Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' #========================================================================== _journal_coden_Cambridge 0222 #============================================================================== _audit_creation_date ? _audit_creation_method SHELXL-97 _audit_update_record ; ? ; # 1. Submission Details _publ_contact_author_name 'Guido Pampaloni' _publ_contact_author_address ; Dipartimento di Chimica e Chimica Industriale Universit di Pisa Via risorgimento 35 56126 Pisa Italy ; _publ_contact_author_email pampa@dcci.unipi.it _publ_contact_author_fax '0039-50-2219 219' _publ_contact_author_phone '0039-50-2219 246' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_section_title ; Bis(arylimino)pyridine Derivatives of Group 4 Metals: Preparation, Characterization and Activity in Ethylene Polymerization ; loop_ _publ_author_name _publ_author_address F.Calderazzo ; Dipartimento di Chimica e Chimica industriale Universit di Pisa Via Risorgimento 35 56126 Pisa Italy ; U.Englert ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; G.Pampaloni ; Dipartimento di Chimica e Chimica industriale Universit di Pisa Via Risorgimento 35 56126 Pisa Italy ; R.Santi ; Polimeri Europa, Centro Ricerche Novara Via G. Fauser 4 28100 Novara Italy ; A.Sommazzi ; Polimeri Europa, Centro Ricerche Novara Via G. Fauser 4 28100 Novara Italy ; M.Zinna ; Dipartimento di Chimica e Chimica industriale Universit di Pisa Via Risorgimento 35 56126 Pisa Italy ; _publ_section_references ; Bruker (1999). SAINT+. Version 6.02. Bruker AXS Inc., Madison, Wisconson, USA. Bruker (2001). SMART. Version 5.624. Bruker AXS Inc., Madison, Wisconson, USA. Sheldrick, G. M. (1996). SADABS. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXS-97. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of Gottingen, Germany. Sheldrick, G. M. (1998). SHELXTL. Version 5.1. Bruker AXS Inc., Madison, Wisconson, USA. Spek, A. L. (1990). Acta Cryst. A46, C-34. ; _publ_section_acknowledgements ; Support from the DFG and the Fonds der Chemischen Industrie is gratefully acknowledged. ; data_gp52 _database_code_depnum_ccdc_archive 'CCDC 252936' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [2,6?bis[1?(2,6?diisopropylphenylimino)ethyl]pyridine]trichlototitanium(III) ; _chemical_name_common ;(2,6?bis(1?(2,6?diisopropylphenylimino)ethyl)pyridine)trichlot otitanium(iii) ; _chemical_formula_moiety ? _chemical_formula_sum C87H110Cl6N6Ti2 _chemical_formula_weight 1548.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti .2776 .4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.761(5) _cell_length_b 16.266(4) _cell_length_c 31.141(6) _cell_angle_alpha 90.00 _cell_angle_beta 128.189(10) _cell_angle_gamma 90.00 _cell_volume 8266(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 942 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 19.41 _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 0.434 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (1996)' _exptl_absorpt_correction_T_min 0.8454 _exptl_absorpt_correction_T_max 0.9338 _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104563 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.25 _reflns_number_total 18429 _reflns_number_gt 11870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+12.5239P] 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 18429 _refine_ls_number_parameters 933 _refine_ls_number_restraints 196 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1877 _refine_ls_wR_factor_gt 0.1627 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.063 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti -0.00492(4) 0.10351(4) 0.29649(3) 0.03085(17) Uani 1 d . . . Cl1 Cl 0.07674(6) 0.12352(6) 0.26911(4) 0.0391(2) Uani 1 d . . . Cl2 Cl -0.09616(6) 0.06211(6) 0.31659(4) 0.0391(2) Uani 1 d . . . Cl3 Cl -0.03853(6) 0.23991(6) 0.29033(5) 0.0441(3) Uani 1 d . . . N1 N 0.03002(18) -0.02340(19) 0.31614(13) 0.0317(7) Uani 1 d . . . N2 N 0.10682(18) 0.0977(2) 0.38281(12) 0.0317(7) Uani 1 d . . . N3 N -0.08456(18) 0.02970(19) 0.21807(13) 0.0320(7) Uani 1 d . . . C1 C 0.0923(2) -0.0448(2) 0.36750(15) 0.0333(8) Uani 1 d . . . C2 C 0.1356(2) 0.0264(3) 0.40397(15) 0.0339(8) Uani 1 d . . . C3 C 0.1507(2) 0.1695(2) 0.41643(15) 0.0328(8) Uani 1 d . . . C4 C 0.1230(2) 0.2086(3) 0.44251(16) 0.0406(10) Uani 1 d . . . C5 C 0.0536(3) 0.1745(4) 0.4410(2) 0.0616(15) Uani 1 d . . . H5 H 0.0208 0.1360 0.4093 0.074 Uiso 1 calc R . . C6 C 0.0866(4) 0.1276(4) 0.4920(3) 0.083(2) Uani 1 d . . . H6A H 0.1126 0.1656 0.5229 0.124 Uiso 1 calc R . . H6B H 0.1271 0.0875 0.4986 0.124 Uiso 1 calc R . . H6C H 0.0416 0.0987 0.4879 0.124 Uiso 1 calc R . . C7 C -0.0023(4) 0.2396(5) 0.4347(4) 0.127(4) Uani 1 d . . . H7A H -0.0530 0.2142 0.4243 0.190 Uiso 1 calc R . . H7B H -0.0154 0.2783 0.4062 0.190 Uiso 1 calc R . . H7C H 0.0246 0.2690 0.4693 0.190 Uiso 1 calc R . . C8 C 0.1648(2) 0.2782(3) 0.47350(16) 0.0442(11) Uani 1 d . . . H8 H 0.1471 0.3054 0.4915 0.053 Uiso 1 calc R . . C9 C 0.2310(3) 0.3087(3) 0.47881(17) 0.0432(10) Uani 1 d . . . H9 H 0.2577 0.3572 0.4996 0.052 Uiso 1 calc R . . C10 C 0.2585(2) 0.2689(2) 0.45397(16) 0.0370(9) Uani 1 d . . . H10 H 0.3049 0.2898 0.4583 0.044 Uiso 1 calc R . . C11 C 0.2196(2) 0.1984(2) 0.42244(15) 0.0314(8) Uani 1 d . . . C12 C 0.2580(2) 0.1549(2) 0.39989(16) 0.0350(9) Uani 1 d . . . H12 H 0.2234 0.1061 0.3784 0.042 Uiso 1 calc R . . C13 C 0.2619(2) 0.2106(2) 0.36230(17) 0.0380(9) Uani 1 d . . . H13A H 0.2062 0.2254 0.3305 0.057 Uiso 1 calc R . . H13B H 0.2894 0.1818 0.3501 0.057 Uiso 1 calc R . . H13C H 0.2925 0.2606 0.3821 0.057 Uiso 1 calc R . . C14 C 0.3444(2) 0.1245(3) 0.44665(18) 0.0433(10) Uani 1 d . . . H14A H 0.3796 0.1717 0.4677 0.065 Uiso 1 calc R . . H14B H 0.3671 0.0943 0.4315 0.065 Uiso 1 calc R . . H14C H 0.3417 0.0882 0.4706 0.065 Uiso 1 calc R . . C15 C 0.2089(2) 0.0097(3) 0.46183(16) 0.0422(10) Uani 1 d . . . H15A H 0.2305 0.0618 0.4818 0.063 Uiso 1 calc R . . H15B H 0.2512 -0.0179 0.4622 0.063 Uiso 1 calc R . . H15C H 0.1929 -0.0256 0.4793 0.063 Uiso 1 calc R . . C16 C 0.1115(2) -0.1267(3) 0.38258(18) 0.0411(10) Uani 1 d . . . H16 H 0.1564 -0.1411 0.4190 0.049 Uiso 1 calc R . . C17 C 0.0649(3) -0.1865(3) 0.34423(18) 0.0434(10) Uani 1 d . . . H17 H 0.0777 -0.2429 0.3538 0.052 Uiso 1 calc R . . C18 C -0.0010(2) -0.1644(2) 0.29125(18) 0.0397(9) Uani 1 d . . . H18 H -0.0342 -0.2051 0.2643 0.048 Uiso 1 calc R . . C19 C -0.0171(2) -0.0820(2) 0.27870(16) 0.0340(8) Uani 1 d . . . C20 C -0.0818(2) -0.0488(2) 0.22361(16) 0.0353(9) Uani 1 d . . . C21 C -0.1343(2) 0.0631(2) 0.16305(15) 0.0341(9) Uani 1 d . . . C22 C -0.2092(2) 0.1022(2) 0.14217(16) 0.0381(9) Uani 1 d . . . C23 C -0.2412(3) 0.1093(3) 0.17399(18) 0.0465(11) Uani 1 d . . . H23 H -0.1962 0.0930 0.2126 0.056 Uiso 1 calc R . . C24 C -0.2664(3) 0.1976(3) 0.1746(2) 0.0560(12) Uani 1 d . . . H24A H -0.2197 0.2345 0.1895 0.084 Uiso 1 calc R . . H24B H -0.2840 0.2002 0.1975 0.084 Uiso 1 calc R . . H24C H -0.3118 0.2145 0.1373 0.084 Uiso 1 calc R . . C25 C -0.3135(3) 0.0506(3) 0.1514(2) 0.0644(14) Uani 1 d . . . H25A H -0.3588 0.0658 0.1136 0.097 Uiso 1 calc R . . H25B H -0.3318 0.0545 0.1738 0.097 Uiso 1 calc R . . H25C H -0.2963 -0.0059 0.1524 0.097 Uiso 1 calc R . . C26 C -0.2563(3) 0.1299(3) 0.08851(19) 0.0487(11) Uani 1 d . . . H26 H -0.3079 0.1546 0.0730 0.058 Uiso 1 calc R . . C27 C -0.2309(3) 0.1227(3) 0.05702(18) 0.0489(11) Uani 1 d . . . H27 H -0.2639 0.1430 0.0206 0.059 Uiso 1 calc R . . C28 C -0.1569(3) 0.0857(3) 0.07904(17) 0.0437(10) Uani 1 d . . . H28 H -0.1392 0.0812 0.0574 0.052 Uiso 1 calc R . . C29 C -0.1072(2) 0.0546(2) 0.13182(16) 0.0374(9) Uani 1 d . . . C30 C -0.0284(3) 0.0109(3) 0.15085(18) 0.0438(10) Uani 1 d . . . H30 H 0.0021 -0.0050 0.1900 0.053 Uiso 1 calc R . . C31 C 0.0270(3) 0.0662(3) 0.14684(19) 0.0536(12) Uani 1 d . . . H31A H 0.0014 0.0763 0.1083 0.080 Uiso 1 calc R . . H31B H 0.0801 0.0393 0.1645 0.080 Uiso 1 calc R . . H31C H 0.0351 0.1186 0.1651 0.080 Uiso 1 calc R . . C32 C -0.0468(3) -0.0675(3) 0.1177(2) 0.0549(12) Uani 1 d . . . H32A H -0.0711 -0.0527 0.0800 0.082 Uiso 1 calc R . . H32B H -0.0853 -0.1018 0.1180 0.082 Uiso 1 calc R . . H32C H 0.0042 -0.0980 0.1340 0.082 Uiso 1 calc R . . C33 C -0.1380(3) -0.1095(3) 0.17939(17) 0.0464(11) Uani 1 d . . . H33A H -0.1701 -0.1381 0.1882 0.070 Uiso 1 calc R . . H33B H -0.1056 -0.1496 0.1765 0.070 Uiso 1 calc R . . H33C H -0.1751 -0.0805 0.1445 0.070 Uiso 1 calc R . . Ti2 Ti 0.59496(4) 0.38239(4) 0.29776(3) 0.02945(16) Uani 1 d . . . Cl4 Cl 0.53114(6) 0.42568(6) 0.20813(4) 0.0357(2) Uani 1 d . . . Cl5 Cl 0.67665(7) 0.33010(7) 0.38935(4) 0.0454(3) Uani 1 d . . . Cl6 Cl 0.55687(9) 0.49571(6) 0.32127(5) 0.0590(3) Uani 1 d . . . N4 N 0.62543(19) 0.26329(18) 0.28533(12) 0.0313(7) Uani 1 d . . . N5 N 0.49434(19) 0.29944(18) 0.27262(12) 0.0305(7) Uani 1 d . . . N6 N 0.70958(19) 0.39545(18) 0.30589(12) 0.0315(7) Uani 1 d . . . C34 C 0.5794(2) 0.1987(2) 0.27818(15) 0.0339(9) Uani 1 d . . . C35 C 0.5034(2) 0.2216(2) 0.26965(15) 0.0328(8) Uani 1 d . . . C36 C 0.4195(2) 0.3286(2) 0.26225(16) 0.0335(8) Uani 1 d . . . C37 C 0.4164(3) 0.3346(2) 0.30567(17) 0.0360(9) Uani 1 d . . . C38 C 0.4848(3) 0.3047(2) 0.36252(16) 0.0388(9) Uani 1 d . . . H38 H 0.5292 0.2820 0.3621 0.047 Uiso 1 calc R . . C39 C 0.5217(3) 0.3743(3) 0.40479(19) 0.0535(12) Uani 1 d . . . H39A H 0.5452 0.4161 0.3955 0.080 Uiso 1 calc R . . H39B H 0.5646 0.3521 0.4412 0.080 Uiso 1 calc R . . H39C H 0.4786 0.3993 0.4047 0.080 Uiso 1 calc R . . C40 C 0.4546(3) 0.2356(3) 0.37932(18) 0.0444(10) Uani 1 d . . . H40A H 0.4140 0.2574 0.3828 0.067 Uiso 1 calc R . . H40B H 0.5010 0.2127 0.4145 0.067 Uiso 1 calc R . . H40C H 0.4295 0.1923 0.3515 0.067 Uiso 1 calc R . . C41 C 0.3456(3) 0.3659(3) 0.29488(19) 0.0453(10) Uani 1 d . . . H41 H 0.3428 0.3715 0.3240 0.054 Uiso 1 calc R . . C42 C 0.2791(3) 0.3890(3) 0.2429(2) 0.0500(11) Uani 1 d . . . H42 H 0.2312 0.4106 0.2364 0.060 Uiso 1 calc R . . C43 C 0.2828(3) 0.3806(2) 0.20058(19) 0.0454(11) Uani 1 d . . . H43 H 0.2367 0.3961 0.1648 0.054 Uiso 1 calc R . . C44 C 0.3522(3) 0.3500(2) 0.20857(17) 0.0382(9) Uani 1 d . . . C45 C 0.3511(3) 0.3366(2) 0.15993(16) 0.0409(10) Uani 1 d . . . H45 H 0.4085 0.3249 0.1740 0.049 Uiso 1 calc R . . C46 C 0.2978(3) 0.2624(3) 0.12618(19) 0.0540(12) Uani 1 d . . . H46A H 0.3213 0.2126 0.1485 0.081 Uiso 1 calc R . . H46B H 0.2956 0.2567 0.0940 0.081 Uiso 1 calc R . . H46C H 0.2422 0.2707 0.1145 0.081 Uiso 1 calc R . . C47 C 0.3209(3) 0.4125(3) 0.12330(19) 0.0531(12) Uani 1 d . . . H47A H 0.2629 0.4220 0.1062 0.080 Uiso 1 calc R . . H47B H 0.3271 0.4038 0.0949 0.080 Uiso 1 calc R . . H47C H 0.3531 0.4605 0.1453 0.080 Uiso 1 calc R . . C48 C 0.4461(3) 0.1557(2) 0.26036(19) 0.0432(10) Uani 1 d . . . H48A H 0.3967 0.1807 0.2523 0.065 Uiso 1 calc R . . H48B H 0.4730 0.1216 0.2932 0.065 Uiso 1 calc R . . H48C H 0.4309 0.1214 0.2295 0.065 Uiso 1 calc R . . C49 C 0.6040(3) 0.1189(2) 0.27943(17) 0.0424(10) Uani 1 d . . . H49 H 0.5710 0.0734 0.2741 0.051 Uiso 1 calc R . . C50 C 0.6770(3) 0.1068(3) 0.28852(19) 0.0486(11) Uani 1 d . . . H50 H 0.6949 0.0526 0.2895 0.058 Uiso 1 calc R . . C51 C 0.7251(3) 0.1742(3) 0.29639(18) 0.0470(11) Uani 1 d . . . H51 H 0.7754 0.1666 0.3023 0.056 Uiso 1 calc R . . C52 C 0.6974(2) 0.2523(2) 0.29535(16) 0.0359(9) Uani 1 d . . . C53 C 0.7424(2) 0.3294(2) 0.30477(16) 0.0362(9) Uani 1 d . . . C54 C 0.7414(2) 0.4761(2) 0.30761(15) 0.0330(8) Uani 1 d . . . C55 C 0.7804(2) 0.5230(2) 0.35576(16) 0.0364(9) Uani 1 d . . . C56 C 0.8046(3) 0.4859(3) 0.40855(16) 0.0427(10) Uani 1 d . . . H56 H 0.7755 0.4321 0.3992 0.051 Uiso 1 calc R . . C57 C 0.8953(4) 0.4680(6) 0.4461(3) 0.111(3) Uani 1 d . . . H57A H 0.9076 0.4261 0.4295 0.166 Uiso 1 calc R . . H57B H 0.9116 0.4479 0.4812 0.166 Uiso 1 calc R . . H57C H 0.9256 0.5184 0.4519 0.166 Uiso 1 calc R . . C58 C 0.7795(5) 0.5378(4) 0.4364(2) 0.094(2) Uani 1 d . . . H58A H 0.8104 0.5895 0.4489 0.141 Uiso 1 calc R . . H58B H 0.7912 0.5078 0.4678 0.141 Uiso 1 calc R . . H58C H 0.7207 0.5497 0.4105 0.141 Uiso 1 calc R . . C59 C 0.7996(3) 0.6040(3) 0.35390(19) 0.0449(10) Uani 1 d . . . H59 H 0.8253 0.6370 0.3858 0.054 Uiso 1 calc R . . C60 C 0.7831(3) 0.6375(3) 0.3083(2) 0.0470(11) Uani 1 d . . . H60 H 0.7940 0.6940 0.3076 0.056 Uiso 1 calc R . . C61 C 0.7504(3) 0.5894(3) 0.26299(19) 0.0431(10) Uani 1 d . . . H61 H 0.7417 0.6127 0.2318 0.052 Uiso 1 calc R . . C62 C 0.7296(2) 0.5073(2) 0.26124(16) 0.0346(8) Uani 1 d . . . C63 C 0.6984(2) 0.4582(3) 0.21051(16) 0.0397(9) Uani 1 d . . . H63 H 0.6813 0.4027 0.2139 0.048 Uiso 1 calc R . . C64 C 0.6246(3) 0.4993(3) 0.15894(17) 0.0465(11) Uani 1 d . . . H64A H 0.5839 0.5130 0.1641 0.070 Uiso 1 calc R . . H64B H 0.6004 0.4617 0.1279 0.070 Uiso 1 calc R . . H64C H 0.6424 0.5497 0.1517 0.070 Uiso 1 calc R . . C65 C 0.7667(3) 0.4470(3) 0.2050(2) 0.0516(11) Uani 1 d . . . H65A H 0.7844 0.5010 0.2019 0.077 Uiso 1 calc R . . H65B H 0.7458 0.4144 0.1724 0.077 Uiso 1 calc R . . H65C H 0.8133 0.4185 0.2374 0.077 Uiso 1 calc R . . C66 C 0.8209(3) 0.3237(3) 0.3131(2) 0.0608(14) Uani 1 d . . . H66A H 0.8098 0.3069 0.2788 0.091 Uiso 1 calc R . . H66B H 0.8565 0.2830 0.3415 0.091 Uiso 1 calc R . . H66C H 0.8480 0.3775 0.3243 0.091 Uiso 1 calc R . . C67 C 0.6108(3) 0.1077(3) 0.50131(17) 0.0492(11) Uani 1 d D . . C68 C 0.6629(3) 0.1696(3) 0.5065(2) 0.0501(12) Uani 1 d D . . H68 H 0.6880 0.2073 0.5361 0.060 Uiso 1 calc R . . C69 C 0.6776(3) 0.1761(3) 0.4698(2) 0.0544(12) Uani 1 d D . . H69 H 0.7126 0.2186 0.4742 0.065 Uiso 1 calc R . . C70 C 0.6421(3) 0.1210(3) 0.4250(2) 0.0562(12) Uani 1 d D . . H70 H 0.6520 0.1260 0.3991 0.067 Uiso 1 calc R . . C71 C 0.5931(3) 0.0605(3) 0.42097(19) 0.0550(12) Uani 1 d D . . H71 H 0.5694 0.0217 0.3921 0.066 Uiso 1 calc R . . C72 C 0.5771(3) 0.0543(3) 0.45792(17) 0.0430(10) Uani 1 d D . . H72 H 0.5418 0.0119 0.4532 0.052 Uiso 1 calc R . . C73 C 0.5933(4) 0.1021(3) 0.5396(2) 0.0654(14) Uani 1 d D . . H73A H 0.5347 0.1116 0.5203 0.098 Uiso 1 calc R . . H73B H 0.6252 0.1436 0.5683 0.098 Uiso 1 calc R . . H73C H 0.6081 0.0472 0.5562 0.098 Uiso 1 calc R . . C74 C 0.4735(3) 0.1706(3) 0.08437(17) 0.0460(11) Uani 1 d D . . C75 C 0.5001(3) 0.2105(3) 0.05861(18) 0.0475(11) Uani 1 d D . . H75 H 0.5273 0.2619 0.0724 0.057 Uiso 1 calc R . . C76 C 0.4884(3) 0.1779(3) 0.01396(19) 0.0523(12) Uani 1 d D . . H76 H 0.5070 0.2068 -0.0030 0.063 Uiso 1 calc R . . C77 C 0.4501(3) 0.1037(3) -0.0064(2) 0.0586(13) Uani 1 d D . . H77 H 0.4425 0.0806 -0.0373 0.070 Uiso 1 calc R . . C78 C 0.4225(3) 0.0629(3) 0.0179(2) 0.0587(13) Uani 1 d D . . H78 H 0.3952 0.0117 0.0036 0.070 Uiso 1 calc R . . C79 C 0.4345(3) 0.0965(3) 0.06334(19) 0.0496(11) Uani 1 d D . . H79 H 0.4154 0.0678 0.0801 0.060 Uiso 1 calc R . . C80 C 0.4887(4) 0.2053(4) 0.1336(2) 0.0742(16) Uani 1 d D . . H80A H 0.4469 0.1854 0.1364 0.111 Uiso 1 calc R . . H80B H 0.4865 0.2654 0.1312 0.111 Uiso 1 calc R . . H80C H 0.5430 0.1882 0.1660 0.111 Uiso 1 calc R . . C81 C 0.9874(5) 0.1709(5) 0.5620(4) 0.117(2) Uani 1 d DU . . C82 C 0.9523(5) 0.2470(4) 0.5444(3) 0.0934(18) Uani 1 d DU . . H82 H 0.9741 0.2964 0.5650 0.112 Uiso 1 calc R . . C83 C 0.8809(5) 0.2406(6) 0.4923(3) 0.116(2) Uani 1 d DU . . H83 H 0.8558 0.2928 0.4784 0.139 Uiso 1 calc R . . C84 C 0.8337(5) 0.1780(5) 0.4533(4) 0.119(3) Uani 1 d DU . . H84 H 0.7819 0.1816 0.4182 0.143 Uiso 1 calc R . . C85 C 0.8810(5) 0.1137(5) 0.4787(4) 0.117(2) Uani 1 d DU . . H85 H 0.8607 0.0664 0.4560 0.141 Uiso 1 calc R . . C86 C 0.9561(4) 0.0966(4) 0.5327(3) 0.0967(19) Uani 1 d DU . . H86 H 0.9804 0.0440 0.5462 0.116 Uiso 1 calc R . . C87 C 1.0590(5) 0.1608(7) 0.6110(4) 0.139(3) Uani 1 d DU . . H87A H 1.0611 0.1061 0.6249 0.208 Uiso 1 calc R . . H87B H 1.0655 0.2028 0.6360 0.208 Uiso 1 calc R . . H87C H 1.1033 0.1661 0.6082 0.208 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0229(3) 0.0268(3) 0.0316(4) -0.0017(3) 0.0113(3) -0.0024(3) Cl1 0.0326(5) 0.0393(5) 0.0398(5) -0.0031(4) 0.0196(4) -0.0052(4) Cl2 0.0268(5) 0.0418(5) 0.0428(5) -0.0015(4) 0.0185(4) -0.0030(4) Cl3 0.0403(6) 0.0304(5) 0.0580(7) -0.0040(4) 0.0285(5) -0.0012(4) N1 0.0223(15) 0.0304(16) 0.0326(17) 0.0005(13) 0.0122(14) -0.0018(13) N2 0.0237(15) 0.0371(18) 0.0314(17) 0.0002(14) 0.0156(14) -0.0031(13) N3 0.0246(15) 0.0273(16) 0.0344(17) 0.0004(13) 0.0134(14) -0.0005(12) C1 0.0281(19) 0.035(2) 0.034(2) 0.0052(16) 0.0176(17) 0.0003(16) C2 0.0235(18) 0.044(2) 0.030(2) 0.0007(17) 0.0148(17) -0.0035(16) C3 0.0232(18) 0.038(2) 0.0273(19) -0.0011(16) 0.0108(16) 0.0009(15) C4 0.0252(19) 0.060(3) 0.030(2) -0.0046(19) 0.0135(17) -0.0007(18) C5 0.041(3) 0.106(4) 0.047(3) -0.032(3) 0.032(2) -0.027(3) C6 0.079(4) 0.066(4) 0.143(6) 0.028(4) 0.088(5) 0.014(3) C7 0.064(4) 0.177(8) 0.173(8) 0.113(7) 0.090(5) 0.062(5) C8 0.029(2) 0.062(3) 0.032(2) -0.012(2) 0.0138(18) 0.0033(19) C9 0.036(2) 0.042(2) 0.040(2) -0.0132(19) 0.018(2) -0.0011(18) C10 0.029(2) 0.034(2) 0.039(2) -0.0055(17) 0.0169(18) -0.0007(16) C11 0.0258(18) 0.0318(19) 0.032(2) -0.0014(16) 0.0157(16) 0.0021(15) C12 0.0276(19) 0.0271(19) 0.044(2) -0.0059(17) 0.0187(18) 0.0000(15) C13 0.036(2) 0.033(2) 0.049(2) -0.0071(18) 0.028(2) -0.0008(17) C14 0.027(2) 0.042(2) 0.052(3) -0.004(2) 0.0197(19) 0.0068(17) C15 0.033(2) 0.048(2) 0.034(2) 0.0049(18) 0.0144(19) 0.0031(18) C16 0.032(2) 0.041(2) 0.043(2) 0.0125(19) 0.0188(19) 0.0072(18) C17 0.043(2) 0.032(2) 0.049(3) 0.0087(19) 0.026(2) 0.0059(18) C18 0.034(2) 0.031(2) 0.047(2) -0.0005(18) 0.022(2) 0.0008(17) C19 0.0294(19) 0.0295(19) 0.038(2) 0.0022(16) 0.0183(18) 0.0015(15) C20 0.0281(19) 0.029(2) 0.037(2) -0.0017(16) 0.0147(18) -0.0015(15) C21 0.0295(19) 0.0265(19) 0.032(2) -0.0022(16) 0.0120(17) -0.0042(15) C22 0.030(2) 0.031(2) 0.038(2) 0.0011(17) 0.0133(18) -0.0005(16) C23 0.031(2) 0.054(3) 0.044(2) 0.009(2) 0.018(2) 0.0087(19) C24 0.038(2) 0.059(3) 0.064(3) -0.008(2) 0.028(2) 0.003(2) C25 0.059(3) 0.055(3) 0.085(4) 0.014(3) 0.048(3) 0.003(2) C26 0.035(2) 0.044(3) 0.047(3) 0.007(2) 0.015(2) 0.0093(19) C27 0.042(2) 0.050(3) 0.035(2) 0.009(2) 0.014(2) 0.006(2) C28 0.042(2) 0.040(2) 0.040(2) 0.0007(18) 0.020(2) 0.0039(18) C29 0.031(2) 0.031(2) 0.035(2) -0.0046(16) 0.0130(18) -0.0033(16) C30 0.034(2) 0.045(2) 0.039(2) 0.0035(19) 0.0161(19) 0.0057(18) C31 0.044(3) 0.067(3) 0.046(3) -0.003(2) 0.026(2) 0.001(2) C32 0.051(3) 0.051(3) 0.056(3) -0.001(2) 0.030(2) 0.013(2) C33 0.042(2) 0.031(2) 0.041(2) -0.0052(18) 0.013(2) -0.0063(18) Ti2 0.0401(4) 0.0213(3) 0.0283(3) 0.0005(3) 0.0218(3) 0.0014(3) Cl4 0.0352(5) 0.0375(5) 0.0305(5) 0.0062(4) 0.0184(4) 0.0002(4) Cl5 0.0558(6) 0.0437(6) 0.0304(5) 0.0027(4) 0.0235(5) -0.0091(5) Cl6 0.1140(11) 0.0282(5) 0.0692(8) 0.0030(5) 0.0737(8) 0.0110(6) N4 0.0351(17) 0.0261(16) 0.0277(16) 0.0003(12) 0.0169(14) 0.0027(13) N5 0.0397(18) 0.0237(15) 0.0282(16) 0.0022(12) 0.0211(15) 0.0019(13) N6 0.0349(17) 0.0282(16) 0.0228(15) -0.0006(12) 0.0135(14) 0.0008(13) C34 0.045(2) 0.0257(19) 0.0279(19) 0.0020(15) 0.0211(18) 0.0031(16) C35 0.045(2) 0.0254(18) 0.0289(19) 0.0006(15) 0.0234(18) -0.0006(16) C36 0.041(2) 0.0197(17) 0.040(2) 0.0045(15) 0.0247(19) 0.0012(15) C37 0.047(2) 0.0222(18) 0.044(2) -0.0003(16) 0.030(2) -0.0003(16) C38 0.048(2) 0.035(2) 0.040(2) -0.0014(18) 0.031(2) -0.0034(18) C39 0.079(3) 0.046(3) 0.050(3) -0.008(2) 0.047(3) -0.012(2) C40 0.048(3) 0.039(2) 0.049(3) 0.007(2) 0.031(2) 0.0017(19) C41 0.056(3) 0.033(2) 0.059(3) 0.003(2) 0.042(3) 0.006(2) C42 0.051(3) 0.034(2) 0.072(3) 0.010(2) 0.041(3) 0.009(2) C43 0.044(2) 0.029(2) 0.052(3) 0.0112(19) 0.025(2) 0.0055(18) C44 0.044(2) 0.0220(18) 0.044(2) 0.0033(16) 0.025(2) -0.0032(16) C45 0.038(2) 0.038(2) 0.033(2) 0.0058(18) 0.0159(19) -0.0062(18) C46 0.058(3) 0.051(3) 0.041(3) -0.002(2) 0.025(2) -0.013(2) C47 0.048(3) 0.049(3) 0.046(3) 0.015(2) 0.021(2) -0.004(2) C48 0.056(3) 0.025(2) 0.057(3) -0.0021(18) 0.039(2) -0.0026(18) C49 0.056(3) 0.027(2) 0.044(2) 0.0009(17) 0.031(2) 0.0030(19) C50 0.062(3) 0.027(2) 0.054(3) 0.0017(19) 0.035(2) 0.011(2) C51 0.046(3) 0.037(2) 0.052(3) 0.005(2) 0.028(2) 0.0103(19) C52 0.038(2) 0.029(2) 0.034(2) 0.0025(16) 0.0190(18) 0.0071(16) C53 0.031(2) 0.034(2) 0.032(2) 0.0010(16) 0.0143(17) 0.0030(16) C54 0.0273(19) 0.031(2) 0.034(2) -0.0010(16) 0.0153(17) 0.0032(15) C55 0.030(2) 0.037(2) 0.037(2) -0.0084(17) 0.0182(18) -0.0012(16) C56 0.041(2) 0.044(2) 0.034(2) -0.0071(18) 0.0182(19) -0.0068(19) C57 0.055(4) 0.173(8) 0.078(4) 0.070(5) 0.027(3) 0.025(4) C58 0.150(7) 0.080(4) 0.053(3) -0.007(3) 0.063(4) 0.021(4) C59 0.041(2) 0.033(2) 0.054(3) -0.015(2) 0.026(2) -0.0049(18) C60 0.044(2) 0.035(2) 0.062(3) -0.003(2) 0.032(2) -0.0026(19) C61 0.040(2) 0.039(2) 0.053(3) 0.004(2) 0.031(2) 0.0017(18) C62 0.0267(19) 0.038(2) 0.034(2) 0.0006(17) 0.0162(17) -0.0017(16) C63 0.037(2) 0.046(2) 0.034(2) -0.0032(18) 0.0204(19) -0.0056(18) C64 0.043(2) 0.059(3) 0.036(2) 0.008(2) 0.024(2) -0.003(2) C65 0.050(3) 0.058(3) 0.053(3) -0.007(2) 0.035(2) -0.004(2) C66 0.035(2) 0.048(3) 0.085(4) 0.008(3) 0.030(3) 0.008(2) C67 0.049(3) 0.046(3) 0.039(2) 0.007(2) 0.020(2) 0.014(2) C68 0.047(3) 0.030(2) 0.055(3) 0.003(2) 0.023(2) 0.0026(19) C69 0.051(3) 0.042(3) 0.057(3) 0.009(2) 0.026(3) 0.004(2) C70 0.047(3) 0.048(3) 0.068(3) 0.014(2) 0.033(3) 0.010(2) C71 0.047(3) 0.063(3) 0.041(3) 0.003(2) 0.020(2) 0.013(2) C72 0.033(2) 0.037(2) 0.043(2) 0.0056(19) 0.016(2) 0.0038(17) C73 0.077(4) 0.058(3) 0.060(3) 0.013(3) 0.042(3) 0.019(3) C74 0.046(3) 0.052(3) 0.039(2) 0.008(2) 0.026(2) 0.016(2) C75 0.036(2) 0.050(3) 0.047(3) 0.012(2) 0.021(2) 0.008(2) C76 0.048(3) 0.066(3) 0.052(3) 0.020(2) 0.036(2) 0.017(2) C77 0.075(4) 0.057(3) 0.053(3) 0.008(2) 0.044(3) 0.019(3) C78 0.072(3) 0.042(3) 0.063(3) 0.005(2) 0.042(3) 0.005(2) C79 0.059(3) 0.049(3) 0.053(3) 0.020(2) 0.041(3) 0.014(2) C80 0.095(5) 0.079(4) 0.061(3) -0.003(3) 0.055(4) 0.006(3) C81 0.127(5) 0.104(4) 0.174(6) 0.037(4) 0.120(4) 0.028(4) C82 0.124(5) 0.073(3) 0.117(4) 0.008(3) 0.091(4) 0.008(3) C83 0.128(6) 0.132(5) 0.111(5) 0.004(4) 0.084(4) -0.024(4) C84 0.077(5) 0.123(6) 0.137(6) 0.020(4) 0.056(4) -0.001(3) C85 0.129(5) 0.125(5) 0.172(5) 0.056(4) 0.130(4) 0.049(4) C86 0.110(4) 0.069(3) 0.177(6) 0.038(3) 0.121(4) 0.023(3) C87 0.123(6) 0.206(9) 0.134(6) 0.052(5) 0.102(4) 0.038(5) _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 N1 2.148(3) . ? Ti1 N2 2.215(3) . ? Ti1 N3 2.268(3) . ? Ti1 Cl3 2.2980(13) . ? Ti1 Cl1 2.3439(13) . ? Ti1 Cl2 2.4287(13) . ? N1 C1 1.339(5) . ? N1 C19 1.347(5) . ? N2 C2 1.284(5) . ? N2 C3 1.454(5) . ? N3 C20 1.285(5) . ? N3 C21 1.453(5) . ? C1 C16 1.386(5) . ? C1 C2 1.475(5) . ? C2 C15 1.498(5) . ? C3 C11 1.405(5) . ? C3 C4 1.405(6) . ? C4 C8 1.389(6) . ? C4 C5 1.517(6) . ? C5 C7 1.491(9) . ? C5 C6 1.492(8) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.372(6) . ? C8 H8 0.9500 . ? C9 C10 1.374(6) . ? C9 H9 0.9500 . ? C10 C11 1.397(5) . ? C10 H10 0.9500 . ? C11 C12 1.522(5) . ? C12 C13 1.522(6) . ? C12 C14 1.534(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.371(6) . ? C16 H16 0.9500 . ? C17 C18 1.390(6) . ? C17 H17 0.9500 . ? C18 C19 1.378(5) . ? C18 H18 0.9500 . ? C19 C20 1.480(5) . ? C20 C33 1.499(5) . ? C21 C29 1.400(6) . ? C21 C22 1.411(5) . ? C22 C26 1.390(6) . ? C22 C23 1.500(6) . ? C23 C24 1.533(6) . ? C23 C25 1.535(7) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.377(7) . ? C26 H26 0.9500 . ? C27 C28 1.373(6) . ? C27 H27 0.9500 . ? C28 C29 1.387(6) . ? C28 H28 0.9500 . ? C29 C30 1.528(6) . ? C30 C31 1.524(6) . ? C30 C32 1.531(6) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? Ti2 N4 2.146(3) . ? Ti2 N5 2.185(3) . ? Ti2 N6 2.242(3) . ? Ti2 Cl6 2.2968(13) . ? Ti2 Cl4 2.3385(12) . ? Ti2 Cl5 2.3986(13) . ? N4 C52 1.335(5) . ? N4 C34 1.342(5) . ? N5 C35 1.293(5) . ? N5 C36 1.458(5) . ? N6 C53 1.283(5) . ? N6 C54 1.454(5) . ? C34 C49 1.388(5) . ? C34 C35 1.476(6) . ? C35 C48 1.491(5) . ? C36 C37 1.396(5) . ? C36 C44 1.407(6) . ? C37 C41 1.386(6) . ? C37 C38 1.509(6) . ? C38 C40 1.528(6) . ? C38 C39 1.535(6) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.381(6) . ? C41 H41 0.9500 . ? C42 C43 1.373(7) . ? C42 H42 0.9500 . ? C43 C44 1.394(6) . ? C43 H43 0.9500 . ? C44 C45 1.517(6) . ? C45 C47 1.528(6) . ? C45 C46 1.532(6) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.372(6) . ? C49 H49 0.9500 . ? C50 C51 1.398(6) . ? C50 H50 0.9500 . ? C51 C52 1.387(6) . ? C51 H51 0.9500 . ? C52 C53 1.481(6) . ? C53 C66 1.487(6) . ? C54 C62 1.401(5) . ? C54 C55 1.409(5) . ? C55 C59 1.389(6) . ? C55 C56 1.515(6) . ? C56 C57 1.508(7) . ? C56 C58 1.515(7) . ? C56 H56 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.352(6) . ? C59 H59 0.9500 . ? C60 C61 1.371(6) . ? C60 H60 0.9500 . ? C61 C62 1.395(6) . ? C61 H61 0.9500 . ? C62 C63 1.512(6) . ? C63 C64 1.526(6) . ? C63 C65 1.540(6) . ? C63 H63 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C72 1.379(6) . ? C67 C68 1.413(6) . ? C67 C73 1.448(6) . ? C68 C69 1.357(6) . ? C68 H68 0.9500 . ? C69 C70 1.421(6) . ? C69 H69 0.9500 . ? C70 C71 1.363(7) . ? C70 H70 0.9500 . ? C71 C72 1.385(6) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C79 1.372(6) . ? C74 C75 1.385(6) . ? C74 C80 1.473(6) . ? C75 C76 1.362(6) . ? C75 H75 0.9500 . ? C76 C77 1.367(6) . ? C76 H76 0.9500 . ? C77 C78 1.370(6) . ? C77 H77 0.9500 . ? C78 C79 1.389(6) . ? C78 H78 0.9500 . ? C79 H79 0.9500 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C87 1.327(10) . ? C81 C82 1.368(8) . ? C81 C86 1.407(9) . ? C82 C83 1.366(9) . ? C82 H82 0.9500 . ? C83 C84 1.414(9) . ? C83 H83 0.9500 . ? C84 C85 1.312(8) . ? C84 H84 0.9500 . ? C85 C86 1.447(9) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti1 N2 72.37(12) . . ? N1 Ti1 N3 72.01(11) . . ? N2 Ti1 N3 143.44(12) . . ? N1 Ti1 Cl3 169.53(10) . . ? N2 Ti1 Cl3 100.30(9) . . ? N3 Ti1 Cl3 116.07(9) . . ? N1 Ti1 Cl1 92.54(9) . . ? N2 Ti1 Cl1 89.83(9) . . ? N3 Ti1 Cl1 83.78(9) . . ? Cl3 Ti1 Cl1 94.94(4) . . ? N1 Ti1 Cl2 80.79(9) . . ? N2 Ti1 Cl2 94.24(9) . . ? N3 Ti1 Cl2 88.01(9) . . ? Cl3 Ti1 Cl2 92.54(4) . . ? Cl1 Ti1 Cl2 170.72(5) . . ? C1 N1 C19 119.8(3) . . ? C1 N1 Ti1 119.8(3) . . ? C19 N1 Ti1 119.8(2) . . ? C2 N2 C3 118.1(3) . . ? C2 N2 Ti1 117.9(3) . . ? C3 N2 Ti1 124.0(2) . . ? C20 N3 C21 118.1(3) . . ? C20 N3 Ti1 116.0(3) . . ? C21 N3 Ti1 125.8(2) . . ? N1 C1 C16 121.2(4) . . ? N1 C1 C2 113.2(3) . . ? C16 C1 C2 125.6(4) . . ? N2 C2 C1 116.4(3) . . ? N2 C2 C15 125.8(4) . . ? C1 C2 C15 117.8(4) . . ? C11 C3 C4 121.3(4) . . ? C11 C3 N2 119.9(3) . . ? C4 C3 N2 118.8(3) . . ? C8 C4 C3 117.8(4) . . ? C8 C4 C5 119.6(4) . . ? C3 C4 C5 122.5(4) . . ? C7 C5 C6 108.2(5) . . ? C7 C5 C4 113.0(5) . . ? C6 C5 C4 110.6(4) . . ? C7 C5 H5 108.3 . . ? C6 C5 H5 108.3 . . ? C4 C5 H5 108.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C4 121.9(4) . . ? C9 C8 H8 119.0 . . ? C4 C8 H8 119.0 . . ? C8 C9 C10 119.7(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 121.5(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C3 117.8(3) . . ? C10 C11 C12 117.8(3) . . ? C3 C11 C12 124.3(3) . . ? C13 C12 C11 111.7(3) . . ? C13 C12 C14 109.6(3) . . ? C11 C12 C14 110.5(3) . . ? C13 C12 H12 108.3 . . ? C11 C12 H12 108.3 . . ? C14 C12 H12 108.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 C15 H15A 109.5 . . ? C2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C1 119.1(4) . . ? C17 C16 H16 120.5 . . ? C1 C16 H16 120.5 . . ? C16 C17 C18 119.8(4) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 118.4(4) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? N1 C19 C18 121.6(4) . . ? N1 C19 C20 113.4(3) . . ? C18 C19 C20 124.8(4) . . ? N3 C20 C19 116.9(3) . . ? N3 C20 C33 125.9(4) . . ? C19 C20 C33 117.2(3) . . ? C29 C21 C22 121.7(4) . . ? C29 C21 N3 119.0(3) . . ? C22 C21 N3 119.3(4) . . ? C26 C22 C21 117.2(4) . . ? C26 C22 C23 119.9(4) . . ? C21 C22 C23 122.8(4) . . ? C22 C23 C24 112.1(4) . . ? C22 C23 C25 110.9(4) . . ? C24 C23 C25 110.0(4) . . ? C22 C23 H23 107.9 . . ? C24 C23 H23 107.9 . . ? C25 C23 H23 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C22 122.3(4) . . ? C27 C26 H26 118.9 . . ? C22 C26 H26 118.9 . . ? C28 C27 C26 119.0(4) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 122.3(4) . . ? C27 C28 H28 118.8 . . ? C29 C28 H28 118.8 . . ? C28 C29 C21 117.5(4) . . ? C28 C29 C30 117.6(4) . . ? C21 C29 C30 124.8(4) . . ? C31 C30 C29 112.0(4) . . ? C31 C30 C32 108.9(4) . . ? C29 C30 C32 111.4(3) . . ? C31 C30 H30 108.2 . . ? C29 C30 H30 108.2 . . ? C32 C30 H30 108.2 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C20 C33 H33A 109.5 . . ? C20 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C20 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 Ti2 N5 72.61(12) . . ? N4 Ti2 N6 72.26(12) . . ? N5 Ti2 N6 144.27(11) . . ? N4 Ti2 Cl6 168.50(9) . . ? N5 Ti2 Cl6 99.69(9) . . ? N6 Ti2 Cl6 116.01(9) . . ? N4 Ti2 Cl4 93.97(9) . . ? N5 Ti2 Cl4 92.73(8) . . ? N6 Ti2 Cl4 83.39(8) . . ? Cl6 Ti2 Cl4 94.94(5) . . ? N4 Ti2 Cl5 79.85(9) . . ? N5 Ti2 Cl5 91.35(9) . . ? N6 Ti2 Cl5 88.77(8) . . ? Cl6 Ti2 Cl5 92.01(5) . . ? Cl4 Ti2 Cl5 171.23(5) . . ? C52 N4 C34 120.8(3) . . ? C52 N4 Ti2 119.4(3) . . ? C34 N4 Ti2 118.5(3) . . ? C35 N5 C36 119.1(3) . . ? C35 N5 Ti2 118.8(3) . . ? C36 N5 Ti2 122.0(2) . . ? C53 N6 C54 121.3(3) . . ? C53 N6 Ti2 117.5(3) . . ? C54 N6 Ti2 121.1(2) . . ? N4 C34 C49 121.1(4) . . ? N4 C34 C35 113.9(3) . . ? C49 C34 C35 125.0(4) . . ? N5 C35 C34 114.9(3) . . ? N5 C35 C48 125.8(4) . . ? C34 C35 C48 119.3(3) . . ? C37 C36 C44 121.9(4) . . ? C37 C36 N5 119.3(3) . . ? C44 C36 N5 118.9(3) . . ? C41 C37 C36 117.9(4) . . ? C41 C37 C38 119.3(4) . . ? C36 C37 C38 122.7(4) . . ? C37 C38 C40 110.5(3) . . ? C37 C38 C39 112.2(4) . . ? C40 C38 C39 110.0(3) . . ? C37 C38 H38 108.0 . . ? C40 C38 H38 108.0 . . ? C39 C38 H38 108.0 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C37 121.8(4) . . ? C42 C41 H41 119.1 . . ? C37 C41 H41 119.1 . . ? C43 C42 C41 119.3(4) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C42 C43 C44 122.0(4) . . ? C42 C43 H43 119.0 . . ? C44 C43 H43 119.0 . . ? C43 C44 C36 117.2(4) . . ? C43 C44 C45 119.9(4) . . ? C36 C44 C45 122.8(4) . . ? C44 C45 C47 112.0(4) . . ? C44 C45 C46 110.9(3) . . ? C47 C45 C46 109.6(4) . . ? C44 C45 H45 108.1 . . ? C47 C45 H45 108.1 . . ? C46 C45 H45 108.1 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C35 C48 H48A 109.5 . . ? C35 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C35 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C34 118.7(4) . . ? C50 C49 H49 120.7 . . ? C34 C49 H49 120.7 . . ? C49 C50 C51 120.1(4) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C52 C51 C50 118.3(4) . . ? C52 C51 H51 120.9 . . ? C50 C51 H51 120.9 . . ? N4 C52 C51 121.0(4) . . ? N4 C52 C53 114.2(3) . . ? C51 C52 C53 124.7(4) . . ? N6 C53 C52 115.7(4) . . ? N6 C53 C66 126.2(4) . . ? C52 C53 C66 118.1(4) . . ? C62 C54 C55 121.3(4) . . ? C62 C54 N6 120.2(3) . . ? C55 C54 N6 118.4(3) . . ? C59 C55 C54 117.4(4) . . ? C59 C55 C56 120.8(4) . . ? C54 C55 C56 121.8(4) . . ? C57 C56 C58 111.7(5) . . ? C57 C56 C55 109.6(4) . . ? C58 C56 C55 113.5(4) . . ? C57 C56 H56 107.2 . . ? C58 C56 H56 107.2 . . ? C55 C56 H56 107.2 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C55 122.2(4) . . ? C60 C59 H59 118.9 . . ? C55 C59 H59 118.9 . . ? C59 C60 C61 119.6(4) . . ? C59 C60 H60 120.2 . . ? C61 C60 H60 120.2 . . ? C60 C61 C62 122.1(4) . . ? C60 C61 H61 119.0 . . ? C62 C61 H61 119.0 . . ? C61 C62 C54 117.0(4) . . ? C61 C62 C63 117.9(4) . . ? C54 C62 C63 125.1(4) . . ? C62 C63 C64 111.8(4) . . ? C62 C63 C65 110.4(3) . . ? C64 C63 C65 109.2(4) . . ? C62 C63 H63 108.5 . . ? C64 C63 H63 108.5 . . ? C65 C63 H63 108.5 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C53 C66 H66A 109.5 . . ? C53 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C53 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C72 C67 C68 116.7(4) . . ? C72 C67 C73 122.3(5) . . ? C68 C67 C73 121.0(4) . . ? C69 C68 C67 121.0(4) . . ? C69 C68 H68 119.5 . . ? C67 C68 H68 119.5 . . ? C68 C69 C70 121.8(5) . . ? C68 C69 H69 119.1 . . ? C70 C69 H69 119.1 . . ? C71 C70 C69 116.8(5) . . ? C71 C70 H70 121.6 . . ? C69 C70 H70 121.6 . . ? C70 C71 C72 121.6(5) . . ? C70 C71 H71 119.2 . . ? C72 C71 H71 119.2 . . ? C67 C72 C71 122.1(4) . . ? C67 C72 H72 118.9 . . ? C71 C72 H72 118.9 . . ? C67 C73 H73A 109.5 . . ? C67 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C67 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C79 C74 C75 117.7(4) . . ? C79 C74 C80 121.1(4) . . ? C75 C74 C80 121.2(5) . . ? C76 C75 C74 121.7(5) . . ? C76 C75 H75 119.2 . . ? C74 C75 H75 119.2 . . ? C75 C76 C77 120.2(4) . . ? C75 C76 H76 119.9 . . ? C77 C76 H76 119.9 . . ? C76 C77 C78 119.6(5) . . ? C76 C77 H77 120.2 . . ? C78 C77 H77 120.2 . . ? C77 C78 C79 120.0(5) . . ? C77 C78 H78 120.0 . . ? C79 C78 H78 120.0 . . ? C74 C79 C78 120.8(4) . . ? C74 C79 H79 119.6 . . ? C78 C79 H79 119.6 . . ? C74 C80 H80A 109.5 . . ? C74 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C74 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C87 C81 C82 120.9(9) . . ? C87 C81 C86 112.2(8) . . ? C82 C81 C86 126.9(9) . . ? C83 C82 C81 108.9(8) . . ? C83 C82 H82 125.5 . . ? C81 C82 H82 125.5 . . ? C82 C83 C84 137.9(9) . . ? C82 C83 H83 111.0 . . ? C84 C83 H83 111.0 . . ? C85 C84 C83 101.1(8) . . ? C85 C84 H84 129.4 . . ? C83 C84 H84 129.4 . . ? C84 C85 C86 136.1(9) . . ? C84 C85 H85 111.9 . . ? C86 C85 H85 111.9 . . ? C81 C86 C85 108.8(7) . . ? C81 C86 H86 125.6 . . ? C85 C86 H86 125.6 . . ? C81 C87 H87A 109.5 . . ? C81 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C81 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? _diffrn_measured_fraction_theta_max .962 _diffrn_reflns_theta_full 27.25 _diffrn_measured_fraction_theta_full .962 _refine_diff_density_max 1.200 _refine_diff_density_min -.801 _refine_diff_density_rms .083 #===END #===END #============================================================================== data_gp48 _database_code_depnum_ccdc_archive 'CCDC 252937' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [2,6?bis[1?(2,6?diisopropylphenylimino)ethyl]pyridine]dichloro (aluminumoxotrichoride)titanium(IV) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H43 Al Cl5 N3 O Ti' _chemical_formula_weight 749.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al .0645 .0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti .2776 .4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.683(4) _cell_length_b 16.764(5) _cell_length_c 17.317(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.791(12) _cell_angle_gamma 90.00 _cell_volume 3656.1(19) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 946 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 25.55 _exptl_crystal_description rod _exptl_crystal_colour brown _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8695 _exptl_absorpt_correction_T_max 0.9257 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59704 _diffrn_reflns_av_R_equivalents 0.1011 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.89 _reflns_number_total 7002 _reflns_number_gt 4543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+3.0000P] 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 7002 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.84055(5) 0.09519(4) 0.26225(4) 0.02800(18) Uani 1 d . . . Cl1 Cl 0.94020(7) 0.08795(6) 0.15699(5) 0.0384(3) Uani 1 d . . . Cl2 Cl 0.90141(9) -0.02429(6) 0.30832(6) 0.0439(3) Uani 1 d . . . Cl3 Cl 0.70953(9) 0.27706(7) 0.41781(7) 0.0528(3) Uani 1 d . . . Cl4 Cl 0.58671(9) 0.09733(7) 0.45987(6) 0.0485(3) Uani 1 d . . . Cl5 Cl 0.52486(8) 0.18803(7) 0.27947(6) 0.0443(3) Uani 1 d . . . Al1 Al 0.64991(9) 0.16556(7) 0.37213(7) 0.0332(3) Uani 1 d . . . N1 N 0.7917(2) 0.20817(17) 0.21273(16) 0.0273(7) Uani 1 d . . . N2 N 0.7056(2) 0.07204(18) 0.17150(16) 0.0265(7) Uani 1 d . . . N3 N 0.9558(2) 0.18570(18) 0.31238(16) 0.0275(7) Uani 1 d . . . C1 C 0.7051(3) 0.2117(2) 0.1598(2) 0.0288(8) Uani 1 d . . . C2 C 0.6587(3) 0.1330(2) 0.1378(2) 0.0303(9) Uani 1 d . . . C3 C 0.6730(3) -0.0082(2) 0.1459(2) 0.0290(8) Uani 1 d . . . C4 C 0.6147(3) -0.0550(2) 0.1930(2) 0.0355(9) Uani 1 d . . . C5 C 0.5784(3) -0.0259(2) 0.2685(2) 0.0371(9) Uani 1 d . . . H5 H 0.6124 0.0270 0.2815 0.045 Uiso 1 calc R . . C6 C 0.4589(3) -0.0145(3) 0.2588(3) 0.0491(11) Uani 1 d . . . H6A H 0.4387 0.0233 0.2164 0.074 Uiso 1 calc R . . H6B H 0.4368 0.0064 0.3072 0.074 Uiso 1 calc R . . H6C H 0.4239 -0.0658 0.2464 0.074 Uiso 1 calc R . . C7 C 0.6119(4) -0.0834(3) 0.3362(2) 0.0514(12) Uani 1 d . . . H7A H 0.5779 -0.1353 0.3252 0.077 Uiso 1 calc R . . H7B H 0.5899 -0.0616 0.3843 0.077 Uiso 1 calc R . . H7C H 0.6892 -0.0899 0.3422 0.077 Uiso 1 calc R . . C8 C 0.5829(3) -0.1299(2) 0.1667(2) 0.0451(11) Uani 1 d . . . H8 H 0.5400 -0.1611 0.1965 0.054 Uiso 1 calc R . . C9 C 0.6112(4) -0.1607(3) 0.0988(2) 0.0468(11) Uani 1 d . . . H9 H 0.5903 -0.2132 0.0830 0.056 Uiso 1 calc R . . C10 C 0.6700(3) -0.1150(2) 0.0537(2) 0.0426(11) Uani 1 d . . . H10 H 0.6908 -0.1371 0.0073 0.051 Uiso 1 calc R . . C11 C 0.7000(3) -0.0368(2) 0.0743(2) 0.0330(9) Uani 1 d . . . C12 C 0.7557(3) 0.0107(3) 0.0168(2) 0.0392(10) Uani 1 d . . . H12 H 0.7708 0.0654 0.0383 0.047 Uiso 1 calc R . . C13 C 0.6848(3) 0.0178(3) -0.0609(2) 0.0431(10) Uani 1 d . . . H13A H 0.6713 -0.0354 -0.0833 0.065 Uiso 1 calc R . . H13B H 0.7204 0.0508 -0.0967 0.065 Uiso 1 calc R . . H13C H 0.6172 0.0427 -0.0523 0.065 Uiso 1 calc R . . C14 C 0.8615(3) -0.0293(3) 0.0038(3) 0.0550(13) Uani 1 d . . . H14A H 0.9057 -0.0355 0.0538 0.083 Uiso 1 calc R . . H14B H 0.8988 0.0040 -0.0308 0.083 Uiso 1 calc R . . H14C H 0.8474 -0.0818 -0.0200 0.083 Uiso 1 calc R . . C15 C 0.5616(3) 0.1305(2) 0.0797(2) 0.0376(10) Uani 1 d . . . H15A H 0.5372 0.0753 0.0726 0.056 Uiso 1 calc R . . H15B H 0.5785 0.1519 0.0299 0.056 Uiso 1 calc R . . H15C H 0.5055 0.1629 0.0984 0.056 Uiso 1 calc R . . C16 C 0.6688(3) 0.2845(2) 0.1287(2) 0.0360(9) Uani 1 d . . . H16 H 0.6088 0.2869 0.0904 0.043 Uiso 1 calc R . . C17 C 0.7214(3) 0.3525(2) 0.1544(2) 0.0392(10) Uani 1 d . . . H17 H 0.6981 0.4027 0.1333 0.047 Uiso 1 calc R . . C18 C 0.8086(3) 0.3490(2) 0.2111(2) 0.0397(10) Uani 1 d . . . H18 H 0.8444 0.3962 0.2298 0.048 Uiso 1 calc R . . C19 C 0.8418(3) 0.2746(2) 0.2395(2) 0.0307(9) Uani 1 d . . . C20 C 0.9353(3) 0.2597(2) 0.2976(2) 0.0309(9) Uani 1 d . . . C21 C 1.0531(3) 0.1640(2) 0.3620(2) 0.0298(9) Uani 1 d . . . C22 C 1.1482(3) 0.1581(2) 0.3279(2) 0.0349(9) Uani 1 d . . . C23 C 1.1568(3) 0.1790(3) 0.2437(2) 0.0463(11) Uani 1 d . . . H23 H 1.0834 0.1885 0.2173 0.056 Uiso 1 calc R . . C24 C 1.2048(4) 0.1137(4) 0.2013(3) 0.0792(19) Uani 1 d . . . H24A H 1.2800 0.1080 0.2214 0.119 Uiso 1 calc R . . H24B H 1.1985 0.1264 0.1457 0.119 Uiso 1 calc R . . H24C H 1.1676 0.0636 0.2088 0.119 Uiso 1 calc R . . C25 C 1.2208(4) 0.2558(3) 0.2371(3) 0.0662(15) Uani 1 d . . . H25A H 1.1883 0.2993 0.2639 0.099 Uiso 1 calc R . . H25B H 1.2210 0.2696 0.1821 0.099 Uiso 1 calc R . . H25C H 1.2939 0.2476 0.2611 0.099 Uiso 1 calc R . . C26 C 1.2387(3) 0.1336(3) 0.3758(2) 0.0449(11) Uani 1 d . . . H26 H 1.3039 0.1284 0.3544 0.054 Uiso 1 calc R . . C27 C 1.2359(3) 0.1168(3) 0.4532(3) 0.0492(12) Uani 1 d . . . H27 H 1.2983 0.0995 0.4844 0.059 Uiso 1 calc R . . C28 C 1.1420(3) 0.1252(3) 0.4853(2) 0.0474(11) Uani 1 d . . . H28 H 1.1409 0.1142 0.5390 0.057 Uiso 1 calc R . . C29 C 1.0485(3) 0.1496(2) 0.4409(2) 0.0345(9) Uani 1 d . . . C30 C 0.9483(3) 0.1623(3) 0.4792(2) 0.0414(10) Uani 1 d . . . H30 H 0.8933 0.1848 0.4390 0.050 Uiso 1 calc R . . C31 C 0.9040(3) 0.0853(3) 0.5087(2) 0.0452(11) Uani 1 d . . . H31A H 0.8936 0.0465 0.4662 0.068 Uiso 1 calc R . . H31B H 0.8357 0.0961 0.5279 0.068 Uiso 1 calc R . . H31C H 0.9539 0.0636 0.5510 0.068 Uiso 1 calc R . . C32 C 0.9674(4) 0.2242(3) 0.5453(3) 0.0579(13) Uani 1 d . . . H32A H 1.0179 0.2026 0.5873 0.087 Uiso 1 calc R . . H32B H 0.9000 0.2361 0.5654 0.087 Uiso 1 calc R . . H32C H 0.9963 0.2732 0.5252 0.087 Uiso 1 calc R . . C33 C 0.9962(4) 0.3287(2) 0.3340(2) 0.0442(10) Uani 1 d . . . H33A H 1.0585 0.3092 0.3676 0.066 Uiso 1 calc R . . H33B H 0.9509 0.3595 0.3652 0.066 Uiso 1 calc R . . H33C H 1.0193 0.3629 0.2933 0.066 Uiso 1 calc R . . O1 O 0.75323(19) 0.11622(14) 0.33229(14) 0.0298(6) Uani 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 0.0267(4) 0.0315(4) 0.0242(4) -0.0008(3) -0.0042(3) 0.0003(3) Cl1 0.0312(5) 0.0530(6) 0.0306(5) -0.0097(5) 0.0024(4) -0.0058(5) Cl2 0.0516(6) 0.0410(6) 0.0375(6) 0.0025(5) -0.0009(5) 0.0129(5) Cl3 0.0478(7) 0.0423(6) 0.0694(8) -0.0164(6) 0.0117(6) -0.0009(5) Cl4 0.0490(7) 0.0626(7) 0.0349(6) -0.0046(5) 0.0092(5) -0.0117(5) Cl5 0.0359(6) 0.0527(7) 0.0442(6) 0.0000(5) 0.0042(5) 0.0125(5) Al1 0.0287(6) 0.0383(7) 0.0330(6) -0.0050(5) 0.0057(5) 0.0011(5) N1 0.0276(16) 0.0323(18) 0.0219(16) 0.0019(13) 0.0021(13) 0.0019(14) N2 0.0197(15) 0.0359(18) 0.0230(16) 0.0026(13) -0.0015(12) 0.0012(13) N3 0.0247(16) 0.0368(19) 0.0205(16) -0.0033(13) 0.0006(12) -0.0006(14) C1 0.026(2) 0.037(2) 0.0247(19) 0.0046(17) 0.0075(16) 0.0053(16) C2 0.027(2) 0.044(2) 0.0193(19) 0.0029(17) 0.0040(15) 0.0000(18) C3 0.0254(19) 0.031(2) 0.027(2) 0.0009(16) -0.0113(16) -0.0005(16) C4 0.032(2) 0.039(2) 0.032(2) 0.0043(18) -0.0075(17) 0.0001(18) C5 0.034(2) 0.043(2) 0.033(2) 0.0033(18) -0.0018(17) -0.0044(18) C6 0.039(2) 0.060(3) 0.048(3) 0.004(2) 0.004(2) -0.005(2) C7 0.060(3) 0.057(3) 0.036(2) 0.003(2) -0.002(2) 0.000(2) C8 0.049(3) 0.041(3) 0.042(3) 0.003(2) -0.008(2) -0.013(2) C9 0.059(3) 0.037(2) 0.040(3) -0.002(2) -0.011(2) -0.003(2) C10 0.051(3) 0.044(3) 0.029(2) -0.0062(19) -0.013(2) 0.006(2) C11 0.026(2) 0.041(2) 0.029(2) 0.0022(18) -0.0074(16) -0.0001(17) C12 0.035(2) 0.052(3) 0.029(2) -0.0090(19) -0.0046(17) -0.0076(19) C13 0.048(3) 0.051(3) 0.029(2) -0.0009(19) -0.0026(19) -0.003(2) C14 0.036(2) 0.085(4) 0.044(3) -0.023(3) 0.003(2) -0.003(2) C15 0.030(2) 0.051(3) 0.030(2) 0.0015(19) -0.0050(17) 0.0055(19) C16 0.032(2) 0.045(2) 0.032(2) 0.0075(19) 0.0066(17) 0.0114(19) C17 0.048(3) 0.040(2) 0.031(2) 0.0095(19) 0.0104(19) 0.012(2) C18 0.050(3) 0.031(2) 0.039(2) 0.0003(18) 0.011(2) 0.0018(19) C19 0.034(2) 0.035(2) 0.0246(19) 0.0016(17) 0.0106(16) 0.0042(18) C20 0.035(2) 0.031(2) 0.027(2) -0.0038(16) 0.0063(16) -0.0029(17) C21 0.031(2) 0.029(2) 0.030(2) -0.0073(16) 0.0005(17) -0.0037(16) C22 0.028(2) 0.042(2) 0.032(2) -0.0077(18) -0.0022(17) -0.0075(17) C23 0.026(2) 0.081(3) 0.031(2) -0.008(2) -0.0006(18) -0.003(2) C24 0.044(3) 0.141(6) 0.049(3) -0.039(3) -0.008(2) 0.022(3) C25 0.037(3) 0.111(5) 0.050(3) 0.016(3) -0.001(2) -0.023(3) C26 0.028(2) 0.060(3) 0.045(3) -0.009(2) -0.0036(19) 0.001(2) C27 0.035(2) 0.065(3) 0.044(3) 0.009(2) -0.012(2) 0.002(2) C28 0.044(3) 0.066(3) 0.030(2) 0.005(2) -0.005(2) -0.001(2) C29 0.034(2) 0.039(2) 0.030(2) -0.0003(18) 0.0009(17) -0.0025(18) C30 0.042(2) 0.055(3) 0.026(2) -0.0040(19) 0.0021(18) 0.001(2) C31 0.040(2) 0.063(3) 0.034(2) -0.001(2) 0.0056(19) -0.003(2) C32 0.063(3) 0.068(3) 0.045(3) -0.019(2) 0.014(2) -0.006(3) C33 0.051(3) 0.036(2) 0.044(2) -0.0033(19) 0.000(2) -0.008(2) O1 0.0278(14) 0.0346(14) 0.0262(13) 0.0004(11) 0.0003(11) -0.0003(11) _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 O1 1.772(3) . ? Ti1 N1 2.140(3) . ? Ti1 N3 2.212(3) . ? Ti1 N2 2.217(3) . ? Ti1 Cl2 2.2580(13) . ? Ti1 Cl1 2.3409(13) . ? Cl3 Al1 2.1332(17) . ? Cl4 Al1 2.1325(16) . ? Cl5 Al1 2.1517(16) . ? Al1 O1 1.758(3) . ? N1 C19 1.337(5) . ? N1 C1 1.346(5) . ? N2 C2 1.287(5) . ? N2 C3 1.460(5) . ? N3 C20 1.287(5) . ? N3 C21 1.464(4) . ? C1 C16 1.389(5) . ? C1 C2 1.476(5) . ? C2 C15 1.496(5) . ? C3 C4 1.403(5) . ? C3 C11 1.409(5) . ? C4 C8 1.381(6) . ? C4 C5 1.517(5) . ? C5 C6 1.518(5) . ? C5 C7 1.538(6) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.370(6) . ? C8 H8 0.9500 . ? C9 C10 1.375(6) . ? C9 H9 0.9500 . ? C10 C11 1.400(5) . ? C10 H10 0.9500 . ? C11 C12 1.514(5) . ? C12 C13 1.532(5) . ? C12 C14 1.540(6) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.370(6) . ? C16 H16 0.9500 . ? C17 C18 1.389(6) . ? C17 H17 0.9500 . ? C18 C19 1.389(5) . ? C18 H18 0.9500 . ? C19 C20 1.483(5) . ? C20 C33 1.490(5) . ? C21 C29 1.396(5) . ? C21 C22 1.408(5) . ? C22 C26 1.397(5) . ? C22 C23 1.517(5) . ? C23 C24 1.489(6) . ? C23 C25 1.533(6) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.373(6) . ? C26 H26 0.9500 . ? C27 C28 1.380(6) . ? C27 H27 0.9500 . ? C28 C29 1.396(5) . ? C28 H28 0.9500 . ? C29 C30 1.516(5) . ? C30 C31 1.521(6) . ? C30 C32 1.541(6) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 O1 Ti1 N1 85.60(11) . . ? O1 Ti1 N3 91.86(11) . . ? N1 Ti1 N3 72.36(11) . . ? O1 Ti1 N2 91.57(11) . . ? N1 Ti1 N2 73.03(11) . . ? N3 Ti1 N2 144.83(11) . . ? O1 Ti1 Cl2 98.62(9) . . ? N1 Ti1 Cl2 175.73(9) . . ? N3 Ti1 Cl2 106.70(9) . . ? N2 Ti1 Cl2 107.35(9) . . ? O1 Ti1 Cl1 169.14(9) . . ? N1 Ti1 Cl1 83.76(8) . . ? N3 Ti1 Cl1 87.05(8) . . ? N2 Ti1 Cl1 83.20(8) . . ? Cl2 Ti1 Cl1 92.04(5) . . ? O1 Al1 Cl4 112.81(10) . . ? O1 Al1 Cl3 108.05(10) . . ? Cl4 Al1 Cl3 110.63(7) . . ? O1 Al1 Cl5 107.92(10) . . ? Cl4 Al1 Cl5 108.61(7) . . ? Cl3 Al1 Cl5 108.71(7) . . ? C19 N1 C1 121.0(3) . . ? C19 N1 Ti1 119.6(2) . . ? C1 N1 Ti1 119.1(2) . . ? C2 N2 C3 119.6(3) . . ? C2 N2 Ti1 117.3(2) . . ? C3 N2 Ti1 122.9(2) . . ? C20 N3 C21 119.5(3) . . ? C20 N3 Ti1 118.3(2) . . ? C21 N3 Ti1 122.1(2) . . ? N1 C1 C16 120.6(4) . . ? N1 C1 C2 113.8(3) . . ? C16 C1 C2 125.6(3) . . ? N2 C2 C1 116.4(3) . . ? N2 C2 C15 125.6(4) . . ? C1 C2 C15 118.0(3) . . ? C4 C3 C11 121.4(3) . . ? C4 C3 N2 119.2(3) . . ? C11 C3 N2 119.4(3) . . ? C8 C4 C3 118.1(4) . . ? C8 C4 C5 118.0(4) . . ? C3 C4 C5 123.8(4) . . ? C4 C5 C6 110.2(3) . . ? C4 C5 C7 111.8(3) . . ? C6 C5 C7 110.2(3) . . ? C4 C5 H5 108.2 . . ? C6 C5 H5 108.2 . . ? C7 C5 H5 108.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C4 122.0(4) . . ? C9 C8 H8 119.0 . . ? C4 C8 H8 119.0 . . ? C8 C9 C10 119.6(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 121.7(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C3 117.2(4) . . ? C10 C11 C12 117.3(4) . . ? C3 C11 C12 125.6(3) . . ? C11 C12 C13 110.3(3) . . ? C11 C12 C14 110.5(4) . . ? C13 C12 C14 109.7(3) . . ? C11 C12 H12 108.8 . . ? C13 C12 H12 108.8 . . ? C14 C12 H12 108.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 C15 H15A 109.5 . . ? C2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C1 118.7(4) . . ? C17 C16 H16 120.7 . . ? C1 C16 H16 120.7 . . ? C16 C17 C18 120.7(4) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 118.1(4) . . ? C19 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? N1 C19 C18 120.9(3) . . ? N1 C19 C20 113.9(3) . . ? C18 C19 C20 125.2(4) . . ? N3 C20 C19 115.1(3) . . ? N3 C20 C33 125.6(4) . . ? C19 C20 C33 119.3(3) . . ? C29 C21 C22 122.4(3) . . ? C29 C21 N3 119.2(3) . . ? C22 C21 N3 118.4(3) . . ? C26 C22 C21 117.1(4) . . ? C26 C22 C23 119.5(4) . . ? C21 C22 C23 123.4(3) . . ? C24 C23 C22 112.5(4) . . ? C24 C23 C25 109.3(4) . . ? C22 C23 C25 111.4(3) . . ? C24 C23 H23 107.8 . . ? C22 C23 H23 107.8 . . ? C25 C23 H23 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C22 121.7(4) . . ? C27 C26 H26 119.1 . . ? C22 C26 H26 119.1 . . ? C26 C27 C28 119.7(4) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C29 121.8(4) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C21 117.2(4) . . ? C28 C29 C30 120.1(4) . . ? C21 C29 C30 122.6(3) . . ? C29 C30 C31 112.9(3) . . ? C29 C30 C32 110.7(3) . . ? C31 C30 C32 110.7(3) . . ? C29 C30 H30 107.4 . . ? C31 C30 H30 107.4 . . ? C32 C30 H30 107.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C20 C33 H33A 109.5 . . ? C20 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C20 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Al1 O1 Ti1 156.55(16) . . ? 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 O1 Ti1 N1 C19 86.4(3) . . . . ? N3 Ti1 N1 C19 -7.0(2) . . . . ? N2 Ti1 N1 C19 179.4(3) . . . . ? Cl2 Ti1 N1 C19 -84.9(12) . . . . ? Cl1 Ti1 N1 C19 -95.9(3) . . . . ? O1 Ti1 N1 C1 -88.0(3) . . . . ? N3 Ti1 N1 C1 178.7(3) . . . . ? N2 Ti1 N1 C1 5.0(2) . . . . ? Cl2 Ti1 N1 C1 100.8(12) . . . . ? Cl1 Ti1 N1 C1 89.8(2) . . . . ? O1 Ti1 N2 C2 80.1(3) . . . . ? N1 Ti1 N2 C2 -4.8(2) . . . . ? N3 Ti1 N2 C2 -15.4(4) . . . . ? Cl2 Ti1 N2 C2 179.6(2) . . . . ? Cl1 Ti1 N2 C2 -90.3(3) . . . . ? O1 Ti1 N2 C3 -103.7(3) . . . . ? N1 Ti1 N2 C3 171.4(3) . . . . ? N3 Ti1 N2 C3 160.9(2) . . . . ? Cl2 Ti1 N2 C3 -4.1(3) . . . . ? Cl1 Ti1 N2 C3 85.9(3) . . . . ? O1 Ti1 N3 C20 -76.9(3) . . . . ? N1 Ti1 N3 C20 7.9(3) . . . . ? N2 Ti1 N3 C20 18.5(4) . . . . ? Cl2 Ti1 N3 C20 -176.5(2) . . . . ? Cl1 Ti1 N3 C20 92.3(3) . . . . ? O1 Ti1 N3 C21 102.4(3) . . . . ? N1 Ti1 N3 C21 -172.8(3) . . . . ? N2 Ti1 N3 C21 -162.2(2) . . . . ? Cl2 Ti1 N3 C21 2.8(3) . . . . ? Cl1 Ti1 N3 C21 -88.4(2) . . . . ? C19 N1 C1 C16 3.2(5) . . . . ? Ti1 N1 C1 C16 177.5(3) . . . . ? C19 N1 C1 C2 -179.0(3) . . . . ? Ti1 N1 C1 C2 -4.7(4) . . . . ? C3 N2 C2 C1 -172.3(3) . . . . ? Ti1 N2 C2 C1 4.0(4) . . . . ? C3 N2 C2 C15 8.5(5) . . . . ? Ti1 N2 C2 C15 -175.2(3) . . . . ? N1 C1 C2 N2 0.3(5) . . . . ? C16 C1 C2 N2 177.9(3) . . . . ? N1 C1 C2 C15 179.6(3) . . . . ? C16 C1 C2 C15 -2.8(5) . . . . ? C2 N2 C3 C4 -106.8(4) . . . . ? Ti1 N2 C3 C4 77.0(4) . . . . ? C2 N2 C3 C11 72.8(4) . . . . ? Ti1 N2 C3 C11 -103.4(3) . . . . ? C11 C3 C4 C8 -1.0(5) . . . . ? N2 C3 C4 C8 178.6(3) . . . . ? C11 C3 C4 C5 -176.7(3) . . . . ? N2 C3 C4 C5 2.9(5) . . . . ? C8 C4 C5 C6 -66.2(5) . . . . ? C3 C4 C5 C6 109.5(4) . . . . ? C8 C4 C5 C7 56.8(5) . . . . ? C3 C4 C5 C7 -127.5(4) . . . . ? C3 C4 C8 C9 3.5(6) . . . . ? C5 C4 C8 C9 179.4(4) . . . . ? C4 C8 C9 C10 -2.3(6) . . . . ? C8 C9 C10 C11 -1.5(6) . . . . ? C9 C10 C11 C3 3.8(6) . . . . ? C9 C10 C11 C12 -174.4(4) . . . . ? C4 C3 C11 C10 -2.5(5) . . . . ? N2 C3 C11 C10 177.9(3) . . . . ? C4 C3 C11 C12 175.6(3) . . . . ? N2 C3 C11 C12 -4.0(5) . . . . ? C10 C11 C12 C13 59.5(5) . . . . ? C3 C11 C12 C13 -118.6(4) . . . . ? C10 C11 C12 C14 -62.0(4) . . . . ? C3 C11 C12 C14 119.9(4) . . . . ? N1 C1 C16 C17 -1.5(5) . . . . ? C2 C1 C16 C17 -179.1(3) . . . . ? C1 C16 C17 C18 -0.7(6) . . . . ? C16 C17 C18 C19 1.3(6) . . . . ? C1 N1 C19 C18 -2.6(5) . . . . ? Ti1 N1 C19 C18 -176.9(3) . . . . ? C1 N1 C19 C20 179.8(3) . . . . ? Ti1 N1 C19 C20 5.6(4) . . . . ? C17 C18 C19 N1 0.3(5) . . . . ? C17 C18 C19 C20 177.6(3) . . . . ? C21 N3 C20 C19 173.1(3) . . . . ? Ti1 N3 C20 C19 -7.6(4) . . . . ? C21 N3 C20 C33 -7.5(5) . . . . ? Ti1 N3 C20 C33 171.9(3) . . . . ? N1 C19 C20 N3 1.5(5) . . . . ? C18 C19 C20 N3 -175.9(3) . . . . ? N1 C19 C20 C33 -178.0(3) . . . . ? C18 C19 C20 C33 4.6(6) . . . . ? C20 N3 C21 C29 96.8(4) . . . . ? Ti1 N3 C21 C29 -82.5(4) . . . . ? C20 N3 C21 C22 -83.5(4) . . . . ? Ti1 N3 C21 C22 97.2(3) . . . . ? C29 C21 C22 C26 2.6(6) . . . . ? N3 C21 C22 C26 -177.0(3) . . . . ? C29 C21 C22 C23 -175.5(4) . . . . ? N3 C21 C22 C23 4.8(5) . . . . ? C26 C22 C23 C24 54.5(5) . . . . ? C21 C22 C23 C24 -127.4(4) . . . . ? C26 C22 C23 C25 -68.7(5) . . . . ? C21 C22 C23 C25 109.4(4) . . . . ? C21 C22 C26 C27 -0.7(6) . . . . ? C23 C22 C26 C27 177.5(4) . . . . ? C22 C26 C27 C28 -1.0(7) . . . . ? C26 C27 C28 C29 0.8(7) . . . . ? C27 C28 C29 C21 1.1(6) . . . . ? C27 C28 C29 C30 -176.8(4) . . . . ? C22 C21 C29 C28 -2.8(6) . . . . ? N3 C21 C29 C28 176.9(3) . . . . ? C22 C21 C29 C30 175.0(4) . . . . ? N3 C21 C29 C30 -5.3(5) . . . . ? C28 C29 C30 C31 -67.5(5) . . . . ? C21 C29 C30 C31 114.8(4) . . . . ? C28 C29 C30 C32 57.3(5) . . . . ? C21 C29 C30 C32 -120.4(4) . . . . ? Cl4 Al1 O1 Ti1 159.4(3) . . . . ? Cl3 Al1 O1 Ti1 -78.0(4) . . . . ? Cl5 Al1 O1 Ti1 39.4(4) . . . . ? N1 Ti1 O1 Al1 15.3(4) . . . . ? N3 Ti1 O1 Al1 87.4(4) . . . . ? N2 Ti1 O1 Al1 -57.6(4) . . . . ? Cl2 Ti1 O1 Al1 -165.4(4) . . . . ? Cl1 Ti1 O1 Al1 3.4(8) . . . . ? _diffrn_measured_fraction_theta_max .949 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full .949 _refine_diff_density_max .616 _refine_diff_density_min -.391 _refine_diff_density_rms .075 #=== END