# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'RSC Advances' _journal_coden_Cambridge 1500 _publ_contact_author_name 'Yahong Li' _publ_contact_author_address ; Suzhou 215006 ; _publ_contact_author_email liyahong@suda.edu.cn loop_ _publ_author_name 'Yanng Zhao.' 'Yahong Li.' data_2t _database_code_depnum_ccdc_archive 'CCDC 783591' #TrackingRef '- 2.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H30 Cl2 N6 Ti' _chemical_formula_sum 'C26 H30 Cl2 N6 Ti' _chemical_formula_weight 545.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' 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' _cell_length_a 11.829(2) _cell_length_b 12.517(3) _cell_length_c 18.391(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2723.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7721 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9003 _exptl_absorpt_correction_T_max 0.9239 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8641 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 25.30 _reflns_number_total 4561 _reflns_number_gt 4214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.5109P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack (1983), 1757 friedel pairs ' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 4561 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.08558(4) -0.00238(4) -0.05334(2) 0.03321(14) Uani 1 1 d . . . Cl2 Cl 0.17423(9) 0.57641(8) 0.33725(5) 0.0615(3) Uani 1 1 d . . . N2 N 0.0792(2) 0.09195(18) 0.04372(11) 0.0311(5) Uani 1 1 d . . . Cl1 Cl -0.05469(10) 0.55507(9) -0.13502(6) 0.0792(4) Uani 1 1 d . . . N1 N 0.0815(2) -0.11915(19) 0.04264(12) 0.0365(6) Uani 1 1 d . . . C7 C 0.0810(3) 0.1990(2) 0.06276(14) 0.0310(6) Uani 1 1 d . . . C6 C 0.1132(2) 0.0405(2) 0.10557(14) 0.0330(7) Uani 1 1 d . . . C8 C 0.1175(2) 0.2053(2) 0.13504(14) 0.0338(7) Uani 1 1 d . . . C15 C 0.1322(3) 0.2989(2) 0.18182(14) 0.0339(7) Uani 1 1 d . . . C20 C 0.2238(3) 0.3044(3) 0.22906(17) 0.0441(8) Uani 1 1 d . . . H20 H 0.2774 0.2490 0.2288 0.053 Uiso 1 1 calc R . . N6 N 0.0992(3) 0.1143(2) -0.11893(13) 0.0539(8) Uani 1 1 d . . . C4 C 0.1388(3) -0.1374(3) 0.16674(18) 0.0419(8) Uani 1 1 d . . . H4 H 0.1634 -0.1055 0.2102 0.050 Uiso 1 1 calc R . . C1 C 0.0711(3) -0.2256(3) 0.03915(18) 0.0438(8) Uani 1 1 d . . . H1 H 0.0477 -0.2565 -0.0049 0.053 Uiso 1 1 calc R . . N3 N 0.1387(2) 0.1039(2) 0.16123(12) 0.0349(6) Uani 1 1 d . . . C18 C 0.1584(3) 0.4708(3) 0.27668(15) 0.0424(8) Uani 1 1 d . . . C13 C 0.0819(3) 0.4591(2) -0.03821(16) 0.0445(8) Uani 1 1 d . . . H13 H 0.1285 0.5196 -0.0429 0.053 Uiso 1 1 calc R . . C5 C 0.1128(2) -0.0750(3) 0.10684(15) 0.0342(7) Uani 1 1 d . . . N5 N 0.2226(2) -0.0710(2) -0.08315(14) 0.0477(7) Uani 1 1 d . . . C14 C 0.1130(3) 0.3761(3) 0.00734(15) 0.0382(7) Uani 1 1 d . . . H14 H 0.1807 0.3809 0.0339 0.046 Uiso 1 1 calc R . . C9 C 0.0456(3) 0.2856(2) 0.01447(14) 0.0336(7) Uani 1 1 d . . . C10 C -0.0554(3) 0.2812(3) -0.02388(16) 0.0416(8) Uani 1 1 d . . . H10 H -0.1028 0.2214 -0.0191 0.050 Uiso 1 1 calc R . . C3 C 0.1282(3) -0.2469(3) 0.1618(2) 0.0491(9) Uani 1 1 d . . . H3 H 0.1446 -0.2906 0.2020 0.059 Uiso 1 1 calc R . . C17 C 0.0682(3) 0.4689(2) 0.23019(14) 0.0388(7) Uani 1 1 d . . . H17 H 0.0153 0.5250 0.2302 0.047 Uiso 1 1 calc R . . N4 N -0.0401(2) -0.0693(2) -0.09626(14) 0.0485(7) Uani 1 1 d . . . C16 C 0.0556(3) 0.3832(3) 0.18305(15) 0.0384(7) Uani 1 1 d . . . H16 H -0.0063 0.3821 0.1511 0.046 Uiso 1 1 calc R . . C19 C 0.2383(3) 0.3893(3) 0.27654(17) 0.0501(9) Uani 1 1 d . . . H19 H 0.3008 0.3916 0.3080 0.060 Uiso 1 1 calc R . . C11 C -0.0866(3) 0.3648(3) -0.06918(17) 0.0500(8) Uani 1 1 d . . . H11 H -0.1551 0.3616 -0.0950 0.060 Uiso 1 1 calc R . . C12 C -0.0175(3) 0.4522(3) -0.07636(16) 0.0488(9) Uani 1 1 d . . . C2 C 0.0932(3) -0.2913(3) 0.09697(18) 0.0496(8) Uani 1 1 d . . . H2 H 0.0846 -0.3656 0.0925 0.060 Uiso 1 1 calc R . . C26 C -0.0514(4) -0.1349(4) -0.1609(2) 0.0790(13) Uani 1 1 d . . . H26A H -0.0962 -0.0972 -0.1968 0.118 Uiso 1 1 calc R . . H26B H -0.0886 -0.2015 -0.1483 0.118 Uiso 1 1 calc R . . H26C H 0.0229 -0.1499 -0.1807 0.118 Uiso 1 1 calc R . . C24 C 0.2013(4) 0.1812(3) -0.1172(2) 0.0830(16) Uani 1 1 d . . . H24A H 0.1797 0.2557 -0.1127 0.125 Uiso 1 1 calc R . . H24B H 0.2437 0.1712 -0.1618 0.125 Uiso 1 1 calc R . . H24C H 0.2477 0.1610 -0.0760 0.125 Uiso 1 1 calc R . . C22 C 0.2653(4) -0.0646(4) -0.1580(2) 0.0746(12) Uani 1 1 d . . . H22A H 0.2840 -0.1358 -0.1751 0.112 Uiso 1 1 calc R . . H22B H 0.3324 -0.0201 -0.1592 0.112 Uiso 1 1 calc R . . H22C H 0.2077 -0.0338 -0.1891 0.112 Uiso 1 1 calc R . . C25 C -0.1467(3) -0.0515(4) -0.0605(3) 0.0803(14) Uani 1 1 d . . . H25A H -0.1811 -0.1196 -0.0488 0.121 Uiso 1 1 calc R . . H25B H -0.1964 -0.0116 -0.0925 0.121 Uiso 1 1 calc R . . H25C H -0.1344 -0.0111 -0.0162 0.121 Uiso 1 1 calc R . . C23 C 0.0257(5) 0.1493(4) -0.17708(19) 0.0954(19) Uani 1 1 d . . . H23A H 0.0606 0.1334 -0.2236 0.143 Uiso 1 1 calc R . . H23B H 0.0134 0.2257 -0.1731 0.143 Uiso 1 1 calc R . . H23C H -0.0462 0.1124 -0.1736 0.143 Uiso 1 1 calc R . . C21 C 0.3058(3) -0.1250(4) -0.0384(2) 0.0729(13) Uani 1 1 d . . . H21A H 0.3780 -0.0890 -0.0429 0.109 Uiso 1 1 calc R . . H21B H 0.3134 -0.1985 -0.0544 0.109 Uiso 1 1 calc R . . H21C H 0.2815 -0.1237 0.0119 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0378(3) 0.0304(3) 0.0314(2) -0.0040(2) 0.0009(2) -0.0022(3) Cl2 0.0800(6) 0.0484(5) 0.0560(5) -0.0210(4) -0.0150(5) -0.0059(5) N2 0.0378(14) 0.0247(12) 0.0307(11) -0.0004(10) 0.0017(11) -0.0019(11) Cl1 0.0931(8) 0.0752(7) 0.0693(6) 0.0397(6) 0.0074(5) 0.0263(6) N1 0.0388(14) 0.0288(13) 0.0418(13) -0.0022(11) 0.0047(13) -0.0023(12) C7 0.0363(16) 0.0247(14) 0.0319(13) -0.0021(11) 0.0003(14) -0.0004(13) C6 0.0392(17) 0.0289(15) 0.0308(13) -0.0008(12) 0.0033(13) -0.0016(13) C8 0.0375(17) 0.0335(17) 0.0303(13) -0.0003(12) 0.0024(13) -0.0006(14) C15 0.0419(17) 0.0319(17) 0.0279(13) 0.0014(12) 0.0016(12) -0.0041(14) C20 0.0475(19) 0.0402(19) 0.0445(16) -0.0011(15) -0.0067(16) 0.0048(16) N6 0.087(2) 0.0404(16) 0.0345(12) -0.0057(12) 0.0066(15) -0.0022(17) C4 0.047(2) 0.0339(18) 0.0443(16) 0.0045(14) -0.0002(16) 0.0014(15) C1 0.0437(19) 0.0341(17) 0.0535(18) -0.0025(15) 0.0010(16) -0.0046(15) N3 0.0424(15) 0.0304(14) 0.0318(11) -0.0008(11) 0.0037(11) -0.0003(11) C18 0.057(2) 0.0353(19) 0.0352(14) -0.0046(14) -0.0021(15) -0.0097(16) C13 0.055(2) 0.0310(16) 0.0476(16) 0.0034(13) 0.0099(16) 0.0009(16) C5 0.0347(17) 0.0305(16) 0.0374(14) -0.0001(13) 0.0061(13) 0.0006(14) N5 0.0434(15) 0.0532(18) 0.0464(14) -0.0094(14) 0.0083(13) -0.0008(14) C14 0.0439(18) 0.0329(17) 0.0376(14) 0.0029(13) -0.0002(14) -0.0019(14) C9 0.0410(18) 0.0314(16) 0.0284(13) -0.0002(12) 0.0031(13) 0.0008(14) C10 0.0406(19) 0.0382(18) 0.0460(16) 0.0021(14) -0.0032(14) -0.0027(15) C3 0.056(2) 0.0355(19) 0.0557(19) 0.0104(16) 0.0008(18) 0.0053(16) C17 0.0428(17) 0.0358(17) 0.0377(14) -0.0053(13) 0.0010(14) -0.0003(14) N4 0.0469(16) 0.0468(17) 0.0519(15) -0.0130(13) -0.0095(13) -0.0007(14) C16 0.0397(18) 0.0372(17) 0.0384(15) -0.0063(13) -0.0029(13) -0.0010(15) C19 0.053(2) 0.052(2) 0.0459(17) -0.0087(17) -0.0151(17) -0.0033(18) C11 0.049(2) 0.053(2) 0.0480(17) 0.0043(16) -0.0084(17) 0.0101(18) C12 0.061(2) 0.048(2) 0.0375(16) 0.0113(15) 0.0065(16) 0.0159(18) C2 0.050(2) 0.0317(17) 0.067(2) 0.0050(16) 0.0043(19) -0.0006(17) C26 0.084(3) 0.068(3) 0.085(3) -0.031(2) -0.032(3) 0.002(2) C24 0.124(4) 0.048(2) 0.077(3) -0.007(2) 0.055(3) -0.032(3) C22 0.088(3) 0.075(3) 0.061(2) -0.019(2) 0.034(2) -0.001(3) C25 0.045(2) 0.085(3) 0.111(3) -0.033(3) -0.007(2) 0.002(2) C23 0.186(6) 0.059(3) 0.041(2) -0.0017(19) -0.020(3) 0.029(3) C21 0.045(2) 0.100(4) 0.074(2) -0.005(3) 0.002(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N4 1.880(3) . ? Ti1 N6 1.902(3) . ? Ti1 N5 1.914(3) . ? Ti1 N2 2.142(2) . ? Ti1 N1 2.292(2) . ? Cl2 C18 1.738(3) . ? N2 C6 1.368(3) . ? N2 C7 1.385(3) . ? Cl1 C12 1.737(3) . ? N1 C1 1.339(4) . ? N1 C5 1.355(4) . ? C7 C8 1.400(4) . ? C7 C9 1.463(4) . ? C6 N3 1.330(4) . ? C6 C5 1.446(4) . ? C8 N3 1.380(4) . ? C8 C15 1.464(4) . ? C15 C20 1.390(4) . ? C15 C16 1.391(4) . ? C20 C19 1.385(5) . ? N6 C23 1.446(5) . ? N6 C24 1.470(5) . ? C4 C3 1.379(5) . ? C4 C5 1.385(4) . ? C1 C2 1.369(5) . ? C18 C17 1.368(4) . ? C18 C19 1.391(5) . ? C13 C12 1.372(5) . ? C13 C14 1.385(4) . ? N5 C21 1.450(5) . ? N5 C22 1.469(4) . ? C14 C9 1.390(4) . ? C9 C10 1.388(4) . ? C10 C11 1.387(4) . ? C3 C2 1.379(5) . ? C17 C16 1.387(4) . ? N4 C25 1.439(5) . ? N4 C26 1.451(5) . ? C11 C12 1.372(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 N4 Ti1 N6 98.21(13) . . ? N4 Ti1 N5 110.46(12) . . ? N6 Ti1 N5 95.24(13) . . ? N4 Ti1 N2 124.57(11) . . ? N6 Ti1 N2 96.20(10) . . ? N5 Ti1 N2 121.06(11) . . ? N4 Ti1 N1 91.29(11) . . ? N6 Ti1 N1 168.59(10) . . ? N5 Ti1 N1 87.28(11) . . ? N2 Ti1 N1 73.08(8) . . ? C6 N2 C7 103.9(2) . . ? C6 N2 Ti1 115.02(18) . . ? C7 N2 Ti1 138.04(18) . . ? C1 N1 C5 118.2(3) . . ? C1 N1 Ti1 126.8(2) . . ? C5 N1 Ti1 113.90(19) . . ? N2 C7 C8 107.4(2) . . ? N2 C7 C9 124.0(2) . . ? C8 C7 C9 128.5(2) . . ? N3 C6 N2 115.2(3) . . ? N3 C6 C5 125.8(3) . . ? N2 C6 C5 118.9(3) . . ? N3 C8 C7 109.6(2) . . ? N3 C8 C15 120.6(2) . . ? C7 C8 C15 129.8(3) . . ? C20 C15 C16 117.3(3) . . ? C20 C15 C8 120.0(3) . . ? C16 C15 C8 122.7(3) . . ? C19 C20 C15 121.9(3) . . ? C23 N6 C24 109.7(4) . . ? C23 N6 Ti1 130.6(3) . . ? C24 N6 Ti1 119.6(3) . . ? C3 C4 C5 119.2(3) . . ? N1 C1 C2 122.9(3) . . ? C6 N3 C8 103.8(2) . . ? C17 C18 C19 121.0(3) . . ? C17 C18 Cl2 119.9(2) . . ? C19 C18 Cl2 119.1(2) . . ? C12 C13 C14 119.2(3) . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C6 113.2(3) . . ? C4 C5 C6 125.2(3) . . ? C21 N5 C22 108.9(3) . . ? C21 N5 Ti1 128.4(2) . . ? C22 N5 Ti1 122.4(3) . . ? C13 C14 C9 121.1(3) . . ? C14 C9 C10 118.5(3) . . ? C14 C9 C7 119.8(3) . . ? C10 C9 C7 121.7(3) . . ? C11 C10 C9 120.3(3) . . ? C4 C3 C2 119.0(3) . . ? C18 C17 C16 119.2(3) . . ? C25 N4 C26 112.4(3) . . ? C25 N4 Ti1 115.6(2) . . ? C26 N4 Ti1 132.0(3) . . ? C17 C16 C15 121.8(3) . . ? C20 C19 C18 118.7(3) . . ? C12 C11 C10 120.0(3) . . ? C11 C12 C13 120.8(3) . . ? C11 C12 Cl1 120.0(3) . . ? C13 C12 Cl1 119.2(3) . . ? C1 C2 C3 119.1(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.222 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.043 # Attachment '- 6thf.txt' data_t _database_code_depnum_ccdc_archive 'CCDC 804537' #TrackingRef '- 6thf.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H36 Cl4 N8 Ti' _chemical_formula_sum 'C44 H36 Cl4 N8 Ti' _chemical_formula_weight 866.51 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9628(18) _cell_length_b 13.517(3) _cell_length_c 19.262(4) _cell_angle_alpha 73.96(3) _cell_angle_beta 87.86(3) _cell_angle_gamma 74.76(3) _cell_volume 2162.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9075 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8293 _exptl_absorpt_correction_T_max 0.9090 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17888 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.1071 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7536 _reflns_number_gt 4809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+1.3678P] 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 7536 _refine_ls_number_parameters 518 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1400 _refine_ls_R_factor_gt 0.0879 _refine_ls_wR_factor_ref 0.1971 _refine_ls_wR_factor_gt 0.1709 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.6204(2) -0.47350(14) 0.05447(9) 0.0718(5) Uani 1 1 d . . . N1 N 0.8957(5) -0.0188(3) 0.1865(2) 0.0399(11) Uani 1 1 d . . . C1 C 0.8916(6) 0.1270(4) 0.0778(3) 0.0410(13) Uani 1 1 d . . . Ti2 Ti 0.97613(11) 0.07559(8) 0.24070(5) 0.0371(3) Uani 1 1 d . . . Cl2 Cl 0.8296(3) -0.38528(16) 0.50173(9) 0.0910(7) Uani 1 1 d . . . N2 N 0.8435(5) -0.0444(3) 0.0789(2) 0.0411(11) Uani 1 1 d . . . C2 C 0.8617(7) 0.1745(5) 0.0048(3) 0.0526(16) Uani 1 1 d . . . H2 H 0.8315 0.1372 -0.0244 0.063 Uiso 1 1 calc R . . Cl3 Cl 1.4527(2) 0.66974(14) 0.28826(11) 0.0740(5) Uani 1 1 d . . . N3 N 0.9360(5) 0.1770(3) 0.1217(2) 0.0378(10) Uani 1 1 d . . . C3 C 0.8758(7) 0.2760(5) -0.0254(3) 0.0577(16) Uani 1 1 d . . . H3 H 0.8553 0.3091 -0.0751 0.069 Uiso 1 1 calc R . . Cl4 Cl 0.6440(2) 0.38806(16) 0.48639(9) 0.0750(5) Uani 1 1 d . . . N4 N 1.1167(5) 0.1802(3) 0.2464(2) 0.0379(10) Uani 1 1 d . . . C4 C 0.9210(7) 0.3290(5) 0.0191(3) 0.0533(16) Uani 1 1 d . . . H4 H 0.9317 0.3987 0.0002 0.064 Uiso 1 1 calc R . . N5 N 1.3095(5) 0.2560(4) 0.1962(2) 0.0432(11) Uani 1 1 d . . . C5 C 0.9496(7) 0.2776(4) 0.0910(3) 0.0485(14) Uani 1 1 d . . . H5 H 0.9802 0.3138 0.1209 0.058 Uiso 1 1 calc R . . N6 N 1.2021(5) 0.0207(3) 0.1836(2) 0.0410(11) Uani 1 1 d . . . C6 C 0.8766(6) 0.0206(4) 0.1129(3) 0.0354(12) Uani 1 1 d . . . N7 N 1.0455(5) -0.0258(3) 0.3312(2) 0.0436(11) Uani 1 1 d . . . C7 C 0.8395(6) -0.1333(4) 0.1337(3) 0.0405(13) Uani 1 1 d . . . N8 N 0.7811(5) 0.1576(4) 0.2578(2) 0.0418(11) Uani 1 1 d . . . C8 C 0.8702(6) -0.1197(4) 0.2000(3) 0.0403(13) Uani 1 1 d . . . C9 C 0.7941(6) -0.2223(4) 0.1168(3) 0.0417(13) Uani 1 1 d . . . C10 C 0.7430(7) -0.2076(5) 0.0467(3) 0.0497(15) Uani 1 1 d . . . H10 H 0.7424 -0.1435 0.0115 0.060 Uiso 1 1 calc R . . C11 C 0.6923(7) -0.2862(5) 0.0270(3) 0.0554(16) Uani 1 1 d . . . H11 H 0.6588 -0.2751 -0.0209 0.066 Uiso 1 1 calc R . . C12 C 0.6921(7) -0.3787(5) 0.0781(3) 0.0519(15) Uani 1 1 d . . . C13 C 0.7434(8) -0.3962(5) 0.1481(3) 0.0609(18) Uani 1 1 d . . . H13 H 0.7427 -0.4602 0.1832 0.073 Uiso 1 1 calc R . . C14 C 0.7956(7) -0.3195(5) 0.1665(3) 0.0574(17) Uani 1 1 d . . . H14 H 0.8335 -0.3331 0.2140 0.069 Uiso 1 1 calc R . . C15 C 0.8630(6) -0.1868(4) 0.2742(3) 0.0391(13) Uani 1 1 d . . . C16 C 0.7210(7) -0.1827(5) 0.3063(3) 0.0506(15) Uani 1 1 d . . . H16 H 0.6309 -0.1371 0.2802 0.061 Uiso 1 1 calc R . . C17 C 0.7088(8) -0.2444(5) 0.3761(3) 0.0573(17) Uani 1 1 d . . . H17 H 0.6120 -0.2403 0.3974 0.069 Uiso 1 1 calc R . . C18 C 0.8420(9) -0.3116(5) 0.4134(3) 0.0560(17) Uani 1 1 d . . . C19 C 0.9836(8) -0.3197(5) 0.3830(3) 0.0590(17) Uani 1 1 d . . . H19 H 1.0731 -0.3666 0.4090 0.071 Uiso 1 1 calc R . . C20 C 0.9927(7) -0.2579(4) 0.3136(3) 0.0490(14) Uani 1 1 d . . . H20 H 1.0896 -0.2642 0.2923 0.059 Uiso 1 1 calc R . . C21 C 1.2930(6) 0.0895(4) 0.1704(3) 0.0416(13) Uani 1 1 d . . . C22 C 1.4255(6) 0.0753(4) 0.1315(3) 0.0419(13) Uani 1 1 d . . . H22 H 1.4874 0.1234 0.1242 0.050 Uiso 1 1 calc R . . C23 C 1.4642(7) -0.0106(5) 0.1040(3) 0.0517(15) Uani 1 1 d . . . H23 H 1.5525 -0.0208 0.0761 0.062 Uiso 1 1 calc R . . C24 C 1.3746(7) -0.0831(5) 0.1166(3) 0.0478(14) Uani 1 1 d . . . H24 H 1.4015 -0.1430 0.0985 0.057 Uiso 1 1 calc R . . C25 C 1.2447(7) -0.0638(5) 0.1566(3) 0.0485(14) Uani 1 1 d . . . H25 H 1.1830 -0.1122 0.1655 0.058 Uiso 1 1 calc R . . C26 C 1.2407(6) 0.1763(4) 0.2030(3) 0.0404(13) Uani 1 1 d . . . C27 C 1.2271(6) 0.3130(4) 0.2399(3) 0.0394(13) Uani 1 1 d . . . C28 C 1.1094(6) 0.2687(4) 0.2712(3) 0.0396(13) Uani 1 1 d . . . C29 C 1.2780(6) 0.4035(4) 0.2514(3) 0.0407(13) Uani 1 1 d . . . C30 C 1.3175(7) 0.4778(4) 0.1938(3) 0.0521(15) Uani 1 1 d . . . H30 H 1.3081 0.4725 0.1466 0.062 Uiso 1 1 calc R . . C31 C 1.3707(7) 0.5598(5) 0.2046(3) 0.0544(15) Uani 1 1 d U . . H31 H 1.3973 0.6098 0.1649 0.065 Uiso 1 1 calc R . . C32 C 1.3845(6) 0.5679(5) 0.2731(3) 0.0495(14) Uani 1 1 d U . . C33 C 1.3461(7) 0.4952(5) 0.3310(3) 0.0567(16) Uani 1 1 d . . . H33 H 1.3563 0.5008 0.3781 0.068 Uiso 1 1 calc R . . C34 C 1.2926(7) 0.4141(5) 0.3204(3) 0.0519(16) Uani 1 1 d . . . H34 H 1.2655 0.3648 0.3604 0.062 Uiso 1 1 calc R . . C35 C 0.9955(6) 0.2999(4) 0.3238(3) 0.0397(13) Uani 1 1 d . . . C36 C 0.9268(7) 0.4058(5) 0.3204(3) 0.0485(15) Uani 1 1 d . . . H36 H 0.9534 0.4597 0.2835 0.058 Uiso 1 1 calc R . . C37 C 0.8202(7) 0.4342(5) 0.3697(3) 0.0557(16) Uani 1 1 d . . . H37 H 0.7764 0.5064 0.3671 0.067 Uiso 1 1 calc R . . C38 C 0.7782(7) 0.3546(6) 0.4234(3) 0.0555(16) Uani 1 1 d . . . C39 C 0.8486(7) 0.2476(5) 0.4291(3) 0.0543(16) Uani 1 1 d . . . H39 H 0.8238 0.1936 0.4665 0.065 Uiso 1 1 calc R . . C40 C 0.9551(7) 0.2222(5) 0.3792(3) 0.0477(14) Uani 1 1 d . . . H40 H 1.0019 0.1499 0.3827 0.057 Uiso 1 1 calc R . . C41 C 0.9591(8) -0.0427(5) 0.3982(3) 0.0591(17) Uani 1 1 d . . . H41A H 0.9485 -0.1152 0.4125 0.089 Uiso 1 1 calc R . . H41B H 0.8572 0.0071 0.3900 0.089 Uiso 1 1 calc R . . H41C H 1.0146 -0.0313 0.4363 0.089 Uiso 1 1 calc R . . C42 C 1.2051(8) -0.0939(6) 0.3483(4) 0.072(2) Uani 1 1 d . . . H42A H 1.2557 -0.0695 0.3816 0.108 Uiso 1 1 calc R . . H42B H 1.2620 -0.0897 0.3042 0.108 Uiso 1 1 calc R . . H42C H 1.2027 -0.1672 0.3703 0.108 Uiso 1 1 calc R . . C43 C 0.6606(7) 0.1027(6) 0.2872(4) 0.0664(18) Uani 1 1 d . . . H43A H 0.6209 0.1227 0.3303 0.100 Uiso 1 1 calc R . . H43B H 0.7048 0.0261 0.2992 0.100 Uiso 1 1 calc R . . H43C H 0.5769 0.1232 0.2513 0.100 Uiso 1 1 calc R . . C44 C 0.7132(7) 0.2735(5) 0.2330(3) 0.0609(17) Uani 1 1 d . . . H44A H 0.6356 0.2895 0.1949 0.091 Uiso 1 1 calc R . . H44B H 0.7937 0.3087 0.2147 0.091 Uiso 1 1 calc R . . H44C H 0.6653 0.2987 0.2731 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0887(14) 0.0617(11) 0.0849(12) -0.0396(9) -0.0044(10) -0.0321(10) N1 0.043(3) 0.045(3) 0.038(2) -0.021(2) 0.008(2) -0.016(2) C1 0.040(3) 0.044(3) 0.036(3) -0.010(3) 0.002(2) -0.007(3) Ti2 0.0357(6) 0.0400(6) 0.0409(5) -0.0172(4) 0.0026(4) -0.0125(5) Cl2 0.141(2) 0.0857(14) 0.0497(10) -0.0086(9) 0.0194(11) -0.0477(14) N2 0.039(3) 0.047(3) 0.042(3) -0.018(2) 0.000(2) -0.013(2) C2 0.061(4) 0.065(4) 0.041(3) -0.020(3) 0.008(3) -0.026(3) Cl3 0.0684(12) 0.0603(11) 0.1141(14) -0.0437(10) 0.0054(10) -0.0316(9) N3 0.037(3) 0.036(3) 0.044(2) -0.017(2) 0.000(2) -0.011(2) C3 0.067(5) 0.055(4) 0.046(3) -0.013(3) 0.002(3) -0.010(3) Cl4 0.0594(11) 0.0989(14) 0.0732(11) -0.0474(11) 0.0163(9) -0.0087(10) N4 0.036(3) 0.039(3) 0.044(2) -0.018(2) 0.001(2) -0.010(2) C4 0.052(4) 0.046(4) 0.055(4) -0.005(3) 0.006(3) -0.012(3) N5 0.036(3) 0.047(3) 0.052(3) -0.019(2) -0.002(2) -0.014(2) C5 0.046(4) 0.044(3) 0.059(4) -0.019(3) 0.003(3) -0.013(3) N6 0.041(3) 0.043(3) 0.044(3) -0.020(2) 0.001(2) -0.010(2) C6 0.026(3) 0.043(3) 0.041(3) -0.018(3) 0.003(2) -0.010(2) N7 0.049(3) 0.041(3) 0.041(3) -0.010(2) -0.003(2) -0.014(2) C7 0.041(3) 0.040(3) 0.045(3) -0.017(3) -0.002(3) -0.014(3) N8 0.034(3) 0.047(3) 0.047(3) -0.019(2) -0.002(2) -0.008(2) C8 0.036(3) 0.046(3) 0.045(3) -0.018(3) -0.002(2) -0.015(3) C9 0.039(3) 0.049(3) 0.041(3) -0.019(3) 0.002(2) -0.009(3) C10 0.060(4) 0.041(3) 0.050(3) -0.018(3) 0.001(3) -0.011(3) C11 0.064(4) 0.059(4) 0.047(3) -0.027(3) -0.009(3) -0.007(3) C12 0.059(4) 0.046(4) 0.055(4) -0.021(3) -0.007(3) -0.012(3) C13 0.083(5) 0.053(4) 0.053(4) -0.009(3) 0.000(3) -0.035(4) C14 0.072(5) 0.050(4) 0.047(3) -0.001(3) -0.015(3) -0.022(3) C15 0.045(3) 0.044(3) 0.039(3) -0.018(3) 0.007(3) -0.024(3) C16 0.047(4) 0.059(4) 0.055(4) -0.024(3) 0.006(3) -0.022(3) C17 0.063(5) 0.075(5) 0.051(4) -0.028(3) 0.014(3) -0.036(4) C18 0.088(5) 0.057(4) 0.035(3) -0.011(3) 0.004(3) -0.041(4) C19 0.069(5) 0.049(4) 0.054(4) -0.002(3) 0.001(3) -0.019(3) C20 0.041(4) 0.046(3) 0.056(4) -0.012(3) 0.007(3) -0.009(3) C21 0.034(3) 0.046(3) 0.047(3) -0.017(3) -0.004(2) -0.010(3) C22 0.035(3) 0.052(4) 0.045(3) -0.024(3) -0.001(2) -0.009(3) C23 0.043(4) 0.064(4) 0.049(3) -0.019(3) 0.009(3) -0.013(3) C24 0.042(4) 0.049(4) 0.052(3) -0.024(3) 0.000(3) 0.000(3) C25 0.044(4) 0.050(4) 0.057(4) -0.027(3) 0.002(3) -0.011(3) C26 0.031(3) 0.045(3) 0.054(3) -0.026(3) 0.006(3) -0.012(3) C27 0.038(3) 0.044(3) 0.044(3) -0.021(3) 0.002(2) -0.014(3) C28 0.042(3) 0.040(3) 0.046(3) -0.022(3) 0.003(3) -0.015(3) C29 0.037(3) 0.043(3) 0.045(3) -0.014(3) 0.001(2) -0.014(3) C30 0.061(4) 0.049(4) 0.050(3) -0.012(3) -0.004(3) -0.022(3) C31 0.054(4) 0.052(3) 0.061(3) -0.011(3) 0.001(3) -0.024(3) C32 0.033(3) 0.047(3) 0.075(4) -0.017(3) 0.004(3) -0.022(3) C33 0.053(4) 0.067(4) 0.066(4) -0.038(3) 0.007(3) -0.022(4) C34 0.068(4) 0.056(4) 0.044(3) -0.017(3) 0.008(3) -0.034(3) C35 0.040(3) 0.036(3) 0.048(3) -0.019(3) 0.002(3) -0.012(3) C36 0.054(4) 0.047(4) 0.046(3) -0.021(3) 0.004(3) -0.008(3) C37 0.055(4) 0.044(4) 0.068(4) -0.028(3) -0.007(3) 0.001(3) C38 0.049(4) 0.077(5) 0.048(4) -0.031(3) 0.005(3) -0.015(4) C39 0.053(4) 0.049(4) 0.060(4) -0.013(3) 0.003(3) -0.012(3) C40 0.047(4) 0.047(4) 0.055(3) -0.023(3) 0.005(3) -0.012(3) C41 0.075(5) 0.056(4) 0.049(4) -0.018(3) 0.002(3) -0.016(4) C42 0.060(5) 0.073(5) 0.069(4) -0.016(4) -0.012(3) 0.003(4) C43 0.050(4) 0.081(5) 0.078(4) -0.030(4) 0.016(3) -0.027(4) C44 0.052(4) 0.057(4) 0.070(4) -0.024(3) -0.004(3) 0.000(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 Cl1 C12 1.744(6) . ? N1 C6 1.370(6) . ? N1 C8 1.394(6) . ? N1 Ti2 2.124(4) . ? C1 N3 1.347(6) . ? C1 C2 1.379(7) . ? C1 C6 1.448(7) . ? Ti2 N8 1.880(5) . ? Ti2 N7 1.902(4) . ? Ti2 N4 2.152(4) . ? Ti2 N3 2.308(4) . ? Ti2 N6 2.314(5) . ? Cl2 C18 1.734(6) . ? N2 C6 1.326(6) . ? N2 C7 1.370(6) . ? C2 C3 1.373(8) . ? C2 H2 0.9400 . ? Cl3 C32 1.741(5) . ? N3 C5 1.360(6) . ? C3 C4 1.388(8) . ? C3 H3 0.9400 . ? Cl4 C38 1.741(6) . ? N4 C26 1.364(6) . ? N4 C28 1.392(6) . ? C4 C5 1.368(8) . ? C4 H4 0.9400 . ? N5 C26 1.350(6) . ? N5 C27 1.365(6) . ? C5 H5 0.9400 . ? N6 C25 1.343(7) . ? N6 C21 1.359(6) . ? N7 C41 1.475(7) . ? N7 C42 1.476(7) . ? C7 C8 1.387(7) . ? C7 C9 1.484(7) . ? N8 C44 1.469(7) . ? N8 C43 1.477(7) . ? C8 C15 1.476(7) . ? C9 C10 1.387(7) . ? C9 C14 1.393(7) . ? C10 C11 1.402(7) . ? C10 H10 0.9400 . ? C11 C12 1.362(8) . ? C11 H11 0.9400 . ? C12 C13 1.378(8) . ? C13 C14 1.374(8) . ? C13 H13 0.9400 . ? C14 H14 0.9400 . ? C15 C20 1.388(7) . ? C15 C16 1.388(7) . ? C16 C17 1.390(8) . ? C16 H16 0.9400 . ? C17 C18 1.379(9) . ? C17 H17 0.9400 . ? C18 C19 1.368(9) . ? C19 C20 1.380(8) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C22 1.378(7) . ? C21 C26 1.446(7) . ? C22 C23 1.366(7) . ? C22 H22 0.9400 . ? C23 C24 1.390(7) . ? C23 H23 0.9400 . ? C24 C25 1.380(7) . ? C24 H24 0.9400 . ? C25 H25 0.9400 . ? C27 C28 1.386(7) . ? C27 C29 1.484(7) . ? C28 C35 1.477(7) . ? C29 C30 1.380(7) . ? C29 C34 1.390(7) . ? C30 C31 1.383(7) . ? C30 H30 0.9400 . ? C31 C32 1.368(8) . ? C31 H31 0.9400 . ? C32 C33 1.368(8) . ? C33 C34 1.372(7) . ? C33 H33 0.9400 . ? C34 H34 0.9400 . ? C35 C36 1.386(7) . ? C35 C40 1.387(7) . ? C36 C37 1.380(8) . ? C36 H36 0.9400 . ? C37 C38 1.392(8) . ? C37 H37 0.9400 . ? C38 C39 1.392(8) . ? C39 C40 1.377(8) . ? C39 H39 0.9400 . ? C40 H40 0.9400 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? 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 C6 N1 C8 103.4(4) . . ? C6 N1 Ti2 115.9(3) . . ? C8 N1 Ti2 140.1(3) . . ? N3 C1 C2 122.0(5) . . ? N3 C1 C6 115.2(4) . . ? C2 C1 C6 122.7(5) . . ? N8 Ti2 N7 104.9(2) . . ? N8 Ti2 N1 97.18(18) . . ? N7 Ti2 N1 100.82(18) . . ? N8 Ti2 N4 100.11(18) . . ? N7 Ti2 N4 96.49(17) . . ? N1 Ti2 N4 151.44(16) . . ? N8 Ti2 N3 87.00(17) . . ? N7 Ti2 N3 167.93(18) . . ? N1 Ti2 N3 75.20(15) . . ? N4 Ti2 N3 83.16(15) . . ? N8 Ti2 N6 160.54(17) . . ? N7 Ti2 N6 94.23(18) . . ? N1 Ti2 N6 82.41(16) . . ? N4 Ti2 N6 73.77(16) . . ? N3 Ti2 N6 74.04(15) . . ? C6 N2 C7 103.6(4) . . ? C3 C2 C1 120.2(6) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C1 N3 C5 117.1(5) . . ? C1 N3 Ti2 113.3(3) . . ? C5 N3 Ti2 129.7(4) . . ? C2 C3 C4 118.6(6) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C26 N4 C28 103.5(4) . . ? C26 N4 Ti2 115.6(3) . . ? C28 N4 Ti2 139.6(4) . . ? C5 C4 C3 118.5(6) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C26 N5 C27 103.3(4) . . ? N3 C5 C4 123.6(5) . . ? N3 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C25 N6 C21 117.5(5) . . ? C25 N6 Ti2 127.9(4) . . ? C21 N6 Ti2 114.3(3) . . ? N2 C6 N1 115.3(4) . . ? N2 C6 C1 124.8(5) . . ? N1 C6 C1 119.9(4) . . ? C41 N7 C42 107.7(5) . . ? C41 N7 Ti2 127.4(4) . . ? C42 N7 Ti2 124.6(4) . . ? N2 C7 C8 110.6(4) . . ? N2 C7 C9 119.4(4) . . ? C8 C7 C9 129.8(5) . . ? C44 N8 C43 110.2(5) . . ? C44 N8 Ti2 129.8(4) . . ? C43 N8 Ti2 118.7(4) . . ? C7 C8 N1 107.1(4) . . ? C7 C8 C15 130.8(5) . . ? N1 C8 C15 121.8(4) . . ? C10 C9 C14 116.9(5) . . ? C10 C9 C7 118.0(5) . . ? C14 C9 C7 125.0(5) . . ? C9 C10 C11 121.6(5) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C12 C11 C10 119.2(5) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 120.7(5) . . ? C11 C12 Cl1 119.0(4) . . ? C13 C12 Cl1 120.3(5) . . ? C14 C13 C12 119.6(5) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C9 122.0(5) . . ? C13 C14 H14 119.0 . . ? C9 C14 H14 119.0 . . ? C20 C15 C16 117.5(5) . . ? C20 C15 C8 122.8(5) . . ? C16 C15 C8 119.7(5) . . ? C15 C16 C17 121.7(6) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C16 118.4(6) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C19 C18 C17 121.6(5) . . ? C19 C18 Cl2 119.4(5) . . ? C17 C18 Cl2 118.9(5) . . ? C18 C19 C20 118.9(6) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C19 C20 C15 121.9(6) . . ? C19 C20 H20 119.1 . . ? C15 C20 H20 119.1 . . ? N6 C21 C22 122.9(5) . . ? N6 C21 C26 113.7(5) . . ? C22 C21 C26 123.4(5) . . ? C23 C22 C21 118.1(5) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 120.7(5) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 117.6(5) . . ? C25 C24 H24 121.2 . . ? C23 C24 H24 121.2 . . ? N6 C25 C24 123.2(5) . . ? N6 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? N5 C26 N4 114.9(5) . . ? N5 C26 C21 124.7(5) . . ? N4 C26 C21 120.4(4) . . ? N5 C27 C28 110.6(4) . . ? N5 C27 C29 119.2(5) . . ? C28 C27 C29 130.1(5) . . ? C27 C28 N4 107.6(4) . . ? C27 C28 C35 130.1(5) . . ? N4 C28 C35 122.2(4) . . ? C30 C29 C34 118.0(5) . . ? C30 C29 C27 120.8(5) . . ? C34 C29 C27 121.2(5) . . ? C29 C30 C31 120.9(5) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 119.8(5) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.3(5) . . ? C33 C32 Cl3 119.0(5) . . ? C31 C32 Cl3 120.7(4) . . ? C32 C33 C34 120.0(5) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C29 121.0(5) . . ? C33 C34 H34 119.5 . . ? C29 C34 H34 119.5 . . ? C36 C35 C40 117.9(5) . . ? C36 C35 C28 122.0(5) . . ? C40 C35 C28 120.0(5) . . ? C37 C36 C35 121.6(6) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C38 119.3(6) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C37 C38 C39 120.2(6) . . ? C37 C38 Cl4 120.2(5) . . ? C39 C38 Cl4 119.5(5) . . ? C40 C39 C38 119.0(6) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C39 C40 C35 122.0(6) . . ? C39 C40 H40 119.0 . . ? C35 C40 H40 119.0 . . ? N7 C41 H41A 109.5 . . ? N7 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N7 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N7 C42 H42A 109.5 . . ? N7 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N7 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N8 C43 H43A 109.5 . . ? N8 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N8 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N8 C44 H44A 109.5 . . ? N8 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N8 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.269 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.065