#------------------------------------------------------------------------------ #$Date: 2021-08-11 01:17:11 +0300 (Wed, 11 Aug 2021) $ #$Revision: 268011 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564337.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1564337 loop_ _publ_author_name 'Takeuchi, Takumi' 'Shishido, Ryosuke' 'Kubota, Koji' 'Ito, Hajime' _publ_section_title ; Synthesis of hydrosilylboronates via the monoborylation of a dihydrosilane Si--H bond and their application for the generation of dialkylhydrosilyl anions ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC01440D _journal_year 2021 _chemical_formula_moiety 'C8 H19 B Si, 2(C3 H6 O)' _chemical_formula_sum 'C14 H31 B O2 Si' _chemical_formula_weight 270.29 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-11-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-02-25 deposited with the CCDC. 2021-08-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.7304(6) _cell_length_b 14.6636(6) _cell_length_c 9.7331(4) _cell_measurement_reflns_used 7744 _cell_measurement_temperature 173 _cell_measurement_theta_max 29.4210 _cell_measurement_theta_min 2.7110 _cell_volume 1816.91(14) _computing_cell_refinement 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 173 _diffrn_detector 'PLATUS 200K area detector' _diffrn_detector_area_resol_mean 5.811 _diffrn_detector_type 'HPC area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.915 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -71.00 56.00 0.50 70.19 -- -1.80 29.00-180.00 254 2 \w 62.00 88.00 0.50 70.19 -- -1.80 29.00-180.00 52 3 \w -65.00 22.00 0.50 70.19 -- 1.80 60.00 -30.00 174 4 \w 20.00 67.00 0.50 70.19 -- 1.80 29.00 -90.00 94 5 \w -88.00 17.00 0.50 70.19 -- 1.80 29.00 -90.00 210 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB P200' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0018029000 _diffrn_orient_matrix_UB_12 0.0284876000 _diffrn_orient_matrix_UB_13 -0.0415851000 _diffrn_orient_matrix_UB_21 0.0353066000 _diffrn_orient_matrix_UB_22 -0.0422501000 _diffrn_orient_matrix_UB_23 -0.0210999000 _diffrn_orient_matrix_UB_31 -0.0637256000 _diffrn_orient_matrix_UB_32 -0.0225686000 _diffrn_orient_matrix_UB_33 -0.0128096000 _diffrn_radiation_monochromator 'multi-layer mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_unetI/netI 0.0524 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.915 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 25184 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.915 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.209 _diffrn_reflns_theta_min 2.634 _diffrn_source 'rotating anode X-ray generator' _diffrn_source_type micromax007 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.62825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 0.988 _exptl_crystal_description plate _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.269 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 2333 _refine_ls_number_restraints 449 _refine_ls_restrained_S_all 0.975 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0772 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1862P)^2^+0.1943P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2346 _refine_ls_wR_factor_ref 0.2568 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1771 _reflns_number_total 2333 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc01440d2.cif _cod_data_source_block t4 _cod_database_code 1564337 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula 'Si C H O B' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.998 _shelx_estimated_absorpt_t_min 0.964 _reflns_odcompleteness_completeness 99.77 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All Si(H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints Si01, Si02, C003, C003, C10, C10, C005, C005, B1, O007, O007, O008, O008, C009, C009, C00A, C00A, C00B, C00B, C00C, C00C, C00D, C00D, C00E, C00E, C00F, C00F, C2, C2, C1, C1, B2 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O1, Si01, Si02, C003, B1, C00E, B2, C00A, C10, C009, C00F, O007, O008, O0, C005, C2, C00D, C1, C00C, C00B with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O1, Si01, C003, B1, Si02, C10, C009, C00A, C00E, C00F, O007, O008, B2, C005, C2, O0, C00D, C00C, C1, C00B, C2A, C4, C0, C1A, C5, C3 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C005, B1, O007, O008, C00B, C00C, C00D, C2, C1, B2, O0, O1, C3, C4, C0, C1A, C2A, C5 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints Si01 \\sim Si02 \\sim C003 \\sim C003 \\sim C10 \\sim C10 \\sim C005 \\sim C005 \\sim B1 \\sim O007 \\sim O007 \\sim O008 \\sim O008 \\sim C009 \\sim C009 \\sim C00A \\sim C00A \\sim C00B \\sim C00B \\sim C00C \\sim C00C \\sim C00D \\sim C00D \\sim C00E \\sim C00E \\sim C00F \\sim C00F \\sim C2 \\sim C2 \\sim C1 \\sim C1 \\sim B2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 O1 \\sim Si01 \\sim Si02 \\sim C003 \\sim B1 \\sim C00E \\sim B2 \\sim C00A \\sim C10 \\sim C009 \\sim C00F \\sim O007 \\sim O008 \\sim O0 \\sim C005 \\sim C2 \\sim C00D \\sim C1 \\sim C00C \\sim C00B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 O1 \\sim Si01 \\sim C003 \\sim B1 \\sim Si02 \\sim C10 \\sim C009 \\sim C00A \\sim C00E \\sim C00F \\sim O007 \\sim O008 \\sim B2 \\sim C005 \\sim C2 \\sim O0 \\sim C00D \\sim C00C \\sim C1 \\sim C00B \\sim C2A \\sim C4 \\sim C0 \\sim C1A \\sim C5 \\sim C3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C005 \\sim B1 \\sim O007 \\sim O008 \\sim C00B \\sim C00C \\sim C00D \\sim C2 \\sim C1 \\sim B2 \\sim O0 \\sim O1 \\sim C3 \\sim C4 \\sim C0 \\sim C1A \\sim C2A \\sim C5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 4. Others Fixed Sof: Si01(0.25) H01(0.25) Si02(0.25) H02(0.25) C005(0.25) B1(0.25) O007(0.25) O008(0.25) C009(0.5) H00A(0.5) H00B(0.5) H00C(0.5) C00A(0.5) H00D(0.5) H00E(0.5) H00F(0.5) C00B(0.25) H00P(0.25) H00Q(0.25) H00R(0.25) C00C(0.25) H00M(0.25) H00N(0.25) H00O(0.25) C00D(0.25) H00S(0.25) H00T(0.25) H00U(0.25) C00E(0.5) H00G(0.5) H00H(0.5) H00I(0.5) C00F(0.5) H00J(0.5) H00K(0.5) H00L(0.5) C2(0.25) C1(0.25) H1A(0.25) H1B(0.25) H1C(0.25) B2(0.25) O0(0.25) O1(0.25) C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25) C4(0.25) H4A(0.25) H4B(0.25) H4C(0.25) C0(0.25) C1A(0.25) H1AA(0.25) H1AB(0.25) H1AC(0.25) C2A(0.25) C5(0.25) H5A(0.25) H5B(0.25) H5C(0.25) 5.a Ternary CH refined with riding coordinates: Si01(H01), Si02(H02) 5.b Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C009(H00A,H00B,H00C), C00A(H00D,H00E,H00F), C00B(H00P, H00Q,H00R), C00C(H00M,H00N,H00O), C00D(H00S,H00T,H00U), C00E(H00G,H00H,H00I), C00F(H00J,H00K,H00L), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C1A(H1AA,H1AB,H1AC), C5(H5A,H5B,H5C) ; _shelx_res_file ; TITL t4_a.res in Pnma t4.res created by SHELXL-2018/1 at 09:23:23 on 26-Nov-2020 REM Old TITL T4 in Pnam #62 REM SHELXT solution in Pnma REM R1 0.284, Rweak 0.021, Alpha 0.049, Orientation a'=-a, b'=c, c'=b REM Formula found by SHELXT: C23 O2 Si2 CELL 0.71073 12.7304 14.6636 9.7331 90 90 90 ZERR 4 0.0006 0.0006 0.0004 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H B O Si UNIT 56 124 4 8 4 DELU Si01 Si02 C003 C003 C10 C10 C005 C005 B1 O007 O007 O008 O008 C009 C009 = C00A C00A C00B C00B C00C C00C C00D C00D C00E C00E C00F C00F C2 C2 C1 C1 B2 DELU O1 Si01 Si02 C003 B1 C00E B2 C00A C10 C009 C00F O007 O008 O0 C005 C2 = C00D C1 C00C C00B DELU O1 Si01 C003 B1 Si02 C10 C009 C00A C00E C00F O007 O008 B2 C005 C2 O0 = C00D C00C C1 C00B C2A C4 C0 C1A C5 C3 DELU C005 B1 O007 O008 C00B C00C C00D C2 C1 B2 O0 O1 C3 C4 C0 C1A C2A C5 SIMU 0.04 0.08 1.7 Si01 Si02 C003 C003 C10 C10 C005 C005 B1 O007 O007 O008 = O008 C009 C009 C00A C00A C00B C00B C00C C00C C00D C00D C00E C00E C00F C00F = C2 C2 C1 C1 B2 SIMU 0.04 0.08 1.7 O1 Si01 Si02 C003 B1 C00E B2 C00A C10 C009 C00F O007 = O008 O0 C005 C2 C00D C1 C00C C00B SIMU 0.04 0.08 1.7 O1 Si01 C003 B1 Si02 C10 C009 C00A C00E C00F O007 O008 = B2 C005 C2 O0 C00D C00C C1 C00B C2A C4 C0 C1A C5 C3 SIMU 0.04 0.08 1.7 C005 B1 O007 O008 C00B C00C C00D C2 C1 B2 O0 O1 C3 C4 C0 = C1A C2A C5 L.S. 10 PLAN 20 SIZE 0.3 0.3 0.02 TEMP -100.15 CONF LIST 6 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.186200 0.194300 FVAR 0.67218 PART 1 SI01 5 0.687124 0.250000 0.677080 10.25000 0.03096 0.04234 = 0.03116 0.00000 0.00165 0.00000 AFIX 13 H01 2 0.630261 0.250000 0.747965 10.25000 -1.20000 AFIX 0 PART 0 PART 2 SI02 5 0.756729 0.250000 0.604993 10.25000 0.04247 0.06623 = 0.05026 0.00000 -0.00242 0.00000 AFIX 13 H02 2 0.826045 0.250000 0.556657 10.25000 -1.20000 AFIX 0 PART 0 C003 1 0.755386 0.361414 0.699060 11.00000 0.07325 0.05101 = 0.05442 -0.00344 -0.01056 -0.00443 C10 1 0.819272 0.368161 0.830542 11.00000 0.11200 0.08419 = 0.08358 -0.00687 -0.03666 -0.02130 AFIX 137 H10A 2 0.780209 0.339918 0.906153 11.00000 -1.50000 H10B 2 0.832418 0.432456 0.851978 11.00000 -1.50000 H10C 2 0.886392 0.336460 0.818294 11.00000 -1.50000 AFIX 0 PART -3 C005 1 0.547347 0.195048 0.268823 10.25000 0.04685 0.05657 = 0.04540 0.00534 -0.01667 -0.01447 PART 0 PART 1 B1 3 0.610581 0.250000 0.493808 10.25000 0.02952 0.04579 = 0.04407 0.00000 0.00353 0.00000 PART 0 PART -3 O007 4 0.652030 0.202792 0.382280 10.25000 0.05231 0.09545 = 0.05383 -0.03179 -0.03050 0.01060 PART 0 PART -2 O008 4 0.522158 0.209414 0.470793 10.25000 0.04041 0.07923 = 0.05282 0.01372 -0.01243 -0.01701 PART 0 PART 1 C009 1 0.680921 0.437946 0.687517 10.50000 0.08322 0.04586 = 0.10034 -0.00830 -0.00889 0.00393 AFIX 137 H00A 2 0.647875 0.436916 0.596592 10.50000 -1.50000 H00B 2 0.718613 0.495649 0.699765 10.50000 -1.50000 H00C 2 0.626742 0.432178 0.758517 10.50000 -1.50000 AFIX 0 C00A 1 0.843829 0.374639 0.584046 10.50000 0.08835 0.06501 = 0.07913 -0.00770 0.02531 -0.03318 AFIX 137 H00D 2 0.897467 0.327184 0.594267 10.50000 -1.50000 H00E 2 0.876414 0.434778 0.594652 10.50000 -1.50000 H00F 2 0.811793 0.370058 0.492752 10.50000 -1.50000 AFIX 0 PART 0 PART -2 C00B 1 0.392508 0.215168 0.305901 10.25000 0.04567 0.08502 = 0.04306 -0.00350 0.00444 -0.02370 AFIX 137 H00P 2 0.364820 0.164519 0.360709 10.25000 -1.50000 H00Q 2 0.370438 0.207960 0.210054 10.25000 -1.50000 H00R 2 0.365377 0.272944 0.341985 10.25000 -1.50000 AFIX 0 PART 0 PART -3 C00C 1 0.604964 0.202522 0.136901 10.25000 0.04740 0.13305 = 0.03734 -0.02616 0.00310 0.01726 AFIX 137 H00M 2 0.657264 0.251366 0.143499 10.25000 -1.50000 H00N 2 0.555340 0.216495 0.062861 10.25000 -1.50000 H00O 2 0.640369 0.144643 0.117153 10.25000 -1.50000 AFIX 0 PART 0 PART -2 C00D 1 0.561744 0.133708 0.216497 10.25000 0.09512 0.09166 = 0.11210 -0.03946 -0.01013 0.03671 AFIX 137 H00S 2 0.508933 0.115022 0.148864 10.25000 -1.50000 H00T 2 0.580687 0.081362 0.273984 10.25000 -1.50000 H00U 2 0.624395 0.156120 0.168717 10.25000 -1.50000 AFIX 0 PART 0 PART 2 C00E 1 0.632898 0.375150 0.761357 10.50000 0.10630 0.11680 = 0.14100 -0.05729 0.01204 0.02617 AFIX 137 H00G 2 0.584771 0.389246 0.685696 10.50000 -1.50000 H00H 2 0.632392 0.425359 0.827805 10.50000 -1.50000 H00I 2 0.610298 0.318831 0.806797 10.50000 -1.50000 AFIX 0 C00F 1 0.766969 0.437385 0.600251 10.50000 0.22133 0.06923 = 0.11403 0.02220 -0.05092 -0.04182 AFIX 137 H00J 2 0.838590 0.437579 0.563335 10.50000 -1.50000 H00K 2 0.753281 0.495354 0.647051 10.50000 -1.50000 H00L 2 0.716713 0.429559 0.524897 10.50000 -1.50000 AFIX 0 PART 0 PART -2 C2 1 0.513445 0.215293 0.313698 10.25000 0.03915 0.06002 = 0.05862 -0.01198 -0.01194 0.00314 PART 0 PART -3 C1 1 0.504060 0.115786 0.298787 10.25000 0.09566 0.03663 = 0.08399 0.00244 -0.04295 -0.01707 AFIX 137 H1A 2 0.490135 0.112713 0.397705 10.25000 -1.50000 H1B 2 0.551980 0.066434 0.272685 10.25000 -1.50000 H1C 2 0.437903 0.109317 0.248234 10.25000 -1.50000 AFIX 0 PART 0 PART 2 B2 3 0.650034 0.250000 0.449104 10.25000 0.04214 0.05407 = 0.05852 0.00000 -0.01896 0.00000 PART 0 PART -1 O0 4 0.560839 0.201573 0.443499 10.25000 0.06758 0.07821 = 0.07257 0.02571 -0.02813 -0.01560 PART 0 PART -4 O1 4 0.645679 0.184781 0.351980 10.25000 0.08857 0.05742 = 0.06588 -0.02096 -0.05153 0.01521 C3 1 0.594515 0.181776 0.107413 10.25000 0.10565 0.11703 = 0.04838 -0.02481 -0.00077 0.02038 AFIX 137 H3A 2 0.650480 0.222167 0.074597 10.25000 -1.50000 H3B 2 0.530932 0.191718 0.052665 10.25000 -1.50000 H3C 2 0.617001 0.118149 0.098238 10.25000 -1.50000 AFIX 0 PART 0 PART -1 C4 1 0.553316 0.128945 0.253610 10.25000 0.09067 0.06072 = 0.09983 -0.01238 -0.04351 -0.02550 AFIX 137 H4A 2 0.531567 0.123844 0.157331 10.25000 -1.50000 H4B 2 0.533770 0.073219 0.302964 10.25000 -1.50000 H4C 2 0.629613 0.137292 0.258222 10.25000 -1.50000 AFIX 0 PART 0 PART -4 C0 1 0.568833 0.204741 0.274536 10.25000 0.02834 0.07987 = 0.05282 -0.01600 -0.01605 0.00063 C1A 1 0.484103 0.113821 0.301982 10.25000 0.15941 0.11345 = 0.07872 -0.00302 -0.02092 -0.07870 AFIX 137 H1AA 2 0.524749 0.057296 0.309699 10.25000 -1.50000 H1AB 2 0.435104 0.108954 0.224671 10.25000 -1.50000 H1AC 2 0.444612 0.123876 0.387073 10.25000 -1.50000 AFIX 0 PART 0 PART -1 C2A 1 0.499743 0.209271 0.318375 10.25000 0.06458 0.06924 = 0.05408 0.01258 -0.00930 -0.02679 C5 1 0.389902 0.197391 0.311349 10.25000 0.06959 0.17118 = 0.09347 0.03898 -0.01932 -0.03222 AFIX 137 H5A 2 0.372704 0.132986 0.326079 10.25000 -1.50000 H5B 2 0.364669 0.216448 0.220660 10.25000 -1.50000 H5C 2 0.356032 0.234487 0.382427 10.25000 -1.50000 AFIX 0 HKLF 4 REM t4_a.res in Pnma REM R1 = 0.0772 for 1771 Fo > 4sig(Fo) and 0.0948 for all 2333 data REM 236 parameters refined using 449 restraints END WGHT 0.1868 0.1933 REM Highest difference peak 0.269, deepest hole -0.593, 1-sigma level 0.057 Q1 1 0.8715 0.3811 0.7571 11.00000 0.05 0.22 Q2 1 0.6841 0.2500 0.3225 10.50000 0.05 0.21 Q3 1 0.8196 0.3697 0.5341 11.00000 0.05 0.17 Q4 1 0.6004 0.2500 0.7985 10.50000 0.05 0.17 Q5 1 0.7457 0.3109 0.6677 11.00000 0.05 0.16 Q6 1 0.8837 0.4205 0.8261 11.00000 0.05 0.16 Q7 1 0.6096 0.2500 0.1530 10.50000 0.05 0.15 Q8 1 0.6817 0.4418 0.5488 11.00000 0.05 0.14 Q9 1 0.5858 0.2500 0.2395 10.50000 0.05 0.13 Q10 1 0.8765 0.3333 0.5343 11.00000 0.05 0.12 Q11 1 1.0043 0.4774 0.6163 11.00000 0.05 0.12 Q12 1 0.4794 0.1022 0.3698 11.00000 0.05 0.12 Q13 1 0.6414 0.4399 0.7888 11.00000 0.05 0.12 Q14 1 0.8005 0.4921 0.6348 11.00000 0.05 0.11 Q15 1 0.6592 0.1898 0.3139 11.00000 0.05 0.11 Q16 1 0.9628 0.4437 0.6156 11.00000 0.05 0.11 Q17 1 0.7847 0.4165 0.4834 11.00000 0.05 0.10 Q18 1 0.8624 0.3178 0.8657 11.00000 0.05 0.10 Q19 1 0.8820 0.3058 0.8498 11.00000 0.05 0.10 Q20 1 0.6821 0.4141 0.7123 11.00000 0.05 0.10 ; _shelx_res_checksum 84467 _shelx_hkl_file ; 0 -2 0 7191.90 762.54 0 3 0 1.36 0.29 0 -3 0 1.13 0.27 0 -3 0 1.21 0.33 0 -4 0 1090.00 110.60 0 4 0 1135.82 110.61 0 -4 0 915.07 110.60 0 -5 0 -0.36 0.27 0 5 0 -0.18 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-0.60 0.86 -2 -5 11 0.56 0.79 -2 5 -11 0.66 0.95 -2 -6 11 -0.79 1.15 2 6 11 -0.87 0.86 -2 -6 11 -0.31 0.82 -2 6 -11 1.71 0.98 -2 -7 11 1.18 1.10 2 7 11 0.22 0.94 -2 -7 11 0.02 0.77 -2 7 -11 1.23 0.93 -2 -8 11 -0.37 1.22 2 8 11 0.22 0.82 -2 -8 11 1.74 0.83 2 9 11 3.94 0.93 -2 -9 11 1.91 0.90 2 10 11 0.40 0.90 3 -8 11 1.67 1.10 -3 7 11 1.21 1.06 3 -7 11 2.84 1.03 -3 6 11 3.95 1.10 3 -6 11 5.47 1.08 3 6 -11 2.88 1.04 -3 5 11 4.25 1.04 3 -5 11 2.45 0.96 3 5 -11 3.97 1.05 -3 4 11 8.32 1.27 3 -4 11 7.28 1.17 3 4 -11 6.74 1.21 -3 3 11 6.58 1.11 3 -3 11 4.95 1.05 3 3 -11 5.96 1.06 3 -2 11 8.55 1.12 3 2 -11 6.13 1.14 -3 1 11 13.35 2.02 3 -1 11 16.85 1.85 3 -1 11 18.15 1.87 3 1 -11 13.23 1.86 -3 0 11 6.77 1.32 3 0 11 6.79 1.00 -3 0 11 7.21 1.14 3 0 11 6.55 1.05 3 0 -11 4.96 1.01 -3 -1 11 14.27 2.07 3 1 11 16.15 1.86 -3 -1 11 17.91 1.97 3 1 11 18.44 1.94 3 -1 -11 13.83 1.87 -3 -2 11 9.11 1.46 -3 -2 11 8.78 1.23 3 2 11 7.69 1.20 -3 -3 11 6.17 1.29 -3 -3 11 6.35 1.07 3 3 11 5.66 1.04 -3 -4 11 9.25 1.38 -3 -4 11 6.87 1.15 3 4 11 6.85 1.17 -3 -5 11 3.96 1.26 3 5 11 4.27 0.96 -3 -5 11 4.61 0.98 -3 -6 11 2.31 1.20 3 6 11 3.99 0.91 -3 -6 11 4.23 0.95 -3 -7 11 0.14 1.18 3 7 11 1.56 0.90 -3 -7 11 0.62 0.80 -3 -8 11 1.64 1.25 3 8 11 1.89 0.91 -3 -8 11 1.19 0.88 3 9 11 0.83 0.82 -3 -9 11 -0.70 0.85 3 10 11 2.38 0.94 4 -8 11 -0.07 0.97 4 -7 11 1.11 0.99 -4 6 11 -0.53 1.00 4 -6 11 1.30 0.92 -4 5 11 -0.07 1.02 4 -5 11 0.50 0.89 4 5 -11 -0.16 0.90 -4 4 11 3.18 0.96 4 -4 11 3.00 0.90 4 4 -11 3.15 0.96 4 -3 11 1.75 0.79 4 3 -11 0.18 0.81 -4 2 11 0.28 1.08 4 -2 11 1.08 0.77 4 2 -11 0.83 0.79 -4 1 11 10.72 1.43 4 -1 11 10.15 1.32 4 1 -11 8.90 1.34 -4 0 11 1.21 1.18 -4 0 11 0.05 0.86 4 0 11 0.28 0.72 4 0 -11 -0.02 0.73 -4 -1 11 7.51 1.61 4 1 11 9.64 1.24 -4 -1 11 13.61 1.61 4 -1 -11 8.47 1.26 4 1 11 10.07 1.30 -4 -2 11 0.16 1.16 -4 -2 11 -0.38 0.97 4 2 11 1.04 0.80 -4 -3 11 2.16 1.17 -4 -3 11 0.62 0.85 4 3 11 1.67 0.74 -4 -4 11 1.43 1.26 -4 -4 11 3.23 0.93 4 4 11 4.20 0.89 -4 -5 11 0.40 0.84 4 5 11 -0.61 0.79 -4 -6 11 0.70 1.19 -4 -6 11 0.59 0.85 4 6 11 0.18 0.74 -4 -7 11 -1.03 1.30 4 7 11 0.12 0.81 -4 -7 11 1.76 0.78 4 8 11 -1.27 0.86 -4 -8 11 -0.04 0.83 4 9 11 6.12 1.10 -4 -9 11 5.64 1.04 5 -7 11 -0.68 0.97 5 -6 11 2.05 0.99 5 -5 11 -0.99 0.87 5 5 -11 -0.39 0.94 -5 4 11 3.48 1.08 5 -4 11 3.46 0.96 5 4 -11 4.18 0.99 5 -3 11 -0.66 0.79 5 3 -11 0.54 0.84 5 -2 11 2.84 0.81 5 2 -11 1.63 0.82 -5 2 11 1.33 1.16 -5 1 11 1.45 1.20 -5 1 11 1.04 0.91 5 -1 11 0.63 0.72 5 1 -11 -1.54 0.79 -5 0 11 2.07 0.96 5 0 11 3.20 0.76 5 0 -11 2.62 0.84 -5 -1 11 1.39 1.28 -5 -1 11 0.38 0.89 5 -1 -11 -0.41 0.72 -5 -2 11 2.03 1.37 -5 -2 11 2.83 0.95 5 2 11 1.73 0.76 -5 -3 11 -0.79 1.36 -5 -3 11 -1.61 1.00 5 3 11 0.39 0.72 -5 -4 11 2.99 1.31 -5 -4 11 6.35 1.30 5 4 11 3.00 0.88 -5 -5 11 -0.06 1.39 -5 -5 11 -0.68 1.02 5 5 11 -1.02 0.78 -5 -6 11 5.36 1.34 -5 -6 11 3.71 1.01 5 6 11 2.86 0.89 -5 -7 11 -1.07 1.42 -5 -7 11 -0.46 0.96 5 7 11 -0.06 0.79 5 8 11 1.02 0.85 -5 -8 11 0.93 0.93 5 9 11 2.82 1.00 6 -7 11 4.22 1.11 6 -6 11 0.97 0.90 6 -5 11 1.10 0.98 6 -4 11 3.33 0.96 6 4 -11 3.43 0.96 6 -3 11 0.82 0.82 6 3 -11 0.98 0.86 -6 2 11 1.74 1.02 6 -2 11 0.98 0.80 6 2 -11 1.15 0.87 -6 2 11 0.19 1.21 -6 1 11 16.02 1.88 6 -1 11 15.97 1.76 6 1 -11 13.81 1.78 -6 1 11 11.66 2.01 -6 0 11 1.13 1.31 -6 0 11 0.93 0.92 6 0 11 0.22 0.67 6 0 -11 0.02 0.77 -6 -1 11 15.35 1.91 -6 -2 11 2.55 1.32 -6 -2 11 0.81 0.89 -6 -3 11 0.69 1.45 -6 -3 11 0.27 0.92 6 3 11 -0.56 0.73 -6 -4 11 2.76 1.43 -6 -4 11 5.40 1.07 6 4 11 3.25 0.91 -6 -5 11 0.03 1.36 -6 -5 11 -0.77 0.92 6 5 11 0.02 0.80 -6 -6 11 -1.06 1.37 -6 -6 11 1.05 0.95 6 6 11 1.05 0.81 -6 -7 11 6.06 1.09 6 7 11 4.85 1.01 6 8 11 1.08 0.79 7 -6 11 0.92 1.00 7 -5 11 3.50 1.09 7 -4 11 0.53 0.87 7 -3 11 0.11 0.87 7 3 -11 -0.43 0.86 7 -2 11 0.81 0.79 7 2 -11 0.52 0.84 7 -2 11 -0.75 1.31 7 -1 11 0.81 0.78 7 1 -11 -0.21 0.80 -7 1 11 -1.26 1.28 7 0 -11 0.61 0.82 -7 0 11 1.11 1.31 -7 -1 11 1.20 1.43 -7 -4 11 -0.11 1.48 7 4 11 -0.42 0.80 -7 -5 11 3.10 1.56 7 5 11 2.57 0.85 7 6 11 0.43 0.84 7 7 11 1.54 0.88 8 -5 11 -1.07 0.99 8 -4 11 0.34 0.94 8 -3 11 1.90 0.99 8 -2 11 -0.35 0.89 8 1 -11 2.69 0.91 -8 1 11 4.70 1.52 -8 0 11 0.55 1.35 -8 -1 11 1.84 1.50 -8 -2 11 0.45 1.52 -8 -3 11 1.20 1.54 8 4 11 0.63 0.75 8 5 11 -0.27 0.78 8 6 11 0.57 0.77 9 -4 11 2.31 1.05 9 -3 11 3.07 1.07 -9 0 11 -1.73 1.56 -9 -1 11 0.86 1.48 -9 -2 11 2.59 1.59 0 0 12 -0.09 0.88 0 -1 12 -0.44 0.95 0 1 12 0.70 0.92 0 -2 12 0.30 0.95 0 2 12 -0.16 0.91 0 -3 12 -0.04 0.94 0 3 -12 -0.45 0.86 0 -4 12 2.08 1.06 0 4 -12 2.70 1.00 0 -5 12 0.75 1.00 0 5 -12 0.47 0.97 0 -6 12 5.62 1.27 0 -7 12 -2.46 1.19 1 -7 12 0.64 1.05 1 -6 12 4.80 1.19 1 -5 12 0.49 0.92 1 5 -12 0.02 0.92 1 -4 12 5.05 1.14 1 4 -12 6.44 1.15 1 -3 12 -0.86 0.95 1 3 -12 0.19 0.90 1 -2 12 15.01 1.89 1 -1 12 0.26 0.90 1 0 12 32.87 3.64 -1 -1 12 0.85 0.99 1 1 12 1.59 0.89 -1 -2 12 13.62 2.14 1 2 12 19.65 2.05 -1 -3 12 -0.31 1.02 -1 -4 12 5.66 1.33 -1 4 -12 7.18 1.17 -1 -5 12 -0.80 1.06 -1 5 -12 0.15 1.01 -1 -6 12 5.68 1.34 2 -6 12 1.88 1.03 2 -5 12 3.23 1.03 2 5 -12 2.62 0.97 2 -4 12 1.96 0.96 2 4 -12 1.96 0.94 2 -3 12 2.90 0.94 2 3 -12 2.19 0.91 2 -2 12 1.31 0.82 -2 -1 12 -0.28 1.09 -2 -2 12 1.33 1.07 -2 -3 12 3.09 1.25 -2 -4 12 0.64 1.10 -2 -5 12 2.07 1.13 -2 -6 12 1.63 1.27 3 -6 12 3.61 1.12 3 -5 12 4.11 1.10 3 -4 12 0.68 0.91 3 4 -12 0.02 0.97 3 -3 12 2.11 0.94 3 3 -12 2.72 0.96 3 -2 12 3.64 0.93 -3 -1 12 3.87 1.25 -3 -2 12 3.99 1.29 -3 -3 12 4.06 1.31 -3 -4 12 -0.11 1.23 -3 -5 12 4.19 1.34 -3 -6 12 2.22 1.23 4 -6 12 -0.46 0.98 4 -5 12 3.93 1.10 4 -4 12 1.24 0.94 4 -3 12 7.42 1.15 4 3 -12 5.39 1.13 -4 -1 12 -0.23 1.29 -4 -2 12 1.68 1.32 -4 -3 12 4.59 1.38 -4 -4 12 2.13 1.45 -4 -5 12 2.61 1.36 5 -5 12 3.03 1.03 5 -4 12 -0.04 1.00 -5 -2 12 0.51 1.41 -5 -3 12 1.35 1.51 -5 -4 12 -2.33 1.55 -5 -5 12 3.63 1.57 6 -5 12 -0.30 1.03 -6 -3 12 0.76 1.52 -6 -4 12 -0.96 1.53 -7 -2 12 2.57 1.61 0 0 0 0.00 0.00 TITL T4 in P222 REM P222 (#16 in standard setting) CELL 0.71073 9.733105 12.730414 14.663567 90.0000 90.0000 90.0000 ZERR 26.00 0.000397 0.000577 0.000644 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z SYMM -x, y,-z SYMM x,-y,-z SFAC C H B O Si UNIT 26.00 26.00 26.00 26.00 26.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 88494 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.289 _oxdiff_exptl_absorpt_empirical_full_min 0.540 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si01 Si 0.68712(8) 0.250000 0.67708(10) 0.0348(4) Uani 0.5 2 d S TU P A 1 H01 H 0.630261 0.250000 0.747965 0.042 Uiso 0.5 2 calc RS T P A 1 Si02 Si 0.75673(10) 0.250000 0.60499(14) 0.0530(4) Uani 0.5 2 d S TU P A 2 H02 H 0.826045 0.250000 0.556657 0.064 Uiso 0.5 2 calc RS T P A 2 C003 C 0.75539(17) 0.36141(13) 0.6991(2) 0.0596(5) Uani 1 1 d . U . . . C10 C 0.8193(3) 0.3682(2) 0.8305(3) 0.0933(9) Uani 1 1 d . U . . . H10A H 0.780209 0.339918 0.906153 0.140 Uiso 1 1 calc GR . . . . H10B H 0.832418 0.432456 0.851978 0.140 Uiso 1 1 calc GR . . . . H10C H 0.886392 0.336460 0.818294 0.140 Uiso 1 1 calc GR . . . . C005 C 0.547(2) 0.1950(19) 0.269(3) 0.050(4) Uani 0.25 1 d . U . B -3 B1 B 0.6106(6) 0.250000 0.4938(7) 0.0398(14) Uani 0.5 2 d S TU P A 1 O007 O 0.6520(11) 0.2028(10) 0.3823(12) 0.067(3) Uani 0.25 1 d . U . B -3 O008 O 0.5222(6) 0.2094(8) 0.4708(10) 0.0575(19) Uani 0.25 1 d . U . A -2 C009 C 0.6809(4) 0.4379(3) 0.6875(6) 0.0765(13) Uani 0.5 1 d . U . A 1 H00A H 0.647875 0.436916 0.596592 0.115 Uiso 0.5 1 calc GR . . A 1 H00B H 0.718613 0.495649 0.699765 0.115 Uiso 0.5 1 calc GR . . A 1 H00C H 0.626742 0.432178 0.758517 0.115 Uiso 0.5 1 calc GR . . A 1 C00A C 0.8438(4) 0.3746(3) 0.5840(5) 0.0775(13) Uani 0.5 1 d . U . A 1 H00D H 0.897467 0.327184 0.594267 0.116 Uiso 0.5 1 calc GR . . A 1 H00E H 0.876414 0.434778 0.594652 0.116 Uiso 0.5 1 calc GR . . A 1 H00F H 0.811793 0.370058 0.492752 0.116 Uiso 0.5 1 calc GR . . A 1 C00B C 0.3925(15) 0.2152(17) 0.3059(18) 0.058(3) Uani 0.25 1 d . U . A -2 H00P H 0.364820 0.164519 0.360709 0.087 Uiso 0.25 1 calc GR . . A -2 H00Q H 0.370438 0.207960 0.210054 0.087 Uiso 0.25 1 calc GR . . A -2 H00R H 0.365377 0.272944 0.341985 0.087 Uiso 0.25 1 calc GR . . A -2 C00C C 0.6050(12) 0.2025(15) 0.1369(13) 0.073(4) Uani 0.25 1 d . U . B -3 H00M H 0.657264 0.251366 0.143499 0.109 Uiso 0.25 1 calc GR . . B -3 H00N H 0.555340 0.216495 0.062861 0.109 Uiso 0.25 1 calc GR . . B -3 H00O H 0.640369 0.144643 0.117153 0.109 Uiso 0.25 1 calc GR . . B -3 C00D C 0.562(2) 0.134(2) 0.216(3) 0.100(8) Uani 0.25 1 d . U . A -2 H00S H 0.508933 0.115022 0.148864 0.149 Uiso 0.25 1 calc GR . . A -2 H00T H 0.580687 0.081362 0.273984 0.149 Uiso 0.25 1 calc GR . . A -2 H00U H 0.624395 0.156120 0.168717 0.149 Uiso 0.25 1 calc GR . . A -2 C00E C 0.6329(5) 0.3751(5) 0.7614(9) 0.121(2) Uani 0.5 1 d . U . A 2 H00G H 0.584771 0.389246 0.685696 0.182 Uiso 0.5 1 calc GR . . A 2 H00H H 0.632392 0.425359 0.827805 0.182 Uiso 0.5 1 calc GR . . A 2 H00I H 0.610298 0.318831 0.806797 0.182 Uiso 0.5 1 calc GR . . A 2 C00F C 0.7670(8) 0.4374(5) 0.6003(8) 0.135(3) Uani 0.5 1 d . U . A 2 H00J H 0.838590 0.437579 0.563335 0.202 Uiso 0.5 1 calc GR . . A 2 H00K H 0.753281 0.495354 0.647051 0.202 Uiso 0.5 1 calc GR . . A 2 H00L H 0.716713 0.429559 0.524897 0.202 Uiso 0.5 1 calc GR . . A 2 C2 C 0.513(2) 0.2153(18) 0.314(4) 0.053(4) Uani 0.25 1 d . U . A -2 C1 C 0.5041(19) 0.1158(11) 0.299(3) 0.072(5) Uani 0.25 1 d . U . B -3 H1A H 0.490135 0.112713 0.397705 0.108 Uiso 0.25 1 calc GR . . B -3 H1B H 0.551980 0.066434 0.272685 0.108 Uiso 0.25 1 calc GR . . B -3 H1C H 0.437903 0.109317 0.248234 0.108 Uiso 0.25 1 calc GR . . B -3 B2 B 0.6500(7) 0.250000 0.4491(12) 0.0516(15) Uani 0.5 2 d S TU P A 2 O0 O 0.5608(7) 0.2016(9) 0.4435(11) 0.073(3) Uani 0.25 1 d . U . A -1 O1 O 0.6457(14) 0.1848(9) 0.3520(13) 0.071(3) Uani 0.25 1 d . U . C -4 C3 C 0.595(2) 0.1818(17) 0.1074(17) 0.090(5) Uani 0.25 1 d . U . C -4 H3A H 0.650480 0.222167 0.074597 0.136 Uiso 0.25 1 calc GR . . C -4 H3B H 0.530932 0.191718 0.052665 0.136 Uiso 0.25 1 calc GR . . C -4 H3C H 0.617001 0.118149 0.098238 0.136 Uiso 0.25 1 calc GR . . C -4 C4 C 0.553(2) 0.1289(18) 0.254(3) 0.084(5) Uani 0.25 1 d . U . A -1 H4A H 0.531567 0.123844 0.157331 0.126 Uiso 0.25 1 calc GR . . A -1 H4B H 0.533770 0.073219 0.302964 0.126 Uiso 0.25 1 calc GR . . A -1 H4C H 0.629613 0.137292 0.258222 0.126 Uiso 0.25 1 calc GR . . A -1 C0 C 0.5688(16) 0.2047(19) 0.275(3) 0.054(4) Uani 0.25 1 d . U . C -4 C1A C 0.484(3) 0.114(2) 0.302(3) 0.117(9) Uani 0.25 1 d . U . C -4 H1AA H 0.524749 0.057296 0.309699 0.176 Uiso 0.25 1 calc GR . . C -4 H1AB H 0.435104 0.108954 0.224671 0.176 Uiso 0.25 1 calc GR . . C -4 H1AC H 0.444612 0.123876 0.387073 0.176 Uiso 0.25 1 calc GR . . C -4 C2A C 0.500(2) 0.209(2) 0.318(4) 0.063(4) Uani 0.25 1 d . U . A -1 C5 C 0.390(2) 0.197(2) 0.311(3) 0.111(9) Uani 0.25 1 d . U . A -1 H5A H 0.372704 0.132986 0.326079 0.167 Uiso 0.25 1 calc GR . . A -1 H5B H 0.364669 0.216448 0.220660 0.167 Uiso 0.25 1 calc GR . . A -1 H5C H 0.356032 0.234487 0.382427 0.167 Uiso 0.25 1 calc GR . . A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si01 0.0310(6) 0.0423(6) 0.0312(6) 0.000 0.0017(4) 0.000 Si02 0.0425(7) 0.0662(9) 0.0503(8) 0.000 -0.0024(5) 0.000 C003 0.0733(12) 0.0510(9) 0.0544(11) -0.0034(7) -0.0106(8) -0.0044(8) C10 0.112(2) 0.0842(16) 0.0836(17) -0.0069(12) -0.0367(15) -0.0213(14) C005 0.047(11) 0.057(8) 0.045(6) 0.005(6) -0.017(6) -0.014(7) B1 0.030(3) 0.046(3) 0.044(3) 0.000 0.004(2) 0.000 O007 0.052(4) 0.095(8) 0.054(5) -0.032(4) -0.031(4) 0.011(4) O008 0.040(4) 0.079(4) 0.053(3) 0.014(3) -0.012(3) -0.017(3) C009 0.083(3) 0.0459(19) 0.100(4) -0.008(2) -0.009(2) 0.0039(18) C00A 0.088(3) 0.065(2) 0.079(3) -0.0077(19) 0.025(2) -0.033(2) C00B 0.046(5) 0.085(6) 0.043(5) -0.004(4) 0.004(3) -0.024(4) C00C 0.047(4) 0.133(12) 0.037(5) -0.026(5) 0.003(4) 0.017(5) C00D 0.095(11) 0.092(12) 0.112(13) -0.039(10) -0.010(9) 0.037(9) C00E 0.106(4) 0.117(5) 0.141(6) -0.057(4) 0.012(4) 0.026(4) C00F 0.221(9) 0.069(3) 0.114(5) 0.022(3) -0.051(5) -0.042(5) C2 0.039(7) 0.060(8) 0.059(6) -0.012(6) -0.012(5) 0.003(6) C1 0.096(11) 0.037(5) 0.084(11) 0.002(6) -0.043(7) -0.017(6) B2 0.042(4) 0.054(4) 0.059(5) 0.000 -0.019(3) 0.000 O0 0.068(7) 0.078(4) 0.073(6) 0.026(4) -0.028(5) -0.016(5) O1 0.089(5) 0.057(4) 0.066(6) -0.021(4) -0.052(5) 0.015(4) C3 0.106(11) 0.117(11) 0.048(6) -0.025(7) -0.001(6) 0.020(8) C4 0.091(10) 0.061(9) 0.100(12) -0.012(7) -0.044(8) -0.026(7) C0 0.028(6) 0.080(9) 0.053(5) -0.016(5) -0.016(5) 0.001(5) C1A 0.159(16) 0.113(14) 0.079(11) -0.003(9) -0.021(10) -0.079(12) C2A 0.065(9) 0.069(7) 0.054(6) 0.013(5) -0.009(7) -0.027(7) C5 0.070(7) 0.17(2) 0.093(11) 0.039(11) -0.019(7) -0.032(10) 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' 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 C003 Si01 H01 105.0 7_565 . ? C003 Si01 H01 105.0 . . ? C003 Si01 C003 122.57(14) . 7_565 ? C003 Si01 B1 108.93(11) . . ? C003 Si01 B1 108.93(11) 7_565 . ? B1 Si01 H01 105.0 . . ? C003 Si02 H02 103.8 7_565 . ? C003 Si02 H02 103.8 . . ? C003 Si02 C003 121.46(14) . 7_565 ? C003 Si02 B2 110.99(14) . . ? C003 Si02 B2 110.99(15) 7_565 . ? B2 Si02 H02 103.8 . . ? C10 C003 Si01 113.80(16) . . ? C10 C003 Si02 117.62(17) . . ? C10 C003 C00A 101.8(3) . . ? C10 C003 C00E 100.6(3) . . ? C009 C003 Si01 111.0(2) . . ? C009 C003 C10 111.0(3) . . ? C009 C003 C00A 107.9(3) . . ? C00A C003 Si01 110.75(19) . . ? C00E C003 Si02 106.8(3) . . ? C00F C003 Si02 109.8(3) . . ? C00F C003 C10 116.4(3) . . ? C00F C003 C00E 103.7(6) . . ? C003 C10 H10A 109.5 . . ? C003 C10 H10B 109.5 . . ? C003 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C00C C005 O007 99.6(16) . . ? C1 C005 O007 103.8(16) . . ? C1 C005 C00C 118(3) . . ? O0 B1 Si01 133.3(7) . . ? C2 O008 B2 85.9(11) . . ? C003 C009 H00A 109.5 . . ? C003 C009 H00B 109.5 . . ? C003 C009 H00C 109.5 . . ? H00A C009 H00B 109.5 . . ? H00A C009 H00C 109.5 . . ? H00B C009 H00C 109.5 . . ? C003 C00A H00D 109.5 . . ? C003 C00A H00E 109.5 . . ? C003 C00A H00F 109.5 . . ? H00D C00A H00E 109.5 . . ? H00D C00A H00F 109.5 . . ? H00E C00A H00F 109.5 . . ? H00P C00B H00Q 109.5 . . ? H00P C00B H00R 109.5 . . ? H00Q C00B H00R 109.5 . . ? C2 C00B H00P 109.5 . . ? C2 C00B H00Q 109.5 . . ? C2 C00B H00R 109.5 . . ? C005 C00C H00M 109.5 . . ? C005 C00C H00N 109.5 . . ? C005 C00C H00O 109.5 . . ? H00M C00C H00N 109.5 . . ? H00M C00C H00O 109.5 . . ? H00N C00C H00O 109.5 . . ? H00S C00D H00T 109.5 . . ? H00S C00D H00U 109.5 . . ? H00T C00D H00U 109.5 . . ? C2 C00D H00S 109.5 . . ? C2 C00D H00T 109.5 . . ? C2 C00D H00U 109.5 . . ? C003 C00E H00G 109.5 . . ? C003 C00E H00H 109.5 . . ? C003 C00E H00I 109.5 . . ? H00G C00E H00H 109.5 . . ? H00G C00E H00I 109.5 . . ? H00H C00E H00I 109.5 . . ? C003 C00F H00J 109.5 . . ? C003 C00F H00K 109.5 . . ? C003 C00F H00L 109.5 . . ? H00J C00F H00K 109.5 . . ? H00J C00F H00L 109.5 . . ? H00K C00F H00L 109.5 . . ? O008 C2 C00B 97.0(19) . . ? O008 C2 C00D 120(2) . . ? C00B C2 C00D 110(2) . . ? C005 C1 H1A 109.5 . . ? C005 C1 H1B 109.5 . . ? C005 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O008 B2 Si02 122.1(7) . . ? B1 O0 C2A 130.6(16) . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C0 C3 H3A 109.5 . . ? C0 C3 H3B 109.5 . . ? C0 C3 H3C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2A C4 H4A 109.5 . . ? C2A C4 H4B 109.5 . . ? C2A C4 H4C 109.5 . . ? O1 C0 C3 112(2) . . ? O1 C0 C1A 102(2) . . ? C3 C0 C1A 96.6(19) . . ? C0 C1A H1AA 109.5 . . ? C0 C1A H1AB 109.5 . . ? C0 C1A H1AC 109.5 . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? O0 C2A C4 93(2) . . ? C5 C2A O0 124(3) . . ? C5 C2A C4 109(3) . . ? C2A C5 H5A 109.5 . . ? C2A C5 H5B 109.5 . . ? C2A C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? 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 Si01 H01 1.0000 . ? Si01 C003 1.8628(19) 7_565 ? Si01 C003 1.8628(19) . ? Si01 B1 2.033(7) . ? Si02 H02 1.0000 . ? Si02 C003 1.873(2) . ? Si02 C003 1.873(2) 7_565 ? Si02 B2 2.036(7) . ? C003 C10 1.520(3) . ? C003 C009 1.473(5) . ? C003 C00A 1.600(5) . ? C003 C00E 1.685(7) . ? C003 C00F 1.479(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C005 O007 1.73(3) . ? C005 C00C 1.48(4) . ? C005 C1 1.32(3) . ? B1 O0 1.070(13) . ? O008 C2 1.54(4) . ? O008 B2 1.746(13) . ? C009 H00A 0.9800 . ? C009 H00B 0.9800 . ? C009 H00C 0.9800 . ? C00A H00D 0.9800 . ? C00A H00E 0.9800 . ? C00A H00F 0.9800 . ? C00B H00P 0.9800 . ? C00B H00Q 0.9800 . ? C00B H00R 0.9800 . ? C00B C2 1.54(3) . ? C00C H00M 0.9800 . ? C00C H00N 0.9800 . ? C00C H00O 0.9800 . ? C00D H00S 0.9800 . ? C00D H00T 0.9800 . ? C00D H00U 0.9800 . ? C00D C2 1.64(4) . ? C00E H00G 0.9800 . ? C00E H00H 0.9800 . ? C00E H00I 0.9800 . ? C00F H00J 0.9800 . ? C00F H00K 0.9800 . ? C00F H00L 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O0 C2A 1.45(4) . ? O1 C0 1.27(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3 C0 1.69(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4 C2A 1.50(5) . ? C0 C1A 1.74(4) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C2A C5 1.41(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? 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 Si01 B1 O0 C2A 173(2) . . . . ? C003 Si01 C003 C10 -48.9(3) 7_565 . . . ? C003 Si01 C003 C009 -175.1(2) 7_565 . . . ? C003 Si01 C003 C00A 65.0(3) 7_565 . . . ? C003 Si02 C003 C10 38.4(3) 7_565 . . . ? C003 Si02 C003 C00E -73.6(4) 7_565 . . . ? C003 Si02 C003 C00F 174.7(4) 7_565 . . . ? B1 Si01 C003 C10 -177.7(3) . . . . ? B1 Si01 C003 C009 56.1(3) . . . . ? B1 Si01 C003 C00A -63.7(3) . . . . ? B1 O0 C2A C4 123(2) . . . . ? B1 O0 C2A C5 -121(3) . . . . ? C2 O008 B2 Si02 -168.8(10) . . . . ? B2 Si02 C003 C10 171.6(4) . . . . ? B2 Si02 C003 C00E 59.6(5) . . . . ? B2 Si02 C003 C00F -52.2(6) . . . . ? B2 O008 C2 C00B -160.7(15) . . . . ? B2 O008 C2 C00D 81(2) . . . . ?