# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1162 data_Dalton_8/06393A # Local code TIPYEN _audit_creation_date 98-08-08 _audit_creation_method CRYSTALS _publ_contact_letter ; REVISED CIF FOR MANUSCRIPT 8/06393A These are the revised CIF data for Compound 4 of the following paper. Please destroy previous versions of the cif. ; _publ_section_title ; Reactions of Titanium Imido Complexes with alpha-Diimines: Complexation Versus Ti=N/C=N Bond Metathesis ; _publ_contact_author ; Dr P Mountford Department of Chemistry University of Nottingham Nottingham NG7 2RD ; _publ_contact_author_phone '+44 (0)115 951 3513' _publ_contact_author_fax '+44 (0)115 951 3563' _publ_contact_author_email Philip.Mountford@nott.ac.uk loop_ _publ_author_name _publ_author_address 'McInnes, Jackie M.' ; Department of Chemistry University of Nottingham Nottingham NG7 2RD England U.K. ; 'Blake, Alexander J.' ; Department of Chemistry University of Nottingham Nottingham NG7 2RD England U.K. ; 'Mountford, Philip' ; Department of Chemistry University of Nottingham Nottingham NG7 2RD England U.K. ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. Carruthers, J.R. and Watkin, D.J. (1979), (Chebychev Weighting) Acta Cryst, A35, 698-699 Stoe & Cie (1995a) STADI4, diffractometer control program for Windows. Stoe & Cie, Darmstadt, Germany. Stoe & Cie (1995b) XRED, data reduction program for Windows. Stoe & Cie, Darmstadt, Germany. Watkin, D.J., Prout, C.K. Carruthers, R.J. & Betteridge, P. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; _publ_section_exptl_refinement ; Initial isotropic refinements and examination of Fourier maps suggested that the CH2Cl2 molecule had an occupancy of less than unity. Setting the C and Cl atoms' U[iso] to values comparable to those of atoms in the transition metal fragment and refinement of the occupancy factors of this group suggested an occupancy of ca. 0.8. This value was then assumed for the remainder of the structure determination. ; _chemical_name_systematic ; [Ti(N-2,6-C6H3Pri2)Cl2(py){1,2-N2(Ph)2C2Me2}] ; _cell_length_a 11.093(3) _cell_angle_alpha 82.49(3) _cell_length_b 12.533(5) _cell_angle_beta 85.22(3) _cell_length_c 12.687(5) _cell_angle_gamma 85.28(3) _cell_volume 1738.1(8) _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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C34 H40 Cl4 N4 Ti1' _chemical_formula_moiety ' C34 H40 Cl4 N4 Ti1' _chemical_compound_source ; [Ti(N-2,6-C6H3Pri2)Cl2(py)3] + 1,2-N2(Ph)2C2Me2 ; _chemical_formula_weight 694.43 _cell_measurement_reflns_used 34 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.6 _cell_measurement_temperature 150.0(2) _cell_formula_units_Z 2 _exptl_crystal_description block _exptl_crystal_colour orange/brown _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.27 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.33 _exptl_crystal_F_000 724 _exptl_absorpt_correction_type 'Numerical: face indexing' _exptl_absorpt_correction_T_min 0.8004 _exptl_absorpt_correction_T_max 0.8683 _exptl_absorpt_coefficient_mu 0.58 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 1.00 0.00 0.0810 0.00 -1.00 0.00 0.0810 1.00 0.00 0.00 0.1360 -1.00 0.00 0.00 0.1360 0.00 -1.00 -2.00 0.1130 0.00 1.00 2.00 0.1130 _diffrn_standards_interval_time 60 _diffrn_standards_interval_count ? _diffrn_standards_number 3 _diffrn_standards_decay_% 'variation +/-15' _diffrn_ambient_temperature 150.0(2) _diffrn_reflns_number 6159 _diffrn_measurement_device 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ; Scan width (omega) = 0.92 - 1.69, scan ratio 2theta:omega = 1.00 I(Net) and sigma(I) from profile fitting (Clegg, 1981) ; _diffrn_radiation_collimation '0.5 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo-K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_sigmaI/netI 0.0605 _reflns_d_resolution_high 0.840 _reflns_d_resolution_low 7.984 _reflns_number_total 5722 _diffrn_reflns_av_R_equivalents 0.040 _reflns_number_observed 4220 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _reflns_observed_criterion >2.00\s(I) _refine_diff_density_min -0.56 _refine_diff_density_max 0.63 _refine_ls_number_reflns 4220 _refine_ls_number_parameters 388 _refine_ls_R_factor_obs 0.0802 _refine_ls_wR_factor_obs 0.0886 _refine_ls_goodness_of_fit_obs 0.8766 _refine_ls_shift/esd_max 0.018 _refine_ls_structure_factor_coef F _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack 'not measured' _refine_ls_extinction_method 'not required' _refine_ls_extinction_coef 'not measured' _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods: SIR92' _atom_sites_solution_hydrogens geometric _computing_data_collection 'STADI4 (Stoe & Cie 1995a)' _computing_cell_refinement 'STADI4 (Stoe & Cie 1995a)' _computing_data_reduction ; X-RED (Stoe & Cie, 1995b) CRYSTALS (Watkin et al, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Ti1 0.24637(8) 0.30815(8) 0.09288(8) 0.0233 1.0000 Uani N1 0.2449(4) 0.2460(4) 0.2229(4) 0.0252 1.0000 Uani N2 0.2658(4) 0.4742(4) 0.1240(4) 0.0241 1.0000 Uani N3 0.2482(4) 0.4214(4) -0.0668(4) 0.0233 1.0000 Uani N4 0.2293(4) 0.1609(4) 0.0165(4) 0.0296 1.0000 Uani Cl1 0.4596(1) 0.2939(1) 0.0417(1) 0.0328 1.0000 Uani Cl2 0.0344(1) 0.3547(1) 0.0786(1) 0.0303 1.0000 Uani C1 0.2431(5) 0.1946(4) 0.3265(5) 0.0249 1.0000 Uani C2 0.3521(5) 0.1672(4) 0.3773(5) 0.0284 1.0000 Uani C3 0.3488(5) 0.1026(5) 0.4765(5) 0.0318 1.0000 Uani C4 0.2412(5) 0.0679(5) 0.5255(5) 0.0326 1.0000 Uani C5 0.1310(5) 0.1015(5) 0.4789(5) 0.0313 1.0000 Uani C6 0.1314(5) 0.1659(5) 0.3814(5) 0.0300 1.0000 Uani C7 0.4699(5) 0.2096(5) 0.3291(5) 0.0337 1.0000 Uani C8 0.5360(6) 0.2590(7) 0.4097(6) 0.0517 1.0000 Uani C9 0.5530(6) 0.1227(6) 0.2820(6) 0.0494 1.0000 Uani C10 0.0134(5) 0.2040(5) 0.3323(5) 0.0293 1.0000 Uani C11 -0.0887(6) 0.2344(7) 0.4128(6) 0.0561 1.0000 Uani C12 -0.0268(7) 0.1215(6) 0.2667(6) 0.0507 1.0000 Uani C13 0.2580(4) 0.5535(4) 0.0484(5) 0.0252 1.0000 Uani C14 0.2575(4) 0.5208(4) -0.0619(4) 0.0239 1.0000 Uani C15 0.2425(5) 0.6699(4) 0.0623(5) 0.0319 1.0000 Uani C16 0.2727(5) 0.6060(5) -0.1572(5) 0.0309 1.0000 Uani C17 0.2792(5) 0.4973(5) 0.2319(5) 0.0295 1.0000 Uani C18 0.1888(6) 0.4740(5) 0.3104(5) 0.0350 1.0000 Uani C19 0.2032(6) 0.4935(6) 0.4132(6) 0.0448 1.0000 Uani C20 0.3088(7) 0.5343(6) 0.4369(6) 0.0511 1.0000 Uani C21 0.3985(7) 0.5548(6) 0.3588(6) 0.0489 1.0000 Uani C22 0.3853(6) 0.5369(5) 0.2549(6) 0.0390 1.0000 Uani C23 0.2328(5) 0.3845(4) -0.1669(4) 0.0252 1.0000 Uani C24 0.3226(6) 0.3167(5) -0.2121(5) 0.0361 1.0000 Uani C25 0.3034(6) 0.2777(6) -0.3053(5) 0.0426 1.0000 Uani C26 0.1954(7) 0.3014(6) -0.3526(6) 0.0468 1.0000 Uani C27 0.1051(6) 0.3655(6) -0.3052(5) 0.0400 1.0000 Uani C28 0.1229(6) 0.4080(5) -0.2124(5) 0.0367 1.0000 Uani C29 0.3109(6) 0.0755(5) 0.0360(6) 0.0418 1.0000 Uani C30 0.3072(8) -0.0190(6) -0.0069(7) 0.0564 1.0000 Uani C31 0.2165(8) -0.0312(6) -0.0713(7) 0.0574 1.0000 Uani C32 0.1312(7) 0.0548(6) -0.0919(7) 0.0514 1.0000 Uani C33 0.1426(6) 0.1473(5) -0.0471(5) 0.0356 1.0000 Uani H31 0.4228(5) 0.0824(5) 0.5105(5) 0.0430 1.0000 Uiso H41 0.2410(5) 0.0207(5) 0.5916(5) 0.0437 1.0000 Uiso H51 0.0555(5) 0.0799(5) 0.5147(5) 0.0409 1.0000 Uiso H71 0.4478(5) 0.2641(5) 0.2721(5) 0.0447 1.0000 Uiso H81 0.6106(6) 0.2849(7) 0.3761(6) 0.0692 1.0000 Uiso H82 0.5531(6) 0.2055(7) 0.4689(6) 0.0692 1.0000 Uiso H83 0.4856(6) 0.3180(7) 0.4345(6) 0.0692 1.0000 Uiso H91 0.6269(6) 0.1528(6) 0.2520(6) 0.0628 1.0000 Uiso H92 0.5709(6) 0.0649(6) 0.3372(6) 0.0628 1.0000 Uiso H93 0.5139(6) 0.0955(6) 0.2274(6) 0.0628 1.0000 Uiso H101 0.0312(5) 0.2692(5) 0.2869(5) 0.0409 1.0000 Uiso H111 -0.1604(6) 0.2577(7) 0.3763(6) 0.0689 1.0000 Uiso H112 -0.0661(6) 0.2918(7) 0.4487(6) 0.0689 1.0000 Uiso H113 -0.1043(6) 0.1727(7) 0.4640(6) 0.0689 1.0000 Uiso H121 -0.1018(7) 0.1481(6) 0.2367(6) 0.0689 1.0000 Uiso H122 -0.0381(7) 0.0548(6) 0.3116(6) 0.0689 1.0000 Uiso H123 0.0341(7) 0.1098(6) 0.2103(6) 0.0689 1.0000 Uiso H151 0.2394(5) 0.7122(4) -0.0063(5) 0.0429 1.0000 Uiso H152 0.3095(5) 0.6888(4) 0.0975(5) 0.0429 1.0000 Uiso H153 0.1683(5) 0.6837(4) 0.1045(5) 0.0429 1.0000 Uiso H161 0.2776(5) 0.6749(5) -0.1332(5) 0.0415 1.0000 Uiso H162 0.3456(5) 0.5881(5) -0.1995(5) 0.0415 1.0000 Uiso H163 0.2043(5) 0.6090(5) -0.1995(5) 0.0415 1.0000 Uiso H181 0.1165(6) 0.4442(5) 0.2941(5) 0.0475 1.0000 Uiso H191 0.1401(6) 0.4785(6) 0.4684(6) 0.0580 1.0000 Uiso H201 0.3183(7) 0.5481(6) 0.5083(6) 0.0680 1.0000 Uiso H211 0.4718(7) 0.5822(6) 0.3759(6) 0.0670 1.0000 Uiso H221 0.4487(6) 0.5514(5) 0.1999(6) 0.0547 1.0000 Uiso H241 0.3972(6) 0.2974(5) -0.1788(5) 0.0490 1.0000 Uiso H251 0.3661(6) 0.2327(6) -0.3379(5) 0.0571 1.0000 Uiso H261 0.1834(7) 0.2739(6) -0.4179(6) 0.0620 1.0000 Uiso H271 0.0289(6) 0.3807(6) -0.3369(5) 0.0547 1.0000 Uiso H281 0.0599(6) 0.4530(5) -0.1801(5) 0.0476 1.0000 Uiso H291 0.3735(6) 0.0813(5) 0.0824(6) 0.0555 1.0000 Uiso H301 0.3685(8) -0.0765(6) 0.0074(7) 0.0741 1.0000 Uiso H311 0.2121(8) -0.0974(6) -0.1007(7) 0.0779 1.0000 Uiso H321 0.0662(7) 0.0499(6) -0.1361(7) 0.0699 1.0000 Uiso H331 0.0839(6) 0.2068(5) -0.0627(5) 0.0491 1.0000 Uiso C101 0.2575(9) 0.904(1) 0.311(1) 0.0937 1.0000 Uani Cl101 0.1347(2) 0.8363(2) 0.2833(2) 0.0635 1.0000 Uani Cl102 0.3959(2) 0.8557(2) 0.2548(2) 0.0707 1.0000 Uani H1011 0.2440(9) 0.979(1) 0.284(1) 0.0500 1.0000 Uiso H1012 0.2616(9) 0.896(1) 0.387(1) 0.0500 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 0.0226(5) 0.0224(5) 0.0240(5) 0.0010(4) -0.0039(4) -0.0008(4) N1 0.023(2) 0.030(2) 0.022(2) 0.000(2) -0.003(2) -0.001(2) N2 0.023(2) 0.029(2) 0.022(2) -0.005(2) -0.005(2) -0.003(2) N3 0.018(2) 0.026(2) 0.026(2) -0.001(2) -0.001(2) -0.002(2) N4 0.038(3) 0.028(3) 0.022(2) -0.000(2) -0.002(2) -0.004(2) Cl1 0.0226(6) 0.0437(8) 0.0312(8) -0.0017(7) -0.0026(5) -0.0010(5) Cl2 0.0234(6) 0.0324(7) 0.0337(8) 0.0015(6) -0.0049(5) 0.0012(5) C1 0.029(3) 0.020(3) 0.026(3) -0.002(2) -0.005(2) -0.000(2) C2 0.028(3) 0.026(3) 0.029(3) 0.003(3) -0.004(2) 0.004(2) C3 0.031(3) 0.034(3) 0.028(3) 0.006(3) -0.009(2) 0.005(2) C4 0.034(3) 0.036(3) 0.027(3) 0.003(3) -0.006(2) -0.002(2) C5 0.038(3) 0.037(3) 0.020(3) -0.003(3) -0.003(2) -0.007(2) C6 0.034(3) 0.025(3) 0.030(3) -0.001(3) 0.001(2) -0.003(2) C7 0.026(3) 0.041(3) 0.032(3) 0.005(3) -0.009(2) -0.000(2) C8 0.041(4) 0.069(5) 0.047(4) 0.004(4) -0.012(3) -0.027(3) C9 0.038(4) 0.056(4) 0.047(4) 0.009(4) 0.008(3) 0.005(3) C10 0.023(3) 0.034(3) 0.031(3) -0.004(3) -0.001(2) -0.004(2) C11 0.040(4) 0.083(6) 0.040(4) 0.003(4) -0.003(3) 0.009(4) C12 0.054(4) 0.043(4) 0.056(5) 0.010(4) -0.025(3) -0.009(3) C13 0.020(3) 0.025(3) 0.030(3) -0.001(3) -0.002(2) -0.004(2) C14 0.022(3) 0.028(3) 0.021(3) 0.001(2) -0.003(2) -0.003(2) C15 0.032(3) 0.025(3) 0.037(3) -0.001(3) 0.002(2) 0.001(2) C16 0.029(3) 0.029(3) 0.032(3) 0.007(3) -0.002(2) -0.003(2) C17 0.036(3) 0.028(3) 0.025(3) -0.003(3) -0.007(2) 0.003(2) C18 0.045(3) 0.034(3) 0.025(3) -0.002(3) -0.001(3) -0.002(3) C19 0.053(4) 0.050(4) 0.029(4) 0.001(3) -0.004(3) 0.004(3) C20 0.074(5) 0.050(4) 0.033(4) -0.012(3) -0.019(3) 0.003(4) C21 0.052(4) 0.063(5) 0.036(4) -0.007(4) -0.017(3) -0.016(3) C22 0.037(3) 0.043(4) 0.040(4) -0.009(3) -0.008(3) -0.007(3) C23 0.025(3) 0.029(3) 0.020(3) 0.001(2) -0.002(2) -0.001(2) C24 0.037(3) 0.043(4) 0.029(3) -0.005(3) -0.004(2) 0.001(3) C25 0.045(4) 0.049(4) 0.032(4) -0.007(3) -0.005(3) 0.007(3) C26 0.063(4) 0.046(4) 0.032(4) -0.011(3) -0.014(3) 0.011(3) C27 0.041(3) 0.045(4) 0.034(4) -0.005(3) -0.017(3) 0.007(3) C28 0.039(3) 0.038(3) 0.028(3) 0.005(3) -0.001(3) 0.006(3) C29 0.062(4) 0.027(3) 0.041(4) -0.016(3) -0.018(3) 0.007(3) C30 0.072(5) 0.040(4) 0.057(5) -0.010(4) -0.023(4) 0.019(4) C31 0.077(5) 0.038(4) 0.061(5) -0.013(4) -0.012(4) -0.006(4) C32 0.068(5) 0.039(4) 0.054(5) -0.010(4) -0.027(4) -0.009(3) C33 0.048(4) 0.031(3) 0.030(3) -0.006(3) -0.010(3) -0.007(3) C101 0.081(7) 0.098(8) 0.108(9) -0.053(7) 0.035(6) -0.023(6) Cl101 0.066(1) 0.068(1) 0.059(1) -0.021(1) -0.0035(9) -0.002(1) Cl102 0.062(1) 0.059(1) 0.087(2) -0.006(1) -0.006(1) 0.0143(9) 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 . N1 . 1.729(4) yes Ti1 . N2 . 2.200(5) yes Ti1 . N3 . 2.317(4) yes Ti1 . N4 . 2.222(5) yes Ti1 . Cl1 . 2.399(2) yes Ti1 . Cl2 . 2.391(2) yes N1 . C1 . 1.385(7) yes N2 . C13 . 1.290(7) yes N2 . C17 . 1.457(8) yes N3 . C14 . 1.268(7) yes N3 . C23 . 1.434(8) yes N4 . C29 . 1.355(8) yes N4 . C33 . 1.341(8) yes C1 . C2 . 1.414(8) yes C1 . C6 . 1.419(8) yes C2 . C3 . 1.404(8) yes C2 . C7 . 1.504(8) yes C3 . C4 . 1.375(8) yes C4 . C5 . 1.412(8) yes C5 . C6 . 1.385(8) yes C6 . C10 . 1.512(8) yes C7 . C8 . 1.53(1) yes C7 . C9 . 1.52(1) yes C10 . C11 . 1.519(9) yes C10 . C12 . 1.52(1) yes C13 . C14 . 1.509(8) yes C13 . C15 . 1.487(8) yes C14 . C16 . 1.513(7) yes C17 . C18 . 1.374(8) yes C17 . C22 . 1.381(9) yes C18 . C19 . 1.38(1) yes C19 . C20 . 1.39(1) yes C20 . C21 . 1.36(1) yes C21 . C22 . 1.39(1) yes C23 . C24 . 1.391(8) yes C23 . C28 . 1.387(8) yes C24 . C25 . 1.38(1) yes C25 . C26 . 1.38(1) yes C26 . C27 . 1.38(1) yes C27 . C28 . 1.39(1) yes C29 . C30 . 1.37(1) yes C30 . C31 . 1.38(1) yes C31 . C32 . 1.39(1) yes C32 . C33 . 1.38(1) yes C101 . Cl101 . 1.74(1) yes C101 . Cl102 . 1.734(9) 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 N1 . Ti1 . N2 . 98.3(2) yes N1 . Ti1 . N3 . 169.1(2) yes N2 . Ti1 . N3 . 70.8(2) yes N1 . Ti1 . N4 . 97.0(2) yes N2 . Ti1 . N4 . 164.6(2) yes N3 . Ti1 . N4 . 93.8(2) yes N1 . Ti1 . Cl1 . 100.7(1) yes N2 . Ti1 . Cl1 . 88.2(1) yes N3 . Ti1 . Cl1 . 80.5(1) yes N4 . Ti1 . Cl1 . 88.3(1) yes N1 . Ti1 . Cl2 . 100.4(1) yes N2 . Ti1 . Cl2 . 88.4(1) yes N3 . Ti1 . Cl2 . 78.7(1) yes N4 . Ti1 . Cl2 . 89.4(1) yes Cl1 . Ti1 . Cl2 . 158.94(6) yes Ti1 . N1 . C1 . 179.0(4) yes Ti1 . N2 . C13 . 120.6(4) yes Ti1 . N2 . C17 . 120.4(3) yes C13 . N2 . C17 . 118.9(5) yes Ti1 . N3 . C14 . 116.7(4) yes Ti1 . N3 . C23 . 122.9(3) yes C14 . N3 . C23 . 120.3(5) yes Ti1 . N4 . C29 . 118.6(4) yes Ti1 . N4 . C33 . 125.6(4) yes C29 . N4 . C33 . 115.7(6) yes N1 . C1 . C2 . 120.6(5) yes N1 . C1 . C6 . 119.9(5) yes C2 . C1 . C6 . 119.4(5) yes C1 . C2 . C3 . 119.1(5) yes C1 . C2 . C7 . 121.2(5) yes C3 . C2 . C7 . 119.7(5) yes C2 . C3 . C4 . 121.0(5) yes C3 . C4 . C5 . 120.1(5) yes C4 . C5 . C6 . 120.1(5) yes C1 . C6 . C5 . 119.9(5) yes C1 . C6 . C10 . 119.8(5) yes C5 . C6 . C10 . 120.2(5) yes C2 . C7 . C8 . 111.9(5) yes C2 . C7 . C9 . 111.8(5) yes C8 . C7 . C9 . 109.6(6) yes C6 . C10 . C11 . 113.7(6) yes C6 . C10 . C12 . 111.6(5) yes C11 . C10 . C12 . 110.1(6) yes N2 . C13 . C14 . 114.9(5) yes N2 . C13 . C15 . 125.9(5) yes C14 . C13 . C15 . 119.2(5) yes N3 . C14 . C13 . 116.2(5) yes N3 . C14 . C16 . 125.0(5) yes C13 . C14 . C16 . 118.8(5) yes N2 . C17 . C18 . 119.5(5) yes N2 . C17 . C22 . 119.4(6) yes C18 . C17 . C22 . 121.0(6) yes C17 . C18 . C19 . 119.3(6) yes C18 . C19 . C20 . 120.1(7) yes C19 . C20 . C21 . 119.8(7) yes C20 . C21 . C22 . 120.9(7) yes C17 . C22 . C21 . 118.8(6) yes N3 . C23 . C24 . 120.2(5) yes N3 . C23 . C28 . 119.2(5) yes C24 . C23 . C28 . 120.2(6) yes C23 . C24 . C25 . 119.3(6) yes C24 . C25 . C26 . 121.3(6) yes C25 . C26 . C27 . 119.1(7) yes C26 . C27 . C28 . 120.9(6) yes C23 . C28 . C27 . 119.1(6) yes N4 . C29 . C30 . 122.8(6) yes C29 . C30 . C31 . 120.2(7) yes C30 . C31 . C32 . 118.1(8) yes C31 . C32 . C33 . 118.0(7) yes N4 . C33 . C32 . 125.1(6) yes Cl101 . C101 . Cl102 . 114.0(6) yes # ======= END