#------------------------------------------------------------------------------ #$Date: 2014-07-11 21:33:45 +0300 (Fri, 11 Jul 2014) $ #$Revision: 120075 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/07/51/4075181.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4075181 loop_ _publ_author_name 'Bolton, Paul D.' 'Clot, Eric' 'Adams, Nico' 'Dubberley, Stuart R.' 'Cowley, Andrew R.' 'Mountford, Philip' _publ_section_title ; Experimental and DFT Studies of Cationic Imido Titanium Alkyls:  Agostic Interactions and C−H Bond and Solvent Activation Reactions of Isolobal Analogues of Group 4 Metallocenium Cations ; _journal_issue 11 _journal_name_full Organometallics _journal_page_first 2806 _journal_volume 25 _journal_year 2006 _chemical_compound_source ; synthesis as described ; _chemical_formula_moiety ' C42 H35 B1 Cl1 F20 N5 Ti1 ' _chemical_formula_sum 'C42 H35 B Cl F20 N5 Ti' _chemical_formula_weight 1083.90 _chemical_name_systematic ; [Ti(tBu)(Me3[9]aneN3)Cl(py)][B(ArF)4] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 90.9546(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.1935(2) _cell_length_b 21.1046(3) _cell_length_c 15.6878(3) _cell_measurement_reflns_used 46808 _cell_measurement_temperature 150 _cell_measurement_theta_max 28 _cell_measurement_theta_min 5 _cell_volume 4367.56(12) _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 46808 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_min 5.11 _diffrn_standards_decay_% 0.00 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_crystal_colour ' pale orange ' _exptl_crystal_density_diffrn 1.648 _exptl_crystal_description ' plate ' _exptl_crystal_F_000 2186.739 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.81 _refine_diff_density_min -1.04 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0386 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 626 _refine_ls_number_reflns 5541 _refine_ls_R_factor_gt 0.0580 _refine_ls_shift/su_max 0.023421 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 0.931 0.531 0.506 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0680 _reflns_limit_h_max 17 _reflns_limit_h_min -17 _reflns_limit_k_max 27 _reflns_limit_k_min 0 _reflns_limit_l_max 20 _reflns_limit_l_min 0 _reflns_number_gt 5541 _reflns_number_total 9953 _reflns_threshold_expression >3.00\s(I) _[local]_cod_data_source_file om060096rsi20060131_031028.cif _[local]_cod_data_source_block compound_9-B(ArF)4 _[local]_cod_cif_authors_sg_H-M 'P 1 21/c 1 ' _[local]_cod_chemical_formula_sum_orig ' C42 H35 B1 Cl1 F20 N5 Ti1 ' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 4367.6(1) _cod_database_code 4075181 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ti1 0.50378(5) 0.38726(3) 0.20738(5) 0.0315 1.0000 Uani Cl1 0.48913(9) 0.38398(6) 0.05591(7) 0.0484 1.0000 Uani N3 0.5414(2) 0.42270(16) 0.3411(2) 0.0404 1.0000 Uani C31 0.4911(3) 0.3867(3) 0.4069(3) 0.0506 1.0000 Uani N6 0.6684(3) 0.41202(17) 0.1963(2) 0.0423 1.0000 Uani C61 0.7234(3) 0.3652(2) 0.1454(3) 0.0459 1.0000 Uani N9 0.5032(3) 0.50026(16) 0.1958(2) 0.0408 1.0000 Uani C91 0.4213(4) 0.5249(2) 0.1414(4) 0.0510 1.0000 Uani C1 0.4694(6) 0.5226(3) 0.2875(4) 0.041(2) 0.593(9) Uiso C2 0.5350(6) 0.4903(3) 0.3555(4) 0.040(2) 0.593(9) Uiso C4 0.6541(4) 0.3990(4) 0.3501(4) 0.0368(18) 0.593(9) Uiso C5 0.7145(5) 0.4277(4) 0.2786(4) 0.0391(19) 0.593(9) Uiso C7 0.6675(5) 0.4754(3) 0.1408(4) 0.0375(19) 0.593(9) Uiso C8 0.6002(4) 0.5259(3) 0.1796(4) 0.0330(17) 0.593(9) Uiso C51 0.523(1) 0.5323(4) 0.2729(5) 0.057(4) 0.407(9) Uiso C52 0.4931(9) 0.4920(4) 0.3474(6) 0.046(3) 0.407(9) Uiso C54 0.6503(6) 0.4278(5) 0.3543(6) 0.040(3) 0.407(9) Uiso C55 0.7106(7) 0.3920(5) 0.2889(5) 0.041(3) 0.407(9) Uiso C57 0.6935(6) 0.4745(4) 0.1749(8) 0.046(3) 0.407(9) Uiso C58 0.6014(6) 0.5082(5) 0.1364(6) 0.039(3) 0.407(9) Uiso N1 0.5147(3) 0.30955(17) 0.2306(2) 0.0394 1.0000 Uani C10 0.5136(4) 0.2412(2) 0.2399(4) 0.0479 1.0000 Uani C11 0.4259(5) 0.2209(3) 0.2940(5) 0.0705 1.0000 Uani C12 0.4979(5) 0.2133(3) 0.1480(5) 0.0718 1.0000 Uani C13 0.6149(4) 0.2178(2) 0.2775(4) 0.0654 1.0000 Uani N2 0.3322(2) 0.38298(16) 0.2194(2) 0.0340 1.0000 Uani C14 0.2722(3) 0.40789(19) 0.2779(3) 0.0376 1.0000 Uani C15 0.1699(3) 0.3948(2) 0.2841(3) 0.0430 1.0000 Uani C16 0.1262(3) 0.3546(2) 0.2250(3) 0.0408 1.0000 Uani C17 0.1852(3) 0.3289(2) 0.1629(3) 0.0400 1.0000 Uani C18 0.2875(3) 0.3440(2) 0.1615(3) 0.0386 1.0000 Uani B1 -0.0009(3) 0.11609(19) 0.2358(3) 0.0237 1.0000 Uani C19 -0.0923(3) 0.14189(17) 0.1707(2) 0.0248 1.0000 Uani C20 -0.1844(3) 0.11284(17) 0.1535(2) 0.0257 1.0000 Uani C21 -0.2541(3) 0.1351(2) 0.0943(3) 0.0321 1.0000 Uani C22 -0.2338(3) 0.1886(2) 0.0484(3) 0.0352 1.0000 Uani C23 -0.1435(3) 0.21911(19) 0.0615(2) 0.0342 1.0000 Uani C24 -0.0751(3) 0.19489(18) 0.1205(2) 0.0289 1.0000 Uani F1 -0.21234(16) 0.0595(1) 0.19463(14) 0.0310 1.0000 Uani F2 -0.34324(17) 0.10413(12) 0.08185(16) 0.0412 1.0000 Uani F3 -0.3025(2) 0.21066(13) -0.00967(17) 0.0513 1.0000 Uani F4 -0.1223(2) 0.27203(12) 0.01712(16) 0.0462 1.0000 Uani F5 0.01312(17) 0.22699(11) 0.12908(15) 0.0371 1.0000 Uani C25 -0.0413(3) 0.06311(17) 0.3055(2) 0.0233 1.0000 Uani C26 0.0044(3) 0.00614(18) 0.3280(2) 0.0257 1.0000 Uani C27 -0.0277(3) -0.03293(19) 0.3930(2) 0.0324 1.0000 Uani C28 -0.1102(3) -0.0156(2) 0.4398(2) 0.0358 1.0000 Uani C29 -0.1574(3) 0.0404(2) 0.4216(2) 0.0341 1.0000 Uani C30 -0.1227(3) 0.07853(19) 0.3570(2) 0.0286 1.0000 Uani F6 0.08662(16) -0.0154(1) 0.28619(14) 0.0336 1.0000 Uani F7 0.02170(19) -0.08708(11) 0.41099(15) 0.0422 1.0000 Uani F8 -0.1435(2) -0.05313(13) 0.50283(15) 0.0502 1.0000 Uani F9 -0.23756(19) 0.05908(14) 0.46802(15) 0.0476 1.0000 Uani F10 -0.17257(17) 0.13357(11) 0.34384(14) 0.0358 1.0000 Uani C32 0.0460(3) 0.17098(17) 0.3005(2) 0.0266 1.0000 Uani C33 0.1343(3) 0.15817(18) 0.3470(2) 0.0303 1.0000 Uani C34 0.1759(3) 0.1975(2) 0.4080(2) 0.0381 1.0000 Uani C35 0.1276(4) 0.2531(2) 0.4265(3) 0.0451 1.0000 Uani C36 0.0394(4) 0.2688(2) 0.3839(3) 0.0415 1.0000 Uani C37 0.0006(3) 0.22751(18) 0.3232(2) 0.0321 1.0000 Uani F11 0.18475(16) 0.10366(11) 0.33232(14) 0.0331 1.0000 Uani F12 0.2627(2) 0.18178(14) 0.44910(16) 0.0529 1.0000 Uani F13 0.1682(3) 0.29288(15) 0.48568(18) 0.0681 1.0000 Uani F14 -0.0080(2) 0.32320(12) 0.40199(19) 0.0581 1.0000 Uani F15 -0.08696(19) 0.24749(11) 0.28487(16) 0.0419 1.0000 Uani C38 0.0824(3) 0.08791(17) 0.1680(2) 0.0239 1.0000 Uani C39 0.0613(3) 0.03299(17) 0.1225(2) 0.0252 1.0000 Uani C40 0.1222(3) 0.00666(18) 0.0612(2) 0.0289 1.0000 Uani C41 0.2096(3) 0.03803(18) 0.0401(2) 0.0283 1.0000 Uani C42 0.2350(3) 0.09273(17) 0.0810(2) 0.0265 1.0000 Uani C43 0.1722(3) 0.11694(17) 0.1435(2) 0.0239 1.0000 Uani F16 -0.02561(16) 0.0011(1) 0.13831(13) 0.0314 1.0000 Uani F17 0.09740(19) -0.04827(11) 0.02336(14) 0.0385 1.0000 Uani F18 0.27080(18) 0.01420(11) -0.02058(14) 0.0397 1.0000 Uani F19 0.32169(17) 0.12311(11) 0.06134(15) 0.0373 1.0000 Uani F20 0.20383(16) 0.1718(1) 0.17941(14) 0.0306 1.0000 Uani H311 0.4973 0.3404 0.3945 0.0607 1.0000 Uiso H312 0.5234 0.3963 0.4635 0.0607 1.0000 Uiso H313 0.4178 0.3987 0.4079 0.0607 1.0000 Uiso H611 0.6859 0.3577 0.0904 0.0552 1.0000 Uiso H612 0.7929 0.3815 0.1333 0.0552 1.0000 Uiso H613 0.7289 0.3245 0.1778 0.0552 1.0000 Uiso H911 0.4345 0.5135 0.0807 0.0611 1.0000 Uiso H912 0.4180 0.5720 0.1472 0.0611 1.0000 Uiso H913 0.3555 0.5059 0.1590 0.0611 1.0000 Uiso H11 0.4774 0.5696 0.2924 0.0497 0.5934 Uiso H12 0.3967 0.5110 0.2960 0.0497 0.5934 Uiso H21 0.6048 0.5087 0.3543 0.0480 0.5934 Uiso H22 0.5049 0.4980 0.4127 0.0480 0.5934 Uiso H41 0.6834 0.4127 0.4063 0.0441 0.5934 Uiso H42 0.6562 0.3518 0.3461 0.0441 0.5934 Uiso H51 0.7162 0.4748 0.2854 0.0469 0.5934 Uiso H52 0.7853 0.4108 0.2811 0.0469 0.5934 Uiso H71 0.7382 0.4922 0.1376 0.0450 0.5934 Uiso H72 0.6416 0.4654 0.0820 0.0450 0.5934 Uiso H81 0.6317 0.5411 0.2343 0.0396 0.5934 Uiso H82 0.5931 0.5622 0.1390 0.0396 0.5934 Uiso H511 0.5966 0.5424 0.2775 0.0681 0.4066 Uiso H512 0.4827 0.5726 0.2735 0.0681 0.4066 Uiso H521 0.5177 0.5126 0.4013 0.0550 0.4066 Uiso H522 0.4176 0.4882 0.3482 0.0550 0.4066 Uiso H541 0.6696 0.4736 0.3516 0.0483 0.4066 Uiso H542 0.6680 0.4107 0.4121 0.0483 0.4066 Uiso H551 0.7841 0.4032 0.2947 0.0496 0.4066 Uiso H552 0.7020 0.3454 0.2973 0.0496 0.4066 Uiso H571 0.7168 0.4975 0.2273 0.0549 0.4066 Uiso H572 0.7492 0.4741 0.1324 0.0549 0.4066 Uiso H581 0.6172 0.5544 0.1305 0.0473 0.4066 Uiso H582 0.5859 0.4899 0.0789 0.0473 0.4066 Uiso H111 0.4260 0.1737 0.2999 0.0848 1.0000 Uiso H112 0.4327 0.2407 0.3518 0.0848 1.0000 Uiso H113 0.3608 0.2349 0.2664 0.0848 1.0000 Uiso H121 0.4966 0.1660 0.1510 0.0860 1.0000 Uiso H122 0.5548 0.2272 0.1111 0.0860 1.0000 Uiso H123 0.4322 0.2290 0.1233 0.0860 1.0000 Uiso H131 0.6130 0.1706 0.2835 0.0783 1.0000 Uiso H132 0.6266 0.2375 0.3348 0.0783 1.0000 Uiso H133 0.6711 0.2300 0.2388 0.0783 1.0000 Uiso H141 0.3031 0.4380 0.3201 0.0451 1.0000 Uiso H151 0.1288 0.4140 0.3304 0.0518 1.0000 Uiso H161 0.0523 0.3444 0.2274 0.0489 1.0000 Uiso H171 0.1550 0.2996 0.1192 0.0479 1.0000 Uiso H181 0.3301 0.3253 0.1157 0.0464 1.0000 Uiso 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 0.0259(3) 0.0299(4) 0.0389(4) -0.0057(3) 0.0032(3) -0.0033(3) Cl1 0.0528(7) 0.0610(7) 0.0314(5) -0.0027(5) 0.0021(5) -0.0139(6) N3 0.0379(19) 0.043(2) 0.040(2) -0.0003(16) -0.0033(15) -0.0074(16) C31 0.037(2) 0.088(4) 0.026(2) -0.006(2) 0.0002(17) -0.006(2) N6 0.039(2) 0.046(2) 0.041(2) -0.0017(17) 0.0033(16) -0.0046(17) C61 0.034(2) 0.049(3) 0.055(3) 0.005(2) 0.012(2) 0.000(2) N9 0.041(2) 0.0275(17) 0.054(2) 0.0034(16) -0.0041(17) -0.0015(15) C91 0.047(3) 0.035(2) 0.071(3) 0.008(2) -0.003(2) 0.002(2) N1 0.0270(17) 0.0396(19) 0.052(2) -0.0059(17) 0.0021(15) -0.0022(15) C10 0.042(3) 0.029(2) 0.073(3) 0.004(2) 0.001(2) -0.0035(19) C11 0.064(4) 0.042(3) 0.107(5) 0.022(3) 0.013(3) -0.009(3) C12 0.077(4) 0.039(3) 0.099(5) -0.020(3) -0.012(3) 0.003(3) C13 0.057(3) 0.036(3) 0.102(5) 0.008(3) -0.012(3) 0.003(2) N2 0.0267(17) 0.0316(17) 0.043(2) -0.0044(15) 0.0003(14) -0.0023(14) C14 0.035(2) 0.031(2) 0.047(2) -0.0062(18) 0.0049(18) -0.0004(17) C15 0.036(2) 0.035(2) 0.058(3) 0.007(2) 0.011(2) 0.0090(18) C16 0.028(2) 0.041(2) 0.054(3) 0.020(2) -0.0037(19) -0.0038(18) C17 0.032(2) 0.041(2) 0.047(3) 0.005(2) -0.0073(19) -0.0109(18) C18 0.034(2) 0.040(2) 0.042(2) -0.0072(19) -0.0002(18) -0.0018(18) B1 0.0231(19) 0.0236(19) 0.024(2) -0.0026(16) 0.0019(15) -0.0001(16) C19 0.0276(18) 0.0249(18) 0.0220(17) -0.0021(14) 0.0040(14) 0.0033(15) C20 0.0295(19) 0.0260(17) 0.0216(17) -0.0006(15) 0.0044(14) 0.0033(16) C21 0.0285(19) 0.037(2) 0.031(2) -0.0069(17) 0.0007(16) 0.0000(17) C22 0.038(2) 0.039(2) 0.028(2) 0.0001(17) -0.0039(17) 0.0080(18) C23 0.042(2) 0.031(2) 0.030(2) 0.0060(16) 0.0082(17) 0.0073(17) C24 0.0267(19) 0.0298(19) 0.030(2) -0.0035(16) 0.0050(15) 0.0007(15) F1 0.0288(11) 0.0324(12) 0.0316(11) 0.0020(9) -0.0014(9) -0.0061(9) F2 0.0309(12) 0.0469(14) 0.0453(14) -0.0040(11) -0.010(1) -0.001(1) F3 0.0505(15) 0.0575(16) 0.0453(15) 0.0117(13) -0.0151(12) 0.0106(13) F4 0.0544(15) 0.0404(14) 0.0439(14) 0.0182(11) 0.0059(12) 0.0059(12) F5 0.0360(13) 0.0331(12) 0.0423(13) 0.006(1) 0.003(1) -0.004(1) C25 0.0222(17) 0.0291(18) 0.0185(16) -0.0017(14) -0.0002(13) -0.0029(14) C26 0.0255(18) 0.0290(19) 0.0226(17) 0.0008(15) -0.0002(14) -0.0058(15) C27 0.036(2) 0.033(2) 0.0282(19) 0.0041(16) -0.0067(16) -0.0053(17) C28 0.042(2) 0.044(2) 0.0210(18) 0.0055(17) -0.0016(16) -0.0177(19) C29 0.032(2) 0.051(2) 0.0193(17) -0.0045(17) 0.0036(15) -0.0083(18) C30 0.0282(19) 0.035(2) 0.0226(18) -0.0033(16) 0.0014(14) -0.0041(16) F6 0.0327(12) 0.0330(12) 0.0351(12) 0.004(1) 0.0055(9) 0.0046(9) F7 0.0521(15) 0.0365(13) 0.0376(13) 0.0119(11) -0.0088(11) -0.0024(11) F8 0.0595(17) 0.0625(17) 0.0288(12) 0.0160(12) 0.0058(11) -0.0208(13) F9 0.0382(13) 0.0754(19) 0.0296(12) -0.0033(12) 0.014(1) -0.0051(13) F10 0.0341(12) 0.0418(13) 0.0319(12) -0.003(1) 0.0083(9) 0.007(1) C32 0.031(2) 0.0281(18) 0.0209(17) -0.0027(15) 0.0038(14) -0.0063(15) C33 0.037(2) 0.032(2) 0.0223(18) -0.0005(15) 0.0057(15) -0.0074(17) C34 0.042(2) 0.051(3) 0.0223(19) -0.0034(18) 0.0022(17) -0.018(2) C35 0.062(3) 0.046(3) 0.028(2) -0.0131(19) 0.010(2) -0.025(2) C36 0.058(3) 0.028(2) 0.038(2) -0.0108(18) 0.020(2) -0.009(2) C37 0.040(2) 0.028(2) 0.0284(19) -0.0043(16) 0.0066(17) -0.0042(17) F11 0.0305(11) 0.0393(12) 0.0293(11) 0.001(1) -0.0026(9) -0.001(1) F12 0.0491(16) 0.076(2) 0.0330(13) -0.0032(13) -0.0108(11) -0.0215(14) F13 0.098(2) 0.0666(19) 0.0404(16) -0.0290(14) 0.0042(15) -0.0372(18) F14 0.087(2) 0.0326(14) 0.0558(17) -0.0172(12) 0.0254(15) -0.0051(13) F15 0.0485(15) 0.0322(12) 0.0455(14) -0.007(1) 0.0086(12) 0.0086(11) C38 0.0281(18) 0.0252(17) 0.0184(16) 0.0037(14) 0.0016(14) 0.0024(15) C39 0.0271(18) 0.0238(17) 0.0245(18) -0.0006(14) 0.0007(14) -0.0051(14) C40 0.037(2) 0.0270(19) 0.0225(18) -0.0026(15) -0.0023(15) 0.0034(16) C41 0.032(2) 0.032(2) 0.0209(18) 0.0024(15) 0.0061(15) 0.0100(16) C42 0.0218(18) 0.0292(19) 0.0287(19) 0.0079(15) 0.0052(14) -0.0007(15) C43 0.0263(18) 0.0225(17) 0.0230(17) 0.0004(14) 0.0003(14) -0.0015(15) F16 0.0326(12) 0.0309(11) 0.0310(11) -0.0047(9) 0.0048(9) -0.0092(9) F17 0.0514(15) 0.0325(12) 0.0317(12) -0.010(1) 0.004(1) -0.0021(11) F18 0.0446(13) 0.0443(14) 0.0306(12) -0.004(1) 0.014(1) 0.0099(11) F19 0.0293(12) 0.0435(14) 0.0396(13) 0.003(1) 0.011(1) -0.004(1) F20 0.0324(12) 0.0291(11) 0.0304(11) -0.0037(9) 0.0054(9) -0.0088(9) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 International_Tables_Vol_IV_Table_2.2B loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl1 Ti1 N3 160.5(1) yes Cl1 Ti1 N6 89.5(1) yes N3 Ti1 N6 78.36(12) yes Cl1 Ti1 N9 87.32(9) yes N3 Ti1 N9 75.07(12) yes N6 Ti1 N9 76.32(12) yes Cl1 Ti1 N1 101.11(14) yes N3 Ti1 N1 95.96(16) yes N6 Ti1 N1 99.45(15) yes N9 Ti1 N1 170.62(16) yes Cl1 Ti1 N2 91.0(1) yes N3 Ti1 N2 97.98(12) yes N6 Ti1 N2 168.80(13) yes N9 Ti1 N2 92.53(12) yes N1 Ti1 N2 91.42(14) yes Ti1 N3 C31 112.9(3) yes Ti1 N3 C2 117.1(3) yes C31 N3 C2 112.1(4) yes Ti1 N3 C4 99.8(3) yes C31 N3 C4 102.3(4) yes C2 N3 C4 110.9(4) yes Ti1 N3 C52 106.0(4) yes C31 N3 C52 104.3(4) yes Ti1 N3 C54 110.9(4) yes C31 N3 C54 113.7(5) yes C52 N3 C54 108.5(6) yes Ti1 N6 C61 111.9(3) yes Ti1 N6 C5 112.0(3) yes C61 N6 C5 115.6(4) yes Ti1 N6 C7 103.8(3) yes C61 N6 C7 105.5(4) yes C5 N6 C7 107.0(4) yes Ti1 N6 C55 101.0(4) yes C61 N6 C55 98.5(4) yes Ti1 N6 C57 118.1(4) yes C61 N6 C57 112.4(5) yes C55 N6 C57 112.6(6) yes Ti1 N9 C91 113.6(3) yes Ti1 N9 C1 103.2(3) yes C91 N9 C1 102.0(4) yes Ti1 N9 C8 113.1(3) yes C91 N9 C8 114.9(4) yes C1 N9 C8 108.6(4) yes Ti1 N9 C51 114.5(4) yes C91 N9 C51 117.0(6) yes C91 N9 C58 102.6(4) yes C51 N9 C58 108.0(6) yes N9 C1 C2 109.7(4) yes N3 C2 C1 111.5(5) yes N3 C4 C5 108.4(4) yes N6 C5 C4 110.4(5) yes N6 C7 C8 111.6(4) yes N9 C8 C7 109.9(4) yes N9 C51 C52 110.5(6) yes N3 C52 C51 111.2(6) yes N3 C54 C55 113.4(6) yes N6 C55 C54 107.7(6) yes N6 C57 C58 110.1(6) yes N9 C58 C57 111.4(6) yes Ti1 N1 C10 171.4(3) yes N1 C10 C11 110.3(4) yes N1 C10 C12 106.4(4) yes C11 C10 C12 108.7(5) yes N1 C10 C13 110.4(4) yes C11 C10 C13 111.3(5) yes C12 C10 C13 109.6(5) yes Ti1 N2 C14 130.2(3) yes Ti1 N2 C18 113.0(3) yes C14 N2 C18 116.5(3) yes N2 C14 C15 124.2(4) yes C14 C15 C16 118.4(4) yes C15 C16 C17 119.1(4) yes C16 C17 C18 119.0(4) yes N2 C18 C17 122.9(4) yes C19 B1 C25 112.9(3) yes C19 B1 C32 114.1(3) yes C25 B1 C32 100.8(3) yes C19 B1 C38 101.9(3) yes C25 B1 C38 114.0(3) yes C32 B1 C38 113.7(3) yes B1 C19 C20 127.0(3) yes B1 C19 C24 119.3(3) yes C20 C19 C24 113.4(3) yes C19 C20 C21 123.6(3) yes C19 C20 F1 121.4(3) yes C21 C20 F1 115.0(3) yes C20 C21 C22 120.1(4) yes C20 C21 F2 119.9(4) yes C22 C21 F2 119.9(4) yes C21 C22 C23 119.2(4) yes C21 C22 F3 120.1(4) yes C23 C22 F3 120.7(4) yes C22 C23 C24 119.0(4) yes C22 C23 F4 120.0(4) yes C24 C23 F4 120.9(4) yes C19 C24 C23 124.6(4) yes C19 C24 F5 119.7(3) yes C23 C24 F5 115.7(3) yes B1 C25 C26 127.5(3) yes B1 C25 C30 119.0(3) yes C26 C25 C30 113.0(3) yes C25 C26 C27 124.5(3) yes C25 C26 F6 121.0(3) yes C27 C26 F6 114.5(3) yes C26 C27 C28 119.4(4) yes C26 C27 F7 120.6(4) yes C28 C27 F7 120.1(3) yes C27 C28 C29 118.8(4) yes C27 C28 F8 120.4(4) yes C29 C28 F8 120.7(4) yes C28 C29 C30 120.2(4) yes C28 C29 F9 119.8(4) yes C30 C29 F9 119.9(4) yes C25 C30 C29 124.0(4) yes C25 C30 F10 119.5(3) yes C29 C30 F10 116.6(3) yes B1 C32 C33 119.1(3) yes B1 C32 C37 127.1(3) yes C33 C32 C37 113.3(3) yes C32 C33 C34 124.6(4) yes C32 C33 F11 119.2(3) yes C34 C33 F11 116.2(4) yes C33 C34 C35 119.0(4) yes C33 C34 F12 120.7(4) yes C35 C34 F12 120.3(4) yes C34 C35 C36 119.9(4) yes C34 C35 F13 119.8(5) yes C36 C35 F13 120.4(4) yes C35 C36 C37 118.9(4) yes C35 C36 F14 119.9(4) yes C37 C36 F14 121.2(5) yes C32 C37 C36 124.3(4) yes C32 C37 F15 121.4(3) yes C36 C37 F15 114.2(4) yes B1 C38 C39 120.1(3) yes B1 C38 C43 126.6(3) yes C39 C38 C43 113.0(3) yes C38 C39 C40 125.5(3) yes C38 C39 F16 118.9(3) yes C40 C39 F16 115.6(3) yes C39 C40 C41 118.3(3) yes C39 C40 F17 121.1(3) yes C41 C40 F17 120.6(3) yes C40 C41 C42 119.7(3) yes C40 C41 F18 120.2(3) yes C42 C41 F18 120.1(3) yes C41 C42 C43 120.0(3) yes C41 C42 F19 119.8(3) yes C43 C42 F19 120.2(3) yes C38 C43 C42 123.5(3) yes C38 C43 F20 121.3(3) yes C42 C43 F20 115.2(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ti1 Cl1 2.3819(13) yes Ti1 N3 2.275(4) yes Ti1 N6 2.244(4) yes Ti1 N9 2.392(3) yes Ti1 N1 1.686(4) yes Ti1 N2 2.277(3) yes N3 C31 1.451(6) yes N3 C2 1.446(6) yes N3 C4 1.573(6) yes N3 C52 1.598(8) yes N3 C54 1.453(7) yes N6 C61 1.470(6) yes N6 C5 1.456(6) yes N6 C7 1.597(6) yes N6 C55 1.605(7) yes N6 C57 1.402(8) yes N9 C91 1.462(6) yes N9 C1 1.585(6) yes N9 C8 1.416(6) yes N9 C51 1.405(8) yes N9 C58 1.617(7) yes C1 C2 1.523(7) yes C4 C5 1.513(7) yes C7 C8 1.519(7) yes C51 C52 1.503(9) yes C54 C55 1.511(8) yes C54 H541 1.000(11) no C57 C58 1.524(8) yes N1 C10 1.451(6) yes C10 C11 1.509(8) yes C10 C12 1.567(9) yes C10 C13 1.533(7) yes N2 C14 1.330(5) yes N2 C18 1.353(5) yes C14 C15 1.382(6) yes C15 C16 1.375(7) yes C16 C17 1.370(7) yes C17 C18 1.388(6) yes B1 C19 1.659(5) yes B1 C25 1.659(5) yes B1 C32 1.654(5) yes B1 C38 1.652(5) yes C19 C20 1.384(5) yes C19 C24 1.389(5) yes C20 C21 1.379(5) yes C20 F1 1.352(4) yes C21 C22 1.368(6) yes C21 F2 1.357(5) yes C22 C23 1.366(6) yes C22 F3 1.356(5) yes C23 C24 1.381(6) yes C23 F4 1.347(5) yes C24 F5 1.351(4) yes C25 C26 1.388(5) yes C25 C30 1.392(5) yes C26 C27 1.383(5) yes C26 F6 1.355(4) yes C27 C28 1.373(6) yes C27 F7 1.344(5) yes C28 C29 1.364(6) yes C28 F8 1.347(4) yes C29 C30 1.378(5) yes C29 F9 1.353(5) yes C30 F10 1.349(5) yes C32 C33 1.391(6) yes C32 C37 1.383(5) yes C33 C34 1.375(6) yes C33 F11 1.351(5) yes C34 C35 1.368(7) yes C34 F12 1.347(5) yes C35 C36 1.373(7) yes C35 F13 1.355(5) yes C36 C37 1.384(6) yes C36 F14 1.339(5) yes C37 F15 1.361(5) yes C38 C39 1.387(5) yes C38 C43 1.394(5) yes C39 C40 1.380(5) yes C39 F16 1.355(4) yes C40 C41 1.375(6) yes C40 F17 1.341(4) yes C41 C42 1.360(5) yes C41 F18 1.356(4) yes C42 C43 1.391(5) yes C42 F19 1.351(4) yes C43 F20 1.350(4) yes _journal_paper_doi 10.1021/om060096r