# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Eslava, Salvador' _publ_contact_author_email se296@cam.ac.uk _publ_section_title ; Heterometallic cobalt(II)-titanium(IV) oxo cages; key building blocks for hybrid materials ; loop_ _publ_author_name S.Eslava F.Hengesbach M.McPartlin D.S.Wright # Attachment '1.CIF.txt' data_dw0936 _database_code_depnum_ccdc_archive 'CCDC 766941' #TrackingRef '1.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H95 Cl Co O24 Ti7' _chemical_formula_sum 'C38 H95 Cl Co O24 Ti7' _chemical_formula_weight 1365.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0624(1) _cell_length_b 13.6868(1) _cell_length_c 20.1758(3) _cell_angle_alpha 77.100(1) _cell_angle_beta 87.298(1) _cell_angle_gamma 72.081(1) _cell_volume 3088.54(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 111033 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 33.14 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1426 _exptl_absorpt_coefficient_mu 1.229 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; Some of the -OEt groups are poorly resolved: the C-C distances in these groups were assigned a common variable distance for the refinement (final value 1.49(1) Angstrom). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 80300 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 33.18 _reflns_number_total 23022 _reflns_number_gt 13330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+1.0003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23022 _refine_ls_number_parameters 641 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 4.179 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Co1 Co -0.03646(12) 0.58220(10) 0.20470(7) 0.0312(3) Uani 1 1 d . . . Ti1 Ti 0.36651(16) 0.01409(14) 0.27032(9) 0.0308(4) Uani 1 1 d . . . Ti2 Ti 0.08904(15) 0.11605(13) 0.25504(9) 0.0260(4) Uani 1 1 d . . . Ti3 Ti -0.02857(14) 0.34148(13) 0.28651(9) 0.0254(4) Uani 1 1 d . . . Ti4 Ti 0.14350(14) 0.45619(13) 0.32980(9) 0.0244(4) Uani 1 1 d . . . Ti5 Ti 0.22815(14) 0.44121(13) 0.17779(9) 0.0255(4) Uani 1 1 d . . . Ti6 Ti 0.33608(15) 0.21566(14) 0.14885(9) 0.0288(4) Uani 1 1 d . . . Ti7 Ti 0.23829(14) 0.24798(12) 0.29364(8) 0.0226(3) Uani 1 1 d . . . Cl1 Cl -0.1682(3) 0.7373(2) 0.15484(17) 0.0529(8) Uani 1 1 d . . . O01 O 0.0973(5) 0.2153(5) 0.3184(3) 0.0237(13) Uani 1 1 d . . . O1 O 0.2375(5) 0.1502(5) 0.2263(3) 0.0247(13) Uani 1 1 d . . . O2 O 0.1111(5) 0.3972(5) 0.2494(3) 0.0226(12) Uani 1 1 d . . . O02 O 0.3258(5) 0.3030(5) 0.2198(3) 0.0248(13) Uani 1 1 d . . . O11 O 0.3850(7) -0.0684(6) 0.2106(4) 0.046(2) Uani 1 1 d . . . O12 O 0.4751(6) -0.0786(5) 0.3324(4) 0.0407(18) Uani 1 1 d . . . O13 O 0.2194(6) -0.0136(5) 0.3041(4) 0.0321(15) Uani 1 1 d . . . O21 O -0.0116(6) 0.0696(5) 0.3152(4) 0.0338(16) Uani 1 1 d . . . O22 O 0.0612(6) 0.0615(5) 0.1869(4) 0.0343(16) Uani 1 1 d . . . O23 O -0.0178(6) 0.2623(5) 0.2127(3) 0.0295(14) Uani 1 1 d . . . O31 O -0.1512(6) 0.3111(6) 0.3274(4) 0.0366(17) Uani 1 1 d . . . O32 O -0.1205(6) 0.4757(5) 0.2283(4) 0.0318(15) Uani 1 1 d . . . O33 O 0.0065(5) 0.4057(5) 0.3600(3) 0.0276(14) Uani 1 1 d . . . O41 O 0.1817(6) 0.4969(5) 0.4023(3) 0.0308(15) Uani 1 1 d . . . O42 O 0.0258(6) 0.5939(5) 0.2904(4) 0.0306(15) Uani 1 1 d . . . O43 O 0.2500(6) 0.5000(5) 0.2574(3) 0.0284(14) Uani 1 1 d . . . O51 O 0.3302(6) 0.4917(6) 0.1281(4) 0.0363(16) Uani 1 1 d . . . O52 O 0.0903(6) 0.5567(5) 0.1381(3) 0.0316(15) Uani 1 1 d . . . O53 O 0.2061(6) 0.3513(5) 0.1161(3) 0.0276(14) Uani 1 1 d . . . O61 O 0.4510(7) 0.2549(7) 0.0992(4) 0.0448(19) Uani 1 1 d . . . O62 O 0.3005(7) 0.1479(6) 0.0915(4) 0.0379(17) Uani 1 1 d . . . O63 O 0.4587(6) 0.0978(6) 0.2115(4) 0.0361(16) Uani 1 1 d . . . O71 O 0.3517(6) 0.1184(5) 0.3373(3) 0.0291(14) Uani 1 1 d . . . O72 O 0.2500(5) 0.3203(5) 0.3562(3) 0.0258(13) Uani 1 1 d . . . C11 C 0.4728(13) -0.1103(10) 0.1656(7) 0.061(4) Uani 1 1 d D . . H11A H 0.5508 -0.1276 0.1868 0.073 Uiso 1 1 calc R . . H11B H 0.4681 -0.0570 0.1228 0.073 Uiso 1 1 calc R . . C12 C 0.4568(18) -0.2061(13) 0.1506(10) 0.096(6) Uani 1 1 d D . . H12A H 0.5170 -0.2339 0.1195 0.144 Uiso 1 1 calc R . . H12B H 0.3797 -0.1886 0.1294 0.144 Uiso 1 1 calc R . . H12C H 0.4630 -0.2592 0.1930 0.144 Uiso 1 1 calc R . . C13 C 0.5496(12) -0.1825(9) 0.3382(6) 0.052(3) Uani 1 1 d D . . H13A H 0.6088 -0.1837 0.3025 0.062 Uiso 1 1 calc R . . H13B H 0.5036 -0.2283 0.3314 0.062 Uiso 1 1 calc R . . C14 C 0.6090(15) -0.2238(13) 0.4065(7) 0.088(6) Uani 1 1 d D . . H14A H 0.6602 -0.2959 0.4093 0.132 Uiso 1 1 calc R . . H14B H 0.5505 -0.2236 0.4418 0.132 Uiso 1 1 calc R . . H14C H 0.6554 -0.1790 0.4130 0.132 Uiso 1 1 calc R . . C15 C 0.2072(11) -0.1174(8) 0.3198(6) 0.045(3) Uani 1 1 d D . . H15A H 0.2527 -0.1580 0.2874 0.054 Uiso 1 1 calc R . . H15B H 0.1243 -0.1120 0.3142 0.054 Uiso 1 1 calc R . . C16 C 0.2483(14) -0.1756(11) 0.3913(7) 0.066(4) Uani 1 1 d D . . H16A H 0.2382 -0.2457 0.3999 0.099 Uiso 1 1 calc R . . H16B H 0.2025 -0.1363 0.4237 0.099 Uiso 1 1 calc R . . H16C H 0.3308 -0.1826 0.3969 0.099 Uiso 1 1 calc R . . C21 C -0.0132(10) 0.0537(9) 0.3876(5) 0.041(3) Uani 1 1 d D . . H21A H -0.0482 0.1223 0.4003 0.049 Uiso 1 1 calc R . . H21B H 0.0677 0.0240 0.4061 0.049 Uiso 1 1 calc R . . C22 C -0.0818(14) -0.0194(12) 0.4182(7) 0.068(4) Uani 1 1 d D . . H22A H -0.0811 -0.0288 0.4678 0.102 Uiso 1 1 calc R . . H22B H -0.0466 -0.0878 0.4062 0.102 Uiso 1 1 calc R . . H22C H -0.1623 0.0105 0.4007 0.102 Uiso 1 1 calc R . . C23 C 0.0138(12) -0.0154(10) 0.1739(7) 0.055(3) Uani 1 1 d D . . H23A H -0.0456 -0.0250 0.2082 0.066 Uiso 1 1 calc R . . H23B H 0.0765 -0.0834 0.1791 0.066 Uiso 1 1 calc R . . C24 C -0.0408(13) 0.0128(11) 0.1046(7) 0.067(4) Uani 1 1 d D . . H24A H -0.0717 -0.0430 0.0986 0.101 Uiso 1 1 calc R . . H24B H 0.0179 0.0209 0.0703 0.101 Uiso 1 1 calc R . . H24C H -0.1043 0.0792 0.0994 0.101 Uiso 1 1 calc R . . C25 C -0.0805(12) 0.2943(10) 0.1486(7) 0.063(4) Uani 1 1 d D . . H25A H -0.0951 0.3707 0.1307 0.075 Uiso 1 1 calc R . . H25B H -0.0329 0.2567 0.1154 0.075 Uiso 1 1 calc R . . C26 C -0.1914(13) 0.2709(15) 0.1570(11) 0.100(7) Uani 1 1 d D . . H26A H -0.2331 0.2931 0.1130 0.150 Uiso 1 1 calc R . . H26B H -0.2388 0.3090 0.1894 0.150 Uiso 1 1 calc R . . H26C H -0.1767 0.1951 0.1741 0.150 Uiso 1 1 calc R . . C31 C -0.2486(11) 0.2715(12) 0.3375(7) 0.061(4) Uani 1 1 d D . . H31A H -0.2253 0.1991 0.3297 0.073 Uiso 1 1 calc R . . H31B H -0.3117 0.3160 0.3043 0.073 Uiso 1 1 calc R . . C32 C -0.2917(15) 0.2706(16) 0.4072(8) 0.086(5) Uani 1 1 d D . . H32A H -0.3584 0.2430 0.4132 0.129 Uiso 1 1 calc R . . H32B H -0.3160 0.3424 0.4147 0.129 Uiso 1 1 calc R . . H32C H -0.2295 0.2257 0.4400 0.129 Uiso 1 1 calc R . . C33 C -0.2457(9) 0.5170(9) 0.2252(7) 0.046(3) Uani 1 1 d D . . H33A H -0.2792 0.4588 0.2273 0.055 Uiso 1 1 calc R . . H33B H -0.2708 0.5679 0.1813 0.055 Uiso 1 1 calc R . . C34 C -0.2911(11) 0.5708(11) 0.2827(8) 0.061(4) Uani 1 1 d D . . H34A H -0.3763 0.5980 0.2792 0.091 Uiso 1 1 calc R . . H34B H -0.2591 0.6293 0.2801 0.091 Uiso 1 1 calc R . . H34C H -0.2674 0.5203 0.3262 0.091 Uiso 1 1 calc R . . C35 C -0.0470(10) 0.4114(9) 0.4244(6) 0.044(3) Uani 1 1 d D . . H35A H -0.1310 0.4202 0.4198 0.053 Uiso 1 1 calc R . . H35B H -0.0395 0.4736 0.4389 0.053 Uiso 1 1 calc R . . C36 C 0.0079(14) 0.3145(12) 0.4774(7) 0.069(4) Uani 1 1 d D . . H36A H -0.0307 0.3207 0.5208 0.104 Uiso 1 1 calc R . . H36B H 0.0908 0.3064 0.4827 0.104 Uiso 1 1 calc R . . H36C H -0.0005 0.2530 0.4635 0.104 Uiso 1 1 calc R . . C41 C 0.2542(9) 0.4492(8) 0.4603(5) 0.036(2) Uani 1 1 d D . . H41A H 0.3042 0.3788 0.4554 0.044 Uiso 1 1 calc R . . H41B H 0.2053 0.4391 0.5005 0.044 Uiso 1 1 calc R . . C42 C 0.3303(11) 0.5121(10) 0.4724(7) 0.054(3) Uani 1 1 d D . . H42A H 0.3791 0.4750 0.5133 0.081 Uiso 1 1 calc R . . H42B H 0.2814 0.5812 0.4786 0.081 Uiso 1 1 calc R . . H42C H 0.3801 0.5213 0.4332 0.081 Uiso 1 1 calc R . . C43 C 0.0285(10) 0.6935(8) 0.2998(7) 0.045(3) Uani 1 1 d D . . H43A H 0.0481 0.7344 0.2564 0.054 Uiso 1 1 calc R . . H43B H 0.0901 0.6824 0.3339 0.054 Uiso 1 1 calc R . . C44 C -0.0853(13) 0.7544(12) 0.3230(9) 0.075(5) Uani 1 1 d . . . H44A H -0.0810 0.8227 0.3280 0.112 Uiso 1 1 calc R . . H44B H -0.1035 0.7152 0.3668 0.112 Uiso 1 1 calc R . . H44C H -0.1465 0.7653 0.2894 0.112 Uiso 1 1 calc R . . C45 C 0.3436(10) 0.5380(10) 0.2698(6) 0.049(3) Uani 1 1 d D . . H45A H 0.3182 0.5859 0.3016 0.059 Uiso 1 1 calc R . . H45B H 0.3649 0.5782 0.2266 0.059 Uiso 1 1 calc R . . C46 C 0.4461(11) 0.4489(12) 0.2993(8) 0.065(4) Uani 1 1 d D . . H46A H 0.5092 0.4759 0.3080 0.097 Uiso 1 1 calc R . . H46B H 0.4723 0.4025 0.2673 0.097 Uiso 1 1 calc R . . H46C H 0.4249 0.4093 0.3421 0.097 Uiso 1 1 calc R . . C51 C 0.4157(11) 0.5104(14) 0.0818(7) 0.066(4) Uani 1 1 d D . . H51A H 0.3885 0.5841 0.0557 0.080 Uiso 1 1 calc R . . H51B H 0.4267 0.4639 0.0493 0.080 Uiso 1 1 calc R . . C52 C 0.5276(11) 0.4916(16) 0.1155(8) 0.076(5) Uani 1 1 d D . . H52A H 0.5844 0.5055 0.0812 0.114 Uiso 1 1 calc R . . H52B H 0.5557 0.4183 0.1407 0.114 Uiso 1 1 calc R . . H52C H 0.5176 0.5386 0.1470 0.114 Uiso 1 1 calc R . . C53 C 0.0905(11) 0.6381(8) 0.0788(6) 0.042(3) Uani 1 1 d D . . H53A H 0.0116 0.6671 0.0574 0.050 Uiso 1 1 calc R . . H53B H 0.1451 0.6073 0.0454 0.050 Uiso 1 1 calc R . . C54 C 0.1259(13) 0.7256(9) 0.0962(7) 0.059(4) Uani 1 1 d D . . H54A H 0.1249 0.7793 0.0547 0.088 Uiso 1 1 calc R . . H54B H 0.2047 0.6975 0.1165 0.088 Uiso 1 1 calc R . . H54C H 0.0713 0.7572 0.1286 0.088 Uiso 1 1 calc R . . C55 C 0.1406(9) 0.3809(8) 0.0535(5) 0.036(2) Uani 1 1 d D . . H55A H 0.0724 0.4431 0.0549 0.044 Uiso 1 1 calc R . . H55B H 0.1112 0.3226 0.0490 0.044 Uiso 1 1 calc R . . C56 C 0.2107(11) 0.4065(10) -0.0077(5) 0.046(3) Uani 1 1 d D . . H56A H 0.1617 0.4261 -0.0489 0.070 Uiso 1 1 calc R . . H56B H 0.2775 0.3448 -0.0100 0.070 Uiso 1 1 calc R . . H56C H 0.2385 0.4653 -0.0041 0.070 Uiso 1 1 calc R . . C61 C 0.5067(13) 0.225(2) 0.0405(10) 0.102(7) Uani 1 1 d D . . H61A H 0.4873 0.1620 0.0344 0.122 Uiso 1 1 calc R . . H61B H 0.4743 0.2822 0.0005 0.122 Uiso 1 1 calc R . . C62 C 0.6305(13) 0.2010(17) 0.0414(10) 0.099(7) Uani 1 1 d D . . H62A H 0.6613 0.1811 -0.0011 0.148 Uiso 1 1 calc R . . H62B H 0.6641 0.1426 0.0799 0.148 Uiso 1 1 calc R . . H62C H 0.6511 0.2631 0.0460 0.148 Uiso 1 1 calc R . . C63 C 0.2405(12) 0.0937(11) 0.0623(7) 0.055(3) Uani 1 1 d D . . H63A H 0.1586 0.1379 0.0521 0.066 Uiso 1 1 calc R . . H63B H 0.2403 0.0280 0.0950 0.066 Uiso 1 1 calc R . . C64 C 0.2973(16) 0.0678(13) -0.0018(7) 0.082(5) Uani 1 1 d D . . H64A H 0.2546 0.0303 -0.0215 0.123 Uiso 1 1 calc R . . H64B H 0.3780 0.0231 0.0085 0.123 Uiso 1 1 calc R . . H64C H 0.2966 0.1329 -0.0343 0.123 Uiso 1 1 calc R . . C65 C 0.5620(11) 0.1206(11) 0.2353(7) 0.061(4) Uani 1 1 d D . . H65A H 0.5754 0.1815 0.2027 0.074 Uiso 1 1 calc R . . H65B H 0.5457 0.1397 0.2801 0.074 Uiso 1 1 calc R . . C66 C 0.6677(12) 0.0296(13) 0.2413(12) 0.098(7) Uani 1 1 d D . . H66A H 0.7332 0.0470 0.2573 0.147 Uiso 1 1 calc R . . H66B H 0.6853 0.0117 0.1968 0.147 Uiso 1 1 calc R . . H66C H 0.6549 -0.0307 0.2738 0.147 Uiso 1 1 calc R . . C71 C 0.4038(9) 0.0961(9) 0.4034(5) 0.039(2) Uani 1 1 d D . . H71A H 0.4163 0.1607 0.4117 0.046 Uiso 1 1 calc R . . H71B H 0.4807 0.0419 0.4055 0.046 Uiso 1 1 calc R . . C72 C 0.3285(12) 0.0581(12) 0.4573(6) 0.060(4) Uani 1 1 d D . . H72A H 0.3660 0.0434 0.5020 0.091 Uiso 1 1 calc R . . H72B H 0.3172 -0.0064 0.4495 0.091 Uiso 1 1 calc R . . H72C H 0.2528 0.1122 0.4557 0.091 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0311(7) 0.0263(7) 0.0342(8) -0.0064(5) -0.0064(5) -0.0051(5) Ti1 0.0333(9) 0.0246(9) 0.0273(9) -0.0056(7) -0.0017(7) 0.0021(7) Ti2 0.0306(9) 0.0217(8) 0.0264(8) -0.0072(6) 0.0006(6) -0.0077(7) Ti3 0.0218(8) 0.0238(8) 0.0319(9) -0.0096(7) 0.0023(6) -0.0066(6) Ti4 0.0256(8) 0.0231(8) 0.0250(8) -0.0070(6) -0.0010(6) -0.0068(6) Ti5 0.0271(8) 0.0251(8) 0.0239(8) -0.0027(6) 0.0001(6) -0.0093(7) Ti6 0.0289(9) 0.0295(9) 0.0235(8) -0.0060(7) 0.0038(6) -0.0027(7) Ti7 0.0226(8) 0.0221(8) 0.0217(8) -0.0048(6) 0.0004(6) -0.0047(6) Cl1 0.0514(17) 0.0341(15) 0.060(2) -0.0034(13) -0.0169(14) 0.0043(12) O01 0.026(3) 0.021(3) 0.025(3) -0.006(2) 0.003(2) -0.007(2) O1 0.025(3) 0.022(3) 0.024(3) -0.005(2) 0.000(2) -0.003(3) O2 0.022(3) 0.022(3) 0.024(3) -0.006(2) 0.000(2) -0.006(2) O02 0.021(3) 0.026(3) 0.024(3) -0.004(3) 0.001(2) -0.005(3) O11 0.057(5) 0.036(4) 0.038(4) -0.017(3) 0.001(4) 0.003(4) O12 0.042(4) 0.027(4) 0.040(4) -0.005(3) -0.007(3) 0.007(3) O13 0.041(4) 0.020(3) 0.032(4) -0.002(3) -0.001(3) -0.007(3) O21 0.040(4) 0.032(4) 0.034(4) -0.009(3) 0.006(3) -0.018(3) O22 0.043(4) 0.030(4) 0.033(4) -0.013(3) -0.002(3) -0.012(3) O23 0.031(3) 0.025(3) 0.031(4) -0.008(3) -0.006(3) -0.004(3) O31 0.025(3) 0.039(4) 0.050(5) -0.016(3) 0.009(3) -0.013(3) O32 0.023(3) 0.025(3) 0.046(4) -0.012(3) -0.004(3) -0.002(3) O33 0.028(3) 0.027(3) 0.029(3) -0.012(3) 0.007(3) -0.008(3) O41 0.035(4) 0.029(4) 0.029(4) -0.010(3) -0.005(3) -0.007(3) O42 0.034(4) 0.021(3) 0.035(4) -0.009(3) -0.005(3) -0.004(3) O43 0.030(3) 0.032(4) 0.028(3) -0.006(3) 0.000(3) -0.016(3) O51 0.041(4) 0.041(4) 0.030(4) -0.002(3) 0.005(3) -0.021(3) O52 0.038(4) 0.024(3) 0.029(4) 0.000(3) -0.005(3) -0.007(3) O53 0.030(3) 0.028(3) 0.023(3) -0.004(3) -0.002(3) -0.007(3) O61 0.037(4) 0.060(5) 0.034(4) -0.009(4) 0.014(3) -0.013(4) O62 0.047(4) 0.036(4) 0.029(4) -0.013(3) 0.003(3) -0.006(3) O63 0.028(4) 0.039(4) 0.032(4) -0.007(3) 0.002(3) 0.002(3) O71 0.030(3) 0.027(3) 0.024(3) -0.005(3) -0.005(3) 0.000(3) O72 0.028(3) 0.024(3) 0.023(3) -0.007(3) -0.003(2) -0.005(3) C11 0.072(9) 0.056(8) 0.040(7) -0.019(6) 0.004(6) 0.007(7) C12 0.136(17) 0.068(11) 0.080(13) -0.048(10) 0.011(11) -0.004(11) C13 0.059(8) 0.032(6) 0.047(7) -0.006(5) -0.008(6) 0.010(5) C14 0.098(13) 0.068(10) 0.055(9) -0.003(8) -0.031(9) 0.034(9) C15 0.062(8) 0.023(5) 0.049(7) -0.003(5) -0.002(6) -0.013(5) C16 0.076(10) 0.043(8) 0.067(10) 0.018(7) -0.011(8) -0.020(7) C21 0.054(7) 0.042(6) 0.032(6) -0.009(5) 0.009(5) -0.025(5) C22 0.106(12) 0.072(10) 0.048(8) -0.012(7) 0.022(8) -0.062(10) C23 0.070(9) 0.042(7) 0.061(9) -0.020(6) -0.014(7) -0.021(6) C24 0.072(10) 0.058(9) 0.077(10) -0.032(8) -0.028(8) -0.012(7) C25 0.072(9) 0.040(7) 0.068(9) -0.022(6) -0.030(7) 0.007(6) C26 0.063(11) 0.099(14) 0.146(19) -0.071(14) -0.028(11) -0.001(10) C31 0.040(7) 0.070(9) 0.078(10) -0.015(8) 0.012(7) -0.026(7) C32 0.068(11) 0.115(15) 0.084(13) -0.029(11) 0.030(9) -0.041(10) C33 0.024(5) 0.036(6) 0.077(9) -0.016(6) -0.011(5) -0.003(4) C34 0.034(6) 0.047(7) 0.100(12) -0.028(8) 0.012(7) -0.005(5) C35 0.043(6) 0.060(8) 0.041(6) -0.027(6) 0.017(5) -0.024(6) C36 0.085(11) 0.098(12) 0.033(7) -0.001(7) 0.003(7) -0.049(10) C41 0.042(6) 0.036(6) 0.030(5) -0.011(4) -0.005(4) -0.007(5) C42 0.059(8) 0.062(8) 0.049(8) -0.014(6) -0.015(6) -0.025(7) C43 0.051(7) 0.028(5) 0.058(8) -0.014(5) -0.011(6) -0.011(5) C44 0.069(10) 0.057(9) 0.095(12) -0.048(9) -0.020(9) 0.012(7) C45 0.047(7) 0.074(9) 0.043(7) -0.021(6) 0.008(5) -0.038(7) C46 0.050(8) 0.091(11) 0.062(9) -0.015(8) -0.007(7) -0.033(8) C51 0.061(9) 0.101(12) 0.046(8) -0.002(8) 0.014(6) -0.049(9) C52 0.042(7) 0.139(16) 0.056(9) -0.029(10) 0.016(6) -0.038(9) C53 0.055(7) 0.030(5) 0.033(6) 0.003(4) -0.005(5) -0.008(5) C54 0.077(10) 0.032(6) 0.066(9) 0.000(6) 0.003(7) -0.021(6) C55 0.043(6) 0.034(5) 0.031(5) -0.006(4) -0.010(4) -0.010(5) C56 0.061(8) 0.048(7) 0.026(5) -0.004(5) -0.002(5) -0.012(6) C61 0.070(11) 0.18(2) 0.080(13) -0.069(14) 0.046(10) -0.051(13) C62 0.060(10) 0.137(18) 0.096(15) -0.062(13) 0.021(10) -0.003(11) C63 0.059(8) 0.051(8) 0.060(9) -0.025(7) -0.004(6) -0.013(6) C64 0.131(15) 0.064(10) 0.045(8) -0.025(7) -0.013(9) -0.008(10) C65 0.042(7) 0.078(10) 0.052(8) 0.000(7) 0.002(6) -0.011(7) C66 0.042(8) 0.085(12) 0.144(19) 0.011(12) -0.005(10) -0.012(8) C71 0.042(6) 0.036(6) 0.031(5) -0.007(4) -0.012(4) 0.000(5) C72 0.076(10) 0.071(9) 0.028(6) -0.002(6) -0.005(6) -0.020(8) _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_site_symmetry_2 _geom_bond_publ_flag Co1 O42 1.976(7) . ? Co1 O32 1.983(7) . ? Co1 O52 1.988(7) . ? Co1 Cl1 2.272(3) . ? Ti1 O11 1.790(8) . ? Ti1 O12 1.821(7) . ? Ti1 O13 1.985(7) . ? Ti1 O63 2.002(8) . ? Ti1 O1 2.071(6) . ? Ti1 O71 2.139(7) . ? Ti1 Ti6 3.193(2) . ? Ti1 Ti2 3.206(2) . ? Ti1 Ti7 3.228(2) . ? Ti2 O22 1.794(7) . ? Ti2 O21 1.828(7) . ? Ti2 O1 2.015(6) . ? Ti2 O23 2.038(6) . ? Ti2 O13 2.060(7) . ? Ti2 O01 2.087(6) . ? Ti2 Ti7 3.141(2) . ? Ti2 Ti3 3.167(2) . ? Ti3 O31 1.776(7) . ? Ti3 O01 1.919(6) . ? Ti3 O32 1.973(7) . ? Ti3 O33 2.006(7) . ? Ti3 O23 2.006(7) . ? Ti3 O2 2.098(6) . ? Ti3 Ti7 3.074(2) . ? Ti3 Ti4 3.213(2) . ? Ti4 O41 1.802(7) . ? Ti4 O72 1.883(6) . ? Ti4 O42 1.998(6) . ? Ti4 O33 2.000(7) . ? Ti4 O43 2.013(7) . ? Ti4 O2 2.068(6) . ? Ti4 Ti7 2.967(2) . ? Ti4 Ti5 3.217(2) . ? Ti5 O51 1.759(7) . ? Ti5 O02 1.921(6) . ? Ti5 O52 1.961(7) . ? Ti5 O43 2.010(7) . ? Ti5 O53 2.013(7) . ? Ti5 O2 2.094(6) . ? Ti5 Ti7 3.089(2) . ? Ti5 Ti6 3.135(2) . ? Ti6 O62 1.775(7) . ? Ti6 O61 1.817(8) . ? Ti6 O53 2.024(6) . ? Ti6 O02 2.036(6) . ? Ti6 O63 2.046(7) . ? Ti6 O1 2.124(7) . ? Ti6 Ti7 3.170(2) . ? Ti7 O72 1.804(6) . ? Ti7 O01 1.906(6) . ? Ti7 O71 1.927(6) . ? Ti7 O02 1.934(6) . ? Ti7 O1 2.111(6) . ? Ti7 O2 2.170(6) . ? O11 C11 1.429(14) . ? O12 C13 1.412(13) . ? O13 C15 1.437(12) . ? O21 C21 1.428(12) . ? O22 C23 1.418(13) . ? O23 C25 1.439(14) . ? O31 C31 1.427(13) . ? O32 C33 1.439(11) . ? O33 C35 1.430(12) . ? O41 C41 1.402(11) . ? O42 C43 1.427(12) . ? O43 C45 1.433(12) . ? O51 C51 1.402(13) . ? O52 C53 1.443(12) . ? O53 C55 1.433(11) . ? O61 C61 1.413(16) . ? O62 C63 1.410(14) . ? O63 C65 1.498(15) . ? O71 C71 1.431(11) . ? C11 C12 1.478(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.491(14) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.508(13) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 C22 1.501(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.492(14) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.463(15) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C32 1.475(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.505(14) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.493(14) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C41 C42 1.498(13) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.485(18) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.479(14) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C51 C52 1.465(14) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.502(13) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.500(12) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C61 C62 1.428(15) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.497(14) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.470(14) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C71 C72 1.491(13) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O42 Co1 O32 107.4(3) . . ? O42 Co1 O52 110.0(3) . . ? O32 Co1 O52 116.5(3) . . ? O42 Co1 Cl1 110.4(2) . . ? O32 Co1 Cl1 107.4(2) . . ? O52 Co1 Cl1 105.2(2) . . ? O11 Ti1 O12 96.4(4) . . ? O11 Ti1 O13 92.6(4) . . ? O12 Ti1 O13 103.0(3) . . ? O11 Ti1 O63 90.1(4) . . ? O12 Ti1 O63 102.8(3) . . ? O13 Ti1 O63 153.6(3) . . ? O11 Ti1 O1 104.2(3) . . ? O12 Ti1 O1 159.4(3) . . ? O13 Ti1 O1 76.0(3) . . ? O63 Ti1 O1 77.9(3) . . ? O11 Ti1 O71 176.0(4) . . ? O12 Ti1 O71 84.4(3) . . ? O13 Ti1 O71 91.0(3) . . ? O63 Ti1 O71 85.9(3) . . ? O1 Ti1 O71 75.1(2) . . ? O11 Ti1 Ti6 90.6(3) . . ? O12 Ti1 Ti6 140.7(3) . . ? O13 Ti1 Ti6 115.3(2) . . ? O63 Ti1 Ti6 38.41(19) . . ? O1 Ti1 Ti6 41.07(18) . . ? O71 Ti1 Ti6 86.40(18) . . ? O11 Ti1 Ti2 98.0(3) . . ? O12 Ti1 Ti2 139.1(3) . . ? O13 Ti1 Ti2 38.42(19) . . ? O63 Ti1 Ti2 115.2(2) . . ? O1 Ti1 Ti2 37.70(18) . . ? O71 Ti1 Ti2 83.80(18) . . ? Ti6 Ti1 Ti2 77.16(6) . . ? O11 Ti1 Ti7 143.7(3) . . ? O12 Ti1 Ti7 119.6(2) . . ? O13 Ti1 Ti7 84.2(2) . . ? O63 Ti1 Ti7 78.2(2) . . ? O1 Ti1 Ti7 39.93(18) . . ? O71 Ti1 Ti7 35.23(17) . . ? Ti6 Ti1 Ti7 59.18(5) . . ? Ti2 Ti1 Ti7 58.46(5) . . ? O22 Ti2 O21 96.8(3) . . ? O22 Ti2 O1 102.3(3) . . ? O21 Ti2 O1 155.6(3) . . ? O22 Ti2 O23 92.7(3) . . ? O21 Ti2 O23 99.3(3) . . ? O1 Ti2 O23 94.8(3) . . ? O22 Ti2 O13 97.5(3) . . ? O21 Ti2 O13 87.1(3) . . ? O1 Ti2 O13 75.6(3) . . ? O23 Ti2 O13 167.2(3) . . ? O22 Ti2 O01 165.4(3) . . ? O21 Ti2 O01 87.6(3) . . ? O1 Ti2 O01 77.7(2) . . ? O23 Ti2 O01 72.9(2) . . ? O13 Ti2 O01 96.6(3) . . ? O22 Ti2 Ti7 141.9(2) . . ? O21 Ti2 Ti7 121.2(2) . . ? O1 Ti2 Ti7 41.56(18) . . ? O23 Ti2 Ti7 81.87(19) . . ? O13 Ti2 Ti7 85.4(2) . . ? O01 Ti2 Ti7 36.12(17) . . ? O22 Ti2 Ti3 130.1(2) . . ? O21 Ti2 Ti3 87.2(2) . . ? O1 Ti2 Ti3 91.89(18) . . ? O23 Ti2 Ti3 38.09(19) . . ? O13 Ti2 Ti3 132.4(2) . . ? O01 Ti2 Ti3 35.94(17) . . ? Ti7 Ti2 Ti3 58.31(5) . . ? O22 Ti2 Ti1 99.8(2) . . ? O21 Ti2 Ti1 122.9(2) . . ? O1 Ti2 Ti1 38.94(17) . . ? O23 Ti2 Ti1 133.6(2) . . ? O13 Ti2 Ti1 36.8(2) . . ? O01 Ti2 Ti1 89.28(17) . . ? Ti7 Ti2 Ti1 61.13(5) . . ? Ti3 Ti2 Ti1 119.36(7) . . ? O31 Ti3 O01 103.0(3) . . ? O31 Ti3 O32 94.9(3) . . ? O01 Ti3 O32 160.4(3) . . ? O31 Ti3 O33 94.6(3) . . ? O01 Ti3 O33 91.0(3) . . ? O32 Ti3 O33 95.5(3) . . ? O31 Ti3 O23 97.2(3) . . ? O01 Ti3 O23 77.2(3) . . ? O32 Ti3 O23 92.9(3) . . ? O33 Ti3 O23 164.9(3) . . ? O31 Ti3 O2 169.6(3) . . ? O01 Ti3 O2 81.2(2) . . ? O32 Ti3 O2 82.5(3) . . ? O33 Ti3 O2 75.8(3) . . ? O23 Ti3 O2 93.0(3) . . ? O31 Ti3 Ti7 138.3(3) . . ? O01 Ti3 Ti7 36.38(18) . . ? O32 Ti3 Ti7 126.7(2) . . ? O33 Ti3 Ti7 80.80(19) . . ? O23 Ti3 Ti7 84.12(19) . . ? O2 Ti3 Ti7 44.87(16) . . ? O31 Ti3 Ti2 95.4(2) . . ? O01 Ti3 Ti2 39.66(19) . . ? O32 Ti3 Ti2 131.5(2) . . ? O33 Ti3 Ti2 130.6(2) . . ? O23 Ti3 Ti2 38.79(18) . . ? O2 Ti3 Ti2 93.84(17) . . ? Ti7 Ti3 Ti2 60.42(5) . . ? O31 Ti3 Ti4 131.2(3) . . ? O01 Ti3 Ti4 84.01(19) . . ? O32 Ti3 Ti4 90.2(2) . . ? O33 Ti3 Ti4 36.60(18) . . ? O23 Ti3 Ti4 131.1(2) . . ? O2 Ti3 Ti4 39.19(17) . . ? Ti7 Ti3 Ti4 56.28(5) . . ? Ti2 Ti3 Ti4 116.66(6) . . ? O41 Ti4 O72 92.5(3) . . ? O41 Ti4 O42 95.4(3) . . ? O72 Ti4 O42 172.1(3) . . ? O41 Ti4 O33 104.2(3) . . ? O72 Ti4 O33 92.7(3) . . ? O42 Ti4 O33 85.6(3) . . ? O41 Ti4 O43 103.3(3) . . ? O72 Ti4 O43 91.8(3) . . ? O42 Ti4 O43 86.0(3) . . ? O33 Ti4 O43 151.8(3) . . ? O41 Ti4 O2 175.0(3) . . ? O72 Ti4 O2 82.5(3) . . ? O42 Ti4 O2 89.6(3) . . ? O33 Ti4 O2 76.6(3) . . ? O43 Ti4 O2 76.5(3) . . ? O41 Ti4 Ti7 128.0(2) . . ? O72 Ti4 Ti7 35.52(19) . . ? O42 Ti4 Ti7 136.6(2) . . ? O33 Ti4 Ti7 83.68(19) . . ? O43 Ti4 Ti7 84.0(2) . . ? O2 Ti4 Ti7 46.98(17) . . ? O41 Ti4 Ti3 140.5(2) . . ? O72 Ti4 Ti3 85.95(19) . . ? O42 Ti4 Ti3 88.1(2) . . ? O33 Ti4 Ti3 36.73(19) . . ? O43 Ti4 Ti3 116.14(19) . . ? O2 Ti4 Ti3 39.86(17) . . ? Ti7 Ti4 Ti3 59.49(5) . . ? O41 Ti4 Ti5 139.8(2) . . ? O72 Ti4 Ti5 85.5(2) . . ? O42 Ti4 Ti5 88.3(2) . . ? O33 Ti4 Ti5 116.0(2) . . ? O43 Ti4 Ti5 36.89(19) . . ? O2 Ti4 Ti5 39.67(17) . . ? Ti7 Ti4 Ti5 59.77(5) . . ? Ti3 Ti4 Ti5 79.45(6) . . ? O51 Ti5 O02 100.7(3) . . ? O51 Ti5 O52 95.9(3) . . ? O02 Ti5 O52 160.8(3) . . ? O51 Ti5 O43 93.5(3) . . ? O02 Ti5 O43 92.1(3) . . ? O52 Ti5 O43 96.5(3) . . ? O51 Ti5 O53 97.0(3) . . ? O02 Ti5 O53 76.8(3) . . ? O52 Ti5 O53 91.7(3) . . ? O43 Ti5 O53 165.9(3) . . ? O51 Ti5 O2 169.5(3) . . ? O02 Ti5 O2 81.4(2) . . ? O52 Ti5 O2 84.1(3) . . ? O43 Ti5 O2 76.0(3) . . ? O53 Ti5 O2 93.5(3) . . ? O51 Ti5 Ti7 136.1(3) . . ? O02 Ti5 Ti7 36.89(19) . . ? O52 Ti5 Ti7 128.0(2) . . ? O43 Ti5 Ti7 80.90(19) . . ? O53 Ti5 Ti7 85.01(19) . . ? O2 Ti5 Ti7 44.56(16) . . ? O51 Ti5 Ti6 93.5(3) . . ? O02 Ti5 Ti6 38.93(19) . . ? O52 Ti5 Ti6 130.8(2) . . ? O43 Ti5 Ti6 130.9(2) . . ? O53 Ti5 Ti6 39.20(18) . . ? O2 Ti5 Ti6 94.47(17) . . ? Ti7 Ti5 Ti6 61.25(5) . . ? O51 Ti5 Ti4 130.5(3) . . ? O02 Ti5 Ti4 84.89(19) . . ? O52 Ti5 Ti4 91.7(2) . . ? O43 Ti5 Ti4 36.95(19) . . ? O53 Ti5 Ti4 131.7(2) . . ? O2 Ti5 Ti4 39.09(17) . . ? Ti7 Ti5 Ti4 56.10(5) . . ? Ti6 Ti5 Ti4 117.30(7) . . ? O62 Ti6 O61 96.9(4) . . ? O62 Ti6 O53 95.2(3) . . ? O61 Ti6 O53 96.9(3) . . ? O62 Ti6 O02 163.1(3) . . ? O61 Ti6 O02 97.3(3) . . ? O53 Ti6 O02 74.0(2) . . ? O62 Ti6 O63 102.1(3) . . ? O61 Ti6 O63 90.1(3) . . ? O53 Ti6 O63 160.4(3) . . ? O02 Ti6 O63 87.0(3) . . ? O62 Ti6 O1 91.0(3) . . ? O61 Ti6 O1 165.0(3) . . ? O53 Ti6 O1 95.0(3) . . ? O02 Ti6 O1 77.3(2) . . ? O63 Ti6 O1 75.8(3) . . ? O62 Ti6 Ti5 134.1(2) . . ? O61 Ti6 Ti5 91.5(3) . . ? O53 Ti6 Ti5 38.93(19) . . ? O02 Ti6 Ti5 36.36(17) . . ? O63 Ti6 Ti5 123.0(2) . . ? O1 Ti6 Ti5 92.09(17) . . ? O62 Ti6 Ti7 131.3(3) . . ? O61 Ti6 Ti7 131.7(3) . . ? O53 Ti6 Ti7 82.66(19) . . ? O02 Ti6 Ti7 35.91(18) . . ? O63 Ti6 Ti7 79.1(2) . . ? O1 Ti6 Ti7 41.37(17) . . ? Ti5 Ti6 Ti7 58.66(5) . . ? O62 Ti6 Ti1 90.4(3) . . ? O61 Ti6 Ti1 127.0(3) . . ? O53 Ti6 Ti1 134.7(2) . . ? O02 Ti6 Ti1 88.34(18) . . ? O63 Ti6 Ti1 37.4(2) . . ? O1 Ti6 Ti1 39.82(16) . . ? Ti5 Ti6 Ti1 119.45(7) . . ? Ti7 Ti6 Ti1 60.96(5) . . ? O72 Ti7 O01 101.8(3) . . ? O72 Ti7 O71 95.4(3) . . ? O01 Ti7 O71 100.6(3) . . ? O72 Ti7 O02 101.6(3) . . ? O01 Ti7 O02 145.5(3) . . ? O71 Ti7 O02 102.0(3) . . ? O72 Ti7 O1 174.2(3) . . ? O01 Ti7 O1 79.5(3) . . ? O71 Ti7 O1 78.8(3) . . ? O02 Ti7 O1 79.8(3) . . ? O72 Ti7 O2 81.5(3) . . ? O01 Ti7 O2 79.6(2) . . ? O71 Ti7 O2 176.9(3) . . ? O02 Ti7 O2 79.1(2) . . ? O1 Ti7 O2 104.3(2) . . ? O72 Ti7 Ti4 37.32(19) . . ? O01 Ti7 Ti4 91.44(19) . . ? O71 Ti7 Ti4 132.7(2) . . ? O02 Ti7 Ti4 91.97(19) . . ? O1 Ti7 Ti4 148.49(17) . . ? O2 Ti7 Ti4 44.17(16) . . ? O72 Ti7 Ti3 91.6(2) . . ? O01 Ti7 Ti3 36.68(18) . . ? O71 Ti7 Ti3 137.1(2) . . ? O02 Ti7 Ti3 117.89(19) . . ? O1 Ti7 Ti3 92.69(17) . . ? O2 Ti7 Ti3 43.00(16) . . ? Ti4 Ti7 Ti3 64.24(5) . . ? O72 Ti7 Ti5 90.7(2) . . ? O01 Ti7 Ti5 118.37(19) . . ? O71 Ti7 Ti5 138.3(2) . . ? O02 Ti7 Ti5 36.62(18) . . ? O1 Ti7 Ti5 93.64(18) . . ? O2 Ti7 Ti5 42.61(16) . . ? Ti4 Ti7 Ti5 64.13(6) . . ? Ti3 Ti7 Ti5 83.65(6) . . ? O72 Ti7 Ti2 141.6(2) . . ? O01 Ti7 Ti2 40.21(19) . . ? O71 Ti7 Ti2 89.0(2) . . ? O02 Ti7 Ti2 114.8(2) . . ? O1 Ti7 Ti2 39.28(17) . . ? O2 Ti7 Ti2 93.13(16) . . ? Ti4 Ti7 Ti2 125.46(7) . . ? Ti3 Ti7 Ti2 61.27(5) . . ? Ti5 Ti7 Ti2 110.81(6) . . ? O72 Ti7 Ti6 139.4(2) . . ? O01 Ti7 Ti6 116.5(2) . . ? O71 Ti7 Ti6 90.7(2) . . ? O02 Ti7 Ti6 38.14(19) . . ? O1 Ti7 Ti6 41.69(17) . . ? O2 Ti7 Ti6 91.96(17) . . ? Ti4 Ti7 Ti6 124.16(7) . . ? Ti3 Ti7 Ti6 110.58(7) . . ? Ti5 Ti7 Ti6 60.09(5) . . ? Ti2 Ti7 Ti6 78.42(6) . . ? O72 Ti7 Ti1 135.2(2) . . ? O01 Ti7 Ti1 91.92(19) . . ? O71 Ti7 Ti1 39.8(2) . . ? O02 Ti7 Ti1 89.11(19) . . ? O1 Ti7 Ti1 39.03(16) . . ? O2 Ti7 Ti1 143.28(17) . . ? Ti4 Ti7 Ti1 172.42(7) . . ? Ti3 Ti7 Ti1 121.61(7) . . ? Ti5 Ti7 Ti1 119.78(7) . . ? Ti2 Ti7 Ti1 60.42(5) . . ? Ti6 Ti7 Ti1 59.86(5) . . ? Ti7 O01 Ti3 106.9(3) . . ? Ti7 O01 Ti2 103.7(3) . . ? Ti3 O01 Ti2 104.4(3) . . ? Ti2 O1 Ti1 103.4(3) . . ? Ti2 O1 Ti7 99.2(3) . . ? Ti1 O1 Ti7 101.0(3) . . ? Ti2 O1 Ti6 149.2(3) . . ? Ti1 O1 Ti6 99.1(3) . . ? Ti7 O1 Ti6 96.9(3) . . ? Ti4 O2 Ti5 101.2(3) . . ? Ti4 O2 Ti3 100.9(3) . . ? Ti5 O2 Ti3 157.4(3) . . ? Ti4 O2 Ti7 88.8(2) . . ? Ti5 O2 Ti7 92.8(2) . . ? Ti3 O2 Ti7 92.1(2) . . ? Ti5 O02 Ti7 106.5(3) . . ? Ti5 O02 Ti6 104.7(3) . . ? Ti7 O02 Ti6 106.0(3) . . ? C11 O11 Ti1 137.4(8) . . ? C13 O12 Ti1 135.5(7) . . ? C15 O13 Ti1 122.5(7) . . ? C15 O13 Ti2 122.1(6) . . ? Ti1 O13 Ti2 104.8(3) . . ? C21 O21 Ti2 129.8(6) . . ? C23 O22 Ti2 141.3(8) . . ? C25 O23 Ti3 129.5(7) . . ? C25 O23 Ti2 127.0(7) . . ? Ti3 O23 Ti2 103.1(3) . . ? C31 O31 Ti3 158.1(8) . . ? C33 O32 Ti3 125.6(7) . . ? C33 O32 Co1 115.5(6) . . ? Ti3 O32 Co1 113.8(3) . . ? C35 O33 Ti4 123.9(6) . . ? C35 O33 Ti3 129.4(6) . . ? Ti4 O33 Ti3 106.7(3) . . ? C41 O41 Ti4 136.3(6) . . ? C43 O42 Co1 120.4(6) . . ? C43 O42 Ti4 124.7(6) . . ? Co1 O42 Ti4 108.0(3) . . ? C45 O43 Ti5 127.7(7) . . ? C45 O43 Ti4 123.9(7) . . ? Ti5 O43 Ti4 106.2(3) . . ? C51 O51 Ti5 166.0(9) . . ? C53 O52 Ti5 124.9(7) . . ? C53 O52 Co1 119.7(6) . . ? Ti5 O52 Co1 112.0(3) . . ? C55 O53 Ti5 129.8(6) . . ? C55 O53 Ti6 126.2(6) . . ? Ti5 O53 Ti6 101.9(3) . . ? C61 O61 Ti6 130.7(10) . . ? C63 O62 Ti6 159.9(8) . . ? C65 O63 Ti1 124.9(7) . . ? C65 O63 Ti6 119.2(7) . . ? Ti1 O63 Ti6 104.1(3) . . ? C71 O71 Ti7 126.2(6) . . ? C71 O71 Ti1 128.6(6) . . ? Ti7 O71 Ti1 104.9(3) . . ? Ti7 O72 Ti4 107.2(3) . . ? O11 C11 C12 110.1(13) . . ? O11 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? O11 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O12 C13 C14 110.9(11) . . ? O12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? O12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O13 C15 C16 112.2(10) . . ? O13 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? O13 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O21 C21 C22 111.5(9) . . ? O21 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? O21 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O22 C23 C24 113.1(11) . . ? O22 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? O22 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 O23 110.4(13) . . ? C26 C25 H25A 109.6 . . ? O23 C25 H25A 109.6 . . ? C26 C25 H25B 109.6 . . ? O23 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O31 C31 C32 110.6(12) . . ? O31 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? O31 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O32 C33 C34 111.3(9) . . ? O32 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? O32 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O33 C35 C36 111.5(10) . . ? O33 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? O33 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O41 C41 C42 113.1(9) . . ? O41 C41 H41A 109.0 . . ? C42 C41 H41A 109.0 . . ? O41 C41 H41B 109.0 . . ? C42 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O42 C43 C44 111.6(10) . . ? O42 C43 H43A 109.3 . . ? C44 C43 H43A 109.3 . . ? O42 C43 H43B 109.3 . . ? C44 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O43 C45 C46 110.3(10) . . ? O43 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? O43 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O51 C51 C52 112.4(11) . . ? O51 C51 H51A 109.1 . . ? C52 C51 H51A 109.1 . . ? O51 C51 H51B 109.1 . . ? C52 C51 H51B 109.1 . . ? H51A C51 H51B 107.9 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O52 C53 C54 111.9(9) . . ? O52 C53 H53A 109.2 . . ? C54 C53 H53A 109.2 . . ? O52 C53 H53B 109.2 . . ? C54 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O53 C55 C56 113.0(8) . . ? O53 C55 H55A 109.0 . . ? C56 C55 H55A 109.0 . . ? O53 C55 H55B 109.0 . . ? C56 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C62 C61 O61 115.3(15) . . ? C62 C61 H61A 108.5 . . ? O61 C61 H61A 108.5 . . ? C62 C61 H61B 108.5 . . ? O61 C61 H61B 108.5 . . ? H61A C61 H61B 107.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O62 C63 C64 110.5(12) . . ? O62 C63 H63A 109.6 . . ? C64 C63 H63A 109.6 . . ? O62 C63 H63B 109.6 . . ? C64 C63 H63B 109.6 . . ? H63A C63 H63B 108.1 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 O63 111.7(13) . . ? C66 C65 H65A 109.3 . . ? O63 C65 H65A 109.3 . . ? C66 C65 H65B 109.3 . . ? O63 C65 H65B 109.3 . . ? H65A C65 H65B 107.9 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O71 C71 C72 111.1(9) . . ? O71 C71 H71A 109.4 . . ? C72 C71 H71A 109.4 . . ? O71 C71 H71B 109.4 . . ? C72 C71 H71B 109.4 . . ? H71A C71 H71B 108.0 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 33.18 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.042 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.088 # Attachment '2.cif.txt' data_dw1001 _database_code_depnum_ccdc_archive 'CCDC 766942' #TrackingRef '2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H75 Cl Co O16 Ti4' _chemical_formula_sum 'C30 H75 Cl Co O16 Ti4' _chemical_formula_weight 977.88 _chemical_absolute_configuration ; Flack parameter 0.083(15) ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 21.9917(2) _cell_length_b 10.8628(1) _cell_length_c 22.4581(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.666(1) _cell_angle_gamma 90.00 _cell_volume 4707.46(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 26500 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour purple-green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 1.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.621 _exptl_absorpt_correction_T_max 0.700 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The -OEt groups are poorly resolved: the O-C and C-C distances for these were constrained with DFIX commands and 2 free variables. In addition, two -OEt groups are disordered over two sites & the disordered carbon atoms were assigned isotropic displacement parameters. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 23271 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8218 _reflns_number_gt 7945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+4.9978P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.083(15) _refine_ls_number_reflns 8218 _refine_ls_number_parameters 466 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cl1 Cl 0.97306(9) 1.76116(10) 1.01037(8) 0.0825(4) Uani 1 1 d . . . Ti1 Ti 1.16741(3) 1.48461(6) 1.00289(3) 0.04104(15) Uani 1 1 d . . . Ti2 Ti 0.99220(3) 1.49824(6) 0.82019(3) 0.03681(14) Uani 1 1 d . A . Ti3 Ti 1.02846(3) 1.31687(5) 0.94726(3) 0.03107(12) Uani 1 1 d . A . Ti4 Ti 1.12288(3) 1.31909(6) 0.87110(3) 0.03915(15) Uani 1 1 d . A . Co1 Co 1.01470(3) 1.61053(4) 0.97113(3) 0.04308(12) Uani 1 1 d . A . O1 O 1.07475(12) 1.44186(17) 0.91134(12) 0.0299(4) Uani 1 1 d . . . O11 O 1.19891(15) 1.5978(3) 0.96644(14) 0.0508(7) Uani 1 1 d D . . O12 O 1.24232(16) 1.4782(4) 1.08604(16) 0.0698(10) Uani 1 1 d D . . O13 O 1.11590(13) 1.3541(2) 1.03030(12) 0.0401(5) Uani 1 1 d D . . O21 O 0.90953(16) 1.4976(3) 0.74412(15) 0.0628(9) Uani 1 1 d D . . O22 O 1.03296(15) 1.6075(3) 0.79120(14) 0.0502(7) Uani 1 1 d D . . O23 O 0.95229(11) 1.3565(2) 0.85674(11) 0.0373(5) Uani 1 1 d D . . O31 O 0.99285(14) 1.1931(2) 0.97154(14) 0.0434(6) Uani 1 1 d D . . O41 O 1.19817(13) 1.3409(3) 0.96645(15) 0.0481(6) Uani 1 1 d D . . O42 O 1.03250(14) 1.3541(3) 0.79130(12) 0.0444(6) Uani 1 1 d D . . O43 O 1.07448(17) 1.20583(19) 0.91034(18) 0.0477(5) Uani 1 1 d D . . O44 O 1.16753(14) 1.4231(3) 0.84212(16) 0.0525(7) Uani 1 1 d D . . O45 O 1.14880(18) 1.1783(3) 0.8459(2) 0.0636(9) Uani 1 1 d D . . O51 O 1.11587(15) 1.6116(3) 1.02368(14) 0.0501(7) Uani 1 1 d D . . O52 O 0.97140(14) 1.6235(2) 0.87167(14) 0.0473(6) Uani 1 1 d D . . O53 O 0.98867(11) 1.4433(2) 0.98299(12) 0.0344(5) Uani 1 1 d D . . C41 C 1.2398(3) 1.2450(7) 1.0113(4) 0.106(2) Uani 1 1 d D . . H41A H 1.2127 1.1677 0.9996 0.128 Uiso 1 1 calc R . . H41B H 1.2519 1.2671 1.0585 0.128 Uiso 1 1 calc R . . C42 C 1.0218(3) 1.3374(5) 0.72347(19) 0.0619(12) Uani 1 1 d D B . H42A H 1.0673 1.3333 0.7245 0.074 Uiso 1 1 calc R . . H42B H 0.9962 1.4090 0.6953 0.074 Uiso 1 1 calc R . . C43 C 1.0480(4) 1.0854(5) 0.8850(4) 0.0472(11) Uiso 0.498(6) 1 d PD A 1 H43A H 1.0470 1.0715 0.8410 0.057 Uiso 0.498(6) 1 calc PR A 1 H43B H 1.0003 1.0767 0.8783 0.057 Uiso 0.498(6) 1 calc PR A 1 C43' C 1.0917(4) 1.0792(5) 0.9276(4) 0.0472(11) Uiso 0.502(6) 1 d PD A 2 H43C H 1.0916 1.0599 0.9706 0.057 Uiso 0.502(6) 1 calc PR A 2 H43D H 1.1386 1.0618 0.9337 0.057 Uiso 0.502(6) 1 calc PR A 2 C44 C 1.2383(2) 1.4520(6) 0.8641(3) 0.0813(16) Uani 1 1 d D A . H44A H 1.2656 1.3749 0.8746 0.098 Uiso 1 1 calc R . . H44B H 1.2568 1.5019 0.9060 0.098 Uiso 1 1 calc R . . C45 C 1.1899(4) 1.1495(6) 0.8145(4) 0.108(3) Uani 1 1 d D A . H45A H 1.2389 1.1427 0.8500 0.129 Uiso 1 1 calc R . . H45B H 1.1866 1.2184 0.7842 0.129 Uiso 1 1 calc R . . C11 C 1.1821(3) 1.7053(4) 0.9265(2) 0.0663(12) Uani 1 1 d D . . H11A H 1.1438 1.7488 0.9289 0.080 Uiso 1 1 calc R . . H11B H 1.1660 1.6823 0.8786 0.080 Uiso 1 1 calc R . . C12 C 1.3118(3) 1.5226(9) 1.1148(3) 0.124(3) Uani 1 1 d D . . H12A H 1.3117 1.6075 1.0987 0.149 Uiso 1 1 calc R . . H12B H 1.3386 1.4700 1.0997 0.149 Uiso 1 1 calc R . . C13 C 1.1255(2) 1.3402(4) 1.09766(18) 0.0621(12) Uani 1 1 d D . . H13A H 1.0804 1.3494 1.0970 0.075 Uiso 1 1 calc R . . H13B H 1.1569 1.4054 1.1272 0.075 Uiso 1 1 calc R . . C21 C 0.8739(3) 1.5684(8) 0.6837(4) 0.0765(19) Uiso 0.571(9) 1 d PD B 1 H21A H 0.8957 1.5541 0.6546 0.092 Uiso 0.571(9) 1 calc PR B 1 H21B H 0.8790 1.6568 0.6957 0.092 Uiso 0.571(9) 1 calc PR B 1 C21' C 0.8632(5) 1.4628(10) 0.6756(4) 0.0765(19) Uiso 0.429(9) 1 d PD B 2 H21C H 0.8500 1.3754 0.6746 0.092 Uiso 0.429(9) 1 calc PR B 2 H21D H 0.8873 1.4707 0.6482 0.092 Uiso 0.429(9) 1 calc PR B 2 C22 C 1.0481(4) 1.6563(5) 0.7417(3) 0.0897(18) Uani 1 1 d D B . H22A H 1.0197 1.6131 0.6982 0.108 Uiso 1 1 calc R . . H22B H 1.0975 1.6404 0.7556 0.108 Uiso 1 1 calc R . . C23 C 0.89738(18) 1.2745(4) 0.8149(2) 0.0583(11) Uani 1 1 d D B . H23A H 0.9061 1.1930 0.8373 0.070 Uiso 1 1 calc R . . H23B H 0.8973 1.2636 0.7711 0.070 Uiso 1 1 calc R . . C31 C 0.9673(4) 1.0813(4) 0.9837(4) 0.092(2) Uani 0.623(13) 1 d PD B 1 H31A H 1.0015 1.0153 0.9919 0.111 Uiso 0.623(13) 1 calc PR B 1 H31B H 0.9239 1.0591 0.9425 0.111 Uiso 0.623(13) 1 calc PR B 1 C31' C 0.9673(4) 1.0813(4) 0.9837(4) 0.092(2) Uani 0.377(13) 1 d PD B 2 H31C H 1.0079 1.0307 1.0143 0.111 Uiso 0.377(13) 1 calc PR B 2 H31D H 0.9431 1.0368 0.9400 0.111 Uiso 0.377(13) 1 calc PR B 2 C51 C 1.1506(3) 1.7154(5) 1.0655(2) 0.0770(16) Uani 1 1 d D . . H51A H 1.1239 1.7911 1.0441 0.092 Uiso 1 1 calc R . . H51B H 1.1970 1.7240 1.0690 0.092 Uiso 1 1 calc R . . C52 C 0.9304(2) 1.7292(4) 0.8386(3) 0.0683(13) Uani 1 1 d D B . H52A H 0.9309 1.7429 0.7953 0.082 Uiso 1 1 calc R . . H52B H 0.9510 1.8026 0.8676 0.082 Uiso 1 1 calc R . . C53 C 0.92137(16) 1.4332(3) 0.97795(17) 0.0427(8) Uani 1 1 d D A . H53A H 0.9008 1.3524 0.9581 0.051 Uiso 1 1 calc R . . H53B H 0.8908 1.4984 0.9475 0.051 Uiso 1 1 calc R . . C141 C 1.3028(4) 1.2246(11) 1.0075(6) 0.170(5) Uani 1 1 d D . . H14A H 1.3302 1.1601 1.0398 0.255 Uiso 1 1 calc R . . H14B H 1.3297 1.3010 1.0188 0.255 Uiso 1 1 calc R . . H14C H 1.2911 1.1990 0.9615 0.255 Uiso 1 1 calc R . . C142 C 0.9823(3) 1.2235(5) 0.6925(3) 0.0812(17) Uani 1 1 d D . . H14D H 0.9764 1.2140 0.6467 0.122 Uiso 1 1 calc R B . H14E H 0.9368 1.2284 0.6902 0.122 Uiso 1 1 calc R . . H14F H 1.0077 1.1524 0.7202 0.122 Uiso 1 1 calc R . . C143 C 1.0944(6) 0.9953(10) 0.9357(5) 0.078(2) Uiso 0.498(6) 1 d PD A 1 H14G H 1.0774 0.9118 0.9201 0.118 Uiso 0.498(6) 1 calc PR A 1 H14H H 1.0954 1.0105 0.9791 0.118 Uiso 0.498(6) 1 calc PR A 1 H14I H 1.1413 1.0039 0.9414 0.118 Uiso 0.498(6) 1 calc PR A 1 C243 C 1.0397(6) 1.0035(10) 0.8720(5) 0.078(2) Uiso 0.502(6) 1 d PD A 2 H24A H 1.0507 0.9161 0.8826 0.118 Uiso 0.502(6) 1 calc PR A 2 H24B H 1.0401 1.0235 0.8297 0.118 Uiso 0.502(6) 1 calc PR A 2 H24C H 0.9936 1.0205 0.8668 0.118 Uiso 0.502(6) 1 calc PR A 2 C144 C 1.2456(4) 1.5202(7) 0.8118(4) 0.108(3) Uani 1 1 d D . . H14J H 1.2947 1.5370 0.8275 0.163 Uiso 1 1 calc R A . H14K H 1.2202 1.5982 0.8028 0.163 Uiso 1 1 calc R . . H14L H 1.2267 1.4713 0.7701 0.163 Uiso 1 1 calc R . . C145 C 1.1703(5) 1.0378(6) 0.7757(5) 0.121(3) Uani 1 1 d D . . H14M H 1.2011 1.0235 0.7562 0.182 Uiso 1 1 calc R A . H14N H 1.1224 1.0447 0.7391 0.182 Uiso 1 1 calc R . . H14O H 1.1739 0.9687 0.8053 0.182 Uiso 1 1 calc R . . C111 C 1.2425(4) 1.7891(6) 0.9497(4) 0.095(2) Uani 1 1 d D . . H11C H 1.2293 1.8621 0.9205 0.142 Uiso 1 1 calc R . . H11D H 1.2805 1.7463 0.9473 0.142 Uiso 1 1 calc R . . H11E H 1.2577 1.8143 0.9966 0.142 Uiso 1 1 calc R . . C112 C 1.3446(3) 1.5217(7) 1.1886(3) 0.107(3) Uani 1 1 d D . . H11F H 1.3886 1.5666 1.2074 0.160 Uiso 1 1 calc R . . H11G H 1.3533 1.4365 1.2050 0.160 Uiso 1 1 calc R . . H11H H 1.3139 1.5615 1.2032 0.160 Uiso 1 1 calc R . . C113 C 1.1551(4) 1.2184(6) 1.1255(3) 0.106(3) Uani 1 1 d D . . H11I H 1.1612 1.2105 1.1714 0.159 Uiso 1 1 calc R . . H11J H 1.2002 1.2099 1.1269 0.159 Uiso 1 1 calc R . . H11K H 1.1237 1.1539 1.0965 0.159 Uiso 1 1 calc R . . C121 C 0.8008(3) 1.5385(8) 0.6455(3) 0.113(3) Uani 0.571(9) 1 d PD B 1 H12C H 0.7795 1.5862 0.6033 0.169 Uiso 0.571(9) 1 calc PR B 1 H12D H 0.7781 1.5587 0.6726 0.169 Uiso 0.571(9) 1 calc PR B 1 H12E H 0.7954 1.4504 0.6347 0.169 Uiso 0.571(9) 1 calc PR B 1 C221 C 0.8008(3) 1.5385(8) 0.6455(3) 0.113(3) Uani 0.429(9) 1 d PD B 2 H22C H 0.7697 1.5095 0.5994 0.169 Uiso 0.429(9) 1 calc PR B 2 H22D H 0.8134 1.6245 0.6438 0.169 Uiso 0.429(9) 1 calc PR B 2 H22E H 0.7773 1.5325 0.6730 0.169 Uiso 0.429(9) 1 calc PR B 2 C122 C 1.0351(5) 1.7878(5) 0.7313(5) 0.125(3) Uani 1 1 d D . . H12F H 1.0440 1.8157 0.6948 0.187 Uiso 1 1 calc R B . H12G H 1.0657 1.8318 0.7733 0.187 Uiso 1 1 calc R . . H12H H 0.9867 1.8047 0.7190 0.187 Uiso 1 1 calc R . . C123 C 0.8288(2) 1.3193(5) 0.8018(3) 0.0726(15) Uani 1 1 d D . . H12I H 0.7930 1.2608 0.7724 0.109 Uiso 1 1 calc R B . H12J H 0.8197 1.3998 0.7794 0.109 Uiso 1 1 calc R . . H12K H 0.8280 1.3273 0.8449 0.109 Uiso 1 1 calc R . . C131 C 0.9536(6) 1.0860(8) 1.0413(4) 0.0688(19) Uiso 0.623(13) 1 d PD B 1 H13C H 0.9334 1.0077 1.0448 0.103 Uiso 0.623(13) 1 calc PR B 1 H13D H 0.9212 1.1531 1.0346 0.103 Uiso 0.623(13) 1 calc PR B 1 H13E H 0.9971 1.1004 1.0832 0.103 Uiso 0.623(13) 1 calc PR B 1 C231 C 0.9207(8) 1.0855(13) 1.0128(9) 0.0688(19) Uiso 0.377(13) 1 d PD B 2 H23C H 0.9043 1.0022 1.0141 0.103 Uiso 0.377(13) 1 calc PR B 2 H23D H 0.8810 1.1383 0.9848 0.103 Uiso 0.377(13) 1 calc PR B 2 H23E H 0.9454 1.1188 1.0589 0.103 Uiso 0.377(13) 1 calc PR B 2 C151 C 1.1582(4) 1.7022(7) 1.1341(3) 0.103(2) Uani 1 1 d D . . H15A H 1.1833 1.7734 1.1618 0.154 Uiso 1 1 calc R . . H15B H 1.1841 1.6268 1.1552 0.154 Uiso 1 1 calc R . . H15C H 1.1122 1.6976 1.1310 0.154 Uiso 1 1 calc R . . C152 C 0.8580(2) 1.7149(6) 0.8249(4) 0.094(2) Uani 1 1 d D . . H15D H 0.8312 1.7877 0.8008 0.141 Uiso 1 1 calc R B . H15E H 0.8571 1.7059 0.8678 0.141 Uiso 1 1 calc R . . H15F H 0.8377 1.6416 0.7968 0.141 Uiso 1 1 calc R . . C153 C 0.9259(3) 1.4454(4) 1.0455(2) 0.0597(11) Uani 1 1 d D . . H15G H 0.8793 1.4406 1.0408 0.090 Uiso 1 1 calc R A . H15H H 0.9468 1.5249 1.0654 0.090 Uiso 1 1 calc R . . H15I H 0.9546 1.3787 1.0750 0.090 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.1405(12) 0.0375(5) 0.1222(11) -0.0020(6) 0.1053(11) 0.0115(6) Ti1 0.0352(3) 0.0514(4) 0.0361(3) -0.0036(3) 0.0168(3) -0.0091(3) Ti2 0.0333(3) 0.0479(3) 0.0328(3) 0.0057(2) 0.0187(2) 0.0003(2) Ti3 0.0356(3) 0.0282(2) 0.0364(3) 0.0001(2) 0.0228(2) -0.0008(2) Ti4 0.0423(3) 0.0368(3) 0.0514(4) -0.0042(2) 0.0329(3) -0.0011(2) Co1 0.0603(3) 0.02947(19) 0.0560(3) -0.00134(19) 0.0412(2) -0.00016(19) O1 0.0326(9) 0.0296(9) 0.0303(9) -0.0014(9) 0.0173(7) -0.0004(10) O11 0.0549(16) 0.0521(15) 0.0546(15) -0.0073(12) 0.0336(13) -0.0170(12) O12 0.0461(17) 0.105(3) 0.0456(17) 0.0021(16) 0.0120(13) -0.0181(16) O13 0.0395(12) 0.0482(14) 0.0342(12) 0.0061(10) 0.0190(10) 0.0009(10) O21 0.0455(16) 0.094(2) 0.0405(15) 0.0192(14) 0.0139(13) -0.0063(14) O22 0.0528(15) 0.0552(16) 0.0528(15) 0.0116(12) 0.0336(13) -0.0021(12) O23 0.0350(12) 0.0459(12) 0.0343(12) -0.0046(10) 0.0191(10) -0.0088(10) O31 0.0559(15) 0.0304(11) 0.0585(15) 0.0007(10) 0.0391(13) -0.0032(10) O41 0.0369(13) 0.0554(15) 0.0554(16) 0.0107(13) 0.0248(12) 0.0088(11) O42 0.0516(14) 0.0524(15) 0.0383(13) -0.0105(11) 0.0289(11) -0.0097(11) O43 0.0635(14) 0.0303(10) 0.0715(15) -0.0030(13) 0.0503(13) 0.0010(12) O44 0.0551(16) 0.0514(15) 0.0709(18) -0.0037(13) 0.0462(15) -0.0075(12) O45 0.079(2) 0.0460(16) 0.101(3) -0.0110(15) 0.072(2) 0.0005(14) O51 0.0609(16) 0.0474(14) 0.0521(15) -0.0195(12) 0.0351(13) -0.0176(12) O52 0.0547(14) 0.0452(14) 0.0557(15) 0.0181(11) 0.0375(13) 0.0190(11) O53 0.0391(12) 0.0328(11) 0.0420(12) 0.0010(9) 0.0281(10) 0.0018(9) C41 0.071(4) 0.102(5) 0.131(6) 0.025(4) 0.036(4) 0.034(3) C42 0.072(3) 0.084(3) 0.046(2) -0.017(2) 0.041(2) -0.017(2) C44 0.077(3) 0.086(4) 0.109(5) -0.023(3) 0.066(3) -0.014(3) C45 0.132(6) 0.083(4) 0.179(8) -0.045(5) 0.131(6) -0.014(4) C11 0.079(3) 0.059(2) 0.069(3) -0.003(2) 0.042(2) -0.015(2) C12 0.063(3) 0.195(9) 0.077(4) 0.006(5) 0.004(3) -0.051(5) C13 0.059(3) 0.090(3) 0.034(2) 0.011(2) 0.0207(18) -0.007(2) C22 0.107(5) 0.103(5) 0.083(4) 0.033(3) 0.065(4) 0.011(4) C23 0.053(2) 0.071(3) 0.046(2) -0.0097(18) 0.0193(17) -0.027(2) C31 0.157(6) 0.042(2) 0.139(5) -0.002(3) 0.119(5) -0.024(3) C31' 0.157(6) 0.042(2) 0.139(5) -0.002(3) 0.119(5) -0.024(3) C51 0.106(4) 0.065(3) 0.081(3) -0.043(3) 0.061(3) -0.041(3) C52 0.076(3) 0.056(2) 0.095(3) 0.038(2) 0.059(3) 0.033(2) C53 0.0410(17) 0.0455(18) 0.053(2) -0.0008(15) 0.0314(16) 0.0009(14) C141 0.093(5) 0.208(11) 0.179(10) 0.048(8) 0.042(6) 0.101(7) C142 0.089(4) 0.107(4) 0.047(2) -0.034(3) 0.032(2) -0.025(3) C144 0.122(6) 0.093(4) 0.169(7) -0.005(4) 0.118(6) -0.026(4) C145 0.181(8) 0.079(4) 0.188(8) -0.041(5) 0.157(8) -0.011(4) C111 0.112(5) 0.079(4) 0.113(5) -0.014(3) 0.070(4) -0.045(3) C112 0.053(3) 0.151(7) 0.072(4) -0.028(4) -0.005(3) -0.002(3) C113 0.095(4) 0.140(6) 0.080(4) 0.068(4) 0.039(3) 0.032(4) C121 0.070(4) 0.170(7) 0.062(3) 0.034(4) 0.003(3) 0.029(4) C221 0.070(4) 0.170(7) 0.062(3) 0.034(4) 0.003(3) 0.029(4) C122 0.191(9) 0.078(4) 0.159(7) 0.041(5) 0.127(7) -0.012(5) C123 0.047(2) 0.104(4) 0.061(3) 0.007(3) 0.021(2) -0.023(2) C151 0.119(5) 0.127(6) 0.083(4) -0.055(4) 0.065(4) -0.046(4) C152 0.082(4) 0.107(4) 0.121(5) 0.056(4) 0.072(4) 0.056(3) C153 0.074(3) 0.061(2) 0.072(3) -0.012(2) 0.056(2) -0.009(2) _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_site_symmetry_2 _geom_bond_publ_flag Cl1 Co1 2.2509(12) . ? Ti1 O11 1.791(3) . ? Ti1 O12 1.804(3) . ? Ti1 O51 1.978(3) . ? Ti1 O41 2.024(3) . ? Ti1 O13 2.083(3) . ? Ti1 O1 2.139(2) . ? Ti1 Ti4 3.1893(9) . ? Ti1 Ti3 3.2490(8) . ? Ti2 O22 1.788(3) . ? Ti2 O21 1.801(3) . ? Ti2 O52 1.976(3) . ? Ti2 O42 2.051(3) . ? Ti2 O1 2.073(2) . ? Ti2 O23 2.123(3) . ? Ti2 Ti4 3.1939(9) . ? Ti2 Ti3 3.2371(8) . ? Ti3 O31 1.769(2) . ? Ti3 O23 1.964(2) . ? Ti3 O13 1.975(2) . ? Ti3 O53 1.992(2) . ? Ti3 O43 1.993(3) . ? Ti3 O1 2.078(2) . ? Ti3 Ti4 3.2629(8) . ? Ti4 O44 1.810(3) . ? Ti4 O45 1.815(3) . ? Ti4 O42 1.972(3) . ? Ti4 O41 1.995(3) . ? Ti4 O43 2.079(3) . ? Ti4 O1 2.153(2) . ? Co1 O51 1.956(3) . ? Co1 O53 1.961(2) . ? Co1 O52 1.969(3) . ? O11 C11 1.409(4) . ? O12 C12 1.427(4) . ? O13 C13 1.432(4) . ? O21 C21 1.424(5) . ? O21 C21' 1.429(5) . ? O22 C22 1.409(4) . ? O23 C23 1.430(3) . ? O31 C31 1.418(3) . ? O41 C41 1.434(4) . ? O42 C42 1.437(4) . ? O43 C43' 1.430(5) . ? O43 C43 1.434(5) . ? O44 C44 1.423(4) . ? O45 C45 1.423(4) . ? O51 C51 1.431(4) . ? O52 C52 1.428(3) . ? O53 C53 1.433(3) . ? C41 C141 1.444(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C142 1.479(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C143 1.476(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43' C243 1.475(4) . ? C43' H43C 0.9900 . ? C43' H43D 0.9900 . ? C44 C144 1.461(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C145 1.435(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C11 C111 1.483(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C112 1.458(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C113 1.474(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C21 C121 1.451(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22 C122 1.454(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C123 1.474(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C31 C131 1.463(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C51 C151 1.475(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C152 1.479(4) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C153 1.477(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C142 H14D 0.9800 . ? C142 H14E 0.9800 . ? C142 H14F 0.9800 . ? C143 H14G 0.9800 . ? C143 H14H 0.9800 . ? C143 H14I 0.9800 . ? C243 H24A 0.9800 . ? C243 H24B 0.9800 . ? C243 H24C 0.9800 . ? C144 H14J 0.9800 . ? C144 H14K 0.9800 . ? C144 H14L 0.9800 . ? C145 H14M 0.9800 . ? C145 H14N 0.9800 . ? C145 H14O 0.9800 . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C113 H11I 0.9800 . ? C113 H11J 0.9800 . ? C113 H11K 0.9800 . ? C121 H12C 0.9800 . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C122 H12F 0.9800 . ? C122 H12G 0.9800 . ? C122 H12H 0.9800 . ? C123 H12I 0.9800 . ? C123 H12J 0.9800 . ? C123 H12K 0.9800 . ? C131 H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C231 H23C 0.9800 . ? C231 H23D 0.9800 . ? C231 H23E 0.9800 . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C152 H15D 0.9800 . ? C152 H15E 0.9800 . ? C152 H15F 0.9800 . ? C153 H15G 0.9800 . ? C153 H15H 0.9800 . ? C153 H15I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Ti1 O12 97.95(15) . . ? O11 Ti1 O51 91.15(13) . . ? O12 Ti1 O51 97.17(16) . . ? O11 Ti1 O41 93.86(13) . . ? O12 Ti1 O41 94.15(16) . . ? O51 Ti1 O41 166.88(11) . . ? O11 Ti1 O13 170.67(11) . . ? O12 Ti1 O13 91.36(13) . . ? O51 Ti1 O13 87.16(12) . . ? O41 Ti1 O13 85.94(11) . . ? O11 Ti1 O1 96.24(11) . . ? O12 Ti1 O1 164.23(14) . . ? O51 Ti1 O1 89.36(10) . . ? O41 Ti1 O1 78.05(10) . . ? O13 Ti1 O1 74.58(9) . . ? O11 Ti1 Ti4 88.67(9) . . ? O12 Ti1 Ti4 131.31(14) . . ? O51 Ti1 Ti4 131.04(8) . . ? O41 Ti1 Ti4 37.17(7) . . ? O13 Ti1 Ti4 85.54(7) . . ? O1 Ti1 Ti4 42.16(6) . . ? O11 Ti1 Ti3 135.08(9) . . ? O12 Ti1 Ti3 126.85(12) . . ? O51 Ti1 Ti3 86.69(8) . . ? O41 Ti1 Ti3 81.20(8) . . ? O13 Ti1 Ti3 35.67(6) . . ? O1 Ti1 Ti3 38.93(7) . . ? Ti4 Ti1 Ti3 60.893(18) . . ? O22 Ti2 O21 96.40(14) . . ? O22 Ti2 O52 93.04(13) . . ? O21 Ti2 O52 98.40(15) . . ? O22 Ti2 O42 91.35(13) . . ? O21 Ti2 O42 95.14(15) . . ? O52 Ti2 O42 165.20(10) . . ? O22 Ti2 O1 101.61(12) . . ? O21 Ti2 O1 160.56(13) . . ? O52 Ti2 O1 87.96(10) . . ? O42 Ti2 O1 77.31(10) . . ? O22 Ti2 O23 174.24(13) . . ? O21 Ti2 O23 86.98(12) . . ? O52 Ti2 O23 91.06(11) . . ? O42 Ti2 O23 83.69(11) . . ? O1 Ti2 O23 74.48(9) . . ? O22 Ti2 Ti4 90.73(10) . . ? O21 Ti2 Ti4 131.50(13) . . ? O52 Ti2 Ti4 129.14(8) . . ? O42 Ti2 Ti4 36.60(7) . . ? O1 Ti2 Ti4 41.84(7) . . ? O23 Ti2 Ti4 83.54(7) . . ? O22 Ti2 Ti3 140.42(9) . . ? O21 Ti2 Ti3 122.92(11) . . ? O52 Ti2 Ti3 86.07(7) . . ? O42 Ti2 Ti3 81.56(8) . . ? O1 Ti2 Ti3 38.81(7) . . ? O23 Ti2 Ti3 35.94(6) . . ? Ti4 Ti2 Ti3 60.972(18) . . ? O31 Ti3 O23 101.64(12) . . ? O31 Ti3 O13 103.84(12) . . ? O23 Ti3 O13 153.31(11) . . ? O31 Ti3 O53 93.15(11) . . ? O23 Ti3 O53 86.82(10) . . ? O13 Ti3 O53 83.99(11) . . ? O31 Ti3 O43 93.23(12) . . ? O23 Ti3 O43 93.04(13) . . ? O13 Ti3 O43 93.34(13) . . ? O53 Ti3 O43 173.51(10) . . ? O31 Ti3 O1 171.18(11) . . ? O23 Ti3 O1 77.79(10) . . ? O13 Ti3 O1 78.25(10) . . ? O53 Ti3 O1 95.60(9) . . ? O43 Ti3 O1 78.04(10) . . ? O31 Ti3 Ti2 140.92(9) . . ? O23 Ti3 Ti2 39.38(7) . . ? O13 Ti3 Ti2 115.11(8) . . ? O53 Ti3 Ti2 88.03(7) . . ? O43 Ti3 Ti2 87.77(9) . . ? O1 Ti3 Ti2 38.69(7) . . ? O31 Ti3 Ti1 141.41(9) . . ? O23 Ti3 Ti1 116.94(7) . . ? O13 Ti3 Ti1 37.97(7) . . ? O53 Ti3 Ti1 88.42(7) . . ? O43 Ti3 Ti1 85.86(9) . . ? O1 Ti3 Ti1 40.30(7) . . ? Ti2 Ti3 Ti1 77.651(19) . . ? O31 Ti3 Ti4 130.88(9) . . ? O23 Ti3 Ti4 84.09(8) . . ? O13 Ti3 Ti4 85.26(8) . . ? O53 Ti3 Ti4 135.97(7) . . ? O43 Ti3 Ti4 37.67(8) . . ? O1 Ti3 Ti4 40.38(6) . . ? Ti2 Ti3 Ti4 58.860(19) . . ? Ti1 Ti3 Ti4 58.651(19) . . ? O44 Ti4 O45 96.20(14) . . ? O44 Ti4 O42 92.12(13) . . ? O45 Ti4 O42 102.09(15) . . ? O44 Ti4 O41 89.87(13) . . ? O45 Ti4 O41 102.23(15) . . ? O42 Ti4 O41 155.23(12) . . ? O44 Ti4 O43 176.27(14) . . ? O45 Ti4 O43 86.28(13) . . ? O42 Ti4 O43 90.09(13) . . ? O41 Ti4 O43 86.87(13) . . ? O44 Ti4 O1 103.00(11) . . ? O45 Ti4 O1 160.80(12) . . ? O42 Ti4 O1 77.16(10) . . ? O41 Ti4 O1 78.34(11) . . ? O43 Ti4 O1 74.56(9) . . ? O44 Ti4 Ti1 90.21(10) . . ? O45 Ti4 Ti1 139.65(13) . . ? O42 Ti4 Ti1 117.48(8) . . ? O41 Ti4 Ti1 37.80(8) . . ? O43 Ti4 Ti1 86.10(9) . . ? O1 Ti4 Ti1 41.84(6) . . ? O44 Ti4 Ti2 92.35(10) . . ? O45 Ti4 Ti2 139.91(13) . . ? O42 Ti4 Ti2 38.33(8) . . ? O41 Ti4 Ti2 116.92(9) . . ? O43 Ti4 Ti2 87.51(8) . . ? O1 Ti4 Ti2 39.97(6) . . ? Ti1 Ti4 Ti2 79.14(2) . . ? O44 Ti4 Ti3 141.66(10) . . ? O45 Ti4 Ti3 122.11(11) . . ? O42 Ti4 Ti3 81.97(8) . . ? O41 Ti4 Ti3 81.22(9) . . ? O43 Ti4 Ti3 35.85(7) . . ? O1 Ti4 Ti3 38.71(6) . . ? Ti1 Ti4 Ti3 60.457(18) . . ? Ti2 Ti4 Ti3 60.168(18) . . ? O51 Co1 O53 104.20(11) . . ? O51 Co1 O52 118.38(12) . . ? O53 Co1 O52 101.92(11) . . ? O51 Co1 Cl1 108.55(9) . . ? O53 Co1 Cl1 114.85(8) . . ? O52 Co1 Cl1 109.03(8) . . ? Ti2 O1 Ti3 102.50(10) . . ? Ti2 O1 Ti1 149.81(10) . . ? Ti3 O1 Ti1 100.77(10) . . ? Ti2 O1 Ti4 98.19(10) . . ? Ti3 O1 Ti4 100.91(8) . . ? Ti1 O1 Ti4 96.00(10) . . ? C11 O11 Ti1 145.0(3) . . ? C12 O12 Ti1 134.6(4) . . ? C13 O13 Ti3 124.0(3) . . ? C13 O13 Ti1 124.0(3) . . ? Ti3 O13 Ti1 106.35(11) . . ? C21 O21 C21' 48.3(6) . . ? C21 O21 Ti2 138.2(4) . . ? C21' O21 Ti2 153.6(4) . . ? C22 O22 Ti2 152.5(4) . . ? C23 O23 Ti3 125.2(2) . . ? C23 O23 Ti2 125.0(2) . . ? Ti3 O23 Ti2 104.69(10) . . ? C31 O31 Ti3 170.1(3) . . ? C41 O41 Ti4 126.1(4) . . ? C41 O41 Ti1 120.1(4) . . ? Ti4 O41 Ti1 105.03(11) . . ? C42 O42 Ti4 121.3(3) . . ? C42 O42 Ti2 123.8(3) . . ? Ti4 O42 Ti2 105.06(11) . . ? C43' O43 C43 40.0(4) . . ? C43' O43 Ti3 126.2(4) . . ? C43 O43 Ti3 121.8(4) . . ? C43' O43 Ti4 124.1(4) . . ? C43 O43 Ti4 124.4(4) . . ? Ti3 O43 Ti4 106.48(10) . . ? C44 O44 Ti4 134.8(3) . . ? C45 O45 Ti4 135.2(3) . . ? C51 O51 Co1 119.7(3) . . ? C51 O51 Ti1 121.2(3) . . ? Co1 O51 Ti1 117.92(12) . . ? C52 O52 Co1 119.2(3) . . ? C52 O52 Ti2 121.0(3) . . ? Co1 O52 Ti2 119.53(12) . . ? C53 O53 Co1 114.7(2) . . ? C53 O53 Ti3 123.5(2) . . ? Co1 O53 Ti3 111.76(11) . . ? O41 C41 C141 112.2(5) . . ? O41 C41 H41A 109.2 . . ? C141 C41 H41A 109.2 . . ? O41 C41 H41B 109.2 . . ? C141 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? O42 C42 C142 111.4(4) . . ? O42 C42 H42A 109.4 . . ? C142 C42 H42A 109.4 . . ? O42 C42 H42B 109.4 . . ? C142 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? O43 C43 C143 107.5(6) . . ? O43 C43 H43A 110.2 . . ? C143 C43 H43A 110.2 . . ? O43 C43 H43B 110.2 . . ? C143 C43 H43B 110.2 . . ? H43A C43 H43B 108.5 . . ? O43 C43' C243 108.0(6) . . ? O43 C43' H43C 110.1 . . ? C243 C43' H43C 110.1 . . ? O43 C43' H43D 110.1 . . ? C243 C43' H43D 110.1 . . ? H43C C43' H43D 108.4 . . ? O44 C44 C144 110.9(5) . . ? O44 C44 H44A 109.5 . . ? C144 C44 H44A 109.5 . . ? O44 C44 H44B 109.5 . . ? C144 C44 H44B 109.5 . . ? H44A C44 H44B 108.0 . . ? O45 C45 C145 114.1(5) . . ? O45 C45 H45A 108.7 . . ? C145 C45 H45A 108.7 . . ? O45 C45 H45B 108.7 . . ? C145 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? O11 C11 C111 111.6(5) . . ? O11 C11 H11A 109.3 . . ? C111 C11 H11A 109.3 . . ? O11 C11 H11B 109.3 . . ? C111 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? O12 C12 C112 110.5(5) . . ? O12 C12 H12A 109.6 . . ? C112 C12 H12A 109.6 . . ? O12 C12 H12B 109.6 . . ? C112 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? O13 C13 C113 110.7(4) . . ? O13 C13 H13A 109.5 . . ? C113 C13 H13A 109.5 . . ? O13 C13 H13B 109.5 . . ? C113 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O21 C21 C121 112.9(5) . . ? O21 C21 H21A 109.0 . . ? C121 C21 H21A 109.0 . . ? O21 C21 H21B 109.0 . . ? C121 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? O21 C21' H21C 109.2 . . ? O21 C21' H21D 109.2 . . ? H21C C21' H21D 107.9 . . ? O22 C22 C122 113.1(5) . . ? O22 C22 H22A 109.0 . . ? C122 C22 H22A 109.0 . . ? O22 C22 H22B 109.0 . . ? C122 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? O23 C23 C123 112.7(4) . . ? O23 C23 H23A 109.1 . . ? C123 C23 H23A 109.1 . . ? O23 C23 H23B 109.1 . . ? C123 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? O31 C31 C131 114.2(5) . . ? O31 C31 H31A 108.7 . . ? C131 C31 H31A 108.7 . . ? O31 C31 H31B 108.7 . . ? C131 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? O51 C51 C151 111.5(4) . . ? O51 C51 H51A 109.3 . . ? C151 C51 H51A 109.3 . . ? O51 C51 H51B 109.3 . . ? C151 C51 H51B 109.3 . . ? H51A C51 H51B 108.0 . . ? O52 C52 C152 111.8(4) . . ? O52 C52 H52A 109.3 . . ? C152 C52 H52A 109.3 . . ? O52 C52 H52B 109.3 . . ? C152 C52 H52B 109.3 . . ? H52A C52 H52B 107.9 . . ? O53 C53 C153 110.7(3) . . ? O53 C53 H53A 109.5 . . ? C153 C53 H53A 109.5 . . ? O53 C53 H53B 109.5 . . ? C153 C53 H53B 109.5 . . ? H53A C53 H53B 108.1 . . ? C41 C141 H14A 109.5 . . ? C41 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C41 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C42 C142 H14D 109.5 . . ? C42 C142 H14E 109.5 . . ? H14D C142 H14E 109.5 . . ? C42 C142 H14F 109.5 . . ? H14D C142 H14F 109.5 . . ? H14E C142 H14F 109.5 . . ? C43 C143 H14G 109.5 . . ? C43 C143 H14H 109.5 . . ? H14G C143 H14H 109.5 . . ? C43 C143 H14I 109.5 . . ? H14G C143 H14I 109.5 . . ? H14H C143 H14I 109.5 . . ? C43' C243 H24A 109.5 . . ? C43' C243 H24B 109.5 . . ? H24A C243 H24B 109.5 . . ? C43' C243 H24C 109.5 . . ? H24A C243 H24C 109.5 . . ? H24B C243 H24C 109.5 . . ? C44 C144 H14J 109.5 . . ? C44 C144 H14K 109.5 . . ? H14J C144 H14K 109.5 . . ? C44 C144 H14L 109.5 . . ? H14J C144 H14L 109.5 . . ? H14K C144 H14L 109.5 . . ? C45 C145 H14M 109.5 . . ? C45 C145 H14N 109.5 . . ? H14M C145 H14N 109.5 . . ? C45 C145 H14O 109.5 . . ? H14M C145 H14O 109.5 . . ? H14N C145 H14O 109.5 . . ? C11 C111 H11C 109.5 . . ? C11 C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? C11 C111 H11E 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C12 C112 H11F 109.5 . . ? C12 C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? C12 C112 H11H 109.5 . . ? H11F C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C13 C113 H11I 109.5 . . ? C13 C113 H11J 109.5 . . ? H11I C113 H11J 109.5 . . ? C13 C113 H11K 109.5 . . ? H11I C113 H11K 109.5 . . ? H11J C113 H11K 109.5 . . ? C21 C121 H12C 109.5 . . ? C21 C121 H12D 109.5 . . ? H12C C121 H12D 109.5 . . ? C21 C121 H12E 109.5 . . ? H12C C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? C22 C122 H12F 109.5 . . ? C22 C122 H12G 109.5 . . ? H12F C122 H12G 109.5 . . ? C22 C122 H12H 109.5 . . ? H12F C122 H12H 109.5 . . ? H12G C122 H12H 109.5 . . ? C23 C123 H12I 109.5 . . ? C23 C123 H12J 109.5 . . ? H12I C123 H12J 109.5 . . ? C23 C123 H12K 109.5 . . ? H12I C123 H12K 109.5 . . ? H12J C123 H12K 109.5 . . ? C31 C131 H13C 109.5 . . ? C31 C131 H13D 109.5 . . ? H13C C131 H13D 109.5 . . ? C31 C131 H13E 109.5 . . ? H13C C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? H23C C231 H23D 109.5 . . ? H23C C231 H23E 109.5 . . ? H23D C231 H23E 109.5 . . ? C51 C151 H15A 109.5 . . ? C51 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C51 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C52 C152 H15D 109.5 . . ? C52 C152 H15E 109.5 . . ? H15D C152 H15E 109.5 . . ? C52 C152 H15F 109.5 . . ? H15D C152 H15F 109.5 . . ? H15E C152 H15F 109.5 . . ? C53 C153 H15G 109.5 . . ? C53 C153 H15H 109.5 . . ? H15G C153 H15H 109.5 . . ? C53 C153 H15I 109.5 . . ? H15G C153 H15I 109.5 . . ? H15H C153 H15I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.877 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.061