# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Seth Brown' 'Gregory A. Ellis' 'Vesela Ugrinova' _publ_contact_author_name 'Prof Seth Brown' _publ_contact_author_address ; Chemistry and Biochemistry University of Notre Dame 251 Nieuwland Science Hall Notre Dame Indiana 46556-5670 UNITED STATES OF AMERICA ; _publ_contact_author_email SETH.N.BROWN.114@ND.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Remarkable thermodynamic stability toward hydrolysis of tripodal titanium alkoxides ; data_tioh _database_code_depnum_ccdc_archive 'CCDC 225000' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ; (Hydroxy)(nitrilotris(4,6-di-tert -butyl-o- phenolate))titanium(IV).1.33 tetrahydrofuran . 0.5 benzene ; _chemical_formula_moiety 'Ti(OH)(N(CH2[C6H2(tBu)2O])3 . 1.33 C4H8O . 0.5 C6H6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C53.33 H80.67 N O5.33 Ti' _chemical_formula_weight 869.09 _chemical_melting_point ? _chemical_compound_source ? 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 Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 27.7755(7) _cell_length_b 27.7755(7) _cell_length_c 35.2084(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 23523.4(12) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8095 _cell_measurement_theta_min 2.271 _cell_measurement_theta_max 27.975 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.104 _exptl_crystal_density_method ? _exptl_crystal_F_000 8502 _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type 'empirical using SADABS' _exptl_absorpt_correction_T_min 0.914049 _exptl_absorpt_correction_T_max 1.00000 _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 'Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 84944 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.32 _reflns_number_total 13022 _reflns_number_observed 9863 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The molecule is disordered over two unequally populated orientations which differ in the helical twist of the aminetris(phenoxide) ligand. This disorder affects only the core of the molecule, with the outer parts of the benzene rings and the tert-butyl groups superimposable in the two orientations. The major orientation (C10-C13, C20-C23, C30-C33, and O1-O3) refined to 71.37(9)% occupancy, with the atoms in the minor orientation (C40-C43, C50-C53, C60-C63, and O4-O6 respectively) being given the same thermal parameters as the corresponding atoms in the major orientation. One tert-butyl group (the methyls attached to C300) was also modeled as disordered between two orientations. The tetrahydrofuran hydrogen bonded to the Ti-OH was ordered, but the other THF was disordered around a threefold axis. One of the lattice benzenes was located on a threefold axis and was ordered; the second was located on an inversion center and was disordered over two different orientations. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1252P)^2^+52.0783P] 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 13021 _refine_ls_number_parameters 624 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_obs 0.0760 _refine_ls_wR_factor_all 0.2351 _refine_ls_wR_factor_obs 0.2117 _refine_ls_goodness_of_fit_all 1.052 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.052 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max 0.014 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti Ti 0.11554(2) 0.37533(2) 0.531271(11) 0.03287(13) Uani 1 d . . N N 0.02301(7) 0.32987(7) 0.50865(5) 0.0287(4) Uani 1 d . . O O 0.18674(7) 0.41042(8) 0.54787(5) 0.0438(4) Uani 1 d . . H H 0.20966(7) 0.40474(8) 0.54774(5) 0.053 Uiso 1 d R . O1 O 0.08823(11) 0.40200(10) 0.56598(7) 0.0369(5) Uani 0.6485(11) d P 1 C10 C -0.01535(14) 0.32492(14) 0.53876(9) 0.0300(6) Uani 0.6485(11) d P 1 H10A H -0.01271(14) 0.30273(14) 0.55982(9) 0.036 Uiso 0.6485(11) calc PR 1 H10B H -0.05381(14) 0.30459(14) 0.52879(9) 0.036 Uiso 0.6485(11) calc PR 1 C11 C 0.0485(2) 0.41690(15) 0.56883(10) 0.0349(7) Uani 0.6485(11) d P 1 C12 C -0.0040(2) 0.38023(14) 0.55406(9) 0.0324(6) Uani 0.6485(11) d P 1 C13 C -0.0454(2) 0.39466(15) 0.55514(10) 0.0347(6) Uani 0.6485(11) d P 1 H13 H -0.0813(2) 0.36855(15) 0.54585(10) 0.042 Uiso 0.6485(11) calc PR 1 C14 C -0.03700(13) 0.44604(11) 0.56931(8) 0.0495(7) Uani 1 d . . C15 C 0.01381(14) 0.47849(10) 0.58651(7) 0.0474(7) Uani 1 d . . H15 H 0.01877(14) 0.50969(10) 0.60077(7) 0.057 Uiso 1 calc R . C16 C 0.05846(13) 0.46895(11) 0.58453(8) 0.0498(7) Uani 1 d . . O2 O 0.13032(10) 0.40653(11) 0.48310(7) 0.0354(5) Uani 0.6485(11) d P 1 C20 C 0.01670(14) 0.35974(14) 0.47578(9) 0.0298(6) Uani 0.6485(11) d P 1 H20A H 0.02568(14) 0.39736(14) 0.48417(9) 0.036 Uiso 0.6485(11) calc PR 1 H20B H -0.02269(14) 0.33979(14) 0.46762(9) 0.036 Uiso 0.6485(11) calc PR 1 C21 C 0.11025(15) 0.39242(15) 0.44700(10) 0.0319(6) Uani 0.6485(11) d P 1 C22 C 0.05264(14) 0.36545(14) 0.44213(9) 0.0305(6) Uani 0.6485(11) d P 1 C23 C 0.0303(2) 0.3468(2) 0.40610(10) 0.0333(7) Uani 0.6485(11) d P 1 H23 H -0.0088(2) 0.3290(2) 0.40281(10) 0.040 Uiso 0.6485(11) calc PR 1 C24 C 0.06338(11) 0.35343(12) 0.37506(7) 0.0408(5) Uani 1 d . . C25 C 0.11993(11) 0.38549(10) 0.38082(7) 0.0383(5) Uani 1 d . . H25 H 0.14324(11) 0.39706(10) 0.35904(7) 0.046 Uiso 1 calc R . C26 C 0.14543(11) 0.40220(12) 0.41629(7) 0.0426(6) Uani 1 d . . O3 O 0.10088(10) 0.30244(10) 0.53675(7) 0.0342(4) Uani 0.6485(11) d P 1 C30 C 0.00632(14) 0.27190(14) 0.49503(10) 0.0298(6) Uani 0.6485(11) d P 1 H30A H -0.03148(14) 0.25457(14) 0.48396(10) 0.036 Uiso 0.6485(11) calc PR 1 H30B H 0.03220(14) 0.27439(14) 0.47478(10) 0.036 Uiso 0.6485(11) calc PR 1 C31 C 0.05599(14) 0.25293(14) 0.54683(10) 0.0306(6) Uani 0.6485(11) d P 1 C32 C 0.00687(14) 0.23573(13) 0.52652(9) 0.0304(6) Uani 0.6485(11) d P 1 C33 C -0.0408(2) 0.18569(15) 0.53602(11) 0.0362(7) Uani 0.6485(11) d P 1 H33 H -0.0741(2) 0.17402(15) 0.52208(11) 0.043 Uiso 0.6485(11) calc PR 1 C34 C -0.04015(12) 0.15217(11) 0.56610(8) 0.0487(6) Uani 1 d . . C35 C 0.01030(12) 0.16979(10) 0.58419(7) 0.0423(6) Uani 1 d . . H35 H 0.01250(12) 0.14485(10) 0.60163(7) 0.051 Uiso 1 calc R . C36 C 0.05781(11) 0.22102(10) 0.57880(8) 0.0425(6) Uani 1 d . . O4 O 0.0968(2) 0.4304(2) 0.54520(13) 0.0369(5) Uani 0.3515(11) d P 2 C40 C 0.0067(3) 0.3725(2) 0.4980(2) 0.0300(6) Uani 0.3515(11) d P 2 H40A H 0.0329(3) 0.3972(2) 0.4783(2) 0.036 Uiso 0.3515(11) calc PR 2 H40B H -0.0307(3) 0.3528(2) 0.4864(2) 0.036 Uiso 0.3515(11) calc PR 2 C41 C 0.0531(3) 0.4375(3) 0.5519(2) 0.0349(7) Uani 0.3515(11) d P 2 C42 C 0.0057(3) 0.4081(3) 0.5295(2) 0.0324(6) Uani 0.3515(11) d P 2 C43 C -0.0406(3) 0.4135(3) 0.5357(2) 0.0347(6) Uani 0.3515(11) d P 2 H43 H -0.0722(3) 0.3973(3) 0.5195(2) 0.042 Uiso 0.3515(11) calc PR 2 O5 O 0.1297(2) 0.3700(2) 0.48316(13) 0.0354(5) Uani 0.3515(11) d P 2 C50 C 0.0172(3) 0.2953(3) 0.4766(2) 0.0298(6) Uani 0.3515(11) d P 2 H50A H -0.0224(3) 0.2746(3) 0.4690(2) 0.036 Uiso 0.3515(11) calc PR 2 H50B H 0.0281(3) 0.2678(3) 0.4844(2) 0.036 Uiso 0.3515(11) calc PR 2 C51 C 0.1085(3) 0.3630(3) 0.4476(2) 0.0319(6) Uani 0.3515(11) d P 2 C52 C 0.0515(3) 0.3269(3) 0.4429(2) 0.0305(6) Uani 0.3515(11) d P 2 C53 C 0.0282(3) 0.3184(3) 0.4070(2) 0.0333(7) Uani 0.3515(11) d P 2 H53 H -0.0095(3) 0.2908(3) 0.4029(2) 0.040 Uiso 0.3515(11) calc PR 2 O6 O 0.0867(2) 0.3163(2) 0.56428(13) 0.0342(4) Uani 0.3515(11) d P 2 C60 C -0.0173(3) 0.2947(3) 0.5396(2) 0.0298(6) Uani 0.3515(11) d P 2 H60A H -0.0137(3) 0.3190(3) 0.5613(2) 0.036 Uiso 0.3515(11) calc PR 2 H60B H -0.0558(3) 0.2781(3) 0.5298(2) 0.036 Uiso 0.3515(11) calc PR 2 C61 C 0.0448(3) 0.2626(3) 0.5673(2) 0.0306(6) Uani 0.3515(11) d P 2 C62 C -0.0076(3) 0.2494(2) 0.5532(2) 0.0304(6) Uani 0.3515(11) d P 2 C63 C -0.0499(3) 0.1953(3) 0.5546(2) 0.0362(7) Uani 0.3515(11) d P 2 H63 H -0.0864(3) 0.1866(3) 0.5477(2) 0.043 Uiso 0.3515(11) calc PR 2 C100 C -0.08534(15) 0.45781(12) 0.57045(8) 0.0512(7) Uani 1 d . . C101 C -0.0704(2) 0.5092(2) 0.59515(12) 0.096(2) Uani 1 d . . H10C H -0.0373(2) 0.5415(2) 0.58477(12) 0.144 Uiso 1 calc R . H10D H -0.0629(2) 0.5023(2) 0.62119(12) 0.144 Uiso 1 calc R . H10E H -0.1015(2) 0.5164(2) 0.59520(12) 0.144 Uiso 1 calc R . C102 C -0.1365(2) 0.4087(2) 0.58711(13) 0.0862(14) Uani 1 d . . H10F H -0.1283(2) 0.4016(2) 0.61290(13) 0.129 Uiso 1 calc R . H10G H -0.1474(2) 0.3758(2) 0.57128(13) 0.129 Uiso 1 calc R . H10H H -0.1670(2) 0.4168(2) 0.58796(13) 0.129 Uiso 1 calc R . C103 C -0.0971(2) 0.4698(2) 0.53014(10) 0.0739(10) Uani 1 d . . H10I H -0.0635(2) 0.5017(2) 0.51978(10) 0.111 Uiso 1 calc R . H10J H -0.1274(2) 0.4782(2) 0.53075(10) 0.111 Uiso 1 calc R . H10K H -0.1078(2) 0.4372(2) 0.51408(10) 0.111 Uiso 1 calc R . C110 C 0.11505(15) 0.50670(11) 0.60369(8) 0.0565(8) Uani 1 d . . C111 C 0.1606(2) 0.5337(2) 0.57299(12) 0.0813(12) Uani 1 d . . H11A H 0.1512(2) 0.5551(2) 0.55544(12) 0.122 Uiso 1 calc R . H11B H 0.1632(2) 0.5046(2) 0.55892(12) 0.122 Uiso 1 calc R . H11C H 0.1964(2) 0.5584(2) 0.58512(12) 0.122 Uiso 1 calc R . C112 C 0.1134(2) 0.55260(15) 0.62702(12) 0.0849(14) Uani 1 d . . H11D H 0.1037(2) 0.57481(15) 0.61037(12) 0.127 Uiso 1 calc R . H11E H 0.1499(2) 0.57660(15) 0.63847(12) 0.127 Uiso 1 calc R . H11F H 0.0853(2) 0.53565(15) 0.64710(12) 0.127 Uiso 1 calc R . C113 C 0.1301(2) 0.47350(14) 0.63078(10) 0.0695(10) Uani 1 d . . H11G H 0.1316(2) 0.44378(14) 0.61674(10) 0.104 Uiso 1 calc R . H11H H 0.1020(2) 0.45721(14) 0.65083(10) 0.104 Uiso 1 calc R . H11I H 0.1665(2) 0.49816(14) 0.64220(10) 0.104 Uiso 1 calc R . C200 C 0.03668(12) 0.33503(12) 0.33576(7) 0.0450(6) Uani 1 d . . C201 C 0.0088(2) 0.3664(2) 0.32511(13) 0.0917(15) Uani 1 d . . H20C H 0.0355(2) 0.4064(2) 0.32659(13) 0.138 Uiso 1 calc R . H20D H -0.0221(2) 0.3570(2) 0.34255(13) 0.138 Uiso 1 calc R . H20E H -0.0054(2) 0.3567(2) 0.29910(13) 0.138 Uiso 1 calc R . C202 C 0.0828(2) 0.3499(2) 0.30518(10) 0.094(2) Uani 1 d . . H20F H 0.1029(2) 0.3301(2) 0.31083(10) 0.140 Uiso 1 calc R . H20G H 0.1089(2) 0.3901(2) 0.30553(10) 0.140 Uiso 1 calc R . H20H H 0.0656(2) 0.3389(2) 0.28002(10) 0.140 Uiso 1 calc R . C203 C -0.0002(2) 0.2738(2) 0.33446(13) 0.097(2) Uani 1 d . . H20I H 0.0210(2) 0.2557(2) 0.34183(13) 0.146 Uiso 1 calc R . H20J H -0.0145(2) 0.2624(2) 0.30861(13) 0.146 Uiso 1 calc R . H20K H -0.0313(2) 0.2627(2) 0.35206(13) 0.146 Uiso 1 calc R . C210 C 0.20851(11) 0.43817(12) 0.42147(8) 0.0447(6) Uani 1 d . . C211 C 0.23811(13) 0.4563(2) 0.38281(9) 0.0606(8) Uani 1 d . . H21A H 0.22434(13) 0.4776(2) 0.36893(9) 0.091 Uiso 1 calc R . H21B H 0.23057(13) 0.4234(2) 0.36804(9) 0.091 Uiso 1 calc R . H21C H 0.27825(13) 0.4796(2) 0.38683(9) 0.091 Uiso 1 calc R . C212 C 0.2236(2) 0.4915(2) 0.44360(11) 0.0674(9) Uani 1 d . . H21D H 0.2089(2) 0.5123(2) 0.43026(11) 0.101 Uiso 1 calc R . H21E H 0.2642(2) 0.5144(2) 0.44554(11) 0.101 Uiso 1 calc R . H21F H 0.2075(2) 0.4818(2) 0.46912(11) 0.101 Uiso 1 calc R . C213 C 0.23121(12) 0.40532(14) 0.44195(9) 0.0531(7) Uani 1 d . . H21G H 0.27152(12) 0.42873(14) 0.44509(9) 0.080 Uiso 1 calc R . H21H H 0.22309(12) 0.37237(14) 0.42696(9) 0.080 Uiso 1 calc R . H21I H 0.21361(12) 0.39375(14) 0.46696(9) 0.080 Uiso 1 calc R . C300 C -0.0908(2) 0.09518(14) 0.57256(11) 0.0776(12) Uani 1 d . . C301 C -0.1089(5) 0.0678(4) 0.5342(4) 0.138(5) Uani 0.600(6) d P 1 H30C H -0.1019(5) 0.0961(4) 0.5149(4) 0.207 Uiso 0.600(6) calc PR 1 H30D H -0.1487(5) 0.0404(4) 0.5348(4) 0.207 Uiso 0.600(6) calc PR 1 H30E H -0.0878(5) 0.0492(4) 0.5279(4) 0.207 Uiso 0.600(6) calc PR 1 C302 C -0.0912(3) 0.0742(3) 0.6110(2) 0.100(3) Uani 0.600(6) d P 1 H30F H -0.0758(3) 0.1053(3) 0.6290(2) 0.150 Uiso 0.600(6) calc PR 1 H30G H -0.0687(3) 0.0561(3) 0.6113(2) 0.150 Uiso 0.600(6) calc PR 1 H30H H -0.1295(3) 0.0473(3) 0.6183(2) 0.150 Uiso 0.600(6) calc PR 1 C303 C -0.1455(3) 0.1103(3) 0.5835(3) 0.103(3) Uani 0.600(6) d P 1 H30I H -0.1536(3) 0.1258(3) 0.5610(3) 0.155 Uiso 0.600(6) calc PR 1 H30J H -0.1335(3) 0.1373(3) 0.6043(3) 0.155 Uiso 0.600(6) calc PR 1 H30K H -0.1791(3) 0.0760(3) 0.5911(3) 0.155 Uiso 0.600(6) calc PR 1 C304 C -0.1305(7) 0.0832(6) 0.5926(6) 0.138(5) Uani 0.400(6) d P 2 H30L H -0.1180(7) 0.0950(6) 0.6187(6) 0.207 Uiso 0.400(6) calc PR 2 H30M H -0.1557(7) 0.0429(6) 0.5920(6) 0.207 Uiso 0.400(6) calc PR 2 H30N H -0.1501(7) 0.1020(6) 0.5833(6) 0.207 Uiso 0.400(6) calc PR 2 C305 C -0.1278(5) 0.0731(6) 0.5465(4) 0.100(3) Uani 0.400(6) d P 2 H30O H -0.1098(5) 0.0747(6) 0.5223(4) 0.150 Uiso 0.400(6) calc PR 2 H30P H -0.1481(5) 0.0934(6) 0.5444(4) 0.150 Uiso 0.400(6) calc PR 2 H30Q H -0.1538(5) 0.0342(6) 0.5531(4) 0.150 Uiso 0.400(6) calc PR 2 C306 C -0.0650(4) 0.0496(4) 0.5687(5) 0.103(3) Uani 0.400(6) d P 2 H30R H -0.0330(4) 0.0655(4) 0.5515(5) 0.155 Uiso 0.400(6) calc PR 2 H30S H -0.0941(4) 0.0139(4) 0.5586(5) 0.155 Uiso 0.400(6) calc PR 2 H30T H -0.0535(4) 0.0439(4) 0.5938(5) 0.155 Uiso 0.400(6) calc PR 2 C310 C 0.11316(11) 0.23814(11) 0.59878(7) 0.0390(5) Uani 1 d . . C311 C 0.13359(13) 0.29175(13) 0.62172(10) 0.0564(7) Uani 1 d . . H31A H 0.10554(13) 0.28646(13) 0.64070(10) 0.085 Uiso 1 calc R . H31B H 0.13982(13) 0.32216(13) 0.60460(10) 0.085 Uiso 1 calc R . H31C H 0.16847(13) 0.30094(13) 0.63454(10) 0.085 Uiso 1 calc R . C312 C 0.10748(13) 0.19309(13) 0.62628(9) 0.0548(7) Uani 1 d . . H31D H 0.07940(13) 0.18671(13) 0.64552(9) 0.082 Uiso 1 calc R . H31E H 0.14328(13) 0.20507(13) 0.63872(9) 0.082 Uiso 1 calc R . H31F H 0.09610(13) 0.15856(13) 0.61226(9) 0.082 Uiso 1 calc R . C313 C 0.15712(14) 0.2469(2) 0.56934(9) 0.0584(8) Uani 1 d . . H31G H 0.16155(14) 0.2757(2) 0.55131(9) 0.088 Uiso 1 calc R . H31H H 0.14543(14) 0.2120(2) 0.55568(9) 0.088 Uiso 1 calc R . H31I H 0.19261(14) 0.2585(2) 0.58213(9) 0.088 Uiso 1 calc R . O7 O 0.29121(13) 0.4254(2) 0.55413(13) 0.1139(14) Uani 1 d . . C1 C 0.3216(2) 0.4793(3) 0.53854(13) 0.122(2) Uani 1 d . . H1A H 0.3111(2) 0.4792(3) 0.51166(13) 0.146 Uiso 1 calc R . H1B H 0.3620(2) 0.4929(3) 0.53981(13) 0.146 Uiso 1 calc R . C2 C 0.3069(2) 0.5153(2) 0.56216(15) 0.0857(13) Uani 1 d . . H2A H 0.3389(2) 0.5535(2) 0.56454(15) 0.103 Uiso 1 calc R . H2B H 0.2750(2) 0.5170(2) 0.55120(15) 0.103 Uiso 1 calc R . C3 C 0.2924(2) 0.4862(2) 0.59936(11) 0.0753(11) Uani 1 d . . H3A H 0.3189(2) 0.5097(2) 0.61927(11) 0.090 Uiso 1 calc R . H3B H 0.2543(2) 0.4766(2) 0.60716(11) 0.090 Uiso 1 calc R . C4 C 0.2958(2) 0.4353(2) 0.59291(15) 0.0878(13) Uani 1 d . . H4A H 0.3318(2) 0.4407(2) 0.60232(15) 0.105 Uiso 1 calc R . H4B H 0.2654(2) 0.4034(2) 0.60653(15) 0.105 Uiso 1 calc R . C71 C 0.0021(3) 0.0490(3) 0.6855(3) 0.165(4) Uani 1 d . . H71 H 0.0028(3) 0.0820(3) 0.6775(3) 0.198 Uiso 1 calc R . C72 C 0.0495(3) 0.0496(3) 0.6912(3) 0.146(3) Uani 1 d . . H72 H 0.0827(3) 0.0822(3) 0.6985(3) 0.175 Uiso 1 calc R . C81 C 0.2816(7) 0.6304(13) 0.4959(6) 0.207(11) Uani 0.67 d P . H81A H 0.2739(7) 0.6593(13) 0.4862(6) 0.249 Uiso 0.67 calc PR . H81B H 0.2487(7) 0.5929(13) 0.4929(6) 0.249 Uiso 0.67 calc PR . C82 C 0.3006(7) 0.6394(8) 0.5270(6) 0.231(9) Uani 0.67 d P . H82A H 0.2824(7) 0.6045(8) 0.5419(6) 0.277 Uiso 0.67 calc PR . H82B H 0.2926(7) 0.6665(8) 0.5395(6) 0.277 Uiso 0.67 calc PR . O81 O 0.3344(15) 0.6351(14) 0.4802(11) 0.310(29) Uani 0.33 d P . C91 C 0.2812(8) 0.6492(13) 0.6773(14) 0.208(13) Uani 0.50 d P . H91 H 0.2560(8) 0.6408(13) 0.6979(14) 0.249 Uiso 0.50 calc PR . C92 C 0.3294(50) 0.6418(15) 0.6393(14) 0.314(37) Uani 0.50 d P . H92 H 0.3306(50) 0.6239(15) 0.6167(14) 0.377 Uiso 0.50 calc PR . 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 0.0284(2) 0.0332(2) 0.0298(2) 0.00384(15) -0.00157(14) 0.0100(2) N 0.0311(9) 0.0286(8) 0.0253(8) 0.0014(6) 0.0010(7) 0.0140(7) O 0.0290(8) 0.0528(10) 0.0400(9) 0.0040(8) -0.0078(7) 0.0133(8) O1 0.0393(12) 0.0341(12) 0.0320(11) -0.0025(8) -0.0037(9) 0.0144(10) C10 0.0308(14) 0.0279(14) 0.0276(14) -0.0014(10) 0.0029(11) 0.0119(12) C11 0.044(2) 0.033(2) 0.025(2) 0.0010(11) -0.0013(13) 0.0171(14) C12 0.042(2) 0.0289(14) 0.0255(13) 0.0000(10) 0.0026(11) 0.0171(12) C13 0.045(2) 0.033(2) 0.027(2) -0.0007(11) 0.0012(14) 0.0196(14) C14 0.063(2) 0.0368(13) 0.0488(15) -0.0087(11) 0.0089(13) 0.0248(12) C15 0.081(2) 0.0278(11) 0.0312(12) -0.0032(9) -0.0006(12) 0.0258(12) C16 0.058(2) 0.0337(12) 0.0410(14) -0.0097(10) 0.0013(12) 0.0101(12) O2 0.0329(10) 0.0374(11) 0.0289(10) 0.0040(9) 0.0013(8) 0.0124(10) C20 0.0309(14) 0.0292(13) 0.0273(14) 0.0028(11) 0.0022(11) 0.0133(11) C21 0.0351(14) 0.031(2) 0.0285(13) 0.0030(13) 0.0007(11) 0.0162(15) C22 0.0360(15) 0.0310(13) 0.0264(13) 0.0027(11) 0.0028(11) 0.0182(12) C23 0.0391(15) 0.034(2) 0.0289(13) 0.0036(14) -0.0013(11) 0.020(2) C24 0.0513(14) 0.0530(14) 0.0262(11) 0.0009(10) 0.0003(10) 0.0323(12) C25 0.0501(14) 0.0445(13) 0.0303(11) 0.0071(9) 0.0078(10) 0.0311(11) C26 0.0404(13) 0.059(2) 0.0334(12) 0.0048(11) 0.0062(10) 0.0289(12) O3 0.0304(10) 0.0340(11) 0.0360(11) 0.0050(9) 0.0019(8) 0.0146(9) C30 0.0319(14) 0.0281(14) 0.0288(14) -0.0021(11) 0.0000(11) 0.0145(12) C31 0.0330(14) 0.0301(14) 0.0297(15) -0.0003(12) 0.0021(12) 0.0164(12) C32 0.0341(14) 0.0276(13) 0.0288(13) 0.0000(10) 0.0026(11) 0.0150(12) C33 0.040(2) 0.0290(15) 0.033(2) -0.0032(14) -0.0054(15) 0.0124(12) C34 0.0506(15) 0.0326(12) 0.0488(15) 0.0072(10) -0.0072(12) 0.0101(11) C35 0.0538(15) 0.0334(12) 0.0378(12) 0.0046(9) -0.0038(11) 0.0202(11) C36 0.0424(13) 0.0366(12) 0.0498(14) 0.0034(10) -0.0077(11) 0.0207(11) O4 0.0393(12) 0.0341(12) 0.0320(11) -0.0025(8) -0.0037(9) 0.0144(10) C40 0.0308(14) 0.0279(14) 0.0276(14) -0.0014(10) 0.0029(11) 0.0119(12) C41 0.044(2) 0.033(2) 0.025(2) 0.0010(11) -0.0013(13) 0.0171(14) C42 0.042(2) 0.0289(14) 0.0255(13) 0.0000(10) 0.0026(11) 0.0171(12) C43 0.045(2) 0.033(2) 0.027(2) -0.0007(11) 0.0012(14) 0.0196(14) O5 0.0329(10) 0.0374(11) 0.0289(10) 0.0040(9) 0.0013(8) 0.0124(10) C50 0.0309(14) 0.0292(13) 0.0273(14) 0.0028(11) 0.0022(11) 0.0133(11) C51 0.0351(14) 0.031(2) 0.0285(13) 0.0030(13) 0.0007(11) 0.0162(15) C52 0.0360(15) 0.0310(13) 0.0264(13) 0.0027(11) 0.0028(11) 0.0182(12) C53 0.0391(15) 0.034(2) 0.0289(13) 0.0036(14) -0.0013(11) 0.020(2) O6 0.0304(10) 0.0340(11) 0.0360(11) 0.0050(9) 0.0019(8) 0.0146(9) C60 0.0319(14) 0.0281(14) 0.0288(14) -0.0021(11) 0.0000(11) 0.0145(12) C61 0.0330(14) 0.0301(14) 0.0297(15) -0.0003(12) 0.0021(12) 0.0164(12) C62 0.0341(14) 0.0276(13) 0.0288(13) 0.0000(10) 0.0026(11) 0.0150(12) C63 0.040(2) 0.0290(15) 0.033(2) -0.0032(14) -0.0054(15) 0.0124(12) C100 0.086(2) 0.0487(15) 0.0390(13) 0.0003(11) 0.0050(13) 0.049(2) C101 0.165(5) 0.109(3) 0.075(3) -0.045(2) -0.045(3) 0.115(4) C102 0.091(3) 0.105(3) 0.096(3) 0.043(2) 0.044(2) 0.074(3) C103 0.111(3) 0.064(2) 0.047(2) -0.003(2) -0.010(2) 0.045(2) C110 0.079(2) 0.0314(12) 0.0420(14) -0.0058(10) -0.0167(14) 0.0146(13) C111 0.066(2) 0.061(2) 0.077(2) 0.018(2) -0.015(2) 0.002(2) C112 0.126(4) 0.050(2) 0.081(3) -0.035(2) -0.054(3) 0.046(2) C113 0.101(3) 0.052(2) 0.053(2) 0.0006(14) -0.009(2) 0.036(2) C200 0.057(2) 0.0532(15) 0.0262(11) 0.0010(10) -0.0014(10) 0.0285(13) C201 0.132(4) 0.107(3) 0.076(3) -0.020(2) -0.048(3) 0.089(3) C202 0.083(3) 0.149(4) 0.034(2) -0.007(2) 0.000(2) 0.046(3) C203 0.121(4) 0.058(2) 0.072(3) -0.016(2) -0.017(2) 0.014(2) C210 0.0413(13) 0.0537(15) 0.0403(13) 0.0081(11) 0.0073(10) 0.0247(12) C211 0.049(2) 0.071(2) 0.048(2) 0.0194(14) 0.0113(13) 0.0202(15) C212 0.067(2) 0.065(2) 0.073(2) -0.014(2) -0.012(2) 0.034(2) C213 0.0428(14) 0.066(2) 0.053(2) 0.0109(14) 0.0045(12) 0.0285(14) C300 0.072(2) 0.041(2) 0.071(2) 0.022(2) -0.018(2) -0.009(2) C301 0.094(6) 0.078(5) 0.169(9) -0.049(5) 0.028(6) -0.012(4) C302 0.055(3) 0.085(4) 0.072(3) 0.042(3) -0.023(3) -0.031(3) C303 0.057(3) 0.050(3) 0.194(8) 0.015(4) 0.016(4) 0.020(3) C304 0.094(6) 0.078(5) 0.169(9) -0.049(5) 0.028(6) -0.012(4) C305 0.055(3) 0.085(4) 0.072(3) 0.042(3) -0.023(3) -0.031(3) C306 0.057(3) 0.050(3) 0.194(8) 0.015(4) 0.016(4) 0.020(3) C310 0.0438(13) 0.0440(13) 0.0362(12) -0.0007(10) -0.0015(10) 0.0273(11) C311 0.048(2) 0.054(2) 0.069(2) -0.0191(14) -0.0095(14) 0.0267(14) C312 0.057(2) 0.057(2) 0.055(2) 0.0114(13) -0.0080(13) 0.0322(14) C313 0.054(2) 0.076(2) 0.047(2) 0.0037(14) 0.0074(13) 0.034(2) O7 0.060(2) 0.114(3) 0.167(4) -0.068(3) -0.018(2) 0.043(2) C1 0.045(2) 0.177(6) 0.067(3) -0.035(3) 0.011(2) -0.002(3) C2 0.055(2) 0.060(2) 0.117(4) 0.014(2) -0.021(2) 0.010(2) C3 0.060(2) 0.105(3) 0.055(2) -0.014(2) -0.011(2) 0.037(2) C4 0.066(2) 0.073(3) 0.110(4) 0.000(2) -0.037(2) 0.024(2) C71 0.076(4) 0.106(5) 0.296(11) -0.007(6) -0.029(5) 0.034(4) C72 0.106(5) 0.101(5) 0.224(9) -0.014(5) 0.017(5) 0.046(4) C81 0.120(12) 0.291(27) 0.158(14) -0.096(17) -0.018(11) 0.063(15) C82 0.182(16) 0.197(23) 0.358(27) 0.080(18) 0.023(15) 0.128(15) O81 0.234(33) 0.344(43) 0.432(54) -0.278(42) -0.228(41) 0.206(32) C91 0.074(10) 0.160(18) 0.341(38) 0.018(22) 0.084(16) 0.022(11) C92 0.339(63) 0.118(20) 0.407(54) 0.088(27) 0.122(80) 0.056(37) _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 O5 1.762(5) . ? Ti O1 1.783(3) . ? Ti O 1.810(2) . ? Ti O6 1.834(4) . ? Ti O2 1.855(2) . ? Ti O3 1.865(2) . ? Ti O4 1.909(5) . ? Ti N 2.364(2) . ? N C50 1.436(6) . ? N C10 1.460(4) . ? N C20 1.484(4) . ? N C40 1.512(6) . ? N C30 1.513(4) . ? N C60 1.518(6) . ? O1 C11 1.361(5) . ? C10 C12 1.505(5) . ? C11 C12 1.397(5) . ? C11 C16 1.440(4) . ? C12 C13 1.394(5) . ? C13 C14 1.417(4) . ? C14 C15 1.378(4) . ? C14 C43 1.462(7) . ? C14 C100 1.533(4) . ? C15 C16 1.393(5) . ? C16 C41 1.403(7) . ? C16 C110 1.542(4) . ? O2 C21 1.364(4) . ? C20 C22 1.506(4) . ? C21 C26 1.390(4) . ? C21 C22 1.397(5) . ? C22 C23 1.393(5) . ? C23 C24 1.379(4) . ? C24 C25 1.379(4) . ? C24 C53 1.490(7) . ? C24 C200 1.532(3) . ? C25 C26 1.396(4) . ? C26 C51 1.529(7) . ? C26 C210 1.533(4) . ? O3 C31 1.363(4) . ? C30 C32 1.502(5) . ? C31 C32 1.396(5) . ? C31 C36 1.449(4) . ? C32 C33 1.399(5) . ? C33 C34 1.416(4) . ? C34 C35 1.387(4) . ? C34 C63 1.412(8) . ? C34 C300 1.520(4) . ? C35 C36 1.387(4) . ? C36 C61 1.431(7) . ? C36 C310 1.534(4) . ? O4 C41 1.346(9) . ? C40 C42 1.495(8) . ? C41 C42 1.395(9) . ? C42 C43 1.386(10) . ? O5 C51 1.355(8) . ? C50 C52 1.499(9) . ? C51 C52 1.397(9) . ? C52 C53 1.385(9) . ? O6 C61 1.362(8) . ? C60 C62 1.492(9) . ? C61 C62 1.401(9) . ? C62 C63 1.371(9) . ? C100 C102 1.512(5) . ? C100 C103 1.529(4) . ? C100 C101 1.540(4) . ? C110 C113 1.523(5) . ? C110 C112 1.537(5) . ? C110 C111 1.544(5) . ? C200 C201 1.474(5) . ? C200 C203 1.484(5) . ? C200 C202 1.563(5) . ? C210 C213 1.525(4) . ? C210 C212 1.534(4) . ? C210 C211 1.539(4) . ? C300 C304 1.21(2) . ? C300 C305 1.280(11) . ? C300 C302 1.472(7) . ? C300 C301 1.508(12) . ? C300 C306 1.743(12) . ? C300 C303 1.809(9) . ? C310 C313 1.526(4) . ? C310 C312 1.527(4) . ? C310 C311 1.532(4) . ? O7 C4 1.386(6) . ? O7 C1 1.410(7) . ? C1 C2 1.506(7) . ? C2 C3 1.485(6) . ? C3 C4 1.482(6) . ? C71 C72 1.324(9) . ? C71 C72 1.415(9) 2 ? C72 C71 1.415(9) 3 ? C81 C82 1.19(2) . ? C81 O81 1.51(4) . ? C82 C82 1.46(3) 2_665 ? C82 O81 1.93(5) . ? O81 C81 1.01(3) 2_665 ? O81 O81 1.54(5) 2_665 ? O81 O81 1.54(5) 3_565 ? C91 C91 1.48(4) 15_556 ? C91 C91 1.48(4) 14_456 ? C92 C92 1.11(7) 3_565 ? C92 C91 1.54(7) 2_665 ? C92 C92 2.03(9) 15_556 ? C92 C92 2.03(9) 14_456 ? 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 O5 Ti O 97.2(2) . . ? O1 Ti O 97.59(10) . . ? O5 Ti O6 123.4(2) . . ? O Ti O6 98.5(2) . . ? O1 Ti O2 118.25(12) . . ? O Ti O2 96.71(10) . . ? O1 Ti O3 118.22(11) . . ? O Ti O3 97.94(10) . . ? O2 Ti O3 118.62(12) . . ? O5 Ti O4 118.4(2) . . ? O Ti O4 98.5(2) . . ? O6 Ti O4 112.4(2) . . ? O5 Ti N 81.9(2) . . ? O1 Ti N 83.00(9) . . ? O Ti N 179.15(8) . . ? O6 Ti N 82.15(15) . . ? O2 Ti N 82.47(9) . . ? O3 Ti N 82.30(9) . . ? O4 Ti N 81.72(15) . . ? C10 N C20 109.5(2) . . ? C50 N C40 110.6(4) . . ? C10 N C30 108.0(2) . . ? C20 N C30 106.8(2) . . ? C50 N C60 109.6(4) . . ? C40 N C60 105.5(4) . . ? C50 N Ti 110.5(3) . . ? C10 N Ti 110.7(2) . . ? C20 N Ti 111.4(2) . . ? C40 N Ti 109.7(3) . . ? C30 N Ti 110.4(2) . . ? C60 N Ti 110.9(3) . . ? C11 O1 Ti 139.0(2) . . ? N C10 C12 113.2(3) . . ? O1 C11 C12 117.4(3) . . ? O1 C11 C16 123.8(3) . . ? C12 C11 C16 118.7(3) . . ? C13 C12 C11 119.4(3) . . ? C13 C12 C10 121.4(3) . . ? C11 C12 C10 119.1(3) . . ? C12 C13 C14 123.7(3) . . ? C15 C14 C13 114.4(3) . . ? C15 C14 C43 119.5(4) . . ? C15 C14 C100 124.7(2) . . ? C13 C14 C100 120.2(3) . . ? C43 C14 C100 110.9(4) . . ? C14 C15 C16 124.9(2) . . ? C15 C16 C41 109.4(4) . . ? C15 C16 C11 117.9(3) . . ? C15 C16 C110 123.4(2) . . ? C41 C16 C110 122.4(4) . . ? C11 C16 C110 118.0(3) . . ? C21 O2 Ti 139.0(2) . . ? N C20 C22 114.5(3) . . ? O2 C21 C26 121.5(3) . . ? O2 C21 C22 117.5(3) . . ? C26 C21 C22 120.9(3) . . ? C23 C22 C21 119.2(3) . . ? C23 C22 C20 121.9(3) . . ? C21 C22 C20 118.8(3) . . ? C24 C23 C22 122.0(3) . . ? C23 C24 C25 115.9(3) . . ? C25 C24 C53 118.3(3) . . ? C23 C24 C200 119.5(3) . . ? C25 C24 C200 123.6(2) . . ? C53 C24 C200 114.5(3) . . ? C24 C25 C26 124.8(2) . . ? C21 C26 C25 116.1(3) . . ? C25 C26 C51 111.1(3) . . ? C21 C26 C210 119.8(3) . . ? C25 C26 C210 123.2(2) . . ? C51 C26 C210 121.3(3) . . ? C31 O3 Ti 135.7(2) . . ? C32 C30 N 112.2(3) . . ? O3 C31 C32 117.2(3) . . ? O3 C31 C36 121.7(3) . . ? C32 C31 C36 121.0(3) . . ? C31 C32 C33 119.7(3) . . ? C31 C32 C30 119.0(3) . . ? C33 C32 C30 121.3(3) . . ? C32 C33 C34 121.0(3) . . ? C35 C34 C63 114.9(4) . . ? C35 C34 C33 117.0(3) . . ? C35 C34 C300 123.0(3) . . ? C63 C34 C300 117.1(4) . . ? C33 C34 C300 119.1(3) . . ? C34 C35 C36 125.0(2) . . ? C35 C36 C61 111.8(3) . . ? C35 C36 C31 115.3(2) . . ? C35 C36 C310 123.2(2) . . ? C61 C36 C310 119.9(3) . . ? C31 C36 C310 120.2(2) . . ? C41 O4 Ti 142.2(4) . . ? C42 C40 N 116.5(5) . . ? O4 C41 C42 118.0(6) . . ? O4 C41 C16 114.4(5) . . ? C42 C41 C16 127.0(6) . . ? C43 C42 C41 120.2(6) . . ? C43 C42 C40 120.8(6) . . ? C41 C42 C40 118.9(6) . . ? C42 C43 C14 114.4(6) . . ? C51 O5 Ti 143.2(4) . . ? N C50 C52 113.9(5) . . ? O5 C51 C52 117.9(6) . . ? O5 C51 C26 118.3(5) . . ? C52 C51 C26 122.8(5) . . ? C53 C52 C51 119.7(6) . . ? C53 C52 C50 121.2(6) . . ? C51 C52 C50 119.0(5) . . ? C52 C53 C24 118.7(6) . . ? C61 O6 Ti 141.4(4) . . ? C62 C60 N 112.7(5) . . ? O6 C61 C62 117.7(5) . . ? O6 C61 C36 119.0(5) . . ? C62 C61 C36 122.5(5) . . ? C63 C62 C61 118.8(6) . . ? C63 C62 C60 121.3(6) . . ? C61 C62 C60 119.7(5) . . ? C62 C63 C34 121.2(6) . . ? C102 C100 C103 110.5(3) . . ? C102 C100 C14 110.2(2) . . ? C103 C100 C14 109.1(3) . . ? C102 C100 C101 108.3(3) . . ? C103 C100 C101 108.1(3) . . ? C14 C100 C101 110.7(3) . . ? C113 C110 C112 107.4(3) . . ? C113 C110 C16 110.9(3) . . ? C112 C110 C16 110.8(3) . . ? C113 C110 C111 109.0(3) . . ? C112 C110 C111 109.2(3) . . ? C16 C110 C111 109.5(2) . . ? C201 C200 C203 113.9(4) . . ? C201 C200 C24 110.0(3) . . ? C203 C200 C24 110.6(3) . . ? C201 C200 C202 105.8(3) . . ? C203 C200 C202 106.6(3) . . ? C24 C200 C202 109.7(3) . . ? C213 C210 C26 110.2(2) . . ? C213 C210 C212 110.0(3) . . ? C26 C210 C212 111.2(2) . . ? C213 C210 C211 107.5(2) . . ? C26 C210 C211 111.0(2) . . ? C212 C210 C211 106.8(3) . . ? C304 C300 C305 83.3(12) . . ? C302 C300 C301 133.7(7) . . ? C304 C300 C34 128.1(8) . . ? C305 C300 C34 119.7(5) . . ? C302 C300 C34 111.7(3) . . ? C301 C300 C34 107.0(5) . . ? C304 C300 C306 119.7(12) . . ? C305 C300 C306 96.8(11) . . ? C34 C300 C306 104.0(4) . . ? C302 C300 C303 93.2(6) . . ? C301 C300 C303 101.6(7) . . ? C34 C300 C303 103.8(3) . . ? C313 C310 C312 107.9(2) . . ? C313 C310 C311 109.0(3) . . ? C312 C310 C311 107.4(2) . . ? C313 C310 C36 109.6(2) . . ? C312 C310 C36 111.1(2) . . ? C311 C310 C36 111.7(2) . . ? C4 O7 C1 103.1(3) . . ? O7 C1 C2 105.8(3) . . ? C3 C2 C1 102.5(4) . . ? C4 C3 C2 104.7(4) . . ? O7 C4 C3 107.3(4) . . ? C72 C71 C72 121.1(8) . 2 ? C71 C72 C71 114.7(8) . 3 ? C82 C81 O81 90.4(21) . . ? C81 C82 C82 112.5(14) . 2_665 ? C81 C82 O81 51.5(14) . . ? C82 C82 O81 62.4(10) 2_665 . ? C81 O81 C81 121.5(39) 2_665 . ? C81 O81 O81 68.7(36) 2_665 2_665 ? C81 O81 O81 92.8(16) . 2_665 ? C81 O81 O81 118.3(26) 2_665 3_565 ? C81 O81 O81 38.7(14) . 3_565 ? O81 O81 O81 60.005(13) 2_665 3_565 ? C81 O81 C82 84.3(28) 2_665 . ? C81 O81 C82 38.0(14) . . ? O81 O81 C82 86.1(10) 2_665 . ? O81 O81 C82 61.3(11) 3_565 . ? C91 C91 C91 96.6(46) 15_556 14_456 ? C92 C92 C91 117.8(13) 3_565 2_665 ? C92 C92 C92 90.00(2) 3_565 15_556 ? C91 C92 C92 28.6(26) 2_665 15_556 ? C92 C92 C92 74.1(13) 3_565 14_456 ? C91 C92 C92 48.2(35) 2_665 14_456 ? C92 C92 C92 31.8(25) 15_556 14_456 ? _refine_diff_density_max 0.832 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.077 #===END data_ti-o-ti _database_code_depnum_ccdc_archive 'CCDC 225001' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; mu-oxobis(nitrilotris(4,6-di-tert-butyl-o- phenolate))titanium(IV) tetrabenzene solvate ; _chemical_melting_point ? _chemical_formula_moiety 'O(Ti(N(CH2[C6H2(tBu)2O])3)2 . 4 C6H6' _chemical_formula_sum 'C114 H156 N2 O7 Ti2' _chemical_formula_weight 1762.21 _chemical_compound_source ? 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 15.7339(7) _cell_length_b 16.6517(8) _cell_length_c 20.8769(10) _cell_angle_alpha 78.5890(10) _cell_angle_beta 88.7830(10) _cell_angle_gamma 76.1170(10) _cell_volume 5203.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8016 _cell_measurement_theta_min 2.366 _cell_measurement_theta_max 28.288 _exptl_crystal_description rectangular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type 'empirical using SADABS' _exptl_absorpt_correction_T_min 0.938993 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 56252 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.30 _reflns_number_total 25768 _reflns_number_observed 20329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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(obs) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Four of the tert-butyl groups (those with methyl groups attached to C100, C200, C500, C600) were modeled as disordered with major and minor orientations. The relative populations of the orientations were refined independently, with the major orientations 66.6(4)%, 87.7(3)%, 74.9(6)%, and 83.3(4)% occupied, respectively. ; _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^)+(0.0878P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25768 _refine_ls_number_parameters 1155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_obs 0.0713 _refine_ls_wR_factor_all 0.2039 _refine_ls_wR_factor_obs 0.1932 _refine_ls_goodness_of_fit_all 1.307 _refine_ls_goodness_of_fit_obs 1.399 _refine_ls_restrained_S_all 1.307 _refine_ls_restrained_S_obs 1.399 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti1 Ti 0.06011(2) 0.10465(2) 0.18579(2) 0.01641(9) Uani 1 d . . Ti2 Ti 0.13655(3) 0.22375(2) 0.28675(2) 0.01845(10) Uani 1 d . . O O 0.08685(10) 0.15375(9) 0.25104(7) 0.0199(3) Uani 1 d . . O1 O 0.17044(10) 0.03660(10) 0.17877(7) 0.0212(3) Uani 1 d . . O2 O -0.02011(10) 0.04753(10) 0.22301(7) 0.0204(3) Uani 1 d . . O3 O 0.00747(10) 0.20427(9) 0.12973(7) 0.0224(3) Uani 1 d . . O4 O 0.03789(11) 0.29872(10) 0.30563(8) 0.0246(3) Uani 1 d . . O5 O 0.17969(10) 0.14884(10) 0.36260(7) 0.0236(3) Uani 1 d . . O6 O 0.20020(11) 0.25888(10) 0.21439(8) 0.0261(4) Uani 1 d . . N1 N 0.03167(11) 0.05368(11) 0.09726(8) 0.0169(3) Uani 1 d . . N2 N 0.20278(13) 0.31040(12) 0.32957(9) 0.0229(4) Uani 1 d . . C10 C 0.07736(13) -0.03745(13) 0.10619(10) 0.0185(4) Uani 1 d . . H10A H 0.05638(13) -0.06142(13) 0.07152(10) 0.022 Uiso 1 calc R . H10B H 0.06122(13) -0.06746(13) 0.14878(10) 0.022 Uiso 1 calc R . C11 C 0.21981(14) -0.01653(14) 0.14310(10) 0.0196(4) Uani 1 d . . C12 C 0.17508(14) -0.05353(13) 0.10411(10) 0.0186(4) Uani 1 d . . C13 C 0.22012(14) -0.10766(14) 0.06543(11) 0.0213(4) Uani 1 d . . H13 H 0.18832(14) -0.13186(14) 0.03941(11) 0.026 Uiso 1 calc R . C14 C 0.31146(15) -0.12714(15) 0.06413(11) 0.0238(5) Uani 1 d . . C15 C 0.35401(15) -0.0909(2) 0.10399(12) 0.0272(5) Uani 1 d . . H15 H 0.41619(15) -0.1040(2) 0.10386(12) 0.033 Uiso 1 calc R . C16 C 0.31218(15) -0.0363(2) 0.14456(11) 0.0251(5) Uani 1 d . . C100 C 0.3612(2) -0.1874(2) 0.02178(12) 0.0296(5) Uani 1 d . . C101 C 0.3481(5) -0.2753(3) 0.0485(3) 0.068(2) Uani 0.666(4) d P 1 H10C H 0.2853(5) -0.2728(3) 0.0518(3) 0.103 Uiso 0.666(4) calc PR 1 H10D H 0.3764(5) -0.2968(3) 0.0919(3) 0.103 Uiso 0.666(4) calc PR 1 H10E H 0.3742(5) -0.3131(3) 0.0191(3) 0.103 Uiso 0.666(4) calc PR 1 C102 C 0.3217(3) -0.1597(4) -0.0491(2) 0.0543(14) Uani 0.666(4) d P 1 H10F H 0.3289(3) -0.1030(4) -0.0679(2) 0.082 Uiso 0.666(4) calc PR 1 H10G H 0.2592(3) -0.1590(4) -0.0482(2) 0.082 Uiso 0.666(4) calc PR 1 H10H H 0.3519(3) -0.1995(4) -0.0757(2) 0.082 Uiso 0.666(4) calc PR 1 C103 C 0.4580(3) -0.1871(5) 0.0155(4) 0.067(2) Uani 0.666(4) d P 1 H10I H 0.4635(3) -0.1294(5) -0.0018(4) 0.101 Uiso 0.666(4) calc PR 1 H10J H 0.4851(3) -0.2239(5) -0.0143(4) 0.101 Uiso 0.666(4) calc PR 1 H10K H 0.4874(3) -0.2076(5) 0.0586(4) 0.101 Uiso 0.666(4) calc PR 1 C104 C 0.4181(10) -0.2669(6) 0.0709(6) 0.068(2) Uani 0.334(4) d P 2 H10L H 0.4563(10) -0.2480(6) 0.0981(6) 0.103 Uiso 0.334(4) calc PR 2 H10M H 0.4538(10) -0.3061(6) 0.0460(6) 0.103 Uiso 0.334(4) calc PR 2 H10N H 0.3790(10) -0.2954(6) 0.0989(6) 0.103 Uiso 0.334(4) calc PR 2 C105 C 0.3043(7) -0.2157(8) -0.0184(5) 0.0543(14) Uani 0.334(4) d P 2 H10O H 0.2621(7) -0.2400(8) 0.0093(5) 0.082 Uiso 0.334(4) calc PR 2 H10P H 0.3397(7) -0.2585(8) -0.0405(5) 0.082 Uiso 0.334(4) calc PR 2 H10Q H 0.2729(7) -0.1676(8) -0.0511(5) 0.082 Uiso 0.334(4) calc PR 2 C106 C 0.4275(7) -0.1495(10) -0.0158(7) 0.067(2) Uani 0.334(4) d P 2 H10R H 0.4635(7) -0.1319(10) 0.0140(7) 0.101 Uiso 0.334(4) calc PR 2 H10S H 0.3981(7) -0.1002(10) -0.0484(7) 0.101 Uiso 0.334(4) calc PR 2 H10T H 0.4649(7) -0.1912(10) -0.0379(7) 0.101 Uiso 0.334(4) calc PR 2 C110 C 0.3721(2) -0.0097(2) 0.1896(2) 0.0421(7) Uani 1 d . . C111 C 0.4429(2) 0.0246(3) 0.1487(3) 0.099(2) Uani 1 d . . H11A H 0.4151(2) 0.0746(3) 0.1162(3) 0.149 Uiso 1 calc R . H11B H 0.4765(2) -0.0189(3) 0.1263(3) 0.149 Uiso 1 calc R . H11C H 0.4824(2) 0.0397(3) 0.1774(3) 0.149 Uiso 1 calc R . C112 C 0.4131(3) -0.0880(3) 0.2408(2) 0.084(2) Uani 1 d . . H11D H 0.4426(3) -0.1336(3) 0.2189(2) 0.126 Uiso 1 calc R . H11E H 0.3672(3) -0.1059(3) 0.2684(2) 0.126 Uiso 1 calc R . H11F H 0.4559(3) -0.0747(3) 0.2680(2) 0.126 Uiso 1 calc R . C113 C 0.3270(2) 0.0597(2) 0.22573(13) 0.0337(6) Uani 1 d . . H11G H 0.3000(2) 0.1108(2) 0.19393(13) 0.051 Uiso 1 calc R . H11H H 0.3703(2) 0.0720(2) 0.25299(13) 0.051 Uiso 1 calc R . H11I H 0.2817(2) 0.0408(2) 0.25345(13) 0.051 Uiso 1 calc R . C20 C -0.06477(13) 0.06282(14) 0.09037(10) 0.0197(4) Uani 1 d . . H20A H -0.07736(13) 0.04842(14) 0.04834(10) 0.024 Uiso 1 calc R . H20B H -0.09536(13) 0.12252(14) 0.08894(10) 0.024 Uiso 1 calc R . C21 C -0.07844(14) 0.00386(13) 0.21007(11) 0.0196(4) Uani 1 d . . C22 C -0.10060(13) 0.00800(13) 0.14483(10) 0.0189(4) Uani 1 d . . C23 C -0.15908(14) -0.03720(14) 0.12962(11) 0.0221(4) Uani 1 d . . H23 H -0.17321(14) -0.03451(14) 0.08511(11) 0.026 Uiso 1 calc R . C24 C -0.19682(15) -0.08586(15) 0.17823(12) 0.0251(5) Uani 1 d . . C25 C -0.1733(2) -0.0888(2) 0.24258(12) 0.0278(5) Uani 1 d . . H25 H -0.1989(2) -0.1219(2) 0.27624(12) 0.033 Uiso 1 calc R . C26 C -0.1140(2) -0.04574(14) 0.26109(11) 0.0245(5) Uani 1 d . . C200 C -0.2590(2) -0.1371(2) 0.16030(13) 0.0288(5) Uani 1 d . . C201 C -0.3195(3) -0.0873(3) 0.1006(2) 0.0665(14) Uani 0.877(3) d P 1 H20C H -0.2837(3) -0.0699(3) 0.0639(2) 0.100 Uiso 0.877(3) calc PR 1 H20D H -0.3585(3) -0.0371(3) 0.1123(2) 0.100 Uiso 0.877(3) calc PR 1 H20E H -0.3546(3) -0.1233(3) 0.0881(2) 0.100 Uiso 0.877(3) calc PR 1 C202 C -0.3169(2) -0.1625(3) 0.2157(2) 0.0489(10) Uani 0.877(3) d P 1 H20F H -0.3529(2) -0.1118(3) 0.2286(2) 0.073 Uiso 0.877(3) calc PR 1 H20G H -0.2803(2) -0.1976(3) 0.2532(2) 0.073 Uiso 0.877(3) calc PR 1 H20H H -0.3549(2) -0.1946(3) 0.2013(2) 0.073 Uiso 0.877(3) calc PR 1 C203 C -0.2040(2) -0.2176(2) 0.1417(2) 0.0485(10) Uani 0.877(3) d P 1 H20I H -0.1658(2) -0.2028(2) 0.1058(2) 0.073 Uiso 0.877(3) calc PR 1 H20J H -0.2427(2) -0.2494(2) 0.1277(2) 0.073 Uiso 0.877(3) calc PR 1 H20K H -0.1681(2) -0.2523(2) 0.1796(2) 0.073 Uiso 0.877(3) calc PR 1 C204 C -0.2565(2) -0.1348(2) 0.0863(2) 0.0665(14) Uani 0.123(3) d PR 2 H20L H -0.1996(2) -0.1680(2) 0.0755(2) 0.100 Uiso 0.123(3) calc PR 2 H20M H -0.2651(2) -0.0762(2) 0.0628(2) 0.100 Uiso 0.123(3) calc PR 2 H20N H -0.3032(2) -0.1587(2) 0.0735(2) 0.100 Uiso 0.123(3) calc PR 2 C205 C -0.3364(2) -0.0922(2) 0.1805(2) 0.0489(10) Uani 0.123(3) d PR 2 H20O H -0.3530(2) -0.0362(2) 0.1521(2) 0.073 Uiso 0.123(3) calc PR 2 H20P H -0.3291(2) -0.0861(2) 0.2257(2) 0.073 Uiso 0.123(3) calc PR 2 H20Q H -0.3824(2) -0.1222(2) 0.1782(2) 0.073 Uiso 0.123(3) calc PR 2 C206 C -0.2366(2) -0.2203(2) 0.2040(2) 0.0485(10) Uani 0.123(3) d PR 2 H20R H -0.1815(2) -0.2538(2) 0.1907(2) 0.073 Uiso 0.123(3) calc PR 2 H20S H -0.2834(2) -0.2493(2) 0.2015(2) 0.073 Uiso 0.123(3) calc PR 2 H20T H -0.2301(2) -0.2132(2) 0.2490(2) 0.073 Uiso 0.123(3) calc PR 2 C210 C -0.0838(2) -0.0566(2) 0.33246(12) 0.0332(6) Uani 1 d . . C211 C -0.1390(3) -0.1049(2) 0.38023(14) 0.0591(10) Uani 1 d . . H21A H -0.1181(3) -0.1106(2) 0.42517(14) 0.089 Uiso 1 calc R . H21B H -0.1335(3) -0.1610(2) 0.37039(14) 0.089 Uiso 1 calc R . H21C H -0.2006(3) -0.0737(2) 0.37550(14) 0.089 Uiso 1 calc R . C212 C 0.0127(2) -0.1061(2) 0.33965(15) 0.0473(8) Uani 1 d . . H21D H 0.0333(2) -0.1137(2) 0.38492(15) 0.071 Uiso 1 calc R . H21E H 0.0482(2) -0.0747(2) 0.31031(15) 0.071 Uiso 1 calc R . H21F H 0.0180(2) -0.1614(2) 0.32830(15) 0.071 Uiso 1 calc R . C213 C -0.0929(2) 0.0286(2) 0.35352(13) 0.0382(6) Uani 1 d . . H21G H -0.0730(2) 0.0186(2) 0.39920(13) 0.057 Uiso 1 calc R . H21H H -0.1544(2) 0.0601(2) 0.34903(13) 0.057 Uiso 1 calc R . H21I H -0.0571(2) 0.0614(2) 0.32571(13) 0.057 Uiso 1 calc R . C30 C 0.06394(14) 0.10262(13) 0.03801(10) 0.0188(4) Uani 1 d . . H30A H 0.06374(14) 0.07333(13) 0.00113(10) 0.023 Uiso 1 calc R . H30B H 0.12520(14) 0.10400(13) 0.04646(10) 0.023 Uiso 1 calc R . C31 C -0.02148(15) 0.23753(14) 0.06719(11) 0.0215(4) Uani 1 d . . C32 C 0.00953(14) 0.19178(13) 0.01868(10) 0.0201(4) Uani 1 d . . C33 C -0.01290(15) 0.22700(14) -0.04656(11) 0.0222(4) Uani 1 d . . H33 H 0.00881(15) 0.19539(14) -0.07916(11) 0.027 Uiso 1 calc R . C34 C -0.0668(2) 0.30806(14) -0.06506(11) 0.0242(5) Uani 1 d . . C35 C -0.1029(2) 0.34857(15) -0.01487(12) 0.0264(5) Uani 1 d . . H35 H -0.1423(2) 0.40249(15) -0.02664(12) 0.032 Uiso 1 calc R . C36 C -0.0849(2) 0.31498(14) 0.05155(11) 0.0242(5) Uani 1 d . . C300 C -0.0844(2) 0.3522(2) -0.13699(12) 0.0303(5) Uani 1 d . . C301 C -0.0717(2) 0.2876(2) -0.18230(13) 0.0405(7) Uani 1 d . . H30C H -0.0833(2) 0.3176(2) -0.22779(13) 0.061 Uiso 1 calc R . H30D H -0.1123(2) 0.2511(2) -0.17048(13) 0.061 Uiso 1 calc R . H30E H -0.0113(2) 0.2532(2) -0.17739(13) 0.061 Uiso 1 calc R . C302 C -0.0197(2) 0.4085(2) -0.15505(13) 0.0396(6) Uani 1 d . . H30F H -0.0297(2) 0.4374(2) -0.20089(13) 0.059 Uiso 1 calc R . H30G H 0.0404(2) 0.3736(2) -0.14878(13) 0.059 Uiso 1 calc R . H30H H -0.0285(2) 0.4504(2) -0.12700(13) 0.059 Uiso 1 calc R . C303 C -0.1781(2) 0.4085(2) -0.14872(14) 0.0444(7) Uani 1 d . . H30I H -0.1869(2) 0.4356(2) -0.19502(14) 0.067 Uiso 1 calc R . H30J H -0.1866(2) 0.4519(2) -0.12201(14) 0.067 Uiso 1 calc R . H30K H -0.2204(2) 0.3738(2) -0.13658(14) 0.067 Uiso 1 calc R . C310 C -0.1355(2) 0.35653(15) 0.10500(12) 0.0277(5) Uani 1 d . . C311 C -0.2063(2) 0.4352(2) 0.07538(14) 0.0433(7) Uani 1 d . . H31A H -0.2374(2) 0.4602(2) 0.11054(14) 0.065 Uiso 1 calc R . H31B H -0.2478(2) 0.4193(2) 0.04881(14) 0.065 Uiso 1 calc R . H31C H -0.1788(2) 0.4763(2) 0.04785(14) 0.065 Uiso 1 calc R . C312 C -0.0748(2) 0.3826(2) 0.14978(13) 0.0332(6) Uani 1 d . . H31D H -0.0290(2) 0.3331(2) 0.16929(13) 0.050 Uiso 1 calc R . H31E H -0.1091(2) 0.4059(2) 0.18450(13) 0.050 Uiso 1 calc R . H31F H -0.0479(2) 0.4254(2) 0.12405(13) 0.050 Uiso 1 calc R . C313 C -0.1833(2) 0.2937(2) 0.14570(13) 0.0307(5) Uani 1 d . . H31G H -0.1403(2) 0.2422(2) 0.16568(13) 0.046 Uiso 1 calc R . H31H H -0.2241(2) 0.2798(2) 0.11721(13) 0.046 Uiso 1 calc R . H31I H -0.2160(2) 0.3193(2) 0.18006(13) 0.046 Uiso 1 calc R . C40 C 0.1572(2) 0.39999(15) 0.30098(12) 0.0273(5) Uani 1 d . . H40A H 0.1524(2) 0.40729(15) 0.25286(12) 0.033 Uiso 1 calc R . H40B H 0.1923(2) 0.43821(15) 0.31098(12) 0.033 Uiso 1 calc R . C41 C 0.0119(2) 0.36800(14) 0.33301(11) 0.0239(5) Uani 1 d . . C42 C 0.0665(2) 0.42365(14) 0.32808(11) 0.0249(5) Uani 1 d . . C43 C 0.0393(2) 0.4981(2) 0.35123(12) 0.0296(5) Uani 1 d . . H43 H 0.0766(2) 0.5359(2) 0.34731(12) 0.036 Uiso 1 calc R . C44 C -0.0417(2) 0.5183(2) 0.38017(12) 0.0323(6) Uani 1 d . . C45 C -0.0903(2) 0.4575(2) 0.38946(12) 0.0309(5) Uani 1 d . . H45 H -0.1437(2) 0.4686(2) 0.41183(12) 0.037 Uiso 1 calc R . C46 C -0.0656(2) 0.3809(2) 0.36804(11) 0.0265(5) Uani 1 d . . C400 C -0.0762(2) 0.6050(2) 0.39783(14) 0.0417(7) Uani 1 d . . C401 C -0.1161(3) 0.6659(2) 0.3355(2) 0.084(2) Uani 1 d . . H40C H -0.1617(3) 0.6449(2) 0.3177(2) 0.127 Uiso 1 calc R . H40D H -0.0703(3) 0.6705(2) 0.3033(2) 0.127 Uiso 1 calc R . H40E H -0.1418(3) 0.7217(2) 0.3455(2) 0.127 Uiso 1 calc R . C402 C -0.0060(3) 0.6358(2) 0.4263(2) 0.0749(13) Uani 1 d . . H40F H 0.0188(3) 0.5959(2) 0.4663(2) 0.112 Uiso 1 calc R . H40G H -0.0313(3) 0.6913(2) 0.4367(2) 0.112 Uiso 1 calc R . H40H H 0.0402(3) 0.6402(2) 0.3945(2) 0.112 Uiso 1 calc R . C403 C -0.1490(4) 0.6050(3) 0.4475(3) 0.108(2) Uani 1 d . . H40I H -0.1962(4) 0.5852(3) 0.4305(3) 0.162 Uiso 1 calc R . H40J H -0.1721(4) 0.6624(3) 0.4550(3) 0.162 Uiso 1 calc R . H40K H -0.1255(4) 0.5674(3) 0.4887(3) 0.162 Uiso 1 calc R . C410 C -0.1167(2) 0.3120(2) 0.38521(14) 0.0353(6) Uani 1 d . . C411 C -0.1496(2) 0.2909(2) 0.3236(2) 0.0479(8) Uani 1 d . . H41A H -0.1819(2) 0.2469(2) 0.3360(2) 0.072 Uiso 1 calc R . H41B H -0.0996(2) 0.2707(2) 0.2973(2) 0.072 Uiso 1 calc R . H41C H -0.1884(2) 0.3416(2) 0.2979(2) 0.072 Uiso 1 calc R . C412 C -0.1968(2) 0.3397(2) 0.4267(2) 0.0525(8) Uani 1 d . . H41D H -0.1774(2) 0.3535(2) 0.4666(2) 0.079 Uiso 1 calc R . H41E H -0.2266(2) 0.2936(2) 0.4384(2) 0.079 Uiso 1 calc R . H41F H -0.2374(2) 0.3895(2) 0.4014(2) 0.079 Uiso 1 calc R . C413 C -0.0570(2) 0.2325(2) 0.42676(15) 0.0418(7) Uani 1 d . . H41G H -0.0364(2) 0.2467(2) 0.46609(15) 0.063 Uiso 1 calc R . H41H H -0.0067(2) 0.2111(2) 0.40120(15) 0.063 Uiso 1 calc R . H41I H -0.0900(2) 0.1891(2) 0.43944(15) 0.063 Uiso 1 calc R . C50 C 0.1996(2) 0.2956(2) 0.40196(11) 0.0261(5) Uani 1 d . . H50A H 0.1376(2) 0.3054(2) 0.41473(11) 0.031 Uiso 1 calc R . H50B H 0.2251(2) 0.3374(2) 0.41750(11) 0.031 Uiso 1 calc R . C51 C 0.22855(14) 0.1372(2) 0.41819(11) 0.0233(5) Uani 1 d . . C52 C 0.2473(2) 0.2087(2) 0.43559(11) 0.0248(5) Uani 1 d . . C53 C 0.3059(2) 0.1977(2) 0.48760(12) 0.0279(5) Uani 1 d . . H53 H 0.3207(2) 0.2457(2) 0.49816(12) 0.033 Uiso 1 calc R . C54 C 0.3430(2) 0.1186(2) 0.52412(13) 0.0325(6) Uani 1 d . . C55 C 0.3162(2) 0.0504(2) 0.50917(12) 0.0293(5) Uani 1 d . . H55 H 0.3385(2) -0.0038(2) 0.53570(12) 0.035 Uiso 1 calc R . C56 C 0.2582(2) 0.0570(2) 0.45729(11) 0.0255(5) Uani 1 d . . C500 C 0.4114(2) 0.1085(2) 0.5785(2) 0.0441(7) Uani 1 d . . C501 C 0.4372(5) 0.0220(4) 0.6180(3) 0.087(3) Uani 0.749(6) d P 1 H50C H 0.4588(5) -0.0180(4) 0.5893(3) 0.131 Uiso 0.749(6) calc PR 1 H50D H 0.3863(5) 0.0079(4) 0.6413(3) 0.131 Uiso 0.749(6) calc PR 1 H50E H 0.4836(5) 0.0189(4) 0.6497(3) 0.131 Uiso 0.749(6) calc PR 1 C502 C 0.4960(3) 0.1320(4) 0.5436(3) 0.065(2) Uani 0.749(6) d P 1 H50F H 0.4797(3) 0.1893(4) 0.5172(3) 0.098 Uiso 0.749(6) calc PR 1 H50G H 0.5200(3) 0.0919(4) 0.5153(3) 0.098 Uiso 0.749(6) calc PR 1 H50H H 0.5403(3) 0.1291(4) 0.5768(3) 0.098 Uiso 0.749(6) calc PR 1 C503 C 0.3773(3) 0.1729(4) 0.6218(3) 0.0490(13) Uani 0.749(6) d P 1 H50I H 0.3607(3) 0.2297(4) 0.5945(3) 0.074 Uiso 0.749(6) calc PR 1 H50J H 0.4233(3) 0.1706(4) 0.6535(3) 0.074 Uiso 0.749(6) calc PR 1 H50K H 0.3261(3) 0.1597(4) 0.6451(3) 0.074 Uiso 0.749(6) calc PR 1 C504 C 0.3803(15) 0.0450(12) 0.6445(10) 0.087(3) Uani 0.251(6) d P 2 H50L H 0.3806(15) -0.0097(12) 0.6337(10) 0.131 Uiso 0.251(6) calc PR 2 H50M H 0.3212(15) 0.0716(12) 0.6566(10) 0.131 Uiso 0.251(6) calc PR 2 H50N H 0.4213(15) 0.0367(12) 0.6813(10) 0.131 Uiso 0.251(6) calc PR 2 C505 C 0.4978(8) 0.0583(14) 0.5629(8) 0.065(2) Uani 0.251(6) d P 2 H50O H 0.4896(8) 0.0108(14) 0.5445(8) 0.098 Uiso 0.251(6) calc PR 2 H50P H 0.5344(8) 0.0368(14) 0.6028(8) 0.098 Uiso 0.251(6) calc PR 2 H50Q H 0.5264(8) 0.0941(14) 0.5310(8) 0.098 Uiso 0.251(6) calc PR 2 C506 C 0.4057(12) 0.1819(15) 0.6062(9) 0.0490(13) Uani 0.251(6) d P 2 H50R H 0.3442(12) 0.2073(15) 0.6133(9) 0.074 Uiso 0.251(6) calc PR 2 H50S H 0.4305(12) 0.2230(15) 0.5761(9) 0.074 Uiso 0.251(6) calc PR 2 H50T H 0.4385(12) 0.1657(15) 0.6480(9) 0.074 Uiso 0.251(6) calc PR 2 C510 C 0.2227(2) -0.0185(2) 0.44747(11) 0.0270(5) Uani 1 d . . C511 C 0.2585(2) -0.0974(2) 0.50024(13) 0.0367(6) Uani 1 d . . H51A H 0.2432(2) -0.0846(2) 0.54349(13) 0.055 Uiso 1 calc R . H51B H 0.3223(2) -0.1148(2) 0.49757(13) 0.055 Uiso 1 calc R . H51C H 0.2327(2) -0.1432(2) 0.49337(13) 0.055 Uiso 1 calc R . C512 C 0.1222(2) 0.0050(2) 0.45141(13) 0.0316(5) Uani 1 d . . H51D H 0.0980(2) 0.0554(2) 0.41805(13) 0.047 Uiso 1 calc R . H51E H 0.1058(2) 0.0166(2) 0.49482(13) 0.047 Uiso 1 calc R . H51F H 0.0989(2) -0.0419(2) 0.44388(13) 0.047 Uiso 1 calc R . C513 C 0.2481(2) -0.0412(2) 0.38063(12) 0.0334(6) Uani 1 d . . H51G H 0.2260(2) 0.0082(2) 0.34594(12) 0.050 Uiso 1 calc R . H51H H 0.2225(2) -0.0874(2) 0.37457(12) 0.050 Uiso 1 calc R . H51I H 0.3120(2) -0.0589(2) 0.37876(12) 0.050 Uiso 1 calc R . C60 C 0.2966(2) 0.2930(2) 0.31231(12) 0.0282(5) Uani 1 d . . H60A H 0.3225(2) 0.2317(2) 0.32604(12) 0.034 Uiso 1 calc R . H60B H 0.3272(2) 0.3225(2) 0.33757(12) 0.034 Uiso 1 calc R . C61 C 0.2649(2) 0.29932(15) 0.19383(12) 0.0266(5) Uani 1 d . . C62 C 0.3132(2) 0.3191(2) 0.24141(12) 0.0283(5) Uani 1 d . . C63 C 0.3795(2) 0.3611(2) 0.22385(14) 0.0317(6) Uani 1 d . . H63 H 0.4096(2) 0.3761(2) 0.25692(14) 0.038 Uiso 1 calc R . C64 C 0.4022(2) 0.3813(2) 0.16001(14) 0.0342(6) Uani 1 d . . C65 C 0.3529(2) 0.3612(2) 0.11290(13) 0.0330(6) Uani 1 d . . H65 H 0.3677(2) 0.3753(2) 0.06841(13) 0.040 Uiso 1 calc R . C66 C 0.2834(2) 0.32159(15) 0.12677(12) 0.0291(5) Uani 1 d . . C600 C 0.4771(2) 0.4246(2) 0.1395(2) 0.0383(7) Uani 1 d . . C601 C 0.4429(2) 0.5102(2) 0.0992(2) 0.0519(11) Uani 0.833(4) d P 1 H60C H 0.3991(2) 0.5437(2) 0.1238(2) 0.078 Uiso 0.833(4) calc PR 1 H60D H 0.4158(2) 0.5055(2) 0.0587(2) 0.078 Uiso 0.833(4) calc PR 1 H60E H 0.4911(2) 0.5380(2) 0.0886(2) 0.078 Uiso 0.833(4) calc PR 1 C602 C 0.5454(2) 0.3699(2) 0.1038(2) 0.0395(8) Uani 0.833(4) d P 1 H60F H 0.5665(2) 0.3141(2) 0.1318(2) 0.059 Uiso 0.833(4) calc PR 1 H60G H 0.5946(2) 0.3964(2) 0.0933(2) 0.059 Uiso 0.833(4) calc PR 1 H60H H 0.5193(2) 0.3639(2) 0.0634(2) 0.059 Uiso 0.833(4) calc PR 1 C603 C 0.5279(3) 0.4350(3) 0.2011(2) 0.0490(10) Uani 0.833(4) d P 1 H60I H 0.5514(3) 0.3794(3) 0.2287(2) 0.074 Uiso 0.833(4) calc PR 1 H60J H 0.4875(3) 0.4707(3) 0.2262(2) 0.074 Uiso 0.833(4) calc PR 1 H60K H 0.5762(3) 0.4613(3) 0.1863(2) 0.074 Uiso 0.833(4) calc PR 1 C604 C 0.4661(13) 0.4990(11) 0.1668(12) 0.0519(11) Uani 0.167(4) d P 2 H60L H 0.4066(13) 0.5342(11) 0.1568(12) 0.078 Uiso 0.167(4) calc PR 2 H60M H 0.5086(13) 0.5309(11) 0.1481(12) 0.078 Uiso 0.167(4) calc PR 2 H60N H 0.4757(13) 0.4826(11) 0.2144(12) 0.078 Uiso 0.167(4) calc PR 2 C605 C 0.4576(11) 0.4725(11) 0.0537(9) 0.0395(8) Uani 0.167(4) d P 2 H60O H 0.4027(11) 0.5164(11) 0.0482(9) 0.059 Uiso 0.167(4) calc PR 2 H60P H 0.4533(11) 0.4293(11) 0.0290(9) 0.059 Uiso 0.167(4) calc PR 2 H60Q H 0.5061(11) 0.4977(11) 0.0375(9) 0.059 Uiso 0.167(4) calc PR 2 C606 C 0.5506(13) 0.3663(13) 0.1456(12) 0.0490(10) Uani 0.167(4) d P 2 H60R H 0.5443(13) 0.3212(13) 0.1236(12) 0.074 Uiso 0.167(4) calc PR 2 H60S H 0.5648(13) 0.3429(13) 0.1921(12) 0.074 Uiso 0.167(4) calc PR 2 H60T H 0.5978(13) 0.3912(13) 0.1258(12) 0.074 Uiso 0.167(4) calc PR 2 C610 C 0.2292(2) 0.3088(2) 0.07169(12) 0.0318(6) Uani 1 d . . C611 C 0.2230(2) 0.2165(2) 0.07937(13) 0.0426(7) Uani 1 d . . H61A H 0.1877(2) 0.2112(2) 0.04299(13) 0.064 Uiso 1 calc R . H61B H 0.1953(2) 0.1997(2) 0.12076(13) 0.064 Uiso 1 calc R . H61C H 0.2819(2) 0.1799(2) 0.07924(13) 0.064 Uiso 1 calc R . C612 C 0.1370(2) 0.3660(2) 0.07118(14) 0.0408(7) Uani 1 d . . H61D H 0.1014(2) 0.3584(2) 0.03590(14) 0.061 Uiso 1 calc R . H61E H 0.1406(2) 0.4250(2) 0.06412(14) 0.061 Uiso 1 calc R . H61F H 0.1099(2) 0.3511(2) 0.11319(14) 0.061 Uiso 1 calc R . C613 C 0.2684(2) 0.3310(2) 0.00357(13) 0.0381(6) Uani 1 d . . H61G H 0.2313(2) 0.3218(2) -0.03002(13) 0.057 Uiso 1 calc R . H61H H 0.3275(2) 0.2950(2) 0.00283(13) 0.057 Uiso 1 calc R . H61I H 0.2712(2) 0.3904(2) -0.00516(13) 0.057 Uiso 1 calc R . C71 C -0.3453(5) -0.4238(6) 0.3002(3) 0.155(3) Uani 1 d . . H71 H -0.3350(5) -0.4442(6) 0.3459(3) 0.186 Uiso 1 calc R . C72 C -0.4286(4) -0.3730(6) 0.2767(3) 0.134(3) Uani 1 d . . H72 H -0.4747(4) -0.3597(6) 0.3059(3) 0.160 Uiso 1 calc R . C73 C -0.4403(3) -0.3444(3) 0.2128(3) 0.0767(12) Uani 1 d . . H73 H -0.4957(3) -0.3105(3) 0.1957(3) 0.092 Uiso 1 calc R . C74 C -0.3740(3) -0.3632(2) 0.1716(2) 0.0652(10) Uani 1 d . . H74 H -0.3830(3) -0.3420(2) 0.1259(2) 0.078 Uiso 1 calc R . C75 C -0.2942(3) -0.4126(2) 0.1955(3) 0.0690(11) Uani 1 d . . H75 H -0.2480(3) -0.4247(2) 0.1662(3) 0.083 Uiso 1 calc R . C76 C -0.2807(4) -0.4436(4) 0.2588(3) 0.098(2) Uani 1 d . . H76 H -0.2257(4) -0.4795(4) 0.2749(3) 0.117 Uiso 1 calc R . C81 C -0.2484(3) 0.3675(4) -0.3595(3) 0.100(2) Uani 1 d . . H81 H -0.2340(3) 0.4026(4) -0.3978(3) 0.120 Uiso 1 calc R . C82 C -0.3062(3) 0.4026(4) -0.3130(3) 0.0868(14) Uani 1 d . . H82 H -0.3327(3) 0.4614(4) -0.3203(3) 0.104 Uiso 1 calc R . C83 C -0.3227(3) 0.3490(3) -0.2571(2) 0.0754(12) Uani 1 d . . H83 H -0.3595(3) 0.3721(3) -0.2253(2) 0.090 Uiso 1 calc R . C84 C -0.2876(3) 0.2636(3) -0.2460(2) 0.0744(12) Uani 1 d . . H84 H -0.3010(3) 0.2279(3) -0.2077(2) 0.089 Uiso 1 calc R . C85 C -0.2324(3) 0.2307(3) -0.2917(2) 0.0769(13) Uani 1 d . . H85 H -0.2066(3) 0.1717(3) -0.2842(2) 0.092 Uiso 1 calc R . C86 C -0.2143(3) 0.2814(4) -0.3474(3) 0.0855(14) Uani 1 d . . H86 H -0.1773(3) 0.2569(4) -0.3785(3) 0.103 Uiso 1 calc R . C91 C 0.4437(3) -0.1964(3) -0.3086(3) 0.0875(15) Uani 1 d . . H91 H 0.4851(3) -0.2157(3) -0.3394(3) 0.105 Uiso 1 calc R . C92 C 0.3552(3) -0.1947(3) -0.3145(3) 0.0818(13) Uani 1 d . . H92 H 0.3355(3) -0.2140(3) -0.3500(3) 0.098 Uiso 1 calc R . C93 C 0.2958(3) -0.1657(3) -0.2702(2) 0.0737(12) Uani 1 d . . H93 H 0.2361(3) -0.1665(3) -0.2749(2) 0.088 Uiso 1 calc R . C94 C 0.3213(3) -0.1361(3) -0.2201(2) 0.0717(11) Uani 1 d . . H94 H 0.2793(3) -0.1142(3) -0.1907(2) 0.086 Uiso 1 calc R . C95 C 0.4065(3) -0.1376(3) -0.2115(2) 0.0733(12) Uani 1 d . . H95 H 0.4237(3) -0.1175(3) -0.1755(2) 0.088 Uiso 1 calc R . C96 C 0.4686(3) -0.1672(2) -0.2534(2) 0.0713(12) Uani 1 d . . H96 H 0.5283(3) -0.1685(2) -0.2459(2) 0.086 Uiso 1 calc R . C01 C -0.5831(7) 0.6546(9) -0.5050(7) 0.232(6) Uani 1 d . . H01 H -0.6426(7) 0.6787(9) -0.5184(7) 0.278 Uiso 1 calc R . C02 C -0.5265(7) 0.6341(7) -0.5441(4) 0.177(4) Uani 1 d . . H02 H -0.5435(7) 0.6430(7) -0.5888(4) 0.213 Uiso 1 calc R . C03 C -0.4312(8) 0.5955(8) -0.5248(5) 0.207(5) Uani 1 d . . H03 H -0.3899(8) 0.5756(8) -0.5554(5) 0.248 Uiso 1 calc R . C04 C -0.4070(5) 0.5904(5) -0.4609(5) 0.152(3) Uani 1 d . . H04 H -0.3473(5) 0.5706(5) -0.4470(5) 0.182 Uiso 1 calc R . C05 C -0.4723(6) 0.6150(7) -0.4162(5) 0.177(4) Uani 1 d . . H05 H -0.4541(6) 0.6134(7) -0.3728(5) 0.213 Uiso 1 calc R . C06 C -0.5514(6) 0.6385(9) -0.4302(8) 0.242(7) Uani 1 d . . H06 H -0.5930(6) 0.6468(9) -0.3970(8) 0.290 Uiso 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 Ti1 0.0197(2) 0.0180(2) 0.0134(2) -0.00606(14) 0.00041(13) -0.00561(14) Ti2 0.0235(2) 0.0211(2) 0.0147(2) -0.00829(14) 0.00343(14) -0.0094(2) O 0.0251(8) 0.0221(8) 0.0160(7) -0.0077(6) 0.0011(6) -0.0090(6) O1 0.0198(7) 0.0275(8) 0.0194(8) -0.0113(6) 0.0010(6) -0.0060(6) O2 0.0229(8) 0.0234(8) 0.0191(8) -0.0084(6) 0.0015(6) -0.0102(6) O3 0.0310(8) 0.0188(7) 0.0170(8) -0.0062(6) -0.0006(6) -0.0032(6) O4 0.0290(8) 0.0252(8) 0.0244(8) -0.0133(7) 0.0038(7) -0.0092(7) O5 0.0299(8) 0.0272(8) 0.0174(8) -0.0087(6) -0.0024(6) -0.0105(7) O6 0.0344(9) 0.0302(9) 0.0226(8) -0.0124(7) 0.0106(7) -0.0201(7) N1 0.0183(8) 0.0181(9) 0.0146(8) -0.0037(7) -0.0001(6) -0.0044(7) N2 0.0265(10) 0.0267(10) 0.0200(9) -0.0107(8) 0.0042(7) -0.0102(8) C10 0.0198(10) 0.0178(10) 0.0190(10) -0.0067(8) -0.0010(8) -0.0041(8) C11 0.0205(10) 0.0230(11) 0.0164(10) -0.0075(8) 0.0017(8) -0.0043(8) C12 0.0204(10) 0.0176(10) 0.0172(10) -0.0033(8) -0.0014(8) -0.0034(8) C13 0.0236(11) 0.0211(11) 0.0188(10) -0.0060(8) -0.0026(8) -0.0028(8) C14 0.0227(11) 0.0261(11) 0.0201(11) -0.0079(9) 0.0018(8) 0.0016(9) C15 0.0184(11) 0.0354(13) 0.0279(12) -0.0106(10) -0.0008(9) -0.0028(9) C16 0.0223(11) 0.0311(12) 0.0230(11) -0.0094(9) -0.0005(9) -0.0053(9) C100 0.0277(12) 0.0295(13) 0.0300(13) -0.0134(10) 0.0014(10) 0.0025(10) C101 0.097(4) 0.032(2) 0.067(4) -0.015(2) 0.038(3) 0.004(3) C102 0.053(3) 0.064(3) 0.036(3) -0.030(2) -0.006(2) 0.021(3) C103 0.030(3) 0.102(6) 0.087(5) -0.071(5) 0.011(2) -0.006(3) C104 0.097(4) 0.032(2) 0.067(4) -0.015(2) 0.038(3) 0.004(3) C105 0.053(3) 0.064(3) 0.036(3) -0.030(2) -0.006(2) 0.021(3) C106 0.030(3) 0.102(6) 0.087(5) -0.071(5) 0.011(2) -0.006(3) C110 0.0200(12) 0.066(2) 0.050(2) -0.040(2) -0.0018(11) -0.0070(12) C111 0.045(2) 0.170(5) 0.143(4) -0.131(4) 0.056(2) -0.067(3) C112 0.074(3) 0.083(3) 0.083(3) -0.055(2) -0.059(2) 0.038(2) C113 0.0255(12) 0.051(2) 0.0330(14) -0.0232(12) 0.0016(10) -0.0127(11) C20 0.0186(10) 0.0227(11) 0.0184(10) -0.0073(8) -0.0026(8) -0.0033(8) C21 0.0187(10) 0.0200(10) 0.0214(11) -0.0088(8) 0.0016(8) -0.0038(8) C22 0.0165(10) 0.0209(10) 0.0204(11) -0.0097(8) 0.0013(8) -0.0018(8) C23 0.0194(10) 0.0242(11) 0.0246(11) -0.0110(9) -0.0003(8) -0.0042(9) C24 0.0216(11) 0.0261(12) 0.0319(13) -0.0143(10) 0.0040(9) -0.0074(9) C25 0.0338(13) 0.0293(12) 0.0258(12) -0.0088(10) 0.0073(10) -0.0157(10) C26 0.0301(12) 0.0243(11) 0.0234(11) -0.0098(9) 0.0048(9) -0.0111(9) C200 0.0272(12) 0.0331(13) 0.0335(13) -0.0144(10) 0.0045(10) -0.0156(10) C201 0.059(3) 0.079(3) 0.069(3) 0.008(2) -0.028(2) -0.048(2) C202 0.047(2) 0.074(3) 0.051(2) -0.037(2) 0.023(2) -0.044(2) C203 0.045(2) 0.050(2) 0.071(3) -0.042(2) 0.022(2) -0.028(2) C204 0.059(3) 0.079(3) 0.069(3) 0.008(2) -0.028(2) -0.048(2) C205 0.047(2) 0.074(3) 0.051(2) -0.037(2) 0.023(2) -0.044(2) C206 0.045(2) 0.050(2) 0.071(3) -0.042(2) 0.022(2) -0.028(2) C210 0.054(2) 0.0338(14) 0.0207(12) -0.0068(10) 0.0035(11) -0.0260(12) C211 0.105(3) 0.070(2) 0.0245(15) -0.0077(14) 0.010(2) -0.065(2) C212 0.065(2) 0.038(2) 0.036(2) -0.0029(12) -0.0217(14) -0.0102(15) C213 0.056(2) 0.044(2) 0.0256(13) -0.0165(11) 0.0116(12) -0.0261(14) C30 0.0236(10) 0.0192(10) 0.0140(10) -0.0052(8) 0.0007(8) -0.0046(8) C31 0.0273(11) 0.0203(10) 0.0172(10) -0.0033(8) 0.0001(8) -0.0064(9) C32 0.0240(11) 0.0191(10) 0.0182(10) -0.0041(8) -0.0009(8) -0.0065(8) C33 0.0258(11) 0.0239(11) 0.0183(10) -0.0038(8) -0.0005(8) -0.0093(9) C34 0.0266(11) 0.0239(11) 0.0216(11) -0.0009(9) -0.0019(9) -0.0079(9) C35 0.0292(12) 0.0204(11) 0.0276(12) -0.0026(9) -0.0011(9) -0.0035(9) C36 0.0279(12) 0.0215(11) 0.0236(11) -0.0056(9) 0.0021(9) -0.0060(9) C300 0.0370(14) 0.0301(13) 0.0221(12) 0.0007(9) -0.0048(10) -0.0091(11) C301 0.060(2) 0.038(2) 0.0225(13) -0.0015(11) -0.0095(12) -0.0115(14) C302 0.052(2) 0.0377(15) 0.0278(14) 0.0056(11) -0.0007(12) -0.0184(13) C303 0.046(2) 0.047(2) 0.0303(15) 0.0054(12) -0.0098(12) -0.0032(14) C310 0.0319(13) 0.0215(11) 0.0278(12) -0.0068(9) 0.0051(10) -0.0017(10) C311 0.048(2) 0.0330(15) 0.037(2) -0.0045(12) 0.0076(13) 0.0104(13) C312 0.0434(15) 0.0264(12) 0.0338(14) -0.0149(10) 0.0106(11) -0.0095(11) C313 0.0312(13) 0.0311(13) 0.0305(13) -0.0103(10) 0.0061(10) -0.0058(10) C40 0.0387(13) 0.0242(12) 0.0244(12) -0.0089(9) 0.0073(10) -0.0153(10) C41 0.0293(12) 0.0239(11) 0.0188(11) -0.0092(9) 0.0010(9) -0.0028(9) C42 0.0362(13) 0.0229(11) 0.0178(11) -0.0082(9) 0.0019(9) -0.0077(10) C43 0.0427(14) 0.0260(12) 0.0222(12) -0.0094(9) 0.0023(10) -0.0084(11) C44 0.046(2) 0.0256(12) 0.0228(12) -0.0103(10) -0.0021(11) 0.0002(11) C45 0.0318(13) 0.0341(13) 0.0243(12) -0.0113(10) 0.0022(10) 0.0012(11) C46 0.0288(12) 0.0306(12) 0.0201(11) -0.0097(9) 0.0032(9) -0.0037(10) C400 0.056(2) 0.0292(14) 0.037(2) -0.0154(12) -0.0008(13) 0.0031(13) C401 0.133(4) 0.031(2) 0.074(3) -0.022(2) -0.052(3) 0.024(2) C402 0.081(3) 0.046(2) 0.101(3) -0.050(2) -0.035(2) 0.011(2) C403 0.145(5) 0.060(3) 0.132(5) -0.066(3) 0.080(4) -0.019(3) C410 0.0315(13) 0.0411(15) 0.0376(15) -0.0173(12) 0.0116(11) -0.0102(12) C411 0.037(2) 0.064(2) 0.055(2) -0.031(2) 0.0096(14) -0.0215(15) C412 0.045(2) 0.055(2) 0.063(2) -0.025(2) 0.028(2) -0.016(2) C413 0.049(2) 0.036(2) 0.044(2) -0.0108(12) 0.0184(13) -0.0163(13) C50 0.0310(12) 0.0322(13) 0.0205(11) -0.0141(9) 0.0022(9) -0.0109(10) C51 0.0223(11) 0.0343(13) 0.0169(10) -0.0112(9) 0.0000(8) -0.0085(9) C52 0.0253(11) 0.0329(13) 0.0204(11) -0.0118(9) 0.0025(9) -0.0099(10) C53 0.0250(11) 0.0399(14) 0.0256(12) -0.0175(10) 0.0004(9) -0.0119(10) C54 0.0268(12) 0.047(2) 0.0273(13) -0.0155(11) -0.0047(10) -0.0080(11) C55 0.0275(12) 0.0366(14) 0.0236(12) -0.0096(10) -0.0018(9) -0.0043(10) C56 0.0250(11) 0.0336(13) 0.0199(11) -0.0103(9) 0.0022(9) -0.0072(10) C500 0.0373(15) 0.055(2) 0.041(2) -0.0201(14) -0.0193(13) -0.0036(13) C501 0.114(6) 0.051(3) 0.092(5) -0.003(3) -0.084(5) -0.010(3) C502 0.025(2) 0.119(5) 0.062(3) -0.045(3) -0.005(2) -0.015(3) C503 0.046(4) 0.080(3) 0.027(3) -0.019(3) -0.010(2) -0.018(3) C504 0.114(6) 0.051(3) 0.092(5) -0.003(3) -0.084(5) -0.010(3) C505 0.025(2) 0.119(5) 0.062(3) -0.045(3) -0.005(2) -0.015(3) C506 0.046(4) 0.080(3) 0.027(3) -0.019(3) -0.010(2) -0.018(3) C510 0.0326(13) 0.0304(12) 0.0194(11) -0.0066(9) 0.0003(9) -0.0091(10) C511 0.044(2) 0.0360(15) 0.0295(14) -0.0018(11) -0.0053(11) -0.0124(12) C512 0.0335(13) 0.0385(14) 0.0266(13) -0.0066(10) -0.0011(10) -0.0161(11) C513 0.050(2) 0.0292(13) 0.0249(13) -0.0103(10) 0.0026(11) -0.0121(12) C60 0.0278(12) 0.0354(13) 0.0299(13) -0.0171(10) 0.0071(10) -0.0157(10) C61 0.0319(12) 0.0250(12) 0.0292(12) -0.0133(9) 0.0142(10) -0.0134(10) C62 0.0305(12) 0.0276(12) 0.0331(13) -0.0148(10) 0.0118(10) -0.0130(10) C63 0.0309(13) 0.0303(13) 0.043(2) -0.0197(11) 0.0127(11) -0.0147(11) C64 0.0380(14) 0.0230(12) 0.048(2) -0.0169(11) 0.0197(12) -0.0136(11) C65 0.0422(15) 0.0245(12) 0.0370(14) -0.0127(10) 0.0226(12) -0.0136(11) C66 0.0405(14) 0.0239(12) 0.0276(13) -0.0117(9) 0.0146(10) -0.0129(10) C600 0.0377(15) 0.0279(13) 0.056(2) -0.0147(12) 0.0222(13) -0.0165(11) C601 0.039(2) 0.030(2) 0.084(3) 0.002(2) 0.008(2) -0.0141(15) C602 0.035(2) 0.037(2) 0.052(2) -0.017(2) 0.018(2) -0.0133(14) C603 0.046(2) 0.055(2) 0.060(2) -0.020(2) 0.011(2) -0.034(2) C604 0.039(2) 0.030(2) 0.084(3) 0.002(2) 0.008(2) -0.0141(15) C605 0.035(2) 0.037(2) 0.052(2) -0.017(2) 0.018(2) -0.0133(14) C606 0.046(2) 0.055(2) 0.060(2) -0.020(2) 0.011(2) -0.034(2) C610 0.048(2) 0.0288(13) 0.0237(12) -0.0087(10) 0.0148(11) -0.0167(11) C611 0.081(2) 0.039(2) 0.0211(13) -0.0104(11) 0.0094(13) -0.036(2) C612 0.043(2) 0.050(2) 0.035(2) -0.0138(13) 0.0135(12) -0.0179(14) C613 0.055(2) 0.0338(14) 0.0255(13) -0.0047(11) 0.0165(12) -0.0129(13) C71 0.142(6) 0.261(10) 0.062(4) -0.021(5) -0.009(4) -0.060(7) C72 0.094(4) 0.240(9) 0.087(4) -0.071(5) 0.022(3) -0.048(5) C73 0.067(3) 0.088(3) 0.093(4) -0.036(3) 0.012(2) -0.041(2) C74 0.075(3) 0.052(2) 0.079(3) -0.014(2) 0.009(2) -0.034(2) C75 0.072(3) 0.044(2) 0.102(4) -0.030(2) 0.003(2) -0.020(2) C76 0.092(4) 0.101(4) 0.099(4) -0.021(3) -0.016(3) -0.019(3) C81 0.084(3) 0.117(5) 0.090(4) -0.020(3) 0.007(3) -0.009(3) C82 0.076(3) 0.094(4) 0.092(4) -0.038(3) -0.008(3) -0.006(3) C83 0.061(2) 0.091(3) 0.089(3) -0.046(3) 0.009(2) -0.023(2) C84 0.071(3) 0.090(3) 0.079(3) -0.044(3) 0.010(2) -0.032(2) C85 0.073(3) 0.088(3) 0.082(3) -0.050(3) 0.007(2) -0.015(2) C86 0.066(3) 0.108(4) 0.082(3) -0.042(3) 0.010(2) -0.002(3) C91 0.075(3) 0.057(3) 0.120(4) -0.008(3) 0.006(3) -0.004(2) C92 0.082(3) 0.086(3) 0.085(3) -0.019(3) -0.017(3) -0.033(3) C93 0.062(2) 0.076(3) 0.081(3) -0.012(2) -0.011(2) -0.012(2) C94 0.068(3) 0.062(2) 0.088(3) -0.011(2) -0.006(2) -0.022(2) C95 0.060(2) 0.068(3) 0.089(3) -0.002(2) -0.004(2) -0.019(2) C96 0.056(2) 0.054(2) 0.106(4) -0.011(2) -0.013(2) -0.020(2) C01 0.133(8) 0.363(17) 0.216(12) -0.106(12) 0.084(9) -0.061(9) C02 0.145(8) 0.292(13) 0.124(7) -0.070(7) 0.037(6) -0.087(8) C03 0.185(10) 0.322(15) 0.149(9) -0.121(10) 0.064(8) -0.075(10) C04 0.108(5) 0.145(7) 0.216(10) -0.081(7) 0.014(6) -0.021(5) C05 0.105(5) 0.288(12) 0.170(8) -0.138(8) -0.019(6) -0.030(7) C06 0.114(7) 0.384(17) 0.337(17) -0.278(15) 0.096(9) -0.113(9) _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 O 1.8250(15) . ? Ti1 O2 1.829(2) . ? Ti1 O3 1.850(2) . ? Ti1 O1 1.852(2) . ? Ti1 N1 2.275(2) . ? Ti2 O 1.8254(15) . ? Ti2 O4 1.834(2) . ? Ti2 O5 1.839(2) . ? Ti2 O6 1.869(2) . ? Ti2 N2 2.289(2) . ? O1 C11 1.359(2) . ? O2 C21 1.361(2) . ? O3 C31 1.355(3) . ? O4 C41 1.360(3) . ? O5 C51 1.361(3) . ? O6 C61 1.368(3) . ? N1 C10 1.491(3) . ? N1 C30 1.492(3) . ? N1 C20 1.495(3) . ? N2 C50 1.484(3) . ? N2 C60 1.485(3) . ? N2 C40 1.500(3) . ? C10 C12 1.497(3) . ? C11 C12 1.403(3) . ? C11 C16 1.411(3) . ? C12 C13 1.387(3) . ? C13 C14 1.396(3) . ? C14 C15 1.386(3) . ? C14 C100 1.532(3) . ? C15 C16 1.404(3) . ? C16 C110 1.539(3) . ? C100 C105 1.456(11) . ? C100 C106 1.48(2) . ? C100 C101 1.521(6) . ? C100 C103 1.526(6) . ? C100 C102 1.555(5) . ? C100 C104 1.593(12) . ? C110 C112 1.528(5) . ? C110 C113 1.529(4) . ? C110 C111 1.539(5) . ? C20 C22 1.501(3) . ? C21 C22 1.397(3) . ? C21 C26 1.406(3) . ? C22 C23 1.398(3) . ? C23 C24 1.385(3) . ? C24 C25 1.390(3) . ? C24 C200 1.538(3) . ? C25 C26 1.407(3) . ? C26 C210 1.536(3) . ? C200 C205 1.374(4) . ? C200 C206 1.468(5) . ? C200 C202 1.515(4) . ? C200 C203 1.528(4) . ? C200 C204 1.537(5) . ? C200 C201 1.553(5) . ? C210 C212 1.539(4) . ? C210 C213 1.540(4) . ? C210 C211 1.542(4) . ? C30 C32 1.506(3) . ? C31 C32 1.396(3) . ? C31 C36 1.412(3) . ? C32 C33 1.389(3) . ? C33 C34 1.396(3) . ? C34 C35 1.395(3) . ? C34 C300 1.535(3) . ? C35 C36 1.396(3) . ? C36 C310 1.537(3) . ? C300 C302 1.535(4) . ? C300 C303 1.540(4) . ? C300 C301 1.544(4) . ? C310 C311 1.531(3) . ? C310 C312 1.540(4) . ? C310 C313 1.542(3) . ? C40 C42 1.515(3) . ? C41 C42 1.395(3) . ? C41 C46 1.403(3) . ? C42 C43 1.388(3) . ? C43 C44 1.395(4) . ? C44 C45 1.391(4) . ? C44 C400 1.531(4) . ? C45 C46 1.398(3) . ? C46 C410 1.537(4) . ? C400 C402 1.501(5) . ? C400 C401 1.523(5) . ? C400 C403 1.528(5) . ? C410 C411 1.530(4) . ? C410 C413 1.540(4) . ? C410 C412 1.544(4) . ? C50 C52 1.500(3) . ? C51 C56 1.398(3) . ? C51 C52 1.407(3) . ? C52 C53 1.395(3) . ? C53 C54 1.382(4) . ? C54 C55 1.393(4) . ? C54 C500 1.538(3) . ? C55 C56 1.402(3) . ? C56 C510 1.542(3) . ? C500 C506 1.44(2) . ? C500 C501 1.477(6) . ? C500 C505 1.481(14) . ? C500 C503 1.530(7) . ? C500 C502 1.597(6) . ? C500 C504 1.70(2) . ? C510 C511 1.535(3) . ? C510 C513 1.537(3) . ? C510 C512 1.540(3) . ? C60 C62 1.494(3) . ? C61 C62 1.398(3) . ? C61 C66 1.418(3) . ? C62 C63 1.395(3) . ? C63 C64 1.370(4) . ? C64 C65 1.403(4) . ? C64 C600 1.536(4) . ? C65 C66 1.405(3) . ? C66 C610 1.522(4) . ? C600 C606 1.31(2) . ? C600 C604 1.44(2) . ? C600 C601 1.485(5) . ? C600 C602 1.518(4) . ? C600 C603 1.587(5) . ? C600 C605 1.81(2) . ? C610 C612 1.532(4) . ? C610 C611 1.541(3) . ? C610 C613 1.550(3) . ? C71 C76 1.343(8) . ? C71 C72 1.416(9) . ? C72 C73 1.326(8) . ? C73 C74 1.357(6) . ? C74 C75 1.367(6) . ? C75 C76 1.322(7) . ? C81 C86 1.378(7) . ? C81 C82 1.430(7) . ? C82 C83 1.383(7) . ? C83 C84 1.371(6) . ? C84 C85 1.382(6) . ? C85 C86 1.364(7) . ? C91 C92 1.394(6) . ? C91 C96 1.432(7) . ? C92 C93 1.374(6) . ? C93 C94 1.347(6) . ? C94 C95 1.351(5) . ? C95 C96 1.366(6) . ? C01 C02 1.229(10) . ? C01 C06 1.60(2) . ? C02 C03 1.510(13) . ? C03 C04 1.376(12) . ? C04 C05 1.415(10) . ? C05 C06 1.234(10) . ? 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 O Ti1 O2 103.06(7) . . ? O Ti1 O3 96.09(7) . . ? O2 Ti1 O3 111.91(7) . . ? O Ti1 O1 97.65(7) . . ? O2 Ti1 O1 114.31(7) . . ? O3 Ti1 O1 126.89(7) . . ? O Ti1 N1 174.19(7) . . ? O2 Ti1 N1 82.34(6) . . ? O3 Ti1 N1 79.73(6) . . ? O1 Ti1 N1 81.87(6) . . ? O Ti2 O4 100.19(7) . . ? O Ti2 O5 97.39(7) . . ? O4 Ti2 O5 108.52(7) . . ? O Ti2 O6 97.70(7) . . ? O4 Ti2 O6 117.96(8) . . ? O5 Ti2 O6 127.20(8) . . ? O Ti2 N2 178.15(7) . . ? O4 Ti2 N2 81.46(7) . . ? O5 Ti2 N2 82.82(7) . . ? O6 Ti2 N2 80.75(7) . . ? Ti1 O Ti2 155.54(9) . . ? C11 O1 Ti1 144.26(14) . . ? C21 O2 Ti1 143.51(14) . . ? C31 O3 Ti1 143.31(14) . . ? C41 O4 Ti2 141.7(2) . . ? C51 O5 Ti2 144.37(15) . . ? C61 O6 Ti2 144.21(15) . . ? C10 N1 C30 110.0(2) . . ? C10 N1 C20 109.1(2) . . ? C30 N1 C20 110.2(2) . . ? C10 N1 Ti1 109.49(12) . . ? C30 N1 Ti1 108.53(12) . . ? C20 N1 Ti1 109.54(12) . . ? C50 N2 C60 107.2(2) . . ? C50 N2 C40 109.9(2) . . ? C60 N2 C40 110.6(2) . . ? C50 N2 Ti2 112.23(14) . . ? C60 N2 Ti2 108.91(13) . . ? C40 N2 Ti2 108.02(14) . . ? N1 C10 C12 113.9(2) . . ? O1 C11 C12 117.2(2) . . ? O1 C11 C16 123.1(2) . . ? C12 C11 C16 119.7(2) . . ? C13 C12 C11 121.1(2) . . ? C13 C12 C10 119.1(2) . . ? C11 C12 C10 119.7(2) . . ? C12 C13 C14 121.0(2) . . ? C15 C14 C13 116.7(2) . . ? C15 C14 C100 122.3(2) . . ? C13 C14 C100 121.0(2) . . ? C14 C15 C16 125.0(2) . . ? C15 C16 C11 116.5(2) . . ? C15 C16 C110 116.4(2) . . ? C11 C16 C110 126.9(2) . . ? C105 C100 C106 113.6(7) . . ? C101 C100 C103 112.1(4) . . ? C105 C100 C14 113.6(4) . . ? C106 C100 C14 109.5(5) . . ? C101 C100 C14 108.7(3) . . ? C103 C100 C14 113.5(3) . . ? C101 C100 C102 107.2(4) . . ? C103 C100 C102 105.7(4) . . ? C14 C100 C102 109.5(2) . . ? C105 C100 C104 109.3(7) . . ? C106 C100 C104 103.8(7) . . ? C14 C100 C104 106.3(4) . . ? C112 C110 C113 107.7(3) . . ? C112 C110 C16 107.2(3) . . ? C113 C110 C16 115.7(2) . . ? C112 C110 C111 111.0(3) . . ? C113 C110 C111 105.9(3) . . ? C16 C110 C111 109.3(3) . . ? N1 C20 C22 113.4(2) . . ? O2 C21 C22 118.4(2) . . ? O2 C21 C26 120.7(2) . . ? C22 C21 C26 120.9(2) . . ? C21 C22 C23 120.0(2) . . ? C21 C22 C20 120.9(2) . . ? C23 C22 C20 119.0(2) . . ? C24 C23 C22 121.2(2) . . ? C23 C24 C25 117.3(2) . . ? C23 C24 C200 120.3(2) . . ? C25 C24 C200 122.3(2) . . ? C24 C25 C26 124.2(2) . . ? C21 C26 C25 116.4(2) . . ? C21 C26 C210 121.0(2) . . ? C25 C26 C210 122.5(2) . . ? C205 C200 C206 107.6(3) . . ? C202 C200 C203 107.9(3) . . ? C205 C200 C204 114.0(3) . . ? C206 C200 C204 117.4(2) . . ? C205 C200 C24 99.4(2) . . ? C206 C200 C24 107.4(2) . . ? C202 C200 C24 113.4(2) . . ? C203 C200 C24 108.5(2) . . ? C204 C200 C24 109.3(2) . . ? C202 C200 C201 107.7(3) . . ? C203 C200 C201 107.7(3) . . ? C24 C200 C201 111.4(2) . . ? C26 C210 C212 108.1(2) . . ? C26 C210 C213 112.4(2) . . ? C212 C210 C213 109.5(2) . . ? C26 C210 C211 111.7(2) . . ? C212 C210 C211 109.3(3) . . ? C213 C210 C211 105.8(2) . . ? N1 C30 C32 113.0(2) . . ? O3 C31 C32 118.7(2) . . ? O3 C31 C36 120.9(2) . . ? C32 C31 C36 120.3(2) . . ? C33 C32 C31 120.2(2) . . ? C33 C32 C30 120.4(2) . . ? C31 C32 C30 119.4(2) . . ? C32 C33 C34 121.1(2) . . ? C35 C34 C33 116.9(2) . . ? C35 C34 C300 120.9(2) . . ? C33 C34 C300 122.2(2) . . ? C34 C35 C36 124.2(2) . . ? C35 C36 C31 116.4(2) . . ? C35 C36 C310 122.0(2) . . ? C31 C36 C310 121.5(2) . . ? C34 C300 C302 108.0(2) . . ? C34 C300 C303 111.8(2) . . ? C302 C300 C303 108.3(2) . . ? C34 C300 C301 111.3(2) . . ? C302 C300 C301 109.3(2) . . ? C303 C300 C301 108.1(2) . . ? C311 C310 C36 111.3(2) . . ? C311 C310 C312 108.1(2) . . ? C36 C310 C312 112.0(2) . . ? C311 C310 C313 106.7(2) . . ? C36 C310 C313 108.5(2) . . ? C312 C310 C313 110.0(2) . . ? N2 C40 C42 111.3(2) . . ? O4 C41 C42 118.3(2) . . ? O4 C41 C46 120.8(2) . . ? C42 C41 C46 120.9(2) . . ? C43 C42 C41 119.9(2) . . ? C43 C42 C40 120.4(2) . . ? C41 C42 C40 119.6(2) . . ? C42 C43 C44 121.2(2) . . ? C45 C44 C43 116.8(2) . . ? C45 C44 C400 122.3(2) . . ? C43 C44 C400 120.8(3) . . ? C44 C45 C46 124.3(2) . . ? C45 C46 C41 116.3(2) . . ? C45 C46 C410 122.4(2) . . ? C41 C46 C410 121.2(2) . . ? C402 C400 C401 110.6(3) . . ? C402 C400 C403 107.1(3) . . ? C401 C400 C403 107.0(4) . . ? C402 C400 C44 112.6(2) . . ? C401 C400 C44 107.2(2) . . ? C403 C400 C44 112.1(3) . . ? C411 C410 C46 111.3(2) . . ? C411 C410 C413 110.1(2) . . ? C46 C410 C413 109.1(2) . . ? C411 C410 C412 108.0(2) . . ? C46 C410 C412 111.4(2) . . ? C413 C410 C412 106.9(2) . . ? N2 C50 C52 114.1(2) . . ? O5 C51 C56 121.1(2) . . ? O5 C51 C52 117.9(2) . . ? C56 C51 C52 121.0(2) . . ? C53 C52 C51 119.1(2) . . ? C53 C52 C50 120.5(2) . . ? C51 C52 C50 120.2(2) . . ? C54 C53 C52 121.6(2) . . ? C53 C54 C55 117.4(2) . . ? C53 C54 C500 120.0(2) . . ? C55 C54 C500 122.7(3) . . ? C54 C55 C56 123.9(2) . . ? C51 C56 C55 116.5(2) . . ? C51 C56 C510 121.6(2) . . ? C55 C56 C510 121.7(2) . . ? C506 C500 C505 120.3(10) . . ? C501 C500 C503 111.0(4) . . ? C506 C500 C54 115.2(8) . . ? C501 C500 C54 113.5(3) . . ? C505 C500 C54 110.8(6) . . ? C503 C500 C54 109.5(3) . . ? C501 C500 C502 108.7(4) . . ? C503 C500 C502 107.0(3) . . ? C54 C500 C502 106.9(3) . . ? C506 C500 C504 98.6(10) . . ? C505 C500 C504 103.6(11) . . ? C54 C500 C504 105.5(6) . . ? C511 C510 C513 107.8(2) . . ? C511 C510 C512 108.1(2) . . ? C513 C510 C512 109.2(2) . . ? C511 C510 C56 111.9(2) . . ? C513 C510 C56 110.9(2) . . ? C512 C510 C56 108.8(2) . . ? N2 C60 C62 114.9(2) . . ? O6 C61 C62 117.8(2) . . ? O6 C61 C66 122.2(2) . . ? C62 C61 C66 120.0(2) . . ? C63 C62 C61 120.8(2) . . ? C63 C62 C60 118.7(2) . . ? C61 C62 C60 120.4(2) . . ? C64 C63 C62 121.5(2) . . ? C63 C64 C65 116.8(2) . . ? C63 C64 C600 122.7(3) . . ? C65 C64 C600 120.5(2) . . ? C64 C65 C66 124.7(2) . . ? C65 C66 C61 116.0(2) . . ? C65 C66 C610 120.6(2) . . ? C61 C66 C610 123.3(2) . . ? C606 C600 C604 122.5(12) . . ? C601 C600 C602 111.8(3) . . ? C606 C600 C64 108.2(8) . . ? C604 C600 C64 110.1(8) . . ? C601 C600 C64 110.7(3) . . ? C602 C600 C64 110.1(2) . . ? C601 C600 C603 107.5(3) . . ? C602 C600 C603 105.1(3) . . ? C64 C600 C603 111.6(2) . . ? C606 C600 C605 108.3(12) . . ? C604 C600 C605 100.0(11) . . ? C64 C600 C605 106.4(6) . . ? C66 C610 C612 108.6(2) . . ? C66 C610 C611 112.3(2) . . ? C612 C610 C611 109.3(2) . . ? C66 C610 C613 112.7(2) . . ? C612 C610 C613 108.2(2) . . ? C611 C610 C613 105.6(2) . . ? C76 C71 C72 120.9(6) . . ? C73 C72 C71 118.0(6) . . ? C72 C73 C74 120.6(5) . . ? C73 C74 C75 120.2(5) . . ? C76 C75 C74 120.8(5) . . ? C75 C76 C71 119.4(6) . . ? C86 C81 C82 118.3(5) . . ? C83 C82 C81 118.4(5) . . ? C84 C83 C82 122.3(4) . . ? C83 C84 C85 118.5(5) . . ? C86 C85 C84 121.0(5) . . ? C85 C86 C81 121.5(5) . . ? C92 C91 C96 115.9(5) . . ? C93 C92 C91 121.6(5) . . ? C94 C93 C92 120.7(4) . . ? C93 C94 C95 120.1(5) . . ? C94 C95 C96 121.6(5) . . ? C95 C96 C91 120.0(4) . . ? C02 C01 C06 116.6(10) . . ? C01 C02 C03 123.5(10) . . ? C04 C03 C02 116.9(8) . . ? C03 C04 C05 119.2(8) . . ? C06 C05 C04 124.1(10) . . ? C05 C06 C01 119.1(10) . . ? _refine_diff_density_max 0.589 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.067 #===END data_tiome _database_code_depnum_ccdc_archive 'CCDC 225002' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ; (Methoxy)(nitrilotris(4,6-di-tert -butyl-o- phenolate))titanium(IV) ; _chemical_formula_moiety Ti(OCH3)(N(CH2[C6H2(tBu)2O])3 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H69 N O4 Ti' _chemical_formula_weight 747.92 _chemical_melting_point ? _chemical_compound_source ? 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.7727(7) _cell_length_b 11.7884(6) _cell_length_c 26.8649(13) _cell_angle_alpha 90.00 _cell_angle_beta 93.7760(10) _cell_angle_gamma 90.00 _cell_volume 4352.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9830 _cell_measurement_theta_min 2.191 _cell_measurement_theta_max 28.2765 _exptl_crystal_description 'hexag prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method ? _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type 'empirical using SADABS' _exptl_absorpt_correction_T_min 0.487316 _exptl_absorpt_correction_T_max 1.00000 _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 'Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 45761 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10792 _reflns_number_observed 10214 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The molecule is disordered over two unequally populated orientations which differ in the helical twist of the aminetris(phenoxide) ligand. This disorder affects only the core of the molecule, with the outer parts of the benzene rings and the tert-butyl groups superimposable in the two orientations. The major orientation (C10-C14, C20-C24, C30-C34, and O1-O3) refined to 71.37(9)% occupancy, with the atoms in the minor orientation (C40-C44, C50-C54, C60-C64, and O4-O6 respectively) being given the same thermal parameters as the corresponding atoms in the major orientation. One tert-butyl group was also modeled as disordered between two orientations. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+6.3514P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10792 _refine_ls_number_parameters 537 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_obs 0.0604 _refine_ls_wR_factor_all 0.1283 _refine_ls_wR_factor_obs 0.1268 _refine_ls_goodness_of_fit_all 1.170 _refine_ls_goodness_of_fit_obs 1.190 _refine_ls_restrained_S_all 1.170 _refine_ls_restrained_S_obs 1.190 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti Ti 0.62820(2) 0.86825(3) 0.180500(12) 0.00807(8) Uani 1 d . . O O 0.70473(9) 0.95689(11) 0.22029(5) 0.0139(3) Uani 1 d . . N N 0.52978(10) 0.75056(12) 0.13048(6) 0.0108(3) Uani 1 d . . C C 0.7775(2) 0.9776(2) 0.25774(10) 0.0305(5) Uani 1 d . . H1 H 0.7678(23) 0.9371(29) 0.2865(12) 0.047(9) Uiso 1 d . . H2 H 0.8399(26) 0.9509(30) 0.2485(13) 0.057(10) Uiso 1 d . . H3 H 0.7788(26) 1.0605(34) 0.2665(13) 0.065(11) Uiso 1 d . . O1 O 0.72216(12) 0.81877(15) 0.14105(6) 0.0095(3) Uani 0.7137(9) d P 1 C10 C 0.5606(2) 0.7534(2) 0.08025(9) 0.0095(4) Uani 0.7137(9) d P 1 H10A H 0.5626(2) 0.8333(2) 0.06897(9) 0.011 Uiso 0.7137(9) calc PR 1 H10B H 0.5120(2) 0.7130(2) 0.05801(9) 0.011 Uiso 0.7137(9) calc PR 1 C11 C 0.7380(2) 0.7375(2) 0.10656(9) 0.0082(4) Uani 0.7137(9) d P 1 C12 C 0.6592(2) 0.7003(2) 0.07541(8) 0.0079(4) Uani 0.7137(9) d P 1 C13 C 0.6721(2) 0.6144(2) 0.04068(9) 0.0095(4) Uani 0.7137(9) d P 1 H13 H 0.6177(2) 0.5877(2) 0.02041(9) 0.011 Uiso 0.7137(9) calc PR 1 C14 C 0.7637(4) 0.5670(3) 0.0353(2) 0.0103(7) Uani 0.7137(9) d P 1 C15 C 0.84328(13) 0.60582(15) 0.06750(7) 0.0127(3) Uani 1 d . . H15 H 0.90600(13) 0.57493(15) 0.06350(7) 0.015 Uiso 1 calc R 1 C16 C 0.83326(13) 0.6872(2) 0.10465(7) 0.0154(4) Uani 1 d . . O2 O 0.54250(12) 0.97684(14) 0.15685(6) 0.0099(3) Uani 0.7137(9) d P 1 C20 C 0.4276(2) 0.7877(2) 0.13426(10) 0.0086(5) Uani 0.7137(9) d P 1 H20A H 0.4138(2) 0.7923(2) 0.16991(10) 0.010 Uiso 0.7137(9) calc PR 1 H20B H 0.3835(2) 0.7301(2) 0.11828(10) 0.010 Uiso 0.7137(9) calc PR 1 C21 C 0.4645(2) 0.9943(2) 0.12389(9) 0.0080(4) Uani 0.7137(9) d P 1 C22 C 0.4066(2) 0.9005(2) 0.11015(9) 0.0087(4) Uani 0.7137(9) d P 1 C23 C 0.3248(2) 0.9132(2) 0.07724(9) 0.0109(4) Uani 0.7137(9) d P 1 H23 H 0.2869(2) 0.8485(2) 0.06772(9) 0.013 Uiso 0.7137(9) calc PR 1 C24 C 0.2978(2) 1.0194(2) 0.05805(10) 0.0096(5) Uani 0.7137(9) d P 1 C25 C 0.36074(14) 1.1120(2) 0.07069(7) 0.0151(4) Uani 1 d . . H25 H 0.34409(14) 1.1842(2) 0.05689(7) 0.018 Uiso 1 calc R 1 C26 C 0.4458(2) 1.1039(2) 0.10219(8) 0.0202(4) Uani 1 d . . O3 O 0.59757(12) 0.76447(14) 0.23151(6) 0.0094(3) Uani 0.7137(9) d P 1 C30 C 0.5366(2) 0.6304(2) 0.15132(9) 0.0088(4) Uani 0.7137(9) d P 1 H30A H 0.5034(2) 0.5778(2) 0.12701(9) 0.011 Uiso 0.7137(9) calc PR 1 H30B H 0.6059(2) 0.6079(2) 0.15538(9) 0.011 Uiso 0.7137(9) calc PR 1 C31 C 0.5274(2) 0.6870(2) 0.24020(9) 0.0077(4) Uani 0.7137(9) d P 1 C32 C 0.4919(2) 0.6183(2) 0.20072(9) 0.0081(4) Uani 0.7137(9) d P 1 C33 C 0.4144(2) 0.5446(2) 0.20639(9) 0.0094(4) Uani 0.7137(9) d P 1 H33 H 0.3908(2) 0.4989(2) 0.17910(9) 0.011 Uiso 0.7137(9) calc PR 1 C34 C 0.3713(2) 0.5373(3) 0.25167(14) 0.0106(6) Uani 0.7137(9) d P 1 C35 C 0.41112(13) 0.6029(2) 0.29013(7) 0.0127(3) Uani 1 d . . H35 H 0.38506(13) 0.5949(2) 0.32181(7) 0.015 Uiso 1 calc R 1 C36 C 0.48691(14) 0.6804(2) 0.28617(7) 0.0160(4) Uani 1 d . . O4 O 0.7214(3) 0.7641(4) 0.1613(2) 0.0095(3) Uani 0.2863(9) d P 2 C40 C 0.5659(4) 0.6338(5) 0.1236(2) 0.0095(4) Uani 0.2863(9) d P 2 H40A H 0.5182(4) 0.5925(5) 0.1011(2) 0.011 Uiso 0.2863(9) calc PR 2 H40B H 0.5693(4) 0.5946(5) 0.1562(2) 0.011 Uiso 0.2863(9) calc PR 2 C41 C 0.7414(4) 0.6891(5) 0.1249(2) 0.0082(4) Uani 0.2863(9) d P 2 C42 C 0.6640(4) 0.6266(5) 0.1024(2) 0.0079(4) Uani 0.2863(9) d P 2 C43 C 0.6794(4) 0.5554(5) 0.0619(2) 0.0095(4) Uani 0.2863(9) d P 2 H43 H 0.6259(4) 0.5149(5) 0.0464(2) 0.011 Uiso 0.2863(9) calc PR 2 C44 C 0.7696(12) 0.5427(11) 0.0442(5) 0.0103(7) Uani 0.2863(9) d P 2 O5 O 0.5846(3) 0.9795(4) 0.1294(2) 0.0099(3) Uani 0.2863(9) d P 2 C50 C 0.5211(5) 0.7983(5) 0.0718(2) 0.0086(5) Uani 0.2863(9) d P 2 H50A H 0.5870(5) 0.8083(5) 0.0598(2) 0.010 Uiso 0.2863(9) calc PR 2 H50B H 0.4858(5) 0.7422(5) 0.0499(2) 0.010 Uiso 0.2863(9) calc PR 2 C51 C 0.5056(4) 0.9995(5) 0.0975(2) 0.0080(4) Uani 0.2863(9) d P 2 C52 C 0.4681(4) 0.9089(5) 0.0691(2) 0.0087(4) Uani 0.2863(9) d P 2 C53 C 0.3799(4) 0.9198(5) 0.0411(2) 0.0109(4) Uani 0.2863(9) d P 2 H53 H 0.3548(4) 0.8571(5) 0.0221(2) 0.013 Uiso 0.2863(9) calc PR 2 C54 C 0.3275(5) 1.0213(6) 0.0406(3) 0.0096(5) Uani 0.2863(9) d P 2 O6 O 0.5466(3) 0.8213(4) 0.2236(2) 0.0094(3) Uani 0.2863(9) d P 2 C60 C 0.4278(6) 0.7511(6) 0.1425(3) 0.0088(4) Uani 0.2863(9) d P 2 H60A H 0.3876(6) 0.7084(6) 0.1170(3) 0.011 Uiso 0.2863(9) calc PR 2 H60B H 0.4031(6) 0.8299(6) 0.1434(3) 0.011 Uiso 0.2863(9) calc PR 2 C61 C 0.4833(4) 0.7371(5) 0.2329(2) 0.0077(4) Uani 0.2863(9) d P 2 C62 C 0.4231(4) 0.6958(5) 0.1930(2) 0.0081(4) Uani 0.2863(9) d P 2 C63 C 0.3572(4) 0.6092(5) 0.2000(2) 0.0094(4) Uani 0.2863(9) d P 2 H63 H 0.3176(4) 0.5821(5) 0.1722(2) 0.011 Uiso 0.2863(9) calc PR 2 C64 C 0.3475(7) 0.5609(9) 0.2470(4) 0.0106(6) Uani 0.2863(9) d P 2 C100 C 0.78368(14) 0.4747(2) -0.00338(7) 0.0163(4) Uani 1 d . . C110 C 0.92064(12) 0.73151(15) 0.13751(6) 0.0100(3) Uani 1 d . . C101 C 0.8331(2) 0.5358(2) -0.04542(9) 0.0306(5) Uani 1 d . . H10C H 0.7910(2) 0.5974(2) -0.05860(9) 0.046 Uiso 1 calc R . H10D H 0.8442(2) 0.4818(2) -0.07219(9) 0.046 Uiso 1 calc R . H10E H 0.8955(2) 0.5672(2) -0.03230(9) 0.046 Uiso 1 calc R . C102 C 0.6887(2) 0.4217(2) -0.02561(9) 0.0292(5) Uani 1 d . . H10F H 0.6453(2) 0.4818(2) -0.03898(9) 0.044 Uiso 1 calc R . H10G H 0.6571(2) 0.3801(2) 0.00044(9) 0.044 Uiso 1 calc R . H10H H 0.7032(2) 0.3694(2) -0.05250(9) 0.044 Uiso 1 calc R . C103 C 0.8495(2) 0.3787(2) 0.01708(9) 0.0303(5) Uani 1 d . . H10I H 0.9107(2) 0.4106(2) 0.03152(9) 0.045 Uiso 1 calc R . H10J H 0.8630(2) 0.3267(2) -0.01005(9) 0.045 Uiso 1 calc R . H10K H 0.8168(2) 0.3374(2) 0.04287(9) 0.045 Uiso 1 calc R . C111 C 0.92823(14) 0.8612(2) 0.13327(7) 0.0170(4) Uani 1 d . . H11A H 0.98421(14) 0.8881(2) 0.15443(7) 0.026 Uiso 1 calc R . H11B H 0.86863(14) 0.8961(2) 0.14416(7) 0.026 Uiso 1 calc R . H11C H 0.93668(14) 0.8821(2) 0.09851(7) 0.026 Uiso 1 calc R . C112 C 1.01669(13) 0.6809(2) 0.12183(8) 0.0192(4) Uani 1 d . . H11D H 1.07084(13) 0.7107(2) 0.14345(8) 0.029 Uiso 1 calc R . H11E H 1.02596(13) 0.7014(2) 0.08712(8) 0.029 Uiso 1 calc R . H11F H 1.01459(13) 0.5981(2) 0.12491(8) 0.029 Uiso 1 calc R . C113 C 0.9091(2) 0.6985(2) 0.19222(7) 0.0231(4) Uani 1 d . . H11G H 0.9649(2) 0.7269(2) 0.21309(7) 0.035 Uiso 1 calc R . H11H H 0.9059(2) 0.6157(2) 0.19503(7) 0.035 Uiso 1 calc R . H11I H 0.8490(2) 0.7318(2) 0.20338(7) 0.035 Uiso 1 calc R . C200 C 0.2108(2) 1.0278(2) 0.02084(8) 0.0216(4) Uani 1 d . . C201 C 0.1765(2) 1.1505(2) 0.01411(8) 0.0226(4) Uani 1 d . . H20C H 0.1671(2) 1.1840(2) 0.04683(8) 0.034 Uiso 1 calc R . H20D H 0.1149(2) 1.1520(2) -0.00628(8) 0.034 Uiso 1 calc R . H20E H 0.2256(2) 1.1941(2) -0.00254(8) 0.034 Uiso 1 calc R . C202 C 0.2254(2) 0.9754(2) -0.03026(9) 0.0310(5) Uani 1 d . . H20F H 0.2474(2) 0.8967(2) -0.02594(9) 0.046 Uiso 1 calc R . H20G H 0.2745(2) 1.0190(2) -0.04694(9) 0.046 Uiso 1 calc R . H20H H 0.1637(2) 0.9769(2) -0.05063(9) 0.046 Uiso 1 calc R . C203 C 0.1288(2) 0.9623(2) 0.04479(11) 0.0448(7) Uani 1 d . . H20I H 0.1482(2) 0.8829(2) 0.04968(11) 0.067 Uiso 1 calc R . H20J H 0.0692(2) 0.9660(2) 0.02279(11) 0.067 Uiso 1 calc R . H20K H 0.1169(2) 0.9964(2) 0.07709(11) 0.067 Uiso 1 calc R . C210 C 0.50597(13) 1.20800(15) 0.11844(7) 0.0127(3) Uani 1 d . . C211 C 0.6074(2) 1.1972(3) 0.09866(10) 0.0411(7) Uani 1 d . . H21A H 0.6466(2) 1.2636(3) 0.10891(10) 0.062 Uiso 1 calc R . H21B H 0.6015(2) 1.1926(3) 0.06217(10) 0.062 Uiso 1 calc R . H21C H 0.6391(2) 1.1284(3) 0.11227(10) 0.062 Uiso 1 calc R . C212 C 0.4596(2) 1.3172(2) 0.09705(10) 0.0297(5) Uani 1 d . . H21D H 0.4997(2) 1.3824(2) 0.10805(10) 0.045 Uiso 1 calc R . H21E H 0.3942(2) 1.3257(2) 0.10888(10) 0.045 Uiso 1 calc R . H21F H 0.4554(2) 1.3134(2) 0.06053(10) 0.045 Uiso 1 calc R . C213 C 0.5152(2) 1.2182(2) 0.17532(8) 0.0267(5) Uani 1 d . . H21G H 0.5540(2) 1.2854(2) 0.18486(8) 0.040 Uiso 1 calc R . H21H H 0.5473(2) 1.1504(2) 0.18963(8) 0.040 Uiso 1 calc R . H21I H 0.4503(2) 1.2255(2) 0.18789(8) 0.040 Uiso 1 calc R . C300 C 0.27879(13) 0.4641(2) 0.25760(7) 0.0161(4) Uani 1 d . . C310 C 0.53841(14) 0.7387(2) 0.33124(7) 0.0160(4) Uani 1 d . . C311 C 0.53270(15) 0.8683(2) 0.32759(8) 0.0197(4) Uani 1 d . . H31A H 0.46439(15) 0.8918(2) 0.32332(8) 0.030 Uiso 1 calc R . H31B H 0.56728(15) 0.8941(2) 0.29892(8) 0.030 Uiso 1 calc R . H31C H 0.56278(15) 0.9020(2) 0.35819(8) 0.030 Uiso 1 calc R . C312 C 0.6445(2) 0.7026(2) 0.33779(14) 0.0466(8) Uani 1 d . . H31D H 0.6760(2) 0.7411(2) 0.36691(14) 0.070 Uiso 1 calc R . H31E H 0.6778(2) 0.7232(2) 0.30793(14) 0.070 Uiso 1 calc R . H31F H 0.6483(2) 0.6204(2) 0.34276(14) 0.070 Uiso 1 calc R . C313 C 0.4914(2) 0.7056(3) 0.37972(9) 0.0513(9) Uani 1 d . . H31G H 0.4226(2) 0.7274(3) 0.37720(9) 0.077 Uiso 1 calc R . H31H H 0.5249(2) 0.7450(3) 0.40803(9) 0.077 Uiso 1 calc R . H31I H 0.4969(2) 0.6235(3) 0.38475(9) 0.077 Uiso 1 calc R . C301 C 0.2474(2) 0.3989(2) 0.20934(9) 0.0255(5) Uani 0.918(3) d P 1 H30C H 0.3026(2) 0.3550(2) 0.19847(9) 0.038 Uiso 0.918(3) calc PR 1 H30D H 0.2259(2) 0.4529(2) 0.18318(9) 0.038 Uiso 0.918(3) calc PR 1 H30E H 0.1938(2) 0.3474(2) 0.21576(9) 0.038 Uiso 0.918(3) calc PR 1 C302 C 0.1929(2) 0.5315(2) 0.27399(11) 0.0306(6) Uani 0.918(3) d P 1 H30F H 0.1745(2) 0.5890(2) 0.24875(11) 0.046 Uiso 0.918(3) calc PR 1 H30G H 0.2108(2) 0.5688(2) 0.30588(11) 0.046 Uiso 0.918(3) calc PR 1 H30H H 0.1378(2) 0.4804(2) 0.27793(11) 0.046 Uiso 0.918(3) calc PR 1 C303 C 0.3079(2) 0.3737(2) 0.29715(10) 0.0271(5) Uani 0.918(3) d P 1 H30I H 0.3635(2) 0.3301(2) 0.28646(10) 0.041 Uiso 0.918(3) calc PR 1 H30J H 0.2529(2) 0.3225(2) 0.30113(10) 0.041 Uiso 0.918(3) calc PR 1 H30K H 0.3260(2) 0.4109(2) 0.32906(10) 0.041 Uiso 0.918(3) calc PR 1 C304 C 0.2912(2) 0.3634(2) 0.23765(10) 0.0255(5) Uani 0.082(3) d PR 2 H30L H 0.2411(2) 0.3113(2) 0.24829(10) 0.038 Uiso 0.082(3) calc PR 2 H30M H 0.3557(2) 0.3342(2) 0.24863(10) 0.038 Uiso 0.082(3) calc PR 2 H30N H 0.2859(2) 0.3699(2) 0.20121(10) 0.038 Uiso 0.082(3) calc PR 2 C305 C 0.1940(2) 0.5433(2) 0.22815(10) 0.0306(6) Uani 0.082(3) d PR 2 H30O H 0.1896(2) 0.6163(2) 0.24534(10) 0.046 Uiso 0.082(3) calc PR 2 H30P H 0.1311(2) 0.5043(2) 0.22794(10) 0.046 Uiso 0.082(3) calc PR 2 H30Q H 0.2110(2) 0.5563(2) 0.19376(10) 0.046 Uiso 0.082(3) calc PR 2 C306 C 0.2415(2) 0.4832(2) 0.31205(10) 0.0271(5) Uani 0.082(3) d PR 2 H30R H 0.2379(2) 0.5647(2) 0.31890(10) 0.041 Uiso 0.082(3) calc PR 2 H30S H 0.2868(2) 0.4473(2) 0.33690(10) 0.041 Uiso 0.082(3) calc PR 2 H30T H 0.1768(2) 0.4494(2) 0.31375(10) 0.041 Uiso 0.082(3) calc PR 2 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 0.00561(13) 0.00500(14) 0.01356(15) -0.00228(11) 0.00018(10) -0.00082(10) O 0.0103(6) 0.0117(6) 0.0191(7) -0.0045(5) -0.0031(5) -0.0029(5) N 0.0084(7) 0.0062(6) 0.0179(7) -0.0009(6) 0.0023(5) 0.0008(5) C 0.0231(11) 0.0312(13) 0.0351(13) -0.0099(11) -0.0147(10) -0.0014(9) O1 0.0084(7) 0.0092(8) 0.0110(8) -0.0050(6) 0.0020(6) -0.0015(6) C10 0.0090(10) 0.0107(10) 0.0088(10) -0.0012(8) -0.0001(8) -0.0010(9) C11 0.0109(9) 0.0067(11) 0.0071(11) -0.0009(8) 0.0024(8) -0.0007(9) C12 0.0083(9) 0.0074(9) 0.0079(9) 0.0012(7) 0.0014(7) 0.0000(7) C13 0.0127(10) 0.0078(10) 0.0079(10) -0.0013(7) -0.0008(8) -0.0026(8) C14 0.0155(12) 0.007(2) 0.008(2) -0.0015(12) 0.0025(14) -0.001(2) C15 0.0149(8) 0.0101(8) 0.0134(8) -0.0032(6) 0.0034(6) -0.0002(6) C16 0.0100(8) 0.0184(9) 0.0181(9) -0.0094(7) 0.0043(7) -0.0049(7) O2 0.0104(8) 0.0071(7) 0.0118(8) -0.0009(6) -0.0037(5) 0.0010(6) C20 0.0070(10) 0.0072(11) 0.0115(11) -0.0001(9) 0.0001(8) -0.0005(9) C21 0.0080(10) 0.0084(10) 0.0077(10) -0.0004(8) 0.0007(7) 0.0010(8) C22 0.0091(9) 0.0070(10) 0.0101(10) 0.0006(8) 0.0016(8) 0.0009(8) C23 0.0122(10) 0.0086(10) 0.0118(10) -0.0007(8) 0.0000(8) -0.0006(8) C24 0.0082(13) 0.0098(9) 0.0105(13) 0.0003(10) -0.0006(8) 0.0016(9) C25 0.0194(9) 0.0078(8) 0.0171(9) 0.0005(7) -0.0075(7) 0.0023(7) C26 0.0250(10) 0.0070(8) 0.0265(10) -0.0037(7) -0.0142(8) 0.0024(7) O3 0.0101(7) 0.0089(7) 0.0089(7) 0.0012(6) -0.0006(6) -0.0040(5) C30 0.0103(10) 0.0045(10) 0.0115(11) -0.0002(8) 0.0001(8) -0.0005(8) C31 0.0060(10) 0.0059(10) 0.0111(10) 0.0003(8) -0.0001(8) 0.0002(7) C32 0.0078(9) 0.0063(9) 0.0100(10) 0.0014(8) -0.0001(7) 0.0019(8) C33 0.0087(9) 0.0081(9) 0.0113(10) -0.0006(8) -0.0014(8) -0.0005(7) C34 0.006(2) 0.011(2) 0.0147(12) 0.0032(12) -0.0002(13) 0.0006(11) C35 0.0116(8) 0.0122(8) 0.0149(8) 0.0003(7) 0.0044(6) 0.0001(6) C36 0.0177(9) 0.0163(9) 0.0147(9) -0.0067(7) 0.0057(7) -0.0067(7) O4 0.0084(7) 0.0092(8) 0.0110(8) -0.0050(6) 0.0020(6) -0.0015(6) C40 0.0090(10) 0.0107(10) 0.0088(10) -0.0012(8) -0.0001(8) -0.0010(9) C41 0.0109(9) 0.0067(11) 0.0071(11) -0.0009(8) 0.0024(8) -0.0007(9) C42 0.0083(9) 0.0074(9) 0.0079(9) 0.0012(7) 0.0014(7) 0.0000(7) C43 0.0127(10) 0.0078(10) 0.0079(10) -0.0013(7) -0.0008(8) -0.0026(8) C44 0.0155(12) 0.007(2) 0.008(2) -0.0015(12) 0.0025(14) -0.001(2) O5 0.0104(8) 0.0071(7) 0.0118(8) -0.0009(6) -0.0037(5) 0.0010(6) C50 0.0070(10) 0.0072(11) 0.0115(11) -0.0001(9) 0.0001(8) -0.0005(9) C51 0.0080(10) 0.0084(10) 0.0077(10) -0.0004(8) 0.0007(7) 0.0010(8) C52 0.0091(9) 0.0070(10) 0.0101(10) 0.0006(8) 0.0016(8) 0.0009(8) C53 0.0122(10) 0.0086(10) 0.0118(10) -0.0007(8) 0.0000(8) -0.0006(8) C54 0.0082(13) 0.0098(9) 0.0105(13) 0.0003(10) -0.0006(8) 0.0016(9) O6 0.0101(7) 0.0089(7) 0.0089(7) 0.0012(6) -0.0006(6) -0.0040(5) C60 0.0103(10) 0.0045(10) 0.0115(11) -0.0002(8) 0.0001(8) -0.0005(8) C61 0.0060(10) 0.0059(10) 0.0111(10) 0.0003(8) -0.0001(8) 0.0002(7) C62 0.0078(9) 0.0063(9) 0.0100(10) 0.0014(8) -0.0001(7) 0.0019(8) C63 0.0087(9) 0.0081(9) 0.0113(10) -0.0006(8) -0.0014(8) -0.0005(7) C64 0.006(2) 0.011(2) 0.0147(12) 0.0032(12) -0.0002(13) 0.0006(11) C100 0.0225(9) 0.0135(9) 0.0129(8) -0.0076(7) 0.0017(7) 0.0001(7) C110 0.0087(7) 0.0102(8) 0.0113(8) -0.0017(6) 0.0015(6) -0.0004(6) C101 0.0453(14) 0.0243(11) 0.0239(11) -0.0037(9) 0.0149(10) 0.0024(10) C102 0.0332(12) 0.0255(11) 0.0283(12) -0.0184(9) -0.0034(9) -0.0035(9) C103 0.0460(14) 0.0174(10) 0.0262(11) -0.0069(9) -0.0091(10) 0.0073(10) C111 0.0187(9) 0.0116(8) 0.0202(9) -0.0021(7) -0.0037(7) -0.0025(7) C112 0.0106(8) 0.0245(10) 0.0221(10) -0.0086(8) -0.0008(7) 0.0035(7) C113 0.0397(12) 0.0174(10) 0.0126(9) -0.0007(7) 0.0050(8) -0.0050(9) C200 0.0255(10) 0.0118(9) 0.0250(10) 0.0024(8) -0.0159(8) -0.0016(8) C201 0.0211(10) 0.0165(10) 0.0287(11) 0.0035(8) -0.0103(8) 0.0014(8) C202 0.0379(13) 0.0252(12) 0.0288(12) -0.0018(9) -0.0057(10) 0.0059(10) C203 0.066(2) 0.0261(13) 0.043(2) 0.0051(11) 0.0045(14) -0.0154(13) C210 0.0146(8) 0.0074(8) 0.0156(8) 0.0003(6) -0.0023(7) -0.0018(6) C211 0.0159(10) 0.071(2) 0.0374(14) 0.0176(14) 0.0058(10) 0.0008(12) C212 0.0321(12) 0.0082(9) 0.0459(14) 0.0042(9) -0.0192(10) -0.0047(8) C213 0.0325(12) 0.0288(11) 0.0177(10) -0.0079(9) -0.0058(8) 0.0033(9) C300 0.0118(8) 0.0172(9) 0.0194(9) 0.0010(7) 0.0031(7) -0.0072(7) C310 0.0157(9) 0.0135(9) 0.0182(9) 0.0011(7) -0.0041(7) -0.0026(7) C311 0.0227(10) 0.0135(9) 0.0222(10) -0.0074(8) -0.0029(8) 0.0006(7) C312 0.0214(12) 0.0225(12) 0.093(2) -0.0061(14) -0.0158(13) 0.0019(10) C313 0.076(2) 0.061(2) 0.0152(11) 0.0075(11) -0.0117(12) -0.049(2) C301 0.0232(11) 0.0278(12) 0.0258(12) -0.0049(10) 0.0037(9) -0.0164(10) C302 0.0256(12) 0.0239(12) 0.044(2) 0.0017(11) 0.0139(11) 0.0034(10) C303 0.0189(11) 0.0277(12) 0.0340(13) 0.0081(10) -0.0036(9) -0.0099(9) C304 0.0232(11) 0.0278(12) 0.0258(12) -0.0049(10) 0.0037(9) -0.0164(10) C305 0.0256(12) 0.0239(12) 0.044(2) 0.0017(11) 0.0139(11) 0.0034(10) C306 0.0189(11) 0.0277(12) 0.0340(13) 0.0081(10) -0.0036(9) -0.0099(9) _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 O6 1.755(4) . ? Ti O 1.7880(13) . ? Ti O1 1.822(2) . ? Ti O2 1.827(2) . ? Ti O4 1.873(4) . ? Ti O3 1.905(2) . ? Ti O5 1.964(4) . ? Ti N 2.308(2) . ? O C 1.394(2) . ? N C10 1.441(3) . ? N C60 1.462(8) . ? N C40 1.480(6) . ? N C20 1.484(3) . ? N C30 1.524(3) . ? N C50 1.671(6) . ? O1 C11 1.361(3) . ? C10 C12 1.509(3) . ? C11 C12 1.396(3) . ? C11 C16 1.444(3) . ? C12 C13 1.397(3) . ? C13 C14 1.395(6) . ? C14 C15 1.426(6) . ? C14 C100 1.543(6) . ? C15 C44 1.38(2) . ? C15 C16 1.397(2) . ? C16 C41 1.410(6) . ? C16 C110 1.537(2) . ? O2 C21 1.363(3) . ? C20 C22 1.499(3) . ? C21 C22 1.398(3) . ? C21 C26 1.433(3) . ? C22 C23 1.393(3) . ? C23 C24 1.394(3) . ? C24 C25 1.421(3) . ? C24 C200 1.512(3) . ? C25 C54 1.400(7) . ? C25 C26 1.402(3) . ? C26 C51 1.491(6) . ? C26 C210 1.529(2) . ? O3 C31 1.361(3) . ? C30 C32 1.506(3) . ? C31 C36 1.390(3) . ? C31 C32 1.397(3) . ? C32 C33 1.392(3) . ? C33 C34 1.391(5) . ? C34 C35 1.375(4) . ? C34 C300 1.556(4) . ? C35 C36 1.397(2) . ? C35 C64 1.491(12) . ? C36 C310 1.526(3) . ? C36 C61 1.576(6) . ? O4 C41 1.360(7) . ? C40 C42 1.501(8) . ? C41 C42 1.400(8) . ? C42 C43 1.402(8) . ? C43 C44 1.37(2) . ? C44 C100 1.53(2) . ? O5 C51 1.361(7) . ? C50 C52 1.493(8) . ? C51 C52 1.392(8) . ? C52 C53 1.392(8) . ? C53 C54 1.398(9) . ? C54 C200 1.659(7) . ? O6 C61 1.356(7) . ? C60 C62 1.512(9) . ? C61 C62 1.399(8) . ? C62 C63 1.387(8) . ? C63 C64 1.398(13) . ? C64 C300 1.522(12) . ? C100 C103 1.529(3) . ? C100 C102 1.534(3) . ? C100 C101 1.536(3) . ? C110 C112 1.535(2) . ? C110 C111 1.537(2) . ? C110 C113 1.539(3) . ? C200 C201 1.529(3) . ? C200 C202 1.531(3) . ? C200 C203 1.544(3) . ? C210 C213 1.530(3) . ? C210 C212 1.532(3) . ? C210 C211 1.533(3) . ? C300 C304 1.318(3) . ? C300 C302 1.514(3) . ? C300 C303 1.540(3) . ? C300 C301 1.544(3) . ? C300 C306 1.598(3) . ? C300 C305 1.656(3) . ? C310 C312 1.521(3) . ? C310 C311 1.533(3) . ? C310 C313 1.542(3) . ? 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 O6 Ti O 99.62(14) . . ? O Ti O1 96.98(7) . . ? O Ti O2 98.07(7) . . ? O1 Ti O2 119.31(8) . . ? O6 Ti O4 117.1(2) . . ? O Ti O4 99.18(14) . . ? O Ti O3 95.46(7) . . ? O1 Ti O3 114.34(8) . . ? O2 Ti O3 122.12(8) . . ? O6 Ti O5 119.5(2) . . ? O Ti O5 99.72(13) . . ? O4 Ti O5 115.4(2) . . ? O6 Ti N 79.52(14) . . ? O Ti N 178.69(6) . . ? O1 Ti N 83.18(6) . . ? O2 Ti N 82.96(6) . . ? O4 Ti N 80.38(13) . . ? O3 Ti N 83.30(6) . . ? O5 Ti N 81.58(13) . . ? C O Ti 154.32(15) . . ? C60 N C40 111.6(4) . . ? C10 N C20 113.3(2) . . ? C10 N C30 110.6(2) . . ? C20 N C30 106.5(2) . . ? C60 N C50 101.3(4) . . ? C40 N C50 101.5(3) . . ? C10 N Ti 109.46(12) . . ? C60 N Ti 113.9(3) . . ? C40 N Ti 116.3(2) . . ? C20 N Ti 107.83(13) . . ? C30 N Ti 108.99(12) . . ? C50 N Ti 110.5(2) . . ? C11 O1 Ti 140.7(2) . . ? N C10 C12 113.1(2) . . ? O1 C11 C12 118.4(2) . . ? O1 C11 C16 120.0(2) . . ? C12 C11 C16 121.5(2) . . ? C11 C12 C13 120.0(2) . . ? C11 C12 C10 119.1(2) . . ? C13 C12 C10 120.9(2) . . ? C14 C13 C12 121.0(3) . . ? C13 C14 C15 118.3(4) . . ? C13 C14 C100 123.7(4) . . ? C15 C14 C100 118.1(4) . . ? C44 C15 C16 126.3(7) . . ? C16 C15 C14 123.0(3) . . ? C15 C16 C41 114.8(3) . . ? C15 C16 C11 116.1(2) . . ? C15 C16 C110 122.2(2) . . ? C41 C16 C110 117.5(3) . . ? C11 C16 C110 121.3(2) . . ? C21 O2 Ti 142.7(2) . . ? N C20 C22 112.9(2) . . ? O2 C21 C22 117.6(2) . . ? O2 C21 C26 120.9(2) . . ? C22 C21 C26 121.4(2) . . ? C23 C22 C21 120.3(2) . . ? C23 C22 C20 119.6(2) . . ? C21 C22 C20 119.8(2) . . ? C22 C23 C24 121.1(2) . . ? C23 C24 C25 117.2(2) . . ? C23 C24 C200 118.9(2) . . ? C25 C24 C200 123.4(2) . . ? C54 C25 C26 121.7(3) . . ? C26 C25 C24 124.3(2) . . ? C25 C26 C21 115.3(2) . . ? C25 C26 C51 116.7(3) . . ? C25 C26 C210 122.2(2) . . ? C21 C26 C210 121.9(2) . . ? C51 C26 C210 113.2(3) . . ? C31 O3 Ti 138.40(15) . . ? C32 C30 N 113.1(2) . . ? O3 C31 C36 121.4(2) . . ? O3 C31 C32 118.4(2) . . ? C36 C31 C32 120.1(2) . . ? C33 C32 C31 120.8(2) . . ? C33 C32 C30 121.1(2) . . ? C31 C32 C30 118.1(2) . . ? C32 C33 C34 120.6(3) . . ? C35 C34 C33 116.8(3) . . ? C35 C34 C300 121.6(3) . . ? C33 C34 C300 121.6(3) . . ? C34 C35 C36 125.0(2) . . ? C36 C35 C64 124.2(5) . . ? C31 C36 C35 116.7(2) . . ? C31 C36 C310 119.1(2) . . ? C35 C36 C310 123.0(2) . . ? C35 C36 C61 111.5(3) . . ? C310 C36 C61 121.0(3) . . ? C41 O4 Ti 143.0(4) . . ? N C40 C42 114.7(5) . . ? O4 C41 C42 117.9(5) . . ? O4 C41 C16 121.1(5) . . ? C42 C41 C16 120.2(5) . . ? C41 C42 C43 120.0(5) . . ? C41 C42 C40 119.1(5) . . ? C43 C42 C40 120.9(5) . . ? C44 C43 C42 121.5(9) . . ? C43 C44 C15 116.2(12) . . ? C43 C44 C100 121.0(12) . . ? C15 C44 C100 122.2(12) . . ? C51 O5 Ti 138.7(4) . . ? C52 C50 N 110.1(4) . . ? O5 C51 C52 117.7(5) . . ? O5 C51 C26 120.8(4) . . ? C52 C51 C26 119.5(5) . . ? C51 C52 C53 120.3(5) . . ? C51 C52 C50 118.7(5) . . ? C53 C52 C50 120.9(5) . . ? C52 C53 C54 121.1(6) . . ? C53 C54 C25 119.9(5) . . ? C53 C54 C200 122.1(5) . . ? C25 C54 C200 115.0(4) . . ? C61 O6 Ti 143.1(4) . . ? N C60 C62 107.1(5) . . ? O6 C61 C62 118.0(5) . . ? O6 C61 C36 119.7(4) . . ? C62 C61 C36 122.0(5) . . ? C63 C62 C61 120.8(5) . . ? C63 C62 C60 120.4(6) . . ? C61 C62 C60 118.7(5) . . ? C62 C63 C64 121.6(7) . . ? C63 C64 C35 118.7(8) . . ? C63 C64 C300 124.9(9) . . ? C35 C64 C300 116.3(7) . . ? C44 C100 C103 101.1(5) . . ? C44 C100 C102 112.7(7) . . ? C103 C100 C102 108.0(2) . . ? C44 C100 C101 117.0(5) . . ? C103 C100 C101 109.3(2) . . ? C102 C100 C101 108.2(2) . . ? C103 C100 C14 114.1(2) . . ? C102 C100 C14 111.4(3) . . ? C101 C100 C14 105.8(2) . . ? C16 C110 C112 111.49(14) . . ? C16 C110 C111 110.5(2) . . ? C112 C110 C111 107.6(2) . . ? C16 C110 C113 109.6(2) . . ? C112 C110 C113 108.0(2) . . ? C111 C110 C113 109.5(2) . . ? C24 C200 C201 111.5(2) . . ? C24 C200 C202 114.9(2) . . ? C201 C200 C202 109.5(2) . . ? C24 C200 C203 105.1(2) . . ? C201 C200 C203 107.1(2) . . ? C202 C200 C203 108.3(2) . . ? C201 C200 C54 111.5(3) . . ? C202 C200 C54 95.0(3) . . ? C203 C200 C54 124.3(3) . . ? C26 C210 C213 110.9(2) . . ? C26 C210 C212 111.3(2) . . ? C213 C210 C212 108.3(2) . . ? C26 C210 C211 108.9(2) . . ? C213 C210 C211 109.6(2) . . ? C212 C210 C211 107.9(2) . . ? C304 C300 C64 120.0(4) . . ? C302 C300 C303 109.6(2) . . ? C302 C300 C301 108.9(2) . . ? C303 C300 C301 106.3(2) . . ? C302 C300 C34 113.5(2) . . ? C303 C300 C34 106.1(2) . . ? C301 C300 C34 112.1(2) . . ? C304 C300 C306 123.9(2) . . ? C64 C300 C306 107.9(5) . . ? C304 C300 C305 114.8(2) . . ? C64 C300 C305 85.1(3) . . ? C306 C300 C305 95.6(2) . . ? C312 C310 C36 111.1(2) . . ? C312 C310 C311 109.3(2) . . ? C36 C310 C311 112.3(2) . . ? C312 C310 C313 106.6(2) . . ? C36 C310 C313 110.9(2) . . ? C311 C310 C313 106.5(2) . . ? _refine_diff_density_max 1.179 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.063 #===END