Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 #1. SUBMISSION DETAILS _publ_contact_author_name 'Sonny C. Lee' _publ_contact_author_address ; Department of Chemistry Princeton University Princeton NJ 08544 USA ; _publ_contact_author_email 'sclee@chemvax.princeton.edu' _publ_contact_author_fax '1 609 258 6746' _publ_contact_author_phone '1 609 258 3879' _publ_requested_journal 'Chemical Communication' #2, TITLE AND AUTHOR LIST _publ_section_title ; Bis[hydrotris(pyrazol-1-yl)borato]titanium(II): a stable Tp2M complex of singular reactivity ; loop_ _publ_author_name _publ_author_address 'Kayal, Ajay' ; Department of Chemistry Princeton University Princeton NJ 08544 USA ; 'Kuncheria, Joshi' ; Department of Chemistry Princeton University Princeton NJ 08544 USA ; 'Lee, Sonny C.' ; Department of Chemistry Princeton University Princeton NJ 08544 USA ; #3. RESULTS data_Tp2Ti.C6H6 _database_code_CSD 172870 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H20 B2 N12 Ti, C6 H6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H26 B2 N12 Ti' _chemical_formula_weight 552.09 _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' 'B' 'B' 0.0013 0.0007 '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' '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.175(2) _cell_length_b 16.6805(13) _cell_length_c 7.5680(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.261(3) _cell_angle_gamma 90.00 _cell_volume 2673.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3997 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'block' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method ? _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.359 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number 'none' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3997 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2308 _reflns_number_observed 1619 _reflns_observed_criterion 'I>2\s(I)' _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'DENZO-SMN' _computing_structure_solution 'SIEMENS SHELXTL' _computing_structure_refinement 'SIEMENS SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+1.7270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'constr' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2308 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_obs 0.0450 _refine_ls_wR_factor_all 0.1184 _refine_ls_wR_factor_obs 0.1030 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.023 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max 0.000 _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 0.2500 0.2500 0.0000 0.0265(2) Uani 1 d S . B1 B 0.36703(14) 0.1422(2) -0.1573(4) 0.0278(7) Uani 1 d . . H101 H 0.40258(14) 0.1094(2) -0.2052(4) 0.033 Uiso 1 calc R . N1 N 0.32351(10) 0.18011(13) 0.1418(3) 0.0306(6) Uani 1 d . . N2 N 0.36890(10) 0.14120(13) 0.0463(3) 0.0272(5) Uani 1 d . . N3 N 0.25203(10) 0.35337(13) 0.1835(3) 0.0307(6) Uani 1 d . . N4 N 0.19628(10) 0.39144(13) 0.2232(3) 0.0266(5) Uani 1 d . . N5 N 0.17082(10) 0.21393(14) 0.1733(3) 0.0298(6) Uani 1 d . . N6 N 0.12667(10) 0.26980(13) 0.2207(3) 0.0280(6) Uani 1 d . . C1 C 0.33855(13) 0.1671(2) 0.3109(4) 0.0347(7) Uani 1 d . . H1 H 0.31521(13) 0.1872(2) 0.4082(4) 0.042 Uiso 1 calc R . C2 C 0.39282(13) 0.1203(2) 0.3266(4) 0.0389(8) Uani 1 d . . H2 H 0.41293(13) 0.1026(2) 0.4321(4) 0.047 Uiso 1 calc R . C3 C 0.41061(13) 0.1056(2) 0.1565(4) 0.0331(7) Uani 1 d . . H3 H 0.44645(13) 0.0754(2) 0.1215(4) 0.040 Uiso 1 calc R . C4 C 0.29671(13) 0.3908(2) 0.2763(4) 0.0326(7) Uani 1 d . . H4 H 0.34021(13) 0.3769(2) 0.2748(4) 0.039 Uiso 1 calc R . C5 C 0.27135(14) 0.4527(2) 0.3753(4) 0.0351(7) Uani 1 d . . H5 H 0.29319(14) 0.4883(2) 0.4521(4) 0.042 Uiso 1 calc R . C6 C 0.20831(13) 0.4514(2) 0.3386(4) 0.0318(7) Uani 1 d . . H6 H 0.17776(13) 0.4869(2) 0.3865(4) 0.038 Uiso 1 calc R . C7 C 0.15421(13) 0.1464(2) 0.2548(4) 0.0329(7) Uani 1 d . . H7 H 0.17676(13) 0.0973(2) 0.2468(4) 0.040 Uiso 1 calc R . C8 C 0.09983(14) 0.1571(2) 0.3527(4) 0.0344(7) Uani 1 d . . H8 H 0.07817(14) 0.1184(2) 0.4217(4) 0.041 Uiso 1 calc R . C9 C 0.08413(12) 0.2362(2) 0.3277(4) 0.0295(7) Uani 1 d . . H9 H 0.04884(12) 0.2627(2) 0.3782(4) 0.035 Uiso 1 calc R . C1S C 0.5000 0.4617(3) 0.2500 0.0441(12) Uani 1 d S . H1S H 0.5000 0.5187(3) 0.2500 0.053 Uiso 1 calc SR . C2S C 0.46012(14) 0.4207(2) 0.1403(4) 0.0436(8) Uani 1 d . . H2S H 0.43248(14) 0.4494(2) 0.0638(4) 0.052 Uiso 1 calc R . C3S C 0.45968(14) 0.3384(2) 0.1396(4) 0.0433(8) Uani 1 d . . H3S H 0.43171(14) 0.3102(2) 0.0634(4) 0.052 Uiso 1 calc R . C4S C 0.5000 0.2970(3) 0.2500 0.0421(11) Uani 1 d S . H4S H 0.5000 0.2400(3) 0.2500 0.051 Uiso 1 calc SR . 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 0.0267(4) 0.0297(4) 0.0232(4) -0.0017(3) 0.0031(3) 0.0023(3) B1 0.026(2) 0.031(2) 0.026(2) -0.0003(15) 0.0048(13) 0.0037(14) N1 0.0325(13) 0.0344(14) 0.0249(13) -0.0023(11) 0.0037(10) 0.0032(11) N2 0.0253(12) 0.0275(13) 0.0288(13) 0.0015(11) 0.0011(10) 0.0016(10) N3 0.0279(13) 0.0337(14) 0.0307(14) -0.0042(11) 0.0026(11) 0.0016(11) N4 0.0291(12) 0.0264(13) 0.0242(12) -0.0014(11) 0.0013(10) 0.0015(10) N5 0.0339(13) 0.0289(14) 0.0267(13) 0.0004(12) 0.0048(10) 0.0032(11) N6 0.0275(12) 0.0344(14) 0.0223(12) -0.0010(11) 0.0032(10) 0.0030(11) C1 0.039(2) 0.039(2) 0.026(2) 0.0002(14) 0.0022(13) -0.0024(14) C2 0.039(2) 0.046(2) 0.032(2) 0.006(2) -0.0071(14) -0.0016(15) C3 0.028(2) 0.033(2) 0.039(2) 0.0040(15) -0.0012(13) 0.0015(13) C4 0.026(2) 0.038(2) 0.034(2) 0.0010(15) -0.0011(13) -0.0063(13) C5 0.046(2) 0.032(2) 0.027(2) -0.0031(14) -0.0030(14) -0.0096(14) C6 0.045(2) 0.024(2) 0.027(2) -0.0029(13) 0.0023(13) 0.0010(13) C7 0.040(2) 0.028(2) 0.030(2) 0.0032(14) 0.0032(13) 0.0019(14) C8 0.040(2) 0.033(2) 0.030(2) 0.0040(14) 0.0052(13) -0.0066(14) C9 0.0225(14) 0.043(2) 0.0235(15) -0.0042(14) 0.0049(12) -0.0049(13) C1S 0.044(3) 0.036(3) 0.053(3) 0.000 0.003(2) 0.000 C2S 0.036(2) 0.052(2) 0.043(2) 0.010(2) 0.0001(14) 0.004(2) C3S 0.033(2) 0.058(2) 0.039(2) -0.010(2) 0.0038(14) -0.009(2) C4S 0.041(3) 0.032(3) 0.054(3) 0.000 0.018(2) 0.000 _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 N3 2.214(2) 7 ? Ti1 N3 2.214(2) . ? Ti1 N5 2.216(2) . ? Ti1 N5 2.216(2) 7 ? Ti1 N1 2.218(2) . ? Ti1 N1 2.218(2) 7 ? B1 N4 1.534(4) 7 ? B1 N2 1.541(4) . ? B1 N6 1.550(4) 7 ? N1 C1 1.335(3) . ? N1 N2 1.369(3) . ? N2 C3 1.349(3) . ? N3 C4 1.331(3) . ? N3 N4 1.375(3) . ? N4 C6 1.351(3) . ? N4 B1 1.534(4) 7 ? N5 C7 1.333(3) . ? N5 N6 1.369(3) . ? N6 C9 1.338(3) . ? N6 B1 1.550(4) 7 ? C1 C2 1.394(4) . ? C2 C3 1.365(4) . ? C4 C5 1.385(4) . ? C5 C6 1.362(4) . ? C7 C8 1.384(4) . ? C8 C9 1.373(4) . ? C1S C2S 1.365(4) 2_655 ? C1S C2S 1.365(4) . ? C2S C3S 1.373(4) . ? C3S C4S 1.378(4) . ? C4S C3S 1.378(4) 2_655 ? 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 N3 Ti1 N3 180.0 7 . ? N3 Ti1 N5 98.46(8) 7 . ? N3 Ti1 N5 81.54(8) . . ? N3 Ti1 N5 81.54(8) 7 7 ? N3 Ti1 N5 98.46(8) . 7 ? N5 Ti1 N5 180.0 . 7 ? N3 Ti1 N1 84.60(8) 7 . ? N3 Ti1 N1 95.40(8) . . ? N5 Ti1 N1 95.86(8) . . ? N5 Ti1 N1 84.14(8) 7 . ? N3 Ti1 N1 95.41(8) 7 7 ? N3 Ti1 N1 84.59(8) . 7 ? N5 Ti1 N1 84.14(8) . 7 ? N5 Ti1 N1 95.86(8) 7 7 ? N1 Ti1 N1 180.0 . 7 ? N4 B1 N2 109.8(2) 7 . ? N4 B1 N6 108.8(2) 7 7 ? N2 B1 N6 108.5(2) . 7 ? C1 N1 N2 105.3(2) . . ? C1 N1 Ti1 135.5(2) . . ? N2 N1 Ti1 119.1(2) . . ? C3 N2 N1 109.9(2) . . ? C3 N2 B1 129.5(2) . . ? N1 N2 B1 120.5(2) . . ? C4 N3 N4 106.1(2) . . ? C4 N3 Ti1 135.0(2) . . ? N4 N3 Ti1 118.8(2) . . ? C6 N4 N3 108.9(2) . . ? C6 N4 B1 130.0(2) . 7 ? N3 N4 B1 120.7(2) . 7 ? C7 N5 N6 105.8(2) . . ? C7 N5 Ti1 134.9(2) . . ? N6 N5 Ti1 119.3(2) . . ? C9 N6 N5 109.6(2) . . ? C9 N6 B1 130.1(2) . 7 ? N5 N6 B1 120.2(2) . 7 ? N1 C1 C2 111.5(3) . . ? C3 C2 C1 104.5(3) . . ? N2 C3 C2 108.7(2) . . ? N3 C4 C5 111.0(2) . . ? C6 C5 C4 105.1(2) . . ? N4 C6 C5 109.0(3) . . ? N5 C7 C8 111.1(3) . . ? C9 C8 C7 104.6(3) . . ? N6 C9 C8 108.8(3) . . ? C2S C1S C2S 119.9(4) 2_655 . ? C1S C2S C3S 120.5(3) . . ? C2S C3S C4S 119.7(3) . . ? C3S C4S C3S 119.7(4) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ti1 N1 C1 -141.4(3) 7 . . . ? N3 Ti1 N1 C1 38.6(3) . . . . ? N5 Ti1 N1 C1 -43.5(3) . . . . ? N5 Ti1 N1 C1 136.5(3) 7 . . . ? N1 Ti1 N1 C1 68.6(25) 7 . . . ? N3 Ti1 N1 N2 42.3(2) 7 . . . ? N3 Ti1 N1 N2 -137.7(2) . . . . ? N5 Ti1 N1 N2 140.3(2) . . . . ? N5 Ti1 N1 N2 -39.7(2) 7 . . . ? N1 Ti1 N1 N2 -107.6(24) 7 . . . ? C1 N1 N2 C3 -0.2(3) . . . . ? Ti1 N1 N2 C3 177.1(2) . . . . ? C1 N1 N2 B1 179.6(2) . . . . ? Ti1 N1 N2 B1 -3.2(3) . . . . ? N4 B1 N2 C3 122.8(3) 7 . . . ? N6 B1 N2 C3 -118.4(3) 7 . . . ? N4 B1 N2 N1 -56.9(3) 7 . . . ? N6 B1 N2 N1 61.9(3) 7 . . . ? N3 Ti1 N3 C4 -38.5(165) 7 . . . ? N5 Ti1 N3 C4 130.9(3) . . . . ? N5 Ti1 N3 C4 -49.1(3) 7 . . . ? N1 Ti1 N3 C4 35.7(3) . . . . ? N1 Ti1 N3 C4 -144.3(3) 7 . . . ? N3 Ti1 N3 N4 143.2(164) 7 . . . ? N5 Ti1 N3 N4 -47.5(2) . . . . ? N5 Ti1 N3 N4 132.5(2) 7 . . . ? N1 Ti1 N3 N4 -142.6(2) . . . . ? N1 Ti1 N3 N4 37.4(2) 7 . . . ? C4 N3 N4 C6 0.3(3) . . . . ? Ti1 N3 N4 C6 179.0(2) . . . . ? C4 N3 N4 B1 -172.5(2) . . . 7 ? Ti1 N3 N4 B1 6.3(3) . . . 7 ? N3 Ti1 N5 C7 47.2(3) 7 . . . ? N3 Ti1 N5 C7 -132.8(3) . . . . ? N5 Ti1 N5 C7 -174.9(29) 7 . . . ? N1 Ti1 N5 C7 -38.2(3) . . . . ? N1 Ti1 N5 C7 141.8(3) 7 . . . ? N3 Ti1 N5 N6 -135.1(2) 7 . . . ? N3 Ti1 N5 N6 44.9(2) . . . . ? N5 Ti1 N5 N6 2.7(29) 7 . . . ? N1 Ti1 N5 N6 139.5(2) . . . . ? N1 Ti1 N5 N6 -40.5(2) 7 . . . ? C7 N5 N6 C9 -0.4(3) . . . . ? Ti1 N5 N6 C9 -178.7(2) . . . . ? C7 N5 N6 B1 176.8(2) . . . 7 ? Ti1 N5 N6 B1 -1.5(3) . . . 7 ? N2 N1 C1 C2 -0.1(3) . . . . ? Ti1 N1 C1 C2 -176.7(2) . . . . ? N1 C1 C2 C3 0.4(3) . . . . ? N1 N2 C3 C2 0.4(3) . . . . ? B1 N2 C3 C2 -179.3(3) . . . . ? C1 C2 C3 N2 -0.5(3) . . . . ? N4 N3 C4 C5 -0.2(3) . . . . ? Ti1 N3 C4 C5 -178.7(2) . . . . ? N3 C4 C5 C6 0.1(3) . . . . ? N3 N4 C6 C5 -0.2(3) . . . . ? B1 N4 C6 C5 171.6(3) 7 . . . ? C4 C5 C6 N4 0.1(3) . . . . ? N6 N5 C7 C8 0.6(3) . . . . ? Ti1 N5 C7 C8 178.5(2) . . . . ? N5 C7 C8 C9 -0.6(3) . . . . ? N5 N6 C9 C8 0.1(3) . . . . ? B1 N6 C9 C8 -176.8(3) 7 . . . ? C7 C8 C9 N6 0.3(3) . . . . ? C2S C1S C2S C3S 0.1(2) 2_655 . . . ? C1S C2S C3S C4S -0.3(4) . . . . ? C2S C3S C4S C3S 0.1(2) . . . 2_655 ? _refine_diff_density_max 0.216 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.059 #===END data_[Tp2Ti](PF6) _database_code_CSD 172871 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H20 B2 N12 Ti 1+, F6 P 1-' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H20 B2 F6 N12 P Ti' _chemical_formula_weight 618.95 _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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 'tetragonal' _symmetry_space_group_name_H-M 'I 4/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 13.4375(8) _cell_length_b 13.4375(8) _cell_length_c 14.2741(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2577.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6338 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method ? _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number 'none' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6338 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 26.04 _reflns_number_total 1335 _reflns_number_observed 750 _reflns_observed_criterion 'I>2\s(I)' _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'DENZO-SMN' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SIEMENS SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+5.0704P] 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 1335 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1179 _refine_ls_R_factor_obs 0.0575 _refine_ls_wR_factor_all 0.1894 _refine_ls_wR_factor_obs 0.1457 _refine_ls_goodness_of_fit_all 1.011 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_restrained_S_all 1.011 _refine_ls_restrained_S_obs 1.066 _refine_ls_shift/esd_max 0.000 _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 0.5000 0.0000 0.0000 0.0463(5) Uani 1 d S . B1 B 0.5400(5) 0.2351(5) 0.0000 0.048(2) Uiso 1 d S . H101 H 0.5555(39) 0.3214(41) 0.0000 0.057 Uiso 1 d S . N1 N 0.5501(2) -0.1072(2) 0.0996(3) 0.0475(9) Uani 1 d . . N2 N 0.5207(2) -0.2047(2) 0.0871(3) 0.0481(9) Uani 1 d . . N3 N 0.6373(3) 0.0741(3) 0.0000 0.061(2) Uani 1 d S . N4 N 0.6397(3) 0.1759(3) 0.0000 0.0500(13) Uani 1 d S . C1 C 0.6101(3) -0.1083(3) 0.1744(3) 0.0569(12) Uani 1 d . . H1 H 0.6424(3) -0.0513(3) 0.1993(3) 0.068 Uiso 1 calc R . C2 C 0.6189(3) -0.2021(3) 0.2103(4) 0.0603(12) Uani 1 d . . H2 H 0.6567(3) -0.2221(3) 0.2633(4) 0.072 Uiso 1 calc R . C3 C 0.5619(3) -0.2612(3) 0.1537(4) 0.0556(12) Uani 1 d . . H3 H 0.5529(3) -0.3309(3) 0.1606(4) 0.067 Uiso 1 calc R . C4 C 0.7322(4) 0.0449(5) 0.0000 0.072(2) Uani 1 d S . H4 H 0.7534(4) -0.0226(5) 0.0000 0.086 Uiso 1 calc SR . C5 C 0.7956(5) 0.1258(5) 0.0000 0.068(2) Uani 1 d S . H5 H 0.8663(5) 0.1252(5) 0.0000 0.081 Uiso 1 calc SR . C6 C 0.7339(4) 0.2073(4) 0.0000 0.053(2) Uani 1 d S . H6 H 0.7548(4) 0.2748(4) 0.0000 0.064 Uiso 1 calc SR . P1 P 0.0000 0.0000 0.1979(2) 0.0539(7) Uani 1 d S . F1 F 0.0000 0.0000 0.0878(4) 0.091(2) Uani 1 d S . F2 F 0.1048(2) 0.0570(2) 0.2002(2) 0.0681(8) Uani 1 d . . F3 F 0.0000 0.0000 0.3112(3) 0.0481(12) Uani 1 d S . 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 0.0350(8) 0.0280(8) 0.0760(13) 0.000 0.000 0.0004(6) N1 0.045(2) 0.034(2) 0.063(3) -0.003(2) 0.001(2) -0.0024(14) N2 0.042(2) 0.034(2) 0.068(2) 0.003(2) 0.006(2) 0.0028(14) N3 0.039(3) 0.031(3) 0.112(5) 0.000 0.000 0.001(2) N4 0.040(3) 0.032(2) 0.077(4) 0.000 0.000 -0.004(2) C1 0.054(3) 0.052(3) 0.065(3) -0.009(2) 0.006(2) 0.000(2) C2 0.052(3) 0.067(3) 0.061(3) 0.006(3) 0.001(2) 0.008(2) C3 0.049(2) 0.046(2) 0.072(3) 0.013(2) 0.012(2) 0.012(2) C4 0.037(4) 0.050(4) 0.127(7) 0.000 0.000 0.004(3) C5 0.039(3) 0.054(4) 0.111(7) 0.000 0.000 -0.006(3) C6 0.051(4) 0.039(3) 0.071(5) 0.000 0.000 -0.013(3) P1 0.0583(9) 0.0583(9) 0.045(2) 0.000 0.000 0.000 F1 0.112(3) 0.112(3) 0.050(4) 0.000 0.000 0.000 F2 0.064(2) 0.070(2) 0.070(2) 0.0120(14) 0.0094(14) -0.0086(13) F3 0.051(2) 0.051(2) 0.042(3) 0.000 0.000 0.000 _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 N3 2.096(4) . ? Ti1 N3 2.096(4) 9_655 ? Ti1 N1 2.132(3) . ? Ti1 N1 2.132(3) 2_655 ? Ti1 N1 2.132(3) 9_655 ? Ti1 N1 2.132(3) 10 ? B1 N2 1.542(5) 9_655 ? B1 N2 1.542(5) 2_655 ? B1 N4 1.557(8) . ? N1 C1 1.338(5) . ? N1 N2 1.380(4) . ? N2 C3 1.336(6) . ? N2 B1 1.542(5) 9_655 ? N3 C4 1.335(7) . ? N3 N4 1.369(6) . ? N4 C6 1.334(7) . ? C1 C2 1.365(6) . ? C2 C3 1.368(6) . ? C4 C5 1.381(8) . ? C5 C6 1.374(8) . ? P1 F1 1.571(6) . ? P1 F2 1.603(3) 3 ? P1 F2 1.603(3) . ? P1 F2 1.603(3) 2 ? P1 F2 1.603(3) 4 ? P1 F3 1.617(5) . ? 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 N3 Ti1 N3 180.0 . 9_655 ? N3 Ti1 N1 92.46(12) . . ? N3 Ti1 N1 87.54(12) 9_655 . ? N3 Ti1 N1 87.54(12) . 2_655 ? N3 Ti1 N1 92.46(12) 9_655 2_655 ? N1 Ti1 N1 96.4(2) . 2_655 ? N3 Ti1 N1 87.54(12) . 9_655 ? N3 Ti1 N1 92.46(12) 9_655 9_655 ? N1 Ti1 N1 180.0 . 9_655 ? N1 Ti1 N1 83.6(2) 2_655 9_655 ? N3 Ti1 N1 92.46(12) . 10 ? N3 Ti1 N1 87.54(12) 9_655 10 ? N1 Ti1 N1 83.6(2) . 10 ? N1 Ti1 N1 180.0 2_655 10 ? N1 Ti1 N1 96.4(2) 9_655 10 ? N2 B1 N2 107.4(5) 9_655 2_655 ? N2 B1 N4 108.7(3) 9_655 . ? N2 B1 N4 108.7(3) 2_655 . ? C1 N1 N2 105.3(3) . . ? C1 N1 Ti1 136.9(3) . . ? N2 N1 Ti1 117.7(3) . . ? C3 N2 N1 109.2(4) . . ? C3 N2 B1 130.0(4) . 9_655 ? N1 N2 B1 120.4(4) . 9_655 ? C4 N3 N4 105.7(5) . . ? C4 N3 Ti1 134.6(4) . . ? N4 N3 Ti1 119.7(3) . . ? C6 N4 N3 109.8(4) . . ? C6 N4 B1 130.9(5) . . ? N3 N4 B1 119.3(4) . . ? N1 C1 C2 111.3(4) . . ? C1 C2 C3 105.4(4) . . ? N2 C3 C2 108.8(4) . . ? N3 C4 C5 111.0(6) . . ? C6 C5 C4 104.8(5) . . ? N4 C6 C5 108.7(5) . . ? F1 P1 F2 91.19(14) . 3 ? F1 P1 F2 91.19(13) . . ? F2 P1 F2 89.975(6) 3 . ? F1 P1 F2 91.19(14) . 2 ? F2 P1 F2 89.976(5) 3 2 ? F2 P1 F2 177.6(3) . 2 ? F1 P1 F2 91.19(14) . 4 ? F2 P1 F2 177.6(3) 3 4 ? F2 P1 F2 89.977(6) . 4 ? F2 P1 F2 89.973(5) 2 4 ? F1 P1 F3 180.0 . . ? F2 P1 F3 88.81(14) 3 . ? F2 P1 F3 88.81(14) . . ? F2 P1 F3 88.81(14) 2 . ? F2 P1 F3 88.81(14) 4 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ti1 N1 C1 35.4(4) . . . . ? N3 Ti1 N1 C1 -144.6(4) 9_655 . . . ? N1 Ti1 N1 C1 -52.4(4) 2_655 . . . ? N1 Ti1 N1 C1 127.4(22) 9_655 . . . ? N1 Ti1 N1 C1 127.6(4) 10 . . . ? N3 Ti1 N1 N2 -140.5(3) . . . . ? N3 Ti1 N1 N2 39.5(3) 9_655 . . . ? N1 Ti1 N1 N2 131.7(3) 2_655 . . . ? N1 Ti1 N1 N2 -48.6(22) 9_655 . . . ? N1 Ti1 N1 N2 -48.3(3) 10 . . . ? C1 N1 N2 C3 0.7(4) . . . . ? Ti1 N1 N2 C3 177.8(3) . . . . ? C1 N1 N2 B1 -173.0(4) . . . 9_655 ? Ti1 N1 N2 B1 4.2(5) . . . 9_655 ? N3 Ti1 N3 C4 180.0 9_655 . . . ? N1 Ti1 N3 C4 41.85(9) . . . . ? N1 Ti1 N3 C4 138.15(9) 2_655 . . . ? N1 Ti1 N3 C4 -138.15(9) 9_655 . . . ? N1 Ti1 N3 C4 -41.85(9) 10 . . . ? N3 Ti1 N3 N4 0.0 9_655 . . . ? N1 Ti1 N3 N4 -138.15(9) . . . . ? N1 Ti1 N3 N4 -41.85(9) 2_655 . . . ? N1 Ti1 N3 N4 41.85(9) 9_655 . . . ? N1 Ti1 N3 N4 138.15(9) 10 . . . ? C4 N3 N4 C6 0.0 . . . . ? Ti1 N3 N4 C6 180.0 . . . . ? C4 N3 N4 B1 180.0 . . . . ? Ti1 N3 N4 B1 0.0 . . . . ? N2 B1 N4 C6 121.7(3) 9_655 . . . ? N2 B1 N4 C6 -121.7(3) 2_655 . . . ? N2 B1 N4 N3 -58.3(3) 9_655 . . . ? N2 B1 N4 N3 58.3(3) 2_655 . . . ? N2 N1 C1 C2 -0.7(5) . . . . ? Ti1 N1 C1 C2 -177.0(3) . . . . ? N1 C1 C2 C3 0.5(5) . . . . ? N1 N2 C3 C2 -0.3(5) . . . . ? B1 N2 C3 C2 172.5(4) 9_655 . . . ? C1 C2 C3 N2 -0.1(5) . . . . ? N4 N3 C4 C5 0.0 . . . . ? Ti1 N3 C4 C5 180.0 . . . . ? N3 C4 C5 C6 0.0 . . . . ? N3 N4 C6 C5 0.0 . . . . ? B1 N4 C6 C5 180.0 . . . . ? C4 C5 C6 N4 0.0 . . . . ? _refine_diff_density_max 0.530 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.070 #===END data_[(k2-Tp)(K3-Tp)Ti]2(mu-O).4C6H6 _database_code_CSD 172872 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C36 H40 B4 N24 O Ti2, 4(C6 H6)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H64 B4 N24 O Ti2' _chemical_formula_weight 1276.39 _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' 'B' 'B' 0.0013 0.0007 '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' 'N' 'N' 0.0061 0.0033 '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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 20.5983(6) _cell_length_b 15.6270(6) _cell_length_c 20.2307(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6512.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 27250 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 24.14 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 0.306 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27250 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 24.14 _reflns_number_total 9955 _reflns_number_observed 7077 _reflns_observed_criterion 'I>2\s(I)' _computing_data_collection 'NONIUS-COLLECT' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'DENZO-SMN' _computing_structure_solution 'SIEMENS SHELXTL' _computing_structure_refinement 'SIEMENS SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.4022P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(2) _refine_ls_number_reflns 9955 _refine_ls_number_parameters 837 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_obs 0.0483 _refine_ls_wR_factor_all 0.0970 _refine_ls_wR_factor_obs 0.0843 _refine_ls_goodness_of_fit_all 1.008 _refine_ls_goodness_of_fit_obs 1.057 _refine_ls_restrained_S_all 1.008 _refine_ls_restrained_S_obs 1.057 _refine_ls_shift/esd_max 0.008 _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_1 Ti 0.33381(3) 0.85146(4) 0.29950(3) 0.0277(2) Uani 1 d . . Ti2_1 Ti 0.20007(3) 0.83948(4) 0.41371(4) 0.0299(2) Uani 1 d . . O1_1 O 0.26825(13) 0.85772(14) 0.35887(14) 0.0311(6) Uani 1 d . . N1_1 N 0.3523(2) 0.7162(2) 0.3184(2) 0.0317(8) Uani 1 d . . N2_1 N 0.3520(2) 0.6575(2) 0.2687(2) 0.0341(9) Uani 1 d . . N3_1 N 0.4058(2) 0.8222(2) 0.2183(2) 0.0319(8) Uani 1 d . . N4_1 N 0.3993(2) 0.7490(2) 0.1808(2) 0.0323(9) Uani 1 d . . N5_1 N 0.2671(2) 0.8092(2) 0.2214(2) 0.0323(8) Uani 1 d . . N6_1 N 0.2785(2) 0.7330(2) 0.1886(2) 0.0337(8) Uani 1 d . . N7_1 N 0.4138(2) 0.8882(2) 0.36181(15) 0.0301(8) Uani 1 d . . N8_1 N 0.4194(2) 0.9684(2) 0.38891(15) 0.0315(8) Uani 1 d . . N9_1 N 0.3345(2) 0.9829(2) 0.2668(2) 0.0303(8) Uani 1 d . . N10_1 N 0.34947(14) 1.0505(2) 0.3086(2) 0.0316(8) Uani 1 d . . N11_1 N 0.3855(2) 1.1184(2) 0.4152(2) 0.0360(8) Uani 1 d . . N12_1 N 0.4390(2) 1.1629(2) 0.3950(2) 0.0435(10) Uani 1 d . . N13_1 N 0.1209(2) 0.8638(2) 0.34702(15) 0.0302(8) Uani 1 d . . N14_1 N 0.1012(2) 0.9441(2) 0.3274(2) 0.0320(8) Uani 1 d . . N15_1 N 0.1835(2) 0.9681(2) 0.4503(2) 0.0321(9) Uani 1 d . . N16_1 N 0.15968(15) 1.0332(2) 0.4126(2) 0.0339(8) Uani 1 d . . N17_1 N 0.1186(2) 1.1031(2) 0.3089(2) 0.0362(8) Uani 1 d . . N18_1 N 0.0597(2) 1.1351(2) 0.3277(2) 0.0472(10) Uani 1 d . . N19_1 N 0.2624(2) 0.8070(2) 0.49724(15) 0.0338(8) Uani 1 d . . N20_1 N 0.2523(2) 0.7333(2) 0.5332(2) 0.0427(9) Uani 1 d . . N21_1 N 0.1226(2) 0.8000(2) 0.4863(2) 0.0395(9) Uani 1 d . . N22_1 N 0.1318(2) 0.7297(2) 0.5256(2) 0.0454(10) Uani 1 d . . N23_1 N 0.1967(2) 0.7017(2) 0.3961(2) 0.0343(9) Uani 1 d . . N24_1 N 0.1975(2) 0.6443(2) 0.4476(2) 0.0389(9) Uani 1 d . . B1_1 B 0.3440(2) 0.6872(3) 0.1962(3) 0.0344(13) Uani 1 d . . H101_1 H 0.3473(13) 0.6310(18) 0.1652(14) 0.009(8) Uiso 1 d . . B2_1 B 0.3637(3) 1.0343(3) 0.3837(2) 0.0347(12) Uani 1 d . . H201_1 H 0.3166(14) 1.0116(17) 0.4081(16) 0.016(8) Uiso 1 d . . B3_1 B 0.1485(3) 1.0212(3) 0.3371(3) 0.0370(12) Uani 1 d . . H301_1 H 0.1972(14) 1.0067(17) 0.3116(15) 0.016(8) Uiso 1 d . . B4_1 B 0.1929(3) 0.6760(4) 0.5194(3) 0.047(2) Uani 1 d . . H401_1 H 0.1888(17) 0.6210(22) 0.5563(18) 0.037(10) Uiso 1 d . . C1_1 C 0.3632(2) 0.6713(2) 0.3745(2) 0.0373(11) Uani 1 d . . H1_1 H 0.3655(2) 0.6952(2) 0.4176(2) 0.045 Uiso 1 calc R . C2_1 C 0.3704(2) 0.5855(2) 0.3599(2) 0.0472(12) Uani 1 d . . H2_1 H 0.3791(2) 0.5403(2) 0.3900(2) 0.057 Uiso 1 calc R . C3_1 C 0.3623(2) 0.5793(2) 0.2929(2) 0.0441(11) Uani 1 d . . H3_1 H 0.3638(2) 0.5280(2) 0.2678(2) 0.053 Uiso 1 calc R . C4_1 C 0.4485(2) 0.7438(3) 0.1380(2) 0.0408(11) Uani 1 d . . H4_1 H 0.4548(2) 0.6992(3) 0.1067(2) 0.049 Uiso 1 calc R . C5_1 C 0.4881(2) 0.8129(3) 0.1463(2) 0.0431(11) Uani 1 d . . H5_1 H 0.5267(2) 0.8259(3) 0.1226(2) 0.052 Uiso 1 calc R . C6_1 C 0.4600(2) 0.8598(3) 0.1966(2) 0.0381(11) Uani 1 d . . H6_1 H 0.4770(2) 0.9119(3) 0.2135(2) 0.046 Uiso 1 calc R . C7_1 C 0.2067(2) 0.8315(2) 0.2069(2) 0.0333(11) Uani 1 d . . H7_1 H 0.1860(2) 0.8821(2) 0.2223(2) 0.040 Uiso 1 calc R . C8_1 C 0.1778(2) 0.7712(3) 0.1664(2) 0.0451(12) Uani 1 d . . H8_1 H 0.1347(2) 0.7717(3) 0.1496(2) 0.054 Uiso 1 calc R . C9_1 C 0.2243(2) 0.7110(3) 0.1559(2) 0.0419(11) Uani 1 d . . H9_1 H 0.2193(2) 0.6612(3) 0.1295(2) 0.050 Uiso 1 calc R . C10_1 C 0.4662(2) 0.8455(3) 0.3814(2) 0.0410(11) Uani 1 d . . H10_1 H 0.4748(2) 0.7876(3) 0.3701(2) 0.049 Uiso 1 calc R . C11_1 C 0.5060(2) 0.8942(3) 0.4195(2) 0.0539(13) Uani 1 d . . H11_1 H 0.5463(2) 0.8783(3) 0.4388(2) 0.065 Uiso 1 calc R . C12_1 C 0.4747(2) 0.9716(3) 0.4238(2) 0.0501(12) Uani 1 d . . H12_1 H 0.4899(2) 1.0199(3) 0.4477(2) 0.060 Uiso 1 calc R . C13_1 C 0.3190(2) 1.0191(2) 0.2092(2) 0.0351(10) Uani 1 d . . H13_1 H 0.3075(2) 0.9878(2) 0.1706(2) 0.042 Uiso 1 calc R . C14_1 C 0.3216(2) 1.1075(2) 0.2123(2) 0.0413(11) Uani 1 d . . H14_1 H 0.3120(2) 1.1475(2) 0.1784(2) 0.050 Uiso 1 calc R . C15_1 C 0.3413(2) 1.1240(2) 0.2761(2) 0.0389(11) Uani 1 d . . H15_1 H 0.3481(2) 1.1794(2) 0.2943(2) 0.047 Uiso 1 calc R . C16_1 C 0.3586(2) 1.1567(3) 0.4683(2) 0.0443(11) Uani 1 d . . H16_1 H 0.3208(2) 1.1378(3) 0.4910(2) 0.053 Uiso 1 calc R . C17_1 C 0.3943(2) 1.2265(3) 0.4839(2) 0.0499(12) Uani 1 d . . H17_1 H 0.3871(2) 1.2659(3) 0.5189(2) 0.060 Uiso 1 calc R . C18_1 C 0.4437(2) 1.2277(3) 0.4376(2) 0.0457(12) Uani 1 d . . H18_1 H 0.4770(2) 1.2698(3) 0.4363(2) 0.055 Uiso 1 calc R . C19_1 C 0.0762(2) 0.8095(3) 0.3233(2) 0.0373(11) Uani 1 d . . H19_1 H 0.0774(2) 0.7492(3) 0.3290(2) 0.045 Uiso 1 calc R . C20_1 C 0.0285(2) 0.8529(3) 0.2895(2) 0.0489(12) Uani 1 d . . H20_1 H -0.0086(2) 0.8294(3) 0.2684(2) 0.059 Uiso 1 calc R . C21_1 C 0.0462(2) 0.9379(3) 0.2931(2) 0.0437(11) Uani 1 d . . H21_1 H 0.0230(2) 0.9844(3) 0.2742(2) 0.052 Uiso 1 calc R . C22_1 C 0.1933(2) 1.0009(3) 0.5106(2) 0.0397(11) Uani 1 d . . H22_1 H 0.2093(2) 0.9695(3) 0.5474(2) 0.048 Uiso 1 calc R . C23_1 C 0.1771(2) 1.0867(3) 0.5122(2) 0.0505(13) Uani 1 d . . H23_1 H 0.1797(2) 1.1249(3) 0.5487(2) 0.061 Uiso 1 calc R . C24_1 C 0.1562(2) 1.1042(3) 0.4490(2) 0.0457(12) Uani 1 d . . H24_1 H 0.1416(2) 1.1584(3) 0.4337(2) 0.055 Uiso 1 calc R . C25_1 C 0.1476(2) 1.1556(3) 0.2657(2) 0.0412(11) Uani 1 d . . H25_1 H 0.1888(2) 1.1466(3) 0.2457(2) 0.049 Uiso 1 calc R . C26_1 C 0.1074(2) 1.2248(3) 0.2552(2) 0.0484(12) Uani 1 d . . H26_1 H 0.1145(2) 1.2728(3) 0.2273(2) 0.058 Uiso 1 calc R . C27_1 C 0.0543(2) 1.2080(3) 0.2952(2) 0.0469(11) Uani 1 d . . H27_1 H 0.0178(2) 1.2449(3) 0.2987(2) 0.056 Uiso 1 calc R . C28_1 C 0.3193(2) 0.8387(3) 0.5182(2) 0.0395(11) Uani 1 d . . H28_1 H 0.3385(2) 0.8898(3) 0.5019(2) 0.047 Uiso 1 calc R . C29_1 C 0.3460(2) 0.7876(3) 0.5664(2) 0.0514(13) Uani 1 d . . H29_1 H 0.3858(2) 0.7962(3) 0.5893(2) 0.062 Uiso 1 calc R . C30_1 C 0.3036(2) 0.7227(3) 0.5742(2) 0.0498(12) Uani 1 d . . H30_1 H 0.3089(2) 0.6763(3) 0.6041(2) 0.060 Uiso 1 calc R . C31_1 C 0.0635(2) 0.8307(3) 0.5003(2) 0.0528(13) Uani 1 d . . H31_1 H 0.0445(2) 0.8797(3) 0.4803(2) 0.063 Uiso 1 calc R . C32_1 C 0.0343(3) 0.7804(4) 0.5483(3) 0.072(2) Uani 1 d . . H32_1 H -0.0076(3) 0.7877(4) 0.5671(3) 0.086 Uiso 1 calc R . C33_1 C 0.0786(3) 0.7180(4) 0.5628(2) 0.064(2) Uani 1 d . . H33_1 H 0.0726(3) 0.6734(4) 0.5942(2) 0.077 Uiso 1 calc R . C34_1 C 0.2012(2) 0.6545(2) 0.3409(2) 0.0345(10) Uani 1 d . . H34_1 H 0.2017(2) 0.6771(2) 0.2973(2) 0.041 Uiso 1 calc R . C35_1 C 0.2049(2) 0.5680(3) 0.3563(2) 0.0469(12) Uani 1 d . . H35_1 H 0.2083(2) 0.5216(3) 0.3263(2) 0.056 Uiso 1 calc R . C36_1 C 0.2024(2) 0.5638(2) 0.4238(3) 0.0455(12) Uani 1 d . . H36_1 H 0.2039(2) 0.5130(2) 0.4495(3) 0.055 Uiso 1 calc R . C37_2 C 0.3984(3) 0.8786(3) 0.0002(3) 0.0665(15) Uani 1 d . . H37_2 H 0.4409(3) 0.8958(3) 0.0127(3) 0.080 Uiso 1 calc R . C38_2 C 0.3503(4) 0.8768(4) 0.0455(3) 0.075(2) Uani 1 d . . H38_2 H 0.3593(4) 0.8939(4) 0.0896(3) 0.090 Uiso 1 calc R . C39_2 C 0.2900(3) 0.8514(4) 0.0294(4) 0.090(2) Uani 1 d . . H39_2 H 0.2565(3) 0.8501(4) 0.0616(4) 0.108 Uiso 1 calc R . C40_2 C 0.2779(3) 0.8271(3) -0.0351(5) 0.087(2) Uani 1 d . . H40_2 H 0.2357(3) 0.8085(3) -0.0474(5) 0.105 Uiso 1 calc R . C41_2 C 0.3264(3) 0.8298(3) -0.0815(3) 0.0655(15) Uani 1 d . . H41_2 H 0.3179(3) 0.8135(3) -0.1259(3) 0.079 Uiso 1 calc R . C42_2 C 0.3860(3) 0.8556(3) -0.0634(3) 0.062(2) Uani 1 d . . H42_2 H 0.4197(3) 0.8579(3) -0.0954(3) 0.074 Uiso 1 calc R . C43_3 C -0.1099(2) 0.4871(3) 0.7087(3) 0.0677(15) Uani 1 d . . H43_3 H -0.1471(2) 0.4518(3) 0.7147(3) 0.081 Uiso 1 calc R . C44_3 C -0.0895(3) 0.5072(3) 0.6459(3) 0.0667(15) Uani 1 d . . H44_3 H -0.1120(3) 0.4856(3) 0.6084(3) 0.080 Uiso 1 calc R . C45_3 C -0.0363(3) 0.5588(3) 0.6380(3) 0.0668(15) Uani 1 d . . H45_3 H -0.0215(3) 0.5733(3) 0.5949(3) 0.080 Uiso 1 calc R . C46_3 C -0.0042(2) 0.5898(3) 0.6930(3) 0.0608(14) Uani 1 d . . H46_3 H 0.0323(2) 0.6265(3) 0.6875(3) 0.073 Uiso 1 calc R . C47_3 C -0.0242(2) 0.5685(3) 0.7547(3) 0.0491(12) Uani 1 d . . H47_3 H -0.0013(2) 0.5890(3) 0.7922(3) 0.059 Uiso 1 calc R . C48_3 C -0.0771(2) 0.5175(3) 0.7625(3) 0.0627(14) Uani 1 d . . H48_3 H -0.0913(2) 0.5029(3) 0.8057(3) 0.075 Uiso 1 calc R . C49_4 C 0.2133(3) 0.8709(3) 0.6903(4) 0.082(2) Uani 1 d . . H49_4 H 0.2466(3) 0.8764(3) 0.6581(4) 0.098 Uiso 1 calc R . C50_4 C 0.2295(3) 0.8674(3) 0.7558(4) 0.072(2) Uani 1 d . . H50_4 H 0.2736(3) 0.8698(3) 0.7693(4) 0.087 Uiso 1 calc R . C51_4 C 0.1810(3) 0.8605(3) 0.8014(3) 0.0640(14) Uani 1 d . . H51_4 H 0.1919(3) 0.8581(3) 0.8470(3) 0.077 Uiso 1 calc R . C52_4 C 0.1172(3) 0.8569(3) 0.7831(3) 0.0577(14) Uani 1 d . . H52_4 H 0.0841(3) 0.8528(3) 0.8157(3) 0.069 Uiso 1 calc R . C53_4 C 0.1013(3) 0.8595(3) 0.7166(3) 0.0626(14) Uani 1 d . . H53_4 H 0.0572(3) 0.8564(3) 0.7032(3) 0.075 Uiso 1 calc R . C54_4 C 0.1493(3) 0.8665(3) 0.6706(3) 0.073(2) Uani 1 d . . H54_4 H 0.1387(3) 0.8684(3) 0.6249(3) 0.087 Uiso 1 calc R . C55_5 C 0.3823(6) 1.4661(6) 0.5251(8) 0.129(4) Uani 1 d . . H55_5 H 0.3466(6) 1.4582(6) 0.4961(8) 0.154 Uiso 1 calc R . C56_5 C 0.3715(6) 1.4910(7) 0.5838(9) 0.147(5) Uani 1 d . . H56_5 H 0.3282(6) 1.4986(7) 0.5990(9) 0.176 Uiso 1 calc R . C57_5 C 0.4207(9) 1.5061(5) 0.6232(4) 0.139(5) Uani 1 d . . H57_5 H 0.4123(9) 1.5275(5) 0.6663(4) 0.167 Uiso 1 calc R . C58_5 C 0.4819(6) 1.4926(6) 0.6051(8) 0.126(4) Uani 1 d . . H58_5 H 0.5163(6) 1.5024(6) 0.6356(8) 0.151 Uiso 1 calc R . C59_5 C 0.4952(5) 1.4646(6) 0.5423(9) 0.116(3) Uani 1 d . . H59_5 H 0.5384(5) 1.4553(6) 0.5274(9) 0.139 Uiso 1 calc R . C60_5 C 0.4426(9) 1.4507(4) 0.5024(4) 0.107(3) Uani 1 d . . H60_5 H 0.4487(9) 1.4301(4) 0.4586(4) 0.128 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_1 0.0280(4) 0.0257(4) 0.0292(4) -0.0009(3) -0.0001(4) -0.0015(3) Ti2_1 0.0303(4) 0.0301(4) 0.0292(4) 0.0000(4) 0.0025(4) -0.0040(3) O1_1 0.0345(15) 0.0279(14) 0.0309(14) 0.0014(13) 0.0015(12) -0.0036(13) N1_1 0.037(2) 0.028(2) 0.031(2) -0.003(2) -0.002(2) -0.0025(14) N2_1 0.040(2) 0.025(2) 0.037(2) -0.006(2) -0.002(2) -0.003(2) N3_1 0.030(2) 0.033(2) 0.032(2) -0.001(2) 0.004(2) -0.001(2) N4_1 0.038(2) 0.029(2) 0.031(2) -0.004(2) 0.003(2) 0.000(2) N5_1 0.037(2) 0.031(2) 0.028(2) 0.000(2) -0.003(2) -0.004(2) N6_1 0.036(2) 0.035(2) 0.030(2) -0.002(2) -0.003(2) -0.007(2) N7_1 0.032(2) 0.028(2) 0.031(2) -0.005(2) -0.005(2) 0.000(2) N8_1 0.037(2) 0.029(2) 0.029(2) -0.0003(15) -0.008(2) -0.006(2) N9_1 0.037(2) 0.028(2) 0.026(2) 0.000(2) 0.001(2) 0.001(2) N10_1 0.035(2) 0.024(2) 0.035(2) -0.003(2) 0.002(2) -0.0005(14) N11_1 0.037(2) 0.035(2) 0.036(2) -0.008(2) 0.005(2) -0.005(2) N12_1 0.046(2) 0.033(2) 0.051(3) -0.009(2) 0.005(2) -0.009(2) N13_1 0.029(2) 0.032(2) 0.029(2) 0.001(2) -0.001(2) -0.002(2) N14_1 0.030(2) 0.034(2) 0.032(2) 0.001(2) 0.000(2) 0.001(2) N15_1 0.032(2) 0.036(2) 0.028(2) -0.004(2) 0.003(2) -0.003(2) N16_1 0.044(2) 0.024(2) 0.034(2) -0.001(2) -0.001(2) -0.0009(15) N17_1 0.038(2) 0.033(2) 0.038(2) 0.001(2) 0.002(2) 0.000(2) N18_1 0.037(2) 0.039(2) 0.066(3) 0.005(2) 0.005(2) 0.009(2) N19_1 0.044(2) 0.030(2) 0.027(2) 0.004(2) -0.001(2) -0.001(2) N20_1 0.053(3) 0.042(2) 0.033(2) 0.003(2) -0.007(2) -0.005(2) N21_1 0.037(2) 0.042(2) 0.039(2) -0.001(2) 0.002(2) -0.008(2) N22_1 0.053(3) 0.052(3) 0.032(2) 0.003(2) 0.005(2) -0.023(2) N23_1 0.041(2) 0.030(2) 0.032(2) -0.001(2) 0.001(2) -0.009(2) N24_1 0.052(2) 0.032(2) 0.033(2) 0.007(2) -0.002(2) -0.011(2) B1_1 0.043(3) 0.025(3) 0.035(3) -0.010(2) -0.001(3) 0.001(2) B2_1 0.040(3) 0.031(3) 0.033(3) -0.001(2) 0.002(3) 0.001(2) B3_1 0.042(3) 0.034(3) 0.036(3) 0.001(2) 0.002(3) 0.001(2) B4_1 0.069(4) 0.046(3) 0.027(3) 0.010(3) 0.005(3) -0.018(3) C1_1 0.041(3) 0.041(3) 0.030(3) 0.006(2) -0.008(2) -0.002(2) C2_1 0.056(3) 0.031(3) 0.055(3) 0.016(2) 0.001(3) 0.001(2) C3_1 0.055(3) 0.021(2) 0.056(4) 0.002(2) 0.003(3) 0.000(2) C4_1 0.045(3) 0.043(3) 0.035(3) -0.005(2) 0.006(3) 0.007(2) C5_1 0.037(3) 0.050(3) 0.042(3) -0.003(2) 0.014(2) -0.001(2) C6_1 0.028(3) 0.043(3) 0.044(3) -0.005(2) 0.004(2) -0.006(2) C7_1 0.029(3) 0.037(2) 0.034(3) 0.007(2) -0.001(2) 0.002(2) C8_1 0.036(3) 0.069(3) 0.031(3) -0.003(2) -0.009(2) -0.013(3) C9_1 0.040(3) 0.053(3) 0.032(3) -0.013(2) -0.001(2) -0.015(2) C10_1 0.033(3) 0.036(2) 0.054(3) 0.009(2) -0.007(2) 0.003(2) C11_1 0.044(3) 0.047(3) 0.071(3) 0.007(3) -0.030(3) 0.001(2) C12_1 0.059(3) 0.044(3) 0.047(3) 0.000(2) -0.020(3) -0.015(2) C13_1 0.041(3) 0.038(3) 0.027(3) 0.002(2) -0.001(2) -0.001(2) C14_1 0.048(3) 0.030(2) 0.046(3) 0.015(2) -0.008(2) 0.004(2) C15_1 0.045(3) 0.020(2) 0.051(3) 0.006(2) 0.002(2) 0.000(2) C16_1 0.046(3) 0.044(3) 0.043(3) -0.009(2) 0.007(2) -0.001(2) C17_1 0.058(3) 0.043(3) 0.049(3) -0.018(2) -0.001(3) 0.003(2) C18_1 0.048(3) 0.030(3) 0.059(3) -0.012(2) -0.009(3) -0.006(2) C19_1 0.027(2) 0.039(2) 0.046(3) -0.005(2) 0.000(2) -0.006(2) C20_1 0.043(3) 0.051(3) 0.053(3) -0.007(2) -0.016(3) -0.011(2) C21_1 0.043(3) 0.047(3) 0.042(3) 0.004(2) -0.016(3) 0.007(2) C22_1 0.045(3) 0.041(3) 0.033(3) -0.008(2) -0.001(2) -0.007(2) C23_1 0.065(3) 0.046(3) 0.040(3) -0.015(2) 0.000(3) -0.002(2) C24_1 0.051(3) 0.032(3) 0.055(3) -0.003(2) 0.000(3) 0.004(2) C25_1 0.044(3) 0.042(3) 0.038(3) 0.004(2) 0.004(2) -0.003(2) C26_1 0.055(3) 0.040(3) 0.051(3) 0.011(2) -0.002(3) 0.005(2) C27_1 0.047(3) 0.035(3) 0.058(3) 0.001(2) -0.005(3) 0.011(2) C28_1 0.040(3) 0.038(3) 0.040(3) -0.006(2) -0.005(2) -0.007(2) C29_1 0.045(3) 0.057(3) 0.052(3) 0.005(3) -0.017(3) -0.005(3) C30_1 0.064(4) 0.051(3) 0.035(3) 0.005(2) -0.014(3) 0.007(3) C31_1 0.042(3) 0.063(3) 0.053(3) -0.018(3) 0.008(3) -0.014(3) C32_1 0.041(3) 0.105(5) 0.070(4) -0.023(4) 0.022(3) -0.037(3) C33_1 0.061(4) 0.090(4) 0.041(3) -0.006(3) 0.012(3) -0.038(3) C34_1 0.033(2) 0.034(2) 0.037(3) -0.005(2) -0.005(2) -0.005(2) C35_1 0.055(3) 0.034(3) 0.052(3) -0.012(2) -0.005(3) -0.009(2) C36_1 0.054(3) 0.024(2) 0.058(4) 0.004(2) -0.009(3) -0.006(2) C37_2 0.063(4) 0.081(4) 0.057(4) 0.015(3) -0.003(3) -0.007(3) C38_2 0.096(5) 0.085(4) 0.044(4) 0.017(3) 0.019(4) 0.035(4) C39_2 0.062(5) 0.111(5) 0.096(6) 0.069(4) 0.048(4) 0.043(4) C40_2 0.049(4) 0.060(4) 0.152(7) 0.045(4) -0.014(5) -0.009(3) C41_2 0.088(4) 0.048(3) 0.061(4) -0.003(3) -0.009(4) 0.013(3) C42_2 0.057(4) 0.069(4) 0.061(4) 0.020(3) 0.013(3) 0.019(3) C43_3 0.052(3) 0.082(4) 0.070(4) 0.001(3) 0.002(3) -0.025(3) C44_3 0.070(4) 0.060(4) 0.070(4) 0.002(3) -0.014(3) -0.001(3) C45_3 0.069(4) 0.067(4) 0.064(4) 0.024(3) 0.008(3) -0.003(3) C46_3 0.054(3) 0.059(3) 0.070(4) 0.009(3) 0.000(3) -0.010(3) C47_3 0.043(3) 0.044(3) 0.060(4) -0.002(2) 0.007(3) 0.003(2) C48_3 0.053(3) 0.068(4) 0.068(4) -0.010(3) 0.007(3) -0.006(3) C49_4 0.073(5) 0.064(4) 0.109(6) -0.032(4) 0.022(4) -0.018(3) C50_4 0.061(4) 0.056(4) 0.100(5) -0.017(3) -0.019(4) 0.007(3) C51_4 0.076(4) 0.045(3) 0.071(4) 0.002(3) -0.012(4) 0.002(3) C52_4 0.081(4) 0.031(3) 0.061(4) 0.003(2) 0.007(3) -0.006(3) C53_4 0.062(4) 0.055(3) 0.070(4) -0.002(3) -0.005(3) -0.013(3) C54_4 0.086(5) 0.074(4) 0.058(4) -0.012(3) 0.007(4) -0.027(3) C55_5 0.107(9) 0.099(7) 0.180(13) 0.069(7) -0.051(8) -0.050(6) C56_5 0.152(12) 0.139(9) 0.149(10) 0.096(8) 0.070(11) 0.033(8) C57_5 0.235(15) 0.114(7) 0.069(6) -0.006(5) -0.036(9) 0.044(9) C58_5 0.109(8) 0.108(7) 0.160(12) 0.035(7) -0.063(7) -0.009(6) C59_5 0.103(8) 0.074(5) 0.171(9) 0.064(6) 0.041(8) 0.027(5) C60_5 0.198(10) 0.049(4) 0.073(5) 0.007(3) -0.011(8) 0.012(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1_1 O1_1 1.810(3) . ? Ti1_1 N7_1 2.152(3) . ? Ti1_1 N9_1 2.158(3) . ? Ti1_1 N1_1 2.181(3) . ? Ti1_1 N5_1 2.195(3) . ? Ti1_1 N3_1 2.260(3) . ? Ti2_1 O1_1 1.812(3) . ? Ti2_1 N13_1 2.151(3) . ? Ti2_1 N15_1 2.169(3) . ? Ti2_1 N19_1 2.182(3) . ? Ti2_1 N23_1 2.184(3) . ? Ti2_1 N21_1 2.254(3) . ? N1_1 C1_1 1.352(5) . ? N1_1 N2_1 1.362(4) . ? N2_1 C3_1 1.332(5) . ? N2_1 B1_1 1.548(6) . ? N3_1 C6_1 1.336(5) . ? N3_1 N4_1 1.379(4) . ? N4_1 C4_1 1.335(5) . ? N4_1 B1_1 1.525(6) . ? N5_1 C7_1 1.325(5) . ? N5_1 N6_1 1.383(4) . ? N6_1 C9_1 1.342(5) . ? N6_1 B1_1 1.536(6) . ? N7_1 C10_1 1.330(5) . ? N7_1 N8_1 1.372(4) . ? N8_1 C12_1 1.341(5) . ? N8_1 B2_1 1.547(6) . ? N9_1 C13_1 1.334(5) . ? N9_1 N10_1 1.387(4) . ? N10_1 C15_1 1.334(4) . ? N10_1 B2_1 1.568(6) . ? N11_1 C16_1 1.350(5) . ? N11_1 N12_1 1.365(4) . ? N11_1 B2_1 1.528(5) . ? N12_1 C18_1 1.334(5) . ? N13_1 C19_1 1.341(5) . ? N13_1 N14_1 1.377(4) . ? N14_1 C21_1 1.332(5) . ? N14_1 B3_1 1.562(5) . ? N15_1 C22_1 1.339(5) . ? N15_1 N16_1 1.363(4) . ? N16_1 C24_1 1.334(5) . ? N16_1 B3_1 1.556(6) . ? N17_1 C25_1 1.340(5) . ? N17_1 N18_1 1.365(4) . ? N17_1 B3_1 1.531(5) . ? N18_1 C27_1 1.321(5) . ? N19_1 C28_1 1.340(5) . ? N19_1 N20_1 1.377(4) . ? N20_1 C30_1 1.354(5) . ? N20_1 B4_1 1.542(6) . ? N21_1 C31_1 1.339(5) . ? N21_1 N22_1 1.369(4) . ? N22_1 C33_1 1.343(6) . ? N22_1 B4_1 1.519(7) . ? N23_1 C34_1 1.341(5) . ? N23_1 N24_1 1.375(4) . ? N24_1 C36_1 1.351(5) . ? N24_1 B4_1 1.537(6) . ? C1_1 C2_1 1.380(5) . ? C2_1 C3_1 1.369(6) . ? C4_1 C5_1 1.363(5) . ? C5_1 C6_1 1.382(6) . ? C7_1 C8_1 1.383(5) . ? C8_1 C9_1 1.360(6) . ? C10_1 C11_1 1.358(5) . ? C11_1 C12_1 1.373(6) . ? C13_1 C14_1 1.385(5) . ? C14_1 C15_1 1.378(6) . ? C16_1 C17_1 1.353(5) . ? C17_1 C18_1 1.383(6) . ? C19_1 C20_1 1.376(6) . ? C20_1 C21_1 1.379(5) . ? C22_1 C23_1 1.381(6) . ? C23_1 C24_1 1.377(6) . ? C25_1 C26_1 1.378(6) . ? C26_1 C27_1 1.386(6) . ? C28_1 C29_1 1.377(6) . ? C29_1 C30_1 1.347(6) . ? C31_1 C32_1 1.388(7) . ? C32_1 C33_1 1.367(7) . ? C34_1 C35_1 1.388(5) . ? C35_1 C36_1 1.368(6) . ? C37_2 C38_2 1.350(7) . ? C37_2 C42_2 1.361(7) . ? C38_2 C39_2 1.344(8) . ? C39_2 C40_2 1.382(9) . ? C40_2 C41_2 1.370(8) . ? C41_2 C42_2 1.343(7) . ? C43_3 C48_3 1.368(7) . ? C43_3 C44_3 1.376(7) . ? C44_3 C45_3 1.371(7) . ? C45_3 C46_3 1.382(7) . ? C46_3 C47_3 1.356(6) . ? C47_3 C48_3 1.359(6) . ? C49_4 C50_4 1.367(8) . ? C49_4 C54_4 1.379(7) . ? C50_4 C51_4 1.363(7) . ? C51_4 C52_4 1.366(7) . ? C52_4 C53_4 1.386(7) . ? C53_4 C54_4 1.363(7) . ? C55_5 C56_5 1.270(12) . ? C55_5 C60_5 1.346(11) . ? C56_5 C57_5 1.311(13) . ? C57_5 C58_5 1.329(12) . ? C58_5 C59_5 1.372(11) . ? C59_5 C60_5 1.369(11) . ? 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 O1_1 Ti1_1 N7_1 99.66(13) . . ? O1_1 Ti1_1 N9_1 99.02(11) . . ? N7_1 Ti1_1 N9_1 85.43(12) . . ? O1_1 Ti1_1 N1_1 93.80(11) . . ? N7_1 Ti1_1 N1_1 91.26(12) . . ? N9_1 Ti1_1 N1_1 167.12(12) . . ? O1_1 Ti1_1 N5_1 91.54(12) . . ? N7_1 Ti1_1 N5_1 168.73(12) . . ? N9_1 Ti1_1 N5_1 94.02(12) . . ? N1_1 Ti1_1 N5_1 86.79(12) . . ? O1_1 Ti1_1 N3_1 169.38(11) . . ? N7_1 Ti1_1 N3_1 88.75(12) . . ? N9_1 Ti1_1 N3_1 88.03(12) . . ? N1_1 Ti1_1 N3_1 79.45(12) . . ? N5_1 Ti1_1 N3_1 79.99(12) . . ? O1_1 Ti2_1 N13_1 100.12(13) . . ? O1_1 Ti2_1 N15_1 100.67(11) . . ? N13_1 Ti2_1 N15_1 86.03(12) . . ? O1_1 Ti2_1 N19_1 93.13(12) . . ? N13_1 Ti2_1 N19_1 166.72(13) . . ? N15_1 Ti2_1 N19_1 92.52(13) . . ? O1_1 Ti2_1 N23_1 94.56(11) . . ? N13_1 Ti2_1 N23_1 92.78(12) . . ? N15_1 Ti2_1 N23_1 164.70(12) . . ? N19_1 Ti2_1 N23_1 85.15(12) . . ? O1_1 Ti2_1 N21_1 171.97(13) . . ? N13_1 Ti2_1 N21_1 85.42(12) . . ? N15_1 Ti2_1 N21_1 85.43(12) . . ? N19_1 Ti2_1 N21_1 81.30(13) . . ? N23_1 Ti2_1 N21_1 79.27(12) . . ? Ti1_1 O1_1 Ti2_1 167.41(14) . . ? C1_1 N1_1 N2_1 105.6(3) . . ? C1_1 N1_1 Ti1_1 132.8(3) . . ? N2_1 N1_1 Ti1_1 121.5(2) . . ? C3_1 N2_1 N1_1 110.2(3) . . ? C3_1 N2_1 B1_1 129.8(4) . . ? N1_1 N2_1 B1_1 119.9(3) . . ? C6_1 N3_1 N4_1 105.4(3) . . ? C6_1 N3_1 Ti1_1 134.3(3) . . ? N4_1 N3_1 Ti1_1 120.3(2) . . ? C4_1 N4_1 N3_1 109.5(3) . . ? C4_1 N4_1 B1_1 131.4(4) . . ? N3_1 N4_1 B1_1 119.0(3) . . ? C7_1 N5_1 N6_1 106.2(3) . . ? C7_1 N5_1 Ti1_1 131.9(3) . . ? N6_1 N5_1 Ti1_1 119.9(2) . . ? C9_1 N6_1 N5_1 108.5(3) . . ? C9_1 N6_1 B1_1 131.3(4) . . ? N5_1 N6_1 B1_1 120.1(3) . . ? C10_1 N7_1 N8_1 105.7(3) . . ? C10_1 N7_1 Ti1_1 131.5(3) . . ? N8_1 N7_1 Ti1_1 122.9(2) . . ? C12_1 N8_1 N7_1 108.4(3) . . ? C12_1 N8_1 B2_1 129.9(3) . . ? N7_1 N8_1 B2_1 121.2(3) . . ? C13_1 N9_1 N10_1 105.3(3) . . ? C13_1 N9_1 Ti1_1 132.0(3) . . ? N10_1 N9_1 Ti1_1 122.6(2) . . ? C15_1 N10_1 N9_1 109.1(3) . . ? C15_1 N10_1 B2_1 129.7(3) . . ? N9_1 N10_1 B2_1 120.6(3) . . ? C16_1 N11_1 N12_1 110.1(3) . . ? C16_1 N11_1 B2_1 126.3(4) . . ? N12_1 N11_1 B2_1 123.4(3) . . ? C18_1 N12_1 N11_1 104.6(3) . . ? C19_1 N13_1 N14_1 105.8(3) . . ? C19_1 N13_1 Ti2_1 129.3(3) . . ? N14_1 N13_1 Ti2_1 124.4(2) . . ? C21_1 N14_1 N13_1 109.5(3) . . ? C21_1 N14_1 B3_1 130.7(3) . . ? N13_1 N14_1 B3_1 118.9(3) . . ? C22_1 N15_1 N16_1 106.1(3) . . ? C22_1 N15_1 Ti2_1 130.0(3) . . ? N16_1 N15_1 Ti2_1 123.9(2) . . ? C24_1 N16_1 N15_1 109.4(3) . . ? C24_1 N16_1 B3_1 129.3(4) . . ? N15_1 N16_1 B3_1 120.8(3) . . ? C25_1 N17_1 N18_1 110.7(3) . . ? C25_1 N17_1 B3_1 125.1(4) . . ? N18_1 N17_1 B3_1 124.1(3) . . ? C27_1 N18_1 N17_1 104.6(3) . . ? C28_1 N19_1 N20_1 105.9(3) . . ? C28_1 N19_1 Ti2_1 132.3(3) . . ? N20_1 N19_1 Ti2_1 121.0(3) . . ? C30_1 N20_1 N19_1 107.9(3) . . ? C30_1 N20_1 B4_1 131.2(4) . . ? N19_1 N20_1 B4_1 120.7(4) . . ? C31_1 N21_1 N22_1 106.9(4) . . ? C31_1 N21_1 Ti2_1 133.1(3) . . ? N22_1 N21_1 Ti2_1 120.0(3) . . ? C33_1 N22_1 N21_1 108.8(4) . . ? C33_1 N22_1 B4_1 130.4(4) . . ? N21_1 N22_1 B4_1 120.7(4) . . ? C34_1 N23_1 N24_1 105.8(3) . . ? C34_1 N23_1 Ti2_1 132.5(3) . . ? N24_1 N23_1 Ti2_1 121.2(2) . . ? C36_1 N24_1 N23_1 109.7(3) . . ? C36_1 N24_1 B4_1 129.9(4) . . ? N23_1 N24_1 B4_1 120.4(3) . . ? N4_1 B1_1 N6_1 110.0(3) . . ? N4_1 B1_1 N2_1 107.7(3) . . ? N6_1 B1_1 N2_1 109.2(4) . . ? N11_1 B2_1 N8_1 109.0(4) . . ? N11_1 B2_1 N10_1 108.7(3) . . ? N8_1 B2_1 N10_1 108.2(3) . . ? N17_1 B3_1 N16_1 108.9(3) . . ? N17_1 B3_1 N14_1 110.3(4) . . ? N16_1 B3_1 N14_1 108.0(3) . . ? N22_1 B4_1 N24_1 107.9(4) . . ? N22_1 B4_1 N20_1 108.8(4) . . ? N24_1 B4_1 N20_1 108.0(4) . . ? N1_1 C1_1 C2_1 110.1(4) . . ? C3_1 C2_1 C1_1 105.5(4) . . ? N2_1 C3_1 C2_1 108.6(4) . . ? N4_1 C4_1 C5_1 109.1(4) . . ? C4_1 C5_1 C6_1 105.1(4) . . ? N3_1 C6_1 C5_1 111.0(4) . . ? N5_1 C7_1 C8_1 110.9(4) . . ? C9_1 C8_1 C7_1 105.1(4) . . ? N6_1 C9_1 C8_1 109.3(4) . . ? N7_1 C10_1 C11_1 112.2(4) . . ? C10_1 C11_1 C12_1 104.2(4) . . ? N8_1 C12_1 C11_1 109.4(4) . . ? N9_1 C13_1 C14_1 111.9(4) . . ? C15_1 C14_1 C13_1 103.9(4) . . ? N10_1 C15_1 C14_1 109.7(4) . . ? N11_1 C16_1 C17_1 108.6(4) . . ? C16_1 C17_1 C18_1 104.7(4) . . ? N12_1 C18_1 C17_1 111.9(4) . . ? N13_1 C19_1 C20_1 110.8(4) . . ? C19_1 C20_1 C21_1 105.1(4) . . ? N14_1 C21_1 C20_1 108.8(4) . . ? N15_1 C22_1 C23_1 110.9(4) . . ? C24_1 C23_1 C22_1 104.3(4) . . ? N16_1 C24_1 C23_1 109.3(4) . . ? N17_1 C25_1 C26_1 108.2(4) . . ? C25_1 C26_1 C27_1 103.6(4) . . ? N18_1 C27_1 C26_1 112.8(4) . . ? N19_1 C28_1 C29_1 111.0(4) . . ? C30_1 C29_1 C28_1 105.1(4) . . ? C29_1 C30_1 N20_1 110.0(4) . . ? N21_1 C31_1 C32_1 109.8(5) . . ? C33_1 C32_1 C31_1 105.4(5) . . ? N22_1 C33_1 C32_1 109.1(5) . . ? N23_1 C34_1 C35_1 110.6(4) . . ? C36_1 C35_1 C34_1 105.6(4) . . ? N24_1 C36_1 C35_1 108.3(4) . . ? C38_2 C37_2 C42_2 119.9(6) . . ? C39_2 C38_2 C37_2 121.4(6) . . ? C38_2 C39_2 C40_2 118.4(6) . . ? C41_2 C40_2 C39_2 120.5(6) . . ? C42_2 C41_2 C40_2 119.2(6) . . ? C41_2 C42_2 C37_2 120.6(6) . . ? C48_3 C43_3 C44_3 120.3(5) . . ? C45_3 C44_3 C43_3 119.2(5) . . ? C44_3 C45_3 C46_3 119.7(5) . . ? C47_3 C46_3 C45_3 120.6(5) . . ? C48_3 C47_3 C46_3 119.7(5) . . ? C47_3 C48_3 C43_3 120.5(5) . . ? C50_4 C49_4 C54_4 120.8(6) . . ? C51_4 C50_4 C49_4 118.8(6) . . ? C50_4 C51_4 C52_4 121.6(6) . . ? C51_4 C52_4 C53_4 119.3(5) . . ? C54_4 C53_4 C52_4 119.6(5) . . ? C53_4 C54_4 C49_4 120.0(6) . . ? C56_5 C55_5 C60_5 122.5(11) . . ? C55_5 C56_5 C57_5 119.2(12) . . ? C56_5 C57_5 C58_5 122.6(11) . . ? C57_5 C58_5 C59_5 119.6(10) . . ? C60_5 C59_5 C58_5 116.1(8) . . ? C55_5 C60_5 C59_5 120.0(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7_1 Ti1_1 O1_1 Ti2_1 -121.6(8) . . . . ? N9_1 Ti1_1 O1_1 Ti2_1 151.6(8) . . . . ? N1_1 Ti1_1 O1_1 Ti2_1 -29.6(8) . . . . ? N5_1 Ti1_1 O1_1 Ti2_1 57.2(8) . . . . ? N3_1 Ti1_1 O1_1 Ti2_1 20.4(13) . . . . ? N13_1 Ti2_1 O1_1 Ti1_1 -86.7(8) . . . . ? N15_1 Ti2_1 O1_1 Ti1_1 -174.5(8) . . . . ? N19_1 Ti2_1 O1_1 Ti1_1 92.3(8) . . . . ? N23_1 Ti2_1 O1_1 Ti1_1 7.0(8) . . . . ? N21_1 Ti2_1 O1_1 Ti1_1 46.5(15) . . . . ? O1_1 Ti1_1 N1_1 C1_1 -52.0(4) . . . . ? N7_1 Ti1_1 N1_1 C1_1 47.7(4) . . . . ? N9_1 Ti1_1 N1_1 C1_1 122.6(6) . . . . ? N5_1 Ti1_1 N1_1 C1_1 -143.4(4) . . . . ? N3_1 Ti1_1 N1_1 C1_1 136.2(4) . . . . ? O1_1 Ti1_1 N1_1 N2_1 125.1(3) . . . . ? N7_1 Ti1_1 N1_1 N2_1 -135.2(3) . . . . ? N9_1 Ti1_1 N1_1 N2_1 -60.3(7) . . . . ? N5_1 Ti1_1 N1_1 N2_1 33.7(3) . . . . ? N3_1 Ti1_1 N1_1 N2_1 -46.7(3) . . . . ? C1_1 N1_1 N2_1 C3_1 -0.1(4) . . . . ? Ti1_1 N1_1 N2_1 C3_1 -177.9(3) . . . . ? C1_1 N1_1 N2_1 B1_1 -177.1(3) . . . . ? Ti1_1 N1_1 N2_1 B1_1 5.1(5) . . . . ? O1_1 Ti1_1 N3_1 C6_1 177.5(6) . . . . ? N7_1 Ti1_1 N3_1 C6_1 -39.9(4) . . . . ? N9_1 Ti1_1 N3_1 C6_1 45.6(4) . . . . ? N1_1 Ti1_1 N3_1 C6_1 -131.4(4) . . . . ? N5_1 Ti1_1 N3_1 C6_1 140.0(4) . . . . ? O1_1 Ti1_1 N3_1 N4_1 -5.9(8) . . . . ? N7_1 Ti1_1 N3_1 N4_1 136.7(3) . . . . ? N9_1 Ti1_1 N3_1 N4_1 -137.8(3) . . . . ? N1_1 Ti1_1 N3_1 N4_1 45.2(3) . . . . ? N5_1 Ti1_1 N3_1 N4_1 -43.4(3) . . . . ? C6_1 N3_1 N4_1 C4_1 -0.2(4) . . . . ? Ti1_1 N3_1 N4_1 C4_1 -177.6(3) . . . . ? C6_1 N3_1 N4_1 B1_1 175.9(3) . . . . ? Ti1_1 N3_1 N4_1 B1_1 -1.5(4) . . . . ? O1_1 Ti1_1 N5_1 C7_1 38.1(3) . . . . ? N7_1 Ti1_1 N5_1 C7_1 -147.9(5) . . . . ? N9_1 Ti1_1 N5_1 C7_1 -61.1(4) . . . . ? N1_1 Ti1_1 N5_1 C7_1 131.8(4) . . . . ? N3_1 Ti1_1 N5_1 C7_1 -148.4(4) . . . . ? O1_1 Ti1_1 N5_1 N6_1 -123.5(3) . . . . ? N7_1 Ti1_1 N5_1 N6_1 50.6(7) . . . . ? N9_1 Ti1_1 N5_1 N6_1 137.4(3) . . . . ? N1_1 Ti1_1 N5_1 N6_1 -29.8(3) . . . . ? N3_1 Ti1_1 N5_1 N6_1 50.1(3) . . . . ? C7_1 N5_1 N6_1 C9_1 -0.7(4) . . . . ? Ti1_1 N5_1 N6_1 C9_1 165.1(2) . . . . ? C7_1 N5_1 N6_1 B1_1 -178.3(3) . . . . ? Ti1_1 N5_1 N6_1 B1_1 -12.5(4) . . . . ? O1_1 Ti1_1 N7_1 C10_1 116.0(3) . . . . ? N9_1 Ti1_1 N7_1 C10_1 -145.6(4) . . . . ? N1_1 Ti1_1 N7_1 C10_1 21.9(4) . . . . ? N5_1 Ti1_1 N7_1 C10_1 -58.0(8) . . . . ? N3_1 Ti1_1 N7_1 C10_1 -57.5(4) . . . . ? O1_1 Ti1_1 N7_1 N8_1 -65.6(3) . . . . ? N9_1 Ti1_1 N7_1 N8_1 32.8(3) . . . . ? N1_1 Ti1_1 N7_1 N8_1 -159.6(3) . . . . ? N5_1 Ti1_1 N7_1 N8_1 120.5(6) . . . . ? N3_1 Ti1_1 N7_1 N8_1 120.9(3) . . . . ? C10_1 N7_1 N8_1 C12_1 0.1(4) . . . . ? Ti1_1 N7_1 N8_1 C12_1 -178.7(3) . . . . ? C10_1 N7_1 N8_1 B2_1 -173.1(3) . . . . ? Ti1_1 N7_1 N8_1 B2_1 8.1(4) . . . . ? O1_1 Ti1_1 N9_1 C13_1 -111.8(4) . . . . ? N7_1 Ti1_1 N9_1 C13_1 149.1(4) . . . . ? N1_1 Ti1_1 N9_1 C13_1 73.6(7) . . . . ? N5_1 Ti1_1 N9_1 C13_1 -19.6(4) . . . . ? N3_1 Ti1_1 N9_1 C13_1 60.2(4) . . . . ? O1_1 Ti1_1 N9_1 N10_1 64.0(3) . . . . ? N7_1 Ti1_1 N9_1 N10_1 -35.0(3) . . . . ? N1_1 Ti1_1 N9_1 N10_1 -110.5(6) . . . . ? N5_1 Ti1_1 N9_1 N10_1 156.2(3) . . . . ? N3_1 Ti1_1 N9_1 N10_1 -123.9(3) . . . . ? C13_1 N9_1 N10_1 C15_1 1.4(4) . . . . ? Ti1_1 N9_1 N10_1 C15_1 -175.5(2) . . . . ? C13_1 N9_1 N10_1 B2_1 173.9(4) . . . . ? Ti1_1 N9_1 N10_1 B2_1 -2.9(4) . . . . ? C16_1 N11_1 N12_1 C18_1 0.6(4) . . . . ? B2_1 N11_1 N12_1 C18_1 -175.5(4) . . . . ? O1_1 Ti2_1 N13_1 C19_1 113.2(3) . . . . ? N15_1 Ti2_1 N13_1 C19_1 -146.6(3) . . . . ? N19_1 Ti2_1 N13_1 C19_1 -62.5(7) . . . . ? N23_1 Ti2_1 N13_1 C19_1 18.1(3) . . . . ? N21_1 Ti2_1 N13_1 C19_1 -60.9(3) . . . . ? O1_1 Ti2_1 N13_1 N14_1 -76.4(3) . . . . ? N15_1 Ti2_1 N13_1 N14_1 23.8(3) . . . . ? N19_1 Ti2_1 N13_1 N14_1 107.9(5) . . . . ? N23_1 Ti2_1 N13_1 N14_1 -171.5(3) . . . . ? N21_1 Ti2_1 N13_1 N14_1 109.5(3) . . . . ? C19_1 N13_1 N14_1 C21_1 0.2(4) . . . . ? Ti2_1 N13_1 N14_1 C21_1 -172.0(3) . . . . ? C19_1 N13_1 N14_1 B3_1 -170.2(3) . . . . ? Ti2_1 N13_1 N14_1 B3_1 17.5(4) . . . . ? O1_1 Ti2_1 N15_1 C22_1 -110.4(4) . . . . ? N13_1 Ti2_1 N15_1 C22_1 150.1(4) . . . . ? N19_1 Ti2_1 N15_1 C22_1 -16.7(4) . . . . ? N23_1 Ti2_1 N15_1 C22_1 64.1(7) . . . . ? N21_1 Ti2_1 N15_1 C22_1 64.4(4) . . . . ? O1_1 Ti2_1 N15_1 N16_1 69.6(3) . . . . ? N13_1 Ti2_1 N15_1 N16_1 -29.9(3) . . . . ? N19_1 Ti2_1 N15_1 N16_1 163.3(3) . . . . ? N23_1 Ti2_1 N15_1 N16_1 -115.9(5) . . . . ? N21_1 Ti2_1 N15_1 N16_1 -115.6(3) . . . . ? C22_1 N15_1 N16_1 C24_1 1.0(4) . . . . ? Ti2_1 N15_1 N16_1 C24_1 -179.0(3) . . . . ? C22_1 N15_1 N16_1 B3_1 174.1(4) . . . . ? Ti2_1 N15_1 N16_1 B3_1 -5.9(5) . . . . ? C25_1 N17_1 N18_1 C27_1 -0.3(4) . . . . ? B3_1 N17_1 N18_1 C27_1 176.1(4) . . . . ? O1_1 Ti2_1 N19_1 C28_1 38.5(4) . . . . ? N13_1 Ti2_1 N19_1 C28_1 -145.7(5) . . . . ? N15_1 Ti2_1 N19_1 C28_1 -62.4(4) . . . . ? N23_1 Ti2_1 N19_1 C28_1 132.8(4) . . . . ? N21_1 Ti2_1 N19_1 C28_1 -147.4(4) . . . . ? O1_1 Ti2_1 N19_1 N20_1 -129.4(3) . . . . ? N13_1 Ti2_1 N19_1 N20_1 46.4(7) . . . . ? N15_1 Ti2_1 N19_1 N20_1 129.7(3) . . . . ? N23_1 Ti2_1 N19_1 N20_1 -35.1(3) . . . . ? N21_1 Ti2_1 N19_1 N20_1 44.8(3) . . . . ? C28_1 N19_1 N20_1 C30_1 -0.5(4) . . . . ? Ti2_1 N19_1 N20_1 C30_1 170.2(3) . . . . ? C28_1 N19_1 N20_1 B4_1 -176.3(4) . . . . ? Ti2_1 N19_1 N20_1 B4_1 -5.6(5) . . . . ? O1_1 Ti2_1 N21_1 C31_1 -173.0(8) . . . . ? N13_1 Ti2_1 N21_1 C31_1 -39.0(4) . . . . ? N15_1 Ti2_1 N21_1 C31_1 47.3(4) . . . . ? N19_1 Ti2_1 N21_1 C31_1 140.6(4) . . . . ? N23_1 Ti2_1 N21_1 C31_1 -132.8(4) . . . . ? O1_1 Ti2_1 N21_1 N22_1 5.1(11) . . . . ? N13_1 Ti2_1 N21_1 N22_1 139.0(3) . . . . ? N15_1 Ti2_1 N21_1 N22_1 -134.6(3) . . . . ? N19_1 Ti2_1 N21_1 N22_1 -41.4(3) . . . . ? N23_1 Ti2_1 N21_1 N22_1 45.3(3) . . . . ? C31_1 N21_1 N22_1 C33_1 0.3(5) . . . . ? Ti2_1 N21_1 N22_1 C33_1 -178.2(3) . . . . ? C31_1 N21_1 N22_1 B4_1 176.5(4) . . . . ? Ti2_1 N21_1 N22_1 B4_1 -2.1(5) . . . . ? O1_1 Ti2_1 N23_1 C34_1 -43.8(4) . . . . ? N13_1 Ti2_1 N23_1 C34_1 56.5(4) . . . . ? N15_1 Ti2_1 N23_1 C34_1 141.6(5) . . . . ? N19_1 Ti2_1 N23_1 C34_1 -136.6(4) . . . . ? N21_1 Ti2_1 N23_1 C34_1 141.4(4) . . . . ? O1_1 Ti2_1 N23_1 N24_1 127.3(3) . . . . ? N13_1 Ti2_1 N23_1 N24_1 -132.3(3) . . . . ? N15_1 Ti2_1 N23_1 N24_1 -47.2(6) . . . . ? N19_1 Ti2_1 N23_1 N24_1 34.5(3) . . . . ? N21_1 Ti2_1 N23_1 N24_1 -47.5(3) . . . . ? C34_1 N23_1 N24_1 C36_1 0.0(4) . . . . ? Ti2_1 N23_1 N24_1 C36_1 -173.2(3) . . . . ? C34_1 N23_1 N24_1 B4_1 -179.7(4) . . . . ? Ti2_1 N23_1 N24_1 B4_1 7.0(5) . . . . ? C4_1 N4_1 B1_1 N6_1 -125.0(4) . . . . ? N3_1 N4_1 B1_1 N6_1 59.9(5) . . . . ? C4_1 N4_1 B1_1 N2_1 116.2(5) . . . . ? N3_1 N4_1 B1_1 N2_1 -59.0(4) . . . . ? C9_1 N6_1 B1_1 N4_1 130.3(4) . . . . ? N5_1 N6_1 B1_1 N4_1 -52.8(5) . . . . ? C9_1 N6_1 B1_1 N2_1 -111.7(4) . . . . ? N5_1 N6_1 B1_1 N2_1 65.1(4) . . . . ? C3_1 N2_1 B1_1 N4_1 -117.8(4) . . . . ? N1_1 N2_1 B1_1 N4_1 58.6(5) . . . . ? C3_1 N2_1 B1_1 N6_1 122.8(4) . . . . ? N1_1 N2_1 B1_1 N6_1 -60.7(5) . . . . ? C16_1 N11_1 B2_1 N8_1 -117.6(4) . . . . ? N12_1 N11_1 B2_1 N8_1 57.9(5) . . . . ? C16_1 N11_1 B2_1 N10_1 124.7(4) . . . . ? N12_1 N11_1 B2_1 N10_1 -59.8(5) . . . . ? C12_1 N8_1 B2_1 N11_1 11.3(6) . . . . ? N7_1 N8_1 B2_1 N11_1 -177.1(3) . . . . ? C12_1 N8_1 B2_1 N10_1 129.3(4) . . . . ? N7_1 N8_1 B2_1 N10_1 -59.0(4) . . . . ? C15_1 N10_1 B2_1 N11_1 -15.1(6) . . . . ? N9_1 N10_1 B2_1 N11_1 174.0(3) . . . . ? C15_1 N10_1 B2_1 N8_1 -133.4(4) . . . . ? N9_1 N10_1 B2_1 N8_1 55.8(5) . . . . ? C25_1 N17_1 B3_1 N16_1 114.0(4) . . . . ? N18_1 N17_1 B3_1 N16_1 -62.0(5) . . . . ? C25_1 N17_1 B3_1 N14_1 -127.7(4) . . . . ? N18_1 N17_1 B3_1 N14_1 56.4(5) . . . . ? C24_1 N16_1 B3_1 N17_1 -11.2(6) . . . . ? N15_1 N16_1 B3_1 N17_1 177.2(3) . . . . ? C24_1 N16_1 B3_1 N14_1 -130.9(4) . . . . ? N15_1 N16_1 B3_1 N14_1 57.5(5) . . . . ? C21_1 N14_1 B3_1 N17_1 9.1(6) . . . . ? N13_1 N14_1 B3_1 N17_1 177.2(3) . . . . ? C21_1 N14_1 B3_1 N16_1 128.0(4) . . . . ? N13_1 N14_1 B3_1 N16_1 -63.9(4) . . . . ? C33_1 N22_1 B4_1 N24_1 117.7(5) . . . . ? N21_1 N22_1 B4_1 N24_1 -57.5(5) . . . . ? C33_1 N22_1 B4_1 N20_1 -125.4(5) . . . . ? N21_1 N22_1 B4_1 N20_1 59.4(5) . . . . ? C36_1 N24_1 B4_1 N22_1 -124.1(5) . . . . ? N23_1 N24_1 B4_1 N22_1 55.6(5) . . . . ? C36_1 N24_1 B4_1 N20_1 118.5(5) . . . . ? N23_1 N24_1 B4_1 N20_1 -61.8(5) . . . . ? C30_1 N20_1 B4_1 N22_1 129.5(5) . . . . ? N19_1 N20_1 B4_1 N22_1 -55.9(5) . . . . ? C30_1 N20_1 B4_1 N24_1 -113.7(5) . . . . ? N19_1 N20_1 B4_1 N24_1 61.0(5) . . . . ? N2_1 N1_1 C1_1 C2_1 0.7(4) . . . . ? Ti1_1 N1_1 C1_1 C2_1 178.2(3) . . . . ? N1_1 C1_1 C2_1 C3_1 -1.1(5) . . . . ? N1_1 N2_1 C3_1 C2_1 -0.6(5) . . . . ? B1_1 N2_1 C3_1 C2_1 176.1(4) . . . . ? C1_1 C2_1 C3_1 N2_1 1.1(5) . . . . ? N3_1 N4_1 C4_1 C5_1 0.1(5) . . . . ? B1_1 N4_1 C4_1 C5_1 -175.4(4) . . . . ? N4_1 C4_1 C5_1 C6_1 0.1(5) . . . . ? N4_1 N3_1 C6_1 C5_1 0.2(4) . . . . ? Ti1_1 N3_1 C6_1 C5_1 177.2(3) . . . . ? C4_1 C5_1 C6_1 N3_1 -0.2(5) . . . . ? N6_1 N5_1 C7_1 C8_1 1.1(4) . . . . ? Ti1_1 N5_1 C7_1 C8_1 -162.3(3) . . . . ? N5_1 C7_1 C8_1 C9_1 -1.0(5) . . . . ? N5_1 N6_1 C9_1 C8_1 0.1(5) . . . . ? B1_1 N6_1 C9_1 C8_1 177.3(4) . . . . ? C7_1 C8_1 C9_1 N6_1 0.5(5) . . . . ? N8_1 N7_1 C10_1 C11_1 -0.6(5) . . . . ? Ti1_1 N7_1 C10_1 C11_1 178.1(3) . . . . ? N7_1 C10_1 C11_1 C12_1 0.8(5) . . . . ? N7_1 N8_1 C12_1 C11_1 0.4(5) . . . . ? B2_1 N8_1 C12_1 C11_1 172.9(4) . . . . ? C10_1 C11_1 C12_1 N8_1 -0.7(5) . . . . ? N10_1 N9_1 C13_1 C14_1 -1.6(4) . . . . ? Ti1_1 N9_1 C13_1 C14_1 174.8(3) . . . . ? N9_1 C13_1 C14_1 C15_1 1.2(5) . . . . ? N9_1 N10_1 C15_1 C14_1 -0.7(4) . . . . ? B2_1 N10_1 C15_1 C14_1 -172.3(4) . . . . ? C13_1 C14_1 C15_1 N10_1 -0.3(5) . . . . ? N12_1 N11_1 C16_1 C17_1 -0.3(5) . . . . ? B2_1 N11_1 C16_1 C17_1 175.7(4) . . . . ? N11_1 C16_1 C17_1 C18_1 -0.1(5) . . . . ? N11_1 N12_1 C18_1 C17_1 -0.7(5) . . . . ? C16_1 C17_1 C18_1 N12_1 0.5(5) . . . . ? N14_1 N13_1 C19_1 C20_1 -0.4(4) . . . . ? Ti2_1 N13_1 C19_1 C20_1 171.3(3) . . . . ? N13_1 C19_1 C20_1 C21_1 0.4(5) . . . . ? N13_1 N14_1 C21_1 C20_1 0.0(5) . . . . ? B3_1 N14_1 C21_1 C20_1 169.0(4) . . . . ? C19_1 C20_1 C21_1 N14_1 -0.3(5) . . . . ? N16_1 N15_1 C22_1 C23_1 -0.9(5) . . . . ? Ti2_1 N15_1 C22_1 C23_1 179.1(3) . . . . ? N15_1 C22_1 C23_1 C24_1 0.4(5) . . . . ? N15_1 N16_1 C24_1 C23_1 -0.8(5) . . . . ? B3_1 N16_1 C24_1 C23_1 -173.1(4) . . . . ? C22_1 C23_1 C24_1 N16_1 0.2(5) . . . . ? N18_1 N17_1 C25_1 C26_1 0.2(5) . . . . ? B3_1 N17_1 C25_1 C26_1 -176.2(4) . . . . ? N17_1 C25_1 C26_1 C27_1 0.0(5) . . . . ? N17_1 N18_1 C27_1 C26_1 0.3(5) . . . . ? C25_1 C26_1 C27_1 N18_1 -0.2(5) . . . . ? N20_1 N19_1 C28_1 C29_1 0.1(5) . . . . ? Ti2_1 N19_1 C28_1 C29_1 -169.1(3) . . . . ? N19_1 C28_1 C29_1 C30_1 0.4(5) . . . . ? C28_1 C29_1 C30_1 N20_1 -0.7(5) . . . . ? N19_1 N20_1 C30_1 C29_1 0.7(5) . . . . ? B4_1 N20_1 C30_1 C29_1 175.9(5) . . . . ? N22_1 N21_1 C31_1 C32_1 -0.3(5) . . . . ? Ti2_1 N21_1 C31_1 C32_1 177.9(3) . . . . ? N21_1 C31_1 C32_1 C33_1 0.2(5) . . . . ? N21_1 N22_1 C33_1 C32_1 -0.2(5) . . . . ? B4_1 N22_1 C33_1 C32_1 -175.8(5) . . . . ? C31_1 C32_1 C33_1 N22_1 0.0(6) . . . . ? N24_1 N23_1 C34_1 C35_1 0.0(4) . . . . ? Ti2_1 N23_1 C34_1 C35_1 172.1(3) . . . . ? N23_1 C34_1 C35_1 C36_1 0.0(5) . . . . ? N23_1 N24_1 C36_1 C35_1 0.0(5) . . . . ? B4_1 N24_1 C36_1 C35_1 179.7(5) . . . . ? C34_1 C35_1 C36_1 N24_1 0.0(5) . . . . ? C42_2 C37_2 C38_2 C39_2 1.1(8) . . . . ? C37_2 C38_2 C39_2 C40_2 -0.3(9) . . . . ? C38_2 C39_2 C40_2 C41_2 -0.5(9) . . . . ? C39_2 C40_2 C41_2 C42_2 0.5(8) . . . . ? C40_2 C41_2 C42_2 C37_2 0.3(7) . . . . ? C38_2 C37_2 C42_2 C41_2 -1.1(8) . . . . ? C48_3 C43_3 C44_3 C45_3 -0.7(8) . . . . ? C43_3 C44_3 C45_3 C46_3 -0.1(8) . . . . ? C44_3 C45_3 C46_3 C47_3 1.1(8) . . . . ? C45_3 C46_3 C47_3 C48_3 -1.4(7) . . . . ? C46_3 C47_3 C48_3 C43_3 0.6(8) . . . . ? C44_3 C43_3 C48_3 C47_3 0.5(8) . . . . ? C54_4 C49_4 C50_4 C51_4 -0.7(8) . . . . ? C49_4 C50_4 C51_4 C52_4 0.0(8) . . . . ? C50_4 C51_4 C52_4 C53_4 0.7(7) . . . . ? C51_4 C52_4 C53_4 C54_4 -0.8(7) . . . . ? C52_4 C53_4 C54_4 C49_4 0.1(8) . . . . ? C50_4 C49_4 C54_4 C53_4 0.6(8) . . . . ? C60_5 C55_5 C56_5 C57_5 3.2(14) . . . . ? C55_5 C56_5 C57_5 C58_5 -3.2(15) . . . . ? C56_5 C57_5 C58_5 C59_5 2.2(15) . . . . ? C57_5 C58_5 C59_5 C60_5 -1.2(12) . . . . ? C56_5 C55_5 C60_5 C59_5 -2.4(12) . . . . ? C58_5 C59_5 C60_5 C55_5 1.3(11) . . . . ? _refine_diff_density_max 0.232 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.044 #===END data_(k2-Tp)(k3-Tp)Ti=Se _database_code_CSD 172873 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H20 B2 N12 Se Ti' _chemical_formula_weight 552.94 _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' 'B' 'B' 0.0013 0.0007 '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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.2584(3) _cell_length_b 17.2192(4) _cell_length_c 31.9869(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9505.7(4) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 35264 _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 1.925 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number 'none' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35264 _diffrn_reflns_av_R_equivalents 0.0960 _diffrn_reflns_av_sigmaI/netI 0.0934 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8358 _reflns_number_observed 4832 _reflns_observed_criterion 'I>2\s(I)' _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'DENZO-SMN' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8358 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_obs 0.0524 _refine_ls_wR_factor_all 0.1396 _refine_ls_wR_factor_obs 0.1121 _refine_ls_goodness_of_fit_all 1.006 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 1.006 _refine_ls_restrained_S_obs 1.090 _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 -0.08854(5) 0.46432(5) 0.34676(3) 0.0306(2) Uani 1 d . . Ti2 Ti 0.75370(5) 1.13617(5) 0.10268(3) 0.0271(2) Uani 1 d . . Se1 Se -0.00536(3) 0.39550(3) 0.38651(2) 0.0429(2) Uani 1 d . . Se2 Se 0.83304(3) 1.20255(3) 0.14581(2) 0.0404(2) Uani 1 d . . B1 B -0.2372(4) 0.5784(4) 0.3684(2) 0.042(2) Uani 1 d . . H101 H -0.2808(26) 0.6252(29) 0.3788(14) 0.050 Uiso 1 d . . B2 B 0.0229(3) 0.3770(3) 0.2698(2) 0.0317(15) Uani 1 d . . H201 H 0.0479(23) 0.3470(26) 0.2968(14) 0.038 Uiso 1 d . . B3 B 0.6175(3) 1.0028(4) 0.1215(2) 0.037(2) Uani 1 d . . H301 H 0.5729(24) 0.9606(27) 0.1276(14) 0.044 Uiso 1 d . . B4 B 0.8626(3) 1.2448(3) 0.0318(2) 0.0291(14) Uani 1 d . . H401 H 0.9002(22) 1.2620(25) 0.0594(13) 0.035 Uiso 1 d . . N1 N -0.1940(2) 0.4402(3) 0.37966(12) 0.0365(11) Uani 1 d . . N2 N -0.2515(2) 0.4942(2) 0.38159(13) 0.0341(10) Uani 1 d . . N3 N -0.1684(2) 0.5342(2) 0.30471(13) 0.0332(10) Uani 1 d . . N4 N -0.2247(2) 0.5802(2) 0.32133(13) 0.0347(11) Uani 1 d . . N5 N -0.0929(2) 0.5694(2) 0.38279(12) 0.0354(11) Uani 1 d . . N6 N -0.1626(2) 0.6068(2) 0.39016(12) 0.0326(10) Uani 1 d . . N7 N -0.1153(2) 0.3788(2) 0.30065(12) 0.0311(10) Uani 1 d . . N8 N -0.0659(2) 0.3562(2) 0.26971(12) 0.0302(10) Uani 1 d . . N9 N 0.0563(2) 0.3496(2) 0.22884(13) 0.0345(11) Uani 1 d . . N10 N 0.0324(3) 0.3794(3) 0.19139(14) 0.0470(12) Uani 1 d . . N11 N -0.0073(2) 0.5096(2) 0.30238(12) 0.0307(10) Uani 1 d . . N12 N 0.0312(2) 0.4665(2) 0.27319(12) 0.0282(10) Uani 1 d . . N13 N 0.6452(2) 1.1446(2) 0.13694(12) 0.0332(10) Uani 1 d . . N14 N 0.5984(2) 1.0826(2) 0.14101(13) 0.0352(11) Uani 1 d . . N15 N 0.7612(2) 1.0257(2) 0.13342(13) 0.0334(10) Uani 1 d . . N16 N 0.6977(2) 0.9785(2) 0.13766(13) 0.0361(11) Uani 1 d . . N17 N 0.6743(2) 1.0680(2) 0.05886(13) 0.0326(10) Uani 1 d . . N18 N 0.6238(2) 1.0150(2) 0.07477(13) 0.0323(10) Uani 1 d . . N19 N 0.7260(2) 1.2302(2) 0.06174(12) 0.0291(10) Uani 1 d . . N20 N 0.7765(2) 1.2693(2) 0.03607(12) 0.0295(10) Uani 1 d . . N21 N 0.8966(2) 1.2810(2) -0.00785(13) 0.0338(11) Uani 1 d . . N22 N 0.8613(2) 1.2757(3) -0.04627(14) 0.0435(12) Uani 1 d . . N23 N 0.8363(2) 1.1043(2) 0.05561(12) 0.0279(10) Uani 1 d . . N24 N 0.8661(2) 1.1546(2) 0.02649(12) 0.0298(10) Uani 1 d . . C1 C -0.2210(3) 0.3759(3) 0.3979(2) 0.0405(14) Uani 1 d . . H1 H -0.1927(3) 0.3290(3) 0.4011(2) 0.049 Uiso 1 calc R . C2 C -0.2958(3) 0.3874(4) 0.4114(2) 0.048(2) Uani 1 d . . H2 H -0.3287(3) 0.3508(4) 0.4248(2) 0.058 Uiso 1 calc R . C3 C -0.3124(3) 0.4627(4) 0.4014(2) 0.047(2) Uani 1 d . . H3 H -0.3596(3) 0.4887(4) 0.4074(2) 0.056 Uiso 1 calc R . C4 C -0.1707(3) 0.5469(3) 0.2636(2) 0.0394(14) Uani 1 d . . H4 H -0.1374(3) 0.5223(3) 0.2440(2) 0.047 Uiso 1 calc R . C5 C -0.2272(3) 0.6002(3) 0.2529(2) 0.046(2) Uani 1 d . . H5 H -0.2401(3) 0.6192(3) 0.2259(2) 0.055 Uiso 1 calc R . C6 C -0.2604(3) 0.6191(3) 0.2905(2) 0.0423(14) Uani 1 d . . H6 H -0.3022(3) 0.6544(3) 0.2942(2) 0.051 Uiso 1 calc R . C7 C -0.0413(3) 0.6065(3) 0.4071(2) 0.0422(14) Uani 1 d . . H7 H 0.0120(3) 0.5933(3) 0.4089(2) 0.051 Uiso 1 calc R . C8 C -0.0754(3) 0.6659(3) 0.4291(2) 0.049(2) Uani 1 d . . H8 H -0.0512(3) 0.7011(3) 0.4479(2) 0.059 Uiso 1 calc R . C9 C -0.1528(3) 0.6633(3) 0.4178(2) 0.0450(15) Uani 1 d . . H9 H -0.1923(3) 0.6965(3) 0.4281(2) 0.054 Uiso 1 calc R . C10 C -0.1850(3) 0.3472(3) 0.2912(2) 0.0363(13) Uani 1 d . . H10 H -0.2310(3) 0.3541(3) 0.3071(2) 0.044 Uiso 1 calc R . C11 C -0.1791(3) 0.3036(3) 0.2552(2) 0.0409(14) Uani 1 d . . H11 H -0.2189(3) 0.2744(3) 0.2421(2) 0.049 Uiso 1 calc R . C12 C -0.1039(3) 0.3112(3) 0.2422(2) 0.0370(13) Uani 1 d . . H12 H -0.0822(3) 0.2884(3) 0.2178(2) 0.044 Uiso 1 calc R . C13 C 0.0992(3) 0.2853(3) 0.2221(2) 0.0414(14) Uani 1 d . . H13 H 0.1223(3) 0.2543(3) 0.2433(2) 0.050 Uiso 1 calc R . C14 C 0.1040(3) 0.2719(4) 0.1805(2) 0.058(2) Uani 1 d . . H14 H 0.1303(3) 0.2306(4) 0.1668(2) 0.070 Uiso 1 calc R . C15 C 0.0618(3) 0.3322(4) 0.1623(2) 0.057(2) Uani 1 d . . H15 H 0.0550(3) 0.3388(4) 0.1330(2) 0.068 Uiso 1 calc R . C16 C 0.0142(3) 0.5833(3) 0.2970(2) 0.0335(13) Uani 1 d . . H16 H -0.0049(3) 0.6258(3) 0.3129(2) 0.040 Uiso 1 calc R . C17 C 0.0676(3) 0.5895(3) 0.2653(2) 0.0333(13) Uani 1 d . . H17 H 0.0925(3) 0.6352(3) 0.2554(2) 0.040 Uiso 1 calc R . C18 C 0.0770(3) 0.5150(3) 0.2511(2) 0.0356(13) Uani 1 d . . H18 H 0.1106(3) 0.4997(3) 0.2290(2) 0.043 Uiso 1 calc R . C19 C 0.6113(3) 1.2026(3) 0.1576(2) 0.0393(14) Uani 1 d . . H19 H 0.6313(3) 1.2539(3) 0.1595(2) 0.047 Uiso 1 calc R . C20 C 0.5434(3) 1.1780(4) 0.1758(2) 0.051(2) Uani 1 d . . H20 H 0.5086(3) 1.2076(4) 0.1924(2) 0.062 Uiso 1 calc R . C21 C 0.5371(3) 1.1018(3) 0.1649(2) 0.0449(15) Uani 1 d . . H21 H 0.4963(3) 1.0678(3) 0.1727(2) 0.054 Uiso 1 calc R . C22 C 0.8194(3) 0.9899(3) 0.1533(2) 0.0388(14) Uani 1 d . . H22 H 0.8707(3) 1.0094(3) 0.1555(2) 0.047 Uiso 1 calc R . C23 C 0.7941(4) 0.9208(3) 0.1703(2) 0.053(2) Uani 1 d . . H23 H 0.8239(4) 0.8840(3) 0.1855(2) 0.064 Uiso 1 calc R . C24 C 0.7169(3) 0.9166(3) 0.1605(2) 0.051(2) Uani 1 d . . H24 H 0.6826(3) 0.8761(3) 0.1686(2) 0.061 Uiso 1 calc R . C25 C 0.6692(3) 1.0639(3) 0.0174(2) 0.0408(14) Uani 1 d . . H25 H 0.6981(3) 1.0951(3) -0.0016(2) 0.049 Uiso 1 calc R . C26 C 0.6160(3) 1.0080(4) 0.0058(2) 0.053(2) Uani 1 d . . H26 H 0.6015(3) 0.9934(4) -0.0218(2) 0.063 Uiso 1 calc R . C27 C 0.5888(3) 0.9783(3) 0.0424(2) 0.0457(15) Uani 1 d . . H27 H 0.5512(3) 0.9382(3) 0.0448(2) 0.055 Uiso 1 calc R . C28 C 0.6579(3) 1.2675(3) 0.0583(2) 0.0351(13) Uani 1 d . . H28 H 0.6116(3) 1.2523(3) 0.0721(2) 0.042 Uiso 1 calc R . C29 C 0.6639(3) 1.3307(3) 0.0321(2) 0.0360(13) Uani 1 d . . H29 H 0.6247(3) 1.3669(3) 0.0247(2) 0.043 Uiso 1 calc R . C30 C 0.7399(3) 1.3294(3) 0.0192(2) 0.0371(13) Uani 1 d . . H30 H 0.7628(3) 1.3662(3) 0.0008(2) 0.045 Uiso 1 calc R . C31 C 0.9661(3) 1.3163(3) -0.0117(2) 0.0395(14) Uani 1 d . . H31 H 1.0010(3) 1.3266(3) 0.0106(2) 0.047 Uiso 1 calc R . C32 C 0.9781(3) 1.3348(3) -0.0527(2) 0.045(2) Uani 1 d . . H32 H 1.0217(3) 1.3598(3) -0.0648(2) 0.054 Uiso 1 calc R . C33 C 0.9117(3) 1.3083(3) -0.0724(2) 0.047(2) Uani 1 d . . H33 H 0.9031(3) 1.3129(3) -0.1016(2) 0.057 Uiso 1 calc R . C34 C 0.8547(3) 1.0329(3) 0.0430(2) 0.0359(13) Uani 1 d . . H34 H 0.8409(3) 0.9865(3) 0.0572(2) 0.043 Uiso 1 calc R . C35 C 0.8967(3) 1.0359(3) 0.0064(2) 0.0438(15) Uani 1 d . . H35 H 0.9173(3) 0.9935(3) -0.0090(2) 0.053 Uiso 1 calc R . C36 C 0.9022(3) 1.1136(3) -0.0029(2) 0.0383(14) Uani 1 d . . H36 H 0.9277(3) 1.1348(3) -0.0266(2) 0.046 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 0.0302(5) 0.0311(5) 0.0305(6) -0.0018(4) 0.0012(4) 0.0007(4) Ti2 0.0281(5) 0.0242(5) 0.0291(5) 0.0005(4) 0.0002(4) -0.0008(4) Se1 0.0421(4) 0.0481(4) 0.0386(4) 0.0073(3) -0.0018(3) 0.0088(3) Se2 0.0483(4) 0.0341(3) 0.0389(4) -0.0043(3) -0.0084(3) -0.0060(3) B1 0.034(4) 0.043(4) 0.049(4) -0.002(3) 0.006(3) 0.007(3) B2 0.034(4) 0.032(4) 0.029(4) -0.002(3) -0.002(3) 0.000(3) B3 0.031(4) 0.038(4) 0.041(4) 0.002(3) 0.004(3) -0.008(3) B4 0.028(3) 0.024(3) 0.036(4) -0.002(3) 0.000(3) -0.001(3) N1 0.039(3) 0.039(3) 0.032(3) 0.000(2) 0.005(2) -0.001(2) N2 0.030(2) 0.035(3) 0.037(3) -0.001(2) 0.006(2) 0.000(2) N3 0.032(2) 0.037(3) 0.030(3) -0.001(2) 0.002(2) 0.006(2) N4 0.031(2) 0.031(3) 0.042(3) 0.000(2) -0.003(2) 0.001(2) N5 0.036(3) 0.035(3) 0.036(3) -0.001(2) 0.001(2) -0.002(2) N6 0.035(3) 0.031(3) 0.032(3) -0.003(2) 0.002(2) 0.008(2) N7 0.029(2) 0.033(3) 0.032(3) 0.003(2) 0.002(2) -0.002(2) N8 0.033(2) 0.030(3) 0.028(2) -0.001(2) 0.000(2) -0.001(2) N9 0.037(3) 0.035(3) 0.032(3) -0.002(2) 0.004(2) 0.004(2) N10 0.065(3) 0.048(3) 0.028(3) 0.002(2) 0.004(2) 0.003(3) N11 0.028(2) 0.030(3) 0.034(3) -0.001(2) 0.004(2) 0.003(2) N12 0.029(2) 0.031(2) 0.025(2) -0.001(2) 0.001(2) 0.001(2) N13 0.035(2) 0.031(3) 0.033(3) 0.001(2) 0.006(2) -0.004(2) N14 0.030(2) 0.037(3) 0.038(3) 0.002(2) 0.007(2) 0.000(2) N15 0.033(2) 0.029(2) 0.038(3) 0.000(2) 0.001(2) -0.004(2) N16 0.038(3) 0.031(3) 0.039(3) 0.007(2) -0.002(2) -0.009(2) N17 0.037(2) 0.034(3) 0.027(3) 0.000(2) 0.003(2) -0.004(2) N18 0.030(2) 0.031(3) 0.036(3) 0.000(2) -0.002(2) -0.002(2) N19 0.027(2) 0.026(2) 0.034(3) 0.001(2) 0.000(2) -0.002(2) N20 0.034(2) 0.025(2) 0.030(2) 0.003(2) 0.005(2) -0.002(2) N21 0.034(3) 0.033(3) 0.034(3) 0.004(2) 0.002(2) -0.002(2) N22 0.040(3) 0.053(3) 0.037(3) 0.007(2) 0.001(2) 0.000(2) N23 0.027(2) 0.027(2) 0.030(2) 0.000(2) 0.003(2) -0.004(2) N24 0.028(2) 0.030(3) 0.031(3) 0.002(2) 0.004(2) 0.000(2) C1 0.046(3) 0.043(4) 0.033(3) 0.005(3) 0.002(3) -0.013(3) C2 0.049(4) 0.058(4) 0.038(4) 0.005(3) 0.004(3) -0.025(3) C3 0.037(3) 0.057(4) 0.047(4) -0.001(3) 0.011(3) -0.003(3) C4 0.037(3) 0.048(4) 0.033(4) -0.002(3) 0.001(3) -0.005(3) C5 0.047(4) 0.059(4) 0.031(4) 0.013(3) -0.011(3) -0.001(3) C6 0.036(3) 0.043(4) 0.048(4) 0.011(3) -0.006(3) 0.008(3) C7 0.038(3) 0.049(4) 0.040(4) 0.000(3) -0.007(3) 0.001(3) C8 0.061(4) 0.044(4) 0.042(4) -0.009(3) -0.006(3) -0.004(3) C9 0.060(4) 0.042(4) 0.033(3) -0.002(3) 0.002(3) 0.003(3) C10 0.033(3) 0.034(3) 0.042(4) 0.002(3) 0.001(3) -0.006(3) C11 0.047(4) 0.036(3) 0.039(4) 0.000(3) -0.007(3) -0.014(3) C12 0.051(4) 0.032(3) 0.027(3) -0.006(3) 0.002(3) -0.002(3) C13 0.042(3) 0.034(3) 0.049(4) -0.006(3) 0.006(3) 0.005(3) C14 0.067(4) 0.046(4) 0.062(5) -0.015(4) 0.022(4) 0.001(3) C15 0.075(4) 0.063(5) 0.033(4) -0.011(3) 0.014(3) -0.013(4) C16 0.035(3) 0.027(3) 0.038(3) 0.002(2) 0.000(3) 0.000(2) C17 0.033(3) 0.032(3) 0.035(3) 0.005(2) 0.002(3) -0.002(2) C18 0.035(3) 0.042(3) 0.030(3) 0.003(3) 0.007(3) 0.002(3) C19 0.043(3) 0.039(3) 0.036(3) -0.010(3) 0.006(3) 0.005(3) C20 0.044(4) 0.065(5) 0.045(4) -0.010(3) 0.011(3) 0.011(3) C21 0.037(3) 0.057(4) 0.041(4) -0.005(3) 0.014(3) -0.007(3) C22 0.033(3) 0.037(3) 0.046(4) -0.001(3) -0.013(3) 0.008(3) C23 0.063(4) 0.034(4) 0.062(4) 0.010(3) -0.021(3) 0.004(3) C24 0.061(4) 0.031(3) 0.061(4) 0.018(3) -0.003(3) -0.005(3) C25 0.040(3) 0.050(4) 0.032(4) -0.002(3) 0.004(3) -0.005(3) C26 0.052(4) 0.068(5) 0.037(4) -0.012(3) -0.007(3) -0.011(3) C27 0.040(3) 0.048(4) 0.048(4) -0.015(3) -0.001(3) -0.014(3) C28 0.030(3) 0.037(3) 0.038(3) 0.001(3) -0.002(3) -0.002(3) C29 0.032(3) 0.027(3) 0.048(4) 0.002(3) -0.001(3) 0.010(2) C30 0.047(3) 0.027(3) 0.037(3) 0.011(3) 0.000(3) -0.002(3) C31 0.028(3) 0.032(3) 0.059(4) -0.001(3) 0.003(3) -0.002(2) C32 0.036(3) 0.036(3) 0.064(4) 0.010(3) 0.023(3) 0.004(3) C33 0.053(4) 0.047(4) 0.041(4) 0.011(3) 0.013(3) 0.014(3) C34 0.042(3) 0.019(3) 0.047(4) -0.007(3) 0.002(3) 0.002(2) C35 0.051(4) 0.037(4) 0.043(4) -0.011(3) 0.015(3) 0.007(3) C36 0.035(3) 0.041(4) 0.039(3) 0.002(3) 0.010(3) 0.009(3) _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 N7 2.135(4) . ? Ti1 N11 2.142(4) . ? Ti1 N1 2.143(4) . ? Ti1 N5 2.147(4) . ? Ti1 Se1 2.2544(10) . ? Ti1 N3 2.271(4) . ? Ti2 N19 2.137(4) . ? Ti2 N23 2.144(4) . ? Ti2 N15 2.145(4) . ? Ti2 N13 2.174(4) . ? Ti2 Se2 2.2550(10) . ? Ti2 N17 2.284(4) . ? B1 N4 1.521(8) . ? B1 N2 1.529(8) . ? B1 N6 1.544(7) . ? B2 N9 1.508(7) . ? B2 N12 1.551(7) . ? B2 N8 1.574(7) . ? B3 N18 1.515(7) . ? B3 N16 1.535(7) . ? B3 N14 1.545(7) . ? B4 N21 1.529(7) . ? B4 N20 1.550(6) . ? B4 N24 1.564(7) . ? N1 C1 1.336(6) . ? N1 N2 1.361(5) . ? N2 C3 1.341(6) . ? N3 C4 1.335(6) . ? N3 N4 1.361(5) . ? N4 C6 1.342(6) . ? N5 C7 1.344(6) . ? N5 N6 1.385(5) . ? N6 C9 1.325(6) . ? N7 C10 1.353(6) . ? N7 N8 1.363(5) . ? N8 C12 1.344(6) . ? N9 C13 1.349(6) . ? N9 N10 1.367(5) . ? N10 C15 1.335(7) . ? N11 C16 1.334(6) . ? N11 N12 1.365(5) . ? N12 C18 1.349(6) . ? N13 C19 1.333(6) . ? N13 N14 1.345(5) . ? N14 C21 1.344(6) . ? N15 C22 1.339(6) . ? N15 N16 1.371(5) . ? N16 C24 1.334(6) . ? N17 C25 1.332(6) . ? N17 N18 1.360(5) . ? N18 C27 1.357(6) . ? N19 C28 1.344(6) . ? N19 N20 1.373(5) . ? N20 C30 1.329(6) . ? N21 C31 1.350(6) . ? N21 N22 1.375(5) . ? N22 C33 1.331(6) . ? N23 C34 1.332(6) . ? N23 N24 1.373(5) . ? N24 C36 1.331(6) . ? C1 C2 1.375(7) . ? C2 C3 1.367(7) . ? C4 C5 1.382(7) . ? C5 C6 1.371(7) . ? C7 C8 1.373(7) . ? C8 C9 1.384(7) . ? C10 C11 1.379(7) . ? C11 C12 1.368(7) . ? C13 C14 1.353(7) . ? C14 C15 1.397(8) . ? C16 C17 1.375(7) . ? C17 C18 1.371(6) . ? C19 C20 1.376(7) . ? C20 C21 1.363(8) . ? C22 C23 1.377(7) . ? C23 C24 1.371(7) . ? C25 C26 1.382(7) . ? C26 C27 1.361(7) . ? C28 C29 1.377(7) . ? C29 C30 1.375(6) . ? C31 C32 1.364(7) . ? C32 C33 1.385(7) . ? C34 C35 1.377(7) . ? C35 C36 1.375(7) . ? 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 N7 Ti1 N11 86.26(15) . . ? N7 Ti1 N1 91.3(2) . . ? N11 Ti1 N1 162.1(2) . . ? N7 Ti1 N5 160.9(2) . . ? N11 Ti1 N5 94.1(2) . . ? N1 Ti1 N5 82.5(2) . . ? N7 Ti1 Se1 99.47(11) . . ? N11 Ti1 Se1 98.53(10) . . ? N1 Ti1 Se1 99.33(12) . . ? N5 Ti1 Se1 99.36(12) . . ? N7 Ti1 N3 79.96(15) . . ? N11 Ti1 N3 79.15(14) . . ? N1 Ti1 N3 83.0(2) . . ? N5 Ti1 N3 81.4(2) . . ? Se1 Ti1 N3 177.63(11) . . ? N19 Ti2 N23 84.97(15) . . ? N19 Ti2 N15 165.1(2) . . ? N23 Ti2 N15 93.14(15) . . ? N19 Ti2 N13 93.8(2) . . ? N23 Ti2 N13 160.60(15) . . ? N15 Ti2 N13 83.1(2) . . ? N19 Ti2 Se2 97.26(11) . . ? N23 Ti2 Se2 98.96(10) . . ? N15 Ti2 Se2 97.61(11) . . ? N13 Ti2 Se2 100.40(11) . . ? N19 Ti2 N17 83.07(14) . . ? N23 Ti2 N17 80.57(14) . . ? N15 Ti2 N17 82.06(15) . . ? N13 Ti2 N17 80.06(15) . . ? Se2 Ti2 N17 179.41(11) . . ? N4 B1 N2 108.4(5) . . ? N4 B1 N6 108.7(4) . . ? N2 B1 N6 108.1(5) . . ? N9 B2 N12 109.6(4) . . ? N9 B2 N8 107.4(4) . . ? N12 B2 N8 108.4(4) . . ? N18 B3 N16 107.7(4) . . ? N18 B3 N14 106.8(4) . . ? N16 B3 N14 107.4(4) . . ? N21 B4 N20 109.3(4) . . ? N21 B4 N24 107.4(4) . . ? N20 B4 N24 108.4(4) . . ? C1 N1 N2 107.0(4) . . ? C1 N1 Ti1 132.2(4) . . ? N2 N1 Ti1 120.6(3) . . ? C3 N2 N1 108.4(4) . . ? C3 N2 B1 129.8(5) . . ? N1 N2 B1 121.2(4) . . ? C4 N3 N4 105.6(4) . . ? C4 N3 Ti1 133.5(3) . . ? N4 N3 Ti1 120.7(3) . . ? C6 N4 N3 109.3(4) . . ? C6 N4 B1 132.2(5) . . ? N3 N4 B1 118.5(4) . . ? C7 N5 N6 104.8(4) . . ? C7 N5 Ti1 133.5(4) . . ? N6 N5 Ti1 120.9(3) . . ? C9 N6 N5 110.1(4) . . ? C9 N6 B1 129.8(5) . . ? N5 N6 B1 120.1(4) . . ? C10 N7 N8 106.3(4) . . ? C10 N7 Ti1 128.5(3) . . ? N8 N7 Ti1 124.3(3) . . ? C12 N8 N7 109.5(4) . . ? C12 N8 B2 127.5(4) . . ? N7 N8 B2 122.9(4) . . ? C13 N9 N10 109.5(4) . . ? C13 N9 B2 127.2(5) . . ? N10 N9 B2 121.9(4) . . ? C15 N10 N9 105.5(5) . . ? C16 N11 N12 107.0(4) . . ? C16 N11 Ti1 127.9(3) . . ? N12 N11 Ti1 125.0(3) . . ? C18 N12 N11 107.9(4) . . ? C18 N12 B2 129.1(4) . . ? N11 N12 B2 122.9(4) . . ? C19 N13 N14 106.4(4) . . ? C19 N13 Ti2 132.7(4) . . ? N14 N13 Ti2 120.9(3) . . ? C21 N14 N13 109.4(4) . . ? C21 N14 B3 127.9(5) . . ? N13 N14 B3 122.6(4) . . ? C22 N15 N16 106.2(4) . . ? C22 N15 Ti2 132.2(3) . . ? N16 N15 Ti2 121.5(3) . . ? C24 N16 N15 109.3(4) . . ? C24 N16 B3 128.7(5) . . ? N15 N16 B3 121.7(4) . . ? C25 N17 N18 107.1(4) . . ? C25 N17 Ti2 132.7(3) . . ? N18 N17 Ti2 119.9(3) . . ? C27 N18 N17 108.2(4) . . ? C27 N18 B3 131.1(5) . . ? N17 N18 B3 120.6(4) . . ? C28 N19 N20 105.8(4) . . ? C28 N19 Ti2 127.4(3) . . ? N20 N19 Ti2 126.5(3) . . ? C30 N20 N19 108.8(4) . . ? C30 N20 B4 129.2(4) . . ? N19 N20 B4 121.9(4) . . ? C31 N21 N22 110.0(4) . . ? C31 N21 B4 126.8(5) . . ? N22 N21 B4 122.9(4) . . ? C33 N22 N21 104.1(4) . . ? C34 N23 N24 106.6(4) . . ? C34 N23 Ti2 127.4(3) . . ? N24 N23 Ti2 124.4(3) . . ? C36 N24 N23 108.7(4) . . ? C36 N24 B4 128.4(4) . . ? N23 N24 B4 122.6(4) . . ? N1 C1 C2 110.2(5) . . ? C3 C2 C1 105.0(5) . . ? N2 C3 C2 109.3(5) . . ? N3 C4 C5 111.9(5) . . ? C6 C5 C4 103.7(5) . . ? N4 C6 C5 109.5(5) . . ? N5 C7 C8 111.5(5) . . ? C7 C8 C9 104.8(5) . . ? N6 C9 C8 108.8(5) . . ? N7 C10 C11 109.8(5) . . ? C12 C11 C10 105.8(5) . . ? N8 C12 C11 108.6(5) . . ? N9 C13 C14 109.3(5) . . ? C13 C14 C15 104.6(5) . . ? N10 C15 C14 111.1(5) . . ? N11 C16 C17 110.9(5) . . ? C18 C17 C16 104.5(5) . . ? N12 C18 C17 109.7(4) . . ? N13 C19 C20 110.7(5) . . ? C21 C20 C19 104.8(5) . . ? N14 C21 C20 108.7(5) . . ? N15 C22 C23 110.3(5) . . ? C24 C23 C22 105.3(5) . . ? N16 C24 C23 108.8(5) . . ? N17 C25 C26 110.4(5) . . ? C27 C26 C25 105.1(5) . . ? N18 C27 C26 109.2(5) . . ? N19 C28 C29 111.2(4) . . ? C30 C29 C28 104.0(4) . . ? N20 C30 C29 110.1(4) . . ? N21 C31 C32 109.1(5) . . ? C31 C32 C33 103.6(5) . . ? N22 C33 C32 113.1(5) . . ? N23 C34 C35 110.5(5) . . ? C36 C35 C34 104.9(5) . . ? N24 C36 C35 109.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Ti1 N1 C1 60.8(5) . . . . ? N11 Ti1 N1 C1 142.6(5) . . . . ? N5 Ti1 N1 C1 -137.3(5) . . . . ? Se1 Ti1 N1 C1 -39.0(5) . . . . ? N3 Ti1 N1 C1 140.6(5) . . . . ? N7 Ti1 N1 N2 -112.8(3) . . . . ? N11 Ti1 N1 N2 -31.1(7) . . . . ? N5 Ti1 N1 N2 49.0(3) . . . . ? Se1 Ti1 N1 N2 147.3(3) . . . . ? N3 Ti1 N1 N2 -33.1(3) . . . . ? C1 N1 N2 C3 0.7(5) . . . . ? Ti1 N1 N2 C3 175.9(3) . . . . ? C1 N1 N2 B1 172.4(5) . . . . ? Ti1 N1 N2 B1 -12.5(6) . . . . ? N4 B1 N2 C3 -121.8(6) . . . . ? N6 B1 N2 C3 120.5(5) . . . . ? N4 B1 N2 N1 68.5(6) . . . . ? N6 B1 N2 N1 -49.2(6) . . . . ? N7 Ti1 N3 C4 -50.4(5) . . . . ? N11 Ti1 N3 C4 37.6(5) . . . . ? N1 Ti1 N3 C4 -143.0(5) . . . . ? N5 Ti1 N3 C4 133.6(5) . . . . ? Se1 Ti1 N3 C4 25.6(30) . . . . ? N7 Ti1 N3 N4 135.6(3) . . . . ? N11 Ti1 N3 N4 -136.3(3) . . . . ? N1 Ti1 N3 N4 43.1(3) . . . . ? N5 Ti1 N3 N4 -40.4(3) . . . . ? Se1 Ti1 N3 N4 -148.3(26) . . . . ? C4 N3 N4 C6 0.5(5) . . . . ? Ti1 N3 N4 C6 175.9(3) . . . . ? C4 N3 N4 B1 179.6(4) . . . . ? Ti1 N3 N4 B1 -5.0(5) . . . . ? N2 B1 N4 C6 123.8(6) . . . . ? N6 B1 N4 C6 -119.0(6) . . . . ? N2 B1 N4 N3 -55.0(6) . . . . ? N6 B1 N4 N3 62.2(6) . . . . ? N7 Ti1 N5 C7 -158.4(5) . . . . ? N11 Ti1 N5 C7 -67.9(5) . . . . ? N1 Ti1 N5 C7 129.8(5) . . . . ? Se1 Ti1 N5 C7 31.5(5) . . . . ? N3 Ti1 N5 C7 -146.2(5) . . . . ? N7 Ti1 N5 N6 33.3(7) . . . . ? N11 Ti1 N5 N6 123.7(3) . . . . ? N1 Ti1 N5 N6 -38.6(3) . . . . ? Se1 Ti1 N5 N6 -136.9(3) . . . . ? N3 Ti1 N5 N6 45.4(3) . . . . ? C7 N5 N6 C9 -0.3(5) . . . . ? Ti1 N5 N6 C9 171.1(3) . . . . ? C7 N5 N6 B1 -178.2(5) . . . . ? Ti1 N5 N6 B1 -6.9(6) . . . . ? N4 B1 N6 C9 125.3(6) . . . . ? N2 B1 N6 C9 -117.2(6) . . . . ? N4 B1 N6 N5 -57.2(6) . . . . ? N2 B1 N6 N5 60.2(6) . . . . ? N11 Ti1 N7 C10 -142.6(4) . . . . ? N1 Ti1 N7 C10 19.7(4) . . . . ? N5 Ti1 N7 C10 -50.8(7) . . . . ? Se1 Ti1 N7 C10 119.3(4) . . . . ? N3 Ti1 N7 C10 -63.0(4) . . . . ? N11 Ti1 N7 N8 24.5(3) . . . . ? N1 Ti1 N7 N8 -173.2(3) . . . . ? N5 Ti1 N7 N8 116.3(5) . . . . ? Se1 Ti1 N7 N8 -73.6(3) . . . . ? N3 Ti1 N7 N8 104.1(4) . . . . ? C10 N7 N8 C12 -0.8(5) . . . . ? Ti1 N7 N8 C12 -170.3(3) . . . . ? C10 N7 N8 B2 -176.8(4) . . . . ? Ti1 N7 N8 B2 13.7(6) . . . . ? N9 B2 N8 C12 10.4(7) . . . . ? N12 B2 N8 C12 128.8(5) . . . . ? N9 B2 N8 N7 -174.3(4) . . . . ? N12 B2 N8 N7 -55.9(6) . . . . ? N12 B2 N9 C13 139.9(5) . . . . ? N8 B2 N9 C13 -102.6(5) . . . . ? N12 B2 N9 N10 -54.7(6) . . . . ? N8 B2 N9 N10 62.8(6) . . . . ? C13 N9 N10 C15 -0.4(6) . . . . ? B2 N9 N10 C15 -168.1(5) . . . . ? N7 Ti1 N11 C16 147.9(4) . . . . ? N1 Ti1 N11 C16 65.5(7) . . . . ? N5 Ti1 N11 C16 -12.9(4) . . . . ? Se1 Ti1 N11 C16 -113.0(4) . . . . ? N3 Ti1 N11 C16 67.5(4) . . . . ? N7 Ti1 N11 N12 -30.4(3) . . . . ? N1 Ti1 N11 N12 -112.9(5) . . . . ? N5 Ti1 N11 N12 168.8(3) . . . . ? Se1 Ti1 N11 N12 68.7(3) . . . . ? N3 Ti1 N11 N12 -110.8(3) . . . . ? C16 N11 N12 C18 1.4(5) . . . . ? Ti1 N11 N12 C18 -180.0(3) . . . . ? C16 N11 N12 B2 178.7(4) . . . . ? Ti1 N11 N12 B2 -2.7(6) . . . . ? N9 B2 N12 C18 -17.0(7) . . . . ? N8 B2 N12 C18 -133.9(5) . . . . ? N9 B2 N12 N11 166.3(4) . . . . ? N8 B2 N12 N11 49.3(6) . . . . ? N19 Ti2 N13 C19 -56.4(5) . . . . ? N23 Ti2 N13 C19 -141.9(5) . . . . ? N15 Ti2 N13 C19 138.2(5) . . . . ? Se2 Ti2 N13 C19 41.7(5) . . . . ? N17 Ti2 N13 C19 -138.7(5) . . . . ? N19 Ti2 N13 N14 125.1(3) . . . . ? N23 Ti2 N13 N14 39.6(7) . . . . ? N15 Ti2 N13 N14 -40.3(3) . . . . ? Se2 Ti2 N13 N14 -136.8(3) . . . . ? N17 Ti2 N13 N14 42.8(3) . . . . ? C19 N13 N14 C21 -1.5(5) . . . . ? Ti2 N13 N14 C21 177.3(3) . . . . ? C19 N13 N14 B3 -179.6(4) . . . . ? Ti2 N13 N14 B3 -0.7(6) . . . . ? N18 B3 N14 C21 122.5(5) . . . . ? N16 B3 N14 C21 -122.2(5) . . . . ? N18 B3 N14 N13 -59.8(6) . . . . ? N16 B3 N14 N13 55.5(6) . . . . ? N19 Ti2 N15 C22 146.7(5) . . . . ? N23 Ti2 N15 C22 64.5(5) . . . . ? N13 Ti2 N15 C22 -134.6(5) . . . . ? Se2 Ti2 N15 C22 -35.0(5) . . . . ? N17 Ti2 N15 C22 144.5(5) . . . . ? N19 Ti2 N15 N16 -37.4(8) . . . . ? N23 Ti2 N15 N16 -119.6(3) . . . . ? N13 Ti2 N15 N16 41.3(3) . . . . ? Se2 Ti2 N15 N16 140.9(3) . . . . ? N17 Ti2 N15 N16 -39.6(3) . . . . ? C22 N15 N16 C24 1.4(6) . . . . ? Ti2 N15 N16 C24 -175.4(4) . . . . ? C22 N15 N16 B3 175.5(5) . . . . ? Ti2 N15 N16 B3 -1.4(6) . . . . ? N18 B3 N16 C24 -126.6(6) . . . . ? N14 B3 N16 C24 118.6(6) . . . . ? N18 B3 N16 N15 60.5(6) . . . . ? N14 B3 N16 N15 -54.2(6) . . . . ? N19 Ti2 N17 C25 46.3(5) . . . . ? N23 Ti2 N17 C25 -39.7(5) . . . . ? N15 Ti2 N17 C25 -134.2(5) . . . . ? N13 Ti2 N17 C25 141.4(5) . . . . ? Se2 Ti2 N17 C25 -77.4(112) . . . . ? N19 Ti2 N17 N18 -139.5(3) . . . . ? N23 Ti2 N17 N18 134.4(3) . . . . ? N15 Ti2 N17 N18 39.9(3) . . . . ? N13 Ti2 N17 N18 -44.5(3) . . . . ? Se2 Ti2 N17 N18 96.7(110) . . . . ? C25 N17 N18 C27 0.7(5) . . . . ? Ti2 N17 N18 C27 -174.8(3) . . . . ? C25 N17 N18 B3 177.8(4) . . . . ? Ti2 N17 N18 B3 2.3(6) . . . . ? N16 B3 N18 C27 117.5(5) . . . . ? N14 B3 N18 C27 -127.3(5) . . . . ? N16 B3 N18 N17 -58.8(6) . . . . ? N14 B3 N18 N17 56.4(6) . . . . ? N23 Ti2 N19 C28 152.1(4) . . . . ? N15 Ti2 N19 C28 68.9(8) . . . . ? N13 Ti2 N19 C28 -8.4(4) . . . . ? Se2 Ti2 N19 C28 -109.4(4) . . . . ? N17 Ti2 N19 C28 71.1(4) . . . . ? N23 Ti2 N19 N20 -33.9(3) . . . . ? N15 Ti2 N19 N20 -117.2(6) . . . . ? N13 Ti2 N19 N20 165.5(4) . . . . ? Se2 Ti2 N19 N20 64.5(3) . . . . ? N17 Ti2 N19 N20 -115.0(4) . . . . ? C28 N19 N20 C30 2.1(5) . . . . ? Ti2 N19 N20 C30 -172.9(3) . . . . ? C28 N19 N20 B4 179.0(4) . . . . ? Ti2 N19 N20 B4 3.9(6) . . . . ? N21 B4 N20 C30 -21.5(7) . . . . ? N24 B4 N20 C30 -138.3(5) . . . . ? N21 B4 N20 N19 162.4(4) . . . . ? N24 B4 N20 N19 45.6(6) . . . . ? N20 B4 N21 C31 135.5(5) . . . . ? N24 B4 N21 C31 -107.0(5) . . . . ? N20 B4 N21 N22 -50.1(6) . . . . ? N24 B4 N21 N22 67.3(5) . . . . ? C31 N21 N22 C33 0.2(5) . . . . ? B4 N21 N22 C33 -175.0(4) . . . . ? N19 Ti2 N23 C34 -141.6(4) . . . . ? N15 Ti2 N23 C34 23.6(4) . . . . ? N13 Ti2 N23 C34 -54.6(7) . . . . ? Se2 Ti2 N23 C34 121.8(4) . . . . ? N17 Ti2 N23 C34 -57.9(4) . . . . ? N19 Ti2 N23 N24 22.3(3) . . . . ? N15 Ti2 N23 N24 -172.5(3) . . . . ? N13 Ti2 N23 N24 109.3(5) . . . . ? Se2 Ti2 N23 N24 -74.3(3) . . . . ? N17 Ti2 N23 N24 106.1(3) . . . . ? C34 N23 N24 C36 -0.3(5) . . . . ? Ti2 N23 N24 C36 -167.0(3) . . . . ? C34 N23 N24 B4 -175.0(4) . . . . ? Ti2 N23 N24 B4 18.3(6) . . . . ? N21 B4 N24 C36 10.0(7) . . . . ? N20 B4 N24 C36 128.1(5) . . . . ? N21 B4 N24 N23 -176.4(4) . . . . ? N20 B4 N24 N23 -58.4(6) . . . . ? N2 N1 C1 C2 0.5(6) . . . . ? Ti1 N1 C1 C2 -173.9(3) . . . . ? N1 C1 C2 C3 -1.4(6) . . . . ? N1 N2 C3 C2 -1.7(6) . . . . ? B1 N2 C3 C2 -172.4(5) . . . . ? C1 C2 C3 N2 1.9(6) . . . . ? N4 N3 C4 C5 0.0(6) . . . . ? Ti1 N3 C4 C5 -174.5(4) . . . . ? N3 C4 C5 C6 -0.5(6) . . . . ? N3 N4 C6 C5 -0.8(6) . . . . ? B1 N4 C6 C5 -179.7(5) . . . . ? C4 C5 C6 N4 0.8(6) . . . . ? N6 N5 C7 C8 -0.6(6) . . . . ? Ti1 N5 C7 C8 -170.3(4) . . . . ? N5 C7 C8 C9 1.1(6) . . . . ? N5 N6 C9 C8 1.0(6) . . . . ? B1 N6 C9 C8 178.6(5) . . . . ? C7 C8 C9 N6 -1.3(6) . . . . ? N8 N7 C10 C11 1.5(5) . . . . ? Ti1 N7 C10 C11 170.4(3) . . . . ? N7 C10 C11 C12 -1.6(6) . . . . ? N7 N8 C12 C11 -0.2(6) . . . . ? B2 N8 C12 C11 175.6(5) . . . . ? C10 C11 C12 N8 1.1(6) . . . . ? N10 N9 C13 C14 0.1(6) . . . . ? B2 N9 C13 C14 166.9(5) . . . . ? N9 C13 C14 C15 0.2(6) . . . . ? N9 N10 C15 C14 0.5(6) . . . . ? C13 C14 C15 N10 -0.5(7) . . . . ? N12 N11 C16 C17 -1.4(5) . . . . ? Ti1 N11 C16 C17 -179.9(3) . . . . ? N11 C16 C17 C18 0.8(6) . . . . ? N11 N12 C18 C17 -0.9(5) . . . . ? B2 N12 C18 C17 -178.0(5) . . . . ? C16 C17 C18 N12 0.1(6) . . . . ? N14 N13 C19 C20 1.3(6) . . . . ? Ti2 N13 C19 C20 -177.4(4) . . . . ? N13 C19 C20 C21 -0.5(6) . . . . ? N13 N14 C21 C20 1.2(6) . . . . ? B3 N14 C21 C20 179.2(5) . . . . ? C19 C20 C21 N14 -0.4(6) . . . . ? N16 N15 C22 C23 -0.1(6) . . . . ? Ti2 N15 C22 C23 176.3(4) . . . . ? N15 C22 C23 C24 -1.2(7) . . . . ? N15 N16 C24 C23 -2.2(6) . . . . ? B3 N16 C24 C23 -175.7(5) . . . . ? C22 C23 C24 N16 2.1(7) . . . . ? N18 N17 C25 C26 -0.5(6) . . . . ? Ti2 N17 C25 C26 174.2(4) . . . . ? N17 C25 C26 C27 0.1(6) . . . . ? N17 N18 C27 C26 -0.6(6) . . . . ? B3 N18 C27 C26 -177.3(5) . . . . ? C25 C26 C27 N18 0.3(6) . . . . ? N20 N19 C28 C29 -1.8(5) . . . . ? Ti2 N19 C28 C29 173.1(3) . . . . ? N19 C28 C29 C30 0.8(6) . . . . ? N19 N20 C30 C29 -1.7(6) . . . . ? B4 N20 C30 C29 -178.2(5) . . . . ? C28 C29 C30 N20 0.6(6) . . . . ? N22 N21 C31 C32 -0.2(6) . . . . ? B4 N21 C31 C32 174.8(5) . . . . ? N21 C31 C32 C33 0.0(6) . . . . ? N21 N22 C33 C32 -0.2(6) . . . . ? C31 C32 C33 N22 0.1(6) . . . . ? N24 N23 C34 C35 0.6(5) . . . . ? Ti2 N23 C34 C35 166.8(3) . . . . ? N23 C34 C35 C36 -0.6(6) . . . . ? N23 N24 C36 C35 -0.1(6) . . . . ? B4 N24 C36 C35 174.2(5) . . . . ? C34 C35 C36 N24 0.4(6) . . . . ? _refine_diff_density_max 0.893 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.097 #===END data_(k2-Tp)(k3-Tp)Ti(k2-S2) _database_code_CSD 172874 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H20 B2 N12 S2 Ti' _chemical_formula_weight 538.10 _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' 'B' 'B' 0.0013 0.0007 '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' 'S' 'S' 0.1246 0.1234 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.0677(4) _cell_length_b 17.2213(3) _cell_length_c 32.9623(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9688.5(4) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 26577 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 23.01 _exptl_crystal_description 'block' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 4416 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26577 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 23.01 _reflns_number_total 6675 _reflns_number_observed 5023 _reflns_observed_criterion 'I>2\s(I)' _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'DENZO-SMN' _computing_structure_solution 'SIEMENS SHELXTL' _computing_structure_refinement 'SIEMENS SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+8.8425P] 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 6675 _refine_ls_number_parameters 643 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_obs 0.0440 _refine_ls_wR_factor_all 0.1237 _refine_ls_wR_factor_obs 0.1085 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.096 _refine_ls_restrained_S_all 1.067 _refine_ls_restrained_S_obs 1.096 _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 0.24649(4) -0.14053(4) 0.60453(2) 0.0273(2) Uani 1 d . . Ti2 Ti 0.58828(4) 0.03988(4) 0.64921(2) 0.0282(2) Uani 1 d . . S1 S 0.36163(6) -0.19014(6) 0.63090(3) 0.0392(3) Uani 1 d . . S2 S 0.26637(6) -0.20586(6) 0.66579(3) 0.0398(3) Uani 1 d . . S3 S 0.52499(6) 0.14935(6) 0.62700(3) 0.0411(3) Uani 1 d . . S4 S 0.50782(6) 0.05496(6) 0.59216(3) 0.0413(3) Uani 1 d . . B1 B 0.1160(3) 0.0027(3) 0.61563(15) 0.0400(11) Uani 1 d . . H101 H 0.0719(23) 0.0523(21) 0.6193(11) 0.048 Uiso 1 d . . B2 B 0.3562(3) -0.2500(2) 0.53254(13) 0.0321(10) Uani 1 d . . H201 H 0.3912(20) -0.2681(19) 0.5597(11) 0.039 Uiso 1 d . . B3 B 0.7428(3) -0.0751(3) 0.63336(14) 0.0392(11) Uani 1 d . . H301 H 0.7915(24) -0.1096(22) 0.6276(11) 0.047 Uiso 1 d . . B4 B 0.4818(3) 0.1309(2) 0.72858(13) 0.0330(10) Uani 1 d . . H401 H 0.4503(21) 0.1650(19) 0.7030(11) 0.040 Uiso 1 d . . N1 N 0.2582(2) -0.0258(2) 0.62906(9) 0.0315(7) Uani 1 d . . N2 N 0.1965(2) 0.0248(2) 0.63215(10) 0.0375(8) Uani 1 d . . N3 N 0.1720(2) -0.0774(2) 0.55951(9) 0.0340(7) Uani 1 d . . N4 N 0.1241(2) -0.0175(2) 0.57078(9) 0.0362(8) Uani 1 d . . N5 N 0.1270(2) -0.1385(2) 0.63363(9) 0.0334(7) Uani 1 d . . N6 N 0.0870(2) -0.0705(2) 0.63758(9) 0.0347(8) Uani 1 d . . N7 N 0.3290(2) -0.1103(2) 0.55572(9) 0.0301(7) Uani 1 d . . N8 N 0.3596(2) -0.1602(2) 0.52798(9) 0.0320(7) Uani 1 d . . N9 N 0.3879(2) -0.2862(2) 0.49387(9) 0.0331(7) Uani 1 d . . N10 N 0.3518(2) -0.2818(2) 0.45699(9) 0.0392(8) Uani 1 d . . N11 N 0.2212(2) -0.2385(2) 0.56685(8) 0.0293(7) Uani 1 d . . N12 N 0.2691(2) -0.2743(2) 0.53906(8) 0.0292(7) Uani 1 d . . N13 N 0.6983(2) 0.0625(2) 0.61933(9) 0.0329(7) Uani 1 d . . N14 N 0.7563(2) 0.0080(2) 0.61810(9) 0.0359(8) Uani 1 d . . N15 N 0.6646(2) -0.0269(2) 0.69176(9) 0.0343(7) Uani 1 d . . N16 N 0.7247(2) -0.0720(2) 0.67872(9) 0.0368(8) Uani 1 d . . N17 N 0.5978(2) -0.0763(2) 0.61821(9) 0.0332(7) Uani 1 d . . N18 N 0.6704(2) -0.1079(2) 0.61191(9) 0.0347(7) Uani 1 d . . N19 N 0.6199(2) 0.1242(2) 0.69686(9) 0.0333(7) Uani 1 d . . N20 N 0.5719(2) 0.1474(2) 0.72761(9) 0.0332(7) Uani 1 d . . N21 N 0.4510(2) 0.1564(2) 0.76968(9) 0.0374(8) Uani 1 d . . N22 N 0.4746(2) 0.1226(2) 0.80529(10) 0.0488(9) Uani 1 d . . N23 N 0.5032(2) 0.0010(2) 0.69197(9) 0.0292(7) Uani 1 d . . N24 N 0.4686(2) 0.0422(2) 0.72276(9) 0.0312(7) Uani 1 d . . C1 C 0.3200(2) 0.0105(2) 0.64580(11) 0.0401(10) Uani 1 d . . H1 H 0.3713(2) -0.0107(2) 0.64785(11) 0.048 Uiso 1 calc R . C2 C 0.2982(3) 0.0826(2) 0.65951(14) 0.0563(13) Uani 1 d . . H2 H 0.3304(3) 0.1199(2) 0.67259(14) 0.068 Uiso 1 calc R . C3 C 0.2205(3) 0.0894(2) 0.65041(14) 0.0561(13) Uani 1 d . . H3 H 0.1886(3) 0.1333(2) 0.65619(14) 0.067 Uiso 1 calc R . C4 C 0.1683(2) -0.0808(2) 0.51914(12) 0.0439(10) Uani 1 d . . H4 H 0.1957(2) -0.1173(2) 0.50279(12) 0.053 Uiso 1 calc R . C5 C 0.1187(3) -0.0233(3) 0.50446(13) 0.0578(13) Uani 1 d . . H5 H 0.1061(3) -0.0129(3) 0.47692(13) 0.069 Uiso 1 calc R . C6 C 0.0921(2) 0.0149(3) 0.53767(14) 0.0511(12) Uani 1 d . . H6 H 0.0568(2) 0.0575(3) 0.53753(14) 0.061 Uiso 1 calc R . C7 C 0.0876(2) -0.1902(2) 0.65593(12) 0.0421(10) Uani 1 d . . H7 H 0.1019(2) -0.2433(2) 0.65885(12) 0.051 Uiso 1 calc R . C8 C 0.0234(3) -0.1561(3) 0.67418(14) 0.0531(12) Uani 1 d . . H8 H -0.0143(3) -0.1803(3) 0.69127(14) 0.064 Uiso 1 calc R . C9 C 0.0257(2) -0.0802(3) 0.66232(12) 0.0483(11) Uani 1 d . . H9 H -0.0102(2) -0.0409(3) 0.67029(12) 0.058 Uiso 1 calc R . C10 C 0.3479(2) -0.0387(2) 0.54315(11) 0.0360(9) Uani 1 d . . H10 H 0.3337(2) 0.0078(2) 0.55680(11) 0.043 Uiso 1 calc R . C11 C 0.3905(2) -0.0416(2) 0.50784(12) 0.0434(11) Uani 1 d . . H11 H 0.4114(2) 0.0007(2) 0.49287(12) 0.052 Uiso 1 calc R . C12 C 0.3963(2) -0.1195(2) 0.49895(12) 0.0417(10) Uani 1 d . . H12 H 0.4221(2) -0.1410(2) 0.47601(12) 0.050 Uiso 1 calc R . C13 C 0.4608(2) -0.3171(2) 0.48939(13) 0.0387(10) Uani 1 d . . H13 H 0.4975(2) -0.3254(2) 0.51058(13) 0.046 Uiso 1 calc R . C14 C 0.4722(2) -0.3342(2) 0.44940(13) 0.0438(10) Uani 1 d . . H14 H 0.5173(2) -0.3565(2) 0.43712(13) 0.053 Uiso 1 calc R . C15 C 0.4027(2) -0.3114(2) 0.43070(13) 0.0443(11) Uani 1 d . . H15 H 0.3929(2) -0.3165(2) 0.40245(13) 0.053 Uiso 1 calc R . C16 C 0.1517(2) -0.2755(2) 0.56498(11) 0.0326(9) Uani 1 d . . H16 H 0.1072(2) -0.2629(2) 0.58099(11) 0.039 Uiso 1 calc R . C17 C 0.1545(2) -0.3343(2) 0.53643(11) 0.0379(10) Uani 1 d . . H17 H 0.1136(2) -0.3689(2) 0.52903(11) 0.046 Uiso 1 calc R . C18 C 0.2294(2) -0.3316(2) 0.52111(11) 0.0378(10) Uani 1 d . . H18 H 0.2497(2) -0.3653(2) 0.50087(11) 0.045 Uiso 1 calc R . C19 C 0.7267(2) 0.1263(2) 0.60142(11) 0.0390(10) Uani 1 d . . H19 H 0.6988(2) 0.1736(2) 0.59813(11) 0.047 Uiso 1 calc R . C20 C 0.8028(3) 0.1131(2) 0.58836(12) 0.0466(11) Uani 1 d . . H20 H 0.8363(3) 0.1482(2) 0.57449(12) 0.056 Uiso 1 calc R . C21 C 0.8190(2) 0.0387(3) 0.59980(12) 0.0468(11) Uani 1 d . . H21 H 0.8673(2) 0.0127(3) 0.59543(12) 0.056 Uiso 1 calc R . C22 C 0.6627(2) -0.0347(2) 0.73228(11) 0.0408(10) Uani 1 d . . H22 H 0.6262(2) -0.0098(2) 0.74968(11) 0.049 Uiso 1 calc R . C23 C 0.7215(3) -0.0839(2) 0.74502(13) 0.0512(11) Uani 1 d . . H23 H 0.7332(3) -0.0990(2) 0.77207(13) 0.061 Uiso 1 calc R . C24 C 0.7591(2) -0.1062(2) 0.71066(13) 0.0475(11) Uani 1 d . . H24 H 0.8026(2) -0.1405(2) 0.70944(13) 0.057 Uiso 1 calc R . C25 C 0.5489(2) -0.1170(2) 0.59475(11) 0.0396(10) Uani 1 d . . H25 H 0.4940(2) -0.1083(2) 0.59305(11) 0.047 Uiso 1 calc R . C26 C 0.5888(3) -0.1736(2) 0.57326(13) 0.0489(11) Uani 1 d . . H26 H 0.5677(3) -0.2099(2) 0.55450(13) 0.059 Uiso 1 calc R . C27 C 0.6655(3) -0.1660(2) 0.58494(12) 0.0454(11) Uani 1 d . . H27 H 0.7080(3) -0.1966(2) 0.57551(12) 0.054 Uiso 1 calc R . C28 C 0.6904(2) 0.1535(2) 0.70469(12) 0.0410(10) Uani 1 d . . H28 H 0.7353(2) 0.1463(2) 0.68804(12) 0.049 Uiso 1 calc R . C29 C 0.6896(3) 0.1956(2) 0.74018(12) 0.0458(11) Uani 1 d . . H29 H 0.7322(3) 0.2224(2) 0.75243(12) 0.055 Uiso 1 calc R . C30 C 0.6138(2) 0.1904(2) 0.75405(12) 0.0437(10) Uani 1 d . . H30 H 0.5942(2) 0.2133(2) 0.77822(12) 0.052 Uiso 1 calc R . C31 C 0.4099(2) 0.2219(2) 0.77777(14) 0.0458(11) Uani 1 d . . H31 H 0.3874(2) 0.2555(2) 0.75809(14) 0.055 Uiso 1 calc R . C32 C 0.4059(3) 0.2316(3) 0.81833(14) 0.0563(13) Uani 1 d . . H32 H 0.3811(3) 0.2725(3) 0.83279(14) 0.068 Uiso 1 calc R . C33 C 0.4464(3) 0.1681(3) 0.83435(13) 0.0559(12) Uani 1 d . . H33 H 0.4530(3) 0.1587(3) 0.86254(13) 0.067 Uiso 1 calc R . C34 C 0.4792(2) -0.0726(2) 0.69649(11) 0.0325(9) Uani 1 d . . H34 H 0.4954(2) -0.1145(2) 0.67973(11) 0.039 Uiso 1 calc R . C35 C 0.4283(2) -0.0794(2) 0.72846(11) 0.0387(10) Uani 1 d . . H35 H 0.4025(2) -0.1251(2) 0.73762(11) 0.046 Uiso 1 calc R . C36 C 0.4229(2) -0.0058(2) 0.74436(12) 0.0403(10) Uani 1 d . . H36 H 0.3917(2) 0.0087(2) 0.76700(12) 0.048 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 0.0315(4) 0.0217(4) 0.0285(4) -0.0011(3) -0.0003(3) -0.0006(3) Ti2 0.0284(4) 0.0289(4) 0.0273(4) 0.0008(3) 0.0006(3) 0.0010(3) S1 0.0411(6) 0.0370(6) 0.0396(6) -0.0017(4) -0.0066(5) 0.0039(5) S2 0.0553(7) 0.0321(6) 0.0322(5) 0.0015(4) 0.0011(5) 0.0044(5) S3 0.0450(6) 0.0374(6) 0.0409(6) 0.0063(5) 0.0016(5) 0.0074(5) S4 0.0428(6) 0.0479(7) 0.0331(5) 0.0013(5) -0.0032(5) 0.0037(5) B1 0.035(3) 0.033(3) 0.052(3) -0.002(2) 0.001(2) 0.004(2) B2 0.032(2) 0.028(2) 0.036(2) -0.001(2) 0.003(2) 0.001(2) B3 0.033(3) 0.037(3) 0.048(3) 0.002(2) 0.005(2) 0.007(2) B4 0.036(3) 0.031(3) 0.032(2) -0.001(2) -0.003(2) 0.000(2) N1 0.035(2) 0.024(2) 0.036(2) -0.0003(13) 0.0002(15) -0.0002(14) N2 0.042(2) 0.018(2) 0.052(2) -0.0050(15) 0.000(2) 0.0030(15) N3 0.032(2) 0.035(2) 0.035(2) 0.0037(14) 0.0007(15) 0.0021(15) N4 0.034(2) 0.031(2) 0.043(2) 0.0043(15) -0.004(2) 0.000(2) N5 0.039(2) 0.025(2) 0.036(2) -0.0023(14) 0.006(2) -0.001(2) N6 0.035(2) 0.028(2) 0.041(2) -0.0050(14) 0.004(2) 0.0034(15) N7 0.032(2) 0.023(2) 0.036(2) -0.0007(14) 0.0011(15) -0.0017(14) N8 0.030(2) 0.028(2) 0.038(2) -0.0020(14) 0.0057(15) -0.0020(14) N9 0.031(2) 0.031(2) 0.038(2) -0.0022(14) 0.0019(15) 0.0004(14) N10 0.038(2) 0.044(2) 0.035(2) -0.0052(15) 0.001(2) -0.003(2) N11 0.031(2) 0.024(2) 0.032(2) -0.0034(13) 0.0038(14) -0.0026(14) N12 0.033(2) 0.022(2) 0.033(2) -0.0030(13) 0.0055(14) -0.0015(13) N13 0.033(2) 0.034(2) 0.032(2) -0.0001(14) 0.0035(15) 0.001(2) N14 0.032(2) 0.037(2) 0.039(2) -0.0025(15) 0.003(2) 0.003(2) N15 0.034(2) 0.034(2) 0.035(2) 0.0016(14) -0.0017(15) 0.0025(15) N16 0.032(2) 0.032(2) 0.047(2) 0.003(2) -0.003(2) 0.0046(15) N17 0.035(2) 0.030(2) 0.034(2) -0.0029(14) 0.0006(15) -0.0014(14) N18 0.036(2) 0.032(2) 0.036(2) -0.0020(15) 0.005(2) 0.0026(15) N19 0.035(2) 0.029(2) 0.036(2) -0.0029(14) 0.001(2) -0.0009(14) N20 0.036(2) 0.031(2) 0.033(2) -0.0019(14) 0.001(2) 0.0009(14) N21 0.040(2) 0.034(2) 0.039(2) -0.0031(15) 0.002(2) 0.004(2) N22 0.067(3) 0.046(2) 0.034(2) 0.000(2) 0.006(2) 0.008(2) N23 0.030(2) 0.028(2) 0.030(2) 0.0009(14) -0.0008(14) 0.0013(14) N24 0.031(2) 0.031(2) 0.031(2) -0.0005(14) 0.0018(15) 0.0045(14) C1 0.044(2) 0.032(2) 0.045(2) -0.003(2) -0.011(2) -0.004(2) C2 0.060(3) 0.030(3) 0.078(3) -0.014(2) -0.021(3) -0.006(2) C3 0.059(3) 0.027(3) 0.083(3) -0.015(2) -0.013(3) 0.007(2) C4 0.038(2) 0.058(3) 0.035(2) 0.005(2) 0.000(2) 0.001(2) C5 0.054(3) 0.081(3) 0.038(3) 0.019(2) -0.004(2) 0.011(3) C6 0.042(3) 0.053(3) 0.059(3) 0.020(2) -0.004(2) 0.009(2) C7 0.043(2) 0.036(2) 0.047(2) 0.001(2) 0.008(2) -0.002(2) C8 0.052(3) 0.049(3) 0.059(3) 0.003(2) 0.022(2) -0.007(2) C9 0.043(3) 0.057(3) 0.045(3) -0.010(2) 0.013(2) 0.007(2) C10 0.039(2) 0.026(2) 0.042(2) -0.002(2) 0.001(2) -0.005(2) C11 0.057(3) 0.032(3) 0.041(2) 0.001(2) 0.010(2) -0.012(2) C12 0.049(3) 0.037(3) 0.038(2) -0.003(2) 0.012(2) -0.006(2) C13 0.032(2) 0.030(2) 0.053(3) 0.002(2) 0.006(2) 0.001(2) C14 0.038(2) 0.036(2) 0.058(3) -0.006(2) 0.014(2) -0.003(2) C15 0.049(3) 0.043(3) 0.041(2) -0.011(2) 0.012(2) -0.015(2) C16 0.032(2) 0.030(2) 0.036(2) 0.001(2) 0.003(2) -0.002(2) C17 0.040(2) 0.030(2) 0.043(2) -0.004(2) 0.003(2) -0.009(2) C18 0.048(3) 0.025(2) 0.041(2) -0.007(2) 0.010(2) -0.005(2) C19 0.043(2) 0.034(2) 0.040(2) 0.000(2) 0.007(2) -0.006(2) C20 0.046(3) 0.049(3) 0.045(2) 0.010(2) 0.007(2) -0.010(2) C21 0.029(2) 0.062(3) 0.049(3) 0.004(2) 0.011(2) -0.002(2) C22 0.045(2) 0.046(3) 0.031(2) 0.006(2) -0.005(2) 0.000(2) C23 0.053(3) 0.058(3) 0.042(3) 0.017(2) -0.015(2) 0.001(2) C24 0.041(3) 0.042(3) 0.060(3) 0.011(2) -0.013(2) 0.008(2) C25 0.041(2) 0.042(2) 0.036(2) 0.000(2) 0.000(2) -0.006(2) C26 0.062(3) 0.039(3) 0.046(3) -0.014(2) 0.000(2) -0.011(2) C27 0.054(3) 0.037(3) 0.045(2) -0.006(2) 0.009(2) 0.002(2) C28 0.036(2) 0.039(2) 0.048(2) -0.001(2) 0.003(2) -0.005(2) C29 0.049(3) 0.047(3) 0.042(2) -0.011(2) -0.007(2) -0.012(2) C30 0.054(3) 0.040(2) 0.037(2) -0.013(2) 0.000(2) -0.007(2) C31 0.037(2) 0.041(3) 0.059(3) -0.010(2) 0.005(2) 0.004(2) C32 0.056(3) 0.056(3) 0.057(3) -0.024(2) 0.017(2) 0.005(2) C33 0.071(3) 0.059(3) 0.038(2) -0.007(2) 0.009(2) -0.005(3) C34 0.034(2) 0.028(2) 0.035(2) 0.000(2) -0.001(2) 0.003(2) C35 0.043(2) 0.032(2) 0.042(2) 0.002(2) 0.007(2) -0.007(2) C36 0.037(2) 0.045(3) 0.038(2) 0.002(2) 0.009(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N11 2.139(3) . ? Ti1 N1 2.145(3) . ? Ti1 N7 2.200(3) . ? Ti1 N3 2.236(3) . ? Ti1 N5 2.254(3) . ? Ti1 S1 2.3125(12) . ? Ti1 S2 2.3365(12) . ? Ti2 N23 2.131(3) . ? Ti2 N13 2.157(3) . ? Ti2 N19 2.207(3) . ? Ti2 N15 2.233(3) . ? Ti2 N17 2.253(3) . ? Ti2 S3 2.2929(11) . ? Ti2 S4 2.3430(12) . ? S1 S2 2.0099(14) . ? S3 S4 2.0118(15) . ? B1 N4 1.525(6) . ? B1 N2 1.527(6) . ? B1 N6 1.536(6) . ? B2 N9 1.518(5) . ? B2 N8 1.555(5) . ? B2 N12 1.560(5) . ? B3 N16 1.527(6) . ? B3 N18 1.532(6) . ? B3 N14 1.534(6) . ? B4 N21 1.518(5) . ? B4 N24 1.556(5) . ? B4 N20 1.564(5) . ? N1 C1 1.344(5) . ? N1 N2 1.370(4) . ? N2 C3 1.330(5) . ? N3 C4 1.333(5) . ? N3 N4 1.368(4) . ? N4 C6 1.342(5) . ? N5 C7 1.336(5) . ? N5 N6 1.361(4) . ? N6 C9 1.337(5) . ? N7 C10 1.340(4) . ? N7 N8 1.360(4) . ? N8 C12 1.342(5) . ? N9 C13 1.360(5) . ? N9 N10 1.365(4) . ? N10 C15 1.329(5) . ? N11 C16 1.348(4) . ? N11 N12 1.374(4) . ? N12 C18 1.335(5) . ? N13 C19 1.337(5) . ? N13 N14 1.365(4) . ? N14 C21 1.337(5) . ? N15 C22 1.343(5) . ? N15 N16 1.357(4) . ? N16 C24 1.341(5) . ? N17 C25 1.337(5) . ? N17 N18 1.369(4) . ? N18 C27 1.340(5) . ? N19 C28 1.330(5) . ? N19 N20 1.363(4) . ? N20 C30 1.349(5) . ? N21 C31 1.356(5) . ? N21 N22 1.371(4) . ? N22 C33 1.328(5) . ? N23 C34 1.341(4) . ? N23 N24 1.372(4) . ? N24 C36 1.342(5) . ? C1 C2 1.373(5) . ? C2 C3 1.365(6) . ? C4 C5 1.391(6) . ? C5 C6 1.355(6) . ? C7 C8 1.382(6) . ? C8 C9 1.365(6) . ? C10 C11 1.374(5) . ? C11 C12 1.377(5) . ? C13 C14 1.365(5) . ? C14 C15 1.393(6) . ? C16 C17 1.383(5) . ? C17 C18 1.374(5) . ? C19 C20 1.387(6) . ? C20 C21 1.364(6) . ? C22 C23 1.378(6) . ? C23 C24 1.357(6) . ? C25 C26 1.385(6) . ? C26 C27 1.370(6) . ? C28 C29 1.376(5) . ? C29 C30 1.376(6) . ? C31 C32 1.349(6) . ? C32 C33 1.397(6) . ? C34 C35 1.371(5) . ? C35 C36 1.376(5) . ? 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 N11 Ti1 N1 164.71(11) . . ? N11 Ti1 N7 83.76(11) . . ? N1 Ti1 N7 89.86(11) . . ? N11 Ti1 N3 83.32(11) . . ? N1 Ti1 N3 81.66(11) . . ? N7 Ti1 N3 76.30(11) . . ? N11 Ti1 N5 94.40(11) . . ? N1 Ti1 N5 84.83(11) . . ? N7 Ti1 N5 152.43(11) . . ? N3 Ti1 N5 76.16(11) . . ? N11 Ti1 S1 95.64(8) . . ? N1 Ti1 S1 96.85(9) . . ? N7 Ti1 S1 79.55(8) . . ? N3 Ti1 S1 155.81(9) . . ? N5 Ti1 S1 127.92(8) . . ? N11 Ti1 S2 98.71(8) . . ? N1 Ti1 S2 95.99(8) . . ? N7 Ti1 S2 130.77(8) . . ? N3 Ti1 S2 152.91(9) . . ? N5 Ti1 S2 76.75(8) . . ? S1 Ti1 S2 51.23(4) . . ? N23 Ti2 N13 162.22(11) . . ? N23 Ti2 N19 84.41(11) . . ? N13 Ti2 N19 89.59(11) . . ? N23 Ti2 N15 79.66(11) . . ? N13 Ti2 N15 82.64(11) . . ? N19 Ti2 N15 75.48(11) . . ? N23 Ti2 N17 94.04(11) . . ? N13 Ti2 N17 83.72(11) . . ? N19 Ti2 N17 152.87(11) . . ? N15 Ti2 N17 77.59(11) . . ? N23 Ti2 S3 98.51(8) . . ? N13 Ti2 S3 96.66(9) . . ? N19 Ti2 S3 78.54(8) . . ? N15 Ti2 S3 154.02(9) . . ? N17 Ti2 S3 128.28(8) . . ? N23 Ti2 S4 99.56(8) . . ? N13 Ti2 S4 97.12(9) . . ? N19 Ti2 S4 129.93(8) . . ? N15 Ti2 S4 154.55(9) . . ? N17 Ti2 S4 77.10(8) . . ? S3 Ti2 S4 51.42(4) . . ? S2 S1 Ti1 65.00(4) . . ? S1 S2 Ti1 63.77(4) . . ? S4 S3 Ti2 65.57(4) . . ? S3 S4 Ti2 63.00(4) . . ? N4 B1 N2 108.7(3) . . ? N4 B1 N6 107.3(3) . . ? N2 B1 N6 109.1(3) . . ? N9 B2 N8 108.3(3) . . ? N9 B2 N12 110.2(3) . . ? N8 B2 N12 108.4(3) . . ? N16 B3 N18 107.6(3) . . ? N16 B3 N14 108.6(3) . . ? N18 B3 N14 108.3(3) . . ? N21 B4 N24 110.1(3) . . ? N21 B4 N20 107.9(3) . . ? N24 B4 N20 108.5(3) . . ? C1 N1 N2 106.1(3) . . ? C1 N1 Ti1 131.0(3) . . ? N2 N1 Ti1 122.8(2) . . ? C3 N2 N1 109.2(3) . . ? C3 N2 B1 130.2(3) . . ? N1 N2 B1 120.5(3) . . ? C4 N3 N4 106.0(3) . . ? C4 N3 Ti1 131.9(3) . . ? N4 N3 Ti1 121.8(2) . . ? C6 N4 N3 109.6(3) . . ? C6 N4 B1 131.0(4) . . ? N3 N4 B1 119.3(3) . . ? C7 N5 N6 105.6(3) . . ? C7 N5 Ti1 132.8(3) . . ? N6 N5 Ti1 120.5(2) . . ? C9 N6 N5 110.1(3) . . ? C9 N6 B1 129.9(3) . . ? N5 N6 B1 120.0(3) . . ? C10 N7 N8 106.4(3) . . ? C10 N7 Ti1 126.7(2) . . ? N8 N7 Ti1 126.0(2) . . ? C12 N8 N7 109.2(3) . . ? C12 N8 B2 127.3(3) . . ? N7 N8 B2 123.4(3) . . ? C13 N9 N10 109.7(3) . . ? C13 N9 B2 125.3(3) . . ? N10 N9 B2 124.3(3) . . ? C15 N10 N9 105.3(3) . . ? C16 N11 N12 106.3(3) . . ? C16 N11 Ti1 125.2(2) . . ? N12 N11 Ti1 128.4(2) . . ? C18 N12 N11 109.0(3) . . ? C18 N12 B2 128.4(3) . . ? N11 N12 B2 122.6(3) . . ? C19 N13 N14 106.9(3) . . ? C19 N13 Ti2 131.7(3) . . ? N14 N13 Ti2 121.4(2) . . ? C21 N14 N13 108.7(3) . . ? C21 N14 B3 129.7(3) . . ? N13 N14 B3 121.5(3) . . ? C22 N15 N16 106.0(3) . . ? C22 N15 Ti2 131.5(3) . . ? N16 N15 Ti2 122.5(2) . . ? C24 N16 N15 109.5(3) . . ? C24 N16 B3 131.7(3) . . ? N15 N16 B3 118.9(3) . . ? C25 N17 N18 105.6(3) . . ? C25 N17 Ti2 133.1(3) . . ? N18 N17 Ti2 119.2(2) . . ? C27 N18 N17 109.9(3) . . ? C27 N18 B3 129.1(3) . . ? N17 N18 B3 120.9(3) . . ? C28 N19 N20 106.8(3) . . ? C28 N19 Ti2 127.5(3) . . ? N20 N19 Ti2 125.1(2) . . ? C30 N20 N19 108.8(3) . . ? C30 N20 B4 127.4(3) . . ? N19 N20 B4 123.6(3) . . ? C31 N21 N22 109.7(3) . . ? C31 N21 B4 126.5(3) . . ? N22 N21 B4 122.7(3) . . ? C33 N22 N21 105.1(3) . . ? C34 N23 N24 106.0(3) . . ? C34 N23 Ti2 125.3(2) . . ? N24 N23 Ti2 128.3(2) . . ? C36 N24 N23 108.9(3) . . ? C36 N24 B4 128.6(3) . . ? N23 N24 B4 122.5(3) . . ? N1 C1 C2 110.0(4) . . ? C3 C2 C1 105.6(4) . . ? N2 C3 C2 109.0(4) . . ? N3 C4 C5 110.1(4) . . ? C6 C5 C4 105.6(4) . . ? N4 C6 C5 108.6(4) . . ? N5 C7 C8 110.8(4) . . ? C9 C8 C7 105.0(4) . . ? N6 C9 C8 108.5(4) . . ? N7 C10 C11 110.8(3) . . ? C10 C11 C12 104.7(3) . . ? N8 C12 C11 108.9(3) . . ? N9 C13 C14 108.7(4) . . ? C13 C14 C15 104.2(4) . . ? N10 C15 C14 112.1(4) . . ? N11 C16 C17 110.3(3) . . ? C18 C17 C16 104.9(3) . . ? N12 C18 C17 109.5(3) . . ? N13 C19 C20 110.0(4) . . ? C21 C20 C19 104.9(4) . . ? N14 C21 C20 109.6(4) . . ? N15 C22 C23 110.3(4) . . ? C24 C23 C22 105.3(4) . . ? N16 C24 C23 109.0(4) . . ? N17 C25 C26 110.9(4) . . ? C27 C26 C25 105.0(4) . . ? N18 C27 C26 108.5(4) . . ? N19 C28 C29 110.8(4) . . ? C30 C29 C28 104.9(4) . . ? N20 C30 C29 108.6(3) . . ? C32 C31 N21 108.9(4) . . ? C31 C32 C33 104.6(4) . . ? N22 C33 C32 111.6(4) . . ? N23 C34 C35 111.1(3) . . ? C34 C35 C36 104.8(3) . . ? N24 C36 C35 109.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 Ti1 S1 S2 -96.65(9) . . . . ? N1 Ti1 S1 S2 92.19(9) . . . . ? N7 Ti1 S1 S2 -179.22(9) . . . . ? N3 Ti1 S1 S2 177.1(2) . . . . ? N5 Ti1 S1 S2 3.42(10) . . . . ? S2 Ti1 S1 S2 0.0 . . . . ? Ti1 S1 S2 Ti1 0.0 . . . . ? N11 Ti1 S2 S1 90.26(9) . . . . ? N1 Ti1 S2 S1 -93.99(9) . . . . ? N7 Ti1 S2 S1 1.02(11) . . . . ? N3 Ti1 S2 S1 -177.4(2) . . . . ? N5 Ti1 S2 S1 -177.23(9) . . . . ? S1 Ti1 S2 S1 0.0 . . . . ? N23 Ti2 S3 S4 -95.48(9) . . . . ? N13 Ti2 S3 S4 93.82(9) . . . . ? N19 Ti2 S3 S4 -177.96(9) . . . . ? N15 Ti2 S3 S4 -179.3(2) . . . . ? N17 Ti2 S3 S4 6.57(11) . . . . ? S4 Ti2 S3 S4 0.0 . . . . ? Ti2 S3 S4 Ti2 0.0 . . . . ? N23 Ti2 S4 S3 93.30(9) . . . . ? N13 Ti2 S4 S3 -92.86(9) . . . . ? N19 Ti2 S4 S3 2.61(12) . . . . ? N15 Ti2 S4 S3 179.3(2) . . . . ? N17 Ti2 S4 S3 -174.71(9) . . . . ? S3 Ti2 S4 S3 0.0 . . . . ? N11 Ti1 N1 C1 -130.8(4) . . . . ? N7 Ti1 N1 C1 -65.7(3) . . . . ? N3 Ti1 N1 C1 -141.9(3) . . . . ? N5 Ti1 N1 C1 141.4(3) . . . . ? S1 Ti1 N1 C1 13.7(3) . . . . ? S2 Ti1 N1 C1 65.3(3) . . . . ? N11 Ti1 N1 N2 53.1(6) . . . . ? N7 Ti1 N1 N2 118.2(3) . . . . ? N3 Ti1 N1 N2 42.0(3) . . . . ? N5 Ti1 N1 N2 -34.7(3) . . . . ? S1 Ti1 N1 N2 -162.4(3) . . . . ? S2 Ti1 N1 N2 -110.8(3) . . . . ? C1 N1 N2 C3 -0.3(4) . . . . ? Ti1 N1 N2 C3 176.6(3) . . . . ? C1 N1 N2 B1 179.4(3) . . . . ? Ti1 N1 N2 B1 -3.6(5) . . . . ? N4 B1 N2 C3 123.1(4) . . . . ? N6 B1 N2 C3 -120.2(4) . . . . ? N4 B1 N2 N1 -56.5(4) . . . . ? N6 B1 N2 N1 60.2(4) . . . . ? N11 Ti1 N3 C4 -42.4(4) . . . . ? N1 Ti1 N3 C4 134.7(4) . . . . ? N7 Ti1 N3 C4 42.8(3) . . . . ? N5 Ti1 N3 C4 -138.6(4) . . . . ? S1 Ti1 N3 C4 46.6(5) . . . . ? S2 Ti1 N3 C4 -138.4(3) . . . . ? N11 Ti1 N3 N4 145.1(3) . . . . ? N1 Ti1 N3 N4 -37.8(3) . . . . ? N7 Ti1 N3 N4 -129.7(3) . . . . ? N5 Ti1 N3 N4 48.9(3) . . . . ? S1 Ti1 N3 N4 -126.0(2) . . . . ? S2 Ti1 N3 N4 49.1(4) . . . . ? C4 N3 N4 C6 -0.2(4) . . . . ? Ti1 N3 N4 C6 174.0(3) . . . . ? C4 N3 N4 B1 -179.2(3) . . . . ? Ti1 N3 N4 B1 -5.0(4) . . . . ? N2 B1 N4 C6 -118.6(4) . . . . ? N6 B1 N4 C6 123.6(4) . . . . ? N2 B1 N4 N3 60.1(4) . . . . ? N6 B1 N4 N3 -57.7(4) . . . . ? N11 Ti1 N5 C7 60.6(3) . . . . ? N1 Ti1 N5 C7 -134.8(3) . . . . ? N7 Ti1 N5 C7 145.5(3) . . . . ? N3 Ti1 N5 C7 142.6(4) . . . . ? S1 Ti1 N5 C7 -40.1(4) . . . . ? S2 Ti1 N5 C7 -37.4(3) . . . . ? N11 Ti1 N5 N6 -133.7(3) . . . . ? N1 Ti1 N5 N6 31.0(2) . . . . ? N7 Ti1 N5 N6 -48.8(4) . . . . ? N3 Ti1 N5 N6 -51.7(2) . . . . ? S1 Ti1 N5 N6 125.6(2) . . . . ? S2 Ti1 N5 N6 128.4(3) . . . . ? C7 N5 N6 C9 1.2(4) . . . . ? Ti1 N5 N6 C9 -168.0(3) . . . . ? C7 N5 N6 B1 -179.9(3) . . . . ? Ti1 N5 N6 B1 10.9(4) . . . . ? N4 B1 N6 C9 -127.2(4) . . . . ? N2 B1 N6 C9 115.2(4) . . . . ? N4 B1 N6 N5 54.2(4) . . . . ? N2 B1 N6 N5 -63.4(4) . . . . ? N11 Ti1 N7 C10 145.9(3) . . . . ? N1 Ti1 N7 C10 -20.2(3) . . . . ? N3 Ti1 N7 C10 61.3(3) . . . . ? N5 Ti1 N7 C10 58.3(4) . . . . ? S1 Ti1 N7 C10 -117.2(3) . . . . ? S2 Ti1 N7 C10 -118.0(3) . . . . ? N11 Ti1 N7 N8 -21.5(3) . . . . ? N1 Ti1 N7 N8 172.4(3) . . . . ? N3 Ti1 N7 N8 -106.2(3) . . . . ? N5 Ti1 N7 N8 -109.1(3) . . . . ? S1 Ti1 N7 N8 75.4(3) . . . . ? S2 Ti1 N7 N8 74.6(3) . . . . ? C10 N7 N8 C12 -0.1(4) . . . . ? Ti1 N7 N8 C12 169.4(2) . . . . ? C10 N7 N8 B2 175.6(3) . . . . ? Ti1 N7 N8 B2 -14.9(4) . . . . ? N9 B2 N8 C12 -11.2(5) . . . . ? N12 B2 N8 C12 -130.8(4) . . . . ? N9 B2 N8 N7 173.8(3) . . . . ? N12 B2 N8 N7 54.3(4) . . . . ? N8 B2 N9 C13 102.2(4) . . . . ? N12 B2 N9 C13 -139.4(3) . . . . ? N8 B2 N9 N10 -67.4(4) . . . . ? N12 B2 N9 N10 51.0(4) . . . . ? C13 N9 N10 C15 1.1(4) . . . . ? B2 N9 N10 C15 172.0(3) . . . . ? N1 Ti1 N11 C16 -84.3(5) . . . . ? N7 Ti1 N11 C16 -150.2(3) . . . . ? N3 Ti1 N11 C16 -73.3(3) . . . . ? N5 Ti1 N11 C16 2.2(3) . . . . ? S1 Ti1 N11 C16 131.0(3) . . . . ? S2 Ti1 N11 C16 79.5(3) . . . . ? N1 Ti1 N11 N12 92.8(5) . . . . ? N7 Ti1 N11 N12 27.0(3) . . . . ? N3 Ti1 N11 N12 103.9(3) . . . . ? N5 Ti1 N11 N12 179.3(3) . . . . ? S1 Ti1 N11 N12 -51.8(3) . . . . ? S2 Ti1 N11 N12 -103.4(3) . . . . ? C16 N11 N12 C18 -0.3(4) . . . . ? Ti1 N11 N12 C18 -177.8(2) . . . . ? C16 N11 N12 B2 -178.4(3) . . . . ? Ti1 N11 N12 B2 4.1(4) . . . . ? N9 B2 N12 C18 15.5(5) . . . . ? N8 B2 N12 C18 133.8(4) . . . . ? N9 B2 N12 N11 -166.8(3) . . . . ? N8 B2 N12 N11 -48.5(4) . . . . ? N23 Ti2 N13 C19 -135.5(4) . . . . ? N19 Ti2 N13 C19 -65.5(3) . . . . ? N15 Ti2 N13 C19 -140.9(3) . . . . ? N17 Ti2 N13 C19 140.9(3) . . . . ? S3 Ti2 N13 C19 12.9(3) . . . . ? S4 Ti2 N13 C19 64.8(3) . . . . ? N23 Ti2 N13 N14 40.6(5) . . . . ? N19 Ti2 N13 N14 110.6(3) . . . . ? N15 Ti2 N13 N14 35.2(3) . . . . ? N17 Ti2 N13 N14 -43.1(3) . . . . ? S3 Ti2 N13 N14 -171.0(2) . . . . ? S4 Ti2 N13 N14 -119.2(2) . . . . ? C19 N13 N14 C21 0.3(4) . . . . ? Ti2 N13 N14 C21 -176.7(2) . . . . ? C19 N13 N14 B3 -175.7(3) . . . . ? Ti2 N13 N14 B3 7.4(4) . . . . ? N16 B3 N14 C21 121.9(4) . . . . ? N18 B3 N14 C21 -121.6(4) . . . . ? N16 B3 N14 N13 -63.1(4) . . . . ? N18 B3 N14 N13 53.5(4) . . . . ? N23 Ti2 N15 C22 -37.4(3) . . . . ? N13 Ti2 N15 C22 141.0(3) . . . . ? N19 Ti2 N15 C22 49.5(3) . . . . ? N17 Ti2 N15 C22 -133.9(4) . . . . ? S3 Ti2 N15 C22 50.9(4) . . . . ? S4 Ti2 N15 C22 -127.9(3) . . . . ? N23 Ti2 N15 N16 140.7(3) . . . . ? N13 Ti2 N15 N16 -41.0(3) . . . . ? N19 Ti2 N15 N16 -132.5(3) . . . . ? N17 Ti2 N15 N16 44.2(3) . . . . ? S3 Ti2 N15 N16 -131.1(2) . . . . ? S4 Ti2 N15 N16 50.1(4) . . . . ? C22 N15 N16 C24 -0.3(4) . . . . ? Ti2 N15 N16 C24 -178.8(3) . . . . ? C22 N15 N16 B3 -179.4(3) . . . . ? Ti2 N15 N16 B3 2.1(4) . . . . ? N18 B3 N16 C24 119.7(4) . . . . ? N14 B3 N16 C24 -123.3(4) . . . . ? N18 B3 N16 N15 -61.4(4) . . . . ? N14 B3 N16 N15 55.6(4) . . . . ? N23 Ti2 N17 C25 69.4(3) . . . . ? N13 Ti2 N17 C25 -128.3(3) . . . . ? N19 Ti2 N17 C25 155.1(3) . . . . ? N15 Ti2 N17 C25 147.9(3) . . . . ? S3 Ti2 N17 C25 -34.7(4) . . . . ? S4 Ti2 N17 C25 -29.5(3) . . . . ? N23 Ti2 N17 N18 -129.8(2) . . . . ? N13 Ti2 N17 N18 32.5(2) . . . . ? N19 Ti2 N17 N18 -44.2(4) . . . . ? N15 Ti2 N17 N18 -51.4(2) . . . . ? S3 Ti2 N17 N18 126.0(2) . . . . ? S4 Ti2 N17 N18 131.3(2) . . . . ? C25 N17 N18 C27 0.6(4) . . . . ? Ti2 N17 N18 C27 -164.9(2) . . . . ? C25 N17 N18 B3 178.9(3) . . . . ? Ti2 N17 N18 B3 13.4(4) . . . . ? N16 B3 N18 C27 -129.7(4) . . . . ? N14 B3 N18 C27 113.1(4) . . . . ? N16 B3 N18 N17 52.3(4) . . . . ? N14 B3 N18 N17 -64.9(4) . . . . ? N23 Ti2 N19 C28 147.6(3) . . . . ? N13 Ti2 N19 C28 -15.6(3) . . . . ? N15 Ti2 N19 C28 66.9(3) . . . . ? N17 Ti2 N19 C28 59.7(4) . . . . ? S3 Ti2 N19 C28 -112.5(3) . . . . ? S4 Ti2 N19 C28 -114.6(3) . . . . ? N23 Ti2 N19 N20 -22.3(3) . . . . ? N13 Ti2 N19 N20 174.5(3) . . . . ? N15 Ti2 N19 N20 -103.0(3) . . . . ? N17 Ti2 N19 N20 -110.2(3) . . . . ? S3 Ti2 N19 N20 77.6(2) . . . . ? S4 Ti2 N19 N20 75.5(3) . . . . ? C28 N19 N20 C30 -0.3(4) . . . . ? Ti2 N19 N20 C30 171.4(2) . . . . ? C28 N19 N20 B4 175.1(3) . . . . ? Ti2 N19 N20 B4 -13.3(4) . . . . ? N21 B4 N20 C30 -12.6(5) . . . . ? N24 B4 N20 C30 -131.9(4) . . . . ? N21 B4 N20 N19 172.9(3) . . . . ? N24 B4 N20 N19 53.7(4) . . . . ? N24 B4 N21 C31 -138.1(4) . . . . ? N20 B4 N21 C31 103.6(4) . . . . ? N24 B4 N21 N22 54.9(5) . . . . ? N20 B4 N21 N22 -63.3(4) . . . . ? C31 N21 N22 C33 0.6(5) . . . . ? B4 N21 N22 C33 169.5(4) . . . . ? N13 Ti2 N23 C34 -75.3(5) . . . . ? N19 Ti2 N23 C34 -146.1(3) . . . . ? N15 Ti2 N23 C34 -69.9(3) . . . . ? N17 Ti2 N23 C34 6.7(3) . . . . ? S3 Ti2 N23 C34 136.4(3) . . . . ? S4 Ti2 N23 C34 84.2(3) . . . . ? N13 Ti2 N23 N24 96.8(4) . . . . ? N19 Ti2 N23 N24 26.0(3) . . . . ? N15 Ti2 N23 N24 102.3(3) . . . . ? N17 Ti2 N23 N24 178.9(3) . . . . ? S3 Ti2 N23 N24 -51.5(3) . . . . ? S4 Ti2 N23 N24 -103.6(3) . . . . ? C34 N23 N24 C36 -2.0(4) . . . . ? Ti2 N23 N24 C36 -175.4(2) . . . . ? C34 N23 N24 B4 179.7(3) . . . . ? Ti2 N23 N24 B4 6.3(4) . . . . ? N21 B4 N24 C36 14.2(5) . . . . ? N20 B4 N24 C36 132.0(4) . . . . ? N21 B4 N24 N23 -167.8(3) . . . . ? N20 B4 N24 N23 -49.9(4) . . . . ? N2 N1 C1 C2 0.3(4) . . . . ? Ti1 N1 C1 C2 -176.3(3) . . . . ? N1 C1 C2 C3 -0.2(5) . . . . ? N1 N2 C3 C2 0.2(5) . . . . ? B1 N2 C3 C2 -179.5(4) . . . . ? C1 C2 C3 N2 0.0(5) . . . . ? N4 N3 C4 C5 0.4(5) . . . . ? Ti1 N3 C4 C5 -173.0(3) . . . . ? N3 C4 C5 C6 -0.3(5) . . . . ? N3 N4 C6 C5 0.0(5) . . . . ? B1 N4 C6 C5 178.8(4) . . . . ? C4 C5 C6 N4 0.2(5) . . . . ? N6 N5 C7 C8 -0.3(4) . . . . ? Ti1 N5 C7 C8 167.0(3) . . . . ? N5 C7 C8 C9 -0.7(5) . . . . ? N5 N6 C9 C8 -1.7(5) . . . . ? B1 N6 C9 C8 179.6(4) . . . . ? C7 C8 C9 N6 1.4(5) . . . . ? N8 N7 C10 C11 -0.3(4) . . . . ? Ti1 N7 C10 C11 -169.7(3) . . . . ? N7 C10 C11 C12 0.6(4) . . . . ? N7 N8 C12 C11 0.6(4) . . . . ? B2 N8 C12 C11 -175.0(4) . . . . ? C10 C11 C12 N8 -0.7(5) . . . . ? N10 N9 C13 C14 -0.9(4) . . . . ? B2 N9 C13 C14 -171.7(3) . . . . ? N9 C13 C14 C15 0.3(4) . . . . ? N9 N10 C15 C14 -0.9(4) . . . . ? C13 C14 C15 N10 0.4(5) . . . . ? N12 N11 C16 C17 0.0(4) . . . . ? Ti1 N11 C16 C17 177.6(2) . . . . ? N11 C16 C17 C18 0.3(4) . . . . ? N11 N12 C18 C17 0.5(4) . . . . ? B2 N12 C18 C17 178.4(3) . . . . ? C16 C17 C18 N12 -0.5(4) . . . . ? N14 N13 C19 C20 0.3(4) . . . . ? Ti2 N13 C19 C20 176.8(3) . . . . ? N13 C19 C20 C21 -0.8(5) . . . . ? N13 N14 C21 C20 -0.8(5) . . . . ? B3 N14 C21 C20 174.8(4) . . . . ? C19 C20 C21 N14 0.9(5) . . . . ? N16 N15 C22 C23 0.3(4) . . . . ? Ti2 N15 C22 C23 178.6(3) . . . . ? N15 C22 C23 C24 -0.3(5) . . . . ? N15 N16 C24 C23 0.1(5) . . . . ? B3 N16 C24 C23 179.1(4) . . . . ? C22 C23 C24 N16 0.1(5) . . . . ? N18 N17 C25 C26 -0.6(4) . . . . ? Ti2 N17 C25 C26 162.0(3) . . . . ? N17 C25 C26 C27 0.3(5) . . . . ? N17 N18 C27 C26 -0.4(4) . . . . ? B3 N18 C27 C26 -178.6(4) . . . . ? C25 C26 C27 N18 0.0(5) . . . . ? N20 N19 C28 C29 0.1(4) . . . . ? Ti2 N19 C28 C29 -171.3(3) . . . . ? N19 C28 C29 C30 0.2(5) . . . . ? N19 N20 C30 C29 0.4(4) . . . . ? B4 N20 C30 C29 -174.8(3) . . . . ? C28 C29 C30 N20 -0.3(5) . . . . ? N22 N21 C31 C32 -0.1(5) . . . . ? B4 N21 C31 C32 -168.4(4) . . . . ? N21 C31 C32 C33 -0.4(5) . . . . ? N21 N22 C33 C32 -0.9(5) . . . . ? C31 C32 C33 N22 0.8(5) . . . . ? N24 N23 C34 C35 2.0(4) . . . . ? Ti2 N23 C34 C35 175.6(2) . . . . ? N23 C34 C35 C36 -1.2(4) . . . . ? N23 N24 C36 C35 1.3(4) . . . . ? B4 N24 C36 C35 179.5(3) . . . . ? C34 C35 C36 N24 -0.1(4) . . . . ? _refine_diff_density_max 0.451 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.066 #===END