#------------------------------------------------------------------------------ #$Date: 2018-02-14 09:27:54 +0200 (Wed, 14 Feb 2018) $ #$Revision: 206428 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/01/7230149.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_7230149 loop_ _publ_author_name 'Luo, Derong' 'Zeng, Yi' 'Chen, Xiong' 'Xia, Ping' 'Xie, Guangyong' 'You, Qingliang' 'Zhang, Li' 'Li, Tingcheng' 'Li, Xiangdan' 'Zhang, Aiqing' _publ_section_title ; Synthesis, characterization and olefin polymerization behaviors of phenylene-bridged bis-\b-carbonylenamine binuclear titanium complexes ; _journal_issue 13 _journal_name_full 'RSC Advances' _journal_page_first 6954 _journal_paper_doi 10.1039/C8RA00071A _journal_volume 8 _journal_year 2018 _chemical_formula_sum 'C38 H46 Cl6 N2 O2 S2 Ti2' _chemical_formula_weight 935.39 _chemical_name_systematic ; ? ; _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 geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2017-11-22 deposited with the CCDC. 2018-02-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 108.118(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.572(3) _cell_length_b 14.833(3) _cell_length_c 18.032(3) _cell_measurement_reflns_used 4548 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 47.558 _cell_measurement_theta_min 4.598 _cell_volume 4721.1(15) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 133(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_unetI/netI 0.0788 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 31859 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.500 _diffrn_reflns_theta_min 1.154 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.316 _exptl_crystal_description prismatic _exptl_crystal_F_000 1928 _exptl_crystal_size_max 0.211 _exptl_crystal_size_mid 0.165 _exptl_crystal_size_min 0.112 _platon_squeeze_details ; ; _refine_diff_density_max 1.046 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 477 _refine_ls_number_reflns 8776 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0705 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1198P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1858 _refine_ls_wR_factor_ref 0.2099 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5197 _reflns_number_total 8776 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8ra00071a1.cif _cod_data_source_block dm15328 _cod_original_cell_volume 4721.4(14) _cod_database_code 7230149 _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. ; _shelxl_version_number 2013-4 _shelx_res_file ; TITL dm15328 in P2(1)/c CELL 0.71073 18.5724 14.8334 18.0323 90.000 108.118 90.000 ZERR 4.00 0.0033 0.0026 0.0032 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S Cl Ti UNIT 152 184 8 8 8 24 8 omit -1 1 1 OMIT -3.00 51.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 HTAB C33 Cl4 HTAB C31 Cl6_$2 EQIV $2 -x+1, y-1/2, -z+3/2 HTAB C21 Cl1_$1 HTAB C5 Cl1_$1 EQIV $1 -x, -y+1, -z+1 conf htab mpla c1 > c6 mpla c14 > c19 mpla c27 > c32 TEMP -140 WGHT 0.119800 FVAR 0.86119 MOLE 1 TI1 7 0.016171 0.257218 0.374615 11.00000 0.03571 0.02874 = 0.04074 -0.00169 0.00896 -0.00030 TI2 7 0.426668 0.643050 0.727869 11.00000 0.03664 0.04106 = 0.04516 -0.00190 0.00725 -0.00020 CL1 6 -0.078207 0.289668 0.428152 11.00000 0.04033 0.03607 = 0.05400 0.00001 0.01885 -0.00319 CL2 6 0.100722 0.250585 0.305233 11.00000 0.04684 0.05190 = 0.05360 -0.01194 0.01831 0.00740 CL3 6 -0.033420 0.121120 0.330153 11.00000 0.04801 0.03350 = 0.05370 -0.00754 0.00431 -0.00155 CL4 6 0.321141 0.605198 0.761340 11.00000 0.05192 0.06245 = 0.05438 0.00539 0.01831 -0.00162 CL5 6 0.530539 0.647732 0.685167 11.00000 0.03612 0.05198 = 0.06771 -0.00333 0.01477 0.00156 CL6 6 0.503116 0.649026 0.854051 11.00000 0.04964 0.07449 = 0.05397 -0.00740 0.00486 -0.00378 N1 3 0.051945 0.396331 0.399620 11.00000 0.03168 0.03057 = 0.03392 -0.00182 0.00948 -0.00106 N2 3 0.359628 0.613386 0.609590 11.00000 0.03239 0.03233 = 0.04138 -0.00209 0.01040 -0.00139 O1 4 0.090015 0.233486 0.466389 11.00000 0.03683 0.03033 = 0.04431 0.00025 0.00751 -0.00060 O2 4 0.391539 0.758456 0.704381 11.00000 0.03339 0.03995 = 0.04996 -0.00805 0.00931 0.00006 S1 5 -0.073190 0.342903 0.258810 11.00000 0.04083 0.03635 = 0.03997 -0.00172 0.00729 -0.00189 S2 5 0.445300 0.471429 0.717819 11.00000 0.05113 0.04167 = 0.05973 0.00502 -0.00294 0.00642 C1 1 -0.065992 0.448361 0.307709 11.00000 0.04136 0.03027 = 0.03770 -0.00078 0.01249 0.00042 C2 1 -0.124759 0.509079 0.283370 11.00000 0.03955 0.03926 = 0.04311 0.00204 0.00814 0.00058 AFIX 43 H2 2 -0.167084 0.495846 0.239146 11.00000 -1.20000 AFIX 0 C3 1 -0.122291 0.587861 0.322505 11.00000 0.03864 0.04431 = 0.05672 0.02062 0.01877 0.01295 AFIX 43 H3 2 -0.161390 0.631293 0.304132 11.00000 -1.20000 AFIX 0 C4 1 -0.062111 0.604482 0.389667 11.00000 0.04251 0.03291 = 0.04511 0.00205 0.01935 0.00649 AFIX 43 H4 2 -0.060999 0.659083 0.417537 11.00000 -1.20000 AFIX 0 C5 1 -0.003979 0.543056 0.416540 11.00000 0.04077 0.03514 = 0.03811 0.00184 0.01782 -0.00223 AFIX 43 H5 2 0.035758 0.554255 0.463583 11.00000 -1.20000 AFIX 0 C6 1 -0.004012 0.463784 0.373774 11.00000 0.03836 0.02847 = 0.03740 0.00411 0.01675 -0.00253 C7 1 0.123493 0.415778 0.435067 11.00000 0.03807 0.03702 = 0.03111 -0.00320 0.01486 -0.00426 C8 1 0.177626 0.347827 0.474987 11.00000 0.02778 0.03027 = 0.05133 -0.00378 0.00928 0.00051 AFIX 43 H8 2 0.229678 0.363875 0.489403 11.00000 -1.20000 AFIX 0 C9 1 0.161243 0.263765 0.493719 11.00000 0.03372 0.03363 = 0.04510 -0.00578 0.00716 0.00585 C10 1 0.215103 0.197729 0.542968 11.00000 0.04709 0.02861 = 0.05701 0.00313 0.00019 0.00535 C11 1 0.295278 0.231411 0.571396 11.00000 0.04755 0.05077 = 0.18698 0.03585 -0.02945 -0.00320 AFIX 137 H11A 2 0.311276 0.249680 0.526696 11.00000 -1.50000 H11B 2 0.328545 0.183288 0.600107 11.00000 -1.50000 H11C 2 0.298335 0.283248 0.605937 11.00000 -1.50000 AFIX 0 C12 1 0.191629 0.175420 0.614234 11.00000 0.09089 0.08254 = 0.06384 0.02438 0.02144 0.03544 AFIX 137 H12A 2 0.194671 0.229868 0.645846 11.00000 -1.50000 H12B 2 0.225560 0.129236 0.645277 11.00000 -1.50000 H12C 2 0.139484 0.152739 0.597635 11.00000 -1.50000 AFIX 0 C13 1 0.211345 0.111022 0.495214 11.00000 0.07789 0.03356 = 0.08888 0.00100 0.01722 0.01175 AFIX 137 H13A 2 0.159338 0.087898 0.478548 11.00000 -1.50000 H13B 2 0.245334 0.065680 0.527444 11.00000 -1.50000 H13C 2 0.226969 0.124211 0.449209 11.00000 -1.50000 AFIX 0 C14 1 0.155622 0.507355 0.434827 11.00000 0.03134 0.03133 = 0.03730 0.00117 0.01232 -0.00032 C15 1 0.138605 0.557954 0.367762 11.00000 0.04179 0.04004 = 0.03445 0.00001 0.00738 -0.00363 AFIX 43 H15 2 0.105545 0.534607 0.320304 11.00000 -1.20000 AFIX 0 C16 1 0.169848 0.643330 0.369502 11.00000 0.03895 0.04016 = 0.04397 0.01186 0.01237 0.00634 AFIX 43 H16 2 0.156348 0.678920 0.323420 11.00000 -1.20000 AFIX 0 C17 1 0.219294 0.676661 0.435916 11.00000 0.04140 0.03072 = 0.04785 0.00329 0.01489 -0.00532 AFIX 43 H17 2 0.239444 0.735582 0.436267 11.00000 -1.20000 AFIX 0 C18 1 0.240377 0.625372 0.502828 11.00000 0.03232 0.03308 = 0.03863 -0.00319 0.01374 0.00109 C19 1 0.207984 0.540015 0.502609 11.00000 0.03071 0.02727 = 0.03724 0.00659 0.01391 0.00213 AFIX 43 H19 2 0.221774 0.504474 0.548721 11.00000 -1.20000 AFIX 0 C20 1 0.297709 0.657661 0.575182 11.00000 0.03011 0.02621 = 0.04178 0.00412 0.01097 -0.00158 C21 1 0.276935 0.740663 0.605483 11.00000 0.03502 0.03584 = 0.04848 -0.00044 0.01565 -0.00035 AFIX 43 H21 2 0.226920 0.762559 0.582105 11.00000 -1.20000 AFIX 0 C22 1 0.323821 0.789959 0.665198 11.00000 0.03639 0.03462 = 0.04813 -0.00421 0.01352 -0.00654 C23 1 0.304947 0.878809 0.693762 11.00000 0.03829 0.04724 = 0.06020 -0.00972 0.01475 0.00125 C24 1 0.221441 0.903049 0.655870 11.00000 0.03540 0.04045 = 0.13625 -0.02802 0.01264 0.00354 AFIX 137 H24A 2 0.211503 0.912344 0.599767 11.00000 -1.50000 H24B 2 0.209786 0.958475 0.679426 11.00000 -1.50000 H24C 2 0.189564 0.853850 0.664153 11.00000 -1.50000 AFIX 0 C25 1 0.353594 0.950708 0.672272 11.00000 0.04846 0.03681 = 0.11389 -0.01841 0.02173 -0.00513 AFIX 137 H25A 2 0.407002 0.932924 0.691903 11.00000 -1.50000 H25B 2 0.346649 1.008367 0.695693 11.00000 -1.50000 H25C 2 0.338421 0.957076 0.615397 11.00000 -1.50000 AFIX 0 C26 1 0.325634 0.874153 0.783046 11.00000 0.13860 0.08571 = 0.07550 -0.02849 0.04726 0.02587 AFIX 137 H26A 2 0.300821 0.821842 0.797725 11.00000 -1.50000 H26B 2 0.308600 0.929297 0.802447 11.00000 -1.50000 H26C 2 0.380678 0.868349 0.805924 11.00000 -1.50000 AFIX 0 C27 1 0.383971 0.540472 0.571562 11.00000 0.02962 0.03202 = 0.05374 -0.00126 0.01240 -0.00120 C28 1 0.377761 0.541517 0.492964 11.00000 0.03363 0.04939 = 0.05759 -0.00371 0.02000 0.00152 AFIX 43 H28 2 0.357623 0.593175 0.462406 11.00000 -1.20000 AFIX 0 C29 1 0.400735 0.467626 0.458306 11.00000 0.04909 0.04730 = 0.06310 -0.00763 0.02859 0.00158 AFIX 43 H29 2 0.395635 0.469189 0.404242 11.00000 -1.20000 AFIX 0 C30 1 0.430168 0.393817 0.500701 11.00000 0.04772 0.04707 = 0.08923 -0.02062 0.02946 -0.00262 AFIX 43 H30 2 0.442055 0.341976 0.475844 11.00000 -1.20000 AFIX 0 C31 1 0.442933 0.393953 0.580339 11.00000 0.03522 0.03010 = 0.08854 -0.00055 0.00938 -0.00001 AFIX 43 H31 2 0.467019 0.343824 0.610840 11.00000 -1.20000 AFIX 0 C32 1 0.420811 0.466663 0.615727 11.00000 0.03225 0.03467 = 0.06283 -0.00306 0.00555 0.00031 C33 1 0.374402 0.400375 0.740116 11.00000 0.08203 0.04973 = 0.05805 0.01043 0.00664 -0.00787 AFIX 23 H33A 2 0.324114 0.429819 0.721925 11.00000 -1.20000 H33B 2 0.370937 0.341548 0.713298 11.00000 -1.20000 AFIX 0 C34 1 0.397924 0.386562 0.827247 11.00000 0.13550 0.06004 = 0.07409 0.00588 0.03357 0.02103 AFIX 23 H34A 2 0.404291 0.445687 0.853980 11.00000 -1.20000 H34B 2 0.446995 0.354323 0.844837 11.00000 -1.20000 AFIX 0 C35 1 0.337989 0.332236 0.847756 11.00000 0.16603 0.11784 = 0.13110 0.05654 0.10231 0.05373 AFIX 137 H35A 2 0.288889 0.362527 0.827270 11.00000 -1.50000 H35B 2 0.351298 0.326962 0.904602 11.00000 -1.50000 H35C 2 0.334891 0.271970 0.824702 11.00000 -1.50000 AFIX 0 C36 1 -0.030356 0.364374 0.182526 11.00000 0.06203 0.04470 = 0.03632 -0.00507 0.01870 -0.00038 AFIX 23 H36A 2 0.015533 0.401808 0.204161 11.00000 -1.20000 H36B 2 -0.014368 0.306324 0.165534 11.00000 -1.20000 AFIX 0 C37 1 -0.082522 0.411002 0.113563 11.00000 0.05857 0.05709 = 0.05161 -0.00273 0.01490 -0.00606 AFIX 23 H37A 2 -0.096323 0.470792 0.129455 11.00000 -1.20000 H37B 2 -0.129558 0.375284 0.092934 11.00000 -1.20000 AFIX 0 C38 1 -0.045024 0.422834 0.049868 11.00000 0.09333 0.05704 = 0.04691 -0.01361 0.02214 -0.00228 AFIX 137 H38A 2 0.002153 0.456960 0.070712 11.00000 -1.50000 H38B 2 -0.079364 0.455642 0.005774 11.00000 -1.50000 H38C 2 -0.033801 0.363494 0.032247 11.00000 -1.50000 AFIX 0 HKLF 4 REM dm15328 in P2(1)/c REM R1 = 0.0705 for 5197 Fo > 4sig(Fo) and 0.1093 for all 8776 data REM 477 parameters refined using 0 restraints END WGHT 0.1192 0.0000 REM Instructions for potential hydrogen bonds HTAB C5 Cl1_$1 HTAB C21 Cl1_$1 HTAB C31 Cl6_$2 HTAB C33 Cl4 REM Highest difference peak 1.046, deepest hole -0.532, 1-sigma level 0.100 Q1 1 0.1435 0.2785 0.2806 11.00000 0.05 1.05 Q2 1 0.4107 0.4789 0.7473 11.00000 0.05 0.71 Q3 1 0.4985 0.6434 0.7215 11.00000 0.05 0.66 Q4 1 0.5799 0.2904 0.9808 11.00000 0.05 0.63 Q5 1 -0.0749 0.1605 0.2625 11.00000 0.05 0.58 Q6 1 0.2942 0.9174 0.4475 11.00000 0.05 0.56 Q7 1 -0.0295 0.3844 0.3303 11.00000 0.05 0.56 Q8 1 -0.0207 0.3024 0.3084 11.00000 0.05 0.55 Q9 1 0.3764 0.6364 0.8059 11.00000 0.05 0.55 Q10 1 0.3764 0.6460 0.7461 11.00000 0.05 0.54 Q11 1 0.0874 0.2999 0.2608 11.00000 0.05 0.51 Q12 1 0.1031 0.2512 0.4372 11.00000 0.05 0.50 Q13 1 0.3763 0.3239 0.7831 11.00000 0.05 0.49 Q14 1 0.0032 0.1342 0.3017 11.00000 0.05 0.48 Q15 1 0.0508 0.2978 0.3312 11.00000 0.05 0.46 Q16 1 0.2992 0.2382 0.5478 11.00000 0.05 0.46 Q17 1 0.3913 0.6207 0.6440 11.00000 0.05 0.46 Q18 1 0.2828 0.6376 0.7850 11.00000 0.05 0.45 Q19 1 -0.0993 0.3766 0.2878 11.00000 0.05 0.44 Q20 1 0.0090 0.1587 0.3679 11.00000 0.05 0.43 ; _shelx_res_checksum 42444 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 Ti1 Ti 0.01617(5) 0.25722(6) 0.37461(5) 0.0357(3) Uani 1 1 d . . Ti2 Ti 0.42667(6) 0.64305(7) 0.72787(6) 0.0422(3) Uani 1 1 d . . Cl1 Cl -0.07821(8) 0.28967(8) 0.42815(8) 0.0425(3) Uani 1 1 d . . Cl2 Cl 0.10072(8) 0.25059(10) 0.30523(8) 0.0502(4) Uani 1 1 d . . Cl3 Cl -0.03342(8) 0.12112(9) 0.33015(8) 0.0477(4) Uani 1 1 d . . Cl4 Cl 0.32114(9) 0.60520(11) 0.76134(9) 0.0558(4) Uani 1 1 d . . Cl5 Cl 0.53054(8) 0.64773(10) 0.68517(9) 0.0523(4) Uani 1 1 d . . Cl6 Cl 0.50312(9) 0.64903(12) 0.85405(9) 0.0619(4) Uani 1 1 d . . N1 N 0.0519(2) 0.3963(3) 0.3996(2) 0.0322(9) Uani 1 1 d . . N2 N 0.3596(2) 0.6134(3) 0.6096(2) 0.0356(10) Uani 1 1 d . . O1 O 0.0900(2) 0.2335(2) 0.4664(2) 0.0383(8) Uani 1 1 d . . O2 O 0.3915(2) 0.7585(2) 0.7044(2) 0.0419(9) Uani 1 1 d . . S1 S -0.07319(8) 0.34290(9) 0.25881(8) 0.0403(3) Uani 1 1 d . . S2 S 0.44530(9) 0.47143(10) 0.71782(9) 0.0555(4) Uani 1 1 d . . C1 C -0.0660(3) 0.4484(3) 0.3077(3) 0.0364(12) Uani 1 1 d . . C2 C -0.1248(3) 0.5091(4) 0.2834(3) 0.0417(13) Uani 1 1 d . . H2 H -0.1671 0.4958 0.2391 0.050 Uiso 1 1 calc R U C3 C -0.1223(3) 0.5879(4) 0.3225(3) 0.0456(14) Uani 1 1 d . . H3 H -0.1614 0.6313 0.3041 0.055 Uiso 1 1 calc R U C4 C -0.0621(3) 0.6045(3) 0.3897(3) 0.0389(12) Uani 1 1 d . . H4 H -0.0610 0.6591 0.4175 0.047 Uiso 1 1 calc R U C5 C -0.0040(3) 0.5431(3) 0.4165(3) 0.0367(12) Uani 1 1 d . . H5 H 0.0358 0.5543 0.4636 0.044 Uiso 1 1 calc R U C6 C -0.0040(3) 0.4638(3) 0.3738(3) 0.0336(11) Uani 1 1 d . . C7 C 0.1235(3) 0.4158(3) 0.4351(3) 0.0345(11) Uani 1 1 d . . C8 C 0.1776(3) 0.3478(3) 0.4750(3) 0.0372(12) Uani 1 1 d . . H8 H 0.2297 0.3639 0.4894 0.045 Uiso 1 1 calc R U C9 C 0.1612(3) 0.2638(3) 0.4937(3) 0.0387(12) Uani 1 1 d . . C10 C 0.2151(3) 0.1977(3) 0.5430(3) 0.0479(15) Uani 1 1 d . . C11 C 0.2953(4) 0.2314(5) 0.5714(6) 0.110(4) Uani 1 1 d . . H11A H 0.3113 0.2497 0.5267 0.165 Uiso 1 1 calc R U H11B H 0.3285 0.1833 0.6001 0.165 Uiso 1 1 calc R U H11C H 0.2983 0.2832 0.6059 0.165 Uiso 1 1 calc R U C12 C 0.1916(5) 0.1754(5) 0.6142(4) 0.080(2) Uani 1 1 d . . H12A H 0.1947 0.2299 0.6458 0.120 Uiso 1 1 calc R U H12B H 0.2256 0.1292 0.6453 0.120 Uiso 1 1 calc R U H12C H 0.1395 0.1527 0.5976 0.120 Uiso 1 1 calc R U C13 C 0.2113(4) 0.1110(4) 0.4952(4) 0.069(2) Uani 1 1 d . . H13A H 0.1593 0.0879 0.4785 0.103 Uiso 1 1 calc R U H13B H 0.2453 0.0657 0.5274 0.103 Uiso 1 1 calc R U H13C H 0.2270 0.1242 0.4492 0.103 Uiso 1 1 calc R U C14 C 0.1556(3) 0.5074(3) 0.4348(3) 0.0329(11) Uani 1 1 d . . C15 C 0.1386(3) 0.5580(3) 0.3678(3) 0.0398(12) Uani 1 1 d . . H15 H 0.1055 0.5346 0.3203 0.048 Uiso 1 1 calc R U C16 C 0.1698(3) 0.6433(4) 0.3695(3) 0.0411(13) Uani 1 1 d . . H16 H 0.1563 0.6789 0.3234 0.049 Uiso 1 1 calc R U C17 C 0.2193(3) 0.6767(3) 0.4359(3) 0.0398(12) Uani 1 1 d . . H17 H 0.2394 0.7356 0.4363 0.048 Uiso 1 1 calc R U C18 C 0.2404(3) 0.6254(3) 0.5028(3) 0.0341(11) Uani 1 1 d . . C19 C 0.2080(3) 0.5400(3) 0.5026(3) 0.0310(11) Uani 1 1 d . . H19 H 0.2218 0.5045 0.5487 0.037 Uiso 1 1 calc R U C20 C 0.2977(3) 0.6577(3) 0.5752(3) 0.0328(11) Uani 1 1 d . . C21 C 0.2769(3) 0.7407(3) 0.6055(3) 0.0392(12) Uani 1 1 d . . H21 H 0.2269 0.7626 0.5821 0.047 Uiso 1 1 calc R U C22 C 0.3238(3) 0.7900(3) 0.6652(3) 0.0396(12) Uani 1 1 d . . C23 C 0.3049(3) 0.8788(4) 0.6938(4) 0.0487(14) Uani 1 1 d . . C24 C 0.2214(3) 0.9030(4) 0.6559(5) 0.074(2) Uani 1 1 d . . H24A H 0.2115 0.9123 0.5998 0.111 Uiso 1 1 calc R U H24B H 0.2098 0.9585 0.6794 0.111 Uiso 1 1 calc R U H24C H 0.1896 0.8539 0.6642 0.111 Uiso 1 1 calc R U C25 C 0.3536(4) 0.9507(4) 0.6723(5) 0.0672(19) Uani 1 1 d . . H25A H 0.4070 0.9329 0.6919 0.101 Uiso 1 1 calc R U H25B H 0.3466 1.0084 0.6957 0.101 Uiso 1 1 calc R U H25C H 0.3384 0.9571 0.6154 0.101 Uiso 1 1 calc R U C26 C 0.3256(6) 0.8742(6) 0.7830(4) 0.097(3) Uani 1 1 d . . H26A H 0.3008 0.8218 0.7977 0.145 Uiso 1 1 calc R U H26B H 0.3086 0.9293 0.8024 0.145 Uiso 1 1 calc R U H26C H 0.3807 0.8683 0.8059 0.145 Uiso 1 1 calc R U C27 C 0.3840(3) 0.5405(3) 0.5716(3) 0.0386(12) Uani 1 1 d . . C28 C 0.3778(3) 0.5415(4) 0.4930(3) 0.0455(13) Uani 1 1 d . . H28 H 0.3576 0.5932 0.4624 0.055 Uiso 1 1 calc R U C29 C 0.4007(3) 0.4676(4) 0.4583(4) 0.0506(15) Uani 1 1 d . . H29 H 0.3956 0.4692 0.4042 0.061 Uiso 1 1 calc R U C30 C 0.4302(4) 0.3938(4) 0.5007(4) 0.0595(17) Uani 1 1 d . . H30 H 0.4421 0.3420 0.4758 0.071 Uiso 1 1 calc R U C31 C 0.4429(3) 0.3940(4) 0.5803(4) 0.0536(16) Uani 1 1 d . . H31 H 0.4670 0.3438 0.6108 0.064 Uiso 1 1 calc R U C32 C 0.4208(3) 0.4667(4) 0.6157(3) 0.0454(14) Uani 1 1 d . . C33 C 0.3744(4) 0.4004(4) 0.7401(4) 0.0667(19) Uani 1 1 d . . H33A H 0.3241 0.4298 0.7219 0.080 Uiso 1 1 calc R U H33B H 0.3709 0.3415 0.7133 0.080 Uiso 1 1 calc R U C34 C 0.3979(6) 0.3866(5) 0.8272(5) 0.090(3) Uani 1 1 d . . H34A H 0.4043 0.4457 0.8540 0.108 Uiso 1 1 calc R U H34B H 0.4470 0.3543 0.8448 0.108 Uiso 1 1 calc R U C35 C 0.3380(7) 0.3322(7) 0.8478(6) 0.125(4) Uani 1 1 d . . H35A H 0.2889 0.3625 0.8273 0.188 Uiso 1 1 calc R U H35B H 0.3513 0.3270 0.9046 0.188 Uiso 1 1 calc R U H35C H 0.3349 0.2720 0.8247 0.188 Uiso 1 1 calc R U C36 C -0.0304(4) 0.3644(4) 0.1825(3) 0.0469(14) Uani 1 1 d . . H36A H 0.0155 0.4018 0.2042 0.056 Uiso 1 1 calc R U H36B H -0.0144 0.3063 0.1655 0.056 Uiso 1 1 calc R U C37 C -0.0825(4) 0.4110(4) 0.1136(3) 0.0563(16) Uani 1 1 d . . H37A H -0.0963 0.4708 0.1295 0.068 Uiso 1 1 calc R U H37B H -0.1296 0.3753 0.0929 0.068 Uiso 1 1 calc R U C38 C -0.0450(4) 0.4228(4) 0.0499(4) 0.0657(19) Uani 1 1 d . . H38A H 0.0022 0.4570 0.0707 0.099 Uiso 1 1 calc R U H38B H -0.0794 0.4556 0.0058 0.099 Uiso 1 1 calc R U H38C H -0.0338 0.3635 0.0322 0.099 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 Ti1 0.0357(5) 0.0287(5) 0.0407(5) -0.0017(4) 0.0090(4) -0.0003(4) Ti2 0.0366(6) 0.0411(6) 0.0452(6) -0.0019(4) 0.0073(4) -0.0002(4) Cl1 0.0403(8) 0.0361(7) 0.0540(8) 0.0000(6) 0.0188(6) -0.0032(6) Cl2 0.0468(9) 0.0519(8) 0.0536(8) -0.0119(6) 0.0183(7) 0.0074(7) Cl3 0.0480(9) 0.0335(7) 0.0537(8) -0.0075(6) 0.0043(6) -0.0015(6) Cl4 0.0519(9) 0.0624(10) 0.0544(9) 0.0054(7) 0.0183(7) -0.0016(7) Cl5 0.0361(8) 0.0520(8) 0.0677(10) -0.0033(7) 0.0148(7) 0.0016(6) Cl6 0.0496(10) 0.0745(11) 0.0540(9) -0.0074(8) 0.0049(7) -0.0038(8) N1 0.032(2) 0.031(2) 0.034(2) -0.0018(17) 0.0095(18) -0.0011(18) N2 0.032(2) 0.032(2) 0.041(2) -0.0021(18) 0.0104(19) -0.0014(18) O1 0.037(2) 0.0303(18) 0.044(2) 0.0002(15) 0.0075(16) -0.0006(15) O2 0.033(2) 0.040(2) 0.050(2) -0.0081(16) 0.0093(17) 0.0001(16) S1 0.0408(8) 0.0363(7) 0.0400(7) -0.0017(5) 0.0073(6) -0.0019(6) S2 0.0511(10) 0.0417(8) 0.0597(10) 0.0050(7) -0.0029(7) 0.0064(7) C1 0.041(3) 0.030(3) 0.038(3) -0.001(2) 0.012(2) 0.000(2) C2 0.040(3) 0.039(3) 0.043(3) 0.002(2) 0.008(3) 0.001(2) C3 0.039(3) 0.044(3) 0.057(4) 0.021(3) 0.019(3) 0.013(3) C4 0.043(3) 0.033(3) 0.045(3) 0.002(2) 0.019(3) 0.006(2) C5 0.041(3) 0.035(3) 0.038(3) 0.002(2) 0.018(2) -0.002(2) C6 0.038(3) 0.028(3) 0.037(3) 0.004(2) 0.017(2) -0.003(2) C7 0.038(3) 0.037(3) 0.031(3) -0.003(2) 0.015(2) -0.004(2) C8 0.028(3) 0.030(3) 0.051(3) -0.004(2) 0.009(2) 0.001(2) C9 0.034(3) 0.034(3) 0.045(3) -0.006(2) 0.007(2) 0.006(2) C10 0.047(4) 0.029(3) 0.057(4) 0.003(2) 0.000(3) 0.005(2) C11 0.048(5) 0.051(4) 0.187(9) 0.036(5) -0.029(5) -0.003(3) C12 0.091(6) 0.083(5) 0.064(5) 0.024(4) 0.021(4) 0.035(5) C13 0.078(5) 0.034(3) 0.089(5) 0.001(3) 0.017(4) 0.012(3) C14 0.031(3) 0.031(3) 0.037(3) 0.001(2) 0.012(2) 0.000(2) C15 0.042(3) 0.040(3) 0.034(3) 0.000(2) 0.007(2) -0.004(2) C16 0.039(3) 0.040(3) 0.044(3) 0.012(2) 0.012(2) 0.006(2) C17 0.041(3) 0.031(3) 0.048(3) 0.003(2) 0.015(3) -0.005(2) C18 0.032(3) 0.033(3) 0.039(3) -0.003(2) 0.014(2) 0.001(2) C19 0.031(3) 0.027(2) 0.037(3) 0.007(2) 0.014(2) 0.002(2) C20 0.030(3) 0.026(2) 0.042(3) 0.004(2) 0.011(2) -0.002(2) C21 0.035(3) 0.036(3) 0.048(3) 0.000(2) 0.016(2) 0.000(2) C22 0.036(3) 0.035(3) 0.048(3) -0.004(2) 0.014(3) -0.007(2) C23 0.038(3) 0.047(3) 0.060(4) -0.010(3) 0.015(3) 0.001(3) C24 0.035(4) 0.040(3) 0.136(7) -0.028(4) 0.013(4) 0.004(3) C25 0.048(4) 0.037(3) 0.114(6) -0.018(3) 0.022(4) -0.005(3) C26 0.139(9) 0.086(6) 0.075(5) -0.028(4) 0.047(5) 0.026(5) C27 0.030(3) 0.032(3) 0.054(3) -0.001(2) 0.012(2) -0.001(2) C28 0.034(3) 0.049(3) 0.058(4) -0.004(3) 0.020(3) 0.002(3) C29 0.049(4) 0.047(3) 0.063(4) -0.008(3) 0.029(3) 0.002(3) C30 0.048(4) 0.047(4) 0.089(5) -0.021(3) 0.029(4) -0.003(3) C31 0.035(3) 0.030(3) 0.089(5) -0.001(3) 0.009(3) 0.000(2) C32 0.032(3) 0.035(3) 0.063(4) -0.003(3) 0.006(3) 0.000(2) C33 0.082(5) 0.050(4) 0.058(4) 0.010(3) 0.007(4) -0.008(3) C34 0.135(8) 0.060(5) 0.074(5) 0.006(4) 0.034(5) 0.021(5) C35 0.166(11) 0.118(8) 0.131(9) 0.057(7) 0.102(8) 0.054(8) C36 0.062(4) 0.045(3) 0.036(3) -0.005(2) 0.019(3) 0.000(3) C37 0.059(4) 0.057(4) 0.052(4) -0.003(3) 0.015(3) -0.006(3) C38 0.093(6) 0.057(4) 0.047(4) -0.014(3) 0.022(4) -0.002(4) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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 O1 Ti1 N1 84.26(15) O1 Ti1 Cl3 104.94(12) N1 Ti1 Cl3 170.77(12) O1 Ti1 Cl2 92.15(13) N1 Ti1 Cl2 86.38(12) Cl3 Ti1 Cl2 92.34(6) O1 Ti1 Cl1 96.64(13) N1 Ti1 Cl1 86.44(12) Cl3 Ti1 Cl1 93.22(6) Cl2 Ti1 Cl1 168.04(7) O1 Ti1 S1 161.35(12) N1 Ti1 S1 77.11(11) Cl3 Ti1 S1 93.71(6) Cl2 Ti1 S1 87.51(6) Cl1 Ti1 S1 81.57(6) O2 Ti2 N2 84.69(16) O2 Ti2 Cl6 105.11(12) N2 Ti2 Cl6 170.20(13) O2 Ti2 Cl5 99.81(13) N2 Ti2 Cl5 87.78(12) Cl6 Ti2 Cl5 90.35(7) O2 Ti2 Cl4 91.01(13) N2 Ti2 Cl4 86.13(12) Cl6 Ti2 Cl4 93.72(7) Cl5 Ti2 Cl4 167.04(7) O2 Ti2 S2 161.71(12) N2 Ti2 S2 77.18(12) Cl6 Ti2 S2 93.03(6) Cl5 Ti2 S2 82.01(6) Cl4 Ti2 S2 85.48(7) C7 N1 C6 122.2(4) C7 N1 Ti1 120.5(3) C6 N1 Ti1 117.3(3) C20 N2 C27 121.2(4) C20 N2 Ti2 121.4(3) C27 N2 Ti2 117.3(3) C9 O1 Ti1 130.3(3) C22 O2 Ti2 131.6(3) C1 S1 C36 103.7(3) C1 S1 Ti1 95.87(17) C36 S1 Ti1 112.2(2) C32 S2 C33 103.8(3) C32 S2 Ti2 96.70(18) C33 S2 Ti2 115.6(3) C2 C1 C6 121.8(5) C2 C1 S1 119.1(4) C6 C1 S1 118.8(4) C3 C2 C1 120.1(5) C3 C2 H2 119.9 C1 C2 H2 119.9 C2 C3 C4 119.5(5) C2 C3 H3 120.2 C4 C3 H3 120.2 C5 C4 C3 121.2(5) C5 C4 H4 119.4 C3 C4 H4 119.4 C4 C5 C6 119.5(5) C4 C5 H5 120.2 C6 C5 H5 120.2 C1 C6 C5 117.7(5) C1 C6 N1 119.5(4) C5 C6 N1 122.4(4) N1 C7 C8 122.0(5) N1 C7 C14 123.1(4) C8 C7 C14 114.9(4) C9 C8 C7 126.3(5) C9 C8 H8 116.9 C7 C8 H8 116.9 O1 C9 C8 119.4(5) O1 C9 C10 113.9(5) C8 C9 C10 126.7(5) C9 C10 C11 113.4(5) C9 C10 C12 109.5(5) C11 C10 C12 107.4(7) C9 C10 C13 108.2(5) C11 C10 C13 109.7(6) C12 C10 C13 108.5(5) C10 C11 H11A 109.5 C10 C11 H11B 109.5 H11A C11 H11B 109.5 C10 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C10 C12 H12A 109.5 C10 C12 H12B 109.5 H12A C12 H12B 109.5 C10 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C10 C13 H13A 109.5 C10 C13 H13B 109.5 H13A C13 H13B 109.5 C10 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C15 C14 C19 119.3(4) C15 C14 C7 121.3(4) C19 C14 C7 119.2(4) C14 C15 C16 119.9(5) C14 C15 H15 120.1 C16 C15 H15 120.1 C17 C16 C15 121.1(5) C17 C16 H16 119.5 C15 C16 H16 119.5 C16 C17 C18 120.2(5) C16 C17 H17 119.9 C18 C17 H17 119.9 C17 C18 C19 119.5(5) C17 C18 C20 121.5(4) C19 C18 C20 119.0(4) C14 C19 C18 120.0(4) C14 C19 H19 120.0 C18 C19 H19 120.0 N2 C20 C21 123.3(5) N2 C20 C18 122.8(4) C21 C20 C18 113.8(4) C22 C21 C20 125.0(5) C22 C21 H21 117.5 C20 C21 H21 117.5 O2 C22 C21 119.9(5) O2 C22 C23 114.4(5) C21 C22 C23 125.6(5) C22 C23 C25 107.9(5) C22 C23 C24 111.5(5) C25 C23 C24 108.7(5) C22 C23 C26 108.2(5) C25 C23 C26 108.9(6) C24 C23 C26 111.5(6) C23 C24 H24A 109.5 C23 C24 H24B 109.5 H24A C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C23 C25 H25A 109.5 C23 C25 H25B 109.5 H25A C25 H25B 109.5 C23 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C23 C26 H26A 109.5 C23 C26 H26B 109.5 H26A C26 H26B 109.5 C23 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C28 C27 C32 117.4(5) C28 C27 N2 123.0(5) C32 C27 N2 119.4(5) C27 C28 C29 120.7(5) C27 C28 H28 119.7 C29 C28 H28 119.7 C30 C29 C28 120.7(6) C30 C29 H29 119.6 C28 C29 H29 119.6 C29 C30 C31 119.7(6) C29 C30 H30 120.1 C31 C30 H30 120.1 C32 C31 C30 120.2(6) C32 C31 H31 119.9 C30 C31 H31 119.9 C31 C32 C27 120.7(6) C31 C32 S2 120.0(5) C27 C32 S2 119.1(4) C34 C33 S2 108.2(6) C34 C33 H33A 110.1 S2 C33 H33A 110.1 C34 C33 H33B 110.1 S2 C33 H33B 110.1 H33A C33 H33B 108.4 C33 C34 C35 109.3(8) C33 C34 H34A 109.8 C35 C34 H34A 109.8 C33 C34 H34B 109.8 C35 C34 H34B 109.8 H34A C34 H34B 108.3 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 S1 112.9(4) C37 C36 H36A 109.0 S1 C36 H36A 109.0 C37 C36 H36B 109.0 S1 C36 H36B 109.0 H36A C36 H36B 107.8 C36 C37 C38 110.6(6) C36 C37 H37A 109.5 C38 C37 H37A 109.5 C36 C37 H37B 109.5 C38 C37 H37B 109.5 H37A C37 H37B 108.1 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 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ti1 O1 1.825(3) Ti1 N1 2.172(4) Ti1 Cl3 2.2599(16) Ti1 Cl2 2.2941(17) Ti1 Cl1 2.2997(16) Ti1 S1 2.5642(16) Ti2 O2 1.834(4) Ti2 N2 2.154(4) Ti2 Cl6 2.2785(19) Ti2 Cl5 2.2898(18) Ti2 Cl4 2.2927(19) Ti2 S2 2.5831(18) N1 C7 1.315(6) N1 C6 1.413(6) N2 C20 1.302(6) N2 C27 1.427(7) O1 C9 1.338(6) O2 C22 1.322(6) S1 C1 1.780(5) S1 C36 1.819(6) S2 C32 1.755(6) S2 C33 1.826(7) C1 C2 1.377(7) C1 C6 1.394(7) C2 C3 1.359(8) C2 H2 0.9500 C3 C4 1.391(8) C3 H3 0.9500 C4 C5 1.380(7) C4 H4 0.9500 C5 C6 1.406(7) C5 H5 0.9500 C7 C8 1.447(7) C7 C14 1.484(7) C8 C9 1.351(7) C8 H8 0.9500 C9 C10 1.482(7) C10 C11 1.502(9) C10 C12 1.516(9) C10 C13 1.537(8) C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 C15 1.374(7) C14 C19 1.391(7) C15 C16 1.389(7) C15 H15 0.9500 C16 C17 1.356(8) C16 H16 0.9500 C17 C18 1.376(7) C17 H17 0.9500 C18 C19 1.401(7) C18 C20 1.484(7) C19 H19 0.9500 C20 C21 1.447(7) C21 C22 1.367(7) C21 H21 0.9500 C22 C23 1.496(8) C23 C25 1.524(9) C23 C24 1.530(8) C23 C26 1.536(9) C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 C28 1.386(8) C27 C32 1.401(7) C28 C29 1.393(8) C28 H28 0.9500 C29 C30 1.350(9) C29 H29 0.9500 C30 C31 1.381(9) C30 H30 0.9500 C31 C32 1.379(8) C31 H31 0.9500 C33 C34 1.508(10) C33 H33A 0.9900 C33 H33B 0.9900 C34 C35 1.510(13) C34 H34A 0.9900 C34 H34B 0.9900 C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C36 C37 1.488(8) C36 H36A 0.9900 C36 H36B 0.9900 C37 C38 1.527(9) C37 H37A 0.9900 C37 H37B 0.9900 C38 H38A 0.9800 C38 H38B 0.9800 C38 H38C 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C33 H33A Cl4 0.99 2.70 3.254(7) 115.6 . C31 H31 Cl6 0.95 2.97 3.856(6) 155.1 2_646 C21 H21 Cl1 0.95 2.82 3.578(5) 137.6 3_566 C5 H5 Cl1 0.95 2.97 3.697(5) 134.1 3_566 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 N1 Ti1 O1 C9 -45.2(4) Cl3 Ti1 O1 C9 133.9(4) Cl2 Ti1 O1 C9 41.0(4) Cl1 Ti1 O1 C9 -130.9(4) S1 Ti1 O1 C9 -47.6(7) N2 Ti2 O2 C22 41.6(4) Cl6 Ti2 O2 C22 -138.5(4) Cl5 Ti2 O2 C22 128.4(4) Cl4 Ti2 O2 C22 -44.4(4) S2 Ti2 O2 C22 34.2(7) C36 S1 C1 C2 91.2(5) Ti1 S1 C1 C2 -154.1(4) C36 S1 C1 C6 -94.3(4) Ti1 S1 C1 C6 20.3(4) C6 C1 C2 C3 2.1(8) S1 C1 C2 C3 176.4(4) C1 C2 C3 C4 -3.5(8) C2 C3 C4 C5 1.3(8) C3 C4 C5 C6 2.4(8) C2 C1 C6 C5 1.5(7) S1 C1 C6 C5 -172.8(4) C2 C1 C6 N1 175.2(5) S1 C1 C6 N1 0.9(6) C4 C5 C6 C1 -3.7(7) C4 C5 C6 N1 -177.2(4) C7 N1 C6 C1 148.8(5) Ti1 N1 C6 C1 -28.9(6) C7 N1 C6 C5 -37.8(7) Ti1 N1 C6 C5 144.5(4) C6 N1 C7 C8 167.5(4) Ti1 N1 C7 C8 -14.9(6) C6 N1 C7 C14 -14.9(7) Ti1 N1 C7 C14 162.7(4) N1 C7 C8 C9 -13.1(8) C14 C7 C8 C9 169.2(5) Ti1 O1 C9 C8 32.6(7) Ti1 O1 C9 C10 -147.2(4) C7 C8 C9 O1 8.4(8) C7 C8 C9 C10 -171.8(5) O1 C9 C10 C11 178.3(6) C8 C9 C10 C11 -1.5(10) O1 C9 C10 C12 -61.7(6) C8 C9 C10 C12 118.5(7) O1 C9 C10 C13 56.3(7) C8 C9 C10 C13 -123.4(6) N1 C7 C14 C15 -44.2(7) C8 C7 C14 C15 133.5(5) N1 C7 C14 C19 140.2(5) C8 C7 C14 C19 -42.1(6) C19 C14 C15 C16 -4.2(8) C7 C14 C15 C16 -179.8(5) C14 C15 C16 C17 2.4(8) C15 C16 C17 C18 1.1(9) C16 C17 C18 C19 -2.6(8) C16 C17 C18 C20 176.4(5) C15 C14 C19 C18 2.7(7) C7 C14 C19 C18 178.3(4) C17 C18 C19 C14 0.7(7) C20 C18 C19 C14 -178.3(5) C27 N2 C20 C21 -169.6(5) Ti2 N2 C20 C21 13.3(7) C27 N2 C20 C18 13.1(7) Ti2 N2 C20 C18 -164.1(4) C17 C18 C20 N2 -122.2(6) C19 C18 C20 N2 56.8(7) C17 C18 C20 C21 60.2(7) C19 C18 C20 C21 -120.8(5) N2 C20 C21 C22 11.2(8) C18 C20 C21 C22 -171.2(5) Ti2 O2 C22 C21 -31.0(7) Ti2 O2 C22 C23 147.3(4) C20 C21 C22 O2 -6.1(8) C20 C21 C22 C23 175.8(5) O2 C22 C23 C25 70.8(6) C21 C22 C23 C25 -111.0(6) O2 C22 C23 C24 -169.9(5) C21 C22 C23 C24 8.3(8) O2 C22 C23 C26 -46.9(7) C21 C22 C23 C26 131.3(7) C20 N2 C27 C28 39.2(7) Ti2 N2 C27 C28 -143.5(4) C20 N2 C27 C32 -145.5(5) Ti2 N2 C27 C32 31.8(6) C32 C27 C28 C29 6.2(8) N2 C27 C28 C29 -178.4(5) C27 C28 C29 C30 -0.6(9) C28 C29 C30 C31 -4.9(9) C29 C30 C31 C32 4.6(9) C30 C31 C32 C27 1.2(9) C30 C31 C32 S2 -173.8(5) C28 C27 C32 C31 -6.4(8) N2 C27 C32 C31 178.0(5) C28 C27 C32 S2 168.6(4) N2 C27 C32 S2 -7.0(7) C33 S2 C32 C31 -81.1(5) Ti2 S2 C32 C31 160.4(4) C33 S2 C32 C27 103.8(5) Ti2 S2 C32 C27 -14.7(5) C32 S2 C33 C34 170.3(5) Ti2 S2 C33 C34 -85.1(5) S2 C33 C34 C35 176.9(6) C1 S1 C36 C37 -79.8(5) Ti1 S1 C36 C37 177.8(4) S1 C36 C37 C38 -177.1(4) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.500 262 91 ' ' 2 0.235 0.093 0.786 50 2 ' ' 3 0.500 0.500 0.000 263 91 ' ' 4 0.235 0.407 0.286 50 2 ' ' 5 0.765 0.593 0.714 50 2 ' ' 6 0.765 0.907 0.214 50 2 ' '