#------------------------------------------------------------------------------ #$Date: 2020-04-28 01:09:58 +0300 (Tue, 28 Apr 2020) $ #$Revision: 251196 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557925.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_1557925 loop_ _publ_author_name 'Curbet, Idriss' 'Colombel-Rouen, Sophie' 'Manguin, Romane' 'Clermont, Anthony' 'Quelhas, Alexandre' 'M\"uller, Daniel S.' 'Roisnel, Thierry' 'Basle, Olivier' 'Trolez, Yann' 'Mauduit, Marc' _publ_section_title ; Expedient Synthesis of Conjugated Triynes via Alkyne Metathesis ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D0SC01124J _journal_year 2020 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C34 H36 Si' _chemical_formula_sum 'C34 H36 Si' _chemical_formula_weight 472.72 _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 _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_update_record ; 2019-05-10 deposited with the CCDC. 2020-04-27 downloaded from the CCDC. ; _cell_angle_alpha 76.313(5) _cell_angle_beta 77.803(5) _cell_angle_gamma 83.761(5) _cell_formula_units_Z 2 _cell_length_a 8.5423(11) _cell_length_b 10.4335(14) _cell_length_c 16.821(2) _cell_measurement_reflns_used 9754 _cell_measurement_temperature 150 _cell_measurement_theta_max 27.5274 _cell_measurement_theta_min 2.5398 _cell_measurement_wavelength 0.71073 _cell_volume 1421.0(3) _computing_cell_refinement 'APEX3 (Bruker, 2015)' _computing_data_collection 'SAINT (Bruker, 2014)' _computing_data_reduction 'SAINT (Bruker, 2014)' _computing_molecular_graphics 'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2016)' _computing_publication_material 'CRYSCALC (T. Roisnel, local program, 2019)' _computing_structure_refinement 'SHELXL-2018_3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT (G. Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_detector '(CMOS) PHOTON 100' _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'D8 VENTURE Bruker AXS' _diffrn_measurement_method 'rotation images' _diffrn_radiation_monochromator 'multilayer monochromator' _diffrn_radiation_probe x-ray _diffrn_radiation_source 'Incoatec microfocus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_unetI/netI 0.0601 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 26302 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.582 _diffrn_reflns_theta_min 2.444 _diffrn_source_current 1.0 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.105 _exptl_crystal_description plate _exptl_crystal_F_000 508 _exptl_crystal_size_max 0.420 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.453 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.054 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 322 _refine_ls_number_reflns 6444 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0477 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.7359P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1191 _refine_ls_wR_factor_ref 0.1301 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5125 _reflns_number_total 6444 _reflns_threshold_expression >2sigma(I) _cod_data_source_file d0sc01124j2.cif _cod_data_source_block ANC41_2 _cod_database_code 1557925 _shelx_res_file ; TITL import_a.res in P-1 (created by CRYSCALC) job.res created by SHELXL-2018/3 at 17:39:13 on 07-May-2019 CELL 0.71073 8.5423 10.4335 16.8209 76.313 77.803 83.761 ZERR 2.00 0.0011 0.0014 0.0023 0.005 0.005 0.005 LATT 1 SFAC C H SI UNIT 68 72 2 MERG 2 FMAP 2 PLAN 20 SIZE 0.09 0.28 0.42 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.048600 0.735900 FVAR 0.83196 SI1 3 0.792396 0.277179 0.014966 11.00000 0.02279 0.02201 = 0.01558 -0.00881 -0.00211 0.00382 C1 1 0.632521 0.250260 -0.039970 11.00000 0.03425 0.03171 = 0.02074 -0.00405 -0.00990 -0.00600 AFIX 13 H1 2 0.627435 0.330823 -0.085683 11.00000 -1.20000 AFIX 0 C2 1 0.677424 0.134450 -0.083220 11.00000 0.05573 0.06242 = 0.03954 -0.03077 -0.00345 -0.01884 AFIX 137 H2A 2 0.685529 0.052150 -0.041306 11.00000 -1.50000 H2B 2 0.780858 0.148046 -0.121595 11.00000 -1.50000 H2C 2 0.594691 0.128862 -0.114504 11.00000 -1.50000 AFIX 0 C3 1 0.463247 0.240355 0.012402 11.00000 0.03166 0.05058 = 0.03869 -0.00983 -0.01024 -0.00743 AFIX 137 H3A 2 0.387000 0.238038 -0.023274 11.00000 -1.50000 H3B 2 0.435155 0.317246 0.037783 11.00000 -1.50000 H3C 2 0.458881 0.159419 0.056331 11.00000 -1.50000 AFIX 0 C4 1 0.869657 0.121217 0.080745 11.00000 0.03581 0.02986 = 0.02165 -0.00925 -0.00358 0.01369 AFIX 13 H4 2 0.924701 0.063294 0.042266 11.00000 -1.20000 AFIX 0 C5 1 0.734331 0.044758 0.141958 11.00000 0.05541 0.03373 = 0.02707 0.00185 -0.00108 0.00821 AFIX 137 H5A 2 0.779850 -0.036095 0.174349 11.00000 -1.50000 H5B 2 0.660502 0.021552 0.110949 11.00000 -1.50000 H5C 2 0.675976 0.099853 0.179778 11.00000 -1.50000 AFIX 0 C6 1 0.993908 0.147984 0.127655 11.00000 0.04776 0.05856 = 0.04726 -0.00994 -0.02614 0.01844 AFIX 137 H6A 2 0.942999 0.202988 0.167002 11.00000 -1.50000 H6B 2 1.081910 0.194124 0.087717 11.00000 -1.50000 H6C 2 1.036249 0.063951 0.158237 11.00000 -1.50000 AFIX 0 C7 1 0.960159 0.368385 -0.061044 11.00000 0.02753 0.03323 = 0.02519 -0.01429 0.00122 -0.00365 AFIX 13 H7 2 1.026146 0.398699 -0.027255 11.00000 -1.20000 AFIX 0 C8 1 1.072660 0.279559 -0.112371 11.00000 0.03802 0.05489 = 0.04702 -0.03090 0.01716 -0.01162 AFIX 137 H8A 2 1.014124 0.251531 -0.148925 11.00000 -1.50000 H8B 2 1.111509 0.201590 -0.074657 11.00000 -1.50000 H8C 2 1.164080 0.328919 -0.146259 11.00000 -1.50000 AFIX 0 C9 1 0.899539 0.492300 -0.117980 11.00000 0.04776 0.04614 = 0.03470 0.00391 -0.00122 -0.01422 AFIX 137 H9A 2 0.990594 0.544181 -0.149481 11.00000 -1.50000 H9B 2 0.824695 0.545597 -0.084158 11.00000 -1.50000 H9C 2 0.844451 0.466593 -0.156817 11.00000 -1.50000 AFIX 0 C10 1 0.697372 0.383909 0.087845 11.00000 0.02476 0.02428 = 0.01977 -0.00735 -0.00324 0.00334 C11 1 0.627505 0.448482 0.137180 11.00000 0.02287 0.02169 = 0.01829 -0.00568 -0.00337 0.00356 C12 1 0.545561 0.521519 0.192510 11.00000 0.02087 0.02260 = 0.01754 -0.00510 -0.00398 0.00353 C13 1 0.469670 0.586256 0.239952 11.00000 0.02213 0.02293 = 0.01686 -0.00583 -0.00455 0.00340 C14 1 0.379356 0.660183 0.292655 11.00000 0.02131 0.02335 = 0.01812 -0.00673 -0.00452 0.00299 C15 1 0.297879 0.724895 0.337920 11.00000 0.01889 0.02279 = 0.01741 -0.00641 -0.00507 0.00230 C16 1 0.197264 0.805840 0.392804 11.00000 0.01657 0.01894 = 0.01529 -0.00743 -0.00248 0.00348 C17 1 0.268353 0.942866 0.370766 11.00000 0.01162 0.02083 = 0.01683 -0.00624 -0.00043 0.00257 C18 1 0.291160 1.014006 0.288284 11.00000 0.02427 0.02967 = 0.01724 -0.00654 -0.00219 0.00035 AFIX 43 H18 2 0.267957 0.975908 0.246393 11.00000 -1.20000 AFIX 0 C19 1 0.347186 1.139400 0.266831 11.00000 0.03110 0.03228 = 0.02241 0.00139 0.00079 -0.00302 AFIX 43 H19 2 0.359947 1.187684 0.210625 11.00000 -1.20000 AFIX 0 C20 1 0.384768 1.194854 0.327008 11.00000 0.02808 0.02578 = 0.03602 -0.00295 0.00091 -0.00656 AFIX 43 H20 2 0.424295 1.280683 0.312132 11.00000 -1.20000 AFIX 0 C21 1 0.364540 1.124911 0.408565 11.00000 0.02730 0.02822 = 0.03072 -0.01024 -0.00466 -0.00574 AFIX 43 H21 2 0.390504 1.162606 0.449959 11.00000 -1.20000 AFIX 0 C22 1 0.306343 0.999494 0.430573 11.00000 0.02038 0.02477 = 0.01880 -0.00704 -0.00305 -0.00036 AFIX 43 H22 2 0.292439 0.952116 0.487003 11.00000 -1.20000 AFIX 0 C23 1 0.024550 0.820247 0.375697 11.00000 0.01639 0.02463 = 0.01369 -0.00595 -0.00191 -0.00019 C24 1 -0.066666 0.938671 0.372747 11.00000 0.02104 0.02700 = 0.02061 -0.00907 -0.00435 0.00230 AFIX 43 H24 2 -0.021651 1.013739 0.379678 11.00000 -1.20000 AFIX 0 C25 1 -0.222976 0.949104 0.359796 11.00000 0.02092 0.03780 = 0.02269 -0.00685 -0.00435 0.00678 AFIX 43 H25 2 -0.284287 1.031008 0.357919 11.00000 -1.20000 AFIX 0 C26 1 -0.289515 0.841043 0.349653 11.00000 0.01650 0.05304 = 0.02610 -0.00603 -0.00449 -0.00520 AFIX 43 H26 2 -0.396384 0.848217 0.340436 11.00000 -1.20000 AFIX 0 C27 1 -0.200380 0.722749 0.352944 11.00000 0.02826 0.04375 = 0.04611 -0.01342 -0.00595 -0.01417 AFIX 43 H27 2 -0.246289 0.648024 0.346130 11.00000 -1.20000 AFIX 0 C28 1 -0.044493 0.711288 0.366072 11.00000 0.02593 0.02723 = 0.03892 -0.00992 -0.00560 -0.00330 AFIX 43 H28 2 0.015679 0.628806 0.368532 11.00000 -1.20000 AFIX 0 C29 1 0.199783 0.737004 0.484697 11.00000 0.02180 0.01652 = 0.01680 -0.00529 -0.00406 -0.00041 C30 1 0.065728 0.744378 0.546793 11.00000 0.02659 0.02876 = 0.02015 -0.00504 -0.00206 0.00521 AFIX 43 H30 2 -0.032260 0.785686 0.532433 11.00000 -1.20000 AFIX 0 C31 1 0.073859 0.691572 0.630126 11.00000 0.03695 0.03776 = 0.01871 -0.00375 0.00263 0.00479 AFIX 43 H31 2 -0.018606 0.697106 0.672264 11.00000 -1.20000 AFIX 0 C32 1 0.214682 0.631594 0.651706 11.00000 0.04435 0.03312 = 0.01754 0.00036 -0.00818 0.00004 AFIX 43 H32 2 0.220173 0.596864 0.708667 11.00000 -1.20000 AFIX 0 C33 1 0.348926 0.621893 0.590030 11.00000 0.03256 0.02804 = 0.02666 -0.00077 -0.01340 0.00199 AFIX 43 H33 2 0.446178 0.579280 0.604641 11.00000 -1.20000 AFIX 0 C34 1 0.341163 0.674488 0.506896 11.00000 0.02260 0.02473 = 0.02141 -0.00404 -0.00424 0.00032 AFIX 43 H34 2 0.433413 0.667623 0.464851 11.00000 -1.20000 AFIX 0 HKLF 4 REM import_a.res in P-1 (created by CRYSCALC) REM wR2 = 0.1301, GooF = S = 1.029, Restrained GooF = 1.029 for all data REM R1 = 0.0477 for 5125 Fo > 4sig(Fo) and 0.0648 for all 6444 data REM 322 parameters refined using 0 restraints END WGHT 0.0499 0.6993 REM Highest difference peak 0.453, deepest hole -0.368, 1-sigma level 0.054 Q1 1 0.8343 0.1966 0.0542 11.00000 0.05 0.45 Q2 1 -0.0160 0.8829 0.3695 11.00000 0.05 0.29 Q3 1 0.2814 0.7401 0.4990 11.00000 0.05 0.25 Q4 1 0.2339 0.8783 0.3796 11.00000 0.05 0.25 Q5 1 0.7201 0.3473 0.0469 11.00000 0.05 0.24 Q6 1 -0.1375 0.9418 0.3546 11.00000 0.05 0.24 Q7 1 -0.0218 0.7626 0.3893 11.00000 0.05 0.24 Q8 1 0.2516 0.6789 0.4922 11.00000 0.05 0.24 Q9 1 0.2523 0.7787 0.3630 11.00000 0.05 0.23 Q10 1 -0.2188 0.7949 0.3363 11.00000 0.05 0.23 Q11 1 0.1373 0.7352 0.5131 11.00000 0.05 0.23 Q12 1 0.4632 0.5655 0.1949 11.00000 0.05 0.22 Q13 1 0.1035 0.8173 0.3798 11.00000 0.05 0.21 Q14 1 -0.1205 0.7369 0.3534 11.00000 0.05 0.21 Q15 1 -0.0132 0.8203 0.5421 11.00000 0.05 0.20 Q16 1 0.8298 0.0588 0.1225 11.00000 0.05 0.20 Q17 1 -0.2363 0.9018 0.3415 11.00000 0.05 0.20 Q18 1 0.7005 0.2757 -0.0120 11.00000 0.05 0.20 Q19 1 1.0585 0.2348 0.1119 11.00000 0.05 0.20 Q20 1 -0.2454 0.7834 0.3635 11.00000 0.05 0.20 ; _shelx_res_checksum 58247 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 0.79240(5) 0.27718(4) 0.01497(2) 0.01997(12) Uani 1 1 d . . . . . C1 C 0.6325(2) 0.25026(18) -0.03997(10) 0.0282(4) Uani 1 1 d . . . . . H1 H 0.627435 0.330823 -0.085683 0.034 Uiso 1 1 calc R U . . . C2 C 0.6774(3) 0.1344(2) -0.08322(14) 0.0489(6) Uani 1 1 d . . . . . H2A H 0.685529 0.052150 -0.041306 0.073 Uiso 1 1 calc R U . . . H2B H 0.780858 0.148046 -0.121595 0.073 Uiso 1 1 calc R U . . . H2C H 0.594691 0.128862 -0.114504 0.073 Uiso 1 1 calc R U . . . C3 C 0.4632(2) 0.2404(2) 0.01240(13) 0.0394(5) Uani 1 1 d . . . . . H3A H 0.387000 0.238038 -0.023274 0.059 Uiso 1 1 calc R U . . . H3B H 0.435155 0.317246 0.037783 0.059 Uiso 1 1 calc R U . . . H3C H 0.458881 0.159419 0.056331 0.059 Uiso 1 1 calc R U . . . C4 C 0.8697(2) 0.12122(17) 0.08074(10) 0.0300(4) Uani 1 1 d . . . . . H4 H 0.924701 0.063294 0.042266 0.036 Uiso 1 1 calc R U . . . C5 C 0.7343(3) 0.0448(2) 0.14196(12) 0.0421(5) Uani 1 1 d . . . . . H5A H 0.779850 -0.036095 0.174349 0.063 Uiso 1 1 calc R U . . . H5B H 0.660502 0.021552 0.110949 0.063 Uiso 1 1 calc R U . . . H5C H 0.675976 0.099853 0.179778 0.063 Uiso 1 1 calc R U . . . C6 C 0.9939(3) 0.1480(2) 0.12766(14) 0.0506(6) Uani 1 1 d . . . . . H6A H 0.942999 0.202988 0.167002 0.076 Uiso 1 1 calc R U . . . H6B H 1.081910 0.194124 0.087717 0.076 Uiso 1 1 calc R U . . . H6C H 1.036249 0.063951 0.158237 0.076 Uiso 1 1 calc R U . . . C7 C 0.9602(2) 0.36839(18) -0.06104(10) 0.0281(4) Uani 1 1 d . . . . . H7 H 1.026146 0.398699 -0.027255 0.034 Uiso 1 1 calc R U . . . C8 C 1.0727(3) 0.2796(2) -0.11237(14) 0.0464(5) Uani 1 1 d . . . . . H8A H 1.014124 0.251531 -0.148925 0.070 Uiso 1 1 calc R U . . . H8B H 1.111509 0.201590 -0.074657 0.070 Uiso 1 1 calc R U . . . H8C H 1.164080 0.328919 -0.146259 0.070 Uiso 1 1 calc R U . . . C9 C 0.8995(3) 0.4923(2) -0.11798(13) 0.0452(5) Uani 1 1 d . . . . . H9A H 0.990594 0.544181 -0.149481 0.068 Uiso 1 1 calc R U . . . H9B H 0.824695 0.545597 -0.084158 0.068 Uiso 1 1 calc R U . . . H9C H 0.844451 0.466593 -0.156817 0.068 Uiso 1 1 calc R U . . . C10 C 0.6974(2) 0.38391(16) 0.08784(10) 0.0230(3) Uani 1 1 d . . . . . C11 C 0.62751(19) 0.44848(15) 0.13718(9) 0.0212(3) Uani 1 1 d . . . . . C12 C 0.54556(19) 0.52152(15) 0.19251(9) 0.0205(3) Uani 1 1 d . . . . . C13 C 0.46967(19) 0.58626(15) 0.23995(9) 0.0206(3) Uani 1 1 d . . . . . C14 C 0.37936(19) 0.66018(15) 0.29266(9) 0.0208(3) Uani 1 1 d . . . . . C15 C 0.29788(18) 0.72490(15) 0.33792(9) 0.0194(3) Uani 1 1 d . . . . . C16 C 0.19726(18) 0.80584(14) 0.39280(9) 0.0167(3) Uani 1 1 d . . . . . C17 C 0.26835(17) 0.94287(15) 0.37077(9) 0.0167(3) Uani 1 1 d . . . . . C18 C 0.2912(2) 1.01401(16) 0.28828(9) 0.0239(3) Uani 1 1 d . . . . . H18 H 0.267957 0.975908 0.246393 0.029 Uiso 1 1 calc R U . . . C19 C 0.3472(2) 1.13940(18) 0.26683(11) 0.0307(4) Uani 1 1 d . . . . . H19 H 0.359947 1.187684 0.210625 0.037 Uiso 1 1 calc R U . . . C20 C 0.3848(2) 1.19485(18) 0.32701(11) 0.0313(4) Uani 1 1 d . . . . . H20 H 0.424295 1.280683 0.312132 0.038 Uiso 1 1 calc R U . . . C21 C 0.3645(2) 1.12491(17) 0.40856(11) 0.0279(4) Uani 1 1 d . . . . . H21 H 0.390504 1.162606 0.449959 0.034 Uiso 1 1 calc R U . . . C22 C 0.30634(19) 0.99949(16) 0.43057(9) 0.0211(3) Uani 1 1 d . . . . . H22 H 0.292439 0.952116 0.487003 0.025 Uiso 1 1 calc R U . . . C23 C 0.02455(18) 0.82025(15) 0.37570(9) 0.0182(3) Uani 1 1 d . . . . . C24 C -0.06667(19) 0.93867(16) 0.37275(9) 0.0225(3) Uani 1 1 d . . . . . H24 H -0.021651 1.013739 0.379678 0.027 Uiso 1 1 calc R U . . . C25 C -0.2230(2) 0.94910(18) 0.35980(10) 0.0277(4) Uani 1 1 d . . . . . H25 H -0.284287 1.031008 0.357919 0.033 Uiso 1 1 calc R U . . . C26 C -0.2895(2) 0.8410(2) 0.34965(11) 0.0320(4) Uani 1 1 d . . . . . H26 H -0.396384 0.848217 0.340436 0.038 Uiso 1 1 calc R U . . . C27 C -0.2004(2) 0.7227(2) 0.35294(13) 0.0380(4) Uani 1 1 d . . . . . H27 H -0.246289 0.648024 0.346130 0.046 Uiso 1 1 calc R U . . . C28 C -0.0445(2) 0.71129(18) 0.36607(11) 0.0302(4) Uani 1 1 d . . . . . H28 H 0.015679 0.628806 0.368532 0.036 Uiso 1 1 calc R U . . . C29 C 0.19978(18) 0.73700(14) 0.48470(9) 0.0181(3) Uani 1 1 d . . . . . C30 C 0.0657(2) 0.74438(17) 0.54679(10) 0.0261(4) Uani 1 1 d . . . . . H30 H -0.032260 0.785686 0.532433 0.031 Uiso 1 1 calc R U . . . C31 C 0.0739(2) 0.69157(19) 0.63013(10) 0.0333(4) Uani 1 1 d . . . . . H31 H -0.018606 0.697106 0.672264 0.040 Uiso 1 1 calc R U . . . C32 C 0.2147(2) 0.63159(18) 0.65171(10) 0.0325(4) Uani 1 1 d . . . . . H32 H 0.220173 0.596864 0.708667 0.039 Uiso 1 1 calc R U . . . C33 C 0.3489(2) 0.62189(17) 0.59003(10) 0.0291(4) Uani 1 1 d . . . . . H33 H 0.446178 0.579280 0.604641 0.035 Uiso 1 1 calc R U . . . C34 C 0.3412(2) 0.67449(16) 0.50690(10) 0.0232(3) Uani 1 1 d . . . . . H34 H 0.433413 0.667623 0.464851 0.028 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 0.0228(2) 0.0220(2) 0.0156(2) -0.00881(16) -0.00211(16) 0.00382(17) C1 0.0342(10) 0.0317(9) 0.0207(8) -0.0040(7) -0.0099(7) -0.0060(7) C2 0.0557(14) 0.0624(14) 0.0395(11) -0.0308(11) -0.0035(10) -0.0188(11) C3 0.0317(10) 0.0506(12) 0.0387(10) -0.0098(9) -0.0102(8) -0.0074(9) C4 0.0358(10) 0.0299(9) 0.0217(8) -0.0092(7) -0.0036(7) 0.0137(7) C5 0.0554(13) 0.0337(10) 0.0271(9) 0.0019(8) -0.0011(9) 0.0082(9) C6 0.0478(13) 0.0586(14) 0.0473(12) -0.0099(11) -0.0261(10) 0.0184(11) C7 0.0275(9) 0.0332(9) 0.0252(8) -0.0143(7) 0.0012(7) -0.0036(7) C8 0.0380(12) 0.0549(13) 0.0470(12) -0.0309(10) 0.0172(9) -0.0116(10) C9 0.0478(13) 0.0461(12) 0.0347(10) 0.0039(9) -0.0012(9) -0.0142(10) C10 0.0248(8) 0.0243(8) 0.0198(7) -0.0074(6) -0.0032(6) 0.0033(6) C11 0.0229(8) 0.0217(8) 0.0183(7) -0.0057(6) -0.0034(6) 0.0036(6) C12 0.0209(8) 0.0226(8) 0.0175(7) -0.0051(6) -0.0040(6) 0.0035(6) C13 0.0221(8) 0.0229(8) 0.0169(7) -0.0058(6) -0.0045(6) 0.0034(6) C14 0.0213(8) 0.0233(8) 0.0181(7) -0.0067(6) -0.0045(6) 0.0030(6) C15 0.0189(7) 0.0228(8) 0.0174(7) -0.0064(6) -0.0051(6) 0.0023(6) C16 0.0166(7) 0.0189(7) 0.0153(7) -0.0074(5) -0.0025(5) 0.0035(6) C17 0.0116(7) 0.0208(7) 0.0168(7) -0.0062(6) -0.0004(5) 0.0026(5) C18 0.0243(8) 0.0297(9) 0.0172(7) -0.0065(6) -0.0022(6) 0.0004(7) C19 0.0311(9) 0.0323(9) 0.0224(8) 0.0014(7) 0.0008(7) -0.0030(7) C20 0.0281(9) 0.0258(9) 0.0360(9) -0.0030(7) 0.0009(7) -0.0066(7) C21 0.0273(9) 0.0282(9) 0.0307(9) -0.0102(7) -0.0047(7) -0.0057(7) C22 0.0204(8) 0.0248(8) 0.0188(7) -0.0070(6) -0.0030(6) -0.0004(6) C23 0.0164(7) 0.0246(8) 0.0137(6) -0.0059(6) -0.0019(5) -0.0002(6) C24 0.0210(8) 0.0270(8) 0.0206(7) -0.0091(6) -0.0044(6) 0.0023(6) C25 0.0209(8) 0.0378(10) 0.0227(8) -0.0068(7) -0.0043(6) 0.0068(7) C26 0.0165(8) 0.0530(12) 0.0261(8) -0.0060(8) -0.0045(6) -0.0052(8) C27 0.0283(10) 0.0437(11) 0.0461(11) -0.0134(9) -0.0060(8) -0.0142(8) C28 0.0259(9) 0.0272(9) 0.0389(10) -0.0099(7) -0.0056(7) -0.0033(7) C29 0.0218(8) 0.0165(7) 0.0168(7) -0.0053(6) -0.0041(6) -0.0004(6) C30 0.0266(9) 0.0288(9) 0.0202(7) -0.0050(6) -0.0021(6) 0.0052(7) C31 0.0369(10) 0.0378(10) 0.0187(8) -0.0037(7) 0.0026(7) 0.0048(8) C32 0.0444(11) 0.0331(9) 0.0175(8) 0.0004(7) -0.0082(7) 0.0000(8) C33 0.0326(10) 0.0280(9) 0.0267(8) -0.0008(7) -0.0134(7) 0.0020(7) C34 0.0226(8) 0.0247(8) 0.0214(7) -0.0040(6) -0.0042(6) 0.0003(6) 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 C10 Si1 C4 106.14(7) . . ? C10 Si1 C1 106.64(8) . . ? C4 Si1 C1 113.54(8) . . ? C10 Si1 C7 107.57(8) . . ? C4 Si1 C7 111.65(8) . . ? C1 Si1 C7 110.89(8) . . ? C3 C1 C2 110.74(16) . . ? C3 C1 Si1 115.63(12) . . ? C2 C1 Si1 112.57(14) . . ? C3 C1 H1 105.7 . . ? C2 C1 H1 105.7 . . ? Si1 C1 H1 105.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C6 110.12(16) . . ? C5 C4 Si1 112.27(13) . . ? C6 C4 Si1 112.00(14) . . ? C5 C4 H4 107.4 . . ? C6 C4 H4 107.4 . . ? Si1 C4 H4 107.4 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C7 C8 110.85(16) . . ? C9 C7 Si1 112.57(13) . . ? C8 C7 Si1 112.77(13) . . ? C9 C7 H7 106.7 . . ? C8 C7 H7 106.7 . . ? Si1 C7 H7 106.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 Si1 175.93(15) . . ? C10 C11 C12 178.84(18) . . ? C13 C12 C11 178.04(17) . . ? C12 C13 C14 178.19(17) . . ? C15 C14 C13 178.68(17) . . ? C14 C15 C16 179.32(16) . . ? C15 C16 C17 107.57(12) . . ? C15 C16 C29 109.09(12) . . ? C17 C16 C29 110.77(11) . . ? C15 C16 C23 108.37(12) . . ? C17 C16 C23 110.18(12) . . ? C29 C16 C23 110.77(12) . . ? C22 C17 C18 118.59(14) . . ? C22 C17 C16 122.39(13) . . ? C18 C17 C16 118.99(13) . . ? C19 C18 C17 120.68(15) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 120.20(15) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 119.65(16) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.32(16) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C17 C22 C21 120.53(15) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C28 118.56(15) . . ? C24 C23 C16 121.42(14) . . ? C28 C23 C16 119.98(14) . . ? C23 C24 C25 120.79(16) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 120.14(16) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 119.57(16) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 120.70(18) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C23 120.23(17) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? C30 C29 C34 118.90(14) . . ? C30 C29 C16 121.05(13) . . ? C34 C29 C16 119.89(13) . . ? C29 C30 C31 120.39(16) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 120.38(16) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 119.74(15) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 119.99(16) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C29 C34 C33 120.59(15) . . ? C29 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? 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 1.8522(16) . ? Si1 C4 1.8790(17) . ? Si1 C1 1.8808(17) . ? Si1 C7 1.8816(18) . ? C1 C3 1.526(3) . ? C1 C2 1.528(3) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.530(3) . ? C4 C6 1.533(3) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.528(3) . ? C7 C8 1.537(2) . ? C7 H7 1.0000 . ? 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 C11 1.211(2) . ? C11 C12 1.372(2) . ? C12 C13 1.206(2) . ? C13 C14 1.372(2) . ? C14 C15 1.199(2) . ? C15 C16 1.477(2) . ? C16 C17 1.547(2) . ? C16 C29 1.546(2) . ? C16 C23 1.547(2) . ? C17 C22 1.388(2) . ? C17 C18 1.394(2) . ? C18 C19 1.382(2) . ? C18 H18 0.9500 . ? C19 C20 1.385(3) . ? C19 H19 0.9500 . ? C20 C21 1.378(2) . ? C20 H20 0.9500 . ? C21 C22 1.390(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.384(2) . ? C23 C28 1.393(2) . ? C24 C25 1.386(2) . ? C24 H24 0.9500 . ? C25 C26 1.376(3) . ? C25 H25 0.9500 . ? C26 C27 1.374(3) . ? C26 H26 0.9500 . ? C27 C28 1.383(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.386(2) . ? C29 C34 1.388(2) . ? C30 C31 1.393(2) . ? C30 H30 0.9500 . ? C31 C32 1.373(3) . ? C31 H31 0.9500 . ? C32 C33 1.387(3) . ? C32 H32 0.9500 . ? C33 C34 1.389(2) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? 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 C1 C3 -35.03(16) . . . . ? C4 Si1 C1 C3 81.49(16) . . . . ? C7 Si1 C1 C3 -151.86(14) . . . . ? C10 Si1 C1 C2 -163.70(13) . . . . ? C4 Si1 C1 C2 -47.17(16) . . . . ? C7 Si1 C1 C2 79.48(15) . . . . ? C10 Si1 C4 C5 63.98(15) . . . . ? C1 Si1 C4 C5 -52.84(15) . . . . ? C7 Si1 C4 C5 -179.09(13) . . . . ? C10 Si1 C4 C6 -60.52(15) . . . . ? C1 Si1 C4 C6 -177.34(13) . . . . ? C7 Si1 C4 C6 56.41(16) . . . . ? C10 Si1 C7 C9 -66.59(15) . . . . ? C4 Si1 C7 C9 177.35(13) . . . . ? C1 Si1 C7 C9 49.67(15) . . . . ? C10 Si1 C7 C8 167.08(14) . . . . ? C4 Si1 C7 C8 51.02(16) . . . . ? C1 Si1 C7 C8 -76.67(16) . . . . ? C15 C16 C17 C22 -127.42(15) . . . . ? C29 C16 C17 C22 -8.28(19) . . . . ? C23 C16 C17 C22 114.65(15) . . . . ? C15 C16 C17 C18 54.40(17) . . . . ? C29 C16 C17 C18 173.54(13) . . . . ? C23 C16 C17 C18 -63.54(17) . . . . ? C22 C17 C18 C19 -1.4(2) . . . . ? C16 C17 C18 C19 176.90(15) . . . . ? C17 C18 C19 C20 1.4(3) . . . . ? C18 C19 C20 C21 -0.6(3) . . . . ? C19 C20 C21 C22 -0.2(3) . . . . ? C18 C17 C22 C21 0.5(2) . . . . ? C16 C17 C22 C21 -177.65(14) . . . . ? C20 C21 C22 C17 0.2(3) . . . . ? C15 C16 C23 C24 -139.70(14) . . . . ? C17 C16 C23 C24 -22.26(18) . . . . ? C29 C16 C23 C24 100.67(16) . . . . ? C15 C16 C23 C28 42.79(19) . . . . ? C17 C16 C23 C28 160.23(14) . . . . ? C29 C16 C23 C28 -76.85(17) . . . . ? C28 C23 C24 C25 -0.5(2) . . . . ? C16 C23 C24 C25 -178.08(14) . . . . ? C23 C24 C25 C26 0.0(2) . . . . ? C24 C25 C26 C27 0.4(3) . . . . ? C25 C26 C27 C28 -0.2(3) . . . . ? C26 C27 C28 C23 -0.4(3) . . . . ? C24 C23 C28 C27 0.7(3) . . . . ? C16 C23 C28 C27 178.30(16) . . . . ? C15 C16 C29 C30 -145.67(15) . . . . ? C17 C16 C29 C30 96.11(17) . . . . ? C23 C16 C29 C30 -26.47(19) . . . . ? C15 C16 C29 C34 38.93(19) . . . . ? C17 C16 C29 C34 -79.29(17) . . . . ? C23 C16 C29 C34 158.13(14) . . . . ? C34 C29 C30 C31 1.0(2) . . . . ? C16 C29 C30 C31 -174.50(15) . . . . ? C29 C30 C31 C32 0.0(3) . . . . ? C30 C31 C32 C33 -0.9(3) . . . . ? C31 C32 C33 C34 0.9(3) . . . . ? C30 C29 C34 C33 -0.9(2) . . . . ? C16 C29 C34 C33 174.56(14) . . . . ? C32 C33 C34 C29 0.0(3) . . . . ?