# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Claire Carmalt' _publ_contact_author_email C.J.CARMALT@UCL.AC.UK _publ_section_title ; Syntheses, X-ray Structures and CVD of Titanium(IV) Arsine Complexes ; _publ_requested_category FM loop_ _publ_author_name 'Claire Carmalt' 'Ivan Parkin' 'David Pugh' 'Tegan Thomas' # Attachment 'Compound_1-CCDC762189.cif' data_str0711 _database_code_depnum_ccdc_archive 'CCDC 762189' #TrackingRef 'Compound_1-CCDC762189.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H15 As Cl4 Ti' _chemical_formula_sum 'C18 H15 As Cl4 Ti' _chemical_formula_weight 495.92 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5026(19) _cell_length_b 11.324(2) _cell_length_c 18.683(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.501(4) _cell_angle_gamma 90.00 _cell_volume 2008.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4235 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 28.03 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5104 _exptl_absorpt_correction_T_max 0.9500 _exptl_absorpt_process_details 'SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16527 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4787 _reflns_number_gt 4014 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _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^)+(0.0001P)^2^+21.3923P] 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 4787 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1380 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.182 _refine_ls_shift/su_max 0.012 _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 C1 C 0.1211(6) 0.7379(5) -0.0341(3) 0.0147(12) Uani 1 1 d . . . C2 C 0.1965(7) 0.6721(6) -0.0817(4) 0.0220(14) Uani 1 1 d . . . H2 H 0.2781 0.6300 -0.0653 0.026 Uiso 1 1 calc R . . C3 C 0.1527(8) 0.6679(7) -0.1536(4) 0.0304(17) Uani 1 1 d . . . H3 H 0.2046 0.6229 -0.1863 0.036 Uiso 1 1 calc R . . C4 C 0.0345(8) 0.7287(7) -0.1776(4) 0.0302(17) Uani 1 1 d . . . H4 H 0.0048 0.7256 -0.2268 0.036 Uiso 1 1 calc R . . C5 C -0.0413(8) 0.7946(6) -0.1299(4) 0.0260(15) Uani 1 1 d . . . H5 H -0.1225 0.8370 -0.1466 0.031 Uiso 1 1 calc R . . C6 C 0.0016(7) 0.7987(6) -0.0577(3) 0.0183(13) Uani 1 1 d . . . H6 H -0.0508 0.8430 -0.0249 0.022 Uiso 1 1 calc R . . C7 C 0.0096(7) 0.7714(6) 0.1144(3) 0.0178(13) Uani 1 1 d . . . C8 C -0.0360(8) 0.8817(6) 0.1310(4) 0.0245(15) Uani 1 1 d . . . H8 H 0.0185 0.9491 0.1199 0.029 Uiso 1 1 calc R . . C9 C -0.1656(9) 0.8952(8) 0.1651(4) 0.036(2) Uani 1 1 d . . . H9 H -0.1975 0.9719 0.1772 0.044 Uiso 1 1 calc R . . C10 C -0.2450(8) 0.7987(8) 0.1806(4) 0.0367(19) Uani 1 1 d . . . H10 H -0.3319 0.8078 0.2033 0.044 Uiso 1 1 calc R . . C11 C -0.1972(7) 0.6875(8) 0.1629(4) 0.0319(18) Uani 1 1 d . . . H11 H -0.2521 0.6203 0.1738 0.038 Uiso 1 1 calc R . . C12 C -0.0712(7) 0.6723(7) 0.1299(4) 0.0302(17) Uani 1 1 d . . . H12 H -0.0400 0.5954 0.1178 0.036 Uiso 1 1 calc R . . C13 C 0.2755(7) 0.8997(6) 0.0726(4) 0.0200(13) Uani 1 1 d . . . C14 C 0.2810(8) 0.9738(6) 0.0142(4) 0.0260(15) Uani 1 1 d . . . H14 H 0.2378 0.9503 -0.0304 0.031 Uiso 1 1 calc R . . C15 C 0.3486(8) 1.0821(6) 0.0197(4) 0.0300(17) Uani 1 1 d . . . H15 H 0.3488 1.1334 -0.0205 0.036 Uiso 1 1 calc R . . C16 C 0.4157(8) 1.1155(7) 0.0834(5) 0.0331(18) Uani 1 1 d . . . H16 H 0.4640 1.1889 0.0868 0.040 Uiso 1 1 calc R . . C17 C 0.4126(9) 1.0422(7) 0.1424(4) 0.0351(18) Uani 1 1 d . . . H17 H 0.4595 1.0661 0.1859 0.042 Uiso 1 1 calc R . . C18 C 0.3416(9) 0.9325(7) 0.1398(4) 0.0327(18) Uani 1 1 d . . . H18 H 0.3380 0.8830 0.1807 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.4839(2) 0.41986(16) 0.16714(10) 0.0330(4) Uani 1 1 d . . . Cl2 Cl 0.1917(2) 0.45314(16) 0.05936(11) 0.0333(4) Uani 1 1 d . . . Cl3 Cl 0.3001(2) 0.64588(17) 0.22071(9) 0.0316(4) Uani 1 1 d . . . Cl4 Cl 0.50560(18) 0.64315(16) 0.04985(10) 0.0265(4) Uani 1 1 d . . . Ti1 Ti 0.34842(12) 0.56248(10) 0.11709(6) 0.0168(2) Uani 1 1 d . . . As1 As 0.18449(7) 0.74643(6) 0.06614(3) 0.01533(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.015(3) 0.012(3) 0.018(3) 0.004(2) 0.001(2) -0.003(2) C2 0.019(3) 0.027(4) 0.020(3) 0.000(3) 0.004(3) 0.006(3) C3 0.035(4) 0.042(5) 0.014(3) -0.007(3) 0.002(3) 0.002(4) C4 0.041(4) 0.032(4) 0.018(3) -0.003(3) -0.001(3) -0.005(3) C5 0.027(4) 0.027(4) 0.024(4) 0.009(3) -0.005(3) -0.003(3) C6 0.016(3) 0.020(3) 0.018(3) -0.004(3) -0.004(2) 0.002(2) C7 0.021(3) 0.017(3) 0.016(3) 0.001(2) -0.001(2) 0.003(2) C8 0.028(4) 0.022(3) 0.024(4) -0.003(3) 0.005(3) 0.003(3) C9 0.042(5) 0.043(5) 0.025(4) -0.008(3) 0.003(3) 0.028(4) C10 0.019(4) 0.056(5) 0.035(4) 0.002(4) 0.002(3) 0.010(4) C11 0.016(3) 0.046(5) 0.034(4) -0.002(4) 0.005(3) -0.004(3) C12 0.020(4) 0.032(4) 0.038(4) -0.008(3) 0.000(3) 0.003(3) C13 0.022(3) 0.016(3) 0.022(3) 0.004(3) 0.000(3) 0.000(3) C14 0.029(4) 0.024(4) 0.025(4) 0.000(3) 0.000(3) -0.002(3) C15 0.038(4) 0.019(3) 0.033(4) -0.002(3) 0.001(3) -0.008(3) C16 0.029(4) 0.021(4) 0.049(5) -0.001(3) 0.000(4) -0.008(3) C17 0.043(5) 0.026(4) 0.035(4) -0.006(3) -0.009(4) -0.009(3) C18 0.054(5) 0.036(4) 0.008(3) 0.009(3) 0.000(3) 0.001(4) Cl1 0.0377(10) 0.0274(9) 0.0337(10) 0.0056(8) 0.0013(8) 0.0176(8) Cl2 0.0302(9) 0.0228(8) 0.0465(12) -0.0026(8) -0.0010(8) -0.0076(7) Cl3 0.0448(11) 0.0324(9) 0.0179(8) 0.0025(7) 0.0033(7) 0.0166(8) Cl4 0.0215(8) 0.0269(8) 0.0314(9) 0.0029(7) 0.0063(7) -0.0047(7) Ti1 0.0173(5) 0.0139(5) 0.0192(6) 0.0010(5) 0.0010(4) 0.0022(4) As1 0.0181(3) 0.0129(3) 0.0149(3) 0.0001(3) -0.0006(2) 0.0011(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 C1 C6 1.384(8) . ? C1 C2 1.384(9) . ? C1 As1 1.945(6) . ? C2 C3 1.389(9) . ? C2 H2 0.9500 . ? C3 C4 1.376(11) . ? C3 H3 0.9500 . ? C4 C5 1.387(10) . ? C4 H4 0.9500 . ? C5 C6 1.393(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.363(9) . ? C7 C12 1.397(10) . ? C7 As1 1.945(6) . ? C8 C9 1.419(10) . ? C8 H8 0.9500 . ? C9 C10 1.367(12) . ? C9 H9 0.9500 . ? C10 C11 1.383(11) . ? C10 H10 0.9500 . ? C11 C12 1.381(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.379(9) . ? C13 C18 1.427(9) . ? C13 As1 1.941(7) . ? C14 C15 1.386(10) . ? C14 H14 0.9500 . ? C15 C16 1.379(11) . ? C15 H15 0.9500 . ? C16 C17 1.381(11) . ? C16 H16 0.9500 . ? C17 C18 1.414(11) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? Cl1 Ti1 2.244(2) . ? Cl2 Ti1 2.185(2) . ? Cl3 Ti1 2.220(2) . ? Cl4 Ti1 2.193(2) . ? Ti1 As1 2.7465(13) . ? 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 C1 C2 120.2(6) . . ? C6 C1 As1 119.9(5) . . ? C2 C1 As1 119.9(5) . . ? C1 C2 C3 119.9(6) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 120.2(7) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.0(7) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.1(7) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 119.6(6) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C8 C7 C12 120.4(6) . . ? C8 C7 As1 121.7(5) . . ? C12 C7 As1 117.9(5) . . ? C7 C8 C9 119.4(7) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 120.5(7) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.2(7) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 121.4(8) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C7 119.2(7) . . ? C11 C12 H12 120.4 . . ? C7 C12 H12 120.4 . . ? C14 C13 C18 120.5(6) . . ? C14 C13 As1 121.7(5) . . ? C18 C13 As1 117.7(5) . . ? C13 C14 C15 120.8(7) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 120.2(7) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.9(7) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 121.9(7) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C13 116.7(7) . . ? C17 C18 H18 121.6 . . ? C13 C18 H18 121.6 . . ? Cl2 Ti1 Cl4 114.84(9) . . ? Cl2 Ti1 Cl3 120.60(9) . . ? Cl4 Ti1 Cl3 119.63(9) . . ? Cl2 Ti1 Cl1 99.45(9) . . ? Cl4 Ti1 Cl1 98.40(8) . . ? Cl3 Ti1 Cl1 94.56(8) . . ? Cl2 Ti1 As1 83.95(6) . . ? Cl4 Ti1 As1 82.86(6) . . ? Cl3 Ti1 As1 81.02(6) . . ? Cl1 Ti1 As1 175.41(8) . . ? C13 As1 C1 102.9(3) . . ? C13 As1 C7 103.2(3) . . ? C1 As1 C7 102.6(3) . . ? C13 As1 Ti1 114.34(19) . . ? C1 As1 Ti1 116.32(18) . . ? C7 As1 Ti1 115.63(19) . . ? 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 C6 C1 C2 C3 0.5(10) . . . . ? As1 C1 C2 C3 -178.8(6) . . . . ? C1 C2 C3 C4 -0.1(11) . . . . ? C2 C3 C4 C5 0.1(12) . . . . ? C3 C4 C5 C6 -0.4(11) . . . . ? C2 C1 C6 C5 -0.9(10) . . . . ? As1 C1 C6 C5 178.4(5) . . . . ? C4 C5 C6 C1 0.8(10) . . . . ? C12 C7 C8 C9 0.8(11) . . . . ? As1 C7 C8 C9 178.9(5) . . . . ? C7 C8 C9 C10 -0.6(11) . . . . ? C8 C9 C10 C11 0.2(12) . . . . ? C9 C10 C11 C12 -0.1(13) . . . . ? C10 C11 C12 C7 0.4(12) . . . . ? C8 C7 C12 C11 -0.7(11) . . . . ? As1 C7 C12 C11 -178.8(6) . . . . ? C18 C13 C14 C15 -1.0(11) . . . . ? As1 C13 C14 C15 -178.9(6) . . . . ? C13 C14 C15 C16 2.2(12) . . . . ? C14 C15 C16 C17 -1.6(12) . . . . ? C15 C16 C17 C18 -0.2(13) . . . . ? C16 C17 C18 C13 1.3(12) . . . . ? C14 C13 C18 C17 -0.7(11) . . . . ? As1 C13 C18 C17 177.3(6) . . . . ? C14 C13 As1 C1 1.1(6) . . . . ? C18 C13 As1 C1 -176.9(6) . . . . ? C14 C13 As1 C7 -105.4(6) . . . . ? C18 C13 As1 C7 76.6(6) . . . . ? C14 C13 As1 Ti1 128.1(5) . . . . ? C18 C13 As1 Ti1 -49.8(6) . . . . ? C6 C1 As1 C13 -77.8(5) . . . . ? C2 C1 As1 C13 101.5(5) . . . . ? C6 C1 As1 C7 29.2(5) . . . . ? C2 C1 As1 C7 -151.6(5) . . . . ? C6 C1 As1 Ti1 156.4(4) . . . . ? C2 C1 As1 Ti1 -24.3(6) . . . . ? C8 C7 As1 C13 12.4(6) . . . . ? C12 C7 As1 C13 -169.5(5) . . . . ? C8 C7 As1 C1 -94.3(6) . . . . ? C12 C7 As1 C1 83.8(6) . . . . ? C8 C7 As1 Ti1 138.0(5) . . . . ? C12 C7 As1 Ti1 -43.9(6) . . . . ? Cl2 Ti1 As1 C13 -164.6(2) . . . . ? Cl4 Ti1 As1 C13 -48.5(2) . . . . ? Cl3 Ti1 As1 C13 73.1(2) . . . . ? Cl2 Ti1 As1 C1 -44.8(2) . . . . ? Cl4 Ti1 As1 C1 71.2(2) . . . . ? Cl3 Ti1 As1 C1 -167.1(2) . . . . ? Cl2 Ti1 As1 C7 75.7(2) . . . . ? Cl4 Ti1 As1 C7 -168.2(2) . . . . ? Cl3 Ti1 As1 C7 -46.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.093 _refine_diff_density_min -1.321 _refine_diff_density_rms 0.174 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 762190' #TrackingRef 'Combined_CIF_-_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 As2 Cl4 Ti' _chemical_formula_sum 'C36 H30 As2 Cl4 Ti' _chemical_formula_weight 802.14 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.686(3) _cell_length_b 9.789(3) _cell_length_c 10.237(3) _cell_angle_alpha 108.824(5) _cell_angle_beta 111.489(5) _cell_angle_gamma 92.081(5) _cell_volume 841.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2262 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.67 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 402 _exptl_absorpt_coefficient_mu 2.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4672 _exptl_absorpt_correction_T_max 0.9528 _exptl_absorpt_process_details 'SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6969 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 28.40 _reflns_number_total 3757 _reflns_number_gt 2810 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _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. Further investigation into the disorder of the phenyl rings revealed that the disorder was indeed random and not indicative of a larger unit cell or a merohedral twin. ; _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^)+(0.0585P)^2^+0.6576P] 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 3757 _refine_ls_number_parameters 305 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.014 _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 Ti1 Ti 0.5000 1.0000 1.0000 0.0262(2) Uani 1 2 d S . . Cl1 Cl 0.33439(12) 1.14532(13) 0.92470(12) 0.0393(3) Uani 1 1 d . . . Cl2 Cl 0.39361(11) 0.97771(13) 1.15807(11) 0.0366(3) Uani 1 1 d . . . As1 As 0.29341(4) 0.76969(5) 0.77039(4) 0.02779(14) Uani 1 1 d D . . C1A C 0.1270(7) 0.7174(8) 0.8199(8) 0.0292(8) Uani 0.663(3) 1 d P A 1 C2A C 0.0500(8) 0.8282(9) 0.8642(9) 0.0451(19) Uani 0.663(3) 1 d P A 1 H2A H 0.0820 0.9254 0.8746 0.054 Uiso 0.663(3) 1 calc PR A 1 C3A C -0.0741(11) 0.7958(12) 0.8933(12) 0.056(3) Uani 0.663(3) 1 d P A 1 H3A H -0.1279 0.8709 0.9225 0.067 Uiso 0.663(3) 1 calc PR A 1 C4A C -0.1189(13) 0.6564(13) 0.8802(14) 0.052(3) Uani 0.663(3) 1 d P A 1 H4A H -0.2033 0.6352 0.9011 0.063 Uiso 0.663(3) 1 calc PR A 1 C5A C -0.0433(8) 0.5477(8) 0.8373(8) 0.0410(17) Uani 0.663(3) 1 d P A 1 H5A H -0.0750 0.4514 0.8297 0.049 Uiso 0.663(3) 1 calc PR A 1 C6A C 0.0797(7) 0.5756(8) 0.8045(7) 0.0351(9) Uani 0.663(3) 1 d P A 1 H6A H 0.1304 0.4988 0.7721 0.042 Uiso 0.663(3) 1 calc PR A 1 C7A C 0.1975(7) 0.7952(9) 0.5831(7) 0.0292(8) Uani 0.663(3) 1 d PD A 1 C8A C 0.0418(7) 0.7767(7) 0.5169(7) 0.0326(14) Uani 0.663(3) 1 d P A 1 H8A H -0.0175 0.7433 0.5603 0.039 Uiso 0.663(3) 1 calc PR A 1 C9A C -0.0267(8) 0.8069(8) 0.3880(7) 0.0405(17) Uani 0.663(3) 1 d P A 1 H9A H -0.1335 0.7919 0.3409 0.049 Uiso 0.663(3) 1 calc PR A 1 C10A C 0.0583(10) 0.8584(8) 0.3278(8) 0.0466(19) Uani 0.663(3) 1 d P A 1 H10A H 0.0111 0.8788 0.2385 0.056 Uiso 0.663(3) 1 calc PR A 1 C11A C 0.210(3) 0.8803(15) 0.396(2) 0.052(4) Uani 0.663(3) 1 d P A 1 H11A H 0.2682 0.9212 0.3558 0.062 Uiso 0.663(3) 1 calc PR A 1 C12A C 0.2863(9) 0.8452(11) 0.5235(8) 0.0421(18) Uani 0.663(3) 1 d P A 1 H12A H 0.3930 0.8553 0.5663 0.050 Uiso 0.663(3) 1 calc PR A 1 C13A C 0.3649(8) 0.5824(7) 0.7201(10) 0.0292(8) Uani 0.663(3) 1 d PD A 1 C14A C 0.3182(9) 0.4907(9) 0.5652(9) 0.050(2) Uani 0.663(3) 1 d P A 1 H14A H 0.2547 0.5219 0.4885 0.060 Uiso 0.663(3) 1 calc PR A 1 C15A C 0.3652(10) 0.3564(9) 0.5266(11) 0.057(2) Uani 0.663(3) 1 d P A 1 H15A H 0.3366 0.2976 0.4236 0.068 Uiso 0.663(3) 1 calc PR A 1 C16A C 0.4515(9) 0.3092(11) 0.6352(14) 0.054(3) Uani 0.663(3) 1 d P A 1 H16A H 0.4817 0.2164 0.6079 0.065 Uiso 0.663(3) 1 calc PR A 1 C17A C 0.4963(10) 0.3943(12) 0.7853(14) 0.062(3) Uani 0.663(3) 1 d P A 1 H17A H 0.5586 0.3615 0.8612 0.074 Uiso 0.663(3) 1 calc PR A 1 C18A C 0.4492(7) 0.5289(8) 0.8243(8) 0.0351(9) Uani 0.663(3) 1 d P A 1 H18A H 0.4772 0.5852 0.9278 0.042 Uiso 0.663(3) 1 calc PR A 1 C1B C 0.0927(13) 0.7619(15) 0.7783(15) 0.0292(8) Uani 0.337(3) 1 d P A 2 C2B C 0.0854(14) 0.7315(14) 0.8998(13) 0.028(3) Uani 0.337(3) 1 d P A 2 H2B H 0.1728 0.7198 0.9744 0.034 Uiso 0.337(3) 1 calc PR A 2 C3B C -0.0545(18) 0.719(2) 0.9077(16) 0.029(3) Uani 0.337(3) 1 d P A 2 H3B H -0.0623 0.6972 0.9889 0.034 Uiso 0.337(3) 1 calc PR A 2 C4B C -0.1821(17) 0.7372(16) 0.8014(18) 0.040(3) Uani 0.337(3) 1 d P A 2 H4B H -0.2764 0.7282 0.8096 0.048 Uiso 0.337(3) 1 calc PR A 2 C5B C -0.1713(14) 0.7685(15) 0.6832(15) 0.037(3) Uani 0.337(3) 1 d P A 2 H5B H -0.2585 0.7808 0.6089 0.044 Uiso 0.337(3) 1 calc PR A 2 C6B C -0.0336(13) 0.7821(15) 0.6727(15) 0.0351(9) Uani 0.337(3) 1 d P A 2 H6B H -0.0262 0.8054 0.5920 0.042 Uiso 0.337(3) 1 calc PR A 2 C7B C 0.2405(14) 0.7911(18) 0.5733(12) 0.0292(8) Uani 0.337(3) 1 d PD A 2 C8B C 0.1849(14) 0.6649(14) 0.4385(13) 0.031(3) Uani 0.337(3) 1 d P A 2 H8B H 0.1788 0.5706 0.4455 0.037 Uiso 0.337(3) 1 calc PR A 2 C9B C 0.1393(14) 0.6750(15) 0.2976(14) 0.036(3) Uani 0.337(3) 1 d P A 2 H9B H 0.1037 0.5879 0.2106 0.043 Uiso 0.337(3) 1 calc PR A 2 C10B C 0.1447(14) 0.8068(15) 0.2816(15) 0.033(3) Uani 0.337(3) 1 d P A 2 H10B H 0.1038 0.8117 0.1839 0.040 Uiso 0.337(3) 1 calc PR A 2 C11B C 0.207(6) 0.930(4) 0.403(5) 0.052(4) Uani 0.337(3) 1 d P A 2 H11B H 0.2249 1.0210 0.3916 0.062 Uiso 0.337(3) 1 calc PR A 2 C12B C 0.2468(16) 0.9224(16) 0.5482(15) 0.031(3) Uani 0.337(3) 1 d P A 2 H12B H 0.2791 1.0116 0.6327 0.037 Uiso 0.337(3) 1 calc PR A 2 C13B C 0.3295(16) 0.5722(11) 0.725(2) 0.0292(8) Uani 0.337(3) 1 d PD A 2 C14B C 0.2392(13) 0.4737(13) 0.7301(13) 0.028(3) Uani 0.337(3) 1 d P A 2 H14B H 0.1496 0.4940 0.7446 0.034 Uiso 0.337(3) 1 calc PR A 2 C15B C 0.2829(15) 0.3345(14) 0.7124(14) 0.035(3) Uani 0.337(3) 1 d P A 2 H15B H 0.2177 0.2547 0.7044 0.043 Uiso 0.337(3) 1 calc PR A 2 C16B C 0.422(2) 0.3163(19) 0.707(2) 0.041(4) Uani 0.337(3) 1 d P A 2 H16B H 0.4532 0.2240 0.6984 0.049 Uiso 0.337(3) 1 calc PR A 2 C17B C 0.5137(16) 0.4254(18) 0.7129(17) 0.040(3) Uani 0.337(3) 1 d P A 2 H17B H 0.6075 0.4097 0.7064 0.048 Uiso 0.337(3) 1 calc PR A 2 C18B C 0.4718(14) 0.5626(16) 0.7289(15) 0.0351(9) Uani 0.337(3) 1 d P A 2 H18B H 0.5376 0.6445 0.7415 0.042 Uiso 0.337(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0233(5) 0.0412(6) 0.0186(5) 0.0137(4) 0.0097(4) 0.0183(4) Cl1 0.0398(6) 0.0554(7) 0.0325(5) 0.0220(5) 0.0176(5) 0.0333(5) Cl2 0.0340(5) 0.0601(7) 0.0279(5) 0.0231(5) 0.0183(4) 0.0222(5) As1 0.0237(2) 0.0427(3) 0.0240(2) 0.01532(18) 0.01360(17) 0.01313(17) C1A 0.021(2) 0.0382(17) 0.0369(16) 0.0231(14) 0.0118(16) 0.0119(14) C2A 0.054(4) 0.051(5) 0.078(5) 0.050(4) 0.052(4) 0.039(4) C3A 0.063(6) 0.068(6) 0.098(8) 0.063(7) 0.067(6) 0.053(6) C4A 0.065(7) 0.064(7) 0.078(7) 0.051(6) 0.058(6) 0.038(5) C5A 0.050(4) 0.039(4) 0.052(4) 0.024(3) 0.033(4) 0.018(3) C6A 0.0293(19) 0.045(3) 0.040(2) 0.026(2) 0.0142(18) 0.0113(18) C7A 0.021(2) 0.0382(17) 0.0369(16) 0.0231(14) 0.0118(16) 0.0119(14) C8A 0.030(3) 0.041(4) 0.026(3) 0.012(3) 0.009(3) 0.014(3) C9A 0.039(4) 0.050(4) 0.029(3) 0.016(3) 0.007(3) 0.023(3) C10A 0.065(5) 0.036(4) 0.027(4) 0.016(3) 0.001(4) 0.016(4) C11A 0.062(4) 0.066(12) 0.035(4) 0.033(9) 0.016(3) -0.009(9) C12A 0.038(4) 0.062(6) 0.029(4) 0.021(4) 0.012(3) 0.003(4) C13A 0.021(2) 0.0382(17) 0.0369(16) 0.0231(14) 0.0118(16) 0.0119(14) C14A 0.073(5) 0.063(5) 0.054(5) 0.044(4) 0.045(4) 0.053(4) C15A 0.082(6) 0.051(5) 0.077(6) 0.036(5) 0.063(5) 0.039(4) C16A 0.042(4) 0.046(6) 0.102(8) 0.051(6) 0.037(5) 0.024(4) C17A 0.029(4) 0.054(6) 0.107(9) 0.062(7) 0.002(5) 0.009(4) C18A 0.0293(19) 0.045(3) 0.040(2) 0.026(2) 0.0142(18) 0.0113(18) C1B 0.021(2) 0.0382(17) 0.0369(16) 0.0231(14) 0.0118(16) 0.0119(14) C2B 0.036(6) 0.039(7) 0.020(6) 0.014(5) 0.019(5) 0.013(5) C3B 0.034(9) 0.039(11) 0.020(6) 0.016(7) 0.013(6) 0.020(7) C4B 0.032(7) 0.042(8) 0.052(9) 0.006(7) 0.033(7) 0.016(6) C5B 0.029(6) 0.040(8) 0.043(8) 0.016(6) 0.014(6) 0.018(6) C6B 0.0293(19) 0.045(3) 0.040(2) 0.026(2) 0.0142(18) 0.0113(18) C7B 0.021(2) 0.0382(17) 0.0369(16) 0.0231(14) 0.0118(16) 0.0119(14) C8B 0.038(7) 0.029(7) 0.025(6) 0.004(5) 0.019(5) -0.007(5) C9B 0.034(7) 0.039(8) 0.030(7) 0.005(6) 0.015(6) -0.007(6) C10B 0.028(6) 0.044(8) 0.030(7) 0.022(6) 0.008(6) -0.001(6) C11B 0.062(4) 0.066(12) 0.035(4) 0.033(9) 0.016(3) -0.009(9) C12B 0.039(7) 0.023(7) 0.022(6) 0.012(6) -0.001(6) -0.002(6) C13B 0.021(2) 0.0382(17) 0.0369(16) 0.0231(14) 0.0118(16) 0.0119(14) C14B 0.032(6) 0.031(7) 0.033(6) 0.023(5) 0.015(5) 0.011(5) C15B 0.042(7) 0.023(6) 0.038(7) 0.020(6) 0.004(6) 0.003(5) C16B 0.056(11) 0.028(8) 0.035(9) 0.012(7) 0.012(8) 0.021(8) C17B 0.032(7) 0.044(10) 0.030(7) 0.004(7) 0.005(6) 0.020(7) C18B 0.0293(19) 0.045(3) 0.040(2) 0.026(2) 0.0142(18) 0.0113(18) _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 Cl1 2.2713(11) 2_677 ? Ti1 Cl1 2.2713(11) . ? Ti1 Cl2 2.2719(11) . ? Ti1 Cl2 2.2719(11) 2_677 ? Ti1 As1 2.7238(7) . ? Ti1 As1 2.7238(7) 2_677 ? As1 C7A 1.903(6) . ? As1 C13B 1.914(9) . ? As1 C1A 1.955(6) . ? As1 C13A 1.963(6) . ? As1 C1B 1.975(12) . ? As1 C7B 1.975(9) . ? C1A C6A 1.386(9) . ? C1A C2A 1.388(9) . ? C2A C3A 1.389(10) . ? C2A H2A 0.9500 . ? C3A C4A 1.365(14) . ? C3A H3A 0.9500 . ? C4A C5A 1.361(12) . ? C4A H4A 0.9500 . ? C5A C6A 1.392(9) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7A C12A 1.378(10) . ? C7A C8A 1.385(8) . ? C8A C9A 1.376(8) . ? C8A H8A 0.9500 . ? C9A C10A 1.361(11) . ? C9A H9A 0.9500 . ? C10A C11A 1.35(2) . ? C10A H10A 0.9500 . ? C11A C12A 1.403(19) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A C18A 1.354(10) . ? C13A C14A 1.432(11) . ? C14A C15A 1.391(10) . ? C14A H14A 0.9500 . ? C15A C16A 1.352(12) . ? C15A H15A 0.9500 . ? C16A C17A 1.379(17) . ? C16A H16A 0.9500 . ? C17A C18A 1.394(12) . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C1B C6B 1.375(17) . ? C1B C2B 1.393(17) . ? C2B C3B 1.39(2) . ? C2B H2B 0.9500 . ? C3B C4B 1.38(2) . ? C3B H3B 0.9500 . ? C4B C5B 1.38(2) . ? C4B H4B 0.9500 . ? C5B C6B 1.381(17) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C7B C12B 1.39(2) . ? C7B C8B 1.424(19) . ? C8B C9B 1.383(17) . ? C8B H8B 0.9500 . ? C9B C10B 1.353(18) . ? C9B H9B 0.9500 . ? C10B C11B 1.34(5) . ? C10B H10B 0.9500 . ? C11B C12B 1.43(4) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B C14B 1.302(17) . ? C13B C18B 1.373(16) . ? C14B C15B 1.417(17) . ? C14B H14B 0.9500 . ? C15B C16B 1.39(2) . ? C15B H15B 0.9500 . ? C16B C17B 1.33(3) . ? C16B H16B 0.9500 . ? C17B C18B 1.39(2) . ? C17B H17B 0.9500 . ? C18B H18B 0.9500 . ? 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 Cl1 Ti1 Cl1 180.0 2_677 . ? Cl1 Ti1 Cl2 89.99(4) 2_677 . ? Cl1 Ti1 Cl2 90.01(4) . . ? Cl1 Ti1 Cl2 90.01(4) 2_677 2_677 ? Cl1 Ti1 Cl2 89.99(4) . 2_677 ? Cl2 Ti1 Cl2 180.0 . 2_677 ? Cl1 Ti1 As1 93.32(4) 2_677 . ? Cl1 Ti1 As1 86.68(4) . . ? Cl2 Ti1 As1 90.36(4) . . ? Cl2 Ti1 As1 89.64(4) 2_677 . ? Cl1 Ti1 As1 86.68(4) 2_677 2_677 ? Cl1 Ti1 As1 93.32(4) . 2_677 ? Cl2 Ti1 As1 89.64(4) . 2_677 ? Cl2 Ti1 As1 90.36(4) 2_677 2_677 ? As1 Ti1 As1 180.0 . 2_677 ? C7A As1 C13B 106.9(6) . . ? C7A As1 C1A 104.3(3) . . ? C13B As1 C1A 90.2(4) . . ? C7A As1 C13A 104.9(3) . . ? C1A As1 C13A 101.3(3) . . ? C7A As1 C1B 86.1(4) . . ? C13B As1 C1B 105.4(5) . . ? C13A As1 C1B 116.5(4) . . ? C13B As1 C7B 101.4(7) . . ? C1A As1 C7B 117.2(4) . . ? C13A As1 C7B 97.2(5) . . ? C1B As1 C7B 99.5(5) . . ? C7A As1 Ti1 116.8(2) . . ? C13B As1 Ti1 122.4(5) . . ? C1A As1 Ti1 111.9(2) . . ? C13A As1 Ti1 115.9(2) . . ? C1B As1 Ti1 112.9(4) . . ? C7B As1 Ti1 112.3(5) . . ? C6A C1A C2A 120.0(6) . . ? C6A C1A As1 122.9(5) . . ? C2A C1A As1 117.0(5) . . ? C1A C2A C3A 119.5(7) . . ? C1A C2A H2A 120.2 . . ? C3A C2A H2A 120.2 . . ? C4A C3A C2A 120.2(8) . . ? C4A C3A H3A 119.9 . . ? C2A C3A H3A 119.9 . . ? C5A C4A C3A 120.4(8) . . ? C5A C4A H4A 119.8 . . ? C3A C4A H4A 119.8 . . ? C4A C5A C6A 120.9(8) . . ? C4A C5A H5A 119.6 . . ? C6A C5A H5A 119.6 . . ? C1A C6A C5A 118.9(6) . . ? C1A C6A H6A 120.6 . . ? C5A C6A H6A 120.6 . . ? C12A C7A C8A 121.3(6) . . ? C12A C7A As1 118.5(5) . . ? C8A C7A As1 119.9(5) . . ? C9A C8A C7A 119.8(6) . . ? C9A C8A H8A 120.1 . . ? C7A C8A H8A 120.1 . . ? C10A C9A C8A 120.1(6) . . ? C10A C9A H9A 119.9 . . ? C8A C9A H9A 119.9 . . ? C11A C10A C9A 119.6(9) . . ? C11A C10A H10A 120.2 . . ? C9A C10A H10A 120.2 . . ? C10A C11A C12A 122.8(14) . . ? C10A C11A H11A 118.6 . . ? C12A C11A H11A 118.6 . . ? C7A C12A C11A 116.3(11) . . ? C7A C12A H12A 121.9 . . ? C11A C12A H12A 121.9 . . ? C18A C13A C14A 117.0(6) . . ? C18A C13A As1 123.6(6) . . ? C14A C13A As1 119.2(5) . . ? C15A C14A C13A 120.3(7) . . ? C15A C14A H14A 119.8 . . ? C13A C14A H14A 119.8 . . ? C16A C15A C14A 120.2(9) . . ? C16A C15A H15A 119.9 . . ? C14A C15A H15A 119.9 . . ? C15A C16A C17A 120.7(8) . . ? C15A C16A H16A 119.7 . . ? C17A C16A H16A 119.7 . . ? C16A C17A C18A 119.3(8) . . ? C16A C17A H17A 120.4 . . ? C18A C17A H17A 120.4 . . ? C13A C18A C17A 122.4(8) . . ? C13A C18A H18A 118.8 . . ? C17A C18A H18A 118.8 . . ? C6B C1B C2B 120.9(11) . . ? C6B C1B As1 124.1(10) . . ? C2B C1B As1 115.1(9) . . ? C3B C2B C1B 117.5(12) . . ? C3B C2B H2B 121.3 . . ? C1B C2B H2B 121.3 . . ? C4B C3B C2B 122.1(16) . . ? C4B C3B H3B 118.9 . . ? C2B C3B H3B 118.9 . . ? C3B C4B C5B 119.1(14) . . ? C3B C4B H4B 120.4 . . ? C5B C4B H4B 120.4 . . ? C4B C5B C6B 120.1(12) . . ? C4B C5B H5B 120.0 . . ? C6B C5B H5B 120.0 . . ? C1B C6B C5B 120.3(12) . . ? C1B C6B H6B 119.8 . . ? C5B C6B H6B 119.8 . . ? C12B C7B C8B 113.4(10) . . ? C12B C7B As1 126.4(11) . . ? C8B C7B As1 120.2(10) . . ? C9B C8B C7B 122.2(12) . . ? C9B C8B H8B 118.9 . . ? C7B C8B H8B 118.9 . . ? C10B C9B C8B 121.1(12) . . ? C10B C9B H9B 119.5 . . ? C8B C9B H9B 119.5 . . ? C11B C10B C9B 120.4(19) . . ? C11B C10B H10B 119.8 . . ? C9B C10B H10B 119.8 . . ? C10B C11B C12B 119(2) . . ? C10B C11B H11B 120.6 . . ? C12B C11B H11B 120.6 . . ? C7B C12B C11B 123.5(19) . . ? C7B C12B H12B 118.3 . . ? C11B C12B H12B 118.3 . . ? C14B C13B C18B 126.7(11) . . ? C14B C13B As1 119.3(9) . . ? C18B C13B As1 111.9(9) . . ? C13B C14B C15B 115.9(11) . . ? C13B C14B H14B 122.1 . . ? C15B C14B H14B 122.1 . . ? C16B C15B C14B 119.1(12) . . ? C16B C15B H15B 120.4 . . ? C14B C15B H15B 120.4 . . ? C17B C16B C15B 121.5(13) . . ? C17B C16B H16B 119.2 . . ? C15B C16B H16B 119.2 . . ? C16B C17B C18B 120.0(13) . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C13B C18B C17B 115.9(12) . . ? C13B C18B H18B 122.0 . . ? C17B C18B H18B 122.0 . . ? 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 Cl1 Ti1 As1 C7A -137.2(2) 2_677 . . . ? Cl1 Ti1 As1 C7A 42.8(2) . . . . ? Cl2 Ti1 As1 C7A 132.8(2) . . . . ? Cl2 Ti1 As1 C7A -47.2(2) 2_677 . . . ? Cl1 Ti1 As1 C13B -2.2(5) 2_677 . . . ? Cl1 Ti1 As1 C13B 177.8(5) . . . . ? Cl2 Ti1 As1 C13B -92.2(5) . . . . ? Cl2 Ti1 As1 C13B 87.8(5) 2_677 . . . ? Cl1 Ti1 As1 C1A 102.7(2) 2_677 . . . ? Cl1 Ti1 As1 C1A -77.3(2) . . . . ? Cl2 Ti1 As1 C1A 12.7(2) . . . . ? Cl2 Ti1 As1 C1A -167.3(2) 2_677 . . . ? Cl1 Ti1 As1 C13A -12.7(2) 2_677 . . . ? Cl1 Ti1 As1 C13A 167.3(2) . . . . ? Cl2 Ti1 As1 C13A -102.7(2) . . . . ? Cl2 Ti1 As1 C13A 77.3(2) 2_677 . . . ? Cl1 Ti1 As1 C1B 125.3(4) 2_677 . . . ? Cl1 Ti1 As1 C1B -54.7(4) . . . . ? Cl2 Ti1 As1 C1B 35.3(4) . . . . ? Cl2 Ti1 As1 C1B -144.7(4) 2_677 . . . ? Cl1 Ti1 As1 C7B -123.1(4) 2_677 . . . ? Cl1 Ti1 As1 C7B 56.9(4) . . . . ? Cl2 Ti1 As1 C7B 146.9(4) . . . . ? Cl2 Ti1 As1 C7B -33.1(4) 2_677 . . . ? C7A As1 C1A C6A 104.2(6) . . . . ? C13B As1 C1A C6A -3.3(8) . . . . ? C13A As1 C1A C6A -4.6(6) . . . . ? C1B As1 C1A C6A 134.2(16) . . . . ? C7B As1 C1A C6A 99.7(8) . . . . ? Ti1 As1 C1A C6A -128.6(5) . . . . ? C7A As1 C1A C2A -72.2(6) . . . . ? C13B As1 C1A C2A -179.7(8) . . . . ? C13A As1 C1A C2A 179.0(6) . . . . ? C1B As1 C1A C2A -42.2(13) . . . . ? C7B As1 C1A C2A -76.8(8) . . . . ? Ti1 As1 C1A C2A 54.9(6) . . . . ? C6A C1A C2A C3A 0.2(12) . . . . ? As1 C1A C2A C3A 176.7(7) . . . . ? C1A C2A C3A C4A 0.8(16) . . . . ? C2A C3A C4A C5A -0.5(18) . . . . ? C3A C4A C5A C6A -0.7(16) . . . . ? C2A C1A C6A C5A -1.4(10) . . . . ? As1 C1A C6A C5A -177.7(5) . . . . ? C4A C5A C6A C1A 1.6(12) . . . . ? C13B As1 C7A C12A -90.7(8) . . . . ? C1A As1 C7A C12A 174.6(7) . . . . ? C13A As1 C7A C12A -79.3(7) . . . . ? C1B As1 C7A C12A 164.4(8) . . . . ? C7B As1 C7A C12A -23(2) . . . . ? Ti1 As1 C7A C12A 50.6(8) . . . . ? C13B As1 C7A C8A 95.2(7) . . . . ? C1A As1 C7A C8A 0.6(7) . . . . ? C13A As1 C7A C8A 106.7(6) . . . . ? C1B As1 C7A C8A -9.7(7) . . . . ? C7B As1 C7A C8A 163(3) . . . . ? Ti1 As1 C7A C8A -123.4(6) . . . . ? C12A C7A C8A C9A 0.8(12) . . . . ? As1 C7A C8A C9A 174.6(5) . . . . ? C7A C8A C9A C10A -1.7(10) . . . . ? C8A C9A C10A C11A -0.3(13) . . . . ? C9A C10A C11A C12A 3.3(19) . . . . ? C8A C7A C12A C11A 2.0(14) . . . . ? As1 C7A C12A C11A -172.0(9) . . . . ? C10A C11A C12A C7A -4(2) . . . . ? C7A As1 C13A C18A 175.2(6) . . . . ? C13B As1 C13A C18A -83(4) . . . . ? C1A As1 C13A C18A -76.5(6) . . . . ? C1B As1 C13A C18A -91.7(7) . . . . ? C7B As1 C13A C18A 163.9(6) . . . . ? Ti1 As1 C13A C18A 44.8(6) . . . . ? C7A As1 C13A C14A -9.4(6) . . . . ? C13B As1 C13A C14A 92(4) . . . . ? C1A As1 C13A C14A 99.0(6) . . . . ? C1B As1 C13A C14A 83.8(7) . . . . ? C7B As1 C13A C14A -20.7(7) . . . . ? Ti1 As1 C13A C14A -139.7(5) . . . . ? C18A C13A C14A C15A -3.1(11) . . . . ? As1 C13A C14A C15A -178.9(6) . . . . ? C13A C14A C15A C16A 2.1(13) . . . . ? C14A C15A C16A C17A -1.1(14) . . . . ? C15A C16A C17A C18A 1.2(15) . . . . ? C14A C13A C18A C17A 3.3(10) . . . . ? As1 C13A C18A C17A 178.9(6) . . . . ? C16A C17A C18A C13A -2.4(14) . . . . ? C7A As1 C1B C6B -3.5(12) . . . . ? C13B As1 C1B C6B -110.0(13) . . . . ? C1A As1 C1B C6B -155(2) . . . . ? C13A As1 C1B C6B -108.3(12) . . . . ? C7B As1 C1B C6B -5.3(13) . . . . ? Ti1 As1 C1B C6B 113.9(11) . . . . ? C7A As1 C1B C2B 175.5(10) . . . . ? C13B As1 C1B C2B 69.0(12) . . . . ? C1A As1 C1B C2B 24.5(10) . . . . ? C13A As1 C1B C2B 70.7(11) . . . . ? C7B As1 C1B C2B 173.7(11) . . . . ? Ti1 As1 C1B C2B -67.1(10) . . . . ? C6B C1B C2B C3B 2(2) . . . . ? As1 C1B C2B C3B -177.5(12) . . . . ? C1B C2B C3B C4B -1(2) . . . . ? C2B C3B C4B C5B 0(3) . . . . ? C3B C4B C5B C6B 0(2) . . . . ? C2B C1B C6B C5B -2(2) . . . . ? As1 C1B C6B C5B 177.2(10) . . . . ? C4B C5B C6B C1B 1(2) . . . . ? C7A As1 C7B C12B 85(3) . . . . ? C13B As1 C7B C12B -159.4(13) . . . . ? C1A As1 C7B C12B 104.5(13) . . . . ? C13A As1 C7B C12B -148.9(12) . . . . ? C1B As1 C7B C12B 92.6(13) . . . . ? Ti1 As1 C7B C12B -27.1(14) . . . . ? C7A As1 C7B C8B -93(3) . . . . ? C13B As1 C7B C8B 22.9(10) . . . . ? C1A As1 C7B C8B -73.2(10) . . . . ? C13A As1 C7B C8B 33.4(10) . . . . ? C1B As1 C7B C8B -85.1(11) . . . . ? Ti1 As1 C7B C8B 155.3(9) . . . . ? C12B C7B C8B C9B -1.2(18) . . . . ? As1 C7B C8B C9B 176.7(9) . . . . ? C7B C8B C9B C10B -0.5(19) . . . . ? C8B C9B C10B C11B 6(3) . . . . ? C9B C10B C11B C12B -9(5) . . . . ? C8B C7B C12B C11B -2(3) . . . . ? As1 C7B C12B C11B 180(3) . . . . ? C10B C11B C12B C7B 8(5) . . . . ? C7A As1 C13B C14B -100.9(14) . . . . ? C1A As1 C13B C14B 4.2(14) . . . . ? C13A As1 C13B C14B 178(5) . . . . ? C1B As1 C13B C14B -10.3(16) . . . . ? C7B As1 C13B C14B -113.7(15) . . . . ? Ti1 As1 C13B C14B 120.5(13) . . . . ? C7A As1 C13B C18B 94.6(12) . . . . ? C1A As1 C13B C18B -160.3(12) . . . . ? C13A As1 C13B C18B 13(3) . . . . ? C1B As1 C13B C18B -174.8(11) . . . . ? C7B As1 C13B C18B 81.8(12) . . . . ? Ti1 As1 C13B C18B -44.1(14) . . . . ? C18B C13B C14B C15B -11(2) . . . . ? As1 C13B C14B C15B -173.1(10) . . . . ? C13B C14B C15B C16B 6(2) . . . . ? C14B C15B C16B C17B -2(2) . . . . ? C15B C16B C17B C18B 2(3) . . . . ? C14B C13B C18B C17B 10(3) . . . . ? As1 C13B C18B C17B 173.6(11) . . . . ? C16B C17B C18B C13B -5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.230 _refine_diff_density_min -1.291 _refine_diff_density_rms 0.105 # Attachment 'Compound_5-CCDC762191.cif' data_str0696 _database_code_depnum_ccdc_archive 'CCDC 762191' #TrackingRef 'Compound_5-CCDC762191.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 As Cl4 N3 Ti' _chemical_formula_sum 'C6 H18 As Cl4 N3 Ti' _chemical_formula_weight 396.85 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5866(16) _cell_length_b 15.623(3) _cell_length_c 9.8386(16) _cell_angle_alpha 90.00 _cell_angle_beta 92.562(3) _cell_angle_gamma 90.00 _cell_volume 1472.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5908 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 3.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3787 _exptl_absorpt_correction_T_max 0.7002 _exptl_absorpt_process_details 'SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12201 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.31 _reflns_number_total 3496 _reflns_number_gt 3304 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0216P)^2^+2.0024P] 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 3496 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.004 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 C1 C 0.9046(3) 0.05794(18) 0.6605(3) 0.0252(6) Uani 1 1 d . . . H1A H 0.9649 0.0125 0.6987 0.038 Uiso 1 1 calc R . . H1B H 0.9565 0.1120 0.6604 0.038 Uiso 1 1 calc R . . H1C H 0.8742 0.0430 0.5670 0.038 Uiso 1 1 calc R . . C2 C 0.7099(3) -0.01805(16) 0.7458(3) 0.0233(6) Uani 1 1 d . . . H2A H 0.6750 -0.0324 0.6535 0.035 Uiso 1 1 calc R . . H2B H 0.6317 -0.0164 0.8066 0.035 Uiso 1 1 calc R . . H2C H 0.7774 -0.0615 0.7779 0.035 Uiso 1 1 calc R . . C3 C 0.5566(3) 0.11766(18) 1.0005(3) 0.0232(6) Uani 1 1 d . . . H3A H 0.5853 0.1033 1.0946 0.035 Uiso 1 1 calc R . . H3B H 0.5391 0.0649 0.9486 0.035 Uiso 1 1 calc R . . H3C H 0.4710 0.1520 0.9996 0.035 Uiso 1 1 calc R . . C4 C 0.6915(3) 0.24674(17) 1.0200(3) 0.0233(6) Uani 1 1 d . . . H4A H 0.6060 0.2812 1.0158 0.035 Uiso 1 1 calc R . . H4B H 0.7681 0.2799 0.9834 0.035 Uiso 1 1 calc R . . H4C H 0.7153 0.2314 1.1148 0.035 Uiso 1 1 calc R . . C5 C 0.7001(3) 0.26074(17) 0.4322(3) 0.0219(5) Uani 1 1 d . . . H5A H 0.7912 0.2504 0.3940 0.033 Uiso 1 1 calc R . . H5B H 0.7067 0.3097 0.4944 0.033 Uiso 1 1 calc R . . H5C H 0.6309 0.2730 0.3584 0.033 Uiso 1 1 calc R . . C6 C 0.6353(3) 0.11162(18) 0.4163(3) 0.0270(6) Uani 1 1 d . . . H6A H 0.5567 0.1234 0.3519 0.040 Uiso 1 1 calc R . . H6B H 0.6148 0.0607 0.4701 0.040 Uiso 1 1 calc R . . H6C H 0.7198 0.1016 0.3661 0.040 Uiso 1 1 calc R . . N1 N 0.7795(2) 0.06764(13) 0.7450(2) 0.0171(4) Uani 1 1 d . . . N2 N 0.6689(2) 0.16719(13) 0.9379(2) 0.0168(4) Uani 1 1 d . . . N3 N 0.6572(2) 0.18466(14) 0.5066(2) 0.0185(4) Uani 1 1 d . . . Cl1 Cl 0.51488(6) 0.31031(4) 0.72551(6) 0.01980(13) Uani 1 1 d . . . Cl2 Cl 0.85459(6) 0.25923(4) 0.73446(6) 0.01874(13) Uani 1 1 d . . . Cl3 Cl 0.44308(6) 0.10057(4) 0.68908(7) 0.02311(14) Uani 1 1 d . . . Cl4 Cl 0.81359(7) -0.00102(4) 1.05177(7) 0.02715(15) Uani 1 1 d . . . Ti1 Ti 0.63915(4) 0.18561(3) 0.69446(4) 0.01401(10) Uani 1 1 d . . . As1 As 0.84390(3) 0.111689(16) 0.92104(3) 0.01620(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0240(14) 0.0260(14) 0.0260(14) -0.0018(11) 0.0068(11) 0.0057(11) C2 0.0266(14) 0.0125(12) 0.0306(15) -0.0024(10) -0.0012(11) 0.0005(10) C3 0.0182(12) 0.0279(14) 0.0241(14) 0.0040(11) 0.0063(10) 0.0001(10) C4 0.0294(14) 0.0232(14) 0.0171(13) -0.0053(10) -0.0012(11) 0.0026(11) C5 0.0213(13) 0.0260(14) 0.0185(12) 0.0013(11) 0.0012(10) 0.0001(10) C6 0.0342(15) 0.0242(14) 0.0220(14) -0.0064(11) -0.0044(11) -0.0004(11) N1 0.0168(10) 0.0155(10) 0.0191(10) -0.0003(8) 0.0020(8) 0.0006(8) N2 0.0167(10) 0.0161(10) 0.0176(10) 0.0012(8) 0.0014(8) 0.0020(8) N3 0.0189(10) 0.0210(11) 0.0154(10) -0.0013(8) -0.0011(8) -0.0011(8) Cl1 0.0186(3) 0.0155(3) 0.0252(3) -0.0005(2) -0.0002(2) 0.0023(2) Cl2 0.0157(3) 0.0182(3) 0.0222(3) 0.0020(2) -0.0013(2) -0.0046(2) Cl3 0.0183(3) 0.0183(3) 0.0324(4) 0.0007(3) -0.0023(2) -0.0049(2) Cl4 0.0289(3) 0.0233(3) 0.0292(3) 0.0113(3) 0.0004(3) 0.0030(3) Ti1 0.0138(2) 0.0123(2) 0.0158(2) 0.00012(16) -0.00080(16) -0.00102(15) As1 0.01473(13) 0.01630(13) 0.01748(13) 0.00248(10) -0.00010(9) 0.00116(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.497(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.496(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 N2 1.482(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N2 1.493(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.464(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N3 1.456(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? N1 As1 1.939(2) . ? N1 Ti1 2.323(2) . ? N2 As1 1.903(2) . ? N2 Ti1 2.417(2) . ? N3 Ti1 1.864(2) . ? Cl1 Ti1 2.3110(8) . ? Cl2 Ti1 2.3814(8) . ? Cl3 Ti1 2.3004(8) . ? Cl4 As1 2.2075(7) . ? Ti1 As1 3.1249(6) . ? 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 N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 N1 C1 106.3(2) . . ? C2 N1 As1 115.93(16) . . ? C1 N1 As1 107.55(16) . . ? C2 N1 Ti1 117.18(15) . . ? C1 N1 Ti1 115.59(16) . . ? As1 N1 Ti1 93.89(8) . . ? C3 N2 C4 107.5(2) . . ? C3 N2 As1 117.26(16) . . ? C4 N2 As1 108.62(16) . . ? C3 N2 Ti1 114.72(16) . . ? C4 N2 Ti1 116.44(15) . . ? As1 N2 Ti1 91.90(8) . . ? C6 N3 C5 111.6(2) . . ? C6 N3 Ti1 126.45(18) . . ? C5 N3 Ti1 121.98(17) . . ? N3 Ti1 Cl3 94.85(7) . . ? N3 Ti1 Cl1 102.07(7) . . ? Cl3 Ti1 Cl1 93.69(3) . . ? N3 Ti1 N1 97.32(9) . . ? Cl3 Ti1 N1 90.67(6) . . ? Cl1 Ti1 N1 159.67(6) . . ? N3 Ti1 Cl2 92.83(7) . . ? Cl3 Ti1 Cl2 169.89(3) . . ? Cl1 Ti1 Cl2 91.11(3) . . ? N1 Ti1 Cl2 81.84(6) . . ? N3 Ti1 N2 165.86(9) . . ? Cl3 Ti1 N2 90.81(5) . . ? Cl1 Ti1 N2 90.46(5) . . ? N1 Ti1 N2 69.62(7) . . ? Cl2 Ti1 N2 80.25(5) . . ? N3 Ti1 As1 128.40(7) . . ? Cl3 Ti1 As1 106.83(2) . . ? Cl1 Ti1 As1 121.89(2) . . ? N1 Ti1 As1 38.24(5) . . ? Cl2 Ti1 As1 63.14(2) . . ? N2 Ti1 As1 37.48(5) . . ? N2 As1 N1 89.60(9) . . ? N2 As1 Cl4 99.97(7) . . ? N1 As1 Cl4 101.09(7) . . ? N2 As1 Ti1 50.62(6) . . ? N1 As1 Ti1 47.87(6) . . ? Cl4 As1 Ti1 128.00(2) . . ? 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 C6 N3 Ti1 Cl3 -40.2(2) . . . . ? C5 N3 Ti1 Cl3 141.31(18) . . . . ? C6 N3 Ti1 Cl1 -135.0(2) . . . . ? C5 N3 Ti1 Cl1 46.5(2) . . . . ? C6 N3 Ti1 N1 51.1(2) . . . . ? C5 N3 Ti1 N1 -127.39(19) . . . . ? C6 N3 Ti1 Cl2 133.2(2) . . . . ? C5 N3 Ti1 Cl2 -45.26(19) . . . . ? C6 N3 Ti1 N2 73.1(4) . . . . ? C5 N3 Ti1 N2 -105.4(4) . . . . ? C6 N3 Ti1 As1 75.8(2) . . . . ? C5 N3 Ti1 As1 -102.71(19) . . . . ? C2 N1 Ti1 N3 -90.07(18) . . . . ? C1 N1 Ti1 N3 36.51(19) . . . . ? As1 N1 Ti1 N3 148.08(9) . . . . ? C2 N1 Ti1 Cl3 4.91(17) . . . . ? C1 N1 Ti1 Cl3 131.49(17) . . . . ? As1 N1 Ti1 Cl3 -116.94(7) . . . . ? C2 N1 Ti1 Cl1 107.4(2) . . . . ? C1 N1 Ti1 Cl1 -125.98(19) . . . . ? As1 N1 Ti1 Cl1 -14.4(2) . . . . ? C2 N1 Ti1 Cl2 178.10(17) . . . . ? C1 N1 Ti1 Cl2 -55.31(17) . . . . ? As1 N1 Ti1 Cl2 56.26(6) . . . . ? C2 N1 Ti1 N2 95.52(18) . . . . ? C1 N1 Ti1 N2 -137.90(19) . . . . ? As1 N1 Ti1 N2 -26.33(7) . . . . ? C2 N1 Ti1 As1 121.8(2) . . . . ? C1 N1 Ti1 As1 -111.6(2) . . . . ? C3 N2 Ti1 N3 -117.8(4) . . . . ? C4 N2 Ti1 N3 115.4(4) . . . . ? As1 N2 Ti1 N3 3.5(4) . . . . ? C3 N2 Ti1 Cl3 -4.10(16) . . . . ? C4 N2 Ti1 Cl3 -130.86(17) . . . . ? As1 N2 Ti1 Cl3 117.23(7) . . . . ? C3 N2 Ti1 Cl1 89.60(16) . . . . ? C4 N2 Ti1 Cl1 -37.16(17) . . . . ? As1 N2 Ti1 Cl1 -149.08(7) . . . . ? C3 N2 Ti1 N1 -94.51(17) . . . . ? C4 N2 Ti1 N1 138.73(18) . . . . ? As1 N2 Ti1 N1 26.81(7) . . . . ? C3 N2 Ti1 Cl2 -179.35(17) . . . . ? C4 N2 Ti1 Cl2 53.89(16) . . . . ? As1 N2 Ti1 Cl2 -58.03(6) . . . . ? C3 N2 Ti1 As1 -121.3(2) . . . . ? C4 N2 Ti1 As1 111.92(19) . . . . ? C3 N2 As1 N1 88.76(19) . . . . ? C4 N2 As1 N1 -149.21(17) . . . . ? Ti1 N2 As1 N1 -30.44(8) . . . . ? C3 N2 As1 Cl4 -12.43(19) . . . . ? C4 N2 As1 Cl4 109.60(15) . . . . ? Ti1 N2 As1 Cl4 -131.64(5) . . . . ? C3 N2 As1 Ti1 119.2(2) . . . . ? C4 N2 As1 Ti1 -118.77(18) . . . . ? C2 N1 As1 N2 -90.96(17) . . . . ? C1 N1 As1 N2 150.27(17) . . . . ? Ti1 N1 As1 N2 31.87(8) . . . . ? C2 N1 As1 Cl4 9.12(17) . . . . ? C1 N1 As1 Cl4 -109.64(15) . . . . ? Ti1 N1 As1 Cl4 131.96(5) . . . . ? C2 N1 As1 Ti1 -122.84(19) . . . . ? C1 N1 As1 Ti1 118.40(18) . . . . ? N3 Ti1 As1 N2 -178.91(12) . . . . ? Cl3 Ti1 As1 N2 -68.27(9) . . . . ? Cl1 Ti1 As1 N2 37.25(8) . . . . ? N1 Ti1 As1 N2 -136.91(12) . . . . ? Cl2 Ti1 As1 N2 110.41(8) . . . . ? N3 Ti1 As1 N1 -42.00(12) . . . . ? Cl3 Ti1 As1 N1 68.64(9) . . . . ? Cl1 Ti1 As1 N1 174.16(9) . . . . ? Cl2 Ti1 As1 N1 -112.68(9) . . . . ? N2 Ti1 As1 N1 136.91(12) . . . . ? N3 Ti1 As1 Cl4 -109.83(9) . . . . ? Cl3 Ti1 As1 Cl4 0.82(4) . . . . ? Cl1 Ti1 As1 Cl4 106.33(4) . . . . ? N1 Ti1 As1 Cl4 -67.83(9) . . . . ? Cl2 Ti1 As1 Cl4 179.49(3) . . . . ? N2 Ti1 As1 Cl4 69.08(9) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.585 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.093