# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Philip Mountford' 'Paul D. Bolton' 'Eric Clot' 'Andrew R. Cowley' _publ_contact_author_name 'Dr Philip Mountford' _publ_contact_author_address ; Chemistry Research Laboratory Oxford University Mansfield Road Oxford OX1 3TA UK ; _publ_contact_author_email PHILIP.MOUNTFORD@CHEMISTRY.OXFORD.AC.UK _publ_contact_author_phone '+44 1865 285140' _contact_author_fax '+44 1865 285141' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Well-defined imidotitanium alkyl cations: alpha-C-H or beta-Si-C agostic interactions, migratory insertion vs [2+2] cycloaddition, and the first structurally authenticated AlMe3 adduct of any transition metal alkyl cation ; data_Compound_6-BArF4 _database_code_depnum_ccdc_archive 'CCDC 268643' # Local code ARC735 _chemical_name_systematic ; [Ti(NtBu)(Me3[9]aneN3){Me3SiCH2C(NiPr)2}][B(C6F5)4] ; #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_special_details ; Geometric restraints were applied to the bond lengths and angles of the disordered groups. The lengths of sets of chemically-equivalent bonds were restrained to their common means (su 0.02\%A) and similarly sets of equivalent angles were restrained to their common means (su 2\%) ; #============================================================= _cell_length_a 11.9619(2) _cell_angle_alpha 75.5723(5) _cell_length_b 12.7619(2) _cell_angle_beta 80.1952(5) _cell_length_c 17.9840(2) _cell_angle_gamma 86.9238(5) _cell_volume 2619.78(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 ' 0.0033 0.0016 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 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 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 'F ' 0.0171 0.0103 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 ' 0.0061 0.0033 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 'Si ' 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 International_Tables_Vol_IV_Table_2.2B 'Ti ' 0.2776 0.4457 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 _cell_formula_units_Z 2 _chemical_formula_sum ' C48 H55 B1 F20 N6 Si Ti ' _chemical_formula_moiety ' C24 H55 N6 Si Ti, C24 B F20 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 1182.76 _cell_measurement_reflns_used 53966 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' pink ' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_max 0.38 _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 0.299 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.95 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 53966 _reflns_number_total 11970 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_theta_min 5.132 _diffrn_reflns_theta_max 27.557 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.557 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -15 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _refine_diff_density_min -0.48 _refine_diff_density_max 0.48 _refine_ls_number_reflns 7976 _refine_ls_number_restraints 48 _refine_ls_number_parameters 687 #_refine_ls_R_factor_ref 0.0402 _refine_ls_wR_factor_ref 0.0476 _refine_ls_goodness_of_fit_ref 1.0982 #_reflns_number_all 11970 _refine_ls_R_factor_all 0.0652 _refine_ls_wR_factor_all 0.0703 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 7976 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_gt 0.0476 _refine_ls_shift/su_max 0.031229 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.663 0.427 0.335 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group Ti1 Ti 0.09971(3) 0.37486(3) 0.27022(2) 0.0194 1.0000 Uani . . . . . N1 N 0.21905(15) 0.36288(14) 0.31225(10) 0.0258 1.0000 Uani . . . . . C1 C 0.32221(19) 0.35708(19) 0.34688(14) 0.0348 1.0000 Uani D . . . . C2 C 0.3112(4) 0.4441(4) 0.3954(3) 0.0414(14) 0.614(11) Uiso D . P 1 1 C3 C 0.4253(4) 0.3824(5) 0.2845(3) 0.0520(15) 0.614(11) Uiso D . P 1 1 C4 C 0.3337(4) 0.2456(4) 0.4018(3) 0.0395(12) 0.614(11) Uiso D . P 1 1 C52 C 0.3498(8) 0.4641(6) 0.3597(6) 0.055(3) 0.386(11) Uiso D . P 1 2 C53 C 0.4248(6) 0.3254(8) 0.2881(4) 0.051(2) 0.386(11) Uiso D . P 1 2 C54 C 0.3189(7) 0.2661(6) 0.4223(5) 0.041(2) 0.386(11) Uiso D . P 1 2 N2 N 0.13457(14) 0.49642(13) 0.16605(9) 0.0223 1.0000 Uani . . . . . C5 C 0.07576(17) 0.57011(16) 0.19934(11) 0.0216 1.0000 Uani . . . . . N3 N 0.02827(14) 0.53024(13) 0.27360(9) 0.0220 1.0000 Uani . . . . . C6 C 0.20725(19) 0.53249(17) 0.09020(12) 0.0284 1.0000 Uani . . . . . C7 C 0.3214(3) 0.4761(3) 0.0885(2) 0.0637 1.0000 Uani . . . . . C8 C 0.1500(3) 0.5201(3) 0.02357(15) 0.0679 1.0000 Uani . . . . . C9 C 0.06290(19) 0.68516(16) 0.15531(12) 0.0268 1.0000 Uani . . . . . Si1 Si 0.17741(5) 0.78317(5) 0.15079(4) 0.0306 1.0000 Uani . . . . . C10 C 0.2260(2) 0.8494(2) 0.04741(17) 0.0471 1.0000 Uani . . . . . C11 C 0.1170(3) 0.8874(2) 0.20166(18) 0.0485 1.0000 Uani . . . . . C12 C 0.2942(2) 0.7087(2) 0.19666(17) 0.0422 1.0000 Uani . . . . . C13 C -0.02021(19) 0.60399(17) 0.32227(12) 0.0277 1.0000 Uani . . . . . C14 C 0.0539(3) 0.6055(3) 0.38259(18) 0.0535 1.0000 Uani . . . . . C15 C -0.1413(2) 0.5779(2) 0.36140(18) 0.0460 1.0000 Uani . . . . . N4 N -0.08092(15) 0.34714(14) 0.22290(10) 0.0270 1.0000 Uani D . . . . N5 N -0.00886(14) 0.25859(14) 0.36995(10) 0.0237 1.0000 Uani D . . . . N6 N 0.12066(15) 0.21485(14) 0.23237(10) 0.0266 1.0000 Uani D . . . . C16 C -0.1616(3) 0.2787(4) 0.2855(2) 0.0265(10) 0.518(6) Uiso D . P 2 1 C17 C -0.1340(3) 0.2845(4) 0.3632(2) 0.0259(10) 0.518(6) Uiso D . P 2 1 C18 C 0.0171(4) 0.1444(3) 0.3668(2) 0.0263(10) 0.518(6) Uiso D . P 2 1 C19 C 0.1214(4) 0.1329(3) 0.3097(2) 0.0267(10) 0.518(6) Uiso D . P 2 1 C20 C 0.0308(4) 0.1859(4) 0.1923(3) 0.0306(11) 0.518(6) Uiso D . P 2 1 C21 C -0.0382(4) 0.2838(4) 0.1612(3) 0.0282(10) 0.518(6) Uiso D . P 2 1 C66 C -0.1653(4) 0.3282(4) 0.2985(3) 0.0283(11) 0.482(6) Uiso D . P 2 2 C67 C -0.1239(4) 0.2399(5) 0.3616(3) 0.0253(11) 0.482(6) Uiso D . P 2 2 C68 C 0.0608(5) 0.1544(4) 0.3759(3) 0.0255(11) 0.482(6) Uiso D . P 2 2 C69 C 0.0793(5) 0.1230(4) 0.2981(3) 0.0295(11) 0.482(6) Uiso D . P 2 2 C70 C 0.0550(4) 0.2292(5) 0.1665(3) 0.0343(12) 0.482(6) Uiso D . P 2 2 C71 C -0.0684(5) 0.2557(4) 0.1892(3) 0.0326(12) 0.482(6) Uiso D . P 2 2 C22 C -0.1323(2) 0.4447(2) 0.17822(15) 0.0375 1.0000 Uani . . . . . C23 C 0.0005(2) 0.2846(2) 0.44434(13) 0.0351 1.0000 Uani . . . . . C24 C 0.2365(2) 0.2019(2) 0.19271(19) 0.0490 1.0000 Uani . . . . . B1 B 0.39925(19) 0.07004(18) 0.74857(14) 0.0224 1.0000 Uani . . . . . C25 C 0.50398(17) 0.14364(16) 0.69023(12) 0.0228 1.0000 Uani . . . . . C26 C 0.47731(17) 0.24034(17) 0.63977(13) 0.0261 1.0000 Uani . . . . . C27 C 0.55427(19) 0.30466(17) 0.58404(13) 0.0285 1.0000 Uani . . . . . C28 C 0.66702(18) 0.27342(17) 0.57554(12) 0.0268 1.0000 Uani . . . . . C29 C 0.69876(17) 0.17823(17) 0.62243(12) 0.0246 1.0000 Uani . . . . . C30 C 0.61759(17) 0.11552(16) 0.67760(12) 0.0226 1.0000 Uani . . . . . F1 F 0.36828(10) 0.27579(10) 0.64521(8) 0.0342 1.0000 Uani . . . . . F2 F 0.52171(13) 0.39648(11) 0.53745(8) 0.0415 1.0000 Uani . . . . . F3 F 0.74423(12) 0.33535(11) 0.52142(8) 0.0378 1.0000 Uani . . . . . F4 F 0.80839(10) 0.14558(11) 0.61428(8) 0.0335 1.0000 Uani . . . . . F5 F 0.65720(10) 0.02146(10) 0.71919(7) 0.0293 1.0000 Uani . . . . . C31 C 0.44061(16) -0.03743(16) 0.81117(12) 0.0227 1.0000 Uani . . . . . C32 C 0.50732(17) -0.02389(16) 0.86431(12) 0.0244 1.0000 Uani . . . . . C33 C 0.53626(18) -0.10534(19) 0.92456(13) 0.0298 1.0000 Uani . . . . . C34 C 0.49733(19) -0.20843(18) 0.93504(13) 0.0315 1.0000 Uani . . . . . C35 C 0.43067(19) -0.22723(17) 0.88466(14) 0.0312 1.0000 Uani . . . . . C36 C 0.40368(17) -0.14266(17) 0.82499(13) 0.0270 1.0000 Uani . . . . . F6 F 0.54751(11) 0.07543(10) 0.85838(7) 0.0309 1.0000 Uani . . . . . F7 F 0.60205(13) -0.08529(12) 0.97316(8) 0.0422 1.0000 Uani . . . . . F8 F 0.52246(14) -0.28853(12) 0.99420(9) 0.0469 1.0000 Uani . . . . . F9 F 0.38981(14) -0.32690(11) 0.89459(9) 0.0452 1.0000 Uani . . . . . F10 F 0.33491(12) -0.16997(10) 0.78038(8) 0.0366 1.0000 Uani . . . . . C37 C 0.33107(17) 0.04007(16) 0.68385(12) 0.0249 1.0000 Uani . . . . . C38 C 0.38751(18) -0.02030(17) 0.63398(13) 0.0280 1.0000 Uani . . . . . C39 C 0.3470(2) -0.03862(18) 0.57125(13) 0.0338 1.0000 Uani . . . . . C40 C 0.2438(2) 0.00472(19) 0.55498(14) 0.0357 1.0000 Uani . . . . . C41 C 0.18376(19) 0.06480(18) 0.60176(14) 0.0320 1.0000 Uani . . . . . C42 C 0.22739(18) 0.08170(17) 0.66451(13) 0.0271 1.0000 Uani . . . . . F11 F 0.49050(11) -0.06379(11) 0.64571(8) 0.0347 1.0000 Uani . . . . . F12 F 0.40718(14) -0.09856(13) 0.52585(9) 0.0485 1.0000 Uani . . . . . F13 F 0.20159(15) -0.01292(13) 0.49404(9) 0.0501 1.0000 Uani . . . . . F14 F 0.08144(13) 0.10742(12) 0.58707(9) 0.0468 1.0000 Uani . . . . . F15 F 0.16262(11) 0.14504(11) 0.70537(8) 0.0339 1.0000 Uani . . . . . C43 C 0.32061(17) 0.13591(17) 0.80769(12) 0.0249 1.0000 Uani . . . . . C44 C 0.22319(18) 0.08797(18) 0.85474(13) 0.0288 1.0000 Uani . . . . . C45 C 0.1574(2) 0.1297(2) 0.91158(14) 0.0371 1.0000 Uani . . . . . C46 C 0.1889(2) 0.2249(2) 0.92470(14) 0.0383 1.0000 Uani . . . . . C47 C 0.2839(2) 0.2765(2) 0.88053(14) 0.0345 1.0000 Uani . . . . . C48 C 0.34750(18) 0.23204(18) 0.82375(13) 0.0281 1.0000 Uani . . . . . F16 F 0.18807(11) -0.00644(11) 0.84521(8) 0.0355 1.0000 Uani . . . . . F17 F 0.06343(13) 0.07906(14) 0.95394(9) 0.0526 1.0000 Uani . . . . . F18 F 0.12554(15) 0.26615(15) 0.98052(9) 0.0560 1.0000 Uani . . . . . F19 F 0.31517(13) 0.37019(12) 0.89250(10) 0.0471 1.0000 Uani . . . . . F20 F 0.44033(11) 0.28823(11) 0.78474(8) 0.0360 1.0000 Uani . . . . . H21 H 0.3807 0.4420 0.4197 0.0497 0.614 Uiso . . . 1 1 H22 H 0.2431 0.4287 0.4370 0.0497 0.614 Uiso . . . 1 1 H23 H 0.3028 0.5175 0.3604 0.0497 0.614 Uiso . . . 1 1 H31 H 0.4947 0.3780 0.3093 0.0624 0.614 Uiso . . . 1 1 H32 H 0.4175 0.4570 0.2512 0.0624 0.614 Uiso . . . 1 1 H33 H 0.4322 0.3289 0.2516 0.0624 0.614 Uiso . . . 1 1 H41 H 0.4044 0.2427 0.4250 0.0474 0.614 Uiso . . . 1 1 H42 H 0.2664 0.2326 0.4442 0.0474 0.614 Uiso . . . 1 1 H43 H 0.3378 0.1886 0.3720 0.0474 0.614 Uiso . . . 1 1 H521 H 0.4206 0.4564 0.3833 0.0665 0.386 Uiso . . . 1 2 H522 H 0.2856 0.4878 0.3956 0.0665 0.386 Uiso . . . 1 2 H523 H 0.3615 0.5192 0.3087 0.0665 0.386 Uiso . . . 1 2 H531 H 0.4963 0.3209 0.3105 0.0610 0.386 Uiso . . . 1 2 H532 H 0.4328 0.3816 0.2376 0.0610 0.386 Uiso . . . 1 2 H533 H 0.4100 0.2536 0.2789 0.0610 0.386 Uiso . . . 1 2 H541 H 0.3912 0.2659 0.4434 0.0488 0.386 Uiso . . . 1 2 H542 H 0.2534 0.2789 0.4618 0.0488 0.386 Uiso . . . 1 2 H543 H 0.3102 0.1946 0.4106 0.0488 0.386 Uiso . . . 1 2 H61 H 0.2201 0.6115 0.0826 0.0335 1.0000 Uiso . . . . . H71 H 0.3685 0.5026 0.0361 0.0647 1.0000 Uiso . . . . . H72 H 0.3606 0.4920 0.1292 0.0647 1.0000 Uiso . . . . . H73 H 0.3107 0.3962 0.0990 0.0647 1.0000 Uiso . . . . . H81 H 0.2023 0.5455 -0.0268 0.0822 1.0000 Uiso . . . . . H82 H 0.0785 0.5644 0.0228 0.0822 1.0000 Uiso . . . . . H83 H 0.1317 0.4423 0.0309 0.0822 1.0000 Uiso . . . . . H91 H -0.0099 0.7138 0.1798 0.0319 1.0000 Uiso . . . . . H92 H 0.0577 0.6843 0.1005 0.0319 1.0000 Uiso . . . . . H101 H 0.2870 0.9020 0.0434 0.0547 1.0000 Uiso . . . . . H102 H 0.1608 0.8886 0.0241 0.0547 1.0000 Uiso . . . . . H103 H 0.2565 0.7934 0.0188 0.0547 1.0000 Uiso . . . . . H111 H 0.1773 0.9398 0.1995 0.0598 1.0000 Uiso . . . . . H112 H 0.0539 0.9267 0.1758 0.0598 1.0000 Uiso . . . . . H113 H 0.0870 0.8521 0.2572 0.0598 1.0000 Uiso . . . . . H121 H 0.3554 0.7603 0.1945 0.0516 1.0000 Uiso . . . . . H122 H 0.2651 0.6726 0.2522 0.0516 1.0000 Uiso . . . . . H123 H 0.3256 0.6527 0.1682 0.0516 1.0000 Uiso . . . . . H131 H -0.0222 0.6775 0.2863 0.0332 1.0000 Uiso . . . . . H141 H 0.0199 0.6559 0.4151 0.0714 1.0000 Uiso . . . . . H142 H 0.1315 0.6306 0.3558 0.0714 1.0000 Uiso . . . . . H143 H 0.0592 0.5309 0.4166 0.0714 1.0000 Uiso . . . . . H151 H -0.1692 0.6307 0.3934 0.0561 1.0000 Uiso . . . . . H152 H -0.1443 0.5029 0.3957 0.0561 1.0000 Uiso . . . . . H153 H -0.1905 0.5829 0.3209 0.0561 1.0000 Uiso . . . . . H161 H -0.2408 0.3057 0.2811 0.0318 0.518 Uiso . . . 2 1 H162 H -0.1545 0.2021 0.2807 0.0318 0.518 Uiso . . . 2 1 H171 H -0.1517 0.3593 0.3702 0.0311 0.518 Uiso . . . 2 1 H172 H -0.1821 0.2313 0.4052 0.0311 0.518 Uiso . . . 2 1 H181 H 0.0287 0.1017 0.4197 0.0315 0.518 Uiso . . . 2 1 H182 H -0.0489 0.1149 0.3514 0.0315 0.518 Uiso . . . 2 1 H191 H 0.1899 0.1445 0.3315 0.0320 0.518 Uiso . . . 2 1 H192 H 0.1243 0.0583 0.3010 0.0320 0.518 Uiso . . . 2 1 H201 H -0.0204 0.1309 0.2303 0.0367 0.518 Uiso . . . 2 1 H202 H 0.0678 0.1550 0.1482 0.0367 0.518 Uiso . . . 2 1 H211 H 0.0099 0.3324 0.1163 0.0339 0.518 Uiso . . . 2 1 H212 H -0.1050 0.2600 0.1432 0.0339 0.518 Uiso . . . 2 1 H661 H -0.1756 0.3968 0.3163 0.0340 0.482 Uiso . . . 2 2 H662 H -0.2396 0.3065 0.2888 0.0340 0.482 Uiso . . . 2 2 H671 H -0.1750 0.2378 0.4121 0.0304 0.482 Uiso . . . 2 2 H672 H -0.1264 0.1689 0.3479 0.0304 0.482 Uiso . . . 2 2 H681 H 0.1359 0.1654 0.3899 0.0307 0.482 Uiso . . . 2 2 H682 H 0.0195 0.0953 0.4171 0.0307 0.482 Uiso . . . 2 2 H691 H 0.1366 0.0627 0.3000 0.0354 0.482 Uiso . . . 2 2 H692 H 0.0058 0.0979 0.2896 0.0354 0.482 Uiso . . . 2 2 H701 H 0.0894 0.2895 0.1228 0.0411 0.482 Uiso . . . 2 2 H702 H 0.0604 0.1606 0.1486 0.0411 0.482 Uiso . . . 2 2 H711 H -0.1056 0.1918 0.2280 0.0392 0.482 Uiso . . . 2 2 H712 H -0.1058 0.2725 0.1418 0.0392 0.482 Uiso . . . 2 2 H221 H -0.2029 0.4247 0.1624 0.0468 1.0000 Uiso . . . . . H222 H -0.1516 0.4978 0.2111 0.0468 1.0000 Uiso . . . . . H223 H -0.0773 0.4779 0.1307 0.0468 1.0000 Uiso . . . . . H231 H -0.0471 0.2336 0.4881 0.0418 1.0000 Uiso . . . . . H232 H -0.0265 0.3606 0.4427 0.0418 1.0000 Uiso . . . . . H233 H 0.0815 0.2773 0.4524 0.0418 1.0000 Uiso . . . . . H241 H 0.2433 0.1317 0.1769 0.0562 1.0000 Uiso . . . . . H242 H 0.2915 0.2021 0.2288 0.0562 1.0000 Uiso . . . . . H243 H 0.2537 0.2630 0.1454 0.0562 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 0.02300(17) 0.01771(16) 0.01723(16) -0.00461(12) -0.00261(13) 0.00097(12) N1 0.0270(9) 0.0239(8) 0.0255(9) -0.0039(7) -0.0050(7) 0.0005(7) C1 0.0295(11) 0.0377(12) 0.0377(13) -0.0049(10) -0.0140(10) 0.0007(9) N2 0.0278(9) 0.0214(8) 0.0170(8) -0.0052(6) -0.0009(7) -0.0002(6) C5 0.0250(10) 0.0207(9) 0.0207(9) -0.0059(7) -0.0071(8) 0.0012(7) N3 0.0277(9) 0.0205(8) 0.0182(8) -0.0068(6) -0.0024(7) 0.0023(6) C6 0.0372(12) 0.0259(10) 0.0206(10) -0.0066(8) 0.0030(9) -0.0060(9) C7 0.0544(18) 0.0464(16) 0.0611(19) 0.0121(14) 0.0295(15) 0.0132(13) C8 0.090(2) 0.095(3) 0.0201(12) -0.0166(14) 0.0054(14) -0.050(2) C9 0.0349(11) 0.0216(10) 0.0233(10) -0.0042(8) -0.0061(8) 0.0017(8) Si1 0.0329(3) 0.0247(3) 0.0344(3) -0.0076(2) -0.0046(3) -0.0026(2) C10 0.0421(14) 0.0428(15) 0.0519(16) -0.0088(12) 0.0028(12) -0.0085(11) C11 0.0489(16) 0.0443(15) 0.0562(17) -0.0218(13) -0.0031(13) -0.0085(12) C12 0.0395(13) 0.0363(13) 0.0531(16) -0.0068(11) -0.0183(12) -0.0053(10) C13 0.0357(11) 0.0237(10) 0.0237(10) -0.0090(8) -0.0007(9) 0.0037(8) C14 0.0592(18) 0.070(2) 0.0491(16) -0.0449(15) -0.0160(14) 0.0068(15) C15 0.0358(13) 0.0466(15) 0.0579(17) -0.0279(13) 0.0068(12) 0.0061(11) N4 0.0298(9) 0.0273(9) 0.0246(9) -0.0052(7) -0.0078(7) -0.0012(7) N5 0.0271(9) 0.0241(8) 0.0184(8) -0.0043(7) -0.0009(7) 0.0003(7) N6 0.0306(9) 0.0224(8) 0.0254(9) -0.0071(7) 0.0012(7) 0.0010(7) C22 0.0423(13) 0.0349(12) 0.0398(13) -0.0059(10) -0.0243(11) 0.0013(10) C23 0.0402(13) 0.0459(14) 0.0183(10) -0.0045(9) -0.0049(9) -0.0071(10) C24 0.0402(14) 0.0303(12) 0.0700(19) -0.0182(12) 0.0173(13) 0.0017(10) B1 0.0196(10) 0.0214(10) 0.0257(11) -0.0043(9) -0.0045(8) 0.0012(8) C25 0.0233(10) 0.0207(9) 0.0249(10) -0.0059(8) -0.0054(8) 0.0002(7) C26 0.0226(10) 0.0257(10) 0.0306(11) -0.0069(8) -0.0060(8) 0.0017(8) C27 0.0349(11) 0.0212(10) 0.0282(11) -0.0018(8) -0.0082(9) 0.0001(8) C28 0.0297(11) 0.0281(11) 0.0219(10) -0.0069(8) 0.0012(8) -0.0068(8) C29 0.0213(9) 0.0297(11) 0.0245(10) -0.0109(8) -0.0020(8) 0.0001(8) C30 0.0255(10) 0.0208(9) 0.0216(9) -0.0048(7) -0.0056(8) 0.0019(7) F1 0.0240(6) 0.0280(6) 0.0457(8) 0.0008(6) -0.0084(6) 0.0049(5) F2 0.0451(8) 0.0289(7) 0.0416(8) 0.0102(6) -0.0102(6) -0.0005(6) F3 0.0365(7) 0.0395(7) 0.0296(7) -0.0003(6) 0.0068(6) -0.0104(6) F4 0.0216(6) 0.0421(7) 0.0342(7) -0.0095(6) 0.0020(5) 0.0019(5) F5 0.0231(6) 0.0276(6) 0.0327(7) -0.0006(5) -0.0043(5) 0.0062(5) C31 0.0195(9) 0.0234(10) 0.0230(9) -0.0036(8) -0.0011(7) 0.0022(7) C32 0.0209(9) 0.0235(10) 0.0264(10) -0.0034(8) -0.0017(8) 0.0008(7) C33 0.0262(10) 0.0391(12) 0.0238(10) -0.0062(9) -0.0060(8) 0.0020(9) C34 0.0334(12) 0.0305(11) 0.0243(10) 0.0021(9) -0.0018(9) 0.0054(9) C35 0.0322(11) 0.0219(10) 0.0342(11) -0.0006(9) 0.0007(9) -0.0019(8) C36 0.0226(10) 0.0265(10) 0.0310(11) -0.0061(9) -0.0038(8) -0.0007(8) F6 0.0343(7) 0.0279(6) 0.0318(7) -0.0051(5) -0.0103(5) -0.0053(5) F7 0.0457(8) 0.0488(9) 0.0334(7) -0.0036(6) -0.0194(6) -0.0002(7) F8 0.0585(10) 0.0383(8) 0.0349(8) 0.0093(6) -0.0120(7) 0.0074(7) F9 0.0555(9) 0.0227(7) 0.0514(9) 0.0032(6) -0.0082(7) -0.0083(6) F10 0.0383(7) 0.0284(7) 0.0450(8) -0.0049(6) -0.0153(6) -0.0087(5) C37 0.0257(10) 0.0214(9) 0.0266(10) -0.0024(8) -0.0053(8) -0.0029(8) C38 0.0266(10) 0.0257(10) 0.0319(11) -0.0059(9) -0.0067(9) -0.0010(8) C39 0.0447(13) 0.0289(11) 0.0297(11) -0.0090(9) -0.0070(10) -0.0062(10) C40 0.0475(14) 0.0323(12) 0.0283(11) -0.0001(9) -0.0165(10) -0.0105(10) C41 0.0300(11) 0.0274(11) 0.0362(12) 0.0042(9) -0.0152(9) -0.0049(9) C42 0.0262(10) 0.0233(10) 0.0301(11) -0.0014(8) -0.0070(8) -0.0013(8) F11 0.0300(7) 0.0367(7) 0.0424(8) -0.0191(6) -0.0082(6) 0.0080(5) F12 0.0613(10) 0.0505(9) 0.0421(8) -0.0262(7) -0.0089(7) -0.0009(7) F13 0.0694(11) 0.0500(9) 0.0379(8) -0.0076(7) -0.0294(8) -0.0115(8) F14 0.0405(8) 0.0462(8) 0.0550(9) 0.0005(7) -0.0308(7) 0.0019(6) F15 0.0254(6) 0.0350(7) 0.0412(7) -0.0073(6) -0.0103(5) 0.0076(5) C43 0.0225(10) 0.0253(10) 0.0263(10) -0.0043(8) -0.0069(8) 0.0051(8) C44 0.0245(10) 0.0299(11) 0.0299(11) -0.0037(9) -0.0051(9) 0.0027(8) C45 0.0264(11) 0.0505(14) 0.0283(11) -0.0038(10) 0.0025(9) 0.0047(10) C46 0.0368(13) 0.0532(15) 0.0269(11) -0.0167(11) -0.0058(10) 0.0162(11) C47 0.0356(12) 0.0389(13) 0.0354(12) -0.0172(10) -0.0148(10) 0.0113(10) C48 0.0248(10) 0.0301(11) 0.0307(11) -0.0091(9) -0.0069(8) 0.0045(8) F16 0.0283(7) 0.0327(7) 0.0418(8) -0.0046(6) -0.0001(6) -0.0055(5) F17 0.0369(8) 0.0652(11) 0.0439(9) -0.0052(8) 0.0141(7) -0.0016(7) F18 0.0539(10) 0.0772(12) 0.0412(9) -0.0314(9) -0.0005(7) 0.0185(8) F19 0.0518(9) 0.0451(9) 0.0575(10) -0.0322(8) -0.0194(8) 0.0121(7) F20 0.0289(7) 0.0334(7) 0.0493(8) -0.0175(6) -0.0040(6) -0.0032(5) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N6 . 2.2968(17) yes Ti1 . N5 . 2.2787(17) yes Ti1 . N4 . 2.5252(18) yes Ti1 . N3 . 2.1276(16) yes Ti1 . N2 . 2.1083(17) yes Ti1 . N1 . 1.7085(18) yes N1 . C1 . 1.465(3) yes C1 . C4 . 1.531(5) yes C1 . C3 . 1.509(5) yes C1 . C2 . 1.562(5) yes C1 . C54 . 1.547(6) yes C1 . C53 . 1.583(7) yes C1 . C52 . 1.502(7) yes C2 . H23 . 1.000 no C2 . H22 . 1.000 no C2 . H21 . 1.000 no C3 . H33 . 1.000 no C3 . H32 . 1.000 no C3 . H31 . 1.000 no C4 . H43 . 1.000 no C4 . H42 . 1.000 no C4 . H41 . 1.000 no C52 . H523 . 1.000 no C52 . H522 . 1.000 no C52 . H521 . 1.000 no C53 . H533 . 1.000 no C53 . H532 . 1.000 no C53 . H531 . 1.000 no C54 . H543 . 1.000 no C54 . H542 . 1.000 no C54 . H541 . 1.000 no N2 . C6 . 1.468(3) yes N2 . C5 . 1.343(3) yes C5 . C9 . 1.498(3) yes C5 . N3 . 1.341(3) yes N3 . C13 . 1.472(2) yes C6 . H61 . 1.000 no C6 . C8 . 1.521(4) yes C6 . C7 . 1.508(4) yes C7 . H73 . 1.000 no C7 . H72 . 1.000 no C7 . H71 . 1.000 no C8 . H83 . 1.000 no C8 . H82 . 1.000 no C8 . H81 . 1.000 no C9 . H92 . 1.000 no C9 . H91 . 1.000 no C9 . Si1 . 1.882(2) yes Si1 . C12 . 1.843(3) yes Si1 . C11 . 1.845(3) yes Si1 . C10 . 1.847(3) yes C10 . H103 . 1.000 no C10 . H102 . 1.000 no C10 . H101 . 1.000 no C11 . H113 . 1.000 no C11 . H112 . 1.000 no C11 . H111 . 1.000 no C12 . H123 . 1.000 no C12 . H122 . 1.000 no C12 . H121 . 1.000 no C13 . H131 . 1.000 no C13 . C15 . 1.514(3) yes C13 . C14 . 1.518(4) yes C14 . H143 . 1.000 no C14 . H142 . 1.000 no C14 . H141 . 1.000 no C15 . H153 . 1.000 no C15 . H152 . 1.000 no C15 . H151 . 1.000 no N4 . C22 . 1.470(3) yes N4 . C21 . 1.534(5) yes N4 . C16 . 1.480(4) yes N4 . C22 . 1.470(3) yes N4 . C71 . 1.433(5) yes N4 . C66 . 1.523(5) yes N5 . C23 . 1.479(3) yes N5 . C18 . 1.487(4) yes N5 . C17 . 1.534(4) yes N5 . C23 . 1.479(3) yes N5 . C68 . 1.521(5) yes N5 . C67 . 1.448(5) yes N6 . C24 . 1.468(3) yes N6 . C20 . 1.500(5) yes N6 . C19 . 1.519(5) yes N6 . C24 . 1.468(3) yes N6 . C70 . 1.499(5) yes N6 . C69 . 1.480(5) yes C16 . H162 . 1.000 no C16 . H161 . 1.000 no C16 . C17 . 1.510(6) yes C17 . H172 . 1.000 no C17 . H171 . 1.000 no C18 . H182 . 1.000 no C18 . H181 . 1.000 no C18 . C19 . 1.501(6) yes C19 . H192 . 1.000 no C19 . H191 . 1.000 no C20 . H202 . 1.000 no C20 . H201 . 1.000 no C20 . C21 . 1.501(6) yes C21 . H212 . 1.000 no C21 . H211 . 1.000 no C66 . H662 . 1.000 no C66 . H661 . 1.000 no C66 . C67 . 1.515(6) yes C67 . H672 . 1.000 no C67 . H671 . 1.000 no C68 . H682 . 1.000 no C68 . H681 . 1.000 no C68 . C69 . 1.526(6) yes C69 . H692 . 1.000 no C69 . H691 . 1.000 no C70 . H702 . 1.000 no C70 . H701 . 1.000 no C70 . C71 . 1.507(7) yes C71 . H712 . 1.000 no C71 . H711 . 1.000 no C22 . H223 . 1.000 no C22 . H222 . 1.000 no C22 . H221 . 1.000 no C23 . H233 . 1.000 no C23 . H232 . 1.000 no C23 . H231 . 1.000 no C24 . H243 . 1.000 no C24 . H242 . 1.000 no C24 . H241 . 1.000 no B1 . C43 . 1.656(3) yes B1 . C37 . 1.657(3) yes B1 . C31 . 1.656(3) yes B1 . C25 . 1.655(3) yes C25 . C30 . 1.382(3) yes C25 . C26 . 1.395(3) yes C26 . F1 . 1.353(2) yes C26 . C27 . 1.372(3) yes C27 . F2 . 1.342(2) yes C27 . C28 . 1.380(3) yes C28 . F3 . 1.347(2) yes C28 . C29 . 1.371(3) yes C29 . F4 . 1.349(2) yes C29 . C30 . 1.388(3) yes C30 . F5 . 1.355(2) yes C31 . C36 . 1.386(3) yes C31 . C32 . 1.392(3) yes C32 . F6 . 1.353(2) yes C32 . C33 . 1.379(3) yes C33 . F7 . 1.348(3) yes C33 . C34 . 1.377(3) yes C34 . F8 . 1.342(3) yes C34 . C35 . 1.374(3) yes C35 . F9 . 1.346(3) yes C35 . C36 . 1.387(3) yes C36 . F10 . 1.355(3) yes C37 . C42 . 1.388(3) yes C37 . C38 . 1.391(3) yes C38 . F11 . 1.352(2) yes C38 . C39 . 1.375(3) yes C39 . F12 . 1.350(3) yes C39 . C40 . 1.374(4) yes C40 . F13 . 1.353(3) yes C40 . C41 . 1.367(4) yes C41 . F14 . 1.353(3) yes C41 . C42 . 1.388(3) yes C42 . F15 . 1.352(3) yes C43 . C48 . 1.394(3) yes C43 . C44 . 1.390(3) yes C44 . F16 . 1.356(3) yes C44 . C45 . 1.378(3) yes C45 . F17 . 1.343(3) yes C45 . C46 . 1.377(4) yes C46 . F18 . 1.350(3) yes C46 . C47 . 1.367(4) yes C47 . F19 . 1.349(3) yes C47 . C48 . 1.386(3) yes C48 . F20 . 1.345(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N6 . Ti1 . N5 . 77.06(6) yes N6 . Ti1 . N4 . 72.96(6) yes N5 . Ti1 . N4 . 72.96(6) yes N6 . Ti1 . N3 . 155.59(7) yes N5 . Ti1 . N3 . 104.38(6) yes N4 . Ti1 . N3 . 84.07(6) yes N6 . Ti1 . C5 . 133.90(6) yes N5 . Ti1 . C5 . 133.79(6) yes N4 . Ti1 . C5 . 84.30(6) yes N3 . Ti1 . C5 . 32.07(6) yes N6 . Ti1 . N2 . 104.97(6) yes N5 . Ti1 . N2 . 156.84(7) yes N4 . Ti1 . N2 . 85.46(6) yes N3 . Ti1 . N2 . 64.18(6) yes C5 . Ti1 . N2 . 32.11(6) yes N6 . Ti1 . N1 . 97.25(8) yes N5 . Ti1 . N1 . 96.68(7) yes N4 . Ti1 . N1 . 166.92(7) yes N3 . Ti1 . N1 . 106.66(8) yes C5 . Ti1 . N1 . 108.77(7) yes N2 . Ti1 . N1 . 105.80(8) yes C1 . N1 . Ti1 . 177.77(15) yes C4 . C1 . C3 . 111.1(3) yes C4 . C1 . C2 . 108.5(3) yes C3 . C1 . C2 . 108.4(3) yes C4 . C1 . N1 . 110.3(2) yes C3 . C1 . N1 . 110.7(3) yes C2 . C1 . N1 . 107.8(2) yes C54 . C1 . C53 . 104.9(5) yes C54 . C1 . C52 . 111.2(5) yes C53 . C1 . C52 . 107.2(5) yes C54 . C1 . N1 . 112.9(3) yes C53 . C1 . N1 . 108.0(3) yes C52 . C1 . N1 . 112.2(4) yes H23 . C2 . H22 . 109.480 no H23 . C2 . H21 . 109.468 no H22 . C2 . H21 . 109.483 no H23 . C2 . C1 . 109.461 no H22 . C2 . C1 . 109.472 no H21 . C2 . C1 . 109.463 no H33 . C3 . H32 . 109.476 no H33 . C3 . H31 . 109.471 no H32 . C3 . H31 . 109.481 no H33 . C3 . C1 . 109.463 no H32 . C3 . C1 . 109.470 no H31 . C3 . C1 . 109.467 no H43 . C4 . H42 . 109.476 no H43 . C4 . H41 . 109.485 no H42 . C4 . H41 . 109.463 no H43 . C4 . C1 . 109.476 no H42 . C4 . C1 . 109.460 no H41 . C4 . C1 . 109.467 no H523 . C52 . H522 . 109.477 no H523 . C52 . H521 . 109.456 no H522 . C52 . H521 . 109.499 no H523 . C52 . C1 . 109.449 no H522 . C52 . C1 . 109.481 no H521 . C52 . C1 . 109.466 no H533 . C53 . H532 . 109.475 no H533 . C53 . H531 . 109.469 no H532 . C53 . H531 . 109.484 no H533 . C53 . C1 . 109.461 no H532 . C53 . C1 . 109.472 no H531 . C53 . C1 . 109.468 no H543 . C54 . H542 . 109.484 no H543 . C54 . H541 . 109.496 no H542 . C54 . H541 . 109.456 no H543 . C54 . C1 . 109.480 no H542 . C54 . C1 . 109.451 no H541 . C54 . C1 . 109.460 no C6 . N2 . C5 . 119.40(17) yes C6 . N2 . Ti1 . 147.10(14) yes C5 . N2 . Ti1 . 91.33(12) yes C9 . C5 . N3 . 124.12(17) yes C9 . C5 . N2 . 121.94(18) yes N3 . C5 . N2 . 113.92(17) yes C9 . C5 . Ti1 . 178.47(14) yes N3 . C5 . Ti1 . 57.38(10) yes N2 . C5 . Ti1 . 56.56(10) yes C13 . N3 . Ti1 . 146.89(13) yes C13 . N3 . C5 . 120.17(17) yes Ti1 . N3 . C5 . 90.55(12) yes H61 . C6 . C8 . 107.249 no H61 . C6 . C7 . 107.719 no C8 . C6 . C7 . 111.1(3) yes H61 . C6 . N2 . 106.656 no C8 . C6 . N2 . 112.10(19) yes C7 . C6 . N2 . 111.67(19) yes H73 . C7 . H72 . 109.476 no H73 . C7 . H71 . 109.476 no H72 . C7 . H71 . 109.476 no H73 . C7 . C6 . 109.466 no H72 . C7 . C6 . 109.467 no H71 . C7 . C6 . 109.467 no H83 . C8 . H82 . 109.476 no H83 . C8 . H81 . 109.476 no H82 . C8 . H81 . 109.476 no H83 . C8 . C6 . 109.467 no H82 . C8 . C6 . 109.467 no H81 . C8 . C6 . 109.467 no H92 . C9 . H91 . 109.467 no H92 . C9 . Si1 . 107.271 no H91 . C9 . Si1 . 107.271 no H92 . C9 . C5 . 107.271 no H91 . C9 . C5 . 107.271 no Si1 . C9 . C5 . 118.11(15) yes C12 . Si1 . C11 . 110.84(14) yes C12 . Si1 . C10 . 111.33(13) yes C11 . Si1 . C10 . 108.70(14) yes C12 . Si1 . C9 . 109.04(11) yes C11 . Si1 . C9 . 108.98(11) yes C10 . Si1 . C9 . 107.88(11) yes H103 . C10 . H102 . 109.476 no H103 . C10 . H101 . 109.476 no H102 . C10 . H101 . 109.476 no H103 . C10 . Si1 . 109.467 no H102 . C10 . Si1 . 109.467 no H101 . C10 . Si1 . 109.467 no H113 . C11 . H112 . 109.476 no H113 . C11 . H111 . 109.476 no H112 . C11 . H111 . 109.476 no H113 . C11 . Si1 . 109.466 no H112 . C11 . Si1 . 109.467 no H111 . C11 . Si1 . 109.467 no H123 . C12 . H122 . 109.476 no H123 . C12 . H121 . 109.476 no H122 . C12 . H121 . 109.476 no H123 . C12 . Si1 . 109.467 no H122 . C12 . Si1 . 109.466 no H121 . C12 . Si1 . 109.467 no H131 . C13 . C15 . 106.542 no H131 . C13 . C14 . 109.754 no C15 . C13 . C14 . 110.2(2) yes H131 . C13 . N3 . 106.260 no C15 . C13 . N3 . 113.43(18) yes C14 . C13 . N3 . 110.46(19) yes H143 . C14 . H142 . 109.476 no H143 . C14 . H141 . 109.476 no H142 . C14 . H141 . 109.476 no H143 . C14 . C13 . 109.467 no H142 . C14 . C13 . 109.466 no H141 . C14 . C13 . 109.467 no H153 . C15 . H152 . 109.476 no H153 . C15 . H151 . 109.476 no H152 . C15 . H151 . 109.476 no H153 . C15 . C13 . 109.466 no H152 . C15 . C13 . 109.467 no H151 . C15 . C13 . 109.466 no C22 . N4 . C21 . 102.9(2) yes C22 . N4 . C16 . 114.3(2) yes C21 . N4 . C16 . 108.6(3) yes C22 . N4 . Ti1 . 116.04(13) yes C21 . N4 . Ti1 . 102.10(19) yes C16 . N4 . Ti1 . 111.46(18) yes C22 . N4 . C71 . 115.9(3) yes C22 . N4 . C66 . 99.4(2) yes C71 . N4 . C66 . 113.0(3) yes C22 . N4 . Ti1 . 116.04(13) yes C71 . N4 . Ti1 . 110.0(2) yes C66 . N4 . Ti1 . 101.00(19) yes C23 . N5 . C18 . 115.6(2) yes C23 . N5 . C17 . 102.4(2) yes C18 . N5 . C17 . 109.7(3) yes C23 . N5 . Ti1 . 109.43(13) yes C18 . N5 . Ti1 . 110.94(18) yes C17 . N5 . Ti1 . 108.24(19) yes C23 . N5 . C68 . 101.3(2) yes C23 . N5 . C67 . 113.9(2) yes C68 . N5 . C67 . 110.2(3) yes C23 . N5 . Ti1 . 109.43(13) yes C68 . N5 . Ti1 . 101.7(2) yes C67 . N5 . Ti1 . 118.2(2) yes C24 . N6 . C20 . 113.5(2) yes C24 . N6 . C19 . 101.1(2) yes C20 . N6 . C19 . 109.5(3) yes C24 . N6 . Ti1 . 111.15(14) yes C20 . N6 . Ti1 . 117.9(2) yes C19 . N6 . Ti1 . 101.67(19) yes C24 . N6 . C70 . 101.0(3) yes C24 . N6 . C69 . 115.0(3) yes C70 . N6 . C69 . 112.3(3) yes C24 . N6 . Ti1 . 111.15(14) yes C70 . N6 . Ti1 . 105.8(2) yes C69 . N6 . Ti1 . 110.8(2) yes H162 . C16 . H161 . 109.467 no H162 . C16 . C17 . 109.636 no H161 . C16 . C17 . 109.636 no H162 . C16 . N4 . 109.635 no H161 . C16 . N4 . 109.636 no C17 . C16 . N4 . 108.8(3) yes H172 . C17 . H171 . 109.467 no H172 . C17 . C16 . 108.689 no H171 . C17 . C16 . 108.688 no H172 . C17 . N5 . 108.689 no H171 . C17 . N5 . 108.688 no C16 . C17 . N5 . 112.6(3) yes H182 . C18 . H181 . 109.466 no H182 . C18 . C19 . 108.601 no H181 . C18 . C19 . 108.603 no H182 . C18 . N5 . 108.602 no H181 . C18 . N5 . 108.603 no C19 . C18 . N5 . 112.9(3) yes H192 . C19 . H191 . 109.466 no H192 . C19 . C18 . 109.053 no H191 . C19 . C18 . 109.052 no H192 . C19 . N6 . 109.053 no H191 . C19 . N6 . 109.052 no C18 . C19 . N6 . 111.1(3) yes H202 . C20 . H201 . 109.466 no H202 . C20 . C21 . 109.113 no H201 . C20 . C21 . 109.113 no H202 . C20 . N6 . 109.113 no H201 . C20 . N6 . 109.113 no C21 . C20 . N6 . 110.9(3) yes H212 . C21 . H211 . 109.466 no H212 . C21 . C20 . 108.801 no H211 . C21 . C20 . 108.800 no H212 . C21 . N4 . 108.801 no H211 . C21 . N4 . 108.800 no C20 . C21 . N4 . 112.1(3) yes H662 . C66 . H661 . 109.467 no H662 . C66 . C67 . 109.004 no H661 . C66 . C67 . 109.005 no H662 . C66 . N4 . 109.004 no H661 . C66 . N4 . 109.005 no C67 . C66 . N4 . 111.3(3) yes H672 . C67 . H671 . 109.467 no H672 . C67 . N5 . 108.921 no H671 . C67 . N5 . 108.921 no H672 . C67 . C66 . 108.921 no H671 . C67 . C66 . 108.920 no N5 . C67 . C66 . 111.7(4) yes H682 . C68 . H681 . 109.467 no H682 . C68 . C69 . 109.341 no H681 . C68 . C69 . 109.342 no H682 . C68 . N5 . 109.342 no H681 . C68 . N5 . 109.343 no C69 . C68 . N5 . 110.0(4) yes H692 . C69 . H691 . 109.467 no H692 . C69 . N6 . 108.856 no H691 . C69 . N6 . 108.855 no H692 . C69 . C68 . 108.856 no H691 . C69 . C68 . 108.855 no N6 . C69 . C68 . 111.9(4) yes H702 . C70 . H701 . 109.467 no H702 . C70 . C71 . 108.677 no H701 . C70 . C71 . 108.678 no H702 . C70 . N6 . 108.677 no H701 . C70 . N6 . 108.677 no C71 . C70 . N6 . 112.6(4) yes H712 . C71 . H711 . 109.467 no H712 . C71 . N4 . 109.077 no H711 . C71 . N4 . 109.078 no H712 . C71 . C70 . 109.077 no H711 . C71 . C70 . 109.078 no N4 . C71 . C70 . 111.0(4) yes H223 . C22 . H222 . 109.476 no H223 . C22 . H221 . 109.476 no H222 . C22 . H221 . 109.476 no H223 . C22 . N4 . 109.466 no H222 . C22 . N4 . 109.467 no H221 . C22 . N4 . 109.466 no H233 . C23 . H232 . 109.476 no H233 . C23 . H231 . 109.476 no H232 . C23 . H231 . 109.476 no H233 . C23 . N5 . 109.467 no H232 . C23 . N5 . 109.467 no H231 . C23 . N5 . 109.467 no H243 . C24 . H242 . 109.476 no H243 . C24 . H241 . 109.476 no H242 . C24 . H241 . 109.476 no H243 . C24 . N6 . 109.467 no H242 . C24 . N6 . 109.467 no H241 . C24 . N6 . 109.467 no C43 . B1 . C37 . 114.00(16) yes C43 . B1 . C31 . 101.53(16) yes C37 . B1 . C31 . 113.72(16) yes C43 . B1 . C25 . 113.01(16) yes C37 . B1 . C25 . 100.54(16) yes C31 . B1 . C25 . 114.65(16) yes C30 . C25 . C26 . 113.22(18) yes C30 . C25 . B1 . 127.65(18) yes C26 . C25 . B1 . 118.64(17) yes F1 . C26 . C27 . 116.12(19) yes F1 . C26 . C25 . 119.01(18) yes C27 . C26 . C25 . 124.87(19) yes F2 . C27 . C28 . 119.62(19) yes F2 . C27 . C26 . 121.3(2) yes C28 . C27 . C26 . 119.12(19) yes F3 . C28 . C29 . 120.74(19) yes F3 . C28 . C27 . 120.24(19) yes C29 . C28 . C27 . 119.02(19) yes F4 . C29 . C30 . 120.39(18) yes F4 . C29 . C28 . 119.89(18) yes C30 . C29 . C28 . 119.71(19) yes F5 . C30 . C25 . 120.97(18) yes F5 . C30 . C29 . 115.00(17) yes C25 . C30 . C29 . 124.02(19) yes C36 . C31 . C32 . 113.08(18) yes C36 . C31 . B1 . 126.81(18) yes C32 . C31 . B1 . 119.51(18) yes F6 . C32 . C33 . 115.99(19) yes F6 . C32 . C31 . 119.28(18) yes C33 . C32 . C31 . 124.7(2) yes F7 . C33 . C34 . 119.7(2) yes F7 . C33 . C32 . 120.9(2) yes C34 . C33 . C32 . 119.4(2) yes F8 . C34 . C35 . 120.7(2) yes F8 . C34 . C33 . 120.5(2) yes C35 . C34 . C33 . 118.8(2) yes F9 . C35 . C36 . 120.4(2) yes F9 . C35 . C34 . 119.9(2) yes C36 . C35 . C34 . 119.7(2) yes F10 . C36 . C31 . 121.17(19) yes F10 . C36 . C35 . 114.53(19) yes C31 . C36 . C35 . 124.3(2) yes C42 . C37 . C38 . 113.39(19) yes C42 . C37 . B1 . 127.16(18) yes C38 . C37 . B1 . 118.71(18) yes F11 . C38 . C39 . 116.0(2) yes F11 . C38 . C37 . 119.24(19) yes C39 . C38 . C37 . 124.7(2) yes F12 . C39 . C40 . 119.8(2) yes F12 . C39 . C38 . 120.9(2) yes C40 . C39 . C38 . 119.2(2) yes F13 . C40 . C41 . 120.5(2) yes F13 . C40 . C39 . 120.4(2) yes C41 . C40 . C39 . 119.0(2) yes F14 . C41 . C42 . 120.0(2) yes F14 . C41 . C40 . 119.9(2) yes C42 . C41 . C40 . 120.1(2) yes F15 . C42 . C37 . 121.37(19) yes F15 . C42 . C41 . 115.10(19) yes C37 . C42 . C41 . 123.5(2) yes C48 . C43 . C44 . 113.25(19) yes C48 . C43 . B1 . 126.91(19) yes C44 . C43 . B1 . 119.37(18) yes F16 . C44 . C45 . 116.3(2) yes F16 . C44 . C43 . 119.10(19) yes C45 . C44 . C43 . 124.6(2) yes F17 . C45 . C46 . 119.8(2) yes F17 . C45 . C44 . 121.0(2) yes C46 . C45 . C44 . 119.2(2) yes F18 . C46 . C47 . 121.0(2) yes F18 . C46 . C45 . 119.7(2) yes C47 . C46 . C45 . 119.3(2) yes F19 . C47 . C48 . 120.5(2) yes F19 . C47 . C46 . 119.9(2) yes C48 . C47 . C46 . 119.7(2) yes F20 . C48 . C47 . 114.8(2) yes F20 . C48 . C43 . 121.28(19) yes C47 . C48 . C43 . 123.9(2) yes ##end data_Compound_7-BArF4 _database_code_depnum_ccdc_archive 'CCDC 268644' # Local code ARC1127 _chemical_name_systematic ; [Ti(NtBu)(Me3[9]aneN3)(u-Me)2AlMe2][B(C6F5)4] ; #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_melting_point ? _exptl_crystal_thermal_history ; The material was crystallised at ambient temperature. A suitable crystal was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. ; _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed #============================================================= _cell_length_a 13.7837(2) _cell_angle_alpha 90 _cell_length_b 19.5766(3) _cell_angle_beta 109.7558(7) _cell_length_c 18.6673(2) _cell_angle_gamma 90 _cell_volume 4740.67(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 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 ' 0.0033 0.0016 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 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Al ' 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 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 ' 0.1484 0.1585 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 ' 0.0171 0.0103 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 ' 0.0061 0.0033 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 ' 0.2776 0.4457 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 _cell_formula_units_Z 4 _chemical_formula_sum ' C42 H44 Al B Cl2 F20 N4 Ti ' _chemical_formula_moiety ' C17 H42 Al N4 Ti, C24 B F20, C H2 Cl2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1141.40 _cell_measurement_reflns_used 47232 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' orange-yellow ' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.428 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.97 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 47232 _reflns_number_total 10760 #11071 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_min 5.110 _diffrn_reflns_theta_max 27.482 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.482 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _refine_diff_density_min -0.38 _refine_diff_density_max 0.56 _refine_ls_number_reflns 7266 _refine_ls_number_restraints 10 _refine_ls_number_parameters 716 #_refine_ls_R_factor_ref 0.0359 _refine_ls_wR_factor_ref 0.0371 _refine_ls_goodness_of_fit_ref 1.1037 #_reflns_number_all 10760 _refine_ls_R_factor_all 0.0658 _refine_ls_wR_factor_all 0.0533 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 7266 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_gt 0.0371 _refine_ls_shift/su_max 0.045157 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.85 -0.349 1.07 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group Ti1 Ti 0.68419(2) 0.315521(17) 0.631507(18) 0.0131 1.0000 Uani . . . . . C1 C 0.81217(15) 0.23313(10) 0.64361(12) 0.0192 1.0000 Uani . . . . . C2 C 0.56218(17) 0.23082(11) 0.62494(14) 0.0239 1.0000 Uani . . . . . Al1 Al 0.68194(5) 0.17121(3) 0.61584(4) 0.0211 1.0000 Uani . . . . . C3 C 0.6499(2) 0.12888(14) 0.51518(16) 0.0384 1.0000 Uani . . . . . C4 C 0.7067(2) 0.10083(12) 0.69633(17) 0.0358 1.0000 Uani . . . . . N1 N 0.65174(12) 0.32699(8) 0.53612(9) 0.0169 1.0000 Uani . . . . . C5 C 0.62440(17) 0.33346(11) 0.45361(11) 0.0242 1.0000 Uani . . . . . C6 C 0.6200(2) 0.40894(13) 0.43199(13) 0.0388 1.0000 Uani . . . . . C7 C 0.5193(2) 0.30068(15) 0.41513(13) 0.0416 1.0000 Uani . . . . . C8 C 0.7076(2) 0.29801(15) 0.43008(13) 0.0405 1.0000 Uani . . . . . N2 N 0.73270(13) 0.31786(9) 0.76837(9) 0.0230 1.0000 Uani . . . . . N3 N 0.79723(12) 0.40474(8) 0.66767(10) 0.0203 1.0000 Uani . . . . . N4 N 0.58371(12) 0.39946(8) 0.65553(9) 0.0182 1.0000 Uani . . . . . C9 C 0.83981(17) 0.34536(12) 0.79326(12) 0.0288 1.0000 Uani . . . . . C10 C 0.84821(17) 0.41061(12) 0.75250(13) 0.0290 1.0000 Uani . . . . . C11 C 0.72896(16) 0.46523(10) 0.63777(13) 0.0248 1.0000 Uani . . . . . C12 C 0.63917(16) 0.46667(10) 0.66623(13) 0.0241 1.0000 Uani . . . . . C13 C 0.56405(17) 0.37952(11) 0.72665(12) 0.0259 1.0000 Uani . . . . . C14 C 0.66227(18) 0.36527(12) 0.79135(12) 0.0305 1.0000 Uani . . . . . C15 C 0.73589(19) 0.25115(13) 0.80677(12) 0.0327 1.0000 Uani . . . . . C16 C 0.87699(16) 0.40575(11) 0.63061(14) 0.0271 1.0000 Uani . . . . . C17 C 0.48254(15) 0.40726(11) 0.59372(13) 0.0250 1.0000 Uani . . . . . B1 B 0.17271(16) 0.19434(11) 0.60739(12) 0.0156 1.0000 Uani . . . . . C18 C 0.26061(14) 0.13995(10) 0.60036(11) 0.0167 1.0000 Uani . . . . . C19 C 0.31436(16) 0.09936(10) 0.66235(11) 0.0198 1.0000 Uani . . . . . C20 C 0.38800(16) 0.05184(11) 0.66253(11) 0.0238 1.0000 Uani . . . . . C21 C 0.41133(16) 0.04074(11) 0.59728(12) 0.0233 1.0000 Uani . . . . . C22 C 0.35812(16) 0.07734(11) 0.53321(11) 0.0219 1.0000 Uani . . . . . C23 C 0.28546(15) 0.12520(10) 0.53578(11) 0.0195 1.0000 Uani . . . . . F1 F 0.29558(10) 0.10673(7) 0.72863(7) 0.0288 1.0000 Uani . . . . . F2 F 0.43889(11) 0.01640(7) 0.72629(7) 0.0355 1.0000 Uani . . . . . F3 F 0.48440(10) -0.00432(7) 0.59719(8) 0.0333 1.0000 Uani . . . . . F4 F 0.37756(11) 0.06696(7) 0.46777(7) 0.0335 1.0000 Uani . . . . . F5 F 0.23873(10) 0.15854(7) 0.46956(6) 0.0267 1.0000 Uani . . . . . C24 C 0.13807(14) 0.25121(10) 0.53730(11) 0.0172 1.0000 Uani . . . . . C25 C 0.21343(15) 0.28882(10) 0.52068(11) 0.0195 1.0000 Uani . . . . . C26 C 0.19520(16) 0.33854(11) 0.46573(12) 0.0236 1.0000 Uani . . . . . C27 C 0.09527(17) 0.35469(11) 0.42338(12) 0.0268 1.0000 Uani . . . . . C28 C 0.01627(16) 0.32101(11) 0.43806(12) 0.0254 1.0000 Uani . . . . . C29 C 0.03875(15) 0.27130(10) 0.49420(11) 0.0207 1.0000 Uani . . . . . F6 F 0.31446(9) 0.27590(6) 0.56039(7) 0.0258 1.0000 Uani . . . . . F7 F 0.27377(10) 0.37176(7) 0.45283(8) 0.0359 1.0000 Uani . . . . . F8 F 0.07449(11) 0.40356(8) 0.36937(8) 0.0421 1.0000 Uani . . . . . F9 F -0.08169(10) 0.33642(7) 0.39702(8) 0.0387 1.0000 Uani . . . . . F10 F -0.04463(9) 0.24217(6) 0.50455(7) 0.0273 1.0000 Uani . . . . . C30 C 0.07851(14) 0.14269(9) 0.60988(10) 0.0156 1.0000 Uani . . . . . C31 C 0.01992(15) 0.10773(10) 0.54462(11) 0.0183 1.0000 Uani . . . . . C32 C -0.05605(15) 0.06072(10) 0.54149(11) 0.0200 1.0000 Uani . . . . . C33 C -0.07505(16) 0.04396(10) 0.60718(12) 0.0232 1.0000 Uani . . . . . C34 C -0.01826(16) 0.07571(11) 0.67365(12) 0.0229 1.0000 Uani . . . . . C35 C 0.05587(15) 0.12330(10) 0.67410(11) 0.0190 1.0000 Uani . . . . . F11 F 0.03829(9) 0.11863(6) 0.47863(6) 0.0234 1.0000 Uani . . . . . F12 F -0.10942(10) 0.02900(6) 0.47609(7) 0.0279 1.0000 Uani . . . . . F13 F -0.14635(10) -0.00315(7) 0.60644(8) 0.0339 1.0000 Uani . . . . . F14 F -0.03420(11) 0.05915(7) 0.73930(7) 0.0347 1.0000 Uani . . . . . F15 F 0.10714(10) 0.15034(7) 0.74354(6) 0.0263 1.0000 Uani . . . . . C36 C 0.21529(14) 0.24383(10) 0.68394(10) 0.0161 1.0000 Uani . . . . . C37 C 0.14485(14) 0.28137(10) 0.70653(11) 0.0196 1.0000 Uani . . . . . C38 C 0.16989(16) 0.32378(11) 0.76919(12) 0.0239 1.0000 Uani . . . . . C39 C 0.27159(17) 0.33271(11) 0.81277(11) 0.0253 1.0000 Uani . . . . . C40 C 0.34553(15) 0.29894(11) 0.79193(11) 0.0219 1.0000 Uani . . . . . C41 C 0.31676(14) 0.25631(10) 0.72931(11) 0.0183 1.0000 Uani . . . . . F16 F 0.04310(9) 0.27588(7) 0.66588(7) 0.0285 1.0000 Uani . . . . . F17 F 0.09537(11) 0.35635(8) 0.78782(9) 0.0406 1.0000 Uani . . . . . F18 F 0.29786(11) 0.37361(8) 0.87381(8) 0.0427 1.0000 Uani . . . . . F19 F 0.44629(9) 0.30805(8) 0.83266(7) 0.0335 1.0000 Uani . . . . . F20 F 0.39630(9) 0.22621(7) 0.71440(7) 0.0260 1.0000 Uani . . . . . C42 C 0.1988(10) 0.5053(8) 0.6569(6) 0.0614 0.521(4) Uani D U P 1 1 Cl1 Cl 0.30948(16) 0.47506(10) 0.72449(19) 0.0760 0.521(4) Uani D U P 1 1 Cl2 Cl 0.1647(3) 0.4550(2) 0.5763(2) 0.1562 0.521(4) Uani D U P 1 1 C43 C 0.1701(11) 0.5120(8) 0.6361(6) 0.0571 0.479(4) Uani D U P 1 -2 Cl3 Cl 0.2642(3) 0.44715(16) 0.6639(3) 0.1039 0.479(4) Uani D U P 1 -2 Cl4 Cl 0.0925(3) 0.50198(15) 0.54092(13) 0.1063 0.479(4) Uani D U P 1 -2 H1 H 0.856(2) 0.2232(15) 0.6969(17) 0.041(7) 1.0000 Uiso . . . . . H2 H 0.840(2) 0.2072(15) 0.6112(16) 0.042(8) 1.0000 Uiso . . . . . H3 H 0.833(2) 0.2783(16) 0.6330(17) 0.046(8) 1.0000 Uiso . . . . . H4 H 0.552(2) 0.2235(17) 0.6734(19) 0.056(9) 1.0000 Uiso . . . . . H5 H 0.516(2) 0.1974(14) 0.5904(16) 0.038(7) 1.0000 Uiso . . . . . H6 H 0.530(2) 0.2742(16) 0.6033(17) 0.046(8) 1.0000 Uiso . . . . . H7 H 0.627(4) 0.161(3) 0.469(3) 0.117(17) 1.0000 Uiso . . . . . H8 H 0.598(4) 0.097(2) 0.511(2) 0.097(14) 1.0000 Uiso . . . . . H9 H 0.710(4) 0.106(3) 0.512(3) 0.120(17) 1.0000 Uiso . . . . . H10 H 0.700(3) 0.057(2) 0.674(2) 0.079(12) 1.0000 Uiso . . . . . H11 H 0.655(3) 0.100(2) 0.720(2) 0.092(14) 1.0000 Uiso . . . . . H12 H 0.771(3) 0.1034(19) 0.736(2) 0.068(11) 1.0000 Uiso . . . . . H61 H 0.6013 0.4133 0.3755 0.0457 1.0000 Uiso . . . . . H62 H 0.6889 0.4304 0.4576 0.0457 1.0000 Uiso . . . . . H63 H 0.5669 0.4326 0.4487 0.0457 1.0000 Uiso . . . . . H71 H 0.5001 0.3049 0.3586 0.0461 1.0000 Uiso . . . . . H72 H 0.4665 0.3243 0.4321 0.0461 1.0000 Uiso . . . . . H73 H 0.5224 0.2513 0.4294 0.0461 1.0000 Uiso . . . . . H81 H 0.6903 0.3019 0.3737 0.0507 1.0000 Uiso . . . . . H82 H 0.7757 0.3202 0.4563 0.0507 1.0000 Uiso . . . . . H83 H 0.7113 0.2487 0.4448 0.0507 1.0000 Uiso . . . . . H91 H 0.8626 0.3547 0.8492 0.0310 1.0000 Uiso . . . . . H92 H 0.8860 0.3103 0.7828 0.0310 1.0000 Uiso . . . . . H101 H 0.9228 0.4216 0.7640 0.0317 1.0000 Uiso . . . . . H102 H 0.8145 0.4484 0.7715 0.0317 1.0000 Uiso . . . . . H111 H 0.7703 0.5079 0.6546 0.0292 1.0000 Uiso . . . . . H112 H 0.7022 0.4632 0.5809 0.0292 1.0000 Uiso . . . . . H121 H 0.6651 0.4781 0.7217 0.0280 1.0000 Uiso . . . . . H122 H 0.5896 0.5027 0.6378 0.0280 1.0000 Uiso . . . . . H131 H 0.5266 0.4176 0.7418 0.0331 1.0000 Uiso . . . . . H132 H 0.5204 0.3374 0.7163 0.0331 1.0000 Uiso . . . . . H141 H 0.6991 0.4094 0.8090 0.0375 1.0000 Uiso . . . . . H142 H 0.6447 0.3439 0.8340 0.0375 1.0000 Uiso . . . . . H151 H 0.6649 0.2314 0.7911 0.0397 1.0000 Uiso . . . . . H152 H 0.7625 0.2579 0.8632 0.0397 1.0000 Uiso . . . . . H153 H 0.7824 0.2192 0.7919 0.0397 1.0000 Uiso . . . . . H161 H 0.8431 0.4019 0.5742 0.0334 1.0000 Uiso . . . . . H162 H 0.9164 0.4496 0.6430 0.0334 1.0000 Uiso . . . . . H163 H 0.9253 0.3665 0.6496 0.0334 1.0000 Uiso . . . . . H171 H 0.4445 0.3629 0.5858 0.0284 1.0000 Uiso . . . . . H172 H 0.4412 0.4433 0.6082 0.0284 1.0000 Uiso . . . . . H173 H 0.4940 0.4209 0.5456 0.0284 1.0000 Uiso . . . . . H421 H 0.2109 0.5531 0.6429 0.0746 0.5213 Uiso . . . 1 1 H422 H 0.1415 0.5050 0.6784 0.0746 0.5213 Uiso . . . 1 1 H431 H 0.2052 0.5574 0.6426 0.0711 0.4787 Uiso . . . 1 -2 H432 H 0.1259 0.5098 0.6689 0.0711 0.4787 Uiso . . . 1 -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01296(15) 0.01118(14) 0.01461(15) -0.00073(12) 0.00407(11) 0.00031(12) C1 0.0167(9) 0.0152(9) 0.0263(10) 0.0000(8) 0.0081(8) 0.0026(7) C2 0.0201(10) 0.0196(10) 0.0338(12) -0.0002(9) 0.0118(9) -0.0018(8) Al1 0.0218(3) 0.0123(3) 0.0295(3) -0.0008(2) 0.0091(3) -0.0007(2) C3 0.0479(16) 0.0247(12) 0.0401(14) -0.0119(11) 0.0118(12) -0.0033(11) C4 0.0421(15) 0.0185(11) 0.0488(15) 0.0102(11) 0.0180(13) 0.0014(10) N1 0.0181(8) 0.0152(8) 0.0175(7) -0.0010(6) 0.0060(6) 0.0009(6) C5 0.0278(11) 0.0273(11) 0.0154(9) 0.0008(8) 0.0046(8) 0.0052(8) C6 0.0551(16) 0.0370(14) 0.0221(11) 0.0118(10) 0.0099(11) 0.0117(12) C7 0.0388(14) 0.0540(17) 0.0223(11) -0.0043(11) -0.0024(10) -0.0056(12) C8 0.0505(15) 0.0536(16) 0.0227(11) 0.0061(11) 0.0194(11) 0.0200(13) N2 0.0259(9) 0.0248(9) 0.0175(8) -0.0003(7) 0.0065(7) 0.0066(7) N3 0.0153(8) 0.0150(8) 0.0285(9) -0.0033(7) 0.0045(7) -0.0003(6) N4 0.0169(8) 0.0164(8) 0.0208(8) -0.0014(6) 0.0057(6) 0.0017(6) C9 0.0269(11) 0.0308(11) 0.0198(10) -0.0053(9) -0.0037(8) 0.0045(9) C10 0.0216(11) 0.0276(11) 0.0300(12) -0.0100(9) -0.0014(9) 0.0000(9) C11 0.0240(10) 0.0104(9) 0.0385(12) -0.0002(8) 0.0086(9) 0.0005(8) C12 0.0209(10) 0.0152(9) 0.0339(11) -0.0049(8) 0.0061(9) 0.0024(8) C13 0.0291(11) 0.0278(11) 0.0258(11) -0.0013(9) 0.0158(9) 0.0053(9) C14 0.0358(13) 0.0361(13) 0.0218(10) -0.0026(9) 0.0126(9) 0.0104(10) C15 0.0433(14) 0.0354(12) 0.0206(11) 0.0072(9) 0.0121(10) 0.0073(11) C16 0.0175(10) 0.0225(10) 0.0435(13) -0.0009(9) 0.0132(9) -0.0042(8) C17 0.0164(10) 0.0236(10) 0.0309(11) -0.0030(9) 0.0025(8) 0.0056(8) B1 0.0149(9) 0.0168(10) 0.0151(9) 0.0022(8) 0.0050(8) 0.0017(8) C18 0.0162(9) 0.0174(9) 0.0165(9) 0.0001(7) 0.0056(7) 0.0008(7) C19 0.0240(10) 0.0210(10) 0.0159(9) 0.0016(7) 0.0089(8) 0.0042(8) C20 0.0239(11) 0.0239(10) 0.0201(10) 0.0027(8) 0.0031(8) 0.0081(8) C21 0.0215(10) 0.0209(10) 0.0272(10) -0.0056(8) 0.0077(8) 0.0069(8) C22 0.0228(10) 0.0262(10) 0.0189(10) -0.0053(8) 0.0099(8) -0.0007(8) C23 0.0193(9) 0.0225(10) 0.0151(9) 0.0021(7) 0.0039(7) -0.0001(8) F1 0.0399(7) 0.0335(7) 0.0167(6) 0.0098(5) 0.0146(5) 0.0171(6) F2 0.0420(8) 0.0365(8) 0.0244(6) 0.0092(6) 0.0067(6) 0.0231(6) F3 0.0285(7) 0.0334(7) 0.0372(7) -0.0086(6) 0.0100(6) 0.0145(6) F4 0.0404(8) 0.0420(8) 0.0249(6) -0.0055(6) 0.0197(6) 0.0082(6) F5 0.0329(7) 0.0335(7) 0.0139(5) 0.0048(5) 0.0080(5) 0.0066(5) C24 0.0173(9) 0.0183(9) 0.0161(9) 0.0012(7) 0.0056(7) 0.0003(7) C25 0.0149(9) 0.0214(10) 0.0198(9) 0.0017(8) 0.0027(7) -0.0011(7) C26 0.0200(10) 0.0234(10) 0.0271(10) 0.0051(8) 0.0076(8) -0.0055(8) C27 0.0300(11) 0.0232(11) 0.0234(10) 0.0121(8) 0.0039(9) 0.0010(9) C28 0.0185(10) 0.0253(11) 0.0259(10) 0.0094(9) -0.0011(8) 0.0031(8) C29 0.0162(9) 0.0208(10) 0.0237(10) 0.0045(8) 0.0050(8) -0.0004(8) F6 0.0137(6) 0.0304(6) 0.0304(6) 0.0095(5) 0.0036(5) -0.0018(5) F7 0.0273(7) 0.0392(8) 0.0416(8) 0.0172(6) 0.0120(6) -0.0092(6) F8 0.0387(8) 0.0403(8) 0.0410(8) 0.0292(7) 0.0053(6) -0.0004(6) F9 0.0197(6) 0.0419(8) 0.0440(8) 0.0223(6) -0.0028(6) 0.0047(6) F10 0.0131(5) 0.0288(7) 0.0378(7) 0.0122(5) 0.0056(5) 0.0011(5) C30 0.0153(9) 0.0147(9) 0.0163(9) 0.0015(7) 0.0047(7) 0.0028(7) C31 0.0209(10) 0.0175(9) 0.0172(9) 0.0046(7) 0.0073(8) 0.0027(7) C32 0.0194(10) 0.0166(9) 0.0206(10) -0.0016(7) 0.0023(8) 0.0008(7) C33 0.0196(10) 0.0184(10) 0.0320(11) 0.0028(8) 0.0092(8) -0.0034(8) C34 0.0259(11) 0.0258(11) 0.0206(10) 0.0060(8) 0.0126(8) 0.0004(8) C35 0.0203(10) 0.0216(10) 0.0149(9) 0.0002(7) 0.0058(7) 0.0002(8) F11 0.0299(6) 0.0259(6) 0.0143(5) 0.0006(5) 0.0074(5) -0.0047(5) F12 0.0302(7) 0.0216(6) 0.0256(6) -0.0027(5) 0.0012(5) -0.0062(5) F13 0.0327(7) 0.0292(7) 0.0410(8) 0.0026(6) 0.0142(6) -0.0136(6) F14 0.0396(8) 0.0437(8) 0.0275(7) 0.0043(6) 0.0205(6) -0.0119(6) F15 0.0309(7) 0.0328(7) 0.0172(6) -0.0027(5) 0.0108(5) -0.0071(5) C36 0.0158(9) 0.0162(9) 0.0162(9) 0.0032(7) 0.0052(7) 0.0017(7) C37 0.0115(9) 0.0207(9) 0.0245(10) -0.0017(8) 0.0033(7) 0.0003(7) C38 0.0232(10) 0.0208(10) 0.0298(11) -0.0043(8) 0.0114(8) 0.0043(8) C39 0.0310(11) 0.0255(11) 0.0185(9) -0.0049(8) 0.0073(8) -0.0019(9) C40 0.0177(9) 0.0294(11) 0.0151(9) 0.0001(8) 0.0010(7) -0.0048(8) C41 0.0160(9) 0.0225(10) 0.0179(9) 0.0029(7) 0.0078(7) 0.0004(7) F16 0.0149(6) 0.0292(7) 0.0375(7) -0.0091(6) 0.0036(5) 0.0038(5) F17 0.0314(7) 0.0436(8) 0.0480(9) -0.0210(7) 0.0148(6) 0.0088(6) F18 0.0416(8) 0.0510(9) 0.0322(7) -0.0242(7) 0.0081(6) -0.0039(7) F19 0.0186(6) 0.0525(9) 0.0238(6) -0.0070(6) -0.0001(5) -0.0060(6) F20 0.0135(5) 0.0409(7) 0.0243(6) -0.0041(5) 0.0074(5) 0.0023(5) C42 0.056(6) 0.072(7) 0.059(5) -0.039(5) 0.023(3) 0.013(3) Cl1 0.0579(11) 0.0383(9) 0.129(2) 0.0176(11) 0.0284(12) 0.0076(7) Cl2 0.169(3) 0.172(4) 0.116(3) -0.117(3) 0.034(3) -0.012(3) C43 0.064(8) 0.062(5) 0.052(4) -0.003(5) 0.028(3) 0.010(4) Cl3 0.104(2) 0.0667(17) 0.168(4) 0.062(2) 0.082(3) 0.0314(17) Cl4 0.171(3) 0.0804(18) 0.0529(12) -0.0256(12) 0.0185(15) -0.0121(19) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . C1 . 2.344(2) yes Ti1 . C2 . 2.335(2) yes Ti1 . N1 . 1.6978(16) yes Ti1 . N2 . 2.4128(16) yes Ti1 . N3 . 2.2854(16) yes Ti1 . N4 . 2.2890(16) yes C1 . Al1 . 2.081(2) yes C1 . H1 . 0.99(3) no C1 . H2 . 0.97(3) no C1 . H3 . 0.97(3) no C2 . Al1 . 2.075(2) yes C2 . H4 . 0.97(3) no C2 . H5 . 0.99(3) no C2 . H6 . 0.98(3) no Al1 . C3 . 1.963(3) yes Al1 . C4 . 1.981(3) yes C3 . H7 . 1.03(5) no C3 . H8 . 0.93(5) no C3 . H9 . 0.96(5) no C4 . H10 . 0.94(4) no C4 . H11 . 0.95(5) no C4 . H12 . 0.95(4) no N1 . C5 . 1.462(3) yes C5 . C6 . 1.528(3) yes C5 . C7 . 1.524(3) yes C5 . C8 . 1.527(3) yes C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no N2 . C9 . 1.491(3) yes N2 . C14 . 1.506(3) yes N2 . C15 . 1.483(3) yes N3 . C10 . 1.504(3) yes N3 . C11 . 1.498(3) yes N3 . C16 . 1.484(3) yes N4 . C12 . 1.501(3) yes N4 . C13 . 1.494(3) yes N4 . C17 . 1.487(3) yes C9 . C10 . 1.511(3) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C11 . C12 . 1.503(3) yes C11 . H111 . 1.000 no C11 . H112 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C13 . C14 . 1.505(3) yes C13 . H131 . 1.000 no C13 . H132 . 1.000 no C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . H151 . 1.000 no C15 . H152 . 1.000 no C15 . H153 . 1.000 no C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no B1 . C18 . 1.651(3) yes B1 . C24 . 1.661(3) yes B1 . C30 . 1.659(3) yes B1 . C36 . 1.661(3) yes C18 . C19 . 1.393(3) yes C18 . C23 . 1.390(3) yes C19 . C20 . 1.376(3) yes C19 . F1 . 1.355(2) yes C20 . C21 . 1.378(3) yes C20 . F2 . 1.351(2) yes C21 . C22 . 1.374(3) yes C21 . F3 . 1.339(2) yes C22 . C23 . 1.384(3) yes C22 . F4 . 1.352(2) yes C23 . F5 . 1.353(2) yes C24 . C25 . 1.391(3) yes C24 . C29 . 1.390(3) yes C25 . C26 . 1.374(3) yes C25 . F6 . 1.362(2) yes C26 . C27 . 1.373(3) yes C26 . F7 . 1.353(2) yes C27 . C28 . 1.377(3) yes C27 . F8 . 1.349(2) yes C28 . C29 . 1.386(3) yes C28 . F9 . 1.342(2) yes C29 . F10 . 1.354(2) yes C30 . C31 . 1.393(3) yes C30 . C35 . 1.390(3) yes C31 . C32 . 1.380(3) yes C31 . F11 . 1.356(2) yes C32 . C33 . 1.377(3) yes C32 . F12 . 1.345(2) yes C33 . C34 . 1.372(3) yes C33 . F13 . 1.344(2) yes C34 . C35 . 1.381(3) yes C34 . F14 . 1.355(2) yes C35 . F15 . 1.357(2) yes C36 . C37 . 1.392(3) yes C36 . C41 . 1.390(3) yes C37 . C38 . 1.380(3) yes C37 . F16 . 1.355(2) yes C38 . C39 . 1.374(3) yes C38 . F17 . 1.351(2) yes C39 . C40 . 1.377(3) yes C39 . F18 . 1.338(2) yes C40 . C41 . 1.381(3) yes C40 . F19 . 1.351(2) yes C41 . F20 . 1.354(2) yes C42 . Cl1 . 1.723(7) yes C42 . Cl2 . 1.726(7) yes C42 . H421 . 1.000 no C42 . H422 . 1.000 no C43 . Cl3 . 1.762(9) yes C43 . Cl4 . 1.747(8) yes C43 . H431 . 1.000 no C43 . H432 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . Ti1 . C2 . 91.24(7) yes C1 . Ti1 . Al1 . 46.13(5) yes C2 . Ti1 . Al1 . 46.01(5) yes C1 . Ti1 . N1 . 96.61(8) yes C2 . Ti1 . N1 . 96.26(8) yes Al1 . Ti1 . N1 . 91.93(6) yes C1 . Ti1 . N2 . 88.90(7) yes C2 . Ti1 . N2 . 90.34(8) yes Al1 . Ti1 . N2 . 96.74(5) yes N1 . Ti1 . N2 . 171.29(7) yes C1 . Ti1 . N3 . 94.69(7) yes C2 . Ti1 . N3 . 164.83(7) yes Al1 . Ti1 . N3 . 140.67(4) yes N1 . Ti1 . N3 . 96.91(7) yes N2 . Ti1 . N3 . 75.84(6) yes C1 . Ti1 . N4 . 163.85(7) yes C2 . Ti1 . N4 . 92.71(7) yes Al1 . Ti1 . N4 . 138.44(5) yes N1 . Ti1 . N4 . 98.52(7) yes N2 . Ti1 . N4 . 75.43(6) yes N3 . Ti1 . N4 . 77.92(6) yes Ti1 . C1 . Al1 . 79.58(7) yes Ti1 . C1 . H1 . 114.6(16) no Al1 . C1 . H1 . 108.6(16) no Ti1 . C1 . H2 . 138.6(17) no Al1 . C1 . H2 . 91.9(17) no H1 . C1 . H2 . 107(2) no Ti1 . C1 . H3 . 67.6(17) no Al1 . C1 . H3 . 140.3(17) no H1 . C1 . H3 . 105(2) no H2 . C1 . H3 . 98(2) no Ti1 . C2 . Al1 . 79.92(7) yes Ti1 . C2 . H4 . 112.4(19) no Al1 . C2 . H4 . 111.1(19) no Ti1 . C2 . H5 . 143.3(16) no Al1 . C2 . H5 . 86.1(16) no H4 . C2 . H5 . 104(2) no Ti1 . C2 . H6 . 68.1(17) no Al1 . C2 . H6 . 135.9(17) no H4 . C2 . H6 . 109(3) no H5 . C2 . H6 . 102(2) no Ti1 . Al1 . C1 . 54.29(6) yes Ti1 . Al1 . C2 . 54.07(6) yes C1 . Al1 . C2 . 107.16(8) yes Ti1 . Al1 . C3 . 120.65(9) yes C1 . Al1 . C3 . 112.34(11) yes C2 . Al1 . C3 . 112.84(12) yes Ti1 . Al1 . C4 . 128.37(9) yes C1 . Al1 . C4 . 107.66(11) yes C2 . Al1 . C4 . 105.47(11) yes C3 . Al1 . C4 . 110.97(12) yes Al1 . C3 . H7 . 117(3) no Al1 . C3 . H8 . 107(3) no H7 . C3 . H8 . 109(4) no Al1 . C3 . H9 . 110(3) no H7 . C3 . H9 . 105(4) no H8 . C3 . H9 . 109(4) no Al1 . C4 . H10 . 110(2) no Al1 . C4 . H11 . 113(3) no H10 . C4 . H11 . 103(3) no Al1 . C4 . H12 . 116(2) no H10 . C4 . H12 . 108(3) no H11 . C4 . H12 . 107(3) no Ti1 . N1 . C5 . 177.34(14) yes N1 . C5 . C6 . 109.59(17) yes N1 . C5 . C7 . 109.01(18) yes C6 . C5 . C7 . 109.6(2) yes N1 . C5 . C8 . 108.21(17) yes C6 . C5 . C8 . 109.3(2) yes C7 . C5 . C8 . 111.1(2) yes C5 . C6 . H61 . 109.467 no C5 . C6 . H62 . 109.467 no H61 . C6 . H62 . 109.476 no C5 . C6 . H63 . 109.467 no H61 . C6 . H63 . 109.476 no H62 . C6 . H63 . 109.476 no C5 . C7 . H71 . 109.467 no C5 . C7 . H72 . 109.467 no H71 . C7 . H72 . 109.476 no C5 . C7 . H73 . 109.467 no H71 . C7 . H73 . 109.476 no H72 . C7 . H73 . 109.476 no C5 . C8 . H81 . 109.467 no C5 . C8 . H82 . 109.466 no H81 . C8 . H82 . 109.475 no C5 . C8 . H83 . 109.467 no H81 . C8 . H83 . 109.476 no H82 . C8 . H83 . 109.476 no Ti1 . N2 . C9 . 103.16(12) yes Ti1 . N2 . C14 . 109.80(12) yes C9 . N2 . C14 . 110.76(17) yes Ti1 . N2 . C15 . 116.58(13) yes C9 . N2 . C15 . 107.64(17) yes C14 . N2 . C15 . 108.75(17) yes Ti1 . N3 . C10 . 113.49(13) yes Ti1 . N3 . C11 . 102.38(11) yes C10 . N3 . C11 . 110.06(16) yes Ti1 . N3 . C16 . 114.27(12) yes C10 . N3 . C16 . 109.50(16) yes C11 . N3 . C16 . 106.67(16) yes Ti1 . N4 . C12 . 109.92(11) yes Ti1 . N4 . C13 . 106.86(12) yes C12 . N4 . C13 . 110.37(16) yes Ti1 . N4 . C17 . 113.11(12) yes C12 . N4 . C17 . 108.38(15) yes C13 . N4 . C17 . 108.18(16) yes N2 . C9 . C10 . 112.63(17) yes N2 . C9 . H91 . 108.677 no C10 . C9 . H91 . 108.678 no N2 . C9 . H92 . 108.677 no C10 . C9 . H92 . 108.677 no H91 . C9 . H92 . 109.467 no N3 . C10 . C9 . 112.18(17) yes N3 . C10 . H101 . 108.791 no C9 . C10 . H101 . 108.791 no N3 . C10 . H102 . 108.791 no C9 . C10 . H102 . 108.791 no H101 . C10 . H102 . 109.467 no N3 . C11 . C12 . 111.82(17) yes N3 . C11 . H111 . 108.882 no C12 . C11 . H111 . 108.882 no N3 . C11 . H112 . 108.883 no C12 . C11 . H112 . 108.883 no H111 . C11 . H112 . 109.467 no N4 . C12 . C11 . 112.32(16) yes N4 . C12 . H121 . 108.755 no C11 . C12 . H121 . 108.755 no N4 . C12 . H122 . 108.754 no C11 . C12 . H122 . 108.755 no H121 . C12 . H122 . 109.467 no N4 . C13 . C14 . 112.18(17) yes N4 . C13 . H131 . 108.791 no C14 . C13 . H131 . 108.790 no N4 . C13 . H132 . 108.791 no C14 . C13 . H132 . 108.791 no H131 . C13 . H132 . 109.467 no N2 . C14 . C13 . 112.16(17) yes N2 . C14 . H141 . 108.797 no C13 . C14 . H141 . 108.797 no N2 . C14 . H142 . 108.796 no C13 . C14 . H142 . 108.797 no H141 . C14 . H142 . 109.467 no N2 . C15 . H151 . 109.467 no N2 . C15 . H152 . 109.467 no H151 . C15 . H152 . 109.475 no N2 . C15 . H153 . 109.467 no H151 . C15 . H153 . 109.476 no H152 . C15 . H153 . 109.476 no N3 . C16 . H161 . 109.467 no N3 . C16 . H162 . 109.467 no H161 . C16 . H162 . 109.476 no N3 . C16 . H163 . 109.467 no H161 . C16 . H163 . 109.476 no H162 . C16 . H163 . 109.476 no N4 . C17 . H171 . 109.467 no N4 . C17 . H172 . 109.467 no H171 . C17 . H172 . 109.476 no N4 . C17 . H173 . 109.467 no H171 . C17 . H173 . 109.476 no H172 . C17 . H173 . 109.476 no C18 . B1 . C24 . 113.14(15) yes C18 . B1 . C30 . 102.21(15) yes C24 . B1 . C30 . 114.30(15) yes C18 . B1 . C36 . 112.90(15) yes C24 . B1 . C36 . 102.16(15) yes C30 . B1 . C36 . 112.57(15) yes B1 . C18 . C19 . 120.03(16) yes B1 . C18 . C23 . 127.24(17) yes C19 . C18 . C23 . 112.59(17) yes C18 . C19 . C20 . 124.93(18) yes C18 . C19 . F1 . 119.06(17) yes C20 . C19 . F1 . 115.99(17) yes C19 . C20 . C21 . 119.79(18) yes C19 . C20 . F2 . 120.82(18) yes C21 . C20 . F2 . 119.39(18) yes C20 . C21 . C22 . 118.14(18) yes C20 . C21 . F3 . 120.35(19) yes C22 . C21 . F3 . 121.51(19) yes C21 . C22 . C23 . 120.16(18) yes C21 . C22 . F4 . 119.85(18) yes C23 . C22 . F4 . 119.99(18) yes C18 . C23 . C22 . 124.32(18) yes C18 . C23 . F5 . 120.75(17) yes C22 . C23 . F5 . 114.93(17) yes B1 . C24 . C25 . 119.54(16) yes B1 . C24 . C29 . 127.63(17) yes C25 . C24 . C29 . 112.63(17) yes C24 . C25 . C26 . 125.41(18) yes C24 . C25 . F6 . 118.92(17) yes C26 . C25 . F6 . 115.66(17) yes C25 . C26 . C27 . 119.17(19) yes C25 . C26 . F7 . 121.20(18) yes C27 . C26 . F7 . 119.63(18) yes C26 . C27 . C28 . 118.81(18) yes C26 . C27 . F8 . 120.79(19) yes C28 . C27 . F8 . 120.39(19) yes C27 . C28 . C29 . 119.78(18) yes C27 . C28 . F9 . 119.29(18) yes C29 . C28 . F9 . 120.93(19) yes C24 . C29 . C28 . 124.13(18) yes C24 . C29 . F10 . 121.04(17) yes C28 . C29 . F10 . 114.83(17) yes B1 . C30 . C31 . 120.20(16) yes B1 . C30 . C35 . 126.65(17) yes C31 . C30 . C35 . 112.79(17) yes C30 . C31 . C32 . 124.89(18) yes C30 . C31 . F11 . 119.10(17) yes C32 . C31 . F11 . 116.01(17) yes C31 . C32 . C33 . 119.41(18) yes C31 . C32 . F12 . 121.35(18) yes C33 . C32 . F12 . 119.19(18) yes C32 . C33 . C34 . 118.38(18) yes C32 . C33 . F13 . 120.84(19) yes C34 . C33 . F13 . 120.78(19) yes C33 . C34 . C35 . 120.40(18) yes C33 . C34 . F14 . 119.48(18) yes C35 . C34 . F14 . 120.11(19) yes C30 . C35 . C34 . 124.10(18) yes C30 . C35 . F15 . 121.41(17) yes C34 . C35 . F15 . 114.49(17) yes B1 . C36 . C37 . 119.26(16) yes B1 . C36 . C41 . 128.09(17) yes C37 . C36 . C41 . 112.58(17) yes C36 . C37 . C38 . 125.05(18) yes C36 . C37 . F16 . 118.99(17) yes C38 . C37 . F16 . 115.94(17) yes C37 . C38 . C39 . 119.43(18) yes C37 . C38 . F17 . 120.56(18) yes C39 . C38 . F17 . 120.01(19) yes C38 . C39 . C40 . 118.45(18) yes C38 . C39 . F18 . 120.57(19) yes C40 . C39 . F18 . 120.98(19) yes C39 . C40 . C41 . 120.08(18) yes C39 . C40 . F19 . 119.74(18) yes C41 . C40 . F19 . 120.17(18) yes C36 . C41 . C40 . 124.32(18) yes C36 . C41 . F20 . 121.08(17) yes C40 . C41 . F20 . 114.60(17) yes Cl1 . C42 . Cl2 . 110.8(4) yes Cl1 . C42 . H421 . 109.132 no Cl2 . C42 . H421 . 109.132 no Cl1 . C42 . H422 . 109.132 no Cl2 . C42 . H422 . 109.132 no H421 . C42 . H422 . 109.467 no Cl3 . C43 . Cl4 . 110.8(5) yes Cl3 . C43 . H431 . 109.130 no Cl4 . C43 . H431 . 109.129 no Cl3 . C43 . H432 . 109.131 no Cl4 . C43 . H432 . 109.129 no H431 . C43 . H432 . 109.466 no ##end