# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ? _publ_contact_author_email zujinzhao@gmail.com _publ_contact_author_phone ? _publ_contact_author_name 'Zujin Zhao' _publ_author_name 'Zujin Zhao' data_tao1cult _database_code_depnum_ccdc_archive 'CCDC 886291' #TrackingRef '- D-1-NpTPS.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 'C50 H38 Si, C4 H8 O' _chemical_formula_sum 'C54 H46 O Si' _chemical_formula_weight 739.00 _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' O O 0.0492 0.0322 '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 triclinic _symmetry_space_group_name_H-M P-1 _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.9439(6) _cell_length_b 13.7898(7) _cell_length_c 14.4698(7) _cell_angle_alpha 101.357(4) _cell_angle_beta 99.878(4) _cell_angle_gamma 97.211(4) _cell_volume 2080.31(19) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5699 _cell_measurement_temperature 173.00(14) _cell_measurement_theta_max 71.5203 _cell_measurement_theta_min 4.6950 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.81815 _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 1.180 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_unetI/netI 0.0416 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 12066 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.50 _diffrn_reflns_theta_min 5.77 _diffrn_ambient_temperature 173.00(14) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.965 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 38.00 71.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -180.0000 33 #__ type_ start__ end____ width___ exp.time_ 2 omega 34.00 77.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 150.0000 43 #__ type_ start__ end____ width___ exp.time_ 3 omega -14.00 75.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -57.0000 150.0000 89 #__ type_ start__ end____ width___ exp.time_ 4 omega 34.00 124.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 57.0000 -60.0000 90 #__ type_ start__ end____ width___ exp.time_ 5 omega -18.00 93.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -19.0000 -30.0000 111 #__ type_ start__ end____ width___ exp.time_ 6 omega 78.00 127.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 161.0000 -114.0000 49 #__ type_ start__ end____ width___ exp.time_ 7 omega -141.00 -53.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 -90.0000 88 #__ type_ start__ end____ width___ exp.time_ 8 omega 39.00 68.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -120.0000 29 #__ type_ start__ end____ width___ exp.time_ 9 omega 41.00 70.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 -132.0000 29 #__ type_ start__ end____ width___ exp.time_ 10 omega 41.00 72.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 60.0000 31 #__ type_ start__ end____ width___ exp.time_ 11 omega 37.00 72.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 0.0000 35 #__ type_ start__ end____ width___ exp.time_ 12 omega 50.00 83.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -30.0000 33 #__ type_ start__ end____ width___ exp.time_ 13 omega 40.00 66.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 14 omega 87.00 178.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 38.0000 -180.0000 91 #__ type_ start__ end____ width___ exp.time_ 15 omega 46.00 71.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 16 omega 37.00 70.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 150.0000 33 #__ type_ start__ end____ width___ exp.time_ 17 omega 42.00 70.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -60.0000 28 #__ type_ start__ end____ width___ exp.time_ 18 omega 89.00 145.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 -132.0000 56 #__ type_ start__ end____ width___ exp.time_ 19 omega 82.00 146.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 74.0000 64 #__ type_ start__ end____ width___ exp.time_ 20 omega 82.00 148.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -30.0000 66 #__ type_ start__ end____ width___ exp.time_ 21 omega 38.00 71.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -150.0000 33 #__ type_ start__ end____ width___ exp.time_ 22 omega 38.00 70.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 150.0000 32 #__ type_ start__ end____ width___ exp.time_ 23 omega 92.00 147.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 150.0000 55 #__ type_ start__ end____ width___ exp.time_ 24 omega 86.00 136.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 38.0000 120.0000 50 #__ type_ start__ end____ width___ exp.time_ 25 omega 143.00 175.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 38.0000 120.0000 32 #__ type_ start__ end____ width___ exp.time_ 26 omega 43.00 69.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 74.0000 26 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0584400000 _diffrn_orient_matrix_UB_12 -0.1024772000 _diffrn_orient_matrix_UB_13 -0.0673933000 _diffrn_orient_matrix_UB_21 -0.0164881000 _diffrn_orient_matrix_UB_22 0.0501241000 _diffrn_orient_matrix_UB_23 -0.0865476000 _diffrn_orient_matrix_UB_31 0.1315310000 _diffrn_orient_matrix_UB_32 -0.0182610000 _diffrn_orient_matrix_UB_33 -0.0161508000 _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 5909 _reflns_number_total 7231 _reflns_odcompleteness_completeness 97.97 _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 0.809 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.052 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 502 _refine_ls_number_reflns 7231 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0670 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+0.9034P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1726 _refine_ls_wR_factor_ref 0.1828 _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 0.27807(6) 0.54655(4) 0.54542(4) 0.03925(18) Uani 1 1 d . . . C1 C 0.2218(2) 0.40805(16) 0.50965(16) 0.0390(5) Uani 1 1 d . . . C2 C 0.1996(2) 0.38016(16) 0.41224(16) 0.0377(5) Uani 1 1 d . . . C3 C 0.2277(2) 0.46262(16) 0.36089(16) 0.0381(5) Uani 1 1 d . . . C4 C 0.2706(2) 0.55568(16) 0.41707(16) 0.0395(5) Uani 1 1 d . . . C10 C 0.1605(3) 0.60527(19) 0.6064(2) 0.0541(6) Uani 1 1 d . . . H10A H 0.1882 0.6780 0.6264 0.081 Uiso 1 1 calc R . . H10B H 0.1524 0.5779 0.6630 0.081 Uiso 1 1 calc R . . H10C H 0.0789 0.5909 0.5617 0.081 Uiso 1 1 calc R . . C11 C 0.1836(2) 0.35023(16) 0.57916(16) 0.0402(5) Uani 1 1 d . . . C12 C 0.0696(2) 0.28457(17) 0.56026(17) 0.0434(5) Uani 1 1 d . . . H12 H 0.0182 0.2691 0.4976 0.052 Uiso 1 1 calc R . . C13 C 0.0302(2) 0.24176(17) 0.63108(17) 0.0452(5) Uani 1 1 d . . . H13 H -0.0482 0.1979 0.6160 0.054 Uiso 1 1 calc R . . C14 C 0.1020(2) 0.26101(17) 0.72344(17) 0.0462(5) Uani 1 1 d . . . C15 C 0.2175(3) 0.3244(2) 0.74196(19) 0.0548(6) Uani 1 1 d . . . H15 H 0.2701 0.3379 0.8040 0.066 Uiso 1 1 calc R . . C16 C 0.2566(3) 0.3678(2) 0.67119(18) 0.0518(6) Uani 1 1 d . . . H16 H 0.3356 0.4109 0.6860 0.062 Uiso 1 1 calc R . . C20 C 0.4397(3) 0.5913(2) 0.6191(2) 0.0564(6) Uani 1 1 d . . . H20A H 0.4962 0.5462 0.5966 0.085 Uiso 1 1 calc R . . H20B H 0.4384 0.5921 0.6868 0.085 Uiso 1 1 calc R . . H20C H 0.4697 0.6592 0.6127 0.085 Uiso 1 1 calc R . . C21 C 0.1526(2) 0.27541(17) 0.35736(17) 0.0444(5) Uani 1 1 d . . . C22 C 0.2160(3) 0.1996(2) 0.3828(2) 0.0630(8) Uani 1 1 d . . . H22 H 0.2886 0.2168 0.4331 0.076 Uiso 1 1 calc R . . C23 C 0.1758(5) 0.1014(2) 0.3369(3) 0.0895(13) Uani 1 1 d . . . H23 H 0.2195 0.0512 0.3564 0.107 Uiso 1 1 calc R . . C24 C 0.0749(6) 0.0753(3) 0.2646(3) 0.1038(17) Uani 1 1 d . . . H24 H 0.0484 0.0068 0.2327 0.125 Uiso 1 1 calc R . . C25 C 0.0087(4) 0.1478(3) 0.2358(2) 0.0878(13) Uani 1 1 d . . . H25 H -0.0630 0.1288 0.1848 0.105 Uiso 1 1 calc R . . C26 C 0.0485(3) 0.2499(2) 0.28264(18) 0.0580(7) Uani 1 1 d . . . H26 H 0.0046 0.3001 0.2632 0.070 Uiso 1 1 calc R . . C31 C 0.2041(2) 0.44121(17) 0.25402(16) 0.0427(5) Uani 1 1 d . . . C32 C 0.2607(2) 0.37146(18) 0.19991(17) 0.0470(5) Uani 1 1 d . . . H32 H 0.3150 0.3341 0.2313 0.056 Uiso 1 1 calc R . . C33 C 0.2382(3) 0.3563(2) 0.10034(19) 0.0608(7) Uani 1 1 d . . . H33 H 0.2776 0.3091 0.0639 0.073 Uiso 1 1 calc R . . C34 C 0.1593(4) 0.4094(3) 0.0547(2) 0.0786(10) Uani 1 1 d . . . H34 H 0.1445 0.3992 -0.0134 0.094 Uiso 1 1 calc R . . C35 C 0.1010(4) 0.4778(3) 0.1071(2) 0.0839(11) Uani 1 1 d . . . H35 H 0.0455 0.5140 0.0751 0.101 Uiso 1 1 calc R . . C36 C 0.1237(3) 0.4934(2) 0.2068(2) 0.0614(7) Uani 1 1 d . . . H36 H 0.0836 0.5404 0.2428 0.074 Uiso 1 1 calc R . . C41 C 0.3187(2) 0.64689(17) 0.38632(16) 0.0442(5) Uani 1 1 d . . . C42 C 0.3851(3) 0.64518(19) 0.3120(2) 0.0554(7) Uani 1 1 d . . . H42 H 0.3986 0.5828 0.2771 0.066 Uiso 1 1 calc R . . C43 C 0.4319(3) 0.7334(2) 0.2884(2) 0.0644(8) Uani 1 1 d . . . H43 H 0.4788 0.7304 0.2388 0.077 Uiso 1 1 calc R . . C44 C 0.4114(3) 0.8261(2) 0.3358(2) 0.0539(6) Uani 1 1 d . . . C45 C 0.3489(3) 0.8286(2) 0.4110(2) 0.0636(8) Uani 1 1 d . . . H45 H 0.3364 0.8912 0.4461 0.076 Uiso 1 1 calc R . . C46 C 0.3041(3) 0.74087(19) 0.4357(2) 0.0581(7) Uani 1 1 d . . . H46 H 0.2620 0.7448 0.4882 0.070 Uiso 1 1 calc R . . C51 C 0.0546(3) 0.22127(17) 0.80126(17) 0.0480(6) Uani 1 1 d . . . C52 C 0.1266(3) 0.16864(17) 0.85988(17) 0.0491(6) Uani 1 1 d . . . C53 C 0.2418(3) 0.1393(2) 0.84211(18) 0.0560(6) Uani 1 1 d . . . H53 H 0.2747 0.1568 0.7898 0.067 Uiso 1 1 calc R . . C54 C 0.3059(4) 0.0869(2) 0.8985(2) 0.0684(8) Uani 1 1 d . . . H54 H 0.3825 0.0676 0.8849 0.082 Uiso 1 1 calc R . . C55 C 0.2595(4) 0.0608(2) 0.9771(2) 0.0748(9) Uani 1 1 d . . . H55 H 0.3055 0.0249 1.0168 0.090 Uiso 1 1 calc R . . C56 C 0.1501(4) 0.0867(2) 0.9961(2) 0.0683(8) Uani 1 1 d . . . H56 H 0.1204 0.0691 1.0495 0.082 Uiso 1 1 calc R . . C57 C 0.0783(3) 0.13950(19) 0.93807(18) 0.0571(7) Uani 1 1 d . . . C58 C -0.0387(3) 0.1617(2) 0.9540(2) 0.0655(8) Uani 1 1 d . . . H58 H -0.0694 0.1442 1.0071 0.079 Uiso 1 1 calc R . . C59 C -0.1098(3) 0.2082(2) 0.8942(2) 0.0680(8) Uani 1 1 d . . . H59 H -0.1905 0.2204 0.9045 0.082 Uiso 1 1 calc R . . C60 C -0.0628(3) 0.2378(2) 0.8178(2) 0.0567(6) Uani 1 1 d . . . H60 H -0.1127 0.2699 0.7765 0.068 Uiso 1 1 calc R . . C61 C 0.4647(3) 0.9209(2) 0.31183(19) 0.0539(6) Uani 1 1 d . . . C62 C 0.5922(3) 0.9621(2) 0.3462(2) 0.0564(7) Uani 1 1 d . . . C63 C 0.6803(3) 0.91674(19) 0.40586(18) 0.0528(6) Uani 1 1 d . . . H63 H 0.6507 0.8571 0.4243 0.063 Uiso 1 1 calc R . . C64 C 0.8007(3) 0.9573(3) 0.4346(2) 0.0715(8) Uani 1 1 d . . . H64 H 0.8553 0.9257 0.4729 0.086 Uiso 1 1 calc R . . C65 C 0.8482(3) 1.0428(3) 0.4108(3) 0.0753(9) Uani 1 1 d . . . H65 H 0.9350 1.0701 0.4320 0.090 Uiso 1 1 calc R . . C66 C 0.7720(3) 1.0884(2) 0.3573(2) 0.0601(7) Uani 1 1 d . . . H66 H 0.8079 1.1481 0.3419 0.072 Uiso 1 1 calc R . . C67 C 0.6423(3) 1.05408(17) 0.32208(18) 0.0497(6) Uani 1 1 d . . . C68 C 0.5648(3) 1.1032(2) 0.2675(2) 0.0669(8) Uani 1 1 d . . . H68 H 0.5969 1.1644 0.2529 0.080 Uiso 1 1 calc R . . C69 C 0.4370(4) 1.0596(3) 0.2344(3) 0.0768(9) Uani 1 1 d . . . H69 H 0.3808 1.0912 0.1973 0.092 Uiso 1 1 calc R . . C70 C 0.3951(3) 0.9697(2) 0.2573(2) 0.0606(7) Uani 1 1 d . . . H70 H 0.3097 0.9403 0.2319 0.073 Uiso 1 1 calc R . . O1S O 0.558(2) 0.3453(16) -0.0003(14) 0.257(8) Uiso 0.50 1 d PD A 1 C2S C 0.5667(19) 0.2784(15) 0.0689(14) 0.198(7) Uiso 0.50 1 d PD A 1 H2SC H 0.4881 0.2732 0.0940 0.238 Uiso 0.50 1 calc PR A 1 H2SD H 0.5728 0.2105 0.0337 0.238 Uiso 0.50 1 calc PR A 1 C3S C 0.6732(15) 0.3108(12) 0.1507(12) 0.155(5) Uiso 0.50 1 d PD A 1 H3SC H 0.6485 0.3258 0.2140 0.186 Uiso 0.50 1 calc PR A 1 H3SD H 0.7369 0.2658 0.1507 0.186 Uiso 0.50 1 calc PR A 1 C4S C 0.706(2) 0.3985(16) 0.1140(18) 0.208(9) Uiso 0.50 1 d PD A 1 H4SC H 0.7609 0.4517 0.1659 0.250 Uiso 0.50 1 calc PR A 1 H4SD H 0.7526 0.3816 0.0616 0.250 Uiso 0.50 1 calc PR A 1 C5S C 0.596(2) 0.4329(16) 0.0788(17) 0.220(9) Uiso 0.50 1 d PD A 1 H5SC H 0.6119 0.4964 0.0575 0.264 Uiso 0.50 1 calc PR A 1 H5SD H 0.5372 0.4381 0.1240 0.264 Uiso 0.50 1 calc PR A 1 O1SA O 0.7261(14) 0.2723(12) 0.1066(11) 0.197(5) Uiso 0.50 1 d P B 2 C2SA C 0.7637(15) 0.3588(13) 0.1059(11) 0.146(5) Uiso 0.50 1 d P B 2 H2SA H 0.8473 0.3649 0.0881 0.175 Uiso 0.50 1 calc PR B 2 H2SB H 0.7711 0.4026 0.1703 0.175 Uiso 0.50 1 calc PR B 2 C3SA C 0.670(2) 0.3885(15) 0.0333(15) 0.181(6) Uiso 0.50 1 d P B 2 H3SA H 0.7104 0.4153 -0.0146 0.218 Uiso 0.50 1 calc PR B 2 H3SB H 0.6241 0.4389 0.0644 0.218 Uiso 0.50 1 calc PR B 2 C4SA C 0.5805(15) 0.2860(13) -0.0139(12) 0.145(5) Uiso 0.50 1 d P B 2 H4SA H 0.4914 0.2926 -0.0142 0.174 Uiso 0.50 1 calc PR B 2 H4SB H 0.5904 0.2604 -0.0806 0.174 Uiso 0.50 1 calc PR B 2 C5SA C 0.6185(14) 0.2282(11) 0.0418(11) 0.139(4) Uiso 0.50 1 d P B 2 H5SA H 0.6332 0.1653 0.0020 0.166 Uiso 0.50 1 calc PR B 2 H5SB H 0.5518 0.2106 0.0769 0.166 Uiso 0.50 1 calc PR B 2 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 0.0454(3) 0.0361(3) 0.0368(3) 0.0103(2) 0.0104(2) 0.0022(2) C1 0.0411(11) 0.0361(10) 0.0411(11) 0.0128(9) 0.0080(9) 0.0050(9) C2 0.0359(11) 0.0370(11) 0.0425(11) 0.0125(9) 0.0099(9) 0.0060(8) C3 0.0405(11) 0.0377(11) 0.0387(11) 0.0131(9) 0.0091(9) 0.0073(8) C4 0.0451(12) 0.0380(11) 0.0383(11) 0.0121(9) 0.0117(9) 0.0071(9) C10 0.0680(17) 0.0484(13) 0.0540(14) 0.0169(11) 0.0255(12) 0.0128(12) C11 0.0474(12) 0.0342(10) 0.0420(11) 0.0135(9) 0.0113(9) 0.0067(9) C12 0.0464(13) 0.0406(11) 0.0423(12) 0.0115(9) 0.0071(10) 0.0030(9) C13 0.0495(13) 0.0405(11) 0.0454(12) 0.0113(9) 0.0133(10) -0.0010(10) C14 0.0600(15) 0.0382(11) 0.0417(12) 0.0109(9) 0.0150(10) 0.0028(10) C15 0.0618(15) 0.0581(15) 0.0415(12) 0.0186(11) 0.0048(11) -0.0058(12) C16 0.0538(14) 0.0535(14) 0.0453(13) 0.0181(11) 0.0056(11) -0.0067(11) C20 0.0526(14) 0.0583(15) 0.0516(14) 0.0111(12) 0.0034(11) -0.0040(12) C21 0.0547(14) 0.0380(11) 0.0427(12) 0.0085(9) 0.0228(10) -0.0013(10) C22 0.093(2) 0.0442(13) 0.0669(17) 0.0203(12) 0.0435(16) 0.0191(13) C23 0.162(4) 0.0410(15) 0.082(2) 0.0109(16) 0.072(3) 0.016(2) C24 0.187(5) 0.0436(17) 0.085(3) 0.0004(18) 0.084(3) -0.019(2) C25 0.102(3) 0.096(3) 0.0452(16) -0.0107(16) 0.0360(17) -0.045(2) C26 0.0604(16) 0.0641(16) 0.0433(13) 0.0020(11) 0.0244(12) -0.0164(13) C31 0.0496(13) 0.0385(11) 0.0377(11) 0.0100(9) 0.0073(9) -0.0007(9) C32 0.0528(14) 0.0442(12) 0.0416(12) 0.0090(9) 0.0115(10) -0.0025(10) C33 0.0772(19) 0.0548(15) 0.0442(14) 0.0022(11) 0.0182(13) -0.0059(13) C34 0.116(3) 0.076(2) 0.0351(14) 0.0103(13) 0.0011(15) 0.0036(19) C35 0.122(3) 0.076(2) 0.0467(16) 0.0173(15) -0.0123(17) 0.025(2) C36 0.081(2) 0.0544(15) 0.0471(14) 0.0140(12) 0.0010(13) 0.0171(14) C41 0.0570(14) 0.0380(11) 0.0399(11) 0.0117(9) 0.0152(10) 0.0040(10) C42 0.0757(18) 0.0391(12) 0.0559(15) 0.0093(11) 0.0310(13) 0.0038(11) C43 0.090(2) 0.0481(14) 0.0620(16) 0.0118(12) 0.0423(16) 0.0025(13) C44 0.0595(15) 0.0489(14) 0.0543(14) 0.0159(11) 0.0132(12) 0.0034(11) C45 0.092(2) 0.0416(13) 0.0641(17) 0.0112(12) 0.0376(16) 0.0073(13) C46 0.085(2) 0.0429(13) 0.0545(15) 0.0138(11) 0.0348(14) 0.0080(12) C51 0.0639(15) 0.0391(11) 0.0394(12) 0.0062(9) 0.0168(11) -0.0020(10) C52 0.0681(16) 0.0383(11) 0.0380(12) 0.0056(9) 0.0145(11) -0.0031(10) C53 0.0773(18) 0.0513(14) 0.0404(12) 0.0127(11) 0.0145(12) 0.0066(13) C54 0.088(2) 0.0636(17) 0.0531(16) 0.0137(13) 0.0095(15) 0.0167(15) C55 0.116(3) 0.0589(17) 0.0480(15) 0.0204(13) 0.0048(17) 0.0118(18) C56 0.106(3) 0.0524(15) 0.0457(15) 0.0163(12) 0.0177(15) -0.0020(16) C57 0.087(2) 0.0422(13) 0.0382(12) 0.0081(10) 0.0162(12) -0.0073(12) C58 0.088(2) 0.0605(16) 0.0483(15) 0.0127(12) 0.0290(14) -0.0081(15) C59 0.076(2) 0.0674(18) 0.0618(17) 0.0097(14) 0.0329(15) -0.0026(15) C60 0.0660(17) 0.0538(14) 0.0521(14) 0.0129(12) 0.0207(12) 0.0024(12) C61 0.0612(16) 0.0496(13) 0.0531(14) 0.0148(11) 0.0166(12) 0.0056(11) C62 0.0651(16) 0.0496(14) 0.0537(14) 0.0006(11) 0.0292(13) -0.0002(12) C63 0.0716(17) 0.0435(12) 0.0462(13) 0.0129(10) 0.0161(12) 0.0096(11) C64 0.0585(18) 0.079(2) 0.0681(19) -0.0010(16) 0.0112(14) 0.0094(15) C65 0.0650(19) 0.079(2) 0.075(2) -0.0012(17) 0.0180(16) 0.0089(16) C66 0.0662(17) 0.0494(14) 0.0616(16) 0.0019(12) 0.0257(14) -0.0033(12) C67 0.0621(15) 0.0388(12) 0.0506(13) 0.0068(10) 0.0259(12) 0.0018(10) C68 0.084(2) 0.0571(16) 0.0632(17) 0.0163(13) 0.0199(15) 0.0124(15) C69 0.106(3) 0.0642(18) 0.076(2) 0.0364(16) 0.0252(19) 0.0297(18) C70 0.0686(17) 0.0541(15) 0.0605(16) 0.0229(13) 0.0078(13) 0.0067(13) _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 1.871(2) . ? Si1 C4 1.875(2) . ? Si1 C10 1.860(3) . ? Si1 C20 1.862(3) . ? C1 C2 1.356(3) . ? C1 C11 1.483(3) . ? C2 C3 1.504(3) . ? C2 C21 1.484(3) . ? C3 C4 1.355(3) . ? C3 C31 1.486(3) . ? C4 C41 1.480(3) . ? C11 C12 1.398(3) . ? C11 C16 1.389(3) . ? C12 C13 1.382(3) . ? C13 C14 1.386(4) . ? C14 C15 1.395(4) . ? C14 C51 1.486(3) . ? C15 C16 1.385(3) . ? C21 C22 1.398(4) . ? C21 C26 1.385(4) . ? C22 C23 1.365(5) . ? C23 C24 1.341(7) . ? C24 C25 1.394(7) . ? C25 C26 1.414(5) . ? C31 C32 1.393(3) . ? C31 C36 1.380(4) . ? C32 C33 1.388(4) . ? C33 C34 1.368(5) . ? C34 C35 1.381(5) . ? C35 C36 1.389(4) . ? C41 C42 1.396(3) . ? C41 C46 1.394(3) . ? C42 C43 1.387(4) . ? C43 C44 1.390(4) . ? C44 C45 1.378(4) . ? C44 C61 1.492(3) . ? C45 C46 1.383(4) . ? C51 C52 1.422(4) . ? C51 C60 1.385(4) . ? C52 C53 1.421(4) . ? C52 C57 1.432(3) . ? C53 C54 1.357(4) . ? C54 C55 1.414(5) . ? C55 C56 1.348(5) . ? C56 C57 1.418(5) . ? C57 C58 1.399(5) . ? C58 C59 1.370(5) . ? C59 C60 1.406(4) . ? C61 C62 1.404(4) . ? C61 C70 1.337(4) . ? C62 C63 1.465(4) . ? C62 C67 1.447(4) . ? C63 C64 1.325(4) . ? C64 C65 1.359(5) . ? C65 C66 1.339(5) . ? C66 C67 1.410(4) . ? C67 C68 1.388(4) . ? C68 C69 1.412(5) . ? C69 C70 1.388(4) . ? O1S C2S 1.489(16) . ? O1S C5S 1.452(16) . ? C2S C3S 1.465(13) . ? C2S C4S 2.02(3) . ? C3S C4S 1.443(16) . ? C4S C5S 1.403(17) . ? O1SA C2SA 1.215(17) . ? O1SA C5SA 1.360(17) . ? C2SA C3SA 1.49(3) . ? C3SA C4SA 1.57(2) . ? C4SA C5SA 1.30(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 C4 92.09(10) . . ? C10 Si1 C1 107.80(11) . . ? C10 Si1 C4 115.95(12) . . ? C10 Si1 C20 110.74(13) . . ? C20 Si1 C1 117.60(12) . . ? C20 Si1 C4 111.68(11) . . ? C2 C1 Si1 108.04(15) . . ? C2 C1 C11 128.7(2) . . ? C11 C1 Si1 121.85(16) . . ? C1 C2 C3 115.78(19) . . ? C1 C2 C21 123.55(19) . . ? C21 C2 C3 120.66(19) . . ? C4 C3 C2 116.39(19) . . ? C4 C3 C31 123.10(19) . . ? C31 C3 C2 120.47(19) . . ? C3 C4 Si1 107.66(16) . . ? C3 C4 C41 127.3(2) . . ? C41 C4 Si1 124.68(16) . . ? C12 C11 C1 123.0(2) . . ? C16 C11 C1 119.8(2) . . ? C16 C11 C12 116.9(2) . . ? C13 C12 C11 121.2(2) . . ? C12 C13 C14 121.8(2) . . ? C13 C14 C15 117.2(2) . . ? C13 C14 C51 121.5(2) . . ? C15 C14 C51 121.2(2) . . ? C16 C15 C14 121.0(2) . . ? C15 C16 C11 121.8(2) . . ? C22 C21 C2 118.4(2) . . ? C26 C21 C2 122.6(2) . . ? C26 C21 C22 118.9(3) . . ? C23 C22 C21 121.4(4) . . ? C24 C23 C22 120.5(4) . . ? C23 C24 C25 120.5(3) . . ? C24 C25 C26 119.8(4) . . ? C21 C26 C25 118.8(3) . . ? C32 C31 C3 122.7(2) . . ? C36 C31 C3 118.5(2) . . ? C36 C31 C32 118.9(2) . . ? C33 C32 C31 120.4(3) . . ? C34 C33 C32 120.0(3) . . ? C33 C34 C35 120.4(3) . . ? C34 C35 C36 119.7(3) . . ? C31 C36 C35 120.7(3) . . ? C42 C41 C4 123.3(2) . . ? C46 C41 C4 119.9(2) . . ? C46 C41 C42 116.7(2) . . ? C43 C42 C41 120.9(2) . . ? C42 C43 C44 121.5(2) . . ? C43 C44 C61 121.2(2) . . ? C45 C44 C43 117.9(2) . . ? C45 C44 C61 120.7(2) . . ? C44 C45 C46 120.6(2) . . ? C45 C46 C41 122.3(2) . . ? C52 C51 C14 122.3(2) . . ? C60 C51 C14 118.5(2) . . ? C60 C51 C52 119.3(2) . . ? C51 C52 C57 118.8(3) . . ? C53 C52 C51 123.1(2) . . ? C53 C52 C57 118.0(3) . . ? C54 C53 C52 121.2(3) . . ? C53 C54 C55 120.4(3) . . ? C56 C55 C54 120.2(3) . . ? C55 C56 C57 121.5(3) . . ? C56 C57 C52 118.6(3) . . ? C58 C57 C52 119.6(3) . . ? C58 C57 C56 121.8(3) . . ? C59 C58 C57 121.1(3) . . ? C58 C59 C60 119.7(3) . . ? C51 C60 C59 121.4(3) . . ? C62 C61 C44 120.3(3) . . ? C70 C61 C44 122.4(3) . . ? C70 C61 C62 117.2(3) . . ? C61 C62 C63 123.5(2) . . ? C61 C62 C67 119.6(3) . . ? C67 C62 C63 116.9(2) . . ? C64 C63 C62 121.2(3) . . ? C63 C64 C65 122.0(3) . . ? C66 C65 C64 119.6(3) . . ? C65 C66 C67 124.7(3) . . ? C66 C67 C62 115.7(3) . . ? C68 C67 C62 120.7(3) . . ? C68 C67 C66 123.6(3) . . ? C67 C68 C69 118.1(3) . . ? C70 C69 C68 118.6(3) . . ? C61 C70 C69 125.7(3) . . ? C5S O1S C2S 90.4(16) . . ? O1S C2S C4S 69.6(12) . . ? C3S C2S O1S 115.1(16) . . ? C3S C2S C4S 45.5(8) . . ? C4S C3S C2S 88.1(16) . . ? C3S C4S C2S 46.4(9) . . ? C5S C4S C2S 72.5(15) . . ? C5S C4S C3S 109(2) . . ? C4S C5S O1S 91.8(18) . . ? C2SA O1SA C5SA 115.4(15) . . ? O1SA C2SA C3SA 107.0(16) . . ? C2SA C3SA C4SA 101.8(15) . . ? C5SA C4SA C3SA 102.7(15) . . ? C4SA C5SA O1SA 112.2(15) . . ? # Attachment '- D-2-NpTPS.cif' data_tao2 _database_code_depnum_ccdc_archive 'CCDC 886292' #TrackingRef '- D-2-NpTPS.cif' _audit_creation_date 2012-02-23 _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 'C50 H38 Si' _chemical_formula_sum 'C50 H38 Si' _chemical_formula_weight 666.89 _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/c _space_group_IT_number 13 _space_group_name_Hall '-P 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 '-x, -y, -z' 4 'x, -y, z-1/2' _cell_length_a 25.5955(3) _cell_length_b 10.43900(10) _cell_length_c 13.54670(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.9540(10) _cell_angle_gamma 90.00 _cell_volume 3619.06(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9505 _cell_measurement_temperature 173.00(14) _cell_measurement_theta_max 71.4290 _cell_measurement_theta_min 3.6636 _exptl_absorpt_coefficient_mu 0.828 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.88035 _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 1.224 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1408 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 21793 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.49 _diffrn_reflns_theta_min 5.35 _diffrn_ambient_temperature 173.00(14) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 37.00 68.20 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 30.0000 39 #__ type_ start__ end____ width___ exp.time_ 2 omega -9.00 50.20 0.8000 3.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -113.0000 53.0000 74 #__ type_ start__ end____ width___ exp.time_ 3 omega -112.00 -26.40 0.8000 5.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 125.0000 -90.0000 107 #__ type_ start__ end____ width___ exp.time_ 4 omega -14.00 75.60 0.8000 5.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -57.0000 150.0000 112 #__ type_ start__ end____ width___ exp.time_ 5 omega 11.00 126.20 0.8000 5.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 19.0000 -30.0000 144 #__ type_ start__ end____ width___ exp.time_ 6 omega -86.00 3.60 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 64.0000 120.0000 112 #__ type_ start__ end____ width___ exp.time_ 7 omega -68.00 8.00 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 25.0000 90.0000 95 #__ type_ start__ end____ width___ exp.time_ 8 omega 39.00 71.00 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 90.0000 40 #__ type_ start__ end____ width___ exp.time_ 9 omega 40.00 71.20 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -180.0000 39 #__ type_ start__ end____ width___ exp.time_ 10 omega 39.00 71.00 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 0.0000 40 #__ type_ start__ end____ width___ exp.time_ 11 omega 51.00 83.00 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -150.0000 40 #__ type_ start__ end____ width___ exp.time_ 12 omega 39.00 70.20 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -90.0000 39 #__ type_ start__ end____ width___ exp.time_ 13 omega 37.00 61.80 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -120.0000 31 #__ type_ start__ end____ width___ exp.time_ 14 omega 41.00 70.60 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -60.0000 37 #__ type_ start__ end____ width___ exp.time_ 15 omega 41.00 70.60 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 120.0000 37 #__ type_ start__ end____ width___ exp.time_ 16 omega 41.00 70.60 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 150.0000 37 #__ type_ start__ end____ width___ exp.time_ 17 omega 41.00 70.60 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -30.0000 37 #__ type_ start__ end____ width___ exp.time_ 18 omega 104.00 172.00 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 50.0000 -90.0000 85 #__ type_ start__ end____ width___ exp.time_ 19 omega 43.00 177.40 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 0.0000 -120.0000 168 #__ type_ start__ end____ width___ exp.time_ 20 omega 125.00 149.00 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 -115.0000 30 #__ type_ start__ end____ width___ exp.time_ 21 omega 42.00 123.60 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 120.0000 102 #__ type_ start__ end____ width___ exp.time_ 22 omega 39.00 148.60 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -30.0000 137 #__ type_ start__ end____ width___ exp.time_ 23 omega 49.00 110.60 0.8000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 -115.0000 77 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0896621000 _diffrn_orient_matrix_UB_12 0.0866163000 _diffrn_orient_matrix_UB_13 -0.0101862000 _diffrn_orient_matrix_UB_21 0.0298959000 _diffrn_orient_matrix_UB_22 -0.0078404000 _diffrn_orient_matrix_UB_23 0.0582522000 _diffrn_orient_matrix_UB_31 0.0632205000 _diffrn_orient_matrix_UB_32 -0.1192687000 _diffrn_orient_matrix_UB_33 -0.0112637000 _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 5615 _reflns_number_total 6474 _reflns_odcompleteness_completeness 99.70 _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 ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 0.217 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.030 _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 463 _refine_ls_number_reflns 6474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0363 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.4033P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1002 _refine_ls_wR_factor_ref 0.1041 _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 iterative _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 0.0000 -0.06538(4) 0.2500 0.03311(12) Uani 1 2 d S . . C1 C 0.02082(5) 0.17574(12) 0.29033(8) 0.0333(3) Uani 1 1 d . . . C2 C 0.03546(5) 0.05891(12) 0.32460(9) 0.0346(3) Uani 1 1 d . . . C10 C -0.04661(6) -0.17072(14) 0.31513(11) 0.0504(4) Uani 1 1 d . . . H10A H -0.0697 -0.2128 0.2667 0.076 Uiso 1 1 calc R . . H10B H -0.0675 -0.1192 0.3603 0.076 Uiso 1 1 calc R . . H10C H -0.0272 -0.2358 0.3528 0.076 Uiso 1 1 calc R . . C11 C 0.04340(5) 0.29927(12) 0.32596(9) 0.0364(3) Uani 1 1 d . . . C12 C 0.04117(6) 0.33294(14) 0.42461(10) 0.0481(3) Uani 1 1 d . . . H12 H 0.0248 0.2771 0.4700 0.058 Uiso 1 1 calc R . . C13 C 0.06269(8) 0.44752(16) 0.45800(13) 0.0622(4) Uani 1 1 d . . . H13 H 0.0603 0.4702 0.5257 0.075 Uiso 1 1 calc R . . C14 C 0.08734(7) 0.52807(16) 0.39381(15) 0.0662(5) Uani 1 1 d . . . H14 H 0.1025 0.6058 0.4170 0.079 Uiso 1 1 calc R . . C15 C 0.09004(7) 0.49559(15) 0.29540(15) 0.0633(4) Uani 1 1 d . . . H15 H 0.1073 0.5509 0.2508 0.076 Uiso 1 1 calc R . . C16 C 0.06771(6) 0.38256(14) 0.26119(11) 0.0484(3) Uani 1 1 d . . . H16 H 0.0690 0.3619 0.1930 0.058 Uiso 1 1 calc R . . C21 C 0.07641(5) 0.02558(12) 0.39848(8) 0.0342(3) Uani 1 1 d . . . C22 C 0.06460(5) -0.06666(13) 0.46960(10) 0.0400(3) Uani 1 1 d . . . H22 H 0.0304 -0.1017 0.4709 0.048 Uiso 1 1 calc R . . C23 C 0.10144(5) -0.10796(13) 0.53792(9) 0.0413(3) Uani 1 1 d . . . H23 H 0.0918 -0.1696 0.5859 0.050 Uiso 1 1 calc R . . C24 C 0.15239(5) -0.06148(12) 0.53818(9) 0.0371(3) Uani 1 1 d . . . C25 C 0.16461(5) 0.03009(13) 0.46676(10) 0.0411(3) Uani 1 1 d . . . H25 H 0.1991 0.0634 0.4647 0.049 Uiso 1 1 calc R . . C26 C 0.12746(5) 0.07330(13) 0.39884(9) 0.0401(3) Uani 1 1 d . . . H26 H 0.1369 0.1364 0.3518 0.048 Uiso 1 1 calc R . . C27 C 0.19067(5) -0.10854(13) 0.61349(9) 0.0397(3) Uani 1 1 d . . . C28 C 0.18729(6) -0.23685(14) 0.64789(11) 0.0471(3) Uani 1 1 d . . . H28 H 0.1623 -0.2931 0.6186 0.057 Uiso 1 1 calc R . . C29 C 0.21922(6) -0.28083(16) 0.72209(11) 0.0537(4) Uani 1 1 d . . . H29 H 0.2160 -0.3670 0.7438 0.064 Uiso 1 1 calc R . . C30 C 0.25696(6) -0.20051(16) 0.76714(10) 0.0510(4) Uani 1 1 d . . . C31 C 0.28970(7) -0.2425(2) 0.84651(12) 0.0653(5) Uani 1 1 d . . . H31 H 0.2869 -0.3279 0.8700 0.078 Uiso 1 1 calc R . . C32 C 0.32506(7) -0.1611(2) 0.88920(13) 0.0752(6) Uani 1 1 d . . . H32 H 0.3465 -0.1898 0.9426 0.090 Uiso 1 1 calc R . . C33 C 0.32986(7) -0.0357(2) 0.85475(15) 0.0768(6) Uani 1 1 d . . . H33 H 0.3547 0.0201 0.8851 0.092 Uiso 1 1 calc R . . C34 C 0.29936(6) 0.00839(19) 0.77781(12) 0.0612(4) Uani 1 1 d . . . H34 H 0.3032 0.0939 0.7552 0.073 Uiso 1 1 calc R . . C35 C 0.26209(6) -0.07350(15) 0.73209(10) 0.0479(3) Uani 1 1 d . . . C36 C 0.22839(5) -0.03039(14) 0.65458(10) 0.0434(3) Uani 1 1 d . . . H36 H 0.2320 0.0546 0.6306 0.052 Uiso 1 1 calc R . . Si1A Si 0.5000 0.67777(4) 0.7500 0.03768(13) Uani 1 2 d S . . C1A C 0.48034(5) 0.43714(12) 0.70802(9) 0.0364(3) Uani 1 1 d . . . C2A C 0.46229(5) 0.55336(12) 0.67856(9) 0.0390(3) Uani 1 1 d . . . C10A C 0.46152(6) 0.77916(14) 0.83502(11) 0.0484(3) Uani 1 1 d . . . H10D H 0.4846 0.8132 0.8871 0.073 Uiso 1 1 calc R . . H10E H 0.4340 0.7274 0.8647 0.073 Uiso 1 1 calc R . . H10F H 0.4457 0.8503 0.7980 0.073 Uiso 1 1 calc R . . C11A C 0.46586(5) 0.31034(12) 0.66442(9) 0.0372(3) Uani 1 1 d . . . C12A C 0.41488(6) 0.26617(15) 0.66232(11) 0.0507(3) Uani 1 1 d . . . H12A H 0.3874 0.3204 0.6833 0.061 Uiso 1 1 calc R . . C13A C 0.40365(7) 0.14238(18) 0.62947(12) 0.0629(5) Uani 1 1 d . . . H13A H 0.3686 0.1126 0.6284 0.075 Uiso 1 1 calc R . . C14A C 0.44299(8) 0.06353(15) 0.59877(12) 0.0612(5) Uani 1 1 d . . . H14A H 0.4353 -0.0214 0.5779 0.073 Uiso 1 1 calc R . . C15A C 0.49343(7) 0.10722(14) 0.59818(10) 0.0537(4) Uani 1 1 d . . . H15A H 0.5206 0.0529 0.5758 0.064 Uiso 1 1 calc R . . C16A C 0.50502(6) 0.22989(13) 0.62994(9) 0.0420(3) Uani 1 1 d . . . H16A H 0.5401 0.2597 0.6283 0.050 Uiso 1 1 calc R . . C21A C 0.42440(5) 0.57976(12) 0.59825(9) 0.0390(3) Uani 1 1 d . . . C22A C 0.42111(5) 0.50761(13) 0.51100(9) 0.0403(3) Uani 1 1 d . . . H22A H 0.4458 0.4412 0.5003 0.048 Uiso 1 1 calc R . . C23A C 0.38290(5) 0.53099(13) 0.44051(10) 0.0404(3) Uani 1 1 d . . . H23A H 0.3817 0.4794 0.3827 0.048 Uiso 1 1 calc R . . C24A C 0.34582(5) 0.62843(12) 0.45139(9) 0.0384(3) Uani 1 1 d . . . C25A C 0.35099(6) 0.70504(13) 0.53573(11) 0.0474(3) Uani 1 1 d . . . H25A H 0.3278 0.7750 0.5444 0.057 Uiso 1 1 calc R . . C26A C 0.38915(6) 0.68114(13) 0.60668(10) 0.0471(3) Uani 1 1 d . . . H26A H 0.3915 0.7353 0.6629 0.057 Uiso 1 1 calc R . . C27A C 0.30290(5) 0.64751(13) 0.37788(9) 0.0387(3) Uani 1 1 d . . . C28A C 0.30484(5) 0.59569(13) 0.28468(10) 0.0413(3) Uani 1 1 d . . . H28A H 0.3342 0.5449 0.2678 0.050 Uiso 1 1 calc R . . C29A C 0.26491(5) 0.61507(13) 0.21305(10) 0.0425(3) Uani 1 1 d . . . C30A C 0.26787(7) 0.56242(16) 0.11680(11) 0.0563(4) Uani 1 1 d . . . H30A H 0.2975 0.5131 0.0994 0.068 Uiso 1 1 calc R . . C31A C 0.22878(7) 0.58159(18) 0.04896(12) 0.0626(4) Uani 1 1 d . . . H31A H 0.2308 0.5434 -0.0145 0.075 Uiso 1 1 calc R . . C32A C 0.18556(7) 0.65734(17) 0.07231(13) 0.0627(5) Uani 1 1 d . . . H32A H 0.1588 0.6720 0.0242 0.075 Uiso 1 1 calc R . . C33A C 0.18175(6) 0.71011(17) 0.16379(14) 0.0606(4) Uani 1 1 d . . . H33A H 0.1524 0.7619 0.1785 0.073 Uiso 1 1 calc R . . C34A C 0.22086(5) 0.68912(14) 0.23754(11) 0.0459(3) Uani 1 1 d . . . C35A C 0.21832(6) 0.73855(16) 0.33442(12) 0.0547(4) Uani 1 1 d . . . H35A H 0.1885 0.7864 0.3530 0.066 Uiso 1 1 calc R . . C36A C 0.25752(6) 0.71932(15) 0.40178(11) 0.0493(3) Uani 1 1 d . . . H36A H 0.2546 0.7545 0.4661 0.059 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 0.0381(2) 0.0276(2) 0.0334(2) 0.000 -0.00494(18) 0.000 C1 0.0357(6) 0.0328(6) 0.0314(6) 0.0000(5) -0.0012(5) -0.0019(5) C2 0.0374(6) 0.0328(6) 0.0335(6) 0.0015(5) -0.0027(5) -0.0033(5) C10 0.0600(9) 0.0444(8) 0.0468(7) -0.0032(6) -0.0008(6) -0.0186(7) C11 0.0371(6) 0.0300(6) 0.0420(6) 0.0010(5) -0.0064(5) 0.0005(5) C12 0.0594(9) 0.0425(8) 0.0418(7) -0.0030(6) -0.0099(6) -0.0058(6) C13 0.0761(11) 0.0494(9) 0.0602(9) -0.0147(8) -0.0232(8) -0.0015(8) C14 0.0688(11) 0.0356(8) 0.0934(13) -0.0100(8) -0.0234(9) -0.0097(7) C15 0.0639(10) 0.0368(8) 0.0892(12) 0.0066(8) -0.0004(9) -0.0133(7) C16 0.0543(8) 0.0363(7) 0.0548(8) 0.0031(6) 0.0021(6) -0.0059(6) C21 0.0403(7) 0.0296(6) 0.0326(6) 0.0004(5) -0.0038(5) -0.0004(5) C22 0.0402(7) 0.0377(7) 0.0420(7) 0.0052(5) -0.0026(5) -0.0034(5) C23 0.0469(7) 0.0386(7) 0.0383(6) 0.0079(5) -0.0012(5) 0.0011(6) C24 0.0430(7) 0.0352(6) 0.0328(6) -0.0033(5) -0.0031(5) 0.0051(5) C25 0.0392(7) 0.0414(7) 0.0424(7) 0.0006(6) -0.0060(5) -0.0047(5) C26 0.0434(7) 0.0381(7) 0.0386(6) 0.0066(5) -0.0047(5) -0.0071(5) C27 0.0433(7) 0.0411(7) 0.0347(6) -0.0008(5) -0.0005(5) 0.0083(6) C28 0.0511(8) 0.0418(8) 0.0483(7) 0.0031(6) -0.0038(6) 0.0074(6) C29 0.0581(9) 0.0491(8) 0.0538(8) 0.0109(7) 0.0001(7) 0.0172(7) C30 0.0462(8) 0.0657(10) 0.0410(7) 0.0024(7) 0.0002(6) 0.0204(7) C31 0.0583(10) 0.0859(13) 0.0516(9) 0.0109(9) -0.0044(7) 0.0294(9) C32 0.0582(10) 0.1124(17) 0.0546(9) 0.0000(10) -0.0186(8) 0.0313(11) C33 0.0544(10) 0.1062(17) 0.0691(11) -0.0165(11) -0.0227(8) 0.0171(10) C34 0.0449(8) 0.0782(12) 0.0600(9) -0.0092(9) -0.0122(7) 0.0093(8) C35 0.0415(7) 0.0609(9) 0.0411(7) -0.0033(6) -0.0023(6) 0.0143(6) C36 0.0433(7) 0.0457(8) 0.0411(7) 0.0000(6) -0.0046(5) 0.0065(6) Si1A 0.0521(3) 0.0233(2) 0.0374(2) 0.000 -0.0052(2) 0.000 C1A 0.0452(7) 0.0278(6) 0.0362(6) -0.0011(5) -0.0006(5) 0.0003(5) C2A 0.0497(7) 0.0288(6) 0.0384(6) -0.0020(5) -0.0026(5) 0.0021(5) C10A 0.0628(9) 0.0338(7) 0.0485(7) -0.0062(6) -0.0016(6) 0.0002(6) C11A 0.0527(7) 0.0252(6) 0.0337(6) 0.0022(5) -0.0044(5) -0.0017(5) C12A 0.0539(8) 0.0480(8) 0.0500(8) -0.0025(6) -0.0021(6) -0.0063(7) C13A 0.0739(11) 0.0609(10) 0.0535(8) 0.0009(8) -0.0059(8) -0.0320(9) C14A 0.1026(14) 0.0318(7) 0.0489(8) -0.0043(6) -0.0054(8) -0.0128(8) C15A 0.0861(11) 0.0319(7) 0.0428(7) -0.0039(6) -0.0081(7) 0.0060(7) C16A 0.0582(8) 0.0321(7) 0.0354(6) 0.0002(5) -0.0063(6) 0.0030(6) C21A 0.0491(7) 0.0276(6) 0.0401(6) 0.0011(5) -0.0034(5) 0.0008(5) C22A 0.0477(7) 0.0337(7) 0.0396(6) -0.0019(5) -0.0019(5) 0.0076(5) C23A 0.0461(7) 0.0374(7) 0.0375(6) -0.0021(5) -0.0007(5) 0.0054(5) C24A 0.0426(7) 0.0330(6) 0.0397(6) 0.0026(5) 0.0003(5) 0.0022(5) C25A 0.0565(8) 0.0352(7) 0.0503(8) -0.0046(6) -0.0046(6) 0.0121(6) C26A 0.0616(9) 0.0337(7) 0.0456(7) -0.0080(6) -0.0089(6) 0.0084(6) C27A 0.0387(7) 0.0340(6) 0.0435(7) 0.0032(5) 0.0029(5) 0.0016(5) C28A 0.0406(7) 0.0394(7) 0.0440(7) 0.0030(6) 0.0016(5) 0.0062(5) C29A 0.0411(7) 0.0393(7) 0.0472(7) 0.0066(6) -0.0011(5) -0.0018(6) C30A 0.0631(10) 0.0586(10) 0.0471(8) 0.0017(7) -0.0053(7) 0.0054(7) C31A 0.0737(11) 0.0628(10) 0.0507(8) 0.0057(8) -0.0146(8) -0.0043(8) C32A 0.0579(10) 0.0625(10) 0.0669(10) 0.0156(8) -0.0242(8) -0.0149(8) C33A 0.0381(8) 0.0596(10) 0.0837(12) 0.0111(9) -0.0103(7) -0.0012(7) C34A 0.0356(7) 0.0426(8) 0.0593(8) 0.0073(6) -0.0027(6) -0.0032(5) C35A 0.0382(7) 0.0566(9) 0.0694(10) -0.0018(8) 0.0036(7) 0.0113(6) C36A 0.0445(7) 0.0516(8) 0.0518(8) -0.0054(7) 0.0051(6) 0.0091(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 C2 1.8703(12) 2 ? Si1 C2 1.8703(12) . ? Si1 C10 1.8564(14) 2 ? Si1 C10 1.8564(14) . ? C1 C1 1.514(2) 2 ? C1 C2 1.3555(17) . ? C1 C11 1.4901(17) . ? C2 C21 1.4787(16) . ? C11 C12 1.3840(19) . ? C11 C16 1.3896(19) . ? C12 C13 1.389(2) . ? C13 C14 1.371(3) . ? C14 C15 1.379(3) . ? C15 C16 1.387(2) . ? C21 C22 1.3987(18) . ? C21 C26 1.3984(18) . ? C22 C23 1.3794(18) . ? C23 C24 1.3912(19) . ? C24 C25 1.3992(19) . ? C24 C27 1.4863(17) . ? C25 C26 1.3875(18) . ? C27 C28 1.421(2) . ? C27 C36 1.375(2) . ? C28 C29 1.364(2) . ? C29 C30 1.410(2) . ? C30 C31 1.421(2) . ? C30 C35 1.415(2) . ? C31 C32 1.363(3) . ? C32 C33 1.396(3) . ? C33 C34 1.371(2) . ? C34 C35 1.416(2) . ? C35 C36 1.4209(18) . ? Si1A C2A 1.8772(13) 2_656 ? Si1A C2A 1.8772(13) . ? Si1A C10A 1.8586(15) 2_656 ? Si1A C10A 1.8586(15) . ? C1A C1A 1.506(2) 2_656 ? C1A C2A 1.3559(18) . ? C1A C11A 1.4936(17) . ? C2A C21A 1.4714(18) . ? C11A C12A 1.384(2) . ? C11A C16A 1.394(2) . ? C12A C13A 1.395(2) . ? C13A C14A 1.371(3) . ? C14A C15A 1.370(3) . ? C15A C16A 1.382(2) . ? C21A C22A 1.4029(18) . ? C21A C26A 1.3965(19) . ? C22A C23A 1.3773(18) . ? C23A C24A 1.4007(18) . ? C24A C25A 1.3991(19) . ? C24A C27A 1.4838(18) . ? C25A C26A 1.382(2) . ? C27A C28A 1.3751(19) . ? C27A C36A 1.4243(19) . ? C28A C29A 1.4121(18) . ? C29A C30A 1.418(2) . ? C29A C34A 1.411(2) . ? C30A C31A 1.362(2) . ? C31A C32A 1.400(3) . ? C32A C33A 1.361(3) . ? C33A C34A 1.419(2) . ? C34A C35A 1.413(2) . ? C35A C36A 1.360(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 C2 Si1 C2 92.15(8) . 2 ? C10 Si1 C2 117.65(6) 2 2 ? C10 Si1 C2 110.97(7) . 2 ? C10 Si1 C2 110.97(7) 2 . ? C10 Si1 C2 117.65(6) . . ? C10 Si1 C10 107.35(11) 2 . ? C2 C1 C1 115.76(7) . 2 ? C2 C1 C11 124.34(10) . . ? C11 C1 C1 119.89(6) . 2 ? C1 C2 Si1 108.07(8) . . ? C1 C2 C21 129.22(11) . . ? C21 C2 Si1 122.32(9) . . ? C12 C11 C1 120.71(12) . . ? C12 C11 C16 118.47(13) . . ? C16 C11 C1 120.82(12) . . ? C11 C12 C13 120.71(15) . . ? C14 C13 C12 120.37(16) . . ? C13 C14 C15 119.58(15) . . ? C14 C15 C16 120.34(16) . . ? C15 C16 C11 120.51(15) . . ? C22 C21 C2 117.99(11) . . ? C26 C21 C2 124.77(11) . . ? C26 C21 C22 117.10(11) . . ? C23 C22 C21 121.60(12) . . ? C22 C23 C24 121.53(12) . . ? C23 C24 C25 117.19(11) . . ? C23 C24 C27 119.58(12) . . ? C25 C24 C27 123.22(12) . . ? C26 C25 C24 121.46(12) . . ? C25 C26 C21 121.10(12) . . ? C28 C27 C24 119.57(12) . . ? C36 C27 C24 122.17(12) . . ? C36 C27 C28 118.21(12) . . ? C29 C28 C27 121.31(15) . . ? C28 C29 C30 121.08(15) . . ? C29 C30 C31 122.34(16) . . ? C29 C30 C35 118.59(13) . . ? C35 C30 C31 119.07(16) . . ? C32 C31 C30 120.51(19) . . ? C31 C32 C33 120.28(16) . . ? C34 C33 C32 121.10(19) . . ? C33 C34 C35 120.06(19) . . ? C30 C35 C34 118.98(14) . . ? C30 C35 C36 119.08(14) . . ? C34 C35 C36 121.89(15) . . ? C27 C36 C35 121.66(14) . . ? C2A Si1A C2A 92.45(8) . 2_656 ? C10A Si1A C2A 116.12(6) 2_656 2_656 ? C10A Si1A C2A 110.35(6) . 2_656 ? C10A Si1A C2A 110.35(6) 2_656 . ? C10A Si1A C2A 116.12(6) . . ? C10A Si1A C10A 110.58(10) 2_656 . ? C2A C1A C1A 116.25(7) . 2_656 ? C2A C1A C11A 126.55(11) . . ? C11A C1A C1A 117.18(7) . 2_656 ? C1A C2A Si1A 107.31(9) . . ? C1A C2A C21A 127.04(12) . . ? C21A C2A Si1A 125.35(9) . . ? C12A C11A C1A 122.08(13) . . ? C12A C11A C16A 118.38(13) . . ? C16A C11A C1A 119.43(12) . . ? C11A C12A C13A 120.30(16) . . ? C14A C13A C12A 120.30(16) . . ? C15A C14A C13A 119.95(14) . . ? C14A C15A C16A 120.29(16) . . ? C15A C16A C11A 120.72(15) . . ? C22A C21A C2A 123.50(12) . . ? C26A C21A C2A 120.02(12) . . ? C26A C21A C22A 116.49(12) . . ? C23A C22A C21A 121.39(12) . . ? C22A C23A C24A 122.03(12) . . ? C23A C24A C27A 121.49(12) . . ? C25A C24A C23A 116.48(12) . . ? C25A C24A C27A 122.02(12) . . ? C26A C25A C24A 121.40(13) . . ? C25A C26A C21A 122.02(12) . . ? C28A C27A C24A 121.72(12) . . ? C28A C27A C36A 117.24(12) . . ? C36A C27A C24A 121.03(12) . . ? C27A C28A C29A 122.54(13) . . ? C28A C29A C30A 121.81(13) . . ? C34A C29A C28A 119.27(13) . . ? C34A C29A C30A 118.92(13) . . ? C31A C30A C29A 120.89(16) . . ? C30A C31A C32A 120.32(16) . . ? C33A C32A C31A 120.20(14) . . ? C32A C33A C34A 121.20(16) . . ? C29A C34A C33A 118.42(14) . . ? C29A C34A C35A 117.89(13) . . ? C35A C34A C33A 123.69(14) . . ? C36A C35A C34A 121.64(14) . . ? C35A C36A C27A 121.37(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 C2 C21 C22 -51.48(15) . . . . ? Si1 C2 C21 C26 124.10(13) . . . . ? C1 C1 C2 Si1 3.75(16) 2 . . . ? C1 C1 C2 C21 176.61(13) 2 . . . ? C1 C1 C11 C12 122.71(16) 2 . . . ? C1 C1 C11 C16 -58.1(2) 2 . . . ? C1 C2 C21 C22 136.57(14) . . . . ? C1 C2 C21 C26 -47.9(2) . . . . ? C1 C11 C12 C13 179.34(14) . . . . ? C1 C11 C16 C15 -178.03(14) . . . . ? C2 Si1 C2 C1 -1.41(6) 2 . . . ? C2 Si1 C2 C21 -174.86(13) 2 . . . ? C2 C1 C11 C12 -58.14(19) . . . . ? C2 C1 C11 C16 121.07(15) . . . . ? C2 C21 C22 C23 176.60(12) . . . . ? C2 C21 C26 C25 -175.32(12) . . . . ? C10 Si1 C2 C1 -116.49(10) . . . . ? C10 Si1 C2 C1 119.37(10) 2 . . . ? C10 Si1 C2 C21 -54.09(12) 2 . . . ? C10 Si1 C2 C21 70.06(12) . . . . ? C11 C1 C2 Si1 -175.43(10) . . . . ? C11 C1 C2 C21 -2.6(2) . . . . ? C11 C12 C13 C14 -1.2(3) . . . . ? C12 C11 C16 C15 1.2(2) . . . . ? C12 C13 C14 C15 0.9(3) . . . . ? C13 C14 C15 C16 0.4(3) . . . . ? C14 C15 C16 C11 -1.5(3) . . . . ? C16 C11 C12 C13 0.1(2) . . . . ? C21 C22 C23 C24 -1.2(2) . . . . ? C22 C21 C26 C25 0.3(2) . . . . ? C22 C23 C24 C25 0.6(2) . . . . ? C22 C23 C24 C27 179.79(12) . . . . ? C23 C24 C25 C26 0.3(2) . . . . ? C23 C24 C27 C28 33.10(18) . . . . ? C23 C24 C27 C36 -144.20(14) . . . . ? C24 C25 C26 C21 -0.8(2) . . . . ? C24 C27 C28 C29 -175.13(13) . . . . ? C24 C27 C36 C35 174.91(12) . . . . ? C25 C24 C27 C28 -147.80(14) . . . . ? C25 C24 C27 C36 34.89(19) . . . . ? C26 C21 C22 C23 0.7(2) . . . . ? C27 C24 C25 C26 -178.78(12) . . . . ? C27 C28 C29 C30 -0.3(2) . . . . ? C28 C27 C36 C35 -2.4(2) . . . . ? C28 C29 C30 C31 178.10(15) . . . . ? C28 C29 C30 C35 -1.6(2) . . . . ? C29 C30 C31 C32 -178.82(16) . . . . ? C29 C30 C35 C34 179.10(14) . . . . ? C29 C30 C35 C36 1.4(2) . . . . ? C30 C31 C32 C33 -0.6(3) . . . . ? C30 C35 C36 C27 0.6(2) . . . . ? C31 C30 C35 C34 -0.6(2) . . . . ? C31 C30 C35 C36 -178.28(13) . . . . ? C31 C32 C33 C34 0.0(3) . . . . ? C32 C33 C34 C35 0.2(3) . . . . ? C33 C34 C35 C30 0.1(2) . . . . ? C33 C34 C35 C36 177.67(15) . . . . ? C34 C35 C36 C27 -176.99(14) . . . . ? C35 C30 C31 C32 0.9(2) . . . . ? C36 C27 C28 C29 2.3(2) . . . . ? Si1A C2A C21A C22A 138.52(12) . . . . ? Si1A C2A C21A C26A -41.55(19) . . . . ? C1A C1A C2A Si1A 5.43(18) 2_656 . . . ? C1A C1A C2A C21A 179.36(14) 2_656 . . . ? C1A C1A C11A C12A 121.24(16) 2_656 . . . ? C1A C1A C11A C16A -54.81(19) 2_656 . . . ? C1A C2A C21A C22A -34.4(2) . . . . ? C1A C2A C21A C26A 145.57(15) . . . . ? C1A C11A C12A C13A -173.96(13) . . . . ? C1A C11A C16A C15A 173.64(12) . . . . ? C2A Si1A C2A C1A -2.02(7) 2_656 . . . ? C2A Si1A C2A C21A -176.08(15) 2_656 . . . ? C2A C1A C11A C12A -60.0(2) . . . . ? C2A C1A C11A C16A 123.99(15) . . . . ? C2A C21A C22A C23A 175.95(13) . . . . ? C2A C21A C26A C25A -176.28(14) . . . . ? C10A Si1A C2A C1A -116.14(10) . . . . ? C10A Si1A C2A C1A 117.04(10) 2_656 . . . ? C10A Si1A C2A C21A -57.01(13) 2_656 . . . ? C10A Si1A C2A C21A 69.81(13) . . . . ? C11A C1A C2A Si1A -173.37(11) . . . . ? C11A C1A C2A C21A 0.6(2) . . . . ? C11A C12A C13A C14A -0.2(2) . . . . ? C12A C11A C16A C15A -2.55(19) . . . . ? C12A C13A C14A C15A -1.5(2) . . . . ? C13A C14A C15A C16A 1.1(2) . . . . ? C14A C15A C16A C11A 1.0(2) . . . . ? C16A C11A C12A C13A 2.1(2) . . . . ? C21A C22A C23A C24A 0.8(2) . . . . ? C22A C21A C26A C25A 3.7(2) . . . . ? C22A C23A C24A C25A 2.8(2) . . . . ? C22A C23A C24A C27A -176.20(13) . . . . ? C23A C24A C25A C26A -3.2(2) . . . . ? C23A C24A C27A C28A -17.5(2) . . . . ? C23A C24A C27A C36A 161.64(14) . . . . ? C24A C25A C26A C21A -0.1(2) . . . . ? C24A C27A C28A C29A -178.62(12) . . . . ? C24A C27A C36A C35A 179.18(14) . . . . ? C25A C24A C27A C28A 163.48(14) . . . . ? C25A C24A C27A C36A -17.3(2) . . . . ? C26A C21A C22A C23A -4.0(2) . . . . ? C27A C24A C25A C26A 175.86(14) . . . . ? C27A C28A C29A C30A 179.09(14) . . . . ? C27A C28A C29A C34A -0.7(2) . . . . ? C28A C27A C36A C35A -1.6(2) . . . . ? C28A C29A C30A C31A 179.60(15) . . . . ? C28A C29A C34A C33A 178.48(14) . . . . ? C28A C29A C34A C35A -1.4(2) . . . . ? C29A C30A C31A C32A 2.0(3) . . . . ? C29A C34A C35A C36A 1.9(2) . . . . ? C30A C29A C34A C33A -1.3(2) . . . . ? C30A C29A C34A C35A 178.84(14) . . . . ? C30A C31A C32A C33A -1.4(3) . . . . ? C31A C32A C33A C34A -0.5(3) . . . . ? C32A C33A C34A C29A 1.9(2) . . . . ? C32A C33A C34A C35A -178.27(16) . . . . ? C33A C34A C35A C36A -177.90(16) . . . . ? C34A C29A C30A C31A -0.6(2) . . . . ? C34A C35A C36A C27A -0.4(2) . . . . ? C36A C27A C28A C29A 2.2(2) . . . . ? # Attachment '- compound 3.cif' data_20110302a _database_code_depnum_ccdc_archive 'CCDC 888228' #TrackingRef '- compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H28 Br2 O Si' _chemical_formula_weight 604.44 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.6335(19) _cell_length_b 14.6119(13) _cell_length_c 9.6084(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.327(2) _cell_angle_gamma 90.00 _cell_volume 2818.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5112 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 2.940 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.406 _exptl_absorpt_correction_T_max 0.494 _exptl_absorpt_process_details ? _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 24638 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6440 _reflns_number_gt 3750 _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^+0.2422P] 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 6440 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1756 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Br1 Br 0.24211(2) 0.42033(2) 0.45470(4) 0.09675(13) Uani 1 1 d . . . Br2 Br 0.45830(2) 1.38873(3) 0.49342(5) 0.10739(15) Uani 1 1 d . . . Si1 Si 0.36025(3) 0.89847(5) 0.44146(7) 0.04309(16) Uani 1 1 d . . . C17 C 0.20758(10) 1.07614(15) 0.4422(2) 0.0417(6) Uani 1 1 d . . . C10 C 0.32158(10) 1.01237(16) 0.4584(2) 0.0422(6) Uani 1 1 d . . . C11 C 0.16084(10) 0.88205(15) 0.4323(2) 0.0431(6) Uani 1 1 d . . . C6 C 0.23201(12) 0.69796(17) 0.5226(3) 0.0512(6) Uani 1 1 d . . . H6 H 0.2116 0.7354 0.5780 0.061 Uiso 1 1 calc R . . C2 C 0.29979(13) 0.67896(18) 0.3570(3) 0.0559(7) Uani 1 1 d . . . H2 H 0.3262 0.7034 0.2999 0.067 Uiso 1 1 calc R . . C4 C 0.25408(13) 0.54845(18) 0.4461(3) 0.0549(7) Uani 1 1 d . . . C3 C 0.29175(14) 0.58534(18) 0.3611(3) 0.0625(8) Uani 1 1 d . . . H3 H 0.3120 0.5475 0.3059 0.075 Uiso 1 1 calc R . . C1 C 0.26923(11) 0.73754(16) 0.4364(2) 0.0413(6) Uani 1 1 d . . . C5 C 0.22417(13) 0.60422(18) 0.5289(3) 0.0573(7) Uani 1 1 d . . . H5 H 0.1990 0.5790 0.5882 0.069 Uiso 1 1 calc R . . C16 C 0.13092(12) 0.91391(19) 0.5388(3) 0.0594(7) Uani 1 1 d . . . H16 H 0.1554 0.9480 0.6147 0.071 Uiso 1 1 calc R . . C12 C 0.12267(12) 0.83062(19) 0.3213(3) 0.0577(7) Uani 1 1 d . . . H12 H 0.1423 0.8078 0.2506 0.069 Uiso 1 1 calc R . . C15 C 0.06359(14) 0.8944(2) 0.5314(4) 0.0855(10) Uani 1 1 d . . . H15 H 0.0436 0.9155 0.6026 0.103 Uiso 1 1 calc R . . C14 C 0.02737(14) 0.8447(3) 0.4205(4) 0.0900(12) Uani 1 1 d . . . H14 H -0.0172 0.8321 0.4162 0.108 Uiso 1 1 calc R . . C13 C 0.05677(14) 0.8128(3) 0.3138(4) 0.0839(11) Uani 1 1 d . . . H13 H 0.0319 0.7795 0.2375 0.101 Uiso 1 1 calc R . . C9 C 0.25520(11) 0.99982(16) 0.4453(2) 0.0412(6) Uani 1 1 d . . . C7 C 0.27889(10) 0.83803(15) 0.4317(2) 0.0404(6) Uani 1 1 d . . . C8 C 0.23188(10) 0.90228(16) 0.4357(2) 0.0395(5) Uani 1 1 d . . . C22 C 0.21629(12) 1.13780(19) 0.5534(3) 0.0576(7) Uani 1 1 d . . . H22 H 0.2515 1.1300 0.6326 0.069 Uiso 1 1 calc R . . C18 C 0.15364(12) 1.08902(19) 0.3262(3) 0.0563(7) Uani 1 1 d . . . H18 H 0.1463 1.0479 0.2503 0.068 Uiso 1 1 calc R . . C20 C 0.12154(14) 1.2230(2) 0.4369(4) 0.0836(10) Uani 1 1 d . . . H20 H 0.0927 1.2720 0.4358 0.100 Uiso 1 1 calc R . . C19 C 0.11090(13) 1.1624(2) 0.3230(4) 0.0732(9) Uani 1 1 d . . . H19 H 0.0753 1.1710 0.2449 0.088 Uiso 1 1 calc R . . C21 C 0.17345(15) 1.2111(2) 0.5493(4) 0.0771(9) Uani 1 1 d . . . H21 H 0.1806 1.2525 0.6247 0.093 Uiso 1 1 calc R . . C28 C 0.40875(12) 1.12399(18) 0.5719(3) 0.0554(7) Uani 1 1 d . . . H28 H 0.4251 1.0800 0.6410 0.066 Uiso 1 1 calc R . . C23 C 0.35480(10) 1.10248(16) 0.4627(2) 0.0431(6) Uani 1 1 d . . . C26 C 0.41644(12) 1.27217(18) 0.4791(3) 0.0581(7) Uani 1 1 d . . . C24 C 0.33346(13) 1.16838(18) 0.3588(3) 0.0596(8) Uani 1 1 d . . . H24 H 0.2978 1.1558 0.2823 0.072 Uiso 1 1 calc R . . C27 C 0.43915(13) 1.20808(19) 0.5822(3) 0.0620(8) Uani 1 1 d . . . H27 H 0.4748 1.2212 0.6584 0.074 Uiso 1 1 calc R . . C25 C 0.36465(14) 1.2530(2) 0.3675(3) 0.0659(8) Uani 1 1 d . . . H25 H 0.3501 1.2967 0.2967 0.079 Uiso 1 1 calc R . . C30 C 0.39241(13) 0.8967(2) 0.2760(3) 0.0626(8) Uani 1 1 d . . . H30A H 0.3585 0.9184 0.1969 0.094 Uiso 1 1 calc R . . H30B H 0.4045 0.8352 0.2572 0.094 Uiso 1 1 calc R . . H30C H 0.4308 0.9355 0.2884 0.094 Uiso 1 1 calc R . . C29 C 0.42536(13) 0.8608(2) 0.5985(3) 0.0622(8) Uani 1 1 d . . . H29A H 0.4644 0.8979 0.6063 0.093 Uiso 1 1 calc R . . H29B H 0.4363 0.7979 0.5867 0.093 Uiso 1 1 calc R . . H29C H 0.4090 0.8672 0.6838 0.093 Uiso 1 1 calc R . . O1 O 0.0528(2) 0.4907(3) 0.4385(5) 0.200(2) Uani 1 1 d . . . H1 H 0.0186 0.4607 0.4316 0.300 Uiso 1 1 calc R . . C31 C 0.0415(2) 0.5703(4) 0.4583(6) 0.143(2) Uani 1 1 d . . . H31A H 0.0778 0.5957 0.5284 0.215 Uiso 1 1 calc R . . H31B H 0.0012 0.5748 0.4920 0.215 Uiso 1 1 calc R . . H31C H 0.0363 0.6035 0.3702 0.215 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 Br1 0.1690(3) 0.03859(16) 0.0922(2) -0.00504(14) 0.0496(2) -0.01255(18) Br2 0.1226(3) 0.0651(2) 0.1225(3) 0.0025(2) 0.0038(2) -0.04866(19) Si1 0.0363(3) 0.0412(3) 0.0524(3) 0.0033(3) 0.0117(3) 0.0009(3) C17 0.0396(11) 0.0367(12) 0.0513(12) 0.0012(9) 0.0154(9) -0.0020(9) C10 0.0343(10) 0.0409(12) 0.0501(12) -0.0022(10) 0.0070(9) -0.0022(10) C11 0.0414(11) 0.0370(12) 0.0550(12) 0.0031(10) 0.0195(9) -0.0011(10) C6 0.0639(13) 0.0423(13) 0.0528(13) -0.0012(10) 0.0244(11) -0.0004(12) C2 0.0687(14) 0.0471(14) 0.0594(14) 0.0016(11) 0.0301(11) 0.0026(12) C4 0.0731(16) 0.0371(12) 0.0525(14) -0.0023(11) 0.0100(12) -0.0019(12) C3 0.0880(17) 0.0413(14) 0.0675(15) -0.0039(12) 0.0370(13) 0.0061(13) C1 0.0421(11) 0.0377(11) 0.0440(11) -0.0003(9) 0.0098(9) -0.0018(10) C5 0.0752(15) 0.0432(13) 0.0588(14) 0.0036(11) 0.0263(12) -0.0089(13) C16 0.0570(13) 0.0563(16) 0.0726(16) -0.0030(13) 0.0309(12) -0.0016(12) C12 0.0473(13) 0.0644(17) 0.0634(15) -0.0062(13) 0.0167(11) -0.0137(12) C15 0.0740(15) 0.082(2) 0.121(2) 0.0080(19) 0.0645(15) 0.0060(17) C14 0.0458(14) 0.093(2) 0.133(3) -0.004(2) 0.0253(17) -0.0177(16) C13 0.0575(16) 0.098(2) 0.098(2) -0.009(2) 0.0229(16) -0.0242(17) C9 0.0407(11) 0.0411(12) 0.0415(11) -0.0014(9) 0.0090(9) -0.0024(10) C7 0.0412(11) 0.0384(12) 0.0444(11) 0.0012(9) 0.0154(9) -0.0012(10) C8 0.0371(10) 0.0403(12) 0.0428(11) -0.0004(9) 0.0123(9) -0.0029(10) C22 0.0528(13) 0.0512(14) 0.0713(16) -0.0144(12) 0.0197(12) -0.0056(12) C18 0.0505(13) 0.0560(15) 0.0624(15) 0.0071(12) 0.0129(12) 0.0070(12) C20 0.0656(15) 0.0497(16) 0.148(3) 0.0087(18) 0.0506(17) 0.0151(14) C19 0.0553(15) 0.0635(18) 0.103(2) 0.0222(16) 0.0221(15) 0.0183(14) C21 0.0768(16) 0.0523(16) 0.115(2) -0.0265(16) 0.0491(16) -0.0073(14) C28 0.0482(13) 0.0495(15) 0.0621(15) 0.0079(12) -0.0005(12) -0.0017(12) C23 0.0346(11) 0.0412(12) 0.0537(13) -0.0016(10) 0.0108(10) -0.0012(10) C26 0.0497(13) 0.0464(14) 0.0774(17) -0.0043(13) 0.0131(12) -0.0100(12) C24 0.0505(13) 0.0573(16) 0.0635(16) 0.0091(13) -0.0025(12) -0.0156(12) C27 0.0483(14) 0.0584(16) 0.0733(17) -0.0086(14) 0.0014(13) -0.0092(13) C25 0.0647(15) 0.0509(15) 0.0782(18) 0.0161(14) 0.0086(14) -0.0134(14) C30 0.0498(13) 0.0781(19) 0.0620(15) 0.0005(14) 0.0171(12) -0.0021(14) C29 0.0541(14) 0.0687(17) 0.0619(16) 0.0142(13) 0.0090(12) 0.0060(14) O1 0.262(4) 0.172(4) 0.134(3) 0.002(3) -0.021(3) -0.070(4) C31 0.113(3) 0.170(5) 0.115(3) -0.014(3) -0.040(3) -0.044(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 Br1 C4 1.893(3) . ? Br2 C26 1.900(3) . ? Si1 C29 1.858(3) . ? Si1 C30 1.859(3) . ? Si1 C10 1.869(2) . ? Si1 C7 1.880(2) . ? C17 C22 1.377(3) . ? C17 C18 1.395(3) . ? C17 C9 1.482(3) . ? C10 C9 1.359(3) . ? C10 C23 1.481(3) . ? C11 C16 1.391(4) . ? C11 C12 1.392(3) . ? C11 C8 1.488(3) . ? C6 C1 1.379(3) . ? C6 C5 1.382(4) . ? C6 H6 0.9300 . ? C2 C3 1.380(4) . ? C2 C1 1.391(4) . ? C2 H2 0.9300 . ? C4 C3 1.361(4) . ? C4 C5 1.380(4) . ? C3 H3 0.9300 . ? C1 C7 1.484(3) . ? C5 H5 0.9300 . ? C16 C15 1.404(4) . ? C16 H16 0.9300 . ? C12 C13 1.370(4) . ? C12 H12 0.9300 . ? C15 C14 1.361(5) . ? C15 H15 0.9300 . ? C14 C13 1.386(5) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C9 C8 1.500(3) . ? C7 C8 1.357(3) . ? C22 C21 1.383(4) . ? C22 H22 0.9300 . ? C18 C19 1.385(4) . ? C18 H18 0.9300 . ? C20 C21 1.345(4) . ? C20 C19 1.385(5) . ? C20 H20 0.9300 . ? C19 H19 0.9300 . ? C21 H21 0.9300 . ? C28 C27 1.373(4) . ? C28 C23 1.378(3) . ? C28 H28 0.9300 . ? C23 C24 1.384(3) . ? C26 C25 1.357(4) . ? C26 C27 1.365(4) . ? C24 C25 1.388(4) . ? C24 H24 0.9300 . ? C27 H27 0.9300 . ? C25 H25 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O1 C31 1.210(7) . ? O1 H1 0.8200 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 C29 Si1 C30 110.91(13) . . ? C29 Si1 C10 115.87(12) . . ? C30 Si1 C10 109.31(13) . . ? C29 Si1 C7 111.82(12) . . ? C30 Si1 C7 116.20(11) . . ? C10 Si1 C7 91.63(10) . . ? C22 C17 C18 118.0(2) . . ? C22 C17 C9 120.6(2) . . ? C18 C17 C9 121.4(2) . . ? C9 C10 C23 125.0(2) . . ? C9 C10 Si1 108.25(17) . . ? C23 C10 Si1 126.17(16) . . ? C16 C11 C12 118.4(2) . . ? C16 C11 C8 121.3(2) . . ? C12 C11 C8 120.3(2) . . ? C1 C6 C5 121.9(2) . . ? C1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C3 C2 C1 121.4(3) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C3 C4 C5 120.3(2) . . ? C3 C4 Br1 121.1(2) . . ? C5 C4 Br1 118.6(2) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C6 C1 C2 117.2(2) . . ? C6 C1 C7 122.1(2) . . ? C2 C1 C7 120.7(2) . . ? C4 C5 C6 119.2(3) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C11 C16 C15 119.7(3) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C13 C12 C11 121.5(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C12 C13 C14 119.7(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C10 C9 C17 123.4(2) . . ? C10 C9 C8 115.9(2) . . ? C17 C9 C8 120.78(19) . . ? C8 C7 C1 125.6(2) . . ? C8 C7 Si1 108.03(16) . . ? C1 C7 Si1 126.02(16) . . ? C7 C8 C11 124.7(2) . . ? C7 C8 C9 115.96(19) . . ? C11 C8 C9 119.36(19) . . ? C17 C22 C21 121.0(3) . . ? C17 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C19 C18 C17 120.6(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C19 C18 119.5(3) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C20 C21 C22 120.6(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C27 C28 C23 122.3(2) . . ? C27 C28 H28 118.9 . . ? C23 C28 H28 118.9 . . ? C28 C23 C24 117.2(2) . . ? C28 C23 C10 120.8(2) . . ? C24 C23 C10 122.0(2) . . ? C25 C26 C27 120.5(3) . . ? C25 C26 Br2 120.3(2) . . ? C27 C26 Br2 119.20(19) . . ? C23 C24 C25 120.7(2) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C27 C28 119.2(2) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C26 C25 C24 120.1(3) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 O1 H1 109.5 . . ? O1 C31 H31A 109.5 . . ? O1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.681 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.080