# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- Fuller et al Ti nitrido.cif' _publ_contact_author_name 'Simon J. lancaster' _publ_contact_author_address ;Wolfson Materials and Catalysis Centre, School of Chemistry, University of East Anglia, Norwich Research Park, Norwich, NR4 7TJ UK. ; _publ_contact_author_email S.Lancaster@uea.ac.uk _publ_contact_author_phone '44 1603 592009' _publ_contact_author_fax '44 1603 592003' loop_ _publ_author_name _publ_author_address A.-M.Fuller ;Wolfson Materials and Catalysis Centre, School of Chemistry, University of East Anglia, Norwich Research Park, Norwich, NR4 7TJ UK. ; D.L.Hughes ;Wolfson Materials and Catalysis Centre, School of Chemistry, University of East Anglia, Norwich Research Park, Norwich, NR4 7TJ UK. ; G.A.Jones ;Wolfson Materials and Catalysis Centre, School of Chemistry, University of East Anglia, Norwich Research Park, Norwich, NR4 7TJ UK. ; S.J.Lancaster ;Wolfson Materials and Catalysis Centre, School of Chemistry, University of East Anglia, Norwich Research Park, Norwich, NR4 7TJ UK. ; data_5 _database_code_depnum_ccdc_archive 'CCDC 862683' #TrackingRef '- Fuller et al Ti nitrido.cif' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_formula_structural ; [N(CH3)4][{(C6F5)3B}NTiCl2(NH(CH3)2)], CH2Cl2 ; _chemical_name_common ; [N(CH3)4][{(C6F5)3B}NTiCl2(NH(CH3)2)], CH2Cl2 ; _chemical_melting_point ? _chemical_formula_moiety ; C4 H12 N, C22 H14 B Cl2 F15 N3 Ti, C H2 Cl2 ; _chemical_formula_sum 'C27 H28 B Cl4 F15 N4 Ti' _chemical_formula_weight 894.04 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' 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 Pbca 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 18.3489(2) _cell_length_b 18.8537(2) _cell_length_c 21.0286(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7274.73(13) _cell_formula_units_Z 8 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 36855 _cell_measurement_theta_min 3.1267 _cell_measurement_theta_max 32.1969 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9323 _exptl_absorpt_correction_T_max 1.0611 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 124100 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6385 _reflns_number_gt 5125 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^ > 2\s(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^)+(0.0721P)^2^+15.0718P] 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 6385 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.47086(4) 0.16314(3) 0.74747(3) 0.01656(17) Uani 1 1 d . . . Cl2 Cl 0.36685(5) 0.17082(5) 0.68102(5) 0.0254(2) Uani 1 1 d . . . Cl3 Cl 0.49794(6) 0.11988(6) 0.85127(5) 0.0379(3) Uani 1 1 d . . . N1 N 0.48512(18) 0.05408(17) 0.71186(19) 0.0294(8) Uani 1 1 d . . . H1 H 0.4837 0.0574 0.6687 0.035 Uiso 1 1 calc R . . C2 C 0.5574(3) 0.0232(3) 0.7273(3) 0.0580(17) Uani 1 1 d . . . H2A H 0.5575 0.0072 0.7707 0.087 Uiso 1 1 calc R . . H2B H 0.5944 0.0586 0.7217 0.087 Uiso 1 1 calc R . . H2C H 0.5669 -0.0162 0.6996 0.087 Uiso 1 1 calc R . . C3 C 0.4274(2) 0.0033(2) 0.7291(2) 0.0380(11) Uani 1 1 d . . . H3A H 0.4377 -0.0419 0.7101 0.057 Uiso 1 1 calc R . . H3B H 0.3813 0.0204 0.7139 0.057 Uiso 1 1 calc R . . H3C H 0.4256 -0.0017 0.7745 0.057 Uiso 1 1 calc R . . N11 N 0.43009(17) 0.25721(17) 0.79900(15) 0.0209(7) Uani 1 1 d . . . H11 H 0.4650 0.2674 0.8284 0.025 Uiso 1 1 calc R . . C12 C 0.4241(2) 0.3214(2) 0.7591(2) 0.0290(10) Uani 1 1 d . . . H12A H 0.3893 0.3133 0.7258 0.043 Uiso 1 1 calc R . . H12B H 0.4707 0.3321 0.7408 0.043 Uiso 1 1 calc R . . H12C H 0.4082 0.3606 0.7848 0.043 Uiso 1 1 calc R . . C13 C 0.3625(2) 0.2454(2) 0.8360(2) 0.0301(10) Uani 1 1 d . . . H13A H 0.3528 0.2861 0.8621 0.045 Uiso 1 1 calc R . . H13B H 0.3683 0.2043 0.8625 0.045 Uiso 1 1 calc R . . H13C H 0.3224 0.2380 0.8073 0.045 Uiso 1 1 calc R . . N21 N 0.54165(16) 0.20277(15) 0.71136(14) 0.0165(7) Uani 1 1 d . . . B22 B 0.5930(2) 0.2434(2) 0.6673(2) 0.0167(9) Uani 1 1 d . . . F32 F 0.50675(13) 0.16376(12) 0.57705(11) 0.0284(5) Uani 1 1 d . . . F33 F 0.40463(14) 0.21189(16) 0.49825(13) 0.0462(7) Uani 1 1 d . . . F34 F 0.37641(15) 0.35268(18) 0.48941(14) 0.0540(8) Uani 1 1 d . . . F35 F 0.45339(17) 0.44577(15) 0.56288(15) 0.0524(8) Uani 1 1 d . . . F36 F 0.55528(14) 0.40012(12) 0.64152(12) 0.0345(6) Uani 1 1 d . . . F42 F 0.69892(12) 0.33121(12) 0.60474(10) 0.0244(5) Uani 1 1 d . . . F43 F 0.79334(12) 0.42232(12) 0.65558(11) 0.0279(5) Uani 1 1 d . . . F44 F 0.79481(13) 0.44415(13) 0.78421(12) 0.0326(6) Uani 1 1 d . . . F45 F 0.69658(14) 0.37530(14) 0.85860(11) 0.0352(6) Uani 1 1 d . . . F46 F 0.59948(12) 0.28820(12) 0.80929(10) 0.0262(5) Uani 1 1 d . . . F52 F 0.68624(12) 0.15441(11) 0.74277(10) 0.0213(5) Uani 1 1 d . . . F53 F 0.77787(13) 0.05405(12) 0.70479(11) 0.0299(6) Uani 1 1 d . . . F54 F 0.79837(13) 0.02729(13) 0.57877(12) 0.0345(6) Uani 1 1 d . . . F55 F 0.72673(13) 0.10789(14) 0.49112(11) 0.0349(6) Uani 1 1 d . . . F56 F 0.63813(12) 0.21104(12) 0.52677(10) 0.0266(5) Uani 1 1 d . . . C31 C 0.53818(19) 0.2792(2) 0.61313(18) 0.0191(8) Uani 1 1 d . . . C32 C 0.4963(2) 0.2350(2) 0.57479(19) 0.0239(9) Uani 1 1 d . . . C33 C 0.4429(2) 0.2586(3) 0.5337(2) 0.0305(10) Uani 1 1 d . . . C34 C 0.4289(2) 0.3295(3) 0.5291(2) 0.0348(11) Uani 1 1 d . . . C35 C 0.4673(2) 0.3757(2) 0.5659(2) 0.0333(11) Uani 1 1 d . . . C36 C 0.5206(2) 0.3500(2) 0.60666(19) 0.0238(9) Uani 1 1 d . . . C41 C 0.6445(2) 0.30326(18) 0.70348(17) 0.0162(8) Uani 1 1 d . . . C42 C 0.6957(2) 0.34115(19) 0.66838(16) 0.0169(8) Uani 1 1 d . . . C43 C 0.7450(2) 0.3882(2) 0.69325(18) 0.0210(8) Uani 1 1 d . . . C44 C 0.7462(2) 0.39971(19) 0.75814(19) 0.0219(8) Uani 1 1 d . . . C45 C 0.6962(2) 0.3643(2) 0.79532(18) 0.0224(9) Uani 1 1 d . . . C46 C 0.6470(2) 0.31823(19) 0.76788(18) 0.0180(8) Uani 1 1 d . . . C51 C 0.6534(2) 0.18589(19) 0.63711(17) 0.0159(8) Uani 1 1 d . . . C52 C 0.69371(19) 0.14431(19) 0.67933(17) 0.0163(8) Uani 1 1 d . . . C53 C 0.7416(2) 0.09198(19) 0.66126(18) 0.0201(8) Uani 1 1 d . . . C54 C 0.7526(2) 0.0785(2) 0.59741(19) 0.0221(8) Uani 1 1 d . . . C55 C 0.7162(2) 0.1198(2) 0.55357(18) 0.0235(9) Uani 1 1 d . . . C56 C 0.6694(2) 0.1719(2) 0.57435(17) 0.0195(8) Uani 1 1 d . . . N61 N 0.19516(18) 0.11634(18) 0.56856(15) 0.0223(7) Uani 1 1 d . . . C62 C 0.2026(3) 0.0570(2) 0.6150(2) 0.0378(11) Uani 1 1 d . . . H62A H 0.2125 0.0137 0.5925 0.057 Uiso 1 1 calc R . . H62B H 0.1580 0.0520 0.6385 0.057 Uiso 1 1 calc R . . H62C H 0.2419 0.0670 0.6437 0.057 Uiso 1 1 calc R . . C63 C 0.2641(2) 0.1243(3) 0.5316(2) 0.0431(13) Uani 1 1 d . . . H63A H 0.2734 0.0815 0.5082 0.065 Uiso 1 1 calc R . . H63B H 0.3038 0.1331 0.5603 0.065 Uiso 1 1 calc R . . H63C H 0.2595 0.1633 0.5026 0.065 Uiso 1 1 calc R . . C64 C 0.1328(2) 0.1020(3) 0.5247(2) 0.0316(10) Uani 1 1 d . . . H64A H 0.1275 0.1409 0.4956 0.047 Uiso 1 1 calc R . . H64B H 0.0889 0.0966 0.5490 0.047 Uiso 1 1 calc R . . H64C H 0.1421 0.0592 0.5013 0.047 Uiso 1 1 calc R . . C65 C 0.1809(3) 0.1829(2) 0.6050(2) 0.0330(10) Uani 1 1 d . . . H65A H 0.2209 0.1919 0.6333 0.050 Uiso 1 1 calc R . . H65B H 0.1368 0.1777 0.6292 0.050 Uiso 1 1 calc R . . H65C H 0.1759 0.2219 0.5759 0.050 Uiso 1 1 calc R . . C71 C 0.4456(4) -0.0775(4) 0.5502(3) 0.0664(18) Uani 1 1 d . . . H71A H 0.4545 -0.0865 0.5055 0.080 Uiso 1 1 calc R . . H71B H 0.4070 -0.1092 0.5639 0.080 Uiso 1 1 calc R . . Cl72 Cl 0.41681(9) 0.00688(9) 0.55874(8) 0.0680(4) Uani 1 1 d . . . Cl73 Cl 0.52485(13) -0.09717(12) 0.59310(9) 0.0948(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0123(3) 0.0161(3) 0.0212(3) 0.0039(3) -0.0019(3) -0.0001(3) Cl2 0.0176(5) 0.0293(5) 0.0292(5) -0.0006(4) -0.0071(4) -0.0001(4) Cl3 0.0326(6) 0.0479(7) 0.0331(6) 0.0192(5) -0.0081(5) -0.0006(5) N1 0.0197(18) 0.0171(16) 0.051(2) 0.0009(16) 0.0071(16) -0.0017(14) C2 0.024(3) 0.023(2) 0.128(6) -0.008(3) 0.005(3) 0.006(2) C3 0.030(2) 0.024(2) 0.060(3) 0.003(2) 0.009(2) -0.0058(19) N11 0.0163(16) 0.0234(17) 0.0231(17) -0.0015(14) 0.0005(13) -0.0024(14) C12 0.030(2) 0.021(2) 0.036(2) -0.0008(18) 0.0063(19) 0.0032(18) C13 0.024(2) 0.033(2) 0.034(2) -0.0019(19) 0.0106(18) 0.0002(19) N21 0.0134(16) 0.0149(15) 0.0212(16) 0.0000(12) -0.0022(13) 0.0028(12) B22 0.017(2) 0.015(2) 0.019(2) 0.0009(16) -0.0014(17) 0.0012(17) F32 0.0293(13) 0.0265(12) 0.0293(13) -0.0020(10) -0.0078(10) -0.0068(10) F33 0.0330(15) 0.067(2) 0.0383(15) 0.0012(14) -0.0191(12) -0.0125(14) F34 0.0315(15) 0.086(2) 0.0447(17) 0.0193(16) -0.0154(13) 0.0193(15) F35 0.0550(19) 0.0383(16) 0.0640(19) 0.0145(14) -0.0098(15) 0.0267(14) F36 0.0392(15) 0.0192(12) 0.0451(15) -0.0008(11) -0.0114(12) 0.0067(11) F42 0.0268(12) 0.0296(12) 0.0170(11) 0.0029(9) 0.0005(9) -0.0064(10) F43 0.0227(12) 0.0252(12) 0.0358(13) 0.0040(10) 0.0046(10) -0.0094(10) F44 0.0288(13) 0.0295(13) 0.0394(14) -0.0122(11) -0.0061(11) -0.0104(11) F45 0.0384(15) 0.0481(16) 0.0192(12) -0.0111(11) -0.0015(10) -0.0055(12) F46 0.0265(12) 0.0338(13) 0.0181(11) 0.0010(10) 0.0030(10) -0.0048(10) F52 0.0226(12) 0.0260(12) 0.0154(11) -0.0006(9) -0.0029(9) 0.0046(9) F53 0.0285(13) 0.0264(12) 0.0347(13) 0.0032(10) -0.0078(11) 0.0106(11) F54 0.0300(14) 0.0305(13) 0.0432(15) -0.0101(11) 0.0082(11) 0.0101(11) F55 0.0344(14) 0.0509(16) 0.0193(12) -0.0100(11) 0.0059(10) 0.0025(12) F56 0.0283(13) 0.0359(13) 0.0155(11) 0.0046(10) -0.0020(9) 0.0024(11) C31 0.0114(19) 0.026(2) 0.0199(19) 0.0041(16) 0.0028(15) 0.0019(16) C32 0.020(2) 0.028(2) 0.024(2) 0.0052(17) -0.0001(17) -0.0015(17) C33 0.019(2) 0.049(3) 0.024(2) 0.003(2) -0.0047(17) -0.007(2) C34 0.019(2) 0.056(3) 0.030(2) 0.013(2) -0.0066(18) 0.012(2) C35 0.027(2) 0.036(3) 0.037(3) 0.012(2) -0.001(2) 0.013(2) C36 0.018(2) 0.027(2) 0.027(2) 0.0035(17) 0.0015(17) 0.0058(17) C41 0.0138(18) 0.0137(17) 0.0211(19) 0.0022(15) -0.0021(15) 0.0034(15) C42 0.0184(19) 0.0184(18) 0.0139(18) 0.0017(15) -0.0013(15) 0.0014(15) C43 0.017(2) 0.0192(18) 0.027(2) 0.0056(16) 0.0017(16) 0.0001(15) C44 0.020(2) 0.0161(18) 0.030(2) -0.0062(16) -0.0069(17) -0.0003(16) C45 0.023(2) 0.026(2) 0.018(2) -0.0062(16) -0.0017(16) 0.0036(17) C46 0.0144(18) 0.0191(18) 0.0205(19) 0.0032(15) 0.0017(15) 0.0014(15) C51 0.0140(18) 0.0153(18) 0.0186(19) 0.0001(15) 0.0000(15) -0.0032(15) C52 0.0154(18) 0.0180(18) 0.0154(18) -0.0016(15) -0.0002(15) -0.0047(15) C53 0.0138(19) 0.0187(19) 0.028(2) 0.0033(16) -0.0032(16) -0.0012(16) C54 0.0157(19) 0.0182(19) 0.032(2) -0.0073(17) 0.0047(17) -0.0004(16) C55 0.022(2) 0.029(2) 0.020(2) -0.0075(17) 0.0049(17) -0.0060(18) C56 0.0182(19) 0.0211(19) 0.0191(19) 0.0022(16) -0.0026(15) -0.0048(16) N61 0.0201(17) 0.0305(18) 0.0162(16) 0.0033(14) -0.0010(13) -0.0001(15) C62 0.046(3) 0.029(2) 0.039(3) 0.013(2) -0.003(2) 0.006(2) C63 0.022(2) 0.083(4) 0.025(2) 0.001(2) 0.0037(19) -0.006(2) C64 0.023(2) 0.052(3) 0.021(2) -0.001(2) -0.0036(18) -0.007(2) C65 0.033(3) 0.030(2) 0.036(3) -0.0013(19) -0.009(2) 0.004(2) C71 0.062(4) 0.090(5) 0.047(3) -0.014(3) 0.009(3) -0.010(4) Cl72 0.0688(11) 0.0640(10) 0.0712(10) 0.0044(8) -0.0107(8) 0.0034(8) Cl73 0.1162(17) 0.1016(15) 0.0667(11) -0.0042(10) -0.0069(11) 0.0505(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N21 1.680(3) . ? Ti1 N1 2.204(3) . ? Ti1 N11 2.209(3) . ? Ti1 Cl2 2.3698(11) . ? Ti1 Cl3 2.3826(12) . ? N1 C3 1.472(5) . ? N1 C2 1.484(6) . ? N1 H1 0.9100 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? N11 C12 1.477(5) . ? N11 C13 1.482(5) . ? N11 H11 0.9100 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? N21 B22 1.528(5) . ? B22 C41 1.657(5) . ? B22 C31 1.662(5) . ? B22 C51 1.674(5) . ? F32 C32 1.357(5) . ? F33 C33 1.351(5) . ? F34 C34 1.347(5) . ? F35 C35 1.346(5) . ? F36 C36 1.355(5) . ? F42 C42 1.353(4) . ? F43 C43 1.351(4) . ? F44 C44 1.342(4) . ? F45 C45 1.347(4) . ? F46 C46 1.356(4) . ? F52 C52 1.354(4) . ? F53 C53 1.339(4) . ? F54 C54 1.338(4) . ? F55 C55 1.346(4) . ? F56 C56 1.370(4) . ? C31 C36 1.380(6) . ? C31 C32 1.391(6) . ? C32 C33 1.379(6) . ? C33 C34 1.365(7) . ? C34 C35 1.363(7) . ? C35 C36 1.387(6) . ? C41 C46 1.384(5) . ? C41 C42 1.392(5) . ? C42 C43 1.372(5) . ? C43 C44 1.382(5) . ? C44 C45 1.377(6) . ? C45 C46 1.380(6) . ? C51 C56 1.378(5) . ? C51 C52 1.397(5) . ? C52 C53 1.374(5) . ? C53 C54 1.381(5) . ? C54 C55 1.379(6) . ? C55 C56 1.376(6) . ? N61 C62 1.491(5) . ? N61 C63 1.492(5) . ? N61 C64 1.493(5) . ? N61 C65 1.494(5) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C71 Cl72 1.686(7) . ? C71 Cl73 1.752(7) . ? C71 H71A 0.9700 . ? C71 H71B 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 N21 Ti1 N1 99.77(14) . . ? N21 Ti1 N11 97.26(13) . . ? N1 Ti1 N11 162.94(12) . . ? N21 Ti1 Cl2 109.20(11) . . ? N1 Ti1 Cl2 87.26(10) . . ? N11 Ti1 Cl2 88.13(9) . . ? N21 Ti1 Cl3 113.90(11) . . ? N1 Ti1 Cl3 88.12(11) . . ? N11 Ti1 Cl3 84.04(9) . . ? Cl2 Ti1 Cl3 136.81(5) . . ? C3 N1 C2 109.5(3) . . ? C3 N1 Ti1 116.0(3) . . ? C2 N1 Ti1 113.4(3) . . ? C3 N1 H1 105.7 . . ? C2 N1 H1 105.7 . . ? Ti1 N1 H1 105.7 . . ? 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 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C12 N11 C13 111.0(3) . . ? C12 N11 Ti1 113.9(2) . . ? C13 N11 Ti1 114.8(2) . . ? C12 N11 H11 105.4 . . ? C13 N11 H11 105.4 . . ? Ti1 N11 H11 105.4 . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N11 C13 H13A 109.5 . . ? N11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? B22 N21 Ti1 167.0(3) . . ? N21 B22 C41 114.4(3) . . ? N21 B22 C31 104.2(3) . . ? C41 B22 C31 112.5(3) . . ? N21 B22 C51 108.3(3) . . ? C41 B22 C51 103.8(3) . . ? C31 B22 C51 113.8(3) . . ? C36 C31 C32 113.1(3) . . ? C36 C31 B22 127.0(3) . . ? C32 C31 B22 119.2(3) . . ? F32 C32 C33 116.2(4) . . ? F32 C32 C31 119.6(3) . . ? C33 C32 C31 124.2(4) . . ? F33 C33 C34 120.0(4) . . ? F33 C33 C32 120.4(4) . . ? C34 C33 C32 119.6(4) . . ? F34 C34 C35 120.9(4) . . ? F34 C34 C33 119.8(4) . . ? C35 C34 C33 119.3(4) . . ? F35 C35 C34 120.2(4) . . ? F35 C35 C36 120.4(4) . . ? C34 C35 C36 119.4(4) . . ? F36 C36 C31 120.7(3) . . ? F36 C36 C35 114.9(4) . . ? C31 C36 C35 124.4(4) . . ? C46 C41 C42 113.1(3) . . ? C46 C41 B22 127.4(3) . . ? C42 C41 B22 119.4(3) . . ? F42 C42 C43 116.0(3) . . ? F42 C42 C41 118.9(3) . . ? C43 C42 C41 125.1(3) . . ? F43 C43 C42 121.1(3) . . ? F43 C43 C44 119.7(3) . . ? C42 C43 C44 119.2(3) . . ? F44 C44 C45 120.9(3) . . ? F44 C44 C43 120.8(4) . . ? C45 C44 C43 118.4(3) . . ? F45 C45 C44 118.9(3) . . ? F45 C45 C46 120.9(4) . . ? C44 C45 C46 120.2(3) . . ? F46 C46 C45 114.5(3) . . ? F46 C46 C41 121.4(3) . . ? C45 C46 C41 124.0(3) . . ? C56 C51 C52 112.8(3) . . ? C56 C51 B22 128.9(3) . . ? C52 C51 B22 118.2(3) . . ? F52 C52 C53 116.0(3) . . ? F52 C52 C51 119.6(3) . . ? C53 C52 C51 124.5(3) . . ? F53 C53 C52 120.8(3) . . ? F53 C53 C54 119.5(3) . . ? C52 C53 C54 119.6(3) . . ? F54 C54 C55 121.0(3) . . ? F54 C54 C53 120.6(4) . . ? C55 C54 C53 118.4(3) . . ? F55 C55 C56 121.2(4) . . ? F55 C55 C54 119.3(4) . . ? C56 C55 C54 119.5(4) . . ? F56 C56 C55 114.5(3) . . ? F56 C56 C51 120.5(3) . . ? C55 C56 C51 125.1(4) . . ? C62 N61 C63 109.8(4) . . ? C62 N61 C64 109.7(3) . . ? C63 N61 C64 110.2(3) . . ? C62 N61 C65 108.1(3) . . ? C63 N61 C65 109.3(4) . . ? C64 N61 C65 109.6(3) . . ? N61 C62 H62A 109.5 . . ? N61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N61 C63 H63A 109.5 . . ? N61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N61 C64 H64A 109.5 . . ? N61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N61 C65 H65A 109.5 . . ? N61 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N61 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? Cl72 C71 Cl73 113.9(4) . . ? Cl72 C71 H71A 108.8 . . ? Cl73 C71 H71A 108.8 . . ? Cl72 C71 H71B 108.8 . . ? Cl73 C71 H71B 108.8 . . ? H71A C71 H71B 107.7 . . ? 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 N21 Ti1 N1 C3 -174.5(3) . . . . ? N11 Ti1 N1 C3 9.1(7) . . . . ? Cl2 Ti1 N1 C3 -65.4(3) . . . . ? Cl3 Ti1 N1 C3 71.6(3) . . . . ? N21 Ti1 N1 C2 57.6(4) . . . . ? N11 Ti1 N1 C2 -118.9(5) . . . . ? Cl2 Ti1 N1 C2 166.6(4) . . . . ? Cl3 Ti1 N1 C2 -56.4(4) . . . . ? N21 Ti1 N11 C12 47.4(3) . . . . ? N1 Ti1 N11 C12 -136.1(4) . . . . ? Cl2 Ti1 N11 C12 -61.8(3) . . . . ? Cl3 Ti1 N11 C12 160.8(3) . . . . ? N21 Ti1 N11 C13 177.0(3) . . . . ? N1 Ti1 N11 C13 -6.5(6) . . . . ? Cl2 Ti1 N11 C13 67.8(3) . . . . ? Cl3 Ti1 N11 C13 -69.6(3) . . . . ? N1 Ti1 N21 B22 95.8(12) . . . . ? N11 Ti1 N21 B22 -85.2(12) . . . . ? Cl2 Ti1 N21 B22 5.3(12) . . . . ? Cl3 Ti1 N21 B22 -171.9(11) . . . . ? Ti1 N21 B22 C41 130.2(11) . . . . ? Ti1 N21 B22 C31 6.9(13) . . . . ? Ti1 N21 B22 C51 -114.6(11) . . . . ? N21 B22 C31 C36 109.0(4) . . . . ? C41 B22 C31 C36 -15.6(5) . . . . ? C51 B22 C31 C36 -133.3(4) . . . . ? N21 B22 C31 C32 -61.1(4) . . . . ? C41 B22 C31 C32 174.4(3) . . . . ? C51 B22 C31 C32 56.7(4) . . . . ? C36 C31 C32 F32 -178.8(3) . . . . ? B22 C31 C32 F32 -7.4(5) . . . . ? C36 C31 C32 C33 0.7(6) . . . . ? B22 C31 C32 C33 172.1(4) . . . . ? F32 C32 C33 F33 -0.3(6) . . . . ? C31 C32 C33 F33 -179.8(4) . . . . ? F32 C32 C33 C34 179.6(4) . . . . ? C31 C32 C33 C34 0.1(7) . . . . ? F33 C33 C34 F34 0.4(7) . . . . ? C32 C33 C34 F34 -179.5(4) . . . . ? F33 C33 C34 C35 179.0(4) . . . . ? C32 C33 C34 C35 -0.9(7) . . . . ? F34 C34 C35 F35 -0.2(7) . . . . ? C33 C34 C35 F35 -178.8(4) . . . . ? F34 C34 C35 C36 179.4(4) . . . . ? C33 C34 C35 C36 0.8(7) . . . . ? C32 C31 C36 F36 178.8(3) . . . . ? B22 C31 C36 F36 8.2(6) . . . . ? C32 C31 C36 C35 -0.7(6) . . . . ? B22 C31 C36 C35 -171.3(4) . . . . ? F35 C35 C36 F36 0.1(6) . . . . ? C34 C35 C36 F36 -179.5(4) . . . . ? F35 C35 C36 C31 179.6(4) . . . . ? C34 C35 C36 C31 0.0(7) . . . . ? N21 B22 C41 C46 2.0(5) . . . . ? C31 B22 C41 C46 120.7(4) . . . . ? C51 B22 C41 C46 -115.8(4) . . . . ? N21 B22 C41 C42 177.1(3) . . . . ? C31 B22 C41 C42 -64.2(4) . . . . ? C51 B22 C41 C42 59.3(4) . . . . ? C46 C41 C42 F42 179.9(3) . . . . ? B22 C41 C42 F42 4.1(5) . . . . ? C46 C41 C42 C43 0.8(5) . . . . ? B22 C41 C42 C43 -175.0(3) . . . . ? F42 C42 C43 F43 0.3(5) . . . . ? C41 C42 C43 F43 179.4(3) . . . . ? F42 C42 C43 C44 -178.4(3) . . . . ? C41 C42 C43 C44 0.8(6) . . . . ? F43 C43 C44 F44 -0.2(6) . . . . ? C42 C43 C44 F44 178.5(3) . . . . ? F43 C43 C44 C45 179.9(3) . . . . ? C42 C43 C44 C45 -1.4(6) . . . . ? F44 C44 C45 F45 0.4(6) . . . . ? C43 C44 C45 F45 -179.7(3) . . . . ? F44 C44 C45 C46 -179.3(3) . . . . ? C43 C44 C45 C46 0.6(6) . . . . ? F45 C45 C46 F46 2.0(5) . . . . ? C44 C45 C46 F46 -178.3(3) . . . . ? F45 C45 C46 C41 -178.6(3) . . . . ? C44 C45 C46 C41 1.1(6) . . . . ? C42 C41 C46 F46 177.7(3) . . . . ? B22 C41 C46 F46 -7.0(6) . . . . ? C42 C41 C46 C45 -1.7(5) . . . . ? B22 C41 C46 C45 173.7(4) . . . . ? N21 B22 C51 C56 124.6(4) . . . . ? C41 B22 C51 C56 -113.4(4) . . . . ? C31 B22 C51 C56 9.3(5) . . . . ? N21 B22 C51 C52 -54.3(4) . . . . ? C41 B22 C51 C52 67.7(4) . . . . ? C31 B22 C51 C52 -169.6(3) . . . . ? C56 C51 C52 F52 177.0(3) . . . . ? B22 C51 C52 F52 -3.9(5) . . . . ? C56 C51 C52 C53 -3.4(5) . . . . ? B22 C51 C52 C53 175.6(3) . . . . ? F52 C52 C53 F53 0.0(5) . . . . ? C51 C52 C53 F53 -179.5(3) . . . . ? F52 C52 C53 C54 -179.7(3) . . . . ? C51 C52 C53 C54 0.8(6) . . . . ? F53 C53 C54 F54 1.0(6) . . . . ? C52 C53 C54 F54 -179.3(3) . . . . ? F53 C53 C54 C55 -178.0(3) . . . . ? C52 C53 C54 C55 1.6(6) . . . . ? F54 C54 C55 F55 0.4(6) . . . . ? C53 C54 C55 F55 179.5(3) . . . . ? F54 C54 C55 C56 179.8(3) . . . . ? C53 C54 C55 C56 -1.1(6) . . . . ? F55 C55 C56 F56 -2.7(5) . . . . ? C54 C55 C56 F56 178.0(3) . . . . ? F55 C55 C56 C51 177.5(4) . . . . ? C54 C55 C56 C51 -1.9(6) . . . . ? C52 C51 C56 F56 -175.9(3) . . . . ? B22 C51 C56 F56 5.2(6) . . . . ? C52 C51 C56 C55 4.0(5) . . . . ? B22 C51 C56 C55 -175.0(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl72 0.91 2.79 3.568(4) 144.7 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.220 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.080 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 862684' #TrackingRef '- Fuller et al Ti nitrido.cif' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_formula_structural '[P(C6H5)4][{(C6F5)3BN}TiCl2{NH(CH3)2}2]' _chemical_name_common '[P(C6H5)4][{(C6F5)3BN}TiCl2{NH(CH3)2}2]' _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 P, C22 H14 B Cl2 F15 N3 Ti, C7 H8' _chemical_formula_sum 'C53 H42 B Cl2 F15 N3 P Ti' _chemical_formula_weight 1166.48 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5648(4) _cell_length_b 16.7568(8) _cell_length_c 16.9895(8) _cell_angle_alpha 100.283(4) _cell_angle_beta 97.544(4) _cell_angle_gamma 103.714(4) _cell_volume 2559.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 7542 _cell_measurement_theta_min 3.0914 _cell_measurement_theta_max 32.3277 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9581 _exptl_absorpt_correction_T_max 1.0334 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39544 _diffrn_reflns_av_R_equivalents 0.1214 _diffrn_reflns_av_sigmaI/netI 0.1087 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6669 _reflns_number_gt 4308 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0315P)^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 6669 _refine_ls_number_parameters 742 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.000 _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 0.24209(10) 0.36607(5) 0.86992(5) 0.0192(2) Uani 1 1 d . . . Cl2 Cl 0.35568(13) 0.30836(7) 0.96941(7) 0.0266(3) Uani 1 1 d . . . Cl3 Cl 0.20262(15) 0.49991(7) 0.86488(7) 0.0319(3) Uani 1 1 d . . . F33 F -0.3112(3) 0.27745(17) 0.59105(16) 0.0380(8) Uani 1 1 d . . . F34 F -0.4896(3) 0.12073(17) 0.57754(16) 0.0407(8) Uani 1 1 d . . . F35 F -0.3836(3) 0.00428(17) 0.63982(15) 0.0342(7) Uani 1 1 d . . . F36 F -0.1030(3) 0.03824(15) 0.70575(14) 0.0258(7) Uani 1 1 d . . . F42 F 0.3959(3) 0.13630(16) 0.72078(15) 0.0312(7) Uani 1 1 d . . . F43 F 0.4920(3) 0.05344(17) 0.82464(16) 0.0394(8) Uani 1 1 d . . . F44 F 0.3407(3) 0.00978(17) 0.94187(16) 0.0436(8) Uani 1 1 d . . . F45 F 0.0853(3) 0.05430(17) 0.95301(15) 0.0394(8) Uani 1 1 d . . . F46 F -0.0076(3) 0.14457(16) 0.85414(14) 0.0281(7) Uani 1 1 d . . . F52 F 0.1033(3) 0.05830(16) 0.60330(15) 0.0309(7) Uani 1 1 d . . . F53 F 0.1890(3) 0.04686(18) 0.46041(16) 0.0467(8) Uani 1 1 d . . . F54 F 0.3339(3) 0.18701(19) 0.41490(15) 0.0461(8) Uani 1 1 d . . . F55 F 0.3963(3) 0.33931(17) 0.51951(16) 0.0417(8) Uani 1 1 d . . . F56 F 0.3087(3) 0.35346(16) 0.66109(15) 0.0311(7) Uani 1 1 d . . . N1 N 0.4589(4) 0.4122(3) 0.8356(3) 0.0254(11) Uani 1 1 d . . . N11 N 0.0446(4) 0.3400(3) 0.9291(2) 0.0216(10) Uani 1 1 d . . . N21 N 0.1741(4) 0.2917(2) 0.7853(2) 0.0175(9) Uani 1 1 d . . . C2 C 0.5315(7) 0.3452(4) 0.8111(4) 0.0342(15) Uani 1 1 d . . . C3 C 0.5652(7) 0.4853(4) 0.8928(4) 0.0440(17) Uani 1 1 d . . . C12 C -0.0888(7) 0.3422(5) 0.8773(4) 0.0352(15) Uani 1 1 d . . . C13 C 0.0607(7) 0.3901(4) 1.0114(3) 0.0288(14) Uani 1 1 d . . . C31 C -0.0502(5) 0.1794(3) 0.6888(2) 0.0172(11) Uani 1 1 d . . . C33 C -0.2569(6) 0.2188(3) 0.6214(3) 0.0252(13) Uani 1 1 d . . . C34 C -0.3505(5) 0.1393(3) 0.6146(3) 0.0241(12) Uani 1 1 d . . . C35 C -0.2945(5) 0.0815(3) 0.6453(3) 0.0249(12) Uani 1 1 d . . . C36 C -0.1492(5) 0.1013(3) 0.6801(3) 0.0201(12) Uani 1 1 d . . . C41 C 0.1838(5) 0.1424(3) 0.7783(3) 0.0192(12) Uani 1 1 d . . . C42 C 0.3122(5) 0.1177(3) 0.7774(3) 0.0214(12) Uani 1 1 d . . . C43 C 0.3666(6) 0.0754(3) 0.8302(3) 0.0277(13) Uani 1 1 d . . . C44 C 0.2888(6) 0.0525(3) 0.8899(3) 0.0274(13) Uani 1 1 d . . . C45 C 0.1610(6) 0.0752(3) 0.8949(3) 0.0255(13) Uani 1 1 d . . . C46 C 0.1148(5) 0.1201(3) 0.8417(3) 0.0206(12) Uani 1 1 d . . . C51 C 0.1990(5) 0.2058(3) 0.6404(2) 0.0177(12) Uani 1 1 d . . . C52 C 0.1749(5) 0.1317(3) 0.5846(3) 0.0216(12) Uani 1 1 d . . . C53 C 0.2160(5) 0.1224(3) 0.5099(3) 0.0281(13) Uani 1 1 d . . . C54 C 0.2910(5) 0.1942(4) 0.4878(3) 0.0285(13) Uani 1 1 d . . . C55 C 0.3201(5) 0.2689(3) 0.5396(3) 0.0251(12) Uani 1 1 d . . . C56 C 0.2747(5) 0.2746(3) 0.6143(3) 0.0212(12) Uani 1 1 d . . . B22 B 0.1280(6) 0.2060(3) 0.7246(3) 0.0167(13) Uani 1 1 d . . . P1 P 0.03659(14) 0.24564(8) 0.21995(7) 0.0224(3) Uani 1 1 d . . . C61 C -0.0995(5) 0.2315(3) 0.1322(3) 0.0200(12) Uani 1 1 d . . . C62 C -0.2061(5) 0.2745(3) 0.1365(3) 0.0297(13) Uani 1 1 d . . . H62 H -0.2075 0.3094 0.1853 0.036 Uiso 1 1 calc R . . C63 C -0.3106(6) 0.2660(3) 0.0690(3) 0.0327(14) Uani 1 1 d . . . H63 H -0.3788 0.2974 0.0717 0.039 Uiso 1 1 calc R . . C64 C -0.3135(6) 0.2112(3) -0.0019(3) 0.0326(14) Uani 1 1 d . . . H64 H -0.3852 0.2046 -0.0470 0.039 Uiso 1 1 calc R . . C65 C -0.2114(6) 0.1660(3) -0.0068(3) 0.0337(14) Uani 1 1 d . . . H65 H -0.2150 0.1283 -0.0549 0.040 Uiso 1 1 calc R . . C66 C -0.1038(6) 0.1764(3) 0.0594(3) 0.0297(13) Uani 1 1 d . . . H66 H -0.0336 0.1466 0.0555 0.036 Uiso 1 1 calc R . . C71 C 0.1647(5) 0.1891(3) 0.1919(3) 0.0214(12) Uani 1 1 d . . . C72 C 0.1817(5) 0.1197(3) 0.2224(3) 0.0283(13) Uani 1 1 d . . . H72 H 0.1280 0.1027 0.2611 0.034 Uiso 1 1 calc R . . C73 C 0.2780(6) 0.0759(3) 0.1955(3) 0.0367(15) Uani 1 1 d . . . H73 H 0.2898 0.0298 0.2166 0.044 Uiso 1 1 calc R . . C74 C 0.3568(5) 0.1003(3) 0.1372(3) 0.0299(13) Uani 1 1 d . . . H74 H 0.4203 0.0701 0.1184 0.036 Uiso 1 1 calc R . . C75 C 0.3416(5) 0.1688(3) 0.1072(3) 0.0266(13) Uani 1 1 d . . . H75 H 0.3946 0.1850 0.0679 0.032 Uiso 1 1 calc R . . C76 C 0.2484(5) 0.2140(3) 0.1346(3) 0.0260(13) Uani 1 1 d . . . H76 H 0.2410 0.2615 0.1150 0.031 Uiso 1 1 calc R . . C81 C -0.0529(6) 0.2061(3) 0.2970(3) 0.0251(13) Uani 1 1 d . . . C82 C -0.0018(6) 0.2415(3) 0.3784(3) 0.0345(14) Uani 1 1 d . . . H82 H 0.0775 0.2891 0.3939 0.041 Uiso 1 1 calc R . . C83 C -0.0668(6) 0.2074(4) 0.4377(3) 0.0406(15) Uani 1 1 d . . . H83 H -0.0314 0.2317 0.4926 0.049 Uiso 1 1 calc R . . C84 C -0.1828(7) 0.1380(3) 0.4145(3) 0.0426(16) Uani 1 1 d . . . H84 H -0.2254 0.1141 0.4539 0.051 Uiso 1 1 calc R . . C85 C -0.2377(7) 0.1031(3) 0.3345(4) 0.0580(19) Uani 1 1 d . . . H85 H -0.3188 0.0566 0.3194 0.070 Uiso 1 1 calc R . . C86 C -0.1723(7) 0.1369(3) 0.2755(3) 0.0506(17) Uani 1 1 d . . . H86 H -0.2094 0.1127 0.2208 0.061 Uiso 1 1 calc R . . C91 C 0.1372(5) 0.3539(3) 0.2599(3) 0.0187(12) Uani 1 1 d . . . C92 C 0.2719(6) 0.3696(3) 0.3090(3) 0.0364(14) Uani 1 1 d . . . H92 H 0.3091 0.3247 0.3176 0.044 Uiso 1 1 calc R . . C93 C 0.3530(6) 0.4513(3) 0.3460(3) 0.0393(15) Uani 1 1 d . . . H93 H 0.4441 0.4613 0.3786 0.047 Uiso 1 1 calc R . . C94 C 0.2961(6) 0.5175(3) 0.3336(3) 0.0340(14) Uani 1 1 d . . . H94 H 0.3488 0.5724 0.3584 0.041 Uiso 1 1 calc R . . C95 C 0.1632(6) 0.5026(3) 0.2852(3) 0.0373(14) Uani 1 1 d . . . H95 H 0.1260 0.5478 0.2775 0.045 Uiso 1 1 calc R . . C96 C 0.0821(6) 0.4211(3) 0.2471(3) 0.0326(14) Uani 1 1 d . . . H96 H -0.0077 0.4117 0.2134 0.039 Uiso 1 1 calc R . . C101 C 0.8616(7) 0.5484(3) 0.4691(4) 0.0593(18) Uani 1 1 d . . . H10A H 0.9420 0.5727 0.4448 0.089 Uiso 1 1 calc R . . H10B H 0.8985 0.5394 0.5211 0.089 Uiso 1 1 calc R . . H10C H 0.8001 0.5860 0.4759 0.089 Uiso 1 1 calc R . . C102 C 0.7738(6) 0.4654(3) 0.4145(3) 0.0329(14) Uani 1 1 d . . . C103 C 0.7314(6) 0.3943(4) 0.4463(3) 0.0401(15) Uani 1 1 d . . . H103 H 0.7593 0.3977 0.5016 0.048 Uiso 1 1 calc R . . C104 C 0.6492(6) 0.3194(4) 0.3973(4) 0.0409(15) Uani 1 1 d . . . H104 H 0.6227 0.2724 0.4196 0.049 Uiso 1 1 calc R . . C105 C 0.6057(6) 0.3129(4) 0.3162(4) 0.0415(15) Uani 1 1 d . . . H105 H 0.5491 0.2619 0.2835 0.050 Uiso 1 1 calc R . . C106 C 0.6466(7) 0.3830(4) 0.2829(3) 0.0464(16) Uani 1 1 d . . . H106 H 0.6165 0.3797 0.2278 0.056 Uiso 1 1 calc R . . C107 C 0.7323(6) 0.4576(4) 0.3326(3) 0.0386(15) Uani 1 1 d . . . H107 H 0.7628 0.5039 0.3099 0.046 Uiso 1 1 calc R . . F32 F -0.0302(3) 0.31424(16) 0.65818(15) 0.0301(7) Uani 1 1 d . . . C32 C -0.1141(5) 0.2358(3) 0.6570(3) 0.0223(12) Uani 1 1 d . . . H1 H 0.435(4) 0.430(2) 0.793(2) 0.012(13) Uiso 1 1 d . . . H2A H 0.561(5) 0.326(3) 0.855(3) 0.029(15) Uiso 1 1 d . . . H2B H 0.619(6) 0.366(3) 0.788(3) 0.054(18) Uiso 1 1 d . . . H2C H 0.468(5) 0.303(3) 0.768(3) 0.018(14) Uiso 1 1 d . . . H3A H 0.658(6) 0.506(3) 0.870(3) 0.064(18) Uiso 1 1 d . . . H3B H 0.518(6) 0.531(3) 0.904(3) 0.050(18) Uiso 1 1 d . . . H3C H 0.604(5) 0.467(3) 0.946(3) 0.045(16) Uiso 1 1 d . . . H11 H 0.047(5) 0.290(3) 0.935(3) 0.034(16) Uiso 1 1 d . . . H12A H -0.085(5) 0.401(3) 0.871(2) 0.031(15) Uiso 1 1 d . . . H12B H -0.170(6) 0.329(3) 0.903(3) 0.040(16) Uiso 1 1 d . . . H12C H -0.104(5) 0.303(3) 0.827(3) 0.040(17) Uiso 1 1 d . . . H13A H -0.026(6) 0.378(3) 1.037(3) 0.039(15) Uiso 1 1 d . . . H13B H 0.074(5) 0.450(3) 1.011(2) 0.029(14) Uiso 1 1 d . . . H13C H 0.141(5) 0.380(3) 1.047(2) 0.028(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0165(6) 0.0173(6) 0.0228(5) 0.0054(4) 0.0047(4) 0.0009(4) Cl2 0.0239(8) 0.0278(8) 0.0277(8) 0.0099(6) 0.0015(6) 0.0047(6) Cl3 0.0394(9) 0.0198(8) 0.0399(8) 0.0107(6) 0.0128(7) 0.0082(6) F33 0.0311(19) 0.0383(19) 0.0499(19) 0.0182(15) 0.0009(14) 0.0163(15) F34 0.017(2) 0.057(2) 0.0466(19) 0.0140(15) 0.0001(15) 0.0063(15) F35 0.0199(18) 0.0310(19) 0.0445(18) 0.0096(14) 0.0056(14) -0.0077(15) F36 0.0218(17) 0.0196(17) 0.0345(17) 0.0084(13) 0.0046(13) 0.0013(13) F42 0.0263(18) 0.0394(19) 0.0349(17) 0.0145(14) 0.0115(14) 0.0140(15) F43 0.038(2) 0.041(2) 0.0437(19) 0.0084(14) 0.0008(15) 0.0238(16) F44 0.059(2) 0.038(2) 0.0381(18) 0.0190(15) 0.0004(16) 0.0196(17) F45 0.050(2) 0.040(2) 0.0307(18) 0.0190(15) 0.0140(15) 0.0059(16) F46 0.0252(18) 0.0303(18) 0.0319(17) 0.0103(13) 0.0117(14) 0.0072(14) F52 0.0292(19) 0.0238(18) 0.0346(17) 0.0000(13) 0.0121(14) -0.0013(14) F53 0.036(2) 0.045(2) 0.0433(19) -0.0147(16) 0.0145(15) -0.0042(16) F54 0.039(2) 0.069(2) 0.0233(17) 0.0013(15) 0.0153(15) 0.0021(17) F55 0.044(2) 0.042(2) 0.0421(19) 0.0208(15) 0.0214(15) 0.0016(16) F56 0.042(2) 0.0200(18) 0.0322(17) 0.0082(14) 0.0160(14) 0.0027(14) N1 0.019(3) 0.026(3) 0.027(3) 0.007(2) 0.002(2) 0.000(2) N11 0.022(3) 0.023(3) 0.022(3) 0.007(2) 0.006(2) 0.007(2) N21 0.013(2) 0.025(2) 0.017(2) 0.0088(18) 0.0077(17) 0.0039(18) C2 0.017(4) 0.044(4) 0.041(4) 0.014(4) 0.005(3) 0.006(3) C3 0.021(4) 0.049(5) 0.041(4) -0.009(3) 0.006(3) -0.018(3) C12 0.019(4) 0.053(5) 0.034(4) 0.009(4) 0.006(3) 0.011(3) C13 0.028(4) 0.029(4) 0.026(4) 0.002(3) 0.006(3) 0.002(3) C31 0.018(3) 0.015(3) 0.018(3) 0.004(2) 0.004(2) 0.004(2) C33 0.021(4) 0.037(4) 0.025(3) 0.012(3) 0.005(2) 0.016(3) C34 0.004(3) 0.041(4) 0.025(3) 0.005(2) -0.001(2) 0.004(3) C35 0.015(3) 0.029(3) 0.030(3) 0.011(3) 0.009(3) -0.001(3) C36 0.023(4) 0.023(3) 0.021(3) 0.009(2) 0.007(2) 0.013(3) C41 0.019(3) 0.017(3) 0.018(3) 0.000(2) 0.003(2) -0.001(2) C42 0.020(3) 0.020(3) 0.020(3) 0.000(2) 0.003(2) 0.000(3) C43 0.030(4) 0.022(3) 0.031(3) 0.000(3) -0.005(3) 0.018(3) C44 0.043(4) 0.018(3) 0.017(3) 0.002(2) -0.006(3) 0.009(3) C45 0.034(4) 0.020(3) 0.021(3) 0.004(2) 0.005(3) 0.005(3) C46 0.022(3) 0.015(3) 0.024(3) -0.002(2) 0.002(2) 0.009(2) C51 0.016(3) 0.023(3) 0.015(3) 0.005(2) -0.001(2) 0.009(2) C52 0.013(3) 0.025(3) 0.024(3) 0.007(3) 0.001(2) -0.001(2) C53 0.019(3) 0.032(4) 0.022(3) -0.013(3) -0.001(3) 0.001(3) C54 0.020(3) 0.044(4) 0.017(3) 0.001(3) 0.008(2) 0.004(3) C55 0.021(3) 0.029(4) 0.023(3) 0.011(3) 0.005(2) -0.005(3) C56 0.020(3) 0.019(3) 0.022(3) 0.000(2) -0.003(2) 0.007(2) B22 0.016(4) 0.011(3) 0.021(3) 0.001(3) 0.004(3) 0.002(3) P1 0.0215(9) 0.0200(8) 0.0264(8) 0.0070(6) 0.0090(6) 0.0031(6) C61 0.017(3) 0.017(3) 0.027(3) 0.007(2) 0.012(2) -0.001(2) C62 0.015(3) 0.027(3) 0.039(3) 0.000(2) 0.002(3) -0.003(3) C63 0.019(3) 0.030(4) 0.045(4) 0.004(3) 0.002(3) 0.003(3) C64 0.020(4) 0.041(4) 0.033(3) 0.010(3) 0.002(3) -0.001(3) C65 0.028(4) 0.037(4) 0.033(4) 0.002(3) 0.010(3) 0.004(3) C66 0.022(3) 0.035(4) 0.035(3) 0.009(3) 0.012(3) 0.008(3) C71 0.022(3) 0.020(3) 0.020(3) 0.006(2) 0.003(2) 0.001(2) C72 0.033(4) 0.024(3) 0.033(3) 0.015(2) 0.018(3) 0.006(3) C73 0.047(4) 0.032(4) 0.045(4) 0.021(3) 0.019(3) 0.022(3) C74 0.027(4) 0.036(4) 0.035(3) 0.011(3) 0.012(3) 0.017(3) C75 0.027(3) 0.028(3) 0.030(3) 0.012(3) 0.016(3) 0.008(3) C76 0.031(4) 0.022(3) 0.030(3) 0.011(2) 0.008(3) 0.011(3) C81 0.032(4) 0.021(3) 0.027(3) 0.011(2) 0.012(3) 0.008(3) C82 0.024(4) 0.043(4) 0.036(4) 0.016(3) 0.005(3) 0.002(3) C83 0.029(4) 0.067(5) 0.027(3) 0.017(3) 0.005(3) 0.009(3) C84 0.062(5) 0.034(4) 0.044(4) 0.016(3) 0.034(3) 0.015(3) C85 0.088(6) 0.023(4) 0.052(4) 0.000(3) 0.044(4) -0.018(3) C86 0.072(5) 0.034(4) 0.033(4) -0.001(3) 0.029(3) -0.015(3) C91 0.022(3) 0.014(3) 0.021(3) 0.006(2) 0.005(2) 0.003(2) C92 0.022(4) 0.030(4) 0.057(4) 0.008(3) 0.006(3) 0.008(3) C93 0.019(4) 0.035(4) 0.057(4) 0.002(3) 0.007(3) 0.001(3) C94 0.027(4) 0.021(3) 0.044(4) 0.001(3) 0.012(3) -0.011(3) C95 0.038(4) 0.023(4) 0.052(4) 0.008(3) 0.004(3) 0.012(3) C96 0.027(4) 0.028(4) 0.040(3) 0.009(3) 0.002(3) 0.003(3) C101 0.049(5) 0.048(4) 0.077(5) 0.020(4) 0.003(4) 0.004(3) C102 0.023(4) 0.039(4) 0.040(4) 0.016(3) 0.006(3) 0.008(3) C103 0.031(4) 0.046(4) 0.042(4) 0.012(3) 0.004(3) 0.007(3) C104 0.031(4) 0.041(4) 0.051(4) 0.016(3) 0.012(3) 0.005(3) C105 0.028(4) 0.038(4) 0.056(4) -0.003(3) 0.010(3) 0.014(3) C106 0.051(5) 0.066(5) 0.033(4) 0.011(4) 0.015(3) 0.031(4) C107 0.038(4) 0.046(4) 0.046(4) 0.022(3) 0.018(3) 0.023(3) F32 0.0267(19) 0.0234(18) 0.0395(18) 0.0120(13) 0.0024(14) 0.0034(14) C32 0.021(3) 0.024(3) 0.022(3) 0.007(2) 0.006(2) 0.003(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 N21 1.666(4) . ? Ti1 N1 2.227(4) . ? Ti1 N11 2.244(4) . ? Ti1 Cl2 2.3605(13) . ? Ti1 Cl3 2.3752(14) . ? F33 C33 1.362(5) . ? F34 C34 1.333(5) . ? F35 C35 1.350(5) . ? F36 C36 1.355(4) . ? F42 C42 1.362(5) . ? F43 C43 1.345(5) . ? F44 C44 1.348(5) . ? F45 C45 1.347(5) . ? F46 C46 1.358(5) . ? F52 C52 1.371(5) . ? F53 C53 1.336(5) . ? F54 C54 1.349(5) . ? F55 C55 1.358(5) . ? F56 C56 1.356(5) . ? N1 C2 1.482(7) . ? N1 C3 1.484(7) . ? N1 H1 0.85(4) . ? N11 C12 1.465(6) . ? N11 C13 1.465(6) . ? N11 H11 0.87(4) . ? N21 B22 1.539(6) . ? C2 H2A 0.91(4) . ? C2 H2B 0.98(5) . ? C2 H2C 0.94(4) . ? C3 H3A 1.02(6) . ? C3 H3B 0.98(5) . ? C3 H3C 1.06(4) . ? C12 H12A 1.01(4) . ? C12 H12B 0.94(5) . ? C12 H12C 0.94(5) . ? C13 H13A 0.99(5) . ? C13 H13B 0.98(4) . ? C13 H13C 0.98(4) . ? C31 C32 1.390(6) . ? C31 C36 1.391(6) . ? C31 B22 1.657(7) . ? C33 C32 1.360(6) . ? C33 C34 1.393(6) . ? C34 C35 1.361(6) . ? C35 C36 1.374(6) . ? C41 C42 1.386(6) . ? C41 C46 1.397(6) . ? C41 B22 1.657(6) . ? C42 C43 1.363(6) . ? C43 C44 1.390(7) . ? C44 C45 1.371(6) . ? C45 C46 1.368(6) . ? C51 C52 1.372(6) . ? C51 C56 1.386(6) . ? C51 B22 1.661(6) . ? C52 C53 1.371(6) . ? C53 C54 1.388(6) . ? C54 C55 1.341(6) . ? C55 C56 1.388(6) . ? P1 C71 1.780(5) . ? P1 C61 1.786(5) . ? P1 C81 1.794(5) . ? P1 C91 1.799(5) . ? C61 C62 1.382(6) . ? C61 C66 1.395(6) . ? C62 C63 1.380(6) . ? C62 H62 0.9300 . ? C63 C64 1.372(6) . ? C63 H63 0.9300 . ? C64 C65 1.372(6) . ? C64 H64 0.9300 . ? C65 C66 1.377(6) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 C72 1.388(6) . ? C71 C76 1.398(6) . ? C72 C73 1.381(6) . ? C72 H72 0.9300 . ? C73 C74 1.382(6) . ? C73 H73 0.9300 . ? C74 C75 1.367(6) . ? C74 H74 0.9300 . ? C75 C76 1.374(6) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C81 C86 1.376(7) . ? C81 C82 1.377(6) . ? C82 C83 1.390(6) . ? C82 H82 0.9300 . ? C83 C84 1.360(7) . ? C83 H83 0.9300 . ? C84 C85 1.359(7) . ? C84 H84 0.9300 . ? C85 C86 1.384(7) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C91 C92 1.380(6) . ? C91 C96 1.391(6) . ? C92 C93 1.391(7) . ? C92 H92 0.9300 . ? C93 C94 1.381(6) . ? C93 H93 0.9300 . ? C94 C95 1.363(6) . ? C94 H94 0.9300 . ? C95 C96 1.392(7) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? C101 C102 1.511(7) . ? C101 H10A 0.9600 . ? C101 H10B 0.9600 . ? C101 H10C 0.9600 . ? C102 C107 1.370(7) . ? C102 C103 1.390(6) . ? C103 C104 1.369(7) . ? C103 H103 0.9300 . ? C104 C105 1.362(7) . ? C104 H104 0.9300 . ? C105 C106 1.390(7) . ? C105 H105 0.9300 . ? C106 C107 1.379(8) . ? C106 H106 0.9300 . ? C107 H107 0.9300 . ? F32 C32 1.363(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 N21 Ti1 N1 95.10(16) . . ? N21 Ti1 N11 97.07(17) . . ? N1 Ti1 N11 167.81(16) . . ? N21 Ti1 Cl2 109.04(12) . . ? N1 Ti1 Cl2 89.08(12) . . ? N11 Ti1 Cl2 86.41(11) . . ? N21 Ti1 Cl3 115.68(12) . . ? N1 Ti1 Cl3 87.74(11) . . ? N11 Ti1 Cl3 87.50(12) . . ? Cl2 Ti1 Cl3 135.27(6) . . ? C2 N1 C3 110.0(5) . . ? C2 N1 Ti1 114.1(3) . . ? C3 N1 Ti1 117.1(3) . . ? C2 N1 H1 108(3) . . ? C3 N1 H1 105(3) . . ? Ti1 N1 H1 102(3) . . ? C12 N11 C13 111.0(5) . . ? C12 N11 Ti1 112.7(3) . . ? C13 N11 Ti1 115.7(3) . . ? C12 N11 H11 114(3) . . ? C13 N11 H11 106(3) . . ? Ti1 N11 H11 97(3) . . ? B22 N21 Ti1 161.9(3) . . ? N1 C2 H2A 110(3) . . ? N1 C2 H2B 112(3) . . ? H2A C2 H2B 107(4) . . ? N1 C2 H2C 109(3) . . ? H2A C2 H2C 114(4) . . ? H2B C2 H2C 105(4) . . ? N1 C3 H3A 112(3) . . ? N1 C3 H3B 109(3) . . ? H3A C3 H3B 110(4) . . ? N1 C3 H3C 110(3) . . ? H3A C3 H3C 104(4) . . ? H3B C3 H3C 113(4) . . ? N11 C12 H12A 111(3) . . ? N11 C12 H12B 110(3) . . ? H12A C12 H12B 102(4) . . ? N11 C12 H12C 110(3) . . ? H12A C12 H12C 114(4) . . ? H12B C12 H12C 110(4) . . ? N11 C13 H13A 115(3) . . ? N11 C13 H13B 111(2) . . ? H13A C13 H13B 102(3) . . ? N11 C13 H13C 109(2) . . ? H13A C13 H13C 107(4) . . ? H13B C13 H13C 113(4) . . ? C32 C31 C36 112.4(4) . . ? C32 C31 B22 120.1(4) . . ? C36 C31 B22 127.3(4) . . ? C32 C33 F33 121.5(5) . . ? C32 C33 C34 119.8(4) . . ? F33 C33 C34 118.7(4) . . ? F34 C34 C35 121.6(5) . . ? F34 C34 C33 120.5(4) . . ? C35 C34 C33 117.9(5) . . ? F35 C35 C34 118.9(4) . . ? F35 C35 C36 120.8(4) . . ? C34 C35 C36 120.3(5) . . ? F36 C36 C35 115.6(4) . . ? F36 C36 C31 119.8(4) . . ? C35 C36 C31 124.6(4) . . ? C42 C41 C46 112.0(4) . . ? C42 C41 B22 126.4(4) . . ? C46 C41 B22 120.6(4) . . ? F42 C42 C43 114.6(4) . . ? F42 C42 C41 119.9(4) . . ? C43 C42 C41 125.5(5) . . ? F43 C43 C42 121.6(5) . . ? F43 C43 C44 119.2(4) . . ? C42 C43 C44 119.2(5) . . ? F44 C44 C45 121.7(5) . . ? F44 C44 C43 119.7(5) . . ? C45 C44 C43 118.6(4) . . ? F45 C45 C46 121.4(4) . . ? F45 C45 C44 119.3(4) . . ? C46 C45 C44 119.3(5) . . ? F46 C46 C45 115.5(4) . . ? F46 C46 C41 119.3(4) . . ? C45 C46 C41 125.3(4) . . ? C52 C51 C56 112.5(4) . . ? C52 C51 B22 119.7(4) . . ? C56 C51 B22 127.6(4) . . ? C53 C52 F52 114.9(4) . . ? C53 C52 C51 126.4(5) . . ? F52 C52 C51 118.6(4) . . ? F53 C53 C52 121.7(5) . . ? F53 C53 C54 120.5(4) . . ? C52 C53 C54 117.8(5) . . ? C55 C54 F54 121.6(5) . . ? C55 C54 C53 119.2(5) . . ? F54 C54 C53 119.2(5) . . ? C54 C55 F55 119.8(4) . . ? C54 C55 C56 120.5(5) . . ? F55 C55 C56 119.7(4) . . ? F56 C56 C51 121.2(4) . . ? F56 C56 C55 115.2(4) . . ? C51 C56 C55 123.6(4) . . ? N21 B22 C31 110.4(4) . . ? N21 B22 C41 103.3(3) . . ? C31 B22 C41 114.9(4) . . ? N21 B22 C51 114.3(4) . . ? C31 B22 C51 102.5(3) . . ? C41 B22 C51 111.7(4) . . ? C71 P1 C61 108.3(2) . . ? C71 P1 C81 111.0(2) . . ? C61 P1 C81 108.1(2) . . ? C71 P1 C91 107.3(2) . . ? C61 P1 C91 113.2(2) . . ? C81 P1 C91 109.0(2) . . ? C62 C61 C66 118.6(4) . . ? C62 C61 P1 119.7(4) . . ? C66 C61 P1 121.7(4) . . ? C63 C62 C61 120.8(5) . . ? C63 C62 H62 119.6 . . ? C61 C62 H62 119.6 . . ? C64 C63 C62 119.7(5) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C65 120.4(5) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C64 C65 C66 120.0(5) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 120.4(5) . . ? C65 C66 H66 119.8 . . ? C61 C66 H66 119.8 . . ? C72 C71 C76 118.6(4) . . ? C72 C71 P1 123.0(4) . . ? C76 C71 P1 118.4(3) . . ? C73 C72 C71 120.4(4) . . ? C73 C72 H72 119.8 . . ? C71 C72 H72 119.8 . . ? C72 C73 C74 120.0(4) . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C75 C74 C73 120.1(4) . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.5(4) . . ? C74 C75 H75 119.8 . . ? C76 C75 H75 119.8 . . ? C75 C76 C71 120.4(4) . . ? C75 C76 H76 119.8 . . ? C71 C76 H76 119.8 . . ? C86 C81 C82 118.4(4) . . ? C86 C81 P1 120.1(4) . . ? C82 C81 P1 121.5(4) . . ? C81 C82 C83 121.1(5) . . ? C81 C82 H82 119.5 . . ? C83 C82 H82 119.5 . . ? C84 C83 C82 119.1(5) . . ? C84 C83 H83 120.5 . . ? C82 C83 H83 120.5 . . ? C85 C84 C83 121.0(5) . . ? C85 C84 H84 119.5 . . ? C83 C84 H84 119.5 . . ? C84 C85 C86 119.8(6) . . ? C84 C85 H85 120.1 . . ? C86 C85 H85 120.1 . . ? C81 C86 C85 120.6(5) . . ? C81 C86 H86 119.7 . . ? C85 C86 H86 119.7 . . ? C92 C91 C96 119.3(5) . . ? C92 C91 P1 117.5(3) . . ? C96 C91 P1 123.1(4) . . ? C91 C92 C93 121.2(5) . . ? C91 C92 H92 119.4 . . ? C93 C92 H92 119.4 . . ? C94 C93 C92 119.0(5) . . ? C94 C93 H93 120.5 . . ? C92 C93 H93 120.5 . . ? C95 C94 C93 120.4(5) . . ? C95 C94 H94 119.8 . . ? C93 C94 H94 119.8 . . ? C94 C95 C96 121.1(5) . . ? C94 C95 H95 119.5 . . ? C96 C95 H95 119.5 . . ? C91 C96 C95 119.2(5) . . ? C91 C96 H96 120.4 . . ? C95 C96 H96 120.4 . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C107 C102 C103 117.9(5) . . ? C107 C102 C101 121.4(5) . . ? C103 C102 C101 120.8(5) . . ? C104 C103 C102 120.8(5) . . ? C104 C103 H103 119.6 . . ? C102 C103 H103 119.6 . . ? C105 C104 C103 120.8(5) . . ? C105 C104 H104 119.6 . . ? C103 C104 H104 119.6 . . ? C104 C105 C106 119.5(5) . . ? C104 C105 H105 120.3 . . ? C106 C105 H105 120.3 . . ? C107 C106 C105 119.2(5) . . ? C107 C106 H106 120.4 . . ? C105 C106 H106 120.4 . . ? C102 C107 C106 121.8(5) . . ? C102 C107 H107 119.1 . . ? C106 C107 H107 119.1 . . ? C33 C32 F32 115.4(4) . . ? C33 C32 C31 125.0(5) . . ? F32 C32 C31 119.5(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 N21 Ti1 N1 C2 -52.0(4) . . . . ? N11 Ti1 N1 C2 125.3(7) . . . . ? Cl2 Ti1 N1 C2 57.1(4) . . . . ? Cl3 Ti1 N1 C2 -167.6(4) . . . . ? N21 Ti1 N1 C3 177.5(4) . . . . ? N11 Ti1 N1 C3 -5.2(10) . . . . ? Cl2 Ti1 N1 C3 -73.4(4) . . . . ? Cl3 Ti1 N1 C3 61.9(4) . . . . ? N21 Ti1 N11 C12 -54.6(4) . . . . ? N1 Ti1 N11 C12 128.1(8) . . . . ? Cl2 Ti1 N11 C12 -163.4(4) . . . . ? Cl3 Ti1 N11 C12 61.0(4) . . . . ? N21 Ti1 N11 C13 176.1(4) . . . . ? N1 Ti1 N11 C13 -1.2(10) . . . . ? Cl2 Ti1 N11 C13 67.3(4) . . . . ? Cl3 Ti1 N11 C13 -68.3(4) . . . . ? N1 Ti1 N21 B22 95.8(10) . . . . ? N11 Ti1 N21 B22 -83.7(10) . . . . ? Cl2 Ti1 N21 B22 5.0(11) . . . . ? Cl3 Ti1 N21 B22 -174.3(10) . . . . ? C32 C33 C34 F34 -177.8(4) . . . . ? F33 C33 C34 F34 1.5(6) . . . . ? C32 C33 C34 C35 0.8(7) . . . . ? F33 C33 C34 C35 -179.9(4) . . . . ? F34 C34 C35 F35 -1.8(7) . . . . ? C33 C34 C35 F35 179.6(4) . . . . ? F34 C34 C35 C36 177.3(4) . . . . ? C33 C34 C35 C36 -1.3(7) . . . . ? F35 C35 C36 F36 1.7(6) . . . . ? C34 C35 C36 F36 -177.3(4) . . . . ? F35 C35 C36 C31 -179.5(4) . . . . ? C34 C35 C36 C31 1.5(7) . . . . ? C32 C31 C36 F36 177.9(4) . . . . ? B22 C31 C36 F36 3.1(7) . . . . ? C32 C31 C36 C35 -0.9(6) . . . . ? B22 C31 C36 C35 -175.7(4) . . . . ? C46 C41 C42 F42 -178.3(4) . . . . ? B22 C41 C42 F42 -9.5(7) . . . . ? C46 C41 C42 C43 1.1(7) . . . . ? B22 C41 C42 C43 169.9(5) . . . . ? F42 C42 C43 F43 -1.0(7) . . . . ? C41 C42 C43 F43 179.6(4) . . . . ? F42 C42 C43 C44 -179.3(4) . . . . ? C41 C42 C43 C44 1.3(8) . . . . ? F43 C43 C44 F44 0.8(7) . . . . ? C42 C43 C44 F44 179.2(4) . . . . ? F43 C43 C44 C45 -179.9(4) . . . . ? C42 C43 C44 C45 -1.5(7) . . . . ? F44 C44 C45 F45 0.0(7) . . . . ? C43 C44 C45 F45 -179.3(4) . . . . ? F44 C44 C45 C46 178.6(4) . . . . ? C43 C44 C45 C46 -0.7(7) . . . . ? F45 C45 C46 F46 2.6(7) . . . . ? C44 C45 C46 F46 -176.0(4) . . . . ? F45 C45 C46 C41 -178.0(4) . . . . ? C44 C45 C46 C41 3.4(8) . . . . ? C42 C41 C46 F46 175.9(4) . . . . ? B22 C41 C46 F46 6.3(7) . . . . ? C42 C41 C46 C45 -3.5(7) . . . . ? B22 C41 C46 C45 -173.0(4) . . . . ? C56 C51 C52 C53 -1.0(7) . . . . ? B22 C51 C52 C53 174.5(4) . . . . ? C56 C51 C52 F52 178.8(4) . . . . ? B22 C51 C52 F52 -5.7(6) . . . . ? F52 C52 C53 F53 -0.8(6) . . . . ? C51 C52 C53 F53 179.0(4) . . . . ? F52 C52 C53 C54 -179.1(4) . . . . ? C51 C52 C53 C54 0.8(7) . . . . ? F53 C53 C54 C55 -178.2(4) . . . . ? C52 C53 C54 C55 0.1(7) . . . . ? F53 C53 C54 F54 1.2(7) . . . . ? C52 C53 C54 F54 179.5(4) . . . . ? F54 C54 C55 F55 -0.9(7) . . . . ? C53 C54 C55 F55 178.4(4) . . . . ? F54 C54 C55 C56 -180.0(4) . . . . ? C53 C54 C55 C56 -0.6(7) . . . . ? C52 C51 C56 F56 179.9(4) . . . . ? B22 C51 C56 F56 4.8(7) . . . . ? C52 C51 C56 C55 0.4(6) . . . . ? B22 C51 C56 C55 -174.6(4) . . . . ? C54 C55 C56 F56 -179.2(4) . . . . ? F55 C55 C56 F56 1.8(6) . . . . ? C54 C55 C56 C51 0.4(7) . . . . ? F55 C55 C56 C51 -178.7(4) . . . . ? Ti1 N21 B22 C31 122.2(9) . . . . ? Ti1 N21 B22 C41 -1.2(12) . . . . ? Ti1 N21 B22 C51 -122.8(9) . . . . ? C32 C31 B22 N21 51.0(5) . . . . ? C36 C31 B22 N21 -134.6(4) . . . . ? C32 C31 B22 C41 167.4(4) . . . . ? C36 C31 B22 C41 -18.2(6) . . . . ? C32 C31 B22 C51 -71.2(5) . . . . ? C36 C31 B22 C51 103.2(5) . . . . ? C42 C41 B22 N21 -98.1(5) . . . . ? C46 C41 B22 N21 69.8(5) . . . . ? C42 C41 B22 C31 141.6(5) . . . . ? C46 C41 B22 C31 -50.5(6) . . . . ? C42 C41 B22 C51 25.3(6) . . . . ? C46 C41 B22 C51 -166.8(4) . . . . ? C52 C51 B22 N21 175.0(4) . . . . ? C56 C51 B22 N21 -10.2(6) . . . . ? C52 C51 B22 C31 -65.5(5) . . . . ? C56 C51 B22 C31 109.3(5) . . . . ? C52 C51 B22 C41 58.1(5) . . . . ? C56 C51 B22 C41 -127.1(5) . . . . ? C71 P1 C61 C62 -175.2(4) . . . . ? C81 P1 C61 C62 64.5(4) . . . . ? C91 P1 C61 C62 -56.3(4) . . . . ? C71 P1 C61 C66 6.4(4) . . . . ? C81 P1 C61 C66 -113.9(4) . . . . ? C91 P1 C61 C66 125.3(4) . . . . ? C66 C61 C62 C63 -3.0(7) . . . . ? P1 C61 C62 C63 178.6(4) . . . . ? C61 C62 C63 C64 3.3(7) . . . . ? C62 C63 C64 C65 -1.3(7) . . . . ? C63 C64 C65 C66 -1.0(7) . . . . ? C64 C65 C66 C61 1.3(7) . . . . ? C62 C61 C66 C65 0.6(7) . . . . ? P1 C61 C66 C65 179.0(4) . . . . ? C61 P1 C71 C72 -113.9(4) . . . . ? C81 P1 C71 C72 4.6(5) . . . . ? C91 P1 C71 C72 123.6(4) . . . . ? C61 P1 C71 C76 63.9(4) . . . . ? C81 P1 C71 C76 -177.6(4) . . . . ? C91 P1 C71 C76 -58.6(4) . . . . ? C76 C71 C72 C73 -0.9(7) . . . . ? P1 C71 C72 C73 176.9(4) . . . . ? C71 C72 C73 C74 -0.8(8) . . . . ? C72 C73 C74 C75 1.1(8) . . . . ? C73 C74 C75 C76 0.2(8) . . . . ? C74 C75 C76 C71 -1.9(8) . . . . ? C72 C71 C76 C75 2.2(7) . . . . ? P1 C71 C76 C75 -175.7(4) . . . . ? C71 P1 C81 C86 -83.7(5) . . . . ? C61 P1 C81 C86 35.0(5) . . . . ? C91 P1 C81 C86 158.4(4) . . . . ? C71 P1 C81 C82 93.9(4) . . . . ? C61 P1 C81 C82 -147.4(4) . . . . ? C91 P1 C81 C82 -24.0(5) . . . . ? C86 C81 C82 C83 1.4(8) . . . . ? P1 C81 C82 C83 -176.2(4) . . . . ? C81 C82 C83 C84 -0.2(8) . . . . ? C82 C83 C84 C85 -1.5(9) . . . . ? C83 C84 C85 C86 1.9(9) . . . . ? C82 C81 C86 C85 -1.1(8) . . . . ? P1 C81 C86 C85 176.6(4) . . . . ? C84 C85 C86 C81 -0.5(9) . . . . ? C71 P1 C91 C92 -40.0(4) . . . . ? C61 P1 C91 C92 -159.5(4) . . . . ? C81 P1 C91 C92 80.2(4) . . . . ? C71 P1 C91 C96 143.5(4) . . . . ? C61 P1 C91 C96 24.1(4) . . . . ? C81 P1 C91 C96 -96.2(4) . . . . ? C96 C91 C92 C93 0.2(7) . . . . ? P1 C91 C92 C93 -176.4(4) . . . . ? C91 C92 C93 C94 0.7(8) . . . . ? C92 C93 C94 C95 -0.6(8) . . . . ? C93 C94 C95 C96 -0.2(8) . . . . ? C92 C91 C96 C95 -1.0(7) . . . . ? P1 C91 C96 C95 175.3(4) . . . . ? C94 C95 C96 C91 1.1(8) . . . . ? C107 C102 C103 C104 -0.9(8) . . . . ? C101 C102 C103 C104 178.6(5) . . . . ? C102 C103 C104 C105 -0.6(8) . . . . ? C103 C104 C105 C106 0.6(8) . . . . ? C104 C105 C106 C107 0.9(8) . . . . ? C103 C102 C107 C106 2.4(8) . . . . ? C101 C102 C107 C106 -177.0(5) . . . . ? C105 C106 C107 C102 -2.5(8) . . . . ? F33 C33 C32 F32 -1.5(6) . . . . ? C34 C33 C32 F32 177.8(4) . . . . ? F33 C33 C32 C31 -179.6(4) . . . . ? C34 C33 C32 C31 -0.3(7) . . . . ? C36 C31 C32 C33 0.3(6) . . . . ? B22 C31 C32 C33 175.5(4) . . . . ? C36 C31 C32 F32 -177.7(4) . . . . ? B22 C31 C32 F32 -2.5(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 F56 0.85(4) 2.39(4) 2.998(5) 129(3) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.413 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.055 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 862685' #TrackingRef '- Fuller et al Ti nitrido.cif' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_formula_structural ; [P(C6H5)3{CH2(C6H5)}][{(C6F5)3BN}TiCl2{NH(CH3)2}] ; _chemical_name_common ; [P(C6H5)3{CH2(C6H5)}][{(C6F5)3BN}TiCl2{NH(CH3)2}] ; _chemical_melting_point ? _chemical_formula_moiety 'C25 H22 P, C22 H14 B Cl2 F15 N3 Ti' _chemical_formula_sum 'C47 H36 B Cl2 F15 N3 P Ti' _chemical_formula_weight 1088.37 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7400(3) _cell_length_b 12.8773(3) _cell_length_c 16.3677(4) _cell_angle_alpha 104.704(2) _cell_angle_beta 92.609(2) _cell_angle_gamma 99.717(2) _cell_volume 2348.93(10) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 10654 _cell_measurement_theta_min 3.1613 _cell_measurement_theta_max 32.1308 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9761 _exptl_absorpt_correction_T_max 1.0249 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23726 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10645 _reflns_number_gt 7434 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0426P)^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 10645 _refine_ls_number_parameters 695 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.04744(3) 0.54018(3) 0.26275(2) 0.01847(9) Uani 1 1 d . . . Cl2 Cl -0.07295(5) 0.40802(4) 0.31606(4) 0.02811(13) Uani 1 1 d . . . Cl3 Cl 0.03411(5) 0.68280(4) 0.19704(4) 0.03105(13) Uani 1 1 d . . . N1 N 0.03335(18) 0.66366(15) 0.38368(12) 0.0316(5) Uani 1 1 d . . . C2 C 0.0791(3) 0.6421(2) 0.46141(18) 0.0450(7) Uani 1 1 d . . . C3 C -0.0847(3) 0.6893(3) 0.3919(2) 0.0565(9) Uani 1 1 d . . . N11 N -0.00490(15) 0.42429(14) 0.13646(11) 0.0222(4) Uani 1 1 d . . . C12 C -0.1251(2) 0.4208(2) 0.10333(17) 0.0321(5) Uani 1 1 d . . . C13 C 0.0770(2) 0.43426(19) 0.07184(15) 0.0270(5) Uani 1 1 d . . . N21 N 0.18826(14) 0.53223(12) 0.27255(10) 0.0182(4) Uani 1 1 d . . . B22 B 0.31849(19) 0.53622(17) 0.26833(14) 0.0174(5) Uani 1 1 d . . . F32 F 0.25106(11) 0.45099(10) 0.41073(8) 0.0332(3) Uani 1 1 d . . . F33 F 0.34077(14) 0.52113(12) 0.57131(9) 0.0489(4) Uani 1 1 d . . . F34 F 0.53302(15) 0.68367(12) 0.61795(8) 0.0536(4) Uani 1 1 d . . . F35 F 0.63220(12) 0.77140(11) 0.49817(9) 0.0434(4) Uani 1 1 d . . . F36 F 0.54117(10) 0.71004(9) 0.34024(8) 0.0283(3) Uani 1 1 d . . . F42 F 0.32423(10) 0.77125(8) 0.31795(7) 0.0260(3) Uani 1 1 d . . . F43 F 0.38432(11) 0.91459(9) 0.22863(8) 0.0332(3) Uani 1 1 d . . . F44 F 0.44776(11) 0.84779(10) 0.06827(9) 0.0376(3) Uani 1 1 d . . . F45 F 0.43619(12) 0.62958(11) -0.00366(8) 0.0371(3) Uani 1 1 d . . . F46 F 0.38358(11) 0.48592(9) 0.08478(7) 0.0289(3) Uani 1 1 d . . . F52 F 0.16445(10) 0.30782(9) 0.21519(8) 0.0299(3) Uani 1 1 d . . . F53 F 0.23598(11) 0.12127(9) 0.15820(9) 0.0392(4) Uani 1 1 d . . . F54 F 0.46542(12) 0.11668(9) 0.14115(9) 0.0403(4) Uani 1 1 d . . . F55 F 0.62146(11) 0.30779(10) 0.18150(10) 0.0421(4) Uani 1 1 d . . . F56 F 0.55158(10) 0.49778(9) 0.23822(9) 0.0335(3) Uani 1 1 d . . . C31 C 0.38579(18) 0.57976(15) 0.36598(13) 0.0208(4) Uani 1 1 d . . . C32 C 0.3430(2) 0.53452(16) 0.42964(14) 0.0264(5) Uani 1 1 d . . . C33 C 0.3886(2) 0.56832(18) 0.51326(14) 0.0327(5) Uani 1 1 d . . . C34 C 0.4861(2) 0.64897(19) 0.53705(14) 0.0358(6) Uani 1 1 d . . . C35 C 0.5354(2) 0.69298(17) 0.47642(15) 0.0298(5) Uani 1 1 d . . . C36 C 0.48563(18) 0.65935(16) 0.39395(13) 0.0230(5) Uani 1 1 d . . . C41 C 0.35707(16) 0.62078(14) 0.20877(12) 0.0175(4) Uani 1 1 d . . . C42 C 0.35448(17) 0.73134(15) 0.23837(12) 0.0185(4) Uani 1 1 d . . . C43 C 0.38450(17) 0.80743(15) 0.19389(14) 0.0226(5) Uani 1 1 d . . . C44 C 0.41504(18) 0.77431(17) 0.11236(14) 0.0250(5) Uani 1 1 d . . . C45 C 0.41121(18) 0.66485(17) 0.07690(13) 0.0242(5) Uani 1 1 d . . . C46 C 0.38338(17) 0.59197(15) 0.12545(13) 0.0195(4) Uani 1 1 d . . . C51 C 0.35431(17) 0.41480(14) 0.22974(12) 0.0171(4) Uani 1 1 d . . . C52 C 0.27961(17) 0.31474(15) 0.20841(13) 0.0199(4) Uani 1 1 d . . . C53 C 0.31464(18) 0.21518(15) 0.17842(14) 0.0245(5) Uani 1 1 d . . . C54 C 0.42955(19) 0.21264(15) 0.16951(14) 0.0258(5) Uani 1 1 d . . . C55 C 0.50810(18) 0.30898(17) 0.18981(14) 0.0261(5) Uani 1 1 d . . . C56 C 0.46975(18) 0.40570(15) 0.21948(14) 0.0225(5) Uani 1 1 d . . . P1 P 0.81082(4) 1.03062(4) 0.25218(3) 0.01649(11) Uani 1 1 d . . . C61 C 0.78257(19) 1.12969(17) 0.19610(14) 0.0218(4) Uani 1 1 d . . . C62 C 0.83553(18) 1.12590(14) 0.11350(13) 0.0206(4) Uani 1 1 d . . . C63 C 0.7644(2) 1.10908(16) 0.03934(14) 0.0282(5) Uani 1 1 d . . . H63 H 0.6842 1.0970 0.0404 0.034 Uiso 1 1 calc R . . C64 C 0.8125(2) 1.11026(18) -0.03616(15) 0.0358(6) Uani 1 1 d . . . H64 H 0.7643 1.0986 -0.0856 0.043 Uiso 1 1 calc R . . C65 C 0.9314(2) 1.12866(17) -0.03862(15) 0.0343(6) Uani 1 1 d . . . H65 H 0.9634 1.1311 -0.0892 0.041 Uiso 1 1 calc R . . C66 C 1.0021(2) 1.14341(17) 0.03421(14) 0.0312(5) Uani 1 1 d . . . H66 H 1.0823 1.1542 0.0326 0.037 Uiso 1 1 calc R . . C67 C 0.95473(18) 1.14224(15) 0.11010(13) 0.0238(5) Uani 1 1 d . . . H67 H 1.0033 1.1525 0.1591 0.029 Uiso 1 1 calc R . . C71 C 0.96198(16) 1.04847(15) 0.28476(12) 0.0169(4) Uani 1 1 d . . . C72 C 1.01610(17) 0.95864(15) 0.27190(13) 0.0197(4) Uani 1 1 d . . . H72 H 0.9746 0.8893 0.2446 0.024 Uiso 1 1 calc R . . C73 C 1.13210(18) 0.97264(17) 0.29988(14) 0.0284(5) Uani 1 1 d . . . H73 H 1.1691 0.9128 0.2912 0.034 Uiso 1 1 calc R . . C74 C 1.19292(19) 1.07642(18) 0.34100(15) 0.0338(6) Uani 1 1 d . . . H74 H 1.2708 1.0857 0.3600 0.041 Uiso 1 1 calc R . . C75 C 1.13945(19) 1.16581(17) 0.35397(14) 0.0291(5) Uani 1 1 d . . . H75 H 1.1813 1.2349 0.3815 0.035 Uiso 1 1 calc R . . C76 C 1.02416(18) 1.15331(15) 0.32625(13) 0.0219(4) Uani 1 1 d . . . H76 H 0.9879 1.2136 0.3349 0.026 Uiso 1 1 calc R . . C81 C 0.75866(16) 0.89204(15) 0.19135(13) 0.0182(4) Uani 1 1 d . . . C82 C 0.75346(19) 0.86046(16) 0.10342(13) 0.0262(5) Uani 1 1 d . . . H82 H 0.7727 0.9124 0.0735 0.031 Uiso 1 1 calc R . . C83 C 0.7195(2) 0.75107(16) 0.06053(14) 0.0296(5) Uani 1 1 d . . . H83 H 0.7145 0.7299 0.0016 0.035 Uiso 1 1 calc R . . C84 C 0.69308(18) 0.67352(16) 0.10468(14) 0.0260(5) Uani 1 1 d . . . H84 H 0.6715 0.6001 0.0755 0.031 Uiso 1 1 calc R . . C85 C 0.69856(19) 0.70458(16) 0.19162(14) 0.0302(5) Uani 1 1 d . . . H85 H 0.6812 0.6520 0.2212 0.036 Uiso 1 1 calc R . . C86 C 0.72980(19) 0.81368(16) 0.23547(14) 0.0263(5) Uani 1 1 d . . . H86 H 0.7315 0.8345 0.2943 0.032 Uiso 1 1 calc R . . C91 C 0.73483(17) 1.05560(15) 0.34575(13) 0.0207(4) Uani 1 1 d . . . C92 C 0.7891(2) 1.06542(17) 0.42508(14) 0.0290(5) Uani 1 1 d . . . H92 H 0.8666 1.0587 0.4306 0.035 Uiso 1 1 calc R . . C93 C 0.7283(2) 1.08515(18) 0.49597(15) 0.0347(6) Uani 1 1 d . . . H93 H 0.7650 1.0921 0.5491 0.042 Uiso 1 1 calc R . . C94 C 0.6135(2) 1.09453(17) 0.48828(15) 0.0335(6) Uani 1 1 d . . . H94 H 0.5731 1.1088 0.5363 0.040 Uiso 1 1 calc R . . C95 C 0.5587(2) 1.08282(19) 0.40982(16) 0.0365(6) Uani 1 1 d . . . H95 H 0.4806 1.0876 0.4048 0.044 Uiso 1 1 calc R . . C96 C 0.61810(19) 1.06395(17) 0.33830(15) 0.0291(5) Uani 1 1 d . . . H96 H 0.5805 1.0568 0.2854 0.035 Uiso 1 1 calc R . . H1 H 0.083(2) 0.726(2) 0.3748(16) 0.048(8) Uiso 1 1 d . . . H2A H 0.151(3) 0.633(3) 0.457(2) 0.096(14) Uiso 1 1 d . . . H2B H 0.032(2) 0.575(2) 0.4698(18) 0.064(9) Uiso 1 1 d . . . H2C H 0.078(2) 0.702(2) 0.5121(19) 0.059(8) Uiso 1 1 d . . . H3A H -0.077(3) 0.754(3) 0.447(2) 0.078(10) Uiso 1 1 d . . . H3B H -0.127(3) 0.628(3) 0.402(2) 0.069(11) Uiso 1 1 d . . . H3C H -0.114(3) 0.709(3) 0.338(2) 0.081(11) Uiso 1 1 d . . . H11 H -0.0031(18) 0.3624(17) 0.1479(13) 0.021(6) Uiso 1 1 d . . . H12A H -0.181(2) 0.4058(19) 0.1441(16) 0.044(7) Uiso 1 1 d . . . H12B H -0.1320(18) 0.4910(17) 0.0940(13) 0.024(6) Uiso 1 1 d . . . H12C H -0.146(2) 0.3661(19) 0.0501(16) 0.040(7) Uiso 1 1 d . . . H13A H 0.152(2) 0.4234(17) 0.0926(15) 0.034(6) Uiso 1 1 d . . . H13B H 0.086(2) 0.5077(19) 0.0620(15) 0.035(6) Uiso 1 1 d . . . H13C H 0.0474(19) 0.3803(17) 0.0142(15) 0.029(6) Uiso 1 1 d . . . H61A H 0.806(2) 1.1992(19) 0.2376(15) 0.038(7) Uiso 1 1 d . . . H61B H 0.701(2) 1.1194(17) 0.1908(14) 0.028(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.02091(19) 0.01439(17) 0.0208(2) 0.00442(14) 0.00415(15) 0.00493(14) Cl2 0.0311(3) 0.0230(2) 0.0313(3) 0.0100(2) 0.0089(2) 0.0021(2) Cl3 0.0441(3) 0.0185(2) 0.0338(3) 0.0101(2) 0.0030(3) 0.0103(2) N1 0.0431(12) 0.0239(10) 0.0286(12) 0.0045(8) 0.0123(10) 0.0097(9) C2 0.068(2) 0.0384(15) 0.0262(15) -0.0003(12) 0.0014(14) 0.0194(15) C3 0.065(2) 0.066(2) 0.046(2) 0.0071(17) 0.0232(17) 0.0416(19) N11 0.0243(9) 0.0189(9) 0.0245(10) 0.0081(7) 0.0000(8) 0.0044(7) C12 0.0264(12) 0.0334(13) 0.0334(15) 0.0074(11) -0.0052(11) 0.0012(10) C13 0.0326(13) 0.0285(12) 0.0206(12) 0.0052(10) 0.0036(10) 0.0093(10) N21 0.0215(9) 0.0161(8) 0.0164(9) 0.0034(6) 0.0017(7) 0.0032(7) B22 0.0198(11) 0.0157(10) 0.0157(12) 0.0036(9) 0.0000(9) 0.0022(9) F32 0.0408(8) 0.0303(7) 0.0321(8) 0.0162(6) 0.0067(6) 0.0034(6) F33 0.0761(11) 0.0569(9) 0.0264(8) 0.0246(7) 0.0116(8) 0.0245(8) F34 0.0787(12) 0.0631(10) 0.0177(8) 0.0031(7) -0.0169(7) 0.0268(9) F35 0.0368(8) 0.0433(8) 0.0379(9) -0.0048(6) -0.0186(7) 0.0032(6) F36 0.0255(7) 0.0290(6) 0.0265(7) 0.0053(5) -0.0020(5) -0.0017(5) F42 0.0362(7) 0.0202(6) 0.0195(7) -0.0004(5) 0.0030(5) 0.0081(5) F43 0.0377(8) 0.0164(6) 0.0458(9) 0.0099(5) -0.0004(6) 0.0048(5) F44 0.0352(7) 0.0444(8) 0.0469(9) 0.0345(7) 0.0094(7) 0.0092(6) F45 0.0453(8) 0.0540(8) 0.0205(7) 0.0162(6) 0.0140(6) 0.0202(7) F46 0.0425(8) 0.0244(6) 0.0186(7) 0.0000(5) 0.0050(6) 0.0115(5) F52 0.0191(6) 0.0192(6) 0.0481(8) 0.0049(5) 0.0010(6) 0.0013(5) F53 0.0353(8) 0.0158(6) 0.0583(10) -0.0011(6) -0.0020(7) 0.0002(5) F54 0.0422(8) 0.0221(6) 0.0579(10) 0.0050(6) 0.0100(7) 0.0172(6) F55 0.0248(7) 0.0345(7) 0.0734(11) 0.0179(7) 0.0157(7) 0.0144(6) F56 0.0206(6) 0.0225(6) 0.0565(9) 0.0104(6) 0.0063(6) 0.0009(5) C31 0.0255(11) 0.0186(9) 0.0179(11) 0.0023(8) 0.0001(9) 0.0078(8) C32 0.0335(12) 0.0222(10) 0.0261(13) 0.0080(9) 0.0033(10) 0.0095(9) C33 0.0506(15) 0.0356(12) 0.0201(13) 0.0126(10) 0.0056(11) 0.0220(11) C34 0.0531(16) 0.0390(13) 0.0166(12) 0.0016(10) -0.0088(11) 0.0237(12) C35 0.0328(13) 0.0258(11) 0.0262(13) -0.0022(9) -0.0090(10) 0.0095(10) C36 0.0258(11) 0.0229(10) 0.0202(12) 0.0034(8) -0.0014(9) 0.0083(9) C41 0.0147(9) 0.0187(9) 0.0176(11) 0.0028(8) -0.0016(8) 0.0023(8) C42 0.0182(10) 0.0207(9) 0.0158(11) 0.0027(8) 0.0004(8) 0.0049(8) C43 0.0211(10) 0.0165(9) 0.0296(13) 0.0062(8) -0.0033(9) 0.0031(8) C44 0.0192(10) 0.0313(11) 0.0318(13) 0.0206(10) 0.0031(9) 0.0061(9) C45 0.0210(11) 0.0382(12) 0.0172(11) 0.0114(9) 0.0025(9) 0.0094(9) C46 0.0206(10) 0.0205(9) 0.0174(11) 0.0027(8) 0.0012(8) 0.0076(8) C51 0.0204(10) 0.0185(9) 0.0133(10) 0.0060(8) -0.0003(8) 0.0036(8) C52 0.0177(10) 0.0209(10) 0.0206(11) 0.0050(8) -0.0022(9) 0.0036(8) C53 0.0285(12) 0.0152(9) 0.0264(12) 0.0020(8) -0.0007(10) 0.0014(8) C54 0.0349(12) 0.0174(10) 0.0268(12) 0.0038(8) 0.0044(10) 0.0121(9) C55 0.0220(11) 0.0286(11) 0.0320(13) 0.0116(9) 0.0069(10) 0.0104(9) C56 0.0240(11) 0.0176(10) 0.0262(12) 0.0076(8) 0.0020(9) 0.0016(8) P1 0.0171(3) 0.0160(2) 0.0161(3) 0.00348(19) 0.0011(2) 0.00375(19) C61 0.0208(11) 0.0202(10) 0.0263(12) 0.0078(9) 0.0006(9) 0.0067(8) C62 0.0280(11) 0.0131(9) 0.0206(11) 0.0053(8) 0.0000(9) 0.0028(8) C63 0.0313(12) 0.0269(11) 0.0283(13) 0.0091(9) -0.0024(10) 0.0089(9) C64 0.0565(17) 0.0342(12) 0.0184(13) 0.0049(10) -0.0073(11) 0.0190(12) C65 0.0550(16) 0.0330(12) 0.0200(13) 0.0104(10) 0.0117(12) 0.0152(12) C66 0.0356(13) 0.0277(11) 0.0306(14) 0.0085(10) 0.0089(11) 0.0038(10) C67 0.0276(11) 0.0222(10) 0.0198(11) 0.0069(8) -0.0009(9) -0.0016(9) C71 0.0173(10) 0.0187(9) 0.0137(10) 0.0033(7) -0.0015(8) 0.0030(8) C72 0.0212(10) 0.0167(9) 0.0197(11) 0.0024(8) -0.0006(9) 0.0037(8) C73 0.0258(11) 0.0282(11) 0.0306(13) 0.0033(9) -0.0040(10) 0.0118(9) C74 0.0216(11) 0.0361(12) 0.0395(15) 0.0048(11) -0.0114(10) 0.0058(10) C75 0.0259(11) 0.0233(11) 0.0309(13) 0.0013(9) -0.0085(10) -0.0034(9) C76 0.0254(11) 0.0177(9) 0.0206(11) 0.0018(8) -0.0024(9) 0.0049(8) C81 0.0139(9) 0.0174(9) 0.0207(11) 0.0010(8) 0.0020(8) 0.0017(7) C82 0.0345(12) 0.0216(10) 0.0218(12) 0.0053(9) 0.0055(10) 0.0034(9) C83 0.0394(13) 0.0264(11) 0.0176(12) -0.0020(9) 0.0017(10) 0.0038(10) C84 0.0250(11) 0.0178(10) 0.0294(13) -0.0013(9) 0.0032(10) -0.0010(8) C85 0.0372(13) 0.0214(10) 0.0289(13) 0.0068(9) 0.0066(11) -0.0044(9) C86 0.0320(12) 0.0235(10) 0.0196(12) 0.0037(9) 0.0020(10) -0.0020(9) C91 0.0235(11) 0.0180(9) 0.0188(11) 0.0021(8) 0.0039(9) 0.0023(8) C92 0.0286(12) 0.0342(12) 0.0233(12) 0.0066(9) 0.0022(10) 0.0049(10) C93 0.0453(15) 0.0375(13) 0.0176(12) 0.0052(10) 0.0032(11) 0.0008(11) C94 0.0414(14) 0.0288(12) 0.0260(13) 0.0012(10) 0.0164(11) 0.0003(10) C95 0.0270(12) 0.0431(14) 0.0386(15) 0.0060(11) 0.0129(11) 0.0092(11) C96 0.0258(11) 0.0349(12) 0.0246(13) 0.0042(10) 0.0050(10) 0.0052(10) _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 N21 1.6765(17) . ? Ti1 N11 2.2106(17) . ? Ti1 N1 2.2347(17) . ? Ti1 Cl3 2.3745(6) . ? Ti1 Cl2 2.3894(6) . ? N1 C2 1.467(4) . ? N1 C3 1.482(4) . ? N1 H1 0.95(3) . ? C2 H2A 0.87(4) . ? C2 H2B 0.98(3) . ? C2 H2C 0.98(3) . ? C3 H3A 1.05(3) . ? C3 H3B 0.91(3) . ? C3 H3C 1.05(4) . ? N11 C13 1.476(3) . ? N11 C12 1.478(3) . ? N11 H11 0.87(2) . ? C12 H12A 0.99(3) . ? C12 H12B 0.97(2) . ? C12 H12C 0.96(2) . ? C13 H13A 0.98(3) . ? C13 H13B 0.99(2) . ? C13 H13C 1.02(2) . ? N21 B22 1.526(3) . ? B22 C41 1.660(3) . ? B22 C51 1.663(3) . ? B22 C31 1.665(3) . ? F32 C32 1.351(2) . ? F33 C33 1.347(3) . ? F34 C34 1.344(3) . ? F35 C35 1.353(2) . ? F36 C36 1.351(2) . ? F42 C42 1.360(2) . ? F43 C43 1.353(2) . ? F44 C44 1.346(2) . ? F45 C45 1.344(2) . ? F46 C46 1.359(2) . ? F52 C52 1.351(2) . ? F53 C53 1.348(2) . ? F54 C54 1.350(2) . ? F55 C55 1.346(2) . ? F56 C56 1.352(2) . ? C31 C32 1.391(3) . ? C31 C36 1.393(3) . ? C32 C33 1.379(3) . ? C33 C34 1.376(3) . ? C34 C35 1.367(3) . ? C35 C36 1.377(3) . ? C41 C46 1.383(3) . ? C41 C42 1.389(3) . ? C42 C43 1.372(3) . ? C43 C44 1.377(3) . ? C44 C45 1.374(3) . ? C45 C46 1.385(3) . ? C51 C52 1.383(3) . ? C51 C56 1.394(3) . ? C52 C53 1.390(3) . ? C53 C54 1.368(3) . ? C54 C55 1.370(3) . ? C55 C56 1.375(3) . ? P1 C71 1.789(2) . ? P1 C91 1.793(2) . ? P1 C81 1.7958(18) . ? P1 C61 1.814(2) . ? C61 C62 1.507(3) . ? C61 H61A 0.96(2) . ? C61 H61B 0.94(2) . ? C62 C67 1.385(3) . ? C62 C63 1.389(3) . ? C63 C64 1.384(3) . ? C63 H63 0.9300 . ? C64 C65 1.380(3) . ? C64 H64 0.9300 . ? C65 C66 1.374(3) . ? C65 H65 0.9300 . ? C66 C67 1.387(3) . ? C66 H66 0.9300 . ? C67 H67 0.9300 . ? C71 C72 1.387(3) . ? C71 C76 1.405(2) . ? C72 C73 1.384(3) . ? C72 H72 0.9300 . ? C73 C74 1.388(3) . ? C73 H73 0.9300 . ? C74 C75 1.377(3) . ? C74 H74 0.9300 . ? C75 C76 1.377(3) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C81 C82 1.388(3) . ? C81 C86 1.390(3) . ? C82 C83 1.385(3) . ? C82 H82 0.9300 . ? C83 C84 1.378(3) . ? C83 H83 0.9300 . ? C84 C85 1.372(3) . ? C84 H84 0.9300 . ? C85 C86 1.383(3) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C91 C92 1.387(3) . ? C91 C96 1.395(3) . ? C92 C93 1.382(3) . ? C92 H92 0.9300 . ? C93 C94 1.376(3) . ? C93 H93 0.9300 . ? C94 C95 1.371(4) . ? C94 H94 0.9300 . ? C95 C96 1.379(3) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? 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 N21 Ti1 N11 99.66(7) . . ? N21 Ti1 N1 101.18(8) . . ? N11 Ti1 N1 159.12(7) . . ? N21 Ti1 Cl3 106.86(6) . . ? N11 Ti1 Cl3 87.37(5) . . ? N1 Ti1 Cl3 85.37(5) . . ? N21 Ti1 Cl2 112.54(6) . . ? N11 Ti1 Cl2 85.64(5) . . ? N1 Ti1 Cl2 87.61(5) . . ? Cl3 Ti1 Cl2 140.59(3) . . ? C2 N1 C3 111.0(2) . . ? C2 N1 Ti1 115.75(15) . . ? C3 N1 Ti1 113.25(18) . . ? C2 N1 H1 108.3(16) . . ? C3 N1 H1 107.9(16) . . ? Ti1 N1 H1 99.6(15) . . ? N1 C2 H2A 110(3) . . ? N1 C2 H2B 109.8(18) . . ? H2A C2 H2B 109(3) . . ? N1 C2 H2C 112.9(17) . . ? H2A C2 H2C 108(3) . . ? H2B C2 H2C 108(2) . . ? N1 C3 H3A 105.2(18) . . ? N1 C3 H3B 104(2) . . ? H3A C3 H3B 108(3) . . ? N1 C3 H3C 110.3(18) . . ? H3A C3 H3C 113(2) . . ? H3B C3 H3C 116(3) . . ? C13 N11 C12 111.22(19) . . ? C13 N11 Ti1 115.15(13) . . ? C12 N11 Ti1 113.79(14) . . ? C13 N11 H11 107.2(14) . . ? C12 N11 H11 107.3(14) . . ? Ti1 N11 H11 101.2(14) . . ? N11 C12 H12A 111.1(15) . . ? N11 C12 H12B 109.7(13) . . ? H12A C12 H12B 107.5(19) . . ? N11 C12 H12C 111.1(15) . . ? H12A C12 H12C 109(2) . . ? H12B C12 H12C 108(2) . . ? N11 C13 H13A 108.4(14) . . ? N11 C13 H13B 110.4(13) . . ? H13A C13 H13B 109.1(18) . . ? N11 C13 H13C 111.9(12) . . ? H13A C13 H13C 111.4(17) . . ? H13B C13 H13C 105.7(19) . . ? B22 N21 Ti1 169.19(15) . . ? N21 B22 C41 104.44(16) . . ? N21 B22 C51 113.99(15) . . ? C41 B22 C51 112.02(15) . . ? N21 B22 C31 109.66(16) . . ? C41 B22 C31 112.97(15) . . ? C51 B22 C31 103.98(16) . . ? C32 C31 C36 112.95(19) . . ? C32 C31 B22 119.87(17) . . ? C36 C31 B22 127.18(18) . . ? F32 C32 C33 115.8(2) . . ? F32 C32 C31 119.73(19) . . ? C33 C32 C31 124.5(2) . . ? F33 C33 C34 119.7(2) . . ? F33 C33 C32 120.7(2) . . ? C34 C33 C32 119.5(2) . . ? F34 C34 C35 120.3(2) . . ? F34 C34 C33 121.1(2) . . ? C35 C34 C33 118.6(2) . . ? F35 C35 C34 119.6(2) . . ? F35 C35 C36 120.1(2) . . ? C34 C35 C36 120.2(2) . . ? F36 C36 C35 114.73(18) . . ? F36 C36 C31 121.21(18) . . ? C35 C36 C31 124.1(2) . . ? C46 C41 C42 112.82(18) . . ? C46 C41 B22 126.46(16) . . ? C42 C41 B22 120.45(16) . . ? F42 C42 C43 115.49(16) . . ? F42 C42 C41 119.75(17) . . ? C43 C42 C41 124.72(18) . . ? F43 C43 C42 121.13(18) . . ? F43 C43 C44 119.31(18) . . ? C42 C43 C44 119.56(17) . . ? F44 C44 C45 120.68(19) . . ? F44 C44 C43 120.63(18) . . ? C45 C44 C43 118.68(19) . . ? F45 C45 C44 120.06(19) . . ? F45 C45 C46 120.64(18) . . ? C44 C45 C46 119.29(19) . . ? F46 C46 C41 120.73(17) . . ? F46 C46 C45 114.61(17) . . ? C41 C46 C45 124.66(17) . . ? C52 C51 C56 112.96(17) . . ? C52 C51 B22 126.33(17) . . ? C56 C51 B22 120.66(16) . . ? F52 C52 C51 121.11(17) . . ? F52 C52 C53 114.88(16) . . ? C51 C52 C53 124.01(18) . . ? F53 C53 C54 119.96(17) . . ? F53 C53 C52 120.28(18) . . ? C54 C53 C52 119.76(18) . . ? F54 C54 C53 120.65(18) . . ? F54 C54 C55 120.24(19) . . ? C53 C54 C55 119.12(18) . . ? F55 C55 C54 119.80(18) . . ? F55 C55 C56 120.96(18) . . ? C54 C55 C56 119.23(19) . . ? F56 C56 C55 116.28(18) . . ? F56 C56 C51 118.80(16) . . ? C55 C56 C51 124.91(18) . . ? C71 P1 C91 107.96(9) . . ? C71 P1 C81 109.54(9) . . ? C91 P1 C81 108.29(9) . . ? C71 P1 C61 111.54(10) . . ? C91 P1 C61 106.51(10) . . ? C81 P1 C61 112.79(10) . . ? C62 C61 P1 117.64(14) . . ? C62 C61 H61A 113.1(14) . . ? P1 C61 H61A 104.2(15) . . ? C62 C61 H61B 113.6(14) . . ? P1 C61 H61B 102.9(14) . . ? H61A C61 H61B 103.9(19) . . ? C67 C62 C63 118.84(19) . . ? C67 C62 C61 121.28(19) . . ? C63 C62 C61 119.85(19) . . ? C64 C63 C62 120.3(2) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C65 C64 C63 120.5(2) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C66 C65 C64 119.5(2) . . ? C66 C65 H65 120.2 . . ? C64 C65 H65 120.2 . . ? C65 C66 C67 120.4(2) . . ? C65 C66 H66 119.8 . . ? C67 C66 H66 119.8 . . ? C62 C67 C66 120.5(2) . . ? C62 C67 H67 119.8 . . ? C66 C67 H67 119.8 . . ? C72 C71 C76 120.34(18) . . ? C72 C71 P1 120.04(14) . . ? C76 C71 P1 119.57(15) . . ? C73 C72 C71 119.70(18) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C72 C73 C74 119.6(2) . . ? C72 C73 H73 120.2 . . ? C74 C73 H73 120.2 . . ? C75 C74 C73 120.8(2) . . ? C75 C74 H74 119.6 . . ? C73 C74 H74 119.6 . . ? C74 C75 C76 120.24(19) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C75 C76 C71 119.24(19) . . ? C75 C76 H76 120.4 . . ? C71 C76 H76 120.4 . . ? C82 C81 C86 119.72(17) . . ? C82 C81 P1 122.46(15) . . ? C86 C81 P1 117.69(15) . . ? C83 C82 C81 119.6(2) . . ? C83 C82 H82 120.2 . . ? C81 C82 H82 120.2 . . ? C84 C83 C82 120.4(2) . . ? C84 C83 H83 119.8 . . ? C82 C83 H83 119.8 . . ? C85 C84 C83 120.03(19) . . ? C85 C84 H84 120.0 . . ? C83 C84 H84 120.0 . . ? C84 C85 C86 120.4(2) . . ? C84 C85 H85 119.8 . . ? C86 C85 H85 119.8 . . ? C85 C86 C81 119.8(2) . . ? C85 C86 H86 120.1 . . ? C81 C86 H86 120.1 . . ? C92 C91 C96 119.34(19) . . ? C92 C91 P1 121.46(16) . . ? C96 C91 P1 119.19(17) . . ? C93 C92 C91 120.0(2) . . ? C93 C92 H92 120.0 . . ? C91 C92 H92 120.0 . . ? C94 C93 C92 120.3(2) . . ? C94 C93 H93 119.8 . . ? C92 C93 H93 119.8 . . ? C95 C94 C93 119.9(2) . . ? C95 C94 H94 120.0 . . ? C93 C94 H94 120.0 . . ? C94 C95 C96 120.7(2) . . ? C94 C95 H95 119.7 . . ? C96 C95 H95 119.7 . . ? C95 C96 C91 119.7(2) . . ? C95 C96 H96 120.2 . . ? C91 C96 H96 120.2 . . ? 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 N21 Ti1 N1 C2 -51.3(2) . . . . ? N11 Ti1 N1 C2 132.4(2) . . . . ? Cl3 Ti1 N1 C2 -157.6(2) . . . . ? Cl2 Ti1 N1 C2 61.2(2) . . . . ? N21 Ti1 N1 C3 178.9(2) . . . . ? N11 Ti1 N1 C3 2.6(3) . . . . ? Cl3 Ti1 N1 C3 72.6(2) . . . . ? Cl2 Ti1 N1 C3 -68.6(2) . . . . ? N21 Ti1 N11 C13 -43.43(16) . . . . ? N1 Ti1 N11 C13 132.9(2) . . . . ? Cl3 Ti1 N11 C13 63.24(15) . . . . ? Cl2 Ti1 N11 C13 -155.57(15) . . . . ? N21 Ti1 N11 C12 -173.52(16) . . . . ? N1 Ti1 N11 C12 2.8(3) . . . . ? Cl3 Ti1 N11 C12 -66.86(15) . . . . ? Cl2 Ti1 N11 C12 74.33(15) . . . . ? N11 Ti1 N21 B22 69.8(7) . . . . ? N1 Ti1 N21 B22 -108.9(7) . . . . ? Cl3 Ti1 N21 B22 -20.4(7) . . . . ? Cl2 Ti1 N21 B22 159.1(7) . . . . ? Ti1 N21 B22 C41 11.0(8) . . . . ? Ti1 N21 B22 C51 -111.6(7) . . . . ? Ti1 N21 B22 C31 132.3(7) . . . . ? N21 B22 C31 C32 47.6(2) . . . . ? C41 B22 C31 C32 163.63(17) . . . . ? C51 B22 C31 C32 -74.7(2) . . . . ? N21 B22 C31 C36 -133.1(2) . . . . ? C41 B22 C31 C36 -17.0(3) . . . . ? C51 B22 C31 C36 104.6(2) . . . . ? C36 C31 C32 F32 -175.50(17) . . . . ? B22 C31 C32 F32 3.9(3) . . . . ? C36 C31 C32 C33 3.9(3) . . . . ? B22 C31 C32 C33 -176.6(2) . . . . ? F32 C32 C33 F33 -1.5(3) . . . . ? C31 C32 C33 F33 179.01(19) . . . . ? F32 C32 C33 C34 176.53(19) . . . . ? C31 C32 C33 C34 -2.9(3) . . . . ? F33 C33 C34 F34 -1.7(3) . . . . ? C32 C33 C34 F34 -179.8(2) . . . . ? F33 C33 C34 C35 177.74(19) . . . . ? C32 C33 C34 C35 -0.4(3) . . . . ? F34 C34 C35 F35 0.3(3) . . . . ? C33 C34 C35 F35 -179.2(2) . . . . ? F34 C34 C35 C36 -178.35(19) . . . . ? C33 C34 C35 C36 2.2(3) . . . . ? F35 C35 C36 F36 0.3(3) . . . . ? C34 C35 C36 F36 178.93(19) . . . . ? F35 C35 C36 C31 -179.60(18) . . . . ? C34 C35 C36 C31 -1.0(3) . . . . ? C32 C31 C36 F36 178.15(17) . . . . ? B22 C31 C36 F36 -1.2(3) . . . . ? C32 C31 C36 C35 -2.0(3) . . . . ? B22 C31 C36 C35 178.64(19) . . . . ? N21 B22 C41 C46 -105.3(2) . . . . ? C51 B22 C41 C46 18.5(3) . . . . ? C31 B22 C41 C46 135.6(2) . . . . ? N21 B22 C41 C42 68.2(2) . . . . ? C51 B22 C41 C42 -167.94(18) . . . . ? C31 B22 C41 C42 -50.9(2) . . . . ? C46 C41 C42 F42 176.80(17) . . . . ? B22 C41 C42 F42 2.4(3) . . . . ? C46 C41 C42 C43 -5.5(3) . . . . ? B22 C41 C42 C43 -179.89(19) . . . . ? F42 C42 C43 F43 0.6(3) . . . . ? C41 C42 C43 F43 -177.18(18) . . . . ? F42 C42 C43 C44 -179.23(18) . . . . ? C41 C42 C43 C44 3.0(3) . . . . ? F43 C43 C44 F44 2.0(3) . . . . ? C42 C43 C44 F44 -178.24(18) . . . . ? F43 C43 C44 C45 -177.91(18) . . . . ? C42 C43 C44 C45 1.9(3) . . . . ? F44 C44 C45 F45 -2.4(3) . . . . ? C43 C44 C45 F45 177.44(19) . . . . ? F44 C44 C45 C46 176.48(18) . . . . ? C43 C44 C45 C46 -3.7(3) . . . . ? C42 C41 C46 F46 -176.49(17) . . . . ? B22 C41 C46 F46 -2.5(3) . . . . ? C42 C41 C46 C45 3.6(3) . . . . ? B22 C41 C46 C45 177.56(19) . . . . ? F45 C45 C46 F46 -0.2(3) . . . . ? C44 C45 C46 F46 -179.12(18) . . . . ? F45 C45 C46 C41 179.68(19) . . . . ? C44 C45 C46 C41 0.8(3) . . . . ? N21 B22 C51 C52 -5.1(3) . . . . ? C41 B22 C51 C52 -123.4(2) . . . . ? C31 B22 C51 C52 114.3(2) . . . . ? N21 B22 C51 C56 177.95(18) . . . . ? C41 B22 C51 C56 59.6(2) . . . . ? C31 B22 C51 C56 -62.7(2) . . . . ? C56 C51 C52 F52 179.38(18) . . . . ? B22 C51 C52 F52 2.2(3) . . . . ? C56 C51 C52 C53 -1.1(3) . . . . ? B22 C51 C52 C53 -178.2(2) . . . . ? F52 C52 C53 F53 0.3(3) . . . . ? C51 C52 C53 F53 -179.3(2) . . . . ? F52 C52 C53 C54 -179.6(2) . . . . ? C51 C52 C53 C54 0.8(3) . . . . ? F53 C53 C54 F54 -0.5(3) . . . . ? C52 C53 C54 F54 179.4(2) . . . . ? F53 C53 C54 C55 179.5(2) . . . . ? C52 C53 C54 C55 -0.5(3) . . . . ? F54 C54 C55 F55 -0.1(3) . . . . ? C53 C54 C55 F55 179.9(2) . . . . ? F54 C54 C55 C56 -179.3(2) . . . . ? C53 C54 C55 C56 0.7(3) . . . . ? F55 C55 C56 F56 0.9(3) . . . . ? C54 C55 C56 F56 -179.9(2) . . . . ? F55 C55 C56 C51 179.7(2) . . . . ? C54 C55 C56 C51 -1.1(4) . . . . ? C52 C51 C56 F56 180.00(18) . . . . ? B22 C51 C56 F56 -2.7(3) . . . . ? C52 C51 C56 C55 1.3(3) . . . . ? B22 C51 C56 C55 178.6(2) . . . . ? C71 P1 C61 C62 63.23(18) . . . . ? C91 P1 C61 C62 -179.20(15) . . . . ? C81 P1 C61 C62 -60.54(18) . . . . ? P1 C61 C62 C67 -61.3(2) . . . . ? P1 C61 C62 C63 120.75(19) . . . . ? C67 C62 C63 C64 -0.9(3) . . . . ? C61 C62 C63 C64 177.15(18) . . . . ? C62 C63 C64 C65 -0.3(3) . . . . ? C63 C64 C65 C66 1.5(3) . . . . ? C64 C65 C66 C67 -1.4(3) . . . . ? C63 C62 C67 C66 1.0(3) . . . . ? C61 C62 C67 C66 -177.05(18) . . . . ? C65 C66 C67 C62 0.2(3) . . . . ? C91 P1 C71 C72 109.16(17) . . . . ? C81 P1 C71 C72 -8.6(2) . . . . ? C61 P1 C71 C72 -134.15(17) . . . . ? C91 P1 C71 C76 -68.42(18) . . . . ? C81 P1 C71 C76 173.86(16) . . . . ? C61 P1 C71 C76 48.27(19) . . . . ? C76 C71 C72 C73 -0.2(3) . . . . ? P1 C71 C72 C73 -177.80(17) . . . . ? C71 C72 C73 C74 0.4(3) . . . . ? C72 C73 C74 C75 -0.3(4) . . . . ? C73 C74 C75 C76 0.1(4) . . . . ? C74 C75 C76 C71 0.0(3) . . . . ? C72 C71 C76 C75 0.0(3) . . . . ? P1 C71 C76 C75 177.59(17) . . . . ? C71 P1 C81 C82 -94.14(19) . . . . ? C91 P1 C81 C82 148.35(17) . . . . ? C61 P1 C81 C82 30.7(2) . . . . ? C71 P1 C81 C86 81.74(17) . . . . ? C91 P1 C81 C86 -35.78(19) . . . . ? C61 P1 C81 C86 -153.40(16) . . . . ? C86 C81 C82 C83 0.0(3) . . . . ? P1 C81 C82 C83 175.80(17) . . . . ? C81 C82 C83 C84 -1.2(3) . . . . ? C82 C83 C84 C85 1.0(3) . . . . ? C83 C84 C85 C86 0.4(3) . . . . ? C84 C85 C86 C81 -1.6(3) . . . . ? C82 C81 C86 C85 1.4(3) . . . . ? P1 C81 C86 C85 -174.59(17) . . . . ? C71 P1 C91 C92 -10.90(19) . . . . ? C81 P1 C91 C92 107.63(18) . . . . ? C61 P1 C91 C92 -130.80(17) . . . . ? C71 P1 C91 C96 169.92(16) . . . . ? C81 P1 C91 C96 -71.56(18) . . . . ? C61 P1 C91 C96 50.01(18) . . . . ? C96 C91 C92 C93 -1.1(3) . . . . ? P1 C91 C92 C93 179.71(16) . . . . ? C91 C92 C93 C94 0.4(3) . . . . ? C92 C93 C94 C95 0.9(3) . . . . ? C93 C94 C95 C96 -1.4(3) . . . . ? C94 C95 C96 C91 0.6(3) . . . . ? C92 C91 C96 C95 0.6(3) . . . . ? P1 C91 C96 C95 179.80(16) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.409 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.054 #===END