#------------------------------------------------------------------------------ #$Date: 2019-11-17 10:28:30 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229349 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/75/7047565.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_7047565 loop_ _publ_author_name 'Tsoureas, Nikolaos' 'Green, Jennifer C.' 'Cloke, F Geoffrey N' _publ_section_title ; Bis(pentalene)dititanium chemistry: C-H, C-X and H-H bond activation. ; _journal_issue 41 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 14531 _journal_page_last 14539 _journal_paper_doi 10.1039/c8dt02654h _journal_volume 47 _journal_year 2018 _chemical_formula_moiety 'C81 H121 B N2 Si4 Ti2 . 0.569C7H16 .0.431C7H8' _chemical_formula_sum 'C90 H137.75 B N2 Si4 Ti2' _chemical_formula_weight 1466.73 _chemical_name_common 10 _chemical_name_systematic 10 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2018-09-12 deposited with the CCDC. 2018-09-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.6200(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.4972(3) _cell_length_b 13.1075(2) _cell_length_c 30.6056(5) _cell_measurement_reflns_used 11113 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 71.0970 _cell_measurement_theta_min 3.9550 _cell_volume 8582.4(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8.)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 16.1033 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_unetI/netI 0.0410 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 28273 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.440 _diffrn_reflns_theta_min 3.393 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 2.435 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark green' _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_meas ? _exptl_crystal_description block _exptl_crystal_F_000 3187 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: toluene layered with n-C7H16' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.000 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 990 _refine_ls_number_reflns 16184 _refine_ls_number_restraints 1168 _refine_ls_restrained_S_all 1.000 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0549 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0885P)^2^+4.6982P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1486 _refine_ls_wR_factor_ref 0.1616 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13455 _reflns_number_total 16184 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt02654h2.cif _cod_data_source_block 10 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas Adding full bibliography for 7047563--7047567.cif. ; _cod_database_code 7047565 _shelx_shelxl_version_number 2017/1 _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 0.529 _shelx_estimated_absorpt_t_max 0.793 _oxdiff_exptl_absorpt_empirical_full_min 0.877 _oxdiff_exptl_absorpt_empirical_full_max 1.133 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL 2018ntl11p53_a.res in P2(1)/c shelx.res created by SHELXL-2017/1 at 12:22:40 on 12-Sep-2018 CELL 1.54184 21.4972 13.1075 30.6056 90.000 95.620 90.000 ZERR 4.00 0.0003 0.0002 0.0005 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B N SI TI UNIT 360 551 4 8 16 8 MERG 2 DFIX 1.53 C41A C39A DFIX 1.5 C2S C1S C3S C2S C4S C3S C4S C5S C5S C6S C7S C6S DFIX 1.53 C7S C6S SADI Si3 C39A Si3 C39B SADI C51A B1 C51B B1 SADI C56A C51A C56B C51B C52A C51A C52B C51B SADI C56A C55A C56B C55B C53A C52A C53B C52B SADI C55A C54A C55B C54B C54A C53A C54B C53B SADI 0.01 C43A C42 C43B C42 C44A C42 C44B C42 RIGU EADP C43B C43A EADP C44B C44A EADP C52A C52B EADP C56A C56B EADP C55A C55B EADP C53A C53B EADP C54A C54B EADP C51A C51B FMAP 2 PLAN 10 SIZE 0.100 0.300 0.300 ACTA BOND $H CONF htab LIST 4 L.S. 12 TEMP -100.00 WGHT 0.088500 4.698200 FVAR 0.29039 0.34754 0.32985 0.43126 TI1 6 0.281397 0.565792 0.562942 11.00000 0.03008 0.03163 = 0.03649 -0.00187 0.00820 -0.00133 TI2 6 0.263754 0.679554 0.628047 11.00000 0.02863 0.03240 = 0.03522 -0.00148 0.00912 -0.00172 SI1 5 0.283506 0.297050 0.602196 11.00000 0.03882 0.02964 = 0.05474 0.00092 0.00996 -0.00165 SI2 5 0.387620 0.720031 0.491110 11.00000 0.03385 0.04664 = 0.03664 0.00369 0.01224 0.00262 SI3 5 0.105892 0.828670 0.571708 11.00000 0.02941 0.09013 = 0.05786 -0.01644 0.00672 0.01467 SI4 5 0.443597 0.739299 0.677857 11.00000 0.03356 0.03530 = 0.04237 -0.00082 -0.00034 0.00287 N1 4 0.183605 0.750216 0.706552 11.00000 0.04029 0.04545 = 0.03992 -0.00567 0.01289 -0.00213 N2 4 0.143271 0.611014 0.682395 11.00000 0.04542 0.04816 = 0.05043 -0.00613 0.02199 -0.01065 C1 1 0.189771 0.678171 0.675654 11.00000 0.03669 0.03837 = 0.04328 -0.00181 0.01288 -0.00184 C2 1 0.133450 0.512461 0.661226 11.00000 0.06288 0.05332 = 0.06895 -0.01376 0.03098 -0.02230 AFIX 137 H2A 2 0.159167 0.507582 0.636579 11.00000 -1.50000 H2B 2 0.089265 0.505069 0.650356 11.00000 -1.50000 H2C 2 0.145286 0.458183 0.682448 11.00000 -1.50000 AFIX 0 C3 1 0.225201 0.836642 0.715569 11.00000 0.06449 0.04926 = 0.05248 -0.01368 0.01759 -0.01256 AFIX 137 H3A 2 0.260469 0.831269 0.697692 11.00000 -1.50000 H3B 2 0.240839 0.836864 0.746741 11.00000 -1.50000 H3C 2 0.202352 0.900090 0.708357 11.00000 -1.50000 AFIX 0 C4 1 0.053086 0.583763 0.728486 11.00000 0.09345 0.13876 = 0.09780 -0.04077 0.06658 -0.06061 AFIX 137 H4A 2 0.036264 0.616572 0.753590 11.00000 -1.50000 H4B 2 0.065783 0.513806 0.736350 11.00000 -1.50000 H4C 2 0.020906 0.582427 0.703492 11.00000 -1.50000 AFIX 0 C5 1 0.115282 0.800658 0.766227 11.00000 0.06783 0.09923 = 0.05615 -0.02694 0.02959 -0.00964 AFIX 137 H5A 2 0.079265 0.771941 0.779247 11.00000 -1.50000 H5B 2 0.104029 0.867329 0.753281 11.00000 -1.50000 H5C 2 0.150246 0.808732 0.789028 11.00000 -1.50000 AFIX 0 C6 1 0.108796 0.642820 0.716252 11.00000 0.05557 0.07500 = 0.05287 -0.01211 0.03032 -0.01678 C7 1 0.134018 0.730574 0.731394 11.00000 0.04632 0.06965 = 0.04627 -0.01218 0.02011 -0.00567 C9 1 0.210472 0.389131 0.531265 11.00000 0.07571 0.05980 = 0.06558 0.00600 -0.01386 -0.01060 C10 1 0.147429 0.300234 0.583937 11.00000 0.04750 0.06194 = 0.08763 -0.01106 0.00117 0.00183 AFIX 33 H10A 2 0.146732 0.242939 0.604454 11.00000 -1.50000 H10B 2 0.143201 0.364455 0.599774 11.00000 -1.50000 H10C 2 0.112694 0.293429 0.560877 11.00000 -1.50000 AFIX 0 C11 1 0.209451 0.300047 0.563145 11.00000 0.05065 0.03669 = 0.06435 -0.00666 0.00007 -0.00446 AFIX 13 H11 2 0.209670 0.236529 0.545062 11.00000 -1.20000 AFIX 0 C12 1 0.325663 0.271262 0.693798 11.00000 0.08253 0.06338 = 0.07628 0.01745 -0.01658 -0.01177 AFIX 33 H12A 2 0.340665 0.341705 0.692554 11.00000 -1.50000 H12B 2 0.313065 0.257276 0.723129 11.00000 -1.50000 H12C 2 0.359182 0.224301 0.687630 11.00000 -1.50000 AFIX 0 C13 1 0.269256 0.256350 0.659381 11.00000 0.05013 0.04440 = 0.05822 0.00710 0.00856 -0.00662 AFIX 13 H13 2 0.234989 0.300731 0.668538 11.00000 -1.20000 AFIX 0 C14 1 0.246192 0.145398 0.661708 11.00000 0.07525 0.05393 = 0.07926 0.01639 0.01669 -0.01680 AFIX 33 H14A 2 0.210239 0.135188 0.639881 11.00000 -1.50000 H14B 2 0.279891 0.098721 0.655612 11.00000 -1.50000 H14C 2 0.233773 0.131696 0.691111 11.00000 -1.50000 AFIX 0 C15 1 0.314947 0.106177 0.562251 11.00000 0.11490 0.05251 = 0.11929 -0.00696 0.02756 0.01693 AFIX 33 H15A 2 0.273564 0.112825 0.545972 11.00000 -1.50000 H15B 2 0.343435 0.072468 0.543709 11.00000 -1.50000 H15C 2 0.311632 0.065362 0.588751 11.00000 -1.50000 AFIX 0 C16 1 0.340129 0.211633 0.575179 11.00000 0.06353 0.03888 = 0.10222 -0.00115 0.02929 0.00694 AFIX 13 H16 2 0.346781 0.246122 0.546865 11.00000 -1.20000 AFIX 0 C17 1 0.405527 0.206787 0.601061 11.00000 0.05222 0.05122 = 0.15585 0.02279 0.03485 0.01270 AFIX 33 H17A 2 0.419885 0.276074 0.608685 11.00000 -1.50000 H17B 2 0.403175 0.167055 0.627974 11.00000 -1.50000 H17C 2 0.434978 0.174160 0.582932 11.00000 -1.50000 AFIX 0 C18 1 0.378721 0.515021 0.454514 11.00000 0.06911 0.05413 = 0.06544 -0.00918 0.02288 0.01303 AFIX 33 H18A 2 0.347742 0.502368 0.475339 11.00000 -1.50000 H18B 2 0.357493 0.538849 0.426578 11.00000 -1.50000 H18C 2 0.401311 0.451714 0.449676 11.00000 -1.50000 AFIX 0 C19 1 0.424602 0.595781 0.473023 11.00000 0.04944 0.05950 = 0.04919 0.00305 0.01819 0.01561 AFIX 13 H19 2 0.448030 0.565720 0.499807 11.00000 -1.20000 AFIX 0 C20 1 0.472775 0.614170 0.439615 11.00000 0.06377 0.08461 = 0.06861 -0.00446 0.03581 0.01450 AFIX 33 H20A 2 0.502817 0.666195 0.451055 11.00000 -1.50000 H20B 2 0.494953 0.550426 0.434840 11.00000 -1.50000 H20C 2 0.451135 0.637561 0.411742 11.00000 -1.50000 AFIX 0 C21 1 0.513652 0.773446 0.528136 11.00000 0.03745 0.13040 = 0.08874 -0.01774 0.00749 -0.00408 AFIX 33 H21A 2 0.522101 0.700022 0.527449 11.00000 -1.50000 H21B 2 0.525289 0.805013 0.501073 11.00000 -1.50000 H21C 2 0.538173 0.804115 0.553465 11.00000 -1.50000 AFIX 0 C22 1 0.444019 0.790911 0.531913 11.00000 0.03993 0.05311 = 0.04716 0.00620 0.01087 -0.00347 AFIX 13 H22 2 0.436036 0.764671 0.561533 11.00000 -1.20000 AFIX 0 C23 1 0.431376 0.906271 0.532958 11.00000 0.07439 0.05226 = 0.05594 0.00707 0.00994 -0.01640 AFIX 33 H23A 2 0.386831 0.918106 0.535377 11.00000 -1.50000 H23B 2 0.456061 0.936677 0.558278 11.00000 -1.50000 H23C 2 0.443176 0.937575 0.505886 11.00000 -1.50000 AFIX 0 C24 1 0.408921 0.852821 0.416977 11.00000 0.07624 0.09058 = 0.06291 0.03123 0.02657 0.00743 AFIX 33 H24A 2 0.442608 0.805197 0.411892 11.00000 -1.50000 H24B 2 0.390048 0.879184 0.388776 11.00000 -1.50000 H24C 2 0.425978 0.909626 0.435218 11.00000 -1.50000 AFIX 0 C25 1 0.358890 0.797024 0.440597 11.00000 0.05237 0.05981 = 0.04553 0.01069 0.01100 0.00677 AFIX 13 H25 2 0.339731 0.746209 0.418917 11.00000 -1.20000 AFIX 0 C26 1 0.305663 0.872067 0.448659 11.00000 0.06646 0.07578 = 0.07008 0.02665 0.01219 0.02144 AFIX 33 H26A 2 0.273828 0.836427 0.463706 11.00000 -1.50000 H26B 2 0.322685 0.928879 0.466910 11.00000 -1.50000 H26C 2 0.286755 0.898437 0.420469 11.00000 -1.50000 AFIX 0 C27 1 0.507355 0.548906 0.667579 11.00000 0.05324 0.05327 = 0.07512 -0.00991 -0.00890 0.01895 AFIX 33 H27A 2 0.465545 0.523099 0.657705 11.00000 -1.50000 H27B 2 0.538492 0.512920 0.652000 11.00000 -1.50000 H27C 2 0.516098 0.537476 0.699229 11.00000 -1.50000 AFIX 0 C28 1 0.510375 0.663388 0.657892 11.00000 0.03906 0.04889 = 0.07358 -0.00432 0.00576 0.00832 AFIX 13 H28 2 0.506001 0.670009 0.625184 11.00000 -1.20000 AFIX 0 C29 1 0.575882 0.702321 0.673500 11.00000 0.04012 0.07530 = 0.19411 -0.01290 0.00374 0.00845 AFIX 33 H29A 2 0.578362 0.775558 0.667464 11.00000 -1.50000 H29B 2 0.584428 0.690453 0.705132 11.00000 -1.50000 H29C 2 0.606822 0.665896 0.657903 11.00000 -1.50000 AFIX 0 C30 1 0.503449 0.932707 0.654495 11.00000 0.04312 0.04995 = 0.07278 0.00050 0.00329 -0.01140 AFIX 33 H30A 2 0.534303 0.890503 0.641338 11.00000 -1.50000 H30B 2 0.496260 0.995583 0.637420 11.00000 -1.50000 H30C 2 0.519133 0.949804 0.684755 11.00000 -1.50000 AFIX 0 C31 1 0.441428 0.873175 0.654454 11.00000 0.03523 0.03951 = 0.04809 -0.00003 0.00121 -0.00431 AFIX 13 H31 2 0.425370 0.865587 0.622836 11.00000 -1.20000 AFIX 0 C32 1 0.392662 0.938596 0.675014 11.00000 0.04682 0.03655 = 0.05996 0.00175 0.00202 0.00347 AFIX 33 H32A 2 0.353475 0.900338 0.674869 11.00000 -1.50000 H32B 2 0.408135 0.955705 0.705312 11.00000 -1.50000 H32C 2 0.385262 1.001483 0.657977 11.00000 -1.50000 AFIX 0 C33 1 0.495170 0.821741 0.761549 11.00000 0.08228 0.06111 = 0.05727 -0.00905 -0.01949 -0.00675 AFIX 33 H33A 2 0.490271 0.887829 0.746635 11.00000 -1.50000 H33B 2 0.488727 0.830151 0.792602 11.00000 -1.50000 H33C 2 0.537365 0.795451 0.759106 11.00000 -1.50000 AFIX 0 C34 1 0.446562 0.745792 0.739970 11.00000 0.05604 0.04693 = 0.04382 -0.00306 -0.00692 0.00403 AFIX 13 H34 2 0.404824 0.772107 0.746551 11.00000 -1.20000 AFIX 0 C35 1 0.455043 0.642942 0.763792 11.00000 0.08277 0.05551 = 0.05162 0.00940 -0.00912 0.00646 AFIX 33 H35A 2 0.424435 0.593946 0.750406 11.00000 -1.50000 H35B 2 0.497373 0.617257 0.761340 11.00000 -1.50000 H35C 2 0.448734 0.651957 0.794837 11.00000 -1.50000 AFIX 0 C36 1 0.062052 0.623984 0.565042 11.00000 0.06567 0.14300 = 0.10167 0.00307 0.00683 -0.04480 AFIX 33 H36A 2 0.105399 0.608210 0.575869 11.00000 -1.50000 H36B 2 0.036678 0.628462 0.589887 11.00000 -1.50000 H36C 2 0.045532 0.569962 0.545019 11.00000 -1.50000 AFIX 0 C37 1 0.059836 0.723483 0.541202 11.00000 0.04049 0.14011 = 0.06391 -0.00899 -0.00079 -0.01247 AFIX 13 H37 2 0.081784 0.710772 0.514382 11.00000 -1.20000 AFIX 0 C38 1 -0.007884 0.749992 0.523847 11.00000 0.04692 0.25736 = 0.11154 -0.00472 -0.02224 -0.00533 AFIX 33 H38A 2 -0.008552 0.815408 0.508303 11.00000 -1.50000 H38B 2 -0.024674 0.696470 0.503662 11.00000 -1.50000 H38C 2 -0.033528 0.754971 0.548530 11.00000 -1.50000 AFIX 0 C42 1 0.103396 0.934850 0.531222 11.00000 0.10008 0.08541 = 0.15173 0.00963 -0.00180 0.04639 PART 2 AFIX 13 H42A 2 0.061234 0.944371 0.514818 31.00000 -1.20000 PART 1 AFIX 13 H42 2 0.061060 0.966873 0.530235 -31.00000 -1.20000 AFIX 0 PART 0 C69 1 0.298596 0.818224 0.588199 11.00000 0.03039 0.03239 = 0.03772 0.00301 0.00584 -0.00085 AFIX 43 H69 2 0.338372 0.842666 0.599924 11.00000 -1.20000 AFIX 0 C70 1 0.240048 0.846779 0.601616 11.00000 0.03417 0.03424 = 0.04069 -0.00121 0.00776 0.00404 AFIX 43 H70 2 0.234455 0.899652 0.622099 11.00000 -1.20000 AFIX 0 C71 1 0.314790 0.690784 0.518282 11.00000 0.03352 0.03678 = 0.03459 0.00209 0.00904 0.00179 C72 1 0.369270 0.665936 0.658956 11.00000 0.03507 0.03396 = 0.03663 0.00063 0.00374 0.00207 C73 1 0.321265 0.508951 0.635797 11.00000 0.03324 0.03120 = 0.04197 0.00482 0.00687 -0.00001 C74 1 0.388481 0.556644 0.584857 11.00000 0.03029 0.03317 = 0.04011 0.00289 0.00779 0.00200 AFIX 43 H74 2 0.415757 0.594952 0.568545 11.00000 -1.20000 AFIX 0 C75 1 0.190214 0.786722 0.580735 11.00000 0.03037 0.04082 = 0.03978 -0.00056 0.00801 0.00126 C76 1 0.262718 0.640199 0.494457 11.00000 0.03962 0.04316 = 0.03286 -0.00208 0.00614 0.00176 AFIX 43 H76 2 0.265406 0.602593 0.468173 11.00000 -1.20000 AFIX 0 C77 1 0.320340 0.427488 0.603910 11.00000 0.03620 0.03199 = 0.04591 0.00106 0.00832 0.00057 C78 1 0.286493 0.745104 0.553407 11.00000 0.02870 0.03315 = 0.03511 0.00368 0.00709 -0.00001 C79 1 0.329615 0.627755 0.690352 11.00000 0.04024 0.04392 = 0.03499 0.00210 0.00580 0.00371 AFIX 43 H79 2 0.325393 0.659485 0.717812 11.00000 -1.20000 AFIX 0 C80 1 0.297972 0.539087 0.676194 11.00000 0.03886 0.04075 = 0.04138 0.00683 0.01037 -0.00015 AFIX 43 H80 2 0.266781 0.504975 0.690622 11.00000 -1.20000 AFIX 0 C81 1 0.220242 0.724525 0.549865 11.00000 0.02776 0.03614 = 0.03676 0.00199 0.00657 0.00036 C82 1 0.365880 0.458013 0.575013 11.00000 0.03310 0.03327 = 0.04536 -0.00133 0.00944 0.00403 AFIX 43 H82 2 0.378999 0.416609 0.552146 11.00000 -1.20000 AFIX 0 C83 1 0.207516 0.653009 0.514647 11.00000 0.03293 0.04068 = 0.03905 -0.00254 0.00326 -0.00258 AFIX 43 H83 2 0.168685 0.620265 0.506495 11.00000 -1.20000 AFIX 0 C84 1 0.362731 0.588952 0.624170 11.00000 0.02893 0.03244 = 0.03919 0.00404 0.00544 0.00084 PART 1 C39A 1 0.081541 0.920004 0.615890 21.00000 0.04748 0.10719 = 0.08220 -0.01069 0.00183 0.04564 AFIX 13 H39A 2 0.120178 0.948451 0.632321 21.00000 -1.20000 AFIX 0 C40A 1 0.037443 1.009499 0.601446 21.00000 0.09953 0.14003 = 0.08076 -0.03156 -0.00321 0.08990 AFIX 137 H40A 2 0.041914 1.026644 0.570744 21.00000 -1.50000 H40B 2 0.048332 1.069015 0.620019 21.00000 -1.50000 H40C 2 -0.005883 0.989593 0.604416 21.00000 -1.50000 AFIX 0 C41A 1 0.049307 0.847958 0.647026 21.00000 0.05503 0.21908 = 0.07599 0.02724 0.02744 0.05388 AFIX 137 H41A 2 0.075163 0.787070 0.653121 21.00000 -1.50000 H41B 2 0.008210 0.827745 0.633014 21.00000 -1.50000 H41C 2 0.044195 0.883573 0.674601 21.00000 -1.50000 AFIX 0 C43B 1 0.150307 1.016799 0.540976 -31.00000 0.15367 0.10138 = 0.18511 -0.00970 -0.06460 0.03431 AFIX 137 H43A 2 0.161816 1.020226 0.572726 -31.00000 -1.50000 H43B 2 0.132522 1.082312 0.530613 -31.00000 -1.50000 H43C 2 0.187572 1.001992 0.526031 -31.00000 -1.50000 AFIX 0 C44B 1 0.112654 0.898928 0.484498 -31.00000 0.09741 0.09262 = 0.10114 0.03341 -0.00960 0.01476 AFIX 137 H44A 2 0.107249 0.956851 0.464235 -31.00000 -1.50000 H44B 2 0.081772 0.846125 0.475453 -31.00000 -1.50000 H44C 2 0.154844 0.870903 0.484012 -31.00000 -1.50000 AFIX 0 PART 2 C39B 1 0.073525 0.845260 0.628214 -21.00000 0.03449 0.10059 = 0.06158 -0.01415 0.01666 0.01503 AFIX 13 H39B 2 0.090919 0.787852 0.647166 -21.00000 -1.20000 AFIX 0 C40B 1 0.002359 0.838155 0.626825 -21.00000 0.04277 0.20575 = 0.08731 -0.02623 0.03163 0.01502 AFIX 137 H40D 2 -0.010721 0.857489 0.655475 -21.00000 -1.50000 H40E 2 -0.010957 0.768016 0.619881 -21.00000 -1.50000 H40F 2 -0.016856 0.884408 0.604231 -21.00000 -1.50000 AFIX 0 C41B 1 0.096421 0.942484 0.650541 -21.00000 0.07063 0.11710 = 0.06615 -0.02698 0.00778 0.02719 AFIX 137 H41D 2 0.081701 0.945920 0.679815 -21.00000 -1.50000 H41E 2 0.080244 1.001103 0.633083 -21.00000 -1.50000 H41F 2 0.142218 0.943705 0.653257 -21.00000 -1.50000 AFIX 0 C43A 1 0.125300 1.026251 0.557610 31.00000 0.15367 0.10138 = 0.18511 -0.00970 -0.06460 0.03431 AFIX 137 H43D 2 0.090698 1.074664 0.558449 31.00000 -1.50000 H43E 2 0.159670 1.058960 0.544104 31.00000 -1.50000 H43F 2 0.139893 1.005048 0.587575 31.00000 -1.50000 AFIX 0 C44A 1 0.155884 0.943307 0.502509 31.00000 0.09741 0.09262 = 0.10114 0.03341 -0.00960 0.01476 AFIX 137 H44D 2 0.155399 1.011301 0.489163 31.00000 -1.50000 H44E 2 0.150699 0.891476 0.479361 31.00000 -1.50000 H44F 2 0.195830 0.932665 0.520250 31.00000 -1.50000 AFIX 0 C1S 1 0.028938 0.633708 0.901060 -41.00000 0.18107 0.19298 = 0.24938 -0.08306 0.10631 -0.04918 AFIX 33 H1SA 2 -0.010403 0.668888 0.891869 -41.00000 -1.50000 H1SB 2 0.019933 0.565753 0.912217 -41.00000 -1.50000 H1SC 2 0.052672 0.673126 0.924258 -41.00000 -1.50000 AFIX 0 C2S 1 0.065324 0.623888 0.863856 -41.00000 0.14216 0.11221 = 0.14425 0.03708 0.05053 0.02519 AFIX 23 H2SA 2 0.071788 0.693468 0.852557 -41.00000 -1.20000 H2SB 2 0.039248 0.586747 0.840590 -41.00000 -1.20000 AFIX 0 C3S 1 0.128282 0.572176 0.869336 -41.00000 0.11933 0.09032 = 0.08315 -0.00228 0.01627 -0.00711 AFIX 23 H3SA 2 0.155189 0.610070 0.891904 -41.00000 -1.20000 H3SB 2 0.122421 0.502739 0.880983 -41.00000 -1.20000 AFIX 0 C4S 1 0.161675 0.563022 0.830736 -41.00000 0.11986 0.11870 = 0.09667 0.04749 0.02202 0.01917 AFIX 23 H4SA 2 0.171440 0.632644 0.820888 -41.00000 -1.20000 H4SB 2 0.133184 0.531544 0.807144 -41.00000 -1.20000 AFIX 0 C5S 1 0.219568 0.504418 0.835123 -41.00000 0.08296 0.12398 = 0.05258 0.00471 -0.00509 -0.01671 AFIX 23 H5SA 2 0.209890 0.434791 0.845011 -41.00000 -1.20000 H5SB 2 0.248185 0.535984 0.858618 -41.00000 -1.20000 AFIX 0 C6S 1 0.255118 0.494777 0.793255 -41.00000 0.15041 0.16628 = 0.06716 0.02884 0.02645 0.04446 AFIX 23 H6SA 2 0.227619 0.460517 0.769880 -41.00000 -1.20000 H6SB 2 0.264387 0.564001 0.782693 -41.00000 -1.20000 AFIX 0 C7S 1 0.315356 0.435794 0.801024 -41.00000 0.10955 0.17055 = 0.16251 -0.01876 0.02201 0.02079 AFIX 33 H7SA 2 0.335472 0.432318 0.773679 -41.00000 -1.50000 H7SB 2 0.343282 0.470128 0.823634 -41.00000 -1.50000 H7SC 2 0.306489 0.366576 0.810812 -41.00000 -1.50000 PART 1 AFIX 66 C8S 1 0.196535 0.512637 0.829838 41.00000 0.13668 C13S 1 0.215812 0.414917 0.819780 41.00000 0.18786 AFIX 43 H13S 2 0.190226 0.357837 0.824804 41.00000 -1.20000 AFIX 65 C12S 1 0.272525 0.400714 0.802373 41.00000 0.14662 AFIX 43 H12S 2 0.285700 0.333926 0.795499 41.00000 -1.20000 AFIX 65 C11S 1 0.309962 0.484230 0.795024 41.00000 0.09231 AFIX 43 H11S 2 0.348723 0.474522 0.783126 41.00000 -1.20000 AFIX 65 C10S 1 0.290686 0.581951 0.805081 41.00000 0.09286 AFIX 43 H10S 2 0.316272 0.639030 0.800058 41.00000 -1.20000 AFIX 65 C9S 1 0.233973 0.596156 0.822488 41.00000 0.09927 AFIX 43 H9S 2 0.220799 0.662944 0.829362 41.00000 -1.20000 AFIX 0 C14S 1 0.137207 0.520858 0.855019 41.00000 0.20016 AFIX 33 H14D 2 0.128141 0.592854 0.860263 41.00000 -1.50000 H14E 2 0.101602 0.489748 0.837458 41.00000 -1.50000 H14F 2 0.144537 0.485146 0.883184 41.00000 -1.50000 AFIX 0 PART 0 C45 1 0.120486 0.017636 0.871797 11.00000 0.03844 0.05637 = 0.08051 0.00614 0.00169 0.01235 C46 1 0.119991 0.004870 0.917133 11.00000 0.05116 0.10067 = 0.08349 0.03103 -0.00448 0.00458 AFIX 43 H46 2 0.151306 0.038047 0.936093 11.00000 -1.20000 AFIX 0 C47 1 0.075782 -0.054125 0.935684 11.00000 0.06044 0.11363 = 0.11173 0.05912 0.01002 0.01775 AFIX 43 H47 2 0.076393 -0.059351 0.966682 11.00000 -1.20000 AFIX 0 C48 1 0.030713 -0.105352 0.908461 11.00000 0.04620 0.08410 = 0.15807 0.04348 0.01008 0.00529 AFIX 43 H48 2 0.001124 -0.147976 0.920655 11.00000 -1.20000 AFIX 0 C49 1 0.029198 -0.093980 0.863769 11.00000 0.04676 0.07001 = 0.14483 -0.00871 0.00882 -0.00119 AFIX 43 H49 2 -0.001677 -0.128654 0.844997 11.00000 -1.20000 AFIX 0 C50 1 0.072501 -0.032148 0.845905 11.00000 0.04340 0.06324 = 0.09395 -0.01300 0.00786 0.00799 AFIX 43 H50 2 0.069485 -0.023258 0.814964 11.00000 -1.20000 AFIX 0 C57 1 0.142925 0.141404 0.805336 11.00000 0.05444 0.06948 = 0.06810 0.00179 0.01279 0.01020 C58 1 0.114417 0.236463 0.806389 11.00000 0.16809 0.12343 = 0.10722 -0.01125 -0.02633 0.08254 AFIX 43 H58 2 0.116480 0.271566 0.833649 11.00000 -1.20000 AFIX 0 C59 1 0.083811 0.281950 0.770684 11.00000 0.24260 0.17509 = 0.14617 0.01680 -0.05023 0.11808 AFIX 43 H59 2 0.062992 0.344967 0.774081 11.00000 -1.20000 AFIX 0 C60 1 0.082390 0.239838 0.730857 11.00000 0.09956 0.15684 = 0.11730 0.06824 -0.01035 0.02249 AFIX 43 H60 2 0.061970 0.273190 0.705879 11.00000 -1.20000 AFIX 0 C61 1 0.110840 0.148161 0.726900 11.00000 0.10067 0.19353 = 0.06034 0.03351 0.03011 0.03448 AFIX 43 H61 2 0.110857 0.116858 0.698906 11.00000 -1.20000 AFIX 0 C62 1 0.139775 0.100624 0.763815 11.00000 0.08943 0.11616 = 0.06211 0.01195 0.02418 0.03333 AFIX 43 H62 2 0.158581 0.035956 0.760248 11.00000 -1.20000 AFIX 0 C63 1 0.205523 0.166657 0.885080 11.00000 0.06735 0.05648 = 0.06284 -0.00623 0.01395 -0.00195 C64 1 0.166280 0.229447 0.908085 11.00000 0.10150 0.08436 = 0.09218 -0.02224 0.01553 0.01943 AFIX 43 H64 2 0.122364 0.219395 0.903459 11.00000 -1.20000 AFIX 0 C65 1 0.188710 0.303936 0.936672 11.00000 0.16515 0.08641 = 0.10482 -0.03356 0.03071 0.00533 AFIX 43 H65 2 0.160705 0.343901 0.951696 11.00000 -1.20000 AFIX 0 C66 1 0.252430 0.320754 0.943586 11.00000 0.18719 0.08054 = 0.09945 -0.03624 0.03512 -0.04196 AFIX 43 H66 2 0.268359 0.375362 0.961786 11.00000 -1.20000 AFIX 0 C67 1 0.291331 0.259577 0.924459 11.00000 0.10119 0.14132 = 0.11693 -0.04456 0.02075 -0.05379 AFIX 43 H67 2 0.335184 0.267406 0.931025 11.00000 -1.20000 AFIX 0 C68 1 0.268217 0.183672 0.894707 11.00000 0.07479 0.09862 = 0.09500 -0.03363 0.01525 -0.01812 AFIX 43 H68 2 0.297047 0.142846 0.880826 11.00000 -1.20000 AFIX 0 B1 3 0.174831 0.082813 0.849530 11.00000 0.04475 0.05762 = 0.06318 -0.00751 0.00793 0.00623 PART 1 C51B 1 0.227600 -0.005635 0.840182 -41.00000 0.03840 0.05520 = 0.04940 -0.00711 -0.00165 0.00207 C52B 1 0.228235 -0.107474 0.854830 -41.00000 0.04606 0.06209 = 0.04871 -0.00326 -0.00380 0.01030 AFIX 43 H52B 2 0.196120 -0.130002 0.871763 -41.00000 -1.20000 AFIX 0 C53B 1 0.274505 -0.176450 0.845290 -41.00000 0.06156 0.07692 = 0.05588 -0.01521 -0.01485 0.02804 AFIX 43 H53B 2 0.272941 -0.245026 0.855170 -41.00000 -1.20000 AFIX 0 C54B 1 0.323039 -0.145062 0.821300 -41.00000 0.05003 0.09553 = 0.05631 -0.02366 -0.00658 0.02994 AFIX 43 H54B 2 0.355763 -0.190969 0.816223 -41.00000 -1.20000 AFIX 0 C55B 1 0.323206 -0.047228 0.805048 -41.00000 0.04163 0.08033 = 0.08879 -0.03002 0.00416 0.00406 AFIX 43 H55B 2 0.354589 -0.025892 0.787238 -41.00000 -1.20000 AFIX 0 C56B 1 0.276733 0.019693 0.815131 -41.00000 0.04503 0.06012 = 0.07317 -0.01053 0.00987 -0.00161 AFIX 43 H56B 2 0.278241 0.087500 0.804324 -41.00000 -1.20000 AFIX 0 PART 2 C51A 1 0.232212 0.017040 0.830773 41.00000 0.03840 0.05520 = 0.04940 -0.00711 -0.00165 0.00207 C52A 1 0.246312 -0.078191 0.848888 41.00000 0.04606 0.06209 = 0.04871 -0.00326 -0.00380 0.01030 AFIX 43 H52A 2 0.219816 -0.106700 0.868777 41.00000 -1.20000 AFIX 0 C53A 1 0.299216 -0.133759 0.838417 41.00000 0.06156 0.07692 = 0.05588 -0.01521 -0.01485 0.02804 AFIX 43 H53A 2 0.309353 -0.197995 0.851622 41.00000 -1.20000 AFIX 0 C54A 1 0.335186 -0.092190 0.808773 41.00000 0.05003 0.09553 = 0.05631 -0.02366 -0.00658 0.02994 AFIX 43 H54A 2 0.369917 -0.129519 0.800277 41.00000 -1.20000 AFIX 0 C55A 1 0.322532 0.001190 0.791141 41.00000 0.04163 0.08033 = 0.08879 -0.03002 0.00416 0.00406 AFIX 43 H55A 2 0.349518 0.029713 0.771586 41.00000 -1.20000 AFIX 0 C56A 1 0.271193 0.054865 0.801246 41.00000 0.04503 0.06012 = 0.07317 -0.01053 0.00987 -0.00161 AFIX 43 H56A 2 0.262204 0.119157 0.787749 41.00000 -1.20000 AFIX 0 PART 0 H 2 0.225058 0.587967 0.598524 11.00000 0.05049 H9A 2 0.204015 0.458616 0.548574 11.00000 0.07906 H9B 2 0.252109 0.395337 0.517802 11.00000 0.06611 H9C 2 0.175741 0.389623 0.507248 11.00000 0.08252 HKLF 4 REM 2018ntl11p53_a.res in P2(1)/c REM R1 = 0.0549 for 13455 Fo > 4sig(Fo) and 0.0661 for all 16184 data REM 990 parameters refined using 1168 restraints END WGHT 0.0885 4.6882 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 1.000, deepest hole -0.425, 1-sigma level 0.055 Q1 1 0.0638 1.0230 0.5347 11.00000 0.05 1.00 Q2 1 0.3466 0.1938 0.5361 11.00000 0.05 0.82 Q3 1 0.1287 0.9639 0.5499 11.00000 0.05 0.61 Q4 1 0.2323 0.4162 0.8368 11.00000 0.05 0.47 Q5 1 -0.0230 0.7880 0.5488 11.00000 0.05 0.42 Q6 1 0.5397 0.6675 0.6259 11.00000 0.05 0.41 Q7 1 0.0872 0.1757 0.8153 11.00000 0.05 0.36 Q8 1 0.2000 0.2618 0.8857 11.00000 0.05 0.34 Q9 1 0.4480 0.7456 0.7082 11.00000 0.05 0.33 Q10 1 0.2255 0.3353 0.9170 11.00000 0.05 0.33 ; _shelx_res_checksum 53065 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Ti1 Ti 0.28140(2) 0.56579(3) 0.56294(2) 0.03241(11) Uani 1 1 d . . . . . Ti2 Ti 0.26375(2) 0.67955(3) 0.62805(2) 0.03169(11) Uani 1 1 d . . . . . Si1 Si 0.28351(3) 0.29705(5) 0.60220(2) 0.04071(16) Uani 1 1 d . . . . . Si2 Si 0.38762(3) 0.72003(6) 0.49111(2) 0.03846(16) Uani 1 1 d . . . . . Si3 Si 0.10589(3) 0.82867(8) 0.57171(3) 0.0590(2) Uani 1 1 d D . . . . Si4 Si 0.44360(3) 0.73930(5) 0.67786(2) 0.03734(15) Uani 1 1 d . . . . . N1 N 0.18360(10) 0.75022(17) 0.70655(7) 0.0413(5) Uani 1 1 d . . . . . N2 N 0.14327(11) 0.61101(18) 0.68239(8) 0.0469(5) Uani 1 1 d . . . . . C1 C 0.18977(12) 0.67817(19) 0.67565(8) 0.0389(5) Uani 1 1 d . . . . . C2 C 0.13345(16) 0.5125(2) 0.66123(11) 0.0601(8) Uani 1 1 d . . . . . H2A H 0.159167 0.507582 0.636579 0.090 Uiso 1 1 calc R U . . . H2B H 0.089265 0.505069 0.650356 0.090 Uiso 1 1 calc R U . . . H2C H 0.145286 0.458183 0.682448 0.090 Uiso 1 1 calc R U . . . C3 C 0.22520(16) 0.8366(2) 0.71557(10) 0.0546(7) Uani 1 1 d . . . . . H3A H 0.260469 0.831269 0.697692 0.082 Uiso 1 1 calc R U . . . H3B H 0.240839 0.836864 0.746741 0.082 Uiso 1 1 calc R U . . . H3C H 0.202352 0.900090 0.708357 0.082 Uiso 1 1 calc R U . . . C4 C 0.0531(2) 0.5838(4) 0.72849(16) 0.1062(19) Uani 1 1 d . . . . . H4A H 0.036264 0.616572 0.753590 0.159 Uiso 1 1 calc R U . . . H4B H 0.065783 0.513806 0.736350 0.159 Uiso 1 1 calc R U . . . H4C H 0.020906 0.582427 0.703492 0.159 Uiso 1 1 calc R U . . . C5 C 0.11528(18) 0.8007(3) 0.76623(12) 0.0729(10) Uani 1 1 d . . . . . H5A H 0.079265 0.771941 0.779247 0.109 Uiso 1 1 calc R U . . . H5B H 0.104029 0.867329 0.753281 0.109 Uiso 1 1 calc R U . . . H5C H 0.150246 0.808732 0.789028 0.109 Uiso 1 1 calc R U . . . C6 C 0.10880(15) 0.6428(3) 0.71625(10) 0.0595(8) Uani 1 1 d . . . . . C7 C 0.13402(14) 0.7306(3) 0.73139(10) 0.0531(7) Uani 1 1 d . . . . . C9 C 0.2105(2) 0.3891(3) 0.53126(13) 0.0684(9) Uani 1 1 d . . . . . C10 C 0.14743(15) 0.3002(3) 0.58394(13) 0.0661(9) Uani 1 1 d . . . . . H10A H 0.146732 0.242939 0.604454 0.099 Uiso 1 1 calc R U . . . H10B H 0.143201 0.364455 0.599774 0.099 Uiso 1 1 calc R U . . . H10C H 0.112694 0.293429 0.560877 0.099 Uiso 1 1 calc R U . . . C11 C 0.20945(14) 0.3000(2) 0.56314(11) 0.0509(7) Uani 1 1 d . . . . . H11 H 0.209670 0.236529 0.545062 0.061 Uiso 1 1 calc R U . . . C12 C 0.3257(2) 0.2713(3) 0.69380(13) 0.0757(11) Uani 1 1 d . . . . . H12A H 0.340665 0.341705 0.692554 0.114 Uiso 1 1 calc R U . . . H12B H 0.313065 0.257276 0.723129 0.114 Uiso 1 1 calc R U . . . H12C H 0.359182 0.224301 0.687630 0.114 Uiso 1 1 calc R U . . . C13 C 0.26926(14) 0.2563(2) 0.65938(10) 0.0507(6) Uani 1 1 d . . . . . H13 H 0.234989 0.300731 0.668538 0.061 Uiso 1 1 calc R U . . . C14 C 0.24619(18) 0.1454(3) 0.66171(13) 0.0689(9) Uani 1 1 d . . . . . H14A H 0.210239 0.135188 0.639881 0.103 Uiso 1 1 calc R U . . . H14B H 0.279891 0.098721 0.655612 0.103 Uiso 1 1 calc R U . . . H14C H 0.233773 0.131696 0.691111 0.103 Uiso 1 1 calc R U . . . C15 C 0.3149(3) 0.1062(3) 0.56225(18) 0.0945(14) Uani 1 1 d . . . . . H15A H 0.273564 0.112825 0.545972 0.142 Uiso 1 1 calc R U . . . H15B H 0.343435 0.072468 0.543709 0.142 Uiso 1 1 calc R U . . . H15C H 0.311632 0.065362 0.588751 0.142 Uiso 1 1 calc R U . . . C16 C 0.34013(17) 0.2116(2) 0.57518(14) 0.0668(9) Uani 1 1 d . . . . . H16 H 0.346781 0.246122 0.546865 0.080 Uiso 1 1 calc R U . . . C17 C 0.40553(17) 0.2068(3) 0.60106(18) 0.0848(13) Uani 1 1 d . . . . . H17A H 0.419885 0.276074 0.608685 0.127 Uiso 1 1 calc R U . . . H17B H 0.403175 0.167055 0.627974 0.127 Uiso 1 1 calc R U . . . H17C H 0.434978 0.174160 0.582932 0.127 Uiso 1 1 calc R U . . . C18 C 0.37872(17) 0.5150(3) 0.45451(11) 0.0618(8) Uani 1 1 d . . . . . H18A H 0.347742 0.502368 0.475339 0.093 Uiso 1 1 calc R U . . . H18B H 0.357493 0.538849 0.426578 0.093 Uiso 1 1 calc R U . . . H18C H 0.401311 0.451714 0.449676 0.093 Uiso 1 1 calc R U . . . C19 C 0.42460(14) 0.5958(2) 0.47302(10) 0.0518(7) Uani 1 1 d . . . . . H19 H 0.448030 0.565720 0.499807 0.062 Uiso 1 1 calc R U . . . C20 C 0.47278(17) 0.6142(3) 0.43961(12) 0.0704(10) Uani 1 1 d . . . . . H20A H 0.502817 0.666195 0.451055 0.106 Uiso 1 1 calc R U . . . H20B H 0.494953 0.550426 0.434840 0.106 Uiso 1 1 calc R U . . . H20C H 0.451135 0.637561 0.411742 0.106 Uiso 1 1 calc R U . . . C21 C 0.51365(16) 0.7734(4) 0.52814(15) 0.0854(13) Uani 1 1 d . . . . . H21A H 0.522101 0.700022 0.527449 0.128 Uiso 1 1 calc R U . . . H21B H 0.525289 0.805013 0.501073 0.128 Uiso 1 1 calc R U . . . H21C H 0.538173 0.804115 0.553465 0.128 Uiso 1 1 calc R U . . . C22 C 0.44402(13) 0.7909(2) 0.53191(9) 0.0463(6) Uani 1 1 d . . . . . H22 H 0.436036 0.764671 0.561533 0.056 Uiso 1 1 calc R U . . . C23 C 0.43138(17) 0.9063(2) 0.53296(11) 0.0606(8) Uani 1 1 d . . . . . H23A H 0.386831 0.918106 0.535377 0.091 Uiso 1 1 calc R U . . . H23B H 0.456061 0.936677 0.558278 0.091 Uiso 1 1 calc R U . . . H23C H 0.443176 0.937575 0.505886 0.091 Uiso 1 1 calc R U . . . C24 C 0.40892(19) 0.8528(3) 0.41698(12) 0.0753(11) Uani 1 1 d . . . . . H24A H 0.442608 0.805197 0.411892 0.113 Uiso 1 1 calc R U . . . H24B H 0.390048 0.879184 0.388776 0.113 Uiso 1 1 calc R U . . . H24C H 0.425978 0.909626 0.435218 0.113 Uiso 1 1 calc R U . . . C25 C 0.35889(14) 0.7970(2) 0.44060(10) 0.0522(7) Uani 1 1 d . . . . . H25 H 0.339731 0.746209 0.418917 0.063 Uiso 1 1 calc R U . . . C26 C 0.30566(17) 0.8721(3) 0.44866(12) 0.0704(10) Uani 1 1 d . . . . . H26A H 0.273828 0.836427 0.463706 0.106 Uiso 1 1 calc R U . . . H26B H 0.322685 0.928879 0.466910 0.106 Uiso 1 1 calc R U . . . H26C H 0.286755 0.898437 0.420469 0.106 Uiso 1 1 calc R U . . . C27 C 0.50736(15) 0.5489(2) 0.66758(12) 0.0615(8) Uani 1 1 d . . . . . H27A H 0.465545 0.523099 0.657705 0.092 Uiso 1 1 calc R U . . . H27B H 0.538492 0.512920 0.652000 0.092 Uiso 1 1 calc R U . . . H27C H 0.516098 0.537476 0.699229 0.092 Uiso 1 1 calc R U . . . C28 C 0.51037(13) 0.6634(2) 0.65789(12) 0.0538(7) Uani 1 1 d . . . . . H28 H 0.506001 0.670009 0.625184 0.065 Uiso 1 1 calc R U . . . C29 C 0.57588(17) 0.7023(4) 0.6735(2) 0.1037(18) Uani 1 1 d . . . . . H29A H 0.578362 0.775558 0.667464 0.156 Uiso 1 1 calc R U . . . H29B H 0.584428 0.690453 0.705132 0.156 Uiso 1 1 calc R U . . . H29C H 0.606822 0.665896 0.657903 0.156 Uiso 1 1 calc R U . . . C30 C 0.50345(14) 0.9327(2) 0.65450(11) 0.0554(7) Uani 1 1 d . . . . . H30A H 0.534303 0.890503 0.641338 0.083 Uiso 1 1 calc R U . . . H30B H 0.496260 0.995583 0.637420 0.083 Uiso 1 1 calc R U . . . H30C H 0.519133 0.949804 0.684755 0.083 Uiso 1 1 calc R U . . . C31 C 0.44143(11) 0.8732(2) 0.65445(9) 0.0411(5) Uani 1 1 d . . . . . H31 H 0.425370 0.865587 0.622836 0.049 Uiso 1 1 calc R U . . . C32 C 0.39266(13) 0.9386(2) 0.67501(10) 0.0480(6) Uani 1 1 d . . . . . H32A H 0.353475 0.900338 0.674869 0.072 Uiso 1 1 calc R U . . . H32B H 0.408135 0.955705 0.705312 0.072 Uiso 1 1 calc R U . . . H32C H 0.385262 1.001483 0.657977 0.072 Uiso 1 1 calc R U . . . C33 C 0.49517(19) 0.8217(3) 0.76155(12) 0.0686(10) Uani 1 1 d . . . . . H33A H 0.490271 0.887829 0.746635 0.103 Uiso 1 1 calc R U . . . H33B H 0.488727 0.830151 0.792602 0.103 Uiso 1 1 calc R U . . . H33C H 0.537365 0.795451 0.759106 0.103 Uiso 1 1 calc R U . . . C34 C 0.44656(15) 0.7458(2) 0.73997(9) 0.0497(6) Uani 1 1 d . . . . . H34 H 0.404824 0.772107 0.746551 0.060 Uiso 1 1 calc R U . . . C35 C 0.45504(18) 0.6429(3) 0.76379(11) 0.0643(9) Uani 1 1 d . . . . . H35A H 0.424435 0.593946 0.750406 0.096 Uiso 1 1 calc R U . . . H35B H 0.497373 0.617257 0.761340 0.096 Uiso 1 1 calc R U . . . H35C H 0.448734 0.651957 0.794837 0.096 Uiso 1 1 calc R U . . . C36 C 0.0621(2) 0.6240(5) 0.56504(17) 0.1035(16) Uani 1 1 d . . . . . H36A H 0.105399 0.608210 0.575869 0.155 Uiso 1 1 calc R U . . . H36B H 0.036678 0.628462 0.589887 0.155 Uiso 1 1 calc R U . . . H36C H 0.045532 0.569962 0.545019 0.155 Uiso 1 1 calc R U . . . C37 C 0.05984(16) 0.7235(4) 0.54120(13) 0.0819(12) Uani 1 1 d . . . . . H37 H 0.081784 0.710772 0.514382 0.098 Uiso 1 1 calc R U . . . C38 C -0.0079(2) 0.7500(6) 0.52385(19) 0.141(3) Uani 1 1 d . . . . . H38A H -0.008552 0.815408 0.508303 0.211 Uiso 1 1 calc R U . . . H38B H -0.024674 0.696470 0.503662 0.211 Uiso 1 1 calc R U . . . H38C H -0.033528 0.754971 0.548530 0.211 Uiso 1 1 calc R U . . . C42 C 0.1034(3) 0.9349(4) 0.5312(2) 0.1133(16) Uani 1 1 d D . . . . H42A H 0.061234 0.944371 0.514818 0.136 Uiso 0.330(8) 1 calc R U P A 2 H42 H 0.061060 0.966873 0.530235 0.136 Uiso 0.670(8) 1 calc R U P A 1 C69 C 0.29860(11) 0.81822(17) 0.58820(8) 0.0333(5) Uani 1 1 d . . . . . H69 H 0.338372 0.842666 0.599924 0.040 Uiso 1 1 calc R U . . . C70 C 0.24005(11) 0.84678(18) 0.60162(8) 0.0361(5) Uani 1 1 d . . . . . H70 H 0.234455 0.899652 0.622099 0.043 Uiso 1 1 calc R U . . . C71 C 0.31479(11) 0.69078(18) 0.51828(8) 0.0346(5) Uani 1 1 d . . . . . C72 C 0.36927(11) 0.66594(18) 0.65896(8) 0.0352(5) Uani 1 1 d . . . . . C73 C 0.32126(11) 0.50895(18) 0.63580(8) 0.0353(5) Uani 1 1 d . . . . . C74 C 0.38848(11) 0.55664(18) 0.58486(8) 0.0342(5) Uani 1 1 d . . . . . H74 H 0.415757 0.594952 0.568545 0.041 Uiso 1 1 calc R U . . . C75 C 0.19021(11) 0.78672(19) 0.58074(8) 0.0367(5) Uani 1 1 d . . . . . C76 C 0.26272(12) 0.6402(2) 0.49446(8) 0.0384(5) Uani 1 1 d . . . . . H76 H 0.265406 0.602593 0.468173 0.046 Uiso 1 1 calc R U . . . C77 C 0.32034(11) 0.42749(18) 0.60391(8) 0.0378(5) Uani 1 1 d . . . . . C78 C 0.28649(10) 0.74510(18) 0.55341(7) 0.0321(4) Uani 1 1 d . . . . . C79 C 0.32962(12) 0.6278(2) 0.69035(8) 0.0396(5) Uani 1 1 d . . . . . H79 H 0.325393 0.659485 0.717812 0.047 Uiso 1 1 calc R U . . . C80 C 0.29797(12) 0.5391(2) 0.67619(8) 0.0399(5) Uani 1 1 d . . . . . H80 H 0.266781 0.504975 0.690622 0.048 Uiso 1 1 calc R U . . . C81 C 0.22024(10) 0.72452(18) 0.54986(8) 0.0333(5) Uani 1 1 d . . . . . C82 C 0.36588(11) 0.45801(18) 0.57501(8) 0.0369(5) Uani 1 1 d . . . . . H82 H 0.378999 0.416609 0.552146 0.044 Uiso 1 1 calc R U . . . C83 C 0.20752(11) 0.65301(19) 0.51465(8) 0.0376(5) Uani 1 1 d . . . . . H83 H 0.168685 0.620265 0.506495 0.045 Uiso 1 1 calc R U . . . C84 C 0.36273(10) 0.58895(18) 0.62417(8) 0.0334(5) Uani 1 1 d . . . . . C39A C 0.0815(5) 0.9200(11) 0.6159(4) 0.079(4) Uani 0.348(7) 1 d D . P B 1 H39A H 0.120178 0.948451 0.632321 0.095 Uiso 0.348(7) 1 calc R U P B 1 C40A C 0.0374(7) 1.0095(12) 0.6014(4) 0.108(6) Uani 0.348(7) 1 d . . P B 1 H40A H 0.041914 1.026644 0.570744 0.161 Uiso 0.348(7) 1 calc R U P B 1 H40B H 0.048332 1.069015 0.620019 0.161 Uiso 0.348(7) 1 calc R U P B 1 H40C H -0.005883 0.989593 0.604416 0.161 Uiso 0.348(7) 1 calc R U P B 1 C41A C 0.0493(6) 0.8480(14) 0.6470(5) 0.115(6) Uani 0.348(7) 1 d D . P B 1 H41A H 0.075163 0.787070 0.653121 0.173 Uiso 0.348(7) 1 calc R U P B 1 H41B H 0.008210 0.827745 0.633014 0.173 Uiso 0.348(7) 1 calc R U P B 1 H41C H 0.044195 0.883573 0.674601 0.173 Uiso 0.348(7) 1 calc R U P B 1 C43B C 0.1503(6) 1.0168(10) 0.5410(6) 0.152(5) Uani 0.670(8) 1 d D . P A 1 H43A H 0.161816 1.020226 0.572726 0.228 Uiso 0.670(8) 1 calc R U P A 1 H43B H 0.132522 1.082312 0.530613 0.228 Uiso 0.670(8) 1 calc R U P A 1 H43C H 0.187572 1.001992 0.526031 0.228 Uiso 0.670(8) 1 calc R U P A 1 C44B C 0.1127(4) 0.8989(6) 0.4845(2) 0.0983(19) Uani 0.670(8) 1 d D . P A 1 H44A H 0.107249 0.956851 0.464235 0.147 Uiso 0.670(8) 1 calc R U P A 1 H44B H 0.081772 0.846125 0.475453 0.147 Uiso 0.670(8) 1 calc R U P A 1 H44C H 0.154844 0.870903 0.484012 0.147 Uiso 0.670(8) 1 calc R U P A 1 C39B C 0.0735(2) 0.8453(6) 0.6282(2) 0.0648(16) Uani 0.652(7) 1 d D . P B 2 H39B H 0.090919 0.787852 0.647166 0.078 Uiso 0.652(7) 1 calc R U P B 2 C40B C 0.0024(3) 0.8382(9) 0.6268(2) 0.110(3) Uani 0.652(7) 1 d . . P B 2 H40D H -0.010721 0.857489 0.655475 0.165 Uiso 0.652(7) 1 calc R U P B 2 H40E H -0.010957 0.768016 0.619881 0.165 Uiso 0.652(7) 1 calc R U P B 2 H40F H -0.016856 0.884408 0.604231 0.165 Uiso 0.652(7) 1 calc R U P B 2 C41B C 0.0964(3) 0.9425(6) 0.6505(2) 0.085(2) Uani 0.652(7) 1 d . . P B 2 H41D H 0.081701 0.945920 0.679815 0.127 Uiso 0.652(7) 1 calc R U P B 2 H41E H 0.080244 1.001103 0.633083 0.127 Uiso 0.652(7) 1 calc R U P B 2 H41F H 0.142218 0.943705 0.653257 0.127 Uiso 0.652(7) 1 calc R U P B 2 C43A C 0.1253(15) 1.026(2) 0.5576(13) 0.152(5) Uani 0.330(8) 1 d D . P A 2 H43D H 0.090698 1.074664 0.558449 0.228 Uiso 0.330(8) 1 calc R U P A 2 H43E H 0.159670 1.058960 0.544104 0.228 Uiso 0.330(8) 1 calc R U P A 2 H43F H 0.139893 1.005048 0.587575 0.228 Uiso 0.330(8) 1 calc R U P A 2 C44A C 0.1559(6) 0.9433(13) 0.5025(5) 0.0983(19) Uani 0.330(8) 1 d D . P A 2 H44D H 0.155399 1.011301 0.489163 0.147 Uiso 0.330(8) 1 calc R U P A 2 H44E H 0.150699 0.891476 0.479361 0.147 Uiso 0.330(8) 1 calc R U P A 2 H44F H 0.195830 0.932665 0.520250 0.147 Uiso 0.330(8) 1 calc R U P A 2 C1S C 0.0289(8) 0.6337(13) 0.9011(6) 0.202(8) Uani 0.569(4) 1 d D . P C 2 H1SA H -0.010403 0.668888 0.891869 0.303 Uiso 0.569(4) 1 calc R U P C 2 H1SB H 0.019933 0.565753 0.912217 0.303 Uiso 0.569(4) 1 calc R U P C 2 H1SC H 0.052672 0.673126 0.924258 0.303 Uiso 0.569(4) 1 calc R U P C 2 C2S C 0.0653(5) 0.6239(9) 0.8639(4) 0.130(4) Uani 0.569(4) 1 d D . P C 2 H2SA H 0.071788 0.693468 0.852557 0.157 Uiso 0.569(4) 1 calc R U P C 2 H2SB H 0.039248 0.586747 0.840590 0.157 Uiso 0.569(4) 1 calc R U P C 2 C3S C 0.1283(5) 0.5722(8) 0.8693(3) 0.097(2) Uani 0.569(4) 1 d D . P C 2 H3SA H 0.155189 0.610070 0.891904 0.117 Uiso 0.569(4) 1 calc R U P C 2 H3SB H 0.122421 0.502739 0.880983 0.117 Uiso 0.569(4) 1 calc R U P C 2 C4S C 0.1617(5) 0.5630(8) 0.8307(3) 0.111(3) Uani 0.569(4) 1 d D . P C 2 H4SA H 0.171440 0.632644 0.820888 0.133 Uiso 0.569(4) 1 calc R U P C 2 H4SB H 0.133184 0.531544 0.807144 0.133 Uiso 0.569(4) 1 calc R U P C 2 C5S C 0.2196(5) 0.5044(7) 0.8351(2) 0.087(2) Uani 0.569(4) 1 d D . P C 2 H5SA H 0.209890 0.434791 0.845011 0.105 Uiso 0.569(4) 1 calc R U P C 2 H5SB H 0.248185 0.535984 0.858618 0.105 Uiso 0.569(4) 1 calc R U P C 2 C6S C 0.2551(5) 0.4948(10) 0.7933(3) 0.127(4) Uani 0.569(4) 1 d D . P C 2 H6SA H 0.227619 0.460517 0.769880 0.152 Uiso 0.569(4) 1 calc R U P C 2 H6SB H 0.264387 0.564001 0.782693 0.152 Uiso 0.569(4) 1 calc R U P C 2 C7S C 0.3154(5) 0.4358(12) 0.8010(5) 0.147(5) Uani 0.569(4) 1 d D . P C 2 H7SA H 0.335472 0.432318 0.773679 0.220 Uiso 0.569(4) 1 calc R U P C 2 H7SB H 0.343282 0.470128 0.823634 0.220 Uiso 0.569(4) 1 calc R U P C 2 H7SC H 0.306489 0.366576 0.810812 0.220 Uiso 0.569(4) 1 calc R U P C 2 C8S C 0.1965(4) 0.5126(10) 0.8298(4) 0.137(9) Uiso 0.431(4) 1 d G . P C 1 C13S C 0.2158(6) 0.4149(8) 0.8198(5) 0.188(9) Uiso 0.431(4) 1 d G . P C 1 H13S H 0.190226 0.357837 0.824804 0.225 Uiso 0.431(4) 1 calc R U P C 1 C12S C 0.2725(6) 0.4007(6) 0.8024(4) 0.147(6) Uiso 0.431(4) 1 d G . P C 1 H12S H 0.285700 0.333926 0.795499 0.176 Uiso 0.431(4) 1 calc R U P C 1 C11S C 0.3100(4) 0.4842(7) 0.7950(3) 0.092(4) Uiso 0.431(4) 1 d G . P C 1 H11S H 0.348723 0.474522 0.783126 0.111 Uiso 0.431(4) 1 calc R U P C 1 C10S C 0.2907(4) 0.5820(6) 0.8051(3) 0.093(3) Uiso 0.431(4) 1 d G . P C 1 H10S H 0.316272 0.639030 0.800058 0.111 Uiso 0.431(4) 1 calc R U P C 1 C9S C 0.2340(4) 0.5962(7) 0.8225(3) 0.099(3) Uiso 0.431(4) 1 d G . P C 1 H9S H 0.220799 0.662944 0.829362 0.119 Uiso 0.431(4) 1 calc R U P C 1 C14S C 0.1372(13) 0.521(2) 0.8550(9) 0.200(12) Uiso 0.431(4) 1 d . . P C 1 H14D H 0.128141 0.592854 0.860263 0.300 Uiso 0.431(4) 1 calc R U P C 1 H14E H 0.101602 0.489748 0.837458 0.300 Uiso 0.431(4) 1 calc R U P C 1 H14F H 0.144537 0.485146 0.883184 0.300 Uiso 0.431(4) 1 calc R U P C 1 C45 C 0.12049(14) 0.0176(3) 0.87180(12) 0.0587(8) Uani 1 1 d . . . . . C46 C 0.11999(17) 0.0049(4) 0.91713(14) 0.0792(11) Uani 1 1 d . . . . . H46 H 0.151306 0.038047 0.936093 0.095 Uiso 1 1 calc R U . . . C47 C 0.07578(19) -0.0541(4) 0.93568(17) 0.0952(15) Uani 1 1 d . . . . . H47 H 0.076393 -0.059351 0.966682 0.114 Uiso 1 1 calc R U . . . C48 C 0.03071(18) -0.1054(4) 0.9085(2) 0.0961(15) Uani 1 1 d . . . . . H48 H 0.001124 -0.147976 0.920655 0.115 Uiso 1 1 calc R U . . . C49 C 0.02920(18) -0.0940(3) 0.86377(19) 0.0872(12) Uani 1 1 d . . . . . H49 H -0.001677 -0.128654 0.844997 0.105 Uiso 1 1 calc R U . . . C50 C 0.07250(15) -0.0321(3) 0.84591(14) 0.0668(9) Uani 1 1 d . . . . . H50 H 0.069485 -0.023258 0.814964 0.080 Uiso 1 1 calc R U . . . C57 C 0.14292(16) 0.1414(3) 0.80534(12) 0.0636(8) Uani 1 1 d . . . . . C58 C 0.1144(3) 0.2365(5) 0.8064(2) 0.136(3) Uani 1 1 d . . . . . H58 H 0.116480 0.271566 0.833649 0.163 Uiso 1 1 calc R U . . . C59 C 0.0838(5) 0.2819(7) 0.7707(3) 0.193(5) Uani 1 1 d . . . . . H59 H 0.062992 0.344967 0.774081 0.231 Uiso 1 1 calc R U . . . C60 C 0.0824(3) 0.2398(6) 0.7309(2) 0.126(2) Uani 1 1 d . . . . . H60 H 0.061970 0.273190 0.705879 0.151 Uiso 1 1 calc R U . . . C61 C 0.1108(3) 0.1482(6) 0.72690(15) 0.117(2) Uani 1 1 d . . . . . H61 H 0.110857 0.116858 0.698906 0.140 Uiso 1 1 calc R U . . . C62 C 0.1398(2) 0.1006(4) 0.76382(13) 0.0881(13) Uani 1 1 d . . . . . H62 H 0.158581 0.035956 0.760248 0.106 Uiso 1 1 calc R U . . . C63 C 0.20552(17) 0.1667(3) 0.88508(12) 0.0617(8) Uani 1 1 d . . . . . C64 C 0.1663(3) 0.2294(4) 0.90808(16) 0.0923(13) Uani 1 1 d . . . . . H64 H 0.122364 0.219395 0.903459 0.111 Uiso 1 1 calc R U . . . C65 C 0.1887(4) 0.3039(4) 0.93667(19) 0.1176(19) Uani 1 1 d . . . . . H65 H 0.160705 0.343901 0.951696 0.141 Uiso 1 1 calc R U . . . C66 C 0.2524(4) 0.3208(4) 0.94359(19) 0.121(2) Uani 1 1 d . . . . . H66 H 0.268359 0.375362 0.961786 0.145 Uiso 1 1 calc R U . . . C67 C 0.2913(3) 0.2596(5) 0.9245(2) 0.119(2) Uani 1 1 d . . . . . H67 H 0.335184 0.267406 0.931025 0.143 Uiso 1 1 calc R U . . . C68 C 0.2682(2) 0.1837(4) 0.89471(16) 0.0890(13) Uani 1 1 d . . . . . H68 H 0.297047 0.142846 0.880826 0.107 Uiso 1 1 calc R U . . . B1 B 0.17483(16) 0.0828(3) 0.84953(13) 0.0550(8) Uani 1 1 d D . . . . C51B C 0.2276(6) -0.0056(7) 0.8402(5) 0.0481(15) Uani 0.569(4) 1 d D . P C 1 C52B C 0.2282(3) -0.1075(6) 0.8548(3) 0.0528(15) Uani 0.569(4) 1 d D . P C 1 H52B H 0.196120 -0.130002 0.871763 0.063 Uiso 0.569(4) 1 calc R U P C 1 C53B C 0.2745(3) -0.1764(6) 0.8453(2) 0.0661(16) Uani 0.569(4) 1 d D . P C 1 H53B H 0.272941 -0.245026 0.855170 0.079 Uiso 0.569(4) 1 calc R U P C 1 C54B C 0.3230(3) -0.1451(6) 0.8213(3) 0.0681(18) Uani 0.569(4) 1 d D . P C 1 H54B H 0.355763 -0.190969 0.816223 0.082 Uiso 0.569(4) 1 calc R U P C 1 C55B C 0.3232(4) -0.0472(7) 0.8050(3) 0.0704(18) Uani 0.569(4) 1 d D . P C 1 H55B H 0.354589 -0.025892 0.787238 0.084 Uiso 0.569(4) 1 calc R U P C 1 C56B C 0.2767(4) 0.0197(6) 0.8151(3) 0.0592(16) Uani 0.569(4) 1 d D . P C 1 H56B H 0.278241 0.087500 0.804324 0.071 Uiso 0.569(4) 1 calc R U P C 1 C51A C 0.2322(8) 0.0170(11) 0.8308(7) 0.0481(15) Uani 0.431(4) 1 d D . P C 2 C52A C 0.2463(5) -0.0782(8) 0.8489(4) 0.0528(15) Uani 0.431(4) 1 d D . P C 2 H52A H 0.219816 -0.106700 0.868777 0.063 Uiso 0.431(4) 1 calc R U P C 2 C53A C 0.2992(5) -0.1338(8) 0.8384(3) 0.0661(16) Uani 0.431(4) 1 d D . P C 2 H53A H 0.309353 -0.197995 0.851622 0.079 Uiso 0.431(4) 1 calc R U P C 2 C54A C 0.3352(5) -0.0922(9) 0.8088(3) 0.0681(18) Uani 0.431(4) 1 d D . P C 2 H54A H 0.369917 -0.129519 0.800277 0.082 Uiso 0.431(4) 1 calc R U P C 2 C55A C 0.3225(5) 0.0012(9) 0.7911(4) 0.0704(18) Uani 0.431(4) 1 d D . P C 2 H55A H 0.349518 0.029713 0.771586 0.084 Uiso 0.431(4) 1 calc R U P C 2 C56A C 0.2712(5) 0.0549(8) 0.8012(4) 0.0592(16) Uani 0.431(4) 1 d D . P C 2 H56A H 0.262204 0.119157 0.787749 0.071 Uiso 0.431(4) 1 calc R U P C 2 H H 0.2251(15) 0.588(2) 0.5985(10) 0.050(8) Uiso 1 1 d . . . . . H9A H 0.2040(19) 0.459(3) 0.5486(13) 0.079(12) Uiso 1 1 d . . . . . H9B H 0.2521(19) 0.395(3) 0.5178(12) 0.066(10) Uiso 1 1 d . . . . . H9C H 0.176(2) 0.390(3) 0.5072(14) 0.083(12) Uiso 1 1 d . . . . . 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 Ti1 0.0301(2) 0.0316(2) 0.0365(2) -0.00187(16) 0.00820(16) -0.00133(16) Ti2 0.0286(2) 0.0324(2) 0.0352(2) -0.00148(16) 0.00912(16) -0.00172(15) Si1 0.0388(3) 0.0296(3) 0.0547(4) 0.0009(3) 0.0100(3) -0.0017(3) Si2 0.0339(3) 0.0466(4) 0.0366(3) 0.0037(3) 0.0122(2) 0.0026(3) Si3 0.0294(3) 0.0901(7) 0.0579(5) -0.0164(4) 0.0067(3) 0.0147(4) Si4 0.0336(3) 0.0353(3) 0.0424(3) -0.0008(3) -0.0003(3) 0.0029(3) N1 0.0403(11) 0.0454(12) 0.0399(11) -0.0057(9) 0.0129(9) -0.0021(9) N2 0.0454(12) 0.0482(12) 0.0504(12) -0.0061(10) 0.0220(10) -0.0106(10) C1 0.0367(12) 0.0384(12) 0.0433(13) -0.0018(10) 0.0129(10) -0.0018(10) C2 0.0629(18) 0.0533(17) 0.0690(19) -0.0138(15) 0.0310(16) -0.0223(15) C3 0.0645(18) 0.0493(16) 0.0525(16) -0.0137(13) 0.0176(14) -0.0126(14) C4 0.093(3) 0.139(4) 0.098(3) -0.041(3) 0.067(3) -0.061(3) C5 0.068(2) 0.099(3) 0.0561(19) -0.0269(19) 0.0296(16) -0.010(2) C6 0.0556(17) 0.075(2) 0.0529(16) -0.0121(15) 0.0303(14) -0.0168(15) C7 0.0463(15) 0.0697(19) 0.0463(15) -0.0122(13) 0.0201(12) -0.0057(13) C9 0.076(2) 0.060(2) 0.066(2) 0.0060(16) -0.0139(18) -0.0106(18) C10 0.0475(16) 0.062(2) 0.088(2) -0.0111(17) 0.0012(16) 0.0018(15) C11 0.0506(15) 0.0367(13) 0.0644(18) -0.0067(12) 0.0001(13) -0.0045(12) C12 0.083(3) 0.063(2) 0.076(2) 0.0175(18) -0.0166(19) -0.0118(19) C13 0.0501(15) 0.0444(15) 0.0582(16) 0.0071(12) 0.0086(12) -0.0066(12) C14 0.075(2) 0.0539(18) 0.079(2) 0.0164(17) 0.0167(18) -0.0168(17) C15 0.115(4) 0.053(2) 0.119(4) -0.007(2) 0.028(3) 0.017(2) C16 0.0635(19) 0.0389(15) 0.102(3) -0.0011(16) 0.0293(18) 0.0069(14) C17 0.0522(18) 0.0512(19) 0.156(4) 0.023(2) 0.035(2) 0.0127(15) C18 0.069(2) 0.0541(18) 0.0654(19) -0.0092(15) 0.0229(16) 0.0130(15) C19 0.0494(15) 0.0595(17) 0.0492(15) 0.0030(13) 0.0182(12) 0.0156(13) C20 0.064(2) 0.085(2) 0.069(2) -0.0045(18) 0.0358(17) 0.0145(18) C21 0.0374(16) 0.130(4) 0.089(3) -0.018(3) 0.0075(16) -0.004(2) C22 0.0399(13) 0.0531(15) 0.0472(14) 0.0062(12) 0.0109(11) -0.0035(11) C23 0.074(2) 0.0523(17) 0.0559(17) 0.0071(14) 0.0099(15) -0.0164(15) C24 0.076(2) 0.091(3) 0.063(2) 0.0312(19) 0.0266(18) 0.007(2) C25 0.0524(16) 0.0598(17) 0.0455(14) 0.0107(13) 0.0110(12) 0.0068(13) C26 0.066(2) 0.076(2) 0.070(2) 0.0267(18) 0.0122(16) 0.0214(18) C27 0.0532(17) 0.0533(17) 0.075(2) -0.0099(15) -0.0089(15) 0.0190(14) C28 0.0391(14) 0.0489(16) 0.0736(19) -0.0043(14) 0.0058(13) 0.0083(12) C29 0.0401(18) 0.075(3) 0.194(6) -0.013(3) 0.004(2) 0.0085(18) C30 0.0431(15) 0.0500(16) 0.073(2) 0.0005(14) 0.0033(13) -0.0114(12) C31 0.0352(12) 0.0395(13) 0.0481(14) 0.0000(11) 0.0012(10) -0.0043(10) C32 0.0468(15) 0.0366(13) 0.0600(17) 0.0017(12) 0.0020(12) 0.0035(11) C33 0.082(2) 0.061(2) 0.0573(19) -0.0090(15) -0.0195(17) -0.0067(17) C34 0.0560(16) 0.0469(15) 0.0438(14) -0.0031(12) -0.0069(12) 0.0040(12) C35 0.083(2) 0.0555(18) 0.0516(17) 0.0094(14) -0.0091(16) 0.0065(17) C36 0.066(2) 0.143(4) 0.102(3) 0.003(3) 0.007(2) -0.045(3) C37 0.0405(16) 0.140(4) 0.064(2) -0.009(2) -0.0008(15) -0.012(2) C38 0.047(2) 0.257(8) 0.112(4) -0.005(5) -0.022(2) -0.005(3) C42 0.100(3) 0.085(3) 0.152(4) 0.010(3) -0.002(3) 0.046(3) C69 0.0304(11) 0.0324(11) 0.0377(11) 0.0030(9) 0.0058(9) -0.0009(9) C70 0.0342(11) 0.0342(12) 0.0407(12) -0.0012(9) 0.0078(9) 0.0040(9) C71 0.0335(11) 0.0368(12) 0.0346(11) 0.0021(9) 0.0090(9) 0.0018(9) C72 0.0351(11) 0.0340(11) 0.0366(12) 0.0006(9) 0.0037(9) 0.0021(9) C73 0.0332(11) 0.0312(11) 0.0420(12) 0.0048(9) 0.0069(9) 0.0000(9) C74 0.0303(11) 0.0332(11) 0.0401(12) 0.0029(9) 0.0078(9) 0.0020(9) C75 0.0304(11) 0.0408(13) 0.0398(12) -0.0006(10) 0.0080(9) 0.0013(9) C76 0.0396(12) 0.0432(13) 0.0329(11) -0.0021(10) 0.0061(9) 0.0018(10) C77 0.0362(12) 0.0320(11) 0.0459(13) 0.0011(10) 0.0083(10) 0.0006(9) C78 0.0287(10) 0.0331(11) 0.0351(11) 0.0037(9) 0.0071(8) 0.0000(9) C79 0.0402(12) 0.0439(13) 0.0350(12) 0.0021(10) 0.0058(9) 0.0037(10) C80 0.0389(12) 0.0408(13) 0.0414(13) 0.0068(10) 0.0104(10) -0.0001(10) C81 0.0278(10) 0.0361(12) 0.0368(11) 0.0020(9) 0.0066(8) 0.0004(9) C82 0.0331(11) 0.0333(11) 0.0454(13) -0.0013(10) 0.0094(9) 0.0040(9) C83 0.0329(11) 0.0407(13) 0.0390(12) -0.0025(10) 0.0033(9) -0.0026(10) C84 0.0289(10) 0.0324(11) 0.0392(12) 0.0040(9) 0.0054(9) 0.0008(9) C39A 0.047(5) 0.107(9) 0.082(7) -0.011(6) 0.002(5) 0.046(6) C40A 0.100(9) 0.140(11) 0.081(8) -0.032(7) -0.003(6) 0.090(9) C41A 0.055(8) 0.219(18) 0.076(8) 0.027(10) 0.027(7) 0.054(10) C43B 0.154(11) 0.101(5) 0.185(14) -0.010(6) -0.065(8) 0.034(7) C44B 0.097(4) 0.093(5) 0.101(4) 0.033(3) -0.010(3) 0.015(4) C39B 0.034(3) 0.101(5) 0.062(3) -0.014(3) 0.017(2) 0.015(3) C40B 0.043(3) 0.206(10) 0.087(5) -0.026(5) 0.032(3) 0.015(4) C41B 0.071(4) 0.117(5) 0.066(4) -0.027(3) 0.008(3) 0.027(3) C43A 0.154(11) 0.101(5) 0.185(14) -0.010(6) -0.065(8) 0.034(7) C44A 0.097(4) 0.093(5) 0.101(4) 0.033(3) -0.010(3) 0.015(4) C1S 0.181(14) 0.193(15) 0.249(18) -0.083(14) 0.106(13) -0.049(12) C2S 0.142(9) 0.112(8) 0.144(9) 0.037(7) 0.051(7) 0.025(7) C3S 0.119(6) 0.090(6) 0.083(5) -0.002(5) 0.016(4) -0.007(5) C4S 0.120(7) 0.119(8) 0.097(6) 0.047(6) 0.022(5) 0.019(6) C5S 0.083(5) 0.124(8) 0.053(4) 0.005(4) -0.005(3) -0.017(4) C6S 0.150(9) 0.166(11) 0.067(5) 0.029(6) 0.026(5) 0.044(8) C7S 0.110(9) 0.171(14) 0.163(13) -0.019(10) 0.022(8) 0.021(9) C45 0.0384(14) 0.0564(18) 0.081(2) 0.0061(15) 0.0017(13) 0.0123(13) C46 0.0512(18) 0.101(3) 0.083(2) 0.031(2) -0.0045(17) 0.0046(19) C47 0.060(2) 0.114(4) 0.112(3) 0.059(3) 0.010(2) 0.018(2) C48 0.0462(19) 0.084(3) 0.158(4) 0.043(3) 0.010(2) 0.0053(18) C49 0.0468(18) 0.070(2) 0.145(4) -0.009(3) 0.009(2) -0.0012(17) C50 0.0434(16) 0.063(2) 0.094(3) -0.0130(18) 0.0079(15) 0.0080(14) C57 0.0544(18) 0.069(2) 0.0681(19) 0.0018(16) 0.0128(15) 0.0102(15) C58 0.168(6) 0.123(4) 0.107(4) -0.011(3) -0.026(4) 0.083(4) C59 0.243(10) 0.175(8) 0.146(6) 0.017(5) -0.050(7) 0.118(7) C60 0.100(4) 0.157(5) 0.117(4) 0.068(4) -0.010(3) 0.022(4) C61 0.101(4) 0.194(6) 0.060(2) 0.034(3) 0.030(2) 0.034(4) C62 0.089(3) 0.116(3) 0.062(2) 0.012(2) 0.0242(19) 0.033(3) C63 0.0673(19) 0.0565(18) 0.0628(19) -0.0062(15) 0.0139(15) -0.0019(15) C64 0.102(3) 0.084(3) 0.092(3) -0.022(2) 0.016(2) 0.019(2) C65 0.165(5) 0.086(3) 0.105(4) -0.034(3) 0.031(4) 0.005(4) C66 0.187(6) 0.081(3) 0.099(4) -0.036(3) 0.035(4) -0.042(4) C67 0.101(4) 0.141(5) 0.117(4) -0.045(4) 0.021(3) -0.054(3) C68 0.075(2) 0.099(3) 0.095(3) -0.034(3) 0.015(2) -0.018(2) B1 0.0447(17) 0.0576(19) 0.063(2) -0.0075(16) 0.0079(14) 0.0062(14) C51B 0.038(2) 0.055(4) 0.049(6) -0.007(3) -0.002(2) 0.002(3) C52B 0.046(4) 0.062(4) 0.049(3) -0.003(3) -0.004(3) 0.010(3) C53B 0.062(4) 0.077(5) 0.056(3) -0.015(3) -0.015(3) 0.028(3) C54B 0.050(3) 0.096(5) 0.056(4) -0.024(3) -0.007(2) 0.030(4) C55B 0.042(2) 0.080(6) 0.089(6) -0.030(4) 0.004(3) 0.004(4) C56B 0.045(2) 0.060(5) 0.073(5) -0.011(3) 0.010(3) -0.002(3) C51A 0.038(2) 0.055(4) 0.049(6) -0.007(3) -0.002(2) 0.002(3) C52A 0.046(4) 0.062(4) 0.049(3) -0.003(3) -0.004(3) 0.010(3) C53A 0.062(4) 0.077(5) 0.056(3) -0.015(3) -0.015(3) 0.028(3) C54A 0.050(3) 0.096(5) 0.056(4) -0.024(3) -0.007(2) 0.030(4) C55A 0.042(2) 0.080(6) 0.089(6) -0.030(4) 0.004(3) 0.004(4) C56A 0.045(2) 0.060(5) 0.073(5) -0.011(3) 0.010(3) -0.002(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 '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 C71 Ti1 C82 104.24(9) C71 Ti1 C76 36.36(9) C82 Ti1 C76 117.96(9) C71 Ti1 C77 139.90(9) C82 Ti1 C77 36.32(8) C76 Ti1 C77 147.53(9) C71 Ti1 C74 81.41(8) C82 Ti1 C74 35.21(8) C76 Ti1 C74 111.15(9) C77 Ti1 C74 60.68(8) C71 Ti1 C83 60.71(8) C82 Ti1 C83 150.57(9) C76 Ti1 C83 34.91(9) C77 Ti1 C83 154.92(9) C74 Ti1 C83 142.12(9) C71 Ti1 C78 36.68(8) C82 Ti1 C78 125.63(8) C76 Ti1 C78 58.42(9) C77 Ti1 C78 145.52(9) C74 Ti1 C78 91.72(8) C83 Ti1 C78 58.58(8) C71 Ti1 C73 131.61(8) C82 Ti1 C73 57.45(8) C76 Ti1 C73 167.80(9) C77 Ti1 C73 35.41(8) C74 Ti1 C73 58.07(8) C83 Ti1 C73 151.76(8) C78 Ti1 C73 113.63(8) C71 Ti1 C84 97.21(8) C82 Ti1 C84 57.41(8) C76 Ti1 C84 133.48(8) C77 Ti1 C84 59.34(8) C74 Ti1 C84 34.80(8) C83 Ti1 C84 143.62(8) C78 Ti1 C84 86.18(8) C73 Ti1 C84 34.40(8) C71 Ti1 C81 59.66(8) C82 Ti1 C81 160.21(8) C76 Ti1 C81 57.02(8) C77 Ti1 C81 154.87(8) C74 Ti1 C81 125.65(8) C83 Ti1 C81 34.45(8) C78 Ti1 C81 34.58(7) C73 Ti1 C81 122.78(8) C84 Ti1 C81 110.33(8) C71 Ti1 Ti2 97.31(6) C82 Ti1 Ti2 114.16(7) C76 Ti1 Ti2 115.88(7) C77 Ti1 Ti2 96.23(6) C74 Ti1 Ti2 91.35(6) C83 Ti1 Ti2 93.66(6) C78 Ti1 Ti2 61.86(6) C73 Ti1 Ti2 61.77(6) C84 Ti1 Ti2 58.64(6) C81 Ti1 Ti2 61.08(6) C71 Ti1 H 122.3(10) C82 Ti1 H 126.3(10) C76 Ti1 H 115.4(10) C77 Ti1 H 91.7(10) C74 Ti1 H 123.9(10) C83 Ti1 H 81.0(10) C78 Ti1 H 87.4(10) C73 Ti1 H 71.3(10) C84 Ti1 H 89.4(10) C81 Ti1 H 64.3(10) Ti2 Ti1 H 40.7(10) C71 Ti1 H9A 127.9(10) C82 Ti1 H9A 102.2(11) C76 Ti1 H9A 91.6(11) C77 Ti1 H9A 80.4(11) C74 Ti1 H9A 137.1(11) C83 Ti1 H9A 74.5(11) C78 Ti1 H9A 130.9(11) C73 Ti1 H9A 100.4(11) C84 Ti1 H9A 134.7(10) C81 Ti1 H9A 97.2(11) Ti2 Ti1 H9A 111.4(11) H Ti1 H9A 70.7(15) C1 Ti2 C69 128.36(9) C1 Ti2 C79 83.17(9) C69 Ti2 C79 116.42(9) C1 Ti2 C70 94.93(9) C69 Ti2 C70 34.77(8) C79 Ti2 C70 129.23(9) C1 Ti2 C72 116.56(9) C69 Ti2 C72 85.67(8) C79 Ti2 C72 35.27(8) C70 Ti2 C72 111.68(8) C1 Ti2 C80 78.05(9) C69 Ti2 C80 143.92(8) C79 Ti2 C80 33.82(9) C70 Ti2 C80 161.69(9) C72 Ti2 C80 58.72(8) C1 Ti2 C84 134.17(9) C69 Ti2 C84 91.57(8) C79 Ti2 C84 56.26(8) C70 Ti2 C84 126.12(8) C72 Ti2 C84 35.26(8) C80 Ti2 C84 56.54(8) C1 Ti2 C75 86.11(9) C69 Ti2 C75 58.36(8) C79 Ti2 C75 159.13(9) C70 Ti2 C75 34.20(8) C72 Ti2 C75 143.67(8) C80 Ti2 C75 157.58(8) C84 Ti2 C75 139.04(8) C1 Ti2 C78 142.61(9) C69 Ti2 C78 33.97(8) C79 Ti2 C78 132.28(8) C70 Ti2 C78 55.49(8) C72 Ti2 C78 97.09(8) C80 Ti2 C78 136.99(8) C84 Ti2 C78 82.85(7) C75 Ti2 C78 56.51(7) C1 Ti2 Ti1 131.91(7) C69 Ti2 Ti1 88.13(6) C79 Ti2 Ti1 109.88(7) C70 Ti2 Ti1 108.51(6) C72 Ti2 Ti1 93.32(6) C80 Ti2 Ti1 88.36(6) C84 Ti2 Ti1 58.78(6) C75 Ti2 Ti1 90.58(6) C78 Ti2 Ti1 55.68(5) C1 Ti2 C81 112.96(9) C69 Ti2 C81 56.03(8) C79 Ti2 C81 163.70(8) C70 Ti2 C81 54.58(8) C72 Ti2 C81 129.68(8) C80 Ti2 C81 143.72(9) C84 Ti2 C81 107.88(8) C75 Ti2 C81 33.42(8) C78 Ti2 C81 32.98(7) Ti1 Ti2 C81 58.03(5) C1 Ti2 C73 107.33(9) C69 Ti2 C73 123.28(8) C79 Ti2 C73 55.03(8) C70 Ti2 C73 157.72(8) C72 Ti2 C73 57.53(8) C80 Ti2 C73 33.33(8) C84 Ti2 C73 33.44(7) C75 Ti2 C73 145.79(8) C78 Ti2 C73 104.26(8) Ti1 Ti2 C73 56.80(6) C81 Ti2 C73 114.77(8) C1 Ti2 H 89.9(11) C69 Ti2 H 116.2(11) C79 Ti2 H 117.2(11) C70 Ti2 H 113.5(11) C72 Ti2 H 124.4(11) C80 Ti2 H 83.6(11) C84 Ti2 H 90.8(11) C75 Ti2 H 80.6(11) C78 Ti2 H 83.5(11) Ti1 Ti2 H 42.4(11) C81 Ti2 H 62.8(11) C73 Ti2 H 68.5(11) C77 Si1 C13 109.73(13) C77 Si1 C11 108.89(12) C13 Si1 C11 112.89(14) C77 Si1 C16 105.15(13) C13 Si1 C16 113.99(16) C11 Si1 C16 105.78(16) C71 Si2 C22 108.33(11) C71 Si2 C25 104.46(12) C22 Si2 C25 114.33(14) C71 Si2 C19 109.92(12) C22 Si2 C19 110.48(13) C25 Si2 C19 109.12(14) C42 Si3 C75 106.3(2) C42 Si3 C37 103.7(2) C75 Si3 C37 107.99(16) C42 Si3 C39A 90.6(5) C75 Si3 C39A 113.8(3) C37 Si3 C39A 129.6(4) C42 Si3 C39B 121.4(3) C75 Si3 C39B 108.99(19) C37 Si3 C39B 107.8(2) C31 Si4 C28 110.83(13) C31 Si4 C34 109.54(13) C28 Si4 C34 113.21(14) C31 Si4 C72 111.34(11) C28 Si4 C72 106.03(12) C34 Si4 C72 105.76(13) C1 N1 C7 112.7(2) C1 N1 C3 125.2(2) C7 N1 C3 122.0(2) C1 N2 C6 111.7(2) C1 N2 C2 125.7(2) C6 N2 C2 122.2(2) N1 C1 N2 102.8(2) N1 C1 Ti2 124.66(18) N2 C1 Ti2 132.52(18) N2 C2 H2A 109.5 N2 C2 H2B 109.5 H2A C2 H2B 109.5 N2 C2 H2C 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 N1 C3 H3A 109.5 N1 C3 H3B 109.5 H3A C3 H3B 109.5 N1 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 C6 C4 H4A 109.5 C6 C4 H4B 109.5 H4A C4 H4B 109.5 C6 C4 H4C 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 C7 C5 H5A 109.5 C7 C5 H5B 109.5 H5A C5 H5B 109.5 C7 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 C7 C6 N2 106.7(2) C7 C6 C4 131.6(3) N2 C6 C4 121.7(3) C6 C7 N1 106.0(2) C6 C7 C5 130.5(3) N1 C7 C5 123.4(3) C11 C9 H9A 109(2) C11 C9 H9B 113(2) H9A C9 H9B 107(3) C11 C9 H9C 115(2) H9A C9 H9C 104(3) H9B C9 H9C 109(3) C11 C10 H10A 109.5 C11 C10 H10B 109.5 H10A C10 H10B 109.5 C11 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C9 C11 C10 109.4(3) C9 C11 Si1 110.9(2) C10 C11 Si1 116.7(2) C9 C11 H11 106.4 C10 C11 H11 106.4 Si1 C11 H11 106.4 C13 C12 H12A 109.5 C13 C12 H12B 109.5 H12A C12 H12B 109.5 C13 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C12 C13 C14 108.9(3) C12 C13 Si1 114.3(2) C14 C13 Si1 113.1(2) C12 C13 H13 106.7 C14 C13 H13 106.7 Si1 C13 H13 106.7 C13 C14 H14A 109.5 C13 C14 H14B 109.5 H14A C14 H14B 109.5 C13 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C16 C15 H15A 109.5 C16 C15 H15B 109.5 H15A C15 H15B 109.5 C16 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C15 C16 C17 112.2(3) C15 C16 Si1 114.9(3) C17 C16 Si1 113.0(3) C15 C16 H16 105.2 C17 C16 H16 105.2 Si1 C16 H16 105.2 C16 C17 H17A 109.5 C16 C17 H17B 109.5 H17A C17 H17B 109.5 C16 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C19 C18 H18A 109.5 C19 C18 H18B 109.5 H18A C18 H18B 109.5 C19 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C18 C19 C20 108.4(3) C18 C19 Si2 115.3(2) C20 C19 Si2 112.5(2) C18 C19 H19 106.7 C20 C19 H19 106.7 Si2 C19 H19 106.7 C19 C20 H20A 109.5 C19 C20 H20B 109.5 H20A C20 H20B 109.5 C19 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 C22 C21 H21A 109.5 C22 C21 H21B 109.5 H21A C21 H21B 109.5 C22 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C21 C22 C23 109.0(3) C21 C22 Si2 116.4(2) C23 C22 Si2 113.1(2) C21 C22 H22 105.8 C23 C22 H22 105.8 Si2 C22 H22 105.8 C22 C23 H23A 109.5 C22 C23 H23B 109.5 H23A C23 H23B 109.5 C22 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C25 C24 H24A 109.5 C25 C24 H24B 109.5 H24A C24 H24B 109.5 C25 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C24 C25 C26 109.6(3) C24 C25 Si2 116.7(2) C26 C25 Si2 113.3(2) C24 C25 H25 105.4 C26 C25 H25 105.4 Si2 C25 H25 105.4 C25 C26 H26A 109.5 C25 C26 H26B 109.5 H26A C26 H26B 109.5 C25 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C28 C27 H27A 109.5 C28 C27 H27B 109.5 H27A C27 H27B 109.5 C28 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C29 C28 C27 108.8(3) C29 C28 Si4 115.3(3) C27 C28 Si4 113.8(2) C29 C28 H28 106.1 C27 C28 H28 106.1 Si4 C28 H28 106.1 C28 C29 H29A 109.5 C28 C29 H29B 109.5 H29A C29 H29B 109.5 C28 C29 H29C 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C31 C30 H30A 109.5 C31 C30 H30B 109.5 H30A C30 H30B 109.5 C31 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C32 C31 C30 110.0(2) C32 C31 Si4 110.78(18) C30 C31 Si4 118.58(19) C32 C31 H31 105.5 C30 C31 H31 105.5 Si4 C31 H31 105.5 C31 C32 H32A 109.5 C31 C32 H32B 109.5 H32A C32 H32B 109.5 C31 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C34 C33 H33A 109.5 C34 C33 H33B 109.5 H33A C33 H33B 109.5 C34 C33 H33C 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C35 C34 C33 108.6(3) C35 C34 Si4 115.3(2) C33 C34 Si4 114.4(2) C35 C34 H34 105.9 C33 C34 H34 105.9 Si4 C34 H34 105.9 C34 C35 H35A 109.5 C34 C35 H35B 109.5 H35A C35 H35B 109.5 C34 C35 H35C 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 C37 C36 H36A 109.5 C37 C36 H36B 109.5 H36A C36 H36B 109.5 C37 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C36 C37 C38 110.5(4) C36 C37 Si3 113.9(3) C38 C37 Si3 116.0(4) C36 C37 H37 105.1 C38 C37 H37 105.1 Si3 C37 H37 105.1 C37 C38 H38A 109.5 C37 C38 H38B 109.5 H38A C38 H38B 109.5 C37 C38 H38C 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 C43A C42 C44A 92.4(16) C43B C42 C44B 105.2(9) C43B C42 Si3 115.6(9) C43A C42 Si3 104.6(18) C44A C42 Si3 118.1(6) C44B C42 Si3 113.1(4) C43A C42 H42A 113.2 C44A C42 H42A 113.2 Si3 C42 H42A 113.2 C43B C42 H42 107.5 C44B C42 H42 107.5 Si3 C42 H42 107.5 C70 C69 C78 106.9(2) C70 C69 Ti2 73.49(14) C78 C69 Ti2 79.93(13) C70 C69 H69 126.6 C78 C69 H69 126.6 Ti2 C69 H69 112.7 C69 C70 C75 112.0(2) C69 C70 Ti2 71.74(13) C75 C70 Ti2 76.72(14) C69 C70 H70 124.0 C75 C70 H70 124.0 Ti2 C70 H70 119.0 C76 C71 C78 103.7(2) C76 C71 Si2 120.66(17) C78 C71 Si2 130.24(18) C76 C71 Ti1 72.49(14) C78 C71 Ti1 74.58(13) Si2 C71 Ti1 136.97(12) C79 C72 C84 103.0(2) C79 C72 Si4 120.53(18) C84 C72 Si4 125.92(17) C79 C72 Ti2 71.73(14) C84 C72 Ti2 75.07(13) Si4 C72 Ti2 145.28(12) C80 C73 C84 106.8(2) C80 C73 C77 143.4(2) C84 C73 C77 109.8(2) C80 C73 Ti1 125.87(17) C84 C73 Ti1 73.82(13) C77 C73 Ti1 68.04(13) C80 C73 Ti2 68.43(14) C84 C73 Ti2 69.28(13) C77 C73 Ti2 127.54(17) Ti1 C73 Ti2 61.43(6) C82 C74 C84 107.3(2) C82 C74 Ti1 71.04(13) C84 C74 Ti1 77.04(13) C82 C74 H74 126.3 C84 C74 H74 126.3 Ti1 C74 H74 117.6 C70 C75 C81 103.9(2) C70 C75 Si3 124.88(18) C81 C75 Si3 123.49(18) C70 C75 Ti2 69.08(13) C81 C75 Ti2 76.22(13) Si3 C75 Ti2 143.14(13) C83 C76 C71 111.9(2) C83 C76 Ti1 74.33(14) C71 C76 Ti1 71.15(13) C83 C76 H76 124.1 C71 C76 H76 124.1 Ti1 C76 H76 122.0 C82 C77 C73 104.1(2) C82 C77 Si1 123.02(18) C73 C77 Si1 131.88(18) C82 C77 Ti1 71.39(14) C73 C77 Ti1 76.55(14) Si1 C77 Ti1 124.58(13) C69 C78 C81 106.6(2) C69 C78 C71 143.8(2) C81 C78 C71 109.3(2) C69 C78 Ti1 125.22(16) C81 C78 Ti1 76.52(13) C71 C78 Ti1 68.74(13) C69 C78 Ti2 66.10(12) C81 C78 Ti2 74.22(13) C71 C78 Ti2 128.72(16) Ti1 C78 Ti2 62.46(6) C80 C79 C72 112.7(2) C80 C79 Ti2 75.69(15) C72 C79 Ti2 73.00(14) C80 C79 H79 123.6 C72 C79 H79 123.6 Ti2 C79 H79 119.1 C79 C80 C73 107.3(2) C79 C80 Ti2 70.48(14) C73 C80 Ti2 78.24(14) C79 C80 H80 126.4 C73 C80 H80 126.4 Ti2 C80 H80 117.0 C83 C81 C78 107.0(2) C83 C81 C75 142.6(2) C78 C81 C75 110.2(2) C83 C81 Ti1 68.35(13) C78 C81 Ti1 68.90(13) C75 C81 Ti1 129.24(16) C83 C81 Ti2 125.39(17) C78 C81 Ti2 72.80(13) C75 C81 Ti2 70.35(13) Ti1 C81 Ti2 60.89(5) C74 C82 C77 111.5(2) C74 C82 Ti1 73.75(13) C77 C82 Ti1 72.28(14) C74 C82 H82 124.3 C77 C82 H82 124.3 Ti1 C82 H82 121.3 C76 C83 C81 107.6(2) C76 C83 Ti1 70.76(14) C81 C83 Ti1 77.20(14) C76 C83 H83 126.2 C81 C83 H83 126.2 Ti1 C83 H83 117.8 C74 C84 C73 106.9(2) C74 C84 C72 142.7(2) C73 C84 C72 109.8(2) C74 C84 Ti2 126.24(16) C73 C84 Ti2 77.29(13) C72 C84 Ti2 69.67(13) C74 C84 Ti1 68.16(13) C73 C84 Ti1 71.77(13) C72 C84 Ti1 130.65(16) Ti2 C84 Ti1 62.59(6) C40A C39A C41A 109.8(10) C40A C39A Si3 118.3(8) C41A C39A Si3 102.8(10) C40A C39A H39A 108.5 C41A C39A H39A 108.5 Si3 C39A H39A 108.5 C39A C40A H40A 109.5 C39A C40A H40B 109.5 H40A C40A H40B 109.5 C39A C40A H40C 109.5 H40A C40A H40C 109.5 H40B C40A H40C 109.5 C39A C41A H41A 109.5 C39A C41A H41B 109.5 H41A C41A H41B 109.5 C39A C41A H41C 109.5 H41A C41A H41C 109.5 H41B C41A H41C 109.5 C42 C43B H43A 109.5 C42 C43B H43B 109.5 H43A C43B H43B 109.5 C42 C43B H43C 109.5 H43A C43B H43C 109.5 H43B C43B H43C 109.5 C42 C44B H44A 109.5 C42 C44B H44B 109.5 H44A C44B H44B 109.5 C42 C44B H44C 109.5 H44A C44B H44C 109.5 H44B C44B H44C 109.5 C41B C39B C40B 110.2(6) C41B C39B Si3 111.7(5) C40B C39B Si3 114.5(4) C41B C39B H39B 106.7 C40B C39B H39B 106.7 Si3 C39B H39B 106.7 C39B C40B H40D 109.5 C39B C40B H40E 109.5 H40D C40B H40E 109.5 C39B C40B H40F 109.5 H40D C40B H40F 109.5 H40E C40B H40F 109.5 C39B C41B H41D 109.5 C39B C41B H41E 109.5 H41D C41B H41E 109.5 C39B C41B H41F 109.5 H41D C41B H41F 109.5 H41E C41B H41F 109.5 C42 C43A H43D 109.5 C42 C43A H43E 109.5 H43D C43A H43E 109.5 C42 C43A H43F 109.5 H43D C43A H43F 109.5 H43E C43A H43F 109.5 C42 C44A H44D 109.5 C42 C44A H44E 109.5 H44D C44A H44E 109.5 C42 C44A H44F 109.5 H44D C44A H44F 109.5 H44E C44A H44F 109.5 C2S C1S H1SA 109.5 C2S C1S H1SB 109.5 H1SA C1S H1SB 109.5 C2S C1S H1SC 109.5 H1SA C1S H1SC 109.5 H1SB C1S H1SC 109.5 C1S C2S C3S 120.0(12) C1S C2S H2SA 107.3 C3S C2S H2SA 107.3 C1S C2S H2SB 107.3 C3S C2S H2SB 107.3 H2SA C2S H2SB 106.9 C4S C3S C2S 117.3(8) C4S C3S H3SA 108.0 C2S C3S H3SA 108.0 C4S C3S H3SB 108.0 C2S C3S H3SB 108.0 H3SA C3S H3SB 107.2 C3S C4S C5S 117.1(8) C3S C4S H4SA 108.0 C5S C4S H4SA 108.0 C3S C4S H4SB 108.0 C5S C4S H4SB 108.0 H4SA C4S H4SB 107.3 C4S C5S C6S 116.7(7) C4S C5S H5SA 108.1 C6S C5S H5SA 108.1 C4S C5S H5SB 108.1 C6S C5S H5SB 108.1 H5SA C5S H5SB 107.3 C7S C6S C5S 113.2(9) C7S C6S H6SA 108.9 C5S C6S H6SA 108.9 C7S C6S H6SB 108.9 C5S C6S H6SB 108.9 H6SA C6S H6SB 107.7 C6S C7S H7SA 109.5 C6S C7S H7SB 109.5 H7SA C7S H7SB 109.5 C6S C7S H7SC 109.5 H7SA C7S H7SC 109.5 H7SB C7S H7SC 109.5 C13S C8S C9S 120.0 C13S C8S C14S 116.7(13) C9S C8S C14S 122.7(13) C12S C13S C8S 120.0 C12S C13S H13S 120.0 C8S C13S H13S 120.0 C11S C12S C13S 120.0 C11S C12S H12S 120.0 C13S C12S H12S 120.0 C12S C11S C10S 120.0 C12S C11S H11S 120.0 C10S C11S H11S 120.0 C9S C10S C11S 120.0 C9S C10S H10S 120.0 C11S C10S H10S 120.0 C10S C9S C8S 120.0 C10S C9S H9S 120.0 C8S C9S H9S 120.0 C8S C14S H14D 109.5 C8S C14S H14E 109.5 H14D C14S H14E 109.5 C8S C14S H14F 109.5 H14D C14S H14F 109.5 H14E C14S H14F 109.5 C46 C45 C50 115.4(3) C46 C45 B1 123.2(3) C50 C45 B1 121.4(3) C47 C46 C45 123.0(4) C47 C46 H46 118.5 C45 C46 H46 118.5 C48 C47 C46 119.3(5) C48 C47 H47 120.3 C46 C47 H47 120.3 C49 C48 C47 119.5(4) C49 C48 H48 120.2 C47 C48 H48 120.2 C48 C49 C50 120.3(4) C48 C49 H49 119.8 C50 C49 H49 119.8 C49 C50 C45 122.4(4) C49 C50 H50 118.8 C45 C50 H50 118.8 C62 C57 C58 112.8(4) C62 C57 B1 123.9(3) C58 C57 B1 123.3(4) C59 C58 C57 123.7(6) C59 C58 H58 118.1 C57 C58 H58 118.1 C60 C59 C58 121.3(7) C60 C59 H59 119.4 C58 C59 H59 119.4 C59 C60 C61 118.5(5) C59 C60 H60 120.8 C61 C60 H60 120.8 C60 C61 C62 119.7(5) C60 C61 H61 120.1 C62 C61 H61 120.1 C57 C62 C61 123.9(5) C57 C62 H62 118.1 C61 C62 H62 118.1 C68 C63 C64 114.9(4) C68 C63 B1 125.2(3) C64 C63 B1 120.0(4) C65 C64 C63 123.0(5) C65 C64 H64 118.5 C63 C64 H64 118.5 C64 C65 C66 119.6(5) C64 C65 H65 120.2 C66 C65 H65 120.2 C67 C66 C65 119.4(5) C67 C66 H66 120.3 C65 C66 H66 120.3 C66 C67 C68 120.8(6) C66 C67 H67 119.6 C68 C67 H67 119.6 C63 C68 C67 122.2(5) C63 C68 H68 118.9 C67 C68 H68 118.9 C63 B1 C57 109.9(3) C63 B1 C45 109.2(3) C57 B1 C45 109.1(3) C63 B1 C51A 108.3(9) C57 B1 C51A 102.9(7) C45 B1 C51A 117.2(5) C63 B1 C51B 110.1(7) C57 B1 C51B 114.8(5) C45 B1 C51B 103.4(4) C56B C51B C52B 114.4(6) C56B C51B B1 119.4(6) C52B C51B B1 126.2(6) C53B C52B C51B 122.2(7) C53B C52B H52B 118.9 C51B C52B H52B 118.9 C54B C53B C52B 120.3(7) C54B C53B H53B 119.9 C52B C53B H53B 119.9 C55B C54B C53B 119.6(7) C55B C54B H54B 120.2 C53B C54B H54B 120.2 C54B C55B C56B 118.8(7) C54B C55B H55B 120.6 C56B C55B H55B 120.6 C55B C56B C51B 124.7(7) C55B C56B H56B 117.7 C51B C56B H56B 117.7 C56A C51A C52A 117.5(8) C56A C51A B1 124.1(8) C52A C51A B1 118.1(8) C51A C52A C53A 121.5(9) C51A C52A H52A 119.3 C53A C52A H52A 119.3 C54A C53A C52A 117.8(9) C54A C53A H53A 121.1 C52A C53A H53A 121.1 C55A C54A C53A 121.5(9) C55A C54A H54A 119.3 C53A C54A H54A 119.3 C54A C55A C56A 120.6(10) C54A C55A H55A 119.7 C56A C55A H55A 119.7 C55A C56A C51A 121.1(9) C55A C56A H56A 119.4 C51A C56A H56A 119.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ti1 C71 2.293(2) Ti1 C82 2.302(2) Ti1 C76 2.311(2) Ti1 C77 2.314(2) Ti1 C74 2.337(2) Ti1 C83 2.357(2) Ti1 C78 2.372(2) Ti1 C73 2.426(2) Ti1 C84 2.453(2) Ti1 C81 2.473(2) Ti1 Ti2 2.5467(6) Ti1 H 1.73(3) Ti1 H9A 2.19(4) Ti2 C1 2.260(2) Ti2 C69 2.352(2) Ti2 C79 2.361(2) Ti2 C70 2.374(2) Ti2 C72 2.377(2) Ti2 C80 2.427(3) Ti2 C84 2.450(2) Ti2 C75 2.474(2) Ti2 C78 2.533(2) Ti2 C81 2.551(2) Ti2 C73 2.555(2) Ti2 H 1.67(3) Si1 C77 1.883(3) Si1 C13 1.883(3) Si1 C11 1.895(3) Si1 C16 1.902(3) Si2 C71 1.883(2) Si2 C22 1.896(3) Si2 C25 1.898(3) Si2 C19 1.918(3) Si3 C42 1.861(6) Si3 C75 1.888(2) Si3 C37 1.890(4) Si3 C39A 1.917(10) Si3 C39B 1.939(6) Si4 C31 1.894(3) Si4 C28 1.896(3) Si4 C34 1.898(3) Si4 C72 1.906(3) N1 C1 1.352(3) N1 C7 1.393(3) N1 C3 1.453(4) N2 C1 1.363(3) N2 C6 1.395(4) N2 C2 1.451(4) 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 C6 1.504(4) C4 H4A 0.9800 C4 H4B 0.9800 C4 H4C 0.9800 C5 C7 1.492(4) C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C6 C7 1.335(5) C9 C11 1.523(5) C9 H9A 1.07(4) C9 H9B 1.02(4) C9 H9C 1.00(4) C10 C11 1.533(5) C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 H11 1.0000 C12 C13 1.539(4) C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 C14 1.540(4) C13 H13 1.0000 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 C16 1.523(5) C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C16 C17 1.546(6) C16 H16 1.0000 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 C19 1.518(5) C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 C20 1.544(4) C19 H19 1.0000 C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 C22 1.530(4) C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C22 C23 1.537(4) C22 H22 1.0000 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 C25 1.538(4) C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 C26 1.547(4) C25 H25 1.0000 C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 C28 1.532(4) C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C28 C29 1.530(5) C28 H28 1.0000 C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 C30 C31 1.545(4) C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 C31 C32 1.536(4) C31 H31 1.0000 C32 H32A 0.9800 C32 H32B 0.9800 C32 H32C 0.9800 C33 C34 1.544(4) C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C34 C35 1.535(4) C34 H34 1.0000 C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C36 C37 1.493(7) C36 H36A 0.9800 C36 H36B 0.9800 C36 H36C 0.9800 C37 C38 1.540(5) C37 H37 1.0000 C38 H38A 0.9800 C38 H38B 0.9800 C38 H38C 0.9800 C42 C43B 1.484(8) C42 C43A 1.495(9) C42 C44A 1.501(9) C42 C44B 1.537(7) C42 H42A 1.0000 C42 H42 1.0000 C69 C70 1.412(3) C69 C78 1.437(3) C69 H69 0.9500 C70 C75 1.429(3) C70 H70 0.9500 C71 C76 1.437(3) C71 C78 1.470(3) C72 C79 1.436(3) C72 C84 1.464(3) C73 C80 1.434(3) C73 C84 1.443(3) C73 C77 1.445(3) C74 C82 1.403(3) C74 C84 1.437(3) C74 H74 0.9500 C75 C81 1.447(3) C76 C83 1.401(3) C76 H76 0.9500 C77 C82 1.439(3) C78 C81 1.443(3) C79 C80 1.394(4) C79 H79 0.9500 C80 H80 0.9500 C81 C83 1.434(3) C82 H82 0.9500 C83 H83 0.9500 C39A C40A 1.545(15) C39A C41A 1.552(16) C39A H39A 1.0000 C40A H40A 0.9800 C40A H40B 0.9800 C40A H40C 0.9800 C41A H41A 0.9800 C41A H41B 0.9800 C41A H41C 0.9800 C43B H43A 0.9800 C43B H43B 0.9800 C43B H43C 0.9800 C44B H44A 0.9800 C44B H44B 0.9800 C44B H44C 0.9800 C39B C41B 1.506(10) C39B C40B 1.529(7) C39B H39B 1.0000 C40B H40D 0.9800 C40B H40E 0.9800 C40B H40F 0.9800 C41B H41D 0.9800 C41B H41E 0.9800 C41B H41F 0.9800 C43A H43D 0.9800 C43A H43E 0.9800 C43A H43F 0.9800 C44A H44D 0.9800 C44A H44E 0.9800 C44A H44F 0.9800 C1S C2S 1.449(13) C1S H1SA 0.9800 C1S H1SB 0.9800 C1S H1SC 0.9800 C2S C3S 1.508(12) C2S H2SA 0.9900 C2S H2SB 0.9900 C3S C4S 1.446(11) C3S H3SA 0.9900 C3S H3SB 0.9900 C4S C5S 1.457(12) C4S H4SA 0.9900 C4S H4SB 0.9900 C5S C6S 1.560(10) C5S H5SA 0.9900 C5S H5SB 0.9900 C6S C7S 1.507(11) C6S H6SA 0.9900 C6S H6SB 0.9900 C7S H7SA 0.9800 C7S H7SB 0.9800 C7S H7SC 0.9800 C8S C13S 1.3900 C8S C9S 1.3900 C8S C14S 1.56(3) C13S C12S 1.3900 C13S H13S 0.9500 C12S C11S 1.3900 C12S H12S 0.9500 C11S C10S 1.3900 C11S H11S 0.9500 C10S C9S 1.3900 C10S H10S 0.9500 C9S H9S 0.9500 C14S H14D 0.9800 C14S H14E 0.9800 C14S H14F 0.9800 C45 C46 1.399(5) C45 C50 1.399(5) C45 B1 1.648(5) C46 C47 1.389(6) C46 H46 0.9500 C47 C48 1.388(7) C47 H47 0.9500 C48 C49 1.373(7) C48 H48 0.9500 C49 C50 1.386(6) C49 H49 0.9500 C50 H50 0.9500 C57 C62 1.374(6) C57 C58 1.390(6) C57 B1 1.646(5) C58 C59 1.357(8) C58 H58 0.9500 C59 C60 1.336(10) C59 H59 0.9500 C60 C61 1.359(9) C60 H60 0.9500 C61 C62 1.383(6) C61 H61 0.9500 C62 H62 0.9500 C63 C68 1.369(6) C63 C64 1.415(5) C63 B1 1.639(5) C64 C65 1.367(7) C64 H64 0.9500 C65 C66 1.383(9) C65 H65 0.9500 C66 C67 1.335(8) C66 H66 0.9500 C67 C68 1.406(6) C67 H67 0.9500 C68 H68 0.9500 B1 C51A 1.653(10) B1 C51B 1.666(8) C51B C56B 1.404(8) C51B C52B 1.408(8) C52B C53B 1.396(8) C52B H52B 0.9500 C53B C54B 1.395(9) C53B H53B 0.9500 C54B C55B 1.376(10) C54B H54B 0.9500 C55B C56B 1.387(9) C55B H55B 0.9500 C56B H56B 0.9500 C51A C56A 1.383(10) C51A C52A 1.387(10) C52A C53A 1.414(11) C52A H52A 0.9500 C53A C54A 1.362(12) C53A H53A 0.9500 C54A C55A 1.354(11) C54A H54A 0.9500 C55A C56A 1.369(10) C55A H55A 0.9500 C56A H56A 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 C7 N1 C1 N2 -1.3(3) C3 N1 C1 N2 175.4(3) C7 N1 C1 Ti2 179.9(2) C3 N1 C1 Ti2 -3.4(4) C6 N2 C1 N1 1.1(3) C2 N2 C1 N1 -172.4(3) C6 N2 C1 Ti2 179.7(2) C2 N2 C1 Ti2 6.2(5) C1 N2 C6 C7 -0.5(4) C2 N2 C6 C7 173.2(3) C1 N2 C6 C4 177.2(4) C2 N2 C6 C4 -9.1(6) N2 C6 C7 N1 -0.3(4) C4 C6 C7 N1 -177.7(5) N2 C6 C7 C5 177.6(4) C4 C6 C7 C5 0.2(8) C1 N1 C7 C6 1.0(4) C3 N1 C7 C6 -175.8(3) C1 N1 C7 C5 -177.1(3) C3 N1 C7 C5 6.1(5) C77 Si1 C11 C9 20.9(3) C13 Si1 C11 C9 143.0(3) C16 Si1 C11 C9 -91.7(3) C77 Si1 C11 C10 -105.2(2) C13 Si1 C11 C10 16.9(3) C16 Si1 C11 C10 142.2(2) C77 Si1 C13 C12 -48.0(3) C11 Si1 C13 C12 -169.6(2) C16 Si1 C13 C12 69.6(3) C77 Si1 C13 C14 -173.4(2) C11 Si1 C13 C14 65.0(3) C16 Si1 C13 C14 -55.7(3) C71 Si2 C22 C21 148.5(3) C25 Si2 C22 C21 -95.5(3) C19 Si2 C22 C21 28.1(3) C71 Si2 C22 C23 -84.2(2) C25 Si2 C22 C23 31.8(2) C19 Si2 C22 C23 155.4(2) C71 Si2 C25 C24 166.7(3) C22 Si2 C25 C24 48.5(3) C19 Si2 C25 C24 -75.8(3) C71 Si2 C25 C26 38.1(3) C22 Si2 C25 C26 -80.1(3) C19 Si2 C25 C26 155.6(3) C31 Si4 C28 C29 65.2(4) C34 Si4 C28 C29 -58.4(4) C72 Si4 C28 C29 -173.9(3) C31 Si4 C28 C27 -168.2(2) C34 Si4 C28 C27 68.3(3) C72 Si4 C28 C27 -47.2(3) C28 Si4 C31 C32 -172.99(19) C34 Si4 C31 C32 -47.4(2) C72 Si4 C31 C32 69.2(2) C28 Si4 C31 C30 -44.5(3) C34 Si4 C31 C30 81.1(2) C72 Si4 C31 C30 -162.3(2) C31 Si4 C34 C35 -174.2(2) C28 Si4 C34 C35 -50.0(3) C72 Si4 C34 C35 65.7(3) C31 Si4 C34 C33 -47.2(3) C28 Si4 C34 C33 77.0(3) C72 Si4 C34 C33 -167.3(2) C42 Si3 C37 C36 172.4(3) C75 Si3 C37 C36 59.9(3) C39A Si3 C37 C36 -85.1(6) C39B Si3 C37 C36 -57.7(4) C42 Si3 C37 C38 -57.7(4) C75 Si3 C37 C38 -170.2(3) C39A Si3 C37 C38 44.8(7) C39B Si3 C37 C38 72.2(4) C75 Si3 C42 C43B -49.4(7) C37 Si3 C42 C43B -163.1(7) C39A Si3 C42 C43B 65.7(8) C75 Si3 C42 C43A -79.9(14) C37 Si3 C42 C43A 166.4(14) C39B Si3 C42 C43A 45.2(14) C75 Si3 C42 C44A 21.0(9) C37 Si3 C42 C44A -92.7(9) C39B Si3 C42 C44A 146.1(9) C75 Si3 C42 C44B 72.0(5) C37 Si3 C42 C44B -41.7(5) C39A Si3 C42 C44B -173.0(6) C78 C69 C70 C75 6.9(3) Ti2 C69 C70 C75 -66.79(18) C78 C69 C70 Ti2 73.71(16) C22 Si2 C71 C76 177.9(2) C25 Si2 C71 C76 55.6(2) C19 Si2 C71 C76 -61.3(2) C22 Si2 C71 C78 28.2(3) C25 Si2 C71 C78 -94.0(2) C19 Si2 C71 C78 149.0(2) C22 Si2 C71 Ti1 -85.1(2) C25 Si2 C71 Ti1 152.64(18) C19 Si2 C71 Ti1 35.7(2) C69 C70 C75 C81 -5.4(3) Ti2 C70 C75 C81 -69.09(16) C69 C70 C75 Si3 -155.21(19) Ti2 C70 C75 Si3 141.05(19) C69 C70 C75 Ti2 63.74(18) C42 Si3 C75 C70 67.4(3) C37 Si3 C75 C70 178.1(2) C39A Si3 C75 C70 -30.7(6) C39B Si3 C75 C70 -65.0(3) C42 Si3 C75 C81 -76.8(3) C37 Si3 C75 C81 33.9(3) C39A Si3 C75 C81 -174.9(5) C39B Si3 C75 C81 150.8(3) C42 Si3 C75 Ti2 169.2(3) C37 Si3 C75 Ti2 -80.1(3) C39A Si3 C75 Ti2 71.1(6) C39B Si3 C75 Ti2 36.8(3) C78 C71 C76 C83 -5.0(3) Si2 C71 C76 C83 -161.63(18) Ti1 C71 C76 C83 63.61(19) C78 C71 C76 Ti1 -68.65(15) Si2 C71 C76 Ti1 134.76(17) C80 C73 C77 C82 -172.4(3) C84 C73 C77 C82 4.2(3) Ti1 C73 C77 C82 66.51(16) Ti2 C73 C77 C82 82.7(2) C80 C73 C77 Si1 -3.6(5) C84 C73 C77 Si1 172.95(19) Ti1 C73 C77 Si1 -124.7(2) Ti2 C73 C77 Si1 -108.5(2) C80 C73 C77 Ti1 121.1(4) C84 C73 C77 Ti1 -62.35(17) Ti2 C73 C77 Ti1 16.23(16) C13 Si1 C77 C82 145.2(2) C11 Si1 C77 C82 -90.7(2) C16 Si1 C77 C82 22.2(3) C13 Si1 C77 C73 -21.8(3) C11 Si1 C77 C73 102.3(3) C16 Si1 C77 C73 -144.8(3) C13 Si1 C77 Ti1 -125.57(16) C11 Si1 C77 Ti1 -1.55(19) C16 Si1 C77 Ti1 111.43(19) C70 C69 C78 C81 -5.4(3) Ti2 C69 C78 C81 63.73(16) C70 C69 C78 C71 167.2(3) Ti2 C69 C78 C71 -123.6(3) C70 C69 C78 Ti1 -90.5(2) Ti2 C69 C78 Ti1 -21.28(15) C70 C69 C78 Ti2 -69.18(16) C76 C71 C78 C69 -171.8(3) Si2 C71 C78 C69 -18.4(5) Ti1 C71 C78 C69 121.1(3) C76 C71 C78 C81 0.8(3) Si2 C71 C78 C81 154.19(19) Ti1 C71 C78 C81 -66.35(16) C76 C71 C78 Ti1 67.13(16) Si2 C71 C78 Ti1 -139.5(2) C76 C71 C78 Ti2 85.7(2) Si2 C71 C78 Ti2 -120.88(19) Ti1 C71 C78 Ti2 18.58(16) C84 C72 C79 C80 -3.3(3) Si4 C72 C79 C80 -149.98(19) Ti2 C72 C79 C80 65.91(19) C84 C72 C79 Ti2 -69.21(15) Si4 C72 C79 Ti2 144.11(17) C72 C79 C80 C73 6.1(3) Ti2 C79 C80 C73 70.33(17) C72 C79 C80 Ti2 -64.28(18) C84 C73 C80 C79 -6.1(3) C77 C73 C80 C79 170.4(3) Ti1 C73 C80 C79 -88.0(2) Ti2 C73 C80 C79 -65.04(17) C84 C73 C80 Ti2 58.89(16) C77 C73 C80 Ti2 -124.5(4) Ti1 C73 C80 Ti2 -23.00(17) C69 C78 C81 C83 178.94(19) C71 C78 C81 C83 3.5(3) Ti1 C78 C81 C83 -57.87(17) Ti2 C78 C81 C83 -122.63(18) C69 C78 C81 C75 2.3(3) C71 C78 C81 C75 -173.1(2) Ti1 C78 C81 C75 125.48(18) Ti2 C78 C81 C75 60.71(17) C69 C78 C81 Ti1 -123.19(17) C71 C78 C81 Ti1 61.38(16) Ti2 C78 C81 Ti1 -64.76(4) C69 C78 C81 Ti2 -58.42(15) C71 C78 C81 Ti2 126.14(18) Ti1 C78 C81 Ti2 64.76(4) C70 C75 C81 C83 -173.0(3) Si3 C75 C81 C83 -22.6(5) Ti2 C75 C81 C83 123.1(4) C70 C75 C81 C78 1.7(3) Si3 C75 C81 C78 152.14(18) Ti2 C75 C81 C78 -62.21(17) C70 C75 C81 Ti1 80.5(2) Si3 C75 C81 Ti1 -129.07(17) Ti2 C75 C81 Ti1 16.58(17) C70 C75 C81 Ti2 63.95(16) Si3 C75 C81 Ti2 -145.6(2) C84 C74 C82 C77 6.3(3) Ti1 C74 C82 C77 -62.91(18) C84 C74 C82 Ti1 69.17(16) C73 C77 C82 C74 -6.4(3) Si1 C77 C82 C74 -176.50(18) Ti1 C77 C82 C74 63.81(18) C73 C77 C82 Ti1 -70.25(16) Si1 C77 C82 Ti1 119.69(19) C71 C76 C83 C81 7.4(3) Ti1 C76 C83 C81 69.10(17) C71 C76 C83 Ti1 -61.70(18) C78 C81 C83 C76 -6.5(3) C75 C81 C83 C76 168.3(3) Ti1 C81 C83 C76 -64.75(17) Ti2 C81 C83 C76 -87.2(2) C78 C81 C83 Ti1 58.22(16) C75 C81 C83 Ti1 -127.0(3) Ti2 C81 C83 Ti1 -22.47(15) C82 C74 C84 C73 -3.4(3) Ti1 C74 C84 C73 61.73(16) C82 C74 C84 C72 165.7(3) Ti1 C74 C84 C72 -129.2(3) C82 C74 C84 Ti2 -89.8(2) Ti1 C74 C84 Ti2 -24.67(16) C82 C74 C84 Ti1 -65.10(16) C80 C73 C84 C74 177.3(2) C77 C73 C84 C74 -0.6(3) Ti1 C73 C84 C74 -59.40(16) Ti2 C73 C84 C74 -124.39(17) C80 C73 C84 C72 4.3(3) C77 C73 C84 C72 -173.6(2) Ti1 C73 C84 C72 127.61(18) Ti2 C73 C84 C72 62.61(16) C80 C73 C84 Ti2 -58.35(17) C77 C73 C84 Ti2 123.80(18) Ti1 C73 C84 Ti2 65.00(5) C80 C73 C84 Ti1 -123.35(18) C77 C73 C84 Ti1 58.80(17) Ti2 C73 C84 Ti1 -65.00(5) C79 C72 C84 C74 -169.6(3) Si4 C72 C84 C74 -25.4(4) Ti2 C72 C84 C74 123.6(3) C79 C72 C84 C73 -0.7(3) Si4 C72 C84 C73 143.52(18) Ti2 C72 C84 C73 -67.47(17) C79 C72 C84 Ti2 66.75(15) Si4 C72 C84 Ti2 -149.00(19) C79 C72 C84 Ti1 81.9(2) Si4 C72 C84 Ti1 -133.87(16) Ti2 C72 C84 Ti1 15.14(17) C1S C2S C3S C4S 178.8(12) C2S C3S C4S C5S -174.2(10) C3S C4S C5S C6S 179.8(10) C4S C5S C6S C7S 178.2(11) C9S C8S C13S C12S 0.0 C14S C8S C13S C12S -171.9(16) C8S C13S C12S C11S 0.0 C13S C12S C11S C10S 0.0 C12S C11S C10S C9S 0.0 C11S C10S C9S C8S 0.0 C13S C8S C9S C10S 0.0 C14S C8S C9S C10S 171.4(17) C50 C45 C46 C47 0.9(6) B1 C45 C46 C47 -176.9(4) C45 C46 C47 C48 1.7(7) C46 C47 C48 C49 -2.3(7) C47 C48 C49 C50 0.3(7) C48 C49 C50 C45 2.5(6) C46 C45 C50 C49 -3.0(5) B1 C45 C50 C49 174.8(3) C62 C57 C58 C59 3.3(11) B1 C57 C58 C59 -174.8(8) C57 C58 C59 C60 -4.2(17) C58 C59 C60 C61 2.0(15) C59 C60 C61 C62 0.6(11) C58 C57 C62 C61 -0.6(8) B1 C57 C62 C61 177.4(5) C60 C61 C62 C57 -1.3(9) C68 C63 C64 C65 2.1(7) B1 C63 C64 C65 -177.0(5) C63 C64 C65 C66 0.7(9) C64 C65 C66 C67 -4.4(10) C65 C66 C67 C68 5.1(10) C64 C63 C68 C67 -1.4(7) B1 C63 C68 C67 177.6(5) C66 C67 C68 C63 -2.2(10) C68 C63 B1 C57 -107.2(4) C64 C63 B1 C57 71.8(4) C68 C63 B1 C45 133.2(4) C64 C63 B1 C45 -47.8(5) C68 C63 B1 C51A 4.6(7) C64 C63 B1 C51A -176.4(5) C68 C63 B1 C51B 20.3(6) C64 C63 B1 C51B -160.7(4) C62 C57 B1 C63 148.4(4) C58 C57 B1 C63 -33.8(6) C62 C57 B1 C45 -91.9(4) C58 C57 B1 C45 85.9(6) C62 C57 B1 C51A 33.2(9) C58 C57 B1 C51A -149.0(9) C62 C57 B1 C51B 23.6(7) C58 C57 B1 C51B -158.6(7) C46 C45 B1 C63 -25.0(4) C50 C45 B1 C63 157.3(3) C46 C45 B1 C57 -145.2(3) C50 C45 B1 C57 37.2(4) C46 C45 B1 C51A 98.6(10) C50 C45 B1 C51A -79.1(10) C46 C45 B1 C51B 92.2(7) C50 C45 B1 C51B -85.4(7) C63 B1 C51B C56B -72.9(13) C57 B1 C51B C56B 51.8(15) C45 B1 C51B C56B 170.5(12) C63 B1 C51B C52B 107.7(15) C57 B1 C51B C52B -127.6(13) C45 B1 C51B C52B -8.9(16) C56B C51B C52B C53B 0.5(19) B1 C51B C52B C53B 179.9(10) C51B C52B C53B C54B 1.4(15) C52B C53B C54B C55B -3.5(12) C53B C54B C55B C56B 3.6(13) C54B C55B C56B C51B -1.7(17) C52B C51B C56B C55B 0(2) B1 C51B C56B C55B -179.8(10) C63 B1 C51A C56A -74(2) C57 B1 C51A C56A 42(2) C45 B1 C51A C56A 161.7(16) C63 B1 C51A C52A 99.0(18) C57 B1 C51A C52A -144.6(17) C45 B1 C51A C52A -25(2) C56A C51A C52A C53A 1(3) B1 C51A C52A C53A -172.4(13) C51A C52A C53A C54A -2(2) C52A C53A C54A C55A 2.7(19) C53A C54A C55A C56A -3(2) C54A C55A C56A C51A 2(2) C52A C51A C56A C55A -1(3) B1 C51A C56A C55A 171.9(15)