# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 182/1876 data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,2,2,5-tetrakis[di-tert-butyl(methyl)silyl]-4,7-diphenyl- 1,2,5-trisilabicyclo[4.2.0]hepta-3,6-diene ; _chemical_formula_sum 'C52 H96 Si7' _chemical_formula_weight 917.92 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' _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 13.7380(8) _cell_length_b 14.6250(9) _cell_length_c 15.751(1) _cell_angle_alpha 99.765(3) _cell_angle_beta 114.847(3) _cell_angle_gamma 92.241(3) _cell_volume 2808.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used 26823 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.95 _exptl_crystal_description 'Cube' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.085 _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.201 _exptl_absorpt_correction_type 'none' _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Mac Science DIP2030 Image plate' _diffrn_reflns_number 26823 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.95 _reflns_number_total 12169 _reflns_number_gt 10097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MacScience Xpress' _computing_cell_refinement 'Scalepack' _computing_data_reduction 'Denzo' _computing_structure_solution 'SIR92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material 'CIFTAB' _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^)+(0.1085P)^2^+4.4780P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0211(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12169 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.2015 _refine_ls_wR_factor_gt 0.1851 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.004 _diffrn_orient_matrix_type 'X=UH' _diffrn_orient_matrix_UB_11 0.04762 _diffrn_orient_matrix_UB_12 0.04807 _diffrn_orient_matrix_UB_13 0.04390 _diffrn_orient_matrix_UB_21 -0.01647 _diffrn_orient_matrix_UB_22 -0.02639 _diffrn_orient_matrix_UB_23 0.06238 _diffrn_orient_matrix_UB_31 0.06207 _diffrn_orient_matrix_UB_32 -0.02849 _diffrn_orient_matrix_UB_33 0.02066 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 0.69981(6) 0.19595(5) 0.34413(5) 0.02519(18) Uani 1 1 d . . . Si2 Si 0.66697(6) 0.32161(5) 0.25144(5) 0.02296(17) Uani 1 1 d . . . Si3 Si 0.78245(6) 0.26771(5) 0.18002(5) 0.02307(17) Uani 1 1 d . . . Si4 Si 0.54755(7) 0.07082(5) 0.27274(6) 0.02864(19) Uani 1 1 d . . . Si5 Si 0.82126(8) 0.24253(7) 0.51757(6) 0.0375(2) Uani 1 1 d . . . Si6 Si 0.66444(7) 0.48930(5) 0.29877(6) 0.02808(19) Uani 1 1 d . . . Si7 Si 0.91833(7) 0.34926(5) 0.15012(6) 0.02787(18) Uani 1 1 d . . . C1 C 0.8188(2) 0.15531(18) 0.22621(19) 0.0252(5) Uani 1 1 d . . . C2 C 0.7883(2) 0.13534(19) 0.2928(2) 0.0286(6) Uani 1 1 d . . . H2 H 0.8125 0.0827 0.3217 0.050 Uiso 1 1 d R . . C3 C 0.5732(2) 0.26988(18) 0.11760(19) 0.0248(5) Uani 1 1 d . . . C4 C 0.6414(2) 0.24231(19) 0.0789(2) 0.0262(5) Uani 1 1 d . . . H4 H 0.6220 0.2151 0.0132 0.050 Uiso 1 1 d R . . C5 C 0.8778(2) 0.08739(19) 0.1900(2) 0.0282(6) Uani 1 1 d . . . C6 C 0.8419(3) 0.0526(2) 0.0923(2) 0.0330(6) Uani 1 1 d . . . H6 H 0.7777 0.0722 0.0479 0.050 Uiso 1 1 d R . . C7 C 0.8987(3) -0.0093(2) 0.0587(3) 0.0421(8) Uani 1 1 d . . . H7 H 0.8726 -0.0327 -0.0087 0.050 Uiso 1 1 d R . . C8 C 0.9921(3) -0.0373(2) 0.1227(3) 0.0475(9) Uani 1 1 d . . . H8 H 1.0316 -0.0791 0.0998 0.050 Uiso 1 1 d R . . C9 C 1.0279(3) -0.0047(3) 0.2200(3) 0.0491(9) Uani 1 1 d . . . H9 H 1.0921 -0.0241 0.2645 0.050 Uiso 1 1 d R . . C10 C 0.9708(3) 0.0560(2) 0.2533(3) 0.0400(7) Uani 1 1 d . . . H10 H 0.9946 0.0773 0.3208 0.050 Uiso 1 1 d R . . C11 C 0.4538(2) 0.26323(19) 0.06251(19) 0.0259(5) Uani 1 1 d . . . C12 C 0.3954(2) 0.3275(2) 0.0908(2) 0.0324(6) Uani 1 1 d . . . H12 H 0.4354 0.3753 0.1471 0.050 Uiso 1 1 d R . . C13 C 0.2836(3) 0.3234(2) 0.0396(3) 0.0392(7) Uani 1 1 d . . . H13 H 0.2466 0.3693 0.0594 0.050 Uiso 1 1 d R . . C14 C 0.2285(3) 0.2527(3) -0.0401(2) 0.0397(7) Uani 1 1 d . . . H14 H 0.1526 0.2492 -0.0752 0.050 Uiso 1 1 d R . . C15 C 0.2843(3) 0.1874(2) -0.0693(2) 0.0366(7) Uani 1 1 d . . . H15 H 0.2459 0.1383 -0.1243 0.050 Uiso 1 1 d R . . C16 C 0.3958(2) 0.1926(2) -0.0197(2) 0.0300(6) Uani 1 1 d . . . H16 H 0.4347 0.1480 -0.0414 0.050 Uiso 1 1 d R . . C17 C 0.5276(3) 0.0430(2) 0.1446(2) 0.0340(6) Uani 1 1 d . . . H17A H 0.5131 0.0981 0.1181 0.050 Uiso 1 1 d R . . H17B H 0.4678 -0.0053 0.1082 0.050 Uiso 1 1 d R . . H17C H 0.5919 0.0221 0.1423 0.050 Uiso 1 1 d R . . C18 C 0.4144(3) 0.1117(2) 0.2714(2) 0.0361(7) Uani 1 1 d . . . C19 C 0.4215(3) 0.2184(2) 0.2820(2) 0.0351(6) Uani 1 1 d . . . H19A H 0.4408 0.2358 0.2341 0.050 Uiso 1 1 d R . . H19B H 0.4767 0.2478 0.3443 0.050 Uiso 1 1 d R . . H19C H 0.3537 0.2382 0.2740 0.050 Uiso 1 1 d R . . C20 C 0.3190(3) 0.0689(3) 0.1737(3) 0.0534(10) Uani 1 1 d . . . H20A H 0.3354 0.0827 0.1232 0.050 Uiso 1 1 d R . . H20B H 0.2549 0.0950 0.1701 0.050 Uiso 1 1 d R . . H20C H 0.3078 0.0024 0.1672 0.050 Uiso 1 1 d R . . C21 C 0.3846(4) 0.0874(3) 0.3495(3) 0.0534(10) Uani 1 1 d . . . H21A H 0.4426 0.1132 0.4112 0.050 Uiso 1 1 d R . . H21B H 0.3728 0.0207 0.3416 0.050 Uiso 1 1 d R . . H21C H 0.3199 0.1133 0.3445 0.050 Uiso 1 1 d R . . C22 C 0.5763(3) -0.0471(2) 0.3149(3) 0.0407(8) Uani 1 1 d . . . C23 C 0.4766(4) -0.1198(2) 0.2548(3) 0.0550(10) Uani 1 1 d . . . H23A H 0.4149 -0.0984 0.2634 0.050 Uiso 1 1 d R . . H23B H 0.4891 -0.1783 0.2749 0.050 Uiso 1 1 d R . . H23C H 0.4611 -0.1280 0.1886 0.050 Uiso 1 1 d R . . C24 C 0.6053(5) -0.0393(3) 0.4215(3) 0.0644(12) Uani 1 1 d . . . H24A H 0.5475 -0.0152 0.4346 0.050 Uiso 1 1 d R . . H24B H 0.6708 0.0019 0.4597 0.050 Uiso 1 1 d R . . H24C H 0.6136 -0.1002 0.4367 0.050 Uiso 1 1 d R . . C25 C 0.6700(3) -0.0851(2) 0.2980(3) 0.0474(9) Uani 1 1 d . . . H25A H 0.6542 -0.0904 0.2319 0.050 Uiso 1 1 d R . . H25B H 0.6777 -0.1456 0.3142 0.050 Uiso 1 1 d R . . H25C H 0.7349 -0.0435 0.3372 0.050 Uiso 1 1 d R . . C26 C 0.8866(3) 0.3651(2) 0.5310(3) 0.0460(8) Uani 1 1 d . . . H26A H 0.8330 0.4059 0.5118 0.050 Uiso 1 1 d R . . H26B H 0.9253 0.3625 0.4914 0.050 Uiso 1 1 d R . . H26C H 0.9379 0.3884 0.5965 0.050 Uiso 1 1 d R . . C27 C 0.7470(3) 0.2465(2) 0.5997(2) 0.0360(7) Uani 1 1 d . . . C28 C 0.6274(4) 0.2526(5) 0.5435(4) 0.0790(17) Uani 1 1 d . . . H28A H 0.6195 0.3035 0.5106 0.050 Uiso 1 1 d R . . H28B H 0.5947 0.2629 0.5865 0.050 Uiso 1 1 d R . . H28C H 0.5942 0.1952 0.4978 0.050 Uiso 1 1 d R . . C29 C 0.7905(6) 0.3357(3) 0.6763(4) 0.0825(18) Uani 1 1 d . . . H29A H 0.7874 0.3887 0.6468 0.050 Uiso 1 1 d R . . H29B H 0.8653 0.3328 0.7184 0.050 Uiso 1 1 d R . . H29C H 0.7493 0.3419 0.7121 0.050 Uiso 1 1 d R . . C30 C 0.7552(4) 0.1656(3) 0.6498(3) 0.0554(10) Uani 1 1 d . . . H30A H 0.7280 0.1081 0.6031 0.050 Uiso 1 1 d R . . H30B H 0.7136 0.1732 0.6858 0.050 Uiso 1 1 d R . . H30C H 0.8296 0.1641 0.6922 0.050 Uiso 1 1 d R . . C31 C 0.9459(3) 0.1756(3) 0.5597(3) 0.0439(8) Uani 1 1 d . . . C32 C 1.0173(3) 0.2107(3) 0.6678(3) 0.0581(11) Uani 1 1 d . . . H32A H 0.9775 0.1984 0.7029 0.050 Uiso 1 1 d R . . H32B H 1.0388 0.2768 0.6802 0.050 Uiso 1 1 d R . . H32C H 1.0809 0.1791 0.6875 0.050 Uiso 1 1 d R . . C33 C 0.9157(3) 0.0696(3) 0.5399(3) 0.0539(10) Uani 1 1 d . . . H33A H 0.8728 0.0564 0.5725 0.050 Uiso 1 1 d R . . H33B H 0.9797 0.0393 0.5623 0.050 Uiso 1 1 d R . . H33C H 0.8743 0.0468 0.4724 0.050 Uiso 1 1 d R . . C34 C 1.0151(3) 0.1973(3) 0.5076(3) 0.0453(8) Uani 1 1 d . . . H34A H 1.0352 0.2636 0.5202 0.050 Uiso 1 1 d R . . H34B H 0.9743 0.1746 0.4401 0.050 Uiso 1 1 d R . . H34C H 1.0797 0.1671 0.5300 0.050 Uiso 1 1 d R . . C35 C 0.8117(3) 0.5315(2) 0.3780(2) 0.0394(7) Uani 1 1 d . . . H35A H 0.8378 0.5013 0.4317 0.050 Uiso 1 1 d R . . H35B H 0.8229 0.5980 0.4003 0.050 Uiso 1 1 d R . . H35C H 0.8551 0.5167 0.3425 0.050 Uiso 1 1 d R . . C36 C 0.5878(3) 0.5227(3) 0.3750(2) 0.0419(8) Uani 1 1 d . . . C37 C 0.6370(4) 0.4788(4) 0.4633(3) 0.0615(12) Uani 1 1 d . . . H37A H 0.6298 0.4120 0.4434 0.050 Uiso 1 1 d R . . H37B H 0.6027 0.4951 0.5035 0.050 Uiso 1 1 d R . . H37C H 0.7142 0.5017 0.4983 0.050 Uiso 1 1 d R . . C38 C 0.4663(3) 0.4881(3) 0.3246(3) 0.0485(9) Uani 1 1 d . . . H38A H 0.4575 0.4217 0.3016 0.050 Uiso 1 1 d R . . H38B H 0.4340 0.5183 0.2717 0.050 Uiso 1 1 d R . . H38C H 0.4367 0.5025 0.3687 0.050 Uiso 1 1 d R . . C39 C 0.6046(4) 0.6296(3) 0.4121(3) 0.0555(10) Uani 1 1 d . . . H39A H 0.6829 0.6515 0.4439 0.050 Uiso 1 1 d R . . H39B H 0.5755 0.6440 0.4561 0.050 Uiso 1 1 d R . . H39C H 0.5728 0.6597 0.3592 0.050 Uiso 1 1 d R . . C40 C 0.6212(3) 0.5537(2) 0.1921(2) 0.0331(6) Uani 1 1 d . . . C41 C 0.5068(3) 0.5830(2) 0.1565(3) 0.0431(8) Uani 1 1 d . . . H41A H 0.5014 0.6211 0.2087 0.050 Uiso 1 1 d R . . H41B H 0.4567 0.5282 0.1311 0.050 Uiso 1 1 d R . . H41C H 0.4979 0.6179 0.1074 0.050 Uiso 1 1 d R . . C42 C 0.7005(4) 0.6441(2) 0.2241(3) 0.0473(9) Uani 1 1 d . . . H42A H 0.7001 0.6830 0.2783 0.050 Uiso 1 1 d R . . H42B H 0.6833 0.6770 0.1726 0.050 Uiso 1 1 d R . . H42C H 0.7751 0.6284 0.2413 0.050 Uiso 1 1 d R . . C43 C 0.6283(3) 0.4932(2) 0.1055(2) 0.0357(7) Uani 1 1 d . . . H43A H 0.5814 0.4365 0.0844 0.050 Uiso 1 1 d R . . H43B H 0.7028 0.4783 0.1234 0.050 Uiso 1 1 d R . . H43C H 0.6109 0.5270 0.0546 0.050 Uiso 1 1 d R . . C44 C 0.9291(3) 0.4792(2) 0.1930(3) 0.0445(8) Uani 1 1 d . . . H44A H 0.8629 0.5008 0.1593 0.050 Uiso 1 1 d R . . H44B H 0.9856 0.5104 0.1813 0.050 Uiso 1 1 d R . . H44C H 0.9502 0.4926 0.2603 0.050 Uiso 1 1 d R . . C45 C 0.8749(3) 0.3290(2) 0.0143(2) 0.0348(6) Uani 1 1 d . . . C46 C 0.7787(4) 0.3843(3) -0.0302(3) 0.0507(9) Uani 1 1 d . . . H46A H 0.8010 0.4493 -0.0003 0.050 Uiso 1 1 d R . . H46B H 0.7202 0.3606 -0.0207 0.050 Uiso 1 1 d R . . H46C H 0.7600 0.3770 -0.0974 0.050 Uiso 1 1 d R . . C47 C 0.9675(4) 0.3649(3) -0.0068(3) 0.0517(9) Uani 1 1 d . . . H47A H 0.9931 0.4294 0.0242 0.050 Uiso 1 1 d R . . H47B H 0.9441 0.3588 -0.0745 0.050 Uiso 1 1 d R . . H47C H 1.0279 0.3288 0.0170 0.050 Uiso 1 1 d R . . C48 C 0.8387(3) 0.2256(2) -0.0358(2) 0.0410(7) Uani 1 1 d . . . H48A H 0.7816 0.2022 -0.0234 0.050 Uiso 1 1 d R . . H48B H 0.8990 0.1900 -0.0119 0.050 Uiso 1 1 d R . . H48C H 0.8152 0.2200 -0.1034 0.050 Uiso 1 1 d R . . C49 C 1.0608(3) 0.3181(2) 0.2245(3) 0.0375(7) Uani 1 1 d . . . C50 C 1.1497(3) 0.3959(3) 0.2411(3) 0.0527(9) Uani 1 1 d . . . H50A H 1.1490 0.4029 0.1808 0.050 Uiso 1 1 d R . . H50B H 1.2204 0.3794 0.2804 0.050 Uiso 1 1 d R . . H50C H 1.1399 0.4537 0.2726 0.050 Uiso 1 1 d R . . C51 C 1.0858(3) 0.2266(2) 0.1783(3) 0.0418(8) Uani 1 1 d . . . H51A H 1.0821 0.2315 0.1168 0.050 Uiso 1 1 d R . . H51B H 1.0352 0.1758 0.1709 0.050 Uiso 1 1 d R . . H51C H 1.1582 0.2152 0.2184 0.050 Uiso 1 1 d R . . C52 C 1.0683(3) 0.3099(3) 0.3232(3) 0.0462(8) Uani 1 1 d . . . H52A H 1.0537 0.3671 0.3521 0.050 Uiso 1 1 d R . . H52B H 1.1409 0.2985 0.3633 0.050 Uiso 1 1 d R . . H52C H 1.0179 0.2591 0.3157 0.050 Uiso 1 1 d 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 0.0305(4) 0.0261(4) 0.0262(4) 0.0105(3) 0.0168(3) 0.0088(3) Si2 0.0267(4) 0.0227(3) 0.0241(3) 0.0074(3) 0.0141(3) 0.0070(3) Si3 0.0259(3) 0.0231(3) 0.0256(3) 0.0082(3) 0.0149(3) 0.0064(3) Si4 0.0377(4) 0.0245(4) 0.0318(4) 0.0090(3) 0.0214(4) 0.0057(3) Si5 0.0365(4) 0.0483(5) 0.0301(4) 0.0135(4) 0.0144(4) 0.0092(4) Si6 0.0376(4) 0.0242(4) 0.0279(4) 0.0076(3) 0.0179(3) 0.0100(3) Si7 0.0315(4) 0.0247(4) 0.0344(4) 0.0080(3) 0.0202(3) 0.0042(3) C1 0.0271(12) 0.0259(12) 0.0268(12) 0.0087(10) 0.0141(11) 0.0083(10) C2 0.0334(14) 0.0274(13) 0.0313(13) 0.0137(11) 0.0165(12) 0.0094(11) C3 0.0269(12) 0.0229(11) 0.0281(12) 0.0085(10) 0.0140(11) 0.0059(10) C4 0.0299(13) 0.0266(12) 0.0261(12) 0.0072(10) 0.0150(11) 0.0064(10) C5 0.0337(14) 0.0253(12) 0.0376(15) 0.0123(11) 0.0242(13) 0.0095(11) C6 0.0374(15) 0.0286(13) 0.0399(16) 0.0061(12) 0.0237(14) 0.0041(12) C7 0.0521(19) 0.0341(16) 0.0503(19) 0.0012(14) 0.0345(18) 0.0057(14) C8 0.062(2) 0.0372(17) 0.069(2) 0.0179(16) 0.049(2) 0.0228(16) C9 0.059(2) 0.052(2) 0.061(2) 0.0332(18) 0.040(2) 0.0345(18) C10 0.0495(18) 0.0450(17) 0.0442(17) 0.0255(14) 0.0303(16) 0.0269(15) C11 0.0279(13) 0.0280(12) 0.0255(12) 0.0098(10) 0.0133(11) 0.0052(10) C12 0.0338(14) 0.0346(14) 0.0339(14) 0.0109(12) 0.0175(13) 0.0094(12) C13 0.0334(15) 0.0469(18) 0.0453(18) 0.0166(14) 0.0212(15) 0.0155(14) C14 0.0267(14) 0.0531(19) 0.0406(17) 0.0170(15) 0.0130(13) 0.0064(14) C15 0.0328(15) 0.0403(16) 0.0336(15) 0.0096(13) 0.0112(13) -0.0014(13) C16 0.0310(14) 0.0324(14) 0.0303(14) 0.0088(11) 0.0157(12) 0.0053(11) C17 0.0424(16) 0.0306(14) 0.0331(14) 0.0074(11) 0.0203(13) 0.0014(12) C18 0.0380(16) 0.0333(15) 0.0471(18) 0.0076(13) 0.0283(15) 0.0030(13) C19 0.0342(15) 0.0360(15) 0.0427(16) 0.0141(13) 0.0213(14) 0.0110(12) C20 0.0390(18) 0.050(2) 0.066(2) -0.0061(18) 0.0247(19) -0.0034(16) C21 0.071(3) 0.0417(18) 0.080(3) 0.0210(18) 0.061(2) 0.0112(18) C22 0.062(2) 0.0293(14) 0.0449(18) 0.0162(13) 0.0324(17) 0.0104(14) C23 0.068(3) 0.0314(16) 0.084(3) 0.0167(18) 0.049(2) 0.0025(17) C24 0.104(4) 0.057(2) 0.055(2) 0.031(2) 0.048(3) 0.029(3) C25 0.063(2) 0.0277(15) 0.058(2) 0.0135(14) 0.0295(19) 0.0135(15) C26 0.053(2) 0.0294(15) 0.0466(19) 0.0099(14) 0.0135(17) -0.0061(14) C27 0.0434(17) 0.0432(17) 0.0277(14) 0.0112(12) 0.0195(13) 0.0101(14) C28 0.063(3) 0.145(5) 0.063(3) 0.053(3) 0.045(3) 0.053(3) C29 0.125(5) 0.057(3) 0.093(4) -0.011(3) 0.086(4) -0.013(3) C30 0.071(3) 0.048(2) 0.077(3) 0.034(2) 0.051(2) 0.0194(19) C31 0.0386(17) 0.0468(19) 0.0450(18) 0.0165(15) 0.0142(15) 0.0046(15) C32 0.0415(19) 0.081(3) 0.043(2) 0.016(2) 0.0097(17) 0.003(2) C33 0.053(2) 0.048(2) 0.059(2) 0.0200(18) 0.0191(19) 0.0117(17) C34 0.0359(16) 0.054(2) 0.0461(19) 0.0074(16) 0.0193(15) -0.0002(15) C35 0.0464(18) 0.0291(14) 0.0390(16) 0.0069(12) 0.0150(15) 0.0048(13) C36 0.053(2) 0.0460(18) 0.0368(16) 0.0118(14) 0.0269(16) 0.0230(16) C37 0.080(3) 0.089(3) 0.045(2) 0.032(2) 0.045(2) 0.046(3) C38 0.057(2) 0.058(2) 0.050(2) 0.0154(17) 0.0386(19) 0.0214(18) C39 0.070(3) 0.053(2) 0.0424(19) -0.0024(16) 0.026(2) 0.028(2) C40 0.0465(17) 0.0252(13) 0.0340(15) 0.0111(11) 0.0210(14) 0.0111(12) C41 0.056(2) 0.0413(17) 0.0391(17) 0.0170(14) 0.0224(16) 0.0248(16) C42 0.070(2) 0.0285(15) 0.0471(19) 0.0136(14) 0.0276(19) 0.0038(16) C43 0.0502(18) 0.0330(15) 0.0337(15) 0.0145(12) 0.0239(14) 0.0138(13) C44 0.0466(19) 0.0306(15) 0.062(2) 0.0063(15) 0.0299(18) 0.0006(14) C45 0.0461(17) 0.0350(15) 0.0391(16) 0.0173(12) 0.0291(15) 0.0148(13) C46 0.067(2) 0.057(2) 0.0443(19) 0.0280(17) 0.0308(19) 0.030(2) C47 0.069(2) 0.049(2) 0.062(2) 0.0255(18) 0.047(2) 0.0104(19) C48 0.0521(19) 0.0435(17) 0.0336(15) 0.0079(13) 0.0242(15) 0.0102(15) C49 0.0298(14) 0.0374(16) 0.0467(18) 0.0094(13) 0.0181(14) 0.0006(12) C50 0.0374(18) 0.048(2) 0.072(3) 0.0072(19) 0.0259(19) -0.0031(16) C51 0.0343(15) 0.0412(17) 0.060(2) 0.0171(15) 0.0269(16) 0.0102(14) C52 0.0354(16) 0.055(2) 0.0394(17) 0.0074(15) 0.0089(15) 0.0022(15) _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 1.893(3) . ? Si1 Si4 2.4525(11) . ? Si1 Si2 2.4767(10) . ? Si1 Si5 2.4819(12) . ? Si2 C3 1.943(3) . ? Si2 Si3 2.3877(10) . ? Si2 Si6 2.4454(10) . ? Si3 C4 1.892(3) . ? Si3 C1 1.909(3) . ? Si3 Si7 2.4257(10) . ? Si4 C17 1.887(3) . ? Si4 C18 1.940(3) . ? Si4 C22 1.947(3) . ? Si5 C26 1.911(3) . ? Si5 C31 1.931(4) . ? Si5 C27 1.951(3) . ? Si6 C35 1.884(4) . ? Si6 C36 1.921(4) . ? Si6 C40 1.951(3) . ? Si7 C44 1.883(3) . ? Si7 C45 1.928(3) . ? Si7 C49 1.932(3) . ? C1 C2 1.351(4) . ? C1 C5 1.493(4) . ? C2 H2 0.9598 . ? C3 C4 1.356(4) . ? C3 C11 1.488(4) . ? C4 H4 0.9600 . ? C5 C6 1.396(4) . ? C5 C10 1.403(4) . ? C6 C7 1.396(5) . ? C6 H6 0.9584 . ? C7 C8 1.387(6) . ? C7 H7 0.9592 . ? C8 C9 1.385(6) . ? C8 H8 0.9560 . ? C9 C10 1.385(5) . ? C9 H9 0.9577 . ? C10 H10 0.9601 . ? C11 C12 1.393(4) . ? C11 C16 1.412(4) . ? C12 C13 1.396(4) . ? C12 H12 0.9629 . ? C13 C14 1.385(5) . ? C13 H13 0.9461 . ? C14 C15 1.384(5) . ? C14 H14 0.9473 . ? C15 C16 1.389(4) . ? C15 H15 0.9590 . ? C16 H16 0.9659 . ? C17 H17A 0.9592 . ? C17 H17B 0.9613 . ? C17 H17C 0.9588 . ? C18 C19 1.534(4) . ? C18 C20 1.546(5) . ? C18 C21 1.540(5) . ? C19 H19A 0.9655 . ? C19 H19B 0.9638 . ? C19 H19C 0.9498 . ? C20 H20A 0.9621 . ? C20 H20B 0.9571 . ? C20 H20C 0.9599 . ? C21 H21A 0.9608 . ? C21 H21B 0.9606 . ? C21 H21C 0.9578 . ? C22 C23 1.535(5) . ? C22 C24 1.537(5) . ? C22 C25 1.528(5) . ? C23 H23A 0.9683 . ? C23 H23B 0.9588 . ? C23 H23C 0.9571 . ? C24 H24A 0.9655 . ? C24 H24B 0.9562 . ? C24 H24C 0.9597 . ? C25 H25A 0.9584 . ? C25 H25B 0.9594 . ? C25 H25C 0.9559 . ? C26 H26A 0.9477 . ? C26 H26B 0.9723 . ? C26 H26C 0.9634 . ? C27 C30 1.513(5) . ? C27 C28 1.519(6) . ? C27 C29 1.522(6) . ? C28 H28A 0.9614 . ? C28 H28B 0.9537 . ? C28 H28C 0.9592 . ? C29 H29A 0.9626 . ? C29 H29B 0.9684 . ? C29 H29C 0.9494 . ? C30 H30A 0.9605 . ? C30 H30B 0.9573 . ? C30 H30C 0.9614 . ? C31 C33 1.533(5) . ? C31 C32 1.545(5) . ? C31 C34 1.547(5) . ? C32 H32A 0.9576 . ? C32 H32B 0.9618 . ? C32 H32C 0.9621 . ? C33 H33A 0.9630 . ? C33 H33B 0.9574 . ? C33 H33C 0.9601 . ? C34 H34A 0.9610 . ? C34 H34B 0.9590 . ? C34 H34C 0.9631 . ? C35 H35A 0.9609 . ? C35 H35B 0.9591 . ? C35 H35C 0.9819 . ? C36 C38 1.536(6) . ? C36 C37 1.533(5) . ? C36 C39 1.545(5) . ? C37 H37A 0.9618 . ? C37 H37B 0.9424 . ? C37 H37C 0.9794 . ? C38 H38A 0.9610 . ? C38 H38B 0.9569 . ? C38 H38C 0.9416 . ? C39 H39A 0.9881 . ? C39 H39B 0.9351 . ? C39 H39C 0.9552 . ? C40 C41 1.537(5) . ? C40 C43 1.536(4) . ? C40 C42 1.545(5) . ? C41 H41A 0.9440 . ? C41 H41B 0.9449 . ? C41 H41C 0.9659 . ? C42 H42A 0.9444 . ? C42 H42B 0.9621 . ? C42 H42C 0.9913 . ? C43 H43A 0.9476 . ? C43 H43B 0.9850 . ? C43 H43C 0.9627 . ? C44 H44A 0.9393 . ? C44 H44B 0.9827 . ? C44 H44C 0.9555 . ? C45 C47 1.538(5) . ? C45 C48 1.539(5) . ? C45 C46 1.545(5) . ? C46 H46A 0.9610 . ? C46 H46B 0.9409 . ? C46 H46C 0.9637 . ? C47 H47A 0.9620 . ? C47 H47B 0.9622 . ? C47 H47C 0.9735 . ? C48 H48A 0.9492 . ? C48 H48B 0.9681 . ? C48 H48C 0.9613 . ? C49 C51 1.535(5) . ? C49 C52 1.541(5) . ? C49 C50 1.541(5) . ? C50 H50A 0.9685 . ? C50 H50B 0.9739 . ? C50 H50C 0.9495 . ? C51 H51A 0.9636 . ? C51 H51B 0.9544 . ? C51 H51C 0.9679 . ? C52 H52A 0.9529 . ? C52 H52B 0.9700 . ? C52 H52C 0.9522 . ? 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 Si4 96.85(9) . . ? C2 Si1 Si2 95.83(9) . . ? Si4 Si1 Si2 111.83(4) . . ? C2 Si1 Si5 103.31(10) . . ? Si4 Si1 Si5 124.71(4) . . ? Si2 Si1 Si5 116.46(4) . . ? C3 Si2 Si3 73.72(9) . . ? C3 Si2 Si6 113.75(8) . . ? Si3 Si2 Si6 120.08(4) . . ? C3 Si2 Si1 109.77(8) . . ? Si3 Si2 Si1 92.57(3) . . ? Si6 Si2 Si1 131.02(4) . . ? C4 Si3 C1 107.81(12) . . ? C4 Si3 Si2 75.04(9) . . ? C1 Si3 Si2 101.67(9) . . ? C4 Si3 Si7 116.33(9) . . ? C1 Si3 Si7 115.92(9) . . ? Si2 Si3 Si7 132.27(4) . . ? C17 Si4 C18 107.02(15) . . ? C17 Si4 C22 104.05(14) . . ? C18 Si4 C22 112.75(15) . . ? C17 Si4 Si1 101.56(10) . . ? C18 Si4 Si1 113.51(10) . . ? C22 Si4 Si1 116.33(12) . . ? C26 Si5 C31 101.45(17) . . ? C26 Si5 C27 109.80(17) . . ? C31 Si5 C27 112.28(15) . . ? C26 Si5 Si1 103.67(12) . . ? C31 Si5 Si1 114.23(13) . . ? C27 Si5 Si1 114.16(11) . . ? C35 Si6 C36 106.70(16) . . ? C35 Si6 C40 106.79(15) . . ? C36 Si6 C40 111.60(14) . . ? C35 Si6 Si2 102.11(11) . . ? C36 Si6 Si2 115.41(12) . . ? C40 Si6 Si2 113.18(9) . . ? C44 Si7 C45 106.38(16) . . ? C44 Si7 C49 103.99(16) . . ? C45 Si7 C49 115.09(15) . . ? C44 Si7 Si3 110.42(12) . . ? C45 Si7 Si3 109.46(11) . . ? C49 Si7 Si3 111.22(10) . . ? C2 C1 C5 118.6(2) . . ? C2 C1 Si3 119.0(2) . . ? C5 C1 Si3 122.45(19) . . ? C1 C2 Si1 130.5(2) . . ? C1 C2 H2 119.9 . . ? Si1 C2 H2 109.6 . . ? C4 C3 C11 124.3(3) . . ? C4 C3 Si2 104.7(2) . . ? C11 C3 Si2 130.9(2) . . ? C3 C4 Si3 106.5(2) . . ? C3 C4 H4 126.8 . . ? Si3 C4 H4 126.6 . . ? C6 C5 C10 117.9(3) . . ? C6 C5 C1 121.1(3) . . ? C10 C5 C1 121.0(3) . . ? C7 C6 C5 120.9(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 119.8(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.1(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 119.8 . . ? C9 C10 C5 121.2(3) . . ? C9 C10 H10 120.1 . . ? C5 C10 H10 118.7 . . ? C12 C11 C16 117.7(3) . . ? C12 C11 C3 120.6(3) . . ? C16 C11 C3 121.7(3) . . ? C11 C12 C13 121.7(3) . . ? C11 C12 H12 117.3 . . ? C13 C12 H12 121.1 . . ? C14 C13 C12 119.5(3) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 120.6(3) . . ? C15 C16 H16 120.2 . . ? C11 C16 H16 119.2 . . ? Si4 C17 H17A 109.5 . . ? Si4 C17 H17B 109.5 . . ? H17A C17 H17B 109.6 . . ? Si4 C17 H17C 109.5 . . ? H17A C17 H17C 109.2 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 107.2(3) . . ? C19 C18 C21 107.3(3) . . ? C20 C18 C21 107.4(3) . . ? C19 C18 Si4 109.2(2) . . ? C20 C18 Si4 109.5(2) . . ? C21 C18 Si4 116.0(3) . . ? C18 C19 H19A 109.1 . . ? C18 C19 H19B 109.6 . . ? H19A C19 H19B 108.7 . . ? C18 C19 H19C 109.7 . . ? H19A C19 H19C 109.8 . . ? H19B C19 H19C 110.0 . . ? C18 C20 H20A 109.4 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.6 . . ? C18 C20 H20C 109.4 . . ? H20A C20 H20C 109.6 . . ? H20B C20 H20C 109.4 . . ? C18 C21 H21A 109.2 . . ? C18 C21 H21B 109.8 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.3 . . ? H21A C21 H21C 109.6 . . ? H21B C21 H21C 109.3 . . ? C23 C22 C24 109.5(3) . . ? C23 C22 C25 106.7(3) . . ? C24 C22 C25 107.2(3) . . ? C23 C22 Si4 109.0(3) . . ? C24 C22 Si4 113.4(3) . . ? C25 C22 Si4 110.8(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 110.2 . . ? H23A C23 H23B 108.5 . . ? C22 C23 H23C 109.8 . . ? H23A C23 H23C 108.9 . . ? H23B C23 H23C 109.9 . . ? C22 C24 H24A 109.2 . . ? C22 C24 H24B 110.1 . . ? H24A C24 H24B 109.4 . . ? C22 C24 H24C 109.3 . . ? H24A C24 H24C 108.7 . . ? H24B C24 H24C 110.0 . . ? C22 C25 H25A 109.0 . . ? C22 C25 H25B 108.5 . . ? H25A C25 H25B 109.7 . . ? C22 C25 H25C 109.4 . . ? H25A C25 H25C 110.0 . . ? H25B C25 H25C 110.1 . . ? Si5 C26 H26A 110.2 . . ? Si5 C26 H26B 109.5 . . ? H26A C26 H26B 109.2 . . ? Si5 C26 H26C 109.8 . . ? H26A C26 H26C 110.0 . . ? H26B C26 H26C 108.1 . . ? C30 C27 C28 107.0(4) . . ? C30 C27 C29 107.4(3) . . ? C28 C27 C29 105.5(4) . . ? C30 C27 Si5 116.5(3) . . ? C28 C27 Si5 110.7(2) . . ? C29 C27 Si5 109.1(3) . . ? C27 C28 H28A 108.9 . . ? C27 C28 H28B 109.2 . . ? H28A C28 H28B 110.1 . . ? C27 C28 H28C 109.1 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 110.0 . . ? C27 C29 H29A 109.6 . . ? C27 C29 H29B 109.1 . . ? H29A C29 H29B 108.4 . . ? C27 C29 H29C 109.8 . . ? H29A C29 H29C 110.3 . . ? H29B C29 H29C 109.6 . . ? C27 C30 H30A 109.4 . . ? C27 C30 H30B 109.6 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.4 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.4 . . ? C33 C31 C32 108.8(3) . . ? C33 C31 C34 109.4(3) . . ? C32 C31 C34 106.9(3) . . ? C33 C31 Si5 112.9(3) . . ? C32 C31 Si5 110.3(3) . . ? C34 C31 Si5 108.4(2) . . ? C31 C32 H32A 109.7 . . ? C31 C32 H32B 109.1 . . ? H32A C32 H32B 109.9 . . ? C31 C32 H32C 109.7 . . ? H32A C32 H32C 109.4 . . ? H32B C32 H32C 109.0 . . ? C31 C33 H33A 109.1 . . ? C31 C33 H33B 110.1 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.3 . . ? H33A C33 H33C 109.2 . . ? H33B C33 H33C 109.6 . . ? C31 C34 H34A 110.0 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.4 . . ? C31 C34 H34C 109.7 . . ? H34A C34 H34C 108.9 . . ? H34B C34 H34C 109.2 . . ? Si6 C35 H35A 110.5 . . ? Si6 C35 H35B 111.0 . . ? H35A C35 H35B 109.6 . . ? Si6 C35 H35C 110.4 . . ? H35A C35 H35C 107.8 . . ? H35B C35 H35C 107.5 . . ? C38 C36 C37 107.3(3) . . ? C38 C36 C39 109.3(3) . . ? C37 C36 C39 106.6(3) . . ? C38 C36 Si6 114.6(2) . . ? C37 C36 Si6 107.7(2) . . ? C39 C36 Si6 110.8(3) . . ? C36 C37 H37A 109.4 . . ? C36 C37 H37B 110.2 . . ? H37A C37 H37B 110.7 . . ? C36 C37 H37C 109.1 . . ? H37A C37 H37C 108.0 . . ? H37B C37 H37C 109.4 . . ? C36 C38 H38A 108.1 . . ? C36 C38 H38B 108.0 . . ? H38A C38 H38B 109.6 . . ? C36 C38 H38C 108.8 . . ? H38A C38 H38C 110.8 . . ? H38B C38 H38C 111.5 . . ? C36 C39 H39A 109.0 . . ? C36 C39 H39B 109.8 . . ? H39A C39 H39B 109.2 . . ? C36 C39 H39C 109.4 . . ? H39A C39 H39C 107.4 . . ? H39B C39 H39C 112.0 . . ? C41 C40 C43 106.9(3) . . ? C41 C40 C42 106.8(3) . . ? C43 C40 C42 108.0(3) . . ? C41 C40 Si6 115.8(2) . . ? C43 C40 Si6 110.93(19) . . ? C42 C40 Si6 108.0(2) . . ? C40 C41 H41A 108.0 . . ? C40 C41 H41B 108.1 . . ? H41A C41 H41B 112.2 . . ? C40 C41 H41C 107.3 . . ? H41A C41 H41C 110.4 . . ? H41B C41 H41C 110.5 . . ? C40 C42 H42A 111.0 . . ? C40 C42 H42B 110.6 . . ? H42A C42 H42B 110.7 . . ? C40 C42 H42C 110.0 . . ? H42A C42 H42C 107.9 . . ? H42B C42 H42C 106.5 . . ? C40 C43 H43A 110.4 . . ? C40 C43 H43B 109.7 . . ? H43A C43 H43B 108.6 . . ? C40 C43 H43C 110.3 . . ? H43A C43 H43C 110.5 . . ? H43B C43 H43C 107.2 . . ? Si7 C44 H44A 109.8 . . ? Si7 C44 H44B 108.8 . . ? H44A C44 H44B 109.2 . . ? Si7 C44 H44C 109.4 . . ? H44A C44 H44C 111.6 . . ? H44B C44 H44C 108.1 . . ? C47 C45 C48 108.2(3) . . ? C47 C45 C46 108.1(3) . . ? C48 C45 C46 107.9(3) . . ? C47 C45 Si7 110.9(3) . . ? C48 C45 Si7 113.0(2) . . ? C46 C45 Si7 108.6(2) . . ? C45 C46 H46A 108.6 . . ? C45 C46 H46B 108.8 . . ? H46A C46 H46B 111.3 . . ? C45 C46 H46C 108.3 . . ? H46A C46 H46C 109.0 . . ? H46B C46 H46C 110.8 . . ? C45 C47 H47A 110.7 . . ? C45 C47 H47B 110.8 . . ? H47A C47 H47B 109.1 . . ? C45 C47 H47C 110.2 . . ? H47A C47 H47C 107.9 . . ? H47B C47 H47C 108.1 . . ? C45 C48 H48A 109.4 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.6 . . ? C45 C48 H48C 109.4 . . ? H48A C48 H48C 110.3 . . ? H48B C48 H48C 108.6 . . ? C51 C49 C52 109.3(3) . . ? C51 C49 C50 107.5(3) . . ? C52 C49 C50 107.3(3) . . ? C51 C49 Si7 113.4(2) . . ? C52 C49 Si7 107.7(2) . . ? C50 C49 Si7 111.5(2) . . ? C49 C50 H50A 110.3 . . ? C49 C50 H50B 109.8 . . ? H50A C50 H50B 107.6 . . ? C49 C50 H50C 110.8 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 108.7 . . ? C49 C51 H51A 109.8 . . ? C49 C51 H51B 110.0 . . ? H51A C51 H51B 109.7 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 108.4 . . ? H51B C51 H51C 109.4 . . ? C49 C52 H52A 109.2 . . ? C49 C52 H52B 109.1 . . ? H52A C52 H52B 109.0 . . ? C49 C52 H52C 109.3 . . ? H52A C52 H52C 110.9 . . ? H52B C52 H52C 109.4 . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 3.578 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.084