#------------------------------------------------------------------------------ #$Date: 2020-08-29 04:48:03 +0300 (Sat, 29 Aug 2020) $ #$Revision: 255731 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705318.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_7705318 loop_ _publ_author_name 'Leszczy\'nska, Kinga I.' 'Deglmann, Peter' 'Pr\"asang, Carsten' 'Huch, Volker' 'Zimmer, Michael' 'Schweinfurth, David' 'Scheschkewitz, David' _publ_section_title ; Pentamethylcyclopentadienyl-substituted hypersilylsilylene: reversible and irreversible activation of C=C double bonds and dihydrogen ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02943B _journal_year 2020 _chemical_formula_moiety 'C19 H42 Si5' _chemical_formula_sum 'C19 H42 Si5' _chemical_formula_weight 410.97 _chemical_properties_physical Air-sensitive,Moisture-sensitive _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-05-07 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 89.447(2) _cell_angle_beta 89.918(2) _cell_angle_gamma 87.141(2) _cell_formula_units_Z 2 _cell_length_a 9.0809(7) _cell_length_b 9.9667(9) _cell_length_c 14.8247(13) _cell_measurement_reflns_used 8746 _cell_measurement_temperature 152(2) _cell_measurement_theta_max 32.56 _cell_measurement_theta_min 2.45 _cell_volume 1340.0(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 152(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_unetI/netI 0.0253 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 31847 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.651 _diffrn_reflns_theta_min 1.374 _exptl_absorpt_coefficient_mu 0.268 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_correction_T_min 0.6930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.019 _exptl_crystal_description block _exptl_crystal_F_000 452 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.603 _exptl_crystal_size_mid 0.404 _exptl_crystal_size_min 0.188 _refine_diff_density_max 0.695 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.064 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 231 _refine_ls_number_reflns 9747 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0497 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+1.4996P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1290 _refine_ls_wR_factor_ref 0.1327 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8254 _reflns_number_total 9747 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02943b2.cif _cod_data_source_block sh3832 _cod_database_code 7705318 _shelx_shelxl_version_number 2018/3 _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_min 0.855 _shelx_estimated_absorpt_t_max 0.951 _shelx_res_file ; TITL sh3832 in P-1 sh3832.res created by SHELXL-2018/3 at 13:24:28 on 05-May-2020 CELL 0.71073 9.0809 9.9667 14.8247 89.447 89.918 87.141 ZERR 2.000 0.0007 0.0009 0.0013 0.002 0.002 0.002 LATT 1 SFAC C H Si UNIT 38 84 10 L.S. 10 BOND $H FMAP 2 PLAN -5 OMIT -4 2 4 OMIT 3 2 2 OMIT 0 3 1 OMIT 0 5 2 OMIT 4 3 3 OMIT -2 1 2 ACTA SIZE 0.188 0.404 0.603 TEMP -120.500 WGHT 0.036900 1.499600 FVAR 0.87188 SI1 3 0.844663 0.405323 0.761976 11.00000 0.02335 0.01744 = 0.03405 0.00017 -0.00443 -0.00210 SI2 3 0.657720 0.239716 0.743179 11.00000 0.01897 0.01787 = 0.02287 -0.00025 -0.00169 -0.00157 SI3 3 0.730892 0.108062 0.869419 11.00000 0.03040 0.02922 = 0.02746 0.00770 -0.00475 -0.00602 SI4 3 0.744700 0.125056 0.614459 11.00000 0.02474 0.02563 = 0.02761 -0.00719 -0.00261 -0.00033 SI5 3 0.398085 0.243055 0.739907 11.00000 0.01877 0.03305 = 0.03672 -0.00197 -0.00091 -0.00100 C1 1 0.732955 0.587291 0.796261 11.00000 0.03096 0.01822 = 0.05311 -0.00083 0.00434 -0.00103 C2 1 0.864628 0.633483 0.836895 11.00000 0.03769 0.02568 = 0.03215 -0.00268 -0.00088 -0.00141 C3 1 0.965968 0.658544 0.769340 11.00000 0.02959 0.01990 = 0.03905 -0.00396 -0.00116 -0.00401 C4 1 0.905550 0.626098 0.686465 11.00000 0.04565 0.02354 = 0.03215 -0.00020 -0.00054 0.00062 C5 1 0.758661 0.584167 0.700098 11.00000 0.04201 0.01769 = 0.04484 0.00146 -0.01602 -0.00270 C6 1 0.584245 0.581008 0.840993 11.00000 0.03867 0.03413 = 0.10340 -0.00953 0.02552 -0.00460 AFIX 137 H6A 2 0.597021 0.548347 0.903192 11.00000 -1.50000 H6B 2 0.523705 0.519690 0.807635 11.00000 -1.50000 H6C 2 0.535331 0.670903 0.841234 11.00000 -1.50000 AFIX 0 C7 1 0.888668 0.648746 0.935884 11.00000 0.07919 0.06141 = 0.03334 -0.00926 0.00045 0.00086 AFIX 137 H7A 2 0.987986 0.613332 0.951725 11.00000 -1.50000 H7B 2 0.815553 0.598869 0.969288 11.00000 -1.50000 H7C 2 0.878232 0.744047 0.951560 11.00000 -1.50000 AFIX 0 C8 1 1.122546 0.695143 0.784492 11.00000 0.03295 0.03910 = 0.07604 -0.00877 -0.00122 -0.00888 AFIX 137 H8A 2 1.125328 0.761698 0.832612 11.00000 -1.50000 H8B 2 1.161994 0.733016 0.728746 11.00000 -1.50000 H8C 2 1.182401 0.614576 0.801996 11.00000 -1.50000 AFIX 0 C9 1 0.982216 0.635549 0.597230 11.00000 0.08122 0.05765 = 0.03796 0.00351 0.01273 -0.00008 AFIX 137 H9A 2 1.024287 0.723835 0.591091 11.00000 -1.50000 H9B 2 0.911250 0.623829 0.548540 11.00000 -1.50000 H9C 2 1.061254 0.565162 0.593694 11.00000 -1.50000 AFIX 0 C10 1 0.644709 0.574064 0.627949 11.00000 0.07247 0.03198 = 0.07807 0.01206 -0.04720 -0.01058 AFIX 137 H10A 2 0.592902 0.661809 0.619059 11.00000 -1.50000 H10B 2 0.573906 0.507783 0.646070 11.00000 -1.50000 H10C 2 0.692714 0.545987 0.571482 11.00000 -1.50000 AFIX 0 C11 1 0.929083 0.046745 0.860567 11.00000 0.03631 0.05206 = 0.05620 0.01941 -0.01182 0.00362 AFIX 137 H11A 2 0.991423 0.123764 0.854216 11.00000 -1.50000 H11B 2 0.941939 -0.011057 0.807747 11.00000 -1.50000 H11C 2 0.957396 -0.004498 0.915116 11.00000 -1.50000 AFIX 0 C12 1 0.618042 -0.043626 0.886766 11.00000 0.05711 0.03791 = 0.04921 0.01741 -0.00440 -0.01641 AFIX 137 H12A 2 0.651873 -0.092402 0.941211 11.00000 -1.50000 H12B 2 0.629624 -0.102646 0.834476 11.00000 -1.50000 H12C 2 0.513919 -0.014747 0.893637 11.00000 -1.50000 AFIX 0 C13 1 0.710421 0.213854 0.973019 11.00000 0.06599 0.06249 = 0.02831 -0.00132 -0.00628 -0.01533 AFIX 137 H13A 2 0.606609 0.243177 0.980838 11.00000 -1.50000 H13B 2 0.770035 0.292680 0.966508 11.00000 -1.50000 H13C 2 0.743921 0.160996 1.025858 11.00000 -1.50000 AFIX 0 C14 1 0.948405 0.138323 0.603457 11.00000 0.02903 0.07341 = 0.04337 -0.01602 0.00731 -0.00352 AFIX 137 H14A 2 0.998050 0.089269 0.653307 11.00000 -1.50000 H14B 2 0.972382 0.233041 0.605327 11.00000 -1.50000 H14C 2 0.981658 0.099618 0.545965 11.00000 -1.50000 AFIX 0 C15 1 0.708694 -0.058170 0.615470 11.00000 0.05605 0.02998 = 0.06590 -0.01625 0.00751 -0.00396 AFIX 137 H15A 2 0.746440 -0.099122 0.559659 11.00000 -1.50000 H15B 2 0.602338 -0.069482 0.619925 11.00000 -1.50000 H15C 2 0.758446 -0.101874 0.667356 11.00000 -1.50000 AFIX 0 C16 1 0.657136 0.202886 0.510632 11.00000 0.05753 0.05752 = 0.02754 -0.00780 -0.00988 0.00622 AFIX 137 H16A 2 0.673292 0.299373 0.509276 11.00000 -1.50000 H16B 2 0.551026 0.189169 0.511485 11.00000 -1.50000 H16C 2 0.701367 0.160759 0.456919 11.00000 -1.50000 AFIX 0 C17 1 0.316678 0.286145 0.852821 11.00000 0.03394 0.06525 = 0.04902 -0.00758 0.01337 -0.00882 AFIX 137 H17A 2 0.209225 0.297628 0.847482 11.00000 -1.50000 H17B 2 0.356329 0.369849 0.874089 11.00000 -1.50000 H17C 2 0.341907 0.213493 0.895941 11.00000 -1.50000 AFIX 0 C18 1 0.311055 0.363843 0.655154 11.00000 0.02791 0.05782 = 0.06343 0.01081 -0.00914 0.00486 AFIX 137 H18A 2 0.204200 0.354167 0.654362 11.00000 -1.50000 H18B 2 0.351790 0.344398 0.595169 11.00000 -1.50000 H18C 2 0.331789 0.455955 0.671731 11.00000 -1.50000 AFIX 0 C19 1 0.337882 0.071720 0.709070 11.00000 0.03050 0.04580 = 0.07533 -0.00849 -0.01202 -0.00907 AFIX 137 H19A 2 0.393790 0.003329 0.744682 11.00000 -1.50000 H19B 2 0.356063 0.056382 0.644725 11.00000 -1.50000 H19C 2 0.232403 0.066117 0.721726 11.00000 -1.50000 AFIX 0 HKLF 4 1 -1 0 0 0 1 0 0 0 -1 REM sh3832 in P-1 REM wR2 = 0.132702, GooF = S = 1.07828, Restrained GooF = 1.07828 for all data REM R1 = 0.049688 for 8254 Fo > 4sig(Fo) and 0.058594 for all 9747 data REM 231 parameters refined using 0 restraints END WGHT 0.0431 1.3211 REM Highest difference peak 0.695, deepest hole -0.300, 1-sigma level 0.064 Q1 1 0.7367 0.1404 0.9246 11.00000 0.05 0.70 Q2 1 0.5834 0.5788 0.6799 11.00000 0.05 0.56 Q3 1 0.8425 0.4056 0.7079 11.00000 0.05 0.53 Q4 1 0.7264 0.1094 0.6614 11.00000 0.05 0.50 Q5 1 0.3980 0.2463 0.7960 11.00000 0.05 0.49 ; _shelx_res_checksum 7832 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Si1 Si 0.84466(5) 0.40532(5) 0.76198(4) 0.02491(10) Uani 1 1 d . . . . . Si2 Si 0.65772(5) 0.23972(4) 0.74318(3) 0.01988(9) Uani 1 1 d . . . . . Si3 Si 0.73089(6) 0.10806(5) 0.86942(4) 0.02892(11) Uani 1 1 d . . . . . Si4 Si 0.74470(6) 0.12506(5) 0.61446(3) 0.02598(10) Uani 1 1 d . . . . . Si5 Si 0.39808(5) 0.24306(6) 0.73991(4) 0.02951(11) Uani 1 1 d . . . . . C1 C 0.7330(2) 0.58729(18) 0.79626(16) 0.0341(4) Uani 1 1 d . . . . . C2 C 0.8646(2) 0.63348(19) 0.83690(13) 0.0318(4) Uani 1 1 d . . . . . C3 C 0.9660(2) 0.65854(17) 0.76934(14) 0.0294(3) Uani 1 1 d . . . . . C4 C 0.9055(2) 0.62610(19) 0.68646(14) 0.0339(4) Uani 1 1 d . . . . . C5 C 0.7587(2) 0.58417(18) 0.70010(15) 0.0348(4) Uani 1 1 d . . . . . C6 C 0.5842(3) 0.5810(3) 0.8410(2) 0.0586(8) Uani 1 1 d . . . . . H6A H 0.597021 0.548347 0.903192 0.088 Uiso 1 1 calc R U . . . H6B H 0.523705 0.519690 0.807635 0.088 Uiso 1 1 calc R U . . . H6C H 0.535331 0.670903 0.841234 0.088 Uiso 1 1 calc R U . . . C7 C 0.8887(4) 0.6487(3) 0.93588(17) 0.0581(7) Uani 1 1 d . . . . . H7A H 0.987986 0.613332 0.951725 0.087 Uiso 1 1 calc R U . . . H7B H 0.815553 0.598869 0.969288 0.087 Uiso 1 1 calc R U . . . H7C H 0.878232 0.744047 0.951560 0.087 Uiso 1 1 calc R U . . . C8 C 1.1225(3) 0.6951(2) 0.7845(2) 0.0491(6) Uani 1 1 d . . . . . H8A H 1.125328 0.761698 0.832612 0.074 Uiso 1 1 calc R U . . . H8B H 1.161994 0.733016 0.728746 0.074 Uiso 1 1 calc R U . . . H8C H 1.182401 0.614576 0.801996 0.074 Uiso 1 1 calc R U . . . C9 C 0.9822(4) 0.6355(3) 0.59723(18) 0.0591(7) Uani 1 1 d . . . . . H9A H 1.024287 0.723835 0.591091 0.089 Uiso 1 1 calc R U . . . H9B H 0.911250 0.623829 0.548540 0.089 Uiso 1 1 calc R U . . . H9C H 1.061254 0.565162 0.593694 0.089 Uiso 1 1 calc R U . . . C10 C 0.6447(3) 0.5741(2) 0.6279(2) 0.0606(8) Uani 1 1 d . . . . . H10A H 0.592902 0.661809 0.619059 0.091 Uiso 1 1 calc R U . . . H10B H 0.573906 0.507783 0.646070 0.091 Uiso 1 1 calc R U . . . H10C H 0.692714 0.545987 0.571482 0.091 Uiso 1 1 calc R U . . . C11 C 0.9291(3) 0.0467(3) 0.86057(19) 0.0485(6) Uani 1 1 d . . . . . H11A H 0.991423 0.123764 0.854216 0.073 Uiso 1 1 calc R U . . . H11B H 0.941939 -0.011057 0.807747 0.073 Uiso 1 1 calc R U . . . H11C H 0.957396 -0.004498 0.915116 0.073 Uiso 1 1 calc R U . . . C12 C 0.6180(3) -0.0436(2) 0.88677(18) 0.0477(6) Uani 1 1 d . . . . . H12A H 0.651873 -0.092402 0.941211 0.072 Uiso 1 1 calc R U . . . H12B H 0.629624 -0.102646 0.834476 0.072 Uiso 1 1 calc R U . . . H12C H 0.513919 -0.014747 0.893637 0.072 Uiso 1 1 calc R U . . . C13 C 0.7104(3) 0.2139(3) 0.97302(16) 0.0518(6) Uani 1 1 d . . . . . H13A H 0.606609 0.243177 0.980838 0.078 Uiso 1 1 calc R U . . . H13B H 0.770035 0.292680 0.966508 0.078 Uiso 1 1 calc R U . . . H13C H 0.743921 0.160996 1.025858 0.078 Uiso 1 1 calc R U . . . C14 C 0.9484(2) 0.1383(3) 0.60346(17) 0.0485(6) Uani 1 1 d . . . . . H14A H 0.998050 0.089269 0.653307 0.073 Uiso 1 1 calc R U . . . H14B H 0.972382 0.233041 0.605327 0.073 Uiso 1 1 calc R U . . . H14C H 0.981658 0.099618 0.545965 0.073 Uiso 1 1 calc R U . . . C15 C 0.7087(3) -0.0582(2) 0.6155(2) 0.0505(6) Uani 1 1 d . . . . . H15A H 0.746440 -0.099122 0.559659 0.076 Uiso 1 1 calc R U . . . H15B H 0.602338 -0.069482 0.619925 0.076 Uiso 1 1 calc R U . . . H15C H 0.758446 -0.101874 0.667356 0.076 Uiso 1 1 calc R U . . . C16 C 0.6571(3) 0.2029(3) 0.51063(15) 0.0478(6) Uani 1 1 d . . . . . H16A H 0.673292 0.299373 0.509276 0.072 Uiso 1 1 calc R U . . . H16B H 0.551026 0.189169 0.511485 0.072 Uiso 1 1 calc R U . . . H16C H 0.701367 0.160759 0.456919 0.072 Uiso 1 1 calc R U . . . C17 C 0.3167(3) 0.2861(3) 0.85282(18) 0.0492(6) Uani 1 1 d . . . . . H17A H 0.209225 0.297628 0.847482 0.074 Uiso 1 1 calc R U . . . H17B H 0.356329 0.369849 0.874089 0.074 Uiso 1 1 calc R U . . . H17C H 0.341907 0.213493 0.895941 0.074 Uiso 1 1 calc R U . . . C18 C 0.3111(3) 0.3638(3) 0.65515(19) 0.0500(6) Uani 1 1 d . . . . . H18A H 0.204200 0.354167 0.654362 0.075 Uiso 1 1 calc R U . . . H18B H 0.351790 0.344398 0.595169 0.075 Uiso 1 1 calc R U . . . H18C H 0.331789 0.455955 0.671731 0.075 Uiso 1 1 calc R U . . . C19 C 0.3379(3) 0.0717(3) 0.7091(2) 0.0502(6) Uani 1 1 d . . . . . H19A H 0.393790 0.003329 0.744682 0.075 Uiso 1 1 calc R U . . . H19B H 0.356063 0.056382 0.644725 0.075 Uiso 1 1 calc R U . . . H19C H 0.232403 0.066117 0.721726 0.075 Uiso 1 1 calc R U . . . 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 0.0233(2) 0.01744(19) 0.0340(2) 0.00017(17) -0.00443(17) -0.00210(15) Si2 0.01897(19) 0.01787(18) 0.0229(2) -0.00025(15) -0.00169(15) -0.00157(14) Si3 0.0304(2) 0.0292(2) 0.0275(2) 0.00770(18) -0.00475(18) -0.00602(19) Si4 0.0247(2) 0.0256(2) 0.0276(2) -0.00719(17) -0.00261(17) -0.00033(17) Si5 0.0188(2) 0.0331(3) 0.0367(3) -0.0020(2) -0.00091(18) -0.00100(18) C1 0.0310(9) 0.0182(7) 0.0531(12) -0.0008(7) 0.0043(8) -0.0010(6) C2 0.0377(10) 0.0257(8) 0.0321(9) -0.0027(7) -0.0009(7) -0.0014(7) C3 0.0296(8) 0.0199(7) 0.0390(10) -0.0040(6) -0.0012(7) -0.0040(6) C4 0.0456(11) 0.0235(8) 0.0322(9) -0.0002(7) -0.0005(8) 0.0006(7) C5 0.0420(10) 0.0177(7) 0.0448(11) 0.0015(7) -0.0160(8) -0.0027(7) C6 0.0387(12) 0.0341(11) 0.103(2) -0.0095(13) 0.0255(14) -0.0046(9) C7 0.079(2) 0.0614(17) 0.0333(12) -0.0093(11) 0.0004(12) 0.0009(15) C8 0.0330(11) 0.0391(11) 0.0760(18) -0.0088(11) -0.0012(11) -0.0089(9) C9 0.081(2) 0.0576(16) 0.0380(12) 0.0035(11) 0.0127(13) -0.0001(14) C10 0.0725(18) 0.0320(11) 0.0781(19) 0.0121(11) -0.0472(16) -0.0106(11) C11 0.0363(11) 0.0521(14) 0.0562(14) 0.0194(11) -0.0118(10) 0.0036(10) C12 0.0571(14) 0.0379(11) 0.0492(13) 0.0174(10) -0.0044(11) -0.0164(10) C13 0.0660(17) 0.0625(16) 0.0283(10) -0.0013(10) -0.0063(10) -0.0153(13) C14 0.0290(10) 0.0734(17) 0.0434(12) -0.0160(12) 0.0073(9) -0.0035(10) C15 0.0561(15) 0.0300(10) 0.0659(16) -0.0162(10) 0.0075(12) -0.0040(10) C16 0.0575(14) 0.0575(14) 0.0275(10) -0.0078(9) -0.0099(9) 0.0062(11) C17 0.0339(11) 0.0652(16) 0.0490(13) -0.0076(12) 0.0134(10) -0.0088(10) C18 0.0279(10) 0.0578(15) 0.0634(16) 0.0108(12) -0.0091(10) 0.0049(9) C19 0.0305(10) 0.0458(13) 0.0753(18) -0.0085(12) -0.0120(11) -0.0091(9) 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' 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 C5 40.12(9) . . ? C1 Si1 Si2 106.96(6) . . ? C5 Si1 Si2 106.14(6) . . ? Si4 Si2 Si3 107.18(3) . . ? Si4 Si2 Si5 107.51(3) . . ? Si3 Si2 Si5 106.24(3) . . ? Si4 Si2 Si1 101.52(2) . . ? Si3 Si2 Si1 95.40(2) . . ? Si5 Si2 Si1 136.15(3) . . ? C13 Si3 C11 107.99(13) . . ? C13 Si3 C12 107.64(13) . . ? C11 Si3 C12 107.41(12) . . ? C13 Si3 Si2 108.71(9) . . ? C11 Si3 Si2 111.38(8) . . ? C12 Si3 Si2 113.51(8) . . ? C14 Si4 C15 106.91(13) . . ? C14 Si4 C16 107.57(13) . . ? C15 Si4 C16 108.12(13) . . ? C14 Si4 Si2 110.20(8) . . ? C15 Si4 Si2 113.90(9) . . ? C16 Si4 Si2 109.91(8) . . ? C17 Si5 C18 107.34(13) . . ? C17 Si5 C19 107.75(13) . . ? C18 Si5 C19 106.41(13) . . ? C17 Si5 Si2 111.51(8) . . ? C18 Si5 Si2 114.33(8) . . ? C19 Si5 Si2 109.19(8) . . ? C2 C1 C5 106.77(17) . . ? C2 C1 C6 126.1(2) . . ? C5 C1 C6 125.1(2) . . ? C2 C1 Si1 90.49(12) . . ? C5 C1 Si1 70.39(11) . . ? C6 C1 Si1 117.95(14) . . ? C3 C2 C1 108.83(18) . . ? C3 C2 C7 125.9(2) . . ? C1 C2 C7 125.2(2) . . ? C2 C3 C4 108.76(17) . . ? C2 C3 C8 125.2(2) . . ? C4 C3 C8 125.4(2) . . ? C3 C4 C5 109.27(18) . . ? C3 C4 C9 125.1(2) . . ? C5 C4 C9 125.6(2) . . ? C4 C5 C1 106.32(17) . . ? C4 C5 C10 125.4(2) . . ? C1 C5 C10 126.6(2) . . ? C4 C5 Si1 89.66(12) . . ? C1 C5 Si1 69.49(11) . . ? C10 C5 Si1 118.47(14) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si3 C11 H11A 109.5 . . ? Si3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si3 C12 H12A 109.5 . . ? Si3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C13 H13A 109.5 . . ? Si3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si4 C15 H15A 109.5 . . ? Si4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si4 C16 H16A 109.5 . . ? Si4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si5 C17 H17A 109.5 . . ? Si5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si5 C18 H18A 109.5 . . ? Si5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si5 C19 H19A 109.5 . . ? Si5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 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 Si1 C1 2.0999(19) . ? Si1 C5 2.1119(19) . ? Si1 Si2 2.4441(7) . ? Si2 Si4 2.3492(7) . ? Si2 Si3 2.3526(7) . ? Si2 Si5 2.3569(7) . ? Si3 C13 1.875(3) . ? Si3 C11 1.876(2) . ? Si3 C12 1.884(2) . ? Si4 C14 1.868(2) . ? Si4 C15 1.871(2) . ? Si4 C16 1.877(2) . ? Si5 C17 1.874(2) . ? Si5 C18 1.879(2) . ? Si5 C19 1.880(2) . ? C1 C2 1.438(3) . ? C1 C5 1.445(3) . ? C1 C6 1.507(3) . ? C2 C3 1.388(3) . ? C2 C7 1.494(3) . ? C3 C4 1.394(3) . ? C3 C8 1.503(3) . ? C4 C5 1.431(3) . ? C4 C9 1.498(3) . ? C5 C10 1.497(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ?