Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Tsukasa Matsuo' 'Hiroyuki Kawaguchi' _publ_contact_author_name 'Prof Hiroyuki Kawaguchi' _publ_contact_author_address ; Coordination Chemistry Laboratories Institute for Molecular Science Myodaiji Okazaki Aichi 444-8585 JAPAN ; # SUBMISSION DETAILS _publ_contact_author_email hkawa@ims.ac.jp _publ_contact_author_fax +81-564-55-5245 _publ_contact_author_phone +81-564-55-7290 _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Structures of Titanium Complexes with the Linked Phenoxide Ligand ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation and Rigaku Corporation. (2001). CrystalStructure. Single Crystal Structure Analysis Software. Version 2.00. MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W., CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; data_[Ti(Me-L)Cl]2 _database_code_CSD 172983 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C66.50 H74 Cl2 O6 Ti2 ' _chemical_formula_moiety 'C66.50 H74 Cl2 O6 Ti2 ' _chemical_formula_weight 1136.02 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.8839(5) _cell_length_b 16.0695(6) _cell_length_c 17.2465(9) _cell_angle_alpha 88.638(3) _cell_angle_beta 71.058(1) _cell_angle_gamma 76.614(1) _cell_volume 3025.8(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8663 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'darkred' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type 'REQABA Empirical Absorption Correction' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 0.923 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.32 _diffrn_reflns_number 28599 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9707 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9695 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 13466 _reflns_number_gt 7286 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1780 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 13466 _refine_ls_number_parameters 730 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.001Fo^2^ + 1.000\s^2^(Fo)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0080 _refine_diff_density_max 1.21 _refine_diff_density_min -0.82 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.174 0.200 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ti' 'Ti' 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti(1) Ti 0.55854(6) 0.39924(4) 0.01259(4) 0.0316(2) Uani 1.00 d . . . Ti(2) Ti -0.12777(6) 0.98923(4) 0.48733(4) 0.0298(2) Uani 1.00 d . . . Cl(1) Cl 0.6037(1) 0.28760(6) -0.07996(6) 0.0450(3) Uani 1.00 d . . . Cl(2) Cl -0.30076(9) 0.97955(8) 0.59042(7) 0.0494(3) Uani 1.00 d . . . O(1) O 0.4585(3) 0.3618(2) 0.0975(2) 0.0531(9) Uani 1.00 d . . . O(2) O 0.4976(2) 0.5214(2) 0.0645(2) 0.0304(7) Uani 1.00 d . . . O(3) O 0.7038(3) 0.3936(2) 0.0197(2) 0.0581(10) Uani 1.00 d . . . O(4) O -0.0920(2) 0.8906(2) 0.4318(2) 0.0397(8) Uani 1.00 d . . . O(5) O 0.0456(2) 1.0061(2) 0.4306(2) 0.0313(7) Uani 1.00 d . . . O(6) O -0.1891(3) 1.0774(2) 0.4399(2) 0.0421(8) Uani 1.00 d . . . C(1) C 0.3967(4) 0.3402(3) 0.1741(3) 0.043(1) Uani 1.00 d . . . C(2) C 0.4184(5) 0.2536(3) 0.1921(3) 0.050(1) Uani 1.00 d . . . C(3) C 0.3536(5) 0.2351(3) 0.2709(3) 0.052(1) Uani 1.00 d . . . C(4) C 0.2767(4) 0.2961(3) 0.3296(3) 0.046(1) Uani 1.00 d . . . C(5) C 0.2584(4) 0.3805(3) 0.3078(3) 0.043(1) Uani 1.00 d . . . C(6) C 0.3171(4) 0.4048(2) 0.2298(3) 0.037(1) Uani 1.00 d . . . C(7) C 0.2989(4) 0.4973(2) 0.2075(3) 0.034(1) Uani 1.00 d . . . C(8) C 0.5026(4) 0.5383(2) 0.1429(2) 0.0331(10) Uani 1.00 d . . . C(9) C 0.4035(3) 0.5340(2) 0.2118(2) 0.0309(10) Uani 1.00 d . . . C(10) C 0.4042(4) 0.5615(2) 0.2877(2) 0.037(1) Uani 1.00 d . . . C(11) C 0.4998(4) 0.5914(3) 0.2963(2) 0.040(1) Uani 1.00 d . . . C(12) C 0.6008(4) 0.5883(2) 0.2261(2) 0.038(1) Uani 1.00 d . . . C(13) C 0.6055(4) 0.5610(2) 0.1491(2) 0.033(1) Uani 1.00 d . . . C(14) C 0.7202(4) 0.5538(2) 0.0765(3) 0.038(1) Uani 1.00 d . . . C(15) C 0.8001(4) 0.3935(3) 0.0471(3) 0.045(1) Uani 1.00 d . . . C(16) C 0.8135(4) 0.4701(3) 0.0738(3) 0.037(1) Uani 1.00 d . . . C(17) C 0.9117(4) 0.4671(3) 0.1008(3) 0.046(1) Uani 1.00 d . . . C(18) C 0.9941(4) 0.3914(3) 0.1036(3) 0.056(1) Uani 1.00 d . . . C(19) C 0.9764(4) 0.3167(3) 0.0755(3) 0.060(2) Uani 1.00 d . . . C(20) C 0.8811(4) 0.3153(3) 0.0467(3) 0.059(1) Uani 1.00 d . . . C(21) C 0.5064(7) 0.1867(3) 0.1295(4) 0.090(2) Uani 1.00 d . . . C(22) C 0.2148(6) 0.2724(4) 0.4152(3) 0.073(2) Uani 1.00 d . . . C(23) C 0.4942(5) 0.6283(3) 0.3787(3) 0.059(1) Uani 1.00 d . . . C(24) C 0.6127(7) 0.5933(5) 0.3962(4) 0.103(2) Uani 1.00 d . . . C(25) C 0.3860(8) 0.6145(7) 0.4497(4) 0.188(4) Uani 1.00 d . . . C(26) C 0.4797(7) 0.7269(4) 0.3725(4) 0.090(2) Uani 1.00 d . . . C(27) C 0.8630(5) 0.2337(3) 0.0177(5) 0.101(2) Uani 1.00 d . . . C(28) C 1.0985(5) 0.3886(4) 0.1353(4) 0.087(2) Uani 1.00 d . . . C(29) C -0.0607(4) 0.8303(2) 0.3691(2) 0.034(1) Uani 1.00 d . . . C(30) C -0.1523(4) 0.7996(3) 0.3546(3) 0.036(1) Uani 1.00 d . . . C(31) C -0.1166(4) 0.7378(3) 0.2904(3) 0.047(1) Uani 1.00 d . . . C(32) C 0.0040(4) 0.7081(3) 0.2428(3) 0.045(1) Uani 1.00 d . . . C(33) C 0.0934(4) 0.7410(2) 0.2587(3) 0.038(1) Uani 1.00 d . . . C(34) C 0.0626(4) 0.8035(2) 0.3216(2) 0.0325(10) Uani 1.00 d . . . C(35) C 0.1576(4) 0.8461(2) 0.3331(2) 0.034(1) Uani 1.00 d . . . C(36) C 0.0856(3) 1.0091(2) 0.3451(2) 0.0299(9) Uani 1.00 d . . . C(37) C 0.1450(3) 0.9337(2) 0.2970(2) 0.0292(9) Uani 1.00 d . . . C(38) C 0.1902(3) 0.9386(2) 0.2125(2) 0.0316(10) Uani 1.00 d . . . C(39) C 0.1758(4) 1.0160(2) 0.1747(2) 0.035(1) Uani 1.00 d . . . C(40) C 0.1106(3) 1.0890(3) 0.2252(2) 0.033(1) Uani 1.00 d . . . C(41) C 0.0633(3) 1.0879(2) 0.3108(2) 0.0302(10) Uani 1.00 d . . . C(42) C -0.0115(4) 1.1700(2) 0.3614(2) 0.034(1) Uani 1.00 d . . . C(43) C -0.2241(4) 1.1450(2) 0.3965(2) 0.034(1) Uani 1.00 d . . . C(44) C -0.1406(4) 1.1939(2) 0.3578(2) 0.033(1) Uani 1.00 d . . . C(45) C -0.1803(4) 1.2615(3) 0.3155(3) 0.042(1) Uani 1.00 d . . . C(46) C -0.2963(4) 1.2818(3) 0.3090(3) 0.047(1) Uani 1.00 d . . . C(47) C -0.3768(4) 1.2310(3) 0.3484(3) 0.047(1) Uani 1.00 d . . . C(48) C -0.3431(4) 1.1622(3) 0.3923(3) 0.039(1) Uani 1.00 d . . . C(49) C -0.2844(4) 0.8333(3) 0.4035(3) 0.053(1) Uani 1.00 d . . . C(50) C 0.0382(5) 0.6417(3) 0.1738(3) 0.063(2) Uani 1.00 d . . . C(51) C 0.2273(5) 1.0208(3) 0.0820(3) 0.048(1) Uani 1.00 d . . . C(52) C 0.229(2) 1.106(1) 0.051(1) 0.1278 Uiso 0.50 d P . . C(53) C 0.178(2) 0.963(1) 0.040(1) 0.1364 Uiso 0.50 d P . . C(54) C 0.373(1) 0.9676(8) 0.0555(8) 0.0785 Uiso 0.50 d P . . C(55) C -0.4278(4) 1.1063(3) 0.4330(3) 0.060(1) Uani 1.00 d . . . C(56) C -0.3373(6) 1.3569(4) 0.2617(4) 0.079(2) Uani 1.00 d . . . C(57) C 0.2834(10) 1.1037(7) 0.0619(7) 0.0537 Uiso 0.50 d P . . C(58) C 0.111(1) 1.0417(7) 0.0498(7) 0.0622 Uiso 0.50 d P . . C(59) C 0.310(1) 0.9444(7) 0.0377(7) 0.0646 Uiso 0.50 d P . . C(60) C 0.7376(7) 0.9348(5) 0.1993(4) 0.089(2) Uani 1.00 d . . . C(61) C 0.6096(7) 0.9644(5) 0.2273(4) 0.091(2) Uani 1.00 d . . . C(62) C 0.5373(9) 0.9145(9) 0.2137(6) 0.152(4) Uani 1.00 d . . . C(63) C 0.589(1) 0.8355(9) 0.1697(6) 0.177(5) Uani 1.00 d . . . C(64) C 0.715(1) 0.8087(6) 0.1419(6) 0.156(4) Uani 1.00 d . . . C(65) C 0.7884(8) 0.8589(5) 0.1564(4) 0.088(2) Uani 1.00 d . . . C(66) C 0.8178(9) 0.9868(7) 0.2156(6) 0.153(4) Uani 1.00 d . . . C(67) C -0.061(1) 0.5323(8) 0.4016(8) 0.164(4) Uiso 1.00 d . . . C(68) C 0.015(1) 0.5807(10) 0.423(1) 0.101(4) Uiso 0.50 d P . . C(69) C 0.0567(9) 0.5593(6) 0.4891(7) 0.136(3) Uiso 1.00 d . . . C(70) C 0.093(2) 0.536(1) 0.562(1) 0.106(5) Uiso 0.50 d P . . C(71) C -0.019(1) 0.5151(9) 0.4687(9) 0.091(4) Uiso 0.50 d P . . H(1) H 0.3634(5) 0.1755(3) 0.2846(3) 0.063(2) Uiso 1.00 calc . . . H(2) H 0.2017(4) 0.4245(3) 0.3484(3) 0.051(2) Uiso 1.00 calc . . . H(3) H 0.2953(4) 0.5006(2) 0.1521(3) 0.041(2) Uiso 1.00 calc . . . H(4) H 0.2227(4) 0.5307(2) 0.2454(3) 0.041(2) Uiso 1.00 calc . . . H(5) H 0.3348(4) 0.5596(2) 0.3362(2) 0.043(2) Uiso 1.00 calc . . . H(6) H 0.6709(4) 0.6060(2) 0.2312(2) 0.046(2) Uiso 1.00 calc . . . H(7) H 0.6988(4) 0.5557(2) 0.0266(3) 0.045(2) Uiso 1.00 calc . . . H(8) H 0.7559(4) 0.6016(2) 0.0798(3) 0.045(2) Uiso 1.00 calc . . . H(9) H 0.9233(4) 0.5205(3) 0.1184(3) 0.055(2) Uiso 1.00 calc . . . H(10) H 1.0338(4) 0.2629(3) 0.0760(3) 0.070(2) Uiso 1.00 calc . . . H(11) H 0.5094(7) 0.1306(3) 0.1521(4) 0.096(3) Uiso 1.00 calc . . . H(12) H 0.4810(7) 0.1875(3) 0.0813(4) 0.096(3) Uiso 1.00 calc . . . H(13) H 0.5870(7) 0.1986(3) 0.1141(4) 0.096(3) Uiso 1.00 calc . . . H(14) H 0.2390(6) 0.3012(4) 0.4538(3) 0.086(2) Uiso 1.00 calc . . . H(15) H 0.1267(6) 0.2903(4) 0.4279(3) 0.086(2) Uiso 1.00 calc . . . H(16) H 0.2384(6) 0.2108(4) 0.4192(3) 0.086(2) Uiso 1.00 calc . . . H(17) H 0.6258(7) 0.5318(5) 0.4006(4) 0.119(3) Uiso 1.00 calc . . . H(18) H 0.6802(7) 0.6061(5) 0.3517(4) 0.119(3) Uiso 1.00 calc . . . H(19) H 0.6083(7) 0.6200(5) 0.4473(4) 0.119(3) Uiso 1.00 calc . . . H(20) H 0.3856(8) 0.6405(7) 0.5000(4) 0.190(6) Uiso 1.00 calc . . . H(21) H 0.3110(8) 0.6408(7) 0.4387(4) 0.190(6) Uiso 1.00 calc . . . H(22) H 0.3916(8) 0.5536(7) 0.4556(4) 0.190(6) Uiso 1.00 calc . . . H(23) H 0.4777(7) 0.7521(4) 0.4236(4) 0.107(3) Uiso 1.00 calc . . . H(24) H 0.5487(7) 0.7376(4) 0.3280(4) 0.107(3) Uiso 1.00 calc . . . H(25) H 0.4043(7) 0.7524(4) 0.3616(4) 0.107(3) Uiso 1.00 calc . . . H(26) H 0.7838(5) 0.2256(3) 0.0516(5) 0.110(3) Uiso 1.00 calc . . . H(27) H 0.8654(5) 0.2373(3) -0.0391(5) 0.110(3) Uiso 1.00 calc . . . H(28) H 0.9269(5) 0.1855(3) 0.0220(5) 0.110(3) Uiso 1.00 calc . . . H(29) H 1.0908(5) 0.3529(4) 0.1820(4) 0.101(3) Uiso 1.00 calc . . . H(30) H 1.1757(5) 0.3654(4) 0.0925(4) 0.101(3) Uiso 1.00 calc . . . H(31) H 1.0960(5) 0.4464(4) 0.1522(4) 0.101(3) Uiso 1.00 calc . . . H(32) H -0.1785(4) 0.7147(3) 0.2789(3) 0.056(2) Uiso 1.00 calc . . . H(33) H 0.1786(4) 0.7201(2) 0.2255(3) 0.045(2) Uiso 1.00 calc . . . H(34) H 0.1450(4) 0.8528(2) 0.3913(2) 0.040(2) Uiso 1.00 calc . . . H(35) H 0.2390(4) 0.8109(2) 0.3057(2) 0.040(2) Uiso 1.00 calc . . . H(36) H 0.2337(3) 0.8863(2) 0.1787(2) 0.038(1) Uiso 1.00 calc . . . H(37) H 0.0968(3) 1.1433(3) 0.1999(2) 0.040(1) Uiso 1.00 calc . . . H(38) H -0.0157(4) 1.1619(2) 0.4181(2) 0.040(2) Uiso 1.00 calc . . . H(39) H 0.0285(4) 1.2162(2) 0.3410(2) 0.040(2) Uiso 1.00 calc . . . H(40) H -0.1242(4) 1.2968(3) 0.2886(3) 0.050(2) Uiso 1.00 calc . . . H(41) H -0.4588(4) 1.2439(3) 0.3447(3) 0.055(2) Uiso 1.00 calc . . . H(42) H -0.2918(4) 0.8758(3) 0.4450(3) 0.062(2) Uiso 1.00 calc . . . H(43) H -0.3280(4) 0.8595(3) 0.3669(3) 0.062(2) Uiso 1.00 calc . . . H(44) H -0.3193(4) 0.7868(3) 0.4299(3) 0.063(2) Uiso 1.00 calc . . . H(45) H 0.0137(5) 0.5902(3) 0.1962(3) 0.076(2) Uiso 1.00 calc . . . H(46) H -0.0034(5) 0.6633(3) 0.1348(3) 0.076(2) Uiso 1.00 calc . . . H(47) H 0.1261(5) 0.6284(3) 0.1461(3) 0.076(2) Uiso 1.00 calc . . . H(48) H -0.5007(4) 1.1407(3) 0.4731(3) 0.069(2) Uiso 1.00 calc . . . H(49) H -0.4507(4) 1.0803(3) 0.3919(3) 0.069(2) Uiso 1.00 calc . . . H(50) H -0.3869(4) 1.0618(3) 0.4603(3) 0.069(2) Uiso 1.00 calc . . . H(51) H -0.2711(6) 1.3854(4) 0.2388(4) 0.094(3) Uiso 1.00 calc . . . H(52) H -0.3593(6) 1.3360(4) 0.2176(4) 0.094(3) Uiso 1.00 calc . . . H(53) H -0.4078(6) 1.3971(4) 0.2982(4) 0.094(3) Uiso 1.00 calc . . . H(54) H 0.5713(7) 1.0203(5) 0.2558(4) 0.105(3) Uiso 1.00 calc . . . H(55) H 0.4488(9) 0.9338(9) 0.2351(6) 0.166(5) Uiso 1.00 calc . . . H(56) H 0.538(1) 0.8012(9) 0.1585(6) 0.198(8) Uiso 1.00 calc . . . H(57) H 0.752(1) 0.7528(6) 0.1132(6) 0.165(6) Uiso 1.00 calc . . . H(58) H 0.8767(8) 0.8385(5) 0.1342(4) 0.102(3) Uiso 1.00 calc . . . H(59) H 0.8672(9) 0.9550(7) 0.2466(6) 0.176(5) Uiso 1.00 calc . . . H(60) H 0.8709(9) 1.0011(7) 0.1638(6) 0.176(5) Uiso 1.00 calc . . . H(61) H 0.7660(9) 1.0390(7) 0.2470(6) 0.177(5) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.0366(4) 0.0261(3) 0.0312(4) -0.0034(3) -0.0167(3) -0.0002(3) Ti(2) 0.0251(4) 0.0366(4) 0.0263(4) -0.0104(3) -0.0091(3) 0.0024(3) Cl(1) 0.0595(7) 0.0310(5) 0.0396(6) -0.0024(4) -0.0216(5) -0.0055(4) Cl(2) 0.0324(5) 0.0708(7) 0.0354(6) -0.0223(5) -0.0066(4) 0.0043(5) O(1) 0.079(2) 0.032(1) 0.036(2) -0.016(1) -0.003(2) -0.002(1) O(2) 0.037(1) 0.029(1) 0.025(1) -0.004(1) -0.014(1) -0.001(1) O(3) 0.046(2) 0.040(2) 0.080(2) 0.007(2) -0.038(2) -0.020(1) O(4) 0.032(1) 0.045(2) 0.041(2) -0.018(1) -0.006(1) -0.003(1) O(5) 0.027(1) 0.041(1) 0.023(1) -0.013(1) -0.009(1) 0.005(1) O(6) 0.031(1) 0.047(2) 0.047(2) -0.010(1) -0.015(1) 0.016(1) C(1) 0.052(3) 0.043(2) 0.033(2) -0.022(2) -0.013(2) 0.004(2) C(2) 0.066(3) 0.034(2) 0.044(3) -0.018(2) -0.013(2) 0.002(2) C(3) 0.060(3) 0.044(2) 0.051(3) -0.021(2) -0.019(2) 0.009(2) C(4) 0.045(3) 0.053(3) 0.039(2) -0.016(2) -0.015(2) 0.008(2) C(5) 0.039(2) 0.050(2) 0.039(2) -0.015(2) -0.012(2) 0.001(2) C(6) 0.033(2) 0.039(2) 0.039(2) -0.013(2) -0.017(2) 0.002(2) C(7) 0.031(2) 0.039(2) 0.033(2) -0.006(2) -0.012(2) -0.001(2) C(8) 0.043(2) 0.025(2) 0.029(2) -0.006(1) -0.018(2) -0.001(2) C(9) 0.032(2) 0.029(2) 0.032(2) -0.006(2) -0.013(2) 0.000(2) C(10) 0.044(2) 0.036(2) 0.028(2) -0.010(2) -0.013(2) 0.003(2) C(11) 0.048(2) 0.039(2) 0.031(2) -0.015(2) -0.017(2) 0.003(2) C(12) 0.041(2) 0.039(2) 0.034(2) -0.012(2) -0.019(2) 0.000(2) C(13) 0.038(2) 0.031(2) 0.031(2) -0.010(2) -0.015(2) 0.003(2) C(14) 0.040(2) 0.036(2) 0.037(2) -0.014(2) -0.014(2) 0.002(2) C(15) 0.035(2) 0.046(2) 0.050(3) -0.004(2) -0.025(2) -0.007(2) C(16) 0.031(2) 0.043(2) 0.035(2) -0.008(2) -0.010(2) 0.000(2) C(17) 0.042(2) 0.050(2) 0.047(3) -0.018(2) -0.019(2) 0.001(2) C(18) 0.038(2) 0.065(3) 0.061(3) -0.011(2) -0.022(2) -0.004(2) C(19) 0.044(3) 0.054(3) 0.077(4) 0.004(2) -0.036(3) -0.004(2) C(20) 0.043(3) 0.049(3) 0.079(4) 0.004(2) -0.032(3) -0.017(2) C(21) 0.136(6) 0.037(3) 0.066(4) -0.020(3) 0.004(4) 0.001(3) C(22) 0.090(4) 0.068(3) 0.056(3) -0.036(3) -0.017(3) 0.018(3) C(23) 0.061(3) 0.076(3) 0.032(2) -0.030(2) -0.017(2) -0.004(3) C(24) 0.112(5) 0.126(6) 0.061(4) -0.019(4) -0.057(4) -0.006(4) C(25) 0.160(8) 0.28(1) 0.033(3) -0.164(5) 0.003(4) -0.027(8) C(26) 0.113(6) 0.080(4) 0.074(4) -0.016(3) -0.044(4) -0.029(4) C(27) 0.075(4) 0.048(3) 0.151(7) 0.015(3) -0.077(4) -0.027(3) C(28) 0.056(3) 0.091(4) 0.105(5) -0.022(4) -0.051(4) 0.010(3) C(29) 0.041(2) 0.030(2) 0.029(2) -0.009(2) -0.009(2) 0.000(2) C(30) 0.034(2) 0.039(2) 0.035(2) -0.013(2) -0.010(2) 0.003(2) C(31) 0.045(3) 0.041(2) 0.053(3) -0.015(2) -0.019(2) -0.003(2) C(32) 0.049(3) 0.042(2) 0.044(3) -0.009(2) -0.020(2) -0.001(2) C(33) 0.039(2) 0.033(2) 0.040(2) -0.003(2) -0.012(2) 0.002(2) C(34) 0.035(2) 0.028(2) 0.034(2) -0.008(2) -0.015(2) 0.005(2) C(35) 0.031(2) 0.038(2) 0.032(2) -0.008(2) -0.010(2) 0.002(2) C(36) 0.027(2) 0.039(2) 0.021(2) -0.013(1) -0.009(1) 0.004(2) C(37) 0.022(2) 0.035(2) 0.029(2) -0.008(2) -0.007(2) 0.005(1) C(38) 0.032(2) 0.036(2) 0.026(2) -0.005(2) -0.009(2) -0.002(2) C(39) 0.036(2) 0.040(2) 0.029(2) -0.010(2) -0.011(2) 0.005(2) C(40) 0.030(2) 0.038(2) 0.031(2) -0.009(2) -0.007(2) 0.006(2) C(41) 0.026(2) 0.035(2) 0.029(2) -0.012(2) -0.008(2) 0.003(2) C(42) 0.034(2) 0.035(2) 0.032(2) -0.010(2) -0.008(2) 0.000(2) C(43) 0.034(2) 0.036(2) 0.032(2) -0.002(2) -0.010(2) 0.004(2) C(44) 0.038(2) 0.030(2) 0.030(2) -0.004(2) -0.008(2) -0.002(2) C(45) 0.049(3) 0.037(2) 0.039(2) -0.004(2) -0.007(2) 0.001(2) C(46) 0.052(3) 0.044(2) 0.045(3) 0.005(2) -0.016(2) 0.006(2) C(47) 0.042(3) 0.053(3) 0.044(3) 0.007(2) -0.016(2) -0.001(2) C(48) 0.034(2) 0.048(2) 0.035(2) -0.002(2) -0.012(2) -0.001(2) C(49) 0.041(2) 0.060(3) 0.054(3) -0.020(2) -0.017(2) -0.007(2) C(50) 0.064(3) 0.054(3) 0.070(4) -0.004(3) -0.028(3) -0.020(2) C(51) 0.059(3) 0.052(3) 0.028(2) -0.012(2) -0.004(2) 0.003(2) C(55) 0.031(2) 0.076(3) 0.064(3) -0.008(3) -0.019(2) 0.010(2) C(56) 0.085(4) 0.064(3) 0.086(4) 0.000(3) -0.036(4) 0.029(3) C(60) 0.107(6) 0.093(5) 0.059(4) -0.025(3) -0.033(4) 0.025(4) C(61) 0.084(5) 0.122(6) 0.056(4) 0.007(4) -0.014(4) -0.009(4) C(62) 0.110(7) 0.23(1) 0.077(6) -0.071(7) -0.037(5) 0.028(8) C(63) 0.23(1) 0.19(1) 0.076(7) -0.135(7) -0.085(8) 0.07(1) C(64) 0.24(1) 0.088(6) 0.082(6) -0.045(5) -0.069(9) 0.033(8) C(65) 0.114(6) 0.086(5) 0.053(4) 0.010(3) -0.020(4) 0.015(4) C(66) 0.144(8) 0.198(10) 0.099(7) -0.093(6) -0.042(6) 0.033(8) #------------------------------------------------------------------------------ _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SHELXS97' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti(1) Cl(1) 2.278(1) . . yes Ti(1) O(1) 1.755(3) . . yes Ti(1) O(2) 2.046(2) . . yes Ti(1) O(2) 1.985(3) . 2_665 yes Ti(1) O(3) 1.752(4) . . yes Ti(2) Cl(2) 2.274(1) . . yes Ti(2) O(4) 1.762(3) . . yes Ti(2) O(5) 2.053(3) . . yes Ti(2) O(5) 1.975(3) . 2_576 yes Ti(2) O(6) 1.750(3) . . yes O(1) C(1) 1.369(5) . . yes O(2) C(8) 1.408(5) . . yes O(3) C(15) 1.372(7) . . yes O(4) C(29) 1.367(5) . . yes O(5) C(36) 1.398(4) . . yes O(6) C(43) 1.366(5) . . yes C(1) C(2) 1.401(6) . . yes C(1) C(6) 1.378(5) . . yes C(2) C(3) 1.391(6) . . yes C(2) C(21) 1.490(6) . . yes C(3) C(4) 1.361(6) . . yes C(4) C(5) 1.385(6) . . yes C(4) C(22) 1.505(7) . . yes C(5) C(6) 1.394(6) . . yes C(6) C(7) 1.511(5) . . yes C(7) C(9) 1.516(6) . . yes C(8) C(9) 1.389(5) . . yes C(8) C(13) 1.390(7) . . yes C(9) C(10) 1.395(6) . . yes C(10) C(11) 1.383(7) . . yes C(11) C(12) 1.393(5) . . yes C(11) C(23) 1.527(7) . . yes C(12) C(13) 1.388(6) . . yes C(13) C(14) 1.506(5) . . yes C(14) C(16) 1.523(5) . . yes C(15) C(16) 1.386(7) . . yes C(15) C(20) 1.393(6) . . yes C(16) C(17) 1.380(7) . . yes C(17) C(18) 1.385(6) . . yes C(18) C(19) 1.389(8) . . yes C(18) C(28) 1.502(9) . . yes C(19) C(20) 1.380(9) . . yes C(20) C(27) 1.501(8) . . yes C(23) C(24) 1.514(10) . . yes C(23) C(25) 1.517(9) . . yes C(23) C(26) 1.559(8) . . yes C(29) C(30) 1.386(7) . . yes C(29) C(34) 1.396(5) . . yes C(30) C(31) 1.395(6) . . yes C(30) C(49) 1.495(5) . . yes C(31) C(32) 1.376(6) . . yes C(32) C(33) 1.393(8) . . yes C(32) C(50) 1.505(7) . . yes C(33) C(34) 1.394(6) . . yes C(34) C(35) 1.515(7) . . yes C(35) C(37) 1.521(5) . . yes C(36) C(37) 1.387(5) . . yes C(36) C(41) 1.391(5) . . yes C(37) C(38) 1.387(5) . . yes C(38) C(39) 1.391(5) . . yes C(39) C(40) 1.387(5) . . yes C(39) C(51) 1.523(6) . . yes C(40) C(41) 1.399(5) . . yes C(41) C(42) 1.517(5) . . yes C(42) C(44) 1.515(6) . . yes C(43) C(44) 1.398(6) . . yes C(43) C(48) 1.402(7) . . yes C(44) C(45) 1.373(6) . . yes C(45) C(46) 1.381(8) . . yes C(46) C(47) 1.399(7) . . yes C(46) C(56) 1.516(8) . . yes C(47) C(48) 1.382(6) . . yes C(48) C(55) 1.497(7) . . yes C(51) C(52) 1.46(2) . . yes C(51) C(53) 1.51(3) . . yes C(51) C(54) 1.66(1) . . yes C(51) C(57) 1.61(1) . . yes C(51) C(58) 1.61(1) . . yes C(51) C(59) 1.43(1) . . yes C(52) C(57) 0.72(3) . . yes C(53) C(58) 1.31(2) . . yes C(53) C(59) 1.52(3) . . yes C(54) C(59) 1.04(2) . . yes C(60) C(61) 1.40(1) . . yes C(60) C(65) 1.347(10) . . yes C(60) C(66) 1.50(2) . . yes C(61) C(62) 1.38(2) . . yes C(62) C(63) 1.40(2) . . yes C(63) C(64) 1.37(2) . . yes C(64) C(65) 1.40(2) . . yes C(67) C(68) 1.46(3) . . yes C(67) C(70) 1.32(2) . 2_566 yes C(67) C(71) 1.40(2) . . yes C(68) C(69) 1.39(2) . . yes C(68) C(71) 1.36(2) . . yes C(69) C(70) 1.46(2) . . yes C(69) C(71) 1.40(2) . . yes C(69) C(71) 1.47(2) . 2_566 yes C(70) C(71) 1.54(3) . 2_566 yes C(71) C(71) 1.34(3) . 2_566 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ti(1) O(1) 99.3(1) . . . yes Cl(1) Ti(1) O(2) 159.92(9) . . . yes Cl(1) Ti(1) O(2) 89.55(8) . . 2_665 yes Cl(1) Ti(1) O(3) 100.3(1) . . . yes O(1) Ti(1) O(2) 91.4(1) . . . yes O(1) Ti(1) O(2) 123.4(1) . . 2_665 yes O(1) Ti(1) O(3) 114.3(2) . . . yes O(2) Ti(1) O(2) 70.4(1) . . 2_665 yes O(2) Ti(1) O(3) 90.7(1) . . . yes O(2) Ti(1) O(3) 118.8(1) 2_665 . . yes Cl(2) Ti(2) O(4) 101.10(10) . . . yes Cl(2) Ti(2) O(5) 159.19(10) . . . yes Cl(2) Ti(2) O(5) 89.43(8) . . 2_576 yes Cl(2) Ti(2) O(6) 99.21(9) . . . yes O(4) Ti(2) O(5) 91.4(1) . . . yes O(4) Ti(2) O(5) 116.9(1) . . 2_576 yes O(4) Ti(2) O(6) 113.9(1) . . . yes O(5) Ti(2) O(5) 70.0(1) . . 2_576 yes O(5) Ti(2) O(6) 90.6(1) . . . yes O(5) Ti(2) O(6) 125.5(1) 2_576 . . yes Ti(1) O(1) C(1) 165.5(4) . . . yes Ti(1) O(2) Ti(1) 109.6(1) . . 2_665 yes Ti(1) O(2) C(8) 120.2(2) . . . yes Ti(1) O(2) C(8) 130.1(2) 2_665 . . yes Ti(1) O(3) C(15) 164.7(3) . . . yes Ti(2) O(4) C(29) 162.5(3) . . . yes Ti(2) O(5) Ti(2) 110.0(1) . . 2_576 yes Ti(2) O(5) C(36) 117.9(2) . . . yes Ti(2) O(5) C(36) 132.1(2) 2_576 . . yes Ti(2) O(6) C(43) 173.6(2) . . . yes O(1) C(1) C(2) 118.3(3) . . . yes O(1) C(1) C(6) 118.2(4) . . . yes C(2) C(1) C(6) 123.5(4) . . . yes C(1) C(2) C(3) 116.0(4) . . . yes C(1) C(2) C(21) 120.9(4) . . . yes C(3) C(2) C(21) 123.0(4) . . . yes C(2) C(3) C(4) 123.5(4) . . . yes C(3) C(4) C(5) 117.7(4) . . . yes C(3) C(4) C(22) 121.0(4) . . . yes C(5) C(4) C(22) 121.4(4) . . . yes C(4) C(5) C(6) 122.8(3) . . . yes C(1) C(6) C(5) 116.5(4) . . . yes C(1) C(6) C(7) 121.2(3) . . . yes C(5) C(6) C(7) 122.3(3) . . . yes C(6) C(7) C(9) 110.8(3) . . . yes O(2) C(8) C(9) 119.2(4) . . . yes O(2) C(8) C(13) 119.0(3) . . . yes C(9) C(8) C(13) 121.7(4) . . . yes C(7) C(9) C(8) 122.5(4) . . . yes C(7) C(9) C(10) 119.5(3) . . . yes C(8) C(9) C(10) 117.9(4) . . . yes C(9) C(10) C(11) 122.4(3) . . . yes C(10) C(11) C(12) 117.1(4) . . . yes C(10) C(11) C(23) 121.7(4) . . . yes C(12) C(11) C(23) 121.2(5) . . . yes C(11) C(12) C(13) 122.9(5) . . . yes C(8) C(13) C(12) 117.5(3) . . . yes C(8) C(13) C(14) 122.1(4) . . . yes C(12) C(13) C(14) 120.4(4) . . . yes C(13) C(14) C(16) 111.5(3) . . . yes O(3) C(15) C(16) 119.4(4) . . . yes O(3) C(15) C(20) 118.1(4) . . . yes C(16) C(15) C(20) 122.5(5) . . . yes C(14) C(16) C(15) 121.0(4) . . . yes C(14) C(16) C(17) 121.4(4) . . . yes C(15) C(16) C(17) 117.5(4) . . . yes C(16) C(17) C(18) 122.8(5) . . . yes C(17) C(18) C(19) 117.0(5) . . . yes C(17) C(18) C(28) 122.3(5) . . . yes C(19) C(18) C(28) 120.6(5) . . . yes C(18) C(19) C(20) 123.0(4) . . . yes C(15) C(20) C(19) 117.0(5) . . . yes C(15) C(20) C(27) 120.9(5) . . . yes C(19) C(20) C(27) 122.1(4) . . . yes C(11) C(23) C(24) 111.1(4) . . . yes C(11) C(23) C(25) 113.2(6) . . . yes C(11) C(23) C(26) 107.7(4) . . . yes C(24) C(23) C(25) 110.5(5) . . . yes C(24) C(23) C(26) 106.7(6) . . . yes C(25) C(23) C(26) 107.2(5) . . . yes O(4) C(29) C(30) 118.9(3) . . . yes O(4) C(29) C(34) 118.1(4) . . . yes C(30) C(29) C(34) 123.0(4) . . . yes C(29) C(30) C(31) 117.1(3) . . . yes C(29) C(30) C(49) 121.7(4) . . . yes C(31) C(30) C(49) 121.1(5) . . . yes C(30) C(31) C(32) 122.0(5) . . . yes C(31) C(32) C(33) 119.2(4) . . . yes C(31) C(32) C(50) 120.2(5) . . . yes C(33) C(32) C(50) 120.6(4) . . . yes C(32) C(33) C(34) 121.1(4) . . . yes C(29) C(34) C(33) 117.5(4) . . . yes C(29) C(34) C(35) 121.2(3) . . . yes C(33) C(34) C(35) 121.1(3) . . . yes C(34) C(35) C(37) 109.6(4) . . . yes O(5) C(36) C(37) 119.3(3) . . . yes O(5) C(36) C(41) 118.7(3) . . . yes C(37) C(36) C(41) 122.0(3) . . . yes C(35) C(37) C(36) 122.6(3) . . . yes C(35) C(37) C(38) 119.0(3) . . . yes C(36) C(37) C(38) 118.4(3) . . . yes C(37) C(38) C(39) 122.3(3) . . . yes C(38) C(39) C(40) 117.0(3) . . . yes C(38) C(39) C(51) 121.9(3) . . . yes C(40) C(39) C(51) 121.1(4) . . . yes C(39) C(40) C(41) 123.2(4) . . . yes C(36) C(41) C(40) 117.0(3) . . . yes C(36) C(41) C(42) 123.1(3) . . . yes C(40) C(41) C(42) 119.9(3) . . . yes C(41) C(42) C(44) 111.9(4) . . . yes O(6) C(43) C(44) 119.2(4) . . . yes O(6) C(43) C(48) 118.3(4) . . . yes C(44) C(43) C(48) 122.5(4) . . . yes C(42) C(44) C(43) 120.2(3) . . . yes C(42) C(44) C(45) 122.7(4) . . . yes C(43) C(44) C(45) 117.1(4) . . . yes C(44) C(45) C(46) 123.2(4) . . . yes C(45) C(46) C(47) 117.9(4) . . . yes C(45) C(46) C(56) 121.9(5) . . . yes C(47) C(46) C(56) 120.2(5) . . . yes C(46) C(47) C(48) 122.0(5) . . . yes C(43) C(48) C(47) 117.4(4) . . . yes C(43) C(48) C(55) 120.4(4) . . . yes C(47) C(48) C(55) 122.3(4) . . . yes C(39) C(51) C(52) 116.6(9) . . . yes C(39) C(51) C(53) 109.7(8) . . . yes C(39) C(51) C(54) 105.5(6) . . . yes C(39) C(51) C(57) 109.1(5) . . . yes C(39) C(51) C(58) 106.2(5) . . . yes C(39) C(51) C(59) 115.9(6) . . . yes C(52) C(51) C(53) 117(1) . . . yes C(52) C(51) C(54) 105.6(9) . . . yes C(52) C(51) C(57) 26(1) . . . yes C(52) C(51) C(58) 77(1) . . . yes C(52) C(51) C(59) 122.7(9) . . . yes C(53) C(51) C(54) 100.3(9) . . . yes C(53) C(51) C(57) 138.1(10) . . . yes C(53) C(51) C(58) 49.3(9) . . . yes C(53) C(51) C(59) 62.1(9) . . . yes C(54) C(51) C(57) 84.1(6) . . . yes C(54) C(51) C(58) 142.2(7) . . . yes C(54) C(51) C(59) 38.2(8) . . . yes C(57) C(51) C(58) 104.3(6) . . . yes C(57) C(51) C(59) 112.7(6) . . . yes C(58) C(51) C(59) 107.8(8) . . . yes C(51) C(52) C(57) 88(2) . . . yes C(51) C(53) C(58) 69(1) . . . yes C(51) C(53) C(59) 56(1) . . . yes C(58) C(53) C(59) 120(1) . . . yes C(51) C(54) C(59) 59.0(8) . . . yes C(51) C(57) C(52) 65(1) . . . yes C(51) C(58) C(53) 61(1) . . . yes C(51) C(59) C(53) 61.6(9) . . . yes C(51) C(59) C(54) 82.8(10) . . . yes C(53) C(59) C(54) 144(1) . . . yes C(61) C(60) C(65) 119.2(9) . . . yes C(61) C(60) C(66) 121.0(7) . . . yes C(65) C(60) C(66) 119.8(8) . . . yes C(60) C(61) C(62) 120.1(8) . . . yes C(61) C(62) C(63) 121(1) . . . yes C(62) C(63) C(64) 117(1) . . . yes C(63) C(64) C(65) 121.5(10) . . . yes C(60) C(65) C(64) 120.5(8) . . . yes C(68) C(67) C(70) 125(1) . . 2_566 yes C(68) C(67) C(71) 56(1) . . . yes C(70) C(67) C(71) 68(1) 2_566 . . yes C(67) C(68) C(69) 120(1) . . . yes C(67) C(68) C(71) 59(1) . . . yes C(69) C(68) C(71) 61(1) . . . yes C(68) C(69) C(70) 176(1) . . . yes C(68) C(69) C(71) 58(1) . . . yes C(68) C(69) C(71) 113(1) . . 2_566 yes C(70) C(69) C(71) 118(1) . . . yes C(70) C(69) C(71) 63(1) . . 2_566 yes C(71) C(69) C(71) 55(1) . . 2_566 yes C(67) C(70) C(69) 116(1) 2_566 . . yes C(67) C(70) C(71) 58(1) 2_566 . 2_566 yes C(69) C(70) C(71) 58(1) . . 2_566 yes C(67) C(71) C(68) 63(1) . . . yes C(67) C(71) C(69) 124(1) . . . yes C(67) C(71) C(69) 111(1) . . 2_566 yes C(67) C(71) C(70) 53(1) . . 2_566 yes C(67) C(71) C(71) 169(2) . . 2_566 yes C(68) C(71) C(69) 60(1) . . . yes C(68) C(71) C(69) 174(1) . . 2_566 yes C(68) C(71) C(70) 116(1) . . 2_566 yes C(68) C(71) C(71) 125(2) . . 2_566 yes C(69) C(71) C(69) 124(1) . . 2_566 yes C(69) C(71) C(70) 174(1) . . 2_566 yes C(69) C(71) C(71) 64(1) . . 2_566 yes C(69) C(71) C(70) 58(1) 2_566 . 2_566 yes C(69) C(71) C(71) 59(1) 2_566 . 2_566 yes C(70) C(71) C(71) 117(1) 2_566 . 2_566 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ti(1) O(1) C(1) C(2) -106(1) . . . . yes Ti(1) O(1) C(1) C(6) 73(1) . . . . yes Ti(1) O(2) Ti(1) Cl(1) -179.0(1) . . 2_665 2_665 yes Ti(1) O(2) Ti(1) O(1) -78.2(2) . . 2_665 2_665 yes Ti(1) O(2) Ti(1) O(2) 0.0000(2) . . 2_665 2_665 yes Ti(1) O(2) Ti(1) O(3) 79.5(2) . . 2_665 2_665 yes Ti(1) O(2) C(8) C(9) -89.7(3) . . . . yes Ti(1) O(2) C(8) C(13) 91.8(3) . . . . yes Ti(1) O(2) Ti(1) Cl(1) 3.0(3) . 2_665 2_665 2_665 yes Ti(1) O(2) Ti(1) O(1) 125.2(2) . 2_665 2_665 2_665 yes Ti(1) O(2) Ti(1) O(2) 0.0000(2) . 2_665 2_665 . yes Ti(1) O(2) Ti(1) O(3) -120.4(2) . 2_665 2_665 2_665 yes Ti(1) O(2) C(8) C(9) -92.0(4) . 2_665 2_665 2_665 yes Ti(1) O(2) C(8) C(13) 86.4(4) . 2_665 2_665 2_665 yes Ti(1) O(3) C(15) C(16) -71(1) . . . . yes Ti(1) O(3) C(15) C(20) 108(1) . . . . yes Ti(2) O(4) C(29) C(30) -99.5(9) . . . . yes Ti(2) O(4) C(29) C(34) 79(1) . . . . yes Ti(2) O(5) Ti(2) Cl(2) 176.8(1) . . 2_576 2_576 yes Ti(2) O(5) Ti(2) O(4) -81.1(2) . . 2_576 2_576 yes Ti(2) O(5) Ti(2) O(5) 0.0000(1) . . 2_576 2_576 yes Ti(2) O(5) Ti(2) O(6) 75.8(2) . . 2_576 2_576 yes Ti(2) O(5) C(36) C(37) -89.9(4) . . . . yes Ti(2) O(5) C(36) C(41) 89.4(4) . . . . yes Ti(2) O(5) Ti(2) Cl(2) -9.1(3) . 2_576 2_576 2_576 yes Ti(2) O(5) Ti(2) O(4) 118.2(1) . 2_576 2_576 2_576 yes Ti(2) O(5) Ti(2) O(5) 0.0000(1) . 2_576 2_576 . yes Ti(2) O(5) Ti(2) O(6) -127.8(1) . 2_576 2_576 2_576 yes Ti(2) O(5) C(36) C(37) -87.4(5) . 2_576 2_576 2_576 yes Ti(2) O(5) C(36) C(41) 93.3(4) . 2_576 2_576 2_576 yes Ti(2) O(6) C(43) C(44) -32(3) . . . . yes Ti(2) O(6) C(43) C(48) 146(2) . . . . yes Cl(1) Ti(1) O(1) C(1) 137.2(10) . . . . yes Cl(1) Ti(1) O(2) C(8) 178.4(2) . . . . yes Cl(1) Ti(1) O(2) C(8) 0.6(3) . . 2_665 2_665 yes Cl(1) Ti(1) O(3) C(15) -138(1) . . . . yes Cl(2) Ti(2) O(4) C(29) 132.0(9) . . . . yes Cl(2) Ti(2) O(5) C(36) -173.0(2) . . . . yes Cl(2) Ti(2) O(5) C(36) 0.7(3) . . 2_576 2_576 yes Cl(2) Ti(2) O(6) C(43) -178(2) . . . . yes O(1) Ti(1) O(2) C(8) 56.2(3) . . . . yes O(1) Ti(1) O(2) C(8) -100.3(3) . . 2_665 2_665 yes O(1) Ti(1) O(3) C(15) -33(1) . . . . yes O(1) C(1) C(2) C(3) 179.8(5) . . . . yes O(1) C(1) C(2) C(21) 0.1(9) . . . . yes O(1) C(1) C(6) C(5) -178.4(5) . . . . yes O(1) C(1) C(6) C(7) -0.6(7) . . . . yes O(2) Ti(1) O(1) C(1) -59(1) . . . . yes O(2) Ti(1) O(2) Ti(1) 0.0000(2) . . 2_665 2_665 yes O(2) Ti(1) O(2) C(8) -178.4(4) . . 2_665 2_665 yes O(2) Ti(1) O(3) C(15) 58(1) . . . . yes O(2) Ti(1) O(1) C(1) 127.1(10) . 2_665 2_665 2_665 yes O(2) Ti(1) O(2) Ti(1) 0.0000(1) . 2_665 2_665 . yes O(2) Ti(1) O(2) C(8) 178.6(3) . 2_665 2_665 2_665 yes O(2) Ti(1) O(3) C(15) -126(1) . 2_665 2_665 2_665 yes O(2) C(8) C(9) C(7) 10.5(5) . . . . yes O(2) C(8) C(9) C(10) -172.0(3) . . . . yes O(2) C(8) C(13) C(12) 171.6(3) . . . . yes O(2) C(8) C(13) C(14) -10.5(5) . . . . yes O(3) Ti(1) O(1) C(1) 31(1) . . . . yes O(3) Ti(1) O(2) C(8) -58.2(3) . . . . yes O(3) Ti(1) O(2) C(8) 102.0(3) . . 2_665 2_665 yes O(3) C(15) C(16) C(14) 2.6(6) . . . . yes O(3) C(15) C(16) C(17) -180.0(4) . . . . yes O(3) C(15) C(20) C(19) -179.2(4) . . . . yes O(3) C(15) C(20) C(27) -0.3(7) . . . . yes O(4) Ti(2) O(5) C(36) 59.7(2) . . . . yes O(4) Ti(2) O(5) C(36) -101.5(3) . . 2_576 2_576 yes O(4) Ti(2) O(6) C(43) -71(2) . . . . yes O(4) C(29) C(30) C(31) -179.7(4) . . . . yes O(4) C(29) C(30) C(49) 2.4(6) . . . . yes O(4) C(29) C(34) C(33) 179.1(3) . . . . yes O(4) C(29) C(34) C(35) -6.1(6) . . . . yes O(5) Ti(2) O(4) C(29) -64.7(9) . . . . yes O(5) Ti(2) O(5) Ti(2) 0.0 . . 2_576 2_576 yes O(5) Ti(2) O(5) C(36) 177.5(4) . . 2_576 2_576 yes O(5) Ti(2) O(6) C(43) 20(2) . . . . yes O(5) Ti(2) O(4) C(29) 132.9(9) . 2_576 2_576 2_576 yes O(5) Ti(2) O(5) Ti(2) 0.0000(1) . 2_576 2_576 . yes O(5) Ti(2) O(5) C(36) -177.9(3) . 2_576 2_576 2_576 yes O(5) Ti(2) O(6) C(43) -85(2) . 2_576 2_576 2_576 yes O(5) C(36) C(37) C(35) 6.2(6) . . . . yes O(5) C(36) C(37) C(38) -176.4(4) . . . . yes O(5) C(36) C(41) C(40) 176.6(4) . . . . yes O(5) C(36) C(41) C(42) -5.0(6) . . . . yes O(6) Ti(2) O(4) C(29) 26.6(10) . . . . yes O(6) Ti(2) O(5) C(36) -54.3(2) . . . . yes O(6) Ti(2) O(5) C(36) 101.6(3) . . 2_576 2_576 yes O(6) C(43) C(44) C(42) 2.2(6) . . . . yes O(6) C(43) C(44) C(45) -179.5(4) . . . . yes O(6) C(43) C(48) C(47) 179.8(4) . . . . yes O(6) C(43) C(48) C(55) -1.2(6) . . . . yes C(1) C(2) C(3) C(4) -2.4(9) . . . . yes C(1) C(6) C(5) C(4) -0.6(8) . . . . yes C(1) C(6) C(7) C(9) -78.6(6) . . . . yes C(2) C(1) C(6) C(5) 1.2(8) . . . . yes C(2) C(1) C(6) C(7) 179.0(5) . . . . yes C(2) C(3) C(4) C(5) 3.0(9) . . . . yes C(2) C(3) C(4) C(22) -176.5(6) . . . . yes C(3) C(2) C(1) C(6) 0.2(8) . . . . yes C(3) C(4) C(5) C(6) -1.4(8) . . . . yes C(4) C(3) C(2) C(21) 177.3(6) . . . . yes C(4) C(5) C(6) C(7) -178.3(5) . . . . yes C(5) C(6) C(7) C(9) 99.0(5) . . . . yes C(6) C(1) C(2) C(21) -179.5(6) . . . . yes C(6) C(5) C(4) C(22) 178.1(5) . . . . yes C(6) C(7) C(9) C(8) 97.0(4) . . . . yes C(6) C(7) C(9) C(10) -80.4(4) . . . . yes C(7) C(9) C(8) C(13) -171.0(3) . . . . yes C(7) C(9) C(10) C(11) 176.7(3) . . . . yes C(8) C(9) C(10) C(11) -0.9(5) . . . . yes C(8) C(13) C(12) C(11) 1.8(6) . . . . yes C(8) C(13) C(14) C(16) -96.1(5) . . . . yes C(9) C(8) C(13) C(12) -6.8(5) . . . . yes C(9) C(8) C(13) C(14) 171.1(3) . . . . yes C(9) C(10) C(11) C(12) -3.9(6) . . . . yes C(9) C(10) C(11) C(23) 174.8(4) . . . . yes C(10) C(9) C(8) C(13) 6.4(5) . . . . yes C(10) C(11) C(12) C(13) 3.4(6) . . . . yes C(10) C(11) C(23) C(24) 134.7(5) . . . . yes C(10) C(11) C(23) C(25) 9.7(7) . . . . yes C(10) C(11) C(23) C(26) -108.7(5) . . . . yes C(11) C(12) C(13) C(14) -176.2(4) . . . . yes C(12) C(11) C(23) C(24) -46.7(6) . . . . yes C(12) C(11) C(23) C(25) -171.7(5) . . . . yes C(12) C(11) C(23) C(26) 69.9(5) . . . . yes C(12) C(13) C(14) C(16) 81.7(5) . . . . yes C(13) C(12) C(11) C(23) -175.3(4) . . . . yes C(13) C(14) C(16) C(15) 76.9(5) . . . . yes C(13) C(14) C(16) C(17) -100.5(5) . . . . yes C(14) C(16) C(15) C(20) -177.5(4) . . . . yes C(14) C(16) C(17) C(18) 176.2(4) . . . . yes C(15) C(16) C(17) C(18) -1.3(6) . . . . yes C(15) C(20) C(19) C(18) -0.5(7) . . . . yes C(16) C(15) C(20) C(19) 0.9(7) . . . . yes C(16) C(15) C(20) C(27) 179.8(5) . . . . yes C(16) C(17) C(18) C(19) 1.7(7) . . . . yes C(16) C(17) C(18) C(28) -178.2(4) . . . . yes C(17) C(16) C(15) C(20) -0.1(6) . . . . yes C(17) C(18) C(19) C(20) -0.8(7) . . . . yes C(18) C(19) C(20) C(27) -179.3(5) . . . . yes C(20) C(19) C(18) C(28) 179.1(5) . . . . yes C(29) C(30) C(31) C(32) -0.1(6) . . . . yes C(29) C(34) C(33) C(32) 1.4(6) . . . . yes C(29) C(34) C(35) C(37) -74.0(4) . . . . yes C(30) C(29) C(34) C(33) -2.1(6) . . . . yes C(30) C(29) C(34) C(35) 172.7(4) . . . . yes C(30) C(31) C(32) C(33) -0.5(7) . . . . yes C(30) C(31) C(32) C(50) -179.6(4) . . . . yes C(31) C(30) C(29) C(34) 1.5(6) . . . . yes C(31) C(32) C(33) C(34) -0.2(7) . . . . yes C(32) C(31) C(30) C(49) 177.7(4) . . . . yes C(32) C(33) C(34) C(35) -173.4(4) . . . . yes C(33) C(34) C(35) C(37) 100.6(4) . . . . yes C(34) C(29) C(30) C(49) -176.4(4) . . . . yes C(34) C(33) C(32) C(50) 179.0(4) . . . . yes C(34) C(35) C(37) C(36) 100.3(5) . . . . yes C(34) C(35) C(37) C(38) -77.1(4) . . . . yes C(35) C(37) C(36) C(41) -173.0(4) . . . . yes C(35) C(37) C(38) C(39) 176.2(4) . . . . yes C(36) C(37) C(38) C(39) -1.3(7) . . . . yes C(36) C(41) C(40) C(39) 0.9(7) . . . . yes C(36) C(41) C(42) C(44) -101.3(5) . . . . yes C(37) C(36) C(41) C(40) -4.2(6) . . . . yes C(37) C(36) C(41) C(42) 174.2(4) . . . . yes C(37) C(38) C(39) C(40) -1.8(7) . . . . yes C(37) C(38) C(39) C(51) 179.2(4) . . . . yes C(38) C(37) C(36) C(41) 4.4(6) . . . . yes C(38) C(39) C(40) C(41) 2.0(7) . . . . yes C(38) C(39) C(51) C(52) -167(1) . . . . yes C(38) C(39) C(51) C(53) 56.4(10) . . . . yes C(38) C(39) C(51) C(54) -50.8(8) . . . . yes C(38) C(39) C(51) C(57) -139.8(6) . . . . yes C(38) C(39) C(51) C(58) 108.4(6) . . . . yes C(38) C(39) C(51) C(59) -11.3(9) . . . . yes C(39) C(40) C(41) C(42) -177.5(4) . . . . yes C(39) C(51) C(52) C(57) 79(1) . . . . yes C(39) C(51) C(53) C(58) 94.7(9) . . . . yes C(39) C(51) C(53) C(59) -109.6(7) . . . . yes C(39) C(51) C(54) C(59) 112.4(10) . . . . yes C(39) C(51) C(57) C(52) -111(1) . . . . yes C(39) C(51) C(58) C(53) -102(1) . . . . yes C(39) C(51) C(59) C(53) 99(1) . . . . yes C(39) C(51) C(59) C(54) -82(1) . . . . yes C(40) C(39) C(51) C(52) 13(1) . . . . yes C(40) C(39) C(51) C(53) -122.6(9) . . . . yes C(40) C(39) C(51) C(54) 130.2(7) . . . . yes C(40) C(39) C(51) C(57) 41.2(7) . . . . yes C(40) C(39) C(51) C(58) -70.7(7) . . . . yes C(40) C(39) C(51) C(59) 169.7(8) . . . . yes C(40) C(41) C(42) C(44) 77.0(5) . . . . yes C(41) C(40) C(39) C(51) -179.0(5) . . . . yes C(41) C(42) C(44) C(43) 70.1(5) . . . . yes C(41) C(42) C(44) C(45) -108.1(4) . . . . yes C(42) C(44) C(43) C(48) -177.4(4) . . . . yes C(42) C(44) C(45) C(46) 177.3(4) . . . . yes C(43) C(44) C(45) C(46) -1.0(6) . . . . yes C(43) C(48) C(47) C(46) 0.4(7) . . . . yes C(44) C(43) C(48) C(47) -0.7(6) . . . . yes C(44) C(43) C(48) C(55) 178.3(4) . . . . yes C(44) C(45) C(46) C(47) 0.7(7) . . . . yes C(44) C(45) C(46) C(56) -180.0(4) . . . . yes C(45) C(44) C(43) C(48) 0.9(6) . . . . yes C(45) C(46) C(47) C(48) -0.4(7) . . . . yes C(46) C(47) C(48) C(55) -178.5(4) . . . . yes C(48) C(47) C(46) C(56) -179.7(5) . . . . yes C(51) C(53) C(59) C(54) -2(2) . . . . yes C(51) C(54) C(59) C(53) 2(2) . . . . yes C(51) C(58) C(53) C(59) -23(1) . . . . yes C(51) C(59) C(53) C(58) 26(1) . . . . yes C(52) C(51) C(53) C(58) -41(1) . . . . yes C(52) C(51) C(53) C(59) 114(1) . . . . yes C(52) C(51) C(54) C(59) -123(1) . . . . yes C(52) C(51) C(58) C(53) 143(1) . . . . yes C(52) C(51) C(59) C(53) -105(1) . . . . yes C(52) C(51) C(59) C(54) 72(1) . . . . yes C(52) C(57) C(51) C(53) 45(2) . . . . yes C(52) C(57) C(51) C(54) 143(1) . . . . yes C(52) C(57) C(51) C(58) 1(1) . . . . yes C(52) C(57) C(51) C(59) 118(1) . . . . yes C(53) C(51) C(52) C(57) -147(1) . . . . yes C(53) C(51) C(54) C(59) -1(1) . . . . yes C(53) C(51) C(59) C(54) 178(1) . . . . yes C(53) C(58) C(51) C(54) 43(1) . . . . yes C(53) C(58) C(51) C(57) 142(1) . . . . yes C(53) C(58) C(51) C(59) 22(1) . . . . yes C(53) C(59) C(51) C(54) -178(1) . . . . yes C(53) C(59) C(51) C(57) -133(1) . . . . yes C(53) C(59) C(51) C(58) -19(1) . . . . yes C(54) C(51) C(52) C(57) -37(1) . . . . yes C(54) C(51) C(53) C(58) -154.6(9) . . . . yes C(54) C(51) C(53) C(59) 1.1(9) . . . . yes C(54) C(59) C(51) C(57) 44(1) . . . . yes C(54) C(59) C(51) C(58) 159.1(10) . . . . yes C(54) C(59) C(53) C(58) 23(3) . . . . yes C(57) C(51) C(53) C(58) -61(1) . . . . yes C(57) C(51) C(53) C(59) 93(1) . . . . yes C(57) C(51) C(54) C(59) -139(1) . . . . yes C(57) C(52) C(51) C(58) -178(1) . . . . yes C(57) C(52) C(51) C(59) -75(2) . . . . yes C(58) C(51) C(53) C(59) 155(1) . . . . yes C(58) C(51) C(54) C(59) -33(1) . . . . yes C(58) C(53) C(51) C(59) -155(1) . . . . yes C(60) C(61) C(62) C(63) -2(1) . . . . yes C(60) C(65) C(64) C(63) 0(1) . . . . yes C(61) C(60) C(65) C(64) -1(1) . . . . yes C(61) C(62) C(63) C(64) 1(1) . . . . yes C(62) C(61) C(60) C(65) 2(1) . . . . yes C(62) C(61) C(60) C(66) -178.1(8) . . . . yes C(62) C(63) C(64) C(65) 0(1) . . . . yes C(64) C(65) C(60) C(66) 178.8(8) . . . . yes C(67) C(68) C(69) C(70) -42(19) . . . . yes C(67) C(68) C(69) C(71) -1(1) . . . . yes C(67) C(68) C(69) C(71) 1(1) . . . 2_566 yes C(67) C(68) C(71) C(69) 178(1) . . . . yes C(67) C(68) C(71) C(69) 25(14) . . . 2_566 yes C(67) C(68) C(71) C(70) 3(1) . . . 2_566 yes C(67) C(68) C(71) C(71) 175(2) . . . 2_566 yes C(67) C(70) C(69) C(68) -46(19) . 2_566 2_566 2_566 yes C(67) C(70) C(69) C(71) -1(1) . 2_566 2_566 . yes C(67) C(70) C(69) C(71) -6(1) . 2_566 2_566 2_566 yes C(67) C(70) C(71) C(68) -4(1) . 2_566 . . yes C(67) C(70) C(71) C(69) -63(15) . 2_566 . . yes C(67) C(70) C(71) C(69) 178(1) . 2_566 . 2_566 yes C(67) C(70) C(71) C(71) -176(1) . 2_566 . 2_566 yes C(67) C(71) C(68) C(69) -178(1) . . . . yes C(67) C(71) C(69) C(68) 1(1) . . . . yes C(67) C(71) C(69) C(70) 178(1) . . . . yes C(67) C(71) C(69) C(71) -175(1) . . . 2_566 yes C(67) C(71) C(69) C(68) 178(1) . . 2_566 2_566 yes C(67) C(71) C(69) C(70) 1.5(10) . . 2_566 2_566 yes C(67) C(71) C(69) C(71) 175(1) . . 2_566 2_566 yes C(67) C(71) C(70) C(69) -178(1) . . 2_566 2_566 yes C(67) C(71) C(71) C(67) -180.0000(1) . . 2_566 2_566 yes C(67) C(71) C(71) C(68) -26(10) . . 2_566 2_566 yes C(67) C(71) C(71) C(69) 156(9) . . 2_566 . yes C(67) C(71) C(71) C(69) -23(9) . . 2_566 2_566 yes C(67) C(71) C(71) C(70) 162(8) . . 2_566 . yes C(68) C(67) C(70) C(69) 5(1) . . 2_566 2_566 yes C(68) C(67) C(70) C(71) 4(1) . . 2_566 . yes C(68) C(67) C(71) C(69) -1(1) . . . . yes C(68) C(67) C(71) C(69) -177(1) . . . 2_566 yes C(68) C(67) C(71) C(70) -175(1) . . . 2_566 yes C(68) C(67) C(71) C(71) -156(10) . . . 2_566 yes C(68) C(69) C(70) C(71) 44(18) . . . 2_566 yes C(68) C(69) C(71) C(69) 176(1) . . . 2_566 yes C(68) C(69) C(71) C(70) 61(15) . . . 2_566 yes C(68) C(69) C(71) C(71) 176(1) . . . 2_566 yes C(68) C(69) C(71) C(69) -2(1) . . 2_566 2_566 yes C(68) C(69) C(71) C(70) -177(1) . . 2_566 . yes C(68) C(69) C(71) C(71) -2(1) . . 2_566 . yes C(68) C(71) C(67) C(70) 175(1) . . . 2_566 yes C(68) C(71) C(69) C(70) 177(1) . . . . yes C(68) C(71) C(69) C(71) -176(1) . . . 2_566 yes C(68) C(71) C(69) C(70) -22(14) . . 2_566 2_566 yes C(68) C(71) C(69) C(71) 151(14) . . 2_566 2_566 yes C(68) C(71) C(70) C(69) 177(1) . . 2_566 2_566 yes C(68) C(71) C(71) C(68) 180.0 . . 2_566 2_566 yes C(68) C(71) C(71) C(69) 3(1) . . 2_566 . yes C(68) C(71) C(71) C(69) -176(1) . . 2_566 2_566 yes C(68) C(71) C(71) C(70) 8(2) . . 2_566 . yes C(69) C(68) C(67) C(70) -3(1) . . . 2_566 yes C(69) C(68) C(67) C(71) 1(1) . . . . yes C(69) C(68) C(71) C(70) -174(1) . . . 2_566 yes C(69) C(68) C(71) C(71) -3(1) . . . 2_566 yes C(69) C(70) C(67) C(71) -1(1) . . 2_566 2_566 yes C(69) C(70) C(71) C(71) -5(1) . . 2_566 . yes C(69) C(71) C(67) C(70) 174(1) . . . 2_566 yes C(69) C(71) C(69) C(70) -174(1) . . 2_566 2_566 yes C(69) C(71) C(69) C(71) 0.0000(3) . . 2_566 2_566 yes C(69) C(71) C(71) C(69) 180.0000(3) . . 2_566 2_566 yes C(69) C(71) C(71) C(70) 5(1) . . 2_566 . yes C(69) C(71) C(67) C(70) 1(1) . 2_566 2_566 . yes C(69) C(71) C(69) C(70) 5(1) . 2_566 2_566 2_566 yes C(69) C(71) C(69) C(71) 0.0000(1) . 2_566 2_566 . yes C(69) C(71) C(71) C(69) -180.0000(3) . 2_566 . 2_566 yes C(69) C(71) C(71) C(70) 174(1) . 2_566 . 2_566 yes C(70) C(67) C(68) C(71) 4(1) . 2_566 2_566 2_566 yes C(70) C(67) C(71) C(71) -19(9) . 2_566 2_566 . yes C(70) C(69) C(68) C(71) -40(18) . . . . yes C(70) C(69) C(71) C(71) -5(1) . . . 2_566 yes C(70) C(69) C(71) C(71) 174(1) . . 2_566 . yes C(70) C(71) C(69) C(71) -174(1) . 2_566 . . yes C(70) C(71) C(69) C(71) 115(15) . 2_566 2_566 . yes C(70) C(71) C(71) C(70) -180.0 . 2_566 . 2_566 yes C(71) C(69) C(71) C(69) 0.0 . . 2_566 2_566 yes C(71) C(69) C(71) C(69) 0.0000(1) . 2_566 2_566 . yes C(71) C(69) C(71) C(69) 0.0000(1) . 2_566 2_566 . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(6) C(28) 3.543(9) . 1_455 ? C(31) C(65) 3.296(9) . 1_455 ? C(49) C(55) 3.595(6) . 2_476 ? C(52) C(64) 3.49(2) . 2_675 ? C(54) C(54) 3.39(3) . 2_675 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_Ti(Me-L)Cl(THF)2 _database_code_CSD 172984 _audit_creation_date 'Wed Apr 3 14:11:16 2002' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C48 H71 Cl O8 Ti ' _chemical_formula_moiety 'C48 H71 Cl O8 Ti ' _chemical_formula_weight 859.44 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 12.901(1) _cell_length_b 20.966(1) _cell_length_c 17.2189(3) _cell_angle_alpha 90 _cell_angle_beta 89.0384(5) _cell_angle_gamma 90 _cell_volume 4656.7(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14691 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_type 'REQABA Empirical Absorption Correction' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.943 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.32 _diffrn_reflns_number 43621 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9958 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9958 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 10925 _reflns_number_gt 5820 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1910 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 10635 _refine_ls_number_parameters 612 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.002Fo^2^ + 1.000\s^2^(Fo)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0040 _refine_diff_density_max 1.28 _refine_diff_density_min -0.72 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.174 0.200 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ti' 'Ti' 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti(1) Ti 0.58695(4) 0.15032(3) 0.14556(3) 0.0334(1) Uani 1.00 d . . . Cl(1) Cl 0.73214(6) 0.18215(4) 0.22116(5) 0.0467(2) Uani 1.00 d . . . O(1) O 0.5193(2) 0.1111(1) 0.2240(1) 0.0380(6) Uani 1.00 d . . . O(2) O 0.5029(2) 0.1164(1) 0.0669(1) 0.0354(6) Uani 1.00 d . . . O(3) O 0.5255(2) 0.2272(1) 0.1491(1) 0.0395(6) Uani 1.00 d . . . O(4) O 0.6828(2) 0.1843(1) 0.0471(1) 0.0442(6) Uani 1.00 d . . . O(5) O 0.6775(2) 0.0615(1) 0.1280(1) 0.0417(6) Uani 1.00 d . . . O(6) O 0.2985(5) 0.2048(2) 0.2616(3) 0.143(2) Uani 1.00 d . . . O(7) O 0.077(1) 0.6076(9) 0.1170(7) 0.384(8) Uani 1.00 d . . . O(8) O 0.8651(7) 0.1221(5) -0.2031(5) 0.222(4) Uani 1.00 d . . . C(1) C 0.4672(2) 0.0680(1) 0.2687(2) 0.0357(8) Uani 1.00 d . . . C(2) C 0.4782(3) 0.0716(2) 0.3490(2) 0.0403(9) Uani 1.00 d . . . C(3) C 0.4248(3) 0.0276(2) 0.3947(2) 0.0474(10) Uani 1.00 d . . . C(4) C 0.3621(3) -0.0188(2) 0.3639(2) 0.0478(10) Uani 1.00 d . . . C(5) C 0.3515(3) -0.0205(2) 0.2834(2) 0.0439(9) Uani 1.00 d . . . C(6) C 0.4041(2) 0.0214(1) 0.2341(2) 0.0355(8) Uani 1.00 d . . . C(7) C 0.3947(3) 0.0162(1) 0.1470(2) 0.0392(9) Uani 1.00 d . . . C(8) C 0.3977(2) 0.1210(1) 0.0735(2) 0.0337(8) Uani 1.00 d . . . C(9) C 0.3404(2) 0.0719(1) 0.1096(2) 0.0350(8) Uani 1.00 d . . . C(10) C 0.2328(3) 0.0759(2) 0.1118(2) 0.0397(9) Uani 1.00 d . . . C(11) C 0.1792(3) 0.1273(2) 0.0807(2) 0.0410(9) Uani 1.00 d . . . C(12) C 0.2383(3) 0.1767(2) 0.0483(2) 0.0381(8) Uani 1.00 d . . . C(13) C 0.3464(2) 0.1746(1) 0.0442(2) 0.0338(8) Uani 1.00 d . . . C(14) C 0.4052(3) 0.2311(1) 0.0109(2) 0.0365(8) Uani 1.00 d . . . C(15) C 0.4715(2) 0.2812(1) 0.1346(2) 0.0355(8) Uani 1.00 d . . . C(16) C 0.4113(2) 0.2858(1) 0.0680(2) 0.0358(8) Uani 1.00 d . . . C(17) C 0.3545(3) 0.3415(2) 0.0573(2) 0.0397(9) Uani 1.00 d . . . C(18) C 0.3573(3) 0.3919(2) 0.1095(2) 0.0412(9) Uani 1.00 d . . . C(19) C 0.4196(3) 0.3862(2) 0.1742(2) 0.0441(9) Uani 1.00 d . . . C(20) C 0.4773(3) 0.3311(1) 0.1879(2) 0.0380(8) Uani 1.00 d . . . C(21) C 0.5456(3) 0.1221(2) 0.3834(2) 0.053(1) Uani 1.00 d . . . C(22) C 0.3082(4) -0.0681(2) 0.4143(2) 0.072(1) Uani 1.00 d . . . C(23) C 0.0600(3) 0.1299(2) 0.0821(3) 0.058(1) Uani 1.00 d . . . C(24) C 0.0227(7) 0.1257(6) 0.1690(6) 0.073(3) Uani 0.50 d P . . C(25) C 0.0234(7) 0.0705(6) 0.0361(8) 0.095(4) Uani 0.50 d P . . C(26) C 0.0172(7) 0.1900(5) 0.0481(8) 0.078(3) Uani 0.50 d P . . C(27) C 0.2939(3) 0.4516(2) 0.0975(2) 0.056(1) Uani 1.00 d . . . C(28) C 0.5421(3) 0.3240(2) 0.2590(2) 0.051(1) Uani 1.00 d . . . C(29) C 0.6870(3) 0.1604(2) -0.0321(2) 0.055(1) Uani 1.00 d . . . C(30) C 0.7026(5) 0.2184(3) -0.0818(3) 0.095(2) Uani 1.00 d . . . C(31) C 0.7540(5) 0.2625(3) -0.0343(3) 0.109(2) Uani 1.00 d . . . C(32) C 0.7239(4) 0.2499(2) 0.0472(3) 0.069(1) Uani 1.00 d . . . C(33) C 0.7238(3) 0.0294(2) 0.1951(2) 0.052(1) Uani 1.00 d . . . C(34) C 0.7584(3) -0.0354(2) 0.1663(2) 0.051(1) Uani 1.00 d . . . C(35) C 0.6857(3) -0.0479(2) 0.0999(2) 0.057(1) Uani 1.00 d . . . C(36) C 0.6762(3) 0.0167(2) 0.0633(2) 0.050(1) Uani 1.00 d . . . C(37) C 0.2336(5) 0.2669(3) 0.2591(4) 0.096(2) Uani 1.00 d . . . C(38) C 0.1974(6) 0.2738(3) 0.3380(3) 0.119(2) Uani 1.00 d . . . C(39) C 0.2102(3) 0.2195(2) 0.3793(2) 0.051(1) Uani 1.00 d . . . C(40) C 0.2533(4) 0.1723(2) 0.3295(3) 0.081(2) Uani 1.00 d . . . C(41) C 0.0256(10) 0.6299(6) 0.0431(7) 0.201(5) Uani 1.00 d . . . C(42) C -0.0605(7) 0.5849(7) 0.0421(7) 0.197(5) Uani 1.00 d . . . C(43) C -0.051(2) 0.5483(6) 0.112(1) 0.314(10) Uani 1.00 d . . . C(44) C 0.043(1) 0.5475(8) 0.117(1) 0.290(9) Uani 1.00 d . . . C(45) C 0.9324(10) 0.0760(6) -0.2141(9) 0.210(6) Uani 1.00 d . . . C(46) C 1.0052(9) 0.0952(7) -0.275(1) 0.226(7) Uani 1.00 d . . . C(47) C 0.9571(10) 0.1470(6) -0.3083(6) 0.172(5) Uani 1.00 d . . . C(48) C 0.8904(9) 0.1723(5) -0.2536(7) 0.182(5) Uani 1.00 d . . . C(49) C 0.0228(8) 0.134(1) -0.0047(8) 0.167(6) Uani 0.50 d P . . C(50) C 0.0076(8) 0.0737(8) 0.124(1) 0.148(6) Uani 0.50 d P . . C(51) C 0.0265(8) 0.1932(8) 0.122(1) 0.152(6) Uani 0.50 d P . . H(1) H 0.4320(3) 0.0294(2) 0.4506(2) 0.056(1) Uiso 1.00 calc . . . H(2) H 0.3064(3) -0.0521(2) 0.2606(2) 0.052(1) Uiso 1.00 calc . . . H(3) H 0.4641(3) 0.0133(1) 0.1245(2) 0.047(1) Uiso 1.00 calc . . . H(4) H 0.3567(3) -0.0225(1) 0.1354(2) 0.047(1) Uiso 1.00 calc . . . H(5) H 0.1935(3) 0.0417(2) 0.1361(2) 0.047(1) Uiso 1.00 calc . . . H(6) H 0.2030(3) 0.2136(2) 0.0276(2) 0.046(1) Uiso 1.00 calc . . . H(7) H 0.4750(3) 0.2172(1) -0.0023(2) 0.044(1) Uiso 1.00 calc . . . H(8) H 0.3712(3) 0.2458(1) -0.0356(2) 0.043(1) Uiso 1.00 calc . . . H(9) H 0.3112(3) 0.3450(2) 0.0120(2) 0.047(1) Uiso 1.00 calc . . . H(10) H 0.4247(3) 0.4215(2) 0.2104(2) 0.052(1) Uiso 1.00 calc . . . H(11) H 0.5455(3) 0.1184(2) 0.4396(2) 0.062(1) Uiso 1.00 calc . . . H(12) H 0.6159(3) 0.1175(2) 0.3633(2) 0.062(1) Uiso 1.00 calc . . . H(13) H 0.5188(3) 0.1636(2) 0.3690(2) 0.062(1) Uiso 1.00 calc . . . H(14) H 0.2340(4) -0.0662(2) 0.4068(2) 0.084(2) Uiso 1.00 calc . . . H(15) H 0.3336(4) -0.1102(2) 0.4002(2) 0.084(2) Uiso 1.00 calc . . . H(16) H 0.3232(4) -0.0597(2) 0.4683(2) 0.084(2) Uiso 1.00 calc . . . H(17) H 0.3054(3) 0.4816(2) 0.1394(2) 0.067(2) Uiso 1.00 calc . . . H(18) H 0.3143(3) 0.4710(2) 0.0484(2) 0.067(2) Uiso 1.00 calc . . . H(19) H 0.2210(3) 0.4404(2) 0.0964(2) 0.067(2) Uiso 1.00 calc . . . H(20) H 0.5166(3) 0.2884(2) 0.2898(2) 0.061(1) Uiso 1.00 calc . . . H(21) H 0.6137(3) 0.3163(2) 0.2436(2) 0.060(1) Uiso 1.00 calc . . . H(22) H 0.5377(3) 0.3629(2) 0.2895(2) 0.061(1) Uiso 1.00 calc . . . H(23) H 0.7457(3) 0.1319(2) -0.0387(2) 0.066(2) Uiso 1.00 calc . . . H(24) H 0.6236(3) 0.1378(2) -0.0441(2) 0.066(2) Uiso 1.00 calc . . . H(25) H 0.7436(5) 0.2086(3) -0.1281(3) 0.109(2) Uiso 1.00 calc . . . H(26) H 0.6357(5) 0.2350(3) -0.0968(3) 0.109(2) Uiso 1.00 calc . . . H(27) H 0.8283(5) 0.2571(3) -0.0408(3) 0.130(3) Uiso 1.00 calc . . . H(28) H 0.7351(5) 0.3058(3) -0.0479(3) 0.130(3) Uiso 1.00 calc . . . H(29) H 0.6704(4) 0.2794(2) 0.0646(3) 0.080(2) Uiso 1.00 calc . . . H(30) H 0.7830(4) 0.2531(2) 0.0811(3) 0.080(2) Uiso 1.00 calc . . . H(31) H 0.7822(3) 0.0538(2) 0.2138(2) 0.061(1) Uiso 1.00 calc . . . H(32) H 0.6726(3) 0.0246(2) 0.2366(2) 0.061(1) Uiso 1.00 calc . . . H(33) H 0.8298(3) -0.0338(2) 0.1476(2) 0.060(1) Uiso 1.00 calc . . . H(34) H 0.7516(3) -0.0677(2) 0.2064(2) 0.060(1) Uiso 1.00 calc . . . H(35) H 0.7145(3) -0.0788(2) 0.0637(2) 0.067(2) Uiso 1.00 calc . . . H(36) H 0.6189(3) -0.0628(2) 0.1193(2) 0.067(2) Uiso 1.00 calc . . . H(37) H 0.6119(3) 0.0206(2) 0.0354(2) 0.059(1) Uiso 1.00 calc . . . H(38) H 0.7342(3) 0.0249(2) 0.0281(2) 0.059(1) Uiso 1.00 calc . . . H(39) H 0.2773(5) 0.3029(3) 0.2451(4) 0.114(2) Uiso 1.00 calc . . . H(40) H 0.1771(5) 0.2638(3) 0.2228(4) 0.114(2) Uiso 1.00 calc . . . H(41) H 0.2331(6) 0.3086(3) 0.3633(3) 0.138(3) Uiso 1.00 calc . . . H(42) H 0.1237(6) 0.2828(3) 0.3372(3) 0.138(3) Uiso 1.00 calc . . . H(43) H 0.2582(3) 0.2278(2) 0.4209(2) 0.059(1) Uiso 1.00 calc . . . H(44) H 0.1446(3) 0.2049(2) 0.4012(2) 0.059(1) Uiso 1.00 calc . . . H(45) H 0.1989(4) 0.1435(2) 0.3136(3) 0.096(2) Uiso 1.00 calc . . . H(46) H 0.3066(4) 0.1485(2) 0.3560(3) 0.096(2) Uiso 1.00 calc . . . H(47) H 0.0031(10) 0.6734(6) 0.0521(7) 0.237(6) Uiso 1.00 calc . . . H(48) H 0.0735(10) 0.6287(6) -0.0010(7) 0.237(6) Uiso 1.00 calc . . . H(49) H -0.1237(7) 0.6098(7) 0.0391(7) 0.220(6) Uiso 1.00 calc . . . H(50) H -0.0502(7) 0.5612(7) -0.0058(7) 0.220(6) Uiso 1.00 calc . . . H(51) H -0.104(2) 0.5626(6) 0.149(1) 0.36(1) Uiso 1.00 calc . . . H(52) H -0.069(2) 0.5061(6) 0.093(1) 0.36(1) Uiso 1.00 calc . . . H(53) H 0.084(1) 0.5129(8) 0.095(1) 0.32(1) Uiso 1.00 calc . . . H(54) H 0.035(1) 0.5411(8) 0.172(1) 0.32(1) Uiso 1.00 calc . . . H(55) H 0.8953(10) 0.0383(6) -0.2310(9) 0.239(7) Uiso 1.00 calc . . . H(56) H 0.9694(10) 0.0663(6) -0.1669(9) 0.239(7) Uiso 1.00 calc . . . H(57) H 1.0193(9) 0.0610(7) -0.311(1) 0.257(7) Uiso 1.00 calc . . . H(58) H 1.0696(9) 0.1094(7) -0.252(1) 0.257(7) Uiso 1.00 calc . . . H(59) H 0.9170(10) 0.1318(6) -0.3518(6) 0.201(5) Uiso 1.00 calc . . . H(60) H 1.0076(10) 0.1780(6) -0.3266(6) 0.201(5) Uiso 1.00 calc . . . H(61) H 0.9252(9) 0.2071(5) -0.2277(7) 0.215(6) Uiso 1.00 calc . . . H(62) H 0.8271(9) 0.1879(5) -0.2766(7) 0.215(6) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.0330(3) 0.0311(3) 0.0358(3) 0.0004(2) -0.0042(2) -0.0016(2) Cl(1) 0.0409(5) 0.0442(5) 0.0538(5) -0.0023(4) -0.0130(4) -0.0053(4) O(1) 0.039(1) 0.040(1) 0.035(1) -0.0030(9) -0.0038(9) -0.0011(10) O(2) 0.035(1) 0.037(1) 0.034(1) 0.0007(9) -0.0030(9) -0.0031(9) O(3) 0.042(1) 0.031(1) 0.044(1) 0.0014(9) -0.0056(10) -0.0033(9) O(4) 0.046(1) 0.042(1) 0.045(1) -0.008(1) 0.001(1) 0.002(1) O(5) 0.049(1) 0.035(1) 0.039(1) 0.0091(9) -0.0105(10) -0.0039(10) O(6) 0.172(5) 0.125(4) 0.125(4) 0.031(3) 0.041(4) 0.021(4) O(7) 0.40(2) 0.48(2) 0.23(1) -0.31(1) -0.06(1) 0.09(2) O(8) 0.229(9) 0.189(7) 0.244(9) 0.041(7) 0.087(7) 0.039(7) C(1) 0.038(2) 0.032(2) 0.037(2) 0.004(1) -0.002(1) 0.003(1) C(2) 0.040(2) 0.041(2) 0.039(2) 0.004(1) -0.004(1) 0.000(1) C(3) 0.055(2) 0.047(2) 0.039(2) 0.004(1) -0.001(2) 0.004(2) C(4) 0.054(2) 0.044(2) 0.045(2) 0.003(1) 0.000(2) 0.009(2) C(5) 0.046(2) 0.035(2) 0.050(2) 0.004(1) -0.006(2) 0.005(1) C(6) 0.035(2) 0.032(2) 0.040(2) 0.004(1) -0.003(1) 0.002(1) C(7) 0.041(2) 0.031(2) 0.044(2) -0.001(1) -0.007(1) -0.004(1) C(8) 0.035(2) 0.035(2) 0.030(1) 0.001(1) -0.006(1) -0.007(1) C(9) 0.039(2) 0.032(1) 0.033(2) -0.001(1) -0.007(1) -0.003(1) C(10) 0.037(2) 0.042(2) 0.040(2) -0.006(1) -0.005(1) 0.002(1) C(11) 0.034(2) 0.043(2) 0.045(2) 0.000(1) -0.005(1) -0.001(1) C(12) 0.037(2) 0.037(2) 0.040(2) 0.004(1) -0.009(1) 0.000(1) C(13) 0.038(2) 0.032(1) 0.031(1) -0.002(1) -0.006(1) -0.002(1) C(14) 0.039(2) 0.036(2) 0.034(2) 0.002(1) -0.003(1) -0.001(1) C(15) 0.032(2) 0.032(2) 0.041(2) 0.000(1) 0.000(1) 0.001(1) C(16) 0.037(2) 0.033(2) 0.037(2) -0.001(1) 0.001(1) 0.002(1) C(17) 0.039(2) 0.040(2) 0.041(2) -0.001(1) -0.002(1) 0.005(1) C(18) 0.041(2) 0.032(2) 0.049(2) 0.002(1) 0.000(1) 0.001(1) C(19) 0.045(2) 0.035(2) 0.051(2) 0.001(1) -0.001(2) -0.004(1) C(20) 0.039(2) 0.035(2) 0.041(2) -0.002(1) -0.003(1) -0.002(1) C(21) 0.058(2) 0.060(2) 0.037(2) -0.005(2) -0.009(2) -0.006(2) C(22) 0.095(4) 0.058(2) 0.056(2) -0.022(2) -0.004(2) 0.017(2) C(23) 0.033(2) 0.059(2) 0.074(3) 0.001(2) -0.005(2) 0.010(2) C(24) 0.037(4) 0.094(7) 0.078(6) -0.003(5) 0.010(4) 0.010(5) C(25) 0.042(5) 0.104(8) 0.121(10) -0.022(7) -0.026(6) -0.029(5) C(26) 0.038(5) 0.078(6) 0.104(8) 0.019(6) -0.007(5) 0.023(4) C(27) 0.062(2) 0.041(2) 0.062(2) 0.011(2) -0.008(2) 0.000(2) C(28) 0.058(2) 0.039(2) 0.054(2) 0.002(2) -0.016(2) -0.006(2) C(29) 0.061(2) 0.061(2) 0.043(2) 0.006(2) 0.008(2) -0.003(2) C(30) 0.127(5) 0.086(3) 0.059(3) -0.009(3) 0.011(3) 0.018(3) C(31) 0.131(5) 0.097(4) 0.096(4) -0.053(3) -0.032(4) 0.053(4) C(32) 0.073(3) 0.042(2) 0.084(3) -0.016(2) 0.013(2) 0.000(2) C(33) 0.064(2) 0.041(2) 0.047(2) 0.012(2) -0.018(2) 0.001(2) C(34) 0.054(2) 0.042(2) 0.055(2) 0.012(2) -0.006(2) 0.000(2) C(35) 0.073(3) 0.038(2) 0.055(2) 0.010(2) -0.015(2) -0.010(2) C(36) 0.061(2) 0.047(2) 0.040(2) 0.016(2) -0.007(2) -0.009(2) C(37) 0.088(4) 0.085(4) 0.112(4) 0.023(3) 0.033(3) 0.036(3) C(38) 0.150(6) 0.118(5) 0.076(4) 0.071(3) -0.007(4) -0.024(4) C(39) 0.055(2) 0.063(2) 0.028(2) 0.016(2) 0.009(1) -0.002(2) C(40) 0.100(4) 0.069(3) 0.070(3) 0.012(2) 0.007(3) 0.018(3) C(41) 0.24(1) 0.20(1) 0.154(9) -0.064(8) -0.065(9) 0.03(1) C(42) 0.087(5) 0.26(1) 0.21(1) 0.010(9) -0.031(6) -0.141(7) C(43) 0.36(2) 0.15(1) 0.38(2) 0.06(1) 0.20(2) 0.08(1) C(44) 0.132(10) 0.24(2) 0.42(3) 0.09(2) 0.01(1) 0.06(1) C(45) 0.145(9) 0.159(9) 0.29(2) 0.04(1) -0.008(10) 0.106(8) C(46) 0.144(10) 0.19(1) 0.31(2) 0.07(1) -0.02(1) -0.042(9) C(47) 0.156(9) 0.22(1) 0.132(7) -0.045(8) -0.021(7) 0.036(8) C(48) 0.184(10) 0.136(7) 0.22(1) 0.068(8) 0.037(9) 0.075(7) C(49) 0.051(6) 0.27(2) 0.087(8) -0.01(1) -0.034(6) 0.024(10) C(50) 0.034(5) 0.15(1) 0.21(2) -0.01(1) 0.018(8) 0.096(6) C(51) 0.043(6) 0.14(1) 0.22(2) 0.02(1) 0.017(9) -0.093(7) #------------------------------------------------------------------------------ _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti(1) Cl(1) 2.394(1) . . yes Ti(1) O(1) 1.796(2) . . yes Ti(1) O(2) 1.889(2) . . yes Ti(1) O(3) 1.796(2) . . yes Ti(1) O(4) 2.200(2) . . yes Ti(1) O(5) 2.217(2) . . yes O(1) C(1) 1.356(4) . . yes O(2) C(8) 1.363(4) . . yes O(3) C(15) 1.355(4) . . yes O(4) C(29) 1.453(4) . . yes O(4) C(32) 1.475(4) . . yes O(5) C(33) 1.472(4) . . yes O(5) C(36) 1.457(4) . . yes O(6) C(37) 1.548(8) . . yes O(6) C(40) 1.465(7) . . yes O(7) C(41) 1.52(2) . . yes O(7) C(44) 1.33(2) . . yes O(8) C(45) 1.31(2) . . yes O(8) C(48) 1.40(1) . . yes C(1) C(2) 1.394(4) . . yes C(1) C(6) 1.410(4) . . yes C(2) C(3) 1.388(5) . . yes C(2) C(21) 1.500(5) . . yes C(3) C(4) 1.376(5) . . yes C(4) C(5) 1.396(5) . . yes C(4) C(22) 1.511(6) . . yes C(5) C(6) 1.391(4) . . yes C(6) C(7) 1.510(4) . . yes C(7) C(9) 1.512(4) . . yes C(8) C(9) 1.405(4) . . yes C(8) C(13) 1.403(4) . . yes C(9) C(10) 1.391(4) . . yes C(10) C(11) 1.391(5) . . yes C(11) C(12) 1.396(5) . . yes C(11) C(23) 1.538(5) . . yes C(12) C(13) 1.395(4) . . yes C(13) C(14) 1.515(4) . . yes C(14) C(16) 1.512(4) . . yes C(15) C(16) 1.399(4) . . yes C(15) C(20) 1.396(4) . . yes C(16) C(17) 1.393(4) . . yes C(17) C(18) 1.388(5) . . yes C(18) C(19) 1.389(5) . . yes C(18) C(27) 1.512(5) . . yes C(19) C(20) 1.397(4) . . yes C(20) C(28) 1.500(5) . . yes C(23) C(24) 1.57(1) . . yes C(23) C(25) 1.55(1) . . yes C(23) C(26) 1.50(1) . . yes C(23) C(49) 1.58(1) . . yes C(23) C(50) 1.53(2) . . yes C(23) C(51) 1.55(2) . . yes C(24) C(50) 1.35(2) . . yes C(24) C(51) 1.63(2) . . yes C(25) C(49) 1.51(3) . . yes C(25) C(50) 1.52(2) . . yes C(26) C(49) 1.49(2) . . yes C(26) C(51) 1.28(3) . . yes C(29) C(30) 1.498(6) . . yes C(30) C(31) 1.408(8) . . yes C(31) C(32) 1.473(8) . . yes C(33) C(34) 1.511(5) . . yes C(34) C(35) 1.513(6) . . yes C(35) C(36) 1.500(5) . . yes C(37) C(38) 1.437(9) . . yes C(38) C(39) 1.354(7) . . yes C(39) C(40) 1.417(6) . . yes C(41) C(42) 1.46(2) . . yes C(42) C(43) 1.43(2) . . yes C(43) C(44) 1.22(3) . . yes C(45) C(46) 1.45(2) . . yes C(46) C(47) 1.38(2) . . yes C(47) C(48) 1.37(2) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ti(1) O(1) 95.38(7) . . . yes Cl(1) Ti(1) O(2) 163.55(7) . . . yes Cl(1) Ti(1) O(3) 94.61(8) . . . yes Cl(1) Ti(1) O(4) 83.90(7) . . . yes Cl(1) Ti(1) O(5) 83.85(6) . . . yes O(1) Ti(1) O(2) 95.11(9) . . . yes O(1) Ti(1) O(3) 100.2(1) . . . yes O(1) Ti(1) O(4) 171.08(9) . . . yes O(1) Ti(1) O(5) 88.04(9) . . . yes O(2) Ti(1) O(3) 95.96(10) . . . yes O(2) Ti(1) O(4) 83.77(9) . . . yes O(2) Ti(1) O(5) 83.88(9) . . . yes O(3) Ti(1) O(4) 88.74(9) . . . yes O(3) Ti(1) O(5) 171.75(9) . . . yes O(4) Ti(1) O(5) 83.04(8) . . . yes Ti(1) O(1) C(1) 164.0(2) . . . yes Ti(1) O(2) C(8) 119.7(2) . . . yes Ti(1) O(3) C(15) 166.2(2) . . . yes Ti(1) O(4) C(29) 128.5(2) . . . yes Ti(1) O(4) C(32) 119.9(2) . . . yes C(29) O(4) C(32) 108.3(3) . . . yes Ti(1) O(5) C(33) 119.8(2) . . . yes Ti(1) O(5) C(36) 129.2(2) . . . yes C(33) O(5) C(36) 108.4(2) . . . yes C(37) O(6) C(40) 101.8(4) . . . yes C(41) O(7) C(44) 98(1) . . . yes C(45) O(8) C(48) 108.5(10) . . . yes O(1) C(1) C(2) 118.0(3) . . . yes O(1) C(1) C(6) 120.4(3) . . . yes C(2) C(1) C(6) 121.7(3) . . . yes C(1) C(2) C(3) 118.0(3) . . . yes C(1) C(2) C(21) 119.9(3) . . . yes C(3) C(2) C(21) 122.1(3) . . . yes C(2) C(3) C(4) 122.7(3) . . . yes C(3) C(4) C(5) 117.9(3) . . . yes C(3) C(4) C(22) 122.0(3) . . . yes C(5) C(4) C(22) 120.0(3) . . . yes C(4) C(5) C(6) 122.4(3) . . . yes C(1) C(6) C(5) 117.3(3) . . . yes C(1) C(6) C(7) 121.8(3) . . . yes C(5) C(6) C(7) 121.0(3) . . . yes C(6) C(7) C(9) 114.3(2) . . . yes O(2) C(8) C(9) 120.1(3) . . . yes O(2) C(8) C(13) 120.1(3) . . . yes C(9) C(8) C(13) 119.8(3) . . . yes C(7) C(9) C(8) 120.6(3) . . . yes C(7) C(9) C(10) 120.4(3) . . . yes C(8) C(9) C(10) 119.0(3) . . . yes C(9) C(10) C(11) 122.6(3) . . . yes C(10) C(11) C(12) 117.1(3) . . . yes C(10) C(11) C(23) 121.5(3) . . . yes C(12) C(11) C(23) 121.3(3) . . . yes C(11) C(12) C(13) 122.4(3) . . . yes C(8) C(13) C(12) 119.0(3) . . . yes C(8) C(13) C(14) 121.7(3) . . . yes C(12) C(13) C(14) 119.3(3) . . . yes C(13) C(14) C(16) 112.2(3) . . . yes O(3) C(15) C(16) 120.2(3) . . . yes O(3) C(15) C(20) 118.1(3) . . . yes C(16) C(15) C(20) 121.7(3) . . . yes C(14) C(16) C(15) 121.1(3) . . . yes C(14) C(16) C(17) 121.1(3) . . . yes C(15) C(16) C(17) 117.8(3) . . . yes C(16) C(17) C(18) 122.3(3) . . . yes C(17) C(18) C(19) 118.3(3) . . . yes C(17) C(18) C(27) 121.5(3) . . . yes C(19) C(18) C(27) 120.2(3) . . . yes C(18) C(19) C(20) 121.6(3) . . . yes C(15) C(20) C(19) 118.3(3) . . . yes C(15) C(20) C(28) 120.0(3) . . . yes C(19) C(20) C(28) 121.7(3) . . . yes C(11) C(23) C(24) 107.7(4) . . . yes C(11) C(23) C(25) 106.1(4) . . . yes C(11) C(23) C(26) 113.4(4) . . . yes C(11) C(23) C(49) 107.9(5) . . . yes C(11) C(23) C(50) 114.5(5) . . . yes C(11) C(23) C(51) 107.9(5) . . . yes C(24) C(23) C(25) 110.6(7) . . . yes C(24) C(23) C(26) 108.1(7) . . . yes C(24) C(23) C(49) 144.4(6) . . . yes C(24) C(23) C(50) 51.8(8) . . . yes C(24) C(23) C(51) 63.2(9) . . . yes C(25) C(23) C(26) 110.9(7) . . . yes C(25) C(23) C(49) 57.4(10) . . . yes C(25) C(23) C(50) 59.2(9) . . . yes C(25) C(23) C(51) 145.6(6) . . . yes C(26) C(23) C(49) 57.6(10) . . . yes C(26) C(23) C(50) 131.8(6) . . . yes C(26) C(23) C(51) 49.5(9) . . . yes C(49) C(23) C(50) 110(1) . . . yes C(49) C(23) C(51) 106(1) . . . yes C(50) C(23) C(51) 109.5(9) . . . yes C(23) C(24) C(50) 62.8(9) . . . yes C(23) C(24) C(51) 58.0(8) . . . yes C(50) C(24) C(51) 114(1) . . . yes C(23) C(25) C(49) 62.2(8) . . . yes C(23) C(25) C(50) 59.7(8) . . . yes C(49) C(25) C(50) 115(1) . . . yes C(23) C(26) C(49) 64.0(8) . . . yes C(23) C(26) C(51) 67.3(9) . . . yes C(49) C(26) C(51) 130(1) . . . yes O(4) C(29) C(30) 105.1(3) . . . yes C(29) C(30) C(31) 105.1(4) . . . yes C(30) C(31) C(32) 108.5(5) . . . yes O(4) C(32) C(31) 104.8(4) . . . yes O(5) C(33) C(34) 106.0(3) . . . yes C(33) C(34) C(35) 102.7(3) . . . yes C(34) C(35) C(36) 102.5(3) . . . yes O(5) C(36) C(35) 104.9(3) . . . yes O(6) C(37) C(38) 103.0(5) . . . yes C(37) C(38) C(39) 111.8(5) . . . yes C(38) C(39) C(40) 108.6(4) . . . yes O(6) C(40) C(39) 107.8(4) . . . yes O(7) C(41) C(42) 98(1) . . . yes C(41) C(42) C(43) 105(1) . . . yes C(42) C(43) C(44) 99(1) . . . yes O(7) C(44) C(43) 108(1) . . . yes O(8) C(45) C(46) 108(1) . . . yes C(45) C(46) C(47) 103(1) . . . yes C(46) C(47) C(48) 107(1) . . . yes O(8) C(48) C(47) 105.9(9) . . . yes C(23) C(49) C(25) 60.4(8) . . . yes C(23) C(49) C(26) 58.4(7) . . . yes C(25) C(49) C(26) 114(1) . . . yes C(23) C(50) C(24) 65.4(8) . . . yes C(23) C(50) C(25) 61.1(8) . . . yes C(24) C(50) C(25) 125(1) . . . yes C(23) C(51) C(24) 58.9(7) . . . yes C(23) C(51) C(26) 63.2(10) . . . yes C(24) C(51) C(26) 116(1) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ti(1) O(1) C(1) C(2) 151.8(6) . . . . yes Ti(1) O(1) C(1) C(6) -28.1(9) . . . . yes Ti(1) O(2) C(8) C(9) -91.1(3) . . . . yes Ti(1) O(2) C(8) C(13) 89.0(3) . . . . yes Ti(1) O(3) C(15) C(16) 6(1) . . . . yes Ti(1) O(3) C(15) C(20) -173.5(7) . . . . yes Ti(1) O(4) C(29) C(30) 143.8(3) . . . . yes Ti(1) O(4) C(32) C(31) -162.7(3) . . . . yes Ti(1) O(5) C(33) C(34) 167.9(2) . . . . yes Ti(1) O(5) C(36) C(35) -141.4(2) . . . . yes Cl(1) Ti(1) O(1) C(1) -128.9(7) . . . . yes Cl(1) Ti(1) O(2) C(8) -179.7(2) . . . . yes Cl(1) Ti(1) O(3) C(15) 147.0(9) . . . . yes Cl(1) Ti(1) O(4) C(29) 147.5(3) . . . . yes Cl(1) Ti(1) O(4) C(32) -55.2(3) . . . . yes Cl(1) Ti(1) O(5) C(33) 48.0(2) . . . . yes Cl(1) Ti(1) O(5) C(36) -152.4(2) . . . . yes O(1) Ti(1) O(2) C(8) 50.9(2) . . . . yes O(1) Ti(1) O(3) C(15) -116.7(9) . . . . yes O(1) Ti(1) O(4) C(29) 61.6(7) . . . . yes O(1) Ti(1) O(4) C(32) -141.0(6) . . . . yes O(1) Ti(1) O(5) C(33) -47.7(2) . . . . yes O(1) Ti(1) O(5) C(36) 112.0(3) . . . . yes O(1) C(1) C(2) C(3) 179.9(3) . . . . yes O(1) C(1) C(2) C(21) 0.4(5) . . . . yes O(1) C(1) C(6) C(5) -178.9(3) . . . . yes O(1) C(1) C(6) C(7) 1.9(4) . . . . yes O(2) Ti(1) O(1) C(1) 38.4(7) . . . . yes O(2) Ti(1) O(3) C(15) -20.4(9) . . . . yes O(2) Ti(1) O(4) C(29) -21.6(3) . . . . yes O(2) Ti(1) O(4) C(32) 135.7(3) . . . . yes O(2) Ti(1) O(5) C(33) -143.0(2) . . . . yes O(2) Ti(1) O(5) C(36) 16.7(3) . . . . yes O(2) C(8) C(9) C(7) 4.8(4) . . . . yes O(2) C(8) C(9) C(10) -176.4(3) . . . . yes O(2) C(8) C(13) C(12) 176.8(3) . . . . yes O(2) C(8) C(13) C(14) -5.3(4) . . . . yes O(3) Ti(1) O(1) C(1) 135.5(7) . . . . yes O(3) Ti(1) O(2) C(8) -49.9(2) . . . . yes O(3) Ti(1) O(4) C(29) -117.8(3) . . . . yes O(3) Ti(1) O(4) C(32) 39.6(3) . . . . yes O(3) Ti(1) O(5) C(33) 127.7(6) . . . . yes O(3) Ti(1) O(5) C(36) -72.7(7) . . . . yes O(3) C(15) C(16) C(14) -0.1(4) . . . . yes O(3) C(15) C(16) C(17) 177.8(3) . . . . yes O(3) C(15) C(20) C(19) -178.4(3) . . . . yes O(3) C(15) C(20) C(28) 0.0(4) . . . . yes O(4) Ti(1) O(1) C(1) -43(1) . . . . yes O(4) Ti(1) O(2) C(8) -138.0(2) . . . . yes O(4) Ti(1) O(3) C(15) 63.2(9) . . . . yes O(4) Ti(1) O(5) C(33) 132.6(2) . . . . yes O(4) Ti(1) O(5) C(36) -67.8(3) . . . . yes O(4) C(29) C(30) C(31) 27.3(6) . . . . yes O(4) C(32) C(31) C(30) 19.1(6) . . . . yes O(5) Ti(1) O(1) C(1) -45.2(7) . . . . yes O(5) Ti(1) O(2) C(8) 138.4(2) . . . . yes O(5) Ti(1) O(3) C(15) 68(1) . . . . yes O(5) Ti(1) O(4) C(29) 62.9(3) . . . . yes O(5) Ti(1) O(4) C(32) -139.7(3) . . . . yes O(5) C(33) C(34) C(35) -26.6(4) . . . . yes O(5) C(36) C(35) C(34) -36.3(4) . . . . yes O(6) C(37) C(38) C(39) -14.5(7) . . . . yes O(6) C(40) C(39) C(38) 18.3(6) . . . . yes O(7) C(41) C(42) C(43) 2(1) . . . . yes O(7) C(44) C(43) C(42) 55(1) . . . . yes O(8) C(45) C(46) C(47) -14(1) . . . . yes O(8) C(48) C(47) C(46) -25(1) . . . . yes C(1) C(2) C(3) C(4) -0.1(5) . . . . yes C(1) C(6) C(5) C(4) -2.1(5) . . . . yes C(1) C(6) C(7) C(9) -67.4(4) . . . . yes C(2) C(1) C(6) C(5) 1.1(5) . . . . yes C(2) C(1) C(6) C(7) -178.0(3) . . . . yes C(2) C(3) C(4) C(5) -0.8(5) . . . . yes C(2) C(3) C(4) C(22) 177.2(4) . . . . yes C(3) C(2) C(1) C(6) -0.1(5) . . . . yes C(3) C(4) C(5) C(6) 1.9(5) . . . . yes C(4) C(3) C(2) C(21) 179.5(3) . . . . yes C(4) C(5) C(6) C(7) 177.1(3) . . . . yes C(5) C(6) C(7) C(9) 113.5(3) . . . . yes C(6) C(1) C(2) C(21) -179.7(3) . . . . yes C(6) C(5) C(4) C(22) -176.2(3) . . . . yes C(6) C(7) C(9) C(8) 99.2(3) . . . . yes C(6) C(7) C(9) C(10) -79.6(4) . . . . yes C(7) C(9) C(8) C(13) -175.3(3) . . . . yes C(7) C(9) C(10) C(11) 177.6(3) . . . . yes C(8) C(9) C(10) C(11) -1.2(5) . . . . yes C(8) C(13) C(12) C(11) 0.2(5) . . . . yes C(8) C(13) C(14) C(16) -100.6(3) . . . . yes C(9) C(8) C(13) C(12) -3.0(4) . . . . yes C(9) C(8) C(13) C(14) 174.8(3) . . . . yes C(9) C(10) C(11) C(12) -1.6(5) . . . . yes C(9) C(10) C(11) C(23) 178.5(3) . . . . yes C(10) C(9) C(8) C(13) 3.5(4) . . . . yes C(10) C(11) C(12) C(13) 2.1(5) . . . . yes C(10) C(11) C(23) C(24) 58.6(6) . . . . yes C(10) C(11) C(23) C(25) -59.8(7) . . . . yes C(10) C(11) C(23) C(26) 178.2(6) . . . . yes C(10) C(11) C(23) C(49) -120.0(9) . . . . yes C(10) C(11) C(23) C(50) 3.2(9) . . . . yes C(10) C(11) C(23) C(51) 125.4(9) . . . . yes C(11) C(12) C(13) C(14) -177.7(3) . . . . yes C(11) C(23) C(24) C(50) -107.6(7) . . . . yes C(11) C(23) C(24) C(51) 101.6(6) . . . . yes C(11) C(23) C(25) C(49) -101.2(6) . . . . yes C(11) C(23) C(25) C(50) 109.3(6) . . . . yes C(11) C(23) C(26) C(49) 97.0(7) . . . . yes C(11) C(23) C(26) C(51) -94.1(7) . . . . yes C(11) C(23) C(49) C(25) 98.0(6) . . . . yes C(11) C(23) C(49) C(26) -106.8(6) . . . . yes C(11) C(23) C(50) C(24) 93.8(7) . . . . yes C(11) C(23) C(50) C(25) -94.8(7) . . . . yes C(11) C(23) C(51) C(24) -101.2(5) . . . . yes C(11) C(23) C(51) C(26) 105.8(6) . . . . yes C(12) C(11) C(23) C(24) -121.3(6) . . . . yes C(12) C(11) C(23) C(25) 120.3(6) . . . . yes C(12) C(11) C(23) C(26) -1.7(7) . . . . yes C(12) C(11) C(23) C(49) 60.0(10) . . . . yes C(12) C(11) C(23) C(50) -176.7(8) . . . . yes C(12) C(11) C(23) C(51) -54.5(9) . . . . yes C(12) C(13) C(14) C(16) 77.3(4) . . . . yes C(13) C(12) C(11) C(23) -178.0(3) . . . . yes C(13) C(14) C(16) C(15) 69.5(4) . . . . yes C(13) C(14) C(16) C(17) -108.3(3) . . . . yes C(14) C(16) C(15) C(20) -179.6(3) . . . . yes C(14) C(16) C(17) C(18) 178.9(3) . . . . yes C(15) C(16) C(17) C(18) 1.0(5) . . . . yes C(15) C(20) C(19) C(18) 0.2(5) . . . . yes C(16) C(15) C(20) C(19) 1.2(5) . . . . yes C(16) C(15) C(20) C(28) 179.5(3) . . . . yes C(16) C(17) C(18) C(19) 0.3(5) . . . . yes C(16) C(17) C(18) C(27) -179.1(3) . . . . yes C(17) C(16) C(15) C(20) -1.7(5) . . . . yes C(17) C(18) C(19) C(20) -0.9(5) . . . . yes C(18) C(19) C(20) C(28) -178.1(3) . . . . yes C(20) C(19) C(18) C(27) 178.5(3) . . . . yes C(23) C(24) C(50) C(25) -9.3(9) . . . . yes C(23) C(24) C(51) C(26) 27.0(8) . . . . yes C(23) C(25) C(49) C(26) -23.2(7) . . . . yes C(23) C(25) C(50) C(24) 9.7(9) . . . . yes C(23) C(26) C(49) C(25) 23.7(7) . . . . yes C(23) C(26) C(51) C(24) -25.8(7) . . . . yes C(23) C(49) C(25) C(50) 28.9(7) . . . . yes C(23) C(49) C(26) C(51) -13(1) . . . . yes C(23) C(50) C(24) C(51) 27.0(7) . . . . yes C(23) C(50) C(25) C(49) -29.7(8) . . . . yes C(23) C(51) C(24) C(50) -28.5(8) . . . . yes C(23) C(51) C(26) C(49) 13(1) . . . . yes C(24) C(23) C(25) C(49) 142.3(7) . . . . yes C(24) C(23) C(25) C(50) -7.2(7) . . . . yes C(24) C(23) C(26) C(49) -143.7(7) . . . . yes C(24) C(23) C(26) C(51) 25.3(8) . . . . yes C(24) C(23) C(49) C(25) -79(1) . . . . yes C(24) C(23) C(49) C(26) 75(1) . . . . yes C(24) C(23) C(50) C(25) 171.4(9) . . . . yes C(24) C(23) C(51) C(26) -152.9(8) . . . . yes C(24) C(50) C(23) C(25) -171.4(9) . . . . yes C(24) C(50) C(23) C(26) -80(1) . . . . yes C(24) C(50) C(23) C(49) -144.2(9) . . . . yes C(24) C(50) C(23) C(51) -27.5(9) . . . . yes C(24) C(50) C(25) C(49) -20(1) . . . . yes C(24) C(51) C(23) C(25) 87(1) . . . . yes C(24) C(51) C(23) C(26) 152.9(8) . . . . yes C(24) C(51) C(23) C(49) 143.2(7) . . . . yes C(24) C(51) C(23) C(50) 24.0(8) . . . . yes C(24) C(51) C(26) C(49) -12(1) . . . . yes C(25) C(23) C(24) C(50) 7.9(8) . . . . yes C(25) C(23) C(24) C(51) -142.9(7) . . . . yes C(25) C(23) C(26) C(49) -22.3(8) . . . . yes C(25) C(23) C(26) C(51) 146.7(8) . . . . yes C(25) C(23) C(49) C(26) 155.1(8) . . . . yes C(25) C(23) C(51) C(26) -65(1) . . . . yes C(25) C(49) C(23) C(26) -155.1(8) . . . . yes C(25) C(49) C(23) C(50) -27.7(8) . . . . yes C(25) C(49) C(23) C(51) -146.4(7) . . . . yes C(25) C(49) C(26) C(51) 10(1) . . . . yes C(25) C(50) C(23) C(26) 91(1) . . . . yes C(25) C(50) C(23) C(49) 27.2(9) . . . . yes C(25) C(50) C(23) C(51) 143.9(8) . . . . yes C(25) C(50) C(24) C(51) 17(1) . . . . yes C(26) C(23) C(24) C(50) 129.5(8) . . . . yes C(26) C(23) C(24) C(51) -21.3(7) . . . . yes C(26) C(23) C(25) C(49) 22.3(8) . . . . yes C(26) C(23) C(25) C(50) -127.1(8) . . . . yes C(26) C(49) C(23) C(50) 127.4(8) . . . . yes C(26) C(49) C(23) C(51) 8.7(8) . . . . yes C(26) C(49) C(25) C(50) 5(1) . . . . yes C(26) C(51) C(23) C(49) -9.7(9) . . . . yes C(26) C(51) C(23) C(50) -128.9(9) . . . . yes C(26) C(51) C(24) C(50) -1(1) . . . . yes C(29) O(4) C(32) C(31) -1.2(5) . . . . yes C(29) C(30) C(31) C(32) -28.8(6) . . . . yes C(30) C(29) O(4) C(32) -15.6(4) . . . . yes C(33) O(5) C(36) C(35) 20.1(4) . . . . yes C(33) C(34) C(35) C(36) 38.3(4) . . . . yes C(34) C(33) O(5) C(36) 4.3(4) . . . . yes C(37) O(6) C(40) C(39) -25.8(5) . . . . yes C(37) C(38) C(39) C(40) -1.6(7) . . . . yes C(38) C(37) O(6) C(40) 23.9(6) . . . . yes C(41) O(7) C(44) C(43) -53(1) . . . . yes C(41) C(42) C(43) C(44) -33(1) . . . . yes C(42) C(41) O(7) C(44) 25(1) . . . . yes C(45) O(8) C(48) C(47) 15(1) . . . . yes C(45) C(46) C(47) C(48) 24(1) . . . . yes C(46) C(45) O(8) C(48) 0(1) . . . . yes C(49) C(23) C(24) C(50) 70(1) . . . . yes C(49) C(23) C(24) C(51) -80(1) . . . . yes C(49) C(23) C(25) C(50) -149.5(8) . . . . yes C(49) C(23) C(26) C(51) 169.0(9) . . . . yes C(49) C(25) C(23) C(50) 149.5(8) . . . . yes C(49) C(25) C(23) C(51) 69(1) . . . . yes C(49) C(26) C(23) C(50) -89(1) . . . . yes C(49) C(26) C(23) C(51) -169.0(9) . . . . yes C(50) C(23) C(24) C(51) -150.8(9) . . . . yes C(50) C(23) C(26) C(51) 79(1) . . . . yes C(50) C(24) C(23) C(51) 150.8(9) . . . . yes C(50) C(25) C(23) C(51) -79(1) . . . . yes C(50) C(25) C(23) C(51) -79(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(8) C(35) 3.540(5) . 2_655 ? C(9) C(36) 3.519(4) . 2_655 ? C(25) C(25) 3.27(3) . 2_555 ? C(45) C(50) 3.59(2) . 2_655 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[NET4][Ti2(Me-L)2Cl3] _database_code_CSD 172985 _audit_creation_date 'Wed Apr 3 14:01:34 2002' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C67 H88 Cl9 N O6 Ti2 ' _chemical_formula_moiety 'C67 H88 Cl9 N O6 Ti2 ' _chemical_formula_weight 1418.31 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.448(4) _cell_length_b 15.768(5) _cell_length_c 19.078(5) _cell_angle_alpha 65.464(7) _cell_angle_beta 76.20(1) _cell_angle_gamma 88.95(1) _cell_volume 3558(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11957 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type 'REQABA Empirical Absorption Correction' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.913 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 27952 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9528 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9510 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_gt 11012 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.2530 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 15555 _refine_ls_number_parameters 854 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.007Fo^2^ + 1.000\s^2^(Fo)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 2.25 _refine_diff_density_min -1.68 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.174 0.200 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ti' 'Ti' 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti(1) Ti 0.92130(5) 0.97825(5) 0.24187(4) 0.0110(2) Uani 1.00 d . . . Ti(2) Ti 0.70633(5) 0.90190(5) 0.35959(4) 0.0109(2) Uani 1.00 d . . . Cl(1) Cl 1.06604(8) 0.90222(8) 0.27239(6) 0.0204(3) Uani 1.00 d . . . Cl(2) Cl 0.86720(8) 0.96915(7) 0.38712(6) 0.0168(2) Uani 1.00 d . . . Cl(3) Cl 0.60485(8) 1.00347(8) 0.39777(6) 0.0201(3) Uani 1.00 d . . . Cl(4) Cl 0.5797(3) 0.8464(3) 0.0138(2) 0.120(1) Uani 1.00 d . . . Cl(5) Cl 0.6492(3) 0.6646(2) 0.0977(2) 0.116(1) Uani 1.00 d . . . Cl(6) Cl 0.4747(4) 0.5426(3) 0.2812(3) 0.151(2) Uani 1.00 d . . . Cl(7) Cl 0.4221(3) 0.4581(2) 0.4537(2) 0.114(1) Uani 1.00 d . . . Cl(8) Cl 0.1710(2) 0.6457(1) 0.1836(1) 0.0628(5) Uani 1.00 d . . . Cl(9) Cl 0.1303(1) 0.6399(2) 0.3416(1) 0.0674(5) Uani 1.00 d . . . O(1) O 0.9370(2) 0.9572(2) 0.1543(2) 0.0155(7) Uani 1.00 d . . . O(2) O 0.8311(2) 0.8534(2) 0.3114(2) 0.0116(7) Uani 1.00 d . . . O(3) O 0.6874(2) 0.8051(2) 0.4563(2) 0.0148(7) Uani 1.00 d . . . O(4) O 0.9743(2) 1.0969(2) 0.2035(2) 0.0174(7) Uani 1.00 d . . . O(5) O 0.7747(2) 1.0142(2) 0.2537(2) 0.0117(7) Uani 1.00 d . . . O(6) O 0.6201(2) 0.8662(2) 0.3167(2) 0.0155(7) Uani 1.00 d . . . N(1) N 0.2321(3) 0.9933(3) 0.3999(2) 0.0207(9) Uani 1.00 d . . . C(1) C 0.9700(3) 0.9001(3) 0.1178(2) 0.0138(9) Uani 1.00 d . . . C(2) C 1.0664(3) 0.9255(3) 0.0626(2) 0.0149(10) Uani 1.00 d . . . C(3) C 1.0996(3) 0.8690(3) 0.0234(3) 0.016(1) Uani 1.00 d . . . C(4) C 1.0412(4) 0.7891(3) 0.0366(3) 0.021(1) Uani 1.00 d . . . C(5) C 0.9463(3) 0.7660(3) 0.0924(2) 0.0179(10) Uani 1.00 d . . . C(6) C 0.9085(3) 0.8201(3) 0.1343(2) 0.0134(9) Uani 1.00 d . . . C(7) C 0.8062(3) 0.7899(3) 0.1955(2) 0.0127(9) Uani 1.00 d . . . C(8) C 0.8362(3) 0.7589(3) 0.3297(2) 0.0125(9) Uani 1.00 d . . . C(9) C 0.8180(3) 0.7244(3) 0.2761(2) 0.0139(10) Uani 1.00 d . . . C(10) C 0.8145(3) 0.6287(3) 0.2981(2) 0.0154(10) Uani 1.00 d . . . C(11) C 0.8325(3) 0.5654(3) 0.3707(3) 0.0147(10) Uani 1.00 d . . . C(12) C 0.8541(3) 0.6026(3) 0.4211(3) 0.0141(10) Uani 1.00 d . . . C(13) C 0.8565(3) 0.6981(3) 0.4024(2) 0.0129(9) Uani 1.00 d . . . C(14) C 0.8864(3) 0.7334(3) 0.4573(3) 0.0162(10) Uani 1.00 d . . . C(15) C 0.7088(3) 0.7559(3) 0.5278(2) 0.0144(9) Uani 1.00 d . . . C(16) C 0.8042(3) 0.7201(3) 0.5314(3) 0.0166(10) Uani 1.00 d . . . C(17) C 0.8212(4) 0.6720(3) 0.6076(3) 0.023(1) Uani 1.00 d . . . C(18) C 0.7500(4) 0.6584(3) 0.6766(3) 0.025(1) Uani 1.00 d . . . C(19) C 0.6546(4) 0.6936(3) 0.6704(3) 0.022(1) Uani 1.00 d . . . C(20) C 0.6317(4) 0.7421(3) 0.5970(3) 0.018(1) Uani 1.00 d . . . C(21) C 1.1300(3) 1.0128(3) 0.0456(3) 0.017(1) Uani 1.00 d . . . C(22) C 1.0810(4) 0.7298(3) -0.0064(3) 0.026(1) Uani 1.00 d . . . C(23) C 0.8314(4) 0.4604(3) 0.3892(3) 0.022(1) Uani 1.00 d . . . C(24) C 0.7298(5) 0.4252(4) 0.3856(4) 0.047(2) Uani 1.00 d . . . C(25) C 0.9179(5) 0.4476(4) 0.3281(4) 0.044(2) Uani 1.00 d . . . C(26) C 0.8439(5) 0.4014(3) 0.4737(3) 0.040(1) Uani 1.00 d . . . C(27) C 0.5280(4) 0.7780(4) 0.5907(3) 0.024(1) Uani 1.00 d . . . C(28) C 0.7718(5) 0.6064(4) 0.7580(3) 0.042(2) Uani 1.00 d . . . C(29) C 0.9946(4) 1.1897(3) 0.1842(3) 0.020(1) Uani 1.00 d . . . C(30) C 1.0933(4) 1.2335(3) 0.1370(3) 0.023(1) Uani 1.00 d . . . C(31) C 1.1079(4) 1.3300(4) 0.1123(3) 0.028(1) Uani 1.00 d . . . C(32) C 1.0315(4) 1.3820(3) 0.1337(3) 0.032(1) Uani 1.00 d . . . C(33) C 0.9382(4) 1.3352(3) 0.1831(3) 0.031(1) Uani 1.00 d . . . C(34) C 0.9178(4) 1.2384(3) 0.2106(3) 0.024(1) Uani 1.00 d . . . C(35) C 0.8131(4) 1.1897(3) 0.2641(3) 0.023(1) Uani 1.00 d . . . C(36) C 0.7309(3) 1.0933(3) 0.2111(2) 0.0111(9) Uani 1.00 d . . . C(37) C 0.7438(3) 1.1767(3) 0.2171(2) 0.0165(10) Uani 1.00 d . . . C(38) C 0.6960(3) 1.2542(3) 0.1744(3) 0.019(1) Uani 1.00 d . . . C(39) C 0.6359(3) 1.2506(3) 0.1250(3) 0.018(1) Uani 1.00 d . . . C(40) C 0.6259(3) 1.1660(3) 0.1196(3) 0.017(1) Uani 1.00 d . . . C(41) C 0.6706(3) 1.0870(3) 0.1620(2) 0.0141(10) Uani 1.00 d . . . C(42) C 0.6614(3) 0.9999(3) 0.1486(2) 0.0150(10) Uani 1.00 d . . . C(43) C 0.5501(3) 0.8671(3) 0.2750(3) 0.0162(10) Uani 1.00 d . . . C(44) C 0.5639(3) 0.9337(3) 0.1957(3) 0.0157(10) Uani 1.00 d . . . C(45) C 0.4881(3) 0.9338(3) 0.1575(3) 0.022(1) Uani 1.00 d . . . C(46) C 0.4012(4) 0.8694(4) 0.1948(3) 0.027(1) Uani 1.00 d . . . C(47) C 0.3930(4) 0.8022(4) 0.2724(3) 0.026(1) Uani 1.00 d . . . C(48) C 0.4674(3) 0.7987(3) 0.3135(3) 0.021(1) Uani 1.00 d . . . C(49) C 1.1749(4) 1.1811(4) 0.1119(3) 0.032(1) Uani 1.00 d . . . C(50) C 1.0516(5) 1.4872(4) 0.1012(4) 0.050(2) Uani 1.00 d . . . C(51) C 0.5862(4) 1.3356(3) 0.0760(3) 0.025(1) Uani 1.00 d . . . C(52) C 0.6313(5) 1.3637(4) -0.0132(3) 0.040(2) Uani 1.00 d . . . C(53) C 0.6064(6) 1.4220(4) 0.0899(5) 0.062(2) Uani 1.00 d . . . C(54) C 0.4689(4) 1.3131(4) 0.0964(4) 0.035(2) Uani 1.00 d . . . C(55) C 0.4617(4) 0.7232(4) 0.3944(3) 0.028(1) Uani 1.00 d . . . C(56) C 0.3213(4) 0.8703(5) 0.1508(4) 0.047(2) Uani 1.00 d . . . C(57) C 0.1480(4) 0.9148(4) 0.4268(3) 0.029(1) Uani 1.00 d . . . C(58) C 0.0856(4) 0.8812(4) 0.5107(4) 0.035(1) Uani 1.00 d . . . C(59) C 0.2973(4) 0.9703(4) 0.4597(3) 0.026(1) Uani 1.00 d . . . C(60) C 0.3476(4) 0.8804(4) 0.4754(4) 0.035(1) Uani 1.00 d . . . C(61) C 0.2982(4) 1.0028(4) 0.3187(3) 0.032(1) Uani 1.00 d . . . C(62) C 0.3832(4) 1.0805(5) 0.2795(4) 0.041(2) Uani 1.00 d . . . C(63) C 0.1839(4) 1.0826(3) 0.3952(3) 0.021(1) Uani 1.00 d . . . C(64) C 0.1260(4) 1.1255(4) 0.3307(3) 0.030(1) Uani 1.00 d . . . C(65) C 0.567(1) 0.7441(10) 0.1060(8) 0.146(6) Uani 1.00 d . . . C(66) C 0.3769(8) 0.5038(7) 0.3715(7) 0.095(4) Uani 1.00 d . . . C(67) C 0.0950(4) 0.6837(4) 0.2515(4) 0.036(2) Uani 1.00 d . . . H(1) H 1.1664(3) 0.8857(3) -0.0146(3) 0.019(1) Uiso 1.00 calc . . . H(2) H 0.9048(3) 0.7103(3) 0.1029(2) 0.019(1) Uiso 1.00 calc . . . H(3) H 0.7761(3) 0.8450(3) 0.1986(2) 0.015(1) Uiso 1.00 calc . . . H(4) H 0.7610(3) 0.7584(3) 0.1792(2) 0.015(1) Uiso 1.00 calc . . . H(5) H 0.8003(3) 0.6050(3) 0.2617(2) 0.017(1) Uiso 1.00 calc . . . H(6) H 0.8678(3) 0.5602(3) 0.4712(3) 0.017(1) Uiso 1.00 calc . . . H(7) H 0.9445(3) 0.7011(3) 0.4740(3) 0.019(2) Uiso 1.00 calc . . . H(8) H 0.9069(3) 0.8000(3) 0.4275(3) 0.019(2) Uiso 1.00 calc . . . H(9) H 0.8873(4) 0.6473(3) 0.6112(3) 0.027(2) Uiso 1.00 calc . . . H(10) H 0.6026(4) 0.6839(3) 0.7187(3) 0.024(2) Uiso 1.00 calc . . . H(11) H 1.1455(3) 1.0073(3) 0.0943(3) 0.020(2) Uiso 1.00 calc . . . H(12) H 1.1935(3) 1.0202(3) 0.0058(3) 0.020(2) Uiso 1.00 calc . . . H(13) H 1.0918(3) 1.0668(3) 0.0260(3) 0.020(2) Uiso 1.00 calc . . . H(14) H 1.0304(4) 0.6779(3) 0.0094(3) 0.030(2) Uiso 1.00 calc . . . H(15) H 1.0944(4) 0.7674(3) -0.0634(3) 0.030(2) Uiso 1.00 calc . . . H(16) H 1.1442(4) 0.7058(3) 0.0068(3) 0.030(2) Uiso 1.00 calc . . . H(17) H 0.6747(5) 0.4326(4) 0.4254(4) 0.052(2) Uiso 1.00 calc . . . H(18) H 0.7194(5) 0.4615(4) 0.3331(4) 0.052(2) Uiso 1.00 calc . . . H(19) H 0.7301(5) 0.3596(4) 0.3957(4) 0.052(2) Uiso 1.00 calc . . . H(20) H 0.9183(5) 0.3819(4) 0.3386(4) 0.050(2) Uiso 1.00 calc . . . H(21) H 0.9090(5) 0.4836(4) 0.2751(4) 0.050(2) Uiso 1.00 calc . . . H(22) H 0.9826(5) 0.4693(4) 0.3319(4) 0.050(2) Uiso 1.00 calc . . . H(23) H 0.7884(5) 0.4095(3) 0.5128(3) 0.041(2) Uiso 1.00 calc . . . H(24) H 0.8431(5) 0.3359(3) 0.4836(3) 0.041(2) Uiso 1.00 calc . . . H(25) H 0.9091(5) 0.4219(3) 0.4776(3) 0.041(2) Uiso 1.00 calc . . . H(26) H 0.5361(4) 0.8453(4) 0.5597(3) 0.028(2) Uiso 1.00 calc . . . H(27) H 0.4960(4) 0.7485(4) 0.5650(3) 0.028(2) Uiso 1.00 calc . . . H(28) H 0.4850(4) 0.7628(4) 0.6438(3) 0.028(2) Uiso 1.00 calc . . . H(29) H 0.7232(5) 0.5514(4) 0.7896(3) 0.047(2) Uiso 1.00 calc . . . H(30) H 0.8412(5) 0.5874(4) 0.7511(3) 0.047(2) Uiso 1.00 calc . . . H(31) H 0.7652(5) 0.6473(4) 0.7850(3) 0.047(2) Uiso 1.00 calc . . . H(32) H 1.1741(4) 1.3622(4) 0.0780(3) 0.033(2) Uiso 1.00 calc . . . H(33) H 0.8855(4) 1.3705(3) 0.2001(3) 0.034(2) Uiso 1.00 calc . . . H(34) H 0.8226(4) 1.1288(3) 0.3033(3) 0.027(2) Uiso 1.00 calc . . . H(35) H 0.7810(4) 1.2273(3) 0.2910(3) 0.027(2) Uiso 1.00 calc . . . H(36) H 0.7048(3) 1.3123(3) 0.1791(3) 0.022(2) Uiso 1.00 calc . . . H(37) H 0.5851(3) 1.1617(3) 0.0855(3) 0.020(2) Uiso 1.00 calc . . . H(38) H 0.6658(3) 1.0194(3) 0.0925(2) 0.018(1) Uiso 1.00 calc . . . H(39) H 0.7194(3) 0.9650(3) 0.1621(2) 0.018(1) Uiso 1.00 calc . . . H(40) H 0.4957(3) 0.9802(3) 0.1033(3) 0.026(2) Uiso 1.00 calc . . . H(41) H 0.3336(4) 0.7564(4) 0.2987(3) 0.031(2) Uiso 1.00 calc . . . H(42) H 1.1505(4) 1.1153(4) 0.1354(3) 0.039(2) Uiso 1.00 calc . . . H(43) H 1.1938(4) 1.2048(4) 0.0543(3) 0.039(2) Uiso 1.00 calc . . . H(44) H 1.2345(4) 1.1885(4) 0.1299(3) 0.039(2) Uiso 1.00 calc . . . H(45) H 1.1208(5) 1.5074(4) 0.0670(4) 0.055(2) Uiso 1.00 calc . . . H(46) H 1.0023(5) 1.5167(4) 0.0707(4) 0.055(2) Uiso 1.00 calc . . . H(47) H 1.0438(5) 1.5051(4) 0.1450(4) 0.055(2) Uiso 1.00 calc . . . H(48) H 0.7050(5) 1.3791(4) -0.0268(3) 0.046(2) Uiso 1.00 calc . . . H(49) H 0.6179(5) 1.3112(4) -0.0247(3) 0.046(2) Uiso 1.00 calc . . . H(50) H 0.5998(5) 1.4174(4) -0.0445(3) 0.046(2) Uiso 1.00 calc . . . H(51) H 0.6797(6) 1.4387(4) 0.0769(5) 0.068(3) Uiso 1.00 calc . . . H(52) H 0.5743(6) 1.4745(4) 0.0577(5) 0.068(3) Uiso 1.00 calc . . . H(53) H 0.5767(6) 1.4064(4) 0.1459(5) 0.068(3) Uiso 1.00 calc . . . H(54) H 0.4376(4) 1.3663(4) 0.0641(4) 0.042(2) Uiso 1.00 calc . . . H(55) H 0.4555(4) 1.2596(4) 0.0862(4) 0.042(2) Uiso 1.00 calc . . . H(56) H 0.4400(4) 1.2982(4) 0.1523(4) 0.042(2) Uiso 1.00 calc . . . H(57) H 0.4609(4) 0.7504(4) 0.4317(3) 0.032(2) Uiso 1.00 calc . . . H(58) H 0.3997(4) 0.6816(4) 0.4121(3) 0.032(2) Uiso 1.00 calc . . . H(59) H 0.5214(4) 0.6882(4) 0.3915(3) 0.032(2) Uiso 1.00 calc . . . H(60) H 0.2929(4) 0.9305(5) 0.1345(4) 0.054(2) Uiso 1.00 calc . . . H(61) H 0.3532(4) 0.8600(5) 0.1041(4) 0.054(2) Uiso 1.00 calc . . . H(62) H 0.2667(4) 0.8211(5) 0.1854(4) 0.054(2) Uiso 1.00 calc . . . H(63) H 0.1015(4) 0.9369(4) 0.3924(3) 0.034(2) Uiso 1.00 calc . . . H(64) H 0.1804(4) 0.8619(4) 0.4207(3) 0.034(2) Uiso 1.00 calc . . . H(65) H 0.0516(4) 0.9330(4) 0.5177(4) 0.041(2) Uiso 1.00 calc . . . H(66) H 0.0344(4) 0.8311(4) 0.5230(4) 0.041(2) Uiso 1.00 calc . . . H(67) H 0.1307(4) 0.8584(4) 0.5461(4) 0.041(2) Uiso 1.00 calc . . . H(68) H 0.3511(4) 1.0209(4) 0.4390(3) 0.031(2) Uiso 1.00 calc . . . H(69) H 0.2535(4) 0.9665(4) 0.5095(3) 0.031(2) Uiso 1.00 calc . . . H(70) H 0.2947(4) 0.8288(4) 0.4973(4) 0.041(2) Uiso 1.00 calc . . . H(71) H 0.3917(4) 0.8829(4) 0.4261(4) 0.041(2) Uiso 1.00 calc . . . H(72) H 0.3883(4) 0.8712(4) 0.5133(4) 0.041(2) Uiso 1.00 calc . . . H(73) H 0.3279(4) 0.9443(4) 0.3253(3) 0.036(2) Uiso 1.00 calc . . . H(74) H 0.2531(4) 1.0155(4) 0.2833(3) 0.036(2) Uiso 1.00 calc . . . H(75) H 0.4291(4) 1.0690(5) 0.3140(4) 0.048(2) Uiso 1.00 calc . . . H(76) H 0.4210(4) 1.0823(5) 0.2286(4) 0.048(2) Uiso 1.00 calc . . . H(77) H 0.3548(4) 1.1399(5) 0.2711(4) 0.048(2) Uiso 1.00 calc . . . H(78) H 0.1368(4) 1.0699(3) 0.4463(3) 0.025(2) Uiso 1.00 calc . . . H(79) H 0.2391(4) 1.1286(3) 0.3844(3) 0.025(2) Uiso 1.00 calc . . . H(80) H 0.0985(4) 1.1823(4) 0.3319(3) 0.036(2) Uiso 1.00 calc . . . H(81) H 0.1722(4) 1.1400(4) 0.2788(3) 0.036(2) Uiso 1.00 calc . . . H(82) H 0.0700(4) 1.0808(4) 0.3406(3) 0.036(2) Uiso 1.00 calc . . . H(83) H 0.582(1) 0.7640(10) 0.1443(8) 0.174(9) Uiso 1.00 calc . . . H(84) H 0.497(1) 0.7153(10) 0.1252(8) 0.174(9) Uiso 1.00 calc . . . H(85) H 0.3428(8) 0.5585(7) 0.3717(7) 0.112(5) Uiso 1.00 calc . . . H(86) H 0.3280(8) 0.4585(7) 0.3728(7) 0.112(5) Uiso 1.00 calc . . . H(87) H 0.1015(4) 0.7516(4) 0.2286(4) 0.044(2) Uiso 1.00 calc . . . H(88) H 0.0240(4) 0.6612(4) 0.2619(4) 0.044(2) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.0128(4) 0.0087(3) 0.0111(3) -0.0009(3) -0.0011(3) -0.0044(3) Ti(2) 0.0126(4) 0.0106(4) 0.0094(3) 0.0020(3) -0.0021(3) -0.0022(3) Cl(1) 0.0158(5) 0.0241(5) 0.0205(5) 0.0051(4) -0.0065(4) -0.0120(4) Cl(2) 0.0203(5) 0.0149(5) 0.0146(5) 0.0022(4) -0.0055(4) -0.0078(4) Cl(3) 0.0189(5) 0.0209(5) 0.0204(5) 0.0077(4) -0.0024(4) -0.0091(4) Cl(4) 0.145(3) 0.112(3) 0.097(2) 0.032(2) -0.021(2) -0.058(2) Cl(5) 0.129(3) 0.098(2) 0.118(2) 0.023(2) -0.021(2) -0.059(2) Cl(6) 0.173(4) 0.129(3) 0.148(4) -0.024(3) 0.010(3) -0.031(3) Cl(7) 0.116(2) 0.086(2) 0.134(3) 0.002(2) -0.038(2) -0.041(2) Cl(8) 0.077(1) 0.053(1) 0.056(1) 0.0206(9) -0.0236(9) -0.0363(9) Cl(9) 0.0372(8) 0.104(2) 0.0377(8) -0.0010(9) -0.0117(7) -0.0231(9) O(1) 0.019(1) 0.011(1) 0.015(1) 0.002(1) -0.004(1) -0.007(1) O(2) 0.015(1) 0.008(1) 0.010(1) 0.000(1) -0.001(1) -0.003(1) O(3) 0.016(1) 0.017(1) 0.011(1) 0.001(1) -0.002(1) -0.003(1) O(4) 0.019(2) 0.011(1) 0.020(1) -0.002(1) -0.003(1) -0.007(1) O(5) 0.015(1) 0.009(1) 0.010(1) 0.002(1) -0.004(1) -0.001(1) O(6) 0.015(1) 0.017(1) 0.015(1) -0.001(1) -0.005(1) -0.003(1) N(1) 0.020(2) 0.024(2) 0.018(2) 0.005(2) -0.005(1) -0.013(1) C(1) 0.019(2) 0.009(2) 0.011(2) 0.002(1) -0.007(2) -0.003(1) C(2) 0.020(2) 0.012(2) 0.011(2) 0.002(2) -0.005(2) -0.003(2) C(3) 0.020(2) 0.014(2) 0.013(2) 0.000(2) 0.001(2) -0.002(2) C(4) 0.030(2) 0.013(2) 0.014(2) 0.008(2) -0.008(2) -0.005(2) C(5) 0.028(2) 0.008(2) 0.011(2) 0.001(2) -0.006(2) -0.002(2) C(6) 0.018(2) 0.011(2) 0.010(2) 0.000(1) -0.003(1) -0.002(1) C(7) 0.015(2) 0.012(2) 0.011(2) -0.003(2) -0.003(1) -0.004(1) C(8) 0.015(2) 0.008(2) 0.013(2) 0.001(2) -0.001(1) -0.004(1) C(9) 0.016(2) 0.012(2) 0.013(2) 0.000(2) -0.002(2) -0.006(1) C(10) 0.021(2) 0.009(2) 0.014(2) -0.002(2) -0.001(2) -0.004(1) C(11) 0.018(2) 0.010(2) 0.014(2) -0.003(2) 0.001(2) -0.002(1) C(12) 0.015(2) 0.013(2) 0.015(2) 0.001(2) 0.001(2) -0.003(1) C(13) 0.012(2) 0.015(2) 0.011(2) 0.003(2) -0.001(1) -0.005(1) C(14) 0.017(2) 0.014(2) 0.017(2) 0.005(2) -0.007(2) -0.006(2) C(15) 0.020(2) 0.010(2) 0.011(2) 0.000(1) -0.006(2) -0.003(1) C(16) 0.022(2) 0.011(2) 0.015(2) 0.005(2) -0.004(2) -0.006(2) C(17) 0.030(2) 0.018(2) 0.019(2) 0.013(2) -0.013(2) -0.009(2) C(18) 0.038(3) 0.016(2) 0.013(2) 0.004(2) -0.008(2) -0.003(2) C(19) 0.032(2) 0.018(2) 0.012(2) 0.004(2) -0.002(2) -0.006(2) C(20) 0.025(2) 0.014(2) 0.013(2) 0.003(2) -0.001(2) -0.002(2) C(21) 0.018(2) 0.016(2) 0.017(2) -0.001(2) -0.003(2) -0.007(2) C(22) 0.037(3) 0.017(2) 0.019(2) 0.006(2) -0.002(2) -0.009(2) C(23) 0.029(2) 0.010(2) 0.023(2) 0.000(2) -0.005(2) -0.005(2) C(24) 0.056(4) 0.017(3) 0.057(4) -0.007(3) -0.026(3) -0.007(2) C(25) 0.060(4) 0.025(3) 0.040(3) 0.016(2) -0.005(3) -0.017(3) C(26) 0.061(4) 0.011(2) 0.030(3) 0.008(2) -0.017(3) -0.004(2) C(27) 0.020(2) 0.032(3) 0.018(2) 0.008(2) -0.002(2) -0.005(2) C(28) 0.054(4) 0.046(3) 0.017(2) 0.024(2) -0.016(2) -0.010(3) C(29) 0.029(2) 0.009(2) 0.015(2) -0.005(2) -0.009(2) -0.002(2) C(30) 0.030(2) 0.021(2) 0.017(2) -0.006(2) -0.006(2) -0.007(2) C(31) 0.037(3) 0.023(2) 0.024(2) -0.015(2) -0.005(2) -0.006(2) C(32) 0.046(3) 0.014(2) 0.029(3) -0.007(2) -0.014(2) -0.006(2) C(33) 0.042(3) 0.015(2) 0.029(2) 0.002(2) -0.014(2) -0.012(2) C(34) 0.036(3) 0.012(2) 0.019(2) -0.001(2) -0.014(2) -0.005(2) C(35) 0.032(2) 0.017(2) 0.018(2) 0.004(2) -0.008(2) -0.009(2) C(36) 0.012(2) 0.010(2) 0.011(2) 0.002(1) 0.000(1) -0.002(1) C(37) 0.023(2) 0.012(2) 0.012(2) 0.003(2) -0.001(2) -0.005(2) C(38) 0.025(2) 0.010(2) 0.020(2) 0.006(2) -0.004(2) -0.007(2) C(39) 0.021(2) 0.013(2) 0.020(2) 0.006(2) -0.005(2) -0.001(2) C(40) 0.020(2) 0.017(2) 0.013(2) 0.003(2) -0.006(2) -0.002(2) C(41) 0.015(2) 0.015(2) 0.013(2) 0.002(2) -0.001(2) -0.004(2) C(42) 0.016(2) 0.016(2) 0.014(2) 0.002(2) -0.005(2) -0.006(2) C(43) 0.012(2) 0.016(2) 0.020(2) 0.003(2) -0.004(2) -0.010(1) C(44) 0.017(2) 0.010(2) 0.019(2) 0.003(2) -0.005(2) -0.007(1) C(45) 0.018(2) 0.020(2) 0.027(2) 0.002(2) -0.010(2) -0.009(2) C(46) 0.021(2) 0.029(3) 0.032(3) 0.003(2) -0.011(2) -0.015(2) C(47) 0.021(2) 0.025(2) 0.031(3) -0.005(2) -0.005(2) -0.013(2) C(48) 0.021(2) 0.020(2) 0.021(2) 0.000(2) -0.002(2) -0.011(2) C(49) 0.029(3) 0.034(3) 0.034(3) -0.013(2) 0.001(2) -0.020(2) C(50) 0.066(4) 0.017(3) 0.055(4) -0.009(3) -0.020(3) -0.011(3) C(51) 0.031(3) 0.019(2) 0.025(2) 0.011(2) -0.007(2) 0.000(2) C(52) 0.052(4) 0.036(3) 0.026(3) 0.017(2) -0.007(3) 0.006(3) C(53) 0.076(5) 0.021(3) 0.072(5) 0.023(3) -0.045(4) -0.013(3) C(54) 0.038(3) 0.031(3) 0.036(3) 0.016(2) -0.006(2) -0.006(2) C(55) 0.037(3) 0.023(3) 0.020(2) -0.009(2) -0.002(2) 0.000(2) C(56) 0.024(3) 0.061(4) 0.048(4) 0.000(3) -0.020(3) -0.023(3) C(57) 0.030(3) 0.026(2) 0.029(2) 0.001(2) -0.014(2) -0.016(2) C(58) 0.029(3) 0.031(3) 0.043(3) -0.004(2) -0.008(2) -0.017(2) C(59) 0.021(2) 0.027(2) 0.028(2) 0.010(2) -0.011(2) -0.014(2) C(60) 0.027(3) 0.031(3) 0.044(3) 0.012(2) -0.014(2) -0.016(2) C(61) 0.036(3) 0.037(3) 0.018(2) 0.009(2) -0.004(2) -0.013(2) C(62) 0.033(3) 0.052(4) 0.033(3) 0.009(3) 0.008(2) -0.017(3) C(63) 0.022(2) 0.020(2) 0.021(2) 0.005(2) -0.007(2) -0.009(2) C(64) 0.025(3) 0.036(3) 0.027(3) 0.007(2) -0.012(2) -0.011(2) C(65) 0.15(1) 0.17(1) 0.12(1) 0.103(10) -0.081(9) -0.09(1) C(66) 0.093(7) 0.071(7) 0.114(8) 0.010(6) -0.028(6) -0.049(5) C(67) 0.032(3) 0.037(3) 0.040(3) 0.007(3) -0.011(2) -0.017(2) #------------------------------------------------------------------------------ _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SHELXS97' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti(1) Ti(2) 3.104(1) . . yes Ti(1) Cl(1) 2.332(1) . . yes Ti(1) Cl(2) 2.635(1) . . yes Ti(1) O(1) 1.798(4) . . yes Ti(1) O(2) 2.063(3) . . yes Ti(1) O(4) 1.791(3) . . yes Ti(1) O(5) 2.028(3) . . yes Ti(2) Cl(2) 2.678(2) . . yes Ti(2) Cl(3) 2.318(2) . . yes Ti(2) O(2) 2.011(3) . . yes Ti(2) O(3) 1.802(3) . . yes Ti(2) O(5) 2.065(2) . . yes Ti(2) O(6) 1.786(4) . . yes Cl(4) C(65) 1.80(1) . . yes Cl(5) C(65) 1.69(2) . . yes Cl(6) C(66) 1.77(1) . . yes Cl(7) C(66) 1.69(1) . . yes Cl(8) C(67) 1.753(7) . . yes Cl(9) C(67) 1.745(7) . . yes O(1) C(1) 1.361(6) . . yes O(2) C(8) 1.386(5) . . yes O(3) C(15) 1.360(5) . . yes O(4) C(29) 1.366(6) . . yes O(5) C(36) 1.387(5) . . yes O(6) C(43) 1.366(6) . . yes N(1) C(57) 1.524(7) . . yes N(1) C(59) 1.523(7) . . yes N(1) C(61) 1.540(7) . . yes N(1) C(63) 1.516(7) . . yes C(1) C(2) 1.403(5) . . yes C(1) C(6) 1.400(6) . . yes C(2) C(3) 1.391(7) . . yes C(2) C(21) 1.506(7) . . yes C(3) C(4) 1.394(7) . . yes C(4) C(5) 1.394(6) . . yes C(4) C(22) 1.498(8) . . yes C(5) C(6) 1.407(7) . . yes C(6) C(7) 1.510(5) . . yes C(7) C(9) 1.500(6) . . yes C(8) C(9) 1.409(8) . . yes C(8) C(13) 1.409(6) . . yes C(9) C(10) 1.387(6) . . yes C(10) C(11) 1.406(6) . . yes C(11) C(12) 1.400(8) . . yes C(11) C(23) 1.544(7) . . yes C(12) C(13) 1.395(6) . . yes C(13) C(14) 1.505(8) . . yes C(14) C(16) 1.510(6) . . yes C(15) C(16) 1.396(6) . . yes C(15) C(20) 1.408(6) . . yes C(16) C(17) 1.406(7) . . yes C(17) C(18) 1.366(6) . . yes C(18) C(19) 1.400(7) . . yes C(18) C(28) 1.524(7) . . yes C(19) C(20) 1.395(6) . . yes C(20) C(27) 1.508(7) . . yes C(23) C(24) 1.511(9) . . yes C(23) C(25) 1.513(8) . . yes C(23) C(26) 1.539(7) . . yes C(29) C(30) 1.413(6) . . yes C(29) C(34) 1.399(7) . . yes C(30) C(31) 1.396(7) . . yes C(30) C(49) 1.469(8) . . yes C(31) C(32) 1.393(8) . . yes C(32) C(33) 1.379(7) . . yes C(32) C(50) 1.515(8) . . yes C(33) C(34) 1.401(7) . . yes C(34) C(35) 1.522(6) . . yes C(35) C(37) 1.507(8) . . yes C(36) C(37) 1.384(7) . . yes C(36) C(41) 1.411(7) . . yes C(37) C(38) 1.401(6) . . yes C(38) C(39) 1.398(8) . . yes C(39) C(40) 1.390(8) . . yes C(39) C(51) 1.530(7) . . yes C(40) C(41) 1.390(6) . . yes C(41) C(42) 1.509(7) . . yes C(42) C(44) 1.525(5) . . yes C(43) C(44) 1.408(5) . . yes C(43) C(48) 1.392(6) . . yes C(44) C(45) 1.386(8) . . yes C(45) C(46) 1.397(6) . . yes C(46) C(47) 1.397(7) . . yes C(46) C(56) 1.510(10) . . yes C(47) C(48) 1.399(8) . . yes C(48) C(55) 1.491(6) . . yes C(51) C(52) 1.534(8) . . yes C(51) C(53) 1.53(1) . . yes C(51) C(54) 1.543(8) . . yes C(57) C(58) 1.489(7) . . yes C(59) C(60) 1.505(8) . . yes C(61) C(62) 1.499(8) . . yes C(63) C(64) 1.525(8) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ti(2) Ti(1) Cl(1) 120.03(4) . . . yes Ti(2) Ti(1) Cl(2) 54.89(3) . . . yes Ti(2) Ti(1) O(1) 112.75(10) . . . yes Ti(2) Ti(1) O(2) 39.75(9) . . . yes Ti(2) Ti(1) O(4) 123.6(1) . . . yes Ti(2) Ti(1) O(5) 41.13(7) . . . yes Cl(1) Ti(1) Cl(2) 88.58(5) . . . yes Cl(1) Ti(1) O(1) 92.4(1) . . . yes Cl(1) Ti(1) O(2) 89.55(9) . . . yes Cl(1) Ti(1) O(4) 99.0(1) . . . yes Cl(1) Ti(1) O(5) 160.80(8) . . . yes Cl(2) Ti(1) O(1) 165.34(9) . . . yes Cl(2) Ti(1) O(2) 74.0(1) . . . yes Cl(2) Ti(1) O(4) 90.6(1) . . . yes Cl(2) Ti(1) O(5) 76.25(10) . . . yes O(1) Ti(1) O(2) 91.3(1) . . . yes O(1) Ti(1) O(4) 103.7(1) . . . yes O(1) Ti(1) O(5) 99.4(1) . . . yes O(2) Ti(1) O(4) 162.3(1) . . . yes O(2) Ti(1) O(5) 75.1(1) . . . yes O(4) Ti(1) O(5) 92.9(1) . . . yes Ti(1) Ti(2) Cl(2) 53.60(3) . . . yes Ti(1) Ti(2) Cl(3) 119.05(4) . . . yes Ti(1) Ti(2) O(2) 41.01(8) . . . yes Ti(1) Ti(2) O(3) 123.01(10) . . . yes Ti(1) Ti(2) O(5) 40.23(8) . . . yes Ti(1) Ti(2) O(6) 112.00(9) . . . yes Cl(2) Ti(2) Cl(3) 89.62(5) . . . yes Cl(2) Ti(2) O(2) 73.8(1) . . . yes Cl(2) Ti(2) O(3) 88.4(1) . . . yes Cl(2) Ti(2) O(5) 74.68(10) . . . yes Cl(2) Ti(2) O(6) 165.56(9) . . . yes Cl(3) Ti(2) O(2) 159.52(9) . . . yes Cl(3) Ti(2) O(3) 98.3(1) . . . yes Cl(3) Ti(2) O(5) 88.80(9) . . . yes Cl(3) Ti(2) O(6) 98.1(1) . . . yes O(2) Ti(2) O(3) 93.3(1) . . . yes O(2) Ti(2) O(5) 75.5(1) . . . yes O(2) Ti(2) O(6) 95.8(2) . . . yes O(3) Ti(2) O(5) 161.7(1) . . . yes O(3) Ti(2) O(6) 102.4(1) . . . yes O(5) Ti(2) O(6) 93.2(1) . . . yes Ti(1) Cl(2) Ti(2) 71.51(4) . . . yes Ti(1) O(1) C(1) 147.3(3) . . . yes Ti(1) O(2) Ti(2) 99.2(1) . . . yes Ti(1) O(2) C(8) 139.0(2) . . . yes Ti(2) O(2) C(8) 121.8(2) . . . yes Ti(2) O(3) C(15) 154.3(3) . . . yes Ti(1) O(4) C(29) 167.3(3) . . . yes Ti(1) O(5) Ti(2) 98.6(1) . . . yes Ti(1) O(5) C(36) 132.8(2) . . . yes Ti(2) O(5) C(36) 128.3(2) . . . yes Ti(2) O(6) C(43) 162.6(3) . . . yes C(57) N(1) C(59) 111.0(3) . . . yes C(57) N(1) C(61) 106.2(5) . . . yes C(57) N(1) C(63) 109.7(4) . . . yes C(59) N(1) C(61) 110.5(4) . . . yes C(59) N(1) C(63) 106.9(4) . . . yes C(61) N(1) C(63) 112.5(3) . . . yes O(1) C(1) C(2) 117.5(4) . . . yes O(1) C(1) C(6) 120.7(3) . . . yes C(2) C(1) C(6) 121.9(4) . . . yes C(1) C(2) C(3) 117.9(4) . . . yes C(1) C(2) C(21) 120.4(4) . . . yes C(3) C(2) C(21) 121.7(4) . . . yes C(2) C(3) C(4) 122.9(4) . . . yes C(3) C(4) C(5) 117.3(5) . . . yes C(3) C(4) C(22) 120.8(4) . . . yes C(5) C(4) C(22) 121.8(4) . . . yes C(4) C(5) C(6) 122.6(4) . . . yes C(1) C(6) C(5) 117.4(3) . . . yes C(1) C(6) C(7) 122.6(4) . . . yes C(5) C(6) C(7) 119.9(4) . . . yes C(6) C(7) C(9) 111.4(3) . . . yes O(2) C(8) C(9) 119.4(3) . . . yes O(2) C(8) C(13) 119.8(4) . . . yes C(9) C(8) C(13) 120.7(4) . . . yes C(7) C(9) C(8) 120.9(4) . . . yes C(7) C(9) C(10) 120.2(5) . . . yes C(8) C(9) C(10) 118.9(4) . . . yes C(9) C(10) C(11) 122.1(5) . . . yes C(10) C(11) C(12) 117.4(4) . . . yes C(10) C(11) C(23) 118.9(5) . . . yes C(12) C(11) C(23) 123.7(4) . . . yes C(11) C(12) C(13) 122.7(4) . . . yes C(8) C(13) C(12) 118.1(5) . . . yes C(8) C(13) C(14) 122.2(4) . . . yes C(12) C(13) C(14) 119.6(4) . . . yes C(13) C(14) C(16) 116.2(4) . . . yes O(3) C(15) C(16) 120.4(4) . . . yes O(3) C(15) C(20) 117.7(4) . . . yes C(16) C(15) C(20) 121.9(4) . . . yes C(14) C(16) C(15) 122.0(4) . . . yes C(14) C(16) C(17) 121.1(4) . . . yes C(15) C(16) C(17) 116.8(4) . . . yes C(16) C(17) C(18) 123.7(5) . . . yes C(17) C(18) C(19) 117.6(4) . . . yes C(17) C(18) C(28) 122.0(5) . . . yes C(19) C(18) C(28) 120.4(4) . . . yes C(18) C(19) C(20) 122.2(4) . . . yes C(15) C(20) C(19) 117.7(4) . . . yes C(15) C(20) C(27) 120.3(4) . . . yes C(19) C(20) C(27) 122.0(4) . . . yes C(11) C(23) C(24) 110.3(4) . . . yes C(11) C(23) C(25) 108.6(3) . . . yes C(11) C(23) C(26) 111.3(5) . . . yes C(24) C(23) C(25) 109.7(6) . . . yes C(24) C(23) C(26) 106.9(4) . . . yes C(25) C(23) C(26) 110.1(4) . . . yes O(4) C(29) C(30) 118.3(4) . . . yes O(4) C(29) C(34) 119.6(4) . . . yes C(30) C(29) C(34) 122.1(4) . . . yes C(29) C(30) C(31) 116.5(5) . . . yes C(29) C(30) C(49) 121.8(5) . . . yes C(31) C(30) C(49) 121.6(4) . . . yes C(30) C(31) C(32) 123.0(4) . . . yes C(31) C(32) C(33) 118.2(5) . . . yes C(31) C(32) C(50) 119.9(5) . . . yes C(33) C(32) C(50) 121.9(5) . . . yes C(32) C(33) C(34) 122.1(5) . . . yes C(29) C(34) C(33) 117.8(4) . . . yes C(29) C(34) C(35) 121.6(4) . . . yes C(33) C(34) C(35) 120.4(4) . . . yes C(34) C(35) C(37) 111.6(4) . . . yes O(5) C(36) C(37) 121.5(4) . . . yes O(5) C(36) C(41) 118.5(4) . . . yes C(37) C(36) C(41) 120.0(4) . . . yes C(35) C(37) C(36) 122.4(4) . . . yes C(35) C(37) C(38) 118.1(5) . . . yes C(36) C(37) C(38) 119.4(5) . . . yes C(37) C(38) C(39) 122.2(5) . . . yes C(38) C(39) C(40) 116.7(4) . . . yes C(38) C(39) C(51) 122.6(5) . . . yes C(40) C(39) C(51) 120.6(5) . . . yes C(39) C(40) C(41) 123.0(5) . . . yes C(36) C(41) C(40) 118.6(5) . . . yes C(36) C(41) C(42) 121.7(4) . . . yes C(40) C(41) C(42) 119.4(5) . . . yes C(41) C(42) C(44) 117.2(4) . . . yes O(6) C(43) C(44) 120.5(4) . . . yes O(6) C(43) C(48) 117.3(4) . . . yes C(44) C(43) C(48) 122.2(5) . . . yes C(42) C(44) C(43) 122.9(4) . . . yes C(42) C(44) C(45) 119.1(4) . . . yes C(43) C(44) C(45) 117.9(4) . . . yes C(44) C(45) C(46) 122.1(4) . . . yes C(45) C(46) C(47) 117.9(5) . . . yes C(45) C(46) C(56) 120.6(4) . . . yes C(47) C(46) C(56) 121.4(4) . . . yes C(46) C(47) C(48) 122.3(4) . . . yes C(43) C(48) C(47) 117.5(4) . . . yes C(43) C(48) C(55) 120.5(5) . . . yes C(47) C(48) C(55) 122.1(4) . . . yes C(39) C(51) C(52) 110.1(5) . . . yes C(39) C(51) C(53) 112.6(5) . . . yes C(39) C(51) C(54) 110.5(4) . . . yes C(52) C(51) C(53) 106.1(5) . . . yes C(52) C(51) C(54) 109.1(5) . . . yes C(53) C(51) C(54) 108.3(5) . . . yes N(1) C(57) C(58) 115.7(5) . . . yes N(1) C(59) C(60) 114.6(5) . . . yes N(1) C(61) C(62) 114.7(6) . . . yes N(1) C(63) C(64) 115.7(5) . . . yes Cl(4) C(65) Cl(5) 112.9(7) . . . yes Cl(6) C(66) Cl(7) 113.6(6) . . . yes Cl(8) C(67) Cl(9) 111.7(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ti(1) Ti(2) O(2) C(8) 179.8(4) . . . . yes Ti(1) Ti(2) O(3) C(15) 46.0(8) . . . . yes Ti(1) Ti(2) O(5) C(36) -173.9(5) . . . . yes Ti(1) Ti(2) O(6) C(43) -83.9(9) . . . . yes Ti(1) Cl(2) Ti(2) Cl(3) -127.46(4) . . . . yes Ti(1) Cl(2) Ti(2) O(2) 40.35(7) . . . . yes Ti(1) Cl(2) Ti(2) O(3) 134.2(1) . . . . yes Ti(1) Cl(2) Ti(2) O(5) -38.60(9) . . . . yes Ti(1) Cl(2) Ti(2) O(6) -4.8(4) . . . . yes Ti(1) O(1) C(1) C(2) -100.0(5) . . . . yes Ti(1) O(1) C(1) C(6) 80.8(7) . . . . yes Ti(1) O(2) Ti(2) Cl(2) -52.6(1) . . . . yes Ti(1) O(2) Ti(2) Cl(3) -15.5(4) . . . . yes Ti(1) O(2) Ti(2) O(3) -140.0(2) . . . . yes Ti(1) O(2) Ti(2) O(5) 25.4(1) . . . . yes Ti(1) O(2) Ti(2) O(6) 117.2(1) . . . . yes Ti(1) O(2) C(8) C(9) -79.9(5) . . . . yes Ti(1) O(2) C(8) C(13) 101.8(4) . . . . yes Ti(1) O(4) C(29) C(30) 174(1) . . . . yes Ti(1) O(4) C(29) C(34) -5(1) . . . . yes Ti(1) O(5) Ti(2) Cl(2) 51.0(1) . . . . yes Ti(1) O(5) Ti(2) Cl(3) 141.0(1) . . . . yes Ti(1) O(5) Ti(2) O(2) -25.8(1) . . . . yes Ti(1) O(5) Ti(2) O(3) 27.7(6) . . . . yes Ti(1) O(5) Ti(2) O(6) -121.0(2) . . . . yes Ti(1) O(5) C(36) C(37) -73.2(5) . . . . yes Ti(1) O(5) C(36) C(41) 107.9(4) . . . . yes Ti(2) Ti(1) O(1) C(1) -93.4(5) . . . . yes Ti(2) Ti(1) O(2) C(8) -179.8(5) . . . . yes Ti(2) Ti(1) O(4) C(29) 0(1) . . . . yes Ti(2) Ti(1) O(5) C(36) 173.4(5) . . . . yes Ti(2) Cl(2) Ti(1) Cl(1) -129.00(4) . . . . yes Ti(2) Cl(2) Ti(1) O(1) -35.0(4) . . . . yes Ti(2) Cl(2) Ti(1) O(2) -39.06(9) . . . . yes Ti(2) Cl(2) Ti(1) O(4) 132.0(1) . . . . yes Ti(2) Cl(2) Ti(1) O(5) 39.12(9) . . . . yes Ti(2) O(2) Ti(1) Cl(1) 142.4(1) . . . . yes Ti(2) O(2) Ti(1) Cl(2) 53.7(1) . . . . yes Ti(2) O(2) Ti(1) O(1) -125.2(1) . . . . yes Ti(2) O(2) Ti(1) O(4) 23.1(5) . . . . yes Ti(2) O(2) Ti(1) O(5) -25.9(1) . . . . yes Ti(2) O(2) C(8) C(9) 100.3(4) . . . . yes Ti(2) O(2) C(8) C(13) -77.9(4) . . . . yes Ti(2) O(3) C(15) C(16) -62.5(9) . . . . yes Ti(2) O(3) C(15) C(20) 118.1(6) . . . . yes Ti(2) O(5) Ti(1) Cl(1) -13.0(4) . . . . yes Ti(2) O(5) Ti(1) Cl(2) -51.7(1) . . . . yes Ti(2) O(5) Ti(1) O(1) 114.0(1) . . . . yes Ti(2) O(5) Ti(1) O(2) 25.1(1) . . . . yes Ti(2) O(5) Ti(1) O(4) -141.5(2) . . . . yes Ti(2) O(5) C(36) C(37) 98.5(4) . . . . yes Ti(2) O(5) C(36) C(41) -80.3(5) . . . . yes Ti(2) O(6) C(43) C(44) 48(1) . . . . yes Ti(2) O(6) C(43) C(48) -133.2(7) . . . . yes Cl(1) Ti(1) Ti(2) Cl(2) 63.82(6) . . . . yes Cl(1) Ti(1) Ti(2) Cl(3) 129.05(7) . . . . yes Cl(1) Ti(1) Ti(2) O(2) -44.8(2) . . . . yes Cl(1) Ti(1) Ti(2) O(3) 5.2(2) . . . . yes Cl(1) Ti(1) Ti(2) O(5) 175.1(2) . . . . yes Cl(1) Ti(1) Ti(2) O(6) -117.5(1) . . . . yes Cl(1) Ti(1) O(1) C(1) 30.7(5) . . . . yes Cl(1) Ti(1) O(2) C(8) -37.4(4) . . . . yes Cl(1) Ti(1) O(4) C(29) -136(1) . . . . yes Cl(1) Ti(1) O(5) C(36) 160.5(3) . . . . yes Cl(2) Ti(1) Ti(2) Cl(3) 65.23(6) . . . . yes Cl(2) Ti(1) Ti(2) O(2) -108.6(2) . . . . yes Cl(2) Ti(1) Ti(2) O(3) -58.7(2) . . . . yes Cl(2) Ti(1) Ti(2) O(5) 111.3(2) . . . . yes Cl(2) Ti(1) Ti(2) O(6) 178.7(1) . . . . yes Cl(2) Ti(1) O(1) C(1) -62.8(7) . . . . yes Cl(2) Ti(1) O(2) C(8) -126.1(4) . . . . yes Cl(2) Ti(1) O(4) C(29) -47(1) . . . . yes Cl(2) Ti(1) O(5) C(36) 121.7(4) . . . . yes Cl(2) Ti(2) Ti(1) O(1) 170.9(1) . . . . yes Cl(2) Ti(2) Ti(1) O(2) 108.6(2) . . . . yes Cl(2) Ti(2) Ti(1) O(4) -63.1(1) . . . . yes Cl(2) Ti(2) Ti(1) O(5) -111.3(2) . . . . yes Cl(2) Ti(2) O(2) C(8) 127.3(3) . . . . yes Cl(2) Ti(2) O(3) C(15) 2.6(7) . . . . yes Cl(2) Ti(2) O(5) C(36) -122.8(4) . . . . yes Cl(2) Ti(2) O(6) C(43) -79(1) . . . . yes Cl(3) Ti(2) Ti(1) O(1) -123.8(1) . . . . yes Cl(3) Ti(2) Ti(1) O(2) 173.9(2) . . . . yes Cl(3) Ti(2) Ti(1) O(4) 2.1(2) . . . . yes Cl(3) Ti(2) Ti(1) O(5) -46.1(2) . . . . yes Cl(3) Ti(2) O(2) C(8) 164.4(3) . . . . yes Cl(3) Ti(2) O(3) C(15) -86.8(7) . . . . yes Cl(3) Ti(2) O(5) C(36) -32.9(4) . . . . yes Cl(3) Ti(2) O(6) C(43) 42.0(9) . . . . yes O(1) Ti(1) Ti(2) O(2) 62.3(2) . . . . yes O(1) Ti(1) Ti(2) O(3) 112.3(2) . . . . yes O(1) Ti(1) Ti(2) O(5) -77.8(2) . . . . yes O(1) Ti(1) Ti(2) O(6) -10.3(2) . . . . yes O(1) Ti(1) O(2) C(8) 55.0(5) . . . . yes O(1) Ti(1) O(4) C(29) 128(1) . . . . yes O(1) Ti(1) O(5) C(36) -72.5(4) . . . . yes O(1) C(1) C(2) C(3) -178.4(4) . . . . yes O(1) C(1) C(2) C(21) 0.1(6) . . . . yes O(1) C(1) C(6) C(5) 178.0(4) . . . . yes O(1) C(1) C(6) C(7) -3.0(6) . . . . yes O(2) Ti(1) Ti(2) O(3) 50.0(2) . . . . yes O(2) Ti(1) Ti(2) O(5) -140.1(2) . . . . yes O(2) Ti(1) Ti(2) O(6) -72.6(2) . . . . yes O(2) Ti(1) O(1) C(1) -58.9(5) . . . . yes O(2) Ti(1) O(4) C(29) -18(1) . . . . yes O(2) Ti(1) O(5) C(36) -161.4(5) . . . . yes O(2) Ti(2) Ti(1) O(4) -171.7(2) . . . . yes O(2) Ti(2) Ti(1) O(5) 140.1(2) . . . . yes O(2) Ti(2) O(3) C(15) 76.2(7) . . . . yes O(2) Ti(2) O(5) C(36) 160.3(4) . . . . yes O(2) Ti(2) O(6) C(43) -122.9(9) . . . . yes O(2) C(8) C(9) C(7) 7.6(5) . . . . yes O(2) C(8) C(9) C(10) -174.5(3) . . . . yes O(2) C(8) C(13) C(12) 175.7(3) . . . . yes O(2) C(8) C(13) C(14) -7.9(5) . . . . yes O(3) Ti(2) Ti(1) O(4) -121.8(2) . . . . yes O(3) Ti(2) Ti(1) O(5) -170.0(2) . . . . yes O(3) Ti(2) O(2) C(8) 39.9(3) . . . . yes O(3) Ti(2) O(5) C(36) -146.2(5) . . . . yes O(3) Ti(2) O(6) C(43) 142.4(9) . . . . yes O(3) C(15) C(16) C(14) -0.5(7) . . . . yes O(3) C(15) C(16) C(17) 178.5(4) . . . . yes O(3) C(15) C(20) C(19) -178.4(4) . . . . yes O(3) C(15) C(20) C(27) 2.3(7) . . . . yes O(4) Ti(1) Ti(2) O(5) 48.2(2) . . . . yes O(4) Ti(1) Ti(2) O(6) 115.6(2) . . . . yes O(4) Ti(1) O(1) C(1) 130.6(5) . . . . yes O(4) Ti(1) O(2) C(8) -156.7(5) . . . . yes O(4) Ti(1) O(5) C(36) 31.9(4) . . . . yes O(4) C(29) C(30) C(31) 174.3(5) . . . . yes O(4) C(29) C(30) C(49) -3.0(8) . . . . yes O(4) C(29) C(34) C(33) -173.9(5) . . . . yes O(4) C(29) C(34) C(35) 3.0(8) . . . . yes O(5) Ti(1) Ti(2) O(6) 67.4(2) . . . . yes O(5) Ti(1) O(1) C(1) -134.0(5) . . . . yes O(5) Ti(1) O(2) C(8) 154.3(5) . . . . yes O(5) Ti(1) O(4) C(29) 28(1) . . . . yes O(5) Ti(2) O(2) C(8) -154.8(4) . . . . yes O(5) Ti(2) O(3) C(15) 25(1) . . . . yes O(5) Ti(2) O(6) C(43) -47.2(9) . . . . yes O(5) C(36) C(37) C(35) 5.4(5) . . . . yes O(5) C(36) C(37) C(38) -178.4(3) . . . . yes O(5) C(36) C(41) C(40) 179.5(3) . . . . yes O(5) C(36) C(41) C(42) -6.1(5) . . . . yes O(6) Ti(2) O(2) C(8) -63.0(3) . . . . yes O(6) Ti(2) O(3) C(15) 172.9(7) . . . . yes O(6) Ti(2) O(5) C(36) 65.2(4) . . . . yes O(6) C(43) C(44) C(42) 7.5(7) . . . . yes O(6) C(43) C(44) C(45) -177.3(5) . . . . yes O(6) C(43) C(48) C(47) 177.0(5) . . . . yes O(6) C(43) C(48) C(55) -5.1(7) . . . . yes C(1) C(2) C(3) C(4) 0.2(7) . . . . yes C(1) C(6) C(5) C(4) 0.5(6) . . . . yes C(1) C(6) C(7) C(9) -90.8(5) . . . . yes C(2) C(1) C(6) C(5) -1.1(6) . . . . yes C(2) C(1) C(6) C(7) 177.9(4) . . . . yes C(2) C(3) C(4) C(5) -0.8(7) . . . . yes C(2) C(3) C(4) C(22) -179.2(4) . . . . yes C(3) C(2) C(1) C(6) 0.8(6) . . . . yes C(3) C(4) C(5) C(6) 0.4(7) . . . . yes C(4) C(3) C(2) C(21) -178.3(4) . . . . yes C(4) C(5) C(6) C(7) -178.5(4) . . . . yes C(5) C(6) C(7) C(9) 88.2(5) . . . . yes C(6) C(1) C(2) C(21) 179.3(4) . . . . yes C(6) C(5) C(4) C(22) 178.9(4) . . . . yes C(6) C(7) C(9) C(8) 89.2(5) . . . . yes C(6) C(7) C(9) C(10) -88.7(5) . . . . yes C(7) C(9) C(8) C(13) -174.2(3) . . . . yes C(7) C(9) C(10) C(11) 175.4(4) . . . . yes C(8) C(9) C(10) C(11) -2.6(6) . . . . yes C(8) C(13) C(12) C(11) 0.2(6) . . . . yes C(8) C(13) C(14) C(16) 105.0(4) . . . . yes C(9) C(8) C(13) C(12) -2.6(6) . . . . yes C(9) C(8) C(13) C(14) 173.9(4) . . . . yes C(9) C(10) C(11) C(12) 0.3(6) . . . . yes C(9) C(10) C(11) C(23) -177.6(4) . . . . yes C(10) C(9) C(8) C(13) 3.8(6) . . . . yes C(10) C(11) C(12) C(13) 1.0(6) . . . . yes C(10) C(11) C(23) C(24) -57.0(6) . . . . yes C(10) C(11) C(23) C(25) 63.2(6) . . . . yes C(10) C(11) C(23) C(26) -175.4(4) . . . . yes C(11) C(12) C(13) C(14) -176.4(4) . . . . yes C(12) C(11) C(23) C(24) 125.2(5) . . . . yes C(12) C(11) C(23) C(25) -114.5(5) . . . . yes C(12) C(11) C(23) C(26) 6.8(6) . . . . yes C(12) C(13) C(14) C(16) -78.5(5) . . . . yes C(13) C(12) C(11) C(23) 178.7(4) . . . . yes C(13) C(14) C(16) C(15) -57.0(6) . . . . yes C(13) C(14) C(16) C(17) 124.0(5) . . . . yes C(14) C(16) C(15) C(20) 178.9(5) . . . . yes C(14) C(16) C(17) C(18) 179.5(5) . . . . yes C(15) C(16) C(17) C(18) 0.5(8) . . . . yes C(15) C(20) C(19) C(18) -0.7(8) . . . . yes C(16) C(15) C(20) C(19) 2.1(8) . . . . yes C(16) C(15) C(20) C(27) -177.1(5) . . . . yes C(16) C(17) C(18) C(19) 0.9(8) . . . . yes C(16) C(17) C(18) C(28) -179.6(5) . . . . yes C(17) C(16) C(15) C(20) -2.0(7) . . . . yes C(17) C(18) C(19) C(20) -0.8(8) . . . . yes C(18) C(19) C(20) C(27) 178.6(5) . . . . yes C(20) C(19) C(18) C(28) 179.6(5) . . . . yes C(29) C(30) C(31) C(32) 1.4(9) . . . . yes C(29) C(34) C(33) C(32) -2.1(9) . . . . yes C(29) C(34) C(35) C(37) -80.1(6) . . . . yes C(30) C(29) C(34) C(33) 5.5(8) . . . . yes C(30) C(29) C(34) C(35) -177.6(5) . . . . yes C(30) C(31) C(32) C(33) 1.8(10) . . . . yes C(30) C(31) C(32) C(50) -177.0(6) . . . . yes C(31) C(30) C(29) C(34) -5.2(8) . . . . yes C(31) C(32) C(33) C(34) -1.5(9) . . . . yes C(32) C(31) C(30) C(49) 178.6(6) . . . . yes C(32) C(33) C(34) C(35) -179.0(6) . . . . yes C(33) C(34) C(35) C(37) 96.7(6) . . . . yes C(34) C(29) C(30) C(49) 177.6(5) . . . . yes C(34) C(33) C(32) C(50) 177.3(6) . . . . yes C(34) C(35) C(37) C(36) 98.1(4) . . . . yes C(34) C(35) C(37) C(38) -78.1(5) . . . . yes C(35) C(37) C(36) C(41) -175.8(3) . . . . yes C(35) C(37) C(38) C(39) 175.7(4) . . . . yes C(36) C(37) C(38) C(39) -0.6(6) . . . . yes C(36) C(41) C(40) C(39) -1.6(6) . . . . yes C(36) C(41) C(42) C(44) 101.2(5) . . . . yes C(37) C(36) C(41) C(40) 0.6(5) . . . . yes C(37) C(36) C(41) C(42) 175.1(3) . . . . yes C(37) C(38) C(39) C(40) -0.2(6) . . . . yes C(37) C(38) C(39) C(51) -177.9(4) . . . . yes C(38) C(37) C(36) C(41) 0.4(5) . . . . yes C(38) C(39) C(40) C(41) 1.4(6) . . . . yes C(38) C(39) C(51) C(52) 116.0(6) . . . . yes C(38) C(39) C(51) C(53) -2.2(6) . . . . yes C(38) C(39) C(51) C(54) -123.4(5) . . . . yes C(39) C(40) C(41) C(42) -176.1(4) . . . . yes C(40) C(39) C(51) C(52) -61.6(6) . . . . yes C(40) C(39) C(51) C(53) -179.8(4) . . . . yes C(40) C(39) C(51) C(54) 59.0(6) . . . . yes C(40) C(41) C(42) C(44) -84.5(5) . . . . yes C(41) C(40) C(39) C(51) 179.1(4) . . . . yes C(41) C(42) C(44) C(43) -81.7(6) . . . . yes C(41) C(42) C(44) C(45) 103.1(6) . . . . yes C(42) C(44) C(43) C(48) -170.8(5) . . . . yes C(42) C(44) C(45) C(46) 174.1(5) . . . . yes C(43) C(44) C(45) C(46) -1.3(8) . . . . yes C(43) C(48) C(47) C(46) 1.9(9) . . . . yes C(44) C(43) C(48) C(47) -4.6(8) . . . . yes C(44) C(43) C(48) C(55) 173.3(5) . . . . yes C(44) C(45) C(46) C(47) -1.3(9) . . . . yes C(44) C(45) C(46) C(56) -178.8(6) . . . . yes C(45) C(44) C(43) C(48) 4.4(7) . . . . yes C(45) C(46) C(47) C(48) 1.0(9) . . . . yes C(46) C(47) C(48) C(55) -176.0(6) . . . . yes C(48) C(47) C(46) C(56) 178.5(6) . . . . yes C(57) N(1) C(59) C(60) 57.5(5) . . . . yes C(57) N(1) C(61) C(62) 177.0(4) . . . . yes C(57) N(1) C(63) C(64) -67.0(5) . . . . yes C(58) C(57) N(1) C(59) 49.2(6) . . . . yes C(58) C(57) N(1) C(61) 169.4(4) . . . . yes C(58) C(57) N(1) C(63) -68.7(5) . . . . yes C(59) N(1) C(61) C(62) -62.5(6) . . . . yes C(59) N(1) C(63) C(64) 172.5(3) . . . . yes C(60) C(59) N(1) C(61) -60.0(5) . . . . yes C(60) C(59) N(1) C(63) 177.2(3) . . . . yes C(61) N(1) C(63) C(64) 51.0(5) . . . . yes C(62) C(61) N(1) C(63) 57.0(6) . . . . yes C(62) C(61) N(1) C(63) 57.0(6) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ti(1) Ti(2) 3.104(1) . . ? Ti(1) Cl(2) 2.635(1) . . ? Ti(2) Cl(2) 2.678(2) . . ? Cl(1) C(57) 3.460(7) . 1_655 ? Cl(3) C(59) 3.460(7) . 2_676 ? Cl(8) C(4) 3.599(5) . 1_455 ? Cl(9) C(26) 3.411(7) . 2_666 ? O(1) C(3) 3.505(5) . 2_775 ? C(1) C(21) 3.432(7) . 2_775 ? C(1) C(2) 3.541(5) . 2_775 ? C(2) C(2) 3.412(8) . 2_775 ? C(6) C(21) 3.504(6) . 2_775 ? C(19) C(66) 3.58(2) . 2_666 ? C(22) C(50) 3.485(7) . 1_545 ? C(22) C(29) 3.488(7) . 2_775 ? C(29) C(64) 3.451(8) . 1_655 ? C(30) C(64) 3.503(7) . 1_655 ? C(58) C(64) 3.592(8) . 2_576 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[Ti(Me-L)(DME)]2 _database_code_CSD 176066 _audit_creation_date 'Wed Apr 3 14:04:14 2002' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C64 H82 O10 Ti2 ' _chemical_formula_moiety 'C64 H82 O10 Ti2 ' _chemical_formula_weight 1107.15 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 23.319(9) _cell_length_b 15.250(6) _cell_length_c 16.708(7) _cell_angle_alpha 90 _cell_angle_beta 95.167(6) _cell_angle_gamma 90 _cell_volume 5917(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8741 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 173.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.070 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.327 _exptl_absorpt_correction_type 'REQABA Empirical Absorption Correction' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.977 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 23265 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9940 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9940 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7000 _reflns_number_gt 4792 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1380 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6744 _refine_ls_number_parameters 384 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.000Fo^2^ + 1.000\s^2^(Fo)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.53 _refine_diff_density_min -0.47 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ti' 'Ti' 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti(1) Ti 0.27312(2) 0.31781(3) -0.05884(2) 0.0182(1) Uani 1.00 d . . . O(1) O 0.27925(7) 0.4095(1) 0.01947(9) 0.0228(4) Uani 1.00 d . . . O(2) O 0.30323(6) 0.2295(1) 0.02945(9) 0.0190(4) Uani 1.00 d . . . O(3) O 0.28420(7) 0.2331(1) -0.1396(1) 0.0245(4) Uani 1.00 d . . . O(4) O 0.35246(7) 0.3842(1) -0.1080(1) 0.0296(5) Uani 1.00 d . . . O(5) O 0.24034(7) 0.4137(1) -0.1491(1) 0.0264(4) Uani 1.00 d . . . C(1) C 0.31219(9) 0.4667(2) 0.0637(1) 0.0198(6) Uani 1.00 d . . . C(2) C 0.3045(1) 0.5576(2) 0.0510(1) 0.0241(6) Uani 1.00 d . . . C(3) C 0.3432(1) 0.6156(2) 0.0907(2) 0.0280(7) Uani 1.00 d . . . C(4) C 0.3883(1) 0.5883(2) 0.1451(2) 0.0309(7) Uani 1.00 d . . . C(5) C 0.3914(1) 0.4988(2) 0.1622(2) 0.0261(6) Uani 1.00 d . . . C(6) C 0.3539(1) 0.4376(2) 0.1251(1) 0.0215(6) Uani 1.00 d . . . C(7) C 0.3554(1) 0.3430(2) 0.1515(1) 0.0218(6) Uani 1.00 d . . . C(8) C 0.36161(9) 0.2257(2) 0.0448(1) 0.0187(5) Uani 1.00 d . . . C(9) C 0.3896(1) 0.2813(2) 0.1025(1) 0.0199(5) Uani 1.00 d . . . C(10) C 0.4494(1) 0.2793(2) 0.1141(1) 0.0225(6) Uani 1.00 d . . . C(11) C 0.4830(1) 0.2246(2) 0.0702(1) 0.0227(6) Uani 1.00 d . . . C(12) C 0.4536(1) 0.1686(2) 0.0143(1) 0.0239(6) Uani 1.00 d . . . C(13) C 0.3934(1) 0.1679(2) 0.0006(1) 0.0207(6) Uani 1.00 d . . . C(14) C 0.3624(1) 0.1048(2) -0.0589(1) 0.0231(6) Uani 1.00 d . . . C(15) C 0.3181(1) 0.1855(2) -0.1836(1) 0.0205(6) Uani 1.00 d . . . C(16) C 0.3605(1) 0.1286(2) -0.1478(1) 0.0219(6) Uani 1.00 d . . . C(17) C 0.3978(1) 0.0865(2) -0.1963(2) 0.0256(6) Uani 1.00 d . . . C(18) C 0.3930(1) 0.0963(2) -0.2795(2) 0.0267(6) Uani 1.00 d . . . C(19) C 0.3476(1) 0.1453(2) -0.3144(2) 0.0282(6) Uani 1.00 d . . . C(20) C 0.3095(1) 0.1897(2) -0.2687(1) 0.0233(6) Uani 1.00 d . . . C(21) C 0.2536(1) 0.5900(2) -0.0026(2) 0.0350(7) Uani 1.00 d . . . C(22) C 0.4305(1) 0.6526(2) 0.1869(2) 0.0526(10) Uani 1.00 d . . . C(23) C 0.5488(1) 0.2250(2) 0.0870(2) 0.0317(7) Uani 1.00 d . . . C(24) C 0.5784(1) 0.1724(3) 0.0255(2) 0.061(1) Uani 1.00 d . . . C(25) C 0.5720(1) 0.3191(2) 0.0852(3) 0.065(1) Uani 1.00 d . . . C(26) C 0.5652(1) 0.1861(3) 0.1706(2) 0.063(1) Uani 1.00 d . . . C(27) C 0.2581(1) 0.2381(2) -0.3079(2) 0.0344(7) Uani 1.00 d . . . C(28) C 0.4348(1) 0.0504(2) -0.3300(2) 0.0417(8) Uani 1.00 d . . . C(29) C 0.4110(1) 0.3854(2) -0.0726(2) 0.0439(8) Uani 1.00 d . . . C(30) C 0.3360(1) 0.4680(2) -0.1414(2) 0.0329(7) Uani 1.00 d . . . C(31) C 0.2815(1) 0.4576(2) -0.1941(2) 0.0329(7) Uani 1.00 d . . . C(32) C 0.1850(1) 0.4046(2) -0.1934(2) 0.0367(8) Uani 1.00 d . . . H(1) H 0.3387(1) 0.6778(2) 0.0798(2) 0.033(1) Uiso 1.00 calc . . . H(2) H 0.4214(1) 0.4785(2) 0.2018(2) 0.031(1) Uiso 1.00 calc . . . H(3) H 0.3719(1) 0.3407(2) 0.2069(1) 0.025(1) Uiso 1.00 calc . . . H(4) H 0.3160(1) 0.3219(2) 0.1484(1) 0.025(1) Uiso 1.00 calc . . . H(5) H 0.4687(1) 0.3175(2) 0.1545(1) 0.026(1) Uiso 1.00 calc . . . H(6) H 0.4757(1) 0.1288(2) -0.0162(1) 0.028(1) Uiso 1.00 calc . . . H(7) H 0.3815(1) 0.0484(2) -0.0519(1) 0.028(1) Uiso 1.00 calc . . . H(8) H 0.3230(1) 0.0996(2) -0.0454(1) 0.028(1) Uiso 1.00 calc . . . H(9) H 0.4279(1) 0.0491(2) -0.1712(2) 0.030(1) Uiso 1.00 calc . . . H(10) H 0.3419(1) 0.1493(2) -0.3725(2) 0.033(1) Uiso 1.00 calc . . . H(11) H 0.2293(1) 0.6257(2) 0.0285(2) 0.043(1) Uiso 1.00 calc . . . H(12) H 0.2671(1) 0.6249(2) -0.0457(2) 0.043(1) Uiso 1.00 calc . . . H(13) H 0.2317(1) 0.5404(2) -0.0252(2) 0.042(1) Uiso 1.00 calc . . . H(14) H 0.4585(1) 0.6212(2) 0.2225(2) 0.061(1) Uiso 1.00 calc . . . H(15) H 0.4500(1) 0.6840(2) 0.1468(2) 0.061(1) Uiso 1.00 calc . . . H(16) H 0.4099(1) 0.6941(2) 0.2179(2) 0.061(1) Uiso 1.00 calc . . . H(17) H 0.5651(1) 0.1121(3) 0.0255(2) 0.067(2) Uiso 1.00 calc . . . H(18) H 0.5695(1) 0.1976(3) -0.0275(2) 0.067(2) Uiso 1.00 calc . . . H(19) H 0.6197(1) 0.1739(3) 0.0393(2) 0.067(2) Uiso 1.00 calc . . . H(20) H 0.6133(1) 0.3191(2) 0.0987(3) 0.072(2) Uiso 1.00 calc . . . H(21) H 0.5634(1) 0.3429(2) 0.0316(3) 0.073(2) Uiso 1.00 calc . . . H(22) H 0.5537(1) 0.3550(2) 0.1235(3) 0.072(2) Uiso 1.00 calc . . . H(23) H 0.5464(1) 0.2191(3) 0.2105(2) 0.070(2) Uiso 1.00 calc . . . H(24) H 0.5526(1) 0.1255(3) 0.1710(2) 0.070(2) Uiso 1.00 calc . . . H(25) H 0.6066(1) 0.1888(3) 0.1831(2) 0.070(2) Uiso 1.00 calc . . . H(26) H 0.2367(1) 0.2640(2) -0.2666(2) 0.041(1) Uiso 1.00 calc . . . H(27) H 0.2707(1) 0.2839(2) -0.3425(2) 0.041(1) Uiso 1.00 calc . . . H(28) H 0.2336(1) 0.1972(2) -0.3395(2) 0.041(1) Uiso 1.00 calc . . . H(29) H 0.4142(1) 0.0083(2) -0.3654(2) 0.050(1) Uiso 1.00 calc . . . H(30) H 0.4533(1) 0.0934(2) -0.3618(2) 0.050(1) Uiso 1.00 calc . . . H(31) H 0.4637(1) 0.0202(2) -0.2948(2) 0.050(1) Uiso 1.00 calc . . . H(32) H 0.4209(1) 0.3279(2) -0.0507(2) 0.050(1) Uiso 1.00 calc . . . H(33) H 0.4367(1) 0.4003(2) -0.1130(2) 0.050(1) Uiso 1.00 calc . . . H(34) H 0.4148(1) 0.4286(2) -0.0298(2) 0.051(1) Uiso 1.00 calc . . . H(35) H 0.3299(1) 0.5087(2) -0.0983(2) 0.039(1) Uiso 1.00 calc . . . H(36) H 0.3661(1) 0.4903(2) -0.1723(2) 0.039(1) Uiso 1.00 calc . . . H(37) H 0.2887(1) 0.4227(2) -0.2407(2) 0.038(1) Uiso 1.00 calc . . . H(38) H 0.2665(1) 0.5145(2) -0.2115(2) 0.038(1) Uiso 1.00 calc . . . H(39) H 0.1696(1) 0.4621(2) -0.2078(2) 0.044(1) Uiso 1.00 calc . . . H(40) H 0.1886(1) 0.3706(2) -0.2417(2) 0.044(1) Uiso 1.00 calc . . . H(41) H 0.1592(1) 0.3748(2) -0.1600(2) 0.044(1) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.0178(2) 0.0212(2) 0.0149(2) 0.0019(2) -0.0012(1) 0.0001(2) O(1) 0.0248(9) 0.0235(9) 0.0197(8) 0.0018(7) -0.0043(7) -0.0004(7) O(2) 0.0177(8) 0.0226(9) 0.0162(7) 0.0025(6) -0.0009(6) 0.0014(6) O(3) 0.0235(9) 0.0296(9) 0.0192(8) 0.0039(7) 0.0016(7) -0.0032(7) O(4) 0.0259(9) 0.0321(10) 0.0305(10) 0.0001(8) 0.0015(7) 0.0069(8) O(5) 0.0255(9) 0.0295(10) 0.0238(9) -0.0001(7) -0.0039(7) 0.0070(7) C(1) 0.018(1) 0.024(1) 0.016(1) 0.0026(9) 0.0008(9) -0.0029(9) C(2) 0.025(1) 0.026(1) 0.020(1) 0.0028(10) 0.0011(10) -0.0002(10) C(3) 0.031(1) 0.023(1) 0.030(1) 0.000(1) 0.004(1) -0.004(1) C(4) 0.024(1) 0.032(1) 0.035(1) -0.001(1) 0.000(1) -0.009(1) C(5) 0.021(1) 0.033(1) 0.023(1) 0.005(1) -0.0011(10) -0.006(1) C(6) 0.019(1) 0.028(1) 0.015(1) 0.0057(9) 0.0043(9) -0.0038(9) C(7) 0.019(1) 0.030(1) 0.013(1) 0.0032(9) -0.0019(9) 0.0006(9) C(8) 0.018(1) 0.022(1) 0.015(1) 0.0030(9) 0.0006(9) 0.0033(9) C(9) 0.021(1) 0.023(1) 0.014(1) 0.0047(9) -0.0005(9) 0.0018(9) C(10) 0.022(1) 0.026(1) 0.019(1) 0.0031(10) -0.0032(9) -0.0010(10) C(11) 0.019(1) 0.027(1) 0.021(1) 0.0051(10) -0.0011(9) 0.0017(10) C(12) 0.022(1) 0.029(1) 0.020(1) 0.0064(10) 0.0001(9) -0.0016(10) C(13) 0.023(1) 0.022(1) 0.017(1) 0.0028(9) -0.0013(9) 0.0003(9) C(14) 0.024(1) 0.023(1) 0.022(1) 0.0043(10) 0.0012(9) -0.0026(10) C(15) 0.019(1) 0.022(1) 0.020(1) -0.0044(9) 0.0035(9) -0.0057(9) C(16) 0.022(1) 0.024(1) 0.020(1) -0.0050(10) 0.0006(9) -0.0041(9) C(17) 0.020(1) 0.027(1) 0.029(1) 0.000(1) 0.0011(10) -0.0041(10) C(18) 0.025(1) 0.029(1) 0.026(1) -0.003(1) 0.007(1) -0.006(1) C(19) 0.033(1) 0.029(1) 0.021(1) -0.004(1) 0.006(1) -0.004(1) C(20) 0.027(1) 0.023(1) 0.020(1) -0.0037(10) -0.0002(9) -0.0022(10) C(21) 0.041(2) 0.028(1) 0.035(1) 0.007(1) -0.007(1) 0.001(1) C(22) 0.040(2) 0.040(2) 0.071(2) -0.003(2) -0.017(2) -0.015(1) C(23) 0.019(1) 0.041(2) 0.031(1) 0.005(1) -0.002(1) -0.005(1) C(24) 0.025(2) 0.086(3) 0.057(2) 0.009(2) 0.001(1) -0.025(2) C(25) 0.032(2) 0.059(2) 0.091(3) -0.010(2) 0.012(2) -0.013(2) C(26) 0.032(2) 0.092(3) 0.049(2) 0.016(2) -0.011(1) 0.002(2) C(27) 0.041(2) 0.038(2) 0.020(1) 0.004(1) 0.002(1) -0.003(1) C(28) 0.039(2) 0.051(2) 0.033(1) 0.010(1) 0.015(1) -0.006(1) C(29) 0.026(1) 0.057(2) 0.042(2) -0.004(2) 0.002(1) 0.013(1) C(30) 0.039(1) 0.031(1) 0.028(1) -0.006(1) 0.005(1) 0.005(1) C(31) 0.043(2) 0.031(1) 0.021(1) -0.002(1) 0.003(1) 0.007(1) C(32) 0.031(1) 0.041(2) 0.038(2) 0.005(1) -0.008(1) 0.011(1) #------------------------------------------------------------------------------ _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti(1) Ti(1) 3.1125(9) . 4_555 yes Ti(1) O(1) 1.912(2) . . yes Ti(1) O(2) 2.072(2) . . yes Ti(1) O(2) 2.022(2) . 4_555 yes Ti(1) O(3) 1.902(2) . . yes Ti(1) O(4) 2.323(2) . . yes Ti(1) O(5) 2.188(2) . . yes O(1) C(1) 1.339(3) . . yes O(2) C(8) 1.364(3) . . yes O(3) C(15) 1.342(3) . . yes O(4) C(29) 1.438(3) . . yes O(4) C(30) 1.433(3) . . yes O(5) C(31) 1.437(3) . . yes O(5) C(32) 1.436(3) . . yes C(1) C(2) 1.412(3) . . yes C(1) C(6) 1.420(3) . . yes C(2) C(3) 1.390(3) . . yes C(2) C(21) 1.503(4) . . yes C(3) C(4) 1.390(4) . . yes C(4) C(5) 1.394(4) . . yes C(4) C(22) 1.515(4) . . yes C(5) C(6) 1.386(3) . . yes C(6) C(7) 1.509(3) . . yes C(7) C(9) 1.521(3) . . yes C(8) C(9) 1.401(3) . . yes C(8) C(13) 1.403(3) . . yes C(9) C(10) 1.391(3) . . yes C(10) C(11) 1.396(4) . . yes C(11) C(12) 1.397(3) . . yes C(11) C(23) 1.536(3) . . yes C(12) C(13) 1.401(3) . . yes C(13) C(14) 1.518(3) . . yes C(14) C(16) 1.527(3) . . yes C(15) C(16) 1.406(3) . . yes C(15) C(20) 1.420(3) . . yes C(16) C(17) 1.397(4) . . yes C(17) C(18) 1.392(4) . . yes C(18) C(19) 1.381(4) . . yes C(18) C(28) 1.517(4) . . yes C(19) C(20) 1.396(4) . . yes C(20) C(27) 1.506(4) . . yes C(23) C(24) 1.518(5) . . yes C(23) C(25) 1.535(5) . . yes C(23) C(26) 1.532(4) . . yes C(30) C(31) 1.489(4) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ti(1) Ti(1) O(1) 93.59(5) 4_555 . . yes Ti(1) Ti(1) O(2) 39.93(4) 4_555 . . yes Ti(1) Ti(1) O(2) 41.13(4) 4_555 . 4_555 yes Ti(1) Ti(1) O(3) 94.22(6) 4_555 . . yes Ti(1) Ti(1) O(4) 147.70(5) 4_555 . . yes Ti(1) Ti(1) O(5) 139.45(5) 4_555 . . yes O(1) Ti(1) O(2) 89.34(6) . . . yes O(1) Ti(1) O(2) 96.21(7) . . 4_555 yes O(1) Ti(1) O(3) 167.33(8) . . . yes O(1) Ti(1) O(4) 84.84(7) . . . yes O(1) Ti(1) O(5) 89.01(7) . . . yes O(2) Ti(1) O(2) 81.06(6) . . 4_555 yes O(2) Ti(1) O(3) 90.26(7) . . . yes O(2) Ti(1) O(4) 107.78(6) . . . yes O(2) Ti(1) O(5) 178.18(7) . . . yes O(2) Ti(1) O(3) 96.23(7) 4_555 . . yes O(2) Ti(1) O(4) 171.13(6) 4_555 . . yes O(2) Ti(1) O(5) 98.35(6) 4_555 . . yes O(3) Ti(1) O(4) 83.24(7) . . . yes O(3) Ti(1) O(5) 91.52(7) . . . yes O(4) Ti(1) O(5) 72.84(6) . . . yes Ti(1) O(1) C(1) 149.1(2) . . . yes Ti(1) O(2) Ti(1) 98.94(6) . . 4_555 yes Ti(1) O(2) C(8) 115.5(1) . . . yes Ti(1) O(2) C(8) 145.6(1) 4_555 . . yes Ti(1) O(3) C(15) 151.8(1) . . . yes Ti(1) O(4) C(29) 128.0(2) . . . yes Ti(1) O(4) C(30) 109.5(1) . . . yes C(29) O(4) C(30) 111.1(2) . . . yes Ti(1) O(5) C(31) 117.6(1) . . . yes Ti(1) O(5) C(32) 122.2(2) . . . yes C(31) O(5) C(32) 112.7(2) . . . yes O(1) C(1) C(2) 119.8(2) . . . yes O(1) C(1) C(6) 121.1(2) . . . yes C(2) C(1) C(6) 119.0(2) . . . yes C(1) C(2) C(3) 119.0(2) . . . yes C(1) C(2) C(21) 119.7(2) . . . yes C(3) C(2) C(21) 121.3(2) . . . yes C(2) C(3) C(4) 122.8(2) . . . yes C(3) C(4) C(5) 116.8(2) . . . yes C(3) C(4) C(22) 121.9(3) . . . yes C(5) C(4) C(22) 121.3(2) . . . yes C(4) C(5) C(6) 123.2(2) . . . yes C(1) C(6) C(5) 118.4(2) . . . yes C(1) C(6) C(7) 120.4(2) . . . yes C(5) C(6) C(7) 121.1(2) . . . yes C(6) C(7) C(9) 115.6(2) . . . yes O(2) C(8) C(9) 119.9(2) . . . yes O(2) C(8) C(13) 119.6(2) . . . yes C(9) C(8) C(13) 120.4(2) . . . yes C(7) C(9) C(8) 120.7(2) . . . yes C(7) C(9) C(10) 120.4(2) . . . yes C(8) C(9) C(10) 118.9(2) . . . yes C(9) C(10) C(11) 122.7(2) . . . yes C(10) C(11) C(12) 116.9(2) . . . yes C(10) C(11) C(23) 119.9(2) . . . yes C(12) C(11) C(23) 123.2(2) . . . yes C(11) C(12) C(13) 122.5(2) . . . yes C(8) C(13) C(12) 118.5(2) . . . yes C(8) C(13) C(14) 120.0(2) . . . yes C(12) C(13) C(14) 121.5(2) . . . yes C(13) C(14) C(16) 117.2(2) . . . yes O(3) C(15) C(16) 121.8(2) . . . yes O(3) C(15) C(20) 119.2(2) . . . yes C(16) C(15) C(20) 119.0(2) . . . yes C(14) C(16) C(15) 121.2(2) . . . yes C(14) C(16) C(17) 119.3(2) . . . yes C(15) C(16) C(17) 119.2(2) . . . yes C(16) C(17) C(18) 122.0(2) . . . yes C(17) C(18) C(19) 118.0(2) . . . yes C(17) C(18) C(28) 120.5(2) . . . yes C(19) C(18) C(28) 121.4(2) . . . yes C(18) C(19) C(20) 122.2(2) . . . yes C(15) C(20) C(19) 119.0(2) . . . yes C(15) C(20) C(27) 119.5(2) . . . yes C(19) C(20) C(27) 121.4(2) . . . yes C(11) C(23) C(24) 112.4(2) . . . yes C(11) C(23) C(25) 110.3(2) . . . yes C(11) C(23) C(26) 109.2(2) . . . yes C(24) C(23) C(25) 107.4(3) . . . yes C(24) C(23) C(26) 108.8(3) . . . yes C(25) C(23) C(26) 108.7(3) . . . yes O(4) C(30) C(31) 108.6(2) . . . yes O(5) C(31) C(30) 108.4(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ti(1) Ti(1) O(1) C(1) -118.4(3) . 4_555 4_555 4_555 yes Ti(1) Ti(1) O(2) C(8) 179.7(3) . 4_555 . . yes Ti(1) Ti(1) O(2) C(8) 179.8(2) . 4_555 4_555 4_555 yes Ti(1) Ti(1) O(3) C(15) 112.0(3) . 4_555 4_555 4_555 yes Ti(1) Ti(1) O(4) C(29) 16.7(3) . 4_555 4_555 4_555 yes Ti(1) Ti(1) O(4) C(30) 156.4(1) . 4_555 4_555 4_555 yes Ti(1) Ti(1) O(5) C(31) 174.8(1) . 4_555 4_555 4_555 yes Ti(1) Ti(1) O(5) C(32) 27.1(2) . 4_555 4_555 4_555 yes Ti(1) O(1) C(1) C(2) 115.0(3) . . . . yes Ti(1) O(1) C(1) C(6) -66.8(4) . . . . yes Ti(1) O(2) Ti(1) O(1) 88.35(7) . . 4_555 4_555 yes Ti(1) O(2) Ti(1) O(2) 0.0000(1) . . 4_555 4_555 yes Ti(1) O(2) Ti(1) O(3) -89.28(7) . . 4_555 4_555 yes Ti(1) O(2) Ti(1) O(4) -175.3(4) . . 4_555 4_555 yes Ti(1) O(2) Ti(1) O(5) 178.26(7) . . 4_555 4_555 yes Ti(1) O(2) C(8) C(9) 89.2(2) . . . . yes Ti(1) O(2) C(8) C(13) -88.8(2) . . . . yes Ti(1) O(2) Ti(1) O(1) -96.39(7) . 4_555 4_555 4_555 yes Ti(1) O(2) Ti(1) O(2) 0.0000(1) . 4_555 4_555 . yes Ti(1) O(2) Ti(1) O(3) 96.27(7) . 4_555 4_555 4_555 yes Ti(1) O(2) Ti(1) O(4) 179.25(6) . 4_555 4_555 4_555 yes Ti(1) O(2) Ti(1) O(5) -70(1) . 4_555 4_555 4_555 yes Ti(1) O(2) C(8) C(9) 90.4(3) . 4_555 4_555 4_555 yes Ti(1) O(2) C(8) C(13) -91.6(3) . 4_555 4_555 4_555 yes Ti(1) O(3) C(15) C(16) 58.2(4) . . . . yes Ti(1) O(3) C(15) C(20) -124.5(3) . . . . yes Ti(1) O(4) C(30) C(31) -47.0(2) . . . . yes Ti(1) O(5) C(31) C(30) -32.5(2) . . . . yes O(1) Ti(1) Ti(1) O(1) -180.0 . . 4_555 4_555 yes O(1) Ti(1) Ti(1) O(2) -84.67(8) . . 4_555 . yes O(1) Ti(1) Ti(1) O(2) 95.33(8) . . 4_555 4_555 yes O(1) Ti(1) Ti(1) O(3) 9.98(7) . . 4_555 4_555 yes O(1) Ti(1) Ti(1) O(4) 94.0(1) . . 4_555 4_555 yes O(1) Ti(1) Ti(1) O(5) -87.32(9) . . 4_555 4_555 yes O(1) Ti(1) O(2) C(8) -83.4(1) . . . . yes O(1) Ti(1) O(2) C(8) 92.0(2) . . 4_555 4_555 yes O(1) Ti(1) O(3) C(15) 15.9(6) . . . . yes O(1) Ti(1) O(4) C(29) 71.8(2) . . . . yes O(1) Ti(1) O(4) C(30) -67.8(2) . . . . yes O(1) Ti(1) O(5) C(31) 90.9(2) . . . . yes O(1) Ti(1) O(5) C(32) -121.4(2) . . . . yes O(1) C(1) C(2) C(3) -172.7(2) . . . . yes O(1) C(1) C(2) C(21) 9.5(3) . . . . yes O(1) C(1) C(6) C(5) 172.3(2) . . . . yes O(1) C(1) C(6) C(7) -10.4(3) . . . . yes O(2) Ti(1) Ti(1) O(2) 180.0 . . 4_555 4_555 yes O(2) Ti(1) Ti(1) O(3) 94.65(8) . . 4_555 4_555 yes O(2) Ti(1) Ti(1) O(4) 178.7(1) . . 4_555 4_555 yes O(2) Ti(1) Ti(1) O(5) -2.65(10) . . 4_555 4_555 yes O(2) Ti(1) O(1) C(1) 78.7(3) . . . . yes O(2) Ti(1) O(2) Ti(1) 0.0 . . 4_555 4_555 yes O(2) Ti(1) O(2) C(8) -179.7(3) . . 4_555 4_555 yes O(2) Ti(1) O(3) C(15) -72.3(3) . . . . yes O(2) Ti(1) O(4) C(29) -15.8(2) . . . . yes O(2) Ti(1) O(4) C(30) -155.4(1) . . . . yes O(2) Ti(1) O(5) C(31) 116(1) . . . . yes O(2) Ti(1) O(5) C(32) -96(1) . . . . yes O(2) Ti(1) Ti(1) O(2) 180.0 . 4_555 . 4_555 yes O(2) Ti(1) Ti(1) O(3) 85.35(8) . 4_555 . . yes O(2) Ti(1) Ti(1) O(4) 1.3(1) . 4_555 . . yes O(2) Ti(1) Ti(1) O(5) -177.35(10) . 4_555 . . yes O(2) Ti(1) O(1) C(1) -159.7(3) . 4_555 4_555 4_555 yes O(2) Ti(1) O(2) Ti(1) 0.0 . 4_555 4_555 . yes O(2) Ti(1) O(2) C(8) 179.8(2) . 4_555 4_555 4_555 yes O(2) Ti(1) O(3) C(15) 153.3(3) . 4_555 4_555 4_555 yes O(2) Ti(1) O(4) C(29) -169.0(4) . 4_555 4_555 4_555 yes O(2) Ti(1) O(4) C(30) -29.4(5) . 4_555 4_555 4_555 yes O(2) Ti(1) O(5) C(31) 173.0(2) . 4_555 4_555 4_555 yes O(2) Ti(1) O(5) C(32) 25.3(2) . 4_555 4_555 4_555 yes O(2) C(8) C(9) C(7) 3.1(3) . . . . yes O(2) C(8) C(9) C(10) -176.8(2) . . . . yes O(2) C(8) C(13) C(12) 176.5(2) . . . . yes O(2) C(8) C(13) C(14) -5.0(3) . . . . yes O(3) Ti(1) Ti(1) O(3) 180.0 . . 4_555 4_555 yes O(3) Ti(1) Ti(1) O(4) -96.0(1) . . 4_555 4_555 yes O(3) Ti(1) Ti(1) O(5) 82.70(9) . . 4_555 4_555 yes O(3) Ti(1) O(1) C(1) -9.5(5) . . . . yes O(3) Ti(1) O(2) C(8) 83.9(1) . . . . yes O(3) Ti(1) O(2) C(8) -90.4(2) . . 4_555 4_555 yes O(3) Ti(1) O(4) C(29) -103.9(2) . . . . yes O(3) Ti(1) O(4) C(30) 116.5(2) . . . . yes O(3) Ti(1) O(5) C(31) -76.5(2) . . . . yes O(3) Ti(1) O(5) C(32) 71.2(2) . . . . yes O(3) C(15) C(16) C(14) 11.9(3) . . . . yes O(3) C(15) C(16) C(17) -174.4(2) . . . . yes O(3) C(15) C(20) C(19) 175.2(2) . . . . yes O(3) C(15) C(20) C(27) -7.7(3) . . . . yes O(4) Ti(1) Ti(1) O(4) -180.0 . . 4_555 4_555 yes O(4) Ti(1) Ti(1) O(5) -1.3(1) . . 4_555 4_555 yes O(4) Ti(1) O(1) C(1) -29.2(3) . . . . yes O(4) Ti(1) O(2) C(8) 1.0(2) . . . . yes O(4) Ti(1) O(2) C(8) -4.3(6) . . 4_555 4_555 yes O(4) Ti(1) O(3) C(15) 35.6(3) . . . . yes O(4) Ti(1) O(5) C(31) 6.0(2) . . . . yes O(4) Ti(1) O(5) C(32) 153.7(2) . . . . yes O(4) C(30) C(31) O(5) 52.1(3) . . . . yes O(5) Ti(1) Ti(1) O(5) 180.0 . . 4_555 4_555 yes O(5) Ti(1) O(1) C(1) -102.1(3) . . . . yes O(5) Ti(1) O(2) C(8) -108(1) . . . . yes O(5) Ti(1) O(2) C(8) 2.1(3) . . 4_555 4_555 yes O(5) Ti(1) O(3) C(15) 108.1(3) . . . . yes O(5) Ti(1) O(4) C(29) 162.4(2) . . . . yes O(5) Ti(1) O(4) C(30) 22.8(1) . . . . yes C(1) C(2) C(3) C(4) -2.5(4) . . . . yes C(1) C(6) C(5) C(4) 3.4(4) . . . . yes C(1) C(6) C(7) C(9) 85.9(3) . . . . yes C(2) C(1) C(6) C(5) -9.5(3) . . . . yes C(2) C(1) C(6) C(7) 167.8(2) . . . . yes C(2) C(3) C(4) C(5) -3.6(4) . . . . yes C(2) C(3) C(4) C(22) 179.3(3) . . . . yes C(3) C(2) C(1) C(6) 9.1(3) . . . . yes C(3) C(4) C(5) C(6) 3.1(4) . . . . yes C(4) C(3) C(2) C(21) 175.3(3) . . . . yes C(4) C(5) C(6) C(7) -173.9(2) . . . . yes C(5) C(6) C(7) C(9) -97.0(3) . . . . yes C(6) C(1) C(2) C(21) -168.7(2) . . . . yes C(6) C(5) C(4) C(22) -179.7(3) . . . . yes C(6) C(7) C(9) C(8) -101.9(3) . . . . yes C(6) C(7) C(9) C(10) 78.1(3) . . . . yes C(7) C(9) C(8) C(13) -178.9(2) . . . . yes C(7) C(9) C(10) C(11) -179.4(2) . . . . yes C(8) C(9) C(10) C(11) 0.6(4) . . . . yes C(8) C(13) C(12) C(11) 0.1(4) . . . . yes C(8) C(13) C(14) C(16) 102.2(3) . . . . yes C(9) C(8) C(13) C(12) -1.5(3) . . . . yes C(9) C(8) C(13) C(14) 177.1(2) . . . . yes C(9) C(10) C(11) C(12) -1.9(4) . . . . yes C(9) C(10) C(11) C(23) -179.2(2) . . . . yes C(10) C(9) C(8) C(13) 1.2(3) . . . . yes C(10) C(11) C(12) C(13) 1.6(4) . . . . yes C(10) C(11) C(23) C(24) -171.2(3) . . . . yes C(10) C(11) C(23) C(25) -51.4(3) . . . . yes C(10) C(11) C(23) C(26) 68.0(3) . . . . yes C(11) C(12) C(13) C(14) -178.4(2) . . . . yes C(12) C(11) C(23) C(24) 11.6(4) . . . . yes C(12) C(11) C(23) C(25) 131.4(3) . . . . yes C(12) C(11) C(23) C(26) -109.1(3) . . . . yes C(12) C(13) C(14) C(16) -79.3(3) . . . . yes C(13) C(12) C(11) C(23) 178.8(2) . . . . yes C(13) C(14) C(16) C(15) -84.3(3) . . . . yes C(13) C(14) C(16) C(17) 102.0(3) . . . . yes C(14) C(16) C(15) C(20) -165.4(2) . . . . yes C(14) C(16) C(17) C(18) 171.1(2) . . . . yes C(15) C(16) C(17) C(18) -2.7(4) . . . . yes C(15) C(20) C(19) C(18) 0.9(4) . . . . yes C(16) C(15) C(20) C(19) -7.4(3) . . . . yes C(16) C(15) C(20) C(27) 169.7(2) . . . . yes C(16) C(17) C(18) C(19) -3.8(4) . . . . yes C(16) C(17) C(18) C(28) 179.3(2) . . . . yes C(17) C(16) C(15) C(20) 8.3(3) . . . . yes C(17) C(18) C(19) C(20) 4.7(4) . . . . yes C(18) C(19) C(20) C(27) -176.1(2) . . . . yes C(20) C(19) C(18) C(28) -178.4(2) . . . . yes C(29) O(4) C(30) C(31) 166.1(2) . . . . yes C(30) C(31) O(5) C(32) 176.8(2) . . . . yes C(30) C(31) O(5) C(32) 176.8(2) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ti(1) Ti(1) 3.1125(9) . 4_555 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------