55501 Co(1) N(1) 2.131(3) yes . 65507 Co(1) C(7) 2.991(4) yes . 55501 Co(1) C(7) 2.991(4) yes . 65507 Co(1) C(8) 3.059(5) yes . 55501 Co(1) C(8) 3.059(5) yes . 65507 Co(1) C(9) 2.881(4) yes . 55501 Co(1) C(9) 2.881(4) yes . 65507 S(1) Co(1) 2.2656(9) yes . 55501 S(1) N(1) 3.473(3) yes . 65507 S(1) C(1) 3.272(4) yes . 55501 S(1) C(2) 3.328(5) yes . 55501 S(1) C(3) 3.255(3) yes . 55501 S(1) C(6) 3.457(4) yes . 55501 S(1) C(8) 3.463(5) yes . 65507 Si(1) C(3) 1.895(3) yes . 55501 Si(1) C(4) 2.824(4) yes . 55501 Si(1) C(5) 2.818(4) yes . 55501 Si(1) C(6) 2.802(4) yes . 55501 N(1) Co(1) 2.131(3) yes . 55501 N(1) S(1) 3.473(3) yes . 65507 N(1) N(1) 2.881(4) yes . 65507 N(1) C(9) 2.442(6) yes . 65507 C(1) S(1) 3.272(4) yes . 55501 C(1) C(2) 3.008(7) yes . 55501 C(1) C(3) 3.065(6) yes . 55501 C(1) C(4) 3.368(6) yes . 55501 C(1) C(6) 3.506(7) yes . 55501 C(2) S(1) 3.328(5) yes . 55501 C(2) C(1) 3.008(7) yes . 55501 C(2) C(3) 3.073(5) yes . 55501 C(2) C(4) 3.495(6) yes . 55501 C(2) C(5) 3.413(6) yes . 55501 C(3) S(1) 3.255(3) yes . 55501 C(3) Si(1) 1.895(3) yes . 55501 C(3) C(1) 3.065(6) yes . 55501 C(3) C(2) 3.073(5) yes . 55501 C(3) C(4) 1.544(5) yes . 55501 C(4) Si(1) 2.824(4) yes . 55501 C(4) C(1) 3.368(6) yes . 55501 C(4) C(2) 3.495(6) yes . 55501 C(4) C(3) 1.544(5) yes . 55501 C(4) C(5) 2.497(5) yes . 55501 C(4) C(6) 2.518(6) yes . 55501 C(5) Si(1) 2.818(4) yes . 55501 C(5) C(2) 3.413(6) yes . 55501 C(5) C(4) 2.497(5) yes . 55501 C(5) C(6) 2.494(6) yes . 55501 C(6) S(1) 3.457(4) yes . 55501 C(6) Si(1) 2.802(4) yes . 55501 C(6) C(1) 3.506(7) yes . 55501 C(6) C(4) 2.518(6) yes . 55501 C(6) C(5) 2.494(6) yes . 55501 C(7) Co(1) 2.991(4) yes . 55501 C(7) C(8) 2.398(7) yes . 55501 C(7) C(9) 2.437(6) yes . 55501 C(7) C(9) 3.053(6) yes . 65507 C(8) Co(1) 3.059(5) yes . 55501 C(8) S(1) 3.463(5) yes . 65507 C(8) C(7) 2.398(7) yes . 55501 C(8) C(9) 2.419(7) yes . 55501 C(9) Co(1) 2.881(4) yes . 55501 C(9) N(1) 2.442(6) yes . 65507 C(9) C(7) 2.437(6) yes . 55501 C(9) C(7) 3.053(6) yes . 65507 C(9) C(8) 2.419(7) yes . 55501 #============================================================================== # 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 #============================================================================== #===END data_[Cu(SSiMe2tBu)]4 _database_code_depnum_ccdc_archive 'CCDC 227193' _audit_creation_date 2004-03-03 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H60 Cu4 S4 Si4 ' _chemical_formula_moiety '[Cu(SSiMe2tBu)]4' _chemical_formula_weight 843.50 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 11.404(4) _cell_length_b 13.672(5) _cell_length_c 14.338(5) _cell_angle_alpha 66.800(10) _cell_angle_beta 77.46(2) _cell_angle_gamma 86.71(2) _cell_volume 2004.7(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7283 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880.00 _exptl_absorpt_coefficient_mu 2.434 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.784 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 15506 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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 8699 _reflns_number_gt 6108 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1040 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 8699 _refine_ls_number_parameters 385 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.93 _refine_diff_density_min -0.77 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; 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 Cu(1) Cu 0.10144(4) 0.10567(4) 0.38087(4) 0.02395(13) Uani 1.00 1 d . . . Cu(2) Cu 0.17195(4) -0.07076(4) 0.54008(4) 0.0255(1) Uani 1.00 1 d . . . Cu(3) Cu 0.20093(5) -0.19765(4) 0.41122(4) 0.0265(1) Uani 1.00 1 d . . . Cu(4) Cu 0.09665(5) -0.03769(4) 0.27099(4) 0.0320(2) Uani 1.00 1 d . . . S(1) S 0.08781(9) 0.13422(8) 0.22379(8) 0.0248(3) Uani 1.00 1 d . . . S(2) S 0.09988(8) 0.07928(8) 0.54136(8) 0.0207(2) Uani 1.00 1 d . . . S(3) S 0.28610(9) -0.19971(8) 0.53170(8) 0.0244(3) Uani 1.00 1 d . . . S(4) S 0.10719(10) -0.20659(9) 0.29965(8) 0.0281(3) Uani 1.00 1 d . . . Si(1) Si 0.25714(10) 0.19595(9) 0.11764(9) 0.0237(3) Uani 1.00 1 d . . . Si(2) Si 0.26265(9) 0.15639(9) 0.53964(9) 0.0213(3) Uani 1.00 1 d . . . Si(3) Si 0.20640(10) -0.34488(9) 0.65634(8) 0.0219(3) Uani 1.00 1 d . . . Si(4) Si 0.24218(11) -0.23686(10) 0.18446(10) 0.0303(3) Uani 1.00 1 d . . . C(1) C 0.3861(4) 0.1221(4) 0.1709(4) 0.039(1) Uani 1.00 1 d . . . C(2) C 0.2480(4) 0.1783(4) -0.0024(3) 0.0372(13) Uani 1.00 1 d . . . C(3) C 0.2722(4) 0.3419(4) 0.0907(3) 0.0319(12) Uani 1.00 1 d . . . C(4) C 0.3820(4) 0.3917(4) 0.0017(4) 0.051(2) Uani 1.00 1 d . . . C(5) C 0.1595(4) 0.4012(4) 0.0564(4) 0.042(1) Uani 1.00 1 d . . . C(6) C 0.2895(5) 0.3593(4) 0.1854(4) 0.049(2) Uani 1.00 1 d . . . C(7) C 0.3894(4) 0.1340(4) 0.4445(3) 0.0317(12) Uani 1.00 1 d . . . C(8) C 0.2301(4) 0.3004(3) 0.4986(4) 0.037(1) Uani 1.00 1 d . . . C(9) C 0.2959(4) 0.0989(4) 0.6741(3) 0.0291(12) Uani 1.00 1 d . . . C(10) C 0.4109(4) 0.1559(5) 0.6702(4) 0.064(2) Uani 1.00 1 d . . . C(11) C 0.1948(4) 0.1166(4) 0.7545(4) 0.040(1) Uani 1.00 1 d . . . C(12) C 0.3176(6) -0.0211(5) 0.7103(4) 0.061(2) Uani 1.00 1 d . . . C(13) C 0.0538(4) -0.3727(4) 0.6441(4) 0.0369(13) Uani 1.00 1 d . . . C(14) C 0.1969(4) -0.3277(4) 0.7798(4) 0.041(1) Uani 1.00 1 d . . . C(15) C 0.3125(4) -0.4542(3) 0.6486(3) 0.0260(11) Uani 1.00 1 d . . . C(16) C 0.3341(4) -0.4581(4) 0.5419(4) 0.042(1) Uani 1.00 1 d . . . C(17) C 0.2552(5) -0.5608(4) 0.7283(4) 0.048(2) Uani 1.00 1 d . . . C(18) C 0.4322(4) -0.4366(4) 0.6713(4) 0.044(2) Uani 1.00 1 d . . . C(19) C 0.3026(6) -0.3706(5) 0.2517(5) 0.077(2) Uani 1.00 1 d . . . C(20) C 0.3691(4) -0.1352(5) 0.1266(5) 0.065(2) Uani 1.00 1 d . . . C(21) C 0.1657(4) -0.2371(4) 0.0813(3) 0.0292(11) Uani 1.00 1 d . . . C(22) C 0.2586(4) -0.2628(5) -0.0006(4) 0.050(2) Uani 1.00 1 d . . . C(23) C 0.1131(5) -0.1289(4) 0.0281(4) 0.052(2) Uani 1.00 1 d . . . C(24) C 0.0644(5) -0.3225(5) 0.1272(5) 0.055(2) Uani 1.00 1 d . . . H(1) H 0.3750 0.0469 0.1872 0.050 Uiso 1.00 1 c . . . H(2) H 0.4603 0.1489 0.1199 0.050 Uiso 1.00 1 c . . . H(3) H 0.3901 0.1321 0.2336 0.050 Uiso 1.00 1 c . . . H(4) H 0.1804 0.2166 -0.0294 0.046 Uiso 1.00 1 c . . . H(5) H 0.3217 0.2057 -0.0539 0.046 Uiso 1.00 1 c . . . H(6) H 0.2373 0.1031 0.0133 0.046 Uiso 1.00 1 c . . . H(7) H 0.4544 0.3574 0.0224 0.057 Uiso 1.00 1 c . . . H(8) H 0.3718 0.3815 -0.0593 0.057 Uiso 1.00 1 c . . . H(9) H 0.3888 0.4673 -0.0143 0.057 Uiso 1.00 1 c . . . H(10) H 0.1701 0.4765 0.0396 0.049 Uiso 1.00 1 c . . . H(11) H 0.1476 0.3911 -0.0042 0.048 Uiso 1.00 1 c . . . H(12) H 0.0900 0.3727 0.1126 0.048 Uiso 1.00 1 c . . . H(13) H 0.3600 0.3225 0.2078 0.062 Uiso 1.00 1 c . . . H(14) H 0.3000 0.4348 0.1681 0.062 Uiso 1.00 1 c . . . H(15) H 0.2193 0.3313 0.2410 0.062 Uiso 1.00 1 c . . . H(16) H 0.4050 0.0585 0.4673 0.039 Uiso 1.00 1 c . . . H(17) H 0.3688 0.1594 0.3769 0.039 Uiso 1.00 1 c . . . H(18) H 0.4606 0.1725 0.4400 0.039 Uiso 1.00 1 c . . . H(19) H 0.3008 0.3400 0.4934 0.048 Uiso 1.00 1 c . . . H(20) H 0.2081 0.3260 0.4315 0.048 Uiso 1.00 1 c . . . H(21) H 0.1641 0.3104 0.5492 0.048 Uiso 1.00 1 c . . . H(22) H 0.4316 0.1276 0.7379 0.079 Uiso 1.00 1 c . . . H(23) H 0.4768 0.1459 0.6196 0.079 Uiso 1.00 1 c . . . H(24) H 0.3961 0.2313 0.6501 0.079 Uiso 1.00 1 c . . . H(25) H 0.1804 0.1920 0.7341 0.051 Uiso 1.00 1 c . . . H(26) H 0.1224 0.0796 0.7590 0.051 Uiso 1.00 1 c . . . H(27) H 0.2170 0.0887 0.8216 0.051 Uiso 1.00 1 c . . . H(28) H 0.2443 -0.0575 0.7157 0.077 Uiso 1.00 1 c . . . H(29) H 0.3819 -0.0343 0.6603 0.076 Uiso 1.00 1 c . . . H(30) H 0.3394 -0.0475 0.7775 0.076 Uiso 1.00 1 c . . . H(31) H 0.0026 -0.3136 0.6443 0.041 Uiso 1.00 1 c . . . H(32) H 0.0597 -0.3819 0.5796 0.040 Uiso 1.00 1 c . . . H(33) H 0.0198 -0.4372 0.7020 0.040 Uiso 1.00 1 c . . . H(34) H 0.2768 -0.3127 0.7852 0.048 Uiso 1.00 1 c . . . H(35) H 0.1456 -0.2688 0.7807 0.048 Uiso 1.00 1 c . . . H(36) H 0.1637 -0.3924 0.8379 0.048 Uiso 1.00 1 c . . . H(37) H 0.3875 -0.5152 0.5393 0.052 Uiso 1.00 1 c . . . H(38) H 0.2580 -0.4701 0.5276 0.052 Uiso 1.00 1 c . . . H(39) H 0.3703 -0.3907 0.4904 0.052 Uiso 1.00 1 c . . . H(40) H 0.2415 -0.5601 0.7972 0.053 Uiso 1.00 1 c . . . H(41) H 0.1791 -0.5718 0.7135 0.053 Uiso 1.00 1 c . . . H(42) H 0.3082 -0.6180 0.7251 0.053 Uiso 1.00 1 c . . . H(43) H 0.4849 -0.4942 0.6690 0.054 Uiso 1.00 1 c . . . H(44) H 0.4694 -0.3695 0.6197 0.054 Uiso 1.00 1 c . . . H(45) H 0.4185 -0.4347 0.7397 0.054 Uiso 1.00 1 c . . . H(46) H 0.2373 -0.4235 0.2810 0.100 Uiso 1.00 1 c . . . H(47) H 0.3629 -0.3883 0.2021 0.100 Uiso 1.00 1 c . . . H(48) H 0.3384 -0.3696 0.3068 0.100 Uiso 1.00 1 c . . . H(49) H 0.4053 -0.1344 0.1816 0.092 Uiso 1.00 1 c . . . H(50) H 0.4290 -0.1532 0.0770 0.092 Uiso 1.00 1 c . . . H(51) H 0.3387 -0.0654 0.0919 0.091 Uiso 1.00 1 c . . . H(52) H 0.2911 -0.3320 0.0326 0.067 Uiso 1.00 1 c . . . H(53) H 0.2201 -0.2639 -0.0542 0.067 Uiso 1.00 1 c . . . H(54) H 0.3231 -0.2091 -0.0314 0.067 Uiso 1.00 1 c . . . H(55) H 0.1760 -0.0737 -0.0023 0.061 Uiso 1.00 1 c . . . H(56) H 0.0755 -0.1307 -0.0257 0.061 Uiso 1.00 1 c . . . H(57) H 0.0533 -0.1140 0.0799 0.061 Uiso 1.00 1 c . . . H(58) H 0.0046 -0.3069 0.1785 0.072 Uiso 1.00 1 c . . . H(59) H 0.0273 -0.3234 0.0727 0.072 Uiso 1.00 1 c . . . H(60) H 0.0977 -0.3914 0.1600 0.072 Uiso 1.00 1 c . . . 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 Cu(1) 0.0241(3) 0.0249(3) 0.0225(3) 0.0005(2) -0.0052(2) -0.0087(2) Cu(2) 0.0311(3) 0.0187(3) 0.0282(3) 0.0022(2) -0.0086(2) -0.0095(2) Cu(3) 0.0341(3) 0.0267(3) 0.0195(3) 0.0066(2) -0.0074(2) -0.0099(2) Cu(4) 0.0349(3) 0.0260(3) 0.0401(3) 0.0052(2) -0.0185(3) -0.0132(3) S(1) 0.0240(5) 0.0249(5) 0.0232(5) -0.0004(4) -0.0056(4) -0.0066(4) S(2) 0.0187(5) 0.0215(5) 0.0241(5) -0.0006(4) -0.0034(4) -0.0118(4) S(3) 0.0257(5) 0.0216(5) 0.0259(5) 0.0022(4) -0.0073(4) -0.0085(4) S(4) 0.0345(6) 0.0299(6) 0.0253(6) 0.0085(5) -0.0078(5) -0.0165(5) Si(1) 0.0240(6) 0.0280(6) 0.0201(6) -0.0012(5) -0.0044(5) -0.0102(5) Si(2) 0.0199(5) 0.0238(6) 0.0220(6) -0.0017(4) -0.0044(5) -0.0105(5) Si(3) 0.0250(6) 0.0215(6) 0.0188(6) 0.0055(5) -0.0050(5) -0.0080(5) Si(4) 0.0302(6) 0.0427(8) 0.0305(7) 0.0143(6) -0.0141(5) -0.0253(6) C(1) 0.034(3) 0.050(3) 0.042(3) 0.009(2) -0.013(2) -0.025(3) C(2) 0.040(3) 0.044(3) 0.030(3) 0.005(2) -0.009(2) -0.016(2) C(3) 0.038(2) 0.033(3) 0.022(2) -0.006(2) -0.004(2) -0.007(2) C(4) 0.046(3) 0.042(3) 0.055(3) -0.019(2) -0.003(3) -0.010(3) C(5) 0.054(3) 0.029(3) 0.038(3) 0.003(2) -0.012(2) -0.006(2) C(6) 0.073(4) 0.036(3) 0.045(3) -0.010(3) -0.015(3) -0.021(3) C(7) 0.025(2) 0.044(3) 0.030(2) -0.005(2) -0.006(2) -0.016(2) C(8) 0.041(3) 0.031(3) 0.047(3) -0.004(2) -0.012(2) -0.020(2) C(9) 0.025(2) 0.045(3) 0.025(2) 0.002(2) -0.007(2) -0.020(2) C(10) 0.036(3) 0.116(6) 0.045(3) -0.018(3) -0.016(3) -0.032(4) C(11) 0.038(3) 0.060(3) 0.029(3) 0.012(2) -0.014(2) -0.022(2) C(12) 0.083(4) 0.065(4) 0.044(3) 0.039(4) -0.035(3) -0.022(3) C(13) 0.028(2) 0.037(3) 0.036(3) -0.003(2) 0.001(2) -0.008(2) C(14) 0.048(3) 0.043(3) 0.030(3) 0.012(2) -0.007(2) -0.015(2) C(15) 0.027(2) 0.019(2) 0.025(2) 0.007(2) -0.004(2) -0.004(2) C(16) 0.049(3) 0.033(3) 0.047(3) 0.009(2) -0.007(3) -0.023(2) C(17) 0.058(3) 0.024(3) 0.050(3) 0.006(2) -0.001(3) -0.007(2) C(18) 0.034(3) 0.037(3) 0.065(4) 0.015(2) -0.021(3) -0.019(3) C(19) 0.109(5) 0.082(5) 0.058(4) 0.075(4) -0.042(4) -0.043(4) C(20) 0.034(3) 0.111(5) 0.084(5) -0.007(3) -0.004(3) -0.076(4) C(21) 0.031(2) 0.035(3) 0.021(2) -0.004(2) -0.001(2) -0.012(2) C(22) 0.048(3) 0.078(4) 0.041(3) -0.003(3) -0.001(2) -0.043(3) C(23) 0.058(3) 0.054(3) 0.041(3) 0.009(3) -0.023(3) -0.011(3) C(24) 0.051(3) 0.061(4) 0.067(4) -0.015(3) -0.009(3) -0.040(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; 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 Cu(1) Cu(4) 2.9680(9) yes . . Cu(1) S(1) 2.168(1) yes . . Cu(1) S(2) 2.180(1) yes . . Cu(2) S(2) 2.171(1) yes . . Cu(2) S(3) 2.157(1) yes . . Cu(3) Cu(4) 2.7413(7) yes . . Cu(3) S(3) 2.148(1) yes . . Cu(3) S(4) 2.151(1) yes . . Cu(4) S(1) 2.177(1) yes . . Cu(4) S(4) 2.181(1) yes . . S(1) Si(1) 2.158(1) yes . . S(2) Si(2) 2.178(2) yes . . S(3) Si(3) 2.160(1) yes . . S(4) Si(4) 2.152(2) yes . . Si(1) C(1) 1.864(5) yes . . Si(1) C(2) 1.855(6) yes . . Si(1) C(3) 1.887(5) yes . . Si(2) C(7) 1.861(5) yes . . Si(2) C(8) 1.860(5) yes . . Si(2) C(9) 1.889(5) yes . . Si(3) C(13) 1.861(5) yes . . Si(3) C(14) 1.855(6) yes . . Si(3) C(15) 1.891(4) yes . . Si(4) C(19) 1.871(6) yes . . Si(4) C(20) 1.875(6) yes . . Si(4) C(21) 1.875(5) yes . . C(3) C(4) 1.543(6) yes . . C(3) C(5) 1.546(7) yes . . C(3) C(6) 1.523(8) yes . . C(9) C(10) 1.544(8) yes . . C(9) C(11) 1.525(6) yes . . C(9) C(12) 1.537(7) yes . . C(15) C(16) 1.517(7) yes . . C(15) C(17) 1.527(5) yes . . C(15) C(18) 1.523(7) yes . . C(21) C(22) 1.537(7) yes . . C(21) C(23) 1.529(7) yes . . C(21) C(24) 1.533(7) yes . . 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 Cu(4) Cu(1) S(1) 47.05(3) yes . . . Cu(4) Cu(1) S(2) 133.91(4) yes . . . S(1) Cu(1) S(2) 175.44(4) yes . . . S(2) Cu(2) S(3) 165.58(5) yes . . . Cu(4) Cu(3) S(3) 131.80(4) yes . . . Cu(4) Cu(3) S(4) 51.23(4) yes . . . S(3) Cu(3) S(4) 175.41(4) yes . . . S(1) Cu(4) S(4) 173.45(5) yes . . . S(1) Cu(4) Cu(1) 46.79(4) yes . . . S(1) Cu(4) Cu(3) 135.01(5) yes . . . S(4) Cu(4) Cu(1) 139.68(4) yes . . . S(4) Cu(4) Cu(3) 50.27(4) yes . . . Cu(1) Cu(4) Cu(3) 92.12(2) yes . . . Si(1) S(1) Cu(1) 110.22(7) yes . . . Si(1) S(1) Cu(4) 104.67(6) yes . . . Cu(4) S(1) Cu(1) 86.15(4) yes . . . Si(2) S(2) Cu(1) 106.86(5) yes . . . Si(2) S(2) Cu(2) 99.80(5) yes . . . Cu(1) S(2) Cu(2) 80.54(5) yes . . . Si(3) S(3) Cu(2) 107.83(5) yes . . . Si(3) S(3) Cu(3) 100.14(6) yes . . . Cu(2) S(3) Cu(3) 86.65(4) yes . . . Si(4) S(4) Cu(3) 105.67(6) yes . . . Si(4) S(4) Cu(4) 112.35(5) yes . . . Cu(4) S(4) Cu(3) 78.50(5) yes . . . C(1) Si(1) C(2) 110.2(2) yes . . . C(1) Si(1) C(3) 110.6(2) yes . . . C(1) Si(1) S(1) 111.6(1) yes . . . C(2) Si(1) C(3) 110.4(2) yes . . . C(2) Si(1) S(1) 105.5(2) yes . . . C(3) Si(1) S(1) 108.5(1) yes . . . C(7) Si(2) C(8) 110.8(2) yes . . . C(7) Si(2) C(9) 110.5(2) yes . . . C(7) Si(2) S(2) 109.1(2) yes . . . C(8) Si(2) C(9) 111.5(3) yes . . . C(8) Si(2) S(2) 105.6(2) yes . . . C(9) Si(2) S(2) 109.2(1) yes . . . C(13) Si(3) C(14) 110.0(2) yes . . . C(13) Si(3) C(15) 111.3(2) yes . . . C(13) Si(3) S(3) 111.4(1) yes . . . C(14) Si(3) C(15) 110.7(2) yes . . . C(14) Si(3) S(3) 107.2(2) yes . . . C(15) Si(3) S(3) 106.1(1) yes . . . C(19) Si(4) C(20) 108.9(3) yes . . . C(19) Si(4) C(21) 111.2(3) yes . . . C(19) Si(4) S(4) 106.7(2) yes . . . C(20) Si(4) C(21) 110.4(2) yes . . . C(20) Si(4) S(4) 112.5(2) yes . . . C(21) Si(4) S(4) 107.1(1) yes . . . C(4) C(3) C(5) 108.1(3) yes . . . C(4) C(3) C(6) 108.3(4) yes . . . C(4) C(3) Si(1) 109.2(4) yes . . . C(5) C(3) C(6) 108.6(4) yes . . . C(5) C(3) Si(1) 110.6(4) yes . . . C(6) C(3) Si(1) 111.9(3) yes . . . C(10) C(9) C(11) 108.1(5) yes . . . C(10) C(9) C(12) 108.6(4) yes . . . C(10) C(9) Si(2) 107.7(3) yes . . . C(11) C(9) C(12) 108.3(3) yes . . . C(11) C(9) Si(2) 112.3(3) yes . . . C(12) C(9) Si(2) 111.7(4) yes . . . C(16) C(15) C(17) 108.0(4) yes . . . C(16) C(15) C(18) 109.3(4) yes . . . C(16) C(15) Si(3) 110.8(3) yes . . . C(17) C(15) C(18) 109.6(4) yes . . . C(17) C(15) Si(3) 108.6(3) yes . . . C(18) C(15) Si(3) 110.5(4) yes . . . C(22) C(21) C(23) 108.9(4) yes . . . C(22) C(21) C(24) 108.3(5) yes . . . C(22) C(21) Si(4) 108.6(3) yes . . . C(23) C(21) C(24) 108.7(4) yes . . . C(23) C(21) Si(4) 111.4(4) yes . . . C(24) C(21) Si(4) 110.8(3) yes . . . 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 S(1) Cu(1) Cu(4) Cu(3) 159.42(3) yes . . . . S(1) Cu(1) Cu(4) S(4) 178.54(6) yes . . . . S(2) Cu(1) Cu(4) Cu(3) -26.73(4) yes . . . . S(2) Cu(1) Cu(4) S(1) 173.85(5) yes . . . . S(2) Cu(1) Cu(4) S(4) -7.61(7) yes . . . . Cu(4) Cu(1) S(1) Si(1) -104.22(6) yes . . . . Cu(4) Cu(1) S(2) Cu(2) 23.78(5) yes . . . . Cu(4) Cu(1) S(2) Si(2) 121.24(5) yes . . . . S(3) Cu(2) S(2) Cu(1) 96.4(2) yes . . . . S(3) Cu(2) S(2) Si(2) -9.2(2) yes . . . . S(2) Cu(2) S(3) Cu(3) -123.9(2) yes . . . . S(2) Cu(2) S(3) Si(3) 136.5(2) yes . . . . S(3) Cu(3) Cu(4) Cu(1) -11.49(4) yes . . . . S(3) Cu(3) Cu(4) S(1) 9.76(7) yes . . . . S(3) Cu(3) Cu(4) S(4) -175.49(5) yes . . . . S(4) Cu(3) Cu(4) Cu(1) 164.00(3) yes . . . . S(4) Cu(3) Cu(4) S(1) -174.75(5) yes . . . . Cu(4) Cu(3) S(3) Cu(2) 27.80(5) yes . . . . Cu(4) Cu(3) S(3) Si(3) 135.32(5) yes . . . . Cu(4) Cu(3) S(4) Si(4) 110.24(6) yes . . . . Cu(1) Cu(4) S(1) Si(1) 109.91(7) yes . . . . Cu(3) Cu(4) S(1) Cu(1) -29.80(6) yes . . . . Cu(3) Cu(4) S(1) Si(1) 80.11(7) yes . . . . Cu(1) Cu(4) S(4) Cu(3) -25.19(7) yes . . . . Cu(1) Cu(4) S(4) Si(4) -127.57(7) yes . . . . Cu(3) Cu(4) S(4) Si(4) -102.38(7) yes . . . . Cu(1) S(1) Si(1) C(1) 43.8(2) yes . . . . Cu(1) S(1) Si(1) C(2) 163.4(2) yes . . . . Cu(1) S(1) Si(1) C(3) -78.3(2) yes . . . . Cu(4) S(1) Si(1) C(1) -47.5(2) yes . . . . Cu(4) S(1) Si(1) C(2) 72.1(2) yes . . . . Cu(4) S(1) Si(1) C(3) -169.6(2) yes . . . . Cu(1) S(2) Si(2) C(7) -39.7(1) yes . . . . Cu(1) S(2) Si(2) C(8) 79.5(2) yes . . . . Cu(1) S(2) Si(2) C(9) -160.5(2) yes . . . . Cu(2) S(2) Si(2) C(7) 43.3(1) yes . . . . Cu(2) S(2) Si(2) C(8) 162.5(2) yes . . . . Cu(2) S(2) Si(2) C(9) -77.5(2) yes . . . . Cu(2) S(3) Si(3) C(13) 60.7(2) yes . . . . Cu(2) S(3) Si(3) C(14) -59.7(2) yes . . . . Cu(2) S(3) Si(3) C(15) -177.9(2) yes . . . . Cu(3) S(3) Si(3) C(13) -29.0(2) yes . . . . Cu(3) S(3) Si(3) C(14) -149.4(2) yes . . . . Cu(3) S(3) Si(3) C(15) 92.3(2) yes . . . . Cu(3) S(4) Si(4) C(19) 64.2(3) yes . . . . Cu(3) S(4) Si(4) C(20) -55.2(2) yes . . . . Cu(3) S(4) Si(4) C(21) -176.7(1) yes . . . . Cu(4) S(4) Si(4) C(19) 148.0(3) yes . . . . Cu(4) S(4) Si(4) C(20) 28.6(2) yes . . . . Cu(4) S(4) Si(4) C(21) -92.9(2) yes . . . . S(1) Si(1) C(3) C(4) -170.8(3) yes . . . . S(1) Si(1) C(3) C(5) -52.0(3) yes . . . . S(1) Si(1) C(3) C(6) 69.2(3) yes . . . . C(1) Si(1) C(3) C(4) 66.6(4) yes . . . . C(1) Si(1) C(3) C(5) -174.6(3) yes . . . . C(1) Si(1) C(3) C(6) -53.4(3) yes . . . . C(2) Si(1) C(3) C(4) -55.7(4) yes . . . . C(2) Si(1) C(3) C(5) 63.1(3) yes . . . . C(2) Si(1) C(3) C(6) -175.7(3) yes . . . . S(2) Si(2) C(9) C(10) -179.5(3) yes . . . . S(2) Si(2) C(9) C(11) -60.6(4) yes . . . . S(2) Si(2) C(9) C(12) 61.3(3) yes . . . . C(7) Si(2) C(9) C(10) 60.5(4) yes . . . . C(7) Si(2) C(9) C(11) 179.4(3) yes . . . . C(7) Si(2) C(9) C(12) -58.7(3) yes . . . . C(8) Si(2) C(9) C(10) -63.2(4) yes . . . . C(8) Si(2) C(9) C(11) 55.7(4) yes . . . . C(8) Si(2) C(9) C(12) 177.6(3) yes . . . . S(3) Si(3) C(15) C(16) -56.1(3) yes . . . . S(3) Si(3) C(15) C(17) -174.6(3) yes . . . . S(3) Si(3) C(15) C(18) 65.2(3) yes . . . . C(13) Si(3) C(15) C(16) 65.3(3) yes . . . . C(13) Si(3) C(15) C(17) -53.2(4) yes . . . . C(13) Si(3) C(15) C(18) -173.4(2) yes . . . . C(14) Si(3) C(15) C(16) -172.0(3) yes . . . . C(14) Si(3) C(15) C(17) 69.4(4) yes . . . . C(14) Si(3) C(15) C(18) -50.8(3) yes . . . . S(4) Si(4) C(21) C(22) -177.9(3) yes . . . . S(4) Si(4) C(21) C(23) 62.2(3) yes . . . . S(4) Si(4) C(21) C(24) -59.0(4) yes . . . . C(19) Si(4) C(21) C(22) -61.7(3) yes . . . . C(19) Si(4) C(21) C(23) 178.4(3) yes . . . . C(19) Si(4) C(21) C(24) 57.1(4) yes . . . . C(20) Si(4) C(21) C(22) 59.3(3) yes . . . . C(20) Si(4) C(21) C(23) -60.6(3) yes . . . . C(20) Si(4) C(21) C(24) 178.2(3) yes . . . . 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 Cu(1) Cu(2) 2.8128(6) yes . 55501 Cu(1) Cu(4) 2.9680(9) yes . 55501 Cu(1) S(1) 2.168(1) yes . 55501 Cu(1) S(2) 2.180(1) yes . 55501 Cu(1) Si(1) 3.549(1) yes . 55501 Cu(1) Si(2) 3.500(2) yes . 55501 Cu(1) C(1) 3.867(4) yes . 55501 Cu(1) C(6) 3.881(5) yes . 55501 Cu(1) C(7) 3.673(5) yes . 55501 Cu(2) Cu(1) 2.8128(6) yes . 55501 Cu(2) Cu(3) 2.9541(9) yes . 55501 Cu(2) Cu(4) 3.9809(9) yes . 55501 Cu(2) S(2) 2.171(1) yes . 55501 Cu(2) S(3) 2.157(1) yes . 55501 Cu(2) Si(2) 3.326(1) yes . 55501 Cu(2) Si(3) 3.489(1) yes . 55501 Cu(2) C(7) 3.487(4) yes . 55501 Cu(2) C(12) 3.517(7) yes . 55501 Cu(2) C(13) 3.999(5) yes . 55501 Cu(2) C(14) 3.877(4) yes . 55501 Cu(3) Cu(2) 2.9541(9) yes . 55501 Cu(3) Cu(4) 2.7413(7) yes . 55501 Cu(3) S(3) 2.148(1) yes . 55501 Cu(3) S(4) 2.151(1) yes . 55501 Cu(3) Si(3) 3.304(1) yes . 55501 Cu(3) Si(4) 3.429(2) yes . 55501 Cu(3) C(13) 3.380(4) yes . 55501 Cu(3) C(16) 3.722(5) yes . 55501 Cu(3) C(19) 3.868(8) yes . 55501 Cu(3) C(20) 3.886(6) yes . 55501 Cu(4) Cu(1) 2.9680(9) yes . 55501 Cu(4) Cu(2) 3.9809(9) yes . 55501 Cu(4) Cu(3) 2.7413(7) yes . 55501 Cu(4) Si(1) 3.432(1) yes . 55501 Cu(4) Si(4) 3.600(2) yes . 55501 Cu(4) C(1) 3.746(5) yes . 55501 Cu(4) C(2) 3.949(4) yes . 55501 Cu(4) C(20) 3.824(6) yes . 55501 S(1) Cu(1) 2.168(1) yes . 55501 S(1) Si(1) 2.158(1) yes . 55501 S(1) C(1) 3.330(4) yes . 55501 S(1) C(2) 3.199(5) yes . 55501 S(1) C(3) 3.286(4) yes . 55501 S(1) C(5) 3.512(4) yes . 55501 S(1) C(6) 3.740(6) yes . 55501 S(2) Cu(1) 2.180(1) yes . 55501 S(2) Cu(2) 2.171(1) yes . 55501 S(2) Si(2) 2.178(2) yes . 55501 S(2) C(7) 3.296(4) yes . 55501 S(2) C(8) 3.222(5) yes . 55501 S(2) C(9) 3.318(5) yes . 55501 S(2) C(11) 3.674(6) yes . 55501 S(2) C(12) 3.676(6) yes . 55501 S(3) Cu(2) 2.157(1) yes . 55501 S(3) Cu(3) 2.148(1) yes . 55501 S(3) Si(3) 2.160(1) yes . 55501 S(3) C(13) 3.327(4) yes . 55501 S(3) C(14) 3.237(4) yes . 55501 S(3) C(15) 3.241(4) yes . 55501 S(3) C(16) 3.494(5) yes . 55501 S(3) C(18) 3.604(5) yes . 55501 S(4) Cu(3) 2.151(1) yes . 55501 S(4) Si(4) 2.152(2) yes . 55501 S(4) C(19) 3.231(7) yes . 55501 S(4) C(20) 3.352(5) yes . 55501 S(4) C(21) 3.243(5) yes . 55501 S(4) C(23) 3.595(6) yes . 55501 S(4) C(24) 3.544(8) yes . 55501 Si(1) Cu(1) 3.549(1) yes . 55501 Si(1) Cu(4) 3.432(1) yes . 55501 Si(1) S(1) 2.158(1) yes . 55501 Si(1) C(3) 1.887(5) yes . 55501 Si(1) C(4) 2.803(5) yes . 55501 Si(1) C(5) 2.830(5) yes . 55501 Si(1) C(6) 2.833(7) yes . 55501 Si(2) Cu(1) 3.500(2) yes . 55501 Si(2) Cu(2) 3.326(1) yes . 55501 Si(2) S(2) 2.178(2) yes . 55501 Si(2) C(9) 1.889(5) yes . 55501 Si(2) C(10) 2.780(7) yes . 55501 Si(2) C(11) 2.842(5) yes . 55501 Si(2) C(12) 2.843(5) yes . 55501 Si(3) Cu(2) 3.489(1) yes . 55501 Si(3) Cu(3) 3.304(1) yes . 55501 Si(3) S(3) 2.160(1) yes . 55501 Si(3) C(15) 1.891(4) yes . 55501 Si(3) C(16) 2.813(6) yes . 55501 Si(3) C(17) 2.784(5) yes . 55501 Si(3) C(18) 2.812(5) yes . 55501 Si(4) Cu(3) 3.429(2) yes . 55501 Si(4) Cu(4) 3.600(2) yes . 55501 Si(4) S(4) 2.152(2) yes . 55501 Si(4) C(22) 2.778(7) yes . 55501 Si(4) C(23) 2.819(6) yes . 55501 Si(4) C(24) 2.812(7) yes . 55501 C(1) Cu(1) 3.867(4) yes . 55501 C(1) Cu(4) 3.746(5) yes . 55501 C(1) S(1) 3.330(4) yes . 55501 C(1) C(2) 3.051(7) yes . 55501 C(1) C(3) 3.085(6) yes . 55501 C(1) C(4) 3.529(6) yes . 55501 C(1) C(6) 3.434(8) yes . 55501 C(1) C(7) 3.998(8) yes . 55501 C(1) C(20) 3.84(1) yes . 55501 C(2) Cu(4) 3.949(4) yes . 55501 C(2) S(1) 3.199(5) yes . 55501 C(2) C(1) 3.051(7) yes . 55501 C(2) C(3) 3.073(8) yes . 55501 C(2) C(4) 3.397(9) yes . 55501 C(2) C(5) 3.509(8) yes . 55501 C(3) S(1) 3.286(4) yes . 55501 C(3) Si(1) 1.887(5) yes . 55501 C(3) C(1) 3.085(6) yes . 55501 C(3) C(2) 3.073(8) yes . 55501 C(3) C(4) 1.543(6) yes . 55501 C(3) C(5) 1.546(7) yes . 55501 C(4) Si(1) 2.803(5) yes . 55501 C(4) C(1) 3.529(6) yes . 55501 C(4) C(2) 3.397(9) yes . 55501 C(4) C(3) 1.543(6) yes . 55501 C(4) C(5) 2.500(7) yes . 55501 C(4) C(6) 2.485(8) yes . 55501 C(5) S(1) 3.512(4) yes . 55501 C(5) Si(1) 2.830(5) yes . 55501 C(5) C(2) 3.509(8) yes . 55501 C(5) C(3) 1.546(7) yes . 55501 C(5) C(4) 2.500(7) yes . 55501 C(5) C(6) 2.491(8) yes . 55501 C(6) Cu(1) 3.881(5) yes . 55501 C(6) S(1) 3.740(6) yes . 55501 C(6) Si(1) 2.833(7) yes . 55501 C(6) C(1) 3.434(8) yes . 55501 C(6) C(4) 2.485(8) yes . 55501 C(6) C(5) 2.491(8) yes . 55501 C(7) Cu(1) 3.673(5) yes . 55501 C(7) Cu(2) 3.487(4) yes . 55501 C(7) S(2) 3.296(4) yes . 55501 C(7) C(1) 3.998(8) yes . 55501 C(7) C(8) 3.063(7) yes . 55501 C(7) C(9) 3.081(6) yes . 55501 C(7) C(10) 3.426(9) yes . 55501 C(7) C(12) 3.487(6) yes . 55501 C(8) S(2) 3.222(5) yes . 55501 C(8) C(7) 3.063(7) yes . 55501 C(8) C(9) 3.100(6) yes . 55501 C(8) C(10) 3.481(7) yes . 55501 C(8) C(11) 3.486(6) yes . 55501 C(8) C(16) 3.883(8) yes . 56501 C(9) S(2) 3.318(5) yes . 55501 C(9) Si(2) 1.889(5) yes . 55501 C(9) C(7) 3.081(6) yes . 55501 C(9) C(8) 3.100(6) yes . 55501 C(9) C(10) 1.544(8) yes . 55501 C(10) Si(2) 2.780(7) yes . 55501 C(10) C(7) 3.426(9) yes . 55501 C(10) C(8) 3.481(7) yes . 55501 C(10) C(9) 1.544(8) yes . 55501 C(10) C(11) 2.484(6) yes . 55501 C(10) C(12) 2.50(1) yes . 55501 C(11) S(2) 3.674(6) yes . 55501 C(11) Si(2) 2.842(5) yes . 55501 C(11) C(8) 3.486(6) yes . 55501 C(11) C(10) 2.484(6) yes . 55501 C(11) C(12) 2.482(8) yes . 55501 C(12) Cu(2) 3.517(7) yes . 55501 C(12) S(2) 3.676(6) yes . 55501 C(12) Si(2) 2.843(5) yes . 55501 C(12) C(7) 3.487(6) yes . 55501 C(12) C(10) 2.50(1) yes . 55501 C(12) C(11) 2.482(8) yes . 55501 C(13) Cu(2) 3.999(5) yes . 55501 C(13) Cu(3) 3.380(4) yes . 55501 C(13) S(3) 3.327(4) yes . 55501 C(13) C(14) 3.043(8) yes . 55501 C(13) C(15) 3.098(6) yes . 55501 C(13) C(16) 3.551(7) yes . 55501 C(13) C(17) 3.380(7) yes . 55501 C(14) Cu(2) 3.877(4) yes . 55501 C(14) S(3) 3.237(4) yes . 55501 C(14) C(13) 3.043(8) yes . 55501 C(14) C(15) 3.081(7) yes . 55501 C(14) C(17) 3.541(8) yes . 55501 C(14) C(18) 3.375(7) yes . 55501 C(15) S(3) 3.241(4) yes . 55501 C(15) Si(3) 1.891(4) yes . 55501 C(15) C(13) 3.098(6) yes . 55501 C(15) C(14) 3.081(7) yes . 55501 C(16) Cu(3) 3.722(5) yes . 55501 C(16) S(3) 3.494(5) yes . 55501 C(16) Si(3) 2.813(6) yes . 55501 C(16) C(8) 3.883(8) yes . 54501 C(16) C(13) 3.551(7) yes . 55501 C(16) C(17) 2.463(6) yes . 55501 C(16) C(18) 2.480(9) yes . 55501 C(16) C(19) 3.944(9) yes . 55501 C(17) Si(3) 2.784(5) yes . 55501 C(17) C(13) 3.380(7) yes . 55501 C(17) C(14) 3.541(8) yes . 55501 C(17) C(16) 2.463(6) yes . 55501 C(17) C(18) 2.492(7) yes . 55501 C(18) S(3) 3.604(5) yes . 55501 C(18) Si(3) 2.812(5) yes . 55501 C(18) C(14) 3.375(7) yes . 55501 C(18) C(16) 2.480(9) yes . 55501 C(18) C(17) 2.492(7) yes . 55501 C(19) Cu(3) 3.868(8) yes . 55501 C(19) S(4) 3.231(7) yes . 55501 C(19) C(16) 3.944(9) yes . 55501 C(19) C(20) 3.048(8) yes . 55501 C(19) C(21) 3.091(8) yes . 55501 C(19) C(22) 3.466(8) yes . 55501 C(19) C(24) 3.46(1) yes . 55501 C(20) Cu(3) 3.886(6) yes . 55501 C(20) Cu(4) 3.824(6) yes . 55501 C(20) S(4) 3.352(5) yes . 55501 C(20) C(1) 3.84(1) yes . 55501 C(20) C(19) 3.048(8) yes . 55501 C(20) C(21) 3.079(9) yes . 55501 C(20) C(22) 3.42(1) yes . 55501 C(20) C(23) 3.492(9) yes . 55501 C(21) S(4) 3.243(5) yes . 55501 C(21) C(19) 3.091(8) yes . 55501 C(21) C(20) 3.079(9) yes . 55501 C(22) Si(4) 2.778(7) yes . 55501 C(22) C(14) 3.799(9) yes . 55401 C(22) C(19) 3.466(8) yes . 55501 C(22) C(20) 3.42(1) yes . 55501 C(22) C(23) 2.494(8) yes . 55501 C(22) C(24) 2.488(7) yes . 55501 C(23) S(4) 3.595(6) yes . 55501 C(23) Si(4) 2.819(6) yes . 55501 C(23) C(11) 3.990(6) yes . 55401 C(23) C(20) 3.492(9) yes . 55501 C(23) C(22) 2.494(8) yes . 55501 C(23) C(24) 2.488(7) yes . 55501 C(24) S(4) 3.544(8) yes . 55501 C(24) Si(4) 2.812(7) yes . 55501 C(24) C(19) 3.46(1) yes . 55501 C(24) C(22) 2.488(7) yes . 55501 C(24) C(23) 2.488(7) yes . 55501 #============================================================================== # 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 #============================================================================== data_Cp2Ti(SSiMe3)2 _database_code_depnum_ccdc_archive 'CCDC 227194' _audit_creation_date 2004-03-03 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C16 H28 S2 Si2 Ti ' _chemical_formula_moiety Cp2Ti(SSiMe3)2 _chemical_formula_weight 388.59 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 16.1375(8) _cell_length_b 13.8649(5) _cell_length_c 18.7887(4) _cell_angle_alpha 90 _cell_angle_beta 105.1948(6) _cell_angle_gamma 90 _cell_volume 4056.9(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 14658 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour dark-purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648.00 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.32 _diffrn_reflns_number 76562 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9952 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9940 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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 9652 _reflns_number_gt 6167 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1400 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 9262 _refine_ls_number_parameters 435 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 1.8000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.97 _refine_diff_density_min -0.89 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ti Ti 0.278 0.446 ; 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 Ti(1) Ti 0.14675(4) 0.23081(5) 0.08573(4) 0.0337(2) Uani 1.00 1 d . . . Ti(2) Ti 0.57033(4) 0.41405(4) 0.22812(3) 0.0270(2) Uani 1.00 1 d . . . S(1) S 0.24364(6) 0.15653(7) 0.02358(5) 0.0379(3) Uani 1.00 1 d . . . S(2) S 0.06028(6) 0.33025(7) -0.01328(6) 0.0383(3) Uani 1.00 1 d . . . S(3) S 0.52238(6) 0.26627(6) 0.16231(5) 0.0284(2) Uani 1.00 1 d . . . S(4) S 0.72180(6) 0.40096(7) 0.23135(5) 0.0357(3) Uani 1.00 1 d . . . Si(1) Si 0.20147(7) 0.06727(8) -0.07147(6) 0.0366(3) Uani 1.00 1 d . . . Si(2) Si 0.11640(8) 0.43152(8) -0.07199(7) 0.0433(3) Uani 1.00 1 d . . . Si(3) Si 0.53674(7) 0.24493(7) 0.05288(5) 0.0308(3) Uani 1.00 1 d . . . Si(4) Si 0.79195(7) 0.27512(8) 0.27726(6) 0.0410(3) Uani 1.00 1 d . . . C(1) C 0.0904(3) 0.0927(3) -0.1286(3) 0.0524(13) Uani 1.00 1 d . . . C(2) C 0.2101(3) -0.0638(3) -0.0478(3) 0.0512(13) Uani 1.00 1 d . . . C(3) C 0.2803(3) 0.0928(3) -0.1255(2) 0.0430(12) Uani 1.00 1 d . . . C(4) C 0.1903(3) 0.3700(4) -0.1188(3) 0.063(2) Uani 1.00 1 d . . . C(5) C 0.0238(4) 0.4795(4) -0.1445(3) 0.072(2) Uani 1.00 1 d . . . C(6) C 0.1717(4) 0.5369(4) -0.0190(4) 0.082(2) Uani 1.00 1 d . . . C(7) C 0.0046(3) 0.1935(3) 0.0926(3) 0.0477(13) Uani 1.00 1 d . . . C(8) C 0.0209(3) 0.1352(3) 0.0362(2) 0.0445(12) Uani 1.00 1 d . . . C(9) C 0.0869(3) 0.0724(3) 0.0697(3) 0.0472(13) Uani 1.00 1 d . . . C(10) C 0.1122(3) 0.0917(3) 0.1458(3) 0.0527(13) Uani 1.00 1 d . . . C(11) C 0.0593(3) 0.1647(4) 0.1597(3) 0.054(1) Uani 1.00 1 d . . . C(12) C 0.2872(3) 0.2639(4) 0.1636(2) 0.0535(13) Uani 1.00 1 d . . . C(13) C 0.2309(3) 0.2605(4) 0.2080(2) 0.0552(13) Uani 1.00 1 d . . . C(14) C 0.1720(3) 0.3371(4) 0.1870(2) 0.054(1) Uani 1.00 1 d . . . C(15) C 0.1943(3) 0.3901(3) 0.1313(3) 0.053(1) Uani 1.00 1 d . . . C(16) C 0.2651(3) 0.3433(4) 0.1161(3) 0.056(1) Uani 1.00 1 d . . . C(17) C 0.4391(3) 0.2820(3) -0.0190(2) 0.0527(13) Uani 1.00 1 d . . . C(18) C 0.5470(3) 0.1125(3) 0.0448(2) 0.0452(12) Uani 1.00 1 d . . . C(19) C 0.6327(3) 0.3040(3) 0.0348(3) 0.053(1) Uani 1.00 1 d . . . C(20) C 0.7350(3) 0.1596(3) 0.2473(3) 0.061(2) Uani 1.00 1 d . . . C(21) C 0.8883(3) 0.2780(4) 0.2402(4) 0.084(2) Uani 1.00 1 d . . . C(22) C 0.8289(4) 0.2764(4) 0.3795(3) 0.075(2) Uani 1.00 1 d . . . C(23) C 0.5830(4) 0.5107(3) 0.1262(3) 0.059(2) Uani 1.00 1 d . . . C(24) C 0.5983(3) 0.5702(3) 0.1876(3) 0.0496(13) Uani 1.00 1 d . . . C(25) C 0.5230(3) 0.5768(3) 0.2096(3) 0.0474(13) Uani 1.00 1 d . . . C(26) C 0.4609(3) 0.5198(3) 0.1634(3) 0.054(1) Uani 1.00 1 d . . . C(27) C 0.4984(4) 0.4804(3) 0.1103(3) 0.064(2) Uani 1.00 1 d . . . C(28) C 0.4936(3) 0.3378(3) 0.3063(2) 0.0396(11) Uani 1.00 1 d . . . C(29) C 0.4913(3) 0.4365(3) 0.3183(2) 0.0430(12) Uani 1.00 1 d . . . C(30) C 0.5759(3) 0.4687(3) 0.3486(2) 0.0455(12) Uani 1.00 1 d . . . C(31) C 0.6304(3) 0.3885(3) 0.3574(2) 0.0433(12) Uani 1.00 1 d . . . C(32) C 0.5794(3) 0.3077(3) 0.3307(2) 0.0410(11) Uani 1.00 1 d . . . H(1) H 0.0854 0.1605 -0.1417 0.062 Uiso 1.00 1 c . . . H(2) H 0.0786 0.0540 -0.1731 0.062 Uiso 1.00 1 c . . . H(3) H 0.0495 0.0769 -0.1007 0.062 Uiso 1.00 1 c . . . H(4) H 0.1694 -0.0793 -0.0196 0.063 Uiso 1.00 1 c . . . H(5) H 0.1972 -0.1017 -0.0928 0.063 Uiso 1.00 1 c . . . H(6) H 0.2679 -0.0784 -0.0188 0.063 Uiso 1.00 1 c . . . H(7) H 0.3376 0.0774 -0.0958 0.053 Uiso 1.00 1 c . . . H(8) H 0.2669 0.0534 -0.1697 0.053 Uiso 1.00 1 c . . . H(9) H 0.2777 0.1604 -0.1392 0.053 Uiso 1.00 1 c . . . H(10) H 0.1603 0.3174 -0.1488 0.080 Uiso 1.00 1 c . . . H(11) H 0.2101 0.4155 -0.1500 0.080 Uiso 1.00 1 c . . . H(12) H 0.2391 0.3448 -0.0818 0.080 Uiso 1.00 1 c . . . H(13) H -0.0143 0.5141 -0.1213 0.087 Uiso 1.00 1 c . . . H(14) H 0.0443 0.5229 -0.1767 0.087 Uiso 1.00 1 c . . . H(15) H -0.0069 0.4263 -0.1732 0.087 Uiso 1.00 1 c . . . H(16) H 0.2210 0.5153 0.0193 0.100 Uiso 1.00 1 c . . . H(17) H 0.1905 0.5802 -0.0521 0.100 Uiso 1.00 1 c . . . H(18) H 0.1320 0.5704 0.0033 0.101 Uiso 1.00 1 c . . . H(19) H -0.0419 0.2397 0.0863 0.059 Uiso 1.00 1 c . . . H(20) H -0.0121 0.1335 -0.0150 0.053 Uiso 1.00 1 c . . . H(21) H 0.1081 0.0198 0.0454 0.059 Uiso 1.00 1 c . . . H(22) H 0.1525 0.0540 0.1826 0.064 Uiso 1.00 1 c . . . H(23) H 0.0575 0.1877 0.2080 0.068 Uiso 1.00 1 c . . . H(24) H 0.3373 0.2231 0.1687 0.062 Uiso 1.00 1 c . . . H(25) H 0.2351 0.2177 0.2496 0.064 Uiso 1.00 1 c . . . H(26) H 0.1294 0.3555 0.2125 0.065 Uiso 1.00 1 c . . . H(27) H 0.1695 0.4510 0.1108 0.064 Uiso 1.00 1 c . . . H(28) H 0.2969 0.3653 0.0819 0.067 Uiso 1.00 1 c . . . H(29) H 0.3892 0.2501 -0.0103 0.063 Uiso 1.00 1 c . . . H(30) H 0.4453 0.2640 -0.0673 0.062 Uiso 1.00 1 c . . . H(31) H 0.4320 0.3513 -0.0170 0.062 Uiso 1.00 1 c . . . H(32) H 0.5976 0.0906 0.0816 0.057 Uiso 1.00 1 c . . . H(33) H 0.5524 0.0961 -0.0040 0.057 Uiso 1.00 1 c . . . H(34) H 0.4965 0.0813 0.0530 0.057 Uiso 1.00 1 c . . . H(35) H 0.6280 0.3735 0.0386 0.069 Uiso 1.00 1 c . . . H(36) H 0.6371 0.2873 -0.0142 0.069 Uiso 1.00 1 c . . . H(37) H 0.6835 0.2817 0.0711 0.069 Uiso 1.00 1 c . . . H(38) H 0.7726 0.1058 0.2667 0.073 Uiso 1.00 1 c . . . H(39) H 0.7185 0.1568 0.1938 0.073 Uiso 1.00 1 c . . . H(40) H 0.6841 0.1561 0.2654 0.073 Uiso 1.00 1 c . . . H(41) H 0.9195 0.3377 0.2548 0.105 Uiso 1.00 1 c . . . H(42) H 0.8702 0.2741 0.1868 0.105 Uiso 1.00 1 c . . . H(43) H 0.9252 0.2237 0.2597 0.105 Uiso 1.00 1 c . . . H(44) H 0.7793 0.2755 0.3996 0.086 Uiso 1.00 1 c . . . H(45) H 0.8621 0.3344 0.3957 0.086 Uiso 1.00 1 c . . . H(46) H 0.8642 0.2202 0.3966 0.086 Uiso 1.00 1 c . . . H(47) H 0.6230 0.4984 0.0966 0.074 Uiso 1.00 1 c . . . H(48) H 0.6502 0.6075 0.2072 0.061 Uiso 1.00 1 c . . . H(49) H 0.5141 0.6190 0.2482 0.058 Uiso 1.00 1 c . . . H(50) H 0.4007 0.5168 0.1631 0.063 Uiso 1.00 1 c . . . H(51) H 0.4693 0.4437 0.0670 0.071 Uiso 1.00 1 c . . . H(52) H 0.4443 0.2958 0.2897 0.050 Uiso 1.00 1 c . . . H(53) H 0.4399 0.4754 0.3119 0.055 Uiso 1.00 1 c . . . H(54) H 0.5928 0.5331 0.3671 0.057 Uiso 1.00 1 c . . . H(55) H 0.6912 0.3877 0.3824 0.052 Uiso 1.00 1 c . . . H(56) H 0.5993 0.2415 0.3336 0.050 Uiso 1.00 1 c . . . 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 Ti(1) 0.0265(3) 0.0473(4) 0.0285(3) 0.0017(3) 0.0096(3) -0.0029(3) Ti(2) 0.0320(3) 0.0237(3) 0.0269(3) -0.0017(3) 0.0109(3) -0.0035(3) S(1) 0.0299(5) 0.0524(6) 0.0331(5) 0.0006(4) 0.0115(4) -0.0074(4) S(2) 0.0304(5) 0.0424(5) 0.0423(6) -0.0015(4) 0.0098(4) 0.0029(4) S(3) 0.0356(5) 0.0265(4) 0.0251(4) -0.0048(4) 0.0115(4) -0.0022(4) S(4) 0.0325(5) 0.0389(5) 0.0370(5) -0.0061(4) 0.0113(4) -0.0033(4) Si(1) 0.0374(6) 0.0434(6) 0.0297(5) 0.0023(5) 0.0101(5) -0.0015(5) Si(2) 0.0410(7) 0.0405(6) 0.0515(7) -0.0003(5) 0.0176(6) 0.0050(5) Si(3) 0.0398(6) 0.0295(5) 0.0262(5) -0.0068(4) 0.0140(4) -0.0024(4) Si(4) 0.0325(6) 0.0467(6) 0.0422(6) 0.0046(5) 0.0073(5) -0.0061(5) C(1) 0.048(3) 0.066(3) 0.040(2) -0.001(2) 0.005(2) -0.001(2) C(2) 0.060(3) 0.052(3) 0.046(3) 0.001(2) 0.022(2) -0.001(2) C(3) 0.049(3) 0.050(2) 0.033(2) 0.002(2) 0.015(2) -0.003(2) C(4) 0.065(3) 0.068(3) 0.068(3) 0.013(3) 0.036(3) 0.018(3) C(5) 0.067(4) 0.063(3) 0.088(4) 0.013(3) 0.023(3) 0.036(3) C(6) 0.101(5) 0.057(3) 0.093(5) -0.029(3) 0.036(4) -0.004(3) C(7) 0.029(2) 0.061(3) 0.059(3) 0.002(2) 0.021(2) 0.009(2) C(8) 0.039(2) 0.052(2) 0.041(2) -0.014(2) 0.010(2) 0.003(2) C(9) 0.043(2) 0.049(3) 0.057(3) -0.006(2) 0.025(2) 0.001(2) C(10) 0.043(3) 0.069(3) 0.048(3) 0.012(2) 0.014(2) 0.024(2) C(11) 0.050(3) 0.076(3) 0.043(3) -0.005(3) 0.027(2) 0.002(2) C(12) 0.032(2) 0.084(3) 0.039(2) 0.006(2) -0.000(2) -0.021(2) C(13) 0.046(3) 0.087(3) 0.028(2) 0.013(3) 0.001(2) -0.009(2) C(14) 0.047(3) 0.080(3) 0.036(2) 0.004(2) 0.011(2) -0.018(2) C(15) 0.050(3) 0.055(3) 0.054(3) -0.008(2) 0.011(2) -0.019(2) C(16) 0.044(3) 0.077(3) 0.047(3) -0.023(2) 0.014(2) -0.031(3) C(17) 0.066(3) 0.059(3) 0.031(2) 0.000(2) 0.008(2) 0.001(2) C(18) 0.071(3) 0.033(2) 0.038(2) -0.005(2) 0.026(2) -0.007(2) C(19) 0.066(3) 0.056(3) 0.051(3) -0.025(2) 0.037(3) -0.020(2) C(20) 0.058(3) 0.043(3) 0.081(4) 0.012(2) 0.014(3) -0.002(3) C(21) 0.049(3) 0.094(4) 0.119(5) 0.014(3) 0.041(4) 0.007(4) C(22) 0.082(4) 0.084(4) 0.049(3) 0.029(3) -0.005(3) -0.010(3) C(23) 0.097(4) 0.042(3) 0.046(3) 0.020(3) 0.033(3) 0.016(2) C(24) 0.063(3) 0.025(2) 0.065(3) -0.001(2) 0.024(3) 0.009(2) C(25) 0.068(3) 0.025(2) 0.052(3) 0.009(2) 0.020(2) -0.002(2) C(26) 0.049(3) 0.034(2) 0.074(3) 0.011(2) 0.006(3) 0.011(2) C(27) 0.104(5) 0.033(2) 0.040(3) 0.020(3) -0.010(3) 0.004(2) C(28) 0.045(2) 0.049(2) 0.030(2) -0.013(2) 0.020(2) -0.007(2) C(29) 0.044(2) 0.051(3) 0.043(2) 0.000(2) 0.026(2) -0.007(2) C(30) 0.066(3) 0.044(2) 0.033(2) -0.010(2) 0.025(2) -0.015(2) C(31) 0.041(2) 0.067(3) 0.023(2) -0.006(2) 0.010(2) -0.006(2) C(32) 0.062(3) 0.039(2) 0.026(2) 0.002(2) 0.018(2) -0.001(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; 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 Ti(1) S(1) 2.414(1) yes . . Ti(1) S(2) 2.439(1) yes . . Ti(1) C(7) 2.388(5) yes . . Ti(1) C(8) 2.399(4) yes . . Ti(1) C(9) 2.386(4) yes . . Ti(1) C(10) 2.373(5) yes . . Ti(1) C(11) 2.406(5) yes . . Ti(1) C(12) 2.398(4) yes . . Ti(1) C(13) 2.378(4) yes . . Ti(1) C(14) 2.356(5) yes . . Ti(1) C(15) 2.420(5) yes . . Ti(1) C(16) 2.415(5) yes . . Ti(2) S(3) 2.413(1) yes . . Ti(2) S(4) 2.436(1) yes . . Ti(2) C(23) 2.390(5) yes . . Ti(2) C(24) 2.377(4) yes . . Ti(2) C(25) 2.378(4) yes . . Ti(2) C(26) 2.371(4) yes . . Ti(2) C(27) 2.397(5) yes . . Ti(2) C(28) 2.400(4) yes . . Ti(2) C(29) 2.394(5) yes . . Ti(2) C(30) 2.367(4) yes . . Ti(2) C(31) 2.393(4) yes . . Ti(2) C(32) 2.400(4) yes . . S(1) Si(1) 2.132(1) yes . . S(2) Si(2) 2.129(2) yes . . S(3) Si(3) 2.149(1) yes . . S(4) Si(4) 2.135(1) yes . . Si(1) C(1) 1.865(4) yes . . Si(1) C(2) 1.867(4) yes . . Si(1) C(3) 1.857(5) yes . . Si(2) C(4) 1.864(6) yes . . Si(2) C(5) 1.861(5) yes . . Si(2) C(6) 1.859(6) yes . . Si(3) C(17) 1.858(4) yes . . Si(3) C(18) 1.854(4) yes . . Si(3) C(19) 1.860(5) yes . . Si(4) C(20) 1.859(4) yes . . Si(4) C(21) 1.862(7) yes . . Si(4) C(22) 1.856(5) yes . . C(7) C(8) 1.411(7) yes . . C(7) C(11) 1.395(6) yes . . C(8) C(9) 1.391(6) yes . . C(9) C(10) 1.405(7) yes . . C(10) C(11) 1.391(7) yes . . C(12) C(13) 1.386(7) yes . . C(12) C(16) 1.402(7) yes . . C(13) C(14) 1.411(7) yes . . C(14) C(15) 1.400(7) yes . . C(15) C(16) 1.406(7) yes . . C(23) C(24) 1.387(7) yes . . C(23) C(27) 1.383(9) yes . . C(24) C(25) 1.386(8) yes . . C(25) C(26) 1.388(6) yes . . C(26) C(27) 1.406(8) yes . . C(28) C(29) 1.389(6) yes . . C(28) C(32) 1.403(6) yes . . C(29) C(30) 1.407(6) yes . . C(30) C(31) 1.402(6) yes . . C(31) C(32) 1.402(6) yes . . 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 S(1) Ti(1) S(2) 100.71(4) yes . . . S(1) Ti(1) C(7) 133.4(1) yes . . . S(1) Ti(1) C(8) 99.6(1) yes . . . S(1) Ti(1) C(9) 80.7(1) yes . . . S(1) Ti(1) C(10) 98.4(1) yes . . . S(1) Ti(1) C(11) 132.0(1) yes . . . S(1) Ti(1) C(12) 75.4(1) yes . . . S(1) Ti(1) C(13) 105.2(1) yes . . . S(1) Ti(1) C(14) 131.3(1) yes . . . S(1) Ti(1) C(15) 112.0(1) yes . . . S(1) Ti(1) C(16) 79.5(1) yes . . . S(2) Ti(1) C(7) 78.3(1) yes . . . S(2) Ti(1) C(8) 76.1(1) yes . . . S(2) Ti(1) C(9) 107.0(1) yes . . . S(2) Ti(1) C(10) 131.5(1) yes . . . S(2) Ti(1) C(11) 110.5(1) yes . . . S(2) Ti(1) C(12) 128.1(1) yes . . . S(2) Ti(1) C(13) 135.0(1) yes . . . S(2) Ti(1) C(14) 101.9(1) yes . . . S(2) Ti(1) C(15) 79.6(1) yes . . . S(2) Ti(1) C(16) 94.3(1) yes . . . C(7) Ti(1) C(8) 34.3(2) yes . . . C(7) Ti(1) C(9) 56.3(2) yes . . . C(7) Ti(1) C(10) 56.6(2) yes . . . C(7) Ti(1) C(11) 33.8(1) yes . . . C(7) Ti(1) C(12) 140.9(2) yes . . . C(7) Ti(1) C(13) 107.4(2) yes . . . C(7) Ti(1) C(14) 93.3(2) yes . . . C(7) Ti(1) C(15) 113.5(2) yes . . . C(7) Ti(1) C(16) 147.0(2) yes . . . C(8) Ti(1) C(9) 33.8(1) yes . . . C(8) Ti(1) C(10) 57.0(1) yes . . . C(8) Ti(1) C(11) 56.5(2) yes . . . C(8) Ti(1) C(12) 155.6(2) yes . . . C(8) Ti(1) C(13) 132.9(2) yes . . . C(8) Ti(1) C(14) 127.5(2) yes . . . C(8) Ti(1) C(15) 143.1(2) yes . . . C(8) Ti(1) C(16) 170.0(2) yes . . . C(9) Ti(1) C(10) 34.3(2) yes . . . C(9) Ti(1) C(11) 56.1(2) yes . . . C(9) Ti(1) C(12) 122.7(2) yes . . . C(9) Ti(1) C(13) 113.0(2) yes . . . C(9) Ti(1) C(14) 131.0(2) yes . . . C(9) Ti(1) C(15) 164.8(2) yes . . . C(9) Ti(1) C(16) 153.2(2) yes . . . C(10) Ti(1) C(11) 33.8(2) yes . . . C(10) Ti(1) C(12) 99.7(2) yes . . . C(10) Ti(1) C(13) 80.1(2) yes . . . C(10) Ti(1) C(14) 97.9(2) yes . . . C(10) Ti(1) C(15) 131.7(2) yes . . . C(10) Ti(1) C(16) 133.0(1) yes . . . C(11) Ti(1) C(12) 108.9(2) yes . . . C(11) Ti(1) C(13) 77.4(2) yes . . . C(11) Ti(1) C(14) 77.0(2) yes . . . C(11) Ti(1) C(15) 108.8(2) yes . . . C(11) Ti(1) C(16) 131.0(2) yes . . . C(12) Ti(1) C(13) 33.7(2) yes . . . C(12) Ti(1) C(14) 56.8(2) yes . . . C(12) Ti(1) C(15) 56.5(2) yes . . . C(12) Ti(1) C(16) 33.9(2) yes . . . C(13) Ti(1) C(14) 34.7(2) yes . . . C(13) Ti(1) C(15) 56.8(2) yes . . . C(13) Ti(1) C(16) 56.2(2) yes . . . C(14) Ti(1) C(15) 34.1(2) yes . . . C(14) Ti(1) C(16) 56.4(2) yes . . . C(15) Ti(1) C(16) 33.8(2) yes . . . S(3) Ti(2) S(4) 97.72(4) yes . . . S(3) Ti(2) C(23) 98.5(1) yes . . . S(3) Ti(2) C(24) 132.2(1) yes . . . S(3) Ti(2) C(25) 133.1(1) yes . . . S(3) Ti(2) C(26) 99.6(1) yes . . . S(3) Ti(2) C(27) 80.8(1) yes . . . S(3) Ti(2) C(28) 78.0(1) yes . . . S(3) Ti(2) C(29) 108.3(1) yes . . . S(3) Ti(2) C(30) 133.5(1) yes . . . S(3) Ti(2) C(31) 112.6(1) yes . . . S(3) Ti(2) C(32) 80.44(9) yes . . . S(4) Ti(2) C(23) 76.5(2) yes . . . S(4) Ti(2) C(24) 78.6(1) yes . . . S(4) Ti(2) C(25) 110.9(1) yes . . . S(4) Ti(2) C(26) 131.8(1) yes . . . S(4) Ti(2) C(27) 107.0(2) yes . . . S(4) Ti(2) C(28) 128.8(1) yes . . . S(4) Ti(2) C(29) 135.2(1) yes . . . S(4) Ti(2) C(30) 102.3(1) yes . . . S(4) Ti(2) C(31) 80.0(1) yes . . . S(4) Ti(2) C(32) 94.8(1) yes . . . C(23) Ti(2) C(24) 33.8(2) yes . . . C(23) Ti(2) C(25) 56.1(2) yes . . . C(23) Ti(2) C(26) 56.7(2) yes . . . C(23) Ti(2) C(27) 33.6(2) yes . . . C(23) Ti(2) C(28) 154.6(2) yes . . . C(23) Ti(2) C(29) 131.9(2) yes . . . C(23) Ti(2) C(30) 126.7(2) yes . . . C(23) Ti(2) C(31) 143.1(2) yes . . . C(23) Ti(2) C(32) 171.1(2) yes . . . C(24) Ti(2) C(25) 33.9(2) yes . . . C(24) Ti(2) C(26) 56.7(2) yes . . . C(24) Ti(2) C(27) 56.0(2) yes . . . C(24) Ti(2) C(28) 140.3(2) yes . . . C(24) Ti(2) C(29) 106.8(2) yes . . . C(24) Ti(2) C(30) 93.0(2) yes . . . C(24) Ti(2) C(31) 113.5(2) yes . . . C(24) Ti(2) C(32) 147.1(1) yes . . . C(25) Ti(2) C(26) 34.0(1) yes . . . C(25) Ti(2) C(27) 56.1(2) yes . . . C(25) Ti(2) C(28) 108.0(2) yes . . . C(25) Ti(2) C(29) 76.7(2) yes . . . C(25) Ti(2) C(30) 76.5(2) yes . . . C(25) Ti(2) C(31) 108.5(2) yes . . . C(25) Ti(2) C(32) 130.5(2) yes . . . C(26) Ti(2) C(27) 34.3(2) yes . . . C(26) Ti(2) C(28) 98.7(2) yes . . . C(26) Ti(2) C(29) 79.6(2) yes . . . C(26) Ti(2) C(30) 97.4(2) yes . . . C(26) Ti(2) C(31) 131.4(2) yes . . . C(26) Ti(2) C(32) 132.2(2) yes . . . C(27) Ti(2) C(28) 122.1(2) yes . . . C(27) Ti(2) C(29) 112.6(2) yes . . . C(27) Ti(2) C(30) 130.4(2) yes . . . C(27) Ti(2) C(31) 164.4(2) yes . . . C(27) Ti(2) C(32) 152.9(2) yes . . . C(28) Ti(2) C(29) 33.7(1) yes . . . C(28) Ti(2) C(30) 56.8(1) yes . . . C(28) Ti(2) C(31) 56.7(1) yes . . . C(28) Ti(2) C(32) 34.0(1) yes . . . C(29) Ti(2) C(30) 34.4(2) yes . . . C(29) Ti(2) C(31) 56.7(1) yes . . . C(29) Ti(2) C(32) 56.2(1) yes . . . C(30) Ti(2) C(31) 34.2(2) yes . . . C(30) Ti(2) C(32) 56.6(1) yes . . . C(31) Ti(2) C(32) 34.0(1) yes . . . Si(1) S(1) Ti(1) 123.22(5) yes . . . Si(2) S(2) Ti(1) 122.14(5) yes . . . Si(3) S(3) Ti(2) 120.44(5) yes . . . Si(4) S(4) Ti(2) 119.56(6) yes . . . C(1) Si(1) C(2) 108.8(2) yes . . . C(1) Si(1) C(3) 110.0(2) yes . . . C(1) Si(1) S(1) 114.8(2) yes . . . C(2) Si(1) C(3) 107.2(2) yes . . . C(2) Si(1) S(1) 112.2(1) yes . . . C(3) Si(1) S(1) 103.5(1) yes . . . C(4) Si(2) C(5) 107.9(3) yes . . . C(4) Si(2) C(6) 109.7(3) yes . . . C(4) Si(2) S(2) 110.8(2) yes . . . C(5) Si(2) C(6) 107.0(2) yes . . . C(5) Si(2) S(2) 104.3(2) yes . . . C(6) Si(2) S(2) 116.7(2) yes . . . C(17) Si(3) C(18) 106.9(2) yes . . . C(17) Si(3) C(19) 109.4(2) yes . . . C(17) Si(3) S(3) 112.0(2) yes . . . C(18) Si(3) C(19) 108.9(2) yes . . . C(18) Si(3) S(3) 104.4(2) yes . . . C(19) Si(3) S(3) 114.7(1) yes . . . C(20) Si(4) C(21) 107.5(3) yes . . . C(20) Si(4) C(22) 108.7(3) yes . . . C(20) Si(4) S(4) 114.4(1) yes . . . C(21) Si(4) C(22) 108.3(3) yes . . . C(21) Si(4) S(4) 103.7(2) yes . . . C(22) Si(4) S(4) 113.7(2) yes . . . C(8) C(7) C(11) 108.4(4) yes . . . C(8) C(7) Ti(1) 73.3(3) yes . . . C(11) C(7) Ti(1) 73.8(3) yes . . . C(9) C(8) Ti(1) 72.6(2) yes . . . C(7) C(8) C(9) 106.9(4) yes . . . C(7) C(8) Ti(1) 72.4(2) yes . . . C(10) C(9) Ti(1) 72.3(3) yes . . . C(8) C(9) C(10) 109.0(4) yes . . . C(8) C(9) Ti(1) 73.6(2) yes . . . C(11) C(10) Ti(1) 74.4(3) yes . . . C(9) C(10) C(11) 107.5(4) yes . . . C(9) C(10) Ti(1) 73.3(3) yes . . . C(7) C(11) Ti(1) 72.4(3) yes . . . C(7) C(11) C(10) 108.2(4) yes . . . C(10) C(11) Ti(1) 71.8(3) yes . . . C(13) C(12) C(16) 108.2(4) yes . . . C(13) C(12) Ti(1) 72.3(2) yes . . . C(16) C(12) Ti(1) 73.7(2) yes . . . C(14) C(13) Ti(1) 71.8(2) yes . . . C(12) C(13) C(14) 107.8(4) yes . . . C(12) C(13) Ti(1) 73.9(2) yes . . . C(15) C(14) Ti(1) 75.5(3) yes . . . C(13) C(14) C(15) 108.5(4) yes . . . C(13) C(14) Ti(1) 73.5(3) yes . . . C(16) C(15) Ti(1) 72.9(3) yes . . . C(14) C(15) C(16) 106.9(4) yes . . . C(14) C(15) Ti(1) 70.5(3) yes . . . C(12) C(16) Ti(1) 72.4(3) yes . . . C(12) C(16) C(15) 108.6(5) yes . . . C(15) C(16) Ti(1) 73.3(3) yes . . . C(24) C(23) C(27) 108.1(5) yes . . . C(24) C(23) Ti(2) 72.6(3) yes . . . C(27) C(23) Ti(2) 73.5(3) yes . . . C(25) C(24) Ti(2) 73.1(2) yes . . . C(23) C(24) C(25) 107.9(4) yes . . . C(23) C(24) Ti(2) 73.6(3) yes . . . C(26) C(25) Ti(2) 72.7(2) yes . . . C(24) C(25) C(26) 108.8(4) yes . . . C(24) C(25) Ti(2) 73.0(2) yes . . . C(27) C(26) Ti(2) 73.8(3) yes . . . C(25) C(26) C(27) 106.8(5) yes . . . C(25) C(26) Ti(2) 73.3(2) yes . . . C(23) C(27) Ti(2) 72.9(3) yes . . . C(23) C(27) C(26) 108.3(4) yes . . . C(26) C(27) Ti(2) 71.9(3) yes . . . C(29) C(28) C(32) 107.8(4) yes . . . C(29) C(28) Ti(2) 72.9(3) yes . . . C(32) C(28) Ti(2) 73.0(3) yes . . . C(30) C(29) Ti(2) 71.8(3) yes . . . C(28) C(29) C(30) 108.3(4) yes . . . C(28) C(29) Ti(2) 73.4(3) yes . . . C(31) C(30) Ti(2) 73.9(2) yes . . . C(29) C(30) C(31) 108.0(4) yes . . . C(29) C(30) Ti(2) 73.9(2) yes . . . C(32) C(31) Ti(2) 73.3(2) yes . . . C(30) C(31) C(32) 107.5(4) yes . . . C(30) C(31) Ti(2) 71.9(2) yes . . . C(28) C(32) Ti(2) 73.0(2) yes . . . C(28) C(32) C(31) 108.4(4) yes . . . C(31) C(32) Ti(2) 72.7(2) yes . . . 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 S(2) Ti(1) S(1) Si(1) -60.42(7) yes . . . . C(7) Ti(1) S(1) Si(1) 23.58(9) yes . . . . C(8) Ti(1) S(1) Si(1) 17.10(7) yes . . . . C(9) Ti(1) S(1) Si(1) 45.26(6) yes . . . . C(10) Ti(1) S(1) Si(1) 74.81(6) yes . . . . C(11) Ti(1) S(1) Si(1) 70.18(8) yes . . . . C(12) Ti(1) S(1) Si(1) 172.70(7) yes . . . . C(13) Ti(1) S(1) Si(1) 156.74(6) yes . . . . C(14) Ti(1) S(1) Si(1) -176.85(6) yes . . . . C(15) Ti(1) S(1) Si(1) -143.40(6) yes . . . . C(16) Ti(1) S(1) Si(1) -152.82(6) yes . . . . S(1) Ti(1) S(2) Si(2) -54.29(7) yes . . . . C(7) Ti(1) S(2) Si(2) 173.27(7) yes . . . . C(8) Ti(1) S(2) Si(2) -151.61(7) yes . . . . C(9) Ti(1) S(2) Si(2) -137.74(6) yes . . . . C(10) Ti(1) S(2) Si(2) -165.77(6) yes . . . . C(11) Ti(1) S(2) Si(2) 162.76(6) yes . . . . C(12) Ti(1) S(2) Si(2) 25.5(1) yes . . . . C(13) Ti(1) S(2) Si(2) 70.3(1) yes . . . . C(14) Ti(1) S(2) Si(2) 82.32(7) yes . . . . C(15) Ti(1) S(2) Si(2) 56.39(7) yes . . . . C(16) Ti(1) S(2) Si(2) 25.80(7) yes . . . . S(1) Ti(1) C(7) C(8) -11.4(3) yes . . . . S(1) Ti(1) C(7) C(11) 104.1(3) yes . . . . S(2) Ti(1) C(7) C(8) 82.4(2) yes . . . . S(2) Ti(1) C(7) C(11) -162.1(3) yes . . . . C(8) Ti(1) C(7) C(11) 115.5(3) yes . . . . C(9) Ti(1) C(7) C(8) -37.4(2) yes . . . . C(9) Ti(1) C(7) C(11) 78.1(3) yes . . . . C(10) Ti(1) C(7) C(8) -78.9(2) yes . . . . C(10) Ti(1) C(7) C(11) 36.6(2) yes . . . . C(11) Ti(1) C(7) C(8) -115.5(3) yes . . . . C(12) Ti(1) C(7) C(8) -139.4(2) yes . . . . C(12) Ti(1) C(7) C(11) -23.9(4) yes . . . . C(13) Ti(1) C(7) C(8) -143.9(2) yes . . . . C(13) Ti(1) C(7) C(11) -28.4(3) yes . . . . C(14) Ti(1) C(7) C(8) -176.2(2) yes . . . . C(14) Ti(1) C(7) C(11) -60.7(3) yes . . . . C(15) Ti(1) C(7) C(8) 155.4(2) yes . . . . C(15) Ti(1) C(7) C(11) -89.1(3) yes . . . . C(16) Ti(1) C(7) C(8) 162.1(2) yes . . . . C(16) Ti(1) C(7) C(11) -82.4(3) yes . . . . S(1) Ti(1) C(8) C(7) 171.6(2) yes . . . . S(1) Ti(1) C(8) C(9) 56.9(3) yes . . . . S(2) Ti(1) C(8) C(7) -89.6(2) yes . . . . S(2) Ti(1) C(8) C(9) 155.7(3) yes . . . . C(7) Ti(1) C(8) C(9) -114.7(4) yes . . . . C(9) Ti(1) C(8) C(7) 114.7(3) yes . . . . C(10) Ti(1) C(8) C(7) 77.8(2) yes . . . . C(10) Ti(1) C(8) C(9) -37.0(3) yes . . . . C(11) Ti(1) C(8) C(7) 37.0(2) yes . . . . C(11) Ti(1) C(8) C(9) -77.7(3) yes . . . . C(12) Ti(1) C(8) C(7) 95.9(3) yes . . . . C(12) Ti(1) C(8) C(9) -18.8(5) yes . . . . C(13) Ti(1) C(8) C(7) 50.2(3) yes . . . . C(13) Ti(1) C(8) C(9) -64.5(3) yes . . . . C(14) Ti(1) C(8) C(7) 4.8(3) yes . . . . C(14) Ti(1) C(8) C(9) -109.9(3) yes . . . . C(15) Ti(1) C(8) C(7) -39.4(3) yes . . . . C(15) Ti(1) C(8) C(9) -154.1(2) yes . . . . S(1) Ti(1) C(9) C(8) -123.2(3) yes . . . . S(1) Ti(1) C(9) C(10) 120.1(3) yes . . . . S(2) Ti(1) C(9) C(8) -24.7(3) yes . . . . S(2) Ti(1) C(9) C(10) -141.4(2) yes . . . . C(7) Ti(1) C(9) C(8) 38.0(2) yes . . . . C(7) Ti(1) C(9) C(10) -78.7(3) yes . . . . C(8) Ti(1) C(9) C(10) -116.7(4) yes . . . . C(10) Ti(1) C(9) C(8) 116.7(4) yes . . . . C(11) Ti(1) C(9) C(8) 79.0(3) yes . . . . C(11) Ti(1) C(9) C(10) -37.7(2) yes . . . . C(12) Ti(1) C(9) C(8) 170.9(2) yes . . . . C(12) Ti(1) C(9) C(10) 54.2(3) yes . . . . C(13) Ti(1) C(9) C(8) 134.1(3) yes . . . . C(13) Ti(1) C(9) C(10) 17.4(3) yes . . . . C(14) Ti(1) C(9) C(8) 98.7(3) yes . . . . C(14) Ti(1) C(9) C(10) -18.0(3) yes . . . . C(15) Ti(1) C(9) C(8) 89.0(5) yes . . . . C(15) Ti(1) C(9) C(10) -27.7(6) yes . . . . C(16) Ti(1) C(9) C(8) -165.9(2) yes . . . . C(16) Ti(1) C(9) C(10) 77.5(4) yes . . . . S(1) Ti(1) C(10) C(9) -59.6(3) yes . . . . S(1) Ti(1) C(10) C(11) -173.8(2) yes . . . . S(2) Ti(1) C(10) C(9) 52.8(3) yes . . . . S(2) Ti(1) C(10) C(11) -61.4(3) yes . . . . C(7) Ti(1) C(10) C(9) 77.6(2) yes . . . . C(7) Ti(1) C(10) C(11) -36.6(2) yes . . . . C(8) Ti(1) C(10) C(9) 36.4(2) yes . . . . C(8) Ti(1) C(10) C(11) -77.8(2) yes . . . . C(9) Ti(1) C(10) C(11) -114.2(3) yes . . . . C(11) Ti(1) C(10) C(9) 114.2(3) yes . . . . C(12) Ti(1) C(10) C(9) -136.2(2) yes . . . . C(12) Ti(1) C(10) C(11) 109.7(2) yes . . . . C(13) Ti(1) C(10) C(9) -163.7(3) yes . . . . C(13) Ti(1) C(10) C(11) 82.1(2) yes . . . . C(14) Ti(1) C(10) C(9) 166.4(2) yes . . . . C(14) Ti(1) C(10) C(11) 52.2(2) yes . . . . C(15) Ti(1) C(10) C(9) 170.6(2) yes . . . . C(15) Ti(1) C(10) C(11) 56.4(3) yes . . . . C(16) Ti(1) C(10) C(9) -143.1(2) yes . . . . C(16) Ti(1) C(10) C(11) 102.8(2) yes . . . . S(1) Ti(1) C(11) C(7) -108.5(3) yes . . . . S(1) Ti(1) C(11) C(10) 8.3(3) yes . . . . S(2) Ti(1) C(11) C(7) 18.7(3) yes . . . . S(2) Ti(1) C(11) C(10) 135.4(2) yes . . . . C(7) Ti(1) C(11) C(10) 116.7(3) yes . . . . C(8) Ti(1) C(11) C(7) -37.6(2) yes . . . . C(8) Ti(1) C(11) C(10) 79.2(2) yes . . . . C(9) Ti(1) C(11) C(7) -78.4(3) yes . . . . C(9) Ti(1) C(11) C(10) 38.3(2) yes . . . . C(10) Ti(1) C(11) C(7) -116.7(3) yes . . . . C(12) Ti(1) C(11) C(7) 164.4(2) yes . . . . C(12) Ti(1) C(11) C(10) -78.9(2) yes . . . . C(13) Ti(1) C(11) C(7) 152.3(3) yes . . . . C(13) Ti(1) C(11) C(10) -91.0(2) yes . . . . C(14) Ti(1) C(11) C(7) 116.7(3) yes . . . . C(14) Ti(1) C(11) C(10) -126.6(2) yes . . . . C(15) Ti(1) C(11) C(7) 104.3(3) yes . . . . C(15) Ti(1) C(11) C(10) -138.9(2) yes . . . . C(16) Ti(1) C(11) C(7) 134.3(2) yes . . . . C(16) Ti(1) C(11) C(10) -109.0(2) yes . . . . S(1) Ti(1) C(12) C(13) -151.5(3) yes . . . . S(1) Ti(1) C(12) C(16) 92.8(3) yes . . . . S(2) Ti(1) C(12) C(13) 116.2(3) yes . . . . S(2) Ti(1) C(12) C(16) 0.5(4) yes . . . . C(7) Ti(1) C(12) C(13) -7.8(4) yes . . . . C(7) Ti(1) C(12) C(16) -123.5(3) yes . . . . C(8) Ti(1) C(12) C(13) -70.6(4) yes . . . . C(8) Ti(1) C(12) C(16) 173.7(3) yes . . . . C(9) Ti(1) C(12) C(13) -82.9(3) yes . . . . C(9) Ti(1) C(12) C(16) 161.4(3) yes . . . . C(10) Ti(1) C(12) C(13) -55.2(3) yes . . . . C(10) Ti(1) C(12) C(16) -170.9(3) yes . . . . C(11) Ti(1) C(12) C(13) -21.5(3) yes . . . . C(11) Ti(1) C(12) C(16) -137.3(3) yes . . . . C(13) Ti(1) C(12) C(16) -115.7(4) yes . . . . C(14) Ti(1) C(12) C(13) 37.9(3) yes . . . . C(14) Ti(1) C(12) C(16) -77.8(3) yes . . . . C(15) Ti(1) C(12) C(13) 79.0(3) yes . . . . C(15) Ti(1) C(12) C(16) -36.7(3) yes . . . . C(16) Ti(1) C(12) C(13) 115.7(4) yes . . . . S(1) Ti(1) C(13) C(12) 28.6(3) yes . . . . S(1) Ti(1) C(13) C(14) 144.1(3) yes . . . . S(2) Ti(1) C(13) C(12) -94.3(3) yes . . . . S(2) Ti(1) C(13) C(14) 21.1(4) yes . . . . C(7) Ti(1) C(13) C(12) 174.9(3) yes . . . . C(7) Ti(1) C(13) C(14) -69.7(3) yes . . . . C(8) Ti(1) C(13) C(12) 147.9(3) yes . . . . C(8) Ti(1) C(13) C(14) -96.7(3) yes . . . . C(9) Ti(1) C(13) C(12) 114.8(3) yes . . . . C(9) Ti(1) C(13) C(14) -129.7(3) yes . . . . C(10) Ti(1) C(13) C(12) 124.7(3) yes . . . . C(10) Ti(1) C(13) C(14) -119.8(3) yes . . . . C(11) Ti(1) C(13) C(12) 159.2(3) yes . . . . C(11) Ti(1) C(13) C(14) -85.4(3) yes . . . . C(12) Ti(1) C(13) C(14) 115.4(4) yes . . . . C(14) Ti(1) C(13) C(12) -115.4(4) yes . . . . C(15) Ti(1) C(13) C(12) -78.0(3) yes . . . . C(15) Ti(1) C(13) C(14) 37.4(3) yes . . . . C(16) Ti(1) C(13) C(12) -37.2(3) yes . . . . C(16) Ti(1) C(13) C(14) 78.3(3) yes . . . . S(1) Ti(1) C(14) C(13) -49.0(3) yes . . . . S(1) Ti(1) C(14) C(15) 65.8(3) yes . . . . S(2) Ti(1) C(14) C(13) -164.9(3) yes . . . . S(2) Ti(1) C(14) C(15) -50.2(3) yes . . . . C(7) Ti(1) C(14) C(13) 116.3(3) yes . . . . C(7) Ti(1) C(14) C(15) -128.9(3) yes . . . . C(8) Ti(1) C(14) C(13) 113.6(3) yes . . . . C(8) Ti(1) C(14) C(15) -131.6(2) yes . . . . C(9) Ti(1) C(14) C(13) 69.7(3) yes . . . . C(9) Ti(1) C(14) C(15) -175.5(2) yes . . . . C(10) Ti(1) C(14) C(13) 59.6(3) yes . . . . C(10) Ti(1) C(14) C(15) 174.4(2) yes . . . . C(11) Ti(1) C(14) C(13) 86.4(3) yes . . . . C(11) Ti(1) C(14) C(15) -158.8(3) yes . . . . C(12) Ti(1) C(14) C(13) -36.8(2) yes . . . . C(12) Ti(1) C(14) C(15) 77.9(3) yes . . . . C(13) Ti(1) C(14) C(15) 114.8(4) yes . . . . C(15) Ti(1) C(14) C(13) -114.8(4) yes . . . . C(16) Ti(1) C(14) C(13) -77.7(3) yes . . . . C(16) Ti(1) C(14) C(15) 37.1(2) yes . . . . S(1) Ti(1) C(15) C(14) -132.4(2) yes . . . . S(1) Ti(1) C(15) C(16) -16.8(3) yes . . . . S(2) Ti(1) C(15) C(14) 130.2(3) yes . . . . S(2) Ti(1) C(15) C(16) -114.2(3) yes . . . . C(7) Ti(1) C(15) C(14) 57.9(3) yes . . . . C(7) Ti(1) C(15) C(16) 173.5(2) yes . . . . C(8) Ti(1) C(15) C(14) 80.8(3) yes . . . . C(8) Ti(1) C(15) C(16) -163.6(2) yes . . . . C(9) Ti(1) C(15) C(14) 13.1(6) yes . . . . C(9) Ti(1) C(15) C(16) 128.7(4) yes . . . . C(10) Ti(1) C(15) C(14) -7.5(3) yes . . . . C(10) Ti(1) C(15) C(16) 108.1(3) yes . . . . C(11) Ti(1) C(15) C(14) 21.9(3) yes . . . . C(11) Ti(1) C(15) C(16) 137.5(3) yes . . . . C(12) Ti(1) C(15) C(14) -78.8(2) yes . . . . C(12) Ti(1) C(15) C(16) 36.8(2) yes . . . . C(13) Ti(1) C(15) C(14) -38.1(2) yes . . . . C(13) Ti(1) C(15) C(16) 77.4(3) yes . . . . C(14) Ti(1) C(15) C(16) 115.6(3) yes . . . . C(16) Ti(1) C(15) C(14) -115.6(3) yes . . . . S(1) Ti(1) C(16) C(12) -79.5(3) yes . . . . S(1) Ti(1) C(16) C(15) 164.2(3) yes . . . . S(2) Ti(1) C(16) C(12) -179.6(3) yes . . . . S(2) Ti(1) C(16) C(15) 64.1(3) yes . . . . C(7) Ti(1) C(16) C(12) 105.3(3) yes . . . . C(7) Ti(1) C(16) C(15) -11.0(4) yes . . . . C(9) Ti(1) C(16) C(12) -36.6(5) yes . . . . C(9) Ti(1) C(16) C(15) -153.0(2) yes . . . . C(10) Ti(1) C(16) C(12) 12.3(4) yes . . . . C(10) Ti(1) C(16) C(15) -104.1(3) yes . . . . C(11) Ti(1) C(16) C(12) 58.3(3) yes . . . . C(11) Ti(1) C(16) C(15) -58.0(3) yes . . . . C(12) Ti(1) C(16) C(15) -116.4(4) yes . . . . C(13) Ti(1) C(16) C(12) 37.0(3) yes . . . . C(13) Ti(1) C(16) C(15) -79.3(3) yes . . . . C(14) Ti(1) C(16) C(12) 79.0(3) yes . . . . C(14) Ti(1) C(16) C(15) -37.3(2) yes . . . . C(15) Ti(1) C(16) C(12) 116.4(4) yes . . . . S(4) Ti(2) S(3) Si(3) -61.04(6) yes . . . . C(23) Ti(2) S(3) Si(3) 16.33(6) yes . . . . C(24) Ti(2) S(3) Si(3) 20.52(8) yes . . . . C(25) Ti(2) S(3) Si(3) 67.19(8) yes . . . . C(26) Ti(2) S(3) Si(3) 73.81(6) yes . . . . C(27) Ti(2) S(3) Si(3) 44.98(6) yes . . . . C(28) Ti(2) S(3) Si(3) 170.76(6) yes . . . . C(29) Ti(2) S(3) Si(3) 155.90(5) yes . . . . C(30) Ti(2) S(3) Si(3) -176.28(5) yes . . . . C(31) Ti(2) S(3) Si(3) -143.39(5) yes . . . . C(32) Ti(2) S(3) Si(3) -154.69(6) yes . . . . S(3) Ti(2) S(4) Si(4) -55.49(6) yes . . . . C(23) Ti(2) S(4) Si(4) -152.47(6) yes . . . . C(24) Ti(2) S(4) Si(4) 172.91(6) yes . . . . C(25) Ti(2) S(4) Si(4) 162.38(5) yes . . . . C(26) Ti(2) S(4) Si(4) -165.80(5) yes . . . . C(27) Ti(2) S(4) Si(4) -138.19(5) yes . . . . C(28) Ti(2) S(4) Si(4) 25.28(8) yes . . . . C(29) Ti(2) S(4) Si(4) 70.44(7) yes . . . . C(30) Ti(2) S(4) Si(4) 82.33(6) yes . . . . C(31) Ti(2) S(4) Si(4) 56.21(6) yes . . . . C(32) Ti(2) S(4) Si(4) 25.49(6) yes . . . . S(3) Ti(2) C(23) C(24) 174.4(3) yes . . . . S(3) Ti(2) C(23) C(27) 58.8(3) yes . . . . S(4) Ti(2) C(23) C(24) -89.6(3) yes . . . . S(4) Ti(2) C(23) C(27) 154.8(3) yes . . . . C(24) Ti(2) C(23) C(27) -115.6(4) yes . . . . C(25) Ti(2) C(23) C(24) 37.4(3) yes . . . . C(25) Ti(2) C(23) C(27) -78.2(3) yes . . . . C(26) Ti(2) C(23) C(24) 78.5(3) yes . . . . C(26) Ti(2) C(23) C(27) -37.1(3) yes . . . . C(27) Ti(2) C(23) C(24) 115.6(4) yes . . . . C(28) Ti(2) C(23) C(24) 94.5(4) yes . . . . C(28) Ti(2) C(23) C(27) -21.2(5) yes . . . . C(29) Ti(2) C(23) C(24) 50.2(4) yes . . . . C(29) Ti(2) C(23) C(27) -65.4(3) yes . . . . C(30) Ti(2) C(23) C(24) 5.8(4) yes . . . . C(30) Ti(2) C(23) C(27) -109.8(3) yes . . . . C(31) Ti(2) C(23) C(24) -37.8(5) yes . . . . C(31) Ti(2) C(23) C(27) -153.4(2) yes . . . . S(3) Ti(2) C(24) C(23) -7.5(4) yes . . . . S(3) Ti(2) C(24) C(25) 107.7(3) yes . . . . S(4) Ti(2) C(24) C(23) 82.7(3) yes . . . . S(4) Ti(2) C(24) C(25) -162.2(3) yes . . . . C(23) Ti(2) C(24) C(25) 115.2(3) yes . . . . C(25) Ti(2) C(24) C(23) -115.2(4) yes . . . . C(26) Ti(2) C(24) C(23) -78.5(3) yes . . . . C(26) Ti(2) C(24) C(25) 36.7(2) yes . . . . C(27) Ti(2) C(24) C(23) -37.0(3) yes . . . . C(27) Ti(2) C(24) C(25) 78.2(2) yes . . . . C(28) Ti(2) C(24) C(23) -138.0(3) yes . . . . C(28) Ti(2) C(24) C(25) -22.9(3) yes . . . . C(29) Ti(2) C(24) C(23) -143.3(3) yes . . . . C(29) Ti(2) C(24) C(25) -28.1(3) yes . . . . C(30) Ti(2) C(24) C(23) -175.3(3) yes . . . . C(30) Ti(2) C(24) C(25) -60.2(2) yes . . . . C(31) Ti(2) C(24) C(23) 156.3(3) yes . . . . C(31) Ti(2) C(24) C(25) -88.5(2) yes . . . . C(32) Ti(2) C(24) C(23) 163.8(3) yes . . . . C(32) Ti(2) C(24) C(25) -81.0(3) yes . . . . S(3) Ti(2) C(25) C(24) -104.9(3) yes . . . . S(3) Ti(2) C(25) C(26) 11.7(4) yes . . . . S(4) Ti(2) C(25) C(24) 18.7(3) yes . . . . S(4) Ti(2) C(25) C(26) 135.3(3) yes . . . . C(23) Ti(2) C(25) C(24) -37.4(2) yes . . . . C(23) Ti(2) C(25) C(26) 79.2(3) yes . . . . C(24) Ti(2) C(25) C(26) 116.6(4) yes . . . . C(26) Ti(2) C(25) C(24) -116.6(3) yes . . . . C(27) Ti(2) C(25) C(24) -78.1(3) yes . . . . C(27) Ti(2) C(25) C(26) 38.5(3) yes . . . . C(28) Ti(2) C(25) C(24) 164.9(2) yes . . . . C(28) Ti(2) C(25) C(26) -78.6(3) yes . . . . C(29) Ti(2) C(25) C(24) 152.4(3) yes . . . . C(29) Ti(2) C(25) C(26) -91.0(3) yes . . . . C(30) Ti(2) C(25) C(24) 117.0(2) yes . . . . C(30) Ti(2) C(25) C(26) -126.4(3) yes . . . . C(31) Ti(2) C(25) C(24) 104.8(2) yes . . . . C(31) Ti(2) C(25) C(26) -138.6(3) yes . . . . C(32) Ti(2) C(25) C(24) 135.1(2) yes . . . . C(32) Ti(2) C(25) C(26) -108.3(3) yes . . . . S(3) Ti(2) C(26) C(25) -171.3(3) yes . . . . S(3) Ti(2) C(26) C(27) -57.6(3) yes . . . . S(4) Ti(2) C(26) C(25) -61.8(4) yes . . . . S(4) Ti(2) C(26) C(27) 51.9(3) yes . . . . C(23) Ti(2) C(26) C(25) -77.4(3) yes . . . . C(23) Ti(2) C(26) C(27) 36.3(3) yes . . . . C(24) Ti(2) C(26) C(25) -36.6(3) yes . . . . C(24) Ti(2) C(26) C(27) 77.1(3) yes . . . . C(25) Ti(2) C(26) C(27) 113.7(4) yes . . . . C(27) Ti(2) C(26) C(25) -113.7(4) yes . . . . C(28) Ti(2) C(26) C(25) 109.5(3) yes . . . . C(28) Ti(2) C(26) C(27) -136.8(3) yes . . . . C(29) Ti(2) C(26) C(25) 81.6(3) yes . . . . C(29) Ti(2) C(26) C(27) -164.7(3) yes . . . . C(30) Ti(2) C(26) C(25) 52.1(3) yes . . . . C(30) Ti(2) C(26) C(27) 165.8(3) yes . . . . C(31) Ti(2) C(26) C(25) 56.7(4) yes . . . . C(31) Ti(2) C(26) C(27) 170.4(2) yes . . . . C(32) Ti(2) C(26) C(25) 102.9(3) yes . . . . C(32) Ti(2) C(26) C(27) -143.4(3) yes . . . . S(3) Ti(2) C(27) C(23) -121.0(3) yes . . . . S(3) Ti(2) C(27) C(26) 122.5(3) yes . . . . S(4) Ti(2) C(27) C(23) -25.7(3) yes . . . . S(4) Ti(2) C(27) C(26) -142.2(3) yes . . . . C(23) Ti(2) C(27) C(26) -116.5(3) yes . . . . C(24) Ti(2) C(27) C(23) 37.3(2) yes . . . . C(24) Ti(2) C(27) C(26) -79.2(2) yes . . . . C(25) Ti(2) C(27) C(23) 78.4(3) yes . . . . C(25) Ti(2) C(27) C(26) -38.1(2) yes . . . . C(26) Ti(2) C(27) C(23) 116.5(3) yes . . . . C(28) Ti(2) C(27) C(23) 169.5(3) yes . . . . C(28) Ti(2) C(27) C(26) 53.0(3) yes . . . . C(29) Ti(2) C(27) C(23) 132.9(3) yes . . . . C(29) Ti(2) C(27) C(26) 16.4(3) yes . . . . C(30) Ti(2) C(27) C(23) 97.9(3) yes . . . . C(30) Ti(2) C(27) C(26) -18.6(4) yes . . . . C(31) Ti(2) C(27) C(23) 88.9(7) yes . . . . C(31) Ti(2) C(27) C(26) -27.6(8) yes . . . . C(32) Ti(2) C(27) C(23) -167.8(3) yes . . . . C(32) Ti(2) C(27) C(26) 75.7(4) yes . . . . S(3) Ti(2) C(28) C(29) -154.0(2) yes . . . . S(3) Ti(2) C(28) C(32) 90.7(2) yes . . . . S(4) Ti(2) C(28) C(29) 115.7(2) yes . . . . S(4) Ti(2) C(28) C(32) 0.4(3) yes . . . . C(23) Ti(2) C(28) C(29) -69.4(3) yes . . . . C(23) Ti(2) C(28) C(32) 175.3(2) yes . . . . C(24) Ti(2) C(28) C(29) -9.1(3) yes . . . . C(24) Ti(2) C(28) C(32) -124.5(2) yes . . . . C(25) Ti(2) C(28) C(29) -22.3(2) yes . . . . C(25) Ti(2) C(28) C(32) -137.6(2) yes . . . . C(26) Ti(2) C(28) C(29) -55.9(2) yes . . . . C(26) Ti(2) C(28) C(32) -171.3(2) yes . . . . C(27) Ti(2) C(28) C(29) -83.0(2) yes . . . . C(27) Ti(2) C(28) C(32) 161.6(2) yes . . . . C(29) Ti(2) C(28) C(32) -115.4(3) yes . . . . C(30) Ti(2) C(28) C(29) 37.2(2) yes . . . . C(30) Ti(2) C(28) C(32) -78.1(2) yes . . . . C(31) Ti(2) C(28) C(29) 78.5(2) yes . . . . C(31) Ti(2) C(28) C(32) -36.9(2) yes . . . . C(32) Ti(2) C(28) C(29) 115.4(3) yes . . . . S(3) Ti(2) C(29) C(28) 26.9(2) yes . . . . S(3) Ti(2) C(29) C(30) 143.2(2) yes . . . . S(4) Ti(2) C(29) C(28) -95.4(2) yes . . . . S(4) Ti(2) C(29) C(30) 20.9(3) yes . . . . C(23) Ti(2) C(29) C(28) 147.4(2) yes . . . . C(23) Ti(2) C(29) C(30) -96.3(2) yes . . . . C(24) Ti(2) C(29) C(28) 173.9(2) yes . . . . C(24) Ti(2) C(29) C(30) -69.8(2) yes . . . . C(25) Ti(2) C(29) C(28) 158.3(2) yes . . . . C(25) Ti(2) C(29) C(30) -85.4(2) yes . . . . C(26) Ti(2) C(29) C(28) 123.6(2) yes . . . . C(26) Ti(2) C(29) C(30) -120.1(2) yes . . . . C(27) Ti(2) C(29) C(28) 114.4(2) yes . . . . C(27) Ti(2) C(29) C(30) -129.4(2) yes . . . . C(28) Ti(2) C(29) C(30) 116.3(3) yes . . . . C(30) Ti(2) C(29) C(28) -116.3(3) yes . . . . C(31) Ti(2) C(29) C(28) -78.6(2) yes . . . . C(31) Ti(2) C(29) C(30) 37.7(2) yes . . . . C(32) Ti(2) C(29) C(28) -37.5(2) yes . . . . C(32) Ti(2) C(29) C(30) 78.8(2) yes . . . . S(3) Ti(2) C(30) C(29) -51.7(3) yes . . . . S(3) Ti(2) C(30) C(31) 63.0(3) yes . . . . S(4) Ti(2) C(30) C(29) -165.1(2) yes . . . . S(4) Ti(2) C(30) C(31) -50.4(3) yes . . . . C(23) Ti(2) C(30) C(29) 112.7(2) yes . . . . C(23) Ti(2) C(30) C(31) -132.6(2) yes . . . . C(24) Ti(2) C(30) C(29) 115.9(2) yes . . . . C(24) Ti(2) C(30) C(31) -129.4(3) yes . . . . C(25) Ti(2) C(30) C(29) 86.1(2) yes . . . . C(25) Ti(2) C(30) C(31) -159.2(3) yes . . . . C(26) Ti(2) C(30) C(29) 59.1(2) yes . . . . C(26) Ti(2) C(30) C(31) 173.8(3) yes . . . . C(27) Ti(2) C(30) C(29) 69.6(3) yes . . . . C(27) Ti(2) C(30) C(31) -175.7(2) yes . . . . C(28) Ti(2) C(30) C(29) -36.5(2) yes . . . . C(28) Ti(2) C(30) C(31) 78.2(3) yes . . . . C(29) Ti(2) C(30) C(31) 114.7(3) yes . . . . C(31) Ti(2) C(30) C(29) -114.7(3) yes . . . . C(32) Ti(2) C(30) C(29) -77.4(2) yes . . . . C(32) Ti(2) C(30) C(31) 37.3(2) yes . . . . S(3) Ti(2) C(31) C(30) -135.6(2) yes . . . . S(3) Ti(2) C(31) C(32) -20.2(3) yes . . . . S(4) Ti(2) C(31) C(30) 130.1(3) yes . . . . S(4) Ti(2) C(31) C(32) -114.5(3) yes . . . . C(23) Ti(2) C(31) C(30) 79.2(3) yes . . . . C(23) Ti(2) C(31) C(32) -165.4(2) yes . . . . C(24) Ti(2) C(31) C(30) 57.4(3) yes . . . . C(24) Ti(2) C(31) C(32) 172.7(2) yes . . . . C(25) Ti(2) C(31) C(30) 21.3(3) yes . . . . C(25) Ti(2) C(31) C(32) 136.7(2) yes . . . . C(26) Ti(2) C(31) C(30) -8.2(3) yes . . . . C(26) Ti(2) C(31) C(32) 107.2(3) yes . . . . C(27) Ti(2) C(31) C(30) 12.2(6) yes . . . . C(27) Ti(2) C(31) C(32) 127.5(4) yes . . . . C(28) Ti(2) C(31) C(30) -78.5(3) yes . . . . C(28) Ti(2) C(31) C(32) 36.9(2) yes . . . . C(29) Ti(2) C(31) C(30) -37.9(2) yes . . . . C(29) Ti(2) C(31) C(32) 77.5(3) yes . . . . C(30) Ti(2) C(31) C(32) 115.4(3) yes . . . . C(32) Ti(2) C(31) C(30) -115.4(4) yes . . . . S(3) Ti(2) C(32) C(28) -82.7(2) yes . . . . S(3) Ti(2) C(32) C(31) 161.1(3) yes . . . . S(4) Ti(2) C(32) C(28) -179.7(2) yes . . . . S(4) Ti(2) C(32) C(31) 64.1(3) yes . . . . C(24) Ti(2) C(32) C(28) 103.9(3) yes . . . . C(24) Ti(2) C(32) C(31) -12.3(4) yes . . . . C(25) Ti(2) C(32) C(28) 57.4(2) yes . . . . C(25) Ti(2) C(32) C(31) -58.8(3) yes . . . . C(26) Ti(2) C(32) C(28) 11.7(3) yes . . . . C(26) Ti(2) C(32) C(31) -104.5(3) yes . . . . C(27) Ti(2) C(32) C(28) -35.9(4) yes . . . . C(27) Ti(2) C(32) C(31) -152.1(2) yes . . . . C(28) Ti(2) C(32) C(31) -116.2(3) yes . . . . C(29) Ti(2) C(32) C(28) 37.1(2) yes . . . . C(29) Ti(2) C(32) C(31) -79.1(3) yes . . . . C(30) Ti(2) C(32) C(28) 78.7(2) yes . . . . C(30) Ti(2) C(32) C(31) -37.5(2) yes . . . . C(31) Ti(2) C(32) C(28) 116.2(3) yes . . . . Ti(1) S(1) Si(1) C(1) 26.7(2) yes . . . . Ti(1) S(1) Si(1) C(2) -98.2(2) yes . . . . Ti(1) S(1) Si(1) C(3) 146.5(1) yes . . . . Ti(1) S(2) Si(2) C(4) 60.0(2) yes . . . . Ti(1) S(2) Si(2) C(5) 175.8(2) yes . . . . Ti(1) S(2) Si(2) C(6) -66.5(2) yes . . . . Ti(2) S(3) Si(3) C(17) -93.2(2) yes . . . . Ti(2) S(3) Si(3) C(18) 151.4(2) yes . . . . Ti(2) S(3) Si(3) C(19) 32.3(2) yes . . . . Ti(2) S(4) Si(4) C(20) 44.9(2) yes . . . . Ti(2) S(4) Si(4) C(21) 161.7(2) yes . . . . Ti(2) S(4) Si(4) C(22) -80.9(2) yes . . . . Ti(1) C(7) C(8) C(9) 64.9(3) yes . . . . C(11) C(7) C(8) Ti(1) -66.0(3) yes . . . . C(11) C(7) C(8) C(9) -1.1(5) yes . . . . Ti(1) C(7) C(11) C(10) -63.3(4) yes . . . . C(8) C(7) C(11) Ti(1) 65.7(3) yes . . . . C(8) C(7) C(11) C(10) 2.4(6) yes . . . . Ti(1) C(8) C(9) C(10) 64.2(4) yes . . . . C(7) C(8) C(9) Ti(1) -64.8(3) yes . . . . C(7) C(8) C(9) C(10) -0.6(5) yes . . . . Ti(1) C(9) C(10) C(11) 67.1(4) yes . . . . C(8) C(9) C(10) Ti(1) -65.0(3) yes . . . . C(8) C(9) C(10) C(11) 2.1(6) yes . . . . Ti(1) C(10) C(11) C(7) 63.7(4) yes . . . . C(9) C(10) C(11) Ti(1) -66.4(3) yes . . . . C(9) C(10) C(11) C(7) -2.7(6) yes . . . . Ti(1) C(12) C(13) C(14) -64.3(3) yes . . . . C(16) C(12) C(13) Ti(1) 65.5(3) yes . . . . C(16) C(12) C(13) C(14) 1.3(5) yes . . . . Ti(1) C(12) C(16) C(15) 64.9(3) yes . . . . C(13) C(12) C(16) Ti(1) -64.6(3) yes . . . . C(13) C(12) C(16) C(15) 0.2(5) yes . . . . Ti(1) C(13) C(14) C(15) -68.0(3) yes . . . . C(12) C(13) C(14) Ti(1) 65.7(3) yes . . . . C(12) C(13) C(14) C(15) -2.3(5) yes . . . . Ti(1) C(14) C(15) C(16) -64.3(3) yes . . . . C(13) C(14) C(15) Ti(1) 66.7(3) yes . . . . C(13) C(14) C(15) C(16) 2.4(5) yes . . . . Ti(1) C(15) C(16) C(12) -64.3(3) yes . . . . C(14) C(15) C(16) Ti(1) 62.7(3) yes . . . . C(14) C(15) C(16) C(12) -1.6(5) yes . . . . Ti(2) C(23) C(24) C(25) -65.5(3) yes . . . . C(27) C(23) C(24) Ti(2) 65.4(3) yes . . . . C(27) C(23) C(24) C(25) -0.1(5) yes . . . . Ti(2) C(23) C(27) C(26) 63.6(3) yes . . . . C(24) C(23) C(27) Ti(2) -64.8(3) yes . . . . C(24) C(23) C(27) C(26) -1.2(5) yes . . . . Ti(2) C(24) C(25) C(26) -64.4(3) yes . . . . C(23) C(24) C(25) Ti(2) 65.8(3) yes . . . . C(23) C(24) C(25) C(26) 1.4(5) yes . . . . Ti(2) C(25) C(26) C(27) -66.8(3) yes . . . . C(24) C(25) C(26) Ti(2) 64.6(3) yes . . . . C(24) C(25) C(26) C(27) -2.1(5) yes . . . . Ti(2) C(26) C(27) C(23) -64.3(3) yes . . . . C(25) C(26) C(27) Ti(2) 66.4(3) yes . . . . C(25) C(26) C(27) C(23) 2.1(5) yes . . . . Ti(2) C(28) C(29) C(30) -63.7(3) yes . . . . C(32) C(28) C(29) Ti(2) 65.2(3) yes . . . . C(32) C(28) C(29) C(30) 1.4(5) yes . . . . Ti(2) C(28) C(32) C(31) 64.6(3) yes . . . . C(29) C(28) C(32) Ti(2) -65.1(3) yes . . . . C(29) C(28) C(32) C(31) -0.5(5) yes . . . . Ti(2) C(29) C(30) C(31) -66.6(3) yes . . . . C(28) C(29) C(30) Ti(2) 64.8(3) yes . . . . C(28) C(29) C(30) C(31) -1.8(5) yes . . . . Ti(2) C(30) C(31) C(32) -65.1(3) yes . . . . C(29) C(30) C(31) Ti(2) 66.6(3) yes . . . . C(29) C(30) C(31) C(32) 1.4(5) yes . . . . Ti(2) C(31) C(32) C(28) -64.7(3) yes . . . . C(30) C(31) C(32) Ti(2) 64.2(3) yes . . . . C(30) C(31) C(32) C(28) -0.6(5) yes . . . . 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 Ti(1) S(1) 2.414(1) yes . 55501 Ti(1) S(2) 2.439(1) yes . 55501 Ti(1) C(7) 2.388(5) yes . 55501 Ti(1) C(8) 2.399(4) yes . 55501 Ti(1) C(9) 2.386(4) yes . 55501 Ti(1) C(10) 2.373(5) yes . 55501 Ti(1) C(11) 2.406(5) yes . 55501 Ti(1) C(12) 2.398(4) yes . 55501 Ti(1) C(13) 2.378(4) yes . 55501 Ti(1) C(14) 2.356(5) yes . 55501 Ti(1) C(15) 2.420(5) yes . 55501 Ti(1) C(16) 2.415(5) yes . 55501 Ti(2) S(3) 2.413(1) yes . 55501 Ti(2) S(4) 2.436(1) yes . 55501 Ti(2) C(23) 2.390(5) yes . 55501 Ti(2) C(24) 2.377(4) yes . 55501 Ti(2) C(25) 2.378(4) yes . 55501 Ti(2) C(26) 2.371(4) yes . 55501 Ti(2) C(27) 2.397(5) yes . 55501 Ti(2) C(28) 2.400(4) yes . 55501 Ti(2) C(29) 2.394(5) yes . 55501 Ti(2) C(30) 2.367(4) yes . 55501 Ti(2) C(31) 2.393(4) yes . 55501 Ti(2) C(32) 2.400(4) yes . 55501 S(1) Ti(1) 2.414(1) yes . 55501 S(1) Si(1) 2.132(1) yes . 55501 S(1) C(1) 3.371(4) yes . 55501 S(1) C(2) 3.323(4) yes . 55501 S(1) C(3) 3.137(5) yes . 55501 S(1) C(9) 3.108(5) yes . 55501 S(1) C(12) 2.943(5) yes . 55501 S(1) C(16) 3.087(5) yes . 55501 S(2) Ti(1) 2.439(1) yes . 55501 S(2) C(4) 3.289(6) yes . 55501 S(2) C(5) 3.154(6) yes . 55501 S(2) C(6) 3.399(6) yes . 55501 S(2) C(7) 3.048(5) yes . 55501 S(2) C(8) 2.982(4) yes . 55501 S(2) C(15) 3.109(4) yes . 55501 S(2) C(16) 3.558(4) yes . 55501 S(3) Ti(2) 2.413(1) yes . 55501 S(3) Si(3) 2.149(1) yes . 55501 S(3) C(17) 3.325(4) yes . 55501 S(3) C(18) 3.169(4) yes . 55501 S(3) C(19) 3.380(5) yes . 55501 S(3) C(27) 3.118(4) yes . 55501 S(3) C(28) 3.029(4) yes . 55501 S(3) C(32) 3.108(4) yes . 55501 S(4) Ti(2) 2.436(1) yes . 55501 S(4) Si(4) 2.135(1) yes . 55501 S(4) C(20) 3.361(4) yes . 55501 S(4) C(21) 3.149(6) yes . 55501 S(4) C(22) 3.345(5) yes . 55501 S(4) C(23) 2.986(5) yes . 55501 S(4) C(24) 3.048(4) yes . 55501 S(4) C(31) 3.105(5) yes . 55501 S(4) C(32) 3.561(5) yes . 55501 Si(1) S(1) 2.132(1) yes . 55501 Si(3) S(3) 2.149(1) yes . 55501 Si(3) C(27) 3.544(5) yes . 55501 Si(4) S(4) 2.135(1) yes . 55501 C(1) Ti(1) 3.387(5) yes . 55505 C(1) Ti(2) 3.387(5) yes . 55505 C(1) S(1) 3.371(4) yes . 55501 C(1) S(1) 3.387(5) yes . 55505 C(1) S(2) 3.387(5) yes . 55505 C(1) S(3) 3.387(5) yes . 55505 C(1) S(4) 3.387(5) yes . 55505 C(1) Si(1) 3.387(5) yes . 55505 C(1) Si(2) 3.387(5) yes . 55505 C(1) Si(3) 3.387(5) yes . 55505 C(1) Si(4) 3.387(5) yes . 55505 C(1) C(1) 3.387(7) yes . 55505 C(1) C(2) 3.034(6) yes . 55501 C(1) C(2) 3.387(7) yes . 55505 C(1) C(3) 3.049(7) yes . 55501 C(1) C(3) 3.387(7) yes . 55505 C(1) C(4) 3.387(8) yes . 55505 C(1) C(5) 3.387(8) yes . 55505 C(1) C(6) 3.387(9) yes . 55505 C(1) C(7) 3.387(7) yes . 55505 C(1) C(8) 3.387(7) yes . 55505 C(1) C(9) 3.387(7) yes . 55505 C(1) C(10) 3.387(7) yes . 55505 C(1) C(11) 3.387(7) yes . 55505 C(1) C(12) 3.387(7) yes . 55505 C(1) C(13) 3.387(7) yes . 55505 C(1) C(14) 3.387(7) yes . 55505 C(1) C(15) 3.387(7) yes . 55505 C(1) C(16) 3.387(7) yes . 55505 C(1) C(17) 3.387(7) yes . 55505 C(1) C(18) 3.387(7) yes . 55505 C(1) C(19) 3.387(7) yes . 55505 C(1) C(20) 3.387(8) yes . 55505 C(1) C(21) 3.387(9) yes . 55505 C(1) C(22) 3.387(8) yes . 55505 C(1) C(23) 3.387(8) yes . 55505 C(1) C(24) 3.387(7) yes . 55505 C(1) C(25) 3.387(7) yes . 55505 C(1) C(26) 3.387(8) yes . 55505 C(1) C(27) 3.387(8) yes . 55505 C(1) C(28) 3.387(7) yes . 55505 C(1) C(29) 3.387(7) yes . 55505 C(1) C(30) 3.387(7) yes . 55505 C(1) C(31) 3.387(7) yes . 55505 C(1) C(32) 3.387(7) yes . 55505 C(2) S(1) 3.323(4) yes . 55501 C(2) C(1) 3.034(6) yes . 55501 C(2) C(3) 2.998(7) yes . 55501 C(3) S(1) 3.137(5) yes . 55501 C(3) C(1) 3.049(7) yes . 55501 C(3) C(2) 2.998(7) yes . 55501 C(4) S(2) 3.289(6) yes . 55501 C(4) C(5) 3.012(8) yes . 55501 C(4) C(6) 3.043(8) yes . 55501 C(5) S(2) 3.154(6) yes . 55501 C(5) C(4) 3.012(8) yes . 55501 C(5) C(6) 2.990(8) yes . 55501 C(6) S(2) 3.399(6) yes . 55501 C(6) C(4) 3.043(8) yes . 55501 C(6) C(5) 2.990(8) yes . 55501 C(6) C(15) 3.421(8) yes . 55501 C(7) Ti(1) 2.388(5) yes . 55501 C(7) Ti(1) 3.188(5) yes . 55505 C(7) Ti(2) 3.188(5) yes . 55505 C(7) S(1) 3.188(5) yes . 55505 C(7) S(2) 3.048(5) yes . 55501 C(7) S(2) 3.188(5) yes . 55505 C(7) S(3) 3.188(5) yes . 55505 C(7) S(4) 3.188(5) yes . 55505 C(7) Si(1) 3.188(5) yes . 55505 C(7) Si(2) 3.188(5) yes . 55505 C(7) Si(3) 3.188(5) yes . 55505 C(7) Si(4) 3.188(5) yes . 55505 C(7) C(1) 3.188(7) yes . 55505 C(7) C(2) 3.188(6) yes . 55505 C(7) C(3) 3.188(6) yes . 55505 C(7) C(4) 3.188(7) yes . 55505 C(7) C(5) 3.188(7) yes . 55505 C(7) C(6) 3.188(7) yes . 55505 C(7) C(7) 3.188(7) yes . 55505 C(7) C(8) 3.188(6) yes . 55505 C(7) C(9) 2.251(7) yes . 55501 C(7) C(9) 3.188(6) yes . 55505 C(7) C(10) 2.257(6) yes . 55501 C(7) C(10) 3.188(7) yes . 55505 C(7) C(11) 3.188(7) yes . 55505 C(7) C(12) 3.188(7) yes . 55505 C(7) C(13) 3.188(7) yes . 55505 C(7) C(14) 3.449(6) yes . 55501 C(7) C(14) 3.188(7) yes . 55505 C(7) C(15) 3.188(7) yes . 55505 C(7) C(16) 3.188(7) yes . 55505 C(7) C(17) 3.188(7) yes . 55505 C(7) C(18) 3.188(6) yes . 55505 C(7) C(19) 3.188(6) yes . 55505 C(7) C(20) 3.188(7) yes . 55505 C(7) C(21) 3.188(8) yes . 55505 C(7) C(22) 3.188(7) yes . 55505 C(7) C(23) 3.188(7) yes . 55505 C(7) C(24) 3.188(6) yes . 55505 C(7) C(25) 3.188(6) yes . 55505 C(7) C(26) 3.188(6) yes . 55505 C(7) C(27) 3.188(6) yes . 55505 C(7) C(28) 3.188(6) yes . 55505 C(7) C(29) 3.188(6) yes . 55505 C(7) C(30) 3.188(6) yes . 55505 C(7) C(31) 3.188(6) yes . 55505 C(7) C(32) 3.188(6) yes . 55505 C(8) Ti(1) 2.399(4) yes . 55501 C(8) S(1) 1.992(4) yes . 55505 C(8) S(2) 2.982(4) yes . 55501 C(8) S(2) 1.992(4) yes . 55505 C(8) S(3) 1.992(4) yes . 55505 C(8) S(4) 1.992(4) yes . 55505 C(8) Si(1) 1.992(4) yes . 55505 C(8) Si(2) 1.992(4) yes . 55505 C(8) Si(3) 1.992(4) yes . 55505 C(8) Si(4) 1.992(4) yes . 55505 C(8) C(1) 1.992(6) yes . 55505 C(8) C(2) 1.992(6) yes . 55505 C(8) C(3) 1.992(6) yes . 55505 C(8) C(4) 1.992(7) yes . 55505 C(8) C(5) 1.992(7) yes . 55505 C(8) C(6) 1.992(7) yes . 55505 C(8) C(7) 1.992(6) yes . 55505 C(8) C(8) 1.992(6) yes . 55505 C(8) C(9) 1.992(6) yes . 55505 C(8) C(10) 2.276(6) yes . 55501 C(8) C(10) 1.992(6) yes . 55505 C(8) C(11) 2.276(6) yes . 55501 C(8) C(11) 1.992(6) yes . 55505 C(8) C(12) 1.992(7) yes . 55505 C(8) C(13) 1.992(7) yes . 55505 C(8) C(14) 1.992(6) yes . 55505 C(8) C(15) 1.992(6) yes . 55505 C(8) C(16) 1.992(6) yes . 55505 C(8) C(17) 1.992(6) yes . 55505 C(8) C(18) 1.992(6) yes . 55505 C(8) C(19) 1.992(6) yes . 55505 C(8) C(20) 1.992(6) yes . 55505 C(8) C(21) 1.992(7) yes . 55505 C(8) C(22) 1.992(7) yes . 55505 C(8) C(23) 1.992(6) yes . 55505 C(8) C(24) 1.992(6) yes . 55505 C(8) C(25) 1.992(6) yes . 55505 C(8) C(26) 1.992(6) yes . 55505 C(8) C(27) 1.992(6) yes . 55505 C(8) C(28) 1.992(6) yes . 55505 C(8) C(29) 1.992(6) yes . 55505 C(8) C(30) 1.992(6) yes . 55505 C(8) C(31) 1.992(6) yes . 55505 C(8) C(32) 1.992(6) yes . 55505 C(9) Ti(1) 2.386(4) yes . 55501 C(9) S(1) 3.108(5) yes . 55501 C(9) S(1) 1.930(4) yes . 55505 C(9) S(2) 1.930(4) yes . 55505 C(9) S(3) 1.930(4) yes . 55505 C(9) S(4) 1.930(4) yes . 55505 C(9) Si(1) 1.930(4) yes . 55505 C(9) Si(2) 1.930(4) yes . 55505 C(9) Si(3) 1.930(4) yes . 55505 C(9) Si(4) 1.930(4) yes . 55505 C(9) C(1) 1.930(6) yes . 55505 C(9) C(2) 1.930(6) yes . 55505 C(9) C(3) 1.930(6) yes . 55505 C(9) C(4) 1.930(6) yes . 55505 C(9) C(5) 1.930(7) yes . 55505 C(9) C(6) 1.930(7) yes . 55505 C(9) C(7) 2.251(7) yes . 55501 C(9) C(7) 1.930(6) yes . 55505 C(9) C(8) 1.930(6) yes . 55505 C(9) C(9) 1.930(6) yes . 55505 C(9) C(10) 1.930(6) yes . 55505 C(9) C(11) 2.255(7) yes . 55501 C(9) C(11) 1.930(6) yes . 55505 C(9) C(12) 1.930(6) yes . 55505 C(9) C(13) 1.930(6) yes . 55505 C(9) C(14) 1.930(6) yes . 55505 C(9) C(15) 1.930(6) yes . 55505 C(9) C(16) 1.930(6) yes . 55505 C(9) C(17) 1.930(6) yes . 55505 C(9) C(18) 1.930(6) yes . 55505 C(9) C(19) 1.930(6) yes . 55505 C(9) C(20) 1.930(6) yes . 55505 C(9) C(21) 1.930(7) yes . 55505 C(9) C(22) 1.930(7) yes . 55505 C(9) C(23) 1.930(6) yes . 55505 C(9) C(24) 1.930(6) yes . 55505 C(9) C(25) 1.930(6) yes . 55505 C(9) C(26) 1.930(6) yes . 55505 C(9) C(27) 1.930(6) yes . 55505 C(9) C(28) 1.930(6) yes . 55505 C(9) C(29) 1.930(6) yes . 55505 C(9) C(30) 1.930(6) yes . 55505 C(9) C(31) 1.930(6) yes . 55505 C(9) C(32) 1.930(6) yes . 55505 C(10) Ti(1) 2.373(5) yes . 55501 C(10) Ti(1) 3.130(4) yes . 55505 C(10) Ti(2) 3.130(4) yes . 55505 C(10) S(1) 3.130(4) yes . 55505 C(10) S(2) 3.130(4) yes . 55505 C(10) S(3) 3.130(4) yes . 55505 C(10) S(4) 3.130(4) yes . 55505 C(10) Si(1) 3.130(4) yes . 55505 C(10) Si(2) 3.130(4) yes . 55505 C(10) Si(3) 3.130(4) yes . 55505 C(10) Si(4) 3.130(4) yes . 55505 C(10) C(1) 3.130(6) yes . 55505 C(10) C(2) 3.130(6) yes . 55505 C(10) C(3) 3.130(6) yes . 55505 C(10) C(4) 3.130(7) yes . 55505 C(10) C(5) 3.130(7) yes . 55505 C(10) C(6) 3.130(7) yes . 55505 C(10) C(7) 2.257(6) yes . 55501 C(10) C(7) 3.130(6) yes . 55505 C(10) C(8) 2.276(6) yes . 55501 C(10) C(8) 3.130(6) yes . 55505 C(10) C(9) 3.130(6) yes . 55505 C(10) C(10) 3.130(6) yes . 55505 C(10) C(11) 3.130(6) yes . 55505 C(10) C(12) 3.130(6) yes . 55505 C(10) C(13) 3.056(6) yes . 55501 C(10) C(13) 3.130(6) yes . 55505 C(10) C(14) 3.566(7) yes . 55501 C(10) C(14) 3.130(6) yes . 55505 C(10) C(15) 3.130(6) yes . 55505 C(10) C(16) 3.130(6) yes . 55505 C(10) C(17) 3.130(6) yes . 55505 C(10) C(18) 3.130(6) yes . 55505 C(10) C(19) 3.130(6) yes . 55505 C(10) C(20) 3.130(7) yes . 55505 C(10) C(21) 3.130(8) yes . 55505 C(10) C(22) 3.130(6) yes . 55505 C(10) C(23) 3.130(6) yes . 55505 C(10) C(24) 3.130(6) yes . 55505 C(10) C(25) 3.130(6) yes . 55505 C(10) C(26) 3.130(6) yes . 55505 C(10) C(27) 3.130(6) yes . 55505 C(10) C(28) 3.130(6) yes . 55505 C(10) C(29) 3.130(6) yes . 55505 C(10) C(30) 3.130(6) yes . 55505 C(10) C(31) 3.130(6) yes . 55505 C(10) C(32) 3.130(6) yes . 55505 C(11) Ti(1) 2.406(5) yes . 55501 C(11) C(8) 2.276(6) yes . 55501 C(11) C(9) 2.255(7) yes . 55501 C(11) C(13) 2.990(6) yes . 55501 C(11) C(14) 2.966(7) yes . 55501 C(12) Ti(1) 2.398(4) yes . 55501 C(12) S(1) 2.943(5) yes . 55501 C(12) C(14) 2.260(7) yes . 55501 C(12) C(15) 2.280(7) yes . 55501 C(13) Ti(1) 2.378(4) yes . 55501 C(13) C(10) 3.056(6) yes . 55501 C(13) C(11) 2.990(6) yes . 55501 C(13) C(15) 2.282(7) yes . 55501 C(13) C(16) 2.258(7) yes . 55501 C(14) Ti(1) 2.356(5) yes . 55501 C(14) C(7) 3.449(6) yes . 55501 C(14) C(10) 3.566(7) yes . 55501 C(14) C(11) 2.966(7) yes . 55501 C(14) C(12) 2.260(7) yes . 55501 C(14) C(16) 2.255(7) yes . 55501 C(15) Ti(1) 2.420(5) yes . 55501 C(15) S(2) 3.109(4) yes . 55501 C(15) C(6) 3.421(8) yes . 55501 C(15) C(12) 2.280(7) yes . 55501 C(15) C(13) 2.282(7) yes . 55501 C(16) Ti(1) 2.415(5) yes . 55501 C(16) S(1) 3.087(5) yes . 55501 C(16) S(2) 3.558(4) yes . 55501 C(16) C(13) 2.258(7) yes . 55501 C(16) C(14) 2.255(7) yes . 55501 C(17) S(3) 3.325(4) yes . 55501 C(17) C(18) 2.983(6) yes . 55501 C(17) C(19) 3.036(7) yes . 55501 C(17) C(23) 3.474(7) yes . 66503 C(18) S(3) 3.169(4) yes . 55501 C(18) C(17) 2.983(6) yes . 55501 C(18) C(19) 3.023(6) yes . 55501 C(19) S(3) 3.380(5) yes . 55501 C(19) C(17) 3.036(7) yes . 55501 C(19) C(18) 3.023(6) yes . 55501 C(19) C(23) 3.539(7) yes . 55501 C(20) S(4) 3.361(4) yes . 55501 C(20) C(21) 3.000(8) yes . 55501 C(20) C(22) 3.020(7) yes . 55501 C(21) S(4) 3.149(6) yes . 55501 C(21) C(20) 3.000(8) yes . 55501 C(21) C(22) 3.01(1) yes . 55501 C(22) S(4) 3.345(5) yes . 55501 C(22) C(20) 3.020(7) yes . 55501 C(22) C(21) 3.01(1) yes . 55501 C(22) C(31) 3.485(8) yes . 55501 C(23) Ti(2) 2.390(5) yes . 55501 C(23) S(4) 2.986(5) yes . 55501 C(23) C(17) 3.474(7) yes . 66503 C(23) C(19) 3.539(7) yes . 55501 C(23) C(25) 2.243(8) yes . 55501 C(23) C(26) 2.261(9) yes . 55501 C(24) Ti(2) 2.377(4) yes . 55501 C(24) S(4) 3.048(4) yes . 55501 C(24) C(26) 2.256(7) yes . 55501 C(24) C(27) 2.243(6) yes . 55501 C(24) C(30) 3.441(7) yes . 55501 C(25) Ti(2) 2.378(4) yes . 55501 C(25) C(23) 2.243(8) yes . 55501 C(25) C(27) 2.244(6) yes . 55501 C(25) C(29) 2.960(6) yes . 55501 C(25) C(30) 2.937(6) yes . 55501 C(25) C(32) 3.592(6) yes . 65502 C(26) Ti(2) 2.371(4) yes . 55501 C(26) C(23) 2.261(9) yes . 55501 C(26) C(24) 2.256(7) yes . 55501 C(26) C(29) 3.049(7) yes . 55501 C(26) C(30) 3.560(6) yes . 55501 C(27) Ti(2) 2.397(5) yes . 55501 C(27) S(3) 3.118(4) yes . 55501 C(27) Si(3) 3.544(5) yes . 55501 C(27) C(24) 2.243(6) yes . 55501 C(27) C(25) 2.244(6) yes . 55501 C(28) Ti(2) 2.400(4) yes . 55501 C(28) S(3) 3.029(4) yes . 55501 C(28) C(30) 2.267(6) yes . 55501 C(28) C(31) 2.276(6) yes . 55501 C(29) Ti(2) 2.394(5) yes . 55501 C(29) C(25) 2.960(6) yes . 55501 C(29) C(26) 3.049(7) yes . 55501 C(29) C(31) 2.272(6) yes . 55501 C(29) C(32) 2.257(6) yes . 55501 C(30) Ti(2) 2.367(4) yes . 55501 C(30) C(24) 3.441(7) yes . 55501 C(30) C(25) 2.937(6) yes . 55501 C(30) C(26) 3.560(6) yes . 55501 C(30) C(28) 2.267(6) yes . 55501 C(30) C(32) 2.260(6) yes . 55501 C(31) Ti(2) 2.393(4) yes . 55501 C(31) S(4) 3.105(5) yes . 55501 C(31) C(22) 3.485(8) yes . 55501 C(31) C(28) 2.276(6) yes . 55501 C(31) C(29) 2.272(6) yes . 55501 C(32) Ti(2) 2.400(4) yes . 55501 C(32) S(3) 3.108(4) yes . 55501 C(32) S(4) 3.561(5) yes . 55501 C(32) C(29) 2.257(6) yes . 55501 C(32) C(30) 2.260(6) yes . 55501 #============================================================================== # 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 #============================================================================== #===END data_Cp2Ti(SSiMe2tBu)2 _database_code_depnum_ccdc_archive 'CCDC 227195' _audit_creation_date 2004-03-03 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C22 H40 S2 Si2 Ti ' _chemical_formula_moiety Cp2Ti(SSiMe2tBu)2 _chemical_formula_weight 472.75 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 15.473(7) _cell_length_b 14.607(7) _cell_length_c 11.582(5) _cell_angle_alpha 90 _cell_angle_beta 97.501(7) _cell_angle_gamma 90 _cell_volume 2595.2(21) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8530 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016.00 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 0.982 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 40546 _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9826 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9810 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -100.0 sigma(F^2^). 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 6086 _reflns_number_gt 4783 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1660 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5851 _refine_ls_number_parameters 284 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0033Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.75 _refine_diff_density_min -0.76 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ti Ti 0.278 0.446 ; 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 Ti(1) Ti 0.07462(3) 0.00215(3) 0.26253(4) 0.01276(13) Uani 1.00 1 d . . . S(1) S 0.17700(5) -0.01228(5) 0.12029(6) 0.0161(2) Uani 1.00 1 d . . . S(2) S 0.18057(5) 0.01320(5) 0.43803(6) 0.0164(2) Uani 1.00 1 d . . . Si(1) Si 0.26554(5) -0.12594(6) 0.12870(7) 0.0169(2) Uani 1.00 1 d . . . Si(2) Si 0.27142(5) 0.12506(6) 0.46003(7) 0.0177(2) Uani 1.00 1 d . . . C(1) C 0.0869(2) -0.1593(2) 0.2973(3) 0.0200(8) Uani 1.00 1 d . . . C(2) C 0.0332(2) -0.1468(2) 0.1900(3) 0.0195(7) Uani 1.00 1 d . . . C(3) C -0.0433(2) -0.1023(2) 0.2122(3) 0.0220(8) Uani 1.00 1 d . . . C(4) C -0.0377(2) -0.0880(2) 0.3347(3) 0.0234(8) Uani 1.00 1 d . . . C(5) C 0.0415(2) -0.1238(2) 0.3857(3) 0.0227(8) Uani 1.00 1 d . . . C(6) C 0.0904(2) 0.1636(2) 0.2339(3) 0.0189(7) Uani 1.00 1 d . . . C(7) C 0.0364(2) 0.1517(2) 0.3225(3) 0.0201(8) Uani 1.00 1 d . . . C(8) C -0.0403(2) 0.1091(2) 0.2728(3) 0.0219(8) Uani 1.00 1 d . . . C(9) C -0.0352(2) 0.0951(2) 0.1526(3) 0.0234(8) Uani 1.00 1 d . . . C(10) C 0.0448(2) 0.1297(2) 0.1293(3) 0.0224(8) Uani 1.00 1 d . . . C(11) C 0.2117(2) -0.2383(2) 0.0878(3) 0.0270(9) Uani 1.00 1 d . . . C(12) C 0.3309(2) -0.1360(2) 0.2769(3) 0.0271(9) Uani 1.00 1 d . . . C(13) C 0.3410(2) -0.0987(2) 0.0158(3) 0.0227(8) Uani 1.00 1 d . . . C(14) C 0.4155(2) -0.1697(3) 0.0254(4) 0.0371(11) Uani 1.00 1 d . . . C(15) C 0.3800(3) -0.0023(3) 0.0336(4) 0.0349(10) Uani 1.00 1 d . . . C(16) C 0.2898(2) -0.1051(3) -0.1083(3) 0.0334(10) Uani 1.00 1 d . . . C(17) C 0.2191(2) 0.2389(2) 0.4845(3) 0.0298(9) Uani 1.00 1 d . . . C(18) C 0.3360(2) 0.1339(2) 0.3349(3) 0.0291(9) Uani 1.00 1 d . . . C(19) C 0.3476(2) 0.0977(2) 0.5991(3) 0.0247(8) Uani 1.00 1 d . . . C(20) C 0.4221(3) 0.1686(3) 0.6131(4) 0.0427(11) Uani 1.00 1 d . . . C(21) C 0.3874(3) 0.0012(3) 0.5945(4) 0.0387(11) Uani 1.00 1 d . . . C(22) C 0.2975(3) 0.1043(3) 0.7056(3) 0.0349(10) Uani 1.00 1 d . . . H(1) H 0.1442 -0.1873 0.3083 0.0242 Uiso 1.00 1 c . . . H(2) H 0.0473 -0.1655 0.1143 0.0235 Uiso 1.00 1 c . . . H(3) H -0.0914 -0.0845 0.1542 0.0262 Uiso 1.00 1 c . . . H(4) H -0.0813 -0.0588 0.3754 0.0291 Uiso 1.00 1 c . . . H(5) H 0.0625 -0.1244 0.4684 0.0275 Uiso 1.00 1 c . . . H(6) H 0.1484 0.1899 0.2434 0.0223 Uiso 1.00 1 c . . . H(7) H 0.0505 0.1701 0.4032 0.0240 Uiso 1.00 1 c . . . H(8) H -0.0888 0.0921 0.3136 0.0265 Uiso 1.00 1 c . . . H(9) H -0.0793 0.0665 0.0969 0.0268 Uiso 1.00 1 c . . . H(10) H 0.0654 0.1306 0.0537 0.0268 Uiso 1.00 1 c . . . H(11) H 0.1727 -0.2542 0.1439 0.0334 Uiso 1.00 1 c . . . H(12) H 0.1787 -0.2334 0.0109 0.0334 Uiso 1.00 1 c . . . H(13) H 0.2558 -0.2854 0.0873 0.0333 Uiso 1.00 1 c . . . H(14) H 0.2927 -0.1528 0.3335 0.0326 Uiso 1.00 1 c . . . H(15) H 0.3753 -0.1827 0.2750 0.0326 Uiso 1.00 1 c . . . H(16) H 0.3585 -0.0777 0.2985 0.0324 Uiso 1.00 1 c . . . H(17) H 0.3909 -0.2305 0.0120 0.046 Uiso 1.00 1 c . . . H(18) H 0.4535 -0.1564 -0.0327 0.046 Uiso 1.00 1 c . . . H(19) H 0.4486 -0.1671 0.1024 0.046 Uiso 1.00 1 c . . . H(20) H 0.4141 0.0019 0.1099 0.043 Uiso 1.00 1 c . . . H(21) H 0.4172 0.0097 -0.0259 0.043 Uiso 1.00 1 c . . . H(22) H 0.3333 0.0424 0.0277 0.043 Uiso 1.00 1 c . . . H(23) H 0.2430 -0.0605 -0.1161 0.041 Uiso 1.00 1 c . . . H(24) H 0.3287 -0.0926 -0.1656 0.041 Uiso 1.00 1 c . . . H(25) H 0.2656 -0.1661 -0.1207 0.041 Uiso 1.00 1 c . . . H(26) H 0.2637 0.2856 0.4995 0.035 Uiso 1.00 1 c . . . H(27) H 0.1793 0.2553 0.4159 0.035 Uiso 1.00 1 c . . . H(28) H 0.1871 0.2341 0.5510 0.035 Uiso 1.00 1 c . . . H(29) H 0.3626 0.0752 0.3224 0.036 Uiso 1.00 1 c . . . H(30) H 0.2976 0.1512 0.2653 0.036 Uiso 1.00 1 c . . . H(31) H 0.3812 0.1798 0.3517 0.036 Uiso 1.00 1 c . . . H(32) H 0.4607 0.1570 0.6846 0.050 Uiso 1.00 1 c . . . H(33) H 0.4548 0.1641 0.5473 0.050 Uiso 1.00 1 c . . . H(34) H 0.3976 0.2296 0.6158 0.050 Uiso 1.00 1 c . . . H(35) H 0.3409 -0.0438 0.5867 0.045 Uiso 1.00 1 c . . . H(36) H 0.4195 -0.0029 0.5282 0.045 Uiso 1.00 1 c . . . H(37) H 0.4265 -0.0104 0.6655 0.045 Uiso 1.00 1 c . . . H(38) H 0.2727 0.1650 0.7091 0.041 Uiso 1.00 1 c . . . H(39) H 0.2512 0.0591 0.6981 0.041 Uiso 1.00 1 c . . . H(40) H 0.3369 0.0927 0.7764 0.041 Uiso 1.00 1 c . . . 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 Ti(1) 0.0125(3) 0.0129(3) 0.0129(3) 0.0005(2) 0.0019(2) -0.0008(2) S(1) 0.0155(4) 0.0175(4) 0.0158(4) 0.0006(3) 0.0041(3) -0.0001(3) S(2) 0.0166(4) 0.0170(4) 0.0150(4) -0.0009(3) 0.0000(3) -0.0008(3) Si(1) 0.0159(4) 0.0172(5) 0.0180(4) 0.0005(3) 0.0033(3) -0.0021(3) Si(2) 0.0179(4) 0.0183(5) 0.0167(4) -0.0014(3) 0.0012(3) -0.0017(3) C(1) 0.023(2) 0.013(2) 0.025(2) -0.0031(12) 0.0063(12) 0.0025(12) C(2) 0.023(2) 0.014(2) 0.022(2) -0.0041(12) 0.0050(12) -0.0024(12) C(3) 0.019(2) 0.019(2) 0.028(2) -0.0069(12) 0.0015(12) -0.0006(13) C(4) 0.020(2) 0.021(2) 0.031(2) -0.0050(13) 0.0116(13) -0.0017(13) C(5) 0.026(2) 0.020(2) 0.023(2) -0.0090(13) 0.0070(13) 0.0038(13) C(6) 0.021(2) 0.011(1) 0.024(2) 0.0033(11) 0.0001(12) 0.0022(12) C(7) 0.027(2) 0.013(1) 0.020(2) 0.0060(12) 0.0027(12) -0.0022(12) C(8) 0.018(2) 0.019(2) 0.029(2) 0.0070(12) 0.0053(12) 0.0008(13) C(9) 0.021(2) 0.019(2) 0.027(2) 0.0065(13) -0.0087(13) -0.0003(13) C(10) 0.029(2) 0.020(2) 0.019(2) 0.0098(13) 0.0021(12) 0.0066(12) C(11) 0.028(2) 0.020(2) 0.035(2) 0.001(1) 0.011(1) -0.006(1) C(12) 0.023(2) 0.030(2) 0.027(2) 0.005(1) 0.0008(13) 0.001(1) C(13) 0.021(2) 0.026(2) 0.022(2) 0.0024(13) 0.0074(12) -0.0035(13) C(14) 0.026(2) 0.045(2) 0.043(2) 0.009(2) 0.013(2) -0.007(2) C(15) 0.027(2) 0.034(2) 0.046(2) -0.010(2) 0.016(2) -0.003(2) C(16) 0.031(2) 0.046(2) 0.024(2) 0.003(2) 0.010(1) 0.003(2) C(17) 0.033(2) 0.021(2) 0.033(2) -0.000(1) -0.004(2) -0.008(1) C(18) 0.031(2) 0.030(2) 0.027(2) -0.007(2) 0.009(1) 0.003(1) C(19) 0.019(2) 0.031(2) 0.023(2) -0.0038(13) -0.0033(12) 0.000(1) C(20) 0.027(2) 0.055(3) 0.042(2) -0.013(2) -0.010(2) -0.005(2) C(21) 0.031(2) 0.043(2) 0.039(2) 0.010(2) -0.006(2) 0.005(2) C(22) 0.035(2) 0.050(2) 0.018(2) -0.002(2) -0.001(1) 0.001(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # 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 Ti(1) S(1) 2.4391(9) yes . . Ti(1) S(2) 2.4443(8) yes . . Ti(1) C(1) 2.395(3) yes . . Ti(1) C(2) 2.389(3) yes . . Ti(1) C(3) 2.392(3) yes . . Ti(1) C(4) 2.415(3) yes . . Ti(1) C(5) 2.424(3) yes . . Ti(1) C(6) 2.399(3) yes . . Ti(1) C(7) 2.390(3) yes . . Ti(1) C(8) 2.382(3) yes . . Ti(1) C(9) 2.405(3) yes . . Ti(1) C(10) 2.425(3) yes . . S(1) Si(1) 2.147(1) yes . . S(2) Si(2) 2.149(1) yes . . Si(1) C(11) 1.874(3) yes . . Si(1) C(12) 1.880(3) yes . . Si(1) C(13) 1.904(4) yes . . Si(2) C(17) 1.886(4) yes . . Si(2) C(18) 1.870(4) yes . . Si(2) C(19) 1.910(3) yes . . C(1) C(2) 1.413(4) yes . . C(1) C(5) 1.414(5) yes . . C(2) C(3) 1.404(5) yes . . C(3) C(4) 1.425(5) yes . . C(4) C(5) 1.392(4) yes . . C(6) C(7) 1.416(5) yes . . C(6) C(10) 1.409(4) yes . . C(7) C(8) 1.397(4) yes . . C(8) C(9) 1.420(5) yes . . C(9) C(10) 1.395(5) yes . . C(13) C(14) 1.544(5) yes . . C(13) C(15) 1.536(5) yes . . C(13) C(16) 1.550(5) yes . . C(19) C(20) 1.543(5) yes . . C(19) C(21) 1.541(5) yes . . C(19) C(22) 1.544(5) yes . . 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 S(1) Ti(1) S(2) 98.23(3) yes . . . S(1) Ti(1) C(1) 89.09(8) yes . . . S(1) Ti(1) C(2) 81.48(8) yes . . . S(1) Ti(1) C(3) 108.81(9) yes . . . S(1) Ti(1) C(4) 138.32(8) yes . . . S(1) Ti(1) C(5) 122.53(8) yes . . . S(1) Ti(1) C(6) 84.53(8) yes . . . S(1) Ti(1) C(7) 118.83(8) yes . . . S(1) Ti(1) C(8) 130.19(8) yes . . . S(1) Ti(1) C(9) 99.63(9) yes . . . S(1) Ti(1) C(10) 73.93(8) yes . . . S(2) Ti(1) C(1) 83.99(7) yes . . . S(2) Ti(1) C(2) 118.18(7) yes . . . S(2) Ti(1) C(3) 130.72(8) yes . . . S(2) Ti(1) C(4) 100.55(8) yes . . . S(2) Ti(1) C(5) 74.39(7) yes . . . S(2) Ti(1) C(6) 88.90(7) yes . . . S(2) Ti(1) C(7) 82.10(7) yes . . . S(2) Ti(1) C(8) 109.84(8) yes . . . S(2) Ti(1) C(9) 138.91(8) yes . . . S(2) Ti(1) C(10) 121.97(8) yes . . . C(1) Ti(1) C(2) 34.4(1) yes . . . C(1) Ti(1) C(3) 56.9(1) yes . . . C(1) Ti(1) C(4) 56.6(1) yes . . . C(1) Ti(1) C(5) 34.1(1) yes . . . C(1) Ti(1) C(6) 169.7(1) yes . . . C(1) Ti(1) C(7) 150.3(1) yes . . . C(1) Ti(1) C(8) 132.9(1) yes . . . C(1) Ti(1) C(9) 132.8(1) yes . . . C(1) Ti(1) C(10) 150.2(1) yes . . . C(2) Ti(1) C(3) 34.2(1) yes . . . C(2) Ti(1) C(4) 56.8(1) yes . . . C(2) Ti(1) C(5) 56.5(1) yes . . . C(2) Ti(1) C(6) 151.0(1) yes . . . C(2) Ti(1) C(7) 150.4(1) yes . . . C(2) Ti(1) C(8) 116.6(1) yes . . . C(2) Ti(1) C(9) 100.9(1) yes . . . C(2) Ti(1) C(10) 117.1(1) yes . . . C(3) Ti(1) C(4) 34.5(1) yes . . . C(3) Ti(1) C(5) 56.4(1) yes . . . C(3) Ti(1) C(6) 133.0(1) yes . . . C(3) Ti(1) C(7) 116.4(1) yes . . . C(3) Ti(1) C(8) 83.1(1) yes . . . C(3) Ti(1) C(9) 76.5(1) yes . . . C(3) Ti(1) C(10) 105.0(1) yes . . . C(4) Ti(1) C(5) 33.4(1) yes . . . C(4) Ti(1) C(6) 132.4(1) yes . . . C(4) Ti(1) C(7) 100.4(1) yes . . . C(4) Ti(1) C(8) 76.4(1) yes . . . C(4) Ti(1) C(9) 90.0(1) yes . . . C(4) Ti(1) C(10) 123.6(1) yes . . . C(5) Ti(1) C(6) 149.4(1) yes . . . C(5) Ti(1) C(7) 116.3(1) yes . . . C(5) Ti(1) C(8) 104.6(1) yes . . . C(5) Ti(1) C(9) 123.4(1) yes . . . C(5) Ti(1) C(10) 157.0(1) yes . . . C(6) Ti(1) C(7) 34.4(1) yes . . . C(6) Ti(1) C(8) 56.8(1) yes . . . C(6) Ti(1) C(9) 56.6(1) yes . . . C(6) Ti(1) C(10) 34.0(1) yes . . . C(7) Ti(1) C(8) 34.0(1) yes . . . C(7) Ti(1) C(9) 56.9(1) yes . . . C(7) Ti(1) C(10) 56.5(1) yes . . . C(8) Ti(1) C(9) 34.5(1) yes . . . C(8) Ti(1) C(10) 56.4(1) yes . . . C(9) Ti(1) C(10) 33.6(1) yes . . . Si(1) S(1) Ti(1) 120.21(4) yes . . . Si(2) S(2) Ti(1) 120.41(4) yes . . . C(11) Si(1) C(12) 109.3(2) yes . . . C(11) Si(1) C(13) 107.6(2) yes . . . C(11) Si(1) S(1) 113.9(1) yes . . . C(12) Si(1) C(13) 109.7(1) yes . . . C(12) Si(1) S(1) 111.5(1) yes . . . C(13) Si(1) S(1) 104.6(1) yes . . . C(17) Si(2) C(18) 109.8(2) yes . . . C(17) Si(2) C(19) 106.7(2) yes . . . C(17) Si(2) S(2) 113.6(1) yes . . . C(18) Si(2) C(19) 109.5(1) yes . . . C(18) Si(2) S(2) 111.6(1) yes . . . C(19) Si(2) S(2) 105.2(1) yes . . . C(2) C(1) C(5) 107.4(3) yes . . . C(2) C(1) Ti(1) 72.6(2) yes . . . C(5) C(1) Ti(1) 74.0(2) yes . . . C(3) C(2) Ti(1) 73.0(2) yes . . . C(1) C(2) C(3) 108.2(3) yes . . . C(1) C(2) Ti(1) 73.1(2) yes . . . C(4) C(3) Ti(1) 73.6(2) yes . . . C(2) C(3) C(4) 107.9(3) yes . . . C(2) C(3) Ti(1) 72.8(2) yes . . . C(5) C(4) Ti(1) 73.6(2) yes . . . C(3) C(4) C(5) 107.7(3) yes . . . C(3) C(4) Ti(1) 71.9(2) yes . . . C(1) C(5) Ti(1) 71.9(2) yes . . . C(1) C(5) C(4) 108.9(3) yes . . . C(4) C(5) Ti(1) 72.9(2) yes . . . C(7) C(6) C(10) 107.6(3) yes . . . C(7) C(6) Ti(1) 72.5(2) yes . . . C(10) C(6) Ti(1) 74.0(2) yes . . . C(8) C(7) Ti(1) 72.7(2) yes . . . C(6) C(7) C(8) 107.8(3) yes . . . C(6) C(7) Ti(1) 73.1(2) yes . . . C(9) C(8) Ti(1) 73.7(2) yes . . . C(7) C(8) C(9) 108.4(3) yes . . . C(7) C(8) Ti(1) 73.3(2) yes . . . C(10) C(9) Ti(1) 74.0(2) yes . . . C(8) C(9) C(10) 107.5(3) yes . . . C(8) C(9) Ti(1) 71.8(2) yes . . . C(6) C(10) Ti(1) 72.0(2) yes . . . C(6) C(10) C(9) 108.6(3) yes . . . C(9) C(10) Ti(1) 72.4(2) yes . . . C(14) C(13) C(15) 109.2(3) yes . . . C(14) C(13) C(16) 108.2(3) yes . . . C(14) C(13) Si(1) 109.2(2) yes . . . C(15) C(13) C(16) 108.9(3) yes . . . C(15) C(13) Si(1) 111.4(2) yes . . . C(16) C(13) Si(1) 109.9(2) yes . . . C(20) C(19) C(21) 108.7(3) yes . . . C(20) C(19) C(22) 108.7(3) yes . . . C(20) C(19) Si(2) 108.6(2) yes . . . C(21) C(19) C(22) 109.2(3) yes . . . C(21) C(19) Si(2) 111.6(2) yes . . . C(22) C(19) Si(2) 110.0(2) yes . . . 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 S(2) Ti(1) S(1) Si(1) 61.09(4) yes . . . . C(1) Ti(1) S(1) Si(1) -22.70(4) yes . . . . C(2) Ti(1) S(1) Si(1) -56.35(4) yes . . . . C(3) Ti(1) S(1) Si(1) -77.12(5) yes . . . . C(4) Ti(1) S(1) Si(1) -55.05(6) yes . . . . C(5) Ti(1) S(1) Si(1) -15.59(6) yes . . . . C(6) Ti(1) S(1) Si(1) 149.18(4) yes . . . . C(7) Ti(1) S(1) Si(1) 146.57(4) yes . . . . C(8) Ti(1) S(1) Si(1) -174.08(4) yes . . . . C(9) Ti(1) S(1) Si(1) -156.06(4) yes . . . . C(10) Ti(1) S(1) Si(1) -177.90(4) yes . . . . S(1) Ti(1) S(2) Si(2) 62.12(5) yes . . . . C(1) Ti(1) S(2) Si(2) 150.33(5) yes . . . . C(2) Ti(1) S(2) Si(2) 146.82(4) yes . . . . C(3) Ti(1) S(2) Si(2) -174.21(4) yes . . . . C(4) Ti(1) S(2) Si(2) -155.27(4) yes . . . . C(5) Ti(1) S(2) Si(2) -176.29(5) yes . . . . C(6) Ti(1) S(2) Si(2) -22.19(5) yes . . . . C(7) Ti(1) S(2) Si(2) -56.04(5) yes . . . . C(8) Ti(1) S(2) Si(2) -76.07(5) yes . . . . C(9) Ti(1) S(2) Si(2) -52.90(7) yes . . . . C(10) Ti(1) S(2) Si(2) -14.03(6) yes . . . . S(1) Ti(1) C(1) C(2) -76.1(2) yes . . . . S(1) Ti(1) C(1) C(5) 169.3(2) yes . . . . S(2) Ti(1) C(1) C(2) -174.5(2) yes . . . . S(2) Ti(1) C(1) C(5) 70.9(2) yes . . . . C(2) Ti(1) C(1) C(5) -114.6(2) yes . . . . C(3) Ti(1) C(1) C(2) 37.1(2) yes . . . . C(3) Ti(1) C(1) C(5) -77.5(2) yes . . . . C(4) Ti(1) C(1) C(2) 78.6(2) yes . . . . C(4) Ti(1) C(1) C(5) -35.9(2) yes . . . . C(5) Ti(1) C(1) C(2) 114.6(2) yes . . . . C(6) Ti(1) C(1) C(2) -127.9(4) yes . . . . C(6) Ti(1) C(1) C(5) 117.5(4) yes . . . . C(7) Ti(1) C(1) C(2) 123.0(2) yes . . . . C(7) Ti(1) C(1) C(5) 8.5(3) yes . . . . C(8) Ti(1) C(1) C(2) 73.9(2) yes . . . . C(8) Ti(1) C(1) C(5) -40.7(2) yes . . . . C(9) Ti(1) C(1) C(2) 26.2(2) yes . . . . C(9) Ti(1) C(1) C(5) -88.4(2) yes . . . . C(10) Ti(1) C(1) C(2) -21.9(3) yes . . . . C(10) Ti(1) C(1) C(5) -136.5(2) yes . . . . S(1) Ti(1) C(2) C(1) 101.0(2) yes . . . . S(1) Ti(1) C(2) C(3) -143.3(2) yes . . . . S(2) Ti(1) C(2) C(1) 6.2(2) yes . . . . S(2) Ti(1) C(2) C(3) 121.9(2) yes . . . . C(1) Ti(1) C(2) C(3) 115.7(2) yes . . . . C(3) Ti(1) C(2) C(1) -115.7(2) yes . . . . C(4) Ti(1) C(2) C(1) -78.0(2) yes . . . . C(4) Ti(1) C(2) C(3) 37.7(2) yes . . . . C(5) Ti(1) C(2) C(1) -37.7(2) yes . . . . C(5) Ti(1) C(2) C(3) 78.0(2) yes . . . . C(6) Ti(1) C(2) C(1) 163.1(2) yes . . . . C(6) Ti(1) C(2) C(3) -81.2(2) yes . . . . C(7) Ti(1) C(2) C(1) -122.7(2) yes . . . . C(7) Ti(1) C(2) C(3) -6.9(3) yes . . . . C(8) Ti(1) C(2) C(1) -128.1(2) yes . . . . C(8) Ti(1) C(2) C(3) -12.4(2) yes . . . . C(9) Ti(1) C(2) C(1) -160.8(2) yes . . . . C(9) Ti(1) C(2) C(3) -45.0(2) yes . . . . C(10) Ti(1) C(2) C(1) 168.0(2) yes . . . . C(10) Ti(1) C(2) C(3) -76.3(2) yes . . . . S(1) Ti(1) C(3) C(2) 38.7(2) yes . . . . S(1) Ti(1) C(3) C(4) 153.8(2) yes . . . . S(2) Ti(1) C(3) C(2) -80.9(2) yes . . . . S(2) Ti(1) C(3) C(4) 34.3(2) yes . . . . C(1) Ti(1) C(3) C(2) -37.4(2) yes . . . . C(1) Ti(1) C(3) C(4) 77.8(2) yes . . . . C(2) Ti(1) C(3) C(4) 115.2(2) yes . . . . C(4) Ti(1) C(3) C(2) -115.2(2) yes . . . . C(5) Ti(1) C(3) C(2) -78.4(2) yes . . . . C(5) Ti(1) C(3) C(4) 36.7(2) yes . . . . C(6) Ti(1) C(3) C(2) 139.0(2) yes . . . . C(6) Ti(1) C(3) C(4) -105.8(2) yes . . . . C(7) Ti(1) C(3) C(2) 176.2(2) yes . . . . C(7) Ti(1) C(3) C(4) -68.7(2) yes . . . . C(8) Ti(1) C(3) C(2) 168.9(2) yes . . . . C(8) Ti(1) C(3) C(4) -76.0(2) yes . . . . C(9) Ti(1) C(3) C(2) 134.4(2) yes . . . . C(9) Ti(1) C(3) C(4) -110.4(2) yes . . . . C(10) Ti(1) C(3) C(2) 116.5(2) yes . . . . C(10) Ti(1) C(3) C(4) -128.4(2) yes . . . . S(1) Ti(1) C(4) C(3) -38.9(2) yes . . . . S(1) Ti(1) C(4) C(5) 76.5(2) yes . . . . S(2) Ti(1) C(4) C(3) -154.2(2) yes . . . . S(2) Ti(1) C(4) C(5) -38.8(2) yes . . . . C(1) Ti(1) C(4) C(3) -78.7(2) yes . . . . C(1) Ti(1) C(4) C(5) 36.7(2) yes . . . . C(2) Ti(1) C(4) C(3) -37.4(2) yes . . . . C(2) Ti(1) C(4) C(5) 78.0(2) yes . . . . C(3) Ti(1) C(4) C(5) 115.4(2) yes . . . . C(5) Ti(1) C(4) C(3) -115.4(2) yes . . . . C(6) Ti(1) C(4) C(3) 107.5(2) yes . . . . C(6) Ti(1) C(4) C(5) -137.1(2) yes . . . . C(7) Ti(1) C(4) C(3) 121.9(2) yes . . . . C(7) Ti(1) C(4) C(5) -122.6(2) yes . . . . C(8) Ti(1) C(4) C(3) 97.7(2) yes . . . . C(8) Ti(1) C(4) C(5) -146.9(2) yes . . . . C(9) Ti(1) C(4) C(3) 65.7(2) yes . . . . C(9) Ti(1) C(4) C(5) -178.9(2) yes . . . . C(10) Ti(1) C(4) C(3) 65.4(2) yes . . . . C(10) Ti(1) C(4) C(5) -179.2(2) yes . . . . S(1) Ti(1) C(5) C(1) -12.7(2) yes . . . . S(1) Ti(1) C(5) C(4) -129.9(2) yes . . . . S(2) Ti(1) C(5) C(1) -102.6(2) yes . . . . S(2) Ti(1) C(5) C(4) 140.2(2) yes . . . . C(1) Ti(1) C(5) C(4) -117.2(2) yes . . . . C(2) Ti(1) C(5) C(1) 38.0(1) yes . . . . C(2) Ti(1) C(5) C(4) -79.2(2) yes . . . . C(3) Ti(1) C(5) C(1) 79.3(2) yes . . . . C(3) Ti(1) C(5) C(4) -37.9(2) yes . . . . C(4) Ti(1) C(5) C(1) 117.2(2) yes . . . . C(6) Ti(1) C(5) C(1) -161.8(1) yes . . . . C(6) Ti(1) C(5) C(4) 81.0(2) yes . . . . C(7) Ti(1) C(5) C(1) -175.3(1) yes . . . . C(7) Ti(1) C(5) C(4) 67.5(2) yes . . . . C(8) Ti(1) C(5) C(1) 150.4(2) yes . . . . C(8) Ti(1) C(5) C(4) 33.3(2) yes . . . . C(9) Ti(1) C(5) C(1) 118.5(2) yes . . . . C(9) Ti(1) C(5) C(4) 1.3(2) yes . . . . C(10) Ti(1) C(5) C(1) 118.8(2) yes . . . . C(10) Ti(1) C(5) C(4) 1.7(3) yes . . . . S(1) Ti(1) C(6) C(7) -175.9(2) yes . . . . S(1) Ti(1) C(6) C(10) 69.2(2) yes . . . . S(2) Ti(1) C(6) C(7) -77.6(2) yes . . . . S(2) Ti(1) C(6) C(10) 167.5(2) yes . . . . C(1) Ti(1) C(6) C(7) -123.9(4) yes . . . . C(1) Ti(1) C(6) C(10) 121.2(4) yes . . . . C(2) Ti(1) C(6) C(7) 122.7(2) yes . . . . C(2) Ti(1) C(6) C(10) 7.8(3) yes . . . . C(3) Ti(1) C(6) C(7) 73.4(2) yes . . . . C(3) Ti(1) C(6) C(10) -41.5(2) yes . . . . C(4) Ti(1) C(6) C(7) 25.8(2) yes . . . . C(4) Ti(1) C(6) C(10) -89.1(2) yes . . . . C(5) Ti(1) C(6) C(7) -21.8(3) yes . . . . C(5) Ti(1) C(6) C(10) -136.6(2) yes . . . . C(7) Ti(1) C(6) C(10) -114.9(2) yes . . . . C(8) Ti(1) C(6) C(7) 37.2(1) yes . . . . C(8) Ti(1) C(6) C(10) -77.7(2) yes . . . . C(9) Ti(1) C(6) C(7) 78.7(2) yes . . . . C(9) Ti(1) C(6) C(10) -36.2(2) yes . . . . C(10) Ti(1) C(6) C(7) 114.9(2) yes . . . . S(1) Ti(1) C(7) C(6) 4.6(2) yes . . . . S(1) Ti(1) C(7) C(8) 120.1(2) yes . . . . S(2) Ti(1) C(7) C(6) 99.7(2) yes . . . . S(2) Ti(1) C(7) C(8) -144.9(2) yes . . . . C(1) Ti(1) C(7) C(6) 162.6(1) yes . . . . C(1) Ti(1) C(7) C(8) -82.0(2) yes . . . . C(2) Ti(1) C(7) C(6) -124.2(2) yes . . . . C(2) Ti(1) C(7) C(8) -8.7(3) yes . . . . C(3) Ti(1) C(7) C(6) -128.5(2) yes . . . . C(3) Ti(1) C(7) C(8) -13.1(2) yes . . . . C(4) Ti(1) C(7) C(6) -161.0(2) yes . . . . C(4) Ti(1) C(7) C(8) -45.5(2) yes . . . . C(5) Ti(1) C(7) C(6) 167.9(1) yes . . . . C(5) Ti(1) C(7) C(8) -76.7(2) yes . . . . C(6) Ti(1) C(7) C(8) 115.5(2) yes . . . . C(8) Ti(1) C(7) C(6) -115.5(2) yes . . . . C(9) Ti(1) C(7) C(6) -77.8(2) yes . . . . C(9) Ti(1) C(7) C(8) 37.6(2) yes . . . . C(10) Ti(1) C(7) C(6) -37.4(1) yes . . . . C(10) Ti(1) C(7) C(8) 78.0(2) yes . . . . S(1) Ti(1) C(8) C(7) -82.9(2) yes . . . . S(1) Ti(1) C(8) C(9) 32.6(2) yes . . . . S(2) Ti(1) C(8) C(7) 37.3(2) yes . . . . S(2) Ti(1) C(8) C(9) 152.8(2) yes . . . . C(1) Ti(1) C(8) C(7) 137.9(2) yes . . . . C(1) Ti(1) C(8) C(9) -106.6(2) yes . . . . C(2) Ti(1) C(8) C(7) 175.2(2) yes . . . . C(2) Ti(1) C(8) C(9) -69.3(2) yes . . . . C(3) Ti(1) C(8) C(7) 168.2(2) yes . . . . C(3) Ti(1) C(8) C(9) -76.3(2) yes . . . . C(4) Ti(1) C(8) C(7) 133.8(2) yes . . . . C(4) Ti(1) C(8) C(9) -110.7(2) yes . . . . C(5) Ti(1) C(8) C(7) 115.7(2) yes . . . . C(5) Ti(1) C(8) C(9) -128.8(2) yes . . . . C(6) Ti(1) C(8) C(7) -37.6(2) yes . . . . C(6) Ti(1) C(8) C(9) 77.9(2) yes . . . . C(7) Ti(1) C(8) C(9) 115.5(2) yes . . . . C(9) Ti(1) C(8) C(7) -115.5(2) yes . . . . C(10) Ti(1) C(8) C(7) -78.5(2) yes . . . . C(10) Ti(1) C(8) C(9) 37.0(2) yes . . . . S(1) Ti(1) C(9) C(8) -155.3(2) yes . . . . S(1) Ti(1) C(9) C(10) -40.3(2) yes . . . . S(2) Ti(1) C(9) C(8) -40.8(2) yes . . . . S(2) Ti(1) C(9) C(10) 74.3(2) yes . . . . C(1) Ti(1) C(9) C(8) 106.9(2) yes . . . . C(1) Ti(1) C(9) C(10) -138.0(2) yes . . . . C(2) Ti(1) C(9) C(8) 121.6(2) yes . . . . C(2) Ti(1) C(9) C(10) -123.3(2) yes . . . . C(3) Ti(1) C(9) C(8) 97.5(2) yes . . . . C(3) Ti(1) C(9) C(10) -147.5(2) yes . . . . C(4) Ti(1) C(9) C(8) 65.4(2) yes . . . . C(4) Ti(1) C(9) C(10) -179.5(2) yes . . . . C(5) Ti(1) C(9) C(8) 64.7(2) yes . . . . C(5) Ti(1) C(9) C(10) 179.8(2) yes . . . . C(6) Ti(1) C(9) C(8) -78.5(2) yes . . . . C(6) Ti(1) C(9) C(10) 36.6(2) yes . . . . C(7) Ti(1) C(9) C(8) -37.1(2) yes . . . . C(7) Ti(1) C(9) C(10) 78.0(2) yes . . . . C(8) Ti(1) C(9) C(10) 115.1(2) yes . . . . C(10) Ti(1) C(9) C(8) -115.1(2) yes . . . . S(1) Ti(1) C(10) C(6) -104.5(2) yes . . . . S(1) Ti(1) C(10) C(9) 138.5(2) yes . . . . S(2) Ti(1) C(10) C(6) -14.7(2) yes . . . . S(2) Ti(1) C(10) C(9) -131.8(2) yes . . . . C(1) Ti(1) C(10) C(6) -162.1(2) yes . . . . C(1) Ti(1) C(10) C(9) 80.9(2) yes . . . . C(2) Ti(1) C(10) C(6) -175.8(2) yes . . . . C(2) Ti(1) C(10) C(9) 67.2(2) yes . . . . C(3) Ti(1) C(10) C(6) 149.8(2) yes . . . . C(3) Ti(1) C(10) C(9) 32.8(2) yes . . . . C(4) Ti(1) C(10) C(6) 117.6(2) yes . . . . C(4) Ti(1) C(10) C(9) 0.6(2) yes . . . . C(5) Ti(1) C(10) C(6) 116.5(2) yes . . . . C(5) Ti(1) C(10) C(9) -0.5(3) yes . . . . C(6) Ti(1) C(10) C(9) -117.0(2) yes . . . . C(7) Ti(1) C(10) C(6) 37.9(2) yes . . . . C(7) Ti(1) C(10) C(9) -79.1(2) yes . . . . C(8) Ti(1) C(10) C(6) 79.0(2) yes . . . . C(8) Ti(1) C(10) C(9) -38.0(2) yes . . . . C(9) Ti(1) C(10) C(6) 117.0(2) yes . . . . Ti(1) S(1) Si(1) C(11) 70.4(1) yes . . . . Ti(1) S(1) Si(1) C(12) -53.9(1) yes . . . . Ti(1) S(1) Si(1) C(13) -172.4(1) yes . . . . Ti(1) S(2) Si(2) C(17) 69.7(1) yes . . . . Ti(1) S(2) Si(2) C(18) -55.2(1) yes . . . . Ti(1) S(2) Si(2) C(19) -173.9(1) yes . . . . S(1) Si(1) C(13) C(14) 172.5(2) yes . . . . S(1) Si(1) C(13) C(15) 51.8(2) yes . . . . S(1) Si(1) C(13) C(16) -69.0(2) yes . . . . C(11) Si(1) C(13) C(14) -66.0(2) yes . . . . C(11) Si(1) C(13) C(15) 173.3(2) yes . . . . C(11) Si(1) C(13) C(16) 52.5(3) yes . . . . C(12) Si(1) C(13) C(14) 52.8(2) yes . . . . C(12) Si(1) C(13) C(15) -67.9(2) yes . . . . C(12) Si(1) C(13) C(16) 171.4(2) yes . . . . S(2) Si(2) C(19) C(20) 173.0(2) yes . . . . S(2) Si(2) C(19) C(21) 53.2(3) yes . . . . S(2) Si(2) C(19) C(22) -68.2(3) yes . . . . C(17) Si(2) C(19) C(20) -66.0(3) yes . . . . C(17) Si(2) C(19) C(21) 174.2(2) yes . . . . C(17) Si(2) C(19) C(22) 52.8(3) yes . . . . C(18) Si(2) C(19) C(20) 52.9(3) yes . . . . C(18) Si(2) C(19) C(21) -66.9(3) yes . . . . C(18) Si(2) C(19) C(22) 171.7(2) yes . . . . Ti(1) C(1) C(2) C(3) -65.1(2) yes . . . . C(5) C(1) C(2) Ti(1) 66.4(2) yes . . . . C(5) C(1) C(2) C(3) 1.3(3) yes . . . . Ti(1) C(1) C(5) C(4) 64.0(2) yes . . . . C(2) C(1) C(5) Ti(1) -65.4(2) yes . . . . C(2) C(1) C(5) C(4) -1.4(4) yes . . . . Ti(1) C(2) C(3) C(4) -65.8(2) yes . . . . C(1) C(2) C(3) Ti(1) 65.1(2) yes . . . . C(1) C(2) C(3) C(4) -0.7(4) yes . . . . Ti(1) C(3) C(4) C(5) -65.4(2) yes . . . . C(2) C(3) C(4) Ti(1) 65.3(2) yes . . . . C(2) C(3) C(4) C(5) -0.1(4) yes . . . . Ti(1) C(4) C(5) C(1) -63.3(2) yes . . . . C(3) C(4) C(5) Ti(1) 64.3(2) yes . . . . C(3) C(4) C(5) C(1) 1.0(4) yes . . . . Ti(1) C(6) C(7) C(8) -64.9(2) yes . . . . C(10) C(6) C(7) Ti(1) 66.2(2) yes . . . . C(10) C(6) C(7) C(8) 1.4(3) yes . . . . Ti(1) C(6) C(10) C(9) 63.6(2) yes . . . . C(7) C(6) C(10) Ti(1) -65.2(2) yes . . . . C(7) C(6) C(10) C(9) -1.6(3) yes . . . . Ti(1) C(7) C(8) C(9) -65.9(2) yes . . . . C(6) C(7) C(8) Ti(1) 65.2(2) yes . . . . C(6) C(7) C(8) C(9) -0.7(4) yes . . . . Ti(1) C(8) C(9) C(10) -65.9(2) yes . . . . C(7) C(8) C(9) Ti(1) 65.6(2) yes . . . . C(7) C(8) C(9) C(10) -0.3(4) yes . . . . Ti(1) C(9) C(10) C(6) -63.3(2) yes . . . . C(8) C(9) C(10) Ti(1) 64.5(2) yes . . . . C(8) C(9) C(10) C(6) 1.1(4) yes . . . . 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 Ti(1) Ti(1) 3.1084(6) yes . 55505 Ti(1) S(1) 2.4391(9) yes . 55501 Ti(1) S(2) 2.4443(8) yes . 55501 Ti(1) C(1) 2.395(3) yes . 55501 Ti(1) C(2) 2.389(3) yes . 55501 Ti(1) C(3) 2.392(3) yes . 55501 Ti(1) C(4) 2.415(3) yes . 55501 Ti(1) C(5) 2.424(3) yes . 55501 Ti(1) C(6) 2.399(3) yes . 55501 Ti(1) C(7) 2.390(3) yes . 55501 Ti(1) C(8) 2.382(3) yes . 55501 Ti(1) C(9) 2.405(3) yes . 55501 Ti(1) C(10) 2.425(3) yes . 55501 S(1) Ti(1) 2.4391(9) yes . 55501 S(1) Ti(1) 2.9116(8) yes . 55505 S(1) Si(1) 2.147(1) yes . 55501 S(1) C(1) 3.392(3) yes . 55501 S(1) C(2) 3.151(3) yes . 55501 S(1) C(6) 3.254(3) yes . 55501 S(1) C(10) 2.925(3) yes . 55501 S(1) C(11) 3.374(3) yes . 55501 S(1) C(12) 3.331(3) yes . 55501 S(1) C(13) 3.209(3) yes . 55501 S(1) C(15) 3.424(4) yes . 55501 S(2) Ti(1) 2.4443(8) yes . 55501 S(2) Si(2) 2.149(1) yes . 55501 S(2) C(1) 3.238(3) yes . 55501 S(2) C(5) 2.943(3) yes . 55501 S(2) C(6) 3.392(3) yes . 55501 S(2) C(7) 3.175(3) yes . 55501 S(2) C(17) 3.380(3) yes . 55501 S(2) C(18) 3.327(4) yes . 55501 S(2) C(19) 3.228(3) yes . 55501 S(2) C(21) 3.470(4) yes . 55501 Si(1) S(1) 2.147(1) yes . 55501 Si(1) C(12) 1.880(3) yes . 55501 Si(1) C(13) 1.904(4) yes . 55501 Si(1) C(14) 2.819(4) yes . 55501 Si(1) C(15) 2.850(4) yes . 55501 Si(1) C(16) 2.835(4) yes . 55501 Si(2) S(2) 2.149(1) yes . 55501 Si(2) C(17) 1.886(4) yes . 55501 Si(2) C(19) 1.910(3) yes . 55501 Si(2) C(20) 2.812(4) yes . 55501 Si(2) C(21) 2.862(4) yes . 55501 Si(2) C(22) 2.837(3) yes . 55501 C(1) Ti(1) 2.395(3) yes . 55501 C(1) S(1) 3.392(3) yes . 55501 C(1) S(2) 3.238(3) yes . 55501 C(1) C(3) 2.282(4) yes . 55501 C(1) C(4) 2.282(5) yes . 55501 C(1) C(7) 3.535(4) yes . 54502 C(1) C(8) 3.532(4) yes . 54502 C(1) C(11) 3.488(5) yes . 55501 C(2) Ti(1) 2.389(3) yes . 55501 C(2) Ti(1) 3.068(3) yes . 55505 C(2) S(1) 3.151(3) yes . 55501 C(2) C(4) 2.287(5) yes . 55501 C(2) C(5) 2.278(5) yes . 55501 C(2) C(6) 3.542(4) yes . 54502 C(2) C(7) 3.131(4) yes . 54502 C(2) C(8) 3.592(4) yes . 54502 C(2) C(11) 3.415(5) yes . 55501 C(3) Ti(1) 2.392(3) yes . 55501 C(3) Ti(1) 3.025(3) yes . 55505 C(3) C(1) 2.282(4) yes . 55501 C(3) C(5) 2.275(4) yes . 55501 C(3) C(6) 3.568(4) yes . 54502 C(3) C(8) 3.166(5) yes . 55501 C(3) C(9) 2.971(4) yes . 55501 C(4) Ti(1) 2.415(3) yes . 55501 C(4) C(1) 2.282(5) yes . 55501 C(4) C(2) 2.287(5) yes . 55501 C(4) C(8) 2.966(4) yes . 55501 C(4) C(9) 3.409(5) yes . 55501 C(5) Ti(1) 2.424(3) yes . 55501 C(5) S(2) 2.943(3) yes . 55501 C(5) C(2) 2.278(5) yes . 55501 C(5) C(3) 2.275(4) yes . 55501 C(6) Ti(1) 2.399(3) yes . 55501 C(6) S(1) 3.254(3) yes . 55501 C(6) S(2) 3.392(3) yes . 55501 C(6) C(2) 3.542(4) yes . 55502 C(6) C(3) 3.568(4) yes . 55502 C(6) C(8) 2.273(5) yes . 55501 C(6) C(9) 2.278(4) yes . 55501 C(6) C(17) 3.477(5) yes . 55501 C(7) Ti(1) 2.390(3) yes . 55501 C(7) S(2) 3.175(3) yes . 55501 C(7) C(1) 3.535(4) yes . 55502 C(7) C(2) 3.131(4) yes . 55502 C(7) C(9) 2.284(4) yes . 55501 C(7) C(10) 2.280(4) yes . 55501 C(7) C(17) 3.427(5) yes . 55501 C(8) Ti(1) 2.382(3) yes . 55501 C(8) C(1) 3.532(4) yes . 55502 C(8) C(2) 3.592(4) yes . 55502 C(8) C(3) 3.166(5) yes . 55501 C(8) C(4) 2.966(4) yes . 55501 C(8) C(6) 2.273(5) yes . 55501 C(8) C(10) 2.271(5) yes . 55501 C(9) Ti(1) 2.405(3) yes . 55501 C(9) Ti(1) 2.366(3) yes . 55505 C(9) C(3) 2.971(4) yes . 55501 C(9) C(4) 3.409(5) yes . 55501 C(9) C(6) 2.278(4) yes . 55501 C(9) C(7) 2.284(4) yes . 55501 C(10) Ti(1) 2.425(3) yes . 55501 C(10) Ti(1) 2.458(3) yes . 55505 C(10) S(1) 2.925(3) yes . 55501 C(10) C(7) 2.280(4) yes . 55501 C(10) C(8) 2.271(5) yes . 55501 C(11) S(1) 3.374(3) yes . 55501 C(11) C(1) 3.488(5) yes . 55501 C(11) C(2) 3.415(5) yes . 55501 C(11) C(12) 3.062(5) yes . 55501 C(11) C(13) 3.048(5) yes . 55501 C(11) C(14) 3.473(5) yes . 55501 C(11) C(16) 3.336(5) yes . 55501 C(12) S(1) 3.331(3) yes . 55501 C(12) Si(1) 1.880(3) yes . 55501 C(12) C(11) 3.062(5) yes . 55501 C(12) C(13) 3.096(5) yes . 55501 C(12) C(14) 3.381(5) yes . 55501 C(12) C(15) 3.590(5) yes . 55501 C(13) S(1) 3.209(3) yes . 55501 C(13) Si(1) 1.904(4) yes . 55501 C(13) C(11) 3.048(5) yes . 55501 C(13) C(12) 3.096(5) yes . 55501 C(13) C(14) 1.544(5) yes . 55501 C(13) C(16) 1.550(5) yes . 55501 C(14) Si(1) 2.819(4) yes . 55501 C(14) C(11) 3.473(5) yes . 55501 C(14) C(12) 3.381(5) yes . 55501 C(14) C(13) 1.544(5) yes . 55501 C(14) C(15) 2.511(5) yes . 55501 C(14) C(16) 2.506(5) yes . 55501 C(15) S(1) 3.424(4) yes . 55501 C(15) Si(1) 2.850(4) yes . 55501 C(15) C(12) 3.590(5) yes . 55501 C(15) C(14) 2.511(5) yes . 55501 C(15) C(16) 2.510(5) yes . 55501 C(16) Si(1) 2.835(4) yes . 55501 C(16) C(11) 3.336(5) yes . 55501 C(16) C(13) 1.550(5) yes . 55501 C(16) C(14) 2.506(5) yes . 55501 C(16) C(15) 2.510(5) yes . 55501 C(17) S(2) 3.380(3) yes . 55501 C(17) Si(2) 1.886(4) yes . 55501 C(17) C(6) 3.477(5) yes . 55501 C(17) C(7) 3.427(5) yes . 55501 C(17) C(18) 3.074(5) yes . 55501 C(17) C(19) 3.046(5) yes . 55501 C(17) C(20) 3.452(5) yes . 55501 C(17) C(22) 3.329(5) yes . 55501 C(18) S(2) 3.327(4) yes . 55501 C(18) C(17) 3.074(5) yes . 55501 C(18) C(19) 3.087(5) yes . 55501 C(18) C(20) 3.361(5) yes . 55501 C(18) C(21) 3.579(5) yes . 55501 C(19) S(2) 3.228(3) yes . 55501 C(19) Si(2) 1.910(3) yes . 55501 C(19) C(17) 3.046(5) yes . 55501 C(19) C(18) 3.087(5) yes . 55501 C(19) C(20) 1.543(5) yes . 55501 C(19) C(21) 1.541(5) yes . 55501 C(19) C(22) 1.544(5) yes . 55501 C(20) Si(2) 2.812(4) yes . 55501 C(20) C(17) 3.452(5) yes . 55501 C(20) C(18) 3.361(5) yes . 55501 C(20) C(19) 1.543(5) yes . 55501 C(20) C(21) 2.507(6) yes . 55501 C(20) C(22) 2.508(6) yes . 55501 C(21) S(2) 3.470(4) yes . 55501 C(21) Si(2) 2.862(4) yes . 55501 C(21) C(18) 3.579(5) yes . 55501 C(21) C(19) 1.541(5) yes . 55501 C(21) C(20) 2.507(6) yes . 55501 C(21) C(22) 2.514(6) yes . 55501 C(22) Si(2) 2.837(3) yes . 55501 C(22) C(17) 3.329(5) yes . 55501 C(22) C(19) 1.544(5) yes . 55501 C(22) C(20) 2.508(6) yes . 55501 C(22) C(21) 2.514(6) yes . 55501 #============================================================================== # 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 #============================================================================== #===END data_Ni(SSiMe3)2(dppe) _database_code_depnum_ccdc_archive 'CCDC 227196' _audit_creation_date 2004-03-03 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C32 H42 Ni P2 S2 Si2 ' _chemical_formula_moiety Ni(SSiMe3)2(dppe) _chemical_formula_weight 667.62 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 10.309(6) _cell_length_b 27.50(2) _cell_length_c 13.133(8) _cell_angle_alpha 90 _cell_angle_beta 110.341(7) _cell_angle_gamma 90 _cell_volume 3490.6(34) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10823 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour dark-purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.00 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.772 _exptl_absorpt_correction_T_max 0.966 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 56632 _diffrn_reflns_av_R_equivalents 0.108 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9871 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9855 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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 8089 _reflns_number_gt 3759 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1050 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7915 _refine_ls_number_parameters 394 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.8000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 3.11 _refine_diff_density_min -1.81 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; 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 Ni(1) Ni 0.78766(6) 0.14425(2) 0.72598(5) 0.0266(2) Uani 1.00 1 d . . . S(1) S 0.74633(13) 0.16395(5) 0.55119(10) 0.0336(4) Uani 1.00 1 d . . . S(2) S 0.84737(13) 0.06667(5) 0.71878(11) 0.0332(4) Uani 1.00 1 d . . . P(1) P 0.82917(13) 0.13433(5) 0.89775(10) 0.0267(4) Uani 1.00 1 d . . . P(2) P 0.7155(1) 0.21634(5) 0.74516(10) 0.0280(4) Uani 1.00 1 d . . . Si(1) Si 0.5762(2) 0.12039(6) 0.45525(12) 0.0404(5) Uani 1.00 1 d . . . Si(2) Si 1.0334(2) 0.06632(5) 0.68480(12) 0.0365(5) Uani 1.00 1 d . . . C(1) C 0.4559(5) 0.1612(2) 0.3516(4) 0.052(2) Uani 1.00 1 d . . . C(2) C 0.6320(5) 0.0711(2) 0.3824(4) 0.057(2) Uani 1.00 1 d . . . C(3) C 0.4743(5) 0.0897(2) 0.5300(5) 0.064(2) Uani 1.00 1 d . . . C(4) C 1.0071(6) 0.0700(2) 0.5367(4) 0.065(2) Uani 1.00 1 d . . . C(5) C 1.1174(5) 0.0071(2) 0.7402(4) 0.046(2) Uani 1.00 1 d . . . C(6) C 1.1508(5) 0.1180(2) 0.7510(4) 0.051(2) Uani 1.00 1 d . . . C(7) C 0.8225(5) 0.1940(2) 0.9578(4) 0.029(2) Uani 1.00 1 d . . . C(8) C 0.7004(5) 0.2213(2) 0.8798(4) 0.031(2) Uani 1.00 1 d . . . C(9) C 0.6898(5) 0.1010(2) 0.9230(4) 0.029(2) Uani 1.00 1 d . . . C(10) C 0.5922(5) 0.0767(2) 0.8396(4) 0.039(2) Uani 1.00 1 d . . . C(11) C 0.4809(5) 0.0544(2) 0.8556(5) 0.050(2) Uani 1.00 1 d . . . C(12) C 0.4673(5) 0.0563(2) 0.9560(5) 0.048(2) Uani 1.00 1 d . . . C(13) C 0.5637(6) 0.0796(2) 1.0404(5) 0.045(2) Uani 1.00 1 d . . . C(14) C 0.6751(5) 0.1022(2) 1.0242(4) 0.039(2) Uani 1.00 1 d . . . C(15) C 0.9886(5) 0.1080(2) 0.9891(4) 0.0213(13) Uani 1.00 1 d . . . C(16) C 0.9918(5) 0.0632(2) 1.0389(4) 0.037(2) Uani 1.00 1 d . . . C(17) C 1.1158(6) 0.0447(2) 1.1095(4) 0.044(2) Uani 1.00 1 d . . . C(18) C 1.2352(5) 0.0706(2) 1.1294(4) 0.040(2) Uani 1.00 1 d . . . C(19) C 1.2348(5) 0.1146(2) 1.0807(4) 0.041(2) Uani 1.00 1 d . . . C(20) C 1.1122(5) 0.1331(2) 1.0115(4) 0.033(2) Uani 1.00 1 d . . . C(21) C 0.8396(5) 0.2639(2) 0.7468(4) 0.027(1) Uani 1.00 1 d . . . C(22) C 0.9571(5) 0.2528(2) 0.7232(4) 0.034(2) Uani 1.00 1 d . . . C(23) C 1.0562(5) 0.2882(2) 0.7312(4) 0.040(2) Uani 1.00 1 d . . . C(24) C 1.0384(5) 0.3345(2) 0.7623(4) 0.044(2) Uani 1.00 1 d . . . C(25) C 0.9230(6) 0.3464(2) 0.7873(4) 0.045(2) Uani 1.00 1 d . . . C(26) C 0.8243(5) 0.3108(2) 0.7795(4) 0.036(2) Uani 1.00 1 d . . . C(27) C 0.5463(5) 0.2345(2) 0.6529(4) 0.032(2) Uani 1.00 1 d . . . C(28) C 0.5262(5) 0.2709(2) 0.5767(4) 0.038(2) Uani 1.00 1 d . . . C(29) C 0.3937(7) 0.2799(2) 0.5017(5) 0.054(2) Uani 1.00 1 d . . . C(30) C 0.2839(6) 0.2528(2) 0.5030(5) 0.057(2) Uani 1.00 1 d . . . C(31) C 0.3010(6) 0.2177(2) 0.5804(5) 0.057(2) Uani 1.00 1 d . . . C(32) C 0.4315(6) 0.2084(2) 0.6546(4) 0.045(2) Uani 1.00 1 d . . . H(1) H 0.4185 0.1853 0.3878 0.056 Uiso 1.00 1 c . . . H(2) H 0.5060 0.1775 0.3110 0.056 Uiso 1.00 1 c . . . H(3) H 0.3809 0.1423 0.3023 0.056 Uiso 1.00 1 c . . . H(4) H 0.5517 0.0546 0.3328 0.065 Uiso 1.00 1 c . . . H(5) H 0.6851 0.0854 0.3417 0.065 Uiso 1.00 1 c . . . H(6) H 0.6892 0.0480 0.4345 0.065 Uiso 1.00 1 c . . . H(7) H 0.4419 0.1140 0.5692 0.074 Uiso 1.00 1 c . . . H(8) H 0.3956 0.0730 0.4790 0.074 Uiso 1.00 1 c . . . H(9) H 0.5328 0.0664 0.5810 0.074 Uiso 1.00 1 c . . . H(10) H 0.9652 0.1010 0.5085 0.082 Uiso 1.00 1 c . . . H(11) H 1.0953 0.0671 0.5262 0.082 Uiso 1.00 1 c . . . H(12) H 0.9464 0.0439 0.4986 0.082 Uiso 1.00 1 c . . . H(13) H 1.0557 -0.0194 0.7056 0.056 Uiso 1.00 1 c . . . H(14) H 1.2028 0.0040 0.7253 0.056 Uiso 1.00 1 c . . . H(15) H 1.1374 0.0059 0.8180 0.056 Uiso 1.00 1 c . . . H(16) H 1.1685 0.1174 0.8285 0.062 Uiso 1.00 1 c . . . H(17) H 1.2375 0.1147 0.7381 0.063 Uiso 1.00 1 c . . . H(18) H 1.1074 0.1486 0.7209 0.062 Uiso 1.00 1 c . . . H(19) H 0.8129 0.1903 1.0283 0.036 Uiso 1.00 1 c . . . H(20) H 0.9066 0.2118 0.9658 0.036 Uiso 1.00 1 c . . . H(21) H 0.7014 0.2552 0.9005 0.039 Uiso 1.00 1 c . . . H(22) H 0.6152 0.2062 0.8796 0.039 Uiso 1.00 1 c . . . H(23) H 0.6027 0.0750 0.7691 0.047 Uiso 1.00 1 c . . . H(24) H 0.4123 0.0376 0.7960 0.057 Uiso 1.00 1 c . . . H(25) H 0.3878 0.0411 0.9664 0.059 Uiso 1.00 1 c . . . H(26) H 0.5556 0.0799 1.1118 0.057 Uiso 1.00 1 c . . . H(27) H 0.7433 0.1194 1.0834 0.047 Uiso 1.00 1 c . . . H(28) H 0.9064 0.0451 1.0237 0.041 Uiso 1.00 1 c . . . H(29) H 1.1173 0.0135 1.1446 0.050 Uiso 1.00 1 c . . . H(30) H 1.3217 0.0577 1.1789 0.044 Uiso 1.00 1 c . . . H(31) H 1.3201 0.1326 1.0943 0.045 Uiso 1.00 1 c . . . H(32) H 1.1109 0.1644 0.9770 0.040 Uiso 1.00 1 c . . . H(33) H 0.9696 0.2200 0.7010 0.040 Uiso 1.00 1 c . . . H(34) H 1.1380 0.2799 0.7145 0.047 Uiso 1.00 1 c . . . H(35) H 1.1074 0.3591 0.7659 0.052 Uiso 1.00 1 c . . . H(36) H 0.9114 0.3792 0.8101 0.053 Uiso 1.00 1 c . . . H(37) H 0.7433 0.3188 0.7977 0.044 Uiso 1.00 1 c . . . H(38) H 0.6044 0.2901 0.5753 0.045 Uiso 1.00 1 c . . . H(39) H 0.3793 0.3054 0.4479 0.061 Uiso 1.00 1 c . . . H(40) H 0.1928 0.2584 0.4494 0.061 Uiso 1.00 1 c . . . H(41) H 0.2220 0.1995 0.5837 0.065 Uiso 1.00 1 c . . . H(42) H 0.4444 0.1829 0.7083 0.051 Uiso 1.00 1 c . . . 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 Ni(1) 0.0343(4) 0.0246(4) 0.0203(4) 0.0034(3) 0.0086(3) 0.0006(3) S(1) 0.0443(9) 0.0341(8) 0.0204(7) 0.0038(7) 0.0088(7) 0.0007(6) S(2) 0.0393(8) 0.0286(8) 0.0316(8) 0.0043(7) 0.0124(7) -0.0008(6) P(1) 0.0294(8) 0.0273(8) 0.0221(7) 0.0008(6) 0.0070(6) 0.0013(6) P(2) 0.0367(8) 0.0245(8) 0.0223(8) 0.0039(6) 0.0095(7) 0.0017(6) Si(1) 0.0408(10) 0.0443(10) 0.0320(9) 0.0046(8) 0.0074(8) -0.0040(8) Si(2) 0.0408(9) 0.0353(9) 0.0325(9) 0.0068(8) 0.0119(8) -0.0004(8) C(1) 0.047(4) 0.054(4) 0.039(4) 0.007(3) -0.006(3) -0.000(3) C(2) 0.056(4) 0.051(4) 0.055(4) 0.001(3) 0.007(3) -0.026(3) C(3) 0.057(4) 0.075(5) 0.053(4) -0.015(4) 0.013(4) -0.007(4) C(4) 0.063(4) 0.102(6) 0.041(4) 0.028(4) 0.029(4) -0.001(4) C(5) 0.042(4) 0.038(4) 0.059(4) 0.002(3) 0.018(3) -0.001(3) C(6) 0.050(4) 0.042(4) 0.064(4) -0.002(3) 0.025(3) -0.001(3) C(7) 0.044(3) 0.024(3) 0.023(3) -0.000(2) 0.014(3) -0.004(2) C(8) 0.048(4) 0.016(3) 0.034(3) -0.000(2) 0.021(3) 0.002(2) C(9) 0.030(3) 0.021(3) 0.037(3) 0.001(2) 0.013(3) 0.004(3) C(10) 0.032(3) 0.050(4) 0.034(4) 0.001(3) 0.012(3) -0.001(3) C(11) 0.030(3) 0.064(5) 0.049(4) -0.011(3) 0.003(3) -0.009(3) C(12) 0.032(4) 0.060(4) 0.056(4) -0.002(3) 0.021(3) 0.003(4) C(13) 0.054(4) 0.045(4) 0.044(4) 0.004(3) 0.027(3) 0.007(3) C(14) 0.045(4) 0.041(4) 0.031(3) -0.005(3) 0.014(3) -0.001(3) C(15) 0.024(3) 0.023(3) 0.016(3) 0.004(2) 0.005(2) 0.000(2) C(16) 0.036(3) 0.030(3) 0.037(3) -0.004(3) 0.002(3) 0.006(3) C(17) 0.049(4) 0.032(3) 0.044(4) 0.012(3) 0.007(3) 0.017(3) C(18) 0.028(3) 0.050(4) 0.031(3) 0.005(3) -0.000(3) 0.000(3) C(19) 0.027(3) 0.046(4) 0.040(4) -0.004(3) -0.001(3) 0.005(3) C(20) 0.038(3) 0.031(3) 0.032(3) -0.007(3) 0.012(3) 0.002(3) C(21) 0.036(3) 0.021(3) 0.021(3) 0.003(2) 0.006(2) 0.005(2) C(22) 0.034(3) 0.032(3) 0.034(3) 0.011(3) 0.009(3) 0.001(3) C(23) 0.039(4) 0.049(4) 0.029(3) -0.002(3) 0.009(3) 0.001(3) C(24) 0.042(4) 0.054(4) 0.033(3) -0.015(3) 0.009(3) -0.002(3) C(25) 0.066(4) 0.028(4) 0.039(4) -0.006(3) 0.016(3) -0.005(3) C(26) 0.043(4) 0.034(3) 0.033(3) 0.003(3) 0.018(3) 0.003(3) C(27) 0.035(3) 0.035(3) 0.026(3) 0.005(3) 0.010(3) -0.004(3) C(28) 0.043(4) 0.041(4) 0.029(3) 0.009(3) 0.014(3) -0.001(3) C(29) 0.070(5) 0.047(4) 0.036(4) 0.028(4) 0.009(4) 0.007(3) C(30) 0.051(4) 0.054(5) 0.048(4) 0.022(4) -0.005(4) -0.018(4) C(31) 0.042(4) 0.057(5) 0.064(5) 0.009(3) 0.008(4) -0.012(4) C(32) 0.044(4) 0.039(4) 0.044(4) 0.001(3) 0.006(3) 0.002(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # 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 Ni(1) S(1) 2.250(1) yes . . Ni(1) S(2) 2.231(1) yes . . Ni(1) P(1) 2.162(1) yes . . Ni(1) P(2) 2.163(2) yes . . S(1) Si(1) 2.136(2) yes . . S(2) Si(2) 2.115(2) yes . . P(1) C(7) 1.832(5) yes . . P(1) C(9) 1.828(6) yes . . P(1) C(15) 1.815(4) yes . . P(2) C(8) 1.833(5) yes . . P(2) C(21) 1.824(5) yes . . P(2) C(27) 1.814(5) yes . . Si(1) C(1) 1.865(5) yes . . Si(1) C(2) 1.862(6) yes . . Si(1) C(3) 1.869(7) yes . . Si(2) C(4) 1.870(6) yes . . Si(2) C(5) 1.869(5) yes . . Si(2) C(6) 1.873(5) yes . . C(7) C(8) 1.517(6) yes . . C(9) C(10) 1.375(6) yes . . C(9) C(14) 1.391(8) yes . . C(10) C(11) 1.380(8) yes . . C(11) C(12) 1.375(9) yes . . C(12) C(13) 1.365(7) yes . . C(13) C(14) 1.385(8) yes . . C(15) C(16) 1.389(7) yes . . C(15) C(20) 1.388(7) yes . . C(16) C(17) 1.389(7) yes . . C(17) C(18) 1.367(8) yes . . C(18) C(19) 1.367(8) yes . . C(19) C(20) 1.373(6) yes . . C(21) C(22) 1.386(8) yes . . C(21) C(26) 1.385(7) yes . . C(22) C(23) 1.388(8) yes . . C(23) C(24) 1.368(8) yes . . C(24) C(25) 1.380(9) yes . . C(25) C(26) 1.390(8) yes . . C(27) C(28) 1.377(7) yes . . C(27) C(32) 1.392(8) yes . . C(28) C(29) 1.401(7) yes . . C(29) C(30) 1.36(1) yes . . C(30) C(31) 1.369(9) yes . . C(31) C(32) 1.383(7) yes . . 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 S(1) Ni(1) S(2) 98.29(6) yes . . . S(1) Ni(1) P(1) 173.31(6) yes . . . S(1) Ni(1) P(2) 86.98(5) yes . . . S(2) Ni(1) P(1) 88.06(6) yes . . . S(2) Ni(1) P(2) 172.93(7) yes . . . P(1) Ni(1) P(2) 86.87(6) yes . . . Si(1) S(1) Ni(1) 106.99(8) yes . . . Si(2) S(2) Ni(1) 107.28(7) yes . . . C(7) P(1) C(9) 102.8(2) yes . . . C(7) P(1) C(15) 103.5(2) yes . . . C(7) P(1) Ni(1) 108.2(2) yes . . . C(9) P(1) C(15) 105.5(2) yes . . . C(9) P(1) Ni(1) 111.7(2) yes . . . C(15) P(1) Ni(1) 123.1(2) yes . . . C(8) P(2) C(21) 103.2(2) yes . . . C(8) P(2) C(27) 103.9(2) yes . . . C(8) P(2) Ni(1) 109.2(2) yes . . . C(21) P(2) C(27) 108.5(2) yes . . . C(21) P(2) Ni(1) 113.0(2) yes . . . C(27) P(2) Ni(1) 117.7(2) yes . . . C(1) Si(1) C(2) 108.0(2) yes . . . C(1) Si(1) C(3) 107.6(3) yes . . . C(1) Si(1) S(1) 107.1(2) yes . . . C(2) Si(1) C(3) 105.8(3) yes . . . C(2) Si(1) S(1) 112.0(2) yes . . . C(3) Si(1) S(1) 116.1(2) yes . . . C(4) Si(2) C(5) 109.4(3) yes . . . C(4) Si(2) C(6) 106.2(3) yes . . . C(4) Si(2) S(2) 113.9(2) yes . . . C(5) Si(2) C(6) 110.1(2) yes . . . C(5) Si(2) S(2) 104.7(2) yes . . . C(6) Si(2) S(2) 112.7(2) yes . . . C(8) C(7) P(1) 107.4(3) yes . . . P(2) C(8) C(7) 106.6(4) yes . . . C(10) C(9) C(14) 118.7(5) yes . . . C(10) C(9) P(1) 120.2(4) yes . . . C(14) C(9) P(1) 121.0(3) yes . . . C(11) C(10) C(9) 120.8(5) yes . . . C(12) C(11) C(10) 119.8(5) yes . . . C(13) C(12) C(11) 120.5(6) yes . . . C(14) C(13) C(12) 119.7(6) yes . . . C(9) C(14) C(13) 120.5(4) yes . . . C(16) C(15) C(20) 118.1(4) yes . . . C(16) C(15) P(1) 122.2(3) yes . . . C(20) C(15) P(1) 119.7(3) yes . . . C(17) C(16) C(15) 120.4(5) yes . . . C(18) C(17) C(16) 119.6(5) yes . . . C(19) C(18) C(17) 121.1(4) yes . . . C(20) C(19) C(18) 119.4(5) yes . . . C(15) C(20) C(19) 121.5(5) yes . . . C(22) C(21) C(26) 118.5(5) yes . . . C(22) C(21) P(2) 120.2(4) yes . . . C(26) C(21) P(2) 121.1(4) yes . . . C(23) C(22) C(21) 120.4(5) yes . . . C(24) C(23) C(22) 120.3(5) yes . . . C(25) C(24) C(23) 120.5(5) yes . . . C(26) C(25) C(24) 119.0(5) yes . . . C(21) C(26) C(25) 121.3(5) yes . . . C(28) C(27) C(32) 118.2(4) yes . . . C(28) C(27) P(2) 123.5(4) yes . . . C(32) C(27) P(2) 118.1(4) yes . . . C(29) C(28) C(27) 120.2(5) yes . . . C(30) C(29) C(28) 120.4(5) yes . . . C(31) C(30) C(29) 120.2(5) yes . . . C(32) C(31) C(30) 119.8(6) yes . . . C(27) C(32) C(31) 121.1(5) yes . . . 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 S(2) Ni(1) S(1) Si(1) 63.58(8) yes . . . . P(2) Ni(1) S(1) Si(1) -111.67(7) yes . . . . S(1) Ni(1) S(2) Si(2) 65.43(7) yes . . . . P(1) Ni(1) S(2) Si(2) -112.45(6) yes . . . . S(2) Ni(1) P(1) C(7) 170.9(2) yes . . . . S(2) Ni(1) P(1) C(9) -76.7(2) yes . . . . S(2) Ni(1) P(1) C(15) 50.3(2) yes . . . . P(2) Ni(1) P(1) C(7) -14.1(2) yes . . . . P(2) Ni(1) P(1) C(9) 98.3(2) yes . . . . P(2) Ni(1) P(1) C(15) -134.6(2) yes . . . . S(1) Ni(1) P(2) C(8) 171.9(2) yes . . . . S(1) Ni(1) P(2) C(21) -73.8(2) yes . . . . S(1) Ni(1) P(2) C(27) 53.9(2) yes . . . . P(1) Ni(1) P(2) C(8) -10.7(2) yes . . . . P(1) Ni(1) P(2) C(21) 103.6(2) yes . . . . P(1) Ni(1) P(2) C(27) -128.7(2) yes . . . . Ni(1) S(1) Si(1) C(1) 134.9(2) yes . . . . Ni(1) S(1) Si(1) C(2) -106.9(2) yes . . . . Ni(1) S(1) Si(1) C(3) 14.7(2) yes . . . . Ni(1) S(2) Si(2) C(4) -85.4(2) yes . . . . Ni(1) S(2) Si(2) C(5) 155.2(2) yes . . . . Ni(1) S(2) Si(2) C(6) 35.6(2) yes . . . . Ni(1) P(1) C(7) C(8) 41.6(4) yes . . . . C(9) P(1) C(7) C(8) -76.6(4) yes . . . . C(15) P(1) C(7) C(8) 173.7(3) yes . . . . Ni(1) P(1) C(9) C(10) 14.0(4) yes . . . . Ni(1) P(1) C(9) C(14) -161.9(3) yes . . . . C(7) P(1) C(9) C(10) 129.8(4) yes . . . . C(7) P(1) C(9) C(14) -46.1(4) yes . . . . C(15) P(1) C(9) C(10) -122.1(4) yes . . . . C(15) P(1) C(9) C(14) 62.1(4) yes . . . . Ni(1) P(1) C(15) C(16) -112.9(4) yes . . . . Ni(1) P(1) C(15) C(20) 67.6(5) yes . . . . C(7) P(1) C(15) C(16) 124.4(4) yes . . . . C(7) P(1) C(15) C(20) -55.1(4) yes . . . . C(9) P(1) C(15) C(16) 16.8(5) yes . . . . C(9) P(1) C(15) C(20) -162.8(4) yes . . . . Ni(1) P(2) C(8) C(7) 38.6(3) yes . . . . C(21) P(2) C(8) C(7) -81.9(3) yes . . . . C(27) P(2) C(8) C(7) 164.9(3) yes . . . . Ni(1) P(2) C(21) C(22) 7.9(4) yes . . . . Ni(1) P(2) C(21) C(26) -167.1(3) yes . . . . C(8) P(2) C(21) C(22) 125.7(3) yes . . . . C(8) P(2) C(21) C(26) -49.3(4) yes . . . . C(27) P(2) C(21) C(22) -124.5(3) yes . . . . C(27) P(2) C(21) C(26) 60.5(4) yes . . . . Ni(1) P(2) C(27) C(28) -113.5(4) yes . . . . Ni(1) P(2) C(27) C(32) 62.3(5) yes . . . . C(8) P(2) C(27) C(28) 125.7(5) yes . . . . C(8) P(2) C(27) C(32) -58.5(5) yes . . . . C(21) P(2) C(27) C(28) 16.4(5) yes . . . . C(21) P(2) C(27) C(32) -167.8(4) yes . . . . P(1) C(7) C(8) P(2) -49.3(4) yes . . . . P(1) C(9) C(10) C(11) -175.3(4) yes . . . . C(14) C(9) C(10) C(11) 0.7(7) yes . . . . P(1) C(9) C(14) C(13) 175.5(4) yes . . . . C(10) C(9) C(14) C(13) -0.4(7) yes . . . . C(9) C(10) C(11) C(12) -0.1(8) yes . . . . C(10) C(11) C(12) C(13) -0.7(8) yes . . . . C(11) C(12) C(13) C(14) 0.9(8) yes . . . . C(12) C(13) C(14) C(9) -0.4(8) yes . . . . P(1) C(15) C(16) C(17) -179.1(5) yes . . . . C(20) C(15) C(16) C(17) 0.5(8) yes . . . . P(1) C(15) C(20) C(19) 179.6(5) yes . . . . C(16) C(15) C(20) C(19) -0.0(8) yes . . . . C(15) C(16) C(17) C(18) -0.4(9) yes . . . . C(16) C(17) C(18) C(19) -0.2(9) yes . . . . C(17) C(18) C(19) C(20) 0.7(9) yes . . . . C(18) C(19) C(20) C(15) -0.6(9) yes . . . . P(2) C(21) C(22) C(23) -175.8(4) yes . . . . C(26) C(21) C(22) C(23) -0.6(7) yes . . . . P(2) C(21) C(26) C(25) 176.0(4) yes . . . . C(22) C(21) C(26) C(25) 0.9(7) yes . . . . C(21) C(22) C(23) C(24) -0.2(7) yes . . . . C(22) C(23) C(24) C(25) 0.9(7) yes . . . . C(23) C(24) C(25) C(26) -0.6(7) yes . . . . C(24) C(25) C(26) C(21) -0.3(7) yes . . . . P(2) C(27) C(28) C(29) 174.2(5) yes . . . . C(32) C(27) C(28) C(29) -1.7(8) yes . . . . P(2) C(27) C(32) C(31) -174.6(5) yes . . . . C(28) C(27) C(32) C(31) 1.5(9) yes . . . . C(27) C(28) C(29) C(30) -0.3(9) yes . . . . C(28) C(29) C(30) C(31) 2(1) yes . . . . C(29) C(30) C(31) C(32) -2(1) yes . . . . C(30) C(31) C(32) C(27) 0(1) yes . . . . 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 Ni(1) S(1) 2.250(1) yes . 55501 Ni(1) S(2) 2.231(1) yes . 55501 Ni(1) Si(1) 3.527(1) yes . 55501 Ni(1) Si(2) 3.501(2) yes . 55501 Ni(1) C(7) 3.242(5) yes . 55501 Ni(1) C(8) 3.262(5) yes . 55501 Ni(1) C(9) 3.307(6) yes . 55501 Ni(1) C(10) 3.439(6) yes . 55501 Ni(1) C(15) 3.500(4) yes . 55501 Ni(1) C(21) 3.329(5) yes . 55501 Ni(1) C(22) 3.464(5) yes . 55501 Ni(1) C(27) 3.408(5) yes . 55501 S(1) Ni(1) 2.250(1) yes . 55501 S(1) S(2) 3.390(2) yes . 55501 S(1) P(2) 3.038(2) yes . 55501 S(1) Si(1) 2.136(2) yes . 55501 S(1) C(1) 3.222(4) yes . 55501 S(1) C(2) 3.317(5) yes . 55501 S(1) C(3) 3.401(6) yes . 55501 S(1) C(22) 3.518(5) yes . 55501 S(1) C(27) 3.423(6) yes . 55501 S(2) Ni(1) 2.231(1) yes . 55501 S(2) S(1) 3.390(2) yes . 55501 S(2) P(1) 3.054(2) yes . 55501 S(2) C(4) 3.343(7) yes . 55501 S(2) C(5) 3.157(5) yes . 55501 S(2) C(6) 3.322(5) yes . 55501 S(2) C(10) 3.524(6) yes . 55501 S(2) C(15) 3.524(4) yes . 55501 P(1) S(2) 3.054(2) yes . 55501 P(1) P(2) 2.974(2) yes . 55501 P(1) C(7) 1.832(5) yes . 55501 P(1) C(8) 2.706(5) yes . 55501 P(1) C(10) 2.786(5) yes . 55501 P(1) C(14) 2.810(6) yes . 55501 P(1) C(16) 2.812(5) yes . 55501 P(1) C(20) 2.778(5) yes . 55501 P(2) S(1) 3.038(2) yes . 55501 P(2) P(1) 2.974(2) yes . 55501 P(2) C(7) 2.693(5) yes . 55501 P(2) C(8) 1.833(5) yes . 55501 P(2) C(22) 2.791(6) yes . 55501 P(2) C(26) 2.803(5) yes . 55501 P(2) C(28) 2.819(5) yes . 55501 P(2) C(32) 2.759(5) yes . 55501 Si(1) Ni(1) 3.527(1) yes . 55501 Si(1) S(1) 2.136(2) yes . 55501 Si(2) Ni(1) 3.501(2) yes . 55501 C(1) S(1) 3.222(4) yes . 55501 C(1) C(2) 3.015(7) yes . 55501 C(1) C(3) 3.014(8) yes . 55501 C(2) S(1) 3.317(5) yes . 55501 C(2) C(1) 3.015(7) yes . 55501 C(2) C(3) 2.975(9) yes . 55501 C(3) S(1) 3.401(6) yes . 55501 C(3) C(1) 3.014(8) yes . 55501 C(3) C(2) 2.975(9) yes . 55501 C(4) S(2) 3.343(7) yes . 55501 C(4) C(5) 3.052(7) yes . 55501 C(4) C(6) 2.993(7) yes . 55501 C(5) S(2) 3.157(5) yes . 55501 C(5) C(4) 3.052(7) yes . 55501 C(5) C(6) 3.067(7) yes . 55501 C(6) S(2) 3.322(5) yes . 55501 C(6) C(4) 2.993(7) yes . 55501 C(6) C(5) 3.067(7) yes . 55501 C(7) Ni(1) 3.242(5) yes . 55501 C(7) P(1) 1.832(5) yes . 55501 C(7) P(2) 2.693(5) yes . 55501 C(7) C(9) 2.860(6) yes . 55501 C(7) C(14) 3.219(7) yes . 55501 C(7) C(15) 2.864(6) yes . 55501 C(7) C(20) 3.280(7) yes . 55501 C(7) C(21) 3.427(7) yes . 55501 C(7) C(22) 3.585(6) yes . 55504 C(7) C(23) 3.595(6) yes . 55504 C(8) Ni(1) 3.262(5) yes . 55501 C(8) P(1) 2.706(5) yes . 55501 C(8) P(2) 1.833(5) yes . 55501 C(8) C(9) 3.365(6) yes . 55501 C(8) C(21) 2.867(8) yes . 55501 C(8) C(26) 3.254(7) yes . 55501 C(8) C(27) 2.871(6) yes . 55501 C(8) C(32) 3.295(6) yes . 55501 C(9) Ni(1) 3.307(6) yes . 55501 C(9) C(7) 2.860(6) yes . 55501 C(9) C(8) 3.365(6) yes . 55501 C(9) C(11) 2.396(7) yes . 55501 C(9) C(12) 2.768(8) yes . 55501 C(9) C(13) 2.410(9) yes . 55501 C(9) C(15) 2.901(7) yes . 55501 C(9) C(16) 3.129(6) yes . 55501 C(10) Ni(1) 3.439(6) yes . 55501 C(10) S(2) 3.524(6) yes . 55501 C(10) P(1) 2.786(5) yes . 55501 C(10) C(12) 2.383(9) yes . 55501 C(10) C(13) 2.753(9) yes . 55501 C(10) C(14) 2.378(7) yes . 55501 C(11) C(9) 2.396(7) yes . 55501 C(11) C(13) 2.379(8) yes . 55501 C(11) C(14) 2.749(7) yes . 55501 C(12) C(9) 2.768(8) yes . 55501 C(12) C(10) 2.383(9) yes . 55501 C(12) C(14) 2.378(7) yes . 55501 C(13) C(9) 2.410(9) yes . 55501 C(13) C(10) 2.753(9) yes . 55501 C(13) C(11) 2.379(8) yes . 55501 C(14) P(1) 2.810(6) yes . 55501 C(14) C(7) 3.219(7) yes . 55501 C(14) C(10) 2.378(7) yes . 55501 C(14) C(11) 2.749(7) yes . 55501 C(14) C(12) 2.378(7) yes . 55501 C(14) C(15) 3.423(8) yes . 55501 C(14) C(16) 3.377(8) yes . 55501 C(15) Ni(1) 3.500(4) yes . 55501 C(15) Ni(1) 2.973(4) yes . 65605 C(15) S(1) 2.973(5) yes . 65605 C(15) S(2) 3.524(4) yes . 55501 C(15) S(2) 2.973(5) yes . 65605 C(15) P(1) 2.973(5) yes . 65605 C(15) P(2) 2.973(5) yes . 65605 C(15) Si(1) 2.973(5) yes . 65605 C(15) Si(2) 2.973(5) yes . 65605 C(15) C(1) 2.973(7) yes . 65605 C(15) C(2) 2.973(7) yes . 65605 C(15) C(3) 2.973(7) yes . 65605 C(15) C(4) 2.973(8) yes . 65605 C(15) C(5) 2.973(7) yes . 65605 C(15) C(6) 2.973(7) yes . 65605 C(15) C(7) 2.864(6) yes . 55501 C(15) C(7) 2.973(6) yes . 65605 C(15) C(8) 2.973(6) yes . 65605 C(15) C(9) 2.901(7) yes . 55501 C(15) C(9) 2.973(6) yes . 65605 C(15) C(10) 2.973(7) yes . 65605 C(15) C(11) 2.973(7) yes . 65605 C(15) C(12) 2.973(7) yes . 65605 C(15) C(13) 2.973(7) yes . 65605 C(15) C(14) 3.423(8) yes . 55501 C(15) C(14) 2.973(7) yes . 65605 C(15) C(15) 2.973(6) yes . 65605 C(15) C(16) 2.973(7) yes . 65605 C(15) C(17) 2.410(6) yes . 55501 C(15) C(17) 2.973(7) yes . 65605 C(15) C(18) 2.767(6) yes . 55501 C(15) C(18) 2.973(7) yes . 65605 C(15) C(19) 2.408(6) yes . 55501 C(15) C(19) 2.973(7) yes . 65605 C(15) C(20) 2.973(7) yes . 65605 C(15) C(21) 2.973(6) yes . 65605 C(15) C(22) 2.973(7) yes . 65605 C(15) C(23) 2.973(7) yes . 65605 C(15) C(24) 2.973(7) yes . 65605 C(15) C(25) 2.973(7) yes . 65605 C(15) C(26) 2.973(7) yes . 65605 C(15) C(27) 2.973(7) yes . 65605 C(15) C(28) 2.973(7) yes . 65605 C(15) C(29) 2.973(7) yes . 65605 C(15) C(30) 2.973(8) yes . 65605 C(15) C(31) 2.973(8) yes . 65605 C(15) C(32) 2.973(7) yes . 65605 C(16) S(1) 1.822(5) yes . 65605 C(16) S(2) 1.822(5) yes . 65605 C(16) P(1) 2.812(5) yes . 55501 C(16) C(1) 1.822(7) yes . 65605 C(16) C(2) 1.822(7) yes . 65605 C(16) C(3) 1.822(8) yes . 65605 C(16) C(4) 1.822(8) yes . 65605 C(16) C(5) 1.822(7) yes . 65605 C(16) C(6) 1.822(7) yes . 65605 C(16) C(7) 1.822(7) yes . 65605 C(16) C(8) 1.822(7) yes . 65605 C(16) C(9) 3.129(6) yes . 55501 C(16) C(9) 1.822(7) yes . 65605 C(16) C(10) 1.822(7) yes . 65605 C(16) C(11) 1.822(8) yes . 65605 C(16) C(12) 1.822(8) yes . 65605 C(16) C(13) 1.822(7) yes . 65605 C(16) C(14) 3.377(8) yes . 55501 C(16) C(14) 1.822(7) yes . 65605 C(16) C(15) 1.822(7) yes . 65605 C(16) C(16) 1.822(7) yes . 65605 C(16) C(17) 1.822(7) yes . 65605 C(16) C(18) 2.382(7) yes . 55501 C(16) C(18) 1.822(8) yes . 65605 C(16) C(19) 2.760(7) yes . 55501 C(16) C(19) 1.822(7) yes . 65605 C(16) C(20) 2.382(7) yes . 55501 C(16) C(20) 1.822(7) yes . 65605 C(16) C(21) 1.822(7) yes . 65605 C(16) C(22) 1.822(7) yes . 65605 C(16) C(23) 1.822(8) yes . 65605 C(16) C(24) 1.822(8) yes . 65605 C(16) C(25) 1.822(7) yes . 65605 C(16) C(26) 1.822(7) yes . 65605 C(16) C(27) 1.822(7) yes . 65605 C(16) C(28) 1.822(7) yes . 65605 C(16) C(29) 1.822(8) yes . 65605 C(16) C(30) 1.822(8) yes . 65605 C(16) C(31) 1.822(8) yes . 65605 C(16) C(32) 1.822(7) yes . 65605 C(17) Ni(1) 1.951(5) yes . 65605 C(17) S(1) 1.951(5) yes . 65605 C(17) S(2) 1.951(5) yes . 65605 C(17) P(1) 1.951(5) yes . 65605 C(17) P(2) 1.951(5) yes . 65605 C(17) Si(1) 1.951(5) yes . 65605 C(17) Si(2) 1.951(5) yes . 65605 C(17) C(1) 1.951(7) yes . 65605 C(17) C(2) 1.951(7) yes . 65605 C(17) C(3) 1.951(7) yes . 65605 C(17) C(4) 1.951(7) yes . 65605 C(17) C(5) 1.951(7) yes . 65605 C(17) C(6) 1.951(7) yes . 65605 C(17) C(7) 1.951(6) yes . 65605 C(17) C(8) 1.951(6) yes . 65605 C(17) C(9) 1.951(7) yes . 65605 C(17) C(10) 1.951(7) yes . 65605 C(17) C(11) 1.951(7) yes . 65605 C(17) C(12) 1.951(7) yes . 65605 C(17) C(13) 1.951(7) yes . 65605 C(17) C(14) 1.951(7) yes . 65605 C(17) C(15) 2.410(6) yes . 55501 C(17) C(15) 1.951(6) yes . 65605 C(17) C(16) 1.951(7) yes . 65605 C(17) C(17) 1.951(7) yes . 65605 C(17) C(18) 1.951(7) yes . 65605 C(17) C(19) 2.380(8) yes . 55501 C(17) C(19) 1.951(7) yes . 65605 C(17) C(20) 2.745(7) yes . 55501 C(17) C(20) 1.951(7) yes . 65605 C(17) C(21) 1.951(6) yes . 65605 C(17) C(22) 1.951(7) yes . 65605 C(17) C(23) 1.951(7) yes . 65605 C(17) C(24) 1.951(7) yes . 65605 C(17) C(25) 1.951(7) yes . 65605 C(17) C(26) 1.951(7) yes . 65605 C(17) C(27) 1.951(7) yes . 65605 C(17) C(28) 1.951(7) yes . 65605 C(17) C(29) 1.951(7) yes . 65605 C(17) C(30) 1.951(8) yes . 65605 C(17) C(31) 1.951(8) yes . 65605 C(17) C(32) 1.951(7) yes . 65605 C(18) Ni(1) 3.110(5) yes . 65605 C(18) S(1) 3.110(5) yes . 65605 C(18) S(2) 3.110(5) yes . 65605 C(18) P(1) 3.110(5) yes . 65605 C(18) P(2) 3.110(5) yes . 65605 C(18) Si(1) 3.110(5) yes . 65605 C(18) Si(2) 3.110(5) yes . 65605 C(18) C(1) 3.110(7) yes . 65605 C(18) C(2) 3.110(7) yes . 65605 C(18) C(3) 3.110(7) yes . 65605 C(18) C(4) 3.110(7) yes . 65605 C(18) C(5) 3.110(7) yes . 65605 C(18) C(6) 3.110(7) yes . 65605 C(18) C(7) 3.110(7) yes . 65605 C(18) C(8) 3.110(7) yes . 65605 C(18) C(9) 3.110(7) yes . 65605 C(18) C(10) 3.110(7) yes . 65605 C(18) C(11) 3.110(7) yes . 65605 C(18) C(12) 3.110(7) yes . 65605 C(18) C(13) 3.110(7) yes . 65605 C(18) C(14) 3.110(7) yes . 65605 C(18) C(15) 2.767(6) yes . 55501 C(18) C(15) 3.110(6) yes . 65605 C(18) C(16) 2.382(7) yes . 55501 C(18) C(16) 3.110(7) yes . 65605 C(18) C(17) 3.110(7) yes . 65605 C(18) C(18) 3.110(7) yes . 65605 C(18) C(19) 3.110(7) yes . 65605 C(18) C(20) 2.365(7) yes . 55501 C(18) C(20) 3.110(7) yes . 65605 C(18) C(21) 3.110(7) yes . 65605 C(18) C(22) 3.110(7) yes . 65605 C(18) C(23) 3.110(7) yes . 65605 C(18) C(24) 3.110(7) yes . 65605 C(18) C(25) 3.110(7) yes . 65605 C(18) C(26) 3.110(7) yes . 65605 C(18) C(27) 3.110(7) yes . 65605 C(18) C(28) 3.110(7) yes . 65605 C(18) C(29) 3.110(8) yes . 65605 C(18) C(30) 3.110(8) yes . 65605 C(18) C(31) 3.110(8) yes . 65605 C(18) C(32) 3.110(7) yes . 65605 C(19) C(15) 2.408(6) yes . 55501 C(19) C(16) 2.760(7) yes . 55501 C(19) C(17) 2.380(8) yes . 55501 C(20) P(1) 2.778(5) yes . 55501 C(20) C(7) 3.280(7) yes . 55501 C(20) C(16) 2.382(7) yes . 55501 C(20) C(17) 2.745(7) yes . 55501 C(20) C(18) 2.365(7) yes . 55501 C(21) Ni(1) 3.329(5) yes . 55501 C(21) C(7) 3.427(7) yes . 55501 C(21) C(8) 2.867(8) yes . 55501 C(21) C(23) 2.407(8) yes . 55501 C(21) C(24) 2.779(8) yes . 55501 C(21) C(25) 2.418(7) yes . 55501 C(21) C(27) 2.953(7) yes . 55501 C(21) C(28) 3.232(6) yes . 55501 C(22) Ni(1) 3.464(5) yes . 55501 C(22) S(1) 3.518(5) yes . 55501 C(22) P(2) 2.791(6) yes . 55501 C(22) C(24) 2.391(7) yes . 55501 C(22) C(25) 2.769(7) yes . 55501 C(22) C(26) 2.381(8) yes . 55501 C(23) C(21) 2.407(8) yes . 55501 C(23) C(25) 2.386(8) yes . 55501 C(23) C(26) 2.749(8) yes . 55501 C(24) C(21) 2.779(8) yes . 55501 C(24) C(22) 2.391(7) yes . 55501 C(24) C(26) 2.387(8) yes . 55501 C(25) C(21) 2.418(7) yes . 55501 C(25) C(22) 2.769(7) yes . 55501 C(25) C(23) 2.386(8) yes . 55501 C(26) P(2) 2.803(5) yes . 55501 C(26) C(8) 3.254(7) yes . 55501 C(26) C(22) 2.381(8) yes . 55501 C(26) C(23) 2.749(8) yes . 55501 C(26) C(24) 2.387(8) yes . 55501 C(26) C(27) 3.473(7) yes . 55501 C(26) C(28) 3.472(6) yes . 55501 C(27) Ni(1) 3.408(5) yes . 55501 C(27) S(1) 3.423(6) yes . 55501 C(27) C(8) 2.871(6) yes . 55501 C(27) C(21) 2.953(7) yes . 55501 C(27) C(26) 3.473(7) yes . 55501 C(27) C(29) 2.409(7) yes . 55501 C(27) C(30) 2.783(7) yes . 55501 C(27) C(31) 2.417(7) yes . 55501 C(28) P(2) 2.819(5) yes . 55501 C(28) C(21) 3.232(6) yes . 55501 C(28) C(26) 3.472(6) yes . 55501 C(28) C(30) 2.396(8) yes . 55501 C(28) C(31) 2.758(9) yes . 55501 C(28) C(32) 2.377(8) yes . 55501 C(29) C(27) 2.409(7) yes . 55501 C(29) C(31) 2.37(1) yes . 55501 C(29) C(32) 2.741(8) yes . 55501 C(30) C(27) 2.783(7) yes . 55501 C(30) C(28) 2.396(8) yes . 55501 C(30) C(32) 2.381(7) yes . 55501 C(31) C(27) 2.417(7) yes . 55501 C(31) C(28) 2.758(9) yes . 55501 C(31) C(29) 2.37(1) yes . 55501 C(32) P(2) 2.759(5) yes . 55501 C(32) C(8) 3.295(6) yes . 55501 C(32) C(28) 2.377(8) yes . 55501 C(32) C(29) 2.741(8) yes . 55501 C(32) C(30) 2.381(7) yes . 55501 #============================================================================== # 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 #============================================================================== #===END data_Ni(SSiMe2tBu)2(dppe) _database_code_depnum_ccdc_archive 'CCDC 227197' _audit_creation_date 2004-03-03 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C38 H54 Ni P2 S2 Si2 ' _chemical_formula_moiety Ni(SSiMe2tBu)2(dppe) _chemical_formula_weight 751.78 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 10.802(2) _cell_length_b 26.287(4) _cell_length_c 14.132(2) _cell_angle_alpha 90 _cell_angle_beta 92.561(3) _cell_angle_gamma 90 _cell_volume 4008.7(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8843 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600.00 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.859 _exptl_absorpt_correction_T_max 0.963 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 67758 _diffrn_reflns_av_R_equivalents 0.081 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9817 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.9877 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -100.0 sigma(F^2^). 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 9249 _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 0.0800 _refine_ls_wR_factor_ref 0.2260 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7000 _refine_ls_number_parameters 460 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0045Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 3.63 _refine_diff_density_min -1.66 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; 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 Ni(1) Ni 0.14084(7) 0.15187(3) 0.31370(5) 0.0245(2) Uani 1.00 1 d . . . S(1) S 0.0690(2) 0.16050(5) 0.16240(11) 0.0300(4) Uani 1.00 1 d . . . S(2) S 0.2076(1) 0.07103(5) 0.30957(10) 0.0291(4) Uani 1.00 1 d . . . P(1) P 0.2138(2) 0.15114(6) 0.45900(11) 0.0269(4) Uani 1.00 1 d . . . P(2) P 0.0842(1) 0.22913(6) 0.34269(11) 0.0263(4) Uani 1.00 1 d . . . Si(1) Si -0.0753(2) 0.10605(7) 0.14166(12) 0.0338(5) Uani 1.00 1 d . . . Si(2) Si 0.3500(2) 0.06636(6) 0.21031(13) 0.0335(5) Uani 1.00 1 d . . . C(1) C -0.1706(7) 0.0997(3) 0.2487(5) 0.051(2) Uani 1.00 1 d . . . C(2) C -0.0223(7) 0.0404(2) 0.1132(5) 0.048(2) Uani 1.00 1 d . . . C(3) C -0.1784(6) 0.1289(2) 0.0365(4) 0.036(2) Uani 1.00 1 d . . . C(4) C -0.2869(7) 0.0922(3) 0.0206(5) 0.048(2) Uani 1.00 1 d . . . C(5) C -0.1039(7) 0.1288(3) -0.0523(5) 0.050(2) Uani 1.00 1 d . . . C(6) C -0.2284(7) 0.1817(3) 0.0525(5) 0.056(2) Uani 1.00 1 d . . . C(7) C 0.4597(7) 0.1206(3) 0.2269(6) 0.053(2) Uani 1.00 1 d . . . C(8) C 0.2943(7) 0.0669(3) 0.0832(5) 0.055(2) Uani 1.00 1 d . . . C(9) C 0.4310(6) 0.0027(2) 0.2333(5) 0.036(2) Uani 1.00 1 d . . . C(10) C 0.5156(7) -0.0100(3) 0.1533(5) 0.049(2) Uani 1.00 1 d . . . C(11) C 0.3342(7) -0.0396(2) 0.2412(6) 0.051(2) Uani 1.00 1 d . . . C(12) C 0.5106(7) 0.0047(3) 0.3251(5) 0.054(2) Uani 1.00 1 d . . . C(13) C 0.3821(6) 0.1467(2) 0.4771(4) 0.032(2) Uani 1.00 1 d . . . C(14) C 0.4538(6) 0.1894(3) 0.4596(5) 0.041(2) Uani 1.00 1 d . . . C(15) C 0.5823(7) 0.1860(3) 0.4650(5) 0.049(2) Uani 1.00 1 d . . . C(16) C 0.6397(7) 0.1407(3) 0.4872(5) 0.050(2) Uani 1.00 1 d . . . C(17) C 0.5679(7) 0.0985(3) 0.5053(5) 0.048(2) Uani 1.00 1 d . . . C(18) C 0.4398(6) 0.1011(3) 0.4991(5) 0.041(2) Uani 1.00 1 d . . . C(19) C 0.1423(6) 0.1048(2) 0.5353(4) 0.032(2) Uani 1.00 1 d . . . C(20) C 0.1894(7) 0.0973(3) 0.6281(5) 0.043(2) Uani 1.00 1 d . . . C(21) C 0.1260(8) 0.0661(3) 0.6878(5) 0.053(2) Uani 1.00 1 d . . . C(22) C 0.0173(7) 0.0426(3) 0.6582(6) 0.052(2) Uani 1.00 1 d . . . C(23) C -0.0292(7) 0.0507(3) 0.5674(5) 0.049(2) Uani 1.00 1 d . . . C(24) C 0.0332(6) 0.0811(2) 0.5057(5) 0.040(2) Uani 1.00 1 d . . . C(25) C 0.1768(6) 0.2114(2) 0.5201(4) 0.031(2) Uani 1.00 1 d . . . C(26) C 0.0609(6) 0.2336(2) 0.4692(4) 0.032(2) Uani 1.00 1 d . . . C(27) C -0.0504(5) 0.2599(2) 0.2868(4) 0.028(2) Uani 1.00 1 d . . . C(28) C -0.1666(6) 0.2405(2) 0.3042(5) 0.037(2) Uani 1.00 1 d . . . C(29) C -0.2716(6) 0.2631(3) 0.2657(5) 0.040(2) Uani 1.00 1 d . . . C(30) C -0.2634(6) 0.3046(3) 0.2081(4) 0.040(2) Uani 1.00 1 d . . . C(31) C -0.1467(7) 0.3247(3) 0.1913(5) 0.041(2) Uani 1.00 1 d . . . C(32) C -0.0420(6) 0.3019(2) 0.2300(4) 0.036(2) Uani 1.00 1 d . . . C(33) C 0.2136(5) 0.2717(2) 0.3222(4) 0.028(2) Uani 1.00 1 d . . . C(34) C 0.2930(5) 0.2602(2) 0.2506(4) 0.031(2) Uani 1.00 1 d . . . C(35) C 0.3952(6) 0.2901(3) 0.2360(5) 0.039(2) Uani 1.00 1 d . . . C(36) C 0.4204(7) 0.3317(3) 0.2935(5) 0.047(2) Uani 1.00 1 d . . . C(37) C 0.3430(7) 0.3435(3) 0.3643(5) 0.047(2) Uani 1.00 1 d . . . C(38) C 0.2396(6) 0.3140(2) 0.3794(5) 0.038(2) Uani 1.00 1 d . . . H(1) H -0.2003 0.1329 0.2667 0.062 Uiso 1.00 1 c . . . H(2) H -0.2407 0.0774 0.2345 0.062 Uiso 1.00 1 c . . . H(3) H -0.1198 0.0854 0.3004 0.062 Uiso 1.00 1 c . . . H(4) H -0.0936 0.0187 0.1000 0.058 Uiso 1.00 1 c . . . H(5) H 0.0279 0.0417 0.0581 0.058 Uiso 1.00 1 c . . . H(6) H 0.0266 0.0268 0.1666 0.058 Uiso 1.00 1 c . . . H(7) H -0.3361 0.0917 0.0764 0.058 Uiso 1.00 1 c . . . H(8) H -0.3382 0.1032 -0.0337 0.058 Uiso 1.00 1 c . . . H(9) H -0.2554 0.0583 0.0091 0.058 Uiso 1.00 1 c . . . H(10) H -0.0731 0.0947 -0.0630 0.060 Uiso 1.00 1 c . . . H(11) H -0.1564 0.1393 -0.1063 0.060 Uiso 1.00 1 c . . . H(12) H -0.0346 0.1521 -0.0443 0.060 Uiso 1.00 1 c . . . H(13) H -0.1598 0.2055 0.0597 0.067 Uiso 1.00 1 c . . . H(14) H -0.2818 0.1918 -0.0014 0.067 Uiso 1.00 1 c . . . H(15) H -0.2754 0.1820 0.1094 0.067 Uiso 1.00 1 c . . . H(16) H 0.4905 0.1217 0.2924 0.065 Uiso 1.00 1 c . . . H(17) H 0.5286 0.1162 0.1860 0.065 Uiso 1.00 1 c . . . H(18) H 0.4174 0.1523 0.2110 0.065 Uiso 1.00 1 c . . . H(19) H 0.2536 0.0989 0.0683 0.067 Uiso 1.00 1 c . . . H(20) H 0.3644 0.0626 0.0434 0.067 Uiso 1.00 1 c . . . H(21) H 0.2363 0.0392 0.0720 0.067 Uiso 1.00 1 c . . . H(22) H 0.5550 -0.0426 0.1655 0.059 Uiso 1.00 1 c . . . H(23) H 0.4668 -0.0115 0.0940 0.059 Uiso 1.00 1 c . . . H(24) H 0.5786 0.0161 0.1491 0.059 Uiso 1.00 1 c . . . H(25) H 0.2807 -0.0317 0.2925 0.062 Uiso 1.00 1 c . . . H(26) H 0.2849 -0.0421 0.1823 0.062 Uiso 1.00 1 c . . . H(27) H 0.3759 -0.0717 0.2540 0.062 Uiso 1.00 1 c . . . H(28) H 0.5503 -0.0280 0.3364 0.065 Uiso 1.00 1 c . . . H(29) H 0.5735 0.0307 0.3196 0.065 Uiso 1.00 1 c . . . H(30) H 0.4591 0.0128 0.3776 0.065 Uiso 1.00 1 c . . . H(31) H 0.4139 0.2215 0.4437 0.049 Uiso 1.00 1 c . . . H(32) H 0.6323 0.2158 0.4535 0.058 Uiso 1.00 1 c . . . H(33) H 0.7294 0.1384 0.4905 0.060 Uiso 1.00 1 c . . . H(34) H 0.6080 0.0665 0.5220 0.057 Uiso 1.00 1 c . . . H(35) H 0.3903 0.0711 0.5102 0.048 Uiso 1.00 1 c . . . H(36) H 0.2656 0.1139 0.6498 0.052 Uiso 1.00 1 c . . . H(37) H 0.1593 0.0602 0.7518 0.063 Uiso 1.00 1 c . . . H(38) H -0.0265 0.0209 0.7009 0.063 Uiso 1.00 1 c . . . H(39) H -0.1064 0.0347 0.5463 0.059 Uiso 1.00 1 c . . . H(40) H -0.0001 0.0865 0.4415 0.048 Uiso 1.00 1 c . . . H(41) H 0.1623 0.2048 0.5863 0.038 Uiso 1.00 1 c . . . H(42) H 0.2449 0.2351 0.5156 0.038 Uiso 1.00 1 c . . . H(43) H 0.0495 0.2688 0.4874 0.039 Uiso 1.00 1 c . . . H(44) H -0.0111 0.2139 0.4854 0.039 Uiso 1.00 1 c . . . H(45) H -0.1732 0.2107 0.3442 0.044 Uiso 1.00 1 c . . . H(46) H -0.3525 0.2493 0.2785 0.048 Uiso 1.00 1 c . . . H(47) H -0.3377 0.3203 0.1801 0.047 Uiso 1.00 1 c . . . H(48) H -0.1399 0.3544 0.1511 0.049 Uiso 1.00 1 c . . . H(49) H 0.0391 0.3157 0.2180 0.043 Uiso 1.00 1 c . . . H(50) H 0.2757 0.2308 0.2108 0.037 Uiso 1.00 1 c . . . H(51) H 0.4490 0.2820 0.1849 0.047 Uiso 1.00 1 c . . . H(52) H 0.4938 0.3521 0.2843 0.056 Uiso 1.00 1 c . . . H(53) H 0.3597 0.3733 0.4034 0.057 Uiso 1.00 1 c . . . H(54) H 0.1857 0.3223 0.4303 0.046 Uiso 1.00 1 c . . . 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 Ni(1) 0.0272(5) 0.0232(4) 0.0231(4) 0.0004(3) 0.0008(3) -0.0007(3) S(1) 0.0348(9) 0.0293(8) 0.0256(8) -0.0021(7) -0.0020(7) 0.0010(6) S(2) 0.0337(9) 0.0264(8) 0.0275(8) 0.0015(7) 0.0044(7) 0.0001(6) P(1) 0.0290(9) 0.0272(8) 0.0243(8) -0.0001(7) -0.0007(7) 0.0020(7) P(2) 0.0275(9) 0.0248(8) 0.0267(8) 0.0010(7) 0.0017(7) -0.0018(7) Si(1) 0.0391(11) 0.0342(10) 0.0280(9) -0.0073(8) -0.0002(8) 0.0013(8) Si(2) 0.0387(11) 0.0286(9) 0.0338(10) 0.0051(8) 0.0089(8) 0.0033(8) C(1) 0.055(5) 0.065(5) 0.034(4) -0.019(4) 0.002(4) 0.005(4) C(2) 0.063(5) 0.030(4) 0.051(5) -0.007(3) -0.001(4) 0.002(3) C(3) 0.041(4) 0.040(4) 0.026(3) -0.010(3) -0.001(3) -0.004(3) C(4) 0.044(4) 0.058(5) 0.043(4) -0.013(4) -0.003(3) 0.000(4) C(5) 0.054(5) 0.059(5) 0.037(4) -0.014(4) -0.001(4) -0.000(4) C(6) 0.059(5) 0.059(5) 0.049(5) 0.004(4) -0.014(4) 0.002(4) C(7) 0.055(5) 0.041(4) 0.065(5) 0.000(4) 0.026(4) -0.001(4) C(8) 0.065(5) 0.062(5) 0.040(4) 0.022(4) 0.016(4) 0.008(4) C(9) 0.045(4) 0.030(3) 0.034(4) 0.006(3) 0.008(3) -0.001(3) C(10) 0.051(5) 0.041(4) 0.055(5) 0.012(4) 0.013(4) 0.001(4) C(11) 0.059(5) 0.026(3) 0.070(5) 0.004(3) 0.013(4) -0.005(4) C(12) 0.056(5) 0.048(4) 0.059(5) 0.022(4) 0.005(4) 0.005(4) C(13) 0.036(4) 0.040(4) 0.020(3) -0.001(3) -0.001(3) 0.003(3) C(14) 0.046(4) 0.041(4) 0.035(4) -0.004(3) 0.000(3) 0.004(3) C(15) 0.039(4) 0.069(5) 0.038(4) -0.021(4) 0.001(3) -0.006(4) C(16) 0.036(4) 0.075(5) 0.039(4) -0.001(4) 0.002(3) -0.005(4) C(17) 0.036(4) 0.060(5) 0.047(4) 0.011(4) -0.002(3) 0.008(4) C(18) 0.040(4) 0.047(4) 0.034(4) -0.001(3) -0.010(3) 0.004(3) C(19) 0.035(4) 0.032(3) 0.029(3) 0.004(3) 0.006(3) -0.001(3) C(20) 0.046(4) 0.050(4) 0.033(4) -0.005(3) -0.002(3) -0.000(3) C(21) 0.064(5) 0.056(5) 0.038(4) 0.001(4) 0.008(4) 0.020(4) C(22) 0.056(5) 0.041(4) 0.062(5) -0.008(4) 0.024(4) 0.017(4) C(23) 0.050(5) 0.044(4) 0.055(5) -0.005(4) 0.016(4) -0.003(4) C(24) 0.038(4) 0.043(4) 0.040(4) -0.006(3) 0.006(3) 0.004(3) C(25) 0.033(4) 0.032(3) 0.029(3) -0.004(3) 0.001(3) -0.004(3) C(26) 0.039(4) 0.029(3) 0.030(3) -0.001(3) 0.004(3) -0.002(3) C(27) 0.028(3) 0.032(3) 0.025(3) 0.003(3) 0.004(3) 0.002(3) C(28) 0.032(4) 0.037(4) 0.042(4) -0.002(3) 0.001(3) 0.006(3) C(29) 0.023(4) 0.053(4) 0.044(4) 0.000(3) 0.003(3) 0.008(4) C(30) 0.036(4) 0.050(4) 0.032(4) 0.010(3) -0.002(3) 0.009(3) C(31) 0.055(5) 0.034(4) 0.034(4) 0.006(3) 0.004(3) 0.009(3) C(32) 0.030(4) 0.042(4) 0.034(4) 0.003(3) 0.005(3) 0.010(3) C(33) 0.026(3) 0.022(3) 0.035(3) 0.004(3) -0.001(3) 0.002(3) C(34) 0.027(3) 0.031(3) 0.035(4) 0.000(3) -0.001(3) 0.002(3) C(35) 0.029(4) 0.048(4) 0.041(4) 0.004(3) 0.001(3) 0.002(3) C(36) 0.034(4) 0.049(4) 0.058(5) -0.011(3) -0.000(4) 0.005(4) C(37) 0.046(4) 0.040(4) 0.056(5) -0.009(3) 0.007(4) -0.005(4) C(38) 0.040(4) 0.031(3) 0.045(4) -0.007(3) 0.008(3) -0.005(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # 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 Ni(1) S(1) 2.253(2) yes . . Ni(1) S(2) 2.246(2) yes . . Ni(1) P(1) 2.166(2) yes . . Ni(1) P(2) 2.166(2) yes . . S(1) Si(1) 2.127(2) yes . . S(2) Si(2) 2.131(2) yes . . P(1) C(13) 1.828(6) yes . . P(1) C(19) 1.821(6) yes . . P(1) C(25) 1.855(6) yes . . P(2) C(26) 1.821(6) yes . . P(2) C(27) 1.814(6) yes . . P(2) C(33) 1.824(6) yes . . Si(1) C(1) 1.875(7) yes . . Si(1) C(2) 1.867(7) yes . . Si(1) C(3) 1.913(6) yes . . Si(2) C(7) 1.863(7) yes . . Si(2) C(8) 1.868(7) yes . . Si(2) C(9) 1.909(6) yes . . C(3) C(4) 1.53(1) yes . . C(3) C(5) 1.521(9) yes . . C(3) C(6) 1.51(1) yes . . C(9) C(10) 1.52(1) yes . . C(9) C(11) 1.534(9) yes . . C(9) C(12) 1.53(1) yes . . C(13) C(14) 1.392(9) yes . . C(13) C(18) 1.380(9) yes . . C(14) C(15) 1.39(1) yes . . C(15) C(16) 1.37(1) yes . . C(16) C(17) 1.38(1) yes . . C(17) C(18) 1.38(1) yes . . C(19) C(20) 1.399(9) yes . . C(19) C(24) 1.382(9) yes . . C(20) C(21) 1.38(1) yes . . C(21) C(22) 1.38(1) yes . . C(22) C(23) 1.37(1) yes . . C(23) C(24) 1.38(1) yes . . C(25) C(26) 1.531(8) yes . . C(27) C(28) 1.387(9) yes . . C(27) C(32) 1.371(8) yes . . C(28) C(29) 1.370(9) yes . . C(29) C(30) 1.367(9) yes . . C(30) C(31) 1.40(1) yes . . C(31) C(32) 1.371(9) yes . . C(33) C(34) 1.389(9) yes . . C(33) C(38) 1.396(8) yes . . C(34) C(35) 1.379(9) yes . . C(35) C(36) 1.38(1) yes . . C(36) C(37) 1.37(1) yes . . C(37) C(38) 1.38(1) yes . . 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 S(1) Ni(1) S(2) 99.67(6) yes . . . S(1) Ni(1) P(1) 174.62(7) yes . . . S(1) Ni(1) P(2) 89.82(6) yes . . . S(2) Ni(1) P(1) 84.99(6) yes . . . S(2) Ni(1) P(2) 170.47(7) yes . . . P(1) Ni(1) P(2) 85.58(6) yes . . . Si(1) S(1) Ni(1) 106.39(8) yes . . . Si(2) S(2) Ni(1) 108.28(8) yes . . . C(13) P(1) C(19) 108.6(3) yes . . . C(13) P(1) C(25) 102.9(3) yes . . . C(13) P(1) Ni(1) 116.8(2) yes . . . C(19) P(1) C(25) 100.9(3) yes . . . C(19) P(1) Ni(1) 114.9(2) yes . . . C(25) P(1) Ni(1) 110.9(2) yes . . . C(26) P(2) C(27) 104.8(3) yes . . . C(26) P(2) C(33) 104.9(3) yes . . . C(26) P(2) Ni(1) 107.4(2) yes . . . C(27) P(2) C(33) 105.2(3) yes . . . C(27) P(2) Ni(1) 124.3(2) yes . . . C(33) P(2) Ni(1) 108.7(2) yes . . . C(1) Si(1) C(2) 106.0(3) yes . . . C(1) Si(1) C(3) 109.4(3) yes . . . C(1) Si(1) S(1) 112.0(2) yes . . . C(2) Si(1) C(3) 107.2(3) yes . . . C(2) Si(1) S(1) 115.0(3) yes . . . C(3) Si(1) S(1) 107.1(2) yes . . . C(7) Si(2) C(8) 106.9(3) yes . . . C(7) Si(2) C(9) 111.5(3) yes . . . C(7) Si(2) S(2) 110.3(3) yes . . . C(8) Si(2) C(9) 107.2(3) yes . . . C(8) Si(2) S(2) 114.9(3) yes . . . C(9) Si(2) S(2) 106.1(2) yes . . . C(4) C(3) C(5) 108.0(5) yes . . . C(4) C(3) C(6) 109.0(6) yes . . . C(4) C(3) Si(1) 109.5(4) yes . . . C(5) C(3) C(6) 109.3(6) yes . . . C(5) C(3) Si(1) 109.2(5) yes . . . C(6) C(3) Si(1) 111.8(5) yes . . . C(10) C(9) C(11) 109.2(5) yes . . . C(10) C(9) C(12) 107.7(6) yes . . . C(10) C(9) Si(2) 110.6(4) yes . . . C(11) C(9) C(12) 108.8(6) yes . . . C(11) C(9) Si(2) 109.8(5) yes . . . C(12) C(9) Si(2) 110.6(4) yes . . . C(14) C(13) C(18) 119.4(6) yes . . . C(14) C(13) P(1) 118.8(5) yes . . . C(18) C(13) P(1) 121.5(5) yes . . . C(15) C(14) C(13) 120.1(6) yes . . . C(16) C(15) C(14) 120.5(7) yes . . . C(17) C(16) C(15) 119.1(7) yes . . . C(18) C(17) C(16) 121.0(7) yes . . . C(13) C(18) C(17) 119.8(6) yes . . . C(20) C(19) C(24) 119.3(6) yes . . . C(20) C(19) P(1) 120.3(5) yes . . . C(24) C(19) P(1) 120.0(5) yes . . . C(21) C(20) C(19) 119.2(6) yes . . . C(22) C(21) C(20) 121.3(7) yes . . . C(23) C(22) C(21) 119.1(7) yes . . . C(24) C(23) C(22) 120.8(7) yes . . . C(19) C(24) C(23) 120.2(6) yes . . . C(26) C(25) P(1) 107.2(4) yes . . . P(2) C(26) C(25) 106.9(4) yes . . . C(28) C(27) C(32) 119.0(6) yes . . . C(28) C(27) P(2) 118.2(4) yes . . . C(32) C(27) P(2) 122.8(5) yes . . . C(29) C(28) C(27) 120.6(6) yes . . . C(30) C(29) C(28) 120.5(6) yes . . . C(31) C(30) C(29) 119.1(6) yes . . . C(32) C(31) C(30) 120.1(6) yes . . . C(27) C(32) C(31) 120.7(6) yes . . . C(34) C(33) C(38) 118.8(5) yes . . . C(34) C(33) P(2) 118.9(4) yes . . . C(38) C(33) P(2) 122.2(5) yes . . . C(35) C(34) C(33) 120.6(6) yes . . . C(36) C(35) C(34) 120.1(6) yes . . . C(37) C(36) C(35) 119.9(7) yes . . . C(38) C(37) C(36) 120.6(6) yes . . . C(33) C(38) C(37) 120.0(6) yes . . . 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 S(2) Ni(1) S(1) Si(1) 61.34(8) yes . . . . P(2) Ni(1) S(1) Si(1) -117.74(8) yes . . . . S(1) Ni(1) S(2) Si(2) 61.72(8) yes . . . . P(1) Ni(1) S(2) Si(2) -115.56(8) yes . . . . S(2) Ni(1) P(1) C(13) 67.8(2) yes . . . . S(2) Ni(1) P(1) C(19) -61.2(2) yes . . . . S(2) Ni(1) P(1) C(25) -174.8(2) yes . . . . P(2) Ni(1) P(1) C(13) -113.6(2) yes . . . . P(2) Ni(1) P(1) C(19) 117.4(2) yes . . . . P(2) Ni(1) P(1) C(25) 3.8(2) yes . . . . S(1) Ni(1) P(2) C(26) 155.7(2) yes . . . . S(1) Ni(1) P(2) C(27) 33.1(2) yes . . . . S(1) Ni(1) P(2) C(33) -91.4(2) yes . . . . P(1) Ni(1) P(2) C(26) -27.1(2) yes . . . . P(1) Ni(1) P(2) C(27) -149.7(2) yes . . . . P(1) Ni(1) P(2) C(33) 85.8(2) yes . . . . Ni(1) S(1) Si(1) C(1) 37.9(3) yes . . . . Ni(1) S(1) Si(1) C(2) -83.2(3) yes . . . . Ni(1) S(1) Si(1) C(3) 157.9(2) yes . . . . Ni(1) S(2) Si(2) C(7) 44.6(3) yes . . . . Ni(1) S(2) Si(2) C(8) -76.3(3) yes . . . . Ni(1) S(2) Si(2) C(9) 165.5(2) yes . . . . Ni(1) P(1) C(13) C(14) 74.4(5) yes . . . . Ni(1) P(1) C(13) C(18) -99.6(5) yes . . . . C(19) P(1) C(13) C(14) -153.7(4) yes . . . . C(19) P(1) C(13) C(18) 32.4(6) yes . . . . C(25) P(1) C(13) C(14) -47.3(5) yes . . . . C(25) P(1) C(13) C(18) 138.7(5) yes . . . . Ni(1) P(1) C(19) C(20) 173.8(5) yes . . . . Ni(1) P(1) C(19) C(24) -13.5(6) yes . . . . C(13) P(1) C(19) C(20) 40.9(6) yes . . . . C(13) P(1) C(19) C(24) -146.4(5) yes . . . . C(25) P(1) C(19) C(20) -66.8(5) yes . . . . C(25) P(1) C(19) C(24) 105.9(5) yes . . . . Ni(1) P(1) C(25) C(26) 25.0(4) yes . . . . C(13) P(1) C(25) C(26) 150.6(4) yes . . . . C(19) P(1) C(25) C(26) -97.2(4) yes . . . . Ni(1) P(2) C(26) C(25) 49.9(4) yes . . . . C(27) P(2) C(26) C(25) -176.1(3) yes . . . . C(33) P(2) C(26) C(25) -65.6(4) yes . . . . Ni(1) P(2) C(27) C(28) 64.6(5) yes . . . . Ni(1) P(2) C(27) C(32) -116.7(5) yes . . . . C(26) P(2) C(27) C(28) -59.1(5) yes . . . . C(26) P(2) C(27) C(32) 119.5(5) yes . . . . C(33) P(2) C(27) C(28) -169.4(4) yes . . . . C(33) P(2) C(27) C(32) 9.2(5) yes . . . . Ni(1) P(2) C(33) C(34) 34.0(5) yes . . . . Ni(1) P(2) C(33) C(38) -142.3(5) yes . . . . C(26) P(2) C(33) C(34) 148.6(4) yes . . . . C(26) P(2) C(33) C(38) -27.8(5) yes . . . . C(27) P(2) C(33) C(34) -101.1(5) yes . . . . C(27) P(2) C(33) C(38) 82.5(5) yes . . . . S(1) Si(1) C(3) C(4) -177.8(4) yes . . . . S(1) Si(1) C(3) C(5) 64.2(5) yes . . . . S(1) Si(1) C(3) C(6) -57.0(5) yes . . . . C(1) Si(1) C(3) C(4) -56.2(5) yes . . . . C(1) Si(1) C(3) C(5) -174.2(4) yes . . . . C(1) Si(1) C(3) C(6) 64.7(5) yes . . . . C(2) Si(1) C(3) C(4) 58.3(5) yes . . . . C(2) Si(1) C(3) C(5) -59.7(5) yes . . . . C(2) Si(1) C(3) C(6) 179.2(4) yes . . . . S(2) Si(2) C(9) C(10) 167.8(4) yes . . . . S(2) Si(2) C(9) C(11) 47.1(5) yes . . . . S(2) Si(2) C(9) C(12) -73.0(5) yes . . . . C(7) Si(2) C(9) C(10) -72.1(5) yes . . . . C(7) Si(2) C(9) C(11) 167.3(4) yes . . . . C(7) Si(2) C(9) C(12) 47.1(5) yes . . . . C(8) Si(2) C(9) C(10) 44.5(5) yes . . . . C(8) Si(2) C(9) C(11) -76.1(5) yes . . . . C(8) Si(2) C(9) C(12) 163.8(4) yes . . . . P(1) C(13) C(14) C(15) -174.6(5) yes . . . . C(18) C(13) C(14) C(15) -0.5(9) yes . . . . P(1) C(13) C(18) C(17) 175.2(5) yes . . . . C(14) C(13) C(18) C(17) 1.3(9) yes . . . . C(13) C(14) C(15) C(16) 0(1) yes . . . . C(14) C(15) C(16) C(17) 0(1) yes . . . . C(15) C(16) C(17) C(18) 1(1) yes . . . . C(16) C(17) C(18) C(13) -1(1) yes . . . . P(1) C(19) C(20) C(21) 173.1(6) yes . . . . C(24) C(19) C(20) C(21) 0(1) yes . . . . P(1) C(19) C(24) C(23) -172.1(6) yes . . . . C(20) C(19) C(24) C(23) 0.7(9) yes . . . . C(19) C(20) C(21) C(22) 0(1) yes . . . . C(20) C(21) C(22) C(23) 0(1) yes . . . . C(21) C(22) C(23) C(24) 1(1) yes . . . . C(22) C(23) C(24) C(19) -1(1) yes . . . . P(1) C(25) C(26) P(2) -45.5(5) yes . . . . P(2) C(27) C(28) C(29) 178.4(5) yes . . . . C(32) C(27) C(28) C(29) -0.3(9) yes . . . . P(2) C(27) C(32) C(31) -178.3(5) yes . . . . C(28) C(27) C(32) C(31) 0.4(9) yes . . . . C(27) C(28) C(29) C(30) 0(1) yes . . . . C(28) C(29) C(30) C(31) -1(1) yes . . . . C(29) C(30) C(31) C(32) 1(1) yes . . . . C(30) C(31) C(32) C(27) -1(1) yes . . . . P(2) C(33) C(34) C(35) -176.9(5) yes . . . . C(38) C(33) C(34) C(35) -0.4(9) yes . . . . P(2) C(33) C(38) C(37) 176.4(5) yes . . . . C(34) C(33) C(38) C(37) -0.0(9) yes . . . . C(33) C(34) C(35) C(36) 0(1) yes . . . . C(34) C(35) C(36) C(37) 0(1) yes . . . . C(35) C(36) C(37) C(38) 0(1) yes . . . . C(36) C(37) C(38) C(33) 0(1) yes . . . . 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 Ni(1) S(1) 2.253(2) yes . 55501 Ni(1) S(2) 2.246(2) yes . 55501 Ni(1) Si(1) 3.508(2) yes . 55501 Ni(1) Si(2) 3.548(2) yes . 55501 Ni(1) C(13) 3.406(6) yes . 55501 Ni(1) C(19) 3.366(6) yes . 55501 Ni(1) C(24) 3.529(7) yes . 55501 Ni(1) C(25) 3.317(6) yes . 55501 Ni(1) C(26) 3.219(6) yes . 55501 Ni(1) C(27) 3.523(6) yes . 55501 Ni(1) C(33) 3.248(6) yes . 55501 Ni(1) C(34) 3.425(6) yes . 55501 S(1) Ni(1) 2.253(2) yes . 55501 S(1) S(2) 3.438(2) yes . 55501 S(1) P(2) 3.120(2) yes . 55501 S(1) C(1) 3.321(8) yes . 55501 S(1) C(2) 3.370(6) yes . 55501 S(1) C(3) 3.252(6) yes . 55501 S(1) C(5) 3.590(7) yes . 55501 S(1) C(6) 3.550(8) yes . 55501 S(1) C(27) 3.434(6) yes . 55501 S(2) Ni(1) 2.246(2) yes . 55501 S(2) S(1) 3.438(2) yes . 55501 S(2) P(1) 2.981(2) yes . 55501 S(2) Si(2) 2.131(2) yes . 55501 S(2) C(7) 3.281(8) yes . 55501 S(2) C(8) 3.375(7) yes . 55501 S(2) C(9) 3.231(7) yes . 55501 S(2) C(11) 3.373(7) yes . 55501 S(2) C(13) 3.566(6) yes . 55501 S(2) C(19) 3.415(6) yes . 55501 S(2) C(24) 3.430(7) yes . 55501 P(1) S(2) 2.981(2) yes . 55501 P(1) P(2) 2.943(2) yes . 55501 P(1) C(14) 2.781(7) yes . 55501 P(1) C(18) 2.808(7) yes . 55501 P(1) C(20) 2.800(7) yes . 55501 P(1) C(24) 2.783(7) yes . 55501 P(1) C(25) 1.855(6) yes . 55501 P(1) C(26) 2.732(6) yes . 55501 P(2) S(1) 3.120(2) yes . 55501 P(2) P(1) 2.943(2) yes . 55501 P(2) C(25) 2.698(6) yes . 55501 P(2) C(28) 2.756(6) yes . 55501 P(2) C(32) 2.805(6) yes . 55501 P(2) C(34) 2.777(6) yes . 55501 P(2) C(38) 2.827(6) yes . 55501 Si(1) Ni(1) 3.508(2) yes . 55501 Si(1) Ni(1) 3.548(2) yes . 55505 Si(1) S(1) 3.548(2) yes . 55505 Si(1) S(2) 3.548(2) yes . 55505 Si(1) P(1) 3.548(2) yes . 55505 Si(1) P(2) 3.548(2) yes . 55505 Si(1) Si(1) 3.548(3) yes . 55505 Si(1) Si(2) 3.548(2) yes . 55505 Si(1) C(1) 3.548(8) yes . 55505 Si(1) C(2) 3.548(7) yes . 55505 Si(1) C(3) 1.913(6) yes . 55501 Si(1) C(3) 3.548(7) yes . 55505 Si(1) C(4) 2.818(7) yes . 55501 Si(1) C(4) 3.548(7) yes . 55505 Si(1) C(5) 2.809(7) yes . 55501 Si(1) C(5) 3.548(8) yes . 55505 Si(1) C(6) 2.846(8) yes . 55501 Si(1) C(6) 3.548(8) yes . 55505 Si(1) C(7) 3.548(7) yes . 55505 Si(1) C(8) 3.548(8) yes . 55505 Si(1) C(9) 3.548(6) yes . 55505 Si(1) C(10) 3.548(7) yes . 55505 Si(1) C(11) 3.548(7) yes . 55505 Si(1) C(12) 3.548(7) yes . 55505 Si(1) C(13) 3.548(6) yes . 55505 Si(1) C(14) 3.548(7) yes . 55505 Si(1) C(15) 3.548(8) yes . 55505 Si(1) C(16) 3.548(8) yes . 55505 Si(1) C(17) 3.548(8) yes . 55505 Si(1) C(18) 3.548(7) yes . 55505 Si(1) C(19) 3.548(6) yes . 55505 Si(1) C(20) 3.548(7) yes . 55505 Si(1) C(21) 3.548(8) yes . 55505 Si(1) C(22) 3.548(8) yes . 55505 Si(1) C(23) 3.548(7) yes . 55505 Si(1) C(24) 3.548(7) yes . 55505 Si(1) C(25) 3.548(6) yes . 55505 Si(1) C(26) 3.548(6) yes . 55505 Si(1) C(27) 3.548(6) yes . 55505 Si(1) C(28) 3.548(7) yes . 55505 Si(1) C(29) 3.548(7) yes . 55505 Si(1) C(30) 3.548(7) yes . 55505 Si(1) C(31) 3.548(7) yes . 55505 Si(1) C(32) 3.548(7) yes . 55505 Si(1) C(33) 3.548(6) yes . 55505 Si(1) C(34) 3.548(6) yes . 55505 Si(1) C(35) 3.548(7) yes . 55505 Si(1) C(36) 3.548(7) yes . 55505 Si(1) C(37) 3.548(7) yes . 55505 Si(1) C(38) 3.548(7) yes . 55505 Si(2) Ni(1) 3.548(2) yes . 55501 Si(2) S(2) 2.131(2) yes . 55501 Si(2) C(9) 1.909(6) yes . 55501 Si(2) C(10) 2.829(7) yes . 55501 Si(2) C(11) 2.825(6) yes . 55501 Si(2) C(12) 2.832(7) yes . 55501 C(1) S(1) 3.321(8) yes . 55501 C(1) C(2) 2.99(1) yes . 55501 C(1) C(3) 3.093(9) yes . 55501 C(1) C(4) 3.41(1) yes . 55501 C(1) C(6) 3.55(1) yes . 55501 C(2) Ni(1) 1.945(7) yes . 55505 C(2) S(1) 3.370(6) yes . 55501 C(2) S(1) 1.945(7) yes . 55505 C(2) S(2) 1.945(7) yes . 55505 C(2) P(1) 1.945(7) yes . 55505 C(2) P(2) 1.945(7) yes . 55505 C(2) Si(1) 1.945(7) yes . 55505 C(2) Si(2) 1.945(7) yes . 55505 C(2) C(1) 2.99(1) yes . 55501 C(2) C(1) 1.94(1) yes . 55505 C(2) C(2) 1.94(1) yes . 55505 C(2) C(3) 3.042(9) yes . 55501 C(2) C(3) 1.945(9) yes . 55505 C(2) C(4) 3.38(1) yes . 55501 C(2) C(4) 1.94(1) yes . 55505 C(2) C(5) 3.38(1) yes . 55501 C(2) C(5) 1.94(1) yes . 55505 C(2) C(6) 1.94(1) yes . 55505 C(2) C(7) 1.94(1) yes . 55505 C(2) C(8) 3.53(1) yes . 55501 C(2) C(8) 1.94(1) yes . 55505 C(2) C(9) 1.945(9) yes . 55505 C(2) C(10) 1.94(1) yes . 55505 C(2) C(11) 1.94(1) yes . 55505 C(2) C(12) 1.94(1) yes . 55505 C(2) C(13) 1.945(9) yes . 55505 C(2) C(14) 1.945(9) yes . 55505 C(2) C(15) 1.94(1) yes . 55505 C(2) C(16) 1.94(1) yes . 55505 C(2) C(17) 1.94(1) yes . 55505 C(2) C(18) 1.94(1) yes . 55505 C(2) C(19) 1.945(9) yes . 55505 C(2) C(20) 1.94(1) yes . 55505 C(2) C(21) 1.94(1) yes . 55505 C(2) C(22) 1.94(1) yes . 55505 C(2) C(23) 1.94(1) yes . 55505 C(2) C(24) 1.94(1) yes . 55505 C(2) C(25) 1.945(9) yes . 55505 C(2) C(26) 1.945(9) yes . 55505 C(2) C(27) 1.945(9) yes . 55505 C(2) C(28) 1.945(9) yes . 55505 C(2) C(29) 1.94(1) yes . 55505 C(2) C(30) 1.945(9) yes . 55505 C(2) C(31) 1.945(9) yes . 55505 C(2) C(32) 1.945(9) yes . 55505 C(2) C(33) 1.945(9) yes . 55505 C(2) C(34) 1.945(9) yes . 55505 C(2) C(35) 1.94(1) yes . 55505 C(2) C(36) 1.94(1) yes . 55505 C(2) C(37) 1.94(1) yes . 55505 C(2) C(38) 1.94(1) yes . 55505 C(3) S(1) 3.252(6) yes . 55501 C(3) Si(1) 1.913(6) yes . 55501 C(3) C(1) 3.093(9) yes . 55501 C(3) C(2) 3.042(9) yes . 55501 C(4) Si(1) 2.818(7) yes . 55501 C(4) C(1) 3.41(1) yes . 55501 C(4) C(2) 3.38(1) yes . 55501 C(4) C(5) 2.47(1) yes . 55501 C(4) C(6) 2.47(1) yes . 55501 C(5) S(1) 3.590(7) yes . 55501 C(5) Si(1) 2.809(7) yes . 55501 C(5) C(2) 3.38(1) yes . 55501 C(5) C(4) 2.47(1) yes . 55501 C(5) C(6) 2.47(1) yes . 55501 C(6) S(1) 3.550(8) yes . 55501 C(6) Si(1) 2.846(8) yes . 55501 C(6) C(1) 3.55(1) yes . 55501 C(6) C(4) 2.47(1) yes . 55501 C(6) C(5) 2.47(1) yes . 55501 C(7) S(2) 3.281(8) yes . 55501 C(7) C(8) 3.00(1) yes . 55501 C(7) C(9) 3.117(9) yes . 55501 C(7) C(12) 3.38(1) yes . 55501 C(8) S(2) 3.375(7) yes . 55501 C(8) C(2) 3.53(1) yes . 55501 C(8) C(7) 3.00(1) yes . 55501 C(8) C(9) 3.04(1) yes . 55501 C(8) C(10) 3.25(1) yes . 55501 C(8) C(11) 3.59(1) yes . 55501 C(9) S(2) 3.231(7) yes . 55501 C(9) Si(2) 1.909(6) yes . 55501 C(9) C(7) 3.117(9) yes . 55501 C(9) C(8) 3.04(1) yes . 55501 C(10) Si(2) 2.829(7) yes . 55501 C(10) C(8) 3.25(1) yes . 55501 C(10) C(11) 2.49(1) yes . 55501 C(10) C(12) 2.46(1) yes . 55501 C(11) S(2) 3.373(7) yes . 55501 C(11) Si(2) 2.825(6) yes . 55501 C(11) C(8) 3.59(1) yes . 55501 C(11) C(10) 2.49(1) yes . 55501 C(11) C(12) 2.49(1) yes . 55501 C(12) Si(2) 2.832(7) yes . 55501 C(12) C(7) 3.38(1) yes . 55501 C(12) C(10) 2.46(1) yes . 55501 C(12) C(11) 2.49(1) yes . 55501 C(12) C(17) 3.58(1) yes . 55501 C(13) Ni(1) 3.406(6) yes . 55501 C(13) S(2) 3.566(6) yes . 55501 C(13) C(15) 2.41(1) yes . 55501 C(13) C(16) 2.78(1) yes . 55501 C(13) C(17) 2.392(9) yes . 55501 C(13) C(19) 2.964(9) yes . 55501 C(13) C(20) 3.312(9) yes . 55501 C(13) C(25) 2.880(9) yes . 55501 C(14) P(1) 2.781(7) yes . 55501 C(14) C(16) 2.40(1) yes . 55501 C(14) C(17) 2.75(1) yes . 55501 C(14) C(18) 2.393(9) yes . 55501 C(14) C(25) 3.202(9) yes . 55501 C(15) C(13) 2.41(1) yes . 55501 C(15) C(17) 2.38(1) yes . 55501 C(15) C(18) 2.77(1) yes . 55501 C(16) C(13) 2.78(1) yes . 55501 C(16) C(14) 2.40(1) yes . 55501 C(16) C(18) 2.41(1) yes . 55501 C(16) C(30) 3.551(9) yes . 65504 C(17) C(12) 3.58(1) yes . 55501 C(17) C(13) 2.392(9) yes . 55501 C(17) C(14) 2.75(1) yes . 55501 C(17) C(15) 2.38(1) yes . 55501 C(18) P(1) 2.808(7) yes . 55501 C(18) C(14) 2.393(9) yes . 55501 C(18) C(15) 2.77(1) yes . 55501 C(18) C(16) 2.41(1) yes . 55501 C(18) C(19) 3.277(9) yes . 55501 C(18) C(20) 3.33(1) yes . 55501 C(19) Ni(1) 3.366(6) yes . 55501 C(19) S(2) 3.415(6) yes . 55501 C(19) C(13) 2.964(9) yes . 55501 C(19) C(18) 3.277(9) yes . 55501 C(19) C(21) 2.40(1) yes . 55501 C(19) C(22) 2.78(1) yes . 55501 C(19) C(23) 2.39(1) yes . 55501 C(19) C(25) 2.834(8) yes . 55501 C(20) P(1) 2.800(7) yes . 55501 C(20) C(13) 3.312(9) yes . 55501 C(20) C(18) 3.33(1) yes . 55501 C(20) C(22) 2.40(1) yes . 55501 C(20) C(23) 2.76(1) yes . 55501 C(20) C(24) 2.401(9) yes . 55501 C(20) C(25) 3.365(9) yes . 55501 C(21) C(19) 2.40(1) yes . 55501 C(21) C(23) 2.37(1) yes . 55501 C(21) C(24) 2.75(1) yes . 55501 C(22) C(19) 2.78(1) yes . 55501 C(22) C(20) 2.40(1) yes . 55501 C(22) C(24) 2.39(1) yes . 55501 C(23) C(19) 2.39(1) yes . 55501 C(23) C(20) 2.76(1) yes . 55501 C(23) C(21) 2.37(1) yes . 55501 C(24) Ni(1) 3.529(7) yes . 55501 C(24) S(2) 3.430(7) yes . 55501 C(24) P(1) 2.783(7) yes . 55501 C(24) C(20) 2.401(9) yes . 55501 C(24) C(21) 2.75(1) yes . 55501 C(24) C(22) 2.39(1) yes . 55501 C(25) Ni(1) 3.317(6) yes . 55501 C(25) P(1) 1.855(6) yes . 55501 C(25) P(2) 2.698(6) yes . 55501 C(25) C(13) 2.880(9) yes . 55501 C(25) C(14) 3.202(9) yes . 55501 C(25) C(19) 2.834(8) yes . 55501 C(25) C(20) 3.365(9) yes . 55501 C(25) C(33) 3.255(8) yes . 55501 C(25) C(34) 3.519(8) yes . 55504 C(25) C(38) 3.438(9) yes . 55501 C(26) Ni(1) 3.219(6) yes . 55501 C(26) P(1) 2.732(6) yes . 55501 C(26) C(27) 2.881(8) yes . 55501 C(26) C(28) 3.317(9) yes . 55501 C(26) C(33) 2.889(8) yes . 55501 C(26) C(38) 3.167(9) yes . 55501 C(27) Ni(1) 3.523(6) yes . 55501 C(27) S(1) 3.434(6) yes . 55501 C(27) C(26) 2.881(8) yes . 55501 C(27) C(29) 2.396(9) yes . 55501 C(27) C(30) 2.771(9) yes . 55501 C(27) C(31) 2.382(9) yes . 55501 C(27) C(33) 2.890(8) yes . 55501 C(28) P(2) 2.756(6) yes . 55501 C(28) C(26) 3.317(9) yes . 55501 C(28) C(30) 2.377(9) yes . 55501 C(28) C(31) 2.742(9) yes . 55501 C(28) C(32) 2.376(9) yes . 55501 C(29) C(27) 2.396(9) yes . 55501 C(29) C(31) 2.38(1) yes . 55501 C(29) C(32) 2.749(9) yes . 55501 C(30) C(16) 3.551(9) yes . 45404 C(30) C(27) 2.771(9) yes . 55501 C(30) C(28) 2.377(9) yes . 55501 C(30) C(32) 2.398(9) yes . 55501 C(31) C(27) 2.382(9) yes . 55501 C(31) C(28) 2.742(9) yes . 55501 C(31) C(29) 2.38(1) yes . 55501 C(32) P(2) 2.805(6) yes . 55501 C(32) C(28) 2.376(9) yes . 55501 C(32) C(29) 2.749(9) yes . 55501 C(32) C(30) 2.398(9) yes . 55501 C(32) C(33) 3.104(8) yes . 55501 C(33) Ni(1) 3.248(6) yes . 55501 C(33) C(25) 3.255(8) yes . 55501 C(33) C(26) 2.889(8) yes . 55501 C(33) C(27) 2.890(8) yes . 55501 C(33) C(32) 3.104(8) yes . 55501 C(33) C(35) 2.404(9) yes . 55501 C(33) C(36) 2.779(9) yes . 55501 C(33) C(37) 2.408(9) yes . 55501 C(34) Ni(1) 3.425(6) yes . 55501 C(34) P(2) 2.777(6) yes . 55501 C(34) C(25) 3.519(8) yes . 55404 C(34) C(36) 2.391(9) yes . 55501 C(34) C(37) 2.756(9) yes . 55501 C(34) C(38) 2.396(9) yes . 55501 C(35) C(33) 2.404(9) yes . 55501 C(35) C(37) 2.38(1) yes . 55501 C(35) C(38) 2.76(1) yes . 55501 C(36) C(33) 2.779(9) yes . 55501 C(36) C(34) 2.391(9) yes . 55501 C(36) C(38) 2.39(1) yes . 55501 C(37) C(33) 2.408(9) yes . 55501 C(37) C(34) 2.756(9) yes . 55501 C(37) C(35) 2.38(1) yes . 55501 C(38) P(2) 2.827(6) yes . 55501 C(38) C(25) 3.438(9) yes . 55501 C(38) C(26) 3.167(9) yes . 55501 C(38) C(34) 2.396(9) yes . 55501 C(38) C(35) 2.76(1) yes . 55501 C(38) C(36) 2.39(1) yes . 55501 #============================================================================== # 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 #============================================================================== #===END data_CpTiClS2Ni(dppe) _database_code_depnum_ccdc_archive 'CCDC 227198' _audit_creation_date 2004-03-03 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C31 H29 Cl Ni P2 S2 Ti ' _chemical_formula_moiety CpTiClS2Ni(dppe) _chemical_formula_weight 669.69 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 11.898(5) _cell_length_b 18.473(8) _cell_length_c 14.368(6) _cell_angle_alpha 90 _cell_angle_beta 112.188(5) _cell_angle_gamma 90 _cell_volume 2924.0(22) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10450 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376.00 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.779 _exptl_absorpt_correction_T_max 0.938 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 23085 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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 6540 _reflns_number_gt 5204 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0690 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6540 _refine_ls_number_parameters 372 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.70 _refine_diff_density_min -0.63 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ti Ti 0.278 0.446 ; 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 Ni(1) Ni 0.33778(2) 0.239000(10) 0.59409(2) 0.01391(7) Uani 1.00 1 d . . . Ti(1) Ti 0.33157(3) 0.39169(2) 0.57755(3) 0.01770(10) Uani 1.00 1 d . . . Cl(1) Cl 0.48972(5) 0.43490(4) 0.72023(5) 0.0347(2) Uani 1.00 1 d . . . S(1) S 0.22997(4) 0.31851(3) 0.64132(4) 0.01840(13) Uani 1.00 1 d . . . S(2) S 0.41958(5) 0.30994(3) 0.51291(4) 0.0222(1) Uani 1.00 1 d . . . P(1) P 0.26139(4) 0.16153(3) 0.66601(4) 0.01490(13) Uani 1.00 1 d . . . P(2) P 0.42705(4) 0.14926(3) 0.55340(4) 0.01450(13) Uani 1.00 1 d . . . C(1) C 0.1434(2) 0.4508(1) 0.4860(2) 0.0330(7) Uani 1.00 1 d . . . C(2) C 0.1990(2) 0.4321(1) 0.4187(2) 0.0306(6) Uani 1.00 1 d . . . C(3) C 0.3067(2) 0.4738(1) 0.4440(2) 0.0337(7) Uani 1.00 1 d . . . C(4) C 0.3189(3) 0.5167(1) 0.5270(2) 0.0398(7) Uani 1.00 1 d . . . C(5) C 0.2182(3) 0.5017(1) 0.5544(2) 0.0405(8) Uani 1.00 1 d . . . C(6) C 0.1078(2) 0.13556(12) 0.5858(2) 0.0188(5) Uani 1.00 1 d . . . C(7) C 0.0547(2) 0.16553(13) 0.4899(2) 0.0265(6) Uani 1.00 1 d . . . C(8) C -0.0595(2) 0.1420(2) 0.4252(2) 0.0369(7) Uani 1.00 1 d . . . C(9) C -0.1190(2) 0.0896(2) 0.4565(2) 0.0379(7) Uani 1.00 1 d . . . C(10) C -0.0671(2) 0.0590(2) 0.5511(2) 0.0360(7) Uani 1.00 1 d . . . C(11) C 0.0464(2) 0.0817(1) 0.6160(2) 0.0274(6) Uani 1.00 1 d . . . C(12) C 0.2637(2) 0.17790(11) 0.7915(2) 0.0168(5) Uani 1.00 1 d . . . C(13) C 0.1583(2) 0.19498(12) 0.8076(2) 0.0208(6) Uani 1.00 1 d . . . C(14) C 0.1635(2) 0.20744(13) 0.9044(2) 0.0265(6) Uani 1.00 1 d . . . C(15) C 0.2729(2) 0.20374(13) 0.9853(2) 0.0281(6) Uani 1.00 1 d . . . C(16) C 0.3789(2) 0.18817(13) 0.9701(2) 0.0268(6) Uani 1.00 1 d . . . C(17) C 0.3738(2) 0.17555(12) 0.8734(2) 0.0218(6) Uani 1.00 1 d . . . C(18) C 0.3437(2) 0.07543(11) 0.6781(2) 0.0183(5) Uani 1.00 1 d . . . C(19) C 0.3607(2) 0.06481(11) 0.5788(2) 0.0180(5) Uani 1.00 1 d . . . C(20) C 0.5875(2) 0.14170(12) 0.6322(2) 0.0164(5) Uani 1.00 1 d . . . C(21) C 0.6534(2) 0.20146(12) 0.6824(2) 0.0217(6) Uani 1.00 1 d . . . C(22) C 0.7767(2) 0.19511(13) 0.7400(2) 0.0280(6) Uani 1.00 1 d . . . C(23) C 0.8344(2) 0.1291(1) 0.7482(2) 0.0273(6) Uani 1.00 1 d . . . C(24) C 0.7695(2) 0.06926(13) 0.6995(2) 0.0251(6) Uani 1.00 1 d . . . C(25) C 0.6469(2) 0.07506(12) 0.6417(2) 0.0217(6) Uani 1.00 1 d . . . C(26) C 0.4171(2) 0.13554(11) 0.4246(2) 0.0172(5) Uani 1.00 1 d . . . C(27) C 0.5210(2) 0.13332(12) 0.4008(2) 0.0221(6) Uani 1.00 1 d . . . C(28) C 0.5094(2) 0.11942(13) 0.3016(2) 0.0283(6) Uani 1.00 1 d . . . C(29) C 0.3968(2) 0.10768(13) 0.2276(2) 0.0298(7) Uani 1.00 1 d . . . C(30) C 0.2929(2) 0.11112(13) 0.2503(2) 0.0276(6) Uani 1.00 1 d . . . C(31) C 0.3038(2) 0.12547(12) 0.3483(2) 0.0223(6) Uani 1.00 1 d . . . H(1) H 0.0640 0.4351 0.4821 0.0384 Uiso 1.00 1 c . . . H(2) H 0.1635 0.4022 0.3593 0.0345 Uiso 1.00 1 c . . . H(3) H 0.3580 0.4762 0.4053 0.0410 Uiso 1.00 1 c . . . H(4) H 0.3803 0.5534 0.5566 0.0441 Uiso 1.00 1 c . . . H(5) H 0.1992 0.5267 0.6060 0.0484 Uiso 1.00 1 c . . . H(6) H 0.0977 0.20240 0.4684 0.0301 Uiso 1.00 1 c . . . H(7) H -0.0966 0.1625 0.3583 0.0381 Uiso 1.00 1 c . . . H(8) H -0.1991 0.0740 0.4119 0.0429 Uiso 1.00 1 c . . . H(9) H -0.1099 0.0216 0.5721 0.0448 Uiso 1.00 1 c . . . H(10) H 0.0834 0.0603 0.6823 0.0342 Uiso 1.00 1 c . . . H(11) H 0.0814 0.19821 0.7509 0.0255 Uiso 1.00 1 c . . . H(12) H 0.0898 0.21850 0.9153 0.0352 Uiso 1.00 1 c . . . H(13) H 0.2757 0.21217 1.0528 0.0352 Uiso 1.00 1 c . . . H(14) H 0.4559 0.18623 1.0267 0.0305 Uiso 1.00 1 c . . . H(15) H 0.4476 0.16479 0.8623 0.0262 Uiso 1.00 1 c . . . H(16) H 0.4219 0.07794 0.7334 0.0219 Uiso 1.00 1 c . . . H(17) H 0.2968 0.03589 0.6895 0.0224 Uiso 1.00 1 c . . . H(18) H 0.2830 0.05558 0.5251 0.0218 Uiso 1.00 1 c . . . H(19) H 0.4150 0.02452 0.5839 0.0216 Uiso 1.00 1 c . . . H(20) H 0.6129 0.24772 0.6772 0.0253 Uiso 1.00 1 c . . . H(21) H 0.8223 0.23708 0.7749 0.0315 Uiso 1.00 1 c . . . H(22) H 0.9205 0.1249 0.7880 0.0319 Uiso 1.00 1 c . . . H(23) H 0.8100 0.02292 0.7056 0.0305 Uiso 1.00 1 c . . . H(24) H 0.6014 0.03284 0.6075 0.0263 Uiso 1.00 1 c . . . H(25) H 0.6004 0.14131 0.4530 0.0269 Uiso 1.00 1 c . . . H(26) H 0.5810 0.11840 0.2848 0.0371 Uiso 1.00 1 c . . . H(27) H 0.3897 0.09669 0.1596 0.0373 Uiso 1.00 1 c . . . H(28) H 0.2136 0.10373 0.1979 0.0307 Uiso 1.00 1 c . . . H(29) H 0.2314 0.12839 0.3640 0.0269 Uiso 1.00 1 c . . . 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 Ni(1) 0.01616(13) 0.01179(13) 0.01543(13) 0.00103(10) 0.00784(10) 0.00009(10) Ti(1) 0.0199(2) 0.0141(2) 0.0191(2) 0.0017(2) 0.0073(2) 0.0000(2) Cl(1) 0.0288(3) 0.0370(4) 0.0303(3) -0.0099(3) 0.0020(3) -0.0065(3) S(1) 0.0197(2) 0.0160(3) 0.0230(3) 0.0022(2) 0.0121(2) -0.0006(2) S(2) 0.0318(3) 0.0157(3) 0.0278(3) 0.0037(2) 0.0212(3) 0.0032(2) P(1) 0.0150(2) 0.0157(3) 0.0147(3) -0.0004(2) 0.0065(2) 0.0001(2) P(2) 0.0162(2) 0.0126(3) 0.0158(3) 0.0000(2) 0.0071(2) -0.0020(2) C(1) 0.0279(12) 0.033(2) 0.035(1) 0.0088(11) 0.0078(11) 0.0087(11) C(2) 0.0388(13) 0.0269(13) 0.0200(12) 0.0108(11) 0.0042(10) 0.0052(10) C(3) 0.040(1) 0.027(1) 0.035(1) 0.0061(11) 0.0149(11) 0.0128(11) C(4) 0.052(2) 0.0133(12) 0.044(2) 0.0024(11) 0.0073(13) 0.0036(11) C(5) 0.057(2) 0.027(1) 0.037(2) 0.0208(13) 0.0165(13) 0.0011(12) C(6) 0.0162(10) 0.0206(11) 0.0203(10) 0.0003(8) 0.0076(8) -0.0055(9) C(7) 0.0277(12) 0.0234(13) 0.0239(12) 0.0029(10) 0.0045(10) -0.0028(10) C(8) 0.0330(13) 0.033(2) 0.030(1) 0.0102(11) -0.0059(11) -0.0090(11) C(9) 0.0190(11) 0.040(2) 0.048(2) -0.0030(11) 0.0045(11) -0.0239(13) C(10) 0.0271(12) 0.039(2) 0.046(2) -0.0144(11) 0.0184(12) -0.0202(13) C(11) 0.0264(11) 0.032(1) 0.0272(12) -0.0078(10) 0.0145(10) -0.0090(10) C(12) 0.0219(10) 0.0140(10) 0.0166(10) -0.0022(8) 0.0096(8) 0.0001(8) C(13) 0.0206(10) 0.0212(12) 0.0224(11) -0.0015(9) 0.0102(9) -0.0004(9) C(14) 0.0353(13) 0.0216(12) 0.0316(13) -0.0003(10) 0.0228(11) -0.0016(10) C(15) 0.048(1) 0.0207(12) 0.0201(11) -0.0033(10) 0.0177(11) -0.0015(9) C(16) 0.0335(12) 0.0246(13) 0.0182(11) -0.0034(10) 0.0051(10) 0.0003(10) C(17) 0.0224(10) 0.0219(12) 0.0209(11) -0.0022(9) 0.0080(9) 0.0004(9) C(18) 0.0204(10) 0.0151(11) 0.0200(11) 0.0011(8) 0.0083(9) 0.0014(8) C(19) 0.0209(10) 0.0130(10) 0.0204(11) -0.0024(8) 0.0083(9) -0.0019(8) C(20) 0.0172(9) 0.0194(11) 0.0136(9) 0.0010(8) 0.0068(8) 0.0002(8) C(21) 0.0237(11) 0.0174(11) 0.0227(11) 0.0010(9) 0.0072(9) -0.0000(9) C(22) 0.0262(12) 0.0256(13) 0.0268(12) -0.0072(10) 0.0038(10) -0.0011(10) C(23) 0.0185(11) 0.034(1) 0.0269(12) 0.0010(10) 0.0060(10) 0.0059(11) C(24) 0.0215(11) 0.0253(13) 0.0297(12) 0.0074(9) 0.0110(10) 0.0024(10) C(25) 0.0230(11) 0.0197(12) 0.0234(11) 0.0009(9) 0.0100(9) -0.0034(9) C(26) 0.0243(10) 0.0114(10) 0.0176(10) -0.0013(8) 0.0097(9) -0.0024(8) C(27) 0.0252(11) 0.0211(12) 0.0219(11) -0.0000(9) 0.0109(9) 0.0004(9) C(28) 0.0368(13) 0.029(1) 0.0269(12) 0.0047(11) 0.0213(11) 0.0027(10) C(29) 0.051(2) 0.0231(13) 0.0193(11) -0.0000(11) 0.0179(11) -0.0010(10) C(30) 0.0351(13) 0.0229(13) 0.0192(11) -0.0061(10) 0.0038(10) -0.0020(9) C(31) 0.0258(11) 0.0199(12) 0.0212(11) -0.0035(9) 0.0089(9) -0.0009(9) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # 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 Ni(1) Ti(1) 2.8292(4) yes . . Ni(1) S(1) 2.2182(6) yes . . Ni(1) S(2) 2.2096(7) yes . . Ni(1) P(1) 2.1567(6) yes . . Ni(1) P(2) 2.1649(6) yes . . Ti(1) Cl(1) 2.3381(6) yes . . Ti(1) S(1) 2.2282(7) yes . . Ti(1) S(2) 2.2303(8) yes . . Ti(1) C(1) 2.390(2) yes . . Ti(1) C(2) 2.353(2) yes . . Ti(1) C(3) 2.376(3) yes . . Ti(1) C(4) 2.408(3) yes . . Ti(1) C(5) 2.391(3) yes . . P(1) C(6) 1.819(2) yes . . P(1) C(12) 1.819(2) yes . . P(1) C(18) 1.841(2) yes . . P(2) C(19) 1.846(2) yes . . P(2) C(20) 1.820(2) yes . . P(2) C(26) 1.827(2) yes . . C(1) C(2) 1.405(4) yes . . C(1) C(5) 1.407(3) yes . . C(2) C(3) 1.419(4) yes . . C(3) C(4) 1.392(4) yes . . C(4) C(5) 1.422(5) yes . . C(6) C(7) 1.395(3) yes . . C(6) C(11) 1.397(4) yes . . C(7) C(8) 1.395(3) yes . . C(8) C(9) 1.371(4) yes . . C(9) C(10) 1.385(4) yes . . C(10) C(11) 1.385(3) yes . . C(12) C(13) 1.394(3) yes . . C(12) C(17) 1.392(2) yes . . C(13) C(14) 1.387(4) yes . . C(14) C(15) 1.381(3) yes . . C(15) C(16) 1.389(4) yes . . C(16) C(17) 1.388(4) yes . . C(18) C(19) 1.528(3) yes . . C(20) C(21) 1.388(3) yes . . C(20) C(25) 1.400(3) yes . . C(21) C(22) 1.390(3) yes . . C(22) C(23) 1.383(4) yes . . C(23) C(24) 1.378(3) yes . . C(24) C(25) 1.383(3) yes . . C(26) C(27) 1.402(4) yes . . C(26) C(31) 1.392(3) yes . . C(27) C(28) 1.403(3) yes . . C(28) C(29) 1.377(3) yes . . C(29) C(30) 1.394(4) yes . . C(30) C(31) 1.390(3) yes . . 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 Ti(1) Ni(1) S(1) 50.64(2) yes . . . Ti(1) Ni(1) S(2) 50.74(2) yes . . . Ti(1) Ni(1) P(1) 134.38(2) yes . . . Ti(1) Ni(1) P(2) 137.78(2) yes . . . S(1) Ni(1) S(2) 100.93(2) yes . . . S(1) Ni(1) P(1) 84.02(2) yes . . . S(1) Ni(1) P(2) 171.48(2) yes . . . S(2) Ni(1) P(1) 174.74(3) yes . . . S(2) Ni(1) P(2) 87.29(2) yes . . . P(1) Ni(1) P(2) 87.69(2) yes . . . Cl(1) Ti(1) S(1) 103.21(3) yes . . . Cl(1) Ti(1) S(2) 104.32(3) yes . . . Cl(1) Ti(1) C(1) 127.08(7) yes . . . Cl(1) Ti(1) C(2) 139.89(7) yes . . . Cl(1) Ti(1) C(3) 107.68(6) yes . . . Cl(1) Ti(1) C(4) 82.84(6) yes . . . Cl(1) Ti(1) C(5) 93.25(6) yes . . . Cl(1) Ti(1) Ni(1) 106.25(2) yes . . . S(1) Ti(1) S(2) 99.98(3) yes . . . S(1) Ti(1) C(1) 87.88(7) yes . . . S(1) Ti(1) C(2) 108.81(7) yes . . . S(1) Ti(1) C(3) 142.96(6) yes . . . S(1) Ti(1) C(4) 136.37(8) yes . . . S(1) Ti(1) C(5) 101.99(8) yes . . . S(1) Ti(1) Ni(1) 50.33(2) yes . . . S(2) Ti(1) C(1) 124.73(7) yes . . . S(2) Ti(1) C(2) 93.40(7) yes . . . S(2) Ti(1) C(3) 91.78(7) yes . . . S(2) Ti(1) C(4) 120.63(9) yes . . . S(2) Ti(1) C(5) 147.80(8) yes . . . S(2) Ti(1) Ni(1) 50.09(2) yes . . . C(1) Ti(1) C(2) 34.4(1) yes . . . C(1) Ti(1) C(3) 57.2(1) yes . . . C(1) Ti(1) C(4) 57.07(9) yes . . . C(1) Ti(1) C(5) 34.23(8) yes . . . C(1) Ti(1) Ni(1) 119.43(6) yes . . . C(2) Ti(1) C(3) 34.93(9) yes . . . C(2) Ti(1) C(4) 57.32(8) yes . . . C(2) Ti(1) C(5) 57.25(9) yes . . . C(2) Ti(1) Ni(1) 112.63(6) yes . . . C(3) Ti(1) C(4) 33.8(1) yes . . . C(3) Ti(1) C(5) 56.9(1) yes . . . C(3) Ti(1) Ni(1) 134.11(7) yes . . . C(4) Ti(1) C(5) 34.5(1) yes . . . C(4) Ti(1) Ni(1) 167.93(7) yes . . . C(5) Ti(1) Ni(1) 148.67(7) yes . . . Ti(1) S(1) Ni(1) 79.03(2) yes . . . Ti(1) S(2) Ni(1) 79.17(3) yes . . . C(6) P(1) C(12) 107.9(1) yes . . . C(6) P(1) C(18) 101.74(9) yes . . . C(6) P(1) Ni(1) 112.09(8) yes . . . C(12) P(1) C(18) 104.0(1) yes . . . C(12) P(1) Ni(1) 120.91(7) yes . . . C(18) P(1) Ni(1) 108.24(8) yes . . . C(19) P(2) C(20) 103.79(9) yes . . . C(19) P(2) C(26) 102.4(1) yes . . . C(19) P(2) Ni(1) 107.69(8) yes . . . C(20) P(2) C(26) 105.7(1) yes . . . C(20) P(2) Ni(1) 113.38(8) yes . . . C(26) P(2) Ni(1) 121.94(7) yes . . . C(2) C(1) C(5) 107.9(2) yes . . . Ti(1) C(1) C(2) 71.3(1) yes . . . Ti(1) C(1) C(5) 73.0(1) yes . . . Ti(1) C(2) C(3) 73.4(1) yes . . . Ti(1) C(2) C(1) 74.2(1) yes . . . C(1) C(2) C(3) 107.7(2) yes . . . Ti(1) C(3) C(4) 74.3(2) yes . . . Ti(1) C(3) C(2) 71.7(1) yes . . . C(2) C(3) C(4) 108.6(3) yes . . . Ti(1) C(4) C(5) 72.1(2) yes . . . Ti(1) C(4) C(3) 71.8(2) yes . . . C(3) C(4) C(5) 107.5(2) yes . . . Ti(1) C(5) C(1) 72.8(1) yes . . . Ti(1) C(5) C(4) 73.4(2) yes . . . C(1) C(5) C(4) 108.2(3) yes . . . C(7) C(6) C(11) 119.6(2) yes . . . C(7) C(6) P(1) 119.5(2) yes . . . C(11) C(6) P(1) 120.6(2) yes . . . C(8) C(7) C(6) 119.9(2) yes . . . C(9) C(8) C(7) 119.7(2) yes . . . C(10) C(9) C(8) 121.1(2) yes . . . C(11) C(10) C(9) 119.8(3) yes . . . C(6) C(11) C(10) 119.9(2) yes . . . C(13) C(12) C(17) 119.1(2) yes . . . C(13) C(12) P(1) 121.6(1) yes . . . C(17) C(12) P(1) 119.3(2) yes . . . C(14) C(13) C(12) 120.0(2) yes . . . C(15) C(14) C(13) 120.5(3) yes . . . C(16) C(15) C(14) 120.0(2) yes . . . C(17) C(16) C(15) 119.6(2) yes . . . C(12) C(17) C(16) 120.8(2) yes . . . C(19) C(18) P(1) 106.0(1) yes . . . P(2) C(19) C(18) 107.1(1) yes . . . C(21) C(20) C(25) 118.9(2) yes . . . C(21) C(20) P(2) 121.1(2) yes . . . C(25) C(20) P(2) 120.0(1) yes . . . C(22) C(21) C(20) 120.3(2) yes . . . C(23) C(22) C(21) 120.2(2) yes . . . C(24) C(23) C(22) 120.0(2) yes . . . C(25) C(24) C(23) 120.3(2) yes . . . C(20) C(25) C(24) 120.3(2) yes . . . C(27) C(26) C(31) 119.0(2) yes . . . C(27) C(26) P(2) 121.7(1) yes . . . C(31) C(26) P(2) 119.3(2) yes . . . C(28) C(27) C(26) 119.7(2) yes . . . C(29) C(28) C(27) 120.5(3) yes . . . C(30) C(29) C(28) 120.1(2) yes . . . C(31) C(30) C(29) 119.7(2) yes . . . C(26) C(31) C(30) 121.0(2) yes . . . 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 S(1) Ni(1) Ti(1) Cl(1) 93.87(3) yes . . . . S(1) Ni(1) Ti(1) S(2) -170.85(2) yes . . . . S(1) Ni(1) Ti(1) C(1) -58.46(9) yes . . . . S(1) Ni(1) Ti(1) C(2) -96.21(8) yes . . . . S(1) Ni(1) Ti(1) C(3) -129.81(9) yes . . . . S(1) Ni(1) Ti(1) C(4) -128.2(3) yes . . . . S(1) Ni(1) Ti(1) C(5) -32.5(1) yes . . . . S(2) Ni(1) Ti(1) Cl(1) -95.28(3) yes . . . . S(2) Ni(1) Ti(1) S(1) 170.85(2) yes . . . . S(2) Ni(1) Ti(1) C(1) 112.39(9) yes . . . . S(2) Ni(1) Ti(1) C(2) 74.64(8) yes . . . . S(2) Ni(1) Ti(1) C(3) 41.04(9) yes . . . . S(2) Ni(1) Ti(1) C(4) 42.7(3) yes . . . . S(2) Ni(1) Ti(1) C(5) 138.4(1) yes . . . . P(1) Ni(1) Ti(1) Cl(1) 86.31(3) yes . . . . P(1) Ni(1) Ti(1) S(1) -7.55(2) yes . . . . P(1) Ni(1) Ti(1) S(2) -178.40(2) yes . . . . P(1) Ni(1) Ti(1) C(1) -66.01(9) yes . . . . P(1) Ni(1) Ti(1) C(2) -103.76(8) yes . . . . P(1) Ni(1) Ti(1) C(3) -137.36(9) yes . . . . P(1) Ni(1) Ti(1) C(4) -135.7(3) yes . . . . P(1) Ni(1) Ti(1) C(5) -40.0(1) yes . . . . P(2) Ni(1) Ti(1) Cl(1) -87.91(3) yes . . . . P(2) Ni(1) Ti(1) S(1) 178.22(2) yes . . . . P(2) Ni(1) Ti(1) S(2) 7.37(2) yes . . . . P(2) Ni(1) Ti(1) C(1) 119.76(9) yes . . . . P(2) Ni(1) Ti(1) C(2) 82.01(8) yes . . . . P(2) Ni(1) Ti(1) C(3) 48.41(9) yes . . . . P(2) Ni(1) Ti(1) C(4) 50.0(3) yes . . . . P(2) Ni(1) Ti(1) C(5) 145.8(1) yes . . . . S(2) Ni(1) S(1) Ti(1) -7.20(2) yes . . . . P(1) Ni(1) S(1) Ti(1) 174.58(2) yes . . . . S(1) Ni(1) S(2) Ti(1) 7.19(2) yes . . . . P(2) Ni(1) S(2) Ti(1) -175.05(2) yes . . . . Ti(1) Ni(1) P(1) C(6) 86.42(9) yes . . . . Ti(1) Ni(1) P(1) C(12) -42.57(8) yes . . . . Ti(1) Ni(1) P(1) C(18) -162.18(6) yes . . . . S(1) Ni(1) P(1) C(6) 80.55(8) yes . . . . S(1) Ni(1) P(1) C(12) -48.44(8) yes . . . . S(1) Ni(1) P(1) C(18) -168.05(6) yes . . . . P(2) Ni(1) P(1) C(6) -97.46(9) yes . . . . P(2) Ni(1) P(1) C(12) 133.55(8) yes . . . . P(2) Ni(1) P(1) C(18) 13.94(6) yes . . . . Ti(1) Ni(1) P(2) C(19) -172.46(6) yes . . . . Ti(1) Ni(1) P(2) C(20) 73.31(9) yes . . . . Ti(1) Ni(1) P(2) C(26) -54.85(9) yes . . . . S(2) Ni(1) P(2) C(19) -166.75(6) yes . . . . S(2) Ni(1) P(2) C(20) 79.01(9) yes . . . . S(2) Ni(1) P(2) C(26) -49.14(8) yes . . . . P(1) Ni(1) P(2) C(19) 11.67(6) yes . . . . P(1) Ni(1) P(2) C(20) -102.57(9) yes . . . . P(1) Ni(1) P(2) C(26) 129.28(8) yes . . . . Cl(1) Ti(1) S(1) Ni(1) -100.30(2) yes . . . . S(2) Ti(1) S(1) Ni(1) 7.12(2) yes . . . . C(1) Ti(1) S(1) Ni(1) 132.03(2) yes . . . . C(2) Ti(1) S(1) Ni(1) 104.21(2) yes . . . . C(3) Ti(1) S(1) Ni(1) 113.71(4) yes . . . . C(4) Ti(1) S(1) Ni(1) 166.23(3) yes . . . . C(5) Ti(1) S(1) Ni(1) 163.42(2) yes . . . . Cl(1) Ti(1) S(2) Ni(1) 99.38(2) yes . . . . S(1) Ti(1) S(2) Ni(1) -7.14(2) yes . . . . C(1) Ti(1) S(2) Ni(1) -101.52(3) yes . . . . C(2) Ti(1) S(2) Ni(1) -116.92(2) yes . . . . C(3) Ti(1) S(2) Ni(1) -151.86(2) yes . . . . C(4) Ti(1) S(2) Ni(1) -170.53(2) yes . . . . C(5) Ti(1) S(2) Ni(1) -139.61(4) yes . . . . Ni(1) Ti(1) C(1) C(2) -87.6(2) yes . . . . Ni(1) Ti(1) C(1) C(5) 156.1(2) yes . . . . Cl(1) Ti(1) C(1) C(2) 126.4(1) yes . . . . Cl(1) Ti(1) C(1) C(5) 10.1(2) yes . . . . S(1) Ti(1) C(1) C(2) -128.6(1) yes . . . . S(1) Ti(1) C(1) C(5) 115.1(2) yes . . . . S(2) Ti(1) C(1) C(2) -28.0(2) yes . . . . S(2) Ti(1) C(1) C(5) -144.2(2) yes . . . . C(2) Ti(1) C(1) C(5) -116.3(2) yes . . . . C(3) Ti(1) C(1) C(2) 38.3(1) yes . . . . C(3) Ti(1) C(1) C(5) -77.9(2) yes . . . . C(4) Ti(1) C(1) C(2) 78.9(1) yes . . . . C(4) Ti(1) C(1) C(5) -37.4(2) yes . . . . C(5) Ti(1) C(1) C(2) 116.3(2) yes . . . . Ni(1) Ti(1) C(2) C(1) 109.5(1) yes . . . . Ni(1) Ti(1) C(2) C(3) -136.1(1) yes . . . . Cl(1) Ti(1) C(2) C(1) -85.6(2) yes . . . . Cl(1) Ti(1) C(2) C(3) 28.8(2) yes . . . . S(1) Ti(1) C(2) C(1) 55.5(2) yes . . . . S(1) Ti(1) C(2) C(3) 170.0(1) yes . . . . S(2) Ti(1) C(2) C(1) 157.3(1) yes . . . . S(2) Ti(1) C(2) C(3) -88.2(2) yes . . . . C(1) Ti(1) C(2) C(3) 114.5(2) yes . . . . C(3) Ti(1) C(2) C(1) -114.5(2) yes . . . . C(4) Ti(1) C(2) C(1) -78.1(1) yes . . . . C(4) Ti(1) C(2) C(3) 36.4(1) yes . . . . C(5) Ti(1) C(2) C(1) -36.9(1) yes . . . . C(5) Ti(1) C(2) C(3) 77.6(2) yes . . . . Ni(1) Ti(1) C(3) C(2) 63.1(2) yes . . . . Ni(1) Ti(1) C(3) C(4) 179.4(1) yes . . . . Cl(1) Ti(1) C(3) C(2) -161.0(1) yes . . . . Cl(1) Ti(1) C(3) C(4) -44.7(2) yes . . . . S(1) Ti(1) C(3) C(2) -15.8(2) yes . . . . S(1) Ti(1) C(3) C(4) 100.4(2) yes . . . . S(2) Ti(1) C(3) C(2) 93.4(2) yes . . . . S(2) Ti(1) C(3) C(4) -150.4(2) yes . . . . C(1) Ti(1) C(3) C(2) -37.8(1) yes . . . . C(1) Ti(1) C(3) C(4) 78.5(2) yes . . . . C(2) Ti(1) C(3) C(4) 116.3(2) yes . . . . C(4) Ti(1) C(3) C(2) -116.3(2) yes . . . . C(5) Ti(1) C(3) C(2) -78.8(2) yes . . . . C(5) Ti(1) C(3) C(4) 37.4(1) yes . . . . Ni(1) Ti(1) C(4) C(3) -2.1(5) yes . . . . Ni(1) Ti(1) C(4) C(5) 113.9(4) yes . . . . Cl(1) Ti(1) C(4) C(3) 137.5(2) yes . . . . Cl(1) Ti(1) C(4) C(5) -106.5(1) yes . . . . S(1) Ti(1) C(4) C(3) -120.8(2) yes . . . . S(1) Ti(1) C(4) C(5) -4.9(2) yes . . . . S(2) Ti(1) C(4) C(3) 35.1(2) yes . . . . S(2) Ti(1) C(4) C(5) 151.1(1) yes . . . . C(1) Ti(1) C(4) C(3) -78.8(1) yes . . . . C(1) Ti(1) C(4) C(5) 37.1(1) yes . . . . C(2) Ti(1) C(4) C(3) -37.6(1) yes . . . . C(2) Ti(1) C(4) C(5) 78.4(1) yes . . . . C(3) Ti(1) C(4) C(5) 116.0(2) yes . . . . C(5) Ti(1) C(4) C(3) -116.0(2) yes . . . . Ni(1) Ti(1) C(5) C(1) -42.7(3) yes . . . . Ni(1) Ti(1) C(5) C(4) -158.4(1) yes . . . . Cl(1) Ti(1) C(5) C(1) -172.0(2) yes . . . . Cl(1) Ti(1) C(5) C(4) 72.3(1) yes . . . . S(1) Ti(1) C(5) C(1) -67.7(2) yes . . . . S(1) Ti(1) C(5) C(4) 176.6(1) yes . . . . S(2) Ti(1) C(5) C(1) 64.3(2) yes . . . . S(2) Ti(1) C(5) C(4) -51.4(2) yes . . . . C(1) Ti(1) C(5) C(4) -115.7(2) yes . . . . C(2) Ti(1) C(5) C(1) 37.1(2) yes . . . . C(2) Ti(1) C(5) C(4) -78.6(1) yes . . . . C(3) Ti(1) C(5) C(1) 79.0(2) yes . . . . C(3) Ti(1) C(5) C(4) -36.7(1) yes . . . . C(4) Ti(1) C(5) C(1) 115.7(2) yes . . . . Ni(1) P(1) C(6) C(7) 0.3(2) yes . . . . Ni(1) P(1) C(6) C(11) 175.0(2) yes . . . . C(12) P(1) C(6) C(7) 135.8(2) yes . . . . C(12) P(1) C(6) C(11) -49.5(2) yes . . . . C(18) P(1) C(6) C(7) -115.1(2) yes . . . . C(18) P(1) C(6) C(11) 59.6(2) yes . . . . Ni(1) P(1) C(12) C(13) 108.2(2) yes . . . . Ni(1) P(1) C(12) C(17) -69.8(2) yes . . . . C(6) P(1) C(12) C(13) -22.6(2) yes . . . . C(6) P(1) C(12) C(17) 159.4(2) yes . . . . C(18) P(1) C(12) C(13) -130.1(2) yes . . . . C(18) P(1) C(12) C(17) 51.9(2) yes . . . . Ni(1) P(1) C(18) C(19) -42.1(1) yes . . . . C(6) P(1) C(18) C(19) 76.1(1) yes . . . . C(12) P(1) C(18) C(19) -171.9(1) yes . . . . Ni(1) P(2) C(19) C(18) -40.6(1) yes . . . . C(20) P(2) C(19) C(18) 79.8(1) yes . . . . C(26) P(2) C(19) C(18) -170.3(1) yes . . . . Ni(1) P(2) C(20) C(21) -24.5(2) yes . . . . Ni(1) P(2) C(20) C(25) 156.6(2) yes . . . . C(19) P(2) C(20) C(21) -141.1(2) yes . . . . C(19) P(2) C(20) C(25) 40.1(2) yes . . . . C(26) P(2) C(20) C(21) 111.6(2) yes . . . . C(26) P(2) C(20) C(25) -67.3(2) yes . . . . Ni(1) P(2) C(26) C(27) 121.6(2) yes . . . . Ni(1) P(2) C(26) C(31) -59.8(2) yes . . . . C(19) P(2) C(26) C(27) -118.2(2) yes . . . . C(19) P(2) C(26) C(31) 60.4(2) yes . . . . C(20) P(2) C(26) C(27) -9.9(2) yes . . . . C(20) P(2) C(26) C(31) 168.7(2) yes . . . . Ti(1) C(1) C(2) C(3) -66.3(2) yes . . . . C(5) C(1) C(2) Ti(1) 64.3(2) yes . . . . C(5) C(1) C(2) C(3) -2.0(3) yes . . . . Ti(1) C(1) C(5) C(4) 65.4(2) yes . . . . C(2) C(1) C(5) Ti(1) -63.2(2) yes . . . . C(2) C(1) C(5) C(4) 2.2(3) yes . . . . Ti(1) C(2) C(3) C(4) -65.7(2) yes . . . . C(1) C(2) C(3) Ti(1) 66.8(2) yes . . . . C(1) C(2) C(3) C(4) 1.2(3) yes . . . . Ti(1) C(3) C(4) C(5) -63.8(2) yes . . . . C(2) C(3) C(4) Ti(1) 63.9(2) yes . . . . C(2) C(3) C(4) C(5) 0.2(3) yes . . . . Ti(1) C(4) C(5) C(1) -65.0(2) yes . . . . C(3) C(4) C(5) Ti(1) 63.6(2) yes . . . . C(3) C(4) C(5) C(1) -1.4(3) yes . . . . P(1) C(6) C(7) C(8) 175.3(2) yes . . . . C(11) C(6) C(7) C(8) 0.5(4) yes . . . . P(1) C(6) C(11) C(10) -175.4(2) yes . . . . C(7) C(6) C(11) C(10) -0.7(4) yes . . . . C(6) C(7) C(8) C(9) 0.2(4) yes . . . . C(7) C(8) C(9) C(10) -0.7(5) yes . . . . C(8) C(9) C(10) C(11) 0.5(5) yes . . . . C(9) C(10) C(11) C(6) 0.2(4) yes . . . . P(1) C(12) C(13) C(14) -179.7(2) yes . . . . C(17) C(12) C(13) C(14) -1.7(3) yes . . . . P(1) C(12) C(17) C(16) 179.7(2) yes . . . . C(13) C(12) C(17) C(16) 1.6(3) yes . . . . C(12) C(13) C(14) C(15) 0.6(4) yes . . . . C(13) C(14) C(15) C(16) 0.7(4) yes . . . . C(14) C(15) C(16) C(17) -0.8(4) yes . . . . C(15) C(16) C(17) C(12) -0.4(4) yes . . . . P(1) C(18) C(19) P(2) 51.0(2) yes . . . . P(2) C(20) C(21) C(22) -178.2(2) yes . . . . C(25) C(20) C(21) C(22) 0.7(4) yes . . . . P(2) C(20) C(25) C(24) 178.5(2) yes . . . . C(21) C(20) C(25) C(24) -0.4(4) yes . . . . C(20) C(21) C(22) C(23) -0.3(4) yes . . . . C(21) C(22) C(23) C(24) -0.3(4) yes . . . . C(22) C(23) C(24) C(25) 0.5(4) yes . . . . C(23) C(24) C(25) C(20) -0.2(4) yes . . . . P(2) C(26) C(27) C(28) 177.1(2) yes . . . . C(31) C(26) C(27) C(28) -1.4(3) yes . . . . P(2) C(26) C(31) C(30) -176.6(2) yes . . . . C(27) C(26) C(31) C(30) 2.0(3) yes . . . . C(26) C(27) C(28) C(29) -0.3(3) yes . . . . C(27) C(28) C(29) C(30) 1.4(4) yes . . . . C(28) C(29) C(30) C(31) -0.9(4) yes . . . . C(29) C(30) C(31) C(26) -0.9(3) yes . . . . 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 Ni(1) Ti(1) 2.8292(4) yes . 55501 Ni(1) S(1) 2.2182(6) yes . 55501 Ni(1) S(2) 2.2096(7) yes . 55501 Ni(1) C(6) 3.303(2) yes . 55501 Ni(1) C(7) 3.409(2) yes . 55501 Ni(1) C(12) 3.463(2) yes . 55501 Ni(1) C(18) 3.245(2) yes . 55501 Ni(1) C(19) 3.244(2) yes . 55501 Ni(1) C(20) 3.336(2) yes . 55501 Ni(1) C(21) 3.549(2) yes . 55501 Ni(1) C(26) 3.494(2) yes . 55501 Ti(1) Ni(1) 2.8292(4) yes . 55501 Ti(1) Cl(1) 2.3381(6) yes . 55501 Ti(1) C(1) 2.390(2) yes . 55501 Ti(1) C(2) 2.353(2) yes . 55501 Ti(1) C(3) 2.376(3) yes . 55501 Ti(1) C(4) 2.408(3) yes . 55501 Ti(1) C(5) 2.391(3) yes . 55501 Cl(1) Ti(1) 2.3381(6) yes . 55501 Cl(1) S(1) 3.5794(8) yes . 55501 Cl(1) C(4) 3.140(3) yes . 55501 Cl(1) C(5) 3.438(2) yes . 55501 Cl(1) C(8) 3.513(3) yes . 55504 Cl(1) C(30) 3.570(3) yes . 55504 S(1) Ni(1) 2.2182(6) yes . 55501 S(1) Cl(1) 3.5794(8) yes . 55501 S(1) S(2) 3.4149(9) yes . 55501 S(1) P(1) 2.9283(8) yes . 55501 S(1) C(1) 3.206(3) yes . 55501 S(1) C(5) 3.591(3) yes . 55501 S(1) C(12) 3.303(2) yes . 55501 S(2) Ni(1) 2.2096(7) yes . 55501 S(2) S(1) 3.4149(9) yes . 55501 S(2) P(2) 3.0195(8) yes . 55501 S(2) C(2) 3.337(2) yes . 55501 S(2) C(3) 3.309(3) yes . 55501 S(2) C(21) 3.545(2) yes . 55501 S(2) C(26) 3.459(2) yes . 55501 P(1) S(1) 2.9283(8) yes . 55501 P(1) P(2) 2.9937(9) yes . 55501 P(1) C(7) 2.785(2) yes . 55501 P(1) C(11) 2.801(2) yes . 55501 P(1) C(13) 2.813(3) yes . 55501 P(1) C(17) 2.779(2) yes . 55501 P(1) C(18) 1.841(2) yes . 55501 P(1) C(19) 2.698(2) yes . 55501 P(2) S(2) 3.0195(8) yes . 55501 P(2) P(1) 2.9937(9) yes . 55501 P(2) C(18) 2.719(2) yes . 55501 P(2) C(19) 1.846(2) yes . 55501 P(2) C(21) 2.802(2) yes . 55501 P(2) C(25) 2.797(2) yes . 55501 P(2) C(27) 2.828(3) yes . 55501 P(2) C(31) 2.786(2) yes . 55501 C(1) Ti(1) 2.390(2) yes . 55501 C(1) S(1) 3.206(3) yes . 55501 C(1) C(3) 2.281(4) yes . 55501 C(1) C(4) 2.292(4) yes . 55501 C(2) Ti(1) 2.353(2) yes . 55501 C(2) S(2) 3.337(2) yes . 55501 C(2) C(4) 2.284(3) yes . 55501 C(2) C(5) 2.273(4) yes . 55501 C(3) Ti(1) 2.376(3) yes . 55501 C(3) S(2) 3.309(3) yes . 55501 C(3) C(1) 2.281(4) yes . 55501 C(3) C(5) 2.269(5) yes . 55501 C(4) Ti(1) 2.408(3) yes . 55501 C(4) Cl(1) 3.140(3) yes . 55501 C(4) C(1) 2.292(4) yes . 55501 C(4) C(2) 2.284(3) yes . 55501 C(5) Ti(1) 2.391(3) yes . 55501 C(5) Cl(1) 3.438(2) yes . 55501 C(5) S(1) 3.591(3) yes . 55501 C(5) C(2) 2.273(4) yes . 55501 C(5) C(3) 2.269(5) yes . 55501 C(6) Ni(1) 3.303(2) yes . 55501 C(6) C(8) 2.415(3) yes . 55501 C(6) C(9) 2.769(3) yes . 55501 C(6) C(10) 2.408(3) yes . 55501 C(6) C(12) 2.941(3) yes . 55501 C(6) C(13) 3.205(3) yes . 55501 C(6) C(18) 2.839(3) yes . 55501 C(6) C(19) 3.318(3) yes . 55501 C(7) Ni(1) 3.409(2) yes . 55501 C(7) P(1) 2.785(2) yes . 55501 C(7) C(9) 2.391(4) yes . 55501 C(7) C(10) 2.777(4) yes . 55501 C(7) C(11) 2.413(4) yes . 55501 C(8) C(6) 2.415(3) yes . 55501 C(8) C(10) 2.400(4) yes . 55501 C(8) C(11) 2.781(3) yes . 55501 C(9) C(6) 2.769(3) yes . 55501 C(9) C(7) 2.391(4) yes . 55501 C(9) C(11) 2.396(3) yes . 55501 C(10) C(6) 2.408(3) yes . 55501 C(10) C(7) 2.777(4) yes . 55501 C(10) C(8) 2.400(4) yes . 55501 C(11) P(1) 2.801(2) yes . 55501 C(11) C(7) 2.413(4) yes . 55501 C(11) C(8) 2.781(3) yes . 55501 C(11) C(9) 2.396(3) yes . 55501 C(11) C(12) 3.358(3) yes . 55501 C(11) C(13) 3.311(3) yes . 55501 C(11) C(18) 3.308(3) yes . 55501 C(12) Ni(1) 3.463(2) yes . 55501 C(12) S(1) 3.303(2) yes . 55501 C(12) C(6) 2.941(3) yes . 55501 C(12) C(11) 3.358(3) yes . 55501 C(12) C(14) 2.409(4) yes . 55501 C(12) C(15) 2.786(3) yes . 55501 C(12) C(16) 2.417(3) yes . 55501 C(12) C(18) 2.884(3) yes . 55501 C(13) P(1) 2.813(3) yes . 55501 C(13) C(6) 3.205(3) yes . 55501 C(13) C(11) 3.311(3) yes . 55501 C(13) C(15) 2.403(3) yes . 55501 C(13) C(16) 2.780(3) yes . 55501 C(13) C(17) 2.402(3) yes . 55501 C(14) C(12) 2.409(4) yes . 55501 C(14) C(16) 2.399(3) yes . 55501 C(14) C(17) 2.765(4) yes . 55501 C(15) C(12) 2.786(3) yes . 55501 C(15) C(13) 2.403(3) yes . 55501 C(15) C(17) 2.400(4) yes . 55501 C(16) C(7) 3.363(3) yes . 55504 C(16) C(8) 3.339(4) yes . 55504 C(16) C(12) 2.417(3) yes . 55501 C(16) C(13) 2.780(3) yes . 55501 C(16) C(14) 2.399(3) yes . 55501 C(17) P(1) 2.779(2) yes . 55501 C(17) C(8) 3.478(4) yes . 55504 C(17) C(13) 2.402(3) yes . 55501 C(17) C(14) 2.765(4) yes . 55501 C(17) C(15) 2.400(4) yes . 55501 C(17) C(18) 3.265(3) yes . 55501 C(18) Ni(1) 3.245(2) yes . 55501 C(18) P(1) 1.841(2) yes . 55501 C(18) P(2) 2.719(2) yes . 55501 C(18) C(6) 2.839(3) yes . 55501 C(18) C(11) 3.308(3) yes . 55501 C(18) C(12) 2.884(3) yes . 55501 C(18) C(17) 3.265(3) yes . 55501 C(18) C(20) 3.433(3) yes . 55501 C(19) Ni(1) 3.244(2) yes . 55501 C(19) P(1) 2.698(2) yes . 55501 C(19) P(2) 1.846(2) yes . 55501 C(19) C(6) 3.318(3) yes . 55501 C(19) C(20) 2.885(3) yes . 55501 C(19) C(25) 3.181(3) yes . 55501 C(19) C(26) 2.862(3) yes . 55501 C(19) C(31) 3.314(3) yes . 55501 C(20) Ni(1) 3.336(2) yes . 55501 C(20) C(18) 3.433(3) yes . 55501 C(20) C(19) 2.885(3) yes . 55501 C(20) C(22) 2.410(3) yes . 55501 C(20) C(23) 2.786(3) yes . 55501 C(20) C(24) 2.415(3) yes . 55501 C(20) C(26) 2.908(3) yes . 55501 C(20) C(27) 3.118(3) yes . 55501 C(21) Ni(1) 3.549(2) yes . 55501 C(21) S(2) 3.545(2) yes . 55501 C(21) P(2) 2.802(2) yes . 55501 C(21) C(23) 2.404(3) yes . 55501 C(21) C(24) 2.770(3) yes . 55501 C(21) C(25) 2.401(3) yes . 55501 C(22) C(20) 2.410(3) yes . 55501 C(22) C(24) 2.390(3) yes . 55501 C(22) C(25) 2.766(3) yes . 55501 C(22) C(30) 3.585(3) yes . 55504 C(23) C(2) 3.585(4) yes . 55504 C(23) C(3) 3.512(4) yes . 55504 C(23) C(20) 2.786(3) yes . 55501 C(23) C(21) 2.404(3) yes . 55501 C(23) C(25) 2.395(3) yes . 55501 C(24) C(2) 3.552(4) yes . 55504 C(24) C(3) 3.463(4) yes . 55504 C(24) C(10) 3.390(4) yes . 65501 C(24) C(20) 2.415(3) yes . 55501 C(24) C(21) 2.770(3) yes . 55501 C(24) C(22) 2.390(3) yes . 55501 C(25) P(2) 2.797(2) yes . 55501 C(25) C(19) 3.181(3) yes . 55501 C(25) C(21) 2.401(3) yes . 55501 C(25) C(22) 2.766(3) yes . 55501 C(25) C(23) 2.395(3) yes . 55501 C(25) C(26) 3.466(3) yes . 55501 C(25) C(27) 3.386(3) yes . 55501 C(26) Ni(1) 3.494(2) yes . 55501 C(26) S(2) 3.459(2) yes . 55501 C(26) C(19) 2.862(3) yes . 55501 C(26) C(20) 2.908(3) yes . 55501 C(26) C(25) 3.466(3) yes . 55501 C(26) C(28) 2.425(4) yes . 55501 C(26) C(29) 2.796(3) yes . 55501 C(26) C(30) 2.421(3) yes . 55501 C(27) P(2) 2.828(3) yes . 55501 C(27) C(20) 3.118(3) yes . 55501 C(27) C(25) 3.386(3) yes . 55501 C(27) C(29) 2.413(3) yes . 55501 C(27) C(30) 2.788(3) yes . 55501 C(27) C(31) 2.408(3) yes . 55501 C(28) C(26) 2.425(4) yes . 55501 C(28) C(30) 2.401(3) yes . 55501 C(28) C(31) 2.772(4) yes . 55501 C(29) C(26) 2.796(3) yes . 55501 C(29) C(27) 2.413(3) yes . 55501 C(29) C(31) 2.407(4) yes . 55501 C(30) C(26) 2.421(3) yes . 55501 C(30) C(27) 2.788(3) yes . 55501 C(30) C(28) 2.401(3) yes . 55501 C(31) P(2) 2.786(2) yes . 55501 C(31) C(19) 3.314(3) yes . 55501 C(31) C(27) 2.408(3) yes . 55501 C(31) C(28) 2.772(4) yes . 55501 C(31) C(29) 2.407(4) yes . 55501 #============================================================================== # 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 #==============================================================================