# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_f120319a _database_code_depnum_ccdc_archive 'CCDC 902888' #TrackingRef 'web_deposit_cif_file_0_Xu-QiongXiao_1348557912.compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 S Si8' _chemical_formula_weight 497.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.746(3) _cell_length_b 9.2220(19) _cell_length_c 14.522(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.438(4) _cell_angle_gamma 90.00 _cell_volume 1660.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4842 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.389 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8923 _exptl_absorpt_correction_T_max 0.9622 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9201 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3079 _reflns_number_gt 2581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3079 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 S1 S 0.2500 0.36352(7) 0.2500 0.0695(3) Uani 1 2 d S . . Si1 Si 0.31932(4) 0.22710(5) 0.15711(3) 0.04687(19) Uani 1 1 d . . . Si2 Si 0.27443(4) -0.01589(5) 0.17709(4) 0.0546(2) Uani 1 1 d . . . Si3 Si 0.50626(4) 0.26426(6) 0.20028(5) 0.0654(2) Uani 1 1 d . . . Si4 Si 0.24492(5) 0.31885(7) 0.00517(4) 0.0685(2) Uani 1 1 d . . . C1 C 0.1586(2) -0.0781(3) 0.08128(19) 0.1006(9) Uani 1 1 d . . . H1A H 0.1792 -0.0773 0.0218 0.151 Uiso 1 1 calc R . . H1B H 0.0983 -0.0143 0.0780 0.151 Uiso 1 1 calc R . . H1C H 0.1387 -0.1748 0.0949 0.151 Uiso 1 1 calc R . . C2 C 0.3903(2) -0.1434(3) 0.1788(2) 0.0998(9) Uani 1 1 d . . . H2A H 0.3678 -0.2412 0.1862 0.150 Uiso 1 1 calc R . . H2B H 0.4494 -0.1189 0.2306 0.150 Uiso 1 1 calc R . . H2C H 0.4128 -0.1352 0.1203 0.150 Uiso 1 1 calc R . . C3 C 0.5666(2) 0.1774(4) 0.3169(2) 0.1215(12) Uani 1 1 d . . . H3A H 0.5586 0.0741 0.3111 0.182 Uiso 1 1 calc R . . H3B H 0.5303 0.2121 0.3636 0.182 Uiso 1 1 calc R . . H3C H 0.6418 0.2015 0.3358 0.182 Uiso 1 1 calc R . . C4 C 0.5691(2) 0.1833(3) 0.1074(3) 0.1150(11) Uani 1 1 d . . . H4A H 0.5296 0.2138 0.0459 0.172 Uiso 1 1 calc R . . H4B H 0.5672 0.0794 0.1114 0.172 Uiso 1 1 calc R . . H4C H 0.6426 0.2152 0.1175 0.172 Uiso 1 1 calc R . . C5 C 0.5361(2) 0.4635(3) 0.2109(3) 0.1068(10) Uani 1 1 d . . . H5A H 0.6126 0.4778 0.2319 0.160 Uiso 1 1 calc R . . H5B H 0.5006 0.5056 0.2560 0.160 Uiso 1 1 calc R . . H5C H 0.5106 0.5089 0.1504 0.160 Uiso 1 1 calc R . . C6 C 0.2853(3) 0.5094(3) -0.0028(2) 0.1298(14) Uani 1 1 d . . . H6A H 0.2476 0.5493 -0.0623 0.195 Uiso 1 1 calc R . . H6B H 0.3616 0.5143 0.0019 0.195 Uiso 1 1 calc R . . H6C H 0.2678 0.5639 0.0480 0.195 Uiso 1 1 calc R . . C7 C 0.0956(3) 0.3136(5) -0.0196(3) 0.1540(18) Uani 1 1 d . . . H7A H 0.0720 0.3527 0.0334 0.231 Uiso 1 1 calc R . . H7B H 0.0714 0.2150 -0.0300 0.231 Uiso 1 1 calc R . . H7C H 0.0660 0.3701 -0.0751 0.231 Uiso 1 1 calc R . . C8 C 0.2906(4) 0.2105(4) -0.0883(2) 0.1512(16) Uani 1 1 d . . . H8A H 0.2624 0.2535 -0.1493 0.227 Uiso 1 1 calc R . . H8B H 0.2646 0.1128 -0.0883 0.227 Uiso 1 1 calc R . . H8C H 0.3679 0.2100 -0.0751 0.227 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 S1 0.0976(6) 0.0454(3) 0.0819(6) 0.000 0.0544(5) 0.000 Si1 0.0485(3) 0.0493(3) 0.0447(3) -0.00011(19) 0.0148(2) -0.00179(18) Si2 0.0659(4) 0.0463(3) 0.0528(3) -0.0076(2) 0.0164(3) -0.0027(2) Si3 0.0499(3) 0.0734(4) 0.0752(5) -0.0027(3) 0.0193(3) -0.0067(2) Si4 0.0829(4) 0.0697(4) 0.0511(4) 0.0114(3) 0.0122(3) -0.0043(3) C1 0.124(2) 0.0915(17) 0.0717(16) -0.0113(13) -0.0067(15) -0.0378(16) C2 0.118(2) 0.0689(13) 0.127(3) -0.0078(14) 0.0578(19) 0.0257(14) C3 0.0743(17) 0.159(3) 0.113(3) 0.031(2) -0.0151(17) -0.0092(18) C4 0.0891(19) 0.120(2) 0.158(3) -0.027(2) 0.074(2) -0.0061(17) C5 0.0918(19) 0.0930(18) 0.134(3) -0.0229(18) 0.0230(18) -0.0309(15) C6 0.191(4) 0.0823(18) 0.102(2) 0.0343(16) 0.004(2) -0.022(2) C7 0.086(2) 0.214(4) 0.139(3) 0.089(3) -0.021(2) -0.010(2) C8 0.236(5) 0.158(3) 0.064(2) -0.005(2) 0.044(3) 0.039(3) _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 S1 Si1 2.1766(7) 2 ? S1 Si1 2.1766(7) . ? Si1 Si3 2.3437(9) . ? Si1 Si2 2.3473(8) . ? Si1 Si4 2.3477(9) . ? Si2 C1 1.868(2) . ? Si2 C2 1.884(2) . ? Si2 Si2 2.3420(11) 2 ? Si3 C3 1.869(3) . ? Si3 C5 1.875(3) . ? Si3 C4 1.876(3) . ? Si4 C6 1.842(3) . ? Si4 C7 1.854(3) . ? Si4 C8 1.884(3) . ? 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 Si1 S1 Si1 109.37(4) 2 . ? S1 Si1 Si3 106.47(3) . . ? S1 Si1 Si2 109.23(3) . . ? Si3 Si1 Si2 111.61(3) . . ? S1 Si1 Si4 103.93(3) . . ? Si3 Si1 Si4 111.24(3) . . ? Si2 Si1 Si4 113.80(3) . . ? C1 Si2 C2 107.41(14) . . ? C1 Si2 Si2 110.07(10) . 2 ? C2 Si2 Si2 111.16(10) . 2 ? C1 Si2 Si1 111.98(9) . . ? C2 Si2 Si1 112.62(8) . . ? Si2 Si2 Si1 103.620(18) 2 . ? C3 Si3 C5 108.20(18) . . ? C3 Si3 C4 109.03(17) . . ? C5 Si3 C4 109.68(15) . . ? C3 Si3 Si1 110.99(10) . . ? C5 Si3 Si1 109.86(10) . . ? C4 Si3 Si1 109.07(11) . . ? C6 Si4 C7 107.60(18) . . ? C6 Si4 C8 108.86(19) . . ? C7 Si4 C8 108.7(2) . . ? C6 Si4 Si1 110.17(11) . . ? C7 Si4 Si1 110.19(11) . . ? C8 Si4 Si1 111.18(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.391 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.041 data_f111230a _database_code_depnum_ccdc_archive 'CCDC 902889' #TrackingRef 'web_deposit_cif_file_1_Xu-QiongXiao_1348557912.compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 Se Si8' _chemical_formula_weight 544.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.8893(6) _cell_length_b 9.0602(3) _cell_length_c 14.6504(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.483(5) _cell_angle_gamma 90.00 _cell_volume 1656.50(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.808 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8157 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3381 _reflns_number_gt 2654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.5283P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3381 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Se1 Se 0.2500 0.11345(4) 0.2500 0.06649(16) Uani 1 2 d S . . Si1 Si 0.32003(5) 0.26776(7) 0.15444(4) 0.04461(17) Uani 1 1 d . . . Si2 Si 0.27255(6) 0.51257(8) 0.17746(5) 0.05145(19) Uani 1 1 d . . . Si4 Si 0.50607(6) 0.23411(9) 0.19917(6) 0.0615(2) Uani 1 1 d . . . Si3 Si 0.24416(7) 0.17844(9) 0.00184(5) 0.0647(2) Uani 1 1 d . . . C6 C 0.5680(3) 0.3232(5) 0.1105(3) 0.1149(14) Uani 1 1 d . . . H6A H 0.6443 0.3110 0.1295 0.172 Uiso 1 1 calc R . . H6B H 0.5508 0.4265 0.1063 0.172 Uiso 1 1 calc R . . H6C H 0.5405 0.2778 0.0500 0.172 Uiso 1 1 calc R . . C7 C 0.3859(3) 0.6446(3) 0.1796(3) 0.0914(11) Uani 1 1 d . . . H7A H 0.4055 0.6397 0.1206 0.137 Uiso 1 1 calc R . . H7B H 0.4464 0.6183 0.2299 0.137 Uiso 1 1 calc R . . H7C H 0.3635 0.7432 0.1894 0.137 Uiso 1 1 calc R . . C4 C 0.5394(3) 0.0332(4) 0.2071(3) 0.0947(11) Uani 1 1 d . . . H4A H 0.6155 0.0210 0.2296 0.142 Uiso 1 1 calc R . . H4B H 0.5156 -0.0109 0.1458 0.142 Uiso 1 1 calc R . . H4C H 0.5042 -0.0137 0.2499 0.142 Uiso 1 1 calc R . . C8 C 0.1542(3) 0.5749(4) 0.0824(2) 0.0953(11) Uani 1 1 d . . . H8A H 0.1356 0.6741 0.0951 0.143 Uiso 1 1 calc R . . H8B H 0.0944 0.5108 0.0809 0.143 Uiso 1 1 calc R . . H8C H 0.1719 0.5715 0.0225 0.143 Uiso 1 1 calc R . . C2 C 0.2866(4) 0.2907(5) -0.0889(2) 0.1394(19) Uani 1 1 d . . . H2A H 0.3632 0.2868 -0.0779 0.209 Uiso 1 1 calc R . . H2B H 0.2644 0.3912 -0.0853 0.209 Uiso 1 1 calc R . . H2C H 0.2542 0.2519 -0.1504 0.209 Uiso 1 1 calc R . . C1 C 0.2862(4) -0.0150(4) -0.0076(3) 0.1135(14) Uani 1 1 d . . . H1A H 0.2560 -0.0505 -0.0704 0.170 Uiso 1 1 calc R . . H1B H 0.2613 -0.0751 0.0366 0.170 Uiso 1 1 calc R . . H1C H 0.3629 -0.0199 0.0061 0.170 Uiso 1 1 calc R . . C5 C 0.5643(3) 0.3172(5) 0.3174(3) 0.1170(15) Uani 1 1 d . . . H5A H 0.5305 0.2749 0.3627 0.176 Uiso 1 1 calc R . . H5B H 0.5525 0.4219 0.3143 0.176 Uiso 1 1 calc R . . H5C H 0.6399 0.2977 0.3360 0.176 Uiso 1 1 calc R . . C3 C 0.0950(3) 0.1812(6) -0.0230(3) 0.141(2) Uani 1 1 d . . . H3A H 0.0707 0.2813 -0.0231 0.211 Uiso 1 1 calc R . . H3B H 0.0727 0.1263 0.0248 0.211 Uiso 1 1 calc R . . H3C H 0.0649 0.1373 -0.0835 0.211 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 Se1 0.0951(3) 0.0410(2) 0.0806(3) 0.000 0.0541(3) 0.000 Si1 0.0469(3) 0.0455(4) 0.0432(3) 0.0003(3) 0.0145(3) 0.0009(3) Si2 0.0602(4) 0.0422(4) 0.0522(4) 0.0075(3) 0.0146(3) 0.0025(3) Si4 0.0477(4) 0.0626(5) 0.0767(5) 0.0036(4) 0.0203(4) 0.0044(3) Si3 0.0806(5) 0.0637(5) 0.0483(4) -0.0085(4) 0.0132(4) 0.0027(4) C6 0.093(3) 0.104(3) 0.175(4) 0.035(3) 0.083(3) 0.010(2) C7 0.105(3) 0.0577(19) 0.123(3) 0.0102(18) 0.051(2) -0.0158(18) C4 0.083(2) 0.079(2) 0.122(3) 0.016(2) 0.026(2) 0.0260(19) C8 0.112(3) 0.088(2) 0.073(2) 0.0147(18) 0.000(2) 0.040(2) C2 0.232(6) 0.129(4) 0.064(2) 0.010(2) 0.048(3) -0.024(4) C1 0.161(4) 0.079(3) 0.091(3) -0.027(2) 0.014(3) 0.013(3) C5 0.069(2) 0.145(4) 0.115(3) -0.039(3) -0.017(2) 0.009(2) C3 0.078(3) 0.201(5) 0.119(3) -0.073(4) -0.019(2) 0.009(3) _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 Se1 Si1 2.3155(7) 2 ? Se1 Si1 2.3155(7) . ? Si1 Si4 2.3423(10) . ? Si1 Si2 2.3475(10) . ? Si1 Si3 2.3485(10) . ? Si2 C8 1.877(3) . ? Si2 C7 1.882(3) . ? Si2 Si2 2.3398(14) 2 ? Si4 C5 1.866(4) . ? Si4 C4 1.867(3) . ? Si4 C6 1.870(3) . ? Si3 C1 1.850(4) . ? Si3 C2 1.861(4) . ? Si3 C3 1.865(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 Si1 Se1 Si1 105.72(4) 2 . ? Se1 Si1 Si4 106.19(3) . . ? Se1 Si1 Si2 109.18(3) . . ? Si4 Si1 Si2 111.60(4) . . ? Se1 Si1 Si3 103.59(3) . . ? Si4 Si1 Si3 112.02(4) . . ? Si2 Si1 Si3 113.63(4) . . ? C8 Si2 C7 107.74(18) . . ? C8 Si2 Si2 109.48(13) . 2 ? C7 Si2 Si2 110.66(12) . 2 ? C8 Si2 Si1 111.73(12) . . ? C7 Si2 Si1 111.97(11) . . ? Si2 Si2 Si1 105.27(2) 2 . ? C5 Si4 C4 107.65(19) . . ? C5 Si4 C6 109.2(2) . . ? C4 Si4 C6 109.41(18) . . ? C5 Si4 Si1 110.69(12) . . ? C4 Si4 Si1 110.34(12) . . ? C6 Si4 Si1 109.52(13) . . ? C1 Si3 C2 108.7(2) . . ? C1 Si3 C3 107.7(2) . . ? C2 Si3 C3 109.0(2) . . ? C1 Si3 Si1 109.74(12) . . ? C2 Si3 Si1 111.40(14) . . ? C3 Si3 Si1 110.15(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.633 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.046 data_f120326a _database_code_depnum_ccdc_archive 'CCDC 902890' #TrackingRef 'web_deposit_cif_file_2_Xu-QiongXiao_1348557912.compound4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 Si8 Te2' _chemical_formula_weight 720.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2346(11) _cell_length_b 15.2729(13) _cell_length_c 19.1413(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.656(2) _cell_angle_gamma 90.00 _cell_volume 3475.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7652 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6955 _exptl_absorpt_correction_T_max 0.7577 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20277 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6789 _reflns_number_gt 5417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0378P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6789 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 0.792 _refine_ls_restrained_S_all 0.792 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Te1 Te 0.038605(18) 0.479427(19) 0.111821(12) 0.05432(11) Uani 1 1 d . . . Te2 Te 0.13096(2) 0.599388(17) 0.214522(12) 0.05557(10) Uani 1 1 d . . . Si1 Si 0.20159(8) 0.49664(7) 0.31939(5) 0.0424(2) Uani 1 1 d . . . Si2 Si 0.05481(8) 0.39788(7) 0.32371(5) 0.0496(2) Uani 1 1 d . . . Si3 Si -0.12425(8) 0.45199(7) 0.26594(5) 0.0509(2) Uani 1 1 d . . . Si4 Si -0.15219(7) 0.46248(6) 0.14036(5) 0.0409(2) Uani 1 1 d . . . Si5 Si 0.36785(9) 0.43158(8) 0.30242(6) 0.0570(3) Uani 1 1 d . . . Si6 Si 0.24262(9) 0.59164(8) 0.41974(5) 0.0580(3) Uani 1 1 d . . . Si7 Si -0.26230(9) 0.58342(8) 0.08930(6) 0.0562(3) Uani 1 1 d . . . Si8 Si -0.22638(9) 0.33316(8) 0.07968(6) 0.0579(3) Uani 1 1 d . . . C1 C 0.3519(4) 0.6745(4) 0.4113(3) 0.0968(17) Uani 1 1 d . . . H1A H 0.3544 0.7199 0.4462 0.145 Uiso 1 1 calc R . . H1B H 0.3332 0.6994 0.3639 0.145 Uiso 1 1 calc R . . H1C H 0.4241 0.6465 0.4193 0.145 Uiso 1 1 calc R . . C2 C 0.2948(6) 0.5264(4) 0.5043(2) 0.110(2) Uani 1 1 d . . . H2A H 0.3086 0.5650 0.5450 0.165 Uiso 1 1 calc R . . H2B H 0.3634 0.4971 0.5021 0.165 Uiso 1 1 calc R . . H2C H 0.2392 0.4839 0.5088 0.165 Uiso 1 1 calc R . . C3 C 0.1161(4) 0.6540(4) 0.4286(3) 0.0969(18) Uani 1 1 d . . . H3A H 0.0577 0.6139 0.4331 0.145 Uiso 1 1 calc R . . H3B H 0.0902 0.6898 0.3867 0.145 Uiso 1 1 calc R . . H3C H 0.1349 0.6905 0.4705 0.145 Uiso 1 1 calc R . . C4 C 0.4740(5) 0.5190(4) 0.2987(4) 0.110(2) Uani 1 1 d . . . H4A H 0.5380 0.4933 0.2857 0.165 Uiso 1 1 calc R . . H4B H 0.4975 0.5463 0.3450 0.165 Uiso 1 1 calc R . . H4C H 0.4409 0.5621 0.2636 0.165 Uiso 1 1 calc R . . C5 C 0.4243(4) 0.3553(4) 0.3794(3) 0.0933(16) Uani 1 1 d . . . H5A H 0.3695 0.3109 0.3810 0.140 Uiso 1 1 calc R . . H5B H 0.4402 0.3877 0.4236 0.140 Uiso 1 1 calc R . . H5C H 0.4922 0.3284 0.3729 0.140 Uiso 1 1 calc R . . C6 C 0.3427(4) 0.3667(4) 0.2180(3) 0.1002(18) Uani 1 1 d . . . H6A H 0.3207 0.4052 0.1774 0.150 Uiso 1 1 calc R . . H6B H 0.2839 0.3248 0.2175 0.150 Uiso 1 1 calc R . . H6C H 0.4104 0.3364 0.2154 0.150 Uiso 1 1 calc R . . C7 C 0.0824(4) 0.2892(3) 0.2853(3) 0.0784(13) Uani 1 1 d . . . H7A H 0.1469 0.2624 0.3163 0.118 Uiso 1 1 calc R . . H7B H 0.0964 0.2977 0.2385 0.118 Uiso 1 1 calc R . . H7C H 0.0181 0.2520 0.2815 0.118 Uiso 1 1 calc R . . C8 C 0.0512(4) 0.3767(4) 0.4203(2) 0.0885(15) Uani 1 1 d . . . H8A H -0.0031 0.3319 0.4221 0.133 Uiso 1 1 calc R . . H8B H 0.0307 0.4295 0.4412 0.133 Uiso 1 1 calc R . . H8C H 0.1241 0.3579 0.4467 0.133 Uiso 1 1 calc R . . C9 C -0.1507(4) 0.5612(4) 0.3056(3) 0.0811(14) Uani 1 1 d . . . H9A H -0.2272 0.5787 0.2861 0.122 Uiso 1 1 calc R . . H9B H -0.1007 0.6043 0.2940 0.122 Uiso 1 1 calc R . . H9C H -0.1377 0.5559 0.3569 0.122 Uiso 1 1 calc R . . C10 C -0.2320(4) 0.3726(4) 0.2862(3) 0.0902(15) Uani 1 1 d . . . H10A H -0.2353 0.3786 0.3356 0.135 Uiso 1 1 calc R . . H10B H -0.2107 0.3138 0.2777 0.135 Uiso 1 1 calc R . . H10C H -0.3045 0.3853 0.2557 0.135 Uiso 1 1 calc R . . C11 C -0.1788(5) 0.6863(3) 0.1099(3) 0.1006(18) Uani 1 1 d . . . H11A H -0.1116 0.6815 0.0926 0.151 Uiso 1 1 calc R . . H11B H -0.1590 0.6956 0.1610 0.151 Uiso 1 1 calc R . . H11C H -0.2228 0.7348 0.0869 0.151 Uiso 1 1 calc R . . C12 C -0.3916(4) 0.5942(4) 0.1251(3) 0.0938(17) Uani 1 1 d . . . H12A H -0.4378 0.6407 0.1004 0.141 Uiso 1 1 calc R . . H12B H -0.3702 0.6071 0.1756 0.141 Uiso 1 1 calc R . . H12C H -0.4331 0.5402 0.1177 0.141 Uiso 1 1 calc R . . C13 C -0.3069(5) 0.5700(4) -0.0103(2) 0.0906(16) Uani 1 1 d . . . H13A H -0.3432 0.6226 -0.0314 0.136 Uiso 1 1 calc R . . H13B H -0.3583 0.5218 -0.0217 0.136 Uiso 1 1 calc R . . H13C H -0.2420 0.5588 -0.0290 0.136 Uiso 1 1 calc R . . C14 C -0.3799(4) 0.3272(4) 0.0775(3) 0.1010(18) Uani 1 1 d . . . H14A H -0.4201 0.3687 0.0433 0.152 Uiso 1 1 calc R . . H14B H -0.3911 0.3405 0.1243 0.152 Uiso 1 1 calc R . . H14C H -0.4071 0.2693 0.0638 0.152 Uiso 1 1 calc R . . C15 C -0.1570(5) 0.2329(3) 0.1252(3) 0.0958(17) Uani 1 1 d . . . H15A H -0.1601 0.2336 0.1748 0.144 Uiso 1 1 calc R . . H15B H -0.0799 0.2315 0.1219 0.144 Uiso 1 1 calc R . . H15C H -0.1953 0.1819 0.1022 0.144 Uiso 1 1 calc R . . C16 C -0.2078(6) 0.3337(4) -0.0138(3) 0.112(2) Uani 1 1 d . . . H16A H -0.2606 0.2940 -0.0426 0.168 Uiso 1 1 calc R . . H16B H -0.1326 0.3156 -0.0137 0.168 Uiso 1 1 calc R . . H16C H -0.2205 0.3917 -0.0333 0.168 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 Te1 0.04335(14) 0.0766(2) 0.04553(15) -0.01150(11) 0.01550(10) -0.01034(11) Te2 0.06546(17) 0.04624(17) 0.04722(15) 0.00951(10) -0.00230(11) -0.01217(11) Si1 0.0443(5) 0.0461(5) 0.0367(4) 0.0028(4) 0.0092(4) 0.0034(4) Si2 0.0511(5) 0.0505(6) 0.0483(5) 0.0127(4) 0.0138(4) 0.0026(4) Si3 0.0463(5) 0.0594(7) 0.0513(5) 0.0056(5) 0.0203(4) 0.0051(4) Si4 0.0380(4) 0.0388(5) 0.0462(5) -0.0010(4) 0.0105(4) -0.0013(4) Si5 0.0496(5) 0.0575(7) 0.0651(6) -0.0007(5) 0.0161(5) 0.0080(5) Si6 0.0618(6) 0.0674(8) 0.0434(5) -0.0091(5) 0.0097(4) -0.0018(5) Si7 0.0512(5) 0.0568(7) 0.0590(6) 0.0058(5) 0.0100(4) 0.0116(5) Si8 0.0539(6) 0.0494(6) 0.0719(7) -0.0114(5) 0.0178(5) -0.0149(5) C1 0.095(4) 0.106(4) 0.093(4) -0.031(3) 0.028(3) -0.032(3) C2 0.149(6) 0.118(5) 0.048(3) 0.005(3) -0.008(3) -0.005(4) C3 0.089(3) 0.104(4) 0.105(4) -0.050(3) 0.037(3) 0.000(3) C4 0.079(3) 0.090(4) 0.179(7) -0.011(4) 0.066(4) -0.013(3) C5 0.085(3) 0.084(4) 0.097(4) 0.011(3) -0.006(3) 0.026(3) C6 0.085(3) 0.131(5) 0.085(3) -0.031(3) 0.020(3) 0.033(3) C7 0.067(3) 0.054(3) 0.112(4) 0.006(2) 0.016(2) 0.003(2) C8 0.096(3) 0.105(4) 0.067(3) 0.037(3) 0.023(2) -0.010(3) C9 0.076(3) 0.095(4) 0.072(3) -0.022(3) 0.017(2) 0.022(3) C10 0.073(3) 0.114(4) 0.096(3) 0.016(3) 0.045(3) -0.020(3) C11 0.112(4) 0.047(3) 0.131(5) 0.005(3) 0.003(4) 0.008(3) C12 0.074(3) 0.118(5) 0.096(4) 0.012(3) 0.034(3) 0.035(3) C13 0.093(3) 0.111(4) 0.063(3) 0.019(3) 0.008(2) 0.026(3) C14 0.059(3) 0.108(4) 0.133(5) -0.021(4) 0.017(3) -0.030(3) C15 0.096(4) 0.048(3) 0.138(5) -0.005(3) 0.015(3) 0.002(3) C16 0.168(6) 0.094(4) 0.086(4) -0.038(3) 0.055(4) -0.050(4) _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 Te1 Si4 2.5331(9) . ? Te1 Te2 2.7293(4) . ? Te2 Si1 2.5337(9) . ? Si1 Si5 2.3542(14) . ? Si1 Si2 2.3614(14) . ? Si1 Si6 2.3647(14) . ? Si2 C7 1.878(5) . ? Si2 C8 1.888(4) . ? Si2 Si3 2.3582(14) . ? Si3 C9 1.892(5) . ? Si3 C10 1.897(4) . ? Si3 Si4 2.3522(13) . ? Si4 Si7 2.3579(14) . ? Si4 Si8 2.3614(14) . ? Si5 C6 1.859(5) . ? Si5 C4 1.876(5) . ? Si5 C5 1.877(5) . ? Si6 C3 1.859(5) . ? Si6 C1 1.875(5) . ? Si6 C2 1.879(5) . ? Si7 C11 1.865(5) . ? Si7 C13 1.866(5) . ? Si7 C12 1.874(5) . ? Si8 C16 1.855(5) . ? Si8 C14 1.870(5) . ? Si8 C15 1.864(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 Si4 Te1 Te2 99.16(2) . . ? Si1 Te2 Te1 99.24(3) . . ? Si5 Si1 Si2 115.10(6) . . ? Si5 Si1 Si6 110.27(5) . . ? Si2 Si1 Si6 112.38(5) . . ? Si5 Si1 Te2 107.23(4) . . ? Si2 Si1 Te2 107.66(4) . . ? Si6 Si1 Te2 103.34(5) . . ? C7 Si2 C8 106.2(2) . . ? C7 Si2 Si3 111.06(15) . . ? C8 Si2 Si3 106.57(17) . . ? C7 Si2 Si1 110.01(15) . . ? C8 Si2 Si1 109.74(17) . . ? Si3 Si2 Si1 112.94(5) . . ? C9 Si3 C10 106.7(2) . . ? C9 Si3 Si4 110.67(17) . . ? C10 Si3 Si4 108.20(17) . . ? C9 Si3 Si2 110.41(15) . . ? C10 Si3 Si2 107.07(18) . . ? Si4 Si3 Si2 113.44(5) . . ? Si3 Si4 Si7 114.07(5) . . ? Si3 Si4 Si8 113.08(5) . . ? Si7 Si4 Si8 109.61(5) . . ? Si3 Si4 Te1 107.96(4) . . ? Si7 Si4 Te1 107.22(4) . . ? Si8 Si4 Te1 104.25(4) . . ? C6 Si5 C4 108.7(3) . . ? C6 Si5 C5 107.8(3) . . ? C4 Si5 C5 110.0(3) . . ? C6 Si5 Si1 111.95(16) . . ? C4 Si5 Si1 109.48(19) . . ? C5 Si5 Si1 108.89(19) . . ? C3 Si6 C1 106.8(3) . . ? C3 Si6 C2 108.3(3) . . ? C1 Si6 C2 109.1(3) . . ? C3 Si6 Si1 111.51(17) . . ? C1 Si6 Si1 111.26(16) . . ? C2 Si6 Si1 109.76(19) . . ? C11 Si7 C13 108.8(3) . . ? C11 Si7 C12 108.4(3) . . ? C13 Si7 C12 108.4(2) . . ? C11 Si7 Si4 109.96(17) . . ? C13 Si7 Si4 109.77(18) . . ? C12 Si7 Si4 111.47(18) . . ? C16 Si8 C14 109.2(3) . . ? C16 Si8 C15 107.9(3) . . ? C14 Si8 C15 108.3(3) . . ? C16 Si8 Si4 110.51(18) . . ? C14 Si8 Si4 108.61(19) . . ? C15 Si8 Si4 112.20(18) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.561 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.077 data_f120420b _database_code_depnum_ccdc_archive 'CCDC 902891' #TrackingRef 'web_deposit_cif_file_3_Xu-QiongXiao_1348557912.compound5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 Si8 Te' _chemical_formula_weight 592.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 13.101(8) _cell_length_b 8.912(5) _cell_length_c 14.984(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.666(11) _cell_angle_gamma 90.00 _cell_volume 1676.0(18) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3994 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 26.72 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7988 _exptl_absorpt_correction_T_max 0.8915 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10755 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.60 _reflns_number_total 3831 _reflns_number_gt 2899 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3831 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Te1 Te 0.7500 0.91916(4) 0.2500 0.06749(19) Uani 1 2 d S . . Si1 Si 0.82211(7) 0.73947(10) 0.15132(6) 0.0457(2) Uani 1 1 d . . . Si2 Si 0.77054(8) 0.49497(11) 0.17850(7) 0.0511(3) Uani 1 1 d . . . Si3 Si 1.00763(9) 0.76843(13) 0.19992(9) 0.0643(3) Uani 1 1 d . . . Si4 Si 0.74449(10) 0.82447(14) -0.00191(7) 0.0662(3) Uani 1 1 d . . . C1 C 0.6516(5) 0.4311(6) 0.0841(4) 0.0893(17) Uani 1 1 d . . . H1A H 0.6691 0.4268 0.0262 0.134 Uiso 1 1 calc R . . H1B H 0.5941 0.5005 0.0786 0.134 Uiso 1 1 calc R . . H1C H 0.6305 0.3333 0.0991 0.134 Uiso 1 1 calc R . . C2 C 0.8813(4) 0.3577(5) 0.1826(4) 0.0875(14) Uani 1 1 d . . . H2A H 0.8594 0.2588 0.1947 0.131 Uiso 1 1 calc R . . H2B H 0.9437 0.3861 0.2313 0.131 Uiso 1 1 calc R . . H2C H 0.8972 0.3583 0.1239 0.131 Uiso 1 1 calc R . . C3 C 1.0445(4) 0.9713(6) 0.2026(5) 0.0912(16) Uani 1 1 d . . . H3A H 1.0038 1.0271 0.2352 0.137 Uiso 1 1 calc R . . H3B H 1.0297 1.0084 0.1400 0.137 Uiso 1 1 calc R . . H3C H 1.1191 0.9827 0.2339 0.137 Uiso 1 1 calc R . . C4 C 1.0627(5) 0.6915(8) 0.3206(5) 0.119(2) Uani 1 1 d . . . H4A H 1.1389 0.7001 0.3393 0.178 Uiso 1 1 calc R . . H4B H 1.0431 0.5878 0.3213 0.178 Uiso 1 1 calc R . . H4C H 1.0342 0.7471 0.3629 0.178 Uiso 1 1 calc R . . C5 C 1.0681(5) 0.6693(7) 0.1160(6) 0.112(2) Uani 1 1 d . . . H5A H 1.1443 0.6683 0.1409 0.168 Uiso 1 1 calc R . . H5B H 1.0488 0.7212 0.0574 0.168 Uiso 1 1 calc R . . H5C H 1.0421 0.5681 0.1069 0.168 Uiso 1 1 calc R . . C6 C 0.7838(8) 0.7055(8) -0.0884(4) 0.134(3) Uani 1 1 d . . . H6A H 0.7628 0.6035 -0.0826 0.201 Uiso 1 1 calc R . . H6B H 0.8596 0.7101 -0.0772 0.201 Uiso 1 1 calc R . . H6C H 0.7492 0.7413 -0.1501 0.201 Uiso 1 1 calc R . . C7 C 0.7878(6) 1.0188(6) -0.0137(4) 0.1059(19) Uani 1 1 d . . . H7A H 0.7458 1.0600 -0.0719 0.159 Uiso 1 1 calc R . . H7B H 0.8616 1.0189 -0.0121 0.159 Uiso 1 1 calc R . . H7C H 0.7785 1.0786 0.0367 0.159 Uiso 1 1 calc R . . C8 C 0.5965(5) 0.8250(10) -0.0298(5) 0.133(3) Uani 1 1 d . . . H8A H 0.5765 0.8346 0.0268 0.199 Uiso 1 1 calc R . . H8B H 0.5687 0.7327 -0.0602 0.199 Uiso 1 1 calc R . . H8C H 0.5681 0.9078 -0.0702 0.199 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 Te1 0.1027(3) 0.0330(2) 0.0895(3) 0.000 0.0638(2) 0.000 Si1 0.0518(5) 0.0382(5) 0.0515(5) 0.0002(4) 0.0219(4) -0.0001(4) Si2 0.0605(5) 0.0354(5) 0.0597(5) -0.0072(4) 0.0206(4) -0.0034(4) Si3 0.0512(5) 0.0549(7) 0.0913(8) -0.0033(6) 0.0278(5) -0.0039(4) Si4 0.0865(8) 0.0592(7) 0.0541(6) 0.0071(5) 0.0224(5) -0.0001(6) C1 0.101(4) 0.080(4) 0.075(3) -0.017(2) 0.007(3) -0.032(3) C2 0.105(4) 0.044(2) 0.129(4) -0.005(3) 0.059(3) 0.012(2) C3 0.086(3) 0.064(3) 0.132(4) -0.018(3) 0.045(3) -0.025(3) C4 0.070(3) 0.127(5) 0.130(5) 0.039(4) -0.019(3) -0.016(3) C5 0.089(3) 0.096(4) 0.178(6) -0.034(4) 0.082(4) -0.005(3) C6 0.217(9) 0.114(5) 0.071(3) -0.012(3) 0.042(4) 0.030(5) C7 0.154(6) 0.063(3) 0.101(4) 0.026(3) 0.038(4) -0.004(4) C8 0.083(4) 0.176(7) 0.114(5) 0.054(5) -0.014(3) -0.006(4) _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 Te1 Si1 2.5386(13) . ? Te1 Si1 2.5387(13) 2_655 ? Si1 Si3 2.343(2) . ? Si1 Si2 2.3512(18) . ? Si1 Si4 2.3538(19) . ? Si2 C1 1.867(5) . ? Si2 C2 1.885(5) . ? Si2 Si2 2.354(2) 2_655 ? Si3 C3 1.869(5) . ? Si3 C4 1.874(6) . ? Si3 C5 1.888(6) . ? Si4 C7 1.847(6) . ? Si4 C6 1.858(7) . ? Si4 C8 1.862(7) . ? 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 Si1 Te1 Si1 101.78(6) . 2_655 ? Si3 Si1 Si2 111.85(5) . . ? Si3 Si1 Si4 112.78(6) . . ? Si2 Si1 Si4 113.70(6) . . ? Si3 Si1 Te1 106.00(5) . . ? Si2 Si1 Te1 108.08(6) . . ? Si4 Si1 Te1 103.67(6) . . ? C1 Si2 C2 107.1(3) . . ? C1 Si2 Si1 111.71(17) . . ? C2 Si2 Si1 110.51(18) . . ? C1 Si2 Si2 109.3(2) . 2_655 ? C2 Si2 Si2 110.18(19) . 2_655 ? Si1 Si2 Si2 108.04(4) . 2_655 ? C3 Si3 C4 107.9(3) . . ? C3 Si3 C5 108.1(3) . . ? C4 Si3 C5 110.7(4) . . ? C3 Si3 Si1 110.62(18) . . ? C4 Si3 Si1 109.7(2) . . ? C5 Si3 Si1 109.7(2) . . ? C7 Si4 C6 108.3(4) . . ? C7 Si4 C8 107.8(4) . . ? C6 Si4 C8 108.9(4) . . ? C7 Si4 Si1 109.7(2) . . ? C6 Si4 Si1 111.6(2) . . ? C8 Si4 Si1 110.5(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.904 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.242