# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Roll, Mark' 'Mathur, Priyanka' 'Takahashi, Kunio' 'Kampf, Jeffrey' 'Laine, Richard' _publ_contact_author_name 'Laine, Richard' _publ_contact_author_email talsdad@umich.edu _publ_section_title ; [PhSiO1.5]8 promotes self-bromination to produce [o-BrPhSiO1.5]8. Further bromination gives crystalline [2,5-Br2PhSiO1.5]8 with a density of 2.38 g/cc and calculated refractive index of 1.7 (RI of sapphire is 1.76) or the tetraisocosa bromo compound [Br3PhSiO1.5]8. ; # Attachment '- br3ops 2.cif' data_br3ops _database_code_depnum_ccdc_archive 'CCDC 821599' #TrackingRef '- br3ops 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H16 Br24 O12 Si8, 5(C6 H4 Cl2)' _chemical_formula_sum 'C78 H36 Br24 Cl5 O12 Si8' _chemical_formula_weight 3484.88 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Si Si 0.0817 0.0704 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.5726(10) _cell_length_b 20.4685(13) _cell_length_c 20.6449(13) _cell_angle_alpha 65.3990(10) _cell_angle_beta 74.6160(10) _cell_angle_gamma 82.1720(10) _cell_volume 5766.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9953 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 21.34 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3274 _exptl_absorpt_coefficient_mu 8.573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2789 _exptl_absorpt_correction_T_max 0.3799 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2008/1) Bruker AXS area detector absorption and other corrections, University of Gottingen, Germany 2008. ; _exptl_special_details ; 4095 frames x 30 sec. @ 5.055 cm; 0.5 deg steps in omega, 0.45 deg. in phi ; _diffrn_ambient_temperature 85(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 136685 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 21.40 _reflns_number_total 13049 _reflns_number_gt 10155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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 ; Restraints (DELU/SIMU/DFIX/SAME) were applied as necessary to maintain chemical sensibility for refinement of this low-resolution data set. A large solvent accessible cavity at [0, 0, 0.5] was essentially featureless but is assumed to contain the equivalent of approximately 8 dichlorobenzene lattice solvate molecules. This region was modelled as diffuse scattering by use of teh SQUEEZE subroutine of the PLATON program suite. The solvent void has a total volume of 1964.9 A^3 and a calculated scattering of 1206 electrons per unit cell. Thw bromine sites show significan site occupancy disorder. 0.75 occupancy - Br5 Br8 Br15 Br22 0.50 occupancy - Br7 Br20 0.25 occupancy - Br3 Br6 Br10 Br25 All others at full occupancy. The dichlorobenzene molecule located on a diffrence map is also disordered. - PLATON Reference : A.L.Spek (2008) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. 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^)+(0.1299P)^2^+1.7082P] 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 13049 _refine_ls_number_parameters 967 _refine_ls_number_restraints 296 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.1935 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.092 _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 Br1 Br 0.16160(7) 0.52261(7) -0.13168(7) 0.0604(3) Uani 1 1 d D . . Br2 Br 0.07563(8) 0.35641(7) -0.03578(8) 0.0721(4) Uani 1 1 d D . . Br3 Br 0.0250(3) 0.2957(3) 0.1393(3) 0.0695(14) Uani 0.25 1 d PD A 2 Br4 Br 0.03411(9) 0.39125(6) 0.22533(7) 0.0622(3) Uani 1 1 d D . . Br5 Br -0.16023(15) 0.73918(15) 0.28784(17) 0.0728(7) Uani 0.75 1 d PD . . Br6 Br -0.3684(6) 0.6836(7) 0.3681(5) 0.172(5) Uani 0.25 1 d PD . . Br7 Br -0.4082(2) 0.5172(3) 0.41803(19) 0.0894(14) Uani 0.50 1 d PDU . . Br8 Br -0.2609(4) 0.4165(3) 0.3404(3) 0.166(3) Uani 0.75 1 d PD B 1 Br9 Br -0.11910(9) 0.82562(7) -0.00555(10) 0.0827(5) Uani 1 1 d D . . Br10 Br -0.2575(5) 0.9608(4) 0.0007(6) 0.126(3) Uani 0.25 1 d PD C 2 Br11 Br -0.20936(9) 1.07532(7) 0.04644(9) 0.0847(5) Uani 1 1 d D . . Br12 Br -0.05048(10) 1.03378(7) 0.14305(8) 0.0805(4) Uani 1 1 d D C . Br13 Br 0.33923(8) 0.63698(7) -0.08634(7) 0.0719(4) Uani 1 1 d DU . . Br14 Br 0.1876(3) 0.76386(16) -0.32917(13) 0.1992(16) Uani 1 1 d DU . . Br15 Br 0.0098(2) 0.83067(14) -0.22783(14) 0.1163(9) Uani 0.75 1 d PDU D 1 Br16 Br 0.42548(8) 0.86987(7) -0.03482(11) 0.1023(6) Uani 1 1 d D . . Br17 Br 0.74340(9) 0.71328(10) -0.07306(11) 0.1062(6) Uani 1 1 d D . . Br18 Br 0.63947(8) 0.55982(7) 0.04829(8) 0.0750(4) Uani 1 1 d D . . Br19 Br 0.03727(8) 0.84003(8) 0.29322(8) 0.0757(4) Uani 1 1 d DU . . Br20 Br 0.0700(4) 0.9843(4) 0.3058(4) 0.200(3) Uani 0.50 1 d PDU . . Br21 Br 0.22947(12) 1.09063(11) 0.18419(14) 0.1295(8) Uani 1 1 d DU . . Br22 Br 0.3789(3) 1.0309(3) 0.0657(4) 0.151(3) Uani 0.75 1 d PDU E 1 Br23 Br 0.25845(9) 0.60686(9) 0.41409(8) 0.0819(4) Uani 1 1 d D . . Br24 Br 0.1522(6) 0.6025(6) 0.5744(4) 0.134(3) Uani 0.25 1 d PD F 2 Br25 Br -0.05187(11) 0.56084(9) 0.63832(8) 0.0887(5) Uani 1 1 d D . . Br26 Br -0.17558(8) 0.58914(8) 0.51643(8) 0.0764(4) Uani 1 1 d D F . Br27 Br 0.39103(9) 0.46631(7) 0.10620(7) 0.0738(4) Uani 1 1 d D . . Br28 Br 0.54810(11) 0.31316(11) 0.34434(10) 0.1098(6) Uani 1 1 d D . . Br29 Br 0.41578(9) 0.40412(9) 0.43805(8) 0.0862(5) Uani 1 1 d D . . Si1 Si 0.11599(18) 0.56054(15) 0.12706(16) 0.0434(7) Uani 1 1 d . . . Si2 Si 0.25654(18) 0.55879(15) 0.20410(16) 0.0437(7) Uani 1 1 d . . . Si3 Si 0.12952(19) 0.63551(17) 0.29261(17) 0.0480(7) Uani 1 1 d . . . Si4 Si 0.19032(18) 0.77994(16) 0.17616(18) 0.0492(8) Uani 1 1 d . . . Si5 Si 0.31893(17) 0.71276(15) 0.08185(17) 0.0459(7) Uani 1 1 d . . . Si6 Si 0.17529(18) 0.71639(15) 0.00569(16) 0.0455(7) Uani 1 1 d . . . Si7 Si 0.03849(18) 0.78243(16) 0.09597(18) 0.0490(8) Uani 1 1 d . . . Si8 Si -0.01837(18) 0.63512(16) 0.21148(17) 0.0446(7) Uani 1 1 d . . . O1 O 0.1888(4) 0.5284(3) 0.1782(4) 0.0448(16) Uani 1 1 d . . . O2 O 0.2027(4) 0.5791(4) 0.2740(4) 0.0467(17) Uani 1 1 d . . . O3 O 0.1745(4) 0.7134(4) 0.2543(4) 0.0514(18) Uani 1 1 d . . . O4 O 0.2810(4) 0.7650(4) 0.1246(4) 0.0550(19) Uani 1 1 d . . . O5 O 0.2993(4) 0.6309(4) 0.1377(4) 0.0464(17) Uani 1 1 d . . . O6 O 0.2674(4) 0.7342(4) 0.0178(4) 0.0523(18) Uani 1 1 d . . . O7 O 0.0950(4) 0.7707(3) 0.0224(4) 0.0493(18) Uani 1 1 d . . . O8 O 0.1075(4) 0.7860(3) 0.1404(4) 0.0474(17) Uani 1 1 d . . . O9 O -0.0238(4) 0.7126(4) 0.1459(4) 0.0505(18) Uani 1 1 d . . . O10 O 0.0455(4) 0.6394(4) 0.2590(4) 0.0456(17) Uani 1 1 d . . . O11 O 0.0228(4) 0.5759(3) 0.1770(4) 0.0440(16) Uani 1 1 d . . . O12 O 0.1498(4) 0.6349(3) 0.0611(4) 0.0445(16) Uani 1 1 d . . . C1 C 0.1025(6) 0.4998(6) 0.0846(6) 0.045(3) Uani 1 1 d . . . C2 C 0.1284(6) 0.5240(6) 0.0092(6) 0.048(3) Uani 1 1 d . . . H2 H 0.1519 0.5707 -0.0180 0.058 Uiso 1 1 calc R . . C3 C 0.1218(6) 0.4836(6) -0.0284(3) 0.051(3) Uani 1 1 d D . . C4 C 0.0888(7) 0.4157(6) 0.0106(7) 0.052(3) Uani 1 1 d D A . C5 C 0.0627(6) 0.3909(4) 0.0828(6) 0.053(3) Uani 1 1 d D . . H5 H 0.0381 0.3445 0.1088 0.063 Uiso 0.75 1 calc PR A 1 C6 C 0.0700(6) 0.4303(5) 0.1219(3) 0.045(3) Uani 1 1 d D A . C7 C -0.1306(6) 0.6050(6) 0.2699(6) 0.053(3) Uani 1 1 d D . . C8 C -0.1912(7) 0.6466(4) 0.3025(7) 0.075(4) Uani 1 1 d D . . H8 H -0.1748 0.6929 0.2943 0.091 Uiso 0.25 1 calc PR G 2 C9 C -0.2743(6) 0.6214(7) 0.3463(8) 0.112(6) Uani 1 1 d D . . H9 H -0.3138 0.6489 0.3697 0.135 Uiso 0.75 1 calc PR H 1 C10 C -0.2975(6) 0.5547(8) 0.3548(8) 0.111(6) Uani 1 1 d DU B . H10 H -0.3566 0.5390 0.3793 0.133 Uiso 0.50 1 calc PR I 2 C11 C -0.2357(9) 0.5097(5) 0.3279(8) 0.110(6) Uani 1 1 d DU . . H11 H -0.2479 0.4609 0.3416 0.132 Uiso 0.25 1 calc PR B 2 C12 C -0.1555(8) 0.5400(7) 0.2801(6) 0.080(4) Uani 1 1 d D B . H12 H -0.1175 0.5141 0.2542 0.096 Uiso 1 1 calc R . . C13 C -0.0295(6) 0.8671(5) 0.0756(6) 0.050(3) Uani 1 1 d D . . C14 C -0.0990(7) 0.8843(5) 0.0393(6) 0.061(3) Uani 1 1 d D C . C15 C -0.1478(5) 0.9470(6) 0.0282(6) 0.065(3) Uani 1 1 d D . . H15 H -0.1915 0.9590 0.0002 0.078 Uiso 0.75 1 calc PR C 1 C16 C -0.1342(6) 0.9927(4) 0.0571(7) 0.060(3) Uani 1 1 d D C . C17 C -0.0701(7) 0.9753(5) 0.0978(6) 0.058(3) Uani 1 1 d D . . C18 C -0.0170(7) 0.9131(5) 0.1052(6) 0.051(3) Uani 1 1 d D C . H18 H 0.0286 0.9024 0.1311 0.061 Uiso 1 1 calc R . . C19 C 0.1823(8) 0.7294(6) -0.0885(6) 0.063(3) Uani 1 1 d U . . C20 C 0.2508(6) 0.6977(5) -0.1325(6) 0.065(3) Uani 1 1 d DU . . C21 C 0.2498(10) 0.7075(8) -0.2017(8) 0.088(4) Uani 1 1 d U . . H21 H 0.2949 0.6862 -0.2286 0.106 Uiso 1 1 calc R . . C22 C 0.1830(13) 0.7485(9) -0.2313(5) 0.108(5) Uani 1 1 d DU D . C23 C 0.1114(9) 0.7801(9) -0.1933(9) 0.111(5) Uani 1 1 d DU . . H23 H 0.0627 0.8053 -0.2139 0.133 Uiso 0.25 1 calc PR D 2 C24 C 0.1175(9) 0.7717(7) -0.1231(7) 0.078(4) Uani 1 1 d U D . H24 H 0.0747 0.7965 -0.0984 0.094 Uiso 1 1 calc R . . C25 C 0.4403(6) 0.7173(6) 0.0418(6) 0.052(3) Uani 1 1 d . . . C26 C 0.4855(6) 0.7788(4) -0.0079(7) 0.067(3) Uani 1 1 d D . . C27 C 0.5761(7) 0.7783(7) -0.0425(9) 0.082(4) Uani 1 1 d . . . H27 H 0.6055 0.8216 -0.0758 0.099 Uiso 1 1 calc R . . C28 C 0.6210(4) 0.7120(7) -0.0261(7) 0.069(4) Uani 1 1 d D . . C29 C 0.5787(7) 0.6501(4) 0.0229(7) 0.057(3) Uani 1 1 d D . . C30 C 0.4916(7) 0.6523(6) 0.0558(6) 0.051(3) Uani 1 1 d . . . H30 H 0.4636 0.6086 0.0897 0.061 Uiso 1 1 calc R . . C31 C 0.1987(7) 0.8671(6) 0.1821(7) 0.064(3) Uani 1 1 d U . . C32 C 0.1392(6) 0.8926(6) 0.2296(6) 0.069(3) Uani 1 1 d DU . . C33 C 0.1477(7) 0.9620(7) 0.2295(6) 0.078(3) Uani 1 1 d DU . . H33 H 0.1045 0.9800 0.2608 0.094 Uiso 0.50 1 calc PR J 2 C34 C 0.2178(9) 0.9996(5) 0.1844(11) 0.102(4) Uani 1 1 d DU E . C35 C 0.2793(7) 0.9766(7) 0.1323(8) 0.103(5) Uani 1 1 d DU . . H35 H 0.3251 1.0074 0.0968 0.123 Uiso 0.25 1 calc PR E 2 C36 C 0.2715(8) 0.9094(7) 0.1342(9) 0.089(4) Uani 1 1 d U E . H36 H 0.3154 0.8918 0.1030 0.107 Uiso 1 1 calc R . . C37 C 0.0857(7) 0.6101(6) 0.3921(6) 0.052(3) Uani 1 1 d . . . C38 C 0.1328(4) 0.6005(7) 0.4438(6) 0.059(3) Uani 1 1 d D F . C39 C 0.0931(8) 0.5878(7) 0.5128(7) 0.076(4) Uani 1 1 d D . . H39 H 0.1284 0.5823 0.5460 0.091 Uiso 0.75 1 calc PR F 1 C40 C 0.0009(9) 0.5822(6) 0.5383(4) 0.070(4) Uani 1 1 d D F . C41 C -0.0499(4) 0.5934(6) 0.4884(7) 0.058(3) Uani 1 1 d D . . C42 C -0.0085(8) 0.6062(6) 0.4174(6) 0.055(3) Uani 1 1 d . F . H42 H -0.0436 0.6127 0.3838 0.066 Uiso 1 1 calc R . . C43 C 0.3432(6) 0.4897(6) 0.2382(6) 0.048(3) Uani 1 1 d . . . C44 C 0.3971(8) 0.4517(6) 0.2018(4) 0.060(3) Uani 1 1 d D . . C45 C 0.4591(9) 0.3996(8) 0.2325(8) 0.083(4) Uani 1 1 d . . . H45 H 0.4956 0.3737 0.2058 0.100 Uiso 1 1 calc R . . C46 C 0.4666(8) 0.3861(6) 0.3021(7) 0.084(4) Uani 1 1 d D . . C47 C 0.4105(8) 0.4240(8) 0.3411(4) 0.074(4) Uani 1 1 d D . . C48 C 0.3496(6) 0.4753(6) 0.3089(7) 0.054(3) Uani 1 1 d . . . H48 H 0.3117 0.5008 0.3354 0.065 Uiso 1 1 calc R . . C49 C 0.5245(8) 0.6846(8) 0.2051(8) 0.089(3) Uani 1 1 d DU K . C50 C 0.5806(9) 0.6255(8) 0.2102(9) 0.103(4) Uani 1 1 d DU . . H50A H 0.5574 0.5787 0.2375 0.123 Uiso 0.662(10) 1 calc PR K 1 C51 C 0.6704(9) 0.6329(9) 0.1762(9) 0.106(4) Uani 1 1 d DU K . H51 H 0.7078 0.5917 0.1784 0.127 Uiso 1 1 calc R . . C52 C 0.7046(10) 0.6999(10) 0.1396(11) 0.135(6) Uani 1 1 d DU . . H52 H 0.7668 0.7049 0.1187 0.162 Uiso 1 1 calc R K . C53 C 0.6497(9) 0.7612(9) 0.1323(12) 0.136(6) Uani 1 1 d DU K . H53 H 0.6732 0.8080 0.1078 0.163 Uiso 1 1 calc R . . C54 C 0.5593(8) 0.7508(9) 0.1625(10) 0.114(5) Uani 1 1 d DU . . H54A H 0.5198 0.7916 0.1531 0.137 Uiso 0.338(10) 1 calc PR K 2 Cl1 Cl 0.4131(2) 0.6750(3) 0.2444(3) 0.1094(14) Uani 1 1 d U . . Cl2 Cl 0.4967(5) 0.8301(4) 0.1372(5) 0.132(3) Uani 0.662(10) 1 d PU K 1 Cl2A Cl 0.5610(9) 0.5418(8) 0.2385(8) 0.119(5) Uani 0.338(10) 1 d PU K 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 Br1 0.0456(6) 0.0908(9) 0.0663(8) -0.0564(7) -0.0156(6) 0.0180(6) Br2 0.0652(8) 0.0865(9) 0.1039(10) -0.0742(8) -0.0337(7) 0.0202(7) Br3 0.054(3) 0.068(3) 0.103(4) -0.055(3) -0.009(3) -0.008(2) Br4 0.0799(8) 0.0533(7) 0.0614(8) -0.0289(6) -0.0198(6) 0.0003(6) Br5 0.0548(12) 0.0796(18) 0.099(2) -0.0659(18) -0.0006(14) 0.0184(12) Br6 0.095(5) 0.298(14) 0.103(6) -0.077(7) -0.030(5) 0.062(7) Br7 0.055(2) 0.153(5) 0.065(2) -0.048(3) 0.0140(18) -0.058(3) Br8 0.231(5) 0.175(5) 0.106(3) -0.067(3) 0.033(3) -0.160(5) Br9 0.0639(8) 0.0694(9) 0.1457(14) -0.0646(9) -0.0486(9) 0.0204(7) Br10 0.098(5) 0.104(5) 0.203(9) -0.077(6) -0.075(6) 0.038(4) Br11 0.0639(8) 0.0629(8) 0.1178(12) -0.0399(8) -0.0111(8) 0.0222(7) Br12 0.1010(10) 0.0671(8) 0.0904(10) -0.0561(8) -0.0245(8) 0.0300(7) Br13 0.0562(7) 0.0791(9) 0.0755(9) -0.0417(7) -0.0014(6) 0.0225(6) Br14 0.344(4) 0.180(2) 0.0965(15) -0.0869(16) -0.097(2) 0.116(3) Br15 0.149(2) 0.1193(19) 0.1074(18) -0.0601(15) -0.0832(17) 0.0669(18) Br16 0.0383(7) 0.0531(8) 0.1774(17) -0.0280(9) 0.0047(8) 0.0024(6) Br17 0.0382(7) 0.1224(13) 0.1465(16) -0.0576(12) -0.0061(8) 0.0176(8) Br18 0.0571(7) 0.0822(9) 0.1048(11) -0.0560(8) -0.0374(7) 0.0364(7) Br19 0.0595(8) 0.0930(10) 0.0829(10) -0.0571(8) 0.0073(7) -0.0037(7) Br20 0.194(6) 0.220(6) 0.254(7) -0.171(6) -0.056(5) 0.036(5) Br21 0.0919(12) 0.1119(14) 0.224(2) -0.1225(16) -0.0033(13) -0.0099(10) Br22 0.069(2) 0.094(3) 0.288(7) -0.121(4) 0.053(3) -0.040(2) Br23 0.0591(8) 0.1348(13) 0.0777(9) -0.0657(9) -0.0108(7) -0.0190(8) Br24 0.125(6) 0.189(9) 0.109(6) -0.068(6) -0.038(5) -0.022(6) Br25 0.1064(11) 0.1002(11) 0.0639(9) -0.0483(8) 0.0045(8) -0.0140(9) Br26 0.0583(8) 0.0990(10) 0.0727(9) -0.0486(8) 0.0093(6) -0.0053(7) Br27 0.0884(9) 0.0805(9) 0.0684(9) -0.0495(7) -0.0273(7) 0.0308(7) Br28 0.0808(10) 0.1305(15) 0.1086(13) -0.0415(11) -0.0335(9) 0.0304(10) Br29 0.0595(8) 0.1375(13) 0.0661(9) -0.0400(9) -0.0275(7) 0.0072(8) Si1 0.0413(16) 0.0462(17) 0.0531(18) -0.0302(15) -0.0131(14) 0.0039(13) Si2 0.0403(16) 0.0492(17) 0.0482(18) -0.0285(15) -0.0089(13) 0.0055(13) Si3 0.0395(16) 0.0616(19) 0.0564(19) -0.0390(16) -0.0066(14) -0.0022(14) Si4 0.0322(15) 0.0517(18) 0.075(2) -0.0414(17) -0.0039(14) 0.0000(13) Si5 0.0300(15) 0.0497(18) 0.0605(19) -0.0319(15) -0.0010(14) 0.0050(13) Si6 0.0392(16) 0.0441(17) 0.0527(18) -0.0249(14) -0.0072(13) 0.0117(13) Si7 0.0353(15) 0.0484(17) 0.070(2) -0.0360(16) -0.0072(14) 0.0096(13) Si8 0.0368(15) 0.0518(18) 0.0591(19) -0.0379(16) -0.0084(14) 0.0011(13) O1 0.048(4) 0.043(4) 0.052(4) -0.028(3) -0.012(3) 0.002(3) O2 0.036(4) 0.061(4) 0.053(4) -0.037(4) -0.004(3) 0.000(3) O3 0.038(4) 0.064(5) 0.072(5) -0.047(4) -0.014(4) -0.002(3) O4 0.032(4) 0.056(4) 0.088(6) -0.045(4) -0.006(4) 0.000(3) O5 0.044(4) 0.055(4) 0.047(4) -0.033(4) -0.002(3) 0.003(3) O6 0.036(4) 0.052(4) 0.064(5) -0.027(4) -0.001(3) 0.005(3) O7 0.044(4) 0.045(4) 0.069(5) -0.037(4) -0.011(4) 0.012(3) O8 0.038(4) 0.047(4) 0.066(5) -0.037(4) -0.004(3) 0.003(3) O9 0.032(4) 0.051(4) 0.077(5) -0.034(4) -0.015(3) 0.007(3) O10 0.028(3) 0.066(5) 0.050(4) -0.034(4) 0.002(3) -0.010(3) O11 0.040(4) 0.045(4) 0.055(4) -0.029(3) -0.010(3) 0.001(3) O12 0.041(4) 0.048(4) 0.051(4) -0.030(4) -0.010(3) 0.013(3) C1 0.043(6) 0.053(7) 0.045(7) -0.029(6) -0.014(5) 0.022(5) C2 0.027(5) 0.049(6) 0.076(9) -0.036(6) -0.013(5) 0.009(5) C3 0.041(6) 0.067(8) 0.067(8) -0.045(7) -0.026(6) 0.020(6) C4 0.045(6) 0.069(8) 0.069(9) -0.056(7) -0.019(6) 0.022(6) C5 0.040(6) 0.041(6) 0.099(10) -0.043(7) -0.032(6) 0.010(5) C6 0.037(6) 0.040(6) 0.059(7) -0.023(6) -0.012(5) 0.007(5) C7 0.040(6) 0.085(8) 0.054(7) -0.050(7) -0.004(5) -0.011(6) C8 0.056(8) 0.094(10) 0.106(11) -0.069(9) -0.007(7) -0.024(7) C9 0.030(7) 0.22(2) 0.117(13) -0.110(14) 0.011(8) -0.021(10) C10 0.065(9) 0.191(16) 0.096(11) -0.083(11) 0.018(8) -0.058(10) C11 0.120(12) 0.139(13) 0.111(11) -0.086(10) 0.002(10) -0.068(10) C12 0.074(9) 0.122(12) 0.054(8) -0.050(8) 0.014(7) -0.046(9) C13 0.037(6) 0.047(6) 0.073(8) -0.033(6) -0.013(6) 0.010(5) C14 0.054(7) 0.049(7) 0.091(9) -0.035(7) -0.021(7) -0.001(6) C15 0.032(6) 0.073(9) 0.080(9) -0.032(7) -0.002(6) 0.013(6) C16 0.049(7) 0.042(7) 0.082(9) -0.026(6) -0.007(6) 0.010(5) C17 0.060(7) 0.048(7) 0.060(8) -0.032(6) 0.005(6) 0.011(6) C18 0.050(6) 0.053(7) 0.050(7) -0.028(6) -0.004(5) 0.012(5) C19 0.078(7) 0.064(7) 0.058(7) -0.039(6) -0.021(5) 0.028(5) C20 0.066(7) 0.055(7) 0.065(7) -0.025(6) -0.006(5) 0.012(5) C21 0.109(10) 0.093(10) 0.068(7) -0.052(7) -0.012(6) 0.029(7) C22 0.147(12) 0.115(11) 0.065(8) -0.050(8) -0.033(8) 0.053(9) C23 0.143(10) 0.115(10) 0.089(8) -0.056(8) -0.063(7) 0.074(9) C24 0.098(9) 0.076(8) 0.074(7) -0.046(7) -0.040(7) 0.046(7) C25 0.031(6) 0.066(8) 0.064(7) -0.037(6) -0.008(5) 0.011(6) C26 0.033(6) 0.053(7) 0.097(10) -0.022(7) -0.002(6) 0.003(6) C27 0.034(7) 0.073(9) 0.123(12) -0.030(8) -0.006(7) -0.003(6) C28 0.035(6) 0.080(10) 0.095(10) -0.042(8) -0.018(7) 0.024(7) C29 0.044(7) 0.067(8) 0.079(9) -0.049(7) -0.031(6) 0.029(6) C30 0.049(7) 0.065(7) 0.045(7) -0.027(6) -0.021(5) 0.009(6) C31 0.037(6) 0.065(7) 0.108(9) -0.059(7) -0.007(5) -0.003(5) C32 0.044(6) 0.081(7) 0.098(9) -0.053(7) -0.014(5) -0.002(5) C33 0.055(7) 0.078(7) 0.141(10) -0.077(8) -0.037(5) 0.012(5) C34 0.051(7) 0.094(8) 0.209(13) -0.101(9) -0.038(6) 0.001(6) C35 0.047(7) 0.077(8) 0.198(14) -0.084(9) 0.007(7) -0.021(6) C36 0.036(6) 0.076(7) 0.166(13) -0.075(8) 0.009(6) -0.010(5) C37 0.042(6) 0.075(8) 0.048(7) -0.043(6) 0.017(5) -0.023(5) C38 0.061(7) 0.081(8) 0.051(8) -0.043(6) -0.007(6) -0.011(6) C39 0.064(9) 0.092(10) 0.083(10) -0.053(8) 0.001(8) -0.015(7) C40 0.102(11) 0.060(8) 0.050(8) -0.037(6) 0.011(8) -0.016(7) C41 0.053(7) 0.062(7) 0.068(9) -0.038(6) -0.012(6) 0.001(6) C42 0.065(8) 0.060(7) 0.048(7) -0.034(6) -0.002(6) -0.003(6) C43 0.034(6) 0.068(7) 0.049(7) -0.030(6) -0.013(5) 0.006(5) C44 0.057(7) 0.080(8) 0.065(8) -0.048(7) -0.025(6) 0.014(6) C45 0.084(10) 0.103(11) 0.080(10) -0.055(9) -0.034(8) 0.034(8) C46 0.069(9) 0.099(11) 0.076(10) -0.039(9) -0.004(8) 0.013(8) C47 0.060(8) 0.108(11) 0.052(8) -0.029(7) -0.017(6) 0.011(8) C48 0.026(5) 0.063(7) 0.077(9) -0.037(6) -0.013(5) 0.019(5) C49 0.058(6) 0.133(7) 0.108(11) -0.073(8) -0.029(6) -0.001(5) C50 0.086(7) 0.132(8) 0.122(12) -0.070(9) -0.052(8) 0.017(6) C51 0.089(8) 0.142(10) 0.111(12) -0.079(10) -0.030(8) 0.028(7) C52 0.072(9) 0.169(12) 0.143(15) -0.059(13) -0.007(10) 0.024(7) C53 0.073(7) 0.139(11) 0.167(16) -0.048(12) -0.003(10) -0.001(6) C54 0.061(6) 0.131(8) 0.150(15) -0.065(10) -0.011(8) 0.004(6) Cl1 0.062(2) 0.167(4) 0.109(3) -0.067(3) -0.010(2) -0.016(2) Cl2 0.086(4) 0.118(5) 0.201(9) -0.090(5) -0.004(5) 0.004(4) Cl2A 0.098(9) 0.135(8) 0.131(12) -0.058(9) -0.031(8) -0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C3 1.894(5) . ? Br2 C4 1.891(5) . ? Br3 C5 1.886(5) . ? Br4 C6 1.892(5) . ? Br5 C8 1.900(5) . ? Br6 C9 1.896(5) . ? Br7 C10 1.896(5) . ? Br8 C11 1.899(5) . ? Br9 C14 1.892(5) . ? Br10 C15 1.888(5) . ? Br11 C16 1.889(5) . ? Br12 C17 1.891(5) . ? Br13 C20 1.896(5) . ? Br14 C22 1.893(5) . ? Br15 C23 1.902(5) . ? Br16 C26 1.896(5) . ? Br17 C28 1.894(5) . ? Br18 C29 1.887(5) . ? Br19 C32 1.894(5) . ? Br20 C33 1.894(5) . ? Br21 C34 1.894(5) . ? Br22 C35 1.897(5) . ? Br23 C38 1.895(5) . ? Br24 C39 1.891(5) . ? Br25 C40 1.892(5) . ? Br26 C41 1.891(5) . ? Br27 C44 1.895(5) . ? Br28 C46 1.895(5) . ? Br29 C47 1.892(5) . ? Si1 O12 1.600(7) . ? Si1 O11 1.619(7) . ? Si1 O1 1.640(7) . ? Si1 C1 1.854(10) . ? Si2 O1 1.593(7) . ? Si2 O5 1.612(7) . ? Si2 O2 1.649(7) . ? Si2 C43 1.863(10) . ? Si3 O2 1.600(7) . ? Si3 O10 1.615(7) . ? Si3 O3 1.619(8) . ? Si3 C37 1.850(10) . ? Si4 O3 1.603(8) . ? Si4 O4 1.604(7) . ? Si4 O8 1.615(7) . ? Si4 C31 1.862(11) . ? Si5 O6 1.602(8) . ? Si5 O5 1.605(7) . ? Si5 O4 1.616(7) . ? Si5 C25 1.849(10) . ? Si6 O12 1.612(7) . ? Si6 O7 1.622(7) . ? Si6 O6 1.632(7) . ? Si6 C19 1.824(12) . ? Si7 O8 1.613(7) . ? Si7 O9 1.633(8) . ? Si7 O7 1.636(7) . ? Si7 C13 1.853(9) . ? Si8 O10 1.603(7) . ? Si8 O9 1.610(8) . ? Si8 O11 1.627(7) . ? Si8 C7 1.856(10) . ? C1 C2 1.382(15) . ? C1 C6 1.397(14) . ? C2 C3 1.376(14) . ? C3 C4 1.374(14) . ? C4 C5 1.321(14) . ? C5 C6 1.389(14) . ? C7 C12 1.351(13) . ? C7 C8 1.411(11) . ? C8 C9 1.389(12) . ? C9 C10 1.389(15) . ? C10 C11 1.406(13) . ? C11 C12 1.402(13) . ? C13 C18 1.374(12) . ? C13 C14 1.402(11) . ? C14 C15 1.363(11) . ? C15 C16 1.365(13) . ? C16 C17 1.389(11) . ? C17 C18 1.394(11) . ? C19 C24 1.382(16) . ? C19 C20 1.474(15) . ? C20 C21 1.361(17) . ? C21 C22 1.354(19) . ? C22 C23 1.429(19) . ? C23 C24 1.414(18) . ? C25 C26 1.385(15) . ? C25 C30 1.415(15) . ? C26 C27 1.402(16) . ? C27 C28 1.390(17) . ? C28 C29 1.367(15) . ? C29 C30 1.351(15) . ? C31 C32 1.380(15) . ? C31 C36 1.404(17) . ? C32 C33 1.444(16) . ? C33 C34 1.321(18) . ? C34 C35 1.430(19) . ? C35 C36 1.382(17) . ? C37 C38 1.383(15) . ? C37 C42 1.421(15) . ? C38 C39 1.323(15) . ? C39 C40 1.394(17) . ? C40 C41 1.386(16) . ? C41 C42 1.364(15) . ? C43 C44 1.360(14) . ? C43 C48 1.391(15) . ? C44 C45 1.398(17) . ? C45 C46 1.379(18) . ? C46 C47 1.406(17) . ? C47 C48 1.388(15) . ? C49 C54 1.363(15) . ? C49 C50 1.376(13) . ? C49 Cl1 1.709(13) . ? C50 C51 1.385(14) . ? C50 Cl2A 1.61(2) . ? C51 C52 1.362(16) . ? C52 C53 1.396(14) . ? C53 C54 1.386(14) . ? C54 Cl2 1.729(17) . ? 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 O12 Si1 O11 108.5(3) . . ? O12 Si1 O1 109.4(4) . . ? O11 Si1 O1 108.1(4) . . ? O12 Si1 C1 106.4(4) . . ? O11 Si1 C1 112.0(4) . . ? O1 Si1 C1 112.2(4) . . ? O1 Si2 O5 109.0(4) . . ? O1 Si2 O2 109.7(4) . . ? O5 Si2 O2 108.5(4) . . ? O1 Si2 C43 111.5(4) . . ? O5 Si2 C43 112.2(4) . . ? O2 Si2 C43 105.7(4) . . ? O2 Si3 O10 109.3(4) . . ? O2 Si3 O3 107.7(4) . . ? O10 Si3 O3 109.2(4) . . ? O2 Si3 C37 113.0(5) . . ? O10 Si3 C37 106.7(4) . . ? O3 Si3 C37 110.9(4) . . ? O3 Si4 O4 108.8(4) . . ? O3 Si4 O8 108.2(4) . . ? O4 Si4 O8 109.6(4) . . ? O3 Si4 C31 113.1(5) . . ? O4 Si4 C31 108.5(4) . . ? O8 Si4 C31 108.6(5) . . ? O6 Si5 O5 109.4(4) . . ? O6 Si5 O4 107.6(4) . . ? O5 Si5 O4 109.4(4) . . ? O6 Si5 C25 109.1(4) . . ? O5 Si5 C25 106.8(4) . . ? O4 Si5 C25 114.5(4) . . ? O12 Si6 O7 109.3(4) . . ? O12 Si6 O6 108.4(4) . . ? O7 Si6 O6 110.5(4) . . ? O12 Si6 C19 110.7(5) . . ? O7 Si6 C19 104.6(4) . . ? O6 Si6 C19 113.3(5) . . ? O8 Si7 O9 109.4(4) . . ? O8 Si7 O7 108.8(4) . . ? O9 Si7 O7 107.1(4) . . ? O8 Si7 C13 107.2(4) . . ? O9 Si7 C13 111.2(4) . . ? O7 Si7 C13 113.1(4) . . ? O10 Si8 O9 109.0(4) . . ? O10 Si8 O11 109.3(4) . . ? O9 Si8 O11 109.2(4) . . ? O10 Si8 C7 110.8(4) . . ? O9 Si8 C7 111.4(4) . . ? O11 Si8 C7 107.1(4) . . ? Si2 O1 Si1 137.9(4) . . ? Si3 O2 Si2 140.4(5) . . ? Si4 O3 Si3 138.1(4) . . ? Si4 O4 Si5 139.0(4) . . ? Si5 O5 Si2 164.3(4) . . ? Si5 O6 Si6 139.5(5) . . ? Si6 O7 Si7 134.8(5) . . ? Si7 O8 Si4 167.9(4) . . ? Si8 O9 Si7 138.3(4) . . ? Si8 O10 Si3 164.5(5) . . ? Si1 O11 Si8 137.6(4) . . ? Si1 O12 Si6 169.2(4) . . ? C2 C1 C6 116.0(9) . . ? C2 C1 Si1 117.9(8) . . ? C6 C1 Si1 126.0(7) . . ? C3 C2 C1 123.1(10) . . ? C4 C3 C2 118.8(7) . . ? C4 C3 Br1 122.4(7) . . ? C2 C3 Br1 118.8(8) . . ? C5 C4 C3 119.9(5) . . ? C5 C4 Br2 118.0(8) . . ? C3 C4 Br2 122.1(8) . . ? C4 C5 C6 122.3(6) . . ? C4 C5 Br3 121.5(8) . . ? C6 C5 Br3 115.8(7) . . ? C5 C6 C1 119.8(6) . . ? C5 C6 Br4 120.6(6) . . ? C1 C6 Br4 119.6(7) . . ? C12 C7 C8 118.8(9) . . ? C12 C7 Si8 117.5(7) . . ? C8 C7 Si8 123.7(7) . . ? C9 C8 C7 121.5(7) . . ? C9 C8 Br5 118.1(8) . . ? C7 C8 Br5 120.3(7) . . ? C8 C9 C10 117.8(7) . . ? C8 C9 Br6 122.2(9) . . ? C10 C9 Br6 117.0(9) . . ? C9 C10 C11 121.6(6) . . ? C9 C10 Br7 118.4(9) . . ? C11 C10 Br7 119.2(10) . . ? C12 C11 C10 117.2(8) . . ? C12 C11 Br8 117.9(9) . . ? C10 C11 Br8 124.1(9) . . ? C7 C12 C11 122.1(10) . . ? C18 C13 C14 117.3(8) . . ? C18 C13 Si7 117.2(7) . . ? C14 C13 Si7 125.1(7) . . ? C15 C14 C13 121.7(6) . . ? C15 C14 Br9 117.6(7) . . ? C13 C14 Br9 120.3(6) . . ? C14 C15 C16 120.2(7) . . ? C14 C15 Br10 121.7(7) . . ? C16 C15 Br10 115.3(7) . . ? C15 C16 C17 119.9(5) . . ? C15 C16 Br11 118.7(7) . . ? C17 C16 Br11 121.3(7) . . ? C16 C17 C18 119.3(6) . . ? C16 C17 Br12 122.4(6) . . ? C18 C17 Br12 118.3(7) . . ? C13 C18 C17 121.3(9) . . ? C24 C19 C20 115.2(10) . . ? C24 C19 Si6 118.6(9) . . ? C20 C19 Si6 126.2(8) . . ? C21 C20 C19 123.0(8) . . ? C21 C20 Br13 120.2(9) . . ? C19 C20 Br13 116.7(8) . . ? C22 C21 C20 118.3(11) . . ? C21 C22 C23 123.9(8) . . ? C21 C22 Br14 116.6(10) . . ? C23 C22 Br14 119.5(9) . . ? C24 C23 C22 115.8(7) . . ? C24 C23 Br15 118.0(9) . . ? C22 C23 Br15 126.2(9) . . ? C19 C24 C23 123.5(11) . . ? C26 C25 C30 115.5(9) . . ? C26 C25 Si5 125.5(7) . . ? C30 C25 Si5 118.6(9) . . ? C25 C26 C27 123.4(8) . . ? C25 C26 Br16 120.7(7) . . ? C27 C26 Br16 115.9(8) . . ? C28 C27 C26 117.2(10) . . ? C29 C28 C27 121.1(7) . . ? C29 C28 Br17 122.6(8) . . ? C27 C28 Br17 116.2(9) . . ? C30 C29 C28 120.2(7) . . ? C30 C29 Br18 118.0(8) . . ? C28 C29 Br18 121.8(8) . . ? C29 C30 C25 122.6(10) . . ? C32 C31 C36 118.4(10) . . ? C32 C31 Si4 125.0(8) . . ? C36 C31 Si4 116.7(9) . . ? C31 C32 C33 122.2(7) . . ? C31 C32 Br19 120.6(8) . . ? C33 C32 Br19 117.0(7) . . ? C34 C33 C32 117.4(7) . . ? C34 C33 Br20 124.4(9) . . ? C32 C33 Br20 117.2(8) . . ? C33 C34 C35 122.2(6) . . ? C33 C34 Br21 117.7(10) . . ? C35 C34 Br21 119.9(10) . . ? C36 C35 C34 119.4(8) . . ? C36 C35 Br22 117.6(9) . . ? C34 C35 Br22 122.8(8) . . ? C35 C36 C31 120.0(11) . . ? C38 C37 C42 116.1(9) . . ? C38 C37 Si3 127.7(7) . . ? C42 C37 Si3 115.9(8) . . ? C39 C38 C37 122.3(7) . . ? C39 C38 Br23 118.9(8) . . ? C37 C38 Br23 118.7(7) . . ? C38 C39 C40 121.8(8) . . ? C38 C39 Br24 121.0(9) . . ? C40 C39 Br24 114.9(8) . . ? C41 C40 C39 118.3(6) . . ? C41 C40 Br25 121.7(9) . . ? C39 C40 Br25 120.0(9) . . ? C42 C41 C40 119.5(7) . . ? C42 C41 Br26 118.6(8) . . ? C40 C41 Br26 121.9(8) . . ? C41 C42 C37 121.9(10) . . ? C44 C43 C48 118.5(9) . . ? C44 C43 Si2 126.3(8) . . ? C48 C43 Si2 115.1(7) . . ? C43 C44 C45 122.3(8) . . ? C43 C44 Br27 121.3(8) . . ? C45 C44 Br27 116.3(8) . . ? C46 C45 C44 119.2(11) . . ? C45 C46 C47 119.3(7) . . ? C45 C46 Br28 118.8(9) . . ? C47 C46 Br28 121.7(9) . . ? C48 C47 C46 119.8(7) . . ? C48 C47 Br29 119.7(9) . . ? C46 C47 Br29 120.4(8) . . ? C47 C48 C43 120.8(9) . . ? C54 C49 C50 117.7(12) . . ? C54 C49 Cl1 121.1(10) . . ? C50 C49 Cl1 120.9(11) . . ? C49 C50 C51 121.2(13) . . ? C49 C50 Cl2A 131.7(12) . . ? C51 C50 Cl2A 106.1(12) . . ? C52 C51 C50 119.5(13) . . ? C51 C52 C53 121.0(13) . . ? C54 C53 C52 117.1(14) . . ? C49 C54 C53 122.9(13) . . ? C49 C54 Cl2 124.5(10) . . ? C53 C54 Cl2 112.5(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 21.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.258 _refine_diff_density_min -1.409 _refine_diff_density_rms 0.151 # Attachment '- brops 2.cif' data_brops _database_code_depnum_ccdc_archive 'CCDC 821600' #TrackingRef '- brops 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H24 Br16 O12 Si8, C S2' _chemical_formula_sum 'C49 H24 Br16 O12 S2 Si8' _chemical_formula_weight 2372.08 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7172(9) _cell_length_b 12.7392(9) _cell_length_c 13.0890(9) _cell_angle_alpha 97.592(1) _cell_angle_beta 109.075(1) _cell_angle_gamma 116.231(1) _cell_volume 1699.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9644 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 29.65 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1118 _exptl_absorpt_coefficient_mu 9.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1677 _exptl_absorpt_correction_T_max 0.3812 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2008/1) Bruker AXS area detector absorption and other corrections, University of Gottingen, Germany 2008. ; _exptl_special_details ; 4095 frames x 30 sec. @ 5.055 cm; 0.5 deg. steps in omega, 0.45 in phi ; _diffrn_ambient_temperature 85(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 66787 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 29.65 _reflns_number_total 9554 _reflns_number_gt 8581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART-APEX' _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 ; The carbon disulfide is disordered over two positions. 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^)+(0.0369P)^2^+3.7165P] 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 9554 _refine_ls_number_parameters 410 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.050 _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 0.83252(3) 0.52348(2) 0.39819(2) 0.02114(6) Uani 1 1 d . . . Br2 Br 0.49649(3) -0.07972(3) 0.17062(4) 0.03210(8) Uani 1 1 d . . . Br3 Br 0.20389(3) 0.07790(3) 0.05276(2) 0.02495(6) Uani 1 1 d . . . Br4 Br -0.00150(3) -0.15385(3) -0.49774(2) 0.02608(7) Uani 1 1 d . . . Br5 Br -0.01836(3) 0.23088(3) -0.24463(3) 0.03688(8) Uani 1 1 d . . . Br6 Br -0.00570(3) 0.45651(3) 0.23953(3) 0.03139(7) Uani 1 1 d . . . Br7 Br 0.29125(3) 0.37493(3) 0.27315(3) 0.03014(7) Uani 1 1 d . . . Br8 Br 0.74262(4) 0.92074(3) 0.64340(3) 0.04135(9) Uani 1 1 d . . . Si1 Si 0.58643(7) 0.38209(6) 0.12820(6) 0.01555(13) Uani 1 1 d . . . Si2 Si 0.33578(7) 0.25548(6) -0.09742(6) 0.01528(13) Uani 1 1 d . . . Si3 Si 0.26610(7) 0.45064(6) -0.01872(6) 0.01587(13) Uani 1 1 d . . . Si4 Si 0.51599(7) 0.57679(6) 0.20666(6) 0.01513(12) Uani 1 1 d . . . O1 O 0.46565(18) 0.28194(16) 0.00713(15) 0.0175(3) Uani 1 1 d . . . O2 O 0.28055(19) 0.33264(17) -0.04978(16) 0.0194(4) Uani 1 1 d . . . O3 O 0.37684(18) 0.54041(16) 0.10917(16) 0.0173(3) Uani 1 1 d . . . O4 O 0.54188(18) 0.46409(16) 0.18722(16) 0.0178(3) Uani 1 1 d . . . O5 O 0.37210(18) 0.30241(16) -0.19767(16) 0.0177(3) Uani 1 1 d . . . O6 O 0.29161(18) 0.52857(17) -0.10513(16) 0.0184(3) Uani 1 1 d . . . C1 C 0.6316(3) 0.2948(2) 0.2185(2) 0.0182(5) Uani 1 1 d . . . C2 C 0.5618(3) 0.1647(2) 0.1728(2) 0.0214(5) Uani 1 1 d . . . H2A H 0.4932 0.1241 0.0976 0.026 Uiso 1 1 calc R . . C3 C 0.5925(3) 0.0956(2) 0.2367(3) 0.0239(5) Uani 1 1 d . . . C4 C 0.6914(3) 0.1507(3) 0.3465(3) 0.0263(6) Uani 1 1 d . . . H4A H 0.7105 0.1016 0.3894 0.032 Uiso 1 1 calc R . . C5 C 0.7621(3) 0.2787(3) 0.3931(2) 0.0237(5) Uani 1 1 d . . . H5B H 0.8309 0.3186 0.4682 0.028 Uiso 1 1 calc R . . C6 C 0.7315(3) 0.3481(2) 0.3288(2) 0.0189(5) Uani 1 1 d . . . C7 C 0.1504(3) 0.0139(2) -0.1068(2) 0.0194(5) Uani 1 1 d . . . C8 C 0.0521(3) -0.1088(3) -0.1621(3) 0.0258(6) Uani 1 1 d . . . H8A H 0.0153 -0.1576 -0.1205 0.031 Uiso 1 1 calc R . . C9 C 0.0075(3) -0.1604(2) -0.2791(3) 0.0256(6) Uani 1 1 d . . . H9A H -0.0595 -0.2447 -0.3181 0.031 Uiso 1 1 calc R . . C10 C 0.0621(3) -0.0869(2) -0.3374(2) 0.0191(5) Uani 1 1 d . . . C11 C 0.1614(2) 0.0355(2) -0.2819(2) 0.0175(4) Uani 1 1 d . . . H11A H 0.1978 0.0835 -0.3243 0.021 Uiso 1 1 calc R . . C12 C 0.2091(2) 0.0896(2) -0.1636(2) 0.0161(4) Uani 1 1 d . . . C13 C 0.1061(3) 0.3977(2) -0.0167(2) 0.0189(5) Uani 1 1 d . . . C14 C -0.0117(3) 0.3007(3) -0.1037(2) 0.0241(5) Uani 1 1 d . . . C15 C -0.1273(3) 0.2510(3) -0.0919(3) 0.0285(6) Uani 1 1 d . . . H15A H -0.2061 0.1854 -0.1532 0.034 Uiso 1 1 calc R . . C16 C -0.1261(3) 0.2985(3) 0.0103(3) 0.0279(6) Uani 1 1 d . . . H16A H -0.2037 0.2647 0.0205 0.034 Uiso 1 1 calc R . . C17 C -0.0107(3) 0.3955(3) 0.0973(2) 0.0230(5) Uani 1 1 d . . . C18 C 0.1036(3) 0.4458(2) 0.0844(2) 0.0197(5) Uani 1 1 d . . . H18A H 0.1812 0.5138 0.1449 0.024 Uiso 1 1 calc R . . C19 C 0.5159(3) 0.6170(2) 0.3472(2) 0.0187(5) Uani 1 1 d . . . C20 C 0.4170(3) 0.5391(3) 0.3736(2) 0.0239(5) Uani 1 1 d . . . C21 C 0.4094(3) 0.5758(3) 0.4743(3) 0.0333(7) Uani 1 1 d . . . H21A H 0.3393 0.5218 0.4886 0.040 Uiso 1 1 calc R . . C22 C 0.5036(4) 0.6904(3) 0.5531(3) 0.0361(7) Uani 1 1 d . . . H22A H 0.4985 0.7170 0.6217 0.043 Uiso 1 1 calc R . . C23 C 0.6061(3) 0.7671(3) 0.5318(3) 0.0292(6) Uani 1 1 d . . . C24 C 0.6116(3) 0.7324(3) 0.4297(2) 0.0227(5) Uani 1 1 d . . . H24A H 0.6813 0.7876 0.4158 0.027 Uiso 1 1 calc R . . S1 S 0.5440(4) 0.0395(4) 0.5404(3) 0.0715(9) Uani 0.50 1 d PDU A -1 S2 S 0.3241(3) -0.2183(3) 0.3689(2) 0.0673(7) Uani 0.50 1 d PDU A -1 C25 C 0.4333(9) -0.0957(6) 0.4493(9) 0.058(2) Uani 0.50 1 d PDU A -1 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 0.02089(12) 0.01828(12) 0.01870(12) 0.00106(9) 0.00990(10) 0.00625(10) Br2 0.02609(15) 0.01620(13) 0.0483(2) 0.00788(13) 0.01235(15) 0.00991(11) Br3 0.02636(13) 0.02122(12) 0.01846(12) 0.00445(10) 0.01168(10) 0.00465(10) Br4 0.02822(14) 0.01859(12) 0.01739(12) -0.00194(9) 0.00513(10) 0.00668(11) Br5 0.02752(15) 0.02988(15) 0.03024(15) -0.01154(12) 0.01470(12) 0.00127(12) Br6 0.03489(16) 0.04088(17) 0.02793(14) 0.01018(13) 0.02290(13) 0.02077(14) Br7 0.02558(14) 0.02296(13) 0.02899(14) 0.01010(11) 0.01196(12) 0.00204(11) Br8 0.0521(2) 0.02905(16) 0.02429(15) -0.00518(13) 0.01555(15) 0.01103(16) Si1 0.0164(3) 0.0114(3) 0.0161(3) 0.0018(2) 0.0087(2) 0.0047(2) Si2 0.0164(3) 0.0101(3) 0.0159(3) 0.0009(2) 0.0094(2) 0.0034(2) Si3 0.0159(3) 0.0120(3) 0.0175(3) 0.0018(2) 0.0103(3) 0.0043(2) Si4 0.0165(3) 0.0110(3) 0.0154(3) 0.0013(2) 0.0094(2) 0.0042(2) O1 0.0174(8) 0.0124(8) 0.0176(8) 0.0008(6) 0.0083(7) 0.0045(7) O2 0.0219(9) 0.0146(8) 0.0225(9) 0.0033(7) 0.0139(7) 0.0077(7) O3 0.0176(8) 0.0142(8) 0.0180(8) 0.0024(7) 0.0098(7) 0.0059(7) O4 0.0191(8) 0.0132(8) 0.0189(8) 0.0020(7) 0.0096(7) 0.0066(7) O5 0.0180(8) 0.0124(8) 0.0179(8) 0.0013(6) 0.0105(7) 0.0031(7) O6 0.0171(8) 0.0151(8) 0.0190(8) 0.0034(7) 0.0088(7) 0.0051(7) C1 0.0189(11) 0.0154(11) 0.0216(12) 0.0047(9) 0.0124(10) 0.0078(9) C2 0.0193(12) 0.0159(11) 0.0262(13) 0.0034(10) 0.0116(10) 0.0068(10) C3 0.0221(12) 0.0151(11) 0.0357(15) 0.0076(11) 0.0151(11) 0.0089(10) C4 0.0258(14) 0.0254(13) 0.0343(15) 0.0143(12) 0.0158(12) 0.0151(12) C5 0.0228(13) 0.0256(13) 0.0233(13) 0.0088(11) 0.0106(11) 0.0123(11) C6 0.0193(11) 0.0165(11) 0.0214(12) 0.0039(9) 0.0127(10) 0.0075(9) C7 0.0204(12) 0.0160(11) 0.0175(11) 0.0039(9) 0.0084(9) 0.0063(10) C8 0.0253(13) 0.0168(12) 0.0240(13) 0.0063(10) 0.0103(11) 0.0024(10) C9 0.0237(13) 0.0135(11) 0.0249(13) 0.0024(10) 0.0076(11) 0.0014(10) C10 0.0196(11) 0.0135(11) 0.0174(11) 0.0002(9) 0.0064(9) 0.0057(9) C11 0.0179(11) 0.0130(10) 0.0180(11) 0.0017(9) 0.0087(9) 0.0054(9) C12 0.0149(10) 0.0117(10) 0.0183(11) 0.0019(9) 0.0080(9) 0.0045(9) C13 0.0195(12) 0.0147(11) 0.0209(12) 0.0025(9) 0.0121(10) 0.0063(9) C14 0.0206(12) 0.0191(12) 0.0251(13) -0.0004(10) 0.0134(11) 0.0040(10) C15 0.0186(13) 0.0239(13) 0.0317(15) 0.0018(11) 0.0130(11) 0.0028(11) C16 0.0208(13) 0.0291(14) 0.0343(15) 0.0095(12) 0.0185(12) 0.0089(11) C17 0.0255(13) 0.0245(13) 0.0244(13) 0.0074(10) 0.0167(11) 0.0130(11) C18 0.0198(12) 0.0180(11) 0.0209(12) 0.0043(9) 0.0113(10) 0.0083(10) C19 0.0221(12) 0.0167(11) 0.0174(11) 0.0040(9) 0.0119(10) 0.0081(10) C20 0.0235(13) 0.0228(13) 0.0215(12) 0.0058(10) 0.0125(11) 0.0074(11) C21 0.0327(16) 0.0405(17) 0.0308(15) 0.0130(13) 0.0238(13) 0.0148(14) C22 0.0429(19) 0.0423(18) 0.0262(15) 0.0071(13) 0.0247(14) 0.0189(16) C23 0.0346(16) 0.0244(14) 0.0200(13) -0.0013(11) 0.0133(12) 0.0099(12) C24 0.0260(13) 0.0196(12) 0.0205(12) 0.0037(10) 0.0131(11) 0.0088(11) S1 0.0642(18) 0.106(3) 0.080(2) 0.061(2) 0.0389(14) 0.058(2) S2 0.0882(19) 0.104(2) 0.0622(15) 0.0505(15) 0.0476(14) 0.0736(18) C25 0.064(5) 0.090(5) 0.104(6) 0.087(5) 0.063(4) 0.070(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 Br1 C6 1.906(3) . ? Br2 C3 1.902(3) . ? Br3 C7 1.903(3) . ? Br4 C10 1.896(3) . ? Br5 C14 1.898(3) . ? Br6 C17 1.890(3) . ? Br7 C20 1.898(3) . ? Br8 C23 1.887(3) . ? Si1 O4 1.6139(19) . ? Si1 O6 1.6212(19) 2_665 ? Si1 O1 1.6251(19) . ? Si1 C1 1.852(3) . ? Si2 O2 1.607(2) . ? Si2 O1 1.619(2) . ? Si2 O5 1.6285(19) . ? Si2 C12 1.846(2) . ? Si3 O2 1.609(2) . ? Si3 O6 1.619(2) . ? Si3 O3 1.6195(19) . ? Si3 C13 1.850(3) . ? Si4 O4 1.6157(19) . ? Si4 O3 1.618(2) . ? Si4 O5 1.6213(19) 2_665 ? Si4 C19 1.843(3) . ? O5 Si4 1.6213(19) 2_665 ? O6 Si1 1.6212(19) 2_665 ? C1 C6 1.393(4) . ? C1 C2 1.408(3) . ? C2 C3 1.383(4) . ? C3 C4 1.382(4) . ? C4 C5 1.387(4) . ? C5 C6 1.388(4) . ? C7 C8 1.383(4) . ? C7 C12 1.397(3) . ? C8 C9 1.391(4) . ? C9 C10 1.379(4) . ? C10 C11 1.384(3) . ? C11 C12 1.406(3) . ? C13 C14 1.394(4) . ? C13 C18 1.399(4) . ? C14 C15 1.391(4) . ? C15 C16 1.386(4) . ? C16 C17 1.382(4) . ? C17 C18 1.384(4) . ? C19 C24 1.396(4) . ? C19 C20 1.400(4) . ? C20 C21 1.388(4) . ? C21 C22 1.371(5) . ? C22 C23 1.384(5) . ? C23 C24 1.385(4) . ? S1 C25 1.608(7) . ? S2 C25 1.473(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 O4 Si1 O6 109.56(10) . 2_665 ? O4 Si1 O1 109.00(10) . . ? O6 Si1 O1 109.27(10) 2_665 . ? O4 Si1 C1 111.46(11) . . ? O6 Si1 C1 109.91(11) 2_665 . ? O1 Si1 C1 107.59(11) . . ? O2 Si2 O1 108.27(10) . . ? O2 Si2 O5 108.82(10) . . ? O1 Si2 O5 109.60(10) . . ? O2 Si2 C12 110.23(11) . . ? O1 Si2 C12 112.98(11) . . ? O5 Si2 C12 106.88(10) . . ? O2 Si3 O6 110.16(10) . . ? O2 Si3 O3 108.28(11) . . ? O6 Si3 O3 107.51(10) . . ? O2 Si3 C13 109.02(11) . . ? O6 Si3 C13 114.23(11) . . ? O3 Si3 C13 107.44(11) . . ? O4 Si4 O3 110.50(10) . . ? O4 Si4 O5 109.43(10) . 2_665 ? O3 Si4 O5 107.96(10) . 2_665 ? O4 Si4 C19 111.90(11) . . ? O3 Si4 C19 107.97(11) . . ? O5 Si4 C19 108.98(11) 2_665 . ? Si2 O1 Si1 144.10(13) . . ? Si2 O2 Si3 155.88(13) . . ? Si4 O3 Si3 144.18(13) . . ? Si1 O4 Si4 153.96(13) . . ? Si4 O5 Si2 137.47(12) 2_665 . ? Si3 O6 Si1 137.83(13) . 2_665 ? C6 C1 C2 116.8(2) . . ? C6 C1 Si1 124.93(19) . . ? C2 C1 Si1 118.3(2) . . ? C3 C2 C1 120.4(3) . . ? C4 C3 C2 121.8(3) . . ? C4 C3 Br2 119.5(2) . . ? C2 C3 Br2 118.8(2) . . ? C3 C4 C5 118.9(3) . . ? C4 C5 C6 119.3(3) . . ? C5 C6 C1 122.9(2) . . ? C5 C6 Br1 117.1(2) . . ? C1 C6 Br1 120.1(2) . . ? C8 C7 C12 122.6(2) . . ? C8 C7 Br3 116.9(2) . . ? C12 C7 Br3 120.44(19) . . ? C7 C8 C9 119.6(3) . . ? C10 C9 C8 118.8(2) . . ? C9 C10 C11 121.6(2) . . ? C9 C10 Br4 119.5(2) . . ? C11 C10 Br4 118.9(2) . . ? C10 C11 C12 120.7(2) . . ? C7 C12 C11 116.6(2) . . ? C7 C12 Si2 125.28(19) . . ? C11 C12 Si2 118.00(18) . . ? C14 C13 C18 116.9(2) . . ? C14 C13 Si3 124.3(2) . . ? C18 C13 Si3 118.2(2) . . ? C15 C14 C13 122.6(3) . . ? C15 C14 Br5 117.4(2) . . ? C13 C14 Br5 119.9(2) . . ? C16 C15 C14 119.1(3) . . ? C17 C16 C15 119.2(3) . . ? C16 C17 C18 121.4(3) . . ? C16 C17 Br6 119.7(2) . . ? C18 C17 Br6 118.8(2) . . ? C17 C18 C13 120.7(2) . . ? C24 C19 C20 116.9(2) . . ? C24 C19 Si4 120.4(2) . . ? C20 C19 Si4 122.5(2) . . ? C21 C20 C19 122.2(3) . . ? C21 C20 Br7 117.6(2) . . ? C19 C20 Br7 120.1(2) . . ? C22 C21 C20 119.6(3) . . ? C21 C22 C23 119.5(3) . . ? C22 C23 C24 121.0(3) . . ? C22 C23 Br8 120.1(2) . . ? C24 C23 Br8 118.9(2) . . ? C23 C24 C19 120.7(3) . . ? S2 C25 S1 175.2(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.65 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.429 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.114 # Attachment '- obr8a 2.cif' data_obr8a _database_code_depnum_ccdc_archive 'CCDC 821601' #TrackingRef '- obr8a 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H32 Br8 O12 Si8, 2.5(C8 H10)' _chemical_formula_sum 'C68 H57 Br8 O12 Si8' _chemical_formula_weight 1930.14 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 20.5738(10) _cell_length_b 20.5738(10) _cell_length_c 36.261(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15348.5(19) _cell_formula_units_Z 8 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9816 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.96 _exptl_crystal_description octahedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7624 _exptl_absorpt_coefficient_mu 4.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2779 _exptl_absorpt_correction_T_max 0.3686 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2008/1) Bruker AXS area detector absorption and other corrections, University of Gottingen, Germany 2008. ; _exptl_special_details ; 5280 frames x 30 sec. @ 5.055 cm; 0.5 deg. steps in omega, 0.45 deg. in phi ; _diffrn_ambient_temperature 85(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 333383 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0142 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.34 _reflns_number_total 9574 _reflns_number_gt 8392 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART-APEX' _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 ; The complex lies on a two-fold axis in the crystal lattice. There is one molecule of meta-xylene on a general position, disordered over two sites. It was modeled by placement of partial occupancy atoms with restraints (SAME/DELU/SIMU) applied to maintain chemical sensibility. There is also the equivalent of 0.5 molecule of meta-xylene per Si-O complex located at inversion voids of the lattice. This was modeled by use of the SQUEEZE sub-routine of the PLATON program suite. - PLATON Reference : A.L.Spek (2008) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. Four solvent accessible voids of total volume 1411 A^3 were estimated to hold the contribution of 804 electrons per unit cell due to diffuse solvent scattering. 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^)+(0.0828P)^2^+2.2331P] 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 9574 _refine_ls_number_parameters 490 _refine_ls_number_restraints 262 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.002 _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 0.08376(2) 0.198317(19) -0.183434(9) 0.05718(10) Uani 1 1 d . . . Br2 Br 0.259008(16) 0.22592(2) -0.001935(10) 0.05336(9) Uani 1 1 d . . . Br3 Br 0.053594(15) 0.317434(14) 0.086379(7) 0.03699(7) Uani 1 1 d . . . Br4 Br 0.213477(17) 0.360496(19) -0.101936(14) 0.06793(12) Uani 1 1 d . . . Si1 Si 0.09350(3) 0.19832(3) -0.090080(17) 0.02270(13) Uani 1 1 d . . . Si2 Si 0.09581(3) 0.20179(3) -0.005873(17) 0.02025(13) Uani 1 1 d . . . Si3 Si 0.05256(3) 0.34327(3) -0.005686(17) 0.02032(13) Uani 1 1 d . . . Si4 Si 0.04876(3) 0.34645(3) -0.089815(17) 0.02242(13) Uani 1 1 d . . . O1 O 0.11768(8) 0.18671(8) -0.04800(4) 0.0243(4) Uani 1 1 d . . . O2 O 0.09723(8) 0.27945(8) 0.00047(5) 0.0253(4) Uani 1 1 d . . . O3 O 0.06241(9) 0.36893(8) -0.04757(4) 0.0263(4) Uani 1 1 d . . . O4 O 0.07631(9) 0.27391(8) -0.09587(5) 0.0265(4) Uani 1 1 d . . . O5 O 0.02924(9) 0.15470(8) -0.09715(5) 0.0271(4) Uani 1 1 d . . . O6 O 0.02284(8) 0.17521(8) 0.00013(5) 0.0247(4) Uani 1 1 d . . . C1 C 0.16134(13) 0.17115(12) -0.12001(7) 0.0297(5) Uani 1 1 d . . . C2 C 0.16025(15) 0.17132(13) -0.15857(8) 0.0381(7) Uani 1 1 d . . . C3 C 0.21303(18) 0.15119(17) -0.17968(9) 0.0520(9) Uani 1 1 d . . . H3A H 0.2112 0.1530 -0.2058 0.062 Uiso 1 1 calc R . . C4 C 0.26830(17) 0.12838(17) -0.16201(10) 0.0547(9) Uani 1 1 d . . . H4A H 0.3042 0.1140 -0.1763 0.066 Uiso 1 1 calc R . . C5 C 0.27194(16) 0.12620(17) -0.12404(10) 0.0501(8) Uani 1 1 d . . . H5B H 0.3097 0.1100 -0.1121 0.060 Uiso 1 1 calc R . . C6 C 0.21874(14) 0.14842(14) -0.10340(8) 0.0382(7) Uani 1 1 d . . . H6B H 0.2216 0.1481 -0.0773 0.046 Uiso 1 1 calc R . . C7 C 0.14942(12) 0.15802(11) 0.02681(6) 0.0264(5) Uani 1 1 d . . . C8 C 0.21602(14) 0.16583(15) 0.02928(8) 0.0369(6) Uani 1 1 d . . . C9 C 0.25428(15) 0.12968(18) 0.05371(9) 0.0502(8) Uani 1 1 d . . . H9A H 0.2999 0.1367 0.0551 0.060 Uiso 1 1 calc R . . C10 C 0.22484(17) 0.08360(17) 0.07587(8) 0.0491(8) Uani 1 1 d . . . H10A H 0.2505 0.0583 0.0923 0.059 Uiso 1 1 calc R . . C11 C 0.15850(16) 0.07399(15) 0.07435(7) 0.0420(7) Uani 1 1 d . . . H11A H 0.1384 0.0424 0.0897 0.050 Uiso 1 1 calc R . . C12 C 0.12164(15) 0.11092(13) 0.05033(7) 0.0335(6) Uani 1 1 d . . . H12A H 0.0760 0.1044 0.0496 0.040 Uiso 1 1 calc R . . C13 C 0.07578(11) 0.40811(10) 0.02695(6) 0.0215(5) Uani 1 1 d . . . C14 C 0.07284(11) 0.40033(11) 0.06535(6) 0.0247(5) Uani 1 1 d . . . C15 C 0.08600(13) 0.44984(13) 0.08985(7) 0.0319(6) Uani 1 1 d . . . H15A H 0.0817 0.4433 0.1157 0.038 Uiso 1 1 calc R . . C16 C 0.10560(15) 0.50925(13) 0.07592(8) 0.0394(7) Uani 1 1 d . . . H16A H 0.1154 0.5438 0.0924 0.047 Uiso 1 1 calc R . . C17 C 0.11106(17) 0.51895(13) 0.03857(9) 0.0427(7) Uani 1 1 d . . . H17A H 0.1254 0.5597 0.0293 0.051 Uiso 1 1 calc R . . C18 C 0.09556(14) 0.46894(12) 0.01431(7) 0.0319(6) Uani 1 1 d . . . H18A H 0.0985 0.4764 -0.0115 0.038 Uiso 1 1 calc R . . C19 C 0.08561(13) 0.40636(11) -0.12159(6) 0.0260(5) Uani 1 1 d . . . C20 C 0.15249(14) 0.41401(13) -0.12741(8) 0.0354(6) Uani 1 1 d . . . C21 C 0.17787(16) 0.46090(14) -0.15111(8) 0.0414(7) Uani 1 1 d . . . H21A H 0.2235 0.4641 -0.1548 0.050 Uiso 1 1 calc R . . C22 C 0.13610(17) 0.50268(13) -0.16907(7) 0.0418(7) Uani 1 1 d . . . H22A H 0.1529 0.5347 -0.1853 0.050 Uiso 1 1 calc R . . C23 C 0.07021(18) 0.49806(14) -0.16354(8) 0.0436(8) Uani 1 1 d . . . H23A H 0.0416 0.5276 -0.1755 0.052 Uiso 1 1 calc R . . C24 C 0.04532(15) 0.45006(13) -0.14039(8) 0.0368(6) Uani 1 1 d . . . H24A H -0.0004 0.4469 -0.1373 0.044 Uiso 1 1 calc R . . C25 C 0.2861(3) 0.3530(2) 0.78720(15) 0.0873(15) Uani 0.848(4) 1 d PDU A 1 C26 C 0.2201(3) 0.3368(3) 0.77976(14) 0.0724(13) Uani 0.848(4) 1 d PDU A 1 H26 H 0.2041 0.2949 0.7860 0.087 Uiso 0.848(4) 1 calc PR A 1 C27 C 0.1789(3) 0.3819(3) 0.76334(14) 0.0936(15) Uani 0.848(4) 1 d PDU A 1 C28 C 0.2046(4) 0.4414(3) 0.75370(15) 0.1197(17) Uani 0.848(4) 1 d PDU A 1 H28 H 0.1769 0.4715 0.7415 0.144 Uiso 0.848(4) 1 calc PR A 1 C29 C 0.2648(4) 0.4590(4) 0.76028(17) 0.136(2) Uani 0.848(4) 1 d PDU A 1 H29 H 0.2798 0.5011 0.7538 0.163 Uiso 0.848(4) 1 calc PR A 1 C30 C 0.3072(4) 0.4130(3) 0.77753(16) 0.1118(17) Uani 0.848(4) 1 d PDU A 1 H30 H 0.3511 0.4247 0.7823 0.134 Uiso 0.848(4) 1 calc PR A 1 C31 C 0.3302(3) 0.3016(3) 0.8038(2) 0.111(2) Uani 0.848(4) 1 d PDU A 1 H31A H 0.3756 0.3121 0.7982 0.166 Uiso 0.848(4) 1 calc PR A 1 H31B H 0.3193 0.2590 0.7935 0.166 Uiso 0.848(4) 1 calc PR A 1 H31C H 0.3242 0.3006 0.8306 0.166 Uiso 0.848(4) 1 calc PR A 1 C32 C 0.1087(3) 0.3614(4) 0.7577(2) 0.129(3) Uani 0.848(4) 1 d PDU A 1 H32A H 0.1074 0.3213 0.7431 0.194 Uiso 0.848(4) 1 calc PR A 1 H32B H 0.0852 0.3958 0.7447 0.194 Uiso 0.848(4) 1 calc PR A 1 H32C H 0.0883 0.3536 0.7817 0.194 Uiso 0.848(4) 1 calc PR A 1 C25A C 0.2324(5) 0.3723(5) 0.7767(7) 0.103(4) Uani 0.152(4) 1 d PDU A 2 C26A C 0.1653(6) 0.3565(10) 0.7745(6) 0.105(4) Uani 0.152(4) 1 d PDU A 2 H26A H 0.1480 0.3234 0.7899 0.125 Uiso 0.152(4) 1 calc PR A 2 C27A C 0.1246(5) 0.3890(6) 0.7500(5) 0.101(4) Uani 0.152(4) 1 d PDU A 2 C29A C 0.1469(8) 0.4472(8) 0.7365(7) 0.122(4) Uani 0.152(4) 1 d PDU A 2 H29A H 0.1191 0.4705 0.7203 0.146 Uiso 0.152(4) 1 calc PR A 2 C28A C 0.2041(8) 0.4734(9) 0.7441(6) 0.120(4) Uani 0.152(4) 1 d PDU A 2 H28A H 0.2160 0.5155 0.7357 0.144 Uiso 0.152(4) 1 calc PR A 2 C30A C 0.2474(10) 0.4334(7) 0.7661(8) 0.120(4) Uani 0.152(4) 1 d PDU A 2 H30A H 0.2881 0.4510 0.7735 0.144 Uiso 0.152(4) 1 calc PR A 2 C31A C 0.2768(8) 0.3172(8) 0.7888(8) 0.120(6) Uani 0.152(4) 1 d PDU A 2 H31D H 0.3036 0.3032 0.7679 0.179 Uiso 0.152(4) 1 calc PR A 2 H31E H 0.2504 0.2806 0.7975 0.179 Uiso 0.152(4) 1 calc PR A 2 H31F H 0.3049 0.3323 0.8089 0.179 Uiso 0.152(4) 1 calc PR A 2 C32A C 0.0676(8) 0.3488(11) 0.7362(9) 0.135(9) Uani 0.152(4) 1 d PDU A 2 H32D H 0.0272 0.3735 0.7393 0.203 Uiso 0.152(4) 1 calc PR A 2 H32E H 0.0649 0.3083 0.7503 0.203 Uiso 0.152(4) 1 calc PR A 2 H32F H 0.0739 0.3387 0.7100 0.203 Uiso 0.152(4) 1 calc PR A 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 Br1 0.0769(2) 0.0668(2) 0.02780(14) -0.00209(14) -0.00230(15) 0.01139(18) Br2 0.03531(14) 0.0688(2) 0.05595(19) 0.00201(16) -0.00007(13) -0.01185(14) Br3 0.05024(15) 0.03352(12) 0.02721(12) 0.00363(10) 0.00344(11) -0.00887(11) Br4 0.03924(16) 0.05777(19) 0.1068(3) 0.0334(2) 0.00372(18) 0.00033(14) Si1 0.0307(3) 0.0186(3) 0.0188(3) -0.0013(2) 0.0032(2) -0.0006(2) Si2 0.0231(3) 0.0181(2) 0.0195(3) -0.0009(2) 0.0004(2) 0.0001(2) Si3 0.0260(3) 0.0170(2) 0.0180(3) -0.0016(2) 0.0009(2) -0.0023(2) Si4 0.0321(3) 0.0172(2) 0.0180(3) 0.0010(2) 0.0018(2) -0.0029(2) O1 0.0305(8) 0.0233(7) 0.0192(7) -0.0009(6) 0.0026(6) 0.0024(6) O2 0.0288(8) 0.0189(7) 0.0282(8) -0.0033(6) -0.0010(7) -0.0005(6) O3 0.0381(9) 0.0227(7) 0.0182(7) -0.0009(6) 0.0028(6) -0.0050(7) O4 0.0363(8) 0.0193(7) 0.0238(7) 0.0007(6) 0.0019(7) -0.0013(6) O5 0.0322(8) 0.0218(7) 0.0273(8) -0.0036(6) 0.0006(7) -0.0025(6) O6 0.0253(7) 0.0247(7) 0.0240(7) 0.0009(6) 0.0008(6) -0.0039(6) C1 0.0391(12) 0.0228(10) 0.0272(11) -0.0058(9) 0.0086(10) -0.0039(9) C2 0.0534(16) 0.0318(12) 0.0292(12) -0.0066(10) 0.0095(11) -0.0074(12) C3 0.070(2) 0.0508(17) 0.0347(14) -0.0133(13) 0.0216(14) -0.0107(15) C4 0.0469(16) 0.0527(18) 0.064(2) -0.0197(15) 0.0252(15) -0.0081(14) C5 0.0402(15) 0.0529(17) 0.0573(19) -0.0144(15) 0.0145(14) 0.0008(13) C6 0.0350(13) 0.0412(14) 0.0384(14) -0.0085(12) 0.0079(11) -0.0004(11) C7 0.0329(11) 0.0241(10) 0.0221(10) -0.0058(8) -0.0016(9) 0.0052(9) C8 0.0341(12) 0.0464(15) 0.0301(12) -0.0057(11) -0.0032(10) 0.0053(11) C9 0.0359(14) 0.073(2) 0.0422(15) -0.0157(15) -0.0076(12) 0.0186(14) C10 0.0680(19) 0.0547(17) 0.0246(12) -0.0010(12) -0.0061(13) 0.0283(15) C11 0.0656(18) 0.0392(14) 0.0213(11) 0.0008(10) -0.0025(12) 0.0174(13) C12 0.0463(14) 0.0307(12) 0.0234(11) -0.0002(9) -0.0020(10) 0.0073(11) C13 0.0235(9) 0.0177(9) 0.0234(10) -0.0016(8) -0.0009(8) 0.0011(8) C14 0.0253(10) 0.0241(10) 0.0246(10) -0.0007(8) -0.0021(9) 0.0012(8) C15 0.0358(12) 0.0333(12) 0.0267(11) -0.0062(10) -0.0041(10) 0.0042(10) C16 0.0515(15) 0.0279(12) 0.0388(13) -0.0118(11) -0.0119(12) 0.0025(11) C17 0.0647(18) 0.0203(11) 0.0429(15) 0.0014(11) -0.0083(14) -0.0077(12) C18 0.0455(14) 0.0210(10) 0.0293(12) 0.0019(9) -0.0024(11) -0.0025(10) C19 0.0387(12) 0.0194(9) 0.0200(10) -0.0010(8) 0.0042(9) -0.0044(9) C20 0.0411(13) 0.0285(12) 0.0364(13) 0.0026(10) 0.0078(11) -0.0006(10) C21 0.0487(15) 0.0342(13) 0.0413(14) -0.0013(11) 0.0173(12) -0.0076(12) C22 0.0725(19) 0.0268(12) 0.0259(12) 0.0014(10) 0.0130(12) -0.0104(12) C23 0.0655(19) 0.0296(13) 0.0356(14) 0.0104(11) -0.0074(13) -0.0033(13) C24 0.0457(14) 0.0325(12) 0.0324(13) 0.0085(10) -0.0012(11) -0.0057(11) C25 0.109(3) 0.085(3) 0.068(3) -0.030(2) 0.040(2) -0.031(3) C26 0.100(3) 0.062(3) 0.055(2) -0.008(2) 0.023(2) -0.007(2) C27 0.158(4) 0.072(3) 0.051(2) 0.000(2) 0.033(3) 0.030(3) C28 0.229(4) 0.075(3) 0.054(3) -0.002(2) 0.059(3) 0.040(3) C29 0.237(5) 0.095(4) 0.075(3) -0.014(3) 0.100(3) -0.015(4) C30 0.169(4) 0.091(3) 0.076(3) -0.033(3) 0.068(3) -0.050(3) C31 0.089(4) 0.115(5) 0.129(6) -0.017(4) 0.017(4) -0.011(4) C32 0.152(4) 0.129(5) 0.107(6) -0.008(5) -0.012(5) 0.068(4) C25A 0.150(6) 0.094(6) 0.067(10) -0.014(7) 0.032(8) 0.004(6) C26A 0.148(5) 0.095(8) 0.070(9) -0.021(7) 0.030(7) 0.008(6) C27A 0.136(7) 0.090(7) 0.076(10) -0.019(7) 0.055(7) 0.029(5) C29A 0.189(7) 0.101(8) 0.075(11) -0.011(7) 0.070(8) 0.027(6) C28A 0.211(8) 0.089(8) 0.060(10) -0.004(7) 0.079(8) -0.003(6) C30A 0.193(8) 0.096(6) 0.070(10) -0.020(8) 0.058(8) -0.010(6) C31A 0.153(9) 0.114(9) 0.092(16) -0.032(11) 0.063(12) 0.043(10) C32A 0.156(11) 0.116(14) 0.13(2) -0.01(2) -0.004(11) 0.031(10) _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 C2 1.897(3) . ? Br2 C8 1.895(3) . ? Br3 C14 1.910(2) . ? Br4 C20 1.908(3) . ? Si1 O4 1.6086(17) . ? Si1 O5 1.6184(18) . ? Si1 O1 1.6225(17) . ? Si1 C1 1.854(3) . ? Si2 O6 1.6124(17) . ? Si2 O2 1.6145(17) . ? Si2 O1 1.6224(17) . ? Si2 C7 1.853(2) . ? Si3 O6 1.6111(17) 6_454 ? Si3 O2 1.6181(17) . ? Si3 O3 1.6208(17) . ? Si3 C13 1.846(2) . ? Si4 O4 1.6116(17) . ? Si4 O3 1.6244(17) . ? Si4 O5 1.6268(19) 6_454 ? Si4 C19 1.850(2) . ? O5 Si4 1.6268(19) 6_454 ? O6 Si3 1.6111(17) 6_454 ? C1 C2 1.398(4) . ? C1 C6 1.406(4) . ? C2 C3 1.392(4) . ? C3 C4 1.387(5) . ? C4 C5 1.380(5) . ? C5 C6 1.402(4) . ? C7 C8 1.383(4) . ? C7 C12 1.412(4) . ? C8 C9 1.399(4) . ? C9 C10 1.382(5) . ? C10 C11 1.380(5) . ? C11 C12 1.383(4) . ? C13 C18 1.394(3) . ? C13 C14 1.403(3) . ? C14 C15 1.378(3) . ? C15 C16 1.383(4) . ? C16 C17 1.373(4) . ? C17 C18 1.391(4) . ? C19 C24 1.400(4) . ? C19 C20 1.401(4) . ? C20 C21 1.393(4) . ? C21 C22 1.379(4) . ? C22 C23 1.373(5) . ? C23 C24 1.394(4) . ? C25 C30 1.354(8) . ? C25 C26 1.424(8) . ? C25 C31 1.518(7) . ? C26 C27 1.391(8) . ? C27 C28 1.377(8) . ? C27 C32 1.519(7) . ? C28 C29 1.313(11) . ? C29 C30 1.432(11) . ? C25A C30A 1.350(15) . ? C25A C26A 1.420(14) . ? C25A C31A 1.520(9) . ? C26A C27A 1.390(16) . ? C27A C29A 1.373(16) . ? C27A C32A 1.522(9) . ? C29A C28A 1.323(18) . ? C28A C30A 1.453(19) . ? 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 O4 Si1 O5 109.62(10) . . ? O4 Si1 O1 109.41(9) . . ? O5 Si1 O1 108.53(9) . . ? O4 Si1 C1 112.37(10) . . ? O5 Si1 C1 110.80(10) . . ? O1 Si1 C1 105.98(11) . . ? O6 Si2 O2 109.47(9) . . ? O6 Si2 O1 108.70(9) . . ? O2 Si2 O1 108.55(9) . . ? O6 Si2 C7 107.64(10) . . ? O2 Si2 C7 112.28(10) . . ? O1 Si2 C7 110.14(10) . . ? O6 Si3 O2 109.71(9) 6_454 . ? O6 Si3 O3 108.66(9) 6_454 . ? O2 Si3 O3 108.82(9) . . ? O6 Si3 C13 109.61(10) 6_454 . ? O2 Si3 C13 110.55(9) . . ? O3 Si3 C13 109.45(9) . . ? O4 Si4 O3 109.35(9) . . ? O4 Si4 O5 108.13(9) . 6_454 ? O3 Si4 O5 109.19(9) . 6_454 ? O4 Si4 C19 112.84(10) . . ? O3 Si4 C19 109.08(10) . . ? O5 Si4 C19 108.19(10) 6_454 . ? Si2 O1 Si1 140.56(11) . . ? Si2 O2 Si3 140.64(12) . . ? Si3 O3 Si4 140.29(11) . . ? Si1 O4 Si4 162.73(12) . . ? Si1 O5 Si4 142.01(11) . 6_454 ? Si3 O6 Si2 163.49(12) 6_454 . ? C2 C1 C6 116.3(2) . . ? C2 C1 Si1 124.9(2) . . ? C6 C1 Si1 118.8(2) . . ? C3 C2 C1 122.5(3) . . ? C3 C2 Br1 118.2(2) . . ? C1 C2 Br1 119.3(2) . . ? C4 C3 C2 119.1(3) . . ? C5 C4 C3 121.1(3) . . ? C4 C5 C6 118.6(3) . . ? C5 C6 C1 122.4(3) . . ? C8 C7 C12 116.2(2) . . ? C8 C7 Si2 125.1(2) . . ? C12 C7 Si2 118.62(19) . . ? C7 C8 C9 122.5(3) . . ? C7 C8 Br2 120.0(2) . . ? C9 C8 Br2 117.5(2) . . ? C10 C9 C8 119.1(3) . . ? C11 C10 C9 120.6(3) . . ? C10 C11 C12 119.3(3) . . ? C11 C12 C7 122.4(3) . . ? C18 C13 C14 116.2(2) . . ? C18 C13 Si3 120.90(18) . . ? C14 C13 Si3 122.87(17) . . ? C15 C14 C13 123.2(2) . . ? C15 C14 Br3 116.32(18) . . ? C13 C14 Br3 120.47(17) . . ? C14 C15 C16 118.4(2) . . ? C17 C16 C15 120.8(2) . . ? C16 C17 C18 119.8(3) . . ? C17 C18 C13 121.5(2) . . ? C24 C19 C20 115.8(2) . . ? C24 C19 Si4 119.2(2) . . ? C20 C19 Si4 124.84(19) . . ? C21 C20 C19 122.6(3) . . ? C21 C20 Br4 116.9(2) . . ? C19 C20 Br4 120.54(19) . . ? C22 C21 C20 119.3(3) . . ? C23 C22 C21 120.2(3) . . ? C22 C23 C24 120.0(3) . . ? C23 C24 C19 122.1(3) . . ? C30 C25 C26 118.1(6) . . ? C30 C25 C31 123.0(6) . . ? C26 C25 C31 118.8(5) . . ? C27 C26 C25 120.4(5) . . ? C28 C27 C26 117.9(6) . . ? C28 C27 C32 125.3(6) . . ? C26 C27 C32 116.8(5) . . ? C29 C28 C27 124.1(7) . . ? C28 C29 C30 118.2(7) . . ? C25 C30 C29 121.3(7) . . ? C30A C25A C26A 114.8(13) . . ? C30A C25A C31A 129.6(13) . . ? C26A C25A C31A 115.5(12) . . ? C27A C26A C25A 120.7(14) . . ? C29A C27A C26A 116.5(12) . . ? C29A C27A C32A 127.9(17) . . ? C26A C27A C32A 114.4(15) . . ? C28A C29A C27A 125.3(16) . . ? C29A C28A C30A 115.4(16) . . ? C25A C30A C28A 122.8(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.994 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.121