Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email fanwick@.xray.chem.purdue.edu _publ_contact_author_name 'Prof Ian Rothwell' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name I.Rothwell G.F.Eade P.E.Fanwick data_GE1P15 _database_code_CSD 200530 _audit_creation_date 6-01-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour dark _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C75.50 H56 Br2 O4 Ti2' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 1282.90 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6298(3) _cell_length_b 15.9823(4) _cell_length_c 16.0980(5) _cell_angle_alpha 115.1707(11) _cell_angle_beta 92.5252(13) _cell_angle_gamma 115.7050(14) _cell_volume 2946.5(3) _cell_measurement_reflns_used 30900 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.662 _cell_measurement_temperature 150 _exptl_crystal_F_000 1316 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.1977 _exptl_absorpt_correction_T_max 0.6881 _diffrn_reflns_number 30900 _diffrn_measured_fraction_theta_max 0.9820 _reflns_number_total 13666 _reflns_number_gt 9734 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.081 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.85 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_max 21 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.055 _refine_ls_wR_factor_ref 0.139 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 13201 _refine_ls_d_res_high 0.77 _refine_ls_number_parameters 766 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0963P)^2^+0.0000P] where P3D(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.00 _refine_diff_density_min -1.43 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.13030(3) 0.49035(3) 0.30731(2) 0.02662(11) Uani 1 1 d . . . Br(2) Br 0.37097(3) 0.50624(3) 0.19118(2) 0.02527(11) Uani 1 1 d . . . Ti(1) Ti 0.31457(5) 0.51980(5) 0.33975(4) 0.02099(15) Uani 1 1 d . . . Ti(2) Ti 0.18406(5) 0.47043(5) 0.15652(4) 0.02203(16) Uani 1 1 d . . . O(1) O 0.11065(18) 0.32556(19) 0.08485(17) 0.0242(5) Uani 1 1 d . . . O(2) O 0.29198(19) 0.39153(19) 0.32628(17) 0.0234(5) Uani 1 1 d . . . O(3) O 0.38613(19) 0.6646(2) 0.41690(17) 0.0257(6) Uani 1 1 d . . . O(4) O 0.2138(2) 0.5971(2) 0.16274(17) 0.0263(6) Uani 1 1 d . . . C(11) C 0.3181(3) 0.3192(3) 0.3236(2) 0.0227(8) Uani 1 1 d . . . C(12) C 0.2417(3) 0.2250(3) 0.3195(2) 0.0276(8) Uani 1 1 d . . . C(13) C 0.2723(3) 0.1514(3) 0.3135(3) 0.0360(10) Uani 1 1 d . . . C(14) C 0.3725(3) 0.1690(3) 0.3126(3) 0.0409(11) Uani 1 1 d . . . C(15) C 0.4462(3) 0.2616(3) 0.3179(3) 0.0346(10) Uani 1 1 d . . . C(16) C 0.4232(3) 0.3405(3) 0.3247(2) 0.0256(8) Uani 1 1 d . . . C(21) C 0.0238(3) 0.2265(3) 0.0331(2) 0.0252(8) Uani 1 1 d . . . C(22) C -0.0773(3) 0.2159(3) 0.0333(3) 0.0275(8) Uani 1 1 d . . . C(23) C -0.1656(3) 0.1143(3) -0.0144(3) 0.0330(9) Uani 1 1 d . . . C(24) C -0.1556(3) 0.0245(3) -0.0645(3) 0.0373(10) Uani 1 1 d . . . C(25) C -0.0564(3) 0.0367(3) -0.0676(3) 0.0308(9) Uani 1 1 d . . . C(26) C 0.0348(3) 0.1368(3) -0.0198(3) 0.0268(8) Uani 1 1 d . . . C(31) C 0.4048(3) 0.7566(3) 0.4941(2) 0.0249(8) Uani 1 1 d . . . C(32) C 0.4834(3) 0.8546(3) 0.5066(3) 0.0317(9) Uani 1 1 d . . . C(33) C 0.4966(4) 0.9478(3) 0.5834(3) 0.0390(11) Uani 1 1 d . . . C(34) C 0.4340(4) 0.9441(4) 0.6451(3) 0.0444(12) Uani 1 1 d . . . C(35) C 0.3604(4) 0.8473(4) 0.6337(3) 0.0385(10) Uani 1 1 d . . . C(36) C 0.3444(3) 0.7511(3) 0.5593(3) 0.0312(9) Uani 1 1 d . . . C(41) C 0.2583(3) 0.6730(3) 0.1380(3) 0.0279(8) Uani 1 1 d . . . C(42) C 0.3089(3) 0.6577(3) 0.0643(3) 0.0307(9) Uani 1 1 d . . . C(43) C 0.3622(3) 0.7416(3) 0.0460(3) 0.0369(10) Uani 1 1 d . . . C(44) C 0.3638(4) 0.8364(4) 0.0959(4) 0.0470(12) Uani 1 1 d . . . C(45) C 0.3089(4) 0.8486(4) 0.1640(3) 0.0442(11) Uani 1 1 d . . . C(46) C 0.2546(3) 0.7682(3) 0.1860(3) 0.0342(9) Uani 1 1 d . . . C(121) C 0.1324(3) 0.2025(3) 0.3238(3) 0.0317(9) Uani 1 1 d . . . C(122) C 0.0728(3) 0.2236(3) 0.2728(3) 0.0351(9) Uani 1 1 d . . . C(123) C -0.0282(4) 0.2015(4) 0.2783(4) 0.0483(12) Uani 1 1 d . . . C(124) C -0.0727(4) 0.1568(4) 0.3332(4) 0.0545(14) Uani 1 1 d . . . C(125) C -0.0168(4) 0.1348(4) 0.3821(3) 0.0542(14) Uani 1 1 d . . . C(126) C 0.0851(4) 0.1581(4) 0.3787(3) 0.0454(11) Uani 1 1 d . . . C(161) C 0.5057(3) 0.4417(3) 0.3341(2) 0.0258(8) Uani 1 1 d . . . C(162) C 0.5712(3) 0.4428(4) 0.2735(3) 0.0345(10) Uani 1 1 d . . . C(163) C 0.6481(3) 0.5368(4) 0.2825(3) 0.0413(11) Uani 1 1 d . . . C(164) C 0.6641(4) 0.6341(4) 0.3529(4) 0.0456(12) Uani 1 1 d . . . C(165) C 0.6011(3) 0.6354(3) 0.4156(3) 0.0372(10) Uani 1 1 d . . . C(166) C 0.5240(3) 0.5412(3) 0.4066(3) 0.0268(8) Uani 1 1 d . . . C(221) C -0.0886(3) 0.3116(3) 0.0856(3) 0.0298(9) Uani 1 1 d . . . C(222) C -0.0360(3) 0.4011(3) 0.0748(3) 0.0336(9) Uani 1 1 d . . . C(223) C -0.0428(4) 0.4924(4) 0.1276(3) 0.0463(12) Uani 1 1 d . . . C(224) C -0.1065(4) 0.4931(4) 0.1889(3) 0.0521(15) Uani 1 1 d . . . C(225) C -0.1629(4) 0.4038(4) 0.1962(3) 0.0454(12) Uani 1 1 d . . . C(226) C -0.1536(3) 0.3136(4) 0.1466(3) 0.0386(10) Uani 1 1 d . . . C(261) C 0.1398(3) 0.1476(3) -0.0273(3) 0.0263(8) Uani 1 1 d . . . C(262) C 0.1495(3) 0.0845(3) -0.1152(3) 0.0336(9) Uani 1 1 d . . . C(263) C 0.2457(3) 0.0928(4) -0.1252(3) 0.0393(10) Uani 1 1 d . . . C(264) C 0.3351(3) 0.1651(3) -0.0486(3) 0.0397(10) Uani 1 1 d . . . C(265) C 0.3267(3) 0.2271(3) 0.0393(3) 0.0381(10) Uani 1 1 d . . . C(266) C 0.2307(3) 0.2174(3) 0.0503(3) 0.0300(9) Uani 1 1 d . . . C(321) C 0.2699(3) 0.6481(3) 0.5533(2) 0.0279(8) Uani 1 1 d . . . C(322) C 0.1729(3) 0.6284(4) 0.5737(3) 0.0422(11) Uani 1 1 d . . . C(323) C 0.1064(4) 0.5330(4) 0.5708(3) 0.0473(12) Uani 1 1 d . . . C(324) C 0.1322(4) 0.4550(4) 0.5461(3) 0.0455(12) Uani 1 1 d . . . C(325) C 0.2269(3) 0.4714(3) 0.5266(3) 0.0352(10) Uani 1 1 d . . . C(326) C 0.2951(3) 0.5665(3) 0.5311(2) 0.0285(8) Uani 1 1 d . . . C(361) C 0.5552(3) 0.8608(3) 0.4446(3) 0.0353(9) Uani 1 1 d . . . C(362) C 0.5196(4) 0.8022(3) 0.3444(3) 0.0374(10) Uani 1 1 d . . . C(363) C 0.5893(4) 0.8093(4) 0.2901(3) 0.0460(12) Uani 1 1 d . . . C(364) C 0.6978(4) 0.8761(4) 0.3337(4) 0.0547(13) Uani 1 1 d . . . C(365) C 0.7346(4) 0.9344(4) 0.4319(4) 0.0553(13) Uani 1 1 d . . . C(366) C 0.6647(4) 0.9273(3) 0.4872(3) 0.0460(12) Uani 1 1 d . . . C(421) C 0.3045(3) 0.5539(3) 0.0060(3) 0.0287(8) Uani 1 1 d . . . C(422) C 0.2100(3) 0.4570(3) -0.0281(3) 0.0292(8) Uani 1 1 d . . . C(423) C 0.2035(4) 0.3594(4) -0.0838(3) 0.0377(10) Uani 1 1 d . . . C(424) C 0.2922(4) 0.3567(4) -0.1079(3) 0.0482(12) Uani 1 1 d . . . C(425) C 0.3849(4) 0.4506(4) -0.0777(3) 0.0428(11) Uani 1 1 d . . . C(426) C 0.3919(3) 0.5484(4) -0.0209(3) 0.0339(9) Uani 1 1 d . . . C(461) C 0.1881(3) 0.7805(3) 0.2530(3) 0.0356(10) Uani 1 1 d . . . C(462) C 0.1178(4) 0.8133(4) 0.2397(3) 0.0478(12) Uani 1 1 d . . . C(463) C 0.0507(5) 0.8213(5) 0.2972(4) 0.0650(17) Uani 1 1 d . . . C(464) C 0.0539(5) 0.7955(5) 0.3699(4) 0.0667(17) Uani 1 1 d . . . C(465) C 0.1247(5) 0.7656(4) 0.3850(3) 0.0588(14) Uani 1 1 d . . . C(466) C 0.1912(4) 0.7568(3) 0.3271(3) 0.0442(11) Uani 1 1 d . . . C(901) C 0.4290(5) 0.0165(5) 0.9886(5) 0.0565(14) Uani 1 1 d . . . C(902) C 0.4328(5) 0.8667(6) 0.8563(5) 0.0754(18) Uani 1 1 d . . . C(903) C 0.4682(9) 0.0929(9) 0.0781(8) 0.050(2) Uani 0.50 1 d P . . C(904) C 0.3867(9) 0.9402(9) 0.8984(9) 0.057(3) Uani 0.50 1 d P . . C(905) C 0.4743(9) 0.9470(9) 0.9493(8) 0.054(3) Uani 0.50 1 d P . . H(13) H 0.2228 0.0881 0.3101 0.043 Uiso 1 1 calc R . . H(14) H 0.3901 0.1183 0.3083 0.049 Uiso 1 1 calc R . . H(15) H 0.5140 0.2728 0.3169 0.042 Uiso 1 1 calc R . . H(23) H -0.2323 0.1061 -0.0129 0.040 Uiso 1 1 calc R . . H(24) H -0.2153 -0.0432 -0.0958 0.045 Uiso 1 1 calc R . . H(25) H -0.0505 -0.0235 -0.1024 0.037 Uiso 1 1 calc R . . H(33) H 0.5486 1.0137 0.5933 0.047 Uiso 1 1 calc R . . H(34) H 0.4416 1.0070 0.6940 0.053 Uiso 1 1 calc R . . H(35) H 0.3201 0.8457 0.6766 0.046 Uiso 1 1 calc R . . H(43) H 0.3974 0.7330 -0.0011 0.044 Uiso 1 1 calc R . . H(44) H 0.4016 0.8924 0.0842 0.056 Uiso 1 1 calc R . . H(45) H 0.3082 0.9123 0.1959 0.053 Uiso 1 1 calc R . . H(122) H 0.1019 0.2529 0.2349 0.042 Uiso 1 1 calc R . . H(123) H -0.0664 0.2167 0.2448 0.058 Uiso 1 1 calc R . . H(124) H -0.1408 0.1419 0.3368 0.065 Uiso 1 1 calc R . . H(125) H -0.0475 0.1036 0.4183 0.065 Uiso 1 1 calc R . . H(126) H 0.1226 0.1437 0.4138 0.054 Uiso 1 1 calc R . . H(162) H 0.5623 0.3784 0.2261 0.041 Uiso 1 1 calc R . . H(163) H 0.6903 0.5352 0.2409 0.050 Uiso 1 1 calc R . . H(164) H 0.7159 0.6976 0.3582 0.055 Uiso 1 1 calc R . . H(165) H 0.6114 0.7002 0.4636 0.045 Uiso 1 1 calc R . . H(166) H 0.4830 0.5431 0.4492 0.032 Uiso 1 1 calc R . . H(222) H 0.0043 0.3999 0.0317 0.040 Uiso 1 1 calc R . . H(223) H -0.0048 0.5527 0.1217 0.056 Uiso 1 1 calc R . . H(224) H -0.1108 0.5541 0.2249 0.062 Uiso 1 1 calc R . . H(225) H -0.2083 0.4032 0.2348 0.054 Uiso 1 1 calc R . . H(226) H -0.1908 0.2543 0.1541 0.046 Uiso 1 1 calc R . . H(262) H 0.0900 0.0363 -0.1677 0.040 Uiso 1 1 calc R . . H(263) H 0.2504 0.0495 -0.1838 0.047 Uiso 1 1 calc R . . H(264) H 0.4004 0.1722 -0.0557 0.048 Uiso 1 1 calc R . . H(265) H 0.3867 0.2758 0.0912 0.046 Uiso 1 1 calc R . . H(266) H 0.2261 0.2578 0.1102 0.036 Uiso 1 1 calc R . . H(322) H 0.1529 0.6798 0.5893 0.051 Uiso 1 1 calc R . . H(323) H 0.0430 0.5221 0.5860 0.057 Uiso 1 1 calc R . . H(324) H 0.0856 0.3905 0.5425 0.055 Uiso 1 1 calc R . . H(325) H 0.2450 0.4185 0.5104 0.042 Uiso 1 1 calc R . . H(326) H 0.3598 0.5774 0.5191 0.034 Uiso 1 1 calc R . . H(362) H 0.4475 0.7578 0.3143 0.045 Uiso 1 1 calc R . . H(363) H 0.5640 0.7693 0.2238 0.055 Uiso 1 1 calc R . . H(364) H 0.7449 0.8811 0.2967 0.066 Uiso 1 1 calc R . . H(365) H 0.8068 0.9789 0.4613 0.066 Uiso 1 1 calc R . . H(366) H 0.6906 0.9672 0.5535 0.055 Uiso 1 1 calc R . . H(422) H 0.1499 0.4582 -0.0128 0.035 Uiso 1 1 calc R . . H(423) H 0.1400 0.2962 -0.1048 0.045 Uiso 1 1 calc R . . H(424) H 0.2891 0.2916 -0.1443 0.058 Uiso 1 1 calc R . . H(425) H 0.4438 0.4487 -0.0955 0.051 Uiso 1 1 calc R . . H(426) H 0.4557 0.6110 -0.0004 0.041 Uiso 1 1 calc R . . H(462) H 0.1156 0.8303 0.1914 0.057 Uiso 1 1 calc R . . H(463) H 0.0040 0.8436 0.2876 0.078 Uiso 1 1 calc R . . H(464) H 0.0080 0.7986 0.4077 0.080 Uiso 1 1 calc R . . H(465) H 0.1284 0.7511 0.4348 0.071 Uiso 1 1 calc R . . H(466) H 0.2380 0.7350 0.3374 0.053 Uiso 1 1 calc R . . 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 Br(1) 0.0247(2) 0.0307(2) 0.02401(19) 0.01309(17) 0.00605(15) 0.01397(16) Br(2) 0.02395(19) 0.0246(2) 0.02241(18) 0.00859(16) 0.00456(14) 0.01161(15) Ti(1) 0.0219(3) 0.0167(3) 0.0200(3) 0.0067(3) 0.0025(2) 0.0089(3) Ti(2) 0.0240(3) 0.0175(3) 0.0201(3) 0.0076(3) 0.0025(3) 0.0088(3) O(1) 0.0198(12) 0.0202(13) 0.0250(12) 0.0054(10) 0.0033(10) 0.0101(10) O(2) 0.0244(13) 0.0193(13) 0.0252(12) 0.0093(11) 0.0064(10) 0.0116(10) O(3) 0.0264(13) 0.0237(14) 0.0221(12) 0.0122(11) 0.0063(10) 0.0077(10) O(4) 0.0299(14) 0.0235(14) 0.0268(13) 0.0121(11) 0.0079(11) 0.0148(11) C(11) 0.0286(19) 0.0201(18) 0.0139(15) 0.0114(15) 0.0014(14) 0.0052(13) C(12) 0.032(2) 0.023(2) 0.0210(17) 0.0108(17) 0.0002(15) 0.0091(15) C(13) 0.042(2) 0.020(2) 0.034(2) 0.0075(18) -0.0038(18) 0.0125(17) C(14) 0.041(2) 0.025(2) 0.040(2) 0.0150(19) -0.0091(19) 0.0058(19) C(15) 0.035(2) 0.028(2) 0.030(2) 0.0183(19) -0.0038(17) 0.0046(17) C(16) 0.0269(19) 0.0235(19) 0.0189(16) 0.0116(16) 0.0012(14) 0.0059(14) C(21) 0.0269(19) 0.0209(19) 0.0202(16) 0.0076(16) 0.0024(14) 0.0090(15) C(22) 0.0275(19) 0.028(2) 0.0266(18) 0.0131(17) 0.0077(15) 0.0144(16) C(23) 0.0251(19) 0.026(2) 0.035(2) 0.0049(17) 0.0040(16) 0.0130(17) C(24) 0.029(2) 0.023(2) 0.040(2) 0.0031(17) -0.0001(18) 0.0121(18) C(25) 0.031(2) 0.0166(19) 0.0296(19) 0.0063(16) 0.0020(16) 0.0058(16) C(26) 0.030(2) 0.025(2) 0.0232(17) 0.0112(17) 0.0064(15) 0.0124(16) C(31) 0.031(2) 0.0200(19) 0.0214(17) 0.0158(16) 0.0022(15) 0.0062(14) C(32) 0.038(2) 0.026(2) 0.0272(19) 0.0143(18) 0.0018(17) 0.0123(17) C(33) 0.056(3) 0.019(2) 0.033(2) 0.018(2) 0.003(2) 0.0084(17) C(34) 0.073(3) 0.031(2) 0.029(2) 0.032(2) 0.009(2) 0.0078(18) C(35) 0.052(3) 0.044(3) 0.027(2) 0.034(2) 0.0116(19) 0.0133(19) C(36) 0.035(2) 0.036(2) 0.0266(19) 0.0249(19) 0.0080(16) 0.0117(17) C(41) 0.0240(19) 0.027(2) 0.0289(19) 0.0064(16) 0.0014(15) 0.0173(16) C(42) 0.0271(19) 0.030(2) 0.034(2) 0.0117(17) 0.0016(16) 0.0189(18) C(43) 0.028(2) 0.038(2) 0.048(2) 0.0102(19) 0.0115(18) 0.031(2) C(44) 0.039(3) 0.041(3) 0.063(3) 0.011(2) 0.011(2) 0.038(3) C(45) 0.046(3) 0.026(2) 0.048(3) 0.012(2) 0.000(2) 0.015(2) C(46) 0.030(2) 0.030(2) 0.036(2) 0.0114(18) -0.0021(17) 0.0159(18) C(121) 0.033(2) 0.021(2) 0.0245(18) 0.0042(17) 0.0077(16) 0.0077(16) C(122) 0.034(2) 0.027(2) 0.037(2) 0.0131(18) 0.0084(18) 0.0116(18) C(123) 0.033(2) 0.032(2) 0.064(3) 0.012(2) 0.011(2) 0.014(2) C(124) 0.037(3) 0.031(3) 0.066(3) 0.008(2) 0.023(2) 0.008(2) C(125) 0.053(3) 0.036(3) 0.039(2) 0.002(2) 0.024(2) 0.011(2) C(126) 0.052(3) 0.034(3) 0.034(2) 0.008(2) 0.013(2) 0.018(2) C(161) 0.0222(18) 0.031(2) 0.0201(17) 0.0139(16) 0.0014(14) 0.0099(15) C(162) 0.027(2) 0.047(3) 0.0247(19) 0.021(2) 0.0032(16) 0.0112(18) C(163) 0.034(2) 0.058(3) 0.042(2) 0.023(2) 0.0133(19) 0.033(2) C(164) 0.035(2) 0.043(3) 0.061(3) 0.009(2) 0.005(2) 0.039(3) C(165) 0.037(2) 0.031(2) 0.040(2) 0.016(2) 0.0024(19) 0.0169(19) C(166) 0.0267(19) 0.025(2) 0.0255(18) 0.0131(16) 0.0014(15) 0.0104(16) C(221) 0.0212(18) 0.036(2) 0.0224(18) 0.0123(17) -0.0003(14) 0.0098(16) C(222) 0.025(2) 0.032(2) 0.039(2) 0.0131(18) -0.0016(17) 0.0157(18) C(223) 0.036(2) 0.040(3) 0.053(3) 0.018(2) -0.006(2) 0.017(2) C(224) 0.058(3) 0.046(3) 0.037(2) 0.037(3) -0.008(2) -0.001(2) C(225) 0.047(3) 0.055(3) 0.029(2) 0.034(3) 0.0027(19) 0.009(2) C(226) 0.033(2) 0.046(3) 0.033(2) 0.022(2) 0.0070(18) 0.016(2) C(261) 0.0275(19) 0.025(2) 0.0250(18) 0.0121(16) 0.0048(15) 0.0126(15) C(262) 0.034(2) 0.031(2) 0.0260(19) 0.0144(18) 0.0057(16) 0.0082(17) C(263) 0.044(2) 0.038(3) 0.036(2) 0.025(2) 0.0139(19) 0.0135(19) C(264) 0.031(2) 0.036(2) 0.058(3) 0.020(2) 0.016(2) 0.025(2) C(265) 0.031(2) 0.030(2) 0.045(2) 0.0150(19) 0.0009(18) 0.0136(19) C(266) 0.032(2) 0.024(2) 0.0289(19) 0.0126(17) 0.0047(16) 0.0104(16) C(321) 0.0269(19) 0.033(2) 0.0192(17) 0.0151(17) 0.0026(14) 0.0092(15) C(322) 0.042(2) 0.071(3) 0.0233(19) 0.037(3) 0.0157(18) 0.022(2) C(323) 0.029(2) 0.072(4) 0.037(2) 0.019(2) 0.0151(19) 0.031(2) C(324) 0.041(3) 0.049(3) 0.029(2) 0.006(2) 0.0061(19) 0.024(2) C(325) 0.037(2) 0.037(2) 0.0221(18) 0.0102(19) 0.0034(16) 0.0150(18) C(326) 0.0272(19) 0.036(2) 0.0189(17) 0.0135(17) 0.0030(15) 0.0129(16) C(361) 0.046(2) 0.025(2) 0.035(2) 0.0162(19) 0.0089(19) 0.0175(18) C(362) 0.048(3) 0.030(2) 0.037(2) 0.017(2) 0.0107(19) 0.0218(19) C(363) 0.069(3) 0.027(2) 0.035(2) 0.017(2) 0.016(2) 0.0167(19) C(364) 0.061(3) 0.041(3) 0.056(3) 0.017(3) 0.027(3) 0.027(3) C(365) 0.044(3) 0.038(3) 0.059(3) 0.005(2) 0.012(2) 0.021(2) C(366) 0.045(3) 0.025(2) 0.042(2) 0.001(2) 0.001(2) 0.013(2) C(421) 0.031(2) 0.039(2) 0.0291(19) 0.0192(18) 0.0105(16) 0.0252(18) C(422) 0.029(2) 0.035(2) 0.0290(19) 0.0168(18) 0.0113(16) 0.0189(17) C(423) 0.048(3) 0.043(3) 0.028(2) 0.024(2) 0.0129(19) 0.0209(19) C(424) 0.066(3) 0.061(3) 0.031(2) 0.042(3) 0.019(2) 0.022(2) C(425) 0.050(3) 0.065(3) 0.039(2) 0.040(3) 0.023(2) 0.034(2) C(426) 0.031(2) 0.044(3) 0.032(2) 0.018(2) 0.0110(17) 0.0242(19) C(461) 0.041(2) 0.021(2) 0.030(2) 0.0109(18) 0.0020(18) 0.0061(17) C(462) 0.058(3) 0.040(3) 0.035(2) 0.027(2) 0.004(2) 0.008(2) C(463) 0.069(4) 0.071(4) 0.047(3) 0.049(3) 0.010(3) 0.010(3) C(464) 0.070(4) 0.064(4) 0.041(3) 0.034(3) 0.020(3) 0.004(3) C(465) 0.079(4) 0.050(3) 0.032(2) 0.028(3) 0.019(2) 0.012(2) C(466) 0.058(3) 0.030(2) 0.033(2) 0.021(2) 0.006(2) 0.0097(19) C(901) 0.067(4) 0.069(4) 0.081(4) 0.045(3) 0.049(3) 0.061(4) C(902) 0.086(5) 0.095(5) 0.079(4) 0.054(4) 0.043(4) 0.059(4) C(903) 0.065(7) 0.053(6) 0.061(6) 0.038(6) 0.040(5) 0.042(5) C(904) 0.060(7) 0.060(7) 0.088(8) 0.036(6) 0.037(6) 0.060(7) C(905) 0.072(7) 0.057(7) 0.066(7) 0.037(6) 0.045(6) 0.051(6) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Br(1) Ti(1) 2.5155(7) YES Br(1) Ti(2) 2.5180(8) YES Br(2) Ti(1) 2.5171(7) YES Br(2) Ti(2) 2.5205(7) YES Ti(1) O(3) 1.826(3) YES Ti(1) O(2) 1.840(2) YES Ti(1) Ti(2) 3.0308(8) YES Ti(2) O(1) 1.818(2) YES Ti(2) O(4) 1.833(3) YES O(1) C(21) 1.362(4) YES O(2) C(11) 1.351(4) YES O(3) C(31) 1.359(4) YES O(4) C(41) 1.342(5) YES C(11) C(12) 1.403(5) YES C(11) C(16) 1.422(5) YES C(12) C(13) 1.401(5) YES C(12) C(121) 1.490(6) YES C(13) C(14) 1.368(6) YES C(14) C(15) 1.364(6) YES C(15) C(16) 1.403(5) YES C(16) C(161) 1.476(5) YES C(21) C(26) 1.407(5) YES C(21) C(22) 1.415(5) YES C(22) C(23) 1.388(5) YES C(22) C(221) 1.487(5) YES C(23) C(24) 1.392(6) YES C(24) C(25) 1.384(6) YES C(25) C(26) 1.394(5) YES C(26) C(261) 1.486(5) YES C(31) C(32) 1.402(6) YES C(31) C(36) 1.408(6) YES C(32) C(33) 1.395(5) YES C(32) C(361) 1.482(6) YES C(33) C(34) 1.383(7) YES C(34) C(35) 1.372(7) YES C(35) C(36) 1.396(5) YES C(36) C(321) 1.484(6) YES C(41) C(46) 1.410(6) YES C(41) C(42) 1.417(6) YES C(42) C(43) 1.393(6) YES C(42) C(421) 1.487(6) YES C(43) C(44) 1.370(6) YES C(44) C(45) 1.384(7) YES C(45) C(46) 1.390(6) YES C(46) C(461) 1.493(6) YES C(121) C(126) 1.388(6) YES C(121) C(122) 1.406(6) YES C(122) C(123) 1.378(6) YES C(123) C(124) 1.378(8) YES C(124) C(125) 1.358(7) YES C(125) C(126) 1.381(7) YES C(161) C(162) 1.397(5) YES C(161) C(166) 1.410(5) YES C(162) C(163) 1.371(6) YES C(163) C(164) 1.386(7) YES C(164) C(165) 1.396(7) YES C(165) C(166) 1.373(6) YES C(221) C(222) 1.391(6) YES C(221) C(226) 1.397(6) YES C(222) C(223) 1.393(6) YES C(223) C(224) 1.387(7) YES C(224) C(225) 1.363(7) YES C(225) C(226) 1.391(6) YES C(261) C(266) 1.398(5) YES C(261) C(262) 1.403(5) YES C(262) C(263) 1.379(6) YES C(263) C(264) 1.378(6) YES C(264) C(265) 1.388(6) YES C(265) C(266) 1.372(6) YES C(321) C(322) 1.402(6) YES C(321) C(326) 1.413(5) YES C(322) C(323) 1.386(7) YES C(323) C(324) 1.363(7) YES C(324) C(325) 1.371(6) YES C(325) C(326) 1.377(6) YES C(361) C(362) 1.403(6) YES C(361) C(366) 1.404(6) YES C(362) C(363) 1.370(6) YES C(363) C(364) 1.396(7) YES C(364) C(365) 1.376(7) YES C(365) C(366) 1.384(7) YES C(421) C(426) 1.394(5) YES C(421) C(422) 1.402(5) YES C(422) C(423) 1.385(6) YES C(423) C(424) 1.385(6) YES C(424) C(425) 1.372(7) YES C(425) C(426) 1.388(6) YES C(461) C(462) 1.387(6) YES C(461) C(466) 1.400(6) YES C(462) C(463) 1.387(7) YES C(463) C(464) 1.402(8) YES C(464) C(465) 1.365(8) YES C(465) C(466) 1.386(7) YES C(901) C(903) 1.311(12) YES C(901) C(904) 1.319(13) YES C(901) C(905) 1.415(12) YES C(901) C(905) 1.466(11) YES C(902) C(905) 1.366(12) YES C(902) C(903) 1.450(12) YES C(902) C(904) 1.531(12) YES C(903) C(905) 1.252(13) YES C(903) C(901) 1.311(12) YES C(903) C(902) 1.450(12) YES C(904) C(901) 1.319(13) YES C(904) C(905) 1.428(15) YES C(905) C(903) 1.252(14) YES C(905) C(901) 1.415(12) YES C(905) C(901) 1.466(11) YES C(905) C(905) 1.59(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_publ_flag Ti(1) Br(1) Ti(2) 74.04(2) YES Ti(1) Br(2) Ti(2) 73.97(2) YES O(3) Ti(1) O(2) 145.61(11) YES O(3) Ti(1) Br(1) 98.84(8) YES O(2) Ti(1) Br(1) 102.82(8) YES O(3) Ti(1) Br(2) 100.08(9) YES O(2) Ti(1) Br(2) 99.19(8) YES Br(1) Ti(1) Br(2) 106.05(2) YES O(3) Ti(1) Ti(2) 107.38(8) YES O(2) Ti(1) Ti(2) 106.98(8) YES Br(1) Ti(1) Ti(2) 53.016(19) YES Br(2) Ti(1) Ti(2) 53.066(18) YES O(1) Ti(2) O(4) 146.26(11) YES O(1) Ti(2) Br(1) 98.96(9) YES O(4) Ti(2) Br(1) 102.14(8) YES O(1) Ti(2) Br(2) 101.29(8) YES O(4) Ti(2) Br(2) 97.89(8) YES Br(1) Ti(2) Br(2) 105.87(2) YES O(1) Ti(2) Ti(1) 105.44(8) YES O(4) Ti(2) Ti(1) 108.27(8) YES Br(1) Ti(2) Ti(1) 52.941(18) YES Br(2) Ti(2) Ti(1) 52.961(19) YES C(21) O(1) Ti(2) 156.8(2) YES C(11) O(2) Ti(1) 156.8(2) YES C(31) O(3) Ti(1) 153.3(3) YES C(41) O(4) Ti(2) 153.1(3) YES O(2) C(11) C(12) 119.9(3) YES O(2) C(11) C(16) 118.8(3) YES C(12) C(11) C(16) 121.3(3) YES C(13) C(12) C(11) 117.3(4) YES C(13) C(12) C(121) 119.7(4) YES C(11) C(12) C(121) 123.0(3) YES C(14) C(13) C(12) 122.5(4) YES C(15) C(14) C(13) 119.5(4) YES C(14) C(15) C(16) 122.1(4) YES C(15) C(16) C(11) 117.2(4) YES C(15) C(16) C(161) 121.0(3) YES C(11) C(16) C(161) 121.8(3) YES O(1) C(21) C(26) 120.5(3) YES O(1) C(21) C(22) 118.7(3) YES C(26) C(21) C(22) 120.8(3) YES C(23) C(22) C(21) 118.7(3) YES C(23) C(22) C(221) 120.7(3) YES C(21) C(22) C(221) 120.6(3) YES C(22) C(23) C(24) 120.9(4) YES C(25) C(24) C(23) 119.6(4) YES C(24) C(25) C(26) 121.7(4) YES C(25) C(26) C(21) 118.1(3) YES C(25) C(26) C(261) 120.4(3) YES C(21) C(26) C(261) 121.5(3) YES O(3) C(31) C(32) 119.2(4) YES O(3) C(31) C(36) 119.2(4) YES C(32) C(31) C(36) 121.6(3) YES C(33) C(32) C(31) 117.9(4) YES C(33) C(32) C(361) 120.2(4) YES C(31) C(32) C(361) 121.8(3) YES C(34) C(33) C(32) 121.3(4) YES C(35) C(34) C(33) 119.7(4) YES C(34) C(35) C(36) 121.8(4) YES C(35) C(36) C(31) 117.4(4) YES C(35) C(36) C(321) 120.4(4) YES C(31) C(36) C(321) 122.1(3) YES O(4) C(41) C(46) 119.7(4) YES O(4) C(41) C(42) 120.2(4) YES C(46) C(41) C(42) 120.1(4) YES C(43) C(42) C(41) 118.7(4) YES C(43) C(42) C(421) 120.1(4) YES C(41) C(42) C(421) 121.1(4) YES C(44) C(43) C(42) 121.3(4) YES C(43) C(44) C(45) 119.7(5) YES C(44) C(45) C(46) 121.8(4) YES C(45) C(46) C(41) 118.1(4) YES C(45) C(46) C(461) 120.1(4) YES C(41) C(46) C(461) 121.6(4) YES C(126) C(121) C(122) 117.3(4) YES C(126) C(121) C(12) 120.3(4) YES C(122) C(121) C(12) 122.4(4) YES C(123) C(122) C(121) 120.8(5) YES C(124) C(123) C(122) 120.2(5) YES C(125) C(124) C(123) 119.9(5) YES C(124) C(125) C(126) 120.7(5) YES C(125) C(126) C(121) 121.1(5) YES C(162) C(161) C(166) 117.3(4) YES C(162) C(161) C(16) 121.3(3) YES C(166) C(161) C(16) 121.3(3) YES C(163) C(162) C(161) 121.3(4) YES C(162) C(163) C(164) 120.9(4) YES C(163) C(164) C(165) 119.0(4) YES C(166) C(165) C(164) 120.1(4) YES C(165) C(166) C(161) 121.3(4) YES C(222) C(221) C(226) 118.0(4) YES C(222) C(221) C(22) 121.4(4) YES C(226) C(221) C(22) 120.6(4) YES C(221) C(222) C(223) 121.1(5) YES C(224) C(223) C(222) 119.8(5) YES C(225) C(224) C(223) 119.6(4) YES C(224) C(225) C(226) 121.0(5) YES C(225) C(226) C(221) 120.3(5) YES C(266) C(261) C(262) 117.6(4) YES C(266) C(261) C(26) 123.0(3) YES C(262) C(261) C(26) 119.4(3) YES C(263) C(262) C(261) 121.2(4) YES C(264) C(263) C(262) 120.2(4) YES C(263) C(264) C(265) 119.4(4) YES C(266) C(265) C(264) 120.7(4) YES C(265) C(266) C(261) 120.9(4) YES C(322) C(321) C(326) 116.2(4) YES C(322) C(321) C(36) 121.9(4) YES C(326) C(321) C(36) 121.8(4) YES C(323) C(322) C(321) 120.8(4) YES C(324) C(323) C(322) 121.1(4) YES C(323) C(324) C(325) 120.0(5) YES C(324) C(325) C(326) 119.8(4) YES C(325) C(326) C(321) 122.1(4) YES C(362) C(361) C(366) 117.6(4) YES C(362) C(361) C(32) 123.3(4) YES C(366) C(361) C(32) 119.1(4) YES C(363) C(362) C(361) 121.2(4) YES C(362) C(363) C(364) 120.4(4) YES C(365) C(364) C(363) 119.4(5) YES C(364) C(365) C(366) 120.4(5) YES C(365) C(366) C(361) 120.9(4) YES C(426) C(421) C(422) 117.0(4) YES C(426) C(421) C(42) 122.0(4) YES C(422) C(421) C(42) 121.0(4) YES C(423) C(422) C(421) 122.0(4) YES C(424) C(423) C(422) 119.5(5) YES C(425) C(424) C(423) 119.6(5) YES C(424) C(425) C(426) 121.0(4) YES C(425) C(426) C(421) 120.9(4) YES C(462) C(461) C(466) 118.5(5) YES C(462) C(461) C(46) 118.9(4) YES C(466) C(461) C(46) 122.6(4) YES C(461) C(462) C(463) 121.2(5) YES C(462) C(463) C(464) 119.3(5) YES C(465) C(464) C(463) 119.8(5) YES C(464) C(465) C(466) 120.8(5) YES C(465) C(466) C(461) 120.3(5) YES C(903) C(901) C(904) 177.9(8) YES C(903) C(901) C(905) 54.5(6) YES C(904) C(901) C(905) 127.6(7) YES C(903) C(901) C(905) 120.6(8) YES C(904) C(901) C(905) 61.4(7) YES C(905) C(901) C(905) 67.0(8) YES C(905) C(902) C(903) 52.7(6) YES C(905) C(902) C(904) 58.7(7) YES C(903) C(902) C(904) 110.5(8) YES C(905) C(903) C(901) 67.0(8) YES C(905) C(903) C(902) 60.2(7) YES C(901) C(903) C(902) 127.2(8) YES C(901) C(904) C(905) 64.4(7) YES C(901) C(904) C(902) 119.2(8) YES C(905) C(904) C(902) 54.9(6) YES C(903) C(905) C(902) 67.1(8) YES C(903) C(905) C(901) 58.5(7) YES C(902) C(905) C(901) 125.6(9) YES C(903) C(905) C(904) 132.1(12) YES C(902) C(905) C(904) 66.4(8) YES C(901) C(905) C(904) 164.6(10) YES C(903) C(905) C(901) 167.1(11) YES C(902) C(905) C(901) 120.6(9) YES C(901) C(905) C(901) 113.0(8) YES C(904) C(905) C(901) 54.2(7) YES C(903) C(905) C(905) 115.7(13) YES C(902) C(905) C(905) 170.8(11) YES C(901) C(905) C(905) 58.0(7) YES C(904) C(905) C(905) 108.6(11) YES C(901) C(905) C(905) 55.0(6) YES data_GE1P14 _database_code_CSD 200531 _audit_creation_date 26-03-01 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C36 H26 Br2 O2 Ti1' _chemical_formula_structural ? _chemical_formula_weight 698.33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'p 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 10.4945(3) _cell_length_b 15.3372(4) _cell_length_c 9.5602(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1538.77(17) _cell_measurement_reflns_used 6892 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 2.876 _cell_measurement_temperature 149 _exptl_crystal_F_000 700 # 6. DATA COLLECTION _diffrn_ambient_temperature 149 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.2916 _exptl_absorpt_correction_T_max 0.4872 _diffrn_reflns_number 6892 _reflns_number_total 3568 _reflns_friedl_coverage 0.8330 _reflns_number_gt 3266 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.86 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_max 12 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_ref 0.061 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 3568 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.29 _refine_diff_density_min -0.39 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.14E-01 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(8) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Br 0.66722(3) 0.05154(2) 0.11718(3) 0.03478(8) Uani ? Ti 0.5000 0.0000 -0.02782(6) 0.01870(17) Uani ? O1 0.45078(16) 0.08852(12) -0.12914(17) 0.0192(4) Uani ? C1 0.4177(2) 0.14660(16) -0.2306(2) 0.0163(6) Uani ? C2 0.3052(2) 0.19402(18) -0.2118(3) 0.0183(7) Uani ? C3 0.2694(3) 0.25117(19) -0.3193(3) 0.0250(7) Uani ? C4 0.3423(3) 0.25987(19) -0.4393(3) 0.0285(7) Uani ? C5 0.4534(3) 0.21178(19) -0.4542(3) 0.0249(7) Uani ? C6 0.4941(3) 0.15396(17) -0.3509(2) 0.0190(6) Uani ? C21 0.2251(3) 0.18228(19) -0.0849(3) 0.0227(7) Uani ? C22 0.0963(3) 0.1609(2) -0.0982(3) 0.0304(8) Uani ? C23 0.0217(3) 0.1470(2) 0.0191(3) 0.0419(10) Uani ? C24 0.0725(3) 0.1548(2) 0.1504(3) 0.0389(9) Uani ? C25 0.1998(3) 0.1774(2) 0.1659(3) 0.0337(8) Uani ? C26 0.2757(3) 0.19094(19) 0.0485(3) 0.0260(7) Uani ? C61 0.6114(2) 0.10061(16) -0.3697(2) 0.0168(6) Uani ? C62 0.6320(2) 0.05684(19) -0.4960(2) 0.0203(6) Uani ? C63 0.7379(3) 0.0040(2) -0.5146(3) 0.0260(7) Uani ? C64 0.8249(3) -0.0061(2) -0.4070(3) 0.0289(7) Uani ? C65 0.8081(2) 0.03867(19) -0.2823(3) 0.0257(7) Uani ? C66 0.7030(2) 0.09252(19) -0.2644(3) 0.0222(7) Uani ? H3 0.1953 0.2839 -0.3098 0.0300 Uiso calc H4 0.3168 0.2979 -0.5097 0.0340 Uiso calc H5 0.5019 0.2183 -0.5349 0.0300 Uiso calc H22 0.0602 0.1560 -0.1867 0.0360 Uiso calc H23 -0.0637 0.1321 0.0086 0.0500 Uiso calc H24 0.0220 0.1451 0.2288 0.0470 Uiso calc H25 0.2345 0.1834 0.2549 0.0400 Uiso calc H26 0.3609 0.2059 0.0595 0.0310 Uiso calc H62 0.5738 0.0632 -0.5686 0.0240 Uiso calc H63 0.7505 -0.0246 -0.5993 0.0310 Uiso calc H64 0.8946 -0.0429 -0.4184 0.0350 Uiso calc H65 0.8673 0.0326 -0.2106 0.0310 Uiso calc H66 0.6935 0.1235 -0.1814 0.0270 Uiso 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 Br 0.04909(19) 0.03347(17) 0.02178(12) -0.00488(16) -0.01217(13) -0.00393(13) Ti 0.0276(4) 0.0159(3) 0.0126(3) 0.0037(3) 0.0000 0.0000 O1 0.0205(9) 0.0196(9) 0.0176(7) 0.0039(7) 0.0019(7) 0.0035(7) C1 0.0211(13) 0.0122(13) 0.0157(11) -0.0010(10) -0.0043(10) 0.0019(9) C2 0.0148(14) 0.0194(14) 0.0207(11) 0.0022(10) -0.0008(10) -0.0017(10) C3 0.0263(15) 0.0231(15) 0.0257(12) 0.0090(12) -0.0070(12) 0.0009(12) C4 0.0348(16) 0.0266(16) 0.0242(11) 0.0069(14) -0.0060(13) 0.0063(11) C5 0.0285(15) 0.0265(16) 0.0196(12) 0.0024(12) -0.0011(11) 0.0059(11) C6 0.0196(12) 0.0184(13) 0.0190(11) -0.0006(11) -0.0020(10) 0.0007(9) C21 0.0250(14) 0.0159(14) 0.0271(14) 0.0068(11) 0.0039(11) -0.0029(10) C22 0.0243(15) 0.0314(17) 0.0354(15) 0.0039(12) 0.0043(13) -0.0032(13) C23 0.0298(19) 0.040(2) 0.056(2) 0.0000(15) 0.0146(16) -0.0055(16) C24 0.045(2) 0.0331(19) 0.0387(17) 0.0095(15) 0.0228(15) -0.0018(14) C25 0.051(2) 0.0256(17) 0.0244(12) 0.0078(14) 0.0067(13) -0.0042(11) C26 0.0301(15) 0.0204(15) 0.0276(14) 0.0044(12) 0.0049(12) -0.0029(12) C61 0.0177(11) 0.0137(12) 0.0190(11) -0.0019(9) 0.0005(10) 0.0047(10) C62 0.0204(13) 0.0222(13) 0.0183(10) -0.0025(12) 0.0010(9) 0.0023(10) C63 0.0266(14) 0.0241(15) 0.0273(12) 0.0002(13) 0.0067(11) -0.0028(13) C64 0.0209(13) 0.0277(15) 0.0380(14) 0.0054(14) 0.0065(13) 0.0039(12) C65 0.0188(14) 0.0275(16) 0.0309(12) 0.0006(11) -0.0028(11) 0.0065(12) C66 0.0215(14) 0.0259(15) 0.0193(11) 0.0001(11) 0.0008(10) 0.0029(11) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Br Ti 2.3719(4) YES Ti O(1) 1.7459(17) YES Ti O(1) 1.7459(17) YES Ti Br 2.3720(4) YES O(1) C(1) 1.362(3) YES C(1) C(2) 1.398(4) YES C(1) C(6) 1.406(3) YES C(2) C(3) 1.402(4) YES C(2) C(21) 1.487(4) YES C(3) C(4) 1.385(4) YES C(4) C(5) 1.387(4) YES C(5) C(6) 1.394(3) YES C(6) C(61) 1.490(4) YES C(21) C(26) 1.388(4) YES C(21) C(22) 1.398(4) YES C(22) C(23) 1.384(4) YES C(23) C(24) 1.370(5) YES C(24) C(25) 1.388(5) YES C(25) C(26) 1.392(4) YES C(61) C(66) 1.398(3) YES C(61) C(62) 1.398(3) YES C(62) C(63) 1.387(4) YES C(63) C(64) 1.384(4) YES C(64) C(65) 1.387(4) YES C(65) C(66) 1.388(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_publ_flag O(1) Ti O(1) 112.60(11) YES O(1) Ti Br 106.50(6) YES O(1) Ti Br 111.38(5) YES O(1) Ti Br 111.38(5) YES O(1) Ti Br 106.50(6) YES Br Ti Br 108.48(3) YES C(1) O(1) Ti 168.27(16) YES O(1) C(1) C(2) 117.6(2) YES O(1) C(1) C(6) 119.3(2) YES C(2) C(1) C(6) 123.0(2) YES C(1) C(2) C(3) 117.2(2) YES C(1) C(2) C(21) 121.3(2) YES C(3) C(2) C(21) 121.5(2) YES C(4) C(3) C(2) 121.3(3) YES C(3) C(4) C(5) 119.9(2) YES C(4) C(5) C(6) 121.5(2) YES C(5) C(6) C(1) 117.1(2) YES C(5) C(6) C(61) 121.1(2) YES C(1) C(6) C(61) 121.7(2) YES C(26) C(21) C(22) 118.4(3) YES C(26) C(21) C(2) 121.5(2) YES C(22) C(21) C(2) 120.1(3) YES C(23) C(22) C(21) 120.7(3) YES C(24) C(23) C(22) 120.6(3) YES C(23) C(24) C(25) 119.7(3) YES C(24) C(25) C(26) 120.1(3) YES C(21) C(26) C(25) 120.6(3) YES C(66) C(61) C(62) 118.3(2) YES C(66) C(61) C(6) 122.0(2) YES C(62) C(61) C(6) 119.7(2) YES C(63) C(62) C(61) 121.0(2) YES C(64) C(63) C(62) 119.9(2) YES C(63) C(64) C(65) 119.9(3) YES C(64) C(65) C(66) 120.1(2) YES C(65) C(66) C(61) 120.7(2) YES