# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email seth.n.brown.114@nd.edu _publ_contact_author_name 'Seth Brown' loop_ _publ_author_name 'Mauricio Quiroz-Guzman' 'Allen Oliver' 'Andrew Loza' 'Seth Brown' data_an2ntioipr _database_code_depnum_ccdc_archive 'CCDC 832123' #TrackingRef '- combined.cif' # Collected as MQI-293-1, Jan 2010 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [N,N'-Dimethyl-N,N'-bis-(2-oxido-5-(di-(4-methoxyphenyl)amino)benzyl)- ethylenediamine]titanium(IV) diisopropoxide ; _chemical_name_common (An2N{NMe}salan)Ti(OiPr)2 _chemical_melting_point ? _chemical_formula_moiety 'C52 H62 N4 O8 Ti' _chemical_formula_sum 'C52 H62 N4 O8 Ti' _chemical_formula_weight 918.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6904(6) _cell_length_b 14.3149(8) _cell_length_c 15.9465(8) _cell_angle_alpha 66.280(2) _cell_angle_beta 87.702(2) _cell_angle_gamma 78.741(2) _cell_volume 2393.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9165 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.80 _exptl_crystal_description tablet _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9410 _exptl_absorpt_correction_T_max 0.9767 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. Madison, WI USA. ; _exptl_crystal_recrystallization_method ; Crystals were deposited on standing overnight in hexanes at room temperature. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 34937 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.43 _reflns_number_total 9682 _reflns_number_gt 6830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. One isopropyl group was disordered over two positions, with the major orientation refining to 62.9(8)% occupancy. ; _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^)+(0.0721P)^2^+2.9111P] 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 9682 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1490 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Ti Ti 0.84376(4) 0.74847(4) 0.16226(3) 0.02169(15) Uani 1 1 d . A . O1 O 0.82312(17) 0.79564(15) 0.03209(13) 0.0246(4) Uani 1 1 d . . . O2 O 0.86454(16) 0.66981(15) 0.28937(13) 0.0234(4) Uani 1 1 d . . . O3 O 0.95804(19) 0.81967(17) 0.15707(15) 0.0345(5) Uani 1 1 d . . . O4 O 0.70566(18) 0.83153(15) 0.16594(13) 0.0276(5) Uani 1 1 d . . . O31 O 0.7717(3) 0.7996(2) -0.55520(18) 0.0592(8) Uani 1 1 d . . . O41 O 1.53620(18) 0.77514(18) -0.30514(16) 0.0378(6) Uani 1 1 d . . . O51 O 0.5803(3) 0.0381(2) 0.5632(2) 0.0634(8) Uani 1 1 d . . . O61 O 0.6039(2) 0.45408(19) 0.91617(15) 0.0400(6) Uani 1 1 d . . . N1 N 0.98527(19) 0.62052(18) 0.14230(15) 0.0211(5) Uani 1 1 d . . . N2 N 0.74383(19) 0.61444(18) 0.17669(15) 0.0209(5) Uani 1 1 d . . . N3 N 1.0595(2) 0.7685(2) -0.27123(16) 0.0277(6) Uani 1 1 d . A . N4 N 0.6679(2) 0.3960(2) 0.58941(16) 0.0301(6) Uani 1 1 d . A . C01 C 1.0662(2) 0.5684(2) 0.22483(19) 0.0257(6) Uani 1 1 d . A . H01A H 1.1014 0.6204 0.2343 0.039 Uiso 1 1 calc R . . H01B H 1.1277 0.5164 0.2158 0.039 Uiso 1 1 calc R . . H01C H 1.0226 0.5341 0.2787 0.039 Uiso 1 1 calc R . . C02 C 0.6689(2) 0.6435(2) 0.09349(19) 0.0260(6) Uani 1 1 d . A . H02A H 0.6124 0.7078 0.0835 0.039 Uiso 1 1 calc R . . H02B H 0.6271 0.5875 0.1019 0.039 Uiso 1 1 calc R . . H02C H 0.7177 0.6545 0.0402 0.039 Uiso 1 1 calc R . . C1 C 1.0580(2) 0.6673(2) 0.06339(19) 0.0246(6) Uani 1 1 d . A . H1A H 1.1201 0.6112 0.0598 0.029 Uiso 1 1 calc R . . H1B H 1.0967 0.7165 0.0756 0.029 Uiso 1 1 calc R . . C2 C 0.9306(2) 0.5429(2) 0.12778(19) 0.0227(6) Uani 1 1 d . A . H2A H 0.9895 0.4786 0.1397 0.027 Uiso 1 1 calc R . . H2B H 0.9011 0.5708 0.0633 0.027 Uiso 1 1 calc R . . C3 C 0.8305(2) 0.5178(2) 0.19140(19) 0.0229(6) Uani 1 1 d . A . H3A H 0.7924 0.4681 0.1794 0.027 Uiso 1 1 calc R . . H3B H 0.8609 0.4848 0.2559 0.027 Uiso 1 1 calc R . . C4 C 0.6640(2) 0.5960(2) 0.25520(18) 0.0233(6) Uani 1 1 d . A . H4A H 0.6200 0.5428 0.2570 0.028 Uiso 1 1 calc R . . H4B H 0.6067 0.6612 0.2433 0.028 Uiso 1 1 calc R . . C5A C 0.9515(9) 0.9880(7) 0.1494(6) 0.058(2) Uani 0.629(8) 1 d P A 1 H5A1 H 0.8705 0.9862 0.1670 0.087 Uiso 0.629(8) 1 calc PR A 1 H5A2 H 0.9568 1.0582 0.1052 0.087 Uiso 0.629(8) 1 calc PR A 1 H5A3 H 1.0013 0.9696 0.2039 0.087 Uiso 0.629(8) 1 calc PR A 1 C6A C 0.9907(5) 0.9132(4) 0.1075(5) 0.0429(18) Uani 0.629(8) 1 d P A 1 H6A H 0.9487 0.9426 0.0462 0.051 Uiso 0.629(8) 1 calc PR A 1 C7A C 1.1199(10) 0.9075(9) 0.0894(12) 0.136(7) Uani 0.629(8) 1 d P A 1 H7A1 H 1.1433 0.8656 0.0535 0.204 Uiso 0.629(8) 1 calc PR A 1 H7A2 H 1.1651 0.8752 0.1479 0.204 Uiso 0.629(8) 1 calc PR A 1 H7A3 H 1.1347 0.9778 0.0552 0.204 Uiso 0.629(8) 1 calc PR A 1 C5B C 0.9425(16) 0.9721(13) 0.1973(11) 0.058(2) Uani 0.371(8) 1 d P A 2 H5B1 H 0.8600 0.9684 0.2077 0.087 Uiso 0.371(8) 1 calc PR A 2 H5B2 H 0.9499 1.0256 0.1363 0.087 Uiso 0.371(8) 1 calc PR A 2 H5B3 H 0.9738 0.9899 0.2439 0.087 Uiso 0.371(8) 1 calc PR A 2 C6B C 1.0148(9) 0.8606(9) 0.2040(8) 0.050(3) Uani 0.371(8) 1 d P A 2 H6B H 1.0338 0.8106 0.2692 0.061 Uiso 0.371(8) 1 calc PR A 2 C7B C 1.1217(11) 0.8871(12) 0.1547(10) 0.054(4) Uani 0.371(8) 1 d P A 2 H7B1 H 1.1790 0.8231 0.1655 0.081 Uiso 0.371(8) 1 calc PR A 2 H7B2 H 1.1547 0.9312 0.1770 0.081 Uiso 0.371(8) 1 calc PR A 2 H7B3 H 1.1022 0.9246 0.0888 0.081 Uiso 0.371(8) 1 calc PR A 2 C8 C 0.6484(4) 1.0160(3) 0.0825(3) 0.0636(12) Uani 1 1 d . . . H8A H 0.7237 1.0177 0.0531 0.095 Uiso 1 1 calc R A . H8B H 0.6539 1.0283 0.1382 0.095 Uiso 1 1 calc R . . H8C H 0.5880 1.0702 0.0401 0.095 Uiso 1 1 calc R . . C9 C 0.6175(3) 0.9116(2) 0.1069(2) 0.0298(7) Uani 1 1 d . A . H9 H 0.6115 0.9006 0.0493 0.036 Uiso 1 1 calc R . . C10 C 0.5019(3) 0.9048(3) 0.1526(3) 0.0528(11) Uani 1 1 d . . . H10A H 0.4845 0.8357 0.1677 0.079 Uiso 1 1 calc R A . H10B H 0.4401 0.9579 0.1109 0.079 Uiso 1 1 calc R . . H10C H 0.5060 0.9163 0.2089 0.079 Uiso 1 1 calc R . . C11 C 0.9930(2) 0.7242(2) -0.02849(19) 0.0217(6) Uani 1 1 d . . . C12 C 0.8818(2) 0.7880(2) -0.03955(19) 0.0214(6) Uani 1 1 d . A . C13 C 0.8322(2) 0.8446(2) -0.12792(19) 0.0227(6) Uani 1 1 d . . . H13 H 0.7565 0.8869 -0.1362 0.027 Uiso 1 1 calc R A . C14 C 0.8906(2) 0.8405(2) -0.2038(2) 0.0244(6) Uani 1 1 d . A . H14 H 0.8562 0.8822 -0.2634 0.029 Uiso 1 1 calc R . . C15 C 0.9996(2) 0.7757(2) -0.19362(19) 0.0233(6) Uani 1 1 d . . . C16 C 1.0478(2) 0.7171(2) -0.10551(19) 0.0231(6) Uani 1 1 d . A . H16 H 1.1207 0.6707 -0.0974 0.028 Uiso 1 1 calc R . . C21 C 0.7232(2) 0.5609(2) 0.34816(19) 0.0219(6) Uani 1 1 d . . . C22 C 0.8176(2) 0.6020(2) 0.36089(19) 0.0213(6) Uani 1 1 d . A . C23 C 0.8625(2) 0.5720(2) 0.44923(19) 0.0239(6) Uani 1 1 d . . . H23 H 0.9273 0.5985 0.4580 0.029 Uiso 1 1 calc R A . C24 C 0.8150(3) 0.5044(2) 0.52468(19) 0.0259(6) Uani 1 1 d . A . H24 H 0.8474 0.4848 0.5844 0.031 Uiso 1 1 calc R . . C25 C 0.7197(3) 0.4651(2) 0.51313(19) 0.0254(6) Uani 1 1 d . . . C26 C 0.6765(2) 0.4927(2) 0.42456(19) 0.0241(6) Uani 1 1 d . A . H26 H 0.6133 0.4641 0.4161 0.029 Uiso 1 1 calc R . . C31 C 0.9907(2) 0.7779(2) -0.34712(19) 0.0253(6) Uani 1 1 d . . . C32 C 1.0032(3) 0.8467(3) -0.4355(2) 0.0381(8) Uani 1 1 d . A . H32 H 1.0595 0.8896 -0.4474 0.046 Uiso 1 1 calc R . . C33 C 0.9335(3) 0.8537(3) -0.5078(2) 0.0449(9) Uani 1 1 d . . . H33 H 0.9446 0.8994 -0.5688 0.054 Uiso 1 1 calc R A . C34 C 0.8490(3) 0.7947(3) -0.4907(2) 0.0416(9) Uani 1 1 d . A . C35 C 0.8358(3) 0.7265(3) -0.4025(2) 0.0357(8) Uani 1 1 d . . . H35 H 0.7772 0.6858 -0.3906 0.043 Uiso 1 1 calc R A . C36 C 0.9067(3) 0.7166(2) -0.3315(2) 0.0280(7) Uani 1 1 d . A . H36 H 0.8982 0.6675 -0.2713 0.034 Uiso 1 1 calc R . . C37 C 0.7892(5) 0.8623(4) -0.6485(3) 0.0730(15) Uani 1 1 d . . . H37A H 0.7288 0.8599 -0.6880 0.109 Uiso 1 1 calc R . . H37B H 0.8663 0.8358 -0.6656 0.109 Uiso 1 1 calc R . . H37C H 0.7847 0.9343 -0.6559 0.109 Uiso 1 1 calc R . . C41 C 1.1792(2) 0.7739(2) -0.28033(19) 0.0252(6) Uani 1 1 d . . . C42 C 1.2492(3) 0.7284(2) -0.33285(19) 0.0255(6) Uani 1 1 d . A . H42 H 1.2154 0.6950 -0.3636 0.031 Uiso 1 1 calc R . . C43 C 1.3663(3) 0.7314(2) -0.3404(2) 0.0269(7) Uani 1 1 d . . . H43 H 1.4121 0.7013 -0.3771 0.032 Uiso 1 1 calc R A . C44 C 1.4182(3) 0.7782(2) -0.2946(2) 0.0290(7) Uani 1 1 d . A . C45 C 1.3506(3) 0.8235(3) -0.2431(2) 0.0338(7) Uani 1 1 d . . . H45 H 1.3852 0.8556 -0.2116 0.041 Uiso 1 1 calc R A . C46 C 1.2320(3) 0.8222(2) -0.2369(2) 0.0305(7) Uani 1 1 d . A . H46 H 1.1860 0.8551 -0.2022 0.037 Uiso 1 1 calc R . . C47 C 1.5942(3) 0.8105(4) -0.2496(3) 0.0523(10) Uani 1 1 d . . . H47A H 1.6771 0.8051 -0.2632 0.079 Uiso 1 1 calc R . . H47B H 1.5862 0.7674 -0.1847 0.079 Uiso 1 1 calc R . . H47C H 1.5589 0.8832 -0.2627 0.079 Uiso 1 1 calc R . . C51 C 0.6523(3) 0.3009(2) 0.58602(19) 0.0279(7) Uani 1 1 d . . . C52 C 0.5397(3) 0.2818(3) 0.5859(2) 0.0350(8) Uani 1 1 d . A . H52 H 0.4750 0.3314 0.5899 0.042 Uiso 1 1 calc R . . C53 C 0.5202(3) 0.1934(3) 0.5801(2) 0.0413(8) Uani 1 1 d . . . H53 H 0.4430 0.1813 0.5811 0.050 Uiso 1 1 calc R A . C54 C 0.6119(4) 0.1234(3) 0.5729(2) 0.0451(9) Uani 1 1 d . A . C55 C 0.7245(4) 0.1386(3) 0.5731(3) 0.0504(10) Uani 1 1 d . . . H55 H 0.7881 0.0885 0.5686 0.060 Uiso 1 1 calc R A . C56 C 0.7445(3) 0.2292(3) 0.5798(2) 0.0433(9) Uani 1 1 d . A . H56 H 0.8219 0.2404 0.5801 0.052 Uiso 1 1 calc R . . C57 C 0.6670(4) -0.0244(3) 0.5363(3) 0.0695(13) Uani 1 1 d . . . H57A H 0.6360 -0.0818 0.5331 0.104 Uiso 1 1 calc R . . H57B H 0.7333 -0.0526 0.5809 0.104 Uiso 1 1 calc R . . H57C H 0.6929 0.0171 0.4758 0.104 Uiso 1 1 calc R . . C61 C 0.6527(2) 0.4092(2) 0.6724(2) 0.0271(7) Uani 1 1 d . . . C62 C 0.6580(3) 0.3238(3) 0.7561(2) 0.0300(7) Uani 1 1 d . A . H62 H 0.6731 0.2557 0.7572 0.036 Uiso 1 1 calc R . . C63 C 0.6416(3) 0.3364(3) 0.8381(2) 0.0322(7) Uani 1 1 d . . . H63 H 0.6448 0.2772 0.8942 0.039 Uiso 1 1 calc R A . C64 C 0.6207(3) 0.4340(3) 0.8382(2) 0.0320(7) Uani 1 1 d . A . C65 C 0.6139(2) 0.5206(3) 0.7553(2) 0.0307(7) Uani 1 1 d . . . H65 H 0.5988 0.5885 0.7550 0.037 Uiso 1 1 calc R A . C66 C 0.6291(2) 0.5085(2) 0.6733(2) 0.0281(7) Uani 1 1 d . A . H66 H 0.6236 0.5682 0.6172 0.034 Uiso 1 1 calc R . . C67 C 0.6121(4) 0.3664(4) 1.0043(3) 0.0575(11) Uani 1 1 d . . . H67A H 0.5982 0.3919 1.0531 0.086 Uiso 1 1 calc R . . H67B H 0.6901 0.3226 1.0138 0.086 Uiso 1 1 calc R . . H67C H 0.5534 0.3255 1.0054 0.086 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 Ti 0.0215(3) 0.0256(3) 0.0205(3) -0.0105(2) 0.0019(2) -0.0079(2) O1 0.0233(11) 0.0280(11) 0.0201(10) -0.0083(9) 0.0030(8) -0.0029(8) O2 0.0225(10) 0.0300(11) 0.0211(10) -0.0116(9) 0.0012(8) -0.0100(9) O3 0.0356(13) 0.0350(12) 0.0403(13) -0.0177(11) 0.0059(10) -0.0192(10) O4 0.0305(12) 0.0298(11) 0.0211(10) -0.0113(9) -0.0016(9) 0.0003(9) O31 0.0701(19) 0.0624(18) 0.0469(16) -0.0245(14) -0.0288(14) -0.0048(15) O41 0.0233(11) 0.0502(14) 0.0470(14) -0.0234(12) 0.0066(10) -0.0158(10) O51 0.069(2) 0.0564(18) 0.071(2) -0.0345(16) 0.0187(16) -0.0112(15) O61 0.0394(14) 0.0616(16) 0.0257(12) -0.0230(12) 0.0046(10) -0.0134(12) N1 0.0186(12) 0.0273(13) 0.0176(12) -0.0077(10) -0.0002(9) -0.0074(10) N2 0.0168(12) 0.0289(13) 0.0188(12) -0.0108(10) -0.0008(9) -0.0054(10) N3 0.0202(13) 0.0473(16) 0.0199(13) -0.0170(12) 0.0027(10) -0.0094(11) N4 0.0388(16) 0.0353(15) 0.0208(13) -0.0127(11) 0.0073(11) -0.0157(12) C01 0.0193(15) 0.0345(17) 0.0215(15) -0.0097(13) -0.0019(11) -0.0039(12) C02 0.0230(15) 0.0361(17) 0.0219(15) -0.0127(13) -0.0030(12) -0.0098(13) C1 0.0166(14) 0.0329(16) 0.0243(15) -0.0114(13) 0.0017(11) -0.0057(12) C2 0.0228(15) 0.0250(15) 0.0223(15) -0.0108(12) -0.0009(11) -0.0059(12) C3 0.0235(15) 0.0260(15) 0.0218(15) -0.0110(12) 0.0004(12) -0.0077(12) C4 0.0169(14) 0.0348(16) 0.0211(14) -0.0124(13) 0.0017(11) -0.0091(12) C5A 0.062(4) 0.057(4) 0.074(7) -0.040(6) 0.022(5) -0.030(3) C6A 0.036(3) 0.028(3) 0.067(4) -0.019(3) 0.020(3) -0.015(2) C7A 0.067(7) 0.053(6) 0.289(19) -0.069(10) 0.103(11) -0.036(5) C5B 0.062(4) 0.057(4) 0.074(7) -0.040(6) 0.022(5) -0.030(3) C6B 0.043(6) 0.075(8) 0.064(8) -0.049(7) 0.007(5) -0.034(6) C7B 0.023(6) 0.043(7) 0.090(10) -0.012(7) 0.002(7) -0.027(5) C8 0.057(3) 0.034(2) 0.087(3) -0.012(2) -0.016(2) -0.0044(19) C9 0.0301(17) 0.0322(17) 0.0227(16) -0.0090(13) -0.0046(13) 0.0005(13) C10 0.036(2) 0.055(2) 0.041(2) -0.0015(18) 0.0058(17) 0.0096(18) C11 0.0194(14) 0.0268(15) 0.0202(14) -0.0085(12) 0.0011(11) -0.0096(12) C12 0.0223(15) 0.0255(15) 0.0209(14) -0.0119(12) 0.0046(11) -0.0103(12) C13 0.0201(14) 0.0256(15) 0.0235(15) -0.0102(12) 0.0008(11) -0.0067(12) C14 0.0232(15) 0.0310(16) 0.0214(15) -0.0114(13) -0.0001(12) -0.0087(12) C15 0.0213(15) 0.0330(16) 0.0212(15) -0.0136(13) 0.0049(11) -0.0125(12) C16 0.0163(14) 0.0299(16) 0.0266(15) -0.0139(13) 0.0029(11) -0.0072(12) C21 0.0173(14) 0.0286(15) 0.0213(14) -0.0121(12) 0.0012(11) -0.0035(12) C22 0.0176(14) 0.0241(15) 0.0222(14) -0.0101(12) 0.0030(11) -0.0029(11) C23 0.0177(14) 0.0310(16) 0.0259(15) -0.0140(13) -0.0009(11) -0.0055(12) C24 0.0252(16) 0.0326(16) 0.0186(14) -0.0097(13) -0.0034(12) -0.0033(13) C25 0.0262(16) 0.0294(16) 0.0212(15) -0.0106(13) 0.0039(12) -0.0066(13) C26 0.0185(14) 0.0309(16) 0.0270(16) -0.0145(13) 0.0051(12) -0.0088(12) C31 0.0216(15) 0.0339(16) 0.0225(15) -0.0151(13) -0.0005(12) -0.0015(12) C32 0.0290(18) 0.055(2) 0.0279(18) -0.0125(16) 0.0029(14) -0.0118(16) C33 0.040(2) 0.060(2) 0.0253(18) -0.0110(17) -0.0031(15) -0.0027(18) C34 0.043(2) 0.049(2) 0.036(2) -0.0228(17) -0.0145(16) 0.0009(17) C35 0.0350(19) 0.0337(18) 0.044(2) -0.0210(16) -0.0078(15) -0.0068(14) C36 0.0277(16) 0.0264(16) 0.0295(16) -0.0117(13) -0.0051(13) -0.0020(13) C37 0.105(4) 0.063(3) 0.049(3) -0.027(2) -0.037(3) 0.005(3) C41 0.0226(15) 0.0312(16) 0.0205(15) -0.0084(13) 0.0030(12) -0.0074(13) C42 0.0267(16) 0.0298(16) 0.0195(15) -0.0083(13) 0.0000(12) -0.0080(13) C43 0.0229(16) 0.0317(17) 0.0235(15) -0.0086(13) 0.0054(12) -0.0061(13) C44 0.0221(16) 0.0343(17) 0.0296(17) -0.0099(14) 0.0063(13) -0.0110(13) C45 0.0313(18) 0.047(2) 0.0360(18) -0.0241(16) 0.0062(14) -0.0204(15) C46 0.0297(17) 0.0377(18) 0.0306(17) -0.0185(15) 0.0100(13) -0.0124(14) C47 0.031(2) 0.086(3) 0.056(2) -0.037(2) 0.0096(17) -0.029(2) C51 0.0363(18) 0.0315(16) 0.0165(14) -0.0088(13) 0.0046(12) -0.0106(14) C52 0.0400(19) 0.0371(19) 0.0276(17) -0.0109(15) 0.0004(14) -0.0114(15) C53 0.049(2) 0.044(2) 0.0346(19) -0.0157(16) 0.0049(16) -0.0173(17) C54 0.068(3) 0.041(2) 0.035(2) -0.0173(17) 0.0180(18) -0.0283(19) C55 0.055(3) 0.041(2) 0.047(2) -0.0171(18) 0.0194(19) 0.0037(18) C56 0.038(2) 0.042(2) 0.045(2) -0.0135(17) 0.0167(16) -0.0093(16) C57 0.083(3) 0.043(2) 0.070(3) -0.018(2) 0.011(3) 0.004(2) C61 0.0205(15) 0.0410(18) 0.0240(15) -0.0165(14) 0.0042(12) -0.0086(13) C62 0.0275(17) 0.0368(18) 0.0272(16) -0.0128(14) 0.0060(13) -0.0109(14) C63 0.0266(17) 0.048(2) 0.0235(16) -0.0129(15) 0.0054(13) -0.0140(15) C64 0.0171(15) 0.058(2) 0.0298(17) -0.0254(16) 0.0036(12) -0.0103(14) C65 0.0170(15) 0.0452(19) 0.0381(18) -0.0254(16) 0.0003(13) -0.0055(13) C66 0.0179(15) 0.0390(18) 0.0296(16) -0.0148(14) 0.0005(12) -0.0080(13) C67 0.050(2) 0.092(3) 0.035(2) -0.028(2) 0.0052(18) -0.019(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 Ti O3 1.813(2) . ? Ti O4 1.823(2) . ? Ti O2 1.8793(19) . ? Ti O1 1.9161(19) . ? Ti N1 2.332(2) . ? Ti N2 2.366(2) . ? O1 C12 1.341(3) . ? O2 C22 1.345(3) . ? O3 C6A 1.374(5) . ? O3 C6B 1.374(9) . ? O4 C9 1.418(3) . ? O31 C34 1.367(4) . ? O31 C37 1.426(5) . ? O41 C44 1.378(3) . ? O41 C47 1.430(4) . ? O51 C57 1.390(5) . ? O51 C54 1.408(4) . ? O61 C64 1.383(4) . ? O61 C67 1.450(4) . ? N1 C2 1.481(3) . ? N1 C1 1.488(4) . ? N1 C01 1.489(3) . ? N2 C3 1.485(4) . ? N2 C02 1.486(3) . ? N2 C4 1.499(3) . ? N3 C41 1.416(4) . ? N3 C31 1.426(4) . ? N3 C15 1.427(4) . ? N4 C61 1.410(4) . ? N4 C25 1.425(4) . ? N4 C51 1.430(4) . ? C01 H01A 0.9800 . ? C01 H01B 0.9800 . ? C01 H01C 0.9800 . ? C02 H02A 0.9800 . ? C02 H02B 0.9800 . ? C02 H02C 0.9800 . ? C1 C11 1.509(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.518(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C21 1.509(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5A C6A 1.470(10) . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? C6A C7A 1.518(11) . ? C6A H6A 1.0000 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C5B C6B 1.62(2) . ? C5B H5B1 0.9800 . ? C5B H5B2 0.9800 . ? C5B H5B3 0.9800 . ? C6B C7B 1.480(15) . ? C6B H6B 1.0000 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C8 C9 1.499(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.511(5) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.393(4) . ? C11 C12 1.406(4) . ? C12 C13 1.394(4) . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.394(4) . ? C14 H14 0.9500 . ? C15 C16 1.388(4) . ? C16 H16 0.9500 . ? C21 C26 1.390(4) . ? C21 C22 1.406(4) . ? C22 C23 1.388(4) . ? C23 C24 1.382(4) . ? C23 H23 0.9500 . ? C24 C25 1.392(4) . ? C24 H24 0.9500 . ? C25 C26 1.391(4) . ? C26 H26 0.9500 . ? C31 C32 1.379(4) . ? C31 C36 1.392(4) . ? C32 C33 1.396(5) . ? C32 H32 0.9500 . ? C33 C34 1.372(5) . ? C33 H33 0.9500 . ? C34 C35 1.376(5) . ? C35 C36 1.374(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C41 C46 1.388(4) . ? C41 C42 1.404(4) . ? C42 C43 1.377(4) . ? C42 H42 0.9500 . ? C43 C44 1.391(4) . ? C43 H43 0.9500 . ? C44 C45 1.377(4) . ? C45 C46 1.390(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C51 C56 1.367(5) . ? C51 C52 1.396(4) . ? C52 C53 1.367(5) . ? C52 H52 0.9500 . ? C53 C54 1.353(5) . ? C53 H53 0.9500 . ? C54 C55 1.375(5) . ? C55 C56 1.407(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C61 C62 1.395(4) . ? C61 C66 1.400(4) . ? C62 C63 1.391(4) . ? C62 H62 0.9500 . ? C63 C64 1.371(5) . ? C63 H63 0.9500 . ? C64 C65 1.394(5) . ? C65 C66 1.387(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 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 O3 Ti O4 107.03(10) . . ? O3 Ti O2 94.37(9) . . ? O4 Ti O2 96.51(9) . . ? O3 Ti O1 95.26(9) . . ? O4 Ti O1 90.68(9) . . ? O2 Ti O1 165.75(9) . . ? O3 Ti N1 88.25(9) . . ? O4 Ti N1 163.59(9) . . ? O2 Ti N1 88.03(8) . . ? O1 Ti N1 81.80(8) . . ? O3 Ti N2 162.68(9) . . ? O4 Ti N2 90.01(9) . . ? O2 Ti N2 80.32(8) . . ? O1 Ti N2 87.42(8) . . ? N1 Ti N2 75.16(8) . . ? C12 O1 Ti 139.82(18) . . ? C22 O2 Ti 142.45(17) . . ? C6A O3 C6B 62.6(6) . . ? C6A O3 Ti 141.7(3) . . ? C6B O3 Ti 144.7(5) . . ? C9 O4 Ti 140.92(19) . . ? C34 O31 C37 116.9(3) . . ? C44 O41 C47 116.8(3) . . ? C57 O51 C54 116.5(3) . . ? C64 O61 C67 118.2(3) . . ? C2 N1 C1 109.6(2) . . ? C2 N1 C01 110.0(2) . . ? C1 N1 C01 106.3(2) . . ? C2 N1 Ti 110.80(16) . . ? C1 N1 Ti 110.95(17) . . ? C01 N1 Ti 109.07(17) . . ? C3 N2 C02 109.6(2) . . ? C3 N2 C4 110.1(2) . . ? C02 N2 C4 106.4(2) . . ? C3 N2 Ti 109.09(16) . . ? C02 N2 Ti 111.16(17) . . ? C4 N2 Ti 110.43(16) . . ? C41 N3 C31 120.5(2) . . ? C41 N3 C15 120.6(2) . . ? C31 N3 C15 117.7(2) . . ? C61 N4 C25 122.1(2) . . ? C61 N4 C51 119.5(2) . . ? C25 N4 C51 117.3(2) . . ? N1 C01 H01A 109.5 . . ? N1 C01 H01B 109.5 . . ? H01A C01 H01B 109.5 . . ? N1 C01 H01C 109.5 . . ? H01A C01 H01C 109.5 . . ? H01B C01 H01C 109.5 . . ? N2 C02 H02A 109.5 . . ? N2 C02 H02B 109.5 . . ? H02A C02 H02B 109.5 . . ? N2 C02 H02C 109.5 . . ? H02A C02 H02C 109.5 . . ? H02B C02 H02C 109.5 . . ? N1 C1 C11 115.3(2) . . ? N1 C1 H1A 108.4 . . ? C11 C1 H1A 108.5 . . ? N1 C1 H1B 108.5 . . ? C11 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N1 C2 C3 110.2(2) . . ? N1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C2 110.1(2) . . ? N2 C3 H3A 109.6 . . ? C2 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.2 . . ? N2 C4 C21 115.3(2) . . ? N2 C4 H4A 108.4 . . ? C21 C4 H4A 108.4 . . ? N2 C4 H4B 108.4 . . ? C21 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? C6A C5A H5A1 109.5 . . ? C6A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C6A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? O3 C6A C5A 111.3(5) . . ? O3 C6A C7A 115.6(6) . . ? C5A C6A C7A 109.6(7) . . ? O3 C6A H6A 106.6 . . ? C5A C6A H6A 106.6 . . ? C7A C6A H6A 106.6 . . ? C6A C7A H7A1 109.5 . . ? C6A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C6A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C6B C5B H5B1 109.5 . . ? C6B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C6B C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? O3 C6B C7B 107.1(9) . . ? O3 C6B C5B 111.9(9) . . ? C7B C6B C5B 103.0(10) . . ? O3 C6B H6B 111.5 . . ? C7B C6B H6B 111.5 . . ? C5B C6B H6B 111.5 . . ? C6B C7B H7B1 109.5 . . ? C6B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C6B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 C8 110.5(3) . . ? O4 C9 C10 109.2(3) . . ? C8 C9 C10 111.6(3) . . ? O4 C9 H9 108.5 . . ? C8 C9 H9 108.5 . . ? C10 C9 H9 108.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 119.1(3) . . ? C16 C11 C1 118.5(3) . . ? C12 C11 C1 122.3(2) . . ? O1 C12 C13 119.5(3) . . ? O1 C12 C11 121.9(2) . . ? C13 C12 C11 118.5(3) . . ? C14 C13 C12 121.4(3) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 120.6(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 118.0(3) . . ? C16 C15 N3 120.8(3) . . ? C14 C15 N3 121.2(3) . . ? C15 C16 C11 122.2(3) . . ? C15 C16 H16 118.9 . . ? C11 C16 H16 118.9 . . ? C26 C21 C22 118.9(3) . . ? C26 C21 C4 118.9(2) . . ? C22 C21 C4 121.9(3) . . ? O2 C22 C23 119.8(2) . . ? O2 C22 C21 121.2(2) . . ? C23 C22 C21 118.9(3) . . ? C24 C23 C22 121.6(3) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 118.6(3) . . ? C26 C25 N4 119.9(3) . . ? C24 C25 N4 121.5(3) . . ? C21 C26 C25 121.9(3) . . ? C21 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C32 C31 C36 118.6(3) . . ? C32 C31 N3 122.4(3) . . ? C36 C31 N3 119.0(3) . . ? C31 C32 C33 120.5(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 120.1(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? O31 C34 C33 125.1(3) . . ? O31 C34 C35 115.4(3) . . ? C33 C34 C35 119.5(3) . . ? C36 C35 C34 120.7(3) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 120.6(3) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? O31 C37 H37A 109.5 . . ? O31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C46 C41 C42 117.8(3) . . ? C46 C41 N3 121.6(3) . . ? C42 C41 N3 120.6(3) . . ? C43 C42 C41 120.9(3) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 120.5(3) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C45 C44 O41 124.8(3) . . ? C45 C44 C43 119.3(3) . . ? O41 C44 C43 115.9(3) . . ? C44 C45 C46 120.2(3) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C41 C46 C45 121.3(3) . . ? C41 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? O41 C47 H47A 109.5 . . ? O41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C56 C51 C52 118.6(3) . . ? C56 C51 N4 121.9(3) . . ? C52 C51 N4 119.5(3) . . ? C53 C52 C51 121.6(3) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C54 C53 C52 119.4(3) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 121.1(3) . . ? C53 C54 O51 114.0(3) . . ? C55 C54 O51 124.8(4) . . ? C54 C55 C56 119.4(3) . . ? C54 C55 H55 120.3 . . ? C56 C55 H55 120.3 . . ? C51 C56 C55 119.8(3) . . ? C51 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? O51 C57 H57A 109.5 . . ? O51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C62 C61 C66 117.8(3) . . ? C62 C61 N4 121.0(3) . . ? C66 C61 N4 121.2(3) . . ? C63 C62 C61 121.3(3) . . ? C63 C62 H62 119.4 . . ? C61 C62 H62 119.4 . . ? C64 C63 C62 120.3(3) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 O61 124.4(3) . . ? C63 C64 C65 119.4(3) . . ? O61 C64 C65 116.1(3) . . ? C66 C65 C64 120.4(3) . . ? C66 C65 H65 119.8 . . ? C64 C65 H65 119.8 . . ? C65 C66 C61 120.7(3) . . ? C65 C66 H66 119.6 . . ? C61 C66 H66 119.6 . . ? O61 C67 H67A 109.5 . . ? O61 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O61 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.507 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.069 _vrf_PLAT213_an2ntioipr ; RESPONSE: This carbon is part of a disordered iPr group. It exhibits large thermal motion, despite being modeled over two sites. This large thermal displacement manifests in other alerts below. ; _vrf_PLAT230_an2ntioipr ; RESPONSE: This methoxy group is showing some thermal motion. The carbon is shifting more than the oxygen, hence this alert. ; _vrf_PLAT413_an2ntioipr ; RESPONSE: This close contact is the result of one of the components of the disordered iPr group being in close proximity to a nearby H62/C62 on a neighboring molecule. ; #==END data_salan _database_code_depnum_ccdc_archive 'CCDC 832124' #TrackingRef '- combined.cif' # Collected as nd018 at the synchrotron _audit_creation_method SHELXL-97 _chemical_name_systematic ; [N,N'-Dimethyl-N,N'-bis-(2-oxido-5-(di-(4-methoxyphenyl)amino)benzyl)- ethylenediamine]titanium(IV) \a-oxyisobutyrate ; _chemical_name_common (An2N{NMe}salan)Ti(OCMe2CO2) _chemical_melting_point . _chemical_formula_moiety 'C50 H54 N4 O9 Ti' _chemical_formula_sum 'C50 H54 N4 O9 Ti' _chemical_formula_weight 902.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.3056 0.5263 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.703(2) _cell_length_b 13.811(2) _cell_length_c 14.969(3) _cell_angle_alpha 69.740(2) _cell_angle_beta 79.478(2) _cell_angle_gamma 73.082(2) _cell_volume 2347.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1635 _cell_measurement_theta_min 3.968 _cell_measurement_theta_max 22.971 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9791 _exptl_absorpt_correction_T_max 0.9947 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. Madison, WI USA. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 23821 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.1065 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.97 _diffrn_reflns_theta_max 27.86 _reflns_number_total 8573 _reflns_number_gt 4662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8573 _refine_ls_number_parameters 745 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1272 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 Ti Ti 0.51778(5) -0.01062(5) 0.26355(4) 0.02812(18) Uani 1 1 d . . . O1 O 0.60357(18) 0.08498(18) 0.23652(15) 0.0314(6) Uani 1 1 d . . . O2 O 0.44194(18) 0.00502(18) 0.37694(15) 0.0308(6) Uani 1 1 d . . . O3 O 0.60979(19) -0.14291(19) 0.31595(15) 0.0346(6) Uani 1 1 d . . . O4 O 0.57789(19) -0.05002(19) 0.14432(15) 0.0333(6) Uani 1 1 d . . . O5 O 0.6971(2) -0.1755(2) 0.08811(19) 0.0567(8) Uani 1 1 d . . . O31 O 0.9690(2) 0.6763(2) -0.03244(18) 0.0459(7) Uani 1 1 d . . . O41 O 0.5384(3) 0.5232(3) -0.4110(2) 0.0883(12) Uani 1 1 d . . . O51 O -0.0432(3) -0.4451(3) 0.6179(3) 0.0870(12) Uani 1 1 d . . . O61 O -0.1261(2) 0.1297(2) 0.89054(19) 0.0482(7) Uani 1 1 d . . . N1 N 0.4051(2) 0.1313(2) 0.16660(19) 0.0321(7) Uani 1 1 d . . . N2 N 0.3729(2) -0.0771(2) 0.26078(18) 0.0307(7) Uani 1 1 d . . . N3 N 0.6979(3) 0.4356(2) -0.0610(2) 0.0398(8) Uani 1 1 d . . . N4 N 0.0919(2) -0.1057(2) 0.64277(19) 0.0361(7) Uani 1 1 d . . . C1 C 0.4673(3) 0.1791(3) 0.0741(2) 0.0329(9) Uani 1 1 d . . . C01 C 0.3576(4) 0.2129(3) 0.2165(3) 0.0385(9) Uani 1 1 d . . . C02 C 0.3934(4) -0.1408(4) 0.1943(3) 0.0387(10) Uani 1 1 d . . . C2 C 0.3130(3) 0.0995(3) 0.1440(3) 0.0369(9) Uani 1 1 d . . . C3 C 0.2779(3) 0.0163(3) 0.2319(3) 0.0347(9) Uani 1 1 d . . . C4 C 0.3442(4) -0.1486(3) 0.3580(2) 0.0345(9) Uani 1 1 d . . . C5 C 0.6894(3) -0.1950(3) 0.2564(3) 0.0380(9) Uani 1 1 d . . . C6 C 0.6545(3) -0.1394(3) 0.1537(3) 0.0379(9) Uani 1 1 d . . . C7 C 0.6902(5) -0.3122(4) 0.2887(4) 0.0622(14) Uani 1 1 d . . . C8 C 0.8020(4) -0.1763(5) 0.2581(4) 0.0528(12) Uani 1 1 d . . . C11 C 0.6240(3) 0.1716(3) 0.1638(2) 0.0297(8) Uani 1 1 d . . . C12 C 0.5600(3) 0.2198(3) 0.0859(2) 0.0294(8) Uani 1 1 d . . . C13 C 0.5855(3) 0.3082(3) 0.0139(2) 0.0317(8) Uani 1 1 d . . . C14 C 0.6737(3) 0.3483(3) 0.0158(2) 0.0343(9) Uani 1 1 d . . . C15 C 0.7353(3) 0.3000(3) 0.0951(2) 0.0331(8) Uani 1 1 d . . . C16 C 0.7092(3) 0.2138(3) 0.1680(2) 0.0315(8) Uani 1 1 d . . . C21 C 0.3587(3) -0.0242(3) 0.4435(2) 0.0302(8) Uani 1 1 d . . . C22 C 0.3046(3) -0.0942(3) 0.4340(2) 0.0297(8) Uani 1 1 d . . . C23 C 0.2154(3) -0.1192(3) 0.4995(2) 0.0311(8) Uani 1 1 d . . . C24 C 0.1815(3) -0.0781(3) 0.5765(2) 0.0319(8) Uani 1 1 d . . . C25 C 0.2402(3) -0.0113(3) 0.5861(2) 0.0337(9) Uani 1 1 d . . . C26 C 0.3269(3) 0.0159(3) 0.5198(2) 0.0330(9) Uani 1 1 d . . . C31 C 0.7614(3) 0.5006(3) -0.0525(2) 0.0338(9) Uani 1 1 d . . . C32 C 0.8441(3) 0.5296(3) -0.1239(3) 0.0355(9) Uani 1 1 d . . . C33 C 0.9101(3) 0.5899(3) -0.1164(3) 0.0392(9) Uani 1 1 d . . . C34 C 0.8959(3) 0.6209(3) -0.0355(3) 0.0358(9) Uani 1 1 d . . . C35 C 0.8115(3) 0.5970(3) 0.0352(3) 0.0378(9) Uani 1 1 d . . . C36 C 0.7447(3) 0.5374(3) 0.0258(3) 0.0366(9) Uani 1 1 d . . . C37 C 0.9611(3) 0.7048(3) 0.0521(3) 0.0473(10) Uani 1 1 d . . . H37A H 1.0170 0.7436 0.0454 0.071 Uiso 1 1 calc R . . H37B H 0.9735 0.6401 0.1074 0.071 Uiso 1 1 calc R . . H37C H 0.8874 0.7501 0.0615 0.071 Uiso 1 1 calc R . . C41 C 0.6570(3) 0.4595(3) -0.1508(2) 0.0356(9) Uani 1 1 d . . . C42 C 0.5721(3) 0.5481(3) -0.1821(3) 0.0423(10) Uani 1 1 d . . . C43 C 0.5307(4) 0.5734(4) -0.2694(3) 0.0519(11) Uani 1 1 d . . . C44 C 0.5733(4) 0.5070(3) -0.3246(3) 0.0527(12) Uani 1 1 d . . . C45 C 0.6571(4) 0.4169(3) -0.2928(3) 0.0467(11) Uani 1 1 d . . . C46 C 0.7001(4) 0.3929(3) -0.2068(3) 0.0411(10) Uani 1 1 d . . . C47 C 0.4497(8) 0.6150(5) -0.4436(5) 0.169(4) Uani 1 1 d . . . H47A H 0.4319 0.6187 -0.5059 0.253 Uiso 1 1 calc R . . H47B H 0.4720 0.6794 -0.4497 0.253 Uiso 1 1 calc R . . H47C H 0.3845 0.6097 -0.3974 0.253 Uiso 1 1 calc R . . C51 C 0.0527(3) -0.1930(3) 0.6418(2) 0.0350(9) Uani 1 1 d . . . C52 C 0.1197(4) -0.2957(3) 0.6668(3) 0.0458(10) Uani 1 1 d . . . C53 C 0.0844(5) -0.3784(4) 0.6572(3) 0.0557(13) Uani 1 1 d . . . C54 C -0.0177(4) -0.3574(4) 0.6247(3) 0.0555(12) Uani 1 1 d . . . C55 C -0.0855(4) -0.2563(4) 0.6023(3) 0.0522(12) Uani 1 1 d . . . C56 C -0.0498(3) -0.1741(4) 0.6108(3) 0.0423(10) Uani 1 1 d . . . C57 C -0.1424(7) -0.4284(6) 0.5784(5) 0.128(3) Uani 1 1 d . . . H57A H -0.1505 -0.4965 0.5777 0.191 Uiso 1 1 calc R . . H57B H -0.1402 -0.3795 0.5128 0.191 Uiso 1 1 calc R . . H57C H -0.2052 -0.3974 0.6171 0.191 Uiso 1 1 calc R . . C61 C 0.0350(3) -0.0457(3) 0.7054(2) 0.0343(9) Uani 1 1 d . . . C62 C 0.0101(3) -0.0987(3) 0.8015(2) 0.0332(9) Uani 1 1 d . . . C63 C -0.0437(3) -0.0434(3) 0.8647(3) 0.0355(9) Uani 1 1 d . . . C64 C -0.0723(3) 0.0673(3) 0.8333(3) 0.0358(9) Uani 1 1 d . . . C65 C -0.0488(3) 0.1211(3) 0.7378(3) 0.0376(9) Uani 1 1 d . . . C66 C 0.0033(3) 0.0655(3) 0.6734(3) 0.0347(9) Uani 1 1 d . . . C67 C -0.1708(3) 0.0765(4) 0.9841(3) 0.0523(11) Uani 1 1 d . . . H67A H -0.2070 0.1286 1.0179 0.078 Uiso 1 1 calc R . . H67B H -0.1111 0.0230 1.0201 0.078 Uiso 1 1 calc R . . H67C H -0.2250 0.0416 0.9780 0.078 Uiso 1 1 calc R . . H1B H 0.497(3) 0.125(3) 0.044(2) 0.022(9) Uiso 1 1 d . . . H65 H -0.070(2) 0.194(3) 0.715(2) 0.015(8) Uiso 1 1 d . . . H3B H 0.242(3) 0.047(2) 0.286(2) 0.026(9) Uiso 1 1 d . . . H02B H 0.412(3) -0.094(3) 0.124(3) 0.038(10) Uiso 1 1 d . . . H62 H 0.028(2) -0.172(3) 0.826(2) 0.015(8) Uiso 1 1 d . . . H1A H 0.414(3) 0.242(3) 0.028(2) 0.039(10) Uiso 1 1 d . . . H13 H 0.540(3) 0.342(3) -0.042(3) 0.048(11) Uiso 1 1 d . . . H35 H 0.790(3) 0.621(3) 0.094(2) 0.043(10) Uiso 1 1 d . . . H36 H 0.689(3) 0.515(3) 0.079(3) 0.055(12) Uiso 1 1 d . . . H3A H 0.217(3) -0.004(3) 0.220(2) 0.041(10) Uiso 1 1 d . . . H26 H 0.361(3) 0.062(3) 0.533(2) 0.029(9) Uiso 1 1 d . . . H16 H 0.756(3) 0.177(3) 0.223(2) 0.042(10) Uiso 1 1 d . . . H15 H 0.801(3) 0.321(3) 0.100(2) 0.030(9) Uiso 1 1 d . . . H01A H 0.303(3) 0.185(3) 0.273(3) 0.046(11) Uiso 1 1 d . . . H02A H 0.330(3) -0.166(3) 0.195(2) 0.034(10) Uiso 1 1 d . . . H2A H 0.340(3) 0.071(3) 0.093(2) 0.031(10) Uiso 1 1 d . . . H25 H 0.222(2) 0.012(2) 0.638(2) 0.023(8) Uiso 1 1 d . . . H23 H 0.179(3) -0.163(3) 0.486(2) 0.032(10) Uiso 1 1 d . . . H66 H 0.018(3) 0.099(3) 0.609(3) 0.048(11) Uiso 1 1 d . . . H42 H 0.537(3) 0.596(3) -0.142(2) 0.043(10) Uiso 1 1 d . . . H45 H 0.690(3) 0.370(3) -0.329(3) 0.047(11) Uiso 1 1 d . . . H8A H 0.824(3) -0.212(3) 0.321(3) 0.050(12) Uiso 1 1 d . . . H01C H 0.317(3) 0.283(3) 0.166(3) 0.044(11) Uiso 1 1 d . . . H56 H -0.102(3) -0.097(3) 0.595(2) 0.043(10) Uiso 1 1 d . . . H63 H -0.063(3) -0.089(3) 0.931(3) 0.059(12) Uiso 1 1 d . . . H7A H 0.740(3) -0.350(3) 0.242(3) 0.052(12) Uiso 1 1 d . . . H02C H 0.453(3) -0.208(3) 0.221(3) 0.044(11) Uiso 1 1 d . . . H4B H 0.412(4) -0.204(3) 0.371(3) 0.059(13) Uiso 1 1 d . . . H46 H 0.755(3) 0.332(3) -0.189(2) 0.041(11) Uiso 1 1 d . . . H4A H 0.286(3) -0.181(3) 0.350(3) 0.058(12) Uiso 1 1 d . . . H2B H 0.242(3) 0.170(3) 0.124(3) 0.056(12) Uiso 1 1 d . . . H01B H 0.417(3) 0.231(3) 0.237(2) 0.042(11) Uiso 1 1 d . . . H52 H 0.187(3) -0.310(3) 0.696(3) 0.052(12) Uiso 1 1 d . . . H33 H 0.971(4) 0.606(3) -0.169(3) 0.070(14) Uiso 1 1 d . . . H8C H 0.858(4) -0.216(4) 0.218(3) 0.081(15) Uiso 1 1 d . . . H32 H 0.855(3) 0.511(3) -0.177(3) 0.056(13) Uiso 1 1 d . . . H8B H 0.793(4) -0.088(4) 0.228(3) 0.082(15) Uiso 1 1 d . . . H55 H -0.159(4) -0.240(3) 0.578(3) 0.061(13) Uiso 1 1 d . . . H53 H 0.131(4) -0.448(4) 0.678(3) 0.075(16) Uiso 1 1 d . . . H7C H 0.715(4) -0.344(4) 0.353(4) 0.087(17) Uiso 1 1 d . . . H43 H 0.469(4) 0.639(4) -0.290(3) 0.082(15) Uiso 1 1 d . . . H7B H 0.611(5) -0.324(4) 0.284(3) 0.095(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0286(4) 0.0335(4) 0.0221(3) -0.0090(3) 0.0006(3) -0.0088(3) O1 0.0310(13) 0.0362(15) 0.0251(12) -0.0046(11) -0.0019(10) -0.0116(11) O2 0.0317(13) 0.0373(14) 0.0258(12) -0.0111(11) 0.0028(10) -0.0138(11) O3 0.0397(15) 0.0330(14) 0.0287(13) -0.0089(11) -0.0026(11) -0.0068(12) O4 0.0324(14) 0.0405(16) 0.0262(12) -0.0123(11) -0.0011(11) -0.0065(12) O5 0.0537(18) 0.075(2) 0.0447(16) -0.0392(16) -0.0074(14) 0.0066(16) O31 0.0501(17) 0.0493(17) 0.0440(15) -0.0157(13) -0.0012(13) -0.0213(14) O41 0.144(3) 0.065(2) 0.057(2) -0.0236(18) -0.056(2) 0.007(2) O51 0.120(3) 0.080(3) 0.088(3) -0.044(2) 0.022(2) -0.062(2) O61 0.0486(17) 0.0542(18) 0.0493(16) -0.0309(14) 0.0083(13) -0.0138(14) N1 0.0306(17) 0.0382(18) 0.0275(15) -0.0089(14) -0.0027(13) -0.0101(14) N2 0.0353(17) 0.0356(18) 0.0224(14) -0.0114(13) 0.0001(12) -0.0091(14) N3 0.055(2) 0.041(2) 0.0284(16) -0.0042(14) -0.0070(15) -0.0253(17) N4 0.0376(18) 0.0421(19) 0.0309(16) -0.0156(14) 0.0134(14) -0.0185(15) C1 0.033(2) 0.040(2) 0.0242(18) -0.0069(18) -0.0011(16) -0.0112(18) C01 0.036(2) 0.040(3) 0.038(2) -0.016(2) 0.0041(19) -0.007(2) C02 0.042(2) 0.053(3) 0.031(2) -0.021(2) 0.0046(19) -0.022(2) C2 0.035(2) 0.041(2) 0.034(2) -0.0068(19) -0.0045(18) -0.0149(19) C3 0.031(2) 0.042(2) 0.034(2) -0.0107(18) -0.0001(17) -0.0156(19) C4 0.041(2) 0.035(2) 0.0278(19) -0.0101(17) 0.0074(17) -0.016(2) C5 0.036(2) 0.040(2) 0.039(2) -0.0206(18) -0.0065(17) 0.0008(18) C6 0.029(2) 0.048(3) 0.038(2) -0.0193(19) 0.0006(17) -0.0078(19) C7 0.080(4) 0.041(3) 0.062(3) -0.022(3) -0.017(3) 0.004(3) C8 0.040(3) 0.075(4) 0.049(3) -0.033(3) -0.009(2) -0.002(2) C11 0.033(2) 0.031(2) 0.0241(18) -0.0092(16) 0.0037(15) -0.0093(17) C12 0.0289(19) 0.033(2) 0.0266(18) -0.0088(16) -0.0024(15) -0.0080(16) C13 0.035(2) 0.033(2) 0.0268(18) -0.0094(16) -0.0023(16) -0.0080(17) C14 0.039(2) 0.036(2) 0.0278(19) -0.0098(17) 0.0026(16) -0.0127(18) C15 0.037(2) 0.035(2) 0.0292(19) -0.0080(17) -0.0005(16) -0.0144(18) C16 0.031(2) 0.035(2) 0.0277(19) -0.0096(17) -0.0024(16) -0.0080(17) C21 0.031(2) 0.035(2) 0.0221(17) -0.0076(16) 0.0010(15) -0.0081(17) C22 0.0303(19) 0.033(2) 0.0253(18) -0.0090(16) -0.0030(15) -0.0072(16) C23 0.033(2) 0.031(2) 0.0302(19) -0.0108(16) -0.0013(16) -0.0088(17) C24 0.032(2) 0.036(2) 0.0260(18) -0.0077(16) -0.0009(15) -0.0088(17) C25 0.037(2) 0.044(2) 0.0219(18) -0.0153(17) 0.0020(16) -0.0106(18) C26 0.036(2) 0.041(2) 0.0289(19) -0.0132(17) -0.0032(16) -0.0161(19) C31 0.041(2) 0.028(2) 0.0272(19) -0.0029(16) -0.0052(16) -0.0057(17) C32 0.037(2) 0.039(2) 0.028(2) -0.0079(18) -0.0020(17) -0.0090(18) C33 0.037(2) 0.040(2) 0.035(2) -0.0093(18) -0.0031(18) -0.0056(19) C34 0.033(2) 0.034(2) 0.039(2) -0.0095(17) -0.0015(17) -0.0112(18) C35 0.042(2) 0.037(2) 0.035(2) -0.0144(18) 0.0009(18) -0.0104(19) C36 0.041(2) 0.035(2) 0.031(2) -0.0083(17) 0.0023(18) -0.0112(19) C37 0.049(3) 0.045(3) 0.057(3) -0.025(2) -0.002(2) -0.016(2) C41 0.044(2) 0.037(2) 0.0271(19) -0.0062(17) -0.0033(16) -0.0176(19) C42 0.052(3) 0.035(2) 0.040(2) -0.0160(19) -0.003(2) -0.007(2) C43 0.060(3) 0.043(3) 0.051(3) -0.016(2) -0.024(2) 0.005(2) C44 0.084(3) 0.042(3) 0.034(2) -0.011(2) -0.024(2) -0.007(2) C45 0.069(3) 0.040(3) 0.036(2) -0.020(2) -0.001(2) -0.012(2) C46 0.050(3) 0.034(2) 0.037(2) -0.0107(19) -0.0015(19) -0.010(2) C47 0.264(10) 0.101(5) 0.135(6) -0.061(5) -0.162(7) 0.080(6) C51 0.040(2) 0.039(2) 0.0265(18) -0.0128(17) 0.0074(16) -0.0139(19) C52 0.044(3) 0.047(3) 0.042(2) -0.012(2) 0.008(2) -0.013(2) C53 0.071(3) 0.043(3) 0.047(3) -0.017(2) 0.020(2) -0.017(3) C54 0.078(4) 0.061(3) 0.044(2) -0.026(2) 0.017(2) -0.043(3) C55 0.056(3) 0.073(4) 0.040(2) -0.027(2) 0.006(2) -0.029(3) C56 0.043(2) 0.050(3) 0.034(2) -0.0159(19) 0.0060(18) -0.013(2) C57 0.168(7) 0.144(7) 0.129(6) -0.059(5) -0.003(5) -0.114(6) C61 0.028(2) 0.047(2) 0.0338(19) -0.0207(18) 0.0043(16) -0.0121(18) C62 0.033(2) 0.036(2) 0.0276(19) -0.0086(17) -0.0017(16) -0.0049(18) C63 0.030(2) 0.049(3) 0.027(2) -0.0134(19) 0.0009(16) -0.0096(19) C64 0.028(2) 0.049(3) 0.037(2) -0.0236(19) 0.0003(16) -0.0073(18) C65 0.035(2) 0.029(2) 0.048(2) -0.013(2) -0.0007(18) -0.0068(18) C66 0.031(2) 0.040(2) 0.030(2) -0.0079(18) 0.0046(16) -0.0121(18) C67 0.050(3) 0.069(3) 0.043(2) -0.035(2) 0.006(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 Ti O2 1.842(2) . ? Ti O1 1.844(2) . ? Ti O3 1.849(2) . ? Ti O4 1.999(2) . ? Ti N1 2.270(3) . ? Ti N2 2.295(3) . ? O1 C11 1.364(4) . ? O2 C21 1.363(4) . ? O3 C5 1.423(4) . ? O4 C6 1.312(4) . ? O5 C6 1.222(4) . ? O31 C34 1.379(4) . ? O31 C37 1.429(4) . ? O41 C44 1.367(4) . ? O41 C47 1.434(6) . ? O51 C54 1.381(5) . ? O51 C57 1.414(7) . ? O61 C64 1.378(4) . ? O61 C67 1.436(4) . ? N1 C01 1.488(5) . ? N1 C2 1.491(5) . ? N1 C1 1.500(4) . ? N2 C3 1.486(5) . ? N2 C02 1.487(4) . ? N2 C4 1.498(4) . ? N3 C14 1.413(4) . ? N3 C31 1.419(5) . ? N3 C41 1.425(4) . ? N4 C24 1.415(4) . ? N4 C61 1.425(4) . ? N4 C51 1.438(4) . ? C1 C12 1.505(5) . ? C1 H1B 0.95(3) . ? C1 H1A 1.05(4) . ? C01 H01A 1.03(4) . ? C01 H01C 1.06(4) . ? C01 H01B 0.98(4) . ? C02 H02B 1.05(4) . ? C02 H02A 0.96(4) . ? C02 H02C 1.02(4) . ? C2 C3 1.512(5) . ? C2 H2A 0.94(3) . ? C2 H2B 1.11(4) . ? C3 H3B 1.01(3) . ? C3 H3A 0.95(4) . ? C4 C22 1.509(5) . ? C4 H4B 0.97(4) . ? C4 H4A 1.00(4) . ? C5 C7 1.518(6) . ? C5 C8 1.532(6) . ? C5 C6 1.544(5) . ? C7 H7A 1.02(4) . ? C7 H7C 0.98(5) . ? C7 H7B 1.08(5) . ? C8 H8A 0.95(4) . ? C8 H8C 1.01(5) . ? C8 H8B 1.13(5) . ? C11 C16 1.390(5) . ? C11 C12 1.399(5) . ? C12 C13 1.396(5) . ? C13 C14 1.394(5) . ? C13 H13 1.00(4) . ? C14 C15 1.397(5) . ? C15 C16 1.384(5) . ? C15 H15 0.98(3) . ? C16 H16 1.00(4) . ? C21 C26 1.384(5) . ? C21 C22 1.394(5) . ? C22 C23 1.398(5) . ? C23 C24 1.402(5) . ? C23 H23 0.95(3) . ? C24 C25 1.399(5) . ? C25 C26 1.386(5) . ? C25 H25 0.91(3) . ? C26 H26 0.95(3) . ? C31 C36 1.391(5) . ? C31 C32 1.394(5) . ? C32 C33 1.384(5) . ? C32 H32 0.90(4) . ? C33 C34 1.385(5) . ? C33 H33 1.01(4) . ? C34 C35 1.389(5) . ? C35 C36 1.396(5) . ? C35 H35 1.01(3) . ? C36 H36 0.99(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C41 C42 1.378(5) . ? C41 C46 1.386(5) . ? C42 C43 1.391(5) . ? C42 H42 1.01(4) . ? C43 C44 1.374(6) . ? C43 H43 1.00(5) . ? C44 C45 1.383(6) . ? C45 C46 1.386(5) . ? C45 H45 0.95(4) . ? C46 H46 0.92(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C51 C56 1.385(5) . ? C51 C52 1.386(5) . ? C52 C53 1.401(6) . ? C52 H52 0.97(4) . ? C53 C54 1.385(7) . ? C53 H53 0.95(5) . ? C54 C55 1.373(7) . ? C55 C56 1.389(6) . ? C55 H55 1.00(4) . ? C56 H56 1.05(4) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C61 C62 1.395(5) . ? C61 C66 1.396(5) . ? C62 C63 1.380(5) . ? C62 H62 0.93(3) . ? C63 C64 1.390(5) . ? C63 H63 1.00(4) . ? C64 C65 1.387(5) . ? C65 C66 1.393(5) . ? C65 H65 0.91(3) . ? C66 H66 0.92(4) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 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 O2 Ti O1 100.15(10) . . ? O2 Ti O3 96.66(10) . . ? O1 Ti O3 105.34(11) . . ? O2 Ti O4 166.79(10) . . ? O1 Ti O4 93.03(10) . . ? O3 Ti O4 80.57(10) . . ? O2 Ti N1 96.12(10) . . ? O1 Ti N1 82.25(10) . . ? O3 Ti N1 163.70(10) . . ? O4 Ti N1 84.69(10) . . ? O2 Ti N2 82.66(10) . . ? O1 Ti N2 159.38(10) . . ? O3 Ti N2 94.52(11) . . ? O4 Ti N2 84.67(9) . . ? N1 Ti N2 77.14(10) . . ? C11 O1 Ti 138.4(2) . . ? C21 O2 Ti 142.9(2) . . ? C5 O3 Ti 120.6(2) . . ? C6 O4 Ti 116.6(2) . . ? C34 O31 C37 117.3(3) . . ? C44 O41 C47 116.6(4) . . ? C54 O51 C57 117.7(5) . . ? C64 O61 C67 116.8(3) . . ? C01 N1 C2 108.8(3) . . ? C01 N1 C1 109.1(3) . . ? C2 N1 C1 108.1(3) . . ? C01 N1 Ti 108.6(2) . . ? C2 N1 Ti 111.0(2) . . ? C1 N1 Ti 111.2(2) . . ? C3 N2 C02 109.2(3) . . ? C3 N2 C4 109.6(3) . . ? C02 N2 C4 106.2(3) . . ? C3 N2 Ti 106.3(2) . . ? C02 N2 Ti 114.9(2) . . ? C4 N2 Ti 110.6(2) . . ? C14 N3 C31 122.6(3) . . ? C14 N3 C41 118.9(3) . . ? C31 N3 C41 118.5(3) . . ? C24 N4 C61 122.3(3) . . ? C24 N4 C51 118.4(3) . . ? C61 N4 C51 119.2(3) . . ? N1 C1 C12 113.9(3) . . ? N1 C1 H1B 107.5(19) . . ? C12 C1 H1B 109.2(19) . . ? N1 C1 H1A 110.8(18) . . ? C12 C1 H1A 108.4(19) . . ? H1B C1 H1A 107(3) . . ? N1 C01 H01A 109(2) . . ? N1 C01 H01C 107.2(19) . . ? H01A C01 H01C 111(3) . . ? N1 C01 H01B 110(2) . . ? H01A C01 H01B 113(3) . . ? H01C C01 H01B 107(3) . . ? N2 C02 H02B 109.5(19) . . ? N2 C02 H02A 112(2) . . ? H02B C02 H02A 108(3) . . ? N2 C02 H02C 107(2) . . ? H02B C02 H02C 116(3) . . ? H02A C02 H02C 105(3) . . ? N1 C2 C3 108.3(3) . . ? N1 C2 H2A 108(2) . . ? C3 C2 H2A 110(2) . . ? N1 C2 H2B 110(2) . . ? C3 C2 H2B 109(2) . . ? H2A C2 H2B 111(3) . . ? N2 C3 C2 110.1(3) . . ? N2 C3 H3B 112.6(18) . . ? C2 C3 H3B 112.2(18) . . ? N2 C3 H3A 111(2) . . ? C2 C3 H3A 110(2) . . ? H3B C3 H3A 100(3) . . ? N2 C4 C22 114.6(3) . . ? N2 C4 H4B 103(2) . . ? C22 C4 H4B 113(2) . . ? N2 C4 H4A 107(2) . . ? C22 C4 H4A 111(2) . . ? H4B C4 H4A 109(3) . . ? O3 C5 C7 109.8(3) . . ? O3 C5 C8 108.7(3) . . ? C7 C5 C8 113.0(4) . . ? O3 C5 C6 106.5(3) . . ? C7 C5 C6 110.8(3) . . ? C8 C5 C6 107.8(3) . . ? O5 C6 O4 124.3(3) . . ? O5 C6 C5 122.1(4) . . ? O4 C6 C5 113.5(3) . . ? C5 C7 H7A 112(2) . . ? C5 C7 H7C 107(3) . . ? H7A C7 H7C 111(4) . . ? C5 C7 H7B 112(3) . . ? H7A C7 H7B 101(3) . . ? H7C C7 H7B 114(4) . . ? C5 C8 H8A 108(2) . . ? C5 C8 H8C 108(3) . . ? H8A C8 H8C 104(3) . . ? C5 C8 H8B 106(2) . . ? H8A C8 H8B 118(3) . . ? H8C C8 H8B 112(4) . . ? O1 C11 C16 119.2(3) . . ? O1 C11 C12 121.4(3) . . ? C16 C11 C12 119.4(3) . . ? C13 C12 C11 118.4(3) . . ? C13 C12 C1 118.2(3) . . ? C11 C12 C1 123.3(3) . . ? C14 C13 C12 122.4(3) . . ? C14 C13 H13 119(2) . . ? C12 C13 H13 118(2) . . ? C13 C14 C15 118.1(3) . . ? C13 C14 N3 119.8(3) . . ? C15 C14 N3 122.1(3) . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 116.9(19) . . ? C14 C15 H15 123.0(19) . . ? C15 C16 C11 121.6(3) . . ? C15 C16 H16 120(2) . . ? C11 C16 H16 118(2) . . ? O2 C21 C26 120.5(3) . . ? O2 C21 C22 119.7(3) . . ? C26 C21 C22 119.8(3) . . ? C21 C22 C23 119.4(3) . . ? C21 C22 C4 121.5(3) . . ? C23 C22 C4 119.0(3) . . ? C22 C23 C24 121.3(3) . . ? C22 C23 H23 115(2) . . ? C24 C23 H23 124(2) . . ? C25 C24 C23 117.9(3) . . ? C25 C24 N4 121.8(3) . . ? C23 C24 N4 120.3(3) . . ? C26 C25 C24 121.0(3) . . ? C26 C25 H25 121(2) . . ? C24 C25 H25 118(2) . . ? C21 C26 C25 120.6(4) . . ? C21 C26 H26 125(2) . . ? C25 C26 H26 114.1(19) . . ? C36 C31 C32 117.6(4) . . ? C36 C31 N3 122.3(3) . . ? C32 C31 N3 120.1(3) . . ? C33 C32 C31 121.7(4) . . ? C33 C32 H32 118(3) . . ? C31 C32 H32 121(3) . . ? C32 C33 C34 119.6(4) . . ? C32 C33 H33 118(2) . . ? C34 C33 H33 122(2) . . ? O31 C34 C33 115.4(3) . . ? O31 C34 C35 124.4(3) . . ? C33 C34 C35 120.2(4) . . ? C34 C35 C36 119.2(3) . . ? C34 C35 H35 127(2) . . ? C36 C35 H35 114(2) . . ? C31 C36 C35 121.5(3) . . ? C31 C36 H36 119(2) . . ? C35 C36 H36 119(2) . . ? O31 C37 H37A 109.5 . . ? O31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C42 C41 C46 119.0(4) . . ? C42 C41 N3 120.3(3) . . ? C46 C41 N3 120.6(4) . . ? C41 C42 C43 121.5(4) . . ? C41 C42 H42 121(2) . . ? C43 C42 H42 118(2) . . ? C44 C43 C42 119.3(4) . . ? C44 C43 H43 122(3) . . ? C42 C43 H43 119(3) . . ? O41 C44 C43 124.4(4) . . ? O41 C44 C45 116.1(4) . . ? C43 C44 C45 119.5(4) . . ? C44 C45 C46 121.2(4) . . ? C44 C45 H45 123(2) . . ? C46 C45 H45 116(2) . . ? C41 C46 C45 119.4(4) . . ? C41 C46 H46 123(2) . . ? C45 C46 H46 117(2) . . ? O41 C47 H47A 109.5 . . ? O41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C56 C51 C52 119.7(4) . . ? C56 C51 N4 120.1(4) . . ? C52 C51 N4 120.2(4) . . ? C51 C52 C53 119.5(4) . . ? C51 C52 H52 120(2) . . ? C53 C52 H52 121(2) . . ? C54 C53 C52 119.8(5) . . ? C54 C53 H53 123(3) . . ? C52 C53 H53 117(3) . . ? C55 C54 O51 124.7(5) . . ? C55 C54 C53 120.8(4) . . ? O51 C54 C53 114.5(5) . . ? C54 C55 C56 119.3(4) . . ? C54 C55 H55 122(2) . . ? C56 C55 H55 119(2) . . ? C51 C56 C55 120.9(4) . . ? C51 C56 H56 119(2) . . ? C55 C56 H56 120(2) . . ? O51 C57 H57A 109.5 . . ? O51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C62 C61 C66 118.6(3) . . ? C62 C61 N4 119.5(3) . . ? C66 C61 N4 121.9(3) . . ? C63 C62 C61 121.3(4) . . ? C63 C62 H62 116.6(18) . . ? C61 C62 H62 122.1(18) . . ? C62 C63 C64 120.0(3) . . ? C62 C63 H63 115(2) . . ? C64 C63 H63 125(2) . . ? O61 C64 C65 116.1(3) . . ? O61 C64 C63 124.5(3) . . ? C65 C64 C63 119.4(3) . . ? C64 C65 C66 120.8(4) . . ? C64 C65 H65 121.1(18) . . ? C66 C65 H65 118.1(18) . . ? C65 C66 C61 119.9(3) . . ? C65 C66 H66 123(2) . . ? C61 C66 H66 118(2) . . ? O61 C67 H67A 109.5 . . ? O61 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O61 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.458 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.056 _vrf_PLAT222_salan ; RESPONSE: The large variation in H atom thermal parameters is due to hydrogens being included in their observed positions and refined isotropically. This also leads to a number of alerts below. ; #==END data_twopiv _database_code_depnum_ccdc_archive 'CCDC 832125' #TrackingRef '- combined.cif' # Collected as sb006, 03/09/2010 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [N,N'-Dimethyl-N,N'-bis-(2-oxido-5-bromobenzyl)ethylenediamine](2,2- dimethyl-3-oxidopropanoato)titanium(IV) hemi-hydroxypivalic acid hemi- chloroform solvate ; _chemical_name_common '(Br{NMe}salan)Ti(OCH2C(CH3)2C(O)O) . 0.5 HOCH2C(CH3)2CO2H . 0.5 CHCl3' _chemical_melting_point ? _chemical_formula_moiety 'C23 H28 Br2 N2 O5 Ti, 0.5 (C5 H10 O3), 0.5 (C H Cl3)' _chemical_formula_sum 'C26 H33.50 Br2 Cl1.50 N2 O6.50 Ti' _chemical_formula_weight 738.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.9705(15) _cell_length_b 21.2780(16) _cell_length_c 14.1667(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.6784(12) _cell_angle_gamma 90.00 _cell_volume 5951.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9817 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.34 _exptl_crystal_description tablet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 3.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5713 _exptl_absorpt_correction_T_max 0.7646 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. Madison, WI USA. ; _exptl_crystal_recrystallization_method ; Crystals formed in the mother liquor from the preparative procedure after standing at -35 deg C. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 87013 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 26.45 _reflns_number_total 12258 _reflns_number_gt 9986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The hydroxypivalic acid of solvation was disordered in two orientations which had the CH2OH and COOH group interchanged, with the major orientation refining to 83.2(4)% occupancy. ; _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^)+(0.0384P)^2^+7.0190P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12258 _refine_ls_number_parameters 718 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _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 Ti1 Ti -0.33039(2) 0.63994(2) -0.66122(3) 0.02217(11) Uani 1 1 d . . . Br11 Br -0.594986(16) 0.840700(15) -0.47983(2) 0.03721(8) Uani 1 1 d . . . Br12 Br -0.351076(19) 0.532807(17) -1.17353(2) 0.04369(9) Uani 1 1 d . . . O11 O -0.40228(9) 0.64711(9) -0.59330(14) 0.0259(4) Uani 1 1 d . . . O12 O -0.37946(9) 0.60609(9) -0.77234(13) 0.0266(4) Uani 1 1 d . . . O13 O -0.28997(9) 0.56633(8) -0.62260(14) 0.0250(4) Uani 1 1 d . . . O14 O -0.26582(9) 0.68099(8) -0.55947(14) 0.0258(4) Uani 1 1 d . . . O15 O -0.17871(11) 0.69308(9) -0.44437(15) 0.0344(5) Uani 1 1 d . . . N11 N -0.36061(12) 0.73964(11) -0.70732(17) 0.0270(5) Uani 1 1 d . . . N12 N -0.25392(12) 0.66507(11) -0.75956(17) 0.0281(5) Uani 1 1 d . . . C11 C -0.37211(15) 0.77781(13) -0.6227(2) 0.0297(6) Uani 1 1 d . . . H11A H -0.3794 0.8222 -0.6424 0.036 Uiso 1 1 calc R . . H11B H -0.3310 0.7760 -0.5740 0.036 Uiso 1 1 calc R . . C12 C -0.30471(17) 0.76903(14) -0.7491(3) 0.0389(8) Uani 1 1 d . . . H12A H -0.2680 0.7817 -0.6977 0.047 Uiso 1 1 calc R . . H12B H -0.3214 0.8071 -0.7855 0.047 Uiso 1 1 calc R . . C13 C -0.27770(17) 0.72190(14) -0.8155(2) 0.0369(7) Uani 1 1 d . . . H13A H -0.3139 0.7104 -0.8683 0.044 Uiso 1 1 calc R . . H13B H -0.2398 0.7408 -0.8433 0.044 Uiso 1 1 calc R . . C14 C -0.24609(14) 0.61155(14) -0.8254(2) 0.0288(6) Uani 1 1 d . . . H14A H -0.2297 0.5745 -0.7863 0.035 Uiso 1 1 calc R . . H14B H -0.2106 0.6228 -0.8642 0.035 Uiso 1 1 calc R . . C15 C -0.23571(14) 0.54882(13) -0.5514(2) 0.0279(6) Uani 1 1 d . . . H15A H -0.1929 0.5511 -0.5785 0.034 Uiso 1 1 calc R . . H15B H -0.2422 0.5046 -0.5328 0.034 Uiso 1 1 calc R . . C16 C -0.22918(15) 0.59008(13) -0.4620(2) 0.0292(6) Uani 1 1 d . . . C17 C -0.22257(14) 0.65925(13) -0.4891(2) 0.0269(6) Uani 1 1 d . . . C18 C -0.29216(17) 0.58244(14) -0.4129(2) 0.0347(7) Uani 1 1 d . . . H18A H -0.2876 0.6089 -0.3557 0.052 Uiso 1 1 calc R . . H18B H -0.2966 0.5384 -0.3947 0.052 Uiso 1 1 calc R . . H18C H -0.3325 0.5952 -0.4569 0.052 Uiso 1 1 calc R . . C19 C -0.16585(18) 0.56892(15) -0.3947(3) 0.0430(8) Uani 1 1 d . . . H19A H -0.1605 0.5946 -0.3366 0.065 Uiso 1 1 calc R . . H19B H -0.1259 0.5740 -0.4266 0.065 Uiso 1 1 calc R . . H19C H -0.1706 0.5246 -0.3778 0.065 Uiso 1 1 calc R . . C101 C -0.42345(16) 0.74067(15) -0.7784(2) 0.0353(7) Uani 1 1 d . . . H10A H -0.4604 0.7208 -0.7509 0.053 Uiso 1 1 calc R . . H10B H -0.4158 0.7176 -0.8357 0.053 Uiso 1 1 calc R . . H10C H -0.4356 0.7843 -0.7954 0.053 Uiso 1 1 calc R . . C102 C -0.18445(15) 0.67738(16) -0.7076(2) 0.0384(8) Uani 1 1 d . . . H10D H -0.1682 0.6403 -0.6699 0.058 Uiso 1 1 calc R . . H10E H -0.1857 0.7135 -0.6649 0.058 Uiso 1 1 calc R . . H10F H -0.1538 0.6865 -0.7537 0.058 Uiso 1 1 calc R . . C111 C -0.44337(14) 0.69128(13) -0.56459(19) 0.0235(6) Uani 1 1 d . . . C112 C -0.43230(14) 0.75548(13) -0.5783(2) 0.0254(6) Uani 1 1 d . . . C113 C -0.47763(14) 0.79874(14) -0.5519(2) 0.0278(6) Uani 1 1 d . . . H113 H -0.4709 0.8423 -0.5619 0.033 Uiso 1 1 calc R . . C114 C -0.53262(14) 0.77903(14) -0.5111(2) 0.0273(6) Uani 1 1 d . . . C115 C -0.54347(15) 0.71647(14) -0.4958(2) 0.0297(6) Uani 1 1 d . . . H115 H -0.5813 0.7034 -0.4675 0.036 Uiso 1 1 calc R . . C116 C -0.49853(14) 0.67239(13) -0.52231(19) 0.0263(6) Uani 1 1 d . . . H116 H -0.5055 0.6290 -0.5115 0.032 Uiso 1 1 calc R . . C121 C -0.37152(14) 0.58736(13) -0.8604(2) 0.0253(6) Uani 1 1 d . . . C122 C -0.30878(14) 0.59287(13) -0.8920(2) 0.0264(6) Uani 1 1 d . . . C123 C -0.30361(15) 0.57642(13) -0.9859(2) 0.0294(6) Uani 1 1 d . . . H123 H -0.2618 0.5816 -1.0093 0.035 Uiso 1 1 calc R . . C124 C -0.35917(16) 0.55253(14) -1.0449(2) 0.0308(6) Uani 1 1 d . . . C125 C -0.42034(16) 0.54490(14) -1.0132(2) 0.0330(7) Uani 1 1 d . . . H125 H -0.4577 0.5271 -1.0539 0.040 Uiso 1 1 calc R . . C126 C -0.42701(15) 0.56336(14) -0.9213(2) 0.0306(6) Uani 1 1 d . . . H126 H -0.4696 0.5597 -0.8997 0.037 Uiso 1 1 calc R . . Ti2 Ti 0.13265(2) 0.62157(2) -0.50035(3) 0.02100(11) Uani 1 1 d . . . Br21 Br 0.395178(15) 0.768350(17) -0.76000(2) 0.03829(9) Uani 1 1 d . . . Br22 Br 0.221875(18) 0.578096(15) 0.03471(2) 0.03839(9) Uani 1 1 d . . . O21 O 0.19700(9) 0.61286(9) -0.58138(13) 0.0251(4) Uani 1 1 d . . . O22 O 0.18707(9) 0.59059(9) -0.39306(13) 0.0246(4) Uani 1 1 d . . . O23 O 0.07932(9) 0.55322(9) -0.52864(13) 0.0251(4) Uani 1 1 d . . . O24 O 0.06684(9) 0.66738(9) -0.59449(13) 0.0252(4) Uani 1 1 d . . . O25 O -0.02718(13) 0.68713(10) -0.6922(2) 0.0548(7) Uani 1 1 d . . . N21 N 0.17655(11) 0.71936(10) -0.47706(16) 0.0226(5) Uani 1 1 d . . . N22 N 0.07206(11) 0.66244(11) -0.38901(16) 0.0246(5) Uani 1 1 d . . . C21 C 0.18672(14) 0.74851(13) -0.5695(2) 0.0268(6) Uani 1 1 d . . . H21A H 0.2016 0.7926 -0.5579 0.032 Uiso 1 1 calc R . . H21B H 0.1429 0.7492 -0.6128 0.032 Uiso 1 1 calc R . . C22 C 0.12695(15) 0.75889(13) -0.4344(2) 0.0294(6) Uani 1 1 d . . . H22A H 0.0880 0.7693 -0.4838 0.035 Uiso 1 1 calc R . . H22B H 0.1488 0.7987 -0.4102 0.035 Uiso 1 1 calc R . . C23 C 0.10232(15) 0.72370(13) -0.3531(2) 0.0284(6) Uani 1 1 d . . . H23A H 0.1407 0.7161 -0.3014 0.034 Uiso 1 1 calc R . . H23B H 0.0680 0.7492 -0.3268 0.034 Uiso 1 1 calc R . . C24 C 0.07167(14) 0.61773(14) -0.3072(2) 0.0281(6) Uani 1 1 d . . . H24A H 0.0501 0.5781 -0.3324 0.034 Uiso 1 1 calc R . . H24B H 0.0429 0.6358 -0.2629 0.034 Uiso 1 1 calc R . . C25 C 0.02266(15) 0.53916(13) -0.5973(2) 0.0285(6) Uani 1 1 d . . . H25A H -0.0186 0.5426 -0.5666 0.034 Uiso 1 1 calc R . . H25B H 0.0263 0.4949 -0.6176 0.034 Uiso 1 1 calc R . . C26 C 0.01335(15) 0.58096(13) -0.6871(2) 0.0284(6) Uani 1 1 d . . . C27 C 0.01581(14) 0.64993(14) -0.6569(2) 0.0279(6) Uani 1 1 d . . . C28 C -0.05472(16) 0.56366(15) -0.7459(2) 0.0349(7) Uani 1 1 d . . . H28A H -0.0543 0.5192 -0.7641 0.052 Uiso 1 1 calc R . . H28B H -0.0624 0.5897 -0.8036 0.052 Uiso 1 1 calc R . . H28C H -0.0911 0.5709 -0.7078 0.052 Uiso 1 1 calc R . . C29 C 0.07011(16) 0.56983(15) -0.7475(2) 0.0355(7) Uani 1 1 d . . . H29A H 0.0696 0.5258 -0.7677 0.053 Uiso 1 1 calc R . . H29B H 0.1140 0.5796 -0.7094 0.053 Uiso 1 1 calc R . . H29C H 0.0629 0.5971 -0.8039 0.053 Uiso 1 1 calc R . . C201 C 0.24276(14) 0.71914(14) -0.4136(2) 0.0295(6) Uani 1 1 d . . . H20A H 0.2749 0.6930 -0.4420 0.044 Uiso 1 1 calc R . . H20B H 0.2370 0.7021 -0.3511 0.044 Uiso 1 1 calc R . . H20C H 0.2601 0.7622 -0.4059 0.044 Uiso 1 1 calc R . . C202 C -0.00044(14) 0.67283(15) -0.4293(2) 0.0325(7) Uani 1 1 d . . . H20D H -0.0208 0.6330 -0.4534 0.049 Uiso 1 1 calc R . . H20E H -0.0035 0.7033 -0.4816 0.049 Uiso 1 1 calc R . . H20F H -0.0247 0.6891 -0.3792 0.049 Uiso 1 1 calc R . . C211 C 0.23993(13) 0.64821(13) -0.62339(19) 0.0240(6) Uani 1 1 d . . . C212 C 0.23828(14) 0.71434(14) -0.6181(2) 0.0269(6) Uani 1 1 d . . . C213 C 0.28545(14) 0.74886(14) -0.6592(2) 0.0281(6) Uani 1 1 d . . . H213 H 0.2857 0.7934 -0.6547 0.034 Uiso 1 1 calc R . . C214 C 0.33215(14) 0.71856(15) -0.7066(2) 0.0300(6) Uani 1 1 d . . . C215 C 0.33276(15) 0.65418(15) -0.7148(2) 0.0344(7) Uani 1 1 d . . . H215 H 0.3643 0.6340 -0.7486 0.041 Uiso 1 1 calc R . . C216 C 0.28639(15) 0.61915(14) -0.6728(2) 0.0313(6) Uani 1 1 d . . . H216 H 0.2865 0.5746 -0.6780 0.038 Uiso 1 1 calc R . . C221 C 0.19428(14) 0.58667(12) -0.29729(19) 0.0238(6) Uani 1 1 d . . . C222 C 0.13978(14) 0.60221(13) -0.2508(2) 0.0255(6) Uani 1 1 d . . . C223 C 0.14810(15) 0.59895(13) -0.1513(2) 0.0273(6) Uani 1 1 d . . . H223 H 0.1116 0.6092 -0.1182 0.033 Uiso 1 1 calc R . . C224 C 0.21008(16) 0.58056(13) -0.1013(2) 0.0298(6) Uani 1 1 d . . . C225 C 0.26418(15) 0.56540(13) -0.1470(2) 0.0286(6) Uani 1 1 d . . . H225 H 0.3062 0.5529 -0.1113 0.034 Uiso 1 1 calc R . . C226 C 0.25637(15) 0.56861(13) -0.2455(2) 0.0273(6) Uani 1 1 d . . . H226 H 0.2933 0.5585 -0.2780 0.033 Uiso 1 1 calc R . . O1 O -0.0696(2) 0.81873(16) -0.4251(2) 0.0663(11) Uani 0.832(4) 1 d P A 1 O3 O -0.00316(14) 0.80801(13) -0.6376(2) 0.0328(7) Uani 0.832(4) 1 d P A 1 C1 C -0.10268(19) 0.82948(16) -0.5020(3) 0.0444(8) Uani 0.832(4) 1 d P A 1 C3 C -0.06449(16) 0.84209(16) -0.6595(2) 0.0384(7) Uani 0.832(4) 1 d P A 1 H3A H -0.1015 0.8126 -0.6838 0.046 Uiso 0.832(4) 1 calc PR A 1 H3B H -0.0600 0.8727 -0.7108 0.046 Uiso 0.832(4) 1 calc PR A 1 O1B O -0.1021(10) 0.8202(8) -0.7234(11) 0.0663(11) Uani 0.168(4) 1 d P A 2 O3B O -0.0234(7) 0.7910(7) -0.6056(12) 0.0328(7) Uani 0.168(4) 1 d P A 2 C3B C -0.10268(19) 0.82948(16) -0.5020(3) 0.0444(8) Uani 0.168(4) 1 d P A 2 H3B1 H -0.0644 0.8002 -0.4837 0.053 Uiso 0.168(4) 1 calc PR A 2 H3B2 H -0.1114 0.8516 -0.4436 0.053 Uiso 0.168(4) 1 calc PR A 2 C1B C -0.06449(16) 0.84209(16) -0.6595(2) 0.0384(7) Uani 0.168(4) 1 d P A 2 O2 O -0.15708(14) 0.79705(13) -0.53772(19) 0.0543(7) Uani 1 1 d . . . C2 C -0.08340(16) 0.87717(14) -0.5732(2) 0.0336(7) Uani 1 1 d . . . C4 C -0.14345(19) 0.91979(17) -0.6077(3) 0.0545(11) Uani 1 1 d . A . H4A H -0.1304 0.9504 -0.6533 0.082 Uiso 1 1 calc R . . H4B H -0.1572 0.9420 -0.5531 0.082 Uiso 1 1 calc R . . H4C H -0.1813 0.8944 -0.6390 0.082 Uiso 1 1 calc R . . C5 C -0.0224(2) 0.91542(17) -0.5271(3) 0.0486(9) Uani 1 1 d . A . H5A H -0.0102 0.9461 -0.5732 0.073 Uiso 1 1 calc R . . H5B H 0.0159 0.8872 -0.5075 0.073 Uiso 1 1 calc R . . H5C H -0.0339 0.9375 -0.4710 0.073 Uiso 1 1 calc R . . H2 H -0.169(2) 0.766(2) -0.497(3) 0.073(14) Uiso 1 1 d . . . H3 H -0.014(2) 0.767(2) -0.651(3) 0.063(13) Uiso 1 1 d . . . C0 C 0.43466(19) 0.97949(16) -0.8424(3) 0.0456(8) Uani 1 1 d . . . H0 H 0.4101 1.0180 -0.8259 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.38454(4) 0.94140(5) -0.93831(6) 0.0481(2) Uani 1 1 d . . . Cl2 Cl 0.44727(5) 0.93024(5) -0.74185(7) 0.0534(2) Uani 1 1 d . . . Cl3 Cl 0.51231(6) 1.00260(6) -0.87358(9) 0.0801(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0238(2) 0.0184(2) 0.0264(3) -0.00011(19) 0.01049(19) -0.00108(18) Br11 0.03445(17) 0.03596(17) 0.04303(18) -0.00552(14) 0.01171(13) 0.01096(13) Br12 0.0561(2) 0.0481(2) 0.02575(16) -0.00538(14) 0.00248(14) 0.01146(16) O11 0.0288(10) 0.0201(9) 0.0315(11) 0.0034(8) 0.0136(8) 0.0026(8) O12 0.0261(10) 0.0278(10) 0.0279(10) -0.0010(8) 0.0103(8) -0.0033(8) O13 0.0275(10) 0.0191(10) 0.0295(10) -0.0030(8) 0.0078(8) 0.0004(8) O14 0.0290(10) 0.0177(9) 0.0322(11) -0.0022(8) 0.0097(8) -0.0009(8) O15 0.0361(12) 0.0274(11) 0.0392(12) -0.0073(9) 0.0042(9) -0.0065(9) N11 0.0308(13) 0.0220(12) 0.0310(13) 0.0027(10) 0.0139(10) -0.0011(10) N12 0.0276(12) 0.0267(13) 0.0326(13) -0.0060(10) 0.0134(10) -0.0048(10) C11 0.0355(16) 0.0195(14) 0.0369(17) 0.0014(12) 0.0142(13) 0.0000(12) C12 0.0467(19) 0.0246(16) 0.052(2) 0.0059(14) 0.0275(16) -0.0051(14) C13 0.0456(18) 0.0300(16) 0.0408(18) 0.0032(14) 0.0251(15) -0.0056(14) C14 0.0254(14) 0.0326(16) 0.0309(15) -0.0043(13) 0.0121(12) -0.0005(12) C15 0.0267(14) 0.0201(14) 0.0372(16) -0.0054(12) 0.0055(12) 0.0031(11) C16 0.0336(16) 0.0216(14) 0.0319(16) -0.0040(12) 0.0035(12) -0.0011(12) C17 0.0293(15) 0.0238(14) 0.0299(15) -0.0056(12) 0.0120(12) -0.0006(12) C18 0.0496(19) 0.0251(15) 0.0321(16) 0.0002(13) 0.0149(14) -0.0005(13) C19 0.049(2) 0.0301(17) 0.0442(19) -0.0013(15) -0.0106(16) 0.0016(15) C101 0.0434(18) 0.0318(17) 0.0321(17) 0.0068(13) 0.0102(14) 0.0056(14) C102 0.0298(16) 0.0459(19) 0.0426(19) -0.0141(15) 0.0157(14) -0.0112(14) C111 0.0260(14) 0.0228(14) 0.0229(13) 0.0004(11) 0.0078(11) 0.0036(11) C112 0.0278(14) 0.0249(14) 0.0246(14) 0.0018(11) 0.0073(11) 0.0025(11) C113 0.0307(15) 0.0250(15) 0.0271(15) 0.0008(12) 0.0029(12) 0.0035(12) C114 0.0277(14) 0.0318(16) 0.0229(14) -0.0036(12) 0.0053(11) 0.0079(12) C115 0.0287(15) 0.0358(17) 0.0273(15) -0.0017(13) 0.0126(12) 0.0004(12) C116 0.0311(15) 0.0243(14) 0.0258(14) 0.0008(11) 0.0112(12) 0.0005(11) C121 0.0294(14) 0.0208(14) 0.0267(14) 0.0031(11) 0.0067(11) 0.0020(11) C122 0.0285(15) 0.0221(14) 0.0295(15) 0.0007(12) 0.0075(12) 0.0024(11) C123 0.0345(16) 0.0271(15) 0.0278(15) 0.0033(12) 0.0091(12) 0.0053(12) C124 0.0423(17) 0.0267(15) 0.0232(14) 0.0007(12) 0.0043(13) 0.0064(13) C125 0.0367(17) 0.0283(16) 0.0321(16) 0.0008(13) -0.0012(13) -0.0009(13) C126 0.0288(15) 0.0285(15) 0.0350(16) 0.0048(13) 0.0063(12) -0.0005(12) Ti2 0.0238(2) 0.0191(2) 0.0205(2) -0.00200(19) 0.00460(19) -0.00319(18) Br21 0.02840(16) 0.0545(2) 0.03322(17) 0.00633(15) 0.00870(12) -0.01002(14) Br22 0.0621(2) 0.02949(16) 0.02307(15) 0.00327(12) 0.00467(14) 0.00557(14) O21 0.0287(10) 0.0219(10) 0.0262(10) -0.0012(8) 0.0088(8) -0.0016(8) O22 0.0277(10) 0.0244(10) 0.0216(10) -0.0029(8) 0.0038(8) -0.0006(8) O23 0.0295(10) 0.0219(10) 0.0235(10) -0.0007(8) 0.0028(8) -0.0058(8) O24 0.0261(10) 0.0218(10) 0.0268(10) -0.0025(8) 0.0015(8) -0.0034(8) O25 0.0525(15) 0.0256(12) 0.0745(18) -0.0007(12) -0.0290(13) -0.0003(11) N21 0.0236(11) 0.0212(11) 0.0232(12) -0.0026(9) 0.0046(9) -0.0011(9) N22 0.0253(12) 0.0251(12) 0.0242(12) -0.0033(10) 0.0056(9) -0.0037(9) C21 0.0309(15) 0.0229(14) 0.0266(14) 0.0015(11) 0.0039(12) -0.0037(11) C22 0.0331(16) 0.0228(14) 0.0340(16) -0.0054(12) 0.0104(13) -0.0007(12) C23 0.0337(15) 0.0257(15) 0.0282(15) -0.0051(12) 0.0123(12) -0.0015(12) C24 0.0288(15) 0.0294(15) 0.0271(15) -0.0005(12) 0.0074(12) -0.0063(12) C25 0.0315(15) 0.0222(14) 0.0298(15) -0.0018(12) -0.0019(12) -0.0076(12) C26 0.0311(15) 0.0245(14) 0.0278(15) 0.0000(12) -0.0012(12) -0.0030(12) C27 0.0268(15) 0.0275(15) 0.0280(15) 0.0010(12) 0.0000(12) -0.0035(12) C28 0.0379(17) 0.0308(16) 0.0324(16) -0.0010(13) -0.0057(13) -0.0045(13) C29 0.0407(18) 0.0384(18) 0.0270(16) -0.0077(13) 0.0036(13) -0.0028(14) C201 0.0290(15) 0.0301(16) 0.0283(15) -0.0034(12) 0.0006(12) -0.0074(12) C202 0.0250(15) 0.0404(18) 0.0331(16) -0.0006(14) 0.0070(12) 0.0017(13) C211 0.0225(13) 0.0288(15) 0.0205(13) 0.0003(11) 0.0029(10) -0.0024(11) C212 0.0277(14) 0.0288(15) 0.0236(14) -0.0004(12) 0.0022(11) -0.0033(12) C213 0.0307(15) 0.0266(15) 0.0261(15) 0.0021(12) 0.0016(12) -0.0052(12) C214 0.0246(14) 0.0405(17) 0.0253(15) 0.0057(13) 0.0053(11) -0.0045(12) C215 0.0335(16) 0.0421(18) 0.0304(16) -0.0004(14) 0.0131(13) 0.0068(13) C216 0.0360(16) 0.0271(15) 0.0320(16) 0.0007(13) 0.0092(13) 0.0037(12) C221 0.0312(15) 0.0164(13) 0.0241(14) -0.0032(11) 0.0053(11) -0.0039(11) C222 0.0312(15) 0.0190(13) 0.0261(14) -0.0019(11) 0.0040(11) -0.0065(11) C223 0.0363(16) 0.0204(14) 0.0270(15) -0.0019(11) 0.0107(12) -0.0074(12) C224 0.0501(18) 0.0158(13) 0.0224(14) 0.0018(11) 0.0022(13) -0.0033(12) C225 0.0373(16) 0.0197(14) 0.0276(15) 0.0005(11) 0.0007(12) 0.0004(12) C226 0.0315(15) 0.0211(14) 0.0290(15) -0.0014(12) 0.0041(12) -0.0001(11) O1 0.109(3) 0.053(2) 0.0328(17) 0.0035(14) -0.0007(17) -0.0415(19) O3 0.0269(15) 0.0256(15) 0.0468(18) -0.0004(12) 0.0080(12) 0.0020(11) C1 0.059(2) 0.0382(19) 0.0367(19) -0.0064(15) 0.0105(17) -0.0164(16) C3 0.0321(16) 0.047(2) 0.0361(17) -0.0039(15) 0.0061(13) 0.0106(14) O1B 0.109(3) 0.053(2) 0.0328(17) 0.0035(14) -0.0007(17) -0.0415(19) O3B 0.0269(15) 0.0256(15) 0.0468(18) -0.0004(12) 0.0080(12) 0.0020(11) C3B 0.059(2) 0.0382(19) 0.0367(19) -0.0064(15) 0.0105(17) -0.0164(16) C1B 0.0321(16) 0.047(2) 0.0361(17) -0.0039(15) 0.0061(13) 0.0106(14) O2 0.0624(17) 0.0469(15) 0.0521(16) 0.0114(13) 0.0033(13) -0.0255(13) C2 0.0418(17) 0.0264(15) 0.0359(17) -0.0024(13) 0.0162(14) -0.0041(13) C4 0.052(2) 0.0342(19) 0.087(3) 0.0149(19) 0.042(2) 0.0119(16) C5 0.064(2) 0.0369(19) 0.050(2) -0.0119(16) 0.0266(18) -0.0245(17) C0 0.054(2) 0.0354(19) 0.046(2) -0.0016(16) 0.0027(16) 0.0105(16) Cl1 0.0401(5) 0.0600(6) 0.0432(5) -0.0097(4) 0.0034(4) 0.0158(4) Cl2 0.0561(5) 0.0572(6) 0.0451(5) 0.0077(4) 0.0022(4) -0.0071(4) Cl3 0.0695(7) 0.0938(9) 0.0717(7) 0.0358(7) -0.0065(6) -0.0287(6) _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 Ti1 O13 1.8086(19) . ? Ti1 O11 1.8513(19) . ? Ti1 O12 1.869(2) . ? Ti1 O14 1.986(2) . ? Ti1 N11 2.274(2) . ? Ti1 N12 2.281(2) . ? Br11 C114 1.907(3) . ? Br12 C124 1.901(3) . ? O11 C111 1.350(3) . ? O12 C121 1.341(3) . ? O13 C15 1.415(3) . ? O14 C17 1.302(3) . ? O15 C17 1.233(3) . ? N11 C12 1.479(4) . ? N11 C101 1.486(4) . ? N11 C11 1.495(4) . ? N12 C13 1.484(4) . ? N12 C102 1.492(4) . ? N12 C14 1.495(4) . ? C11 C112 1.514(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.527(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C122 1.503(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.530(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.532(4) . ? C16 C19 1.532(4) . ? C16 C18 1.535(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C111 C116 1.390(4) . ? C111 C112 1.402(4) . ? C112 C113 1.382(4) . ? C113 C114 1.381(4) . ? C113 H113 0.9500 . ? C114 C115 1.371(4) . ? C115 C116 1.388(4) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.395(4) . ? C121 C122 1.398(4) . ? C122 C123 1.393(4) . ? C123 C124 1.382(4) . ? C123 H123 0.9500 . ? C124 C125 1.373(4) . ? C125 C126 1.385(4) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? Ti2 O23 1.8114(18) . ? Ti2 O22 1.8513(19) . ? Ti2 O21 1.8571(19) . ? Ti2 O24 1.9817(19) . ? Ti2 N21 2.263(2) . ? Ti2 N22 2.299(2) . ? Br21 C214 1.889(3) . ? Br22 C224 1.906(3) . ? O21 C211 1.345(3) . ? O22 C221 1.345(3) . ? O23 C25 1.409(3) . ? O24 C27 1.298(3) . ? O25 C27 1.219(4) . ? N21 C201 1.482(3) . ? N21 C21 1.491(3) . ? N21 C22 1.495(3) . ? N22 C202 1.490(4) . ? N22 C23 1.493(4) . ? N22 C24 1.501(4) . ? C21 C212 1.509(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.516(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C222 1.506(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.540(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.527(4) . ? C26 C28 1.529(4) . ? C26 C29 1.538(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 H20D 0.9800 . ? C202 H20E 0.9800 . ? C202 H20F 0.9800 . ? C211 C216 1.389(4) . ? C211 C212 1.410(4) . ? C212 C213 1.389(4) . ? C213 C214 1.388(4) . ? C213 H213 0.9500 . ? C214 C215 1.375(4) . ? C215 C216 1.390(4) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.394(4) . ? C221 C226 1.396(4) . ? C222 C223 1.396(4) . ? C223 C224 1.387(4) . ? C223 H223 0.9500 . ? C224 C225 1.379(4) . ? C225 C226 1.383(4) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? O1 C1 1.207(5) . ? O3 C3 1.417(4) . ? O3 H3 0.91(4) . ? C1 O2 1.321(4) . ? C1 C2 1.521(5) . ? C3 C2 1.527(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O3B H3 0.87(4) . ? O2 H2 0.93(5) . ? C2 C4 1.524(5) . ? C2 C5 1.527(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C0 Cl3 1.746(4) . ? C0 Cl2 1.755(4) . ? C0 Cl1 1.760(4) . ? C0 H0 1.0000 . ? 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 O13 Ti1 O11 105.06(8) . . ? O13 Ti1 O12 94.27(9) . . ? O11 Ti1 O12 96.92(9) . . ? O13 Ti1 O14 87.14(8) . . ? O11 Ti1 O14 93.21(8) . . ? O12 Ti1 O14 169.03(8) . . ? O13 Ti1 N11 169.02(9) . . ? O11 Ti1 N11 83.07(8) . . ? O12 Ti1 N11 92.00(9) . . ? O14 Ti1 N11 85.02(8) . . ? O13 Ti1 N12 94.50(9) . . ? O11 Ti1 N12 160.30(9) . . ? O12 Ti1 N12 83.69(8) . . ? O14 Ti1 N12 85.35(8) . . ? N11 Ti1 N12 77.23(8) . . ? C111 O11 Ti1 140.20(17) . . ? C121 O12 Ti1 141.01(17) . . ? C15 O13 Ti1 134.65(17) . . ? C17 O14 Ti1 133.07(17) . . ? C12 N11 C101 109.5(2) . . ? C12 N11 C11 108.0(2) . . ? C101 N11 C11 108.6(2) . . ? C12 N11 Ti1 109.02(18) . . ? C101 N11 Ti1 111.63(17) . . ? C11 N11 Ti1 110.05(17) . . ? C13 N12 C102 108.6(2) . . ? C13 N12 C14 110.1(2) . . ? C102 N12 C14 105.4(2) . . ? C13 N12 Ti1 109.09(17) . . ? C102 N12 Ti1 113.46(18) . . ? C14 N12 Ti1 110.20(16) . . ? N11 C11 C112 113.0(2) . . ? N11 C11 H11A 109.0 . . ? C112 C11 H11A 109.0 . . ? N11 C11 H11B 109.0 . . ? C112 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N11 C12 C13 109.1(2) . . ? N11 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? N11 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N12 C13 C12 108.7(3) . . ? N12 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? N12 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N12 C14 C122 116.0(2) . . ? N12 C14 H14A 108.3 . . ? C122 C14 H14A 108.3 . . ? N12 C14 H14B 108.3 . . ? C122 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? O13 C15 C16 113.5(2) . . ? O13 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? O13 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C15 C16 C17 110.1(2) . . ? C15 C16 C19 107.8(2) . . ? C17 C16 C19 110.1(2) . . ? C15 C16 C18 109.9(2) . . ? C17 C16 C18 108.8(2) . . ? C19 C16 C18 110.0(3) . . ? O15 C17 O14 121.6(3) . . ? O15 C17 C16 120.9(3) . . ? O14 C17 C16 117.5(2) . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N11 C101 H10A 109.5 . . ? N11 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? N11 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? N12 C102 H10D 109.5 . . ? N12 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? N12 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? O11 C111 C116 119.1(2) . . ? O11 C111 C112 121.4(2) . . ? C116 C111 C112 119.6(2) . . ? C113 C112 C111 119.2(3) . . ? C113 C112 C11 119.8(3) . . ? C111 C112 C11 121.0(2) . . ? C112 C113 C114 120.4(3) . . ? C112 C113 H113 119.8 . . ? C114 C113 H113 119.8 . . ? C115 C114 C113 121.0(3) . . ? C115 C114 Br11 120.5(2) . . ? C113 C114 Br11 118.5(2) . . ? C114 C115 C116 119.3(3) . . ? C114 C115 H115 120.4 . . ? C116 C115 H115 120.4 . . ? C115 C116 C111 120.5(3) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? O12 C121 C126 119.3(2) . . ? O12 C121 C122 120.7(2) . . ? C126 C121 C122 119.9(3) . . ? C123 C122 C121 119.0(3) . . ? C123 C122 C14 119.4(2) . . ? C121 C122 C14 121.5(2) . . ? C124 C123 C122 120.1(3) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C125 C124 C123 121.2(3) . . ? C125 C124 Br12 119.7(2) . . ? C123 C124 Br12 119.0(2) . . ? C124 C125 C126 119.3(3) . . ? C124 C125 H125 120.3 . . ? C126 C125 H125 120.3 . . ? C125 C126 C121 120.4(3) . . ? C125 C126 H126 119.8 . . ? C121 C126 H126 119.8 . . ? O23 Ti2 O22 98.54(9) . . ? O23 Ti2 O21 102.81(8) . . ? O22 Ti2 O21 95.55(8) . . ? O23 Ti2 O24 86.44(8) . . ? O22 Ti2 O24 167.22(8) . . ? O21 Ti2 O24 94.79(8) . . ? O23 Ti2 N21 166.54(9) . . ? O22 Ti2 N21 92.36(8) . . ? O21 Ti2 N21 83.85(8) . . ? O24 Ti2 N21 81.30(8) . . ? O23 Ti2 N22 95.90(8) . . ? O22 Ti2 N22 82.87(8) . . ? O21 Ti2 N22 161.24(8) . . ? O24 Ti2 N22 84.92(8) . . ? N21 Ti2 N22 77.56(8) . . ? C211 O21 Ti2 139.87(17) . . ? C221 O22 Ti2 144.14(18) . . ? C25 O23 Ti2 135.03(17) . . ? C27 O24 Ti2 133.63(18) . . ? C201 N21 C21 107.9(2) . . ? C201 N21 C22 110.0(2) . . ? C21 N21 C22 107.9(2) . . ? C201 N21 Ti2 112.09(17) . . ? C21 N21 Ti2 110.83(16) . . ? C22 N21 Ti2 108.09(16) . . ? C202 N22 C23 108.7(2) . . ? C202 N22 C24 105.8(2) . . ? C23 N22 C24 109.8(2) . . ? C202 N22 Ti2 112.03(17) . . ? C23 N22 Ti2 109.63(16) . . ? C24 N22 Ti2 110.79(17) . . ? N21 C21 C212 113.2(2) . . ? N21 C21 H21A 108.9 . . ? C212 C21 H21A 108.9 . . ? N21 C21 H21B 108.9 . . ? C212 C21 H21B 108.9 . . ? H21A C21 H21B 107.8 . . ? N21 C22 C23 109.9(2) . . ? N21 C22 H22A 109.7 . . ? C23 C22 H22A 109.7 . . ? N21 C22 H22B 109.7 . . ? C23 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? N22 C23 C22 109.5(2) . . ? N22 C23 H23A 109.8 . . ? C22 C23 H23A 109.8 . . ? N22 C23 H23B 109.8 . . ? C22 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? N22 C24 C222 116.0(2) . . ? N22 C24 H24A 108.3 . . ? C222 C24 H24A 108.3 . . ? N22 C24 H24B 108.3 . . ? C222 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? O23 C25 C26 115.6(2) . . ? O23 C25 H25A 108.4 . . ? C26 C25 H25A 108.4 . . ? O23 C25 H25B 108.4 . . ? C26 C25 H25B 108.4 . . ? H25A C25 H25B 107.4 . . ? C27 C26 C28 111.9(2) . . ? C27 C26 C29 108.0(2) . . ? C28 C26 C29 109.2(2) . . ? C27 C26 C25 109.2(2) . . ? C28 C26 C25 107.3(2) . . ? C29 C26 C25 111.3(2) . . ? O25 C27 O24 121.7(3) . . ? O25 C27 C26 121.2(3) . . ? O24 C27 C26 117.0(2) . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N21 C201 H20A 109.5 . . ? N21 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? N21 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? N22 C202 H20D 109.5 . . ? N22 C202 H20E 109.5 . . ? H20D C202 H20E 109.5 . . ? N22 C202 H20F 109.5 . . ? H20D C202 H20F 109.5 . . ? H20E C202 H20F 109.5 . . ? O21 C211 C216 119.5(3) . . ? O21 C211 C212 120.9(2) . . ? C216 C211 C212 119.6(3) . . ? C213 C212 C211 118.9(3) . . ? C213 C212 C21 119.2(3) . . ? C211 C212 C21 121.9(2) . . ? C214 C213 C212 120.3(3) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 119.9 . . ? C215 C214 C213 121.3(3) . . ? C215 C214 Br21 120.7(2) . . ? C213 C214 Br21 118.1(2) . . ? C214 C215 C216 118.9(3) . . ? C214 C215 H215 120.6 . . ? C216 C215 H215 120.6 . . ? C215 C216 C211 121.0(3) . . ? C215 C216 H216 119.5 . . ? C211 C216 H216 119.5 . . ? O22 C221 C222 119.3(2) . . ? O22 C221 C226 119.9(2) . . ? C222 C221 C226 120.8(3) . . ? C223 C222 C221 118.9(3) . . ? C223 C222 C24 120.4(3) . . ? C221 C222 C24 120.6(2) . . ? C224 C223 C222 119.4(3) . . ? C224 C223 H223 120.3 . . ? C222 C223 H223 120.3 . . ? C225 C224 C223 121.8(3) . . ? C225 C224 Br22 118.8(2) . . ? C223 C224 Br22 119.3(2) . . ? C224 C225 C226 119.1(3) . . ? C224 C225 H225 120.5 . . ? C226 C225 H225 120.5 . . ? C225 C226 C221 120.0(3) . . ? C225 C226 H226 120.0 . . ? C221 C226 H226 120.0 . . ? C3 O3 H3 106(3) . . ? O1 C1 O2 123.5(3) . . ? O1 C1 C2 124.5(3) . . ? O2 C1 C2 111.7(3) . . ? O3 C3 C2 112.7(3) . . ? O3 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? O3 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C1 O2 H2 114(3) . . ? C1 C2 C4 110.1(3) . . ? C1 C2 C5 109.7(3) . . ? C4 C2 C5 111.0(3) . . ? C1 C2 C3 108.8(3) . . ? C4 C2 C3 108.1(3) . . ? C5 C2 C3 109.0(3) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Cl3 C0 Cl2 110.4(2) . . ? Cl3 C0 Cl1 110.9(2) . . ? Cl2 C0 Cl1 110.3(2) . . ? Cl3 C0 H0 108.4 . . ? Cl2 C0 H0 108.4 . . ? Cl1 C0 H0 108.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.290 _refine_diff_density_min -1.006 _refine_diff_density_rms 0.072 _vrf_PLAT303_twopiv ; RESPONSE: H3 is one of the hydroxylic protons of the disordered lattice hydroxypivalic acid; both components of the disordered molecule have been modeled as sharing this hydrogen. ; #==END