# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_qui6cult #TrackingRef 'TPS.cif' _audit_creation_date 2012-02-24 _audit_creation_method ; Olex2 1.2-beta (compiled Jan 17 2012 15:45:47, GUI svn.r4036) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H22 Si' _chemical_formula_sum 'C28 H22 Si' _chemical_formula_weight 386.55 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 9.29560(10) _cell_length_b 16.8937(5) _cell_length_c 14.1056(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.130(2) _cell_angle_gamma 90.00 _cell_volume 2105.13(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7181 _cell_measurement_temperature 173.00(14) _cell_measurement_theta_max 71.4442 _cell_measurement_theta_min 3.2938 _exptl_absorpt_coefficient_mu 1.045 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.68100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_unetI/netI 0.0260 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10945 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.47 _diffrn_reflns_theta_min 5.65 _diffrn_ambient_temperature 173.00(14) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 43.00 72.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 90.0000 29 #__ type_ start__ end____ width___ exp.time_ 2 omega 37.00 71.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -90.0000 34 #__ type_ start__ end____ width___ exp.time_ 3 omega -21.00 65.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -150.0000 86 #__ type_ start__ end____ width___ exp.time_ 4 omega -123.00 -25.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 -77.0000 -180.0000 98 #__ type_ start__ end____ width___ exp.time_ 5 omega -17.00 79.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -99.0000 -60.0000 96 #__ type_ start__ end____ width___ exp.time_ 6 omega 25.00 124.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 77.0000 30.0000 99 #__ type_ start__ end____ width___ exp.time_ 7 omega -2.00 90.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -125.0000 150.0000 92 #__ type_ start__ end____ width___ exp.time_ 8 omega -23.00 3.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 64.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 9 omega -87.00 -62.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 64.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 10 omega 90.00 175.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 25.0000 -120.0000 85 #__ type_ start__ end____ width___ exp.time_ 11 omega 37.00 62.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 12 omega 41.00 67.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 13 omega 38.00 145.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -150.0000 107 #__ type_ start__ end____ width___ exp.time_ 14 omega 43.00 83.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 30.0000 40 #__ type_ start__ end____ width___ exp.time_ 15 omega 39.00 66.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -120.0000 27 #__ type_ start__ end____ width___ exp.time_ 16 omega 78.00 177.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 25.0000 150.0000 99 #__ type_ start__ end____ width___ exp.time_ 17 omega 37.00 71.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -150.0000 34 #__ type_ start__ end____ width___ exp.time_ 18 omega 121.00 147.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 19 omega 39.00 105.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 150.0000 66 #__ type_ start__ end____ width___ exp.time_ 20 omega 38.00 71.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -180.0000 33 #__ type_ start__ end____ width___ exp.time_ 21 omega 38.00 64.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 0.0000 26 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1677423000 _diffrn_orient_matrix_UB_12 0.0073013000 _diffrn_orient_matrix_UB_13 0.0060147000 _diffrn_orient_matrix_UB_21 -0.0374310000 _diffrn_orient_matrix_UB_22 0.0738885000 _diffrn_orient_matrix_UB_23 -0.0672742000 _diffrn_orient_matrix_UB_31 0.0291136000 _diffrn_orient_matrix_UB_32 0.0530523000 _diffrn_orient_matrix_UB_33 0.0929544000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 35 _diffrn_source_power 1.75 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3462 _reflns_number_total 3742 _reflns_odcompleteness_completeness 99.48 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.238 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.033 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 3742 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0318 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.5453P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.0860 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Si1 Si 0.41885(3) 0.101152(18) 0.22489(2) 0.02516(11) Uani 1 1 d . . . C1 C 0.25093(13) 0.05289(7) 0.24540(9) 0.0279(2) Uani 1 1 d . . . H1 H 0.2007 0.0705 0.2908 0.033 Uiso 1 1 calc R . . C2 C 0.21173(12) -0.01114(7) 0.18563(8) 0.0246(2) Uani 1 1 d . . . C3 C 0.30702(12) -0.02462(7) 0.11710(8) 0.0243(2) Uani 1 1 d . . . C4 C 0.42128(13) 0.02728(7) 0.12788(8) 0.0268(2) Uani 1 1 d . . . H4 H 0.4919 0.0262 0.0916 0.032 Uiso 1 1 calc R . . C11 C 0.38584(13) 0.20414(7) 0.17427(9) 0.0265(2) Uani 1 1 d . . . C12 C 0.26825(14) 0.21865(8) 0.08610(10) 0.0349(3) Uani 1 1 d . . . H12 H 0.2068 0.1760 0.0525 0.042 Uiso 1 1 calc R . . C13 C 0.24016(16) 0.29454(9) 0.04712(11) 0.0422(3) Uani 1 1 d . . . H13 H 0.1590 0.3035 -0.0124 0.051 Uiso 1 1 calc R . . C14 C 0.32978(16) 0.35722(8) 0.09442(11) 0.0392(3) Uani 1 1 d . . . H14 H 0.3102 0.4091 0.0677 0.047 Uiso 1 1 calc R . . C15 C 0.44772(15) 0.34387(8) 0.18063(10) 0.0348(3) Uani 1 1 d . . . H15 H 0.5104 0.3866 0.2128 0.042 Uiso 1 1 calc R . . C16 C 0.47507(13) 0.26822(7) 0.22049(9) 0.0294(3) Uani 1 1 d . . . H16 H 0.5560 0.2599 0.2803 0.035 Uiso 1 1 calc R . . C21 C 0.08915(12) -0.06656(7) 0.19003(8) 0.0254(2) Uani 1 1 d . . . C22 C -0.04411(14) -0.03650(8) 0.20188(9) 0.0316(3) Uani 1 1 d . . . H22 H -0.0569 0.0191 0.2048 0.038 Uiso 1 1 calc R . . C23 C -0.15834(15) -0.08671(9) 0.20949(11) 0.0391(3) Uani 1 1 d . . . H23 H -0.2483 -0.0653 0.2176 0.047 Uiso 1 1 calc R . . C24 C -0.14123(15) -0.16786(9) 0.20531(10) 0.0393(3) Uani 1 1 d . . . H24 H -0.2194 -0.2023 0.2102 0.047 Uiso 1 1 calc R . . C25 C -0.00986(15) -0.19847(8) 0.19403(9) 0.0347(3) Uani 1 1 d . . . H25 H 0.0023 -0.2542 0.1914 0.042 Uiso 1 1 calc R . . C26 C 0.10469(13) -0.14841(7) 0.18647(8) 0.0291(3) Uani 1 1 d . . . H26 H 0.1946 -0.1703 0.1788 0.035 Uiso 1 1 calc R . . C31 C 0.27913(13) -0.09129(7) 0.04476(8) 0.0248(2) Uani 1 1 d . . . C32 C 0.13548(14) -0.10816(7) -0.02017(9) 0.0297(3) Uani 1 1 d . . . H32 H 0.0516 -0.0764 -0.0192 0.036 Uiso 1 1 calc R . . C33 C 0.11430(15) -0.17116(8) -0.08635(9) 0.0356(3) Uani 1 1 d . . . H33 H 0.0165 -0.1815 -0.1315 0.043 Uiso 1 1 calc R . . C34 C 0.23467(16) -0.21885(8) -0.08688(9) 0.0364(3) Uani 1 1 d . . . H34 H 0.2190 -0.2627 -0.1310 0.044 Uiso 1 1 calc R . . C35 C 0.37833(15) -0.20268(8) -0.02297(9) 0.0334(3) Uani 1 1 d . . . H35 H 0.4614 -0.2353 -0.0234 0.040 Uiso 1 1 calc R . . C36 C 0.40032(13) -0.13877(7) 0.04161(8) 0.0276(2) Uani 1 1 d . . . H36 H 0.4993 -0.1271 0.0843 0.033 Uiso 1 1 calc R . . C41 C 0.58992(14) 0.09499(7) 0.33795(9) 0.0291(3) Uani 1 1 d . . . C42 C 0.73484(16) 0.09800(8) 0.32814(11) 0.0398(3) Uani 1 1 d . . . H42 H 0.7458 0.1050 0.2639 0.048 Uiso 1 1 calc R . . C43 C 0.86273(17) 0.09093(10) 0.41059(13) 0.0508(4) Uani 1 1 d . . . H43 H 0.9603 0.0927 0.4024 0.061 Uiso 1 1 calc R . . C44 C 0.84897(18) 0.08129(9) 0.50453(12) 0.0503(4) Uani 1 1 d . . . H44 H 0.9368 0.0769 0.5610 0.060 Uiso 1 1 calc R . . C45 C 0.70698(19) 0.07812(9) 0.51601(11) 0.0471(4) Uani 1 1 d . . . H45 H 0.6970 0.0715 0.5805 0.056 Uiso 1 1 calc R . . C46 C 0.57874(16) 0.08461(8) 0.43333(10) 0.0380(3) Uani 1 1 d . . . H46 H 0.4815 0.0819 0.4420 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.02472(18) 0.02390(18) 0.02767(18) -0.00266(11) 0.00933(13) -0.00281(11) C1 0.0267(6) 0.0294(6) 0.0297(6) -0.0007(5) 0.0119(5) -0.0007(5) C2 0.0226(5) 0.0254(6) 0.0253(5) 0.0035(4) 0.0065(4) 0.0014(4) C3 0.0244(5) 0.0241(6) 0.0236(5) 0.0020(4) 0.0064(4) 0.0015(4) C4 0.0278(6) 0.0261(6) 0.0283(6) -0.0008(5) 0.0114(5) -0.0009(5) C11 0.0240(5) 0.0267(6) 0.0304(6) -0.0030(5) 0.0107(5) -0.0004(4) C12 0.0290(6) 0.0331(7) 0.0385(7) -0.0040(5) 0.0045(5) -0.0030(5) C13 0.0372(7) 0.0428(8) 0.0394(7) 0.0045(6) 0.0017(6) 0.0062(6) C14 0.0467(8) 0.0282(6) 0.0464(7) 0.0044(6) 0.0197(6) 0.0050(6) C15 0.0381(7) 0.0271(6) 0.0420(7) -0.0066(5) 0.0166(6) -0.0063(5) C16 0.0276(6) 0.0305(6) 0.0302(6) -0.0043(5) 0.0094(5) -0.0022(5) C21 0.0242(5) 0.0293(6) 0.0215(5) 0.0029(4) 0.0052(4) -0.0022(5) C22 0.0284(6) 0.0337(6) 0.0337(6) 0.0022(5) 0.0111(5) -0.0008(5) C23 0.0264(6) 0.0482(8) 0.0451(8) 0.0043(6) 0.0146(6) -0.0020(6) C24 0.0316(7) 0.0444(8) 0.0418(7) 0.0057(6) 0.0111(6) -0.0126(6) C25 0.0367(7) 0.0305(6) 0.0341(6) 0.0061(5) 0.0068(5) -0.0061(5) C26 0.0260(6) 0.0313(6) 0.0286(6) 0.0057(5) 0.0067(5) 0.0003(5) C31 0.0279(6) 0.0245(6) 0.0232(5) 0.0027(4) 0.0094(5) -0.0019(4) C32 0.0278(6) 0.0323(6) 0.0277(6) -0.0003(5) 0.0066(5) 0.0016(5) C33 0.0332(6) 0.0402(7) 0.0295(6) -0.0060(5) 0.0041(5) -0.0055(5) C34 0.0444(7) 0.0322(7) 0.0325(6) -0.0081(5) 0.0120(6) -0.0046(6) C35 0.0360(7) 0.0320(6) 0.0347(6) -0.0020(5) 0.0145(5) 0.0034(5) C36 0.0268(6) 0.0295(6) 0.0267(6) 0.0000(5) 0.0088(5) -0.0014(5) C41 0.0309(6) 0.0234(6) 0.0311(6) -0.0022(5) 0.0066(5) -0.0008(5) C42 0.0326(7) 0.0452(8) 0.0409(8) -0.0012(6) 0.0104(6) -0.0007(6) C43 0.0317(7) 0.0544(9) 0.0596(10) -0.0040(7) 0.0044(7) 0.0002(6) C44 0.0483(9) 0.0403(8) 0.0451(8) -0.0025(6) -0.0105(7) 0.0040(7) C45 0.0627(10) 0.0398(8) 0.0320(7) 0.0000(6) 0.0051(7) -0.0006(7) C46 0.0425(7) 0.0359(7) 0.0351(7) -0.0013(5) 0.0113(6) -0.0019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.8616(12) . ? Si1 C4 1.8574(12) . ? Si1 C11 1.8694(12) . ? Si1 C41 1.8720(13) . ? C1 C2 1.3501(17) . ? C2 C3 1.5178(15) . ? C2 C21 1.4908(15) . ? C3 C4 1.3488(16) . ? C3 C31 1.4874(16) . ? C11 C12 1.3984(17) . ? C11 C16 1.3959(17) . ? C12 C13 1.387(2) . ? C13 C14 1.384(2) . ? C14 C15 1.379(2) . ? C15 C16 1.3876(18) . ? C21 C22 1.3961(17) . ? C21 C26 1.3928(17) . ? C22 C23 1.3890(18) . ? C23 C24 1.383(2) . ? C24 C25 1.380(2) . ? C25 C26 1.3896(17) . ? C31 C32 1.3936(17) . ? C31 C36 1.3949(17) . ? C32 C33 1.3887(18) . ? C33 C34 1.3806(19) . ? C34 C35 1.3861(19) . ? C35 C36 1.3861(17) . ? C41 C42 1.3973(19) . ? C41 C46 1.3923(19) . ? C42 C43 1.386(2) . ? C43 C44 1.380(2) . ? C44 C45 1.380(2) . ? C45 C46 1.389(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Si1 C11 114.90(5) . . ? C1 Si1 C41 111.98(6) . . ? C4 Si1 C1 91.33(5) . . ? C4 Si1 C11 112.46(5) . . ? C4 Si1 C41 112.85(5) . . ? C11 Si1 C41 111.84(5) . . ? C2 C1 Si1 109.29(8) . . ? C1 C2 C3 114.85(10) . . ? C1 C2 C21 122.57(10) . . ? C21 C2 C3 122.51(10) . . ? C4 C3 C2 115.20(10) . . ? C4 C3 C31 122.18(10) . . ? C31 C3 C2 122.60(10) . . ? C3 C4 Si1 109.28(8) . . ? C12 C11 Si1 119.53(9) . . ? C16 C11 Si1 122.71(9) . . ? C16 C11 C12 117.76(11) . . ? C13 C12 C11 120.87(12) . . ? C14 C13 C12 120.35(13) . . ? C15 C14 C13 119.62(12) . . ? C14 C15 C16 120.20(12) . . ? C15 C16 C11 121.18(12) . . ? C22 C21 C2 119.65(11) . . ? C26 C21 C2 122.19(10) . . ? C26 C21 C22 118.11(11) . . ? C23 C22 C21 121.02(12) . . ? C24 C23 C22 120.07(12) . . ? C25 C24 C23 119.59(12) . . ? C24 C25 C26 120.50(12) . . ? C25 C26 C21 120.72(11) . . ? C32 C31 C3 122.18(11) . . ? C32 C31 C36 118.66(11) . . ? C36 C31 C3 119.16(10) . . ? C33 C32 C31 120.33(12) . . ? C34 C33 C32 120.35(12) . . ? C33 C34 C35 119.99(12) . . ? C34 C35 C36 119.74(12) . . ? C35 C36 C31 120.90(11) . . ? C42 C41 Si1 120.21(10) . . ? C46 C41 Si1 122.08(10) . . ? C46 C41 C42 117.67(12) . . ? C43 C42 C41 121.04(14) . . ? C44 C43 C42 120.30(15) . . ? C43 C44 C45 119.67(13) . . ? C44 C45 C46 120.06(14) . . ? C45 C46 C41 121.26(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si1 C1 C2 C3 -2.26(12) . . . . ? Si1 C1 C2 C21 174.93(8) . . . . ? Si1 C11 C12 C13 179.47(11) . . . . ? Si1 C11 C16 C15 179.75(9) . . . . ? Si1 C41 C42 C43 -177.87(11) . . . . ? Si1 C41 C46 C45 178.31(11) . . . . ? C1 Si1 C4 C3 0.01(9) . . . . ? C1 Si1 C11 C12 -54.91(11) . . . . ? C1 Si1 C11 C16 125.63(10) . . . . ? C1 Si1 C41 C42 154.57(10) . . . . ? C1 Si1 C41 C46 -23.16(12) . . . . ? C1 C2 C3 C4 2.44(15) . . . . ? C1 C2 C3 C31 -178.94(10) . . . . ? C1 C2 C21 C22 40.68(16) . . . . ? C1 C2 C21 C26 -136.86(12) . . . . ? C2 C3 C4 Si1 -1.25(12) . . . . ? C2 C3 C31 C32 49.05(16) . . . . ? C2 C3 C31 C36 -130.85(11) . . . . ? C2 C21 C22 C23 -177.90(11) . . . . ? C2 C21 C26 C25 177.88(11) . . . . ? C3 C2 C21 C22 -142.35(11) . . . . ? C3 C2 C21 C26 40.11(15) . . . . ? C3 C31 C32 C33 -179.79(11) . . . . ? C3 C31 C36 C35 178.36(11) . . . . ? C4 Si1 C1 C2 1.32(9) . . . . ? C4 Si1 C11 C12 47.78(11) . . . . ? C4 Si1 C11 C16 -131.68(10) . . . . ? C4 Si1 C41 C42 53.19(12) . . . . ? C4 Si1 C41 C46 -124.54(11) . . . . ? C4 C3 C31 C32 -132.43(13) . . . . ? C4 C3 C31 C36 47.68(16) . . . . ? C11 Si1 C1 C2 116.93(9) . . . . ? C11 Si1 C4 C3 -117.72(9) . . . . ? C11 Si1 C41 C42 -74.81(11) . . . . ? C11 Si1 C41 C46 107.46(11) . . . . ? C11 C12 C13 C14 0.9(2) . . . . ? C12 C11 C16 C15 0.28(18) . . . . ? C12 C13 C14 C15 0.1(2) . . . . ? C13 C14 C15 C16 -0.9(2) . . . . ? C14 C15 C16 C11 0.69(19) . . . . ? C16 C11 C12 C13 -1.05(19) . . . . ? C21 C2 C3 C4 -174.74(10) . . . . ? C21 C2 C3 C31 3.88(16) . . . . ? C21 C22 C23 C24 0.0(2) . . . . ? C22 C21 C26 C25 0.31(17) . . . . ? C22 C23 C24 C25 0.3(2) . . . . ? C23 C24 C25 C26 -0.3(2) . . . . ? C24 C25 C26 C21 -0.05(18) . . . . ? C26 C21 C22 C23 -0.26(17) . . . . ? C31 C3 C4 Si1 -179.88(8) . . . . ? C31 C32 C33 C34 1.53(19) . . . . ? C32 C31 C36 C35 -1.55(17) . . . . ? C32 C33 C34 C35 -1.7(2) . . . . ? C33 C34 C35 C36 0.3(2) . . . . ? C34 C35 C36 C31 1.36(19) . . . . ? C36 C31 C32 C33 0.11(18) . . . . ? C41 Si1 C1 C2 -114.04(9) . . . . ? C41 Si1 C4 C3 114.60(9) . . . . ? C41 Si1 C11 C12 175.99(10) . . . . ? C41 Si1 C11 C16 -3.47(12) . . . . ? C41 C42 C43 C44 -0.5(2) . . . . ? C42 C41 C46 C45 0.5(2) . . . . ? C42 C43 C44 C45 0.5(2) . . . . ? C43 C44 C45 C46 0.0(2) . . . . ? C44 C45 C46 C41 -0.5(2) . . . . ? C46 C41 C42 C43 0.0(2) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 933862' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_qui1 #TrackingRef '19419_web_deposit_cif_file_1_EnguiZHAO_1365821670.TPS-TMSEP.cif' _audit_creation_date 2011-12-21 _audit_creation_method ; Olex2 1.1-beta (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C39 H34 Si2' _chemical_formula_sum 'C39 H34 Si2' _chemical_formula_weight 558.84 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 18.8276(4) _cell_length_b 11.9360(3) _cell_length_c 15.0270(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.794(2) _cell_angle_gamma 90.00 _cell_volume 3265.01(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4532 _cell_measurement_temperature 173.00(14) _cell_measurement_theta_max 71.5772 _cell_measurement_theta_min 3.3698 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.37088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_unetI/netI 0.0641 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 17680 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.48 _diffrn_reflns_theta_min 4.79 _diffrn_ambient_temperature 173.00(14) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.970 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -24.00 41.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 90.0000 65 #__ type_ start__ end____ width___ exp.time_ 2 omega -84.00 -28.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 77.0000 60.0000 56 #__ type_ start__ end____ width___ exp.time_ 3 omega -124.00 -52.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 -57.0000 60.0000 72 #__ type_ start__ end____ width___ exp.time_ 4 omega 36.00 127.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 38.0000 0.0000 91 #__ type_ start__ end____ width___ exp.time_ 5 omega -139.00 -53.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 90.0000 86 #__ type_ start__ end____ width___ exp.time_ 6 omega 37.00 72.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 0.0000 35 #__ type_ start__ end____ width___ exp.time_ 7 omega 38.00 85.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -111.0000 -30.0000 47 #__ type_ start__ end____ width___ exp.time_ 8 omega 123.00 149.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 50.0000 26 #__ type_ start__ end____ width___ exp.time_ 9 omega 37.00 63.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 10 omega 38.00 70.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 120.0000 32 #__ type_ start__ end____ width___ exp.time_ 11 omega 38.00 148.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -90.0000 110 #__ type_ start__ end____ width___ exp.time_ 12 omega 39.00 68.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -90.0000 29 #__ type_ start__ end____ width___ exp.time_ 13 omega 42.00 177.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 12.0000 0.0000 135 #__ type_ start__ end____ width___ exp.time_ 14 omega 39.00 71.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 150.0000 32 #__ type_ start__ end____ width___ exp.time_ 15 omega 37.00 70.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 30.0000 33 #__ type_ start__ end____ width___ exp.time_ 16 omega 40.00 71.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 90.0000 31 #__ type_ start__ end____ width___ exp.time_ 17 omega 46.00 78.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -60.0000 32 #__ type_ start__ end____ width___ exp.time_ 18 omega 88.00 178.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 50.0000 30.0000 90 #__ type_ start__ end____ width___ exp.time_ 19 omega 40.00 104.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 50.0000 64 #__ type_ start__ end____ width___ exp.time_ 20 omega -16.00 61.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -38.0000 -150.0000 77 #__ type_ start__ end____ width___ exp.time_ 21 omega 38.00 149.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 117.0000 111 #__ type_ start__ end____ width___ exp.time_ 22 omega -65.00 -40.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 57.0000 150.0000 25 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0461359000 _diffrn_orient_matrix_UB_12 0.0703245000 _diffrn_orient_matrix_UB_13 0.0681174000 _diffrn_orient_matrix_UB_21 0.0922547000 _diffrn_orient_matrix_UB_22 -0.0590409000 _diffrn_orient_matrix_UB_23 0.0041241000 _diffrn_orient_matrix_UB_31 0.0244432000 _diffrn_orient_matrix_UB_32 0.0906708000 _diffrn_orient_matrix_UB_33 -0.0501329000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 30 _diffrn_source_power 1.5 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4495 _reflns_number_total 5703 _reflns_odcompleteness_completeness 98.05 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.521 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.059 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 373 _refine_ls_number_reflns 5703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0570 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1425 _refine_ls_wR_factor_ref 0.1556 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Si1 Si 0.19827(3) 0.39602(5) 0.42394(4) 0.03666(17) Uani 1 1 d . . . Si2 Si 0.52707(3) 0.29382(6) 0.02281(5) 0.04604(19) Uani 1 1 d . . . C1 C 0.20547(11) 0.48075(17) 0.32092(14) 0.0370(4) Uani 1 1 d . . . C2 C 0.14598(11) 0.54998(17) 0.29834(14) 0.0357(4) Uani 1 1 d . . . C3 C 0.09159(11) 0.53741(17) 0.35608(14) 0.0358(4) Uani 1 1 d . . . C4 C 0.10765(11) 0.45866(18) 0.42227(14) 0.0380(4) Uani 1 1 d . . . H4 H 0.0775 0.4384 0.4617 0.046 Uiso 1 1 calc R . . C10 C 0.48708(18) 0.3273(3) -0.1007(2) 0.0673(7) Uani 1 1 d . . . H10A H 0.4362 0.3007 -0.1194 0.101 Uiso 1 1 calc R . . H10B H 0.5158 0.2903 -0.1381 0.101 Uiso 1 1 calc R . . H10C H 0.4881 0.4085 -0.1097 0.101 Uiso 1 1 calc R . . C11 C 0.26288(11) 0.46875(17) 0.27103(15) 0.0374(4) Uani 1 1 d . . . C12 C 0.24750(11) 0.46904(19) 0.17477(15) 0.0412(5) Uani 1 1 d . . . H12 H 0.1988 0.4841 0.1398 0.049 Uiso 1 1 calc R . . C13 C 0.30121(12) 0.44803(19) 0.12971(16) 0.0439(5) Uani 1 1 d . . . H13 H 0.2890 0.4479 0.0643 0.053 Uiso 1 1 calc R . . C14 C 0.37355(12) 0.42683(19) 0.17894(16) 0.0416(5) Uani 1 1 d . . . C15 C 0.39019(12) 0.4291(2) 0.27482(17) 0.0460(5) Uani 1 1 d . . . H15 H 0.4393 0.4170 0.3096 0.055 Uiso 1 1 calc R . . C16 C 0.33587(12) 0.4488(2) 0.31972(16) 0.0452(5) Uani 1 1 d . . . H16 H 0.3483 0.4489 0.3851 0.054 Uiso 1 1 calc R . . C17 C 0.42736(13) 0.39455(19) 0.13138(18) 0.0463(5) Uani 1 1 d . . . C18 C 0.47019(13) 0.3617(2) 0.08990(18) 0.0486(5) Uani 1 1 d . . . C20 C 0.5211(2) 0.1418(2) 0.0420(3) 0.0749(9) Uani 1 1 d . . . H20A H 0.5444 0.1244 0.1066 0.112 Uiso 1 1 calc R . . H20B H 0.5463 0.1012 0.0023 0.112 Uiso 1 1 calc R . . H20C H 0.4693 0.1191 0.0272 0.112 Uiso 1 1 calc R . . C21 C 0.13502(12) 0.63392(18) 0.22319(15) 0.0396(5) Uani 1 1 d . . . C22 C 0.18677(14) 0.7180(2) 0.22732(19) 0.0506(6) Uani 1 1 d . . . H22 H 0.2288 0.7211 0.2782 0.061 Uiso 1 1 calc R . . C23 C 0.17776(18) 0.7970(2) 0.1584(2) 0.0656(8) Uani 1 1 d . . . H23 H 0.2126 0.8557 0.1632 0.079 Uiso 1 1 calc R . . C24 C 0.11839(18) 0.7914(2) 0.0826(2) 0.0694(8) Uani 1 1 d . . . H24 H 0.1132 0.8444 0.0342 0.083 Uiso 1 1 calc R . . C25 C 0.06663(16) 0.7085(3) 0.07744(19) 0.0636(7) Uani 1 1 d . . . H25 H 0.0257 0.7043 0.0253 0.076 Uiso 1 1 calc R . . C26 C 0.07398(13) 0.6311(2) 0.14779(16) 0.0489(5) Uani 1 1 d . . . H26 H 0.0372 0.5758 0.1447 0.059 Uiso 1 1 calc R . . C30 C 0.62247(15) 0.3472(3) 0.0606(3) 0.0789(10) Uani 1 1 d . . . H30A H 0.6222 0.4291 0.0554 0.118 Uiso 1 1 calc R . . H30B H 0.6518 0.3153 0.0215 0.118 Uiso 1 1 calc R . . H30C H 0.6439 0.3256 0.1247 0.118 Uiso 1 1 calc R . . C31 C 0.02515(12) 0.60961(19) 0.34227(14) 0.0409(5) Uani 1 1 d . . . C32 C 0.02800(15) 0.7256(2) 0.32879(17) 0.0516(6) Uani 1 1 d . . . H32 H 0.0726 0.7599 0.3247 0.062 Uiso 1 1 calc R . . C33 C -0.03473(19) 0.7899(3) 0.3215(2) 0.0674(8) Uani 1 1 d . . . H33 H -0.0328 0.8684 0.3120 0.081 Uiso 1 1 calc R . . C34 C -0.09973(17) 0.7415(3) 0.32774(19) 0.0728(9) Uani 1 1 d . . . H34 H -0.1422 0.7864 0.3231 0.087 Uiso 1 1 calc R . . C35 C -0.10281(15) 0.6274(3) 0.34079(19) 0.0654(8) Uani 1 1 d . . . H35 H -0.1474 0.5937 0.3454 0.079 Uiso 1 1 calc R . . C36 C -0.04092(12) 0.5621(2) 0.34723(16) 0.0503(6) Uani 1 1 d . . . H36 H -0.0438 0.4834 0.3552 0.060 Uiso 1 1 calc R . . C41 C 0.19698(11) 0.24052(19) 0.40785(15) 0.0413(5) Uani 1 1 d . . . C42 C 0.24765(15) 0.1863(2) 0.36999(19) 0.0524(6) Uani 1 1 d . . . H42 H 0.2847 0.2290 0.3531 0.063 Uiso 1 1 calc R . . C43 C 0.24551(17) 0.0713(2) 0.3562(2) 0.0630(7) Uani 1 1 d . . . H43 H 0.2801 0.0362 0.3291 0.076 Uiso 1 1 calc R . . C44 C 0.19275(16) 0.0083(2) 0.3821(2) 0.0641(8) Uani 1 1 d . . . H44 H 0.1914 -0.0707 0.3738 0.077 Uiso 1 1 calc R . . C45 C 0.14222(15) 0.0597(2) 0.4200(2) 0.0635(7) Uani 1 1 d . . . H45 H 0.1058 0.0162 0.4376 0.076 Uiso 1 1 calc R . . C46 C 0.14409(13) 0.1758(2) 0.43276(19) 0.0524(6) Uani 1 1 d . . . H46 H 0.1087 0.2106 0.4588 0.063 Uiso 1 1 calc R . . C51 C 0.27224(11) 0.43760(19) 0.52849(14) 0.0396(4) Uani 1 1 d . . . C52 C 0.29315(14) 0.5489(2) 0.54339(18) 0.0534(6) Uani 1 1 d . . . H52 H 0.2697 0.6043 0.5004 0.064 Uiso 1 1 calc R . . C53 C 0.34786(15) 0.5807(3) 0.6202(2) 0.0612(7) Uani 1 1 d . . . H53 H 0.3616 0.6572 0.6292 0.073 Uiso 1 1 calc R . . C54 C 0.38223(14) 0.5019(3) 0.68330(19) 0.0605(7) Uani 1 1 d . . . H54 H 0.4195 0.5236 0.7359 0.073 Uiso 1 1 calc R . . C55 C 0.36196(18) 0.3911(3) 0.6694(2) 0.0735(9) Uani 1 1 d . . . H55 H 0.3856 0.3360 0.7125 0.088 Uiso 1 1 calc R . . C56 C 0.30736(16) 0.3597(2) 0.59285(19) 0.0602(7) Uani 1 1 d . . . H56 H 0.2937 0.2830 0.5844 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0398(3) 0.0393(3) 0.0308(3) 0.0036(2) 0.0089(2) 0.0057(2) Si2 0.0443(3) 0.0486(4) 0.0479(4) -0.0057(3) 0.0168(3) 0.0004(2) C1 0.0387(10) 0.0413(11) 0.0304(10) 0.0000(8) 0.0079(8) 0.0005(8) C2 0.0385(10) 0.0363(10) 0.0308(10) -0.0029(8) 0.0063(8) -0.0007(8) C3 0.0394(10) 0.0376(10) 0.0291(10) -0.0030(8) 0.0062(8) 0.0004(8) C4 0.0402(10) 0.0426(11) 0.0328(10) 0.0019(8) 0.0125(8) 0.0044(8) C10 0.0846(19) 0.0645(17) 0.0517(16) -0.0028(13) 0.0154(14) -0.0042(14) C11 0.0414(10) 0.0361(10) 0.0353(11) 0.0005(8) 0.0109(8) 0.0013(8) C12 0.0423(10) 0.0455(11) 0.0343(11) -0.0011(9) 0.0069(8) 0.0023(9) C13 0.0497(11) 0.0478(12) 0.0357(11) -0.0024(9) 0.0136(9) 0.0002(10) C14 0.0428(11) 0.0417(11) 0.0433(12) -0.0037(9) 0.0162(9) -0.0023(9) C15 0.0375(10) 0.0537(13) 0.0452(13) 0.0000(10) 0.0079(9) 0.0030(9) C16 0.0451(11) 0.0546(13) 0.0352(11) 0.0009(10) 0.0088(9) 0.0029(10) C17 0.0481(12) 0.0433(12) 0.0489(13) -0.0033(10) 0.0148(10) -0.0033(9) C18 0.0483(12) 0.0507(13) 0.0503(13) -0.0040(11) 0.0194(10) -0.0001(10) C20 0.100(2) 0.0524(15) 0.083(2) 0.0057(15) 0.0420(19) 0.0170(15) C21 0.0434(11) 0.0412(11) 0.0363(11) 0.0032(9) 0.0140(9) 0.0052(9) C22 0.0568(13) 0.0474(13) 0.0510(14) 0.0033(10) 0.0200(11) -0.0018(10) C23 0.0821(19) 0.0499(15) 0.075(2) 0.0159(13) 0.0392(16) -0.0001(13) C24 0.091(2) 0.0645(17) 0.0630(18) 0.0289(14) 0.0384(16) 0.0220(15) C25 0.0642(15) 0.087(2) 0.0406(14) 0.0188(13) 0.0154(12) 0.0232(14) C26 0.0486(12) 0.0606(14) 0.0372(12) 0.0080(10) 0.0105(9) 0.0073(10) C30 0.0453(14) 0.110(3) 0.082(2) -0.028(2) 0.0175(14) -0.0078(15) C31 0.0476(11) 0.0482(12) 0.0268(10) 0.0015(8) 0.0093(8) 0.0096(9) C32 0.0679(15) 0.0474(12) 0.0401(12) 0.0018(10) 0.0148(11) 0.0141(11) C33 0.095(2) 0.0617(16) 0.0439(14) 0.0034(12) 0.0141(14) 0.0350(15) C34 0.0747(19) 0.103(2) 0.0403(14) 0.0053(14) 0.0137(12) 0.0499(18) C35 0.0483(13) 0.105(2) 0.0441(14) 0.0078(14) 0.0130(11) 0.0230(14) C36 0.0464(12) 0.0688(15) 0.0363(12) 0.0068(11) 0.0114(9) 0.0110(11) C41 0.0423(10) 0.0410(11) 0.0366(11) 0.0044(9) 0.0028(8) 0.0071(9) C42 0.0606(14) 0.0474(13) 0.0495(14) 0.0036(11) 0.0146(11) 0.0081(11) C43 0.0781(17) 0.0539(15) 0.0558(16) -0.0019(12) 0.0149(13) 0.0192(13) C44 0.0766(17) 0.0413(13) 0.0631(17) -0.0036(12) -0.0030(14) 0.0071(12) C45 0.0580(14) 0.0503(14) 0.0737(19) 0.0059(13) 0.0011(13) -0.0084(12) C46 0.0469(12) 0.0496(13) 0.0586(15) 0.0015(11) 0.0093(11) 0.0036(10) C51 0.0410(10) 0.0462(11) 0.0321(10) -0.0023(9) 0.0103(8) 0.0036(9) C52 0.0614(14) 0.0520(14) 0.0440(13) 0.0027(11) 0.0083(11) -0.0014(11) C53 0.0624(15) 0.0681(16) 0.0531(15) -0.0124(13) 0.0147(12) -0.0178(13) C54 0.0494(13) 0.087(2) 0.0408(13) -0.0135(13) 0.0044(10) -0.0013(13) C55 0.083(2) 0.0744(19) 0.0479(16) -0.0015(14) -0.0118(14) 0.0195(16) C56 0.0756(17) 0.0506(14) 0.0448(14) 0.0015(11) -0.0022(12) 0.0089(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.883(2) . ? Si1 C4 1.857(2) . ? Si1 C41 1.871(2) . ? Si1 C51 1.881(2) . ? Si2 C10 1.860(3) . ? Si2 C18 1.836(2) . ? Si2 C20 1.845(3) . ? Si2 C30 1.853(3) . ? C1 C2 1.363(3) . ? C1 C11 1.471(3) . ? C2 C3 1.509(3) . ? C2 C21 1.484(3) . ? C3 C4 1.346(3) . ? C3 C31 1.489(3) . ? C11 C12 1.401(3) . ? C11 C16 1.403(3) . ? C12 C13 1.376(3) . ? C13 C14 1.397(3) . ? C14 C15 1.394(3) . ? C14 C17 1.434(3) . ? C15 C16 1.381(3) . ? C17 C18 1.204(4) . ? C21 C22 1.389(3) . ? C21 C26 1.393(3) . ? C22 C23 1.379(4) . ? C23 C24 1.379(5) . ? C24 C25 1.377(4) . ? C25 C26 1.383(4) . ? C31 C32 1.402(3) . ? C31 C36 1.386(3) . ? C32 C33 1.389(4) . ? C33 C34 1.378(5) . ? C34 C35 1.378(5) . ? C35 C36 1.385(4) . ? C41 C42 1.389(3) . ? C41 C46 1.386(3) . ? C42 C43 1.387(4) . ? C43 C44 1.379(4) . ? C44 C45 1.372(4) . ? C45 C46 1.398(4) . ? C51 C52 1.388(3) . ? C51 C56 1.382(3) . ? C52 C53 1.389(4) . ? C53 C54 1.374(4) . ? C54 C55 1.378(4) . ? C55 C56 1.384(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Si1 C1 91.80(9) . . ? C4 Si1 C41 114.58(10) . . ? C4 Si1 C51 112.76(9) . . ? C41 Si1 C1 115.33(10) . . ? C41 Si1 C51 110.62(10) . . ? C51 Si1 C1 110.59(10) . . ? C18 Si2 C10 107.99(14) . . ? C18 Si2 C20 106.31(13) . . ? C18 Si2 C30 109.61(13) . . ? C20 Si2 C10 109.98(16) . . ? C20 Si2 C30 112.57(17) . . ? C30 Si2 C10 110.22(17) . . ? C2 C1 Si1 107.65(15) . . ? C2 C1 C11 126.58(19) . . ? C11 C1 Si1 125.68(15) . . ? C1 C2 C3 115.57(18) . . ? C1 C2 C21 123.0(2) . . ? C21 C2 C3 121.44(18) . . ? C4 C3 C2 115.92(18) . . ? C4 C3 C31 122.0(2) . . ? C31 C3 C2 122.10(18) . . ? C3 C4 Si1 108.87(16) . . ? C12 C11 C1 122.74(18) . . ? C12 C11 C16 117.1(2) . . ? C16 C11 C1 120.01(19) . . ? C13 C12 C11 121.6(2) . . ? C12 C13 C14 120.8(2) . . ? C13 C14 C17 120.1(2) . . ? C15 C14 C13 118.4(2) . . ? C15 C14 C17 121.3(2) . . ? C16 C15 C14 120.6(2) . . ? C15 C16 C11 121.5(2) . . ? C18 C17 C14 176.1(2) . . ? C17 C18 Si2 171.8(2) . . ? C22 C21 C2 119.6(2) . . ? C22 C21 C26 118.5(2) . . ? C26 C21 C2 121.9(2) . . ? C23 C22 C21 120.7(3) . . ? C24 C23 C22 120.4(3) . . ? C25 C24 C23 119.6(2) . . ? C24 C25 C26 120.3(3) . . ? C25 C26 C21 120.4(2) . . ? C32 C31 C3 122.0(2) . . ? C36 C31 C3 119.3(2) . . ? C36 C31 C32 118.7(2) . . ? C33 C32 C31 119.6(3) . . ? C34 C33 C32 121.0(3) . . ? C35 C34 C33 119.6(2) . . ? C34 C35 C36 120.1(3) . . ? C35 C36 C31 121.1(3) . . ? C42 C41 Si1 121.84(19) . . ? C46 C41 Si1 120.33(18) . . ? C46 C41 C42 117.8(2) . . ? C43 C42 C41 121.7(3) . . ? C44 C43 C42 119.5(3) . . ? C45 C44 C43 119.9(3) . . ? C44 C45 C46 120.3(3) . . ? C41 C46 C45 120.7(2) . . ? C52 C51 Si1 120.43(17) . . ? C56 C51 Si1 121.79(19) . . ? C56 C51 C52 117.8(2) . . ? C51 C52 C53 121.0(2) . . ? C54 C53 C52 120.4(3) . . ? C53 C54 C55 119.3(2) . . ? C54 C55 C56 120.3(3) . . ? C51 C56 C55 121.4(3) . . ? _database_code_depnum_ccdc_archive 'CCDC 933863' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_qui2 #TrackingRef '19420_web_deposit_cif_file_2_EnguiZHAO_1365821670.TPS-2TMSEP.cif' _audit_creation_date 2012-01-09 _audit_creation_method ; Olex2 1.1-beta (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C50 H46 Si3, 2(C H2 Cl2)' _chemical_formula_sum 'C52 H50 Cl4 Si3' _chemical_formula_weight 900.99 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y, -z' 3 'x+1/2, y+1/2, z+1/2' 4 '-x+1, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x-1/2, -y, z' 7 '-x+1/2, -y+1/2, -z+1/2' 8 'x, -y+1/2, z+1/2' _cell_length_a 11.2522(2) _cell_length_b 24.9636(4) _cell_length_c 18.4374(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.987(2) _cell_angle_gamma 90.00 _cell_volume 5002.81(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8619 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 71.4589 _cell_measurement_theta_min 3.0455 _exptl_absorpt_coefficient_mu 3.084 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.28463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1888 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_unetI/netI 0.0201 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 15006 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.00 _diffrn_reflns_theta_min 3.05 _diffrn_ambient_temperature 173.00(14) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 37.00 73.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 150.0000 36 #__ type_ start__ end____ width___ exp.time_ 2 omega -69.00 -22.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 -57.0000 -180.0000 47 #__ type_ start__ end____ width___ exp.time_ 3 omega -21.00 18.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 -57.0000 -180.0000 39 #__ type_ start__ end____ width___ exp.time_ 4 omega -112.00 -18.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 125.0000 -180.0000 94 #__ type_ start__ end____ width___ exp.time_ 5 omega 25.00 124.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 77.0000 60.0000 99 #__ type_ start__ end____ width___ exp.time_ 6 omega -7.00 79.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -66.0000 -77.0000 86 #__ type_ start__ end____ width___ exp.time_ 7 omega -6.00 68.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -38.0000 90.0000 74 #__ type_ start__ end____ width___ exp.time_ 8 omega -136.00 -44.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 12.0000 150.0000 92 #__ type_ start__ end____ width___ exp.time_ 9 omega 89.00 178.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 38.0000 90.0000 89 #__ type_ start__ end____ width___ exp.time_ 10 omega 51.00 83.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 30.0000 32 #__ type_ start__ end____ width___ exp.time_ 11 omega 88.00 118.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -120.0000 30 #__ type_ start__ end____ width___ exp.time_ 12 omega 38.00 70.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -180.0000 32 #__ type_ start__ end____ width___ exp.time_ 13 omega 44.00 73.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 90.0000 29 #__ type_ start__ end____ width___ exp.time_ 14 omega 44.00 71.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 150.0000 27 #__ type_ start__ end____ width___ exp.time_ 15 omega 39.00 67.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -120.0000 28 #__ type_ start__ end____ width___ exp.time_ 16 omega 41.00 85.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -111.0000 -30.0000 44 #__ type_ start__ end____ width___ exp.time_ 17 omega 38.00 66.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -150.0000 28 #__ type_ start__ end____ width___ exp.time_ 18 omega 88.00 172.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 64.0000 -180.0000 84 #__ type_ start__ end____ width___ exp.time_ 19 omega 39.00 148.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 0.0000 109 #__ type_ start__ end____ width___ exp.time_ 20 omega 39.00 69.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 60.0000 30 #__ type_ start__ end____ width___ exp.time_ 21 omega 93.00 148.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 60.0000 55 #__ type_ start__ end____ width___ exp.time_ 22 omega 84.00 149.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 150.0000 65 #__ type_ start__ end____ width___ exp.time_ 23 omega 38.00 74.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -60.0000 36 #__ type_ start__ end____ width___ exp.time_ 24 omega 80.00 163.00 1.0000 22.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 77.0000 120.0000 83 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0303795000 _diffrn_orient_matrix_UB_12 -0.0462879000 _diffrn_orient_matrix_UB_13 0.0591640000 _diffrn_orient_matrix_UB_21 -0.0786565000 _diffrn_orient_matrix_UB_22 0.0081467000 _diffrn_orient_matrix_UB_23 -0.0992728000 _diffrn_orient_matrix_UB_31 0.0192262000 _diffrn_orient_matrix_UB_32 -0.0399950000 _diffrn_orient_matrix_UB_33 -0.0887332000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 35 _diffrn_source_power 1.75 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4105 _reflns_number_total 4381 _reflns_odcompleteness_completeness 99.55 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.685 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 270 _refine_ls_number_reflns 4381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0587 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+6.2458P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1619 _refine_ls_wR_factor_ref 0.1644 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Si1 Si 0.2500 0.37203(3) 0.0000 0.0327(2) Uani 1 2 d S . . Si2 Si 0.50753(10) 0.40619(4) 0.56640(4) 0.0704(3) Uani 1 1 d . . . C1 C 0.3841(2) 0.32801(8) -0.00069(11) 0.0364(4) Uani 1 1 d . . . C2 C 0.5038(2) 0.33905(10) 0.04043(13) 0.0432(5) Uani 1 1 d . . . H2 H 0.5195 0.3696 0.0722 0.052 Uiso 1 1 calc R . . C3 C 0.6010(2) 0.30568(12) 0.03547(16) 0.0552(6) Uani 1 1 d . . . H3 H 0.6824 0.3135 0.0639 0.066 Uiso 1 1 calc R . . C4 C 0.5788(3) 0.26152(11) -0.01066(17) 0.0575(7) Uani 1 1 d . . . H4 H 0.6450 0.2388 -0.0139 0.069 Uiso 1 1 calc R . . C5 C 0.4614(3) 0.25011(10) -0.05216(16) 0.0557(6) Uani 1 1 d . . . H5 H 0.4466 0.2199 -0.0845 0.067 Uiso 1 1 calc R . . C6 C 0.3653(2) 0.28266(9) -0.04666(14) 0.0465(5) Uani 1 1 d . . . H6 H 0.2842 0.2741 -0.0748 0.056 Uiso 1 1 calc R . . C10 C 0.28495(18) 0.42413(8) 0.07595(10) 0.0334(4) Uani 1 1 d . . . C11 C 0.32795(19) 0.41561(8) 0.15810(10) 0.0329(4) Uani 1 1 d . . . C12 C 0.2611(2) 0.38390(9) 0.19576(12) 0.0440(5) Uani 1 1 d . . . H12 H 0.1897 0.3657 0.1680 0.053 Uiso 1 1 calc R . . C13 C 0.2976(2) 0.37862(10) 0.27336(12) 0.0469(6) Uani 1 1 d . . . H13 H 0.2499 0.3575 0.2982 0.056 Uiso 1 1 calc R . . C14 C 0.4033(2) 0.40398(9) 0.31510(11) 0.0402(5) Uani 1 1 d . . . C15 C 0.4731(2) 0.43360(9) 0.27733(12) 0.0403(5) Uani 1 1 d . . . H15 H 0.5475 0.4499 0.3047 0.048 Uiso 1 1 calc R . . C16 C 0.4353(2) 0.43962(9) 0.20027(11) 0.0370(5) Uani 1 1 d . . . H16 H 0.4835 0.4606 0.1756 0.044 Uiso 1 1 calc R . . C17 C 0.4388(3) 0.40102(10) 0.39570(13) 0.0477(6) Uani 1 1 d . . . C18 C 0.4669(3) 0.40072(11) 0.46336(14) 0.0570(7) Uani 1 1 d . . . C20 C 0.27033(17) 0.47278(8) 0.04241(10) 0.0317(4) Uani 1 1 d . . . C21 C 0.29269(19) 0.52403(8) 0.08506(11) 0.0338(4) Uani 1 1 d . . . C22 C 0.2294(2) 0.53526(9) 0.13905(12) 0.0386(5) Uani 1 1 d . . . H22 H 0.1693 0.5108 0.1468 0.046 Uiso 1 1 calc R . . C23 C 0.2532(2) 0.58172(10) 0.18157(13) 0.0468(5) Uani 1 1 d . . . H23 H 0.2091 0.5889 0.2180 0.056 Uiso 1 1 calc R . . C24 C 0.3406(3) 0.61755(10) 0.17121(14) 0.0505(6) Uani 1 1 d . . . H24 H 0.3577 0.6491 0.2009 0.061 Uiso 1 1 calc R . . C25 C 0.4032(2) 0.60728(10) 0.11735(14) 0.0491(6) Uani 1 1 d . . . H25 H 0.4631 0.6320 0.1099 0.059 Uiso 1 1 calc R . . C26 C 0.3795(2) 0.56109(9) 0.07410(12) 0.0406(5) Uani 1 1 d . . . H26 H 0.4224 0.5546 0.0369 0.049 Uiso 1 1 calc R . . C31 C 0.3933(5) 0.45195(18) 0.5921(2) 0.1023(14) Uani 1 1 d . . . H31A H 0.4025 0.4881 0.5735 0.153 Uiso 1 1 calc R . . H31B H 0.4078 0.4529 0.6468 0.153 Uiso 1 1 calc R . . H31C H 0.3099 0.4389 0.5694 0.153 Uiso 1 1 calc R . . C32 C 0.4888(7) 0.34092(17) 0.6072(2) 0.142(3) Uani 1 1 d . . . H32A H 0.4054 0.3275 0.5852 0.213 Uiso 1 1 calc R . . H32B H 0.5021 0.3447 0.6616 0.213 Uiso 1 1 calc R . . H32C H 0.5489 0.3156 0.5967 0.213 Uiso 1 1 calc R . . C33 C 0.6577(5) 0.4415(3) 0.5978(2) 0.1196(18) Uani 1 1 d . . . H33A H 0.7223 0.4196 0.5857 0.179 Uiso 1 1 calc R . . H33B H 0.6771 0.4473 0.6522 0.179 Uiso 1 1 calc R . . H33C H 0.6528 0.4761 0.5721 0.179 Uiso 1 1 calc R . . C1S C 0.5290(5) 0.28592(15) 0.2268(2) 0.0915(12) Uani 1 1 d . . . H1SA H 0.5560 0.2700 0.1845 0.110 Uiso 1 1 calc R . . H1SB H 0.4945 0.3218 0.2109 0.110 Uiso 1 1 calc R . . Cl1S Cl 0.41232(12) 0.24491(4) 0.24715(7) 0.0989(4) Uani 1 1 d . . . Cl2S Cl 0.65611(12) 0.29266(7) 0.30433(8) 0.1209(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0447(4) 0.0314(4) 0.0212(4) 0.000 0.0072(3) 0.000 Si2 0.1036(7) 0.0803(6) 0.0233(3) 0.0051(3) 0.0093(4) -0.0165(5) C1 0.0481(11) 0.0352(10) 0.0262(9) 0.0040(8) 0.0104(8) -0.0002(8) C2 0.0480(12) 0.0466(12) 0.0370(11) -0.0032(9) 0.0147(9) -0.0057(9) C3 0.0416(12) 0.0675(16) 0.0576(15) 0.0008(13) 0.0146(11) -0.0013(11) C4 0.0557(14) 0.0533(14) 0.0689(17) 0.0035(12) 0.0258(13) 0.0105(11) C5 0.0660(16) 0.0416(13) 0.0622(16) -0.0069(11) 0.0212(13) 0.0053(11) C6 0.0526(13) 0.0399(12) 0.0435(12) -0.0046(9) 0.0064(10) 0.0030(10) C10 0.0410(10) 0.0366(10) 0.0225(9) -0.0014(7) 0.0081(8) -0.0009(8) C11 0.0453(11) 0.0326(10) 0.0210(9) 0.0000(7) 0.0088(8) 0.0015(8) C12 0.0543(13) 0.0473(12) 0.0292(11) -0.0001(9) 0.0087(9) -0.0131(10) C13 0.0648(15) 0.0489(13) 0.0284(11) 0.0033(9) 0.0148(10) -0.0126(11) C14 0.0589(13) 0.0379(11) 0.0233(10) 0.0007(8) 0.0095(9) 0.0019(9) C15 0.0473(12) 0.0436(11) 0.0272(10) -0.0012(8) 0.0043(8) -0.0021(9) C16 0.0439(11) 0.0417(11) 0.0265(10) 0.0021(8) 0.0107(8) -0.0029(8) C17 0.0696(15) 0.0438(12) 0.0284(12) 0.0023(9) 0.0102(10) -0.0024(11) C18 0.0840(19) 0.0551(15) 0.0292(12) 0.0060(10) 0.0102(11) -0.0056(13) C20 0.0363(10) 0.0362(10) 0.0235(10) -0.0006(7) 0.0093(7) -0.0011(8) C21 0.0412(11) 0.0338(10) 0.0246(9) 0.0005(7) 0.0054(8) 0.0005(8) C22 0.0447(11) 0.0393(11) 0.0322(10) -0.0017(8) 0.0108(9) 0.0010(9) C23 0.0618(14) 0.0460(12) 0.0325(11) -0.0066(9) 0.0120(10) 0.0079(10) C24 0.0676(15) 0.0396(12) 0.0379(12) -0.0089(9) 0.0019(11) -0.0027(11) C25 0.0575(14) 0.0416(12) 0.0439(13) -0.0006(10) 0.0054(10) -0.0101(10) C26 0.0484(12) 0.0425(11) 0.0311(10) 0.0017(8) 0.0107(9) -0.0062(9) C31 0.161(4) 0.094(3) 0.061(2) -0.0224(19) 0.045(2) -0.017(3) C32 0.316(9) 0.069(2) 0.0457(19) 0.0138(17) 0.056(3) -0.006(3) C33 0.124(4) 0.163(5) 0.056(2) 0.006(3) -0.006(2) -0.025(3) C1S 0.142(4) 0.068(2) 0.079(2) 0.0133(17) 0.054(2) 0.017(2) Cl1S 0.1338(9) 0.0692(5) 0.1043(8) -0.0101(5) 0.0500(7) -0.0054(5) Cl2S 0.1074(9) 0.1434(11) 0.1158(10) 0.0194(8) 0.0357(7) 0.0071(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.870(2) 2 ? Si1 C1 1.870(2) . ? Si1 C10 1.877(2) . ? Si1 C10 1.877(2) 2 ? Si2 C18 1.840(3) . ? Si2 C31 1.870(5) . ? Si2 C32 1.830(4) . ? Si2 C33 1.860(5) . ? C1 C2 1.391(3) . ? C1 C6 1.397(3) . ? C2 C3 1.397(4) . ? C3 C4 1.375(4) . ? C4 C5 1.374(4) . ? C5 C6 1.378(4) . ? C10 C11 1.481(3) . ? C10 C20 1.354(3) . ? C11 C12 1.394(3) . ? C11 C16 1.392(3) . ? C12 C13 1.389(3) . ? C13 C14 1.391(3) . ? C14 C15 1.390(3) . ? C14 C17 1.438(3) . ? C15 C16 1.382(3) . ? C17 C18 1.205(4) . ? C20 C20 1.512(4) 2 ? C20 C21 1.489(3) . ? C21 C22 1.394(3) . ? C21 C26 1.397(3) . ? C22 C23 1.387(3) . ? C23 C24 1.379(4) . ? C24 C25 1.382(4) . ? C25 C26 1.388(3) . ? C1S Cl1S 1.780(4) . ? C1S Cl2S 1.750(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Si1 C1 108.00(13) 2 . ? C1 Si1 C10 114.58(8) 2 . ? C1 Si1 C10 113.50(9) . . ? C1 Si1 C10 113.50(9) 2 2 ? C1 Si1 C10 114.58(8) . 2 ? C10 Si1 C10 92.26(13) . 2 ? C18 Si2 C31 107.67(17) . . ? C18 Si2 C33 108.64(17) . . ? C32 Si2 C18 109.53(16) . . ? C32 Si2 C31 106.3(3) . . ? C32 Si2 C33 119.0(3) . . ? C33 Si2 C31 105.1(3) . . ? C2 C1 Si1 123.29(17) . . ? C2 C1 C6 117.7(2) . . ? C6 C1 Si1 118.95(17) . . ? C1 C2 C3 120.7(2) . . ? C4 C3 C2 119.9(2) . . ? C5 C4 C3 120.4(2) . . ? C4 C5 C6 119.8(2) . . ? C5 C6 C1 121.6(2) . . ? C11 C10 Si1 127.84(15) . . ? C20 C10 Si1 107.69(14) . . ? C20 C10 C11 124.39(17) . . ? C12 C11 C10 121.01(19) . . ? C16 C11 C10 121.09(18) . . ? C16 C11 C12 117.90(18) . . ? C13 C12 C11 120.9(2) . . ? C12 C13 C14 120.6(2) . . ? C13 C14 C17 121.2(2) . . ? C15 C14 C13 118.57(19) . . ? C15 C14 C17 120.2(2) . . ? C16 C15 C14 120.6(2) . . ? C15 C16 C11 121.31(19) . . ? C18 C17 C14 177.3(3) . . ? C17 C18 Si2 175.3(2) . . ? C10 C20 C20 116.17(11) . 2 ? C10 C20 C21 123.09(17) . . ? C21 C20 C20 120.73(10) . 2 ? C22 C21 C20 120.16(18) . . ? C22 C21 C26 118.36(19) . . ? C26 C21 C20 121.45(18) . . ? C23 C22 C21 120.8(2) . . ? C24 C23 C22 120.3(2) . . ? C23 C24 C25 119.6(2) . . ? C24 C25 C26 120.6(2) . . ? C25 C26 C21 120.3(2) . . ? Cl2S C1S Cl1S 112.0(2) . . ? _database_code_depnum_ccdc_archive 'CCDC 933864'