data_hsisi #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Norihiro Tokitoh' _publ_contact_author_email 'tokitoh@boc.kuicr.kyoto-u.ac.jp' _publ_contact_author_fax '+81-774-38-3209' _publ_contact_author_phone '+81-774-38-3200' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Organometallics' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Borylsilyl Anions Utilizing Overcrowded Silylboranes and Their Properties ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Takashi Kajiwara' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Nobuhiro Takeda' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Takahiro Sasamori' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Norihiro Tokitoh' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; _publ_section_synopsis ; ; #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HSiSi _chemical_melting_point ? _chemical_formula_moiety 'C39 H80 Si8' _chemical_formula_sum 'C39 H80 Si8' _chemical_formula_weight 773.75 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 9.708(3) _cell_length_b 14.996(4) _cell_length_c 17.847(5) _cell_angle_alpha 79.350(7) _cell_angle_beta 87.704(10) _cell_angle_gamma 81.536(7) _cell_volume 2525.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9434 _exptl_absorpt_correction_T_max 0.9434 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16569 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8683 _reflns_number_gt 6970 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalClear' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1666P)^2^+5.5970P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8683 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.2775 _refine_ls_wR_factor_gt 0.2593 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Si1 Si 0.26310(14) 0.12867(8) 0.25797(7) 0.0277(3) Uani 1 1 d . . . H1 H 0.1721 0.1301 0.1931 0.033 Uiso 1 1 calc R . . Si2 Si 0.18552(18) 0.01572(10) 0.35736(9) 0.0433(4) Uani 1 1 d . . . C1 C 0.2915(10) -0.0155(5) 0.4451(4) 0.076(2) Uani 1 1 d . . . H1 H 0.2780 0.0355 0.4732 0.115 Uiso 1 1 calc R . . H2 H 0.3901 -0.0285 0.4312 0.115 Uiso 1 1 calc R . . H3 H 0.2623 -0.0700 0.4773 0.115 Uiso 1 1 calc R . . C2 C -0.0014(8) 0.0365(5) 0.3842(5) 0.073(2) Uani 1 1 d . . . H4 H -0.0343 -0.0222 0.4040 0.110 Uiso 1 1 calc R . . H5 H -0.0552 0.0678 0.3392 0.110 Uiso 1 1 calc R . . H6 H -0.0134 0.0749 0.4235 0.110 Uiso 1 1 calc R . . C3 C 0.2046(10) -0.0892(4) 0.3132(4) 0.078(3) Uani 1 1 d . . . H7 H 0.3037 -0.1127 0.3085 0.118 Uiso 1 1 calc R . . H8 H 0.1629 -0.0739 0.2625 0.118 Uiso 1 1 calc R . . H9 H 0.1573 -0.1362 0.3454 0.118 Uiso 1 1 calc R . . C4 C 0.4311(5) 0.0590(3) 0.2347(3) 0.0273(10) Uani 1 1 d . . . C5 C 0.4425(5) 0.0017(3) 0.1789(3) 0.0320(11) Uani 1 1 d . . . C6 C 0.5657(6) -0.0582(3) 0.1737(3) 0.0364(12) Uani 1 1 d . . . H10 H 0.5728 -0.0961 0.1362 0.044 Uiso 1 1 calc R . . C7 C 0.6764(6) -0.0647(4) 0.2202(3) 0.0392(12) Uani 1 1 d . . . C8 C 0.6656(6) -0.0077(3) 0.2741(3) 0.0380(12) Uani 1 1 d . . . H11 H 0.7421 -0.0105 0.3064 0.046 Uiso 1 1 calc R . . C9 C 0.5452(5) 0.0534(3) 0.2817(3) 0.0317(11) Uani 1 1 d . . . C10 C 0.3289(7) 0.0031(4) 0.1246(3) 0.0454(14) Uani 1 1 d . . . H12 H 0.3086 0.0645 0.0936 0.068 Uiso 1 1 calc R . . H13 H 0.2451 -0.0128 0.1533 0.068 Uiso 1 1 calc R . . H14 H 0.3585 -0.0415 0.0913 0.068 Uiso 1 1 calc R . . C11 C 0.8075(7) -0.1314(5) 0.2148(4) 0.0562(16) Uani 1 1 d . . . H15 H 0.7930 -0.1926 0.2417 0.084 Uiso 1 1 calc R . . H16 H 0.8846 -0.1114 0.2381 0.084 Uiso 1 1 calc R . . H17 H 0.8300 -0.1336 0.1611 0.084 Uiso 1 1 calc R . . C12 C 0.5425(6) 0.1127(4) 0.3420(3) 0.0383(12) Uani 1 1 d . . . H18 H 0.5613 0.1741 0.3180 0.057 Uiso 1 1 calc R . . H19 H 0.6137 0.0852 0.3800 0.057 Uiso 1 1 calc R . . H20 H 0.4505 0.1174 0.3669 0.057 Uiso 1 1 calc R . . C13 C 0.2803(4) 0.2547(3) 0.2544(2) 0.0194(8) Uani 1 1 d . . . C14 C 0.3250(4) 0.3032(3) 0.1836(2) 0.0171(8) Uani 1 1 d . . . C15 C 0.3397(4) 0.3959(3) 0.1768(2) 0.0182(8) Uani 1 1 d . . . H21 H 0.3718 0.4267 0.1294 0.022 Uiso 1 1 calc R . . C16 C 0.3098(4) 0.4450(3) 0.2354(2) 0.0176(8) Uani 1 1 d . . . C17 C 0.2658(4) 0.3970(3) 0.3046(2) 0.0185(8) Uani 1 1 d . . . H22 H 0.2461 0.4287 0.3461 0.022 Uiso 1 1 calc R . . C18 C 0.2493(4) 0.3043(3) 0.3156(2) 0.0197(8) Uani 1 1 d . . . C19 C 0.3546(4) 0.2620(3) 0.1120(2) 0.0212(9) Uani 1 1 d . . . H23 H 0.3436 0.1959 0.1281 0.025 Uiso 1 1 calc R . . Si3 Si 0.21188(15) 0.31047(9) 0.03864(7) 0.0314(3) Uani 1 1 d . . . Si4 Si 0.54153(13) 0.26111(9) 0.07677(7) 0.0268(3) Uani 1 1 d . . . C20 C 0.0382(6) 0.2937(5) 0.0816(4) 0.0626(18) Uani 1 1 d . . . H24 H -0.0335 0.3162 0.0428 0.094 Uiso 1 1 calc R . . H25 H 0.0199 0.3278 0.1236 0.094 Uiso 1 1 calc R . . H26 H 0.0364 0.2284 0.1010 0.094 Uiso 1 1 calc R . . C21 C 0.2379(7) 0.2472(4) -0.0425(3) 0.0519(15) Uani 1 1 d . . . H27 H 0.2548 0.1812 -0.0227 0.078 Uiso 1 1 calc R . . H28 H 0.3183 0.2656 -0.0734 0.078 Uiso 1 1 calc R . . H29 H 0.1545 0.2617 -0.0741 0.078 Uiso 1 1 calc R . . C22 C 0.1997(6) 0.4361(4) 0.0022(3) 0.0478(14) Uani 1 1 d . . . H30 H 0.2894 0.4502 -0.0203 0.072 Uiso 1 1 calc R . . H31 H 0.1757 0.4694 0.0444 0.072 Uiso 1 1 calc R . . H32 H 0.1274 0.4548 -0.0367 0.072 Uiso 1 1 calc R . . C23 C 0.6599(5) 0.2490(5) 0.1574(3) 0.0490(15) Uani 1 1 d . . . H33 H 0.6615 0.1880 0.1889 0.074 Uiso 1 1 calc R . . H34 H 0.6271 0.2958 0.1883 0.074 Uiso 1 1 calc R . . H35 H 0.7540 0.2568 0.1379 0.074 Uiso 1 1 calc R . . C24 C 0.5907(6) 0.1641(4) 0.0248(3) 0.0415(13) Uani 1 1 d . . . H36 H 0.6875 0.1635 0.0067 0.062 Uiso 1 1 calc R . . H37 H 0.5293 0.1715 -0.0188 0.062 Uiso 1 1 calc R . . H38 H 0.5814 0.1062 0.0592 0.062 Uiso 1 1 calc R . . C25 C 0.5694(7) 0.3665(4) 0.0056(4) 0.0504(15) Uani 1 1 d . . . H39 H 0.5368 0.4213 0.0276 0.076 Uiso 1 1 calc R . . H40 H 0.5171 0.3687 -0.0407 0.076 Uiso 1 1 calc R . . H41 H 0.6688 0.3645 -0.0072 0.076 Uiso 1 1 calc R . . C26 C 0.3258(5) 0.5459(3) 0.2231(2) 0.0232(9) Uani 1 1 d . . . H42 H 0.3555 0.5594 0.1684 0.028 Uiso 1 1 calc R . . Si5 Si 0.15491(14) 0.62402(9) 0.22557(7) 0.0307(3) Uani 1 1 d . . . Si6 Si 0.47913(15) 0.56837(10) 0.27542(9) 0.0377(4) Uani 1 1 d . . . C27 C 0.1057(6) 0.6479(4) 0.3236(3) 0.0421(13) Uani 1 1 d . . . H43 H 0.1726 0.6834 0.3398 0.063 Uiso 1 1 calc R . . H44 H 0.1067 0.5899 0.3594 0.063 Uiso 1 1 calc R . . H45 H 0.0121 0.6831 0.3226 0.063 Uiso 1 1 calc R . . C28 C 0.0166(5) 0.5711(4) 0.1865(3) 0.0447(13) Uani 1 1 d . . . H46 H -0.0738 0.6093 0.1898 0.067 Uiso 1 1 calc R . . H47 H 0.0127 0.5097 0.2162 0.067 Uiso 1 1 calc R . . H48 H 0.0385 0.5668 0.1331 0.067 Uiso 1 1 calc R . . C29 C 0.1683(7) 0.7363(4) 0.1623(3) 0.0524(17) Uani 1 1 d . . . H49 H 0.2028 0.7258 0.1119 0.079 Uiso 1 1 calc R . . H50 H 0.2329 0.7684 0.1844 0.079 Uiso 1 1 calc R . . H51 H 0.0762 0.7736 0.1575 0.079 Uiso 1 1 calc R . . C30 C 0.4580(8) 0.5424(6) 0.3824(4) 0.068(2) Uani 1 1 d . . . H52 H 0.4352 0.4800 0.3981 0.102 Uiso 1 1 calc R . . H53 H 0.3827 0.5862 0.3985 0.102 Uiso 1 1 calc R . . H54 H 0.5450 0.5473 0.4063 0.102 Uiso 1 1 calc R . . C31 C 0.6334(6) 0.4934(5) 0.2474(4) 0.0585(17) Uani 1 1 d . . . H55 H 0.6453 0.5061 0.1919 0.088 Uiso 1 1 calc R . . H56 H 0.6205 0.4291 0.2641 0.088 Uiso 1 1 calc R . . H57 H 0.7163 0.5052 0.2714 0.088 Uiso 1 1 calc R . . C32 C 0.5092(8) 0.6906(4) 0.2474(5) 0.068(2) Uani 1 1 d . . . H58 H 0.5961 0.6986 0.2697 0.103 Uiso 1 1 calc R . . H59 H 0.4314 0.7306 0.2660 0.103 Uiso 1 1 calc R . . H60 H 0.5157 0.7066 0.1917 0.103 Uiso 1 1 calc R . . C33 C 0.1904(5) 0.2632(3) 0.3924(2) 0.0280(10) Uani 1 1 d . . . H61 H 0.2021 0.1957 0.3931 0.034 Uiso 1 1 calc R . . Si7 Si 0.28724(16) 0.27679(10) 0.47884(8) 0.0358(4) Uani 1 1 d . . . Si8 Si -0.00778(14) 0.30107(9) 0.39541(8) 0.0301(3) Uani 1 1 d . . . C34 C 0.4702(7) 0.2680(6) 0.4556(3) 0.081(3) Uani 1 1 d . . . H62 H 0.5226 0.2695 0.5010 0.122 Uiso 1 1 calc R . . H63 H 0.4870 0.3194 0.4153 0.122 Uiso 1 1 calc R . . H64 H 0.5008 0.2102 0.4377 0.122 Uiso 1 1 calc R . . C35 C 0.2174(6) 0.3833(4) 0.5181(3) 0.0443(13) Uani 1 1 d . . . H65 H 0.2638 0.3822 0.5661 0.066 Uiso 1 1 calc R . . H66 H 0.1169 0.3855 0.5273 0.066 Uiso 1 1 calc R . . H67 H 0.2353 0.4376 0.4812 0.066 Uiso 1 1 calc R . . C36 C 0.2701(10) 0.1786(5) 0.5586(4) 0.077(2) Uani 1 1 d . . . H68 H 0.3098 0.1210 0.5425 0.115 Uiso 1 1 calc R . . H69 H 0.1714 0.1771 0.5719 0.115 Uiso 1 1 calc R . . H70 H 0.3201 0.1861 0.6031 0.115 Uiso 1 1 calc R . . C37 C -0.0846(7) 0.2411(5) 0.4861(3) 0.0556(17) Uani 1 1 d . . . H71 H -0.1865 0.2530 0.4837 0.083 Uiso 1 1 calc R . . H72 H -0.0537 0.2641 0.5296 0.083 Uiso 1 1 calc R . . H73 H -0.0537 0.1750 0.4923 0.083 Uiso 1 1 calc R . . C38 C -0.0868(5) 0.2744(4) 0.3095(3) 0.0384(12) Uani 1 1 d . . . H74 H -0.1862 0.2710 0.3192 0.058 Uiso 1 1 calc R . . H75 H -0.0401 0.2154 0.2989 0.058 Uiso 1 1 calc R . . H76 H -0.0756 0.3227 0.2655 0.058 Uiso 1 1 calc R . . C39 C -0.0602(6) 0.4258(4) 0.3939(4) 0.0441(13) Uani 1 1 d . . . H77 H -0.0350 0.4603 0.3443 0.066 Uiso 1 1 calc R . . H78 H -0.0121 0.4445 0.4344 0.066 Uiso 1 1 calc R . . H79 H -0.1611 0.4382 0.4021 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0418(7) 0.0205(6) 0.0236(7) -0.0096(5) 0.0083(5) -0.0096(5) Si2 0.0650(10) 0.0285(8) 0.0391(9) -0.0120(6) 0.0220(7) -0.0146(7) C1 0.101(6) 0.056(4) 0.060(4) 0.021(3) -0.004(4) -0.012(4) C2 0.072(5) 0.053(4) 0.093(6) -0.007(4) 0.034(4) -0.020(4) C3 0.141(8) 0.033(3) 0.069(5) -0.018(3) 0.049(5) -0.040(4) C4 0.030(2) 0.021(2) 0.029(2) -0.0045(18) 0.0040(19) 0.0018(18) C5 0.039(3) 0.024(2) 0.030(3) -0.0024(19) 0.005(2) 0.0016(19) C6 0.050(3) 0.027(2) 0.032(3) -0.012(2) 0.006(2) 0.004(2) C7 0.043(3) 0.035(3) 0.035(3) -0.004(2) 0.004(2) 0.006(2) C8 0.040(3) 0.035(3) 0.035(3) 0.000(2) -0.006(2) 0.002(2) C9 0.039(3) 0.031(3) 0.022(2) -0.0051(19) 0.002(2) 0.001(2) C10 0.078(4) 0.029(3) 0.035(3) -0.014(2) -0.007(3) -0.015(3) C11 0.047(3) 0.056(4) 0.063(4) -0.020(3) -0.002(3) 0.012(3) C12 0.043(3) 0.042(3) 0.031(3) -0.011(2) -0.004(2) -0.002(2) C13 0.022(2) 0.020(2) 0.018(2) -0.0076(16) 0.0014(16) -0.0049(16) C14 0.0164(19) 0.020(2) 0.016(2) -0.0050(16) -0.0013(15) -0.0027(15) C15 0.0183(19) 0.020(2) 0.016(2) -0.0037(16) 0.0027(15) -0.0020(15) C16 0.0157(19) 0.0166(19) 0.021(2) -0.0047(16) -0.0020(16) -0.0021(15) C17 0.022(2) 0.019(2) 0.016(2) -0.0089(16) -0.0012(16) -0.0042(16) C18 0.023(2) 0.020(2) 0.017(2) -0.0048(16) -0.0003(16) -0.0035(16) C19 0.031(2) 0.019(2) 0.016(2) -0.0069(16) 0.0053(17) -0.0071(17) Si3 0.0414(8) 0.0302(7) 0.0247(7) -0.0063(5) -0.0107(6) -0.0076(6) Si4 0.0313(7) 0.0255(6) 0.0258(7) -0.0114(5) 0.0136(5) -0.0069(5) C20 0.041(3) 0.089(5) 0.054(4) -0.005(4) -0.021(3) -0.003(3) C21 0.072(4) 0.054(4) 0.032(3) -0.016(3) -0.016(3) -0.003(3) C22 0.052(3) 0.040(3) 0.049(3) -0.007(3) -0.016(3) 0.002(3) C23 0.023(2) 0.087(5) 0.041(3) -0.021(3) 0.004(2) -0.009(3) C24 0.050(3) 0.033(3) 0.042(3) -0.019(2) 0.018(3) 0.000(2) C25 0.054(4) 0.038(3) 0.057(4) -0.008(3) 0.026(3) -0.008(3) C26 0.029(2) 0.017(2) 0.023(2) -0.0060(17) 0.0073(18) -0.0014(17) Si5 0.0384(7) 0.0224(6) 0.0252(7) -0.0006(5) 0.0111(5) 0.0078(5) Si6 0.0377(8) 0.0352(8) 0.0483(9) -0.0179(6) 0.0056(6) -0.0200(6) C27 0.055(3) 0.034(3) 0.035(3) -0.009(2) 0.018(2) 0.000(2) C28 0.031(3) 0.053(3) 0.044(3) -0.003(3) -0.008(2) 0.010(2) C29 0.076(4) 0.026(3) 0.043(3) 0.003(2) 0.023(3) 0.014(3) C30 0.074(5) 0.095(5) 0.051(4) -0.023(4) -0.017(3) -0.049(4) C31 0.033(3) 0.056(4) 0.092(5) -0.023(4) -0.009(3) -0.009(3) C32 0.070(4) 0.042(4) 0.105(6) -0.026(4) 0.015(4) -0.032(3) C33 0.046(3) 0.023(2) 0.018(2) -0.0101(17) 0.0042(19) -0.0063(19) Si7 0.0491(9) 0.0342(8) 0.0245(7) -0.0087(6) -0.0051(6) -0.0014(6) Si8 0.0322(7) 0.0319(7) 0.0294(7) -0.0114(5) 0.0080(5) -0.0096(5) C34 0.058(4) 0.137(7) 0.016(3) 0.005(3) 0.002(3) 0.069(4) C35 0.053(3) 0.048(3) 0.040(3) -0.027(3) 0.010(3) -0.012(3) C36 0.134(7) 0.057(4) 0.035(3) 0.004(3) -0.023(4) -0.013(4) C37 0.064(4) 0.070(4) 0.042(3) -0.016(3) 0.019(3) -0.036(3) C38 0.035(3) 0.040(3) 0.041(3) -0.012(2) -0.002(2) -0.003(2) C39 0.036(3) 0.038(3) 0.062(4) -0.024(3) 0.008(3) 0.002(2) _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 C4 1.878(5) . ? Si1 C13 1.911(4) . ? Si1 Si2 2.3959(19) . ? Si2 C2 1.854(7) . ? Si2 C1 1.857(8) . ? Si2 C3 1.869(6) . ? C4 C9 1.400(7) . ? C4 C5 1.422(7) . ? C5 C6 1.396(7) . ? C5 C10 1.492(7) . ? C6 C7 1.365(8) . ? C7 C8 1.390(8) . ? C7 C11 1.511(7) . ? C8 C9 1.394(7) . ? C9 C12 1.515(7) . ? C13 C14 1.422(6) . ? C13 C18 1.431(6) . ? C14 C15 1.401(6) . ? C14 C19 1.519(6) . ? C15 C16 1.386(6) . ? C16 C17 1.394(6) . ? C16 C26 1.519(6) . ? C17 C18 1.399(6) . ? C18 C33 1.521(6) . ? C19 Si4 1.896(4) . ? C19 Si3 1.913(4) . ? Si3 C20 1.856(7) . ? Si3 C21 1.862(6) . ? Si3 C22 1.864(6) . ? Si4 C23 1.843(5) . ? Si4 C24 1.860(5) . ? Si4 C25 1.882(6) . ? C26 Si5 1.889(4) . ? C26 Si6 1.891(5) . ? Si5 C29 1.864(5) . ? Si5 C28 1.874(6) . ? Si5 C27 1.879(5) . ? Si6 C31 1.846(6) . ? Si6 C32 1.872(6) . ? Si6 C30 1.886(7) . ? C33 Si7 1.896(5) . ? C33 Si8 1.925(5) . ? Si7 C34 1.799(7) . ? Si7 C36 1.871(7) . ? Si7 C35 1.887(5) . ? Si8 C39 1.860(5) . ? Si8 C38 1.874(5) . ? Si8 C37 1.884(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Si1 C13 112.7(2) . . ? C4 Si1 Si2 97.27(15) . . ? C13 Si1 Si2 131.57(14) . . ? C2 Si2 C1 109.3(4) . . ? C2 Si2 C3 105.0(4) . . ? C1 Si2 C3 106.2(4) . . ? C2 Si2 Si1 115.5(3) . . ? C1 Si2 Si1 116.3(3) . . ? C3 Si2 Si1 103.2(2) . . ? C9 C4 C5 118.2(4) . . ? C9 C4 Si1 118.1(3) . . ? C5 C4 Si1 123.2(4) . . ? C6 C5 C4 119.0(5) . . ? C6 C5 C10 118.1(5) . . ? C4 C5 C10 122.9(4) . . ? C7 C6 C5 123.0(5) . . ? C6 C7 C8 117.9(5) . . ? C6 C7 C11 122.1(5) . . ? C8 C7 C11 120.0(5) . . ? C7 C8 C9 121.6(5) . . ? C8 C9 C4 120.4(4) . . ? C8 C9 C12 118.0(5) . . ? C4 C9 C12 121.6(4) . . ? C14 C13 C18 117.7(4) . . ? C14 C13 Si1 116.3(3) . . ? C18 C13 Si1 125.9(3) . . ? C15 C14 C13 119.5(4) . . ? C15 C14 C19 116.2(3) . . ? C13 C14 C19 124.3(3) . . ? C16 C15 C14 123.4(4) . . ? C15 C16 C17 116.7(4) . . ? C15 C16 C26 120.3(4) . . ? C17 C16 C26 123.0(4) . . ? C16 C17 C18 123.0(4) . . ? C17 C18 C13 119.6(4) . . ? C17 C18 C33 116.9(4) . . ? C13 C18 C33 123.4(4) . . ? C14 C19 Si4 113.4(3) . . ? C14 C19 Si3 110.5(3) . . ? Si4 C19 Si3 117.0(2) . . ? C20 Si3 C21 107.4(3) . . ? C20 Si3 C22 105.0(3) . . ? C21 Si3 C22 109.8(3) . . ? C20 Si3 C19 110.3(2) . . ? C21 Si3 C19 109.3(2) . . ? C22 Si3 C19 114.7(2) . . ? C23 Si4 C24 109.6(3) . . ? C23 Si4 C25 108.9(3) . . ? C24 Si4 C25 105.0(3) . . ? C23 Si4 C19 110.5(2) . . ? C24 Si4 C19 109.4(2) . . ? C25 Si4 C19 113.3(2) . . ? C16 C26 Si5 113.5(3) . . ? C16 C26 Si6 112.9(3) . . ? Si5 C26 Si6 118.6(2) . . ? C29 Si5 C28 107.7(3) . . ? C29 Si5 C27 107.3(3) . . ? C28 Si5 C27 111.0(3) . . ? C29 Si5 C26 109.3(2) . . ? C28 Si5 C26 108.4(2) . . ? C27 Si5 C26 113.0(2) . . ? C31 Si6 C32 108.9(3) . . ? C31 Si6 C30 108.7(4) . . ? C32 Si6 C30 108.0(4) . . ? C31 Si6 C26 106.9(2) . . ? C32 Si6 C26 111.0(3) . . ? C30 Si6 C26 113.2(2) . . ? C18 C33 Si7 115.4(3) . . ? C18 C33 Si8 109.6(3) . . ? Si7 C33 Si8 115.0(2) . . ? C34 Si7 C36 105.4(4) . . ? C34 Si7 C35 113.5(4) . . ? C36 Si7 C35 105.6(3) . . ? C34 Si7 C33 108.4(3) . . ? C36 Si7 C33 109.9(3) . . ? C35 Si7 C33 113.7(2) . . ? C39 Si8 C38 106.6(3) . . ? C39 Si8 C37 105.8(3) . . ? C38 Si8 C37 111.1(3) . . ? C39 Si8 C33 114.5(2) . . ? C38 Si8 C33 108.9(2) . . ? C37 Si8 C33 110.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Si1 Si2 C2 -163.8(3) . . . . ? C13 Si1 Si2 C2 66.8(4) . . . . ? C4 Si1 Si2 C1 66.0(3) . . . . ? C13 Si1 Si2 C1 -63.3(4) . . . . ? C4 Si1 Si2 C3 -49.8(4) . . . . ? C13 Si1 Si2 C3 -179.1(4) . . . . ? C13 Si1 C4 C9 60.8(4) . . . . ? Si2 Si1 C4 C9 -80.3(4) . . . . ? C13 Si1 C4 C5 -128.4(4) . . . . ? Si2 Si1 C4 C5 90.5(4) . . . . ? C9 C4 C5 C6 0.7(7) . . . . ? Si1 C4 C5 C6 -170.1(4) . . . . ? C9 C4 C5 C10 -178.7(5) . . . . ? Si1 C4 C5 C10 10.4(7) . . . . ? C4 C5 C6 C7 0.2(8) . . . . ? C10 C5 C6 C7 179.6(5) . . . . ? C5 C6 C7 C8 -1.0(8) . . . . ? C5 C6 C7 C11 178.6(5) . . . . ? C6 C7 C8 C9 1.0(8) . . . . ? C11 C7 C8 C9 -178.7(5) . . . . ? C7 C8 C9 C4 -0.1(8) . . . . ? C7 C8 C9 C12 179.9(5) . . . . ? C5 C4 C9 C8 -0.7(7) . . . . ? Si1 C4 C9 C8 170.6(4) . . . . ? C5 C4 C9 C12 179.3(5) . . . . ? Si1 C4 C9 C12 -9.4(6) . . . . ? C4 Si1 C13 C14 59.0(4) . . . . ? Si2 Si1 C13 C14 -177.2(2) . . . . ? C4 Si1 C13 C18 -122.6(4) . . . . ? Si2 Si1 C13 C18 1.1(5) . . . . ? C18 C13 C14 C15 1.4(6) . . . . ? Si1 C13 C14 C15 179.9(3) . . . . ? C18 C13 C14 C19 -176.6(4) . . . . ? Si1 C13 C14 C19 1.9(5) . . . . ? C13 C14 C15 C16 -1.6(6) . . . . ? C19 C14 C15 C16 176.6(4) . . . . ? C14 C15 C16 C17 1.4(6) . . . . ? C14 C15 C16 C26 -178.8(4) . . . . ? C15 C16 C17 C18 -1.1(6) . . . . ? C26 C16 C17 C18 179.2(4) . . . . ? C16 C17 C18 C13 1.0(6) . . . . ? C16 C17 C18 C33 -175.6(4) . . . . ? C14 C13 C18 C17 -1.1(6) . . . . ? Si1 C13 C18 C17 -179.4(3) . . . . ? C14 C13 C18 C33 175.3(4) . . . . ? Si1 C13 C18 C33 -3.1(6) . . . . ? C15 C14 C19 Si4 63.4(4) . . . . ? C13 C14 C19 Si4 -118.5(4) . . . . ? C15 C14 C19 Si3 -70.2(4) . . . . ? C13 C14 C19 Si3 107.9(4) . . . . ? C14 C19 Si3 C20 -54.4(4) . . . . ? Si4 C19 Si3 C20 173.9(3) . . . . ? C14 C19 Si3 C21 -172.3(3) . . . . ? Si4 C19 Si3 C21 56.0(3) . . . . ? C14 C19 Si3 C22 63.9(4) . . . . ? Si4 C19 Si3 C22 -67.8(3) . . . . ? C14 C19 Si4 C23 31.1(4) . . . . ? Si3 C19 Si4 C23 161.4(3) . . . . ? C14 C19 Si4 C24 151.8(3) . . . . ? Si3 C19 Si4 C24 -77.8(3) . . . . ? C14 C19 Si4 C25 -91.5(4) . . . . ? Si3 C19 Si4 C25 38.9(3) . . . . ? C15 C16 C26 Si5 112.6(4) . . . . ? C17 C16 C26 Si5 -67.6(5) . . . . ? C15 C16 C26 Si6 -108.8(4) . . . . ? C17 C16 C26 Si6 71.0(4) . . . . ? C16 C26 Si5 C29 -149.8(4) . . . . ? Si6 C26 Si5 C29 74.1(3) . . . . ? C16 C26 Si5 C28 -32.7(4) . . . . ? Si6 C26 Si5 C28 -168.7(3) . . . . ? C16 C26 Si5 C27 90.8(4) . . . . ? Si6 C26 Si5 C27 -45.3(3) . . . . ? C16 C26 Si6 C31 53.3(4) . . . . ? Si5 C26 Si6 C31 -170.4(3) . . . . ? C16 C26 Si6 C32 171.9(4) . . . . ? Si5 C26 Si6 C32 -51.8(4) . . . . ? C16 C26 Si6 C30 -66.4(4) . . . . ? Si5 C26 Si6 C30 70.0(4) . . . . ? C17 C18 C33 Si7 -54.7(5) . . . . ? C13 C18 C33 Si7 128.8(4) . . . . ? C17 C18 C33 Si8 77.0(4) . . . . ? C13 C18 C33 Si8 -99.4(4) . . . . ? C18 C33 Si7 C34 -35.6(5) . . . . ? Si8 C33 Si7 C34 -164.8(3) . . . . ? C18 C33 Si7 C36 -150.3(4) . . . . ? Si8 C33 Si7 C36 80.5(4) . . . . ? C18 C33 Si7 C35 91.6(4) . . . . ? Si8 C33 Si7 C35 -37.6(3) . . . . ? C18 C33 Si8 C39 -66.8(4) . . . . ? Si7 C33 Si8 C39 65.2(3) . . . . ? C18 C33 Si8 C38 52.3(4) . . . . ? Si7 C33 Si8 C38 -175.7(2) . . . . ? C18 C33 Si8 C37 174.3(3) . . . . ? Si7 C33 Si8 C37 -53.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.843 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.120 #===END data_sib2pin2 #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Norihiro Tokitoh' _publ_contact_author_email 'tokitoh@boc.kuicr.kyoto-u.ac.jp' _publ_contact_author_fax '+81-774-38-3209' _publ_contact_author_phone '+81-774-38-3200' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Chemical Communications' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Unprecedented insertion reaction of a silylene into a B-B bond and generation of a novel borylsilyl anion by boron-metal exchange reaction of the resulting diborylsilane ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Takashi Kajiwara' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Nobuhiro Takeda' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Takahiro Sasamori' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Norihiro Tokitoh' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; _publ_section_synopsis ; ; #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common SiB2pin2 _chemical_melting_point ? _chemical_formula_moiety 'C48 H94 B2 O4 Si7 ' _chemical_formula_sum 'C48 H94 B2 O4 Si7' _chemical_formula_weight 953.48 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' 'B' 'B' 0.0013 0.0007 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.189(4) _cell_length_b 13.204(5) _cell_length_c 19.744(7) _cell_angle_alpha 79.858(14) _cell_angle_beta 72.051(13) _cell_angle_gamma 78.938(16) _cell_volume 2943.3(17) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 8644 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.199 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9337 _exptl_absorpt_correction_T_max 0.9708 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19368 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10158 _reflns_number_gt 8057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalClear' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0470P)^2^+1.5773P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10158 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Si1 Si 0.73944(6) 0.26285(5) 0.30307(4) 0.01486(16) Uani 1 1 d . . . B1 B 0.8676(2) 0.1526(2) 0.25525(16) 0.0185(6) Uani 1 1 d . . . O1 O 0.89918(15) 0.12528(13) 0.18804(10) 0.0232(4) Uani 1 1 d . . . C1 C 0.9988(2) 0.0414(2) 0.17946(15) 0.0253(6) Uani 1 1 d . . . C2 C 1.0277(2) 0.0254(2) 0.25348(15) 0.0244(6) Uani 1 1 d . . . O2 O 0.93640(15) 0.09630(14) 0.29615(10) 0.0254(4) Uani 1 1 d . . . C3 C 1.0934(3) 0.0792(3) 0.11513(18) 0.0490(9) Uani 1 1 d . . . H1 H 1.0647 0.0946 0.0726 0.073 Uiso 1 1 calc R . . H2 H 1.1619 0.0252 0.1070 0.073 Uiso 1 1 calc R . . H3 H 1.1149 0.1424 0.1241 0.073 Uiso 1 1 calc R . . C4 C 0.9586(3) -0.0518(2) 0.16379(17) 0.0370(8) Uani 1 1 d . . . H4 H 0.8908 -0.0705 0.2030 0.055 Uiso 1 1 calc R . . H5 H 1.0219 -0.1108 0.1596 0.055 Uiso 1 1 calc R . . H6 H 0.9373 -0.0343 0.1187 0.055 Uiso 1 1 calc R . . C5 C 1.1433(2) 0.0574(2) 0.2504(2) 0.0410(8) Uani 1 1 d . . . H7 H 1.1440 0.1308 0.2305 0.062 Uiso 1 1 calc R . . H8 H 1.2077 0.0145 0.2198 0.062 Uiso 1 1 calc R . . H9 H 1.1521 0.0475 0.2989 0.062 Uiso 1 1 calc R . . C6 C 1.0198(3) -0.0826(2) 0.29499(17) 0.0339(7) Uani 1 1 d . . . H10 H 1.0305 -0.0831 0.3422 0.051 Uiso 1 1 calc R . . H11 H 1.0806 -0.1330 0.2685 0.051 Uiso 1 1 calc R . . H12 H 0.9430 -0.1014 0.3010 0.051 Uiso 1 1 calc R . . B2 B 0.8003(3) 0.2618(2) 0.38934(16) 0.0188(6) Uani 1 1 d . . . O3 O 0.89969(15) 0.29305(14) 0.39251(10) 0.0239(4) Uani 1 1 d . . . C7 C 0.9209(2) 0.2429(2) 0.46110(15) 0.0263(6) Uani 1 1 d . . . C8 C 0.7963(3) 0.2274(2) 0.50809(15) 0.0314(7) Uani 1 1 d . . . O4 O 0.74229(16) 0.21324(15) 0.45426(10) 0.0287(5) Uani 1 1 d . . . C9 C 0.9799(3) 0.3128(2) 0.48772(17) 0.0371(8) Uani 1 1 d . . . H13 H 1.0553 0.3226 0.4528 0.056 Uiso 1 1 calc R . . H14 H 0.9920 0.2805 0.5340 0.056 Uiso 1 1 calc R . . H15 H 0.9304 0.3804 0.4935 0.056 Uiso 1 1 calc R . . C10 C 1.0011(3) 0.1410(2) 0.44581(17) 0.0367(8) Uani 1 1 d . . . H16 H 0.9613 0.0955 0.4302 0.055 Uiso 1 1 calc R . . H17 H 1.0214 0.1068 0.4895 0.055 Uiso 1 1 calc R . . H18 H 1.0723 0.1550 0.4079 0.055 Uiso 1 1 calc R . . C11 C 0.7275(3) 0.3232(3) 0.54137(18) 0.0499(10) Uani 1 1 d . . . H19 H 0.7304 0.3831 0.5040 0.075 Uiso 1 1 calc R . . H20 H 0.7613 0.3363 0.5775 0.075 Uiso 1 1 calc R . . H21 H 0.6463 0.3123 0.5642 0.075 Uiso 1 1 calc R . . C12 C 0.7880(3) 0.1319(3) 0.56364(18) 0.0512(10) Uani 1 1 d . . . H22 H 0.7058 0.1243 0.5865 0.077 Uiso 1 1 calc R . . H23 H 0.8242 0.1394 0.6001 0.077 Uiso 1 1 calc R . . H24 H 0.8285 0.0701 0.5402 0.077 Uiso 1 1 calc R . . C13 C 0.5984(2) 0.20755(19) 0.35411(13) 0.0171(5) Uani 1 1 d . . . C14 C 0.5137(2) 0.2682(2) 0.40365(14) 0.0203(6) Uani 1 1 d . . . C15 C 0.4192(2) 0.2266(2) 0.45194(14) 0.0245(6) Uani 1 1 d . . . H25 H 0.3642 0.2687 0.4851 0.029 Uiso 1 1 calc R . . C16 C 0.4027(2) 0.1248(2) 0.45331(14) 0.0248(6) Uani 1 1 d . . . C17 C 0.4835(2) 0.0657(2) 0.40408(15) 0.0244(6) Uani 1 1 d . . . H26 H 0.4728 -0.0035 0.4036 0.029 Uiso 1 1 calc R . . C18 C 0.5804(2) 0.1045(2) 0.35507(14) 0.0204(6) Uani 1 1 d . . . C19 C 0.5218(2) 0.3808(2) 0.40550(15) 0.0256(6) Uani 1 1 d . . . H27 H 0.4541 0.4100 0.4421 0.038 Uiso 1 1 calc R . . H28 H 0.5230 0.4206 0.3585 0.038 Uiso 1 1 calc R . . H29 H 0.5934 0.3846 0.4171 0.038 Uiso 1 1 calc R . . C20 C 0.2996(2) 0.0811(2) 0.50746(16) 0.0350(7) Uani 1 1 d . . . H30 H 0.2315 0.0998 0.4889 0.052 Uiso 1 1 calc R . . H31 H 0.2824 0.1101 0.5526 0.052 Uiso 1 1 calc R . . H32 H 0.3181 0.0052 0.5159 0.052 Uiso 1 1 calc R . . C21 C 0.6646(2) 0.03067(19) 0.30558(15) 0.0227(6) Uani 1 1 d . . . H33 H 0.7350 0.0072 0.3215 0.034 Uiso 1 1 calc R . . H34 H 0.6857 0.0665 0.2565 0.034 Uiso 1 1 calc R . . H35 H 0.6277 -0.0295 0.3067 0.034 Uiso 1 1 calc R . . C22 C 0.7095(2) 0.38893(18) 0.24192(13) 0.0144(5) Uani 1 1 d . . . C23 C 0.6458(2) 0.38822(18) 0.19233(13) 0.0143(5) Uani 1 1 d . . . C24 C 0.6042(2) 0.48088(19) 0.15654(13) 0.0168(5) Uani 1 1 d . . . H36 H 0.5589 0.4782 0.1256 0.020 Uiso 1 1 calc R . . C25 C 0.6260(2) 0.57745(19) 0.16409(13) 0.0164(5) Uani 1 1 d . . . C26 C 0.6952(2) 0.57757(19) 0.20797(13) 0.0164(5) Uani 1 1 d . . . H37 H 0.7156 0.6419 0.2117 0.020 Uiso 1 1 calc R . . C27 C 0.7368(2) 0.48715(18) 0.24726(13) 0.0147(5) Uani 1 1 d . . . C28 C 0.6269(2) 0.28989(18) 0.16975(14) 0.0174(5) Uani 1 1 d . . . H38 H 0.6589 0.2309 0.2009 0.021 Uiso 1 1 calc R . . C29 C 0.5740(2) 0.67569(19) 0.12535(14) 0.0180(5) Uani 1 1 d . . . H39 H 0.5374 0.6482 0.0948 0.022 Uiso 1 1 calc R . . C30 C 0.8146(2) 0.49986(18) 0.29154(13) 0.0167(5) Uani 1 1 d . . . H40 H 0.8116 0.4364 0.3278 0.020 Uiso 1 1 calc R . . Si2 Si 0.72501(6) 0.27711(6) 0.07429(4) 0.02172(18) Uani 1 1 d . . . C31 C 0.8678(2) 0.3195(2) 0.06297(15) 0.0255(6) Uani 1 1 d . . . H41 H 0.9042 0.2779 0.0987 0.038 Uiso 1 1 calc R . . H42 H 0.8552 0.3932 0.0696 0.038 Uiso 1 1 calc R . . H43 H 0.9191 0.3099 0.0147 0.038 Uiso 1 1 calc R . . C32 C 0.6677(3) 0.3586(2) 0.00102(15) 0.0337(7) Uani 1 1 d . . . H44 H 0.6461 0.4310 0.0110 0.051 Uiso 1 1 calc R . . H45 H 0.5990 0.3325 -0.0012 0.051 Uiso 1 1 calc R . . H46 H 0.7282 0.3548 -0.0450 0.051 Uiso 1 1 calc R . . C33 C 0.7490(3) 0.1386(2) 0.05653(17) 0.0361(7) Uani 1 1 d . . . H47 H 0.8156 0.1279 0.0140 0.054 Uiso 1 1 calc R . . H48 H 0.6791 0.1231 0.0482 0.054 Uiso 1 1 calc R . . H49 H 0.7649 0.0922 0.0981 0.054 Uiso 1 1 calc R . . Si3 Si 0.46718(6) 0.27546(6) 0.18785(4) 0.02208(18) Uani 1 1 d . . . C34 C 0.3732(2) 0.3156(3) 0.27575(16) 0.0355(7) Uani 1 1 d . . . H50 H 0.2910 0.3218 0.2774 0.053 Uiso 1 1 calc R . . H51 H 0.3899 0.3828 0.2814 0.053 Uiso 1 1 calc R . . H52 H 0.3893 0.2632 0.3147 0.053 Uiso 1 1 calc R . . C35 C 0.3947(3) 0.3552(2) 0.12067(17) 0.0353(7) Uani 1 1 d . . . H53 H 0.4398 0.3392 0.0723 0.053 Uiso 1 1 calc R . . H54 H 0.3908 0.4293 0.1233 0.053 Uiso 1 1 calc R . . H55 H 0.3156 0.3386 0.1313 0.053 Uiso 1 1 calc R . . C36 C 0.4590(3) 0.1360(2) 0.18739(18) 0.0368(8) Uani 1 1 d . . . H56 H 0.4909 0.0931 0.2247 0.055 Uiso 1 1 calc R . . H57 H 0.5043 0.1147 0.1404 0.055 Uiso 1 1 calc R . . H58 H 0.3775 0.1269 0.1968 0.055 Uiso 1 1 calc R . . Si4 Si 0.68629(7) 0.75049(6) 0.05707(4) 0.02232(18) Uani 1 1 d . . . C37 C 0.7928(2) 0.6548(2) 0.00156(15) 0.0278(6) Uani 1 1 d . . . H59 H 0.8506 0.6912 -0.0361 0.042 Uiso 1 1 calc R . . H60 H 0.7516 0.6192 -0.0205 0.042 Uiso 1 1 calc R . . H61 H 0.8323 0.6036 0.0320 0.042 Uiso 1 1 calc R . . C38 C 0.6103(3) 0.8508(2) -0.00008(16) 0.0343(7) Uani 1 1 d . . . H62 H 0.5711 0.9101 0.0263 0.051 Uiso 1 1 calc R . . H63 H 0.5526 0.8202 -0.0121 0.051 Uiso 1 1 calc R . . H64 H 0.6677 0.8744 -0.0443 0.051 Uiso 1 1 calc R . . C39 C 0.7668(3) 0.8209(2) 0.09599(16) 0.0305(7) Uani 1 1 d . . . H65 H 0.8124 0.7705 0.1234 0.046 Uiso 1 1 calc R . . H66 H 0.7110 0.8682 0.1278 0.046 Uiso 1 1 calc R . . H67 H 0.8193 0.8609 0.0572 0.046 Uiso 1 1 calc R . . Si5 Si 0.44457(7) 0.74779(6) 0.18849(4) 0.02326(18) Uani 1 1 d . . . C40 C 0.3593(3) 0.6493(2) 0.25195(16) 0.0350(7) Uani 1 1 d . . . H68 H 0.2861 0.6847 0.2809 0.053 Uiso 1 1 calc R . . H69 H 0.4049 0.6095 0.2836 0.053 Uiso 1 1 calc R . . H70 H 0.3421 0.6020 0.2247 0.053 Uiso 1 1 calc R . . C41 C 0.3474(3) 0.8306(3) 0.13636(17) 0.0401(8) Uani 1 1 d . . . H71 H 0.3369 0.7904 0.1021 0.060 Uiso 1 1 calc R . . H72 H 0.3830 0.8920 0.1103 0.060 Uiso 1 1 calc R . . H73 H 0.2714 0.8528 0.1694 0.060 Uiso 1 1 calc R . . C42 C 0.4852(3) 0.8325(2) 0.24056(17) 0.0361(7) Uani 1 1 d . . . H74 H 0.4151 0.8608 0.2761 0.054 Uiso 1 1 calc R . . H75 H 0.5209 0.8898 0.2078 0.054 Uiso 1 1 calc R . . H76 H 0.5409 0.7914 0.2652 0.054 Uiso 1 1 calc R . . Si6 Si 0.97303(6) 0.48921(6) 0.23412(4) 0.02217(18) Uani 1 1 d . . . C43 C 1.0225(2) 0.3541(2) 0.21020(16) 0.0274(6) Uani 1 1 d . . . H77 H 0.9711 0.3373 0.1855 0.041 Uiso 1 1 calc R . . H78 H 1.0199 0.3052 0.2540 0.041 Uiso 1 1 calc R . . H79 H 1.1026 0.3489 0.1786 0.041 Uiso 1 1 calc R . . C44 C 0.9916(3) 0.5805(2) 0.14895(17) 0.0368(8) Uani 1 1 d . . . H80 H 1.0730 0.5694 0.1197 0.055 Uiso 1 1 calc R . . H81 H 0.9708 0.6523 0.1601 0.055 Uiso 1 1 calc R . . H82 H 0.9408 0.5676 0.1224 0.055 Uiso 1 1 calc R . . C45 C 1.0728(2) 0.5152(2) 0.28236(18) 0.0354(7) Uani 1 1 d . . . H83 H 1.0652 0.4675 0.3270 0.053 Uiso 1 1 calc R . . H84 H 1.0520 0.5871 0.2934 0.053 Uiso 1 1 calc R . . H85 H 1.1534 0.5046 0.2519 0.053 Uiso 1 1 calc R . . Si7 Si 0.76347(6) 0.61283(6) 0.34650(4) 0.02178(18) Uani 1 1 d . . . C46 C 0.6018(2) 0.6310(2) 0.38508(15) 0.0278(6) Uani 1 1 d . . . H86 H 0.5763 0.6955 0.4073 0.042 Uiso 1 1 calc R . . H87 H 0.5792 0.5720 0.4214 0.042 Uiso 1 1 calc R . . H88 H 0.5650 0.6351 0.3468 0.042 Uiso 1 1 calc R . . C47 C 0.8061(3) 0.7399(2) 0.29550(17) 0.0315(7) Uani 1 1 d . . . H89 H 0.7853 0.7923 0.3286 0.047 Uiso 1 1 calc R . . H90 H 0.7650 0.7625 0.2587 0.047 Uiso 1 1 calc R . . H91 H 0.8905 0.7312 0.2726 0.047 Uiso 1 1 calc R . . C48 C 0.8290(3) 0.5862(2) 0.42323(17) 0.0361(8) Uani 1 1 d . . . H92 H 0.9111 0.5559 0.4065 0.054 Uiso 1 1 calc R . . H93 H 0.7868 0.5374 0.4612 0.054 Uiso 1 1 calc R . . H94 H 0.8234 0.6514 0.4422 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0143(4) 0.0131(3) 0.0185(4) -0.0015(3) -0.0069(3) -0.0017(3) B1 0.0164(15) 0.0145(14) 0.0249(16) 0.0008(12) -0.0059(13) -0.0063(12) O1 0.0227(10) 0.0193(10) 0.0256(10) -0.0040(8) -0.0072(8) 0.0036(8) C1 0.0231(15) 0.0146(13) 0.0318(16) -0.0026(11) -0.0010(13) 0.0014(11) C2 0.0152(14) 0.0190(14) 0.0377(17) -0.0067(12) -0.0064(12) 0.0016(11) O2 0.0185(10) 0.0254(10) 0.0306(11) -0.0058(8) -0.0084(8) 0.0055(8) C3 0.0328(19) 0.046(2) 0.046(2) 0.0073(17) 0.0069(16) 0.0055(15) C4 0.060(2) 0.0225(16) 0.0326(17) -0.0053(13) -0.0206(16) -0.0027(14) C5 0.0216(16) 0.0357(18) 0.069(2) -0.0243(17) -0.0086(16) -0.0036(13) C6 0.0384(18) 0.0223(15) 0.0447(19) 0.0024(13) -0.0233(15) -0.0007(13) B2 0.0199(16) 0.0155(14) 0.0233(16) -0.0037(12) -0.0099(13) -0.0011(12) O3 0.0234(10) 0.0272(10) 0.0256(10) 0.0016(8) -0.0142(8) -0.0071(8) C7 0.0287(16) 0.0287(15) 0.0269(15) -0.0005(12) -0.0170(13) -0.0050(12) C8 0.0320(17) 0.0446(19) 0.0254(16) -0.0006(13) -0.0189(14) -0.0095(14) O4 0.0267(11) 0.0411(12) 0.0226(10) 0.0032(9) -0.0129(9) -0.0123(9) C9 0.0417(19) 0.0428(19) 0.0385(18) -0.0030(15) -0.0266(16) -0.0109(15) C10 0.0371(18) 0.0372(18) 0.0405(19) -0.0059(14) -0.0232(15) 0.0040(14) C11 0.0355(19) 0.084(3) 0.0353(19) -0.0223(19) -0.0154(16) 0.0014(18) C12 0.053(2) 0.075(3) 0.0344(19) 0.0182(18) -0.0275(17) -0.029(2) C13 0.0155(13) 0.0192(13) 0.0176(13) -0.0019(10) -0.0075(11) -0.0004(10) C14 0.0196(14) 0.0235(14) 0.0208(14) -0.0034(11) -0.0099(12) -0.0034(11) C15 0.0193(14) 0.0317(16) 0.0225(15) -0.0056(12) -0.0051(12) -0.0030(12) C16 0.0219(15) 0.0307(16) 0.0220(14) 0.0052(12) -0.0081(12) -0.0094(12) C17 0.0217(15) 0.0242(15) 0.0291(16) 0.0034(12) -0.0102(12) -0.0087(12) C18 0.0186(14) 0.0216(14) 0.0233(14) 0.0014(11) -0.0108(12) -0.0045(11) C19 0.0207(15) 0.0271(15) 0.0273(15) -0.0098(12) -0.0019(12) -0.0014(12) C20 0.0280(17) 0.0437(19) 0.0303(17) 0.0037(14) -0.0044(14) -0.0125(14) C21 0.0189(14) 0.0144(13) 0.0344(16) -0.0001(11) -0.0065(12) -0.0058(11) C22 0.0125(13) 0.0138(12) 0.0160(13) -0.0032(10) -0.0022(10) -0.0013(10) C23 0.0092(12) 0.0145(12) 0.0180(13) -0.0027(10) -0.0020(10) -0.0016(9) C24 0.0154(13) 0.0189(13) 0.0190(13) -0.0029(10) -0.0080(11) -0.0037(10) C25 0.0141(13) 0.0149(13) 0.0186(13) -0.0010(10) -0.0033(11) -0.0013(10) C26 0.0155(13) 0.0148(12) 0.0185(13) -0.0042(10) -0.0022(11) -0.0039(10) C27 0.0117(12) 0.0154(12) 0.0159(13) -0.0023(10) -0.0016(10) -0.0029(10) C28 0.0208(14) 0.0112(12) 0.0237(14) -0.0004(10) -0.0126(11) -0.0020(10) C29 0.0218(14) 0.0144(13) 0.0215(14) -0.0023(10) -0.0111(11) -0.0034(10) C30 0.0225(14) 0.0116(12) 0.0189(13) -0.0028(10) -0.0098(11) -0.0019(10) Si2 0.0246(4) 0.0196(4) 0.0235(4) -0.0065(3) -0.0096(3) -0.0013(3) C31 0.0266(15) 0.0250(15) 0.0235(15) -0.0003(12) -0.0063(12) -0.0042(12) C32 0.0391(18) 0.0399(18) 0.0225(15) -0.0041(13) -0.0115(14) -0.0018(14) C33 0.0422(19) 0.0302(17) 0.0391(18) -0.0142(14) -0.0114(15) -0.0045(14) Si3 0.0207(4) 0.0212(4) 0.0284(4) -0.0007(3) -0.0125(3) -0.0058(3) C34 0.0212(16) 0.050(2) 0.0363(18) -0.0064(15) -0.0097(14) -0.0032(14) C35 0.0281(17) 0.0434(19) 0.0386(18) 0.0060(15) -0.0197(15) -0.0085(14) C36 0.0357(18) 0.0306(17) 0.052(2) -0.0021(15) -0.0206(16) -0.0136(14) Si4 0.0248(4) 0.0196(4) 0.0233(4) 0.0020(3) -0.0091(3) -0.0055(3) C37 0.0265(16) 0.0305(16) 0.0263(16) -0.0001(12) -0.0090(13) -0.0045(12) C38 0.0327(17) 0.0311(17) 0.0355(18) 0.0094(14) -0.0111(14) -0.0063(13) C39 0.0342(17) 0.0264(16) 0.0334(17) 0.0032(13) -0.0118(14) -0.0129(13) Si5 0.0246(4) 0.0202(4) 0.0245(4) -0.0066(3) -0.0083(3) 0.0037(3) C40 0.0275(17) 0.0380(18) 0.0354(18) -0.0083(14) -0.0010(14) -0.0046(13) C41 0.0365(18) 0.0419(19) 0.0388(19) -0.0136(15) -0.0163(15) 0.0189(15) C42 0.0442(19) 0.0280(16) 0.0365(18) -0.0141(14) -0.0111(15) 0.0021(14) Si6 0.0181(4) 0.0210(4) 0.0290(4) -0.0022(3) -0.0078(3) -0.0059(3) C43 0.0184(14) 0.0285(16) 0.0322(16) -0.0071(12) -0.0016(12) -0.0026(12) C44 0.0236(16) 0.0380(18) 0.0397(19) 0.0091(14) -0.0025(14) -0.0066(13) C45 0.0229(16) 0.0364(18) 0.054(2) -0.0160(15) -0.0162(15) -0.0034(13) Si7 0.0248(4) 0.0180(4) 0.0274(4) -0.0075(3) -0.0129(3) -0.0013(3) C46 0.0299(16) 0.0276(16) 0.0281(16) -0.0120(12) -0.0085(13) -0.0014(12) C47 0.0305(16) 0.0223(15) 0.0464(19) -0.0105(13) -0.0139(14) -0.0043(12) C48 0.0412(19) 0.0370(18) 0.0403(19) -0.0191(15) -0.0250(16) 0.0054(14) _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 C13 1.913(3) . ? Si1 C22 1.922(3) . ? Si1 B1 2.038(3) . ? Si1 B2 2.054(3) . ? B1 O1 1.356(3) . ? B1 O2 1.369(3) . ? O1 C1 1.467(3) . ? C1 C3 1.513(4) . ? C1 C4 1.519(4) . ? C1 C2 1.577(4) . ? C2 O2 1.457(3) . ? C2 C6 1.519(4) . ? C2 C5 1.528(4) . ? B2 O4 1.371(3) . ? B2 O3 1.375(3) . ? O3 C7 1.474(3) . ? C7 C9 1.518(4) . ? C7 C10 1.521(4) . ? C7 C8 1.547(4) . ? C8 O4 1.465(3) . ? C8 C11 1.510(5) . ? C8 C12 1.516(4) . ? C13 C14 1.414(3) . ? C13 C18 1.415(3) . ? C14 C15 1.385(4) . ? C14 C19 1.516(4) . ? C15 C16 1.391(4) . ? C16 C17 1.380(4) . ? C16 C20 1.512(4) . ? C17 C18 1.395(4) . ? C18 C21 1.515(4) . ? C22 C23 1.427(3) . ? C22 C27 1.428(3) . ? C23 C24 1.390(3) . ? C23 C28 1.523(3) . ? C24 C25 1.393(3) . ? C25 C26 1.384(3) . ? C25 C29 1.517(3) . ? C26 C27 1.403(3) . ? C27 C30 1.522(3) . ? C28 Si3 1.908(3) . ? C28 Si2 1.912(3) . ? C29 Si4 1.891(3) . ? C29 Si5 1.892(3) . ? C30 Si7 1.894(3) . ? C30 Si6 1.907(3) . ? Si2 C31 1.867(3) . ? Si2 C33 1.874(3) . ? Si2 C32 1.877(3) . ? Si3 C34 1.863(3) . ? Si3 C36 1.865(3) . ? Si3 C35 1.877(3) . ? Si4 C37 1.861(3) . ? Si4 C39 1.867(3) . ? Si4 C38 1.879(3) . ? Si5 C40 1.866(3) . ? Si5 C42 1.866(3) . ? Si5 C41 1.875(3) . ? Si6 C43 1.864(3) . ? Si6 C44 1.867(3) . ? Si6 C45 1.869(3) . ? Si7 C46 1.865(3) . ? Si7 C48 1.873(3) . ? Si7 C47 1.875(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Si1 C22 111.15(11) . . ? C13 Si1 B1 112.05(11) . . ? C22 Si1 B1 115.65(12) . . ? C13 Si1 B2 97.91(12) . . ? C22 Si1 B2 121.77(11) . . ? B1 Si1 B2 96.46(12) . . ? O1 B1 O2 112.8(2) . . ? O1 B1 Si1 131.0(2) . . ? O2 B1 Si1 116.2(2) . . ? B1 O1 C1 110.0(2) . . ? O1 C1 C3 106.5(2) . . ? O1 C1 C4 106.9(2) . . ? C3 C1 C4 109.8(3) . . ? O1 C1 C2 103.5(2) . . ? C3 C1 C2 115.1(2) . . ? C4 C1 C2 114.4(2) . . ? O2 C2 C6 106.6(2) . . ? O2 C2 C5 106.2(2) . . ? C6 C2 C5 108.8(2) . . ? O2 C2 C1 103.86(19) . . ? C6 C2 C1 115.2(2) . . ? C5 C2 C1 115.3(2) . . ? B1 O2 C2 109.8(2) . . ? O4 B2 O3 111.6(2) . . ? O4 B2 Si1 117.62(19) . . ? O3 B2 Si1 130.4(2) . . ? B2 O3 C7 107.0(2) . . ? O3 C7 C9 109.4(2) . . ? O3 C7 C10 106.7(2) . . ? C9 C7 C10 110.1(2) . . ? O3 C7 C8 101.8(2) . . ? C9 C7 C8 115.2(2) . . ? C10 C7 C8 113.1(2) . . ? O4 C8 C11 106.5(2) . . ? O4 C8 C12 108.1(2) . . ? C11 C8 C12 110.9(3) . . ? O4 C8 C7 101.4(2) . . ? C11 C8 C7 113.3(3) . . ? C12 C8 C7 115.6(3) . . ? B2 O4 C8 108.0(2) . . ? C14 C13 C18 117.1(2) . . ? C14 C13 Si1 117.13(18) . . ? C18 C13 Si1 124.89(19) . . ? C15 C14 C13 120.8(2) . . ? C15 C14 C19 117.6(2) . . ? C13 C14 C19 121.6(2) . . ? C14 C15 C16 121.9(3) . . ? C17 C16 C15 117.8(2) . . ? C17 C16 C20 121.6(3) . . ? C15 C16 C20 120.6(3) . . ? C16 C17 C18 122.0(3) . . ? C17 C18 C13 120.4(2) . . ? C17 C18 C21 116.9(2) . . ? C13 C18 C21 122.7(2) . . ? C23 C22 C27 116.7(2) . . ? C23 C22 Si1 118.69(17) . . ? C27 C22 Si1 124.28(18) . . ? C24 C23 C22 120.5(2) . . ? C24 C23 C28 115.1(2) . . ? C22 C23 C28 124.2(2) . . ? C23 C24 C25 122.9(2) . . ? C26 C25 C24 116.7(2) . . ? C26 C25 C29 123.4(2) . . ? C24 C25 C29 119.9(2) . . ? C25 C26 C27 123.1(2) . . ? C26 C27 C22 119.9(2) . . ? C26 C27 C30 116.7(2) . . ? C22 C27 C30 123.4(2) . . ? C23 C28 Si3 114.51(17) . . ? C23 C28 Si2 108.13(16) . . ? Si3 C28 Si2 116.63(13) . . ? C25 C29 Si4 113.95(17) . . ? C25 C29 Si5 111.61(17) . . ? Si4 C29 Si5 119.77(13) . . ? C27 C30 Si7 116.14(17) . . ? C27 C30 Si6 109.89(17) . . ? Si7 C30 Si6 115.16(13) . . ? C31 Si2 C33 109.84(14) . . ? C31 Si2 C32 105.20(13) . . ? C33 Si2 C32 106.77(14) . . ? C31 Si2 C28 109.79(12) . . ? C33 Si2 C28 109.71(13) . . ? C32 Si2 C28 115.36(12) . . ? C34 Si3 C36 108.39(15) . . ? C34 Si3 C35 104.25(14) . . ? C36 Si3 C35 107.88(14) . . ? C34 Si3 C28 113.20(12) . . ? C36 Si3 C28 108.20(13) . . ? C35 Si3 C28 114.66(12) . . ? C37 Si4 C39 108.87(14) . . ? C37 Si4 C38 110.54(14) . . ? C39 Si4 C38 107.02(14) . . ? C37 Si4 C29 106.98(12) . . ? C39 Si4 C29 114.86(13) . . ? C38 Si4 C29 108.58(13) . . ? C40 Si5 C42 109.34(15) . . ? C40 Si5 C41 107.52(15) . . ? C42 Si5 C41 108.48(15) . . ? C40 Si5 C29 107.89(13) . . ? C42 Si5 C29 113.80(13) . . ? C41 Si5 C29 109.64(13) . . ? C43 Si6 C44 107.97(15) . . ? C43 Si6 C45 107.24(13) . . ? C44 Si6 C45 108.02(15) . . ? C43 Si6 C30 108.87(12) . . ? C44 Si6 C30 112.04(12) . . ? C45 Si6 C30 112.50(13) . . ? C46 Si7 C48 107.51(14) . . ? C46 Si7 C47 108.05(13) . . ? C48 Si7 C47 106.08(14) . . ? C46 Si7 C30 110.91(12) . . ? C48 Si7 C30 109.76(12) . . ? C47 Si7 C30 114.21(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Si1 B1 O1 93.3(3) . . . . ? C22 Si1 B1 O1 -35.5(3) . . . . ? B2 Si1 B1 O1 -165.5(2) . . . . ? C13 Si1 B1 O2 -88.1(2) . . . . ? C22 Si1 B1 O2 143.16(18) . . . . ? B2 Si1 B1 O2 13.2(2) . . . . ? O2 B1 O1 C1 0.6(3) . . . . ? Si1 B1 O1 C1 179.3(2) . . . . ? B1 O1 C1 C3 -124.6(3) . . . . ? B1 O1 C1 C4 118.2(2) . . . . ? B1 O1 C1 C2 -2.9(3) . . . . ? O1 C1 C2 O2 4.0(2) . . . . ? C3 C1 C2 O2 119.7(2) . . . . ? C4 C1 C2 O2 -111.9(3) . . . . ? O1 C1 C2 C6 120.2(2) . . . . ? C3 C1 C2 C6 -124.1(3) . . . . ? C4 C1 C2 C6 4.3(3) . . . . ? O1 C1 C2 C5 -111.8(2) . . . . ? C3 C1 C2 C5 4.0(3) . . . . ? C4 C1 C2 C5 132.4(3) . . . . ? O1 B1 O2 C2 2.3(3) . . . . ? Si1 B1 O2 C2 -176.63(17) . . . . ? C6 C2 O2 B1 -126.0(2) . . . . ? C5 C2 O2 B1 118.1(2) . . . . ? C1 C2 O2 B1 -3.9(3) . . . . ? C13 Si1 B2 O4 8.6(2) . . . . ? C22 Si1 B2 O4 129.5(2) . . . . ? B1 Si1 B2 O4 -104.8(2) . . . . ? C13 Si1 B2 O3 -179.2(2) . . . . ? C22 Si1 B2 O3 -58.2(3) . . . . ? B1 Si1 B2 O3 67.4(3) . . . . ? O4 B2 O3 C7 11.9(3) . . . . ? Si1 B2 O3 C7 -160.7(2) . . . . ? B2 O3 C7 C9 -148.9(2) . . . . ? B2 O3 C7 C10 92.0(3) . . . . ? B2 O3 C7 C8 -26.7(3) . . . . ? O3 C7 C8 O4 30.9(3) . . . . ? C9 C7 C8 O4 149.1(2) . . . . ? C10 C7 C8 O4 -83.1(3) . . . . ? O3 C7 C8 C11 -82.9(3) . . . . ? C9 C7 C8 C11 35.3(3) . . . . ? C10 C7 C8 C11 163.1(2) . . . . ? O3 C7 C8 C12 147.5(3) . . . . ? C9 C7 C8 C12 -94.4(3) . . . . ? C10 C7 C8 C12 33.5(4) . . . . ? O3 B2 O4 C8 9.6(3) . . . . ? Si1 B2 O4 C8 -176.76(18) . . . . ? C11 C8 O4 B2 93.4(3) . . . . ? C12 C8 O4 B2 -147.4(3) . . . . ? C7 C8 O4 B2 -25.4(3) . . . . ? C22 Si1 C13 C14 -64.2(2) . . . . ? B1 Si1 C13 C14 164.67(19) . . . . ? B2 Si1 C13 C14 64.4(2) . . . . ? C22 Si1 C13 C18 126.8(2) . . . . ? B1 Si1 C13 C18 -4.3(3) . . . . ? B2 Si1 C13 C18 -104.6(2) . . . . ? C18 C13 C14 C15 1.6(4) . . . . ? Si1 C13 C14 C15 -168.2(2) . . . . ? C18 C13 C14 C19 -177.7(2) . . . . ? Si1 C13 C14 C19 12.5(3) . . . . ? C13 C14 C15 C16 -0.8(4) . . . . ? C19 C14 C15 C16 178.5(2) . . . . ? C14 C15 C16 C17 -0.6(4) . . . . ? C14 C15 C16 C20 179.1(2) . . . . ? C15 C16 C17 C18 1.2(4) . . . . ? C20 C16 C17 C18 -178.4(3) . . . . ? C16 C17 C18 C13 -0.4(4) . . . . ? C16 C17 C18 C21 178.0(2) . . . . ? C14 C13 C18 C17 -1.0(4) . . . . ? Si1 C13 C18 C17 168.0(2) . . . . ? C14 C13 C18 C21 -179.3(2) . . . . ? Si1 C13 C18 C21 -10.4(4) . . . . ? C13 Si1 C22 C23 -53.1(2) . . . . ? B1 Si1 C22 C23 76.1(2) . . . . ? B2 Si1 C22 C23 -167.49(18) . . . . ? C13 Si1 C22 C27 120.5(2) . . . . ? B1 Si1 C22 C27 -110.3(2) . . . . ? B2 Si1 C22 C27 6.1(3) . . . . ? C27 C22 C23 C24 -5.7(3) . . . . ? Si1 C22 C23 C24 168.38(18) . . . . ? C27 C22 C23 C28 169.0(2) . . . . ? Si1 C22 C23 C28 -16.9(3) . . . . ? C22 C23 C24 C25 3.0(4) . . . . ? C28 C23 C24 C25 -172.2(2) . . . . ? C23 C24 C25 C26 1.9(4) . . . . ? C23 C24 C25 C29 -177.8(2) . . . . ? C24 C25 C26 C27 -3.9(4) . . . . ? C29 C25 C26 C27 175.8(2) . . . . ? C25 C26 C27 C22 1.1(4) . . . . ? C25 C26 C27 C30 178.4(2) . . . . ? C23 C22 C27 C26 3.7(3) . . . . ? Si1 C22 C27 C26 -169.96(18) . . . . ? C23 C22 C27 C30 -173.4(2) . . . . ? Si1 C22 C27 C30 12.9(3) . . . . ? C24 C23 C28 Si3 -62.8(3) . . . . ? C22 C23 C28 Si3 122.3(2) . . . . ? C24 C23 C28 Si2 69.1(2) . . . . ? C22 C23 C28 Si2 -105.9(2) . . . . ? C26 C25 C29 Si4 63.3(3) . . . . ? C24 C25 C29 Si4 -117.1(2) . . . . ? C26 C25 C29 Si5 -76.2(3) . . . . ? C24 C25 C29 Si5 103.4(2) . . . . ? C26 C27 C30 Si7 45.4(3) . . . . ? C22 C27 C30 Si7 -137.4(2) . . . . ? C26 C27 C30 Si6 -87.6(2) . . . . ? C22 C27 C30 Si6 89.7(2) . . . . ? C23 C28 Si2 C31 38.0(2) . . . . ? Si3 C28 Si2 C31 168.72(13) . . . . ? C23 C28 Si2 C33 158.78(17) . . . . ? Si3 C28 Si2 C33 -70.48(17) . . . . ? C23 C28 Si2 C32 -80.6(2) . . . . ? Si3 C28 Si2 C32 50.11(18) . . . . ? C23 C28 Si3 C34 -40.6(2) . . . . ? Si2 C28 Si3 C34 -168.23(14) . . . . ? C23 C28 Si3 C36 -160.69(19) . . . . ? Si2 C28 Si3 C36 71.63(17) . . . . ? C23 C28 Si3 C35 78.9(2) . . . . ? Si2 C28 Si3 C35 -48.80(19) . . . . ? C25 C29 Si4 C37 48.0(2) . . . . ? Si5 C29 Si4 C37 -176.12(14) . . . . ? C25 C29 Si4 C39 -73.0(2) . . . . ? Si5 C29 Si4 C39 62.93(19) . . . . ? C25 C29 Si4 C38 167.27(18) . . . . ? Si5 C29 Si4 C38 -56.81(19) . . . . ? C25 C29 Si5 C40 -39.1(2) . . . . ? Si4 C29 Si5 C40 -175.92(15) . . . . ? C25 C29 Si5 C42 82.5(2) . . . . ? Si4 C29 Si5 C42 -54.41(19) . . . . ? C25 C29 Si5 C41 -155.87(19) . . . . ? Si4 C29 Si5 C41 67.27(19) . . . . ? C27 C30 Si6 C43 -66.14(19) . . . . ? Si7 C30 Si6 C43 160.42(14) . . . . ? C27 C30 Si6 C44 53.2(2) . . . . ? Si7 C30 Si6 C44 -80.23(18) . . . . ? C27 C30 Si6 C45 175.15(17) . . . . ? Si7 C30 Si6 C45 41.71(18) . . . . ? C27 C30 Si7 C46 37.9(2) . . . . ? Si6 C30 Si7 C46 168.39(13) . . . . ? C27 C30 Si7 C48 156.55(19) . . . . ? Si6 C30 Si7 C48 -72.97(17) . . . . ? C27 C30 Si7 C47 -84.5(2) . . . . ? Si6 C30 Si7 C47 46.00(18) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.436 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.056 #===END data_bsitms #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Norihiro Tokitoh' _publ_contact_author_email 'tokitoh@boc.kuicr.kyoto-u.ac.jp' _publ_contact_author_fax '+81-774-38-3209' _publ_contact_author_phone '+81-774-38-3200' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Chemical Communications' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Unprecedented insertion reaction of a silylene into a B-B bond and generation of a novel borylsilyl anion by boron-metal exchange reaction of the resultant diborylsilane ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Takashi Kajiwara' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Nobuhiro Takeda' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Takahiro Sasamori' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Norihiro Tokitoh' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; _publ_section_synopsis ; ; #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BSiTMS _chemical_melting_point ? _chemical_formula_moiety 'C45 H91 B O2 Si8 ' _chemical_formula_sum 'C45 H91 B O2 Si8' _chemical_formula_weight 899.71 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' 'B' 'B' 0.0013 0.0007 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.100(7) _cell_length_b 20.193(10) _cell_length_c 24.014(11) _cell_angle_alpha 65.154(12) _cell_angle_beta 78.169(12) _cell_angle_gamma 88.869(18) _cell_volume 5626(5) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.222 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9569 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31913 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18704 _reflns_number_gt 15139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalClear' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0625P)^2^+3.7118P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18704 _refine_ls_number_parameters 1065 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Si1 Si 0.21131(6) 0.23062(4) -0.54983(3) 0.01850(18) Uani 1 1 d . A 1 Si2 Si 0.23198(6) 0.18619(5) -0.62904(4) 0.0246(2) Uani 1 1 d . A 1 C1 C 0.1559(3) 0.09762(18) -0.60526(15) 0.0343(8) Uani 1 1 d . A 1 H1 H 0.0810 0.1036 -0.5948 0.052 Uiso 1 1 calc R A 1 H2 H 0.1766 0.0598 -0.5685 0.052 Uiso 1 1 calc R A 1 H3 H 0.1702 0.0831 -0.6401 0.052 Uiso 1 1 calc R A 1 C2 C 0.3728(2) 0.1643(2) -0.64085(16) 0.0364(8) Uani 1 1 d . A 1 H4 H 0.3854 0.1396 -0.6688 0.055 Uiso 1 1 calc R A 1 H5 H 0.3884 0.1321 -0.6002 0.055 Uiso 1 1 calc R A 1 H6 H 0.4181 0.2097 -0.6597 0.055 Uiso 1 1 calc R A 1 C3 C 0.2123(3) 0.25220(18) -0.70810(14) 0.0320(8) Uani 1 1 d . A 1 H7 H 0.2349 0.2315 -0.7385 0.048 Uiso 1 1 calc R A 1 H8 H 0.2536 0.2984 -0.7217 0.048 Uiso 1 1 calc R A 1 H9 H 0.1381 0.2613 -0.7054 0.048 Uiso 1 1 calc R A 1 B1 B 0.3150(2) 0.32113(19) -0.59722(15) 0.0221(7) Uani 1 1 d . A 1 O1 O 0.33852(15) 0.37234(11) -0.57810(9) 0.0276(5) Uani 1 1 d . A 1 C4 C 0.4158(2) 0.42767(17) -0.62837(14) 0.0296(7) Uani 1 1 d . A 1 C5 C 0.4407(2) 0.39996(18) -0.68076(14) 0.0308(7) Uani 1 1 d . A 1 O2 O 0.36882(15) 0.33517(11) -0.65650(9) 0.0267(5) Uani 1 1 d . A 1 C6 C 0.5080(3) 0.4298(3) -0.60003(18) 0.0800(18) Uani 1 1 d . A 1 H10 H 0.4868 0.4472 -0.5672 0.120 Uiso 1 1 calc R A 1 H11 H 0.5649 0.4630 -0.6329 0.120 Uiso 1 1 calc R A 1 H12 H 0.5322 0.3805 -0.5816 0.120 Uiso 1 1 calc R A 1 C7 C 0.3658(4) 0.4988(2) -0.6475(2) 0.0780(17) Uani 1 1 d . A 1 H13 H 0.3025 0.4945 -0.6619 0.117 Uiso 1 1 calc R A 1 H14 H 0.4148 0.5374 -0.6817 0.117 Uiso 1 1 calc R A 1 H15 H 0.3473 0.5111 -0.6115 0.117 Uiso 1 1 calc R A 1 C8 C 0.5509(3) 0.3739(3) -0.6903(3) 0.0834(18) Uani 1 1 d . A 1 H16 H 0.5667 0.3435 -0.6493 0.125 Uiso 1 1 calc R A 1 H17 H 0.6019 0.4164 -0.7129 0.125 Uiso 1 1 calc R A 1 H18 H 0.5544 0.3451 -0.7148 0.125 Uiso 1 1 calc R A 1 C9 C 0.4196(5) 0.4510(2) -0.74347(18) 0.0812(17) Uani 1 1 d . A 1 H19 H 0.4279 0.4259 -0.7712 0.122 Uiso 1 1 calc R A 1 H20 H 0.4690 0.4943 -0.7624 0.122 Uiso 1 1 calc R A 1 H21 H 0.3480 0.4659 -0.7377 0.122 Uiso 1 1 calc R A 1 C10 C 0.2656(2) 0.14818(16) -0.49066(13) 0.0204(6) Uani 1 1 d . A 1 C11 C 0.3723(2) 0.14514(17) -0.48716(14) 0.0243(7) Uani 1 1 d . A 1 C12 C 0.4109(2) 0.07934(17) -0.45113(14) 0.0290(7) Uani 1 1 d . A 1 H22 H 0.4828 0.0787 -0.4496 0.035 Uiso 1 1 calc R A 1 C13 C 0.3476(3) 0.01542(17) -0.41776(15) 0.0317(8) Uani 1 1 d . A 1 C14 C 0.2431(2) 0.01821(17) -0.41972(14) 0.0285(7) Uani 1 1 d . A 1 H23 H 0.1980 -0.0251 -0.3960 0.034 Uiso 1 1 calc R A 1 C15 C 0.2013(2) 0.08251(16) -0.45539(14) 0.0235(7) Uani 1 1 d . A 1 C16 C 0.4486(2) 0.21092(17) -0.52113(14) 0.0284(7) Uani 1 1 d . A 1 H24 H 0.5153 0.1989 -0.5081 0.043 Uiso 1 1 calc R A 1 H25 H 0.4209 0.2509 -0.5110 0.043 Uiso 1 1 calc R A 1 H26 H 0.4595 0.2261 -0.5665 0.043 Uiso 1 1 calc R A 1 C17 C 0.3917(3) -0.05579(19) -0.38081(19) 0.0469(10) Uani 1 1 d . A 1 H27 H 0.4114 -0.0821 -0.4072 0.070 Uiso 1 1 calc R A 1 H28 H 0.3387 -0.0860 -0.3434 0.070 Uiso 1 1 calc R A 1 H29 H 0.4535 -0.0454 -0.3679 0.070 Uiso 1 1 calc R A 1 C18 C 0.0851(2) 0.07864(16) -0.45281(14) 0.0260(7) Uani 1 1 d . A 1 H30 H 0.0585 0.0273 -0.4354 0.039 Uiso 1 1 calc R A 1 H31 H 0.0726 0.1048 -0.4953 0.039 Uiso 1 1 calc R A 1 H32 H 0.0491 0.1013 -0.4260 0.039 Uiso 1 1 calc R A 1 C19 C 0.0803(2) 0.24807(15) -0.50667(12) 0.0180(6) Uani 1 1 d . A 1 C20 C 0.0768(2) 0.25144(15) -0.44837(13) 0.0203(6) Uani 1 1 d . A 1 C21 C -0.0192(2) 0.24251(15) -0.40685(13) 0.0217(6) Uani 1 1 d . A 1 H33 H -0.0192 0.2411 -0.3668 0.026 Uiso 1 1 calc R A 1 C22 C -0.1142(2) 0.23566(15) -0.42129(13) 0.0197(6) Uani 1 1 d . A 1 C23 C -0.1110(2) 0.24113(15) -0.48115(13) 0.0206(6) Uani 1 1 d . A 1 H34 H -0.1751 0.2409 -0.4937 0.025 Uiso 1 1 calc R A 1 C24 C -0.0173(2) 0.24703(15) -0.52401(13) 0.0180(6) Uani 1 1 d . A 1 C25 C 0.1711(2) 0.27107(16) -0.42941(13) 0.0224(6) Uani 1 1 d . A 1 H35 H 0.2331 0.2720 -0.4620 0.027 Uiso 1 1 calc R A 1 Si3 Si 0.19946(6) 0.20525(5) -0.35065(4) 0.0273(2) Uani 1 1 d . A 1 Si4 Si 0.16104(6) 0.37042(5) -0.43980(4) 0.0269(2) Uani 1 1 d . A 1 C26 C 0.3442(2) 0.2010(2) -0.35950(16) 0.0389(9) Uani 1 1 d . A 1 H36 H 0.3602 0.1705 -0.3185 0.058 Uiso 1 1 calc R A 1 H37 H 0.3773 0.2505 -0.3756 0.058 Uiso 1 1 calc R A 1 H38 H 0.3710 0.1796 -0.3890 0.058 Uiso 1 1 calc R A 1 C27 C 0.1379(3) 0.11140(19) -0.32009(16) 0.0414(9) Uani 1 1 d . A 1 H39 H 0.1674 0.0893 -0.3486 0.062 Uiso 1 1 calc R A 1 H40 H 0.0623 0.1134 -0.3172 0.062 Uiso 1 1 calc R A 1 H41 H 0.1515 0.0818 -0.2783 0.062 Uiso 1 1 calc R A 1 C28 C 0.1520(3) 0.2344(2) -0.28594(14) 0.0366(8) Uani 1 1 d . A 1 H42 H 0.1684 0.1983 -0.2468 0.055 Uiso 1 1 calc R A 1 H43 H 0.0762 0.2380 -0.2801 0.055 Uiso 1 1 calc R A 1 H44 H 0.1866 0.2822 -0.2969 0.055 Uiso 1 1 calc R A 1 C29 C 0.2930(3) 0.4066(2) -0.44103(16) 0.0393(9) Uani 1 1 d . A 1 H45 H 0.3454 0.4016 -0.4743 0.059 Uiso 1 1 calc R A 1 H46 H 0.3115 0.3786 -0.4003 0.059 Uiso 1 1 calc R A 1 H47 H 0.2908 0.4583 -0.4491 0.059 Uiso 1 1 calc R A 1 C30 C 0.1170(2) 0.42482(17) -0.51435(14) 0.0295(7) Uani 1 1 d . A 1 H48 H 0.0517 0.4014 -0.5138 0.044 Uiso 1 1 calc R A 1 H49 H 0.1709 0.4271 -0.5502 0.044 Uiso 1 1 calc R A 1 H50 H 0.1053 0.4745 -0.5182 0.044 Uiso 1 1 calc R A 1 C31 C 0.0628(3) 0.38619(19) -0.37866(16) 0.0364(8) Uani 1 1 d . A 1 H51 H 0.0522 0.4385 -0.3938 0.055 Uiso 1 1 calc R A 1 H52 H 0.0885 0.3695 -0.3397 0.055 Uiso 1 1 calc R A 1 H53 H -0.0037 0.3588 -0.3705 0.055 Uiso 1 1 calc R A 1 C32 C -0.2150(2) 0.22510(17) -0.37277(14) 0.0249(7) Uani 1 1 d . A 1 H54 H -0.1896 0.2309 -0.3384 0.030 Uiso 1 1 calc R A 1 Si5 Si -0.27486(6) 0.12829(5) -0.33285(4) 0.02442(19) Uani 1 1 d . A 1 Si6 Si -0.30156(6) 0.30339(5) -0.39857(4) 0.02395(19) Uani 1 1 d . A 1 C33 C -0.1710(3) 0.06314(18) -0.32486(17) 0.0404(9) Uani 1 1 d . A 1 H55 H -0.1210 0.0734 -0.3037 0.061 Uiso 1 1 calc R A 1 H56 H -0.1344 0.0686 -0.3667 0.061 Uiso 1 1 calc R A 1 H57 H -0.2025 0.0130 -0.3000 0.061 Uiso 1 1 calc R A 1 C34 C -0.3485(3) 0.1108(2) -0.25218(16) 0.0448(9) Uani 1 1 d . A 1 H58 H -0.4118 0.1377 -0.2550 0.067 Uiso 1 1 calc R A 1 H59 H -0.3044 0.1273 -0.2314 0.067 Uiso 1 1 calc R A 1 H60 H -0.3681 0.0583 -0.2278 0.067 Uiso 1 1 calc R A 1 C35 C -0.3659(3) 0.1090(2) -0.37600(17) 0.0419(9) Uani 1 1 d . A 1 H61 H -0.3833 0.0562 -0.3582 0.063 Uiso 1 1 calc R A 1 H62 H -0.3320 0.1269 -0.4206 0.063 Uiso 1 1 calc R A 1 H63 H -0.4300 0.1339 -0.3717 0.063 Uiso 1 1 calc R A 1 C36 C -0.2173(3) 0.38932(17) -0.42950(16) 0.0352(8) Uani 1 1 d . A 1 H64 H -0.2583 0.4313 -0.4472 0.053 Uiso 1 1 calc R A 1 H65 H -0.1585 0.3898 -0.4624 0.053 Uiso 1 1 calc R A 1 H66 H -0.1906 0.3923 -0.3953 0.053 Uiso 1 1 calc R A 1 C37 C -0.4054(2) 0.29766(19) -0.33028(15) 0.0334(8) Uani 1 1 d . A 1 H67 H -0.3732 0.2926 -0.2954 0.050 Uiso 1 1 calc R A 1 H68 H -0.4545 0.2551 -0.3170 0.050 Uiso 1 1 calc R A 1 H69 H -0.4431 0.3423 -0.3426 0.050 Uiso 1 1 calc R A 1 C38 C -0.3700(2) 0.30777(19) -0.46106(15) 0.0356(8) Uani 1 1 d . A 1 H70 H -0.4193 0.3461 -0.4678 0.053 Uiso 1 1 calc R A 1 H71 H -0.4082 0.2605 -0.4478 0.053 Uiso 1 1 calc R A 1 H72 H -0.3185 0.3190 -0.5003 0.053 Uiso 1 1 calc R A 1 C39 C -0.0256(2) 0.25416(15) -0.58867(13) 0.0200(6) Uani 1 1 d . A 1 H73 H 0.0424 0.2390 -0.6057 0.024 Uiso 1 1 calc R A 1 Si7 Si -0.12946(6) 0.19205(5) -0.59086(4) 0.02376(19) Uani 1 1 d . A 1 Si8 Si -0.02800(6) 0.35501(5) -0.64334(4) 0.0246(2) Uani 1 1 d . A 1 C40 C -0.1494(2) 0.10157(17) -0.52062(14) 0.0284(7) Uani 1 1 d . A 1 H74 H -0.0871 0.0744 -0.5228 0.043 Uiso 1 1 calc R A 1 H75 H -0.2102 0.0735 -0.5200 0.043 Uiso 1 1 calc R A 1 H76 H -0.1615 0.1094 -0.4823 0.043 Uiso 1 1 calc R A 1 C41 C -0.2602(2) 0.23154(19) -0.59455(16) 0.0339(8) Uani 1 1 d . A 1 H77 H -0.3098 0.1971 -0.5964 0.051 Uiso 1 1 calc R A 1 H78 H -0.2530 0.2779 -0.6322 0.051 Uiso 1 1 calc R A 1 H79 H -0.2861 0.2401 -0.5570 0.051 Uiso 1 1 calc R A 1 C42 C -0.0871(2) 0.17710(18) -0.66388(14) 0.0289(7) Uani 1 1 d . A 1 H80 H -0.0250 0.1490 -0.6610 0.043 Uiso 1 1 calc R A 1 H81 H -0.0705 0.2245 -0.7005 0.043 Uiso 1 1 calc R A 1 H82 H -0.1438 0.1499 -0.6683 0.043 Uiso 1 1 calc R A 1 C43 C -0.1307(3) 0.40054(18) -0.60866(16) 0.0351(8) Uani 1 1 d . A 1 H83 H -0.1195 0.3947 -0.5678 0.053 Uiso 1 1 calc R A 1 H84 H -0.1998 0.3781 -0.6031 0.053 Uiso 1 1 calc R A 1 H85 H -0.1266 0.4527 -0.6369 0.053 Uiso 1 1 calc R A 1 C44 C -0.0508(3) 0.37025(18) -0.72227(14) 0.0358(8) Uani 1 1 d . A 1 H86 H -0.0458 0.4229 -0.7492 0.054 Uiso 1 1 calc R A 1 H87 H -0.1206 0.3490 -0.7172 0.054 Uiso 1 1 calc R A 1 H88 H 0.0021 0.3468 -0.7416 0.054 Uiso 1 1 calc R A 1 C45 C 0.1021(2) 0.40151(17) -0.65765(14) 0.0311(7) Uani 1 1 d . A 1 H89 H 0.0978 0.4547 -0.6772 0.047 Uiso 1 1 calc R A 1 H90 H 0.1536 0.3873 -0.6857 0.047 Uiso 1 1 calc R A 1 H91 H 0.1235 0.3871 -0.6176 0.047 Uiso 1 1 calc R A 1 Si9 Si -0.22818(6) 0.27122(5) 0.03864(4) 0.02112(19) Uani 1 1 d . B 2 Si10 Si -0.24022(7) 0.30453(5) 0.12431(4) 0.0299(2) Uani 1 1 d . B 2 C46 C -0.1616(3) 0.39024(19) 0.10671(17) 0.0405(9) Uani 1 1 d . B 2 H92 H -0.1822 0.4314 0.0720 0.061 Uiso 1 1 calc R B 2 H93 H -0.0870 0.3841 0.0948 0.061 Uiso 1 1 calc R B 2 H94 H -0.1743 0.4001 0.1441 0.061 Uiso 1 1 calc R B 2 C47 C -0.2203(2) 0.2315(2) 0.20085(14) 0.0354(8) Uani 1 1 d . B 2 H95 H -0.1464 0.2210 0.1968 0.053 Uiso 1 1 calc R B 2 H96 H -0.2634 0.1869 0.2116 0.053 Uiso 1 1 calc R B 2 H97 H -0.2406 0.2484 0.2340 0.053 Uiso 1 1 calc R B 2 C48 C -0.3797(3) 0.3271(2) 0.13954(17) 0.0498(11) Uani 1 1 d . B 2 H98 H -0.3901 0.3475 0.1706 0.075 Uiso 1 1 calc R B 2 H99 H -0.4260 0.2826 0.1557 0.075 Uiso 1 1 calc R B 2 H100 H -0.3958 0.3631 0.1003 0.075 Uiso 1 1 calc R B 2 B2 B -0.3376(3) 0.1838(2) 0.08091(16) 0.0269(8) Uani 1 1 d . B 2 O3 O -0.38395(17) 0.16263(13) 0.14276(10) 0.0372(6) Uani 1 1 d . B 2 C49 C -0.4548(3) 0.0975(2) 0.16482(15) 0.0412(9) Uani 1 1 d . B 2 C50 C -0.4520(2) 0.08564(17) 0.10433(14) 0.0287(7) Uani 1 1 d . B 2 O4 O -0.37014(16) 0.14019(11) 0.05681(9) 0.0283(5) Uani 1 1 d . B 2 C51 C -0.4118(4) 0.0369(3) 0.2159(2) 0.0847(18) Uani 1 1 d . B 2 H101 H -0.3411 0.0286 0.1981 0.127 Uiso 1 1 calc R B 2 H102 H -0.4572 -0.0082 0.2326 0.127 Uiso 1 1 calc R B 2 H103 H -0.4095 0.0514 0.2498 0.127 Uiso 1 1 calc R B 2 C52 C -0.5608(3) 0.1160(3) 0.1931(2) 0.0736(15) Uani 1 1 d . B 2 H104 H -0.5547 0.1254 0.2292 0.110 Uiso 1 1 calc R B 2 H105 H -0.6126 0.0749 0.2069 0.110 Uiso 1 1 calc R B 2 H106 H -0.5830 0.1597 0.1613 0.110 Uiso 1 1 calc R B 2 C53 C -0.4198(3) 0.0118(2) 0.1084(2) 0.0614(13) Uani 1 1 d . B 2 H107 H -0.4085 0.0123 0.0666 0.092 Uiso 1 1 calc R B 2 H108 H -0.4751 -0.0260 0.1373 0.092 Uiso 1 1 calc R B 2 H109 H -0.3549 0.0013 0.1238 0.092 Uiso 1 1 calc R B 2 C54 C -0.5510(3) 0.1025(2) 0.07969(17) 0.0457(9) Uani 1 1 d . B 2 H110 H -0.5684 0.1522 0.0736 0.068 Uiso 1 1 calc R B 2 H111 H -0.6083 0.0673 0.1100 0.068 Uiso 1 1 calc R B 2 H112 H -0.5405 0.0990 0.0395 0.068 Uiso 1 1 calc R B 2 C55 C -0.2768(2) 0.36074(17) -0.01526(13) 0.0233(7) Uani 1 1 d . B 2 C56 C -0.2072(2) 0.42417(17) -0.04393(14) 0.0259(7) Uani 1 1 d . B 2 C57 C -0.2430(2) 0.49266(17) -0.07395(15) 0.0299(7) Uani 1 1 d . B 2 H113 H -0.1945 0.5345 -0.0928 0.036 Uiso 1 1 calc R B 2 C58 C -0.3469(3) 0.50211(18) -0.07740(15) 0.0324(8) Uani 1 1 d . B 2 C59 C -0.4146(2) 0.44037(18) -0.05096(14) 0.0301(7) Uani 1 1 d . B 2 H114 H -0.4859 0.4455 -0.0538 0.036 Uiso 1 1 calc R B 2 C60 C -0.3822(2) 0.37039(17) -0.02016(14) 0.0262(7) Uani 1 1 d . B 2 C61 C -0.0915(2) 0.42129(17) -0.04536(16) 0.0300(7) Uani 1 1 d . B 2 H115 H -0.0577 0.4043 -0.0768 0.045 Uiso 1 1 calc R B 2 H116 H -0.0808 0.3875 -0.0039 0.045 Uiso 1 1 calc R B 2 H117 H -0.0611 0.4703 -0.0563 0.045 Uiso 1 1 calc R B 2 C62 C -0.3837(3) 0.57781(19) -0.10870(17) 0.0434(9) Uani 1 1 d . B 2 H118 H -0.4462 0.5745 -0.1242 0.065 Uiso 1 1 calc R B 2 H119 H -0.3283 0.6090 -0.1440 0.065 Uiso 1 1 calc R B 2 H120 H -0.4005 0.5989 -0.0782 0.065 Uiso 1 1 calc R B 2 C63 C -0.4639(2) 0.30687(18) 0.00736(15) 0.0315(8) Uani 1 1 d . B 2 H121 H -0.4395 0.2700 -0.0078 0.047 Uiso 1 1 calc R B 2 H122 H -0.5293 0.3243 -0.0056 0.047 Uiso 1 1 calc R B 2 H123 H -0.4760 0.2852 0.0533 0.047 Uiso 1 1 calc R B 2 C64 C -0.1021(2) 0.25299(15) -0.00817(13) 0.0187(6) Uani 1 1 d . B 2 C65 C -0.0042(2) 0.24663(15) 0.00969(13) 0.0209(6) Uani 1 1 d . B 2 C66 C 0.0883(2) 0.25171(15) -0.03412(13) 0.0228(6) Uani 1 1 d . B 2 H124 H 0.1529 0.2473 -0.0212 0.027 Uiso 1 1 calc R B 2 C67 C 0.0893(2) 0.26290(15) -0.09533(13) 0.0215(6) Uani 1 1 d . B 2 C68 C -0.0070(2) 0.26358(15) -0.11107(13) 0.0213(6) Uani 1 1 d . B 2 H125 H -0.0086 0.2691 -0.1521 0.026 Uiso 1 1 calc R B 2 C69 C -0.1023(2) 0.25646(15) -0.06867(13) 0.0208(6) Uani 1 1 d . B 2 C70 C 0.0076(2) 0.23311(16) 0.07557(13) 0.0228(7) Uani 1 1 d . B 2 H126 H -0.0583 0.2487 0.0945 0.027 Uiso 1 1 calc R B 2 Si11 Si 0.11708(6) 0.28917(5) 0.08031(4) 0.0259(2) Uani 1 1 d . B 2 Si12 Si 0.00484(7) 0.13047(5) 0.12527(4) 0.0284(2) Uani 1 1 d . B 2 C71 C 0.1383(2) 0.38359(18) 0.01535(15) 0.0316(7) Uani 1 1 d . B 2 H127 H 0.0822 0.4131 0.0238 0.047 Uiso 1 1 calc R B 2 H128 H 0.1379 0.3812 -0.0245 0.047 Uiso 1 1 calc R B 2 H129 H 0.2058 0.4060 0.0127 0.047 Uiso 1 1 calc R B 2 C72 C 0.2452(2) 0.24606(19) 0.07905(16) 0.0357(8) Uani 1 1 d . B 2 H130 H 0.2970 0.2754 0.0851 0.054 Uiso 1 1 calc R B 2 H131 H 0.2694 0.2439 0.0385 0.054 Uiso 1 1 calc R B 2 H132 H 0.2361 0.1964 0.1129 0.054 Uiso 1 1 calc R B 2 C73 C 0.0825(3) 0.29679(19) 0.15676(15) 0.0351(8) Uani 1 1 d . B 2 H133 H 0.1369 0.3277 0.1589 0.053 Uiso 1 1 calc R B 2 H134 H 0.0769 0.2480 0.1915 0.053 Uiso 1 1 calc R B 2 H135 H 0.0153 0.3187 0.1600 0.053 Uiso 1 1 calc R B 2 C74 C -0.1275(3) 0.08843(18) 0.13767(16) 0.0378(8) Uani 1 1 d . B 2 H136 H -0.1285 0.0352 0.1609 0.057 Uiso 1 1 calc R B 2 H137 H -0.1447 0.1003 0.0969 0.057 Uiso 1 1 calc R B 2 H138 H -0.1790 0.1076 0.1618 0.057 Uiso 1 1 calc R B 2 C75 C 0.1023(3) 0.08620(19) 0.08608(16) 0.0439(9) Uani 1 1 d . B 2 H139 H 0.0926 0.0329 0.1103 0.066 Uiso 1 1 calc R B 2 H140 H 0.1732 0.1032 0.0839 0.066 Uiso 1 1 calc R B 2 H141 H 0.0925 0.0992 0.0435 0.066 Uiso 1 1 calc R B 2 C76 C 0.0306(3) 0.10622(19) 0.20513(15) 0.0385(8) Uani 1 1 d . B 2 H142 H -0.0195 0.1286 0.2271 0.058 Uiso 1 1 calc R B 2 H143 H 0.1019 0.1245 0.2009 0.058 Uiso 1 1 calc R B 2 H144 H 0.0231 0.0529 0.2292 0.058 Uiso 1 1 calc R B 2 C77 C 0.1893(2) 0.27353(17) -0.14386(14) 0.0252(7) Uani 1 1 d . B 2 H145 H 0.1631 0.2772 -0.1813 0.030 Uiso 1 1 calc R B 2 Si13 Si 0.26040(7) 0.36551(5) -0.17261(4) 0.0306(2) Uani 1 1 d . B 2 Si14 Si 0.26478(6) 0.18893(5) -0.12471(4) 0.0277(2) Uani 1 1 d . B 2 C78 C 0.3420(3) 0.3694(2) -0.11820(18) 0.0485(10) Uani 1 1 d . B 2 H146 H 0.4019 0.3397 -0.1195 0.073 Uiso 1 1 calc R B 2 H147 H 0.2996 0.3502 -0.0752 0.073 Uiso 1 1 calc R B 2 H148 H 0.3672 0.4202 -0.1314 0.073 Uiso 1 1 calc R B 2 C79 C 0.1643(3) 0.43628(19) -0.18195(17) 0.0416(9) Uani 1 1 d . B 2 H149 H 0.2015 0.4844 -0.1977 0.062 Uiso 1 1 calc R B 2 H150 H 0.1174 0.4252 -0.1412 0.062 Uiso 1 1 calc R B 2 H151 H 0.1233 0.4365 -0.2119 0.062 Uiso 1 1 calc R B 2 C80 C 0.3487(3) 0.3891(2) -0.25057(18) 0.0527(11) Uani 1 1 d . B 2 H152 H 0.3089 0.3844 -0.2793 0.079 Uiso 1 1 calc R B 2 H153 H 0.4050 0.3558 -0.2458 0.079 Uiso 1 1 calc R B 2 H154 H 0.3789 0.4396 -0.2677 0.079 Uiso 1 1 calc R B 2 C81 C 0.3315(3) 0.1672(2) -0.05809(15) 0.0423(9) Uani 1 1 d . B 2 H155 H 0.2794 0.1598 -0.0199 0.063 Uiso 1 1 calc R B 2 H156 H 0.3820 0.2078 -0.0682 0.063 Uiso 1 1 calc R B 2 H157 H 0.3680 0.1225 -0.0512 0.063 Uiso 1 1 calc R B 2 C82 C 0.1704(3) 0.11070(18) -0.10539(15) 0.0365(8) Uani 1 1 d . B 2 H158 H 0.1398 0.1197 -0.1417 0.055 Uiso 1 1 calc R B 2 H159 H 0.1147 0.1056 -0.0693 0.055 Uiso 1 1 calc R B 2 H160 H 0.2069 0.0656 -0.0950 0.055 Uiso 1 1 calc R B 2 C83 C 0.3702(2) 0.19943(19) -0.19387(15) 0.0357(8) Uani 1 1 d . B 2 H161 H 0.3952 0.1514 -0.1881 0.054 Uiso 1 1 calc R B 2 H162 H 0.4283 0.2320 -0.1976 0.054 Uiso 1 1 calc R B 2 H163 H 0.3424 0.2204 -0.2321 0.054 Uiso 1 1 calc R B 2 C84 C -0.2004(2) 0.24705(16) -0.09005(13) 0.0228(6) Uani 1 1 d . B 2 H164 H -0.2603 0.2458 -0.0561 0.027 Uiso 1 1 calc R B 2 Si15 Si -0.20571(7) 0.15160(5) -0.08850(4) 0.0291(2) Uani 1 1 d . B 2 Si16 Si -0.22504(6) 0.32257(5) -0.16572(4) 0.0265(2) Uani 1 1 d . B 2 C85 C -0.1669(3) 0.08366(18) -0.01686(15) 0.0372(8) Uani 1 1 d . B 2 H165 H -0.1683 0.0352 -0.0169 0.056 Uiso 1 1 calc R B 2 H166 H -0.2157 0.0822 0.0206 0.056 Uiso 1 1 calc R B 2 H167 H -0.0960 0.0978 -0.0164 0.056 Uiso 1 1 calc R B 2 C86 C -0.1149(3) 0.14070(19) -0.15506(15) 0.0379(8) Uani 1 1 d . B 2 H168 H -0.0433 0.1567 -0.1576 0.057 Uiso 1 1 calc R B 2 H169 H -0.1359 0.1706 -0.1946 0.057 Uiso 1 1 calc R B 2 H170 H -0.1181 0.0892 -0.1477 0.057 Uiso 1 1 calc R B 2 C87 C -0.3427(3) 0.1275(2) -0.08973(17) 0.0430(9) Uani 1 1 d . B 2 H171 H -0.3496 0.0761 -0.0825 0.065 Uiso 1 1 calc R B 2 H172 H -0.3578 0.1589 -0.1307 0.065 Uiso 1 1 calc R B 2 H173 H -0.3921 0.1349 -0.0566 0.065 Uiso 1 1 calc R B 2 C88 C -0.1591(3) 0.41220(18) -0.18520(16) 0.0398(9) Uani 1 1 d . B 2 H174 H -0.0842 0.4071 -0.1866 0.060 Uiso 1 1 calc R B 2 H175 H -0.1891 0.4291 -0.1530 0.060 Uiso 1 1 calc R B 2 H176 H -0.1691 0.4478 -0.2263 0.060 Uiso 1 1 calc R B 2 C89 C -0.1815(3) 0.3059(2) -0.23813(15) 0.0381(8) Uani 1 1 d . B 2 H177 H -0.1928 0.3488 -0.2750 0.057 Uiso 1 1 calc R B 2 H178 H -0.2220 0.2630 -0.2336 0.057 Uiso 1 1 calc R B 2 H179 H -0.1070 0.2972 -0.2435 0.057 Uiso 1 1 calc R B 2 C90 C -0.3694(2) 0.3303(2) -0.15693(16) 0.0401(9) Uani 1 1 d . B 2 H180 H -0.3941 0.3522 -0.1276 0.060 Uiso 1 1 calc R B 2 H181 H -0.4049 0.2815 -0.1406 0.060 Uiso 1 1 calc R B 2 H182 H -0.3848 0.3612 -0.1980 0.060 Uiso 1 1 calc R B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0136(4) 0.0230(4) 0.0182(4) -0.0086(3) -0.0027(3) 0.0030(3) Si2 0.0226(4) 0.0316(5) 0.0230(4) -0.0143(4) -0.0072(3) 0.0101(4) C1 0.043(2) 0.0329(19) 0.0345(18) -0.0193(16) -0.0131(15) 0.0128(15) C2 0.0317(18) 0.053(2) 0.0358(19) -0.0278(17) -0.0119(15) 0.0224(16) C3 0.0316(17) 0.042(2) 0.0247(16) -0.0154(15) -0.0080(14) 0.0102(15) B1 0.0143(15) 0.0276(19) 0.0195(16) -0.0064(14) -0.0020(13) 0.0061(14) O1 0.0247(11) 0.0313(12) 0.0219(11) -0.0118(9) 0.0077(9) -0.0082(9) C4 0.0271(16) 0.0294(18) 0.0249(16) -0.0090(14) 0.0054(13) -0.0103(14) C5 0.0255(16) 0.0329(19) 0.0260(16) -0.0097(14) 0.0060(13) -0.0048(14) O2 0.0246(11) 0.0271(12) 0.0219(11) -0.0074(9) 0.0023(9) -0.0043(9) C6 0.054(3) 0.135(5) 0.031(2) -0.020(3) 0.0048(19) -0.059(3) C7 0.097(4) 0.029(2) 0.067(3) -0.011(2) 0.049(3) -0.002(2) C8 0.027(2) 0.084(4) 0.142(5) -0.072(4) 0.029(3) -0.010(2) C9 0.145(5) 0.054(3) 0.029(2) 0.001(2) -0.021(3) -0.034(3) C10 0.0173(14) 0.0285(17) 0.0193(14) -0.0133(13) -0.0055(11) 0.0054(12) C11 0.0184(14) 0.0324(18) 0.0255(16) -0.0156(14) -0.0049(12) 0.0046(13) C12 0.0222(16) 0.038(2) 0.0329(17) -0.0178(15) -0.0138(13) 0.0145(14) C13 0.0351(18) 0.0283(18) 0.0345(18) -0.0121(15) -0.0175(15) 0.0121(15) C14 0.0325(17) 0.0216(17) 0.0313(17) -0.0094(14) -0.0108(14) 0.0039(13) C15 0.0240(15) 0.0224(16) 0.0268(16) -0.0112(13) -0.0096(13) 0.0053(13) C16 0.0162(15) 0.0396(19) 0.0295(17) -0.0139(15) -0.0073(13) 0.0042(13) C17 0.044(2) 0.038(2) 0.063(3) -0.0169(19) -0.033(2) 0.0164(17) C18 0.0240(16) 0.0191(16) 0.0317(17) -0.0069(13) -0.0075(13) 0.0000(12) C19 0.0141(13) 0.0186(15) 0.0198(14) -0.0074(12) -0.0017(11) -0.0002(11) C20 0.0168(14) 0.0200(16) 0.0195(14) -0.0050(12) -0.0018(11) 0.0028(11) C21 0.0224(15) 0.0236(16) 0.0177(14) -0.0083(12) -0.0019(12) 0.0004(12) C22 0.0148(14) 0.0167(15) 0.0232(15) -0.0072(12) 0.0022(11) 0.0004(11) C23 0.0144(14) 0.0196(16) 0.0260(15) -0.0076(13) -0.0051(12) 0.0014(11) C24 0.0176(14) 0.0152(15) 0.0191(14) -0.0051(12) -0.0044(11) 0.0013(11) C25 0.0169(14) 0.0314(18) 0.0194(14) -0.0124(13) -0.0011(11) 0.0008(12) Si3 0.0209(4) 0.0411(6) 0.0210(4) -0.0138(4) -0.0058(3) 0.0041(4) Si4 0.0222(4) 0.0317(5) 0.0265(4) -0.0145(4) 0.0004(3) -0.0047(4) C26 0.0267(17) 0.064(3) 0.0323(18) -0.0238(18) -0.0118(14) 0.0122(16) C27 0.047(2) 0.044(2) 0.0275(18) -0.0075(16) -0.0146(16) 0.0042(17) C28 0.0280(17) 0.059(2) 0.0236(17) -0.0181(16) -0.0054(14) 0.0014(16) C29 0.0308(18) 0.049(2) 0.0368(19) -0.0190(17) -0.0013(15) -0.0140(16) C30 0.0265(16) 0.0288(18) 0.0319(17) -0.0139(14) -0.0010(13) -0.0012(13) C31 0.0369(19) 0.037(2) 0.0369(19) -0.0203(16) 0.0000(15) 0.0001(15) C32 0.0142(14) 0.0328(18) 0.0274(16) -0.0140(14) -0.0012(12) -0.0007(12) Si5 0.0186(4) 0.0271(5) 0.0231(4) -0.0088(4) 0.0014(3) -0.0030(3) Si6 0.0163(4) 0.0291(5) 0.0252(4) -0.0129(4) 0.0012(3) 0.0026(3) C33 0.0279(18) 0.0300(19) 0.048(2) -0.0054(16) -0.0006(16) 0.0010(15) C34 0.043(2) 0.048(2) 0.0312(19) -0.0119(17) 0.0092(16) -0.0104(17) C35 0.0351(19) 0.043(2) 0.047(2) -0.0163(18) -0.0125(17) -0.0057(16) C36 0.0308(18) 0.0302(19) 0.043(2) -0.0184(16) 0.0016(15) 0.0044(14) C37 0.0237(16) 0.041(2) 0.0367(18) -0.0213(16) 0.0026(14) 0.0023(14) C38 0.0274(17) 0.046(2) 0.0334(18) -0.0164(16) -0.0088(14) 0.0115(15) C39 0.0155(14) 0.0213(16) 0.0246(15) -0.0106(13) -0.0062(11) 0.0071(11) Si7 0.0187(4) 0.0295(5) 0.0257(4) -0.0134(4) -0.0072(3) 0.0038(3) Si8 0.0244(4) 0.0256(5) 0.0219(4) -0.0077(4) -0.0064(3) 0.0073(3) C40 0.0264(16) 0.0318(18) 0.0291(17) -0.0147(14) -0.0062(13) -0.0020(13) C41 0.0222(16) 0.046(2) 0.0362(19) -0.0199(16) -0.0071(14) 0.0020(15) C42 0.0283(17) 0.0355(19) 0.0278(16) -0.0161(15) -0.0109(13) 0.0056(14) C43 0.0380(19) 0.0291(19) 0.0361(19) -0.0122(15) -0.0084(15) 0.0114(15) C44 0.045(2) 0.034(2) 0.0273(17) -0.0088(15) -0.0150(15) 0.0141(16) C45 0.0303(17) 0.0293(18) 0.0258(16) -0.0056(14) -0.0033(13) 0.0024(14) Si9 0.0140(4) 0.0284(5) 0.0191(4) -0.0089(3) -0.0026(3) 0.0061(3) Si10 0.0235(4) 0.0450(6) 0.0270(5) -0.0200(4) -0.0088(4) 0.0164(4) C46 0.050(2) 0.044(2) 0.041(2) -0.0281(18) -0.0189(17) 0.0165(18) C47 0.0277(17) 0.057(2) 0.0224(16) -0.0180(16) -0.0048(13) 0.0115(16) C48 0.036(2) 0.089(3) 0.044(2) -0.046(2) -0.0172(17) 0.035(2) B2 0.0148(16) 0.038(2) 0.0196(17) -0.0053(16) -0.0023(13) 0.0072(15) O3 0.0274(12) 0.0541(16) 0.0232(11) -0.0129(11) 0.0022(9) -0.0102(11) C49 0.0285(18) 0.056(2) 0.0251(17) -0.0059(16) 0.0017(14) -0.0160(16) C50 0.0205(15) 0.0286(18) 0.0275(16) -0.0058(14) 0.0013(13) -0.0009(13) O4 0.0247(11) 0.0297(12) 0.0225(11) -0.0069(10) 0.0027(9) -0.0046(9) C51 0.085(4) 0.082(4) 0.047(3) 0.022(2) -0.034(3) -0.041(3) C52 0.039(2) 0.130(4) 0.063(3) -0.067(3) 0.025(2) -0.029(3) C53 0.053(3) 0.036(2) 0.062(3) -0.006(2) 0.024(2) -0.0029(19) C54 0.0273(18) 0.065(3) 0.041(2) -0.0199(19) -0.0048(16) -0.0030(17) C55 0.0187(15) 0.0322(18) 0.0217(15) -0.0135(13) -0.0065(12) 0.0100(13) C56 0.0255(16) 0.0293(18) 0.0263(16) -0.0146(14) -0.0072(13) 0.0091(13) C57 0.0289(17) 0.0286(18) 0.0343(18) -0.0142(15) -0.0103(14) 0.0087(14) C58 0.0329(18) 0.037(2) 0.0303(17) -0.0166(15) -0.0111(14) 0.0190(15) C59 0.0194(15) 0.043(2) 0.0295(17) -0.0158(15) -0.0089(13) 0.0153(14) C60 0.0203(15) 0.0346(18) 0.0234(15) -0.0121(14) -0.0052(12) 0.0081(13) C61 0.0244(16) 0.0241(17) 0.0415(19) -0.0125(15) -0.0107(14) 0.0057(13) C62 0.043(2) 0.041(2) 0.049(2) -0.0182(18) -0.0182(17) 0.0234(17) C63 0.0142(14) 0.046(2) 0.0322(17) -0.0136(15) -0.0068(13) 0.0075(14) C64 0.0144(13) 0.0176(15) 0.0193(14) -0.0043(12) -0.0014(11) 0.0018(11) C65 0.0193(14) 0.0179(15) 0.0214(15) -0.0052(12) -0.0030(12) 0.0039(12) C66 0.0141(14) 0.0226(16) 0.0288(16) -0.0084(13) -0.0047(12) 0.0051(12) C67 0.0190(14) 0.0182(15) 0.0231(15) -0.0069(12) -0.0002(12) 0.0043(12) C68 0.0199(15) 0.0222(16) 0.0176(14) -0.0058(12) -0.0012(11) 0.0032(12) C69 0.0168(14) 0.0187(15) 0.0234(15) -0.0069(12) -0.0014(12) 0.0035(11) C70 0.0159(14) 0.0291(17) 0.0226(15) -0.0099(13) -0.0054(12) 0.0082(12) Si11 0.0177(4) 0.0356(5) 0.0247(4) -0.0126(4) -0.0063(3) 0.0069(4) Si12 0.0274(5) 0.0291(5) 0.0226(4) -0.0061(4) -0.0039(4) 0.0093(4) C71 0.0282(17) 0.038(2) 0.0315(17) -0.0169(15) -0.0078(14) 0.0025(14) C72 0.0198(16) 0.051(2) 0.0349(18) -0.0161(17) -0.0077(14) 0.0054(15) C73 0.0296(18) 0.048(2) 0.0293(17) -0.0165(16) -0.0100(14) 0.0067(15) C74 0.040(2) 0.032(2) 0.0301(18) -0.0033(15) -0.0034(15) -0.0023(15) C75 0.052(2) 0.033(2) 0.0343(19) -0.0069(16) 0.0002(17) 0.0173(17) C76 0.042(2) 0.037(2) 0.0293(18) -0.0064(15) -0.0105(15) 0.0120(16) C77 0.0172(14) 0.0344(18) 0.0213(15) -0.0111(14) -0.0008(12) 0.0043(13) Si13 0.0211(4) 0.0351(5) 0.0310(5) -0.0141(4) 0.0042(4) -0.0030(4) Si14 0.0202(4) 0.0376(5) 0.0208(4) -0.0101(4) -0.0012(3) 0.0119(4) C78 0.0284(19) 0.065(3) 0.054(2) -0.028(2) -0.0064(17) 0.0002(18) C79 0.0322(19) 0.034(2) 0.047(2) -0.0091(17) -0.0024(16) 0.0009(15) C80 0.050(2) 0.047(2) 0.044(2) -0.0148(19) 0.0168(18) -0.0123(19) C81 0.0331(19) 0.063(3) 0.0284(18) -0.0159(17) -0.0112(15) 0.0256(17) C82 0.0355(19) 0.034(2) 0.0312(18) -0.0098(15) 0.0014(15) 0.0076(15) C83 0.0282(17) 0.046(2) 0.0275(17) -0.0145(16) 0.0018(14) 0.0126(15) C84 0.0159(14) 0.0309(18) 0.0208(15) -0.0116(13) -0.0006(12) 0.0022(12) Si15 0.0278(5) 0.0299(5) 0.0264(5) -0.0121(4) 0.0019(4) -0.0025(4) Si16 0.0218(4) 0.0357(5) 0.0200(4) -0.0101(4) -0.0046(3) 0.0050(4) C85 0.041(2) 0.0303(19) 0.0341(19) -0.0122(16) 0.0023(15) 0.0029(15) C86 0.040(2) 0.037(2) 0.0327(18) -0.0153(16) 0.0019(15) 0.0011(16) C87 0.037(2) 0.052(2) 0.040(2) -0.0235(18) -0.0003(16) -0.0088(17) C88 0.046(2) 0.037(2) 0.0295(18) -0.0052(16) -0.0140(16) 0.0049(16) C89 0.0363(19) 0.049(2) 0.0268(17) -0.0149(16) -0.0055(15) 0.0072(16) C90 0.0266(17) 0.055(2) 0.0344(19) -0.0136(17) -0.0119(15) 0.0115(16) _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 C10 1.917(3) . ? Si1 C19 1.923(3) . ? Si1 B1 2.049(4) . ? Si1 Si2 2.3897(14) . ? Si2 C1 1.870(4) . ? Si2 C3 1.873(3) . ? Si2 C2 1.881(3) . ? B1 O1 1.358(4) . ? B1 O2 1.364(4) . ? O1 C4 1.463(3) . ? C4 C7 1.495(5) . ? C4 C6 1.513(5) . ? C4 C5 1.555(4) . ? C5 O2 1.456(4) . ? C5 C9 1.504(5) . ? C5 C8 1.533(5) . ? C10 C15 1.412(4) . ? C10 C11 1.416(4) . ? C11 C12 1.399(4) . ? C11 C16 1.495(4) . ? C12 C13 1.377(5) . ? C13 C14 1.378(4) . ? C13 C17 1.515(4) . ? C14 C15 1.396(4) . ? C15 C18 1.513(4) . ? C19 C20 1.422(4) . ? C19 C24 1.425(4) . ? C20 C21 1.397(4) . ? C20 C25 1.514(4) . ? C21 C22 1.383(4) . ? C22 C23 1.386(4) . ? C22 C32 1.522(4) . ? C23 C24 1.402(4) . ? C24 C39 1.525(4) . ? C25 Si3 1.907(3) . ? C25 Si4 1.920(3) . ? Si3 C27 1.852(4) . ? Si3 C26 1.868(3) . ? Si3 C28 1.872(3) . ? Si4 C30 1.868(3) . ? Si4 C31 1.875(3) . ? Si4 C29 1.879(3) . ? C32 Si5 1.880(3) . ? C32 Si6 1.888(3) . ? Si5 C33 1.856(3) . ? Si5 C34 1.866(3) . ? Si5 C35 1.874(4) . ? Si6 C36 1.854(3) . ? Si6 C37 1.867(3) . ? Si6 C38 1.871(3) . ? C39 Si7 1.892(3) . ? C39 Si8 1.908(3) . ? Si7 C40 1.871(3) . ? Si7 C42 1.874(3) . ? Si7 C41 1.878(3) . ? Si8 C45 1.859(3) . ? Si8 C43 1.866(3) . ? Si8 C44 1.875(3) . ? Si9 C55 1.917(3) . ? Si9 C64 1.921(3) . ? Si9 B2 2.050(4) . ? Si9 Si10 2.3948(15) . ? Si10 C48 1.874(3) . ? Si10 C46 1.874(4) . ? Si10 C47 1.878(3) . ? B2 O4 1.354(4) . ? B2 O3 1.365(4) . ? O3 C49 1.461(4) . ? C49 C51 1.520(5) . ? C49 C52 1.529(5) . ? C49 C50 1.561(5) . ? C50 O4 1.468(3) . ? C50 C54 1.508(5) . ? C50 C53 1.510(5) . ? C55 C56 1.412(4) . ? C55 C60 1.413(4) . ? C56 C57 1.388(4) . ? C56 C61 1.509(4) . ? C57 C58 1.386(4) . ? C58 C59 1.375(5) . ? C58 C62 1.513(4) . ? C59 C60 1.397(4) . ? C60 C63 1.510(4) . ? C64 C65 1.420(4) . ? C64 C69 1.426(4) . ? C65 C66 1.406(4) . ? C65 C70 1.529(4) . ? C66 C67 1.387(4) . ? C67 C68 1.387(4) . ? C67 C77 1.515(4) . ? C68 C69 1.407(4) . ? C69 C84 1.521(4) . ? C70 Si11 1.895(3) . ? C70 Si12 1.905(3) . ? Si11 C71 1.868(3) . ? Si11 C73 1.869(3) . ? Si11 C72 1.876(3) . ? Si12 C74 1.857(4) . ? Si12 C75 1.867(3) . ? Si12 C76 1.871(3) . ? C77 Si13 1.877(3) . ? C77 Si14 1.889(3) . ? Si13 C79 1.858(4) . ? Si13 C80 1.859(4) . ? Si13 C78 1.876(4) . ? Si14 C82 1.862(4) . ? Si14 C81 1.866(3) . ? Si14 C83 1.867(3) . ? C84 Si16 1.903(3) . ? C84 Si15 1.915(3) . ? Si15 C85 1.857(3) . ? Si15 C86 1.877(3) . ? Si15 C87 1.878(4) . ? Si16 C88 1.851(4) . ? Si16 C90 1.870(3) . ? Si16 C89 1.882(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Si1 C19 107.96(12) . . ? C10 Si1 B1 113.97(13) . . ? C19 Si1 B1 114.02(13) . . ? C10 Si1 Si2 95.53(10) . . ? C19 Si1 Si2 125.44(9) . . ? B1 Si1 Si2 98.76(11) . . ? C1 Si2 C3 108.71(15) . . ? C1 Si2 C2 104.57(16) . . ? C3 Si2 C2 106.25(15) . . ? C1 Si2 Si1 115.04(11) . . ? C3 Si2 Si1 116.58(12) . . ? C2 Si2 Si1 104.50(11) . . ? O1 B1 O2 112.7(3) . . ? O1 B1 Si1 128.7(2) . . ? O2 B1 Si1 118.6(2) . . ? B1 O1 C4 109.1(2) . . ? O1 C4 C7 106.9(3) . . ? O1 C4 C6 106.2(3) . . ? C7 C4 C6 111.0(4) . . ? O1 C4 C5 104.5(2) . . ? C7 C4 C5 113.7(3) . . ? C6 C4 C5 113.8(3) . . ? O2 C5 C9 107.0(3) . . ? O2 C5 C8 106.0(3) . . ? C9 C5 C8 109.3(4) . . ? O2 C5 C4 103.6(2) . . ? C9 C5 C4 115.8(3) . . ? C8 C5 C4 114.2(3) . . ? B1 O2 C5 109.9(2) . . ? C15 C10 C11 116.8(3) . . ? C15 C10 Si1 119.1(2) . . ? C11 C10 Si1 123.4(2) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 C16 116.9(3) . . ? C10 C11 C16 122.4(3) . . ? C13 C12 C11 121.9(3) . . ? C12 C13 C14 117.8(3) . . ? C12 C13 C17 121.0(3) . . ? C14 C13 C17 121.1(3) . . ? C13 C14 C15 122.3(3) . . ? C14 C15 C10 120.5(3) . . ? C14 C15 C18 117.1(3) . . ? C10 C15 C18 122.3(2) . . ? C20 C19 C24 116.8(2) . . ? C20 C19 Si1 118.0(2) . . ? C24 C19 Si1 124.4(2) . . ? C21 C20 C19 119.9(3) . . ? C21 C20 C25 115.8(3) . . ? C19 C20 C25 124.1(2) . . ? C22 C21 C20 123.1(3) . . ? C21 C22 C23 116.6(2) . . ? C21 C22 C32 119.5(3) . . ? C23 C22 C32 123.8(3) . . ? C22 C23 C24 122.9(3) . . ? C23 C24 C19 119.8(3) . . ? C23 C24 C39 117.2(2) . . ? C19 C24 C39 123.0(2) . . ? C20 C25 Si3 117.6(2) . . ? C20 C25 Si4 106.63(19) . . ? Si3 C25 Si4 114.28(15) . . ? C27 Si3 C26 109.00(17) . . ? C27 Si3 C28 104.48(16) . . ? C26 Si3 C28 106.87(15) . . ? C27 Si3 C25 114.10(14) . . ? C26 Si3 C25 108.57(14) . . ? C28 Si3 C25 113.50(15) . . ? C30 Si4 C31 103.72(16) . . ? C30 Si4 C29 111.85(15) . . ? C31 Si4 C29 107.65(16) . . ? C30 Si4 C25 108.78(14) . . ? C31 Si4 C25 116.77(14) . . ? C29 Si4 C25 108.09(15) . . ? C22 C32 Si5 113.3(2) . . ? C22 C32 Si6 113.1(2) . . ? Si5 C32 Si6 119.62(15) . . ? C33 Si5 C34 107.80(17) . . ? C33 Si5 C35 108.17(18) . . ? C34 Si5 C35 108.95(18) . . ? C33 Si5 C32 110.21(14) . . ? C34 Si5 C32 108.48(15) . . ? C35 Si5 C32 113.09(15) . . ? C36 Si6 C37 109.58(15) . . ? C36 Si6 C38 108.07(16) . . ? C37 Si6 C38 106.62(15) . . ? C36 Si6 C32 107.20(15) . . ? C37 Si6 C32 110.17(14) . . ? C38 Si6 C32 115.12(15) . . ? C24 C39 Si7 116.76(19) . . ? C24 C39 Si8 109.31(19) . . ? Si7 C39 Si8 114.27(14) . . ? C40 Si7 C42 109.17(15) . . ? C40 Si7 C41 107.47(15) . . ? C42 Si7 C41 106.28(14) . . ? C40 Si7 C39 111.52(13) . . ? C42 Si7 C39 108.50(14) . . ? C41 Si7 C39 113.70(14) . . ? C45 Si8 C43 108.96(16) . . ? C45 Si8 C44 106.63(15) . . ? C43 Si8 C44 107.64(15) . . ? C45 Si8 C39 108.23(13) . . ? C43 Si8 C39 111.91(14) . . ? C44 Si8 C39 113.27(14) . . ? C55 Si9 C64 108.10(12) . . ? C55 Si9 B2 114.71(14) . . ? C64 Si9 B2 113.27(14) . . ? C55 Si9 Si10 94.88(10) . . ? C64 Si9 Si10 125.94(10) . . ? B2 Si9 Si10 98.96(11) . . ? C48 Si10 C46 104.49(18) . . ? C48 Si10 C47 105.92(16) . . ? C46 Si10 C47 108.51(16) . . ? C48 Si10 Si9 103.37(12) . . ? C46 Si10 Si9 115.97(12) . . ? C47 Si10 Si9 117.14(12) . . ? O4 B2 O3 112.7(3) . . ? O4 B2 Si9 129.1(2) . . ? O3 B2 Si9 118.1(3) . . ? B2 O3 C49 109.6(3) . . ? O3 C49 C51 106.3(3) . . ? O3 C49 C52 105.9(3) . . ? C51 C49 C52 110.1(4) . . ? O3 C49 C50 103.8(2) . . ? C51 C49 C50 115.1(4) . . ? C52 C49 C50 114.7(3) . . ? O4 C50 C54 106.4(3) . . ? O4 C50 C53 106.8(2) . . ? C54 C50 C53 109.6(3) . . ? O4 C50 C49 103.7(2) . . ? C54 C50 C49 114.4(3) . . ? C53 C50 C49 115.2(3) . . ? B2 O4 C50 109.6(2) . . ? C56 C55 C60 117.0(3) . . ? C56 C55 Si9 118.0(2) . . ? C60 C55 Si9 124.1(2) . . ? C57 C56 C55 120.6(3) . . ? C57 C56 C61 116.9(3) . . ? C55 C56 C61 122.5(3) . . ? C58 C57 C56 122.2(3) . . ? C59 C58 C57 117.5(3) . . ? C59 C58 C62 121.7(3) . . ? C57 C58 C62 120.8(3) . . ? C58 C59 C60 122.3(3) . . ? C59 C60 C55 120.4(3) . . ? C59 C60 C63 117.4(3) . . ? C55 C60 C63 122.2(3) . . ? C65 C64 C69 117.2(2) . . ? C65 C64 Si9 123.7(2) . . ? C69 C64 Si9 118.4(2) . . ? C66 C65 C64 119.9(3) . . ? C66 C65 C70 116.6(2) . . ? C64 C65 C70 123.5(2) . . ? C67 C66 C65 122.9(3) . . ? C68 C67 C66 116.9(3) . . ? C68 C67 C77 120.1(3) . . ? C66 C67 C77 123.0(3) . . ? C67 C68 C69 122.7(3) . . ? C68 C69 C64 119.8(3) . . ? C68 C69 C84 115.8(3) . . ? C64 C69 C84 124.2(2) . . ? C65 C70 Si11 116.6(2) . . ? C65 C70 Si12 109.1(2) . . ? Si11 C70 Si12 114.59(14) . . ? C71 Si11 C73 108.25(16) . . ? C71 Si11 C72 107.95(15) . . ? C73 Si11 C72 106.17(15) . . ? C71 Si11 C70 112.17(14) . . ? C73 Si11 C70 108.72(14) . . ? C72 Si11 C70 113.30(15) . . ? C74 Si12 C75 108.33(18) . . ? C74 Si12 C76 106.62(16) . . ? C75 Si12 C76 107.38(16) . . ? C74 Si12 C70 108.75(14) . . ? C75 Si12 C70 111.84(14) . . ? C76 Si12 C70 113.67(15) . . ? C67 C77 Si13 112.7(2) . . ? C67 C77 Si14 113.0(2) . . ? Si13 C77 Si14 119.80(16) . . ? C79 Si13 C80 108.12(18) . . ? C79 Si13 C78 108.54(18) . . ? C80 Si13 C78 107.69(19) . . ? C79 Si13 C77 109.47(15) . . ? C80 Si13 C77 109.89(16) . . ? C78 Si13 C77 113.00(16) . . ? C82 Si14 C81 108.99(17) . . ? C82 Si14 C83 109.59(16) . . ? C81 Si14 C83 105.78(16) . . ? C82 Si14 C77 107.17(15) . . ? C81 Si14 C77 114.93(15) . . ? C83 Si14 C77 110.31(14) . . ? C69 C84 Si16 117.8(2) . . ? C69 C84 Si15 107.90(19) . . ? Si16 C84 Si15 113.55(15) . . ? C85 Si15 C86 104.31(16) . . ? C85 Si15 C87 110.54(17) . . ? C86 Si15 C87 107.73(17) . . ? C85 Si15 C84 110.08(15) . . ? C86 Si15 C84 115.73(14) . . ? C87 Si15 C84 108.36(15) . . ? C88 Si16 C90 109.68(17) . . ? C88 Si16 C89 105.11(16) . . ? C90 Si16 C89 105.30(16) . . ? C88 Si16 C84 112.96(14) . . ? C90 Si16 C84 108.22(14) . . ? C89 Si16 C84 115.24(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Si1 Si2 C1 61.15(15) . . . . ? C19 Si1 Si2 C1 -55.54(16) . . . . ? B1 Si1 Si2 C1 176.49(14) . . . . ? C10 Si1 Si2 C3 -169.82(15) . . . . ? C19 Si1 Si2 C3 73.49(16) . . . . ? B1 Si1 Si2 C3 -54.48(15) . . . . ? C10 Si1 Si2 C2 -52.91(15) . . . . ? C19 Si1 Si2 C2 -169.60(16) . . . . ? B1 Si1 Si2 C2 62.43(15) . . . . ? C10 Si1 B1 O1 -81.7(3) . . . . ? C19 Si1 B1 O1 42.9(3) . . . . ? Si2 Si1 B1 O1 178.2(2) . . . . ? C10 Si1 B1 O2 99.3(2) . . . . ? C19 Si1 B1 O2 -136.1(2) . . . . ? Si2 Si1 B1 O2 -0.8(2) . . . . ? O2 B1 O1 C4 0.1(3) . . . . ? Si1 B1 O1 C4 -178.9(2) . . . . ? B1 O1 C4 C7 118.0(3) . . . . ? B1 O1 C4 C6 -123.4(3) . . . . ? B1 O1 C4 C5 -2.9(3) . . . . ? O1 C4 C5 O2 4.3(3) . . . . ? C7 C4 C5 O2 -111.8(3) . . . . ? C6 C4 C5 O2 119.7(3) . . . . ? O1 C4 C5 C9 121.1(3) . . . . ? C7 C4 C5 C9 4.9(5) . . . . ? C6 C4 C5 C9 -123.5(4) . . . . ? O1 C4 C5 C8 -110.5(3) . . . . ? C7 C4 C5 C8 133.3(4) . . . . ? C6 C4 C5 C8 4.9(4) . . . . ? O1 B1 O2 C5 3.0(3) . . . . ? Si1 B1 O2 C5 -177.9(2) . . . . ? C9 C5 O2 B1 -127.3(3) . . . . ? C8 C5 O2 B1 116.1(3) . . . . ? C4 C5 O2 B1 -4.5(3) . . . . ? C19 Si1 C10 C15 52.5(3) . . . . ? B1 Si1 C10 C15 -179.7(2) . . . . ? Si2 Si1 C10 C15 -77.5(2) . . . . ? C19 Si1 C10 C11 -138.0(2) . . . . ? B1 Si1 C10 C11 -10.2(3) . . . . ? Si2 Si1 C10 C11 91.9(2) . . . . ? C15 C10 C11 C12 1.1(4) . . . . ? Si1 C10 C11 C12 -168.6(2) . . . . ? C15 C10 C11 C16 -178.8(3) . . . . ? Si1 C10 C11 C16 11.5(4) . . . . ? C10 C11 C12 C13 -0.1(5) . . . . ? C16 C11 C12 C13 179.8(3) . . . . ? C11 C12 C13 C14 -1.3(5) . . . . ? C11 C12 C13 C17 177.9(3) . . . . ? C12 C13 C14 C15 1.8(5) . . . . ? C17 C13 C14 C15 -177.4(3) . . . . ? C13 C14 C15 C10 -0.8(5) . . . . ? C13 C14 C15 C18 -179.1(3) . . . . ? C11 C10 C15 C14 -0.7(4) . . . . ? Si1 C10 C15 C14 169.5(2) . . . . ? C11 C10 C15 C18 177.5(3) . . . . ? Si1 C10 C15 C18 -12.3(4) . . . . ? C10 Si1 C19 C20 49.3(3) . . . . ? B1 Si1 C19 C20 -78.5(2) . . . . ? Si2 Si1 C19 C20 160.08(18) . . . . ? C10 Si1 C19 C24 -120.9(2) . . . . ? B1 Si1 C19 C24 111.4(2) . . . . ? Si2 Si1 C19 C24 -10.1(3) . . . . ? C24 C19 C20 C21 9.6(4) . . . . ? Si1 C19 C20 C21 -161.3(2) . . . . ? C24 C19 C20 C25 -164.7(3) . . . . ? Si1 C19 C20 C25 24.4(4) . . . . ? C19 C20 C21 C22 -5.0(4) . . . . ? C25 C20 C21 C22 169.8(3) . . . . ? C20 C21 C22 C23 -2.6(4) . . . . ? C20 C21 C22 C32 179.2(3) . . . . ? C21 C22 C23 C24 5.3(4) . . . . ? C32 C22 C23 C24 -176.6(3) . . . . ? C22 C23 C24 C19 -0.4(4) . . . . ? C22 C23 C24 C39 -178.8(3) . . . . ? C20 C19 C24 C23 -7.0(4) . . . . ? Si1 C19 C24 C23 163.2(2) . . . . ? C20 C19 C24 C39 171.3(2) . . . . ? Si1 C19 C24 C39 -18.5(4) . . . . ? C21 C20 C25 Si3 58.4(3) . . . . ? C19 C20 C25 Si3 -127.1(3) . . . . ? C21 C20 C25 Si4 -71.4(3) . . . . ? C19 C20 C25 Si4 103.1(3) . . . . ? C20 C25 Si3 C27 20.4(3) . . . . ? Si4 C25 Si3 C27 146.59(17) . . . . ? C20 C25 Si3 C26 142.2(2) . . . . ? Si4 C25 Si3 C26 -91.63(18) . . . . ? C20 C25 Si3 C28 -99.1(2) . . . . ? Si4 C25 Si3 C28 27.0(2) . . . . ? C20 C25 Si4 C30 -41.4(2) . . . . ? Si3 C25 Si4 C30 -173.05(14) . . . . ? C20 C25 Si4 C31 75.5(2) . . . . ? Si3 C25 Si4 C31 -56.2(2) . . . . ? C20 C25 Si4 C29 -163.01(19) . . . . ? Si3 C25 Si4 C29 65.30(19) . . . . ? C21 C22 C32 Si5 -103.8(3) . . . . ? C23 C22 C32 Si5 78.1(3) . . . . ? C21 C22 C32 Si6 115.9(3) . . . . ? C23 C22 C32 Si6 -62.2(3) . . . . ? C22 C32 Si5 C33 33.1(3) . . . . ? Si6 C32 Si5 C33 170.59(18) . . . . ? C22 C32 Si5 C34 150.9(2) . . . . ? Si6 C32 Si5 C34 -71.6(2) . . . . ? C22 C32 Si5 C35 -88.1(2) . . . . ? Si6 C32 Si5 C35 49.4(2) . . . . ? C22 C32 Si6 C36 -47.1(3) . . . . ? Si5 C32 Si6 C36 175.37(17) . . . . ? C22 C32 Si6 C37 -166.2(2) . . . . ? Si5 C32 Si6 C37 56.2(2) . . . . ? C22 C32 Si6 C38 73.2(3) . . . . ? Si5 C32 Si6 C38 -64.4(2) . . . . ? C23 C24 C39 Si7 -43.4(3) . . . . ? C19 C24 C39 Si7 138.3(2) . . . . ? C23 C24 C39 Si8 88.2(3) . . . . ? C19 C24 C39 Si8 -90.1(3) . . . . ? C24 C39 Si7 C40 -33.2(2) . . . . ? Si8 C39 Si7 C40 -162.56(15) . . . . ? C24 C39 Si7 C42 -153.5(2) . . . . ? Si8 C39 Si7 C42 77.16(18) . . . . ? C24 C39 Si7 C41 88.5(2) . . . . ? Si8 C39 Si7 C41 -40.9(2) . . . . ? C24 C39 Si8 C45 67.4(2) . . . . ? Si7 C39 Si8 C45 -159.67(15) . . . . ? C24 C39 Si8 C43 -52.7(2) . . . . ? Si7 C39 Si8 C43 80.25(19) . . . . ? C24 C39 Si8 C44 -174.60(19) . . . . ? Si7 C39 Si8 C44 -41.7(2) . . . . ? C55 Si9 Si10 C48 55.33(17) . . . . ? C64 Si9 Si10 C48 171.88(18) . . . . ? B2 Si9 Si10 C48 -60.66(18) . . . . ? C55 Si9 Si10 C46 -58.37(16) . . . . ? C64 Si9 Si10 C46 58.18(17) . . . . ? B2 Si9 Si10 C46 -174.36(15) . . . . ? C55 Si9 Si10 C47 171.35(15) . . . . ? C64 Si9 Si10 C47 -72.10(17) . . . . ? B2 Si9 Si10 C47 55.36(16) . . . . ? C55 Si9 B2 O4 79.4(3) . . . . ? C64 Si9 B2 O4 -45.4(3) . . . . ? Si10 Si9 B2 O4 179.0(3) . . . . ? C55 Si9 B2 O3 -103.3(2) . . . . ? C64 Si9 B2 O3 132.0(2) . . . . ? Si10 Si9 B2 O3 -3.6(2) . . . . ? O4 B2 O3 C49 0.8(4) . . . . ? Si9 B2 O3 C49 -177.0(2) . . . . ? B2 O3 C49 C51 117.0(4) . . . . ? B2 O3 C49 C52 -126.0(3) . . . . ? B2 O3 C49 C50 -4.8(3) . . . . ? O3 C49 C50 O4 6.7(3) . . . . ? C51 C49 C50 O4 -109.0(3) . . . . ? C52 C49 C50 O4 121.8(3) . . . . ? O3 C49 C50 C54 -108.7(3) . . . . ? C51 C49 C50 C54 135.6(3) . . . . ? C52 C49 C50 C54 6.3(5) . . . . ? O3 C49 C50 C53 123.0(3) . . . . ? C51 C49 C50 C53 7.3(4) . . . . ? C52 C49 C50 C53 -122.0(4) . . . . ? O3 B2 O4 C50 3.9(3) . . . . ? Si9 B2 O4 C50 -178.6(2) . . . . ? C54 C50 O4 B2 114.4(3) . . . . ? C53 C50 O4 B2 -128.6(3) . . . . ? C49 C50 O4 B2 -6.6(3) . . . . ? C64 Si9 C55 C56 -55.2(3) . . . . ? B2 Si9 C55 C56 177.3(2) . . . . ? Si10 Si9 C55 C56 75.1(2) . . . . ? C64 Si9 C55 C60 135.6(2) . . . . ? B2 Si9 C55 C60 8.2(3) . . . . ? Si10 Si9 C55 C60 -94.0(3) . . . . ? C60 C55 C56 C57 1.6(4) . . . . ? Si9 C55 C56 C57 -168.3(2) . . . . ? C60 C55 C56 C61 -176.5(3) . . . . ? Si9 C55 C56 C61 13.6(4) . . . . ? C55 C56 C57 C58 -0.2(5) . . . . ? C61 C56 C57 C58 178.1(3) . . . . ? C56 C57 C58 C59 -1.5(5) . . . . ? C56 C57 C58 C62 178.0(3) . . . . ? C57 C58 C59 C60 1.6(5) . . . . ? C62 C58 C59 C60 -177.9(3) . . . . ? C58 C59 C60 C55 -0.1(5) . . . . ? C58 C59 C60 C63 179.6(3) . . . . ? C56 C55 C60 C59 -1.5(4) . . . . ? Si9 C55 C60 C59 167.7(2) . . . . ? C56 C55 C60 C63 178.8(3) . . . . ? Si9 C55 C60 C63 -12.0(4) . . . . ? C55 Si9 C64 C65 120.3(2) . . . . ? B2 Si9 C64 C65 -111.4(3) . . . . ? Si10 Si9 C64 C65 10.0(3) . . . . ? C55 Si9 C64 C69 -50.2(3) . . . . ? B2 Si9 C64 C69 78.0(2) . . . . ? Si10 Si9 C64 C69 -160.55(18) . . . . ? C69 C64 C65 C66 6.7(4) . . . . ? Si9 C64 C65 C66 -164.0(2) . . . . ? C69 C64 C65 C70 -172.4(3) . . . . ? Si9 C64 C65 C70 16.9(4) . . . . ? C64 C65 C66 C67 0.0(4) . . . . ? C70 C65 C66 C67 179.1(3) . . . . ? C65 C66 C67 C68 -4.7(4) . . . . ? C65 C66 C67 C77 175.7(3) . . . . ? C66 C67 C68 C69 2.6(4) . . . . ? C77 C67 C68 C69 -177.8(3) . . . . ? C67 C68 C69 C64 4.1(4) . . . . ? C67 C68 C69 C84 -171.3(3) . . . . ? C65 C64 C69 C68 -8.6(4) . . . . ? Si9 C64 C69 C68 162.5(2) . . . . ? C65 C64 C69 C84 166.4(3) . . . . ? Si9 C64 C69 C84 -22.4(4) . . . . ? C66 C65 C70 Si11 44.4(3) . . . . ? C64 C65 C70 Si11 -136.5(2) . . . . ? C66 C65 C70 Si12 -87.4(3) . . . . ? C64 C65 C70 Si12 91.7(3) . . . . ? C65 C70 Si11 C71 35.0(2) . . . . ? Si12 C70 Si11 C71 164.22(15) . . . . ? C65 C70 Si11 C73 154.7(2) . . . . ? Si12 C70 Si11 C73 -76.10(19) . . . . ? C65 C70 Si11 C72 -87.5(2) . . . . ? Si12 C70 Si11 C72 41.7(2) . . . . ? C65 C70 Si12 C74 -66.6(2) . . . . ? Si11 C70 Si12 C74 160.56(16) . . . . ? C65 C70 Si12 C75 53.0(2) . . . . ? Si11 C70 Si12 C75 -79.8(2) . . . . ? C65 C70 Si12 C76 174.79(19) . . . . ? Si11 C70 Si12 C76 42.0(2) . . . . ? C68 C67 C77 Si13 107.5(3) . . . . ? C66 C67 C77 Si13 -73.0(3) . . . . ? C68 C67 C77 Si14 -112.8(3) . . . . ? C66 C67 C77 Si14 66.7(3) . . . . ? C67 C77 Si13 C79 -39.5(3) . . . . ? Si14 C77 Si13 C79 -176.14(18) . . . . ? C67 C77 Si13 C80 -158.1(2) . . . . ? Si14 C77 Si13 C80 65.3(2) . . . . ? C67 C77 Si13 C78 81.6(2) . . . . ? Si14 C77 Si13 C78 -55.0(2) . . . . ? C67 C77 Si14 C82 48.7(3) . . . . ? Si13 C77 Si14 C82 -174.73(17) . . . . ? C67 C77 Si14 C81 -72.6(3) . . . . ? Si13 C77 Si14 C81 64.0(2) . . . . ? C67 C77 Si14 C83 168.0(2) . . . . ? Si13 C77 Si14 C83 -55.5(2) . . . . ? C68 C69 C84 Si16 -59.4(3) . . . . ? C64 C69 C84 Si16 125.4(3) . . . . ? C68 C69 C84 Si15 70.7(3) . . . . ? C64 C69 C84 Si15 -104.5(3) . . . . ? C69 C84 Si15 C85 41.5(2) . . . . ? Si16 C84 Si15 C85 173.96(15) . . . . ? C69 C84 Si15 C86 -76.4(2) . . . . ? Si16 C84 Si15 C86 56.0(2) . . . . ? C69 C84 Si15 C87 162.5(2) . . . . ? Si16 C84 Si15 C87 -65.05(19) . . . . ? C69 C84 Si16 C88 -24.0(3) . . . . ? Si15 C84 Si16 C88 -151.50(16) . . . . ? C69 C84 Si16 C90 -145.7(2) . . . . ? Si15 C84 Si16 C90 86.87(19) . . . . ? C69 C84 Si16 C89 96.8(2) . . . . ? Si15 C84 Si16 C89 -30.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.547 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.061 #===END data_mesib #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Norihiro Tokitoh' _publ_contact_author_email 'tokitoh@boc.kuicr.kyoto-u.ac.jp' _publ_contact_author_fax '+81-774-38-3209' _publ_contact_author_phone '+81-774-38-3200' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Organometallics' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Borylsilyl Anions Utilizing Overcrowded Silylboranes and Their Properties ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Takashi Kajiwara' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Nobuhiro Takeda' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Takahiro Sasamori' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Norihiro Tokitoh' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; _publ_section_synopsis ; ; #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MeSiB _chemical_melting_point ? _chemical_formula_moiety 'C43 H85 B O2 Si7' _chemical_formula_sum 'C43 H85 B O2 Si7' _chemical_formula_weight 841.55 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' 'B' 'B' 0.0013 0.0007 '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 9.220(6) _cell_length_b 12.874(8) _cell_length_c 23.730(14) _cell_angle_alpha 100.332(6) _cell_angle_beta 92.284(9) _cell_angle_gamma 108.119(12) _cell_volume 2620(3) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.213 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9389 _exptl_absorpt_correction_T_max 0.9894 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17308 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9040 _reflns_number_gt 6684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalClear' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0994P)^2^+3.3214P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9040 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1068 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2138 _refine_ls_wR_factor_gt 0.1916 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Si1 Si 0.91588(13) 0.33143(9) 0.33547(5) 0.0191(3) Uani 1 1 d . . . C1 C 1.1256(5) 0.3561(4) 0.3577(2) 0.0351(11) Uani 1 1 d . . . H1 H 1.1883 0.4264 0.3483 0.053 Uiso 1 1 calc R . . H2 H 1.1563 0.2945 0.3369 0.053 Uiso 1 1 calc R . . H3 H 1.1407 0.3601 0.3992 0.053 Uiso 1 1 calc R . . B1 B 0.8223(6) 0.1993(4) 0.3745(2) 0.0248(10) Uani 1 1 d . . . O1 O 0.8981(4) 0.2002(3) 0.42572(14) 0.0369(8) Uani 1 1 d . . . C2 C 0.8163(7) 0.0982(4) 0.4450(2) 0.0458(13) Uani 1 1 d . . . C3 C 0.6546(6) 0.0694(4) 0.4146(2) 0.0452(14) Uani 1 1 d . . . O2 O 0.6897(4) 0.1125(3) 0.36210(13) 0.0394(8) Uani 1 1 d . . . C4 C 0.8969(8) 0.0161(5) 0.4249(3) 0.0578(16) Uani 1 1 d . . . H4 H 0.8855 -0.0023 0.3828 0.087 Uiso 1 1 calc R . . H5 H 0.8521 -0.0519 0.4399 0.087 Uiso 1 1 calc R . . H6 H 1.0061 0.0487 0.4390 0.087 Uiso 1 1 calc R . . C5 C 0.8242(7) 0.1225(5) 0.5105(2) 0.0550(16) Uani 1 1 d . . . H7 H 0.7699 0.0540 0.5236 0.083 Uiso 1 1 calc R . . H8 H 0.7761 0.1795 0.5232 0.083 Uiso 1 1 calc R . . H9 H 0.9317 0.1495 0.5268 0.083 Uiso 1 1 calc R . . C6 C 0.5650(8) -0.0544(4) 0.3981(2) 0.0627(19) Uani 1 1 d . . . H10 H 0.4716 -0.0657 0.3733 0.094 Uiso 1 1 calc R . . H11 H 0.5372 -0.0836 0.4330 0.094 Uiso 1 1 calc R . . H12 H 0.6284 -0.0940 0.3774 0.094 Uiso 1 1 calc R . . C7 C 0.5562(7) 0.1324(5) 0.4454(2) 0.0529(15) Uani 1 1 d . . . H13 H 0.6161 0.2117 0.4570 0.079 Uiso 1 1 calc R . . H14 H 0.5231 0.1024 0.4797 0.079 Uiso 1 1 calc R . . H15 H 0.4659 0.1236 0.4195 0.079 Uiso 1 1 calc R . . C8 C 0.8327(5) 0.4371(3) 0.37796(18) 0.0242(9) Uani 1 1 d . . . C9 C 0.6744(5) 0.4139(4) 0.36898(18) 0.0277(10) Uani 1 1 d . . . C10 C 0.6019(6) 0.4820(4) 0.40079(19) 0.0325(11) Uani 1 1 d . . . H16 H 0.4940 0.4642 0.3933 0.039 Uiso 1 1 calc R . . C11 C 0.6812(6) 0.5744(4) 0.4429(2) 0.0356(11) Uani 1 1 d . . . C12 C 0.8386(6) 0.5956(4) 0.4528(2) 0.0385(12) Uani 1 1 d . . . H17 H 0.8960 0.6582 0.4815 0.046 Uiso 1 1 calc R . . C13 C 0.9167(5) 0.5294(4) 0.42260(19) 0.0308(10) Uani 1 1 d . . . C14 C 0.5775(5) 0.3199(4) 0.3227(2) 0.0322(10) Uani 1 1 d . . . H18 H 0.6070 0.3347 0.2849 0.048 Uiso 1 1 calc R . . H19 H 0.4692 0.3134 0.3249 0.048 Uiso 1 1 calc R . . H20 H 0.5929 0.2501 0.3279 0.048 Uiso 1 1 calc R . . C15 C 0.6004(7) 0.6478(5) 0.4770(2) 0.0486(14) Uani 1 1 d . . . H21 H 0.5945 0.7058 0.4562 0.073 Uiso 1 1 calc R . . H22 H 0.6580 0.6828 0.5148 0.073 Uiso 1 1 calc R . . H23 H 0.4965 0.6021 0.4820 0.073 Uiso 1 1 calc R . . C16 C 1.0861(5) 0.5597(4) 0.44010(19) 0.0330(11) Uani 1 1 d . . . H24 H 1.1444 0.5947 0.4110 0.050 Uiso 1 1 calc R . . H25 H 1.1107 0.4921 0.4434 0.050 Uiso 1 1 calc R . . H26 H 1.1133 0.6120 0.4773 0.050 Uiso 1 1 calc R . . C17 C 0.8890(4) 0.3241(3) 0.25397(16) 0.0153(8) Uani 1 1 d . . . C18 C 0.8029(4) 0.2271(3) 0.21303(16) 0.0165(8) Uani 1 1 d . . . C19 C 0.7952(4) 0.2298(3) 0.15370(17) 0.0198(8) Uani 1 1 d . . . H27 H 0.7364 0.1642 0.1271 0.024 Uiso 1 1 calc R . . C20 C 0.8699(5) 0.3244(3) 0.13285(17) 0.0202(8) Uani 1 1 d . . . C21 C 0.9540(4) 0.4179(3) 0.17295(16) 0.0181(8) Uani 1 1 d . . . H28 H 1.0071 0.4835 0.1597 0.022 Uiso 1 1 calc R . . C22 C 0.9647(4) 0.4205(3) 0.23170(16) 0.0157(8) Uani 1 1 d . . . C23 C 0.7159(4) 0.1171(3) 0.22865(16) 0.0172(8) Uani 1 1 d . . . H29 H 0.7144 0.1356 0.2713 0.021 Uiso 1 1 calc R . . Si2 Si 0.50573(14) 0.05376(10) 0.19959(5) 0.0271(3) Uani 1 1 d . . . Si3 Si 0.82959(14) 0.01558(10) 0.21741(6) 0.0292(3) Uani 1 1 d . . . C24 C 0.4173(5) 0.1601(4) 0.1849(2) 0.0361(11) Uani 1 1 d . . . H30 H 0.3236 0.1232 0.1584 0.054 Uiso 1 1 calc R . . H31 H 0.4901 0.2155 0.1674 0.054 Uiso 1 1 calc R . . H32 H 0.3920 0.1974 0.2211 0.054 Uiso 1 1 calc R . . C25 C 0.3978(5) -0.0197(4) 0.2542(2) 0.0302(10) Uani 1 1 d . . . H33 H 0.4052 0.0346 0.2898 0.045 Uiso 1 1 calc R . . H34 H 0.4420 -0.0762 0.2623 0.045 Uiso 1 1 calc R . . H35 H 0.2898 -0.0558 0.2391 0.045 Uiso 1 1 calc R . . C26 C 0.4701(6) -0.0535(4) 0.1304(2) 0.0409(12) Uani 1 1 d . . . H36 H 0.5067 -0.1146 0.1369 0.061 Uiso 1 1 calc R . . H37 H 0.5253 -0.0185 0.1006 0.061 Uiso 1 1 calc R . . H38 H 0.3600 -0.0830 0.1178 0.061 Uiso 1 1 calc R . . C27 C 1.0229(5) 0.0817(4) 0.2611(2) 0.0434(13) Uani 1 1 d . . . H39 H 1.0818 0.0297 0.2554 0.065 Uiso 1 1 calc R . . H40 H 1.0084 0.0992 0.3020 0.065 Uiso 1 1 calc R . . H41 H 1.0787 0.1505 0.2486 0.065 Uiso 1 1 calc R . . C28 C 0.7294(5) -0.1127(3) 0.2441(2) 0.0295(10) Uani 1 1 d . . . H42 H 0.6416 -0.1593 0.2165 0.044 Uiso 1 1 calc R . . H43 H 0.6934 -0.0920 0.2814 0.044 Uiso 1 1 calc R . . H44 H 0.8005 -0.1543 0.2484 0.044 Uiso 1 1 calc R . . C29 C 0.8706(6) -0.0238(4) 0.1419(2) 0.0435(13) Uani 1 1 d . . . H45 H 0.9298 0.0434 0.1287 0.065 Uiso 1 1 calc R . . H46 H 0.7738 -0.0599 0.1172 0.065 Uiso 1 1 calc R . . H47 H 0.9298 -0.0754 0.1401 0.065 Uiso 1 1 calc R . . C30 C 0.8642(5) 0.3286(3) 0.06945(17) 0.0259(9) Uani 1 1 d . . . H48 H 0.9314 0.4063 0.0692 0.031 Uiso 1 1 calc R . . Si4 Si 0.67062(15) 0.32579(11) 0.03878(5) 0.0322(3) Uani 1 1 d . . . Si5 Si 0.96842(16) 0.23881(11) 0.02757(5) 0.0341(3) Uani 1 1 d . . . C31 C 0.6084(6) 0.4292(4) 0.0886(2) 0.0478(14) Uani 1 1 d . . . H49 H 0.5155 0.4369 0.0709 0.072 Uiso 1 1 calc R . . H50 H 0.6901 0.5016 0.0964 0.072 Uiso 1 1 calc R . . H51 H 0.5869 0.4036 0.1248 0.072 Uiso 1 1 calc R . . C32 C 0.5201(5) 0.1855(4) 0.0289(2) 0.0377(11) Uani 1 1 d . . . H52 H 0.5033 0.1648 0.0665 0.057 Uiso 1 1 calc R . . H53 H 0.5541 0.1300 0.0041 0.057 Uiso 1 1 calc R . . H54 H 0.4242 0.1884 0.0110 0.057 Uiso 1 1 calc R . . C33 C 0.6882(7) 0.3659(5) -0.0339(2) 0.0549(16) Uani 1 1 d . . . H55 H 0.5930 0.3773 -0.0469 0.082 Uiso 1 1 calc R . . H56 H 0.7065 0.3063 -0.0616 0.082 Uiso 1 1 calc R . . H57 H 0.7741 0.4351 -0.0308 0.082 Uiso 1 1 calc R . . C34 C 1.1376(6) 0.2444(5) 0.0746(2) 0.0539(16) Uani 1 1 d . . . H58 H 1.1042 0.2216 0.1104 0.081 Uiso 1 1 calc R . . H59 H 1.2097 0.3207 0.0833 0.081 Uiso 1 1 calc R . . H60 H 1.1881 0.1938 0.0547 0.081 Uiso 1 1 calc R . . C35 C 0.8491(6) 0.0908(4) 0.0016(2) 0.0402(12) Uani 1 1 d . . . H61 H 0.9118 0.0491 -0.0178 0.060 Uiso 1 1 calc R . . H62 H 0.7635 0.0868 -0.0255 0.060 Uiso 1 1 calc R . . H63 H 0.8089 0.0585 0.0344 0.060 Uiso 1 1 calc R . . C36 C 1.0387(9) 0.2972(5) -0.0365(3) 0.069(2) Uani 1 1 d . . . H64 H 1.1028 0.2563 -0.0556 0.104 Uiso 1 1 calc R . . H65 H 1.0993 0.3762 -0.0242 0.104 Uiso 1 1 calc R . . H66 H 0.9509 0.2896 -0.0634 0.104 Uiso 1 1 calc R . . C37 C 1.0637(4) 0.5319(3) 0.26916(17) 0.0175(8) Uani 1 1 d . . . H67 H 1.0581 0.5210 0.3098 0.021 Uiso 1 1 calc R . . Si6 Si 0.97745(12) 0.64696(9) 0.26462(5) 0.0190(3) Uani 1 1 d . . . Si7 Si 1.27396(12) 0.56092(9) 0.25590(5) 0.0215(3) Uani 1 1 d . . . C38 C 0.7676(5) 0.5935(4) 0.2701(2) 0.0396(12) Uani 1 1 d . . . H68 H 0.7499 0.5737 0.3078 0.059 Uiso 1 1 calc R . . H69 H 0.7203 0.5273 0.2397 0.059 Uiso 1 1 calc R . . H70 H 0.7221 0.6514 0.2658 0.059 Uiso 1 1 calc R . . C39 C 0.9999(6) 0.7023(4) 0.19631(19) 0.0321(11) Uani 1 1 d . . . H71 H 0.9678 0.7688 0.2005 0.048 Uiso 1 1 calc R . . H72 H 0.9361 0.6451 0.1643 0.048 Uiso 1 1 calc R . . H73 H 1.1077 0.7220 0.1885 0.048 Uiso 1 1 calc R . . C40 C 1.0683(6) 0.7660(4) 0.3258(2) 0.0378(12) Uani 1 1 d . . . H74 H 1.0182 0.8230 0.3261 0.057 Uiso 1 1 calc R . . H75 H 1.1775 0.7983 0.3215 0.057 Uiso 1 1 calc R . . H76 H 1.0571 0.7395 0.3621 0.057 Uiso 1 1 calc R . . C41 C 1.3171(5) 0.4277(4) 0.2360(2) 0.0346(11) Uani 1 1 d . . . H77 H 1.4246 0.4439 0.2281 0.052 Uiso 1 1 calc R . . H78 H 1.2503 0.3814 0.2015 0.052 Uiso 1 1 calc R . . H79 H 1.2992 0.3877 0.2678 0.052 Uiso 1 1 calc R . . C42 C 1.3352(5) 0.6376(4) 0.1963(2) 0.0357(11) Uani 1 1 d . . . H80 H 1.4401 0.6401 0.1892 0.054 Uiso 1 1 calc R . . H81 H 1.3318 0.7138 0.2074 0.054 Uiso 1 1 calc R . . H82 H 1.2659 0.5989 0.1612 0.054 Uiso 1 1 calc R . . C43 C 1.3945(5) 0.6494(4) 0.3231(2) 0.0328(11) Uani 1 1 d . . . H83 H 1.3750 0.6084 0.3545 0.049 Uiso 1 1 calc R . . H84 H 1.3684 0.7182 0.3333 0.049 Uiso 1 1 calc R . . H85 H 1.5031 0.6681 0.3166 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0247(6) 0.0147(5) 0.0161(6) 0.0039(4) -0.0005(4) 0.0037(5) C1 0.035(3) 0.026(2) 0.040(3) 0.008(2) -0.010(2) 0.005(2) B1 0.033(3) 0.018(2) 0.022(2) 0.0007(19) -0.001(2) 0.008(2) O1 0.047(2) 0.0298(17) 0.0307(18) 0.0117(14) -0.0027(15) 0.0058(15) C2 0.070(4) 0.030(3) 0.037(3) 0.017(2) 0.007(3) 0.010(3) C3 0.063(4) 0.030(3) 0.030(3) 0.013(2) 0.006(2) -0.007(2) O2 0.057(2) 0.0278(17) 0.0221(17) 0.0098(14) 0.0009(15) -0.0053(16) C4 0.082(4) 0.059(4) 0.050(4) 0.031(3) 0.012(3) 0.037(3) C5 0.085(4) 0.039(3) 0.030(3) 0.014(2) -0.005(3) 0.002(3) C6 0.098(5) 0.035(3) 0.031(3) 0.011(2) 0.004(3) -0.014(3) C7 0.059(4) 0.060(4) 0.044(3) 0.022(3) 0.023(3) 0.016(3) C8 0.035(2) 0.019(2) 0.020(2) 0.0064(17) 0.0056(18) 0.0088(18) C9 0.037(3) 0.027(2) 0.023(2) 0.0058(18) 0.0039(19) 0.016(2) C10 0.041(3) 0.033(3) 0.028(2) 0.009(2) 0.003(2) 0.016(2) C11 0.051(3) 0.032(3) 0.029(3) 0.008(2) 0.009(2) 0.019(2) C12 0.064(4) 0.028(2) 0.022(2) 0.0035(19) 0.006(2) 0.014(2) C13 0.045(3) 0.027(2) 0.021(2) 0.0078(18) -0.001(2) 0.011(2) C14 0.033(3) 0.031(2) 0.033(3) 0.003(2) 0.004(2) 0.013(2) C15 0.068(4) 0.045(3) 0.039(3) 0.002(2) 0.005(3) 0.031(3) C16 0.046(3) 0.027(2) 0.018(2) -0.0012(18) -0.004(2) 0.004(2) C17 0.0171(19) 0.0129(18) 0.0165(19) 0.0012(15) 0.0011(15) 0.0065(15) C18 0.020(2) 0.0166(19) 0.0161(19) 0.0046(15) 0.0007(15) 0.0094(16) C19 0.020(2) 0.0175(19) 0.019(2) -0.0026(16) 0.0010(16) 0.0056(16) C20 0.025(2) 0.018(2) 0.018(2) 0.0045(16) 0.0027(17) 0.0086(17) C21 0.019(2) 0.0153(19) 0.020(2) 0.0047(16) 0.0037(16) 0.0055(16) C22 0.0153(19) 0.0155(19) 0.0168(19) 0.0025(15) 0.0000(15) 0.0064(15) C23 0.023(2) 0.0133(18) 0.015(2) 0.0011(15) 0.0028(16) 0.0072(16) Si2 0.0252(6) 0.0240(6) 0.0298(7) 0.0043(5) -0.0007(5) 0.0058(5) Si3 0.0354(7) 0.0215(6) 0.0358(7) 0.0081(5) 0.0128(6) 0.0140(5) C24 0.032(3) 0.043(3) 0.034(3) 0.007(2) 0.001(2) 0.015(2) C25 0.026(2) 0.025(2) 0.037(3) 0.008(2) 0.001(2) 0.0041(19) C26 0.047(3) 0.033(3) 0.033(3) -0.005(2) -0.007(2) 0.007(2) C27 0.033(3) 0.047(3) 0.061(4) 0.018(3) 0.010(2) 0.023(2) C28 0.033(3) 0.021(2) 0.038(3) 0.0104(19) 0.006(2) 0.0112(19) C29 0.057(3) 0.045(3) 0.044(3) 0.016(2) 0.026(3) 0.032(3) C30 0.036(2) 0.020(2) 0.016(2) 0.0022(16) -0.0003(18) 0.0006(18) Si4 0.0402(8) 0.0300(7) 0.0234(7) 0.0075(5) -0.0063(5) 0.0071(6) Si5 0.0429(8) 0.0327(7) 0.0215(7) 0.0013(5) 0.0100(6) 0.0062(6) C31 0.047(3) 0.040(3) 0.057(4) 0.009(3) -0.012(3) 0.016(3) C32 0.034(3) 0.038(3) 0.034(3) 0.001(2) -0.002(2) 0.005(2) C33 0.071(4) 0.049(3) 0.034(3) 0.020(3) -0.013(3) 0.001(3) C34 0.032(3) 0.072(4) 0.049(3) -0.010(3) 0.009(2) 0.016(3) C35 0.047(3) 0.035(3) 0.040(3) 0.001(2) 0.003(2) 0.019(2) C36 0.115(6) 0.046(3) 0.041(3) 0.007(3) 0.044(4) 0.016(4) C37 0.017(2) 0.0126(18) 0.020(2) 0.0021(15) -0.0009(16) 0.0015(15) Si6 0.0231(6) 0.0155(5) 0.0197(6) 0.0050(4) 0.0039(5) 0.0071(4) Si7 0.0183(6) 0.0164(5) 0.0276(6) 0.0025(5) 0.0027(5) 0.0035(4) C38 0.031(3) 0.035(3) 0.064(4) 0.024(3) 0.012(2) 0.020(2) C39 0.045(3) 0.032(2) 0.029(2) 0.014(2) 0.012(2) 0.021(2) C40 0.058(3) 0.028(2) 0.030(3) -0.001(2) -0.001(2) 0.022(2) C41 0.022(2) 0.027(2) 0.052(3) 0.001(2) 0.003(2) 0.0085(19) C42 0.030(3) 0.032(3) 0.044(3) 0.011(2) 0.010(2) 0.005(2) C43 0.022(2) 0.028(2) 0.040(3) -0.004(2) -0.002(2) 0.0030(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.896(5) . ? Si1 C8 1.917(4) . ? Si1 C17 1.921(4) . ? Si1 B1 2.053(5) . ? B1 O2 1.354(6) . ? B1 O1 1.373(6) . ? O1 C2 1.460(6) . ? C2 C4 1.495(8) . ? C2 C5 1.522(7) . ? C2 C3 1.535(8) . ? C3 O2 1.460(5) . ? C3 C6 1.519(7) . ? C3 C7 1.522(8) . ? C8 C9 1.395(6) . ? C8 C13 1.430(6) . ? C9 C10 1.397(6) . ? C9 C14 1.497(6) . ? C10 C11 1.386(7) . ? C11 C12 1.393(7) . ? C11 C15 1.522(7) . ? C12 C13 1.400(7) . ? C13 C16 1.509(7) . ? C17 C18 1.422(5) . ? C17 C22 1.425(5) . ? C18 C19 1.414(5) . ? C18 C23 1.514(5) . ? C19 C20 1.387(5) . ? C20 C21 1.381(5) . ? C20 C30 1.515(5) . ? C21 C22 1.387(5) . ? C22 C37 1.531(5) . ? C23 Si2 1.899(4) . ? C23 Si3 1.904(4) . ? Si2 C24 1.872(5) . ? Si2 C25 1.877(5) . ? Si2 C26 1.891(5) . ? Si3 C28 1.858(4) . ? Si3 C29 1.859(5) . ? Si3 C27 1.889(5) . ? C30 Si4 1.888(5) . ? C30 Si5 1.898(5) . ? Si4 C31 1.861(6) . ? Si4 C32 1.872(5) . ? Si4 C33 1.885(5) . ? Si5 C35 1.855(5) . ? Si5 C34 1.856(6) . ? Si5 C36 1.866(6) . ? C37 Si6 1.903(4) . ? C37 Si7 1.908(4) . ? Si6 C38 1.860(5) . ? Si6 C40 1.862(5) . ? Si6 C39 1.878(4) . ? Si7 C41 1.864(5) . ? Si7 C43 1.870(5) . ? Si7 C42 1.873(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Si1 C8 114.6(2) . . ? C1 Si1 C17 108.78(19) . . ? C8 Si1 C17 111.78(17) . . ? C1 Si1 B1 98.2(2) . . ? C8 Si1 B1 98.97(19) . . ? C17 Si1 B1 124.02(18) . . ? O2 B1 O1 111.0(4) . . ? O2 B1 Si1 132.2(3) . . ? O1 B1 Si1 116.6(3) . . ? B1 O1 C2 107.7(4) . . ? O1 C2 C4 106.3(4) . . ? O1 C2 C5 109.3(4) . . ? C4 C2 C5 110.3(5) . . ? O1 C2 C3 101.6(4) . . ? C4 C2 C3 114.5(5) . . ? C5 C2 C3 114.2(5) . . ? O2 C3 C6 108.8(4) . . ? O2 C3 C7 106.4(4) . . ? C6 C3 C7 110.1(5) . . ? O2 C3 C2 101.1(4) . . ? C6 C3 C2 115.1(5) . . ? C7 C3 C2 114.4(5) . . ? B1 O2 C3 107.7(4) . . ? C9 C8 C13 117.8(4) . . ? C9 C8 Si1 116.7(3) . . ? C13 C8 Si1 125.0(3) . . ? C8 C9 C10 120.9(4) . . ? C8 C9 C14 121.5(4) . . ? C10 C9 C14 117.5(4) . . ? C11 C10 C9 122.6(5) . . ? C10 C11 C12 116.4(4) . . ? C10 C11 C15 121.8(5) . . ? C12 C11 C15 121.8(5) . . ? C11 C12 C13 123.4(5) . . ? C12 C13 C8 118.9(4) . . ? C12 C13 C16 117.2(4) . . ? C8 C13 C16 123.8(4) . . ? C18 C17 C22 116.5(3) . . ? C18 C17 Si1 124.6(3) . . ? C22 C17 Si1 118.8(3) . . ? C19 C18 C17 120.0(3) . . ? C19 C18 C23 116.1(3) . . ? C17 C18 C23 123.9(3) . . ? C20 C19 C18 122.6(4) . . ? C21 C20 C19 116.9(4) . . ? C21 C20 C30 119.7(3) . . ? C19 C20 C30 123.4(4) . . ? C20 C21 C22 123.1(4) . . ? C21 C22 C17 120.9(3) . . ? C21 C22 C37 115.2(3) . . ? C17 C22 C37 123.9(3) . . ? C18 C23 Si2 116.5(3) . . ? C18 C23 Si3 111.2(3) . . ? Si2 C23 Si3 114.5(2) . . ? C24 Si2 C25 108.3(2) . . ? C24 Si2 C26 106.4(2) . . ? C25 Si2 C26 106.8(2) . . ? C24 Si2 C23 113.1(2) . . ? C25 Si2 C23 108.45(19) . . ? C26 Si2 C23 113.5(2) . . ? C28 Si3 C29 109.4(2) . . ? C28 Si3 C27 107.1(2) . . ? C29 Si3 C27 105.8(3) . . ? C28 Si3 C23 110.11(19) . . ? C29 Si3 C23 114.9(2) . . ? C27 Si3 C23 109.2(2) . . ? C20 C30 Si4 112.7(3) . . ? C20 C30 Si5 112.5(3) . . ? Si4 C30 Si5 119.8(2) . . ? C31 Si4 C32 109.0(2) . . ? C31 Si4 C33 109.4(3) . . ? C32 Si4 C33 107.6(2) . . ? C31 Si4 C30 108.2(2) . . ? C32 Si4 C30 113.4(2) . . ? C33 Si4 C30 109.3(2) . . ? C35 Si5 C34 108.9(3) . . ? C35 Si5 C36 107.7(3) . . ? C34 Si5 C36 108.1(3) . . ? C35 Si5 C30 114.2(2) . . ? C34 Si5 C30 108.4(2) . . ? C36 Si5 C30 109.4(2) . . ? C22 C37 Si6 111.4(3) . . ? C22 C37 Si7 110.4(3) . . ? Si6 C37 Si7 117.33(19) . . ? C38 Si6 C40 109.1(2) . . ? C38 Si6 C39 106.2(2) . . ? C40 Si6 C39 107.8(2) . . ? C38 Si6 C37 109.37(19) . . ? C40 Si6 C37 108.68(19) . . ? C39 Si6 C37 115.53(19) . . ? C41 Si7 C43 110.7(2) . . ? C41 Si7 C42 105.6(2) . . ? C43 Si7 C42 106.8(2) . . ? C41 Si7 C37 110.49(19) . . ? C43 Si7 C37 108.14(19) . . ? C42 Si7 C37 115.09(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Si1 B1 O2 -152.1(5) . . . . ? C8 Si1 B1 O2 91.3(5) . . . . ? C17 Si1 B1 O2 -32.8(5) . . . . ? C1 Si1 B1 O1 34.2(4) . . . . ? C8 Si1 B1 O1 -82.4(4) . . . . ? C17 Si1 B1 O1 153.5(3) . . . . ? O2 B1 O1 C2 6.8(5) . . . . ? Si1 B1 O1 C2 -178.2(3) . . . . ? B1 O1 C2 C4 95.7(5) . . . . ? B1 O1 C2 C5 -145.3(5) . . . . ? B1 O1 C2 C3 -24.3(5) . . . . ? O1 C2 C3 O2 31.5(5) . . . . ? C4 C2 C3 O2 -82.5(5) . . . . ? C5 C2 C3 O2 149.0(4) . . . . ? O1 C2 C3 C6 148.6(4) . . . . ? C4 C2 C3 C6 34.6(6) . . . . ? C5 C2 C3 C6 -93.9(6) . . . . ? O1 C2 C3 C7 -82.3(5) . . . . ? C4 C2 C3 C7 163.7(4) . . . . ? C5 C2 C3 C7 35.2(6) . . . . ? O1 B1 O2 C3 15.2(5) . . . . ? Si1 B1 O2 C3 -158.7(4) . . . . ? C6 C3 O2 B1 -150.8(5) . . . . ? C7 C3 O2 B1 90.5(5) . . . . ? C2 C3 O2 B1 -29.2(5) . . . . ? C1 Si1 C8 C9 -171.3(3) . . . . ? C17 Si1 C8 C9 64.4(3) . . . . ? B1 Si1 C8 C9 -67.9(3) . . . . ? C1 Si1 C8 C13 0.8(4) . . . . ? C17 Si1 C8 C13 -123.5(4) . . . . ? B1 Si1 C8 C13 104.2(4) . . . . ? C13 C8 C9 C10 3.0(6) . . . . ? Si1 C8 C9 C10 175.7(3) . . . . ? C13 C8 C9 C14 179.1(4) . . . . ? Si1 C8 C9 C14 -8.1(5) . . . . ? C8 C9 C10 C11 -0.6(7) . . . . ? C14 C9 C10 C11 -176.9(4) . . . . ? C9 C10 C11 C12 -1.0(7) . . . . ? C9 C10 C11 C15 179.9(4) . . . . ? C10 C11 C12 C13 0.3(7) . . . . ? C15 C11 C12 C13 179.4(4) . . . . ? C11 C12 C13 C8 2.0(7) . . . . ? C11 C12 C13 C16 -177.2(4) . . . . ? C9 C8 C13 C12 -3.6(6) . . . . ? Si1 C8 C13 C12 -175.7(3) . . . . ? C9 C8 C13 C16 175.6(4) . . . . ? Si1 C8 C13 C16 3.5(6) . . . . ? C1 Si1 C17 C18 114.0(3) . . . . ? C8 Si1 C17 C18 -118.5(3) . . . . ? B1 Si1 C17 C18 -0.3(4) . . . . ? C1 Si1 C17 C22 -63.3(3) . . . . ? C8 Si1 C17 C22 64.2(3) . . . . ? B1 Si1 C17 C22 -177.6(3) . . . . ? C22 C17 C18 C19 -0.3(5) . . . . ? Si1 C17 C18 C19 -177.7(3) . . . . ? C22 C17 C18 C23 179.7(3) . . . . ? Si1 C17 C18 C23 2.2(5) . . . . ? C17 C18 C19 C20 0.5(6) . . . . ? C23 C18 C19 C20 -179.5(3) . . . . ? C18 C19 C20 C21 0.0(6) . . . . ? C18 C19 C20 C30 179.4(4) . . . . ? C19 C20 C21 C22 -0.6(6) . . . . ? C30 C20 C21 C22 180.0(4) . . . . ? C20 C21 C22 C17 0.8(6) . . . . ? C20 C21 C22 C37 179.9(3) . . . . ? C18 C17 C22 C21 -0.3(5) . . . . ? Si1 C17 C22 C21 177.3(3) . . . . ? C18 C17 C22 C37 -179.4(3) . . . . ? Si1 C17 C22 C37 -1.8(5) . . . . ? C19 C18 C23 Si2 -53.0(4) . . . . ? C17 C18 C23 Si2 127.0(3) . . . . ? C19 C18 C23 Si3 80.5(4) . . . . ? C17 C18 C23 Si3 -99.4(4) . . . . ? C18 C23 Si2 C24 -25.5(4) . . . . ? Si3 C23 Si2 C24 -157.6(2) . . . . ? C18 C23 Si2 C25 -145.6(3) . . . . ? Si3 C23 Si2 C25 82.3(2) . . . . ? C18 C23 Si2 C26 95.8(3) . . . . ? Si3 C23 Si2 C26 -36.2(3) . . . . ? C18 C23 Si3 C28 174.1(3) . . . . ? Si2 C23 Si3 C28 -51.3(3) . . . . ? C18 C23 Si3 C29 -61.9(3) . . . . ? Si2 C23 Si3 C29 72.7(3) . . . . ? C18 C23 Si3 C27 56.7(3) . . . . ? Si2 C23 Si3 C27 -168.7(2) . . . . ? C21 C20 C30 Si4 -109.3(4) . . . . ? C19 C20 C30 Si4 71.3(4) . . . . ? C21 C20 C30 Si5 111.5(4) . . . . ? C19 C20 C30 Si5 -67.9(5) . . . . ? C20 C30 Si4 C31 47.5(4) . . . . ? Si5 C30 Si4 C31 -176.6(3) . . . . ? C20 C30 Si4 C32 -73.5(3) . . . . ? Si5 C30 Si4 C32 62.4(3) . . . . ? C20 C30 Si4 C33 166.5(3) . . . . ? Si5 C30 Si4 C33 -57.7(3) . . . . ? C20 C30 Si5 C35 86.4(3) . . . . ? Si4 C30 Si5 C35 -49.6(3) . . . . ? C20 C30 Si5 C34 -35.2(4) . . . . ? Si4 C30 Si5 C34 -171.1(3) . . . . ? C20 C30 Si5 C36 -152.8(3) . . . . ? Si4 C30 Si5 C36 71.2(3) . . . . ? C21 C22 C37 Si6 64.7(4) . . . . ? C17 C22 C37 Si6 -116.2(3) . . . . ? C21 C22 C37 Si7 -67.5(4) . . . . ? C17 C22 C37 Si7 111.6(3) . . . . ? C22 C37 Si6 C38 44.6(3) . . . . ? Si7 C37 Si6 C38 173.2(2) . . . . ? C22 C37 Si6 C40 163.6(3) . . . . ? Si7 C37 Si6 C40 -67.8(3) . . . . ? C22 C37 Si6 C39 -75.1(3) . . . . ? Si7 C37 Si6 C39 53.5(3) . . . . ? C22 C37 Si7 C41 -30.5(3) . . . . ? Si6 C37 Si7 C41 -159.5(2) . . . . ? C22 C37 Si7 C43 -151.8(3) . . . . ? Si6 C37 Si7 C43 79.2(3) . . . . ? C22 C37 Si7 C42 89.0(3) . . . . ? Si6 C37 Si7 C42 -40.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.785 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.088 #===END data_sihme #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Norihiro Tokitoh' _publ_contact_author_email 'tokitoh@boc.kuicr.kyoto-u.ac.jp' _publ_contact_author_fax '+81-774-38-3209' _publ_contact_author_phone '+81-774-38-3200' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Organometallics' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Borylsilyl Anions Utilizing Overcrowded Silylboranes and Their Properties ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Takashi Kajiwara' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Nobuhiro Takeda' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Takahiro Sasamori' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Norihiro Tokitoh' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; _publ_section_synopsis ; ; #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common SiHMe _chemical_melting_point ? _chemical_formula_moiety 'C37 H74 Si7' _chemical_formula_sum 'C37 H74 Si7' _chemical_formula_weight 715.59 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 11.384(4) _cell_length_b 13.277(5) _cell_length_c 15.422(5) _cell_angle_alpha 79.505(9) _cell_angle_beta 80.473(9) _cell_angle_gamma 87.062(9) _cell_volume 2259.9(14) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9123 _exptl_absorpt_correction_T_max 0.9547 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14864 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7801 _reflns_number_gt 6321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalClear' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0950P)^2^+6.1803P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7801 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.2045 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Si1 Si 0.77786(13) 0.04440(10) 0.37917(9) 0.0360(3) Uani 1 1 d . . . H1 H 0.6609 -0.0056 0.4047 0.043 Uiso 1 1 calc R . . C1 C 0.8391(5) 0.0371(4) 0.4848(3) 0.0470(14) Uani 1 1 d . . . H1 H 0.9219 0.0594 0.4710 0.070 Uiso 1 1 calc R . . H2 H 0.8360 -0.0337 0.5172 0.070 Uiso 1 1 calc R . . H3 H 0.7915 0.0818 0.5219 0.070 Uiso 1 1 calc R . . C2 C 0.8814(4) -0.0469(3) 0.3150(3) 0.0293(10) Uani 1 1 d . . . C3 C 0.8473(4) -0.1488(3) 0.3217(3) 0.0293(10) Uani 1 1 d . . . C4 C 0.9230(4) -0.2162(3) 0.2793(3) 0.0295(10) Uani 1 1 d . . . H4 H 0.8990 -0.2848 0.2848 0.035 Uiso 1 1 calc R . . C5 C 1.0321(4) -0.1873(4) 0.2293(3) 0.0330(11) Uani 1 1 d . . . C6 C 1.0663(4) -0.0864(4) 0.2253(4) 0.0407(12) Uani 1 1 d . . . H5 H 1.1416 -0.0643 0.1927 0.049 Uiso 1 1 calc R . . C7 C 0.9918(4) -0.0181(3) 0.2682(3) 0.0368(12) Uani 1 1 d . . . C8 C 0.7305(4) -0.1897(4) 0.3749(4) 0.0417(12) Uani 1 1 d . . . H6 H 0.7263 -0.2628 0.3731 0.063 Uiso 1 1 calc R . . H7 H 0.6643 -0.1526 0.3490 0.063 Uiso 1 1 calc R . . H8 H 0.7253 -0.1802 0.4369 0.063 Uiso 1 1 calc R . . C9 C 1.1125(5) -0.2612(4) 0.1821(4) 0.0496(14) Uani 1 1 d . . . H9 H 1.1022 -0.3306 0.2167 0.074 Uiso 1 1 calc R . . H10 H 1.1956 -0.2414 0.1762 0.074 Uiso 1 1 calc R . . H11 H 1.0918 -0.2594 0.1226 0.074 Uiso 1 1 calc R . . C10 C 1.0355(5) 0.0886(4) 0.2649(4) 0.0514(15) Uani 1 1 d . . . H12 H 1.0677 0.0910 0.3196 0.077 Uiso 1 1 calc R . . H13 H 0.9691 0.1381 0.2599 0.077 Uiso 1 1 calc R . . H14 H 1.0980 0.1057 0.2130 0.077 Uiso 1 1 calc R . . C11 C 0.7502(4) 0.1730(3) 0.3056(3) 0.0222(9) Uani 1 1 d . . . C12 C 0.6878(4) 0.1703(3) 0.2332(3) 0.0216(9) Uani 1 1 d . . . C13 C 0.6540(4) 0.2613(3) 0.1819(3) 0.0204(8) Uani 1 1 d . . . H15 H 0.6149 0.2574 0.1327 0.025 Uiso 1 1 calc R . . C14 C 0.6746(3) 0.3578(3) 0.1990(3) 0.0190(8) Uani 1 1 d . . . C15 C 0.7360(3) 0.3601(3) 0.2696(3) 0.0200(8) Uani 1 1 d . . . H16 H 0.7526 0.4247 0.2825 0.024 Uiso 1 1 calc R . . C16 C 0.7741(3) 0.2713(3) 0.3222(3) 0.0176(8) Uani 1 1 d . . . C17 C 0.6508(4) 0.0708(3) 0.2099(3) 0.0256(9) Uani 1 1 d . . . H17 H 0.6844 0.0152 0.2524 0.031 Uiso 1 1 calc R . . Si2 Si 0.72348(12) 0.04840(9) 0.09443(8) 0.0296(3) Uani 1 1 d . . . Si3 Si 0.48237(13) 0.05766(10) 0.24058(10) 0.0393(4) Uani 1 1 d . . . C18 C 0.7355(6) -0.0933(4) 0.0961(4) 0.0550(16) Uani 1 1 d . . . H18 H 0.7757 -0.1065 0.0379 0.082 Uiso 1 1 calc R . . H19 H 0.6556 -0.1220 0.1088 0.082 Uiso 1 1 calc R . . H20 H 0.7815 -0.1255 0.1426 0.082 Uiso 1 1 calc R . . C19 C 0.8750(5) 0.1030(4) 0.0656(4) 0.0438(13) Uani 1 1 d . . . H21 H 0.9103 0.0929 0.0053 0.066 Uiso 1 1 calc R . . H22 H 0.9250 0.0684 0.1085 0.066 Uiso 1 1 calc R . . H23 H 0.8695 0.1764 0.0677 0.066 Uiso 1 1 calc R . . C20 C 0.6373(5) 0.1053(4) 0.0031(3) 0.0448(13) Uani 1 1 d . . . H24 H 0.6258 0.1792 0.0022 0.067 Uiso 1 1 calc R . . H25 H 0.5595 0.0730 0.0138 0.067 Uiso 1 1 calc R . . H26 H 0.6814 0.0936 -0.0545 0.067 Uiso 1 1 calc R . . C21 C 0.4411(5) -0.0766(4) 0.2397(4) 0.0507(15) Uani 1 1 d . . . H27 H 0.3564 -0.0859 0.2639 0.076 Uiso 1 1 calc R . . H28 H 0.4890 -0.1246 0.2765 0.076 Uiso 1 1 calc R . . H29 H 0.4563 -0.0897 0.1783 0.076 Uiso 1 1 calc R . . C22 C 0.4326(6) 0.0874(6) 0.3552(5) 0.082(2) Uani 1 1 d . . . H30 H 0.4534 0.1578 0.3563 0.122 Uiso 1 1 calc R . . H31 H 0.4722 0.0399 0.3983 0.122 Uiso 1 1 calc R . . H32 H 0.3461 0.0800 0.3711 0.122 Uiso 1 1 calc R . . C23 C 0.3952(5) 0.1457(5) 0.1666(6) 0.079(2) Uani 1 1 d . . . H33 H 0.3100 0.1383 0.1899 0.118 Uiso 1 1 calc R . . H34 H 0.4116 0.1291 0.1063 0.118 Uiso 1 1 calc R . . H35 H 0.4178 0.2165 0.1644 0.118 Uiso 1 1 calc R . . C24 C 0.6296(4) 0.4531(3) 0.1438(3) 0.0225(9) Uani 1 1 d . . . H36 H 0.5888 0.4259 0.1005 0.027 Uiso 1 1 calc R . . Si4 Si 0.50627(11) 0.52465(9) 0.20725(8) 0.0272(3) Uani 1 1 d . . . Si5 Si 0.75532(11) 0.53013(9) 0.06963(8) 0.0251(3) Uani 1 1 d . . . C25 C 0.4149(4) 0.4307(4) 0.2929(4) 0.0429(13) Uani 1 1 d . . . H37 H 0.3497 0.4670 0.3253 0.064 Uiso 1 1 calc R . . H38 H 0.4650 0.3941 0.3350 0.064 Uiso 1 1 calc R . . H39 H 0.3819 0.3816 0.2636 0.064 Uiso 1 1 calc R . . C26 C 0.5606(5) 0.6229(4) 0.2622(3) 0.0365(11) Uani 1 1 d . . . H40 H 0.5970 0.6786 0.2165 0.055 Uiso 1 1 calc R . . H41 H 0.6198 0.5915 0.2989 0.055 Uiso 1 1 calc R . . H42 H 0.4934 0.6504 0.3002 0.055 Uiso 1 1 calc R . . C27 C 0.4102(5) 0.5927(5) 0.1272(4) 0.0525(15) Uani 1 1 d . . . H43 H 0.3355 0.6151 0.1605 0.079 Uiso 1 1 calc R . . H44 H 0.3929 0.5463 0.0885 0.079 Uiso 1 1 calc R . . H45 H 0.4518 0.6526 0.0907 0.079 Uiso 1 1 calc R . . C28 C 0.8501(4) 0.4397(4) 0.0069(3) 0.0321(10) Uani 1 1 d . . . H46 H 0.7995 0.4004 -0.0198 0.048 Uiso 1 1 calc R . . H47 H 0.8933 0.3926 0.0479 0.048 Uiso 1 1 calc R . . H48 H 0.9072 0.4785 -0.0404 0.048 Uiso 1 1 calc R . . C29 C 0.8485(4) 0.5926(4) 0.1327(3) 0.0337(11) Uani 1 1 d . . . H49 H 0.9099 0.6330 0.0906 0.051 Uiso 1 1 calc R . . H50 H 0.8865 0.5399 0.1729 0.051 Uiso 1 1 calc R . . H51 H 0.7980 0.6376 0.1677 0.051 Uiso 1 1 calc R . . C30 C 0.6950(5) 0.6342(4) -0.0107(3) 0.0427(13) Uani 1 1 d . . . H52 H 0.7605 0.6647 -0.0559 0.064 Uiso 1 1 calc R . . H53 H 0.6554 0.6870 0.0215 0.064 Uiso 1 1 calc R . . H54 H 0.6375 0.6057 -0.0399 0.064 Uiso 1 1 calc R . . C31 C 0.8369(4) 0.2855(3) 0.3988(3) 0.0204(8) Uani 1 1 d . . . H55 H 0.8641 0.2145 0.4226 0.025 Uiso 1 1 calc R . . Si6 Si 0.72433(11) 0.32011(9) 0.49431(8) 0.0262(3) Uani 1 1 d . . . Si7 Si 0.98053(10) 0.35971(8) 0.36596(8) 0.0230(3) Uani 1 1 d . . . C32 C 0.5907(4) 0.2380(4) 0.5120(3) 0.0384(12) Uani 1 1 d . . . H56 H 0.5317 0.2573 0.5604 0.058 Uiso 1 1 calc R . . H57 H 0.6145 0.1659 0.5279 0.058 Uiso 1 1 calc R . . H58 H 0.5559 0.2479 0.4569 0.058 Uiso 1 1 calc R . . C33 C 0.6655(5) 0.4549(4) 0.4762(3) 0.0430(13) Uani 1 1 d . . . H59 H 0.6297 0.4683 0.4216 0.065 Uiso 1 1 calc R . . H60 H 0.7309 0.5021 0.4704 0.065 Uiso 1 1 calc R . . H61 H 0.6051 0.4651 0.5273 0.065 Uiso 1 1 calc R . . C34 C 0.7929(4) 0.2975(4) 0.5981(3) 0.0364(11) Uani 1 1 d . . . H62 H 0.8556 0.3472 0.5924 0.055 Uiso 1 1 calc R . . H63 H 0.8274 0.2279 0.6071 0.055 Uiso 1 1 calc R . . H64 H 0.7317 0.3054 0.6493 0.055 Uiso 1 1 calc R . . C35 C 1.0502(4) 0.3564(3) 0.2480(3) 0.0310(10) Uani 1 1 d . . . H65 H 0.9890 0.3698 0.2093 0.046 Uiso 1 1 calc R . . H66 H 1.0872 0.2887 0.2440 0.046 Uiso 1 1 calc R . . H67 H 1.1111 0.4088 0.2287 0.046 Uiso 1 1 calc R . . C36 C 0.9603(5) 0.4975(3) 0.3768(3) 0.0362(11) Uani 1 1 d . . . H68 H 0.9352 0.5028 0.4398 0.054 Uiso 1 1 calc R . . H69 H 0.8993 0.5294 0.3420 0.054 Uiso 1 1 calc R . . H70 H 1.0358 0.5327 0.3543 0.054 Uiso 1 1 calc R . . C37 C 1.0872(4) 0.2985(4) 0.4411(3) 0.0372(11) Uani 1 1 d . . . H71 H 1.1625 0.3350 0.4251 0.056 Uiso 1 1 calc R . . H72 H 1.1017 0.2268 0.4342 0.056 Uiso 1 1 calc R . . H73 H 1.0532 0.3017 0.5032 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0512(9) 0.0260(7) 0.0326(7) -0.0060(5) -0.0131(6) 0.0061(6) C1 0.075(4) 0.029(3) 0.032(3) 0.002(2) -0.007(3) 0.008(3) C2 0.036(3) 0.022(2) 0.036(3) -0.0071(18) -0.022(2) 0.0053(18) C3 0.036(3) 0.021(2) 0.034(2) -0.0053(18) -0.018(2) 0.0044(18) C4 0.040(3) 0.017(2) 0.036(3) -0.0052(18) -0.020(2) 0.0020(18) C5 0.040(3) 0.031(2) 0.029(2) -0.0042(19) -0.013(2) 0.013(2) C6 0.029(3) 0.044(3) 0.046(3) 0.007(2) -0.013(2) -0.002(2) C7 0.039(3) 0.025(2) 0.051(3) -0.004(2) -0.025(2) 0.003(2) C8 0.040(3) 0.039(3) 0.046(3) -0.004(2) -0.013(2) 0.004(2) C9 0.060(4) 0.050(3) 0.039(3) -0.009(2) -0.012(3) 0.025(3) C10 0.045(3) 0.032(3) 0.081(4) -0.009(3) -0.020(3) -0.006(2) C11 0.032(2) 0.018(2) 0.017(2) -0.0034(16) -0.0074(17) 0.0058(17) C12 0.025(2) 0.0169(19) 0.024(2) -0.0060(16) -0.0075(17) 0.0000(16) C13 0.025(2) 0.019(2) 0.019(2) -0.0083(16) -0.0059(17) -0.0010(16) C14 0.0143(19) 0.024(2) 0.018(2) -0.0050(16) 0.0000(16) 0.0004(15) C15 0.023(2) 0.0188(19) 0.019(2) -0.0079(16) -0.0027(17) -0.0006(16) C16 0.0145(19) 0.021(2) 0.0172(19) -0.0051(16) -0.0010(16) 0.0005(15) C17 0.036(2) 0.016(2) 0.028(2) -0.0049(17) -0.0131(19) -0.0015(17) Si2 0.0455(8) 0.0204(6) 0.0280(7) -0.0090(5) -0.0164(6) 0.0012(5) Si3 0.0439(8) 0.0248(7) 0.0479(8) 0.0000(6) -0.0077(7) -0.0103(6) C18 0.098(5) 0.027(3) 0.045(3) -0.018(2) -0.016(3) 0.008(3) C19 0.044(3) 0.048(3) 0.044(3) -0.018(2) -0.013(2) 0.004(2) C20 0.063(4) 0.042(3) 0.035(3) -0.007(2) -0.025(3) -0.002(3) C21 0.065(4) 0.034(3) 0.059(4) 0.001(2) -0.031(3) -0.019(3) C22 0.066(5) 0.095(6) 0.088(5) -0.049(5) 0.021(4) -0.036(4) C23 0.037(3) 0.057(4) 0.123(6) 0.038(4) -0.018(4) -0.002(3) C24 0.029(2) 0.018(2) 0.023(2) -0.0061(16) -0.0098(18) 0.0020(16) Si4 0.0274(6) 0.0244(6) 0.0328(7) -0.0118(5) -0.0086(5) 0.0083(5) Si5 0.0332(7) 0.0194(6) 0.0221(6) -0.0020(5) -0.0053(5) 0.0004(5) C25 0.034(3) 0.040(3) 0.054(3) -0.019(2) 0.007(2) -0.001(2) C26 0.047(3) 0.028(2) 0.036(3) -0.015(2) -0.004(2) 0.004(2) C27 0.049(3) 0.056(4) 0.059(4) -0.021(3) -0.026(3) 0.031(3) C28 0.033(3) 0.037(3) 0.026(2) -0.009(2) -0.001(2) -0.001(2) C29 0.037(3) 0.029(2) 0.034(3) -0.007(2) -0.002(2) -0.007(2) C30 0.063(4) 0.031(3) 0.033(3) 0.004(2) -0.014(2) 0.005(2) C31 0.025(2) 0.0185(19) 0.019(2) -0.0030(16) -0.0070(17) -0.0007(16) Si6 0.0292(7) 0.0321(7) 0.0191(6) -0.0090(5) -0.0042(5) -0.0008(5) Si7 0.0266(6) 0.0192(6) 0.0246(6) -0.0029(5) -0.0079(5) -0.0031(4) C32 0.033(3) 0.057(3) 0.028(2) -0.017(2) 0.000(2) -0.007(2) C33 0.050(3) 0.042(3) 0.036(3) -0.013(2) -0.002(2) 0.015(2) C34 0.040(3) 0.049(3) 0.022(2) -0.011(2) -0.006(2) -0.003(2) C35 0.034(3) 0.025(2) 0.033(3) -0.0054(19) 0.000(2) -0.0086(19) C36 0.053(3) 0.023(2) 0.037(3) -0.0076(19) -0.014(2) -0.007(2) C37 0.032(3) 0.038(3) 0.043(3) -0.001(2) -0.016(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.860(5) . ? Si1 C11 1.914(4) . ? Si1 C2 1.934(5) . ? C2 C7 1.377(7) . ? C2 C3 1.408(6) . ? C3 C4 1.385(6) . ? C3 C8 1.512(7) . ? C4 C5 1.381(7) . ? C5 C6 1.403(7) . ? C5 C9 1.509(7) . ? C6 C7 1.390(7) . ? C7 C10 1.515(7) . ? C11 C16 1.422(5) . ? C11 C12 1.426(5) . ? C12 C13 1.392(6) . ? C12 C17 1.527(5) . ? C13 C14 1.395(5) . ? C14 C15 1.392(5) . ? C14 C24 1.509(5) . ? C15 C16 1.398(5) . ? C16 C31 1.523(5) . ? C17 Si2 1.904(4) . ? C17 Si3 1.906(5) . ? Si2 C19 1.858(5) . ? Si2 C20 1.875(5) . ? Si2 C18 1.875(5) . ? Si3 C23 1.850(6) . ? Si3 C21 1.870(5) . ? Si3 C22 1.871(7) . ? C24 Si4 1.891(4) . ? C24 Si5 1.893(4) . ? Si4 C25 1.860(5) . ? Si4 C26 1.861(5) . ? Si4 C27 1.864(5) . ? Si5 C30 1.865(5) . ? Si5 C29 1.866(5) . ? Si5 C28 1.868(5) . ? C31 Si6 1.893(4) . ? C31 Si7 1.900(4) . ? Si6 C34 1.864(5) . ? Si6 C33 1.867(5) . ? Si6 C32 1.871(5) . ? Si7 C36 1.866(5) . ? Si7 C35 1.868(5) . ? Si7 C37 1.870(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Si1 C11 121.5(2) . . ? C1 Si1 C2 103.8(2) . . ? C11 Si1 C2 112.60(19) . . ? C7 C2 C3 118.3(4) . . ? C7 C2 Si1 122.3(3) . . ? C3 C2 Si1 119.2(4) . . ? C4 C3 C2 119.8(4) . . ? C4 C3 C8 117.5(4) . . ? C2 C3 C8 122.7(4) . . ? C5 C4 C3 122.5(4) . . ? C4 C5 C6 117.1(4) . . ? C4 C5 C9 121.8(5) . . ? C6 C5 C9 121.1(5) . . ? C7 C6 C5 121.0(5) . . ? C2 C7 C6 121.2(4) . . ? C2 C7 C10 120.0(5) . . ? C6 C7 C10 118.8(5) . . ? C16 C11 C12 117.1(3) . . ? C16 C11 Si1 126.0(3) . . ? C12 C11 Si1 116.6(3) . . ? C13 C12 C11 120.0(4) . . ? C13 C12 C17 116.9(3) . . ? C11 C12 C17 123.1(4) . . ? C12 C13 C14 123.2(4) . . ? C15 C14 C13 116.5(4) . . ? C15 C14 C24 123.1(4) . . ? C13 C14 C24 120.4(4) . . ? C14 C15 C16 122.7(4) . . ? C15 C16 C11 120.5(3) . . ? C15 C16 C31 116.9(3) . . ? C11 C16 C31 122.6(3) . . ? C12 C17 Si2 113.5(3) . . ? C12 C17 Si3 109.7(3) . . ? Si2 C17 Si3 117.8(2) . . ? C19 Si2 C20 107.8(3) . . ? C19 Si2 C18 109.2(3) . . ? C20 Si2 C18 107.3(3) . . ? C19 Si2 C17 110.3(2) . . ? C20 Si2 C17 113.9(2) . . ? C18 Si2 C17 108.2(2) . . ? C23 Si3 C21 108.2(3) . . ? C23 Si3 C22 105.7(4) . . ? C21 Si3 C22 108.8(3) . . ? C23 Si3 C17 114.7(2) . . ? C21 Si3 C17 109.7(2) . . ? C22 Si3 C17 109.5(3) . . ? C14 C24 Si4 114.1(3) . . ? C14 C24 Si5 112.1(3) . . ? Si4 C24 Si5 118.0(2) . . ? C25 Si4 C26 109.4(2) . . ? C25 Si4 C27 109.0(3) . . ? C26 Si4 C27 107.1(2) . . ? C25 Si4 C24 108.9(2) . . ? C26 Si4 C24 113.8(2) . . ? C27 Si4 C24 108.6(2) . . ? C30 Si5 C29 106.9(2) . . ? C30 Si5 C28 109.6(2) . . ? C29 Si5 C28 109.6(2) . . ? C30 Si5 C24 110.4(2) . . ? C29 Si5 C24 113.5(2) . . ? C28 Si5 C24 106.9(2) . . ? C16 C31 Si6 110.0(3) . . ? C16 C31 Si7 115.9(3) . . ? Si6 C31 Si7 118.0(2) . . ? C34 Si6 C33 108.4(2) . . ? C34 Si6 C32 109.2(2) . . ? C33 Si6 C32 105.4(3) . . ? C34 Si6 C31 109.2(2) . . ? C33 Si6 C31 114.9(2) . . ? C32 Si6 C31 109.6(2) . . ? C36 Si7 C35 106.8(2) . . ? C36 Si7 C37 108.3(2) . . ? C35 Si7 C37 108.3(2) . . ? C36 Si7 C31 113.4(2) . . ? C35 Si7 C31 112.01(19) . . ? C37 Si7 C31 107.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Si1 C2 C7 -79.6(4) . . . . ? C11 Si1 C2 C7 53.7(4) . . . . ? C1 Si1 C2 C3 95.4(4) . . . . ? C11 Si1 C2 C3 -131.3(3) . . . . ? C7 C2 C3 C4 -1.9(6) . . . . ? Si1 C2 C3 C4 -177.2(3) . . . . ? C7 C2 C3 C8 177.2(4) . . . . ? Si1 C2 C3 C8 2.0(6) . . . . ? C2 C3 C4 C5 -0.5(7) . . . . ? C8 C3 C4 C5 -179.7(4) . . . . ? C3 C4 C5 C6 2.2(7) . . . . ? C3 C4 C5 C9 -178.8(4) . . . . ? C4 C5 C6 C7 -1.5(7) . . . . ? C9 C5 C6 C7 179.5(4) . . . . ? C3 C2 C7 C6 2.6(7) . . . . ? Si1 C2 C7 C6 177.7(4) . . . . ? C3 C2 C7 C10 -175.7(4) . . . . ? Si1 C2 C7 C10 -0.6(6) . . . . ? C5 C6 C7 C2 -0.9(7) . . . . ? C5 C6 C7 C10 177.4(5) . . . . ? C1 Si1 C11 C16 1.1(5) . . . . ? C2 Si1 C11 C16 -122.9(4) . . . . ? C1 Si1 C11 C12 -171.4(3) . . . . ? C2 Si1 C11 C12 64.6(4) . . . . ? C16 C11 C12 C13 0.6(6) . . . . ? Si1 C11 C12 C13 173.8(3) . . . . ? C16 C11 C12 C17 -177.1(4) . . . . ? Si1 C11 C12 C17 -3.9(5) . . . . ? C11 C12 C13 C14 -2.2(6) . . . . ? C17 C12 C13 C14 175.7(4) . . . . ? C12 C13 C14 C15 2.3(6) . . . . ? C12 C13 C14 C24 -176.6(4) . . . . ? C13 C14 C15 C16 -1.0(6) . . . . ? C24 C14 C15 C16 177.9(4) . . . . ? C14 C15 C16 C11 -0.5(6) . . . . ? C14 C15 C16 C31 -178.2(3) . . . . ? C12 C11 C16 C15 0.7(6) . . . . ? Si1 C11 C16 C15 -171.8(3) . . . . ? C12 C11 C16 C31 178.3(4) . . . . ? Si1 C11 C16 C31 5.8(6) . . . . ? C13 C12 C17 Si2 64.9(4) . . . . ? C11 C12 C17 Si2 -117.4(4) . . . . ? C13 C12 C17 Si3 -69.2(4) . . . . ? C11 C12 C17 Si3 108.6(4) . . . . ? C12 C17 Si2 C19 32.5(4) . . . . ? Si3 C17 Si2 C19 162.6(2) . . . . ? C12 C17 Si2 C20 -88.9(3) . . . . ? Si3 C17 Si2 C20 41.2(3) . . . . ? C12 C17 Si2 C18 151.9(3) . . . . ? Si3 C17 Si2 C18 -78.0(3) . . . . ? C12 C17 Si3 C23 72.2(4) . . . . ? Si2 C17 Si3 C23 -59.6(4) . . . . ? C12 C17 Si3 C21 -165.8(3) . . . . ? Si2 C17 Si3 C21 62.4(3) . . . . ? C12 C17 Si3 C22 -46.4(4) . . . . ? Si2 C17 Si3 C22 -178.2(3) . . . . ? C15 C14 C24 Si4 -67.0(5) . . . . ? C13 C14 C24 Si4 111.9(4) . . . . ? C15 C14 C24 Si5 70.3(4) . . . . ? C13 C14 C24 Si5 -110.8(4) . . . . ? C14 C24 Si4 C25 -32.5(4) . . . . ? Si5 C24 Si4 C25 -167.2(2) . . . . ? C14 C24 Si4 C26 89.7(3) . . . . ? Si5 C24 Si4 C26 -45.0(3) . . . . ? C14 C24 Si4 C27 -151.1(3) . . . . ? Si5 C24 Si4 C27 74.2(3) . . . . ? C14 C24 Si5 C30 170.4(3) . . . . ? Si4 C24 Si5 C30 -54.0(3) . . . . ? C14 C24 Si5 C29 -69.6(3) . . . . ? Si4 C24 Si5 C29 66.0(3) . . . . ? C14 C24 Si5 C28 51.3(3) . . . . ? Si4 C24 Si5 C28 -173.1(2) . . . . ? C15 C16 C31 Si6 75.9(4) . . . . ? C11 C16 C31 Si6 -101.8(4) . . . . ? C15 C16 C31 Si7 -61.2(4) . . . . ? C11 C16 C31 Si7 121.2(4) . . . . ? C16 C31 Si6 C34 162.5(3) . . . . ? Si7 C31 Si6 C34 -61.5(3) . . . . ? C16 C31 Si6 C33 -75.4(3) . . . . ? Si7 C31 Si6 C33 60.6(3) . . . . ? C16 C31 Si6 C32 43.0(3) . . . . ? Si7 C31 Si6 C32 179.0(2) . . . . ? C16 C31 Si7 C36 97.9(3) . . . . ? Si6 C31 Si7 C36 -35.6(3) . . . . ? C16 C31 Si7 C35 -23.1(4) . . . . ? Si6 C31 Si7 C35 -156.6(2) . . . . ? C16 C31 Si7 C37 -142.1(3) . . . . ? Si6 C31 Si7 C37 84.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 3.997 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.091 #===END data_sibpinoh #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Norihiro Tokitoh' _publ_contact_author_email 'tokitoh@boc.kuicr.kyoto-u.ac.jp' _publ_contact_author_fax '+81-774-38-3209' _publ_contact_author_phone '+81-774-38-3200' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Organometallics' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Borylsilyl Anions Utilizing Overcrowded Silylboranes and Their Properties ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Takashi Kajiwara' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Nobuhiro Takeda' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Takahiro Sasamori' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; 'Norihiro Tokitoh' ; ; ; Institute for Chemical Research, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan ; _publ_section_synopsis ; ; #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common SiBpinOH _chemical_melting_point ? _chemical_formula_moiety 'C42 H83 B O2 Si7' _chemical_formula_sum 'C42 H83 B O2 Si7' _chemical_formula_weight 827.52 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' 'B' 'B' 0.0013 0.0007 '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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.738(19) _cell_length_b 13.262(6) _cell_length_c 22.777(12) _cell_angle_alpha 90.00 _cell_angle_beta 110.042(8) _cell_angle_gamma 90.00 _cell_volume 10141(9) _cell_formula_units_Z 8 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9273 _exptl_absorpt_correction_T_max 0.9784 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32784 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI 0.0967 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8933 _reflns_number_gt 6836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalClear' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0507P)^2^+32.0867P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8933 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.1804 _refine_ls_wR_factor_gt 0.1659 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _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 Si1 Si 0.33736(3) 0.08924(9) 0.21218(5) 0.0248(3) Uani 1 1 d . . . H1 H 0.3070 0.1335 0.2353 0.030 Uiso 1 1 calc R . . B1 B 0.31166(14) -0.0225(4) 0.1502(2) 0.0271(11) Uani 1 1 d . . . O1 O 0.28382(8) -0.0232(2) 0.09181(13) 0.0301(7) Uani 1 1 d . . . C1 C 0.26803(14) 0.0655(3) 0.0513(2) 0.0343(11) Uani 1 1 d . . . C2 C 0.23090(15) 0.0249(4) -0.0008(2) 0.0422(12) Uani 1 1 d . . . O2 O 0.24227(11) -0.0656(2) -0.02658(15) 0.0488(9) Uani 1 1 d . . . H2 H 0.2550 -0.1042 0.0027 0.073 Uiso 1 1 calc R . . C3 C 0.25739(14) 0.1494(3) 0.0886(2) 0.0380(11) Uani 1 1 d . . . H3 H 0.2440 0.1204 0.1157 0.057 Uiso 1 1 calc R . . H4 H 0.2396 0.1979 0.0598 0.057 Uiso 1 1 calc R . . H5 H 0.2817 0.1839 0.1144 0.057 Uiso 1 1 calc R . . C4 C 0.30047(14) 0.0996(4) 0.0261(2) 0.0408(12) Uani 1 1 d . . . H6 H 0.3244 0.1185 0.0610 0.061 Uiso 1 1 calc R . . H7 H 0.2910 0.1579 -0.0015 0.061 Uiso 1 1 calc R . . H8 H 0.3069 0.0444 0.0025 0.061 Uiso 1 1 calc R . . C5 C 0.19719(15) -0.0019(4) 0.0232(3) 0.0516(14) Uani 1 1 d . . . H9 H 0.1756 -0.0347 -0.0101 0.077 Uiso 1 1 calc R . . H10 H 0.1871 0.0597 0.0364 0.077 Uiso 1 1 calc R . . H11 H 0.2072 -0.0478 0.0589 0.077 Uiso 1 1 calc R . . C6 C 0.21535(16) 0.0949(4) -0.0561(2) 0.0545(15) Uani 1 1 d . . . H12 H 0.2354 0.1023 -0.0762 0.082 Uiso 1 1 calc R . . H13 H 0.2097 0.1610 -0.0419 0.082 Uiso 1 1 calc R . . H14 H 0.1909 0.0668 -0.0861 0.082 Uiso 1 1 calc R . . C7 C 0.36650(12) 0.1948(3) 0.19207(18) 0.0242(9) Uani 1 1 d . . . C8 C 0.39471(13) 0.1725(3) 0.16276(19) 0.0293(10) Uani 1 1 d . . . C9 C 0.41642(13) 0.2492(3) 0.1483(2) 0.0316(10) Uani 1 1 d . . . H15 H 0.4344 0.2330 0.1272 0.038 Uiso 1 1 calc R . . C10 C 0.41265(14) 0.3493(3) 0.1638(2) 0.0348(11) Uani 1 1 d . . . C11 C 0.38496(13) 0.3703(3) 0.19194(19) 0.0299(10) Uani 1 1 d . . . H16 H 0.3817 0.4382 0.2026 0.036 Uiso 1 1 calc R . . C12 C 0.36159(12) 0.2963(3) 0.20539(18) 0.0266(10) Uani 1 1 d . . . C13 C 0.40230(13) 0.0644(3) 0.1485(2) 0.0344(11) Uani 1 1 d . . . H17 H 0.4216 0.0632 0.1266 0.052 Uiso 1 1 calc R . . H18 H 0.3773 0.0336 0.1220 0.052 Uiso 1 1 calc R . . H19 H 0.4130 0.0264 0.1876 0.052 Uiso 1 1 calc R . . C14 C 0.43845(18) 0.4308(4) 0.1516(3) 0.0574(15) Uani 1 1 d . . . H20 H 0.4244 0.4955 0.1459 0.086 Uiso 1 1 calc R . . H21 H 0.4443 0.4145 0.1137 0.086 Uiso 1 1 calc R . . H22 H 0.4634 0.4355 0.1872 0.086 Uiso 1 1 calc R . . C15 C 0.33137(13) 0.3311(3) 0.2346(2) 0.0332(11) Uani 1 1 d . . . H23 H 0.3339 0.4040 0.2419 0.050 Uiso 1 1 calc R . . H24 H 0.3363 0.2961 0.2744 0.050 Uiso 1 1 calc R . . H25 H 0.3044 0.3155 0.2063 0.050 Uiso 1 1 calc R . . C16 C 0.36753(11) -0.0050(3) 0.27066(17) 0.0210(9) Uani 1 1 d . . . C17 C 0.35814(11) -0.1057(3) 0.25046(17) 0.0197(8) Uani 1 1 d . . . C18 C 0.37893(12) -0.1838(3) 0.28990(18) 0.0225(9) Uani 1 1 d . . . H26 H 0.3727 -0.2517 0.2770 0.027 Uiso 1 1 calc R . . C19 C 0.40837(12) -0.1648(3) 0.34721(18) 0.0222(9) Uani 1 1 d . . . C20 C 0.41611(11) -0.0651(3) 0.36625(18) 0.0210(9) Uani 1 1 d . . . H27 H 0.4360 -0.0512 0.4055 0.025 Uiso 1 1 calc R . . C21 C 0.39589(11) 0.0147(3) 0.33001(18) 0.0217(9) Uani 1 1 d . . . C22 C 0.32570(11) -0.1267(3) 0.18617(18) 0.0236(9) Uani 1 1 d . . . Si2 Si 0.27774(4) -0.16943(10) 0.19948(6) 0.0337(3) Uani 1 1 d . . . Si3 Si 0.34384(4) -0.22521(9) 0.14064(5) 0.0294(3) Uani 1 1 d . . . C23 C 0.25397(13) -0.0578(4) 0.2227(2) 0.0417(12) Uani 1 1 d . . . H28 H 0.2465 -0.0083 0.1887 0.063 Uiso 1 1 calc R . . H29 H 0.2728 -0.0272 0.2604 0.063 Uiso 1 1 calc R . . H30 H 0.2301 -0.0796 0.2312 0.063 Uiso 1 1 calc R . . C24 C 0.24183(13) -0.2262(4) 0.1278(2) 0.0448(13) Uani 1 1 d . . . H31 H 0.2153 -0.2286 0.1315 0.067 Uiso 1 1 calc R . . H32 H 0.2504 -0.2947 0.1224 0.067 Uiso 1 1 calc R . . H33 H 0.2408 -0.1852 0.0914 0.067 Uiso 1 1 calc R . . C25 C 0.28593(15) -0.2629(4) 0.2637(2) 0.0487(14) Uani 1 1 d . . . H34 H 0.2604 -0.2788 0.2687 0.073 Uiso 1 1 calc R . . H35 H 0.3042 -0.2345 0.3027 0.073 Uiso 1 1 calc R . . H36 H 0.2975 -0.3245 0.2534 0.073 Uiso 1 1 calc R . . C26 C 0.39752(13) -0.2049(3) 0.1526(2) 0.0357(11) Uani 1 1 d . . . H37 H 0.4079 -0.2635 0.1368 0.054 Uiso 1 1 calc R . . H38 H 0.4124 -0.1964 0.1973 0.054 Uiso 1 1 calc R . . H39 H 0.4005 -0.1444 0.1299 0.054 Uiso 1 1 calc R . . C27 C 0.31727(14) -0.2178(4) 0.0544(2) 0.0400(12) Uani 1 1 d . . . H40 H 0.3200 -0.1496 0.0398 0.060 Uiso 1 1 calc R . . H41 H 0.2890 -0.2333 0.0450 0.060 Uiso 1 1 calc R . . H42 H 0.3289 -0.2666 0.0333 0.060 Uiso 1 1 calc R . . C28 C 0.33833(14) -0.3595(3) 0.1623(2) 0.0392(12) Uani 1 1 d . . . H43 H 0.3496 -0.4046 0.1385 0.059 Uiso 1 1 calc R . . H44 H 0.3100 -0.3751 0.1526 0.059 Uiso 1 1 calc R . . H45 H 0.3525 -0.3691 0.2071 0.059 Uiso 1 1 calc R . . C29 C 0.43231(13) -0.2490(3) 0.38840(19) 0.0305(10) Uani 1 1 d . . . H46 H 0.4486 -0.2119 0.4269 0.037 Uiso 1 1 calc R . . Si4 Si 0.40208(5) -0.33706(10) 0.41889(6) 0.0470(4) Uani 1 1 d . . . Si5 Si 0.47157(4) -0.29808(11) 0.35743(6) 0.0451(4) Uani 1 1 d . . . C30 C 0.3694(2) -0.2567(4) 0.4484(3) 0.079(2) Uani 1 1 d . . . H47 H 0.3547 -0.2994 0.4680 0.118 Uiso 1 1 calc R . . H48 H 0.3506 -0.2196 0.4134 0.118 Uiso 1 1 calc R . . H49 H 0.3859 -0.2087 0.4792 0.118 Uiso 1 1 calc R . . C31 C 0.37168(16) -0.4305(4) 0.3608(2) 0.0499(14) Uani 1 1 d . . . H50 H 0.3555 -0.4701 0.3796 0.075 Uiso 1 1 calc R . . H51 H 0.3894 -0.4756 0.3484 0.075 Uiso 1 1 calc R . . H52 H 0.3542 -0.3949 0.3239 0.075 Uiso 1 1 calc R . . C32 C 0.4368(2) -0.4136(5) 0.4845(3) 0.103(3) Uani 1 1 d . . . H53 H 0.4558 -0.3686 0.5143 0.154 Uiso 1 1 calc R . . H54 H 0.4513 -0.4616 0.4676 0.154 Uiso 1 1 calc R . . H55 H 0.4214 -0.4505 0.5058 0.154 Uiso 1 1 calc R . . C33 C 0.49315(15) -0.1883(4) 0.3303(3) 0.0621(17) Uani 1 1 d . . . H56 H 0.5146 -0.2111 0.3159 0.093 Uiso 1 1 calc R . . H57 H 0.5039 -0.1406 0.3649 0.093 Uiso 1 1 calc R . . H58 H 0.4724 -0.1551 0.2959 0.093 Uiso 1 1 calc R . . C34 C 0.45167(17) -0.3895(4) 0.2922(2) 0.0542(15) Uani 1 1 d . . . H59 H 0.4297 -0.3583 0.2586 0.081 Uiso 1 1 calc R . . H60 H 0.4419 -0.4497 0.3074 0.081 Uiso 1 1 calc R . . H61 H 0.4729 -0.4087 0.2762 0.081 Uiso 1 1 calc R . . C35 C 0.5124(2) -0.3622(6) 0.4209(3) 0.098(3) Uani 1 1 d . . . H62 H 0.5017 -0.4218 0.4351 0.147 Uiso 1 1 calc R . . H63 H 0.5235 -0.3156 0.4559 0.147 Uiso 1 1 calc R . . H64 H 0.5334 -0.3828 0.4048 0.147 Uiso 1 1 calc R . . C36 C 0.40416(11) 0.1212(3) 0.35618(18) 0.0249(9) Uani 1 1 d . . . H65 H 0.3872 0.1645 0.3212 0.030 Uiso 1 1 calc R . . Si6 Si 0.38082(4) 0.13624(9) 0.41891(6) 0.0309(3) Uani 1 1 d . . . Si7 Si 0.45628(4) 0.16875(9) 0.37054(5) 0.0298(3) Uani 1 1 d . . . C37 C 0.33042(13) 0.0767(3) 0.3898(2) 0.0369(11) Uani 1 1 d . . . H66 H 0.3167 0.0890 0.4197 0.055 Uiso 1 1 calc R . . H67 H 0.3332 0.0040 0.3850 0.055 Uiso 1 1 calc R . . H68 H 0.3149 0.1061 0.3493 0.055 Uiso 1 1 calc R . . C38 C 0.40928(16) 0.0737(4) 0.4947(2) 0.0459(13) Uani 1 1 d . . . H69 H 0.4355 0.1056 0.5126 0.069 Uiso 1 1 calc R . . H70 H 0.4127 0.0020 0.4874 0.069 Uiso 1 1 calc R . . H71 H 0.3946 0.0807 0.5237 0.069 Uiso 1 1 calc R . . C39 C 0.37654(15) 0.2739(3) 0.4341(2) 0.0421(12) Uani 1 1 d . . . H72 H 0.3579 0.2832 0.4569 0.063 Uiso 1 1 calc R . . H73 H 0.3667 0.3102 0.3943 0.063 Uiso 1 1 calc R . . H74 H 0.4028 0.3003 0.4592 0.063 Uiso 1 1 calc R . . C40 C 0.47440(15) 0.1206(5) 0.3088(2) 0.0536(15) Uani 1 1 d . . . H75 H 0.4569 0.1447 0.2680 0.080 Uiso 1 1 calc R . . H76 H 0.4743 0.0467 0.3093 0.080 Uiso 1 1 calc R . . H77 H 0.5016 0.1449 0.3165 0.080 Uiso 1 1 calc R . . C41 C 0.49360(14) 0.1293(4) 0.4472(2) 0.0463(13) Uani 1 1 d . . . H78 H 0.4938 0.0556 0.4505 0.070 Uiso 1 1 calc R . . H79 H 0.4865 0.1587 0.4814 0.070 Uiso 1 1 calc R . . H80 H 0.5201 0.1528 0.4499 0.070 Uiso 1 1 calc R . . C42 C 0.45501(15) 0.3092(4) 0.3681(3) 0.0499(14) Uani 1 1 d . . . H81 H 0.4815 0.3350 0.3722 0.075 Uiso 1 1 calc R . . H82 H 0.4472 0.3349 0.4025 0.075 Uiso 1 1 calc R . . H83 H 0.4357 0.3317 0.3282 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0227(6) 0.0250(6) 0.0257(6) 0.0029(5) 0.0071(5) 0.0020(5) B1 0.020(2) 0.034(3) 0.027(3) 0.000(2) 0.008(2) 0.001(2) O1 0.0291(16) 0.0230(15) 0.0305(16) 0.0018(13) 0.0005(13) 0.0025(12) C1 0.038(3) 0.027(2) 0.030(3) 0.0036(19) 0.001(2) 0.002(2) C2 0.047(3) 0.032(3) 0.036(3) 0.000(2) -0.001(2) 0.003(2) O2 0.053(2) 0.038(2) 0.040(2) -0.0045(16) -0.0052(17) 0.0047(17) C3 0.040(3) 0.030(3) 0.034(3) 0.001(2) 0.000(2) 0.009(2) C4 0.044(3) 0.035(3) 0.041(3) 0.009(2) 0.011(2) 0.004(2) C5 0.036(3) 0.046(3) 0.064(4) -0.001(3) 0.005(3) 0.006(2) C6 0.053(3) 0.044(3) 0.043(3) 0.004(2) -0.014(3) -0.005(3) C7 0.024(2) 0.025(2) 0.021(2) 0.0018(17) 0.0055(18) 0.0029(17) C8 0.029(2) 0.030(2) 0.026(2) -0.0008(19) 0.0047(19) 0.0036(19) C9 0.034(3) 0.035(3) 0.031(3) 0.001(2) 0.017(2) -0.002(2) C10 0.036(3) 0.034(3) 0.037(3) 0.008(2) 0.016(2) -0.002(2) C11 0.036(3) 0.020(2) 0.032(2) 0.0008(19) 0.010(2) 0.0017(19) C12 0.026(2) 0.031(2) 0.019(2) 0.0041(18) 0.0025(18) 0.0068(18) C13 0.031(3) 0.035(3) 0.039(3) -0.004(2) 0.014(2) 0.003(2) C14 0.070(4) 0.038(3) 0.079(4) 0.004(3) 0.044(3) -0.012(3) C15 0.036(3) 0.026(2) 0.041(3) 0.000(2) 0.016(2) 0.005(2) C16 0.017(2) 0.025(2) 0.022(2) 0.0043(17) 0.0079(17) 0.0039(16) C17 0.0150(19) 0.025(2) 0.021(2) 0.0039(17) 0.0088(16) -0.0013(16) C18 0.025(2) 0.019(2) 0.025(2) -0.0001(17) 0.0095(18) 0.0015(17) C19 0.023(2) 0.027(2) 0.019(2) 0.0033(17) 0.0094(17) 0.0069(17) C20 0.017(2) 0.026(2) 0.019(2) -0.0029(17) 0.0045(16) -0.0001(16) C21 0.016(2) 0.026(2) 0.025(2) 0.0033(17) 0.0091(17) 0.0009(16) C22 0.021(2) 0.024(2) 0.022(2) 0.0050(17) 0.0022(17) -0.0023(17) Si2 0.0239(6) 0.0307(7) 0.0446(8) 0.0068(6) 0.0094(6) -0.0039(5) Si3 0.0308(7) 0.0256(6) 0.0267(7) -0.0026(5) 0.0031(5) 0.0035(5) C23 0.027(2) 0.046(3) 0.059(3) 0.008(2) 0.023(2) 0.000(2) C24 0.024(2) 0.039(3) 0.063(3) -0.002(2) 0.004(2) -0.010(2) C25 0.037(3) 0.048(3) 0.066(4) 0.020(3) 0.024(3) 0.000(2) C26 0.041(3) 0.034(3) 0.036(3) -0.003(2) 0.018(2) 0.005(2) C27 0.043(3) 0.036(3) 0.034(3) -0.006(2) 0.004(2) 0.005(2) C28 0.043(3) 0.024(2) 0.044(3) 0.000(2) 0.006(2) 0.005(2) C29 0.039(3) 0.026(2) 0.020(2) 0.0015(18) 0.0020(19) 0.0110(19) Si4 0.0781(11) 0.0272(7) 0.0286(7) 0.0060(6) 0.0090(7) -0.0076(7) Si5 0.0393(8) 0.0494(9) 0.0341(8) -0.0089(6) -0.0034(6) 0.0238(7) C30 0.136(7) 0.051(4) 0.081(5) -0.018(3) 0.080(5) -0.036(4) C31 0.062(4) 0.034(3) 0.045(3) 0.007(2) 0.006(3) 0.002(3) C32 0.147(7) 0.063(4) 0.051(4) 0.029(3) -0.027(4) -0.034(5) C33 0.031(3) 0.078(4) 0.083(4) -0.025(3) 0.026(3) 0.001(3) C34 0.068(4) 0.048(3) 0.043(3) -0.010(3) 0.015(3) 0.017(3) C35 0.095(5) 0.118(6) 0.049(4) -0.020(4) -0.019(3) 0.084(5) C36 0.021(2) 0.022(2) 0.024(2) 0.0032(17) -0.0019(17) 0.0025(17) Si6 0.0330(7) 0.0286(7) 0.0308(7) 0.0002(5) 0.0106(5) 0.0060(5) Si7 0.0255(6) 0.0334(7) 0.0258(7) 0.0028(5) 0.0029(5) -0.0047(5) C37 0.039(3) 0.034(3) 0.045(3) -0.002(2) 0.024(2) -0.002(2) C38 0.054(3) 0.057(3) 0.028(3) 0.006(2) 0.016(2) 0.016(3) C39 0.043(3) 0.035(3) 0.048(3) -0.009(2) 0.015(2) 0.004(2) C40 0.033(3) 0.086(4) 0.043(3) -0.005(3) 0.014(2) -0.019(3) C41 0.033(3) 0.054(3) 0.041(3) 0.003(2) -0.001(2) -0.008(2) C42 0.045(3) 0.037(3) 0.059(3) 0.006(3) 0.005(3) -0.015(2) _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 C16 1.874(4) . ? Si1 C7 1.892(4) . ? Si1 B1 2.036(5) . ? B1 O1 1.361(5) . ? B1 C22 1.597(6) . ? O1 C1 1.482(5) . ? C1 C3 1.525(6) . ? C1 C4 1.529(6) . ? C1 C2 1.543(6) . ? C2 O2 1.453(6) . ? C2 C6 1.509(6) . ? C2 C5 1.526(7) . ? C7 C12 1.405(6) . ? C7 C8 1.418(6) . ? C8 C9 1.385(6) . ? C8 C13 1.516(6) . ? C9 C10 1.393(6) . ? C10 C11 1.379(6) . ? C10 C14 1.507(6) . ? C11 C12 1.389(6) . ? C12 C15 1.521(6) . ? C16 C21 1.408(5) . ? C16 C17 1.415(5) . ? C17 C18 1.406(5) . ? C17 C22 1.550(5) . ? C18 C19 1.391(5) . ? C19 C20 1.390(5) . ? C19 C29 1.520(5) . ? C20 C21 1.383(5) . ? C21 C36 1.522(5) . ? C22 Si3 1.915(4) . ? C22 Si2 1.926(4) . ? Si2 C24 1.856(5) . ? Si2 C25 1.862(5) . ? Si2 C23 1.871(5) . ? Si3 C26 1.862(5) . ? Si3 C27 1.868(5) . ? Si3 C28 1.877(5) . ? C29 Si4 1.878(5) . ? C29 Si5 1.889(5) . ? Si4 C31 1.866(5) . ? Si4 C30 1.867(6) . ? Si4 C32 1.879(6) . ? Si5 C33 1.849(6) . ? Si5 C34 1.860(5) . ? Si5 C35 1.869(5) . ? C36 Si7 1.886(4) . ? C36 Si6 1.896(4) . ? Si6 C37 1.867(5) . ? Si6 C38 1.870(5) . ? Si6 C39 1.875(5) . ? Si7 C40 1.851(5) . ? Si7 C42 1.864(5) . ? Si7 C41 1.873(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Si1 C7 115.78(18) . . ? C16 Si1 B1 91.18(19) . . ? C7 Si1 B1 121.70(19) . . ? O1 B1 C22 119.4(4) . . ? O1 B1 Si1 133.5(3) . . ? C22 B1 Si1 106.6(3) . . ? B1 O1 C1 126.7(3) . . ? O1 C1 C3 110.3(3) . . ? O1 C1 C4 107.0(4) . . ? C3 C1 C4 111.1(4) . . ? O1 C1 C2 104.2(3) . . ? C3 C1 C2 111.8(4) . . ? C4 C1 C2 112.1(4) . . ? O2 C2 C6 104.2(4) . . ? O2 C2 C5 108.5(4) . . ? C6 C2 C5 109.4(4) . . ? O2 C2 C1 108.3(4) . . ? C6 C2 C1 113.6(4) . . ? C5 C2 C1 112.4(4) . . ? C12 C7 C8 117.6(4) . . ? C12 C7 Si1 122.5(3) . . ? C8 C7 Si1 120.0(3) . . ? C9 C8 C7 120.4(4) . . ? C9 C8 C13 119.2(4) . . ? C7 C8 C13 120.4(4) . . ? C8 C9 C10 121.9(4) . . ? C11 C10 C9 117.2(4) . . ? C11 C10 C14 121.6(4) . . ? C9 C10 C14 121.2(4) . . ? C10 C11 C12 122.8(4) . . ? C11 C12 C7 120.0(4) . . ? C11 C12 C15 117.0(4) . . ? C7 C12 C15 123.0(4) . . ? C21 C16 C17 120.0(3) . . ? C21 C16 Si1 127.5(3) . . ? C17 C16 Si1 112.6(3) . . ? C18 C17 C16 118.3(3) . . ? C18 C17 C22 122.1(3) . . ? C16 C17 C22 119.6(3) . . ? C19 C18 C17 122.0(4) . . ? C20 C19 C18 118.1(4) . . ? C20 C19 C29 119.8(4) . . ? C18 C19 C29 122.1(4) . . ? C21 C20 C19 122.3(4) . . ? C20 C21 C16 119.2(4) . . ? C20 C21 C36 119.0(3) . . ? C16 C21 C36 121.8(3) . . ? C17 C22 B1 109.3(3) . . ? C17 C22 Si3 110.6(3) . . ? B1 C22 Si3 114.7(3) . . ? C17 C22 Si2 108.8(3) . . ? B1 C22 Si2 101.3(3) . . ? Si3 C22 Si2 111.7(2) . . ? C24 Si2 C25 107.2(2) . . ? C24 Si2 C23 109.0(2) . . ? C25 Si2 C23 105.6(2) . . ? C24 Si2 C22 111.4(2) . . ? C25 Si2 C22 114.3(2) . . ? C23 Si2 C22 109.05(19) . . ? C26 Si3 C27 105.8(2) . . ? C26 Si3 C28 107.1(2) . . ? C27 Si3 C28 105.4(2) . . ? C26 Si3 C22 110.21(19) . . ? C27 Si3 C22 112.89(19) . . ? C28 Si3 C22 114.8(2) . . ? C19 C29 Si4 114.3(3) . . ? C19 C29 Si5 110.8(3) . . ? Si4 C29 Si5 121.3(2) . . ? C31 Si4 C30 110.5(3) . . ? C31 Si4 C29 114.8(2) . . ? C30 Si4 C29 106.7(2) . . ? C31 Si4 C32 105.7(3) . . ? C30 Si4 C32 110.2(4) . . ? C29 Si4 C32 108.9(3) . . ? C33 Si5 C34 109.6(3) . . ? C33 Si5 C35 108.1(3) . . ? C34 Si5 C35 107.7(3) . . ? C33 Si5 C29 107.5(2) . . ? C34 Si5 C29 113.2(2) . . ? C35 Si5 C29 110.5(3) . . ? C21 C36 Si7 115.2(3) . . ? C21 C36 Si6 108.4(3) . . ? Si7 C36 Si6 119.8(2) . . ? C37 Si6 C38 107.1(2) . . ? C37 Si6 C39 110.3(2) . . ? C38 Si6 C39 108.3(2) . . ? C37 Si6 C36 107.91(19) . . ? C38 Si6 C36 114.1(2) . . ? C39 Si6 C36 109.1(2) . . ? C40 Si7 C42 109.4(3) . . ? C40 Si7 C41 106.8(2) . . ? C42 Si7 C41 108.0(2) . . ? C40 Si7 C36 109.6(2) . . ? C42 Si7 C36 108.5(2) . . ? C41 Si7 C36 114.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Si1 B1 O1 179.0(4) . . . . ? C7 Si1 B1 O1 -59.4(5) . . . . ? C16 Si1 B1 C22 7.3(3) . . . . ? C7 Si1 B1 C22 128.9(3) . . . . ? C22 B1 O1 C1 -178.7(4) . . . . ? Si1 B1 O1 C1 10.5(7) . . . . ? B1 O1 C1 C3 -46.4(6) . . . . ? B1 O1 C1 C4 74.6(5) . . . . ? B1 O1 C1 C2 -166.5(4) . . . . ? O1 C1 C2 O2 -50.9(5) . . . . ? C3 C1 C2 O2 -170.0(4) . . . . ? C4 C1 C2 O2 64.5(5) . . . . ? O1 C1 C2 C6 -166.1(4) . . . . ? C3 C1 C2 C6 74.8(5) . . . . ? C4 C1 C2 C6 -50.7(6) . . . . ? O1 C1 C2 C5 68.9(5) . . . . ? C3 C1 C2 C5 -50.2(5) . . . . ? C4 C1 C2 C5 -175.7(4) . . . . ? C16 Si1 C7 C12 -116.3(3) . . . . ? B1 Si1 C7 C12 134.8(3) . . . . ? C16 Si1 C7 C8 63.4(4) . . . . ? B1 Si1 C7 C8 -45.6(4) . . . . ? C12 C7 C8 C9 0.2(6) . . . . ? Si1 C7 C8 C9 -179.5(3) . . . . ? C12 C7 C8 C13 178.5(4) . . . . ? Si1 C7 C8 C13 -1.2(5) . . . . ? C7 C8 C9 C10 2.5(7) . . . . ? C13 C8 C9 C10 -175.9(4) . . . . ? C8 C9 C10 C11 -2.8(7) . . . . ? C8 C9 C10 C14 175.9(5) . . . . ? C9 C10 C11 C12 0.6(7) . . . . ? C14 C10 C11 C12 -178.1(4) . . . . ? C10 C11 C12 C7 2.0(6) . . . . ? C10 C11 C12 C15 -178.1(4) . . . . ? C8 C7 C12 C11 -2.3(6) . . . . ? Si1 C7 C12 C11 177.3(3) . . . . ? C8 C7 C12 C15 177.8(4) . . . . ? Si1 C7 C12 C15 -2.6(5) . . . . ? C7 Si1 C16 C21 51.6(4) . . . . ? B1 Si1 C16 C21 178.0(4) . . . . ? C7 Si1 C16 C17 -130.6(3) . . . . ? B1 Si1 C16 C17 -4.2(3) . . . . ? C21 C16 C17 C18 -2.5(5) . . . . ? Si1 C16 C17 C18 179.5(3) . . . . ? C21 C16 C17 C22 177.6(3) . . . . ? Si1 C16 C17 C22 -0.3(4) . . . . ? C16 C17 C18 C19 -0.7(6) . . . . ? C22 C17 C18 C19 179.2(3) . . . . ? C17 C18 C19 C20 2.3(6) . . . . ? C17 C18 C19 C29 -176.8(4) . . . . ? C18 C19 C20 C21 -0.7(6) . . . . ? C29 C19 C20 C21 178.5(4) . . . . ? C19 C20 C21 C16 -2.5(6) . . . . ? C19 C20 C21 C36 175.9(4) . . . . ? C17 C16 C21 C20 4.1(6) . . . . ? Si1 C16 C21 C20 -178.3(3) . . . . ? C17 C16 C21 C36 -174.2(3) . . . . ? Si1 C16 C21 C36 3.4(5) . . . . ? C18 C17 C22 B1 -173.6(4) . . . . ? C16 C17 C22 B1 6.3(5) . . . . ? C18 C17 C22 Si3 -46.3(4) . . . . ? C16 C17 C22 Si3 133.5(3) . . . . ? C18 C17 C22 Si2 76.7(4) . . . . ? C16 C17 C22 Si2 -103.5(3) . . . . ? O1 B1 C22 C17 178.5(3) . . . . ? Si1 B1 C22 C17 -8.4(4) . . . . ? O1 B1 C22 Si3 53.6(5) . . . . ? Si1 B1 C22 Si3 -133.3(2) . . . . ? O1 B1 C22 Si2 -66.8(4) . . . . ? Si1 B1 C22 Si2 106.3(2) . . . . ? C17 C22 Si2 C24 -165.8(3) . . . . ? B1 C22 Si2 C24 79.1(3) . . . . ? Si3 C22 Si2 C24 -43.5(3) . . . . ? C17 C22 Si2 C25 -44.1(4) . . . . ? B1 C22 Si2 C25 -159.2(3) . . . . ? Si3 C22 Si2 C25 78.3(3) . . . . ? C17 C22 Si2 C23 73.8(3) . . . . ? B1 C22 Si2 C23 -41.3(3) . . . . ? Si3 C22 Si2 C23 -163.8(2) . . . . ? C17 C22 Si3 C26 -38.8(3) . . . . ? B1 C22 Si3 C26 85.5(3) . . . . ? Si2 C22 Si3 C26 -160.1(2) . . . . ? C17 C22 Si3 C27 -156.9(3) . . . . ? B1 C22 Si3 C27 -32.7(4) . . . . ? Si2 C22 Si3 C27 81.8(3) . . . . ? C17 C22 Si3 C28 82.3(3) . . . . ? B1 C22 Si3 C28 -153.5(3) . . . . ? Si2 C22 Si3 C28 -39.0(3) . . . . ? C20 C19 C29 Si4 116.2(4) . . . . ? C18 C19 C29 Si4 -64.6(4) . . . . ? C20 C19 C29 Si5 -102.4(4) . . . . ? C18 C19 C29 Si5 76.7(4) . . . . ? C19 C29 Si4 C31 76.7(4) . . . . ? Si5 C29 Si4 C31 -60.3(3) . . . . ? C19 C29 Si4 C30 -46.1(4) . . . . ? Si5 C29 Si4 C30 176.9(3) . . . . ? C19 C29 Si4 C32 -165.1(4) . . . . ? Si5 C29 Si4 C32 58.0(4) . . . . ? C19 C29 Si5 C33 40.2(4) . . . . ? Si4 C29 Si5 C33 178.5(3) . . . . ? C19 C29 Si5 C34 -81.0(4) . . . . ? Si4 C29 Si5 C34 57.3(3) . . . . ? C19 C29 Si5 C35 158.0(4) . . . . ? Si4 C29 Si5 C35 -63.7(4) . . . . ? C20 C21 C36 Si7 64.8(4) . . . . ? C16 C21 C36 Si7 -116.8(3) . . . . ? C20 C21 C36 Si6 -72.6(4) . . . . ? C16 C21 C36 Si6 105.7(4) . . . . ? C21 C36 Si6 C37 -42.8(3) . . . . ? Si7 C36 Si6 C37 -177.9(2) . . . . ? C21 C36 Si6 C38 76.1(3) . . . . ? Si7 C36 Si6 C38 -59.1(3) . . . . ? C21 C36 Si6 C39 -162.6(3) . . . . ? Si7 C36 Si6 C39 62.2(3) . . . . ? C21 C36 Si7 C40 36.1(4) . . . . ? Si6 C36 Si7 C40 168.5(3) . . . . ? C21 C36 Si7 C42 155.5(3) . . . . ? Si6 C36 Si7 C42 -72.1(3) . . . . ? C21 C36 Si7 C41 -83.8(3) . . . . ? Si6 C36 Si7 C41 48.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.525 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.069