# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global_1 _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 loop_ _publ_author_name 'Pei Jen Tiong' A.Nova E.Clot P.Mountford data_COMPOUND_2 _database_code_depnum_ccdc_archive 'CCDC 802264' #TrackingRef '- Mountford Xray SI.CIF' # Local code PJT8 _chemical_name_systematic ; Cp*Ti{MeC(NiPr)2}(H){N(NMe2)SiH2Ph} ; _chemical_melting_point ? _publ_section_exptl_refinement ; Si-H and Ti-H hydrogen atoms were located from Fourier maps and positionally and isotropically refined. C-bound H atoms were placed in calculated positions with reference to a Fourier difference map and refined in a riding model. Residual electron density was modelled as a partial occupancy pentane of crystallization disordered across a crystallographic inversion center. It was positionally and anisotropically refined subject to similarity restraints on the ADPs and distance and angle restraints for C-C and C-C-C, respectively. ; _cell_length_a 8.5949(2) _cell_length_b 11.3073(3) _cell_length_c 31.4337(9) _cell_angle_alpha 90 _cell_angle_beta 92.4007(12) _cell_angle_gamma 90 _cell_volume 3052.21(14) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C27.25 H49 N4 Si1 Ti1' _chemical_formula_moiety 'C26 H46 N4 Si1 Ti1, 0.25 (C5 H12)' _chemical_compound_source ? _chemical_formula_weight 508.70 _cell_measurement_reflns_used 6555 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1106 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.93 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 12239 _reflns_number_total 6878 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_min 5.146 _diffrn_reflns_theta_max 27.520 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.319 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 40 _oxford_diffrn_Wilson_B_factor 2.59 _oxford_diffrn_Wilson_scale 19.66 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.51 _refine_diff_density_max 0.85 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 4109 _refine_ls_number_restraints 49 _refine_ls_number_parameters 337 _oxford_refine_ls_R_factor_ref 0.0637 _refine_ls_wR_factor_ref 0.0686 _refine_ls_goodness_of_fit_ref 1.0893 _refine_ls_shift/su_max 0.002707 # The values computed from all data _oxford_reflns_number_all 6878 _refine_ls_R_factor_all 0.1104 _refine_ls_wR_factor_all 0.0921 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4631 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_gt 0.0721 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _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: 0.814 0.609 0.659 0.141 0.191 ; _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # 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_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ti1 Ti 0.77556(6) 0.60429(5) 0.355487(18) 0.0261 1.0000 Uani . . . . . . . N1 N 0.6722(3) 0.4521(3) 0.34400(9) 0.0313 1.0000 Uani . . . . . . . N2 N 0.5424(3) 0.5340(3) 0.33676(9) 0.0298 1.0000 Uani . . . . . . . N3 N 0.6751(3) 0.7799(3) 0.36624(9) 0.0327 1.0000 Uani . . . . . . . N4 N 0.6884(3) 0.6480(3) 0.41805(8) 0.0314 1.0000 Uani . . . . . . . Si1 Si 0.66058(11) 0.30726(9) 0.32713(3) 0.0375 1.0000 Uani . . . . . . . C1 C 0.4796(4) 0.5320(4) 0.29259(12) 0.0397 1.0000 Uani . . . . . . . C2 C 0.4144(4) 0.5186(3) 0.36600(12) 0.0376 1.0000 Uani . . . . . . . C3 C 0.4843(4) 0.2271(3) 0.34474(12) 0.0393 1.0000 Uani . . . . . . . C4 C 0.3654(5) 0.1905(4) 0.31603(14) 0.0446 1.0000 Uani . . . . . . . C5 C 0.2342(5) 0.1312(4) 0.32992(17) 0.0556 1.0000 Uani . . . . . . . C6 C 0.2212(5) 0.1072(4) 0.37262(17) 0.0546 1.0000 Uani . . . . . . . C7 C 0.3368(6) 0.1412(4) 0.40170(16) 0.0551 1.0000 Uani . . . . . . . C8 C 0.4665(5) 0.2002(4) 0.38774(14) 0.0472 1.0000 Uani . . . . . . . C9 C 0.6216(4) 0.7470(3) 0.40346(10) 0.0325 1.0000 Uani . . . . . . . C10 C 0.4944(5) 0.8129(4) 0.42550(13) 0.0474 1.0000 Uani . . . . . . . C11 C 0.6052(4) 0.8798(3) 0.34226(12) 0.0386 1.0000 Uani . . . . . . . C12 C 0.4653(5) 0.8408(4) 0.31449(14) 0.0480 1.0000 Uani . . . . . . . C13 C 0.7243(5) 0.9379(4) 0.31466(15) 0.0516 1.0000 Uani . . . . . . . C14 C 0.6393(4) 0.5922(4) 0.45726(11) 0.0381 1.0000 Uani . . . . . . . C15 C 0.6945(5) 0.4652(4) 0.45912(12) 0.0439 1.0000 Uani . . . . . . . C16 C 0.6943(5) 0.6583(4) 0.49786(12) 0.0506 1.0000 Uani . . . . . . . C17 C 1.0148(4) 0.4993(3) 0.37409(11) 0.0307 1.0000 Uani . . . . . . . C18 C 1.0093(4) 0.5222(3) 0.32943(10) 0.0314 1.0000 Uani . . . . . . . C19 C 1.0179(4) 0.6461(3) 0.32317(11) 0.0323 1.0000 Uani . . . . . . . C20 C 1.0266(4) 0.7000(3) 0.36421(11) 0.0324 1.0000 Uani . . . . . . . C21 C 1.0259(3) 0.6102(3) 0.39512(10) 0.0309 1.0000 Uani . . . . . . . C22 C 1.0297(4) 0.3806(3) 0.39519(13) 0.0418 1.0000 Uani . . . . . . . C23 C 1.0092(4) 0.4328(4) 0.29427(12) 0.0412 1.0000 Uani . . . . . . . C24 C 1.0409(4) 0.7061(4) 0.28159(12) 0.0444 1.0000 Uani . . . . . . . C25 C 1.0502(4) 0.8282(3) 0.37396(14) 0.0435 1.0000 Uani . . . . . . . C26 C 1.0578(4) 0.6303(4) 0.44164(11) 0.0403 1.0000 Uani . . . . . . . C27 C -0.2353(17) 0.3941(15) -0.0278(7) 0.1451 0.5000 Uani D U . . . . . C28 C -0.067(2) 0.424(3) -0.0368(6) 0.1458 0.2500 Uani D U . . . . . C281 C -0.1759(10) 0.485(3) 0.0048(9) 0.1460 0.2500 Uani D U . . . . . C29 C 0.000000(10) 0.500000(10) 0.000000(10) 0.1436 0.5000 Uani DS U . . . . . H1 H 0.755(4) 0.654(3) 0.3065(12) 0.036(10) 1.0000 Uiso . . . . . . . H2 H 0.664(5) 0.290(4) 0.2836(13) 0.046(11) 1.0000 Uiso . . . . . . . H3 H 0.794(4) 0.248(3) 0.3442(10) 0.018(7) 1.0000 Uiso . . . . . . . H11 H 0.3946 0.5864 0.2889 0.0436 1.0000 Uiso R . . . . . . H12 H 0.5584 0.5533 0.2738 0.0436 1.0000 Uiso R . . . . . . H13 H 0.4419 0.4547 0.2852 0.0436 1.0000 Uiso R . . . . . . H21 H 0.3348 0.5746 0.3595 0.0397 1.0000 Uiso R . . . . . . H22 H 0.4533 0.5303 0.3943 0.0397 1.0000 Uiso R . . . . . . H23 H 0.3731 0.4411 0.3632 0.0397 1.0000 Uiso R . . . . . . H41 H 0.3742 0.2078 0.2867 0.0509 1.0000 Uiso R . . . . . . H51 H 0.1548 0.1076 0.3098 0.0586 1.0000 Uiso R . . . . . . H61 H 0.1320 0.0672 0.3821 0.0606 1.0000 Uiso R . . . . . . H71 H 0.3287 0.1241 0.4310 0.0600 1.0000 Uiso R . . . . . . H81 H 0.5462 0.2234 0.4078 0.0509 1.0000 Uiso R . . . . . . H101 H 0.4740 0.7739 0.4514 0.0532 1.0000 Uiso R . . . . . . H102 H 0.5282 0.8913 0.4314 0.0532 1.0000 Uiso R . . . . . . H103 H 0.4022 0.8149 0.4079 0.0532 1.0000 Uiso R . . . . . . H111 H 0.5717 0.9370 0.3619 0.0406 1.0000 Uiso R . . . . . . H121 H 0.4227 0.9072 0.2997 0.0497 1.0000 Uiso R . . . . . . H122 H 0.3886 0.8073 0.3317 0.0497 1.0000 Uiso R . . . . . . H123 H 0.4979 0.7837 0.2947 0.0497 1.0000 Uiso R . . . . . . H131 H 0.6776 1.0023 0.2996 0.0585 1.0000 Uiso R . . . . . . H132 H 0.8103 0.9655 0.3317 0.0585 1.0000 Uiso R . . . . . . H133 H 0.7590 0.8810 0.2950 0.0585 1.0000 Uiso R . . . . . . H141 H 0.5288 0.5916 0.4564 0.0380 1.0000 Uiso R . . . . . . H151 H 0.6618 0.4292 0.4845 0.0469 1.0000 Uiso R . . . . . . H152 H 0.8049 0.4634 0.4587 0.0469 1.0000 Uiso R . . . . . . H153 H 0.6517 0.4235 0.4352 0.0469 1.0000 Uiso R . . . . . . H161 H 0.6585 0.6179 0.5220 0.0551 1.0000 Uiso R . . . . . . H162 H 0.8048 0.6610 0.4993 0.0551 1.0000 Uiso R . . . . . . H163 H 0.6541 0.7365 0.4973 0.0551 1.0000 Uiso R . . . . . . H221 H 1.0312 0.3914 0.4251 0.0438 1.0000 Uiso R . . . . . . H222 H 1.1237 0.3438 0.3875 0.0438 1.0000 Uiso R . . . . . . H223 H 0.9438 0.3321 0.3867 0.0438 1.0000 Uiso R . . . . . . H231 H 1.0037 0.4730 0.2678 0.0454 1.0000 Uiso R . . . . . . H232 H 1.1025 0.3878 0.2965 0.0454 1.0000 Uiso R . . . . . . H233 H 0.9222 0.3817 0.2961 0.0454 1.0000 Uiso R . . . . . . H241 H 1.0434 0.7893 0.2855 0.0526 1.0000 Uiso R . . . . . . H242 H 1.1362 0.6807 0.2704 0.0526 1.0000 Uiso R . . . . . . H243 H 0.9571 0.6860 0.2624 0.0526 1.0000 Uiso R . . . . . . H251 H 0.9622 0.8614 0.3868 0.0426 1.0000 Uiso R . . . . . . H252 H 1.0716 0.8712 0.3490 0.0426 1.0000 Uiso R . . . . . . H253 H 1.1372 0.8361 0.3933 0.0426 1.0000 Uiso R . . . . . . H261 H 0.9873 0.6886 0.4509 0.0388 1.0000 Uiso R . . . . . . H262 H 1.0408 0.5585 0.4563 0.0388 1.0000 Uiso R . . . . . . H263 H 1.1620 0.6561 0.4468 0.0388 1.0000 Uiso R . . . . . . H271 H -0.2828 0.3570 -0.0521 0.1419 0.5000 Uiso R . . . . . . H272 H -0.2969 0.4593 -0.0197 0.1419 0.5000 Uiso R . . . . . . H273 H -0.2271 0.3391 -0.0051 0.1419 0.5000 Uiso R . . . . . . H281 H -0.0745 0.4794 -0.0595 0.1418 0.2500 Uiso R . . . . . . H282 H -0.0047 0.3592 -0.0448 0.1418 0.2500 Uiso R . . . . . . H291 H -0.0490 0.5740 0.0043 0.1383 0.2500 Uiso R . . . . . . H292 H -0.0140 0.4509 0.0240 0.1383 0.2500 Uiso R . . . . . . H2811 H -0.2293 0.5584 0.0026 0.1427 0.2500 Uiso R . . . . . . H2812 H -0.1918 0.4508 0.0318 0.1427 0.2500 Uiso 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 0.0221(3) 0.0315(3) 0.0247(3) 0.0001(2) 0.00072(19) 0.0003(2) N1 0.0226(12) 0.0378(15) 0.0336(14) 0.0007(12) 0.0007(11) 0.0039(11) N2 0.0203(12) 0.0362(15) 0.0328(14) 0.0003(12) -0.0001(10) 0.0009(11) N3 0.0332(14) 0.0320(15) 0.0328(15) -0.0006(12) 0.0009(11) 0.0052(12) N4 0.0306(14) 0.0410(16) 0.0225(13) -0.0021(11) 0.0014(11) 0.0008(12) Si1 0.0332(5) 0.0363(5) 0.0430(6) -0.0061(4) 0.0021(4) -0.0008(4) C1 0.0330(18) 0.045(2) 0.0401(19) -0.0016(16) -0.0063(15) -0.0036(16) C2 0.0246(16) 0.044(2) 0.045(2) -0.0034(16) 0.0029(14) -0.0009(14) C3 0.0385(19) 0.0313(18) 0.048(2) -0.0042(16) -0.0005(16) 0.0000(15) C4 0.044(2) 0.041(2) 0.049(2) -0.0088(17) -0.0006(17) -0.0038(17) C5 0.042(2) 0.043(2) 0.081(3) -0.010(2) -0.007(2) -0.0059(17) C6 0.049(2) 0.034(2) 0.083(3) -0.007(2) 0.017(2) -0.0061(18) C7 0.074(3) 0.034(2) 0.058(3) 0.0033(19) 0.016(2) -0.006(2) C8 0.053(2) 0.041(2) 0.048(2) -0.0002(18) -0.0010(18) -0.0053(18) C9 0.0273(16) 0.0402(19) 0.0301(16) -0.0066(14) 0.0019(13) 0.0015(14) C10 0.043(2) 0.055(2) 0.045(2) -0.0058(18) 0.0081(17) 0.0132(18) C11 0.0383(18) 0.0354(19) 0.0420(19) 0.0009(15) -0.0013(15) 0.0086(15) C12 0.040(2) 0.053(2) 0.050(2) 0.0066(19) -0.0080(18) 0.0093(18) C13 0.053(2) 0.044(2) 0.058(3) 0.0175(19) 0.0022(19) 0.0087(19) C14 0.0309(16) 0.052(2) 0.0320(17) -0.0008(16) 0.0041(13) -0.0035(16) C15 0.041(2) 0.057(2) 0.0338(18) 0.0096(17) 0.0053(15) -0.0028(18) C16 0.047(2) 0.074(3) 0.0306(19) -0.0021(19) 0.0026(16) -0.001(2) C17 0.0200(14) 0.0354(18) 0.0365(17) 0.0016(14) -0.0014(12) 0.0029(13) C18 0.0230(15) 0.0404(19) 0.0310(16) -0.0002(14) 0.0033(12) 0.0020(13) C19 0.0216(15) 0.0409(19) 0.0345(17) 0.0029(14) 0.0023(13) 0.0019(13) C20 0.0237(15) 0.0370(18) 0.0363(18) 0.0014(14) -0.0002(13) -0.0007(13) C21 0.0197(14) 0.0397(18) 0.0332(16) -0.0006(15) -0.0008(12) 0.0012(14) C22 0.0346(18) 0.044(2) 0.047(2) 0.0045(17) -0.0021(15) 0.0036(16) C23 0.0314(17) 0.055(2) 0.0380(19) -0.0099(17) 0.0054(15) 0.0031(16) C24 0.0369(19) 0.059(2) 0.038(2) 0.0106(18) 0.0055(15) -0.0009(18) C25 0.0345(18) 0.041(2) 0.055(2) -0.0010(17) -0.0051(17) -0.0019(16) C26 0.0318(17) 0.056(2) 0.0323(18) -0.0028(16) -0.0039(14) -0.0021(16) C27 0.116(10) 0.116(10) 0.197(16) 0.044(10) -0.069(10) -0.021(8) C28 0.121(11) 0.113(11) 0.199(17) 0.058(11) -0.047(11) -0.021(9) C281 0.115(10) 0.115(11) 0.203(17) 0.054(11) -0.056(11) -0.023(9) C29 0.113(10) 0.111(11) 0.203(17) 0.062(11) -0.048(11) -0.025(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2220(5) 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 . 1.963(3) yes Ti1 . N2 . 2.212(3) yes Ti1 . N3 . 2.197(3) yes Ti1 . N4 . 2.190(3) yes Ti1 . C9 . 2.607(3) yes Ti1 . C17 . 2.425(3) yes Ti1 . C18 . 2.389(3) yes Ti1 . C19 . 2.402(3) yes Ti1 . C20 . 2.419(3) yes Ti1 . C21 . 2.442(3) yes Ti1 . H1 . 1.64(4) no N1 . N2 . 1.460(4) yes N1 . Si1 . 1.723(3) yes N2 . C1 . 1.469(4) yes N2 . C2 . 1.473(4) yes N3 . C9 . 1.328(4) yes N3 . C11 . 1.472(4) yes N4 . C9 . 1.331(5) yes N4 . C14 . 1.462(4) yes Si1 . C3 . 1.869(4) yes Si1 . H2 . 1.38(4) no Si1 . H3 . 1.41(3) no C1 . H11 . 0.958 no C1 . H12 . 0.948 no C1 . H13 . 0.957 no C2 . H21 . 0.949 no C2 . H22 . 0.948 no C2 . H23 . 0.949 no C3 . C4 . 1.397(5) yes C3 . C8 . 1.400(6) yes C4 . C5 . 1.398(6) yes C4 . H41 . 0.948 no C5 . C6 . 1.379(7) yes C5 . H51 . 0.948 no C6 . C7 . 1.377(7) yes C6 . H61 . 0.949 no C7 . C8 . 1.386(6) yes C7 . H71 . 0.948 no C8 . H81 . 0.948 no C9 . C10 . 1.515(5) yes C10 . H101 . 0.948 no C10 . H102 . 0.949 no C10 . H103 . 0.949 no C11 . C12 . 1.521(5) yes C11 . C13 . 1.519(6) yes C11 . H111 . 0.948 no C12 . H121 . 0.948 no C12 . H122 . 0.949 no C12 . H123 . 0.948 no C13 . H131 . 0.948 no C13 . H132 . 0.949 no C13 . H133 . 0.948 no C14 . C15 . 1.513(6) yes C14 . C16 . 1.536(5) yes C14 . H141 . 0.949 no C15 . H151 . 0.948 no C15 . H152 . 0.950 no C15 . H153 . 0.948 no C16 . H161 . 0.948 no C16 . H162 . 0.949 no C16 . H163 . 0.949 no C17 . C18 . 1.426(5) yes C17 . C21 . 1.419(5) yes C17 . C22 . 1.500(5) yes C18 . C19 . 1.418(5) yes C18 . C23 . 1.498(5) yes C19 . C20 . 1.426(5) yes C19 . C24 . 1.493(5) yes C20 . C21 . 1.405(5) yes C20 . C25 . 1.493(5) yes C21 . C26 . 1.494(5) yes C22 . H221 . 0.948 no C22 . H222 . 0.949 no C22 . H223 . 0.949 no C23 . H231 . 0.948 no C23 . H232 . 0.949 no C23 . H233 . 0.949 no C24 . H241 . 0.948 no C24 . H242 . 0.949 no C24 . H243 . 0.948 no C25 . H251 . 0.949 no C25 . H252 . 0.948 no C25 . H253 . 0.948 no C26 . H261 . 0.949 no C26 . H262 . 0.948 no C26 . H263 . 0.949 no C27 . C28 . 1.525(9) yes C27 . C281 . 1.524(9) yes C27 . H271 . 0.948 no C27 . H272 . 0.949 no C27 . H273 . 0.948 no C28 . C29 . 1.533(7) yes C28 . H281 . 0.948 no C28 . H282 . 0.949 no C281 . C29 . 1.535(7) yes C281 . H2811 . 0.949 no C281 . H2812 . 0.948 no C29 . H291 2_565 0.949 no C29 . H292 2_565 0.948 no C29 . H291 . 0.949 no C29 . H292 . 0.948 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 N1 . Ti1 . N2 . 40.38(10) yes N1 . Ti1 . N3 . 130.00(11) yes N2 . Ti1 . N3 . 90.47(11) yes N1 . Ti1 . N4 . 101.18(12) yes N2 . Ti1 . N4 . 88.86(10) yes N3 . Ti1 . N4 . 60.43(11) yes N1 . Ti1 . C9 . 114.35(11) yes N2 . Ti1 . C9 . 84.28(11) yes N3 . Ti1 . C9 . 30.60(11) yes N4 . Ti1 . C9 . 30.67(11) yes N1 . Ti1 . C17 . 89.32(11) yes N2 . Ti1 . C17 . 129.64(11) yes N3 . Ti1 . C17 . 137.74(11) yes N4 . Ti1 . C17 . 102.26(11) yes C9 . Ti1 . C17 . 127.54(11) yes N1 . Ti1 . C18 . 88.68(12) yes N2 . Ti1 . C18 . 122.31(11) yes N3 . Ti1 . C18 . 138.20(12) yes N4 . Ti1 . C18 . 136.04(11) yes C9 . Ti1 . C18 . 153.30(11) yes N1 . Ti1 . C19 . 119.25(12) yes N2 . Ti1 . C19 . 138.58(11) yes N3 . Ti1 . C19 . 103.91(12) yes N4 . Ti1 . C19 . 132.10(11) yes C9 . Ti1 . C19 . 126.35(12) yes N1 . Ti1 . C20 . 143.87(12) yes N2 . Ti1 . C20 . 169.87(11) yes N3 . Ti1 . C20 . 86.13(11) yes N4 . Ti1 . C20 . 97.71(11) yes C9 . Ti1 . C20 . 97.43(11) yes N1 . Ti1 . C21 . 120.02(12) yes N2 . Ti1 . C21 . 156.15(11) yes N3 . Ti1 . C21 . 103.90(11) yes N4 . Ti1 . C21 . 82.12(11) yes C9 . Ti1 . C21 . 98.37(11) yes N1 . Ti1 . H1 . 95.7(13) no N2 . Ti1 . H1 . 79.3(13) no N3 . Ti1 . H1 . 78.9(13) no N4 . Ti1 . H1 . 137.5(13) no C9 . Ti1 . H1 . 107.1(13) no C17 . Ti1 . C18 . 34.46(11) yes C17 . Ti1 . C19 . 57.10(12) yes C18 . Ti1 . C19 . 34.42(12) yes C17 . Ti1 . C20 . 56.51(11) yes C18 . Ti1 . C20 . 56.90(12) yes C19 . Ti1 . C20 . 34.39(12) yes C17 . Ti1 . C21 . 33.90(12) yes C18 . Ti1 . C21 . 56.62(11) yes C19 . Ti1 . C21 . 56.58(11) yes C20 . Ti1 . C21 . 33.61(12) yes C17 . Ti1 . H1 . 116.7(13) no C18 . Ti1 . H1 . 82.5(13) no C19 . Ti1 . H1 . 66.1(13) no C20 . Ti1 . H1 . 90.6(13) no C21 . Ti1 . H1 . 121.7(13) no Ti1 . N1 . N2 . 79.04(17) yes Ti1 . N1 . Si1 . 155.46(17) yes N2 . N1 . Si1 . 121.4(2) yes N1 . N2 . Ti1 . 60.58(14) yes N1 . N2 . C1 . 112.7(3) yes Ti1 . N2 . C1 . 123.4(2) yes N1 . N2 . C2 . 114.4(3) yes Ti1 . N2 . C2 . 124.6(2) yes C1 . N2 . C2 . 109.5(3) yes Ti1 . N3 . C9 . 92.0(2) yes Ti1 . N3 . C11 . 140.3(2) yes C9 . N3 . C11 . 121.1(3) yes Ti1 . N4 . C9 . 92.3(2) yes Ti1 . N4 . C14 . 141.4(2) yes C9 . N4 . C14 . 121.2(3) yes N1 . Si1 . C3 . 114.02(15) yes N1 . Si1 . H2 . 115.7(17) no C3 . Si1 . H2 . 106.0(17) no N1 . Si1 . H3 . 107.1(13) no C3 . Si1 . H3 . 108.4(13) no H2 . Si1 . H3 . 105(2) no N2 . C1 . H11 . 110.6 no N2 . C1 . H12 . 109.8 no H11 . C1 . H12 . 108.9 no N2 . C1 . H13 . 110.5 no H11 . C1 . H13 . 108.0 no H12 . C1 . H13 . 108.9 no N2 . C2 . H21 . 109.6 no N2 . C2 . H22 . 109.0 no H21 . C2 . H22 . 109.5 no N2 . C2 . H23 . 109.8 no H21 . C2 . H23 . 109.4 no H22 . C2 . H23 . 109.5 no Si1 . C3 . C4 . 122.1(3) yes Si1 . C3 . C8 . 120.9(3) yes C4 . C3 . C8 . 116.9(4) yes C3 . C4 . C5 . 121.2(4) yes C3 . C4 . H41 . 118.7 no C5 . C4 . H41 . 120.0 no C4 . C5 . C6 . 119.9(4) yes C4 . C5 . H51 . 119.6 no C6 . C5 . H51 . 120.5 no C5 . C6 . C7 . 120.4(4) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 119.7 no C6 . C7 . C8 . 119.5(4) yes C6 . C7 . H71 . 120.6 no C8 . C7 . H71 . 120.0 no C3 . C8 . C7 . 122.2(4) yes C3 . C8 . H81 . 118.4 no C7 . C8 . H81 . 119.4 no N4 . C9 . N3 . 112.2(3) yes N4 . C9 . Ti1 . 57.07(17) yes N3 . C9 . Ti1 . 57.36(17) yes N4 . C9 . C10 . 124.4(3) yes N3 . C9 . C10 . 123.3(3) yes Ti1 . C9 . C10 . 164.3(3) yes C9 . C10 . H101 . 109.0 no C9 . C10 . H102 . 109.2 no H101 . C10 . H102 . 109.5 no C9 . C10 . H103 . 110.3 no H101 . C10 . H103 . 109.4 no H102 . C10 . H103 . 109.5 no N3 . C11 . C12 . 111.6(3) yes N3 . C11 . C13 . 110.7(3) yes C12 . C11 . C13 . 109.4(3) yes N3 . C11 . H111 . 108.6 no C12 . C11 . H111 . 108.5 no C13 . C11 . H111 . 107.9 no C11 . C12 . H121 . 109.4 no C11 . C12 . H122 . 109.9 no H121 . C12 . H122 . 109.4 no C11 . C12 . H123 . 109.0 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no C11 . C13 . H131 . 109.7 no C11 . C13 . H132 . 110.3 no H131 . C13 . H132 . 109.5 no C11 . C13 . H133 . 108.4 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.4 no N4 . C14 . C15 . 109.9(3) yes N4 . C14 . C16 . 113.6(3) yes C15 . C14 . C16 . 110.1(3) yes N4 . C14 . H141 . 107.6 no C15 . C14 . H141 . 107.8 no C16 . C14 . H141 . 107.5 no C14 . C15 . H151 . 109.7 no C14 . C15 . H152 . 109.4 no H151 . C15 . H152 . 109.5 no C14 . C15 . H153 . 109.3 no H151 . C15 . H153 . 109.4 no H152 . C15 . H153 . 109.5 no C14 . C16 . H161 . 109.4 no C14 . C16 . H162 . 109.2 no H161 . C16 . H162 . 109.5 no C14 . C16 . H163 . 109.8 no H161 . C16 . H163 . 109.4 no H162 . C16 . H163 . 109.5 no Ti1 . C17 . C18 . 71.40(18) yes Ti1 . C17 . C21 . 73.71(18) yes C18 . C17 . C21 . 107.3(3) yes Ti1 . C17 . C22 . 126.9(2) yes C18 . C17 . C22 . 126.6(3) yes C21 . C17 . C22 . 125.6(3) yes Ti1 . C18 . C17 . 74.14(18) yes Ti1 . C18 . C19 . 73.31(19) yes C17 . C18 . C19 . 108.4(3) yes Ti1 . C18 . C23 . 122.7(2) yes C17 . C18 . C23 . 127.1(3) yes C19 . C18 . C23 . 124.3(3) yes Ti1 . C19 . C18 . 72.28(19) yes Ti1 . C19 . C20 . 73.45(19) yes C18 . C19 . C20 . 107.3(3) yes Ti1 . C19 . C24 . 127.5(2) yes C18 . C19 . C24 . 125.5(3) yes C20 . C19 . C24 . 126.4(3) yes Ti1 . C20 . C19 . 72.16(18) yes Ti1 . C20 . C21 . 74.07(18) yes C19 . C20 . C21 . 108.4(3) yes Ti1 . C20 . C25 . 124.8(2) yes C19 . C20 . C25 . 127.0(3) yes C21 . C20 . C25 . 124.3(3) yes Ti1 . C21 . C17 . 72.40(17) yes Ti1 . C21 . C20 . 72.32(18) yes C17 . C21 . C20 . 108.6(3) yes Ti1 . C21 . C26 . 128.7(2) yes C17 . C21 . C26 . 126.6(3) yes C20 . C21 . C26 . 124.1(3) yes C17 . C22 . H221 . 108.7 no C17 . C22 . H222 . 109.7 no H221 . C22 . H222 . 109.5 no C17 . C22 . H223 . 110.0 no H221 . C22 . H223 . 109.4 no H222 . C22 . H223 . 109.5 no C18 . C23 . H231 . 108.8 no C18 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.4 no C18 . C23 . H233 . 110.0 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C19 . C24 . H241 . 109.9 no C19 . C24 . H242 . 109.6 no H241 . C24 . H242 . 109.5 no C19 . C24 . H243 . 108.9 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.6 no C20 . C25 . H251 . 111.6 no C20 . C25 . H252 . 110.9 no H251 . C25 . H252 . 109.5 no C20 . C25 . H253 . 108.6 no H251 . C25 . H253 . 108.2 no H252 . C25 . H253 . 108.0 no C21 . C26 . H261 . 108.2 no C21 . C26 . H262 . 108.7 no H261 . C26 . H262 . 109.4 no C21 . C26 . H263 . 110.2 no H261 . C26 . H263 . 110.1 no H262 . C26 . H263 . 110.1 no C28 . C27 . C281 . 71.4(6) yes C28 . C27 . H271 . 109.2 no C281 . C27 . H271 . 163.8 no C28 . C27 . H272 . 114.9 no C281 . C27 . H272 . 58.0 no H271 . C27 . H272 . 109.4 no C28 . C27 . H273 . 104.2 no C281 . C27 . H273 . 85.6 no H271 . C27 . H273 . 109.4 no H272 . C27 . H273 . 109.5 no C27 . C28 . C29 . 108.3(6) yes C27 . C28 . H281 . 104.5 no C29 . C28 . H281 . 102.1 no C27 . C28 . H282 . 115.2 no C29 . C28 . H282 . 115.8 no H281 . C28 . H282 . 109.5 no C27 . C281 . C29 . 108.2(6) yes C27 . C281 . H2811 . 113.2 no C29 . C281 . H2811 . 111.8 no C27 . C281 . H2812 . 105.6 no C29 . C281 . H2812 . 108.2 no H2811 . C281 . H2812 . 109.4 no C281 . C29 . C281 2_565 179.993 yes C281 . C29 . C28 2_565 109.1(5) yes C281 2_565 C29 . C28 2_565 70.9(5) yes C281 . C29 . C28 . 70.9(5) yes C281 2_565 C29 . C28 . 109.1(5) yes C28 2_565 C29 . C28 . 179.993 yes C281 . C29 . H291 2_565 111.2 no C281 2_565 C29 . H291 2_565 68.8 no C28 2_565 C29 . H291 2_565 116.4 no C28 . C29 . H291 2_565 63.6 no C281 . C29 . H292 2_565 107.5 no C281 2_565 C29 . H292 2_565 72.5 no C28 2_565 C29 . H292 2_565 102.5 no C28 . C29 . H292 2_565 77.5 no H291 2_565 C29 . H292 2_565 109.5 no C281 . C29 . H291 . 68.8 no C281 2_565 C29 . H291 . 111.2 no C28 2_565 C29 . H291 . 63.6 no C28 . C29 . H291 . 116.4 no H291 2_565 C29 . H291 . 180.0 no C281 . C29 . H292 . 72.5 no C281 2_565 C29 . H292 . 107.5 no C28 2_565 C29 . H292 . 77.5 no C28 . C29 . H292 . 102.5 no H291 2_565 C29 . H292 . 70.5 no H292 2_565 C29 . H291 . 70.5 no H292 2_565 C29 . H292 . 180.0 no H291 . C29 . H292 . 109.5 no #===end data_COMPOUND_4 _database_code_depnum_ccdc_archive 'CCDC 802265' #TrackingRef '- Mountford Xray SI.CIF' # Local code pjt9 _chemical_name_systematic ; Cp*Ti{MeC(NiPr)2}(Cl){N(NMe2)SiH2Ph} ; _publ_section_exptl_refinement ; Si-H hydrogen atoms were located from Fourier maps and positionally and isotropically refined. C-bound H atoms were placed in calculated positions with reference to a Fourier difference map and refined in a riding model. ; _cell_length_a 9.8784(2) _cell_length_b 10.3809(3) _cell_length_c 15.6151(4) _cell_angle_alpha 94.6300(11) _cell_angle_beta 99.7244(13) _cell_angle_gamma 114.5284(13) _cell_volume 1415.38(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C26 H45 Cl1 N4 Si1 Ti1' _chemical_formula_moiety 'C26 H45 Cl1 N4 Si1 Ti1' _chemical_compound_source ? _chemical_formula_weight 525.11 _cell_measurement_reflns_used 5873 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 0.460 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 11308 _reflns_number_total 6390 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_min 5.125 _diffrn_reflns_theta_max 27.478 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.554 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.05 _oxford_diffrn_Wilson_scale 7.36 _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.42 _refine_diff_density_max 0.44 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 3817 _refine_ls_number_restraints 0 _refine_ls_number_parameters 306 _oxford_refine_ls_R_factor_ref 0.0481 _refine_ls_wR_factor_ref 0.0548 _refine_ls_goodness_of_fit_ref 1.0956 _refine_ls_shift/su_max 0.000408 # The values computed from all data _oxford_reflns_number_all 6390 _refine_ls_R_factor_all 0.0994 _refine_ls_wR_factor_all 0.0858 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4276 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_gt 0.0585 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _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: 0.993 0.560 0.687 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # 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_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ti1 Ti 0.84365(6) 0.26964(5) 0.74493(3) 0.0213 1.0000 Uani . . . . . . . Cl1 Cl 0.78253(9) 0.39942(8) 0.85865(5) 0.0306 1.0000 Uani . . . . . . . Si1 Si 0.86914(10) -0.03551(9) 0.82763(6) 0.0303 1.0000 Uani . . . . . . . N1 N 0.8840(3) 0.1320(2) 0.80866(16) 0.0243 1.0000 Uani . . . . . . . N2 N 1.0034(3) 0.2627(3) 0.86126(16) 0.0261 1.0000 Uani . . . . . . . N3 N 0.9941(3) 0.4828(3) 0.73132(16) 0.0254 1.0000 Uani . . . . . . . N4 N 1.0305(3) 0.3029(3) 0.67368(16) 0.0240 1.0000 Uani . . . . . . . C1 C 0.9873(4) 0.2786(4) 0.9537(2) 0.0359 1.0000 Uani . . . . . . . C2 C 1.1622(4) 0.2879(4) 0.8626(2) 0.0336 1.0000 Uani . . . . . . . C3 C 0.7227(3) -0.1351(3) 0.8900(2) 0.0280 1.0000 Uani . . . . . . . C4 C 0.6633(4) -0.0700(4) 0.9462(2) 0.0386 1.0000 Uani . . . . . . . C5 C 0.5543(4) -0.1518(4) 0.9897(3) 0.0429 1.0000 Uani . . . . . . . C6 C 0.5010(4) -0.2996(4) 0.9777(3) 0.0411 1.0000 Uani . . . . . . . C7 C 0.5577(4) -0.3654(4) 0.9230(2) 0.0388 1.0000 Uani . . . . . . . C8 C 0.6679(4) -0.2839(3) 0.8799(2) 0.0327 1.0000 Uani . . . . . . . C9 C 1.0910(3) 0.4442(3) 0.70025(19) 0.0245 1.0000 Uani . . . . . . . C10 C 1.2532(4) 0.5449(3) 0.6996(2) 0.0307 1.0000 Uani . . . . . . . C11 C 1.0247(4) 0.6302(3) 0.7669(2) 0.0291 1.0000 Uani . . . . . . . C12 C 1.1498(4) 0.6963(4) 0.8512(2) 0.0412 1.0000 Uani . . . . . . . C13 C 1.0500(5) 0.7281(4) 0.6972(3) 0.0401 1.0000 Uani . . . . . . . C14 C 1.1248(4) 0.2410(3) 0.6389(2) 0.0280 1.0000 Uani . . . . . . . C15 C 1.1287(5) 0.2587(4) 0.5428(2) 0.0413 1.0000 Uani . . . . . . . C16 C 1.0743(4) 0.0839(3) 0.6481(2) 0.0339 1.0000 Uani . . . . . . . C17 C 0.6820(3) 0.1094(3) 0.6043(2) 0.0294 1.0000 Uani . . . . . . . C18 C 0.6015(4) 0.0645(3) 0.6707(2) 0.0340 1.0000 Uani . . . . . . . C19 C 0.5661(3) 0.1748(4) 0.7031(2) 0.0362 1.0000 Uani . . . . . . . C20 C 0.6273(4) 0.2905(4) 0.6572(2) 0.0337 1.0000 Uani . . . . . . . C21 C 0.7014(4) 0.2519(3) 0.5972(2) 0.0303 1.0000 Uani . . . . . . . C22 C 0.7093(4) 0.0133(4) 0.5403(3) 0.0484 1.0000 Uani . . . . . . . C23 C 0.5331(5) -0.0848(4) 0.6914(3) 0.0541 1.0000 Uani . . . . . . . C24 C 0.4638(4) 0.1597(6) 0.7664(3) 0.0598 1.0000 Uani . . . . . . . C25 C 0.6085(5) 0.4265(5) 0.6647(3) 0.0562 1.0000 Uani . . . . . . . C26 C 0.7724(5) 0.3385(4) 0.5312(2) 0.0462 1.0000 Uani . . . . . . . H1 H 0.830(5) -0.126(5) 0.747(3) 0.060(13) 1.0000 Uiso . . . . . . . H2 H 1.007(4) -0.021(4) 0.869(2) 0.039(10) 1.0000 Uiso . . . . . . . H11 H 1.0680 0.3658 0.9863 0.0432 1.0000 Uiso R . . . . . . H12 H 0.9915 0.2000 0.9793 0.0432 1.0000 Uiso R . . . . . . H13 H 0.8922 0.2803 0.9549 0.0432 1.0000 Uiso R . . . . . . H21 H 1.2303 0.3769 0.8993 0.0400 1.0000 Uiso R . . . . . . H22 H 1.1798 0.2124 0.8849 0.0400 1.0000 Uiso R . . . . . . H23 H 1.1789 0.2907 0.8044 0.0400 1.0000 Uiso R . . . . . . H41 H 0.6983 0.0312 0.9544 0.0461 1.0000 Uiso R . . . . . . H51 H 0.5162 -0.1061 1.0279 0.0513 1.0000 Uiso R . . . . . . H61 H 0.4256 -0.3553 1.0072 0.0487 1.0000 Uiso R . . . . . . H71 H 0.5212 -0.4668 0.9147 0.0464 1.0000 Uiso R . . . . . . H81 H 0.7068 -0.3304 0.8427 0.0389 1.0000 Uiso R . . . . . . H101 H 1.3193 0.5165 0.7363 0.0356 1.0000 Uiso R . . . . . . H102 H 1.2770 0.6413 0.7225 0.0356 1.0000 Uiso R . . . . . . H103 H 1.2722 0.5402 0.6421 0.0356 1.0000 Uiso R . . . . . . H111 H 0.9337 0.6230 0.7832 0.0348 1.0000 Uiso R . . . . . . H121 H 1.1638 0.7910 0.8704 0.0496 1.0000 Uiso R . . . . . . H122 H 1.1207 0.6396 0.8956 0.0496 1.0000 Uiso R . . . . . . H123 H 1.2426 0.6992 0.8400 0.0496 1.0000 Uiso R . . . . . . H131 H 1.0695 0.8218 0.7234 0.0484 1.0000 Uiso R . . . . . . H132 H 1.1349 0.7325 0.6745 0.0484 1.0000 Uiso R . . . . . . H133 H 0.9614 0.6911 0.6507 0.0484 1.0000 Uiso R . . . . . . H141 H 1.2264 0.2930 0.6728 0.0334 1.0000 Uiso R . . . . . . H151 H 1.1901 0.2179 0.5227 0.0498 1.0000 Uiso R . . . . . . H152 H 1.1705 0.3580 0.5387 0.0498 1.0000 Uiso R . . . . . . H153 H 1.0279 0.2114 0.5074 0.0498 1.0000 Uiso R . . . . . . H161 H 1.1380 0.0492 0.6249 0.0403 1.0000 Uiso R . . . . . . H162 H 1.0817 0.0751 0.7086 0.0403 1.0000 Uiso R . . . . . . H163 H 0.9715 0.0293 0.6166 0.0403 1.0000 Uiso R . . . . . . H221 H 0.7661 0.0686 0.5021 0.0587 1.0000 Uiso R . . . . . . H222 H 0.7652 -0.0306 0.5714 0.0587 1.0000 Uiso R . . . . . . H223 H 0.6144 -0.0588 0.5067 0.0587 1.0000 Uiso R . . . . . . H231 H 0.4852 -0.0858 0.7394 0.0651 1.0000 Uiso R . . . . . . H232 H 0.6111 -0.1152 0.7067 0.0651 1.0000 Uiso R . . . . . . H233 H 0.4595 -0.1480 0.6412 0.0651 1.0000 Uiso R . . . . . . H241 H 0.4567 0.2474 0.7789 0.0731 1.0000 Uiso R . . . . . . H242 H 0.5051 0.1372 0.8194 0.0731 1.0000 Uiso R . . . . . . H243 H 0.3651 0.0849 0.7409 0.0731 1.0000 Uiso R . . . . . . H251 H 0.6613 0.4854 0.6264 0.0672 1.0000 Uiso R . . . . . . H252 H 0.6493 0.4761 0.7237 0.0672 1.0000 Uiso R . . . . . . H253 H 0.5032 0.4045 0.6486 0.0672 1.0000 Uiso R . . . . . . H261 H 0.7717 0.4298 0.5405 0.0557 1.0000 Uiso R . . . . . . H262 H 0.8747 0.3510 0.5377 0.0557 1.0000 Uiso R . . . . . . H263 H 0.7160 0.2897 0.4735 0.0557 1.0000 Uiso 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 0.0195(3) 0.0207(3) 0.0201(3) 0.00161(19) 0.00272(19) 0.0063(2) Cl1 0.0304(4) 0.0325(4) 0.0276(4) -0.0007(3) 0.0080(3) 0.0128(3) Si1 0.0306(5) 0.0252(4) 0.0391(5) 0.0093(4) 0.0141(4) 0.0128(4) N1 0.0226(12) 0.0221(12) 0.0223(12) 0.0014(9) 0.0036(9) 0.0052(10) N2 0.0261(13) 0.0226(12) 0.0227(12) 0.0011(9) 0.0005(10) 0.0063(10) N3 0.0262(13) 0.0225(12) 0.0247(12) 0.0010(9) 0.0071(10) 0.0079(10) N4 0.0246(12) 0.0218(11) 0.0255(12) 0.0031(9) 0.0066(10) 0.0097(10) C1 0.045(2) 0.0385(18) 0.0204(15) 0.0034(13) 0.0019(13) 0.0166(15) C2 0.0244(15) 0.0354(17) 0.0333(17) 0.0068(13) -0.0022(13) 0.0087(13) C3 0.0273(15) 0.0285(15) 0.0284(15) 0.0059(12) 0.0052(12) 0.0125(13) C4 0.0404(19) 0.0362(18) 0.045(2) 0.0125(15) 0.0199(16) 0.0178(15) C5 0.049(2) 0.048(2) 0.044(2) 0.0190(17) 0.0226(17) 0.0271(18) C6 0.0314(17) 0.048(2) 0.047(2) 0.0250(17) 0.0114(15) 0.0162(16) C7 0.0358(18) 0.0300(16) 0.0406(19) 0.0103(14) 0.0023(15) 0.0066(14) C8 0.0345(17) 0.0260(15) 0.0353(17) 0.0050(13) 0.0059(14) 0.0117(13) C9 0.0257(14) 0.0255(14) 0.0213(13) 0.0065(11) 0.0073(11) 0.0090(12) C10 0.0273(15) 0.0234(14) 0.0387(18) 0.0046(12) 0.0113(13) 0.0071(12) C11 0.0345(16) 0.0212(14) 0.0340(16) 0.0033(12) 0.0104(13) 0.0138(12) C12 0.048(2) 0.0322(17) 0.0334(18) -0.0065(14) 0.0060(15) 0.0109(16) C13 0.051(2) 0.0283(16) 0.047(2) 0.0119(15) 0.0157(17) 0.0201(16) C14 0.0283(15) 0.0288(15) 0.0281(15) 0.0026(12) 0.0086(12) 0.0131(12) C15 0.053(2) 0.0378(18) 0.0359(18) 0.0036(15) 0.0199(16) 0.0195(17) C16 0.0355(18) 0.0283(16) 0.0397(18) 0.0007(13) 0.0089(14) 0.0164(14) C17 0.0257(15) 0.0304(15) 0.0241(15) -0.0044(12) -0.0056(12) 0.0103(13) C18 0.0260(16) 0.0308(16) 0.0310(16) 0.0050(13) -0.0003(13) 0.0013(13) C19 0.0168(14) 0.052(2) 0.0282(16) -0.0012(14) -0.0023(12) 0.0079(14) C20 0.0263(15) 0.0392(17) 0.0330(17) -0.0014(13) -0.0043(13) 0.0172(14) C21 0.0265(15) 0.0319(16) 0.0235(15) 0.0026(12) -0.0048(12) 0.0084(13) C22 0.0354(19) 0.052(2) 0.045(2) -0.0168(17) -0.0049(16) 0.0157(17) C23 0.036(2) 0.039(2) 0.057(2) 0.0135(17) -0.0111(17) -0.0060(16) C24 0.0248(18) 0.089(3) 0.047(2) -0.003(2) 0.0093(16) 0.0082(19) C25 0.056(3) 0.057(2) 0.059(3) -0.006(2) -0.011(2) 0.041(2) C26 0.045(2) 0.046(2) 0.0341(19) 0.0130(16) -0.0003(16) 0.0094(17) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3741(8) 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 . Cl1 . 2.4463(9) yes Ti1 . N1 . 1.939(3) yes Ti1 . N2 . 2.223(3) yes Ti1 . N3 . 2.145(2) yes Ti1 . N4 . 2.234(2) yes Ti1 . C17 . 2.482(3) yes Ti1 . C18 . 2.457(3) yes Ti1 . C19 . 2.442(3) yes Ti1 . C20 . 2.436(3) yes Ti1 . C21 . 2.439(3) yes Si1 . N1 . 1.737(3) yes Si1 . C3 . 1.872(3) yes Si1 . H1 . 1.40(5) no Si1 . H2 . 1.35(4) no N1 . N2 . 1.439(3) yes N2 . C1 . 1.483(4) yes N2 . C2 . 1.476(4) yes N3 . C9 . 1.325(4) yes N3 . C11 . 1.471(4) yes N4 . C9 . 1.331(4) yes N4 . C14 . 1.478(4) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . C4 . 1.407(5) yes C3 . C8 . 1.393(4) yes C4 . C5 . 1.386(5) yes C4 . H41 . 0.950 no C5 . C6 . 1.384(6) yes C5 . H51 . 0.950 no C6 . C7 . 1.377(6) yes C6 . H61 . 0.950 no C7 . C8 . 1.389(5) yes C7 . H71 . 0.950 no C8 . H81 . 0.950 no C9 . C10 . 1.509(4) yes C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . C12 . 1.526(5) yes C11 . C13 . 1.530(5) yes C11 . H111 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . C15 . 1.532(5) yes C14 . C16 . 1.522(4) yes C14 . H141 . 0.950 no C15 . H151 . 0.950 no C15 . H152 . 0.950 no C15 . H153 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no C17 . C18 . 1.404(5) yes C17 . C21 . 1.427(5) yes C17 . C22 . 1.489(5) yes C18 . C19 . 1.410(5) yes C18 . C23 . 1.500(5) yes C19 . C20 . 1.416(5) yes C19 . C24 . 1.500(5) yes C20 . C21 . 1.410(5) yes C20 . C25 . 1.497(5) yes C21 . C26 . 1.494(5) yes C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . H231 . 0.950 no C23 . H232 . 0.950 no C23 . H233 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.950 no C24 . H243 . 0.950 no C25 . H251 . 0.950 no C25 . H252 . 0.950 no C25 . H253 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 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 Cl1 . Ti1 . N1 . 100.95(8) yes Cl1 . Ti1 . N2 . 81.54(7) yes N1 . Ti1 . N2 . 39.72(9) yes Cl1 . Ti1 . N3 . 82.68(7) yes N1 . Ti1 . N3 . 130.54(10) yes N2 . Ti1 . N3 . 93.99(9) yes Cl1 . Ti1 . N4 . 139.68(7) yes N1 . Ti1 . N4 . 92.88(10) yes N2 . Ti1 . N4 . 85.74(9) yes N3 . Ti1 . N4 . 60.16(9) yes Cl1 . Ti1 . C17 . 130.81(8) yes N1 . Ti1 . C17 . 99.81(10) yes N2 . Ti1 . C17 . 137.07(10) yes N3 . Ti1 . C17 . 114.84(10) yes N4 . Ti1 . C17 . 82.53(10) yes Cl1 . Ti1 . C18 . 105.92(9) yes N1 . Ti1 . C18 . 85.35(11) yes N2 . Ti1 . C18 . 124.02(10) yes N3 . Ti1 . C18 . 141.64(11) yes N4 . Ti1 . C18 . 112.86(11) yes Cl1 . Ti1 . C19 . 76.22(8) yes N1 . Ti1 . C19 . 105.82(12) yes N2 . Ti1 . C19 . 133.30(11) yes N3 . Ti1 . C19 . 122.60(12) yes N4 . Ti1 . C19 . 135.76(10) yes Cl1 . Ti1 . C20 . 80.17(8) yes N1 . Ti1 . C20 . 138.77(11) yes N2 . Ti1 . C20 . 160.39(11) yes N3 . Ti1 . C20 . 90.66(11) yes N4 . Ti1 . C20 . 112.95(11) yes Cl1 . Ti1 . C21 . 112.59(8) yes N1 . Ti1 . C21 . 133.49(10) yes N2 . Ti1 . C21 . 165.74(10) yes N3 . Ti1 . C21 . 86.31(10) yes N4 . Ti1 . C21 . 82.04(10) yes C17 . Ti1 . C18 . 33.03(11) yes C17 . Ti1 . C19 . 55.31(11) yes C18 . Ti1 . C19 . 33.45(12) yes C17 . Ti1 . C20 . 55.54(11) yes C18 . Ti1 . C20 . 55.63(12) yes C19 . Ti1 . C20 . 33.75(12) yes C17 . Ti1 . C21 . 33.70(11) yes C18 . Ti1 . C21 . 55.65(11) yes C19 . Ti1 . C21 . 55.89(11) yes C20 . Ti1 . C21 . 33.61(11) yes N1 . Si1 . C3 . 116.44(13) yes N1 . Si1 . H1 . 109.5(19) no C3 . Si1 . H1 . 105.4(18) no N1 . Si1 . H2 . 109.0(16) no C3 . Si1 . H2 . 109.7(16) no H1 . Si1 . H2 . 106(2) no Si1 . N1 . Ti1 . 156.97(15) yes Si1 . N1 . N2 . 121.62(19) yes Ti1 . N1 . N2 . 80.84(15) yes N1 . N2 . Ti1 . 59.45(13) yes N1 . N2 . C1 . 111.9(2) yes Ti1 . N2 . C1 . 125.1(2) yes N1 . N2 . C2 . 117.2(2) yes Ti1 . N2 . C2 . 124.2(2) yes C1 . N2 . C2 . 108.1(2) yes Ti1 . N3 . C9 . 94.90(18) yes Ti1 . N3 . C11 . 136.6(2) yes C9 . N3 . C11 . 125.7(2) yes Ti1 . N4 . C9 . 90.78(17) yes Ti1 . N4 . C14 . 146.75(19) yes C9 . N4 . C14 . 118.7(2) yes N2 . C1 . H11 . 109.4 no N2 . C1 . H12 . 109.5 no H11 . C1 . H12 . 109.5 no N2 . C1 . H13 . 109.5 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no N2 . C2 . H21 . 109.4 no N2 . C2 . H22 . 109.4 no H21 . C2 . H22 . 109.5 no N2 . C2 . H23 . 109.5 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no Si1 . C3 . C4 . 124.5(2) yes Si1 . C3 . C8 . 118.0(2) yes C4 . C3 . C8 . 117.5(3) yes C3 . C4 . C5 . 120.9(3) yes C3 . C4 . H41 . 119.5 no C5 . C4 . H41 . 119.7 no C4 . C5 . C6 . 120.4(4) yes C4 . C5 . H51 . 119.8 no C6 . C5 . H51 . 119.9 no C5 . C6 . C7 . 119.7(3) yes C5 . C6 . H61 . 120.1 no C7 . C6 . H61 . 120.2 no C6 . C7 . C8 . 120.1(3) yes C6 . C7 . H71 . 119.9 no C8 . C7 . H71 . 120.0 no C3 . C8 . C7 . 121.4(3) yes C3 . C8 . H81 . 119.2 no C7 . C8 . H81 . 119.4 no N4 . C9 . N3 . 111.6(3) yes N4 . C9 . C10 . 123.5(3) yes N3 . C9 . C10 . 124.9(3) yes C9 . C10 . H101 . 108.0 no C9 . C10 . H102 . 111.6 no H101 . C10 . H102 . 108.0 no C9 . C10 . H103 . 111.7 no H101 . C10 . H103 . 108.0 no H102 . C10 . H103 . 109.5 no N3 . C11 . C12 . 113.9(3) yes N3 . C11 . C13 . 112.5(3) yes C12 . C11 . C13 . 112.5(3) yes N3 . C11 . H111 . 105.7 no C12 . C11 . H111 . 105.8 no C13 . C11 . H111 . 105.7 no C11 . C12 . H121 . 109.4 no C11 . C12 . H122 . 109.3 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 109.6 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no C11 . C13 . H131 . 109.3 no C11 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no C11 . C13 . H133 . 109.6 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N4 . C14 . C15 . 111.8(3) yes N4 . C14 . C16 . 112.7(2) yes C15 . C14 . C16 . 110.0(3) yes N4 . C14 . H141 . 107.4 no C15 . C14 . H141 . 107.3 no C16 . C14 . H141 . 107.3 no C14 . C15 . H151 . 109.5 no C14 . C15 . H152 . 109.4 no H151 . C15 . H152 . 109.5 no C14 . C15 . H153 . 109.5 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 109.5 no C14 . C16 . H161 . 109.5 no C14 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no C14 . C16 . H163 . 109.4 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no Ti1 . C17 . C18 . 72.49(17) yes Ti1 . C17 . C21 . 71.50(16) yes C18 . C17 . C21 . 107.6(3) yes Ti1 . C17 . C22 . 131.8(2) yes C18 . C17 . C22 . 124.9(3) yes C21 . C17 . C22 . 126.1(3) yes Ti1 . C18 . C17 . 74.48(17) yes Ti1 . C18 . C19 . 72.72(17) yes C17 . C18 . C19 . 108.6(3) yes Ti1 . C18 . C23 . 128.9(2) yes C17 . C18 . C23 . 126.6(4) yes C19 . C18 . C23 . 123.5(3) yes Ti1 . C19 . C18 . 73.84(18) yes Ti1 . C19 . C20 . 72.89(18) yes C18 . C19 . C20 . 107.8(3) yes Ti1 . C19 . C24 . 125.0(2) yes C18 . C19 . C24 . 124.3(4) yes C20 . C19 . C24 . 127.5(4) yes Ti1 . C20 . C19 . 73.37(18) yes Ti1 . C20 . C21 . 73.31(17) yes C19 . C20 . C21 . 108.1(3) yes Ti1 . C20 . C25 . 122.6(2) yes C19 . C20 . C25 . 126.9(3) yes C21 . C20 . C25 . 124.8(3) yes Ti1 . C21 . C17 . 74.80(17) yes Ti1 . C21 . C20 . 73.07(17) yes C17 . C21 . C20 . 107.8(3) yes Ti1 . C21 . C26 . 123.0(2) yes C17 . C21 . C26 . 126.0(3) yes C20 . C21 . C26 . 125.9(3) yes C17 . C22 . H221 . 109.2 no C17 . C22 . H222 . 109.6 no H221 . C22 . H222 . 109.5 no C17 . C22 . H223 . 109.7 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no C18 . C23 . H231 . 109.6 no C18 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.5 no C18 . C23 . H233 . 109.3 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C19 . C24 . H241 . 109.5 no C19 . C24 . H242 . 109.4 no H241 . C24 . H242 . 109.5 no C19 . C24 . H243 . 109.5 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C20 . C25 . H251 . 109.3 no C20 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no C20 . C25 . H253 . 109.6 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no C21 . C26 . H261 . 109.5 no C21 . C26 . H262 . 109.5 no H261 . C26 . H262 . 109.5 no C21 . C26 . H263 . 109.4 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no #===end #===end data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 849349' #TrackingRef '- Mountford Xray SI.CIF' # local code PJT16 _chemical_name_systematic ; Cp*Ti{MeC(NiPr)2}(H){N(NMe2)SiH2ArF} ; _chemical_melting_point ? _publ_section_exptl_refinement ; Si-H and Ti-H hydrogen atoms were located from Fourier maps and positionally and isotropically refined. The CF3 groups were positionally disordered and refined in a two-site model for the F atoms (50% chemical occupancies) subject to loose similarity restraints applied to the adps, C-F distances and F-C-F and C-C-F angles. C-bound H atoms were placed in calculated positions with reference to a Fourier difference map and refined in a riding model. ; _cell_length_a 8.65520(10) _cell_length_b 24.6871(3) _cell_length_c 15.1275(2) _cell_angle_alpha 90 _cell_angle_beta 100.2706(5) _cell_angle_gamma 90 _cell_volume 3180.53(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C28 H44 F6 N4 Si1 Ti1' _chemical_formula_moiety 'C28 H44 F6 N4 Si1 Ti1' _chemical_compound_source ? _chemical_formula_weight 626.66 _cell_measurement_reflns_used 7247 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_min 0.020 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_max 0.150 _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.99 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 12292 _reflns_number_total 7235 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_min 5.111 _diffrn_reflns_theta_max 27.478 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.478 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 32 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 1.87 _oxford_diffrn_Wilson_scale 19.63 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.52 _refine_diff_density_max 0.87 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 4764 _refine_ls_number_restraints 120 _refine_ls_number_parameters 427 _oxford_refine_ls_R_factor_ref 0.0528 _refine_ls_wR_factor_ref 0.0618 _refine_ls_goodness_of_fit_ref 1.1203 _refine_ls_shift/su_max 0.0031504 _refine_ls_shift/su_mean 0.0001831 # The values computed from all data _oxford_reflns_number_all 7235 _refine_ls_R_factor_all 0.0893 _refine_ls_wR_factor_all 0.0883 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5237 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_gt 0.0656 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _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: 0.692 0.439 0.389 ; _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # 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_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ti1 Ti 0.82050(6) 0.62985(2) 0.89165(3) 0.0189 1.0000 Uani . . . . . . . N1 N 0.8879(3) 0.58399(10) 0.79952(16) 0.0229 1.0000 Uani . . . . . . . N2 N 1.0331(3) 0.58846(11) 0.86268(17) 0.0251 1.0000 Uani . . . . . . . N3 N 0.9612(3) 0.67336(10) 1.00319(17) 0.0255 1.0000 Uani . . . . . . . N4 N 0.9278(3) 0.70675(10) 0.86607(17) 0.0240 1.0000 Uani . . . . . . . Si1 Si 0.85927(10) 0.53323(4) 0.72018(6) 0.0274 1.0000 Uani . . . . . . . F1 F 1.3902(11) 0.4208(3) 0.6973(4) 0.0766 0.5000 Uani D U . . . . . F2 F 1.2852(9) 0.3951(2) 0.5729(8) 0.0919 0.5000 Uani D U . . . . . F3 F 1.4859(9) 0.4495(3) 0.5957(8) 0.0932 0.5000 Uani D U . . . . . F4 F 1.1538(12) 0.6008(3) 0.3928(5) 0.0748 0.5000 Uani D U . . . . . F5 F 1.3175(9) 0.6361(3) 0.4933(5) 0.0718 0.5000 Uani D U . . . . . F6 F 1.0857(13) 0.6579(3) 0.4861(7) 0.0940 0.5000 Uani D U . . . . . F11 F 1.3118(11) 0.3989(3) 0.6636(8) 0.0982 0.5000 Uani D U . . . . . F21 F 1.3498(12) 0.4150(4) 0.5322(4) 0.0918 0.5000 Uani D U . . . . . F31 F 1.4926(8) 0.4489(3) 0.6388(7) 0.0866 0.5000 Uani D U . . . . . F41 F 1.2130(10) 0.5975(3) 0.3994(5) 0.0582 0.5000 Uani D U . . . . . F51 F 1.2622(13) 0.6535(3) 0.5094(5) 0.0789 0.5000 Uani D U . . . . . F61 F 1.0294(7) 0.6380(3) 0.4416(5) 0.0623 0.5000 Uani D U . . . . . C1 C 1.0901(4) 0.53651(14) 0.9030(2) 0.0327 1.0000 Uani . . . . . . . C2 C 1.1609(4) 0.61565(14) 0.8270(2) 0.0307 1.0000 Uani . . . . . . . C3 C 1.0204(4) 0.53073(13) 0.6511(2) 0.0280 1.0000 Uani . . . . . . . C4 C 1.1231(4) 0.48699(13) 0.6565(2) 0.0299 1.0000 Uani . . . . . . . C5 C 1.2399(4) 0.48493(13) 0.6044(2) 0.0323 1.0000 Uani D U . . . . . C6 C 1.2558(4) 0.52670(14) 0.5451(2) 0.0349 1.0000 Uani . . . . . . . C7 C 1.1542(4) 0.57020(14) 0.5389(2) 0.0331 1.0000 Uani D U . . . . . C8 C 1.0376(4) 0.57207(13) 0.5908(2) 0.0294 1.0000 Uani . . . . . . . C9 C 1.3478(4) 0.43705(15) 0.6116(3) 0.0511 1.0000 Uani D U . . . . . C10 C 1.1707(5) 0.61526(15) 0.4753(2) 0.0486 1.0000 Uani D U . . . . . C11 C 1.0106(4) 0.70880(12) 0.9489(2) 0.0273 1.0000 Uani . . . . . . . C12 C 1.1498(5) 0.74625(17) 0.9769(3) 0.0456 1.0000 Uani . . . . . . . C13 C 1.0480(4) 0.66386(14) 1.0937(2) 0.0300 1.0000 Uani . . . . . . . C14 C 0.9411(5) 0.64309(17) 1.1560(2) 0.0425 1.0000 Uani . . . . . . . C15 C 1.1829(5) 0.62382(17) 1.0944(2) 0.0438 1.0000 Uani . . . . . . . C16 C 0.9693(4) 0.73972(13) 0.7931(2) 0.0310 1.0000 Uani . . . . . . . C17 C 0.8901(4) 0.71712(15) 0.7027(2) 0.0356 1.0000 Uani . . . . . . . C18 C 0.9281(5) 0.79980(14) 0.7988(3) 0.0445 1.0000 Uani . . . . . . . C19 C 0.5589(3) 0.63579(12) 0.8010(2) 0.0252 1.0000 Uani . . . . . . . C20 C 0.5670(3) 0.59005(12) 0.8585(2) 0.0242 1.0000 Uani . . . . . . . C21 C 0.5879(3) 0.60894(12) 0.9483(2) 0.0240 1.0000 Uani . . . . . . . C22 C 0.5948(3) 0.66625(12) 0.9461(2) 0.0255 1.0000 Uani . . . . . . . C23 C 0.5768(3) 0.68248(12) 0.8551(2) 0.0250 1.0000 Uani . . . . . . . C24 C 0.5167(4) 0.63535(15) 0.6999(2) 0.0357 1.0000 Uani . . . . . . . C25 C 0.5419(4) 0.53156(13) 0.8316(2) 0.0314 1.0000 Uani . . . . . . . C26 C 0.5745(4) 0.57436(14) 1.0288(2) 0.0320 1.0000 Uani . . . . . . . C27 C 0.6037(4) 0.70487(14) 1.0236(2) 0.0345 1.0000 Uani . . . . . . . C28 C 0.5560(4) 0.74033(14) 0.8245(3) 0.0371 1.0000 Uani . . . . . . . H1 H 0.846(5) 0.5849(15) 0.965(3) 0.033(9) 1.0000 Uiso . . . . . . . H2 H 0.862(5) 0.4803(15) 0.757(3) 0.035(10) 1.0000 Uiso . . . . . . . H3 H 0.718(5) 0.5450(16) 0.662(3) 0.037(10) 1.0000 Uiso . . . . . . . H11 H 1.1857 0.5422 0.9437 0.0372 1.0000 Uiso R . . . . . . H12 H 1.0141 0.5216 0.9342 0.0398 1.0000 Uiso R . . . . . . H13 H 1.1074 0.5122 0.8570 0.0398 1.0000 Uiso R . . . . . . H21 H 1.2521 0.6170 0.8725 0.0389 1.0000 Uiso R . . . . . . H22 H 1.1297 0.6514 0.8088 0.0389 1.0000 Uiso R . . . . . . H23 H 1.1835 0.5959 0.7769 0.0389 1.0000 Uiso R . . . . . . H41 H 1.1135 0.4582 0.6968 0.0371 1.0000 Uiso R . . . . . . H61 H 1.3358 0.5256 0.5095 0.0423 1.0000 Uiso R . . . . . . H81 H 0.9679 0.6021 0.5851 0.0366 1.0000 Uiso R . . . . . . H121 H 1.1644 0.7683 0.9276 0.0580 1.0000 Uiso R . . . . . . H122 H 1.1308 0.7686 1.0249 0.0580 1.0000 Uiso R . . . . . . H123 H 1.2415 0.7252 0.9962 0.0580 1.0000 Uiso R . . . . . . H131 H 1.0911 0.6975 1.1167 0.0376 1.0000 Uiso R . . . . . . H141 H 1.0006 0.6373 1.2143 0.0532 1.0000 Uiso R . . . . . . H142 H 0.8613 0.6691 1.1591 0.0532 1.0000 Uiso R . . . . . . H143 H 0.8944 0.6099 1.1332 0.0532 1.0000 Uiso R . . . . . . H151 H 1.2366 0.6188 1.1543 0.0549 1.0000 Uiso R . . . . . . H152 H 1.2537 0.6378 1.0588 0.0549 1.0000 Uiso R . . . . . . H153 H 1.1426 0.5901 1.0705 0.0549 1.0000 Uiso R . . . . . . H161 H 1.0796 0.7371 0.7961 0.0385 1.0000 Uiso R . . . . . . H171 H 0.9174 0.7386 0.6557 0.0447 1.0000 Uiso R . . . . . . H172 H 0.7794 0.7177 0.6993 0.0447 1.0000 Uiso R . . . . . . H173 H 0.9238 0.6809 0.6968 0.0447 1.0000 Uiso R . . . . . . H181 H 0.9583 0.8188 0.7499 0.0547 1.0000 Uiso R . . . . . . H182 H 0.9822 0.8144 0.8537 0.0547 1.0000 Uiso R . . . . . . H183 H 0.8182 0.8035 0.7962 0.0547 1.0000 Uiso R . . . . . . H241 H 0.6058 0.6453 0.6749 0.0447 1.0000 Uiso R . . . . . . H242 H 0.4834 0.6001 0.6799 0.0447 1.0000 Uiso R . . . . . . H243 H 0.4341 0.6605 0.6814 0.0447 1.0000 Uiso R . . . . . . H251 H 0.4847 0.5101 0.8668 0.0391 1.0000 Uiso R . . . . . . H252 H 0.5055 0.5243 0.7697 0.0391 1.0000 Uiso R . . . . . . H253 H 0.6445 0.5165 0.8431 0.0391 1.0000 Uiso R . . . . . . H261 H 0.5926 0.5961 1.0815 0.0397 1.0000 Uiso R . . . . . . H262 H 0.6505 0.5462 1.0342 0.0397 1.0000 Uiso R . . . . . . H263 H 0.4724 0.5590 1.0216 0.0397 1.0000 Uiso R . . . . . . H271 H 0.5186 0.7297 1.0123 0.0431 1.0000 Uiso R . . . . . . H272 H 0.5994 0.6854 1.0772 0.0431 1.0000 Uiso R . . . . . . H273 H 0.6998 0.7244 1.0306 0.0431 1.0000 Uiso R . . . . . . H281 H 0.6421 0.7610 0.8547 0.0463 1.0000 Uiso R . . . . . . H282 H 0.4613 0.7538 0.8398 0.0463 1.0000 Uiso R . . . . . . H283 H 0.5514 0.7423 0.7614 0.0463 1.0000 Uiso 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 0.0168(2) 0.0207(2) 0.0194(2) -0.0001(2) 0.00401(17) 0.0001(2) N1 0.0183(12) 0.0265(12) 0.0239(12) -0.0001(10) 0.0037(9) -0.0010(9) N2 0.0200(12) 0.0310(13) 0.0250(12) 0.0014(10) 0.0058(10) 0.0051(10) N3 0.0271(13) 0.0278(13) 0.0205(12) -0.0018(10) 0.0013(10) -0.0030(10) N4 0.0246(12) 0.0218(12) 0.0254(12) 0.0025(10) 0.0037(10) -0.0038(10) Si1 0.0274(4) 0.0298(4) 0.0264(4) -0.0057(3) 0.0084(3) -0.0020(3) F1 0.090(5) 0.061(4) 0.070(4) -0.003(3) -0.010(4) 0.045(4) F2 0.090(5) 0.038(3) 0.126(6) -0.043(4) -0.037(5) 0.025(3) F3 0.056(4) 0.098(5) 0.142(7) 0.038(5) 0.061(5) 0.028(4) F4 0.099(7) 0.079(5) 0.036(3) 0.014(3) -0.015(4) -0.049(5) F5 0.092(5) 0.074(5) 0.047(3) 0.013(4) 0.008(3) -0.049(4) F6 0.134(7) 0.054(4) 0.114(6) 0.036(4) 0.075(5) 0.029(4) F11 0.087(5) 0.074(5) 0.150(7) 0.051(5) 0.068(5) 0.040(4) F21 0.117(6) 0.083(5) 0.067(4) -0.034(3) -0.007(4) 0.070(4) F31 0.043(4) 0.082(5) 0.118(6) -0.058(5) -0.029(4) 0.024(3) F41 0.073(5) 0.072(4) 0.036(4) 0.005(3) 0.027(3) 0.003(4) F51 0.123(7) 0.049(4) 0.052(4) 0.006(3) -0.019(4) -0.040(4) F61 0.056(3) 0.067(4) 0.063(4) 0.039(3) 0.011(3) 0.010(3) C1 0.0349(17) 0.0331(17) 0.0300(16) 0.0007(13) 0.0058(13) 0.0118(14) C2 0.0199(14) 0.0405(17) 0.0327(16) -0.0026(13) 0.0076(12) -0.0022(13) C3 0.0304(16) 0.0304(16) 0.0236(15) -0.0090(12) 0.0057(12) -0.0028(13) C4 0.0319(16) 0.0312(16) 0.0273(15) -0.0003(13) 0.0070(13) 0.0011(13) C5 0.0310(16) 0.0297(16) 0.0375(18) -0.0051(13) 0.0096(14) 0.0011(13) C6 0.0323(17) 0.0391(19) 0.0357(18) -0.0068(14) 0.0128(14) -0.0034(14) C7 0.0381(18) 0.0338(17) 0.0282(16) -0.0032(13) 0.0086(13) -0.0056(14) C8 0.0335(17) 0.0299(16) 0.0249(15) -0.0032(12) 0.0057(13) 0.0047(13) C9 0.047(2) 0.0417(19) 0.070(2) -0.0007(18) 0.0224(18) 0.0139(16) C10 0.063(2) 0.0438(19) 0.0429(19) 0.0050(16) 0.0206(17) -0.0035(17) C11 0.0265(15) 0.0263(15) 0.0291(15) -0.0014(12) 0.0052(12) -0.0041(12) C12 0.047(2) 0.049(2) 0.0363(19) 0.0005(16) -0.0043(17) -0.0191(18) C13 0.0298(17) 0.0355(17) 0.0226(15) -0.0039(12) -0.0011(12) -0.0018(13) C14 0.043(2) 0.058(2) 0.0266(17) 0.0042(15) 0.0046(15) -0.0059(17) C15 0.044(2) 0.055(2) 0.0292(18) -0.0001(16) -0.0042(15) 0.0091(18) C16 0.0286(16) 0.0322(17) 0.0321(16) 0.0064(13) 0.0051(13) -0.0055(13) C17 0.0422(19) 0.0399(18) 0.0246(15) 0.0103(14) 0.0054(14) -0.0034(15) C18 0.052(2) 0.0321(18) 0.049(2) 0.0111(16) 0.0088(18) -0.0099(16) C19 0.0166(13) 0.0304(15) 0.0289(14) 0.0026(12) 0.0051(11) 0.0028(12) C20 0.0155(13) 0.0281(15) 0.0296(15) -0.0006(12) 0.0059(11) -0.0017(11) C21 0.0189(13) 0.0250(14) 0.0299(15) 0.0019(12) 0.0092(11) -0.0011(11) C22 0.0198(14) 0.0284(15) 0.0297(15) -0.0019(12) 0.0084(12) 0.0010(11) C23 0.0186(14) 0.0256(15) 0.0317(16) 0.0032(12) 0.0066(12) 0.0050(11) C24 0.0315(17) 0.0440(19) 0.0294(16) 0.0053(14) -0.0002(13) 0.0012(15) C25 0.0294(16) 0.0295(16) 0.0365(17) -0.0027(13) 0.0093(14) -0.0064(13) C26 0.0312(17) 0.0335(17) 0.0337(17) 0.0072(13) 0.0123(14) 0.0006(13) C27 0.0344(18) 0.0341(17) 0.0369(17) -0.0066(14) 0.0116(14) 0.0042(14) C28 0.0354(19) 0.0316(17) 0.048(2) 0.0112(15) 0.0161(16) 0.0091(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2485(6) 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 . 1.963(2) yes Ti1 . N2 . 2.215(2) yes Ti1 . N3 . 2.180(3) yes Ti1 . N4 . 2.178(2) yes Ti1 . C19 . 2.434(3) yes Ti1 . C20 . 2.375(3) yes Ti1 . C21 . 2.381(3) yes Ti1 . C22 . 2.424(3) yes Ti1 . C23 . 2.455(3) yes Ti1 . H1 . 1.56(4) no N1 . N2 . 1.441(3) yes N1 . Si1 . 1.722(3) yes N2 . C1 . 1.467(4) yes N2 . C2 . 1.476(4) yes N3 . C11 . 1.322(4) yes N3 . C13 . 1.458(4) yes N4 . C11 . 1.329(4) yes N4 . C16 . 1.467(4) yes Si1 . C3 . 1.886(3) yes Si1 . H2 . 1.42(4) no Si1 . H3 . 1.40(4) no F1 . C9 . 1.345(7) yes F2 . C9 . 1.263(6) yes F3 . C9 . 1.297(7) yes F4 . C10 . 1.280(8) yes F5 . C10 . 1.353(7) yes F6 . C10 . 1.311(7) yes F11 . C9 . 1.300(7) yes F21 . C9 . 1.321(6) yes F31 . C9 . 1.281(7) yes F41 . C10 . 1.338(7) yes F51 . C10 . 1.281(7) yes F61 . C10 . 1.360(6) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . C4 . 1.392(5) yes C3 . C8 . 1.395(5) yes C4 . C5 . 1.388(5) yes C4 . H41 . 0.950 no C5 . C6 . 1.390(5) yes C5 . C9 . 1.499(5) yes C6 . C7 . 1.381(5) yes C6 . H61 . 0.950 no C7 . C8 . 1.385(5) yes C7 . C10 . 1.494(5) yes C8 . H81 . 0.950 no C11 . C12 . 1.518(5) yes C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . C14 . 1.523(5) yes C13 . C15 . 1.528(5) yes C13 . H131 . 0.950 no C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C15 . H151 . 0.950 no C15 . H152 . 0.950 no C15 . H153 . 0.950 no C16 . C17 . 1.522(5) yes C16 . C18 . 1.531(5) yes C16 . H161 . 0.950 no C17 . H171 . 0.950 no C17 . H172 . 0.950 no C17 . H173 . 0.950 no C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no C19 . C20 . 1.420(4) yes C19 . C23 . 1.407(4) yes C19 . C24 . 1.507(4) yes C20 . C21 . 1.417(4) yes C20 . C25 . 1.505(4) yes C21 . C22 . 1.417(4) yes C21 . C26 . 1.509(4) yes C22 . C23 . 1.416(4) yes C22 . C27 . 1.502(4) yes C23 . C28 . 1.502(4) yes C24 . H241 . 0.950 no C24 . H242 . 0.950 no C24 . H243 . 0.950 no C25 . H251 . 0.950 no C25 . H252 . 0.950 no C25 . H253 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no C27 . H271 . 0.950 no C27 . H272 . 0.950 no C27 . H273 . 0.950 no C28 . H281 . 0.950 no C28 . H282 . 0.950 no C28 . H283 . 0.950 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 N1 . Ti1 . N2 . 39.77(10) yes N1 . Ti1 . N3 . 129.65(10) yes N2 . Ti1 . N3 . 90.65(10) yes N1 . Ti1 . N4 . 100.75(10) yes N2 . Ti1 . N4 . 88.37(10) yes N3 . Ti1 . N4 . 60.73(9) yes N1 . Ti1 . C19 . 89.93(10) yes N2 . Ti1 . C19 . 129.66(10) yes N3 . Ti1 . C19 . 137.90(10) yes N4 . Ti1 . C19 . 103.33(10) yes N1 . Ti1 . C20 . 89.53(10) yes N2 . Ti1 . C20 . 122.41(10) yes N3 . Ti1 . C20 . 137.31(10) yes N4 . Ti1 . C20 . 136.90(10) yes C19 . Ti1 . C20 . 34.32(10) yes N1 . Ti1 . C21 . 120.51(10) yes N2 . Ti1 . C21 . 139.15(10) yes N3 . Ti1 . C21 . 102.69(10) yes N4 . Ti1 . C21 . 131.87(10) yes C19 . Ti1 . C21 . 56.94(10) yes N1 . Ti1 . C22 . 144.54(10) yes N2 . Ti1 . C22 . 170.44(10) yes N3 . Ti1 . C22 . 85.81(10) yes N4 . Ti1 . C22 . 97.59(10) yes C19 . Ti1 . C22 . 56.24(10) yes N1 . Ti1 . C23 . 119.83(10) yes N2 . Ti1 . C23 . 155.51(10) yes N3 . Ti1 . C23 . 104.62(10) yes N4 . Ti1 . C23 . 82.83(10) yes C19 . Ti1 . C23 . 33.44(10) yes N1 . Ti1 . H1 . 94.4(14) no N2 . Ti1 . H1 . 78.3(14) no N3 . Ti1 . H1 . 78.9(14) no N4 . Ti1 . H1 . 137.3(14) no C19 . Ti1 . H1 . 116.4(14) no C20 . Ti1 . C21 . 34.67(10) yes C20 . Ti1 . C22 . 56.97(10) yes C21 . Ti1 . C22 . 34.28(10) yes C20 . Ti1 . C23 . 56.42(10) yes C21 . Ti1 . C23 . 56.50(10) yes C22 . Ti1 . C23 . 33.72(10) yes C20 . Ti1 . H1 . 82.2(14) no C21 . Ti1 . H1 . 67.0(14) no C22 . Ti1 . H1 . 92.3(14) no C23 . Ti1 . H1 . 122.9(14) no Ti1 . N1 . N2 . 79.59(15) yes Ti1 . N1 . Si1 . 152.92(15) yes N2 . N1 . Si1 . 121.19(19) yes N1 . N2 . Ti1 . 60.64(13) yes N1 . N2 . C1 . 113.4(2) yes Ti1 . N2 . C1 . 123.4(2) yes N1 . N2 . C2 . 114.5(2) yes Ti1 . N2 . C2 . 124.4(2) yes C1 . N2 . C2 . 109.3(2) yes Ti1 . N3 . C11 . 92.47(19) yes Ti1 . N3 . C13 . 140.4(2) yes C11 . N3 . C13 . 121.3(3) yes Ti1 . N4 . C11 . 92.35(18) yes Ti1 . N4 . C16 . 141.9(2) yes C11 . N4 . C16 . 121.7(3) yes N1 . Si1 . C3 . 112.40(13) yes N1 . Si1 . H2 . 114.0(15) no C3 . Si1 . H2 . 103.1(15) no N1 . Si1 . H3 . 106.7(16) no C3 . Si1 . H3 . 107.7(16) no H2 . Si1 . H3 . 113(2) no N2 . C1 . H11 . 109.2 no N2 . C1 . H12 . 109.5 no H11 . C1 . H12 . 109.6 no N2 . C1 . H13 . 109.5 no H11 . C1 . H13 . 109.6 no H12 . C1 . H13 . 109.5 no N2 . C2 . H21 . 109.4 no N2 . C2 . H22 . 109.6 no H21 . C2 . H22 . 109.5 no N2 . C2 . H23 . 109.4 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no Si1 . C3 . C4 . 121.4(2) yes Si1 . C3 . C8 . 121.0(2) yes C4 . C3 . C8 . 117.6(3) yes C3 . C4 . C5 . 121.1(3) yes C3 . C4 . H41 . 119.3 no C5 . C4 . H41 . 119.5 no C4 . C5 . C6 . 120.3(3) yes C4 . C5 . C9 . 119.7(3) yes C6 . C5 . C9 . 119.9(3) yes C5 . C6 . C7 . 119.1(3) yes C5 . C6 . H61 . 120.7 no C7 . C6 . H61 . 120.2 no C6 . C7 . C8 . 120.4(3) yes C6 . C7 . C10 . 119.4(3) yes C8 . C7 . C10 . 120.2(3) yes C3 . C8 . C7 . 121.4(3) yes C3 . C8 . H81 . 119.3 no C7 . C8 . H81 . 119.3 no C5 . C9 . F1 . 111.3(4) yes C5 . C9 . F21 . 111.6(4) yes F1 . C9 . F21 . 135.1(5) yes C5 . C9 . F11 . 113.6(4) yes F1 . C9 . F11 . 41.7(5) yes F21 . C9 . F11 . 107.2(7) yes C5 . C9 . F3 . 112.5(4) yes F1 . C9 . F3 . 98.4(6) yes F21 . C9 . F3 . 76.6(7) yes F11 . C9 . F3 . 127.7(6) yes C5 . C9 . F31 . 113.9(4) yes F1 . C9 . F31 . 71.0(6) yes F21 . C9 . F31 . 102.5(6) yes F11 . C9 . F31 . 107.2(7) yes F3 . C9 . F31 . 28.9(6) yes C5 . C9 . F2 . 113.8(4) yes F1 . C9 . F2 . 102.9(7) yes F21 . C9 . F2 . 46.8(5) yes F11 . C9 . F2 . 63.7(7) yes F3 . C9 . F2 . 116.2(7) yes F31 . C9 . F2 . 130.5(5) yes C7 . C10 . F61 . 111.5(3) yes C7 . C10 . F5 . 110.4(4) yes F61 . C10 . F5 . 131.9(5) yes C7 . C10 . F41 . 112.4(4) yes F61 . C10 . F41 . 100.3(6) yes F5 . C10 . F41 . 84.7(6) yes C7 . C10 . F6 . 113.4(4) yes F61 . C10 . F6 . 39.5(5) yes F5 . C10 . F6 . 101.3(6) yes F41 . C10 . F6 . 127.9(6) yes C7 . C10 . F51 . 114.4(4) yes F61 . C10 . F51 . 107.3(6) yes F5 . C10 . F51 . 31.4(5) yes F41 . C10 . F51 . 110.0(6) yes F6 . C10 . F51 . 71.2(7) yes C7 . C10 . F4 . 114.4(4) yes F61 . C10 . F4 . 79.1(6) yes F5 . C10 . F4 . 104.0(6) yes F41 . C10 . F4 . 22.4(6) yes F6 . C10 . F4 . 112.0(7) yes F51 . C10 . F4 . 123.5(6) yes N4 . C11 . N3 . 112.4(3) yes N4 . C11 . C12 . 123.7(3) yes N3 . C11 . C12 . 123.9(3) yes C11 . C12 . H121 . 109.8 no C11 . C12 . H122 . 109.3 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 109.3 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no N3 . C13 . C14 . 111.5(3) yes N3 . C13 . C15 . 112.1(3) yes C14 . C13 . C15 . 109.0(3) yes N3 . C13 . H131 . 107.9 no C14 . C13 . H131 . 108.0 no C15 . C13 . H131 . 108.2 no C13 . C14 . H141 . 109.7 no C13 . C14 . H142 . 109.4 no H141 . C14 . H142 . 109.5 no C13 . C14 . H143 . 109.4 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no C13 . C15 . H151 . 109.5 no C13 . C15 . H152 . 109.2 no H151 . C15 . H152 . 109.5 no C13 . C15 . H153 . 109.6 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 109.5 no N4 . C16 . C17 . 109.9(3) yes N4 . C16 . C18 . 113.9(3) yes C17 . C16 . C18 . 109.5(3) yes N4 . C16 . H161 . 107.8 no C17 . C16 . H161 . 107.8 no C18 . C16 . H161 . 107.8 no C16 . C17 . H171 . 109.6 no C16 . C17 . H172 . 109.4 no H171 . C17 . H172 . 109.5 no C16 . C17 . H173 . 109.4 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no C16 . C18 . H181 . 109.5 no C16 . C18 . H182 . 109.5 no H181 . C18 . H182 . 109.5 no C16 . C18 . H183 . 109.4 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no Ti1 . C19 . C20 . 70.57(16) yes Ti1 . C19 . C23 . 74.13(17) yes C20 . C19 . C23 . 107.8(3) yes Ti1 . C19 . C24 . 127.2(2) yes C20 . C19 . C24 . 126.4(3) yes C23 . C19 . C24 . 125.3(3) yes Ti1 . C20 . C19 . 75.11(16) yes Ti1 . C20 . C21 . 72.92(16) yes C19 . C20 . C21 . 108.1(3) yes Ti1 . C20 . C25 . 122.5(2) yes C19 . C20 . C25 . 127.5(3) yes C21 . C20 . C25 . 124.2(3) yes Ti1 . C21 . C20 . 72.42(16) yes Ti1 . C21 . C22 . 74.52(16) yes C20 . C21 . C22 . 107.8(3) yes Ti1 . C21 . C26 . 127.2(2) yes C20 . C21 . C26 . 124.9(3) yes C22 . C21 . C26 . 126.4(3) yes Ti1 . C22 . C21 . 71.20(16) yes Ti1 . C22 . C23 . 74.34(16) yes C21 . C22 . C23 . 107.9(3) yes Ti1 . C22 . C27 . 124.6(2) yes C21 . C22 . C27 . 127.8(3) yes C23 . C22 . C27 . 124.1(3) yes C22 . C23 . Ti1 . 71.94(16) yes C22 . C23 . C19 . 108.4(3) yes Ti1 . C23 . C19 . 72.43(16) yes C22 . C23 . C28 . 123.7(3) yes Ti1 . C23 . C28 . 128.6(2) yes C19 . C23 . C28 . 127.2(3) yes C19 . C24 . H241 . 109.6 no C19 . C24 . H242 . 109.5 no H241 . C24 . H242 . 109.5 no C19 . C24 . H243 . 109.2 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C20 . C25 . H251 . 116.6 no C20 . C25 . H252 . 116.9 no H251 . C25 . H252 . 109.5 no C20 . C25 . H253 . 104.0 no H251 . C25 . H253 . 104.0 no H252 . C25 . H253 . 104.0 no C21 . C26 . H261 . 109.4 no C21 . C26 . H262 . 109.4 no H261 . C26 . H262 . 109.5 no C21 . C26 . H263 . 109.7 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no C22 . C27 . H271 . 109.8 no C22 . C27 . H272 . 109.9 no H271 . C27 . H272 . 109.5 no C22 . C27 . H273 . 109.3 no H271 . C27 . H273 . 109.2 no H272 . C27 . H273 . 109.2 no C23 . C28 . H281 . 108.7 no C23 . C28 . H282 . 108.6 no H281 . C28 . H282 . 109.5 no C23 . C28 . H283 . 109.9 no H281 . C28 . H283 . 110.0 no H282 . C28 . H283 . 110.0 no #===end data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 849350' #TrackingRef '- Mountford Xray SI.CIF' # local code PJT18 _chemical_name_systematic ; Cp*Ti{MeC(NiPr)2}(H){N(NMe2)SiH2ArOMe} ; _chemical_melting_point ? _publ_section_exptl_refinement ; Si-H and Ti-H hydrogen atoms were located from Fourier maps and positionally and isotropically refined. C-bound H atoms were placed in calculated positions with reference to a Fourier difference map and refined in a riding model. ; _cell_length_a 8.57190(10) _cell_length_b 9.90560(10) _cell_length_c 18.2095(2) _cell_angle_alpha 80.3853(4) _cell_angle_beta 87.2553(4) _cell_angle_gamma 71.1128(5) _cell_volume 1442.34(3) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C27 H48 N4 O1 Si1 Ti1' _chemical_formula_moiety 'C27 H48 N4 O1 Si1 Ti1' _chemical_compound_source ? _chemical_formula_weight 520.69 _cell_measurement_reflns_used 6213 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description lath _exptl_crystal_colour yellow _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.500 _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 0.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 11441 _reflns_number_total 6545 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_theta_min 5.121 _diffrn_reflns_theta_max 27.490 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.665 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -12 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 1.75 _oxford_diffrn_Wilson_scale 0.66 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.34 _refine_diff_density_max 0.32 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 5792 _refine_ls_number_restraints 0 _refine_ls_number_parameters 319 _oxford_refine_ls_R_factor_ref 0.0353 _refine_ls_wR_factor_ref 0.0378 _refine_ls_goodness_of_fit_ref 1.0832 _refine_ls_shift/su_max 0.0007284 _refine_ls_shift/su_mean 0.0000467 # The values computed from all data _oxford_reflns_number_all 6545 _refine_ls_R_factor_all 0.0406 _refine_ls_wR_factor_all 0.0412 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5969 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_gt 0.0384 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none _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: 1.23 0.492 0.986 0.122 0.283 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; 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_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ti1 Ti 0.79009(2) 0.57560(2) 0.232446(12) 0.0174 1.0000 Uani . . . . . . . N1 N 0.84042(12) 0.66292(12) 0.31300(6) 0.0221 1.0000 Uani . . . . . . . N2 N 1.00456(12) 0.58547(12) 0.29051(6) 0.0218 1.0000 Uani . . . . . . . N3 N 0.85418(13) 0.71035(11) 0.13518(6) 0.0211 1.0000 Uani . . . . . . . N4 N 0.95394(12) 0.47211(11) 0.14762(6) 0.0205 1.0000 Uani . . . . . . . Si1 Si 0.80603(5) 0.73025(4) 0.39649(2) 0.0272 1.0000 Uani . . . . . . . O1 O 1.33117(12) 0.97892(11) 0.46204(6) 0.0328 1.0000 Uani . . . . . . . C1 C 1.10684(16) 0.67670(16) 0.26199(8) 0.0276 1.0000 Uani . . . . . . . C2 C 1.09626(17) 0.46865(15) 0.34882(8) 0.0284 1.0000 Uani . . . . . . . C3 C 0.95985(17) 0.81576(15) 0.41719(7) 0.0267 1.0000 Uani . . . . . . . C4 C 0.96073(18) 0.94998(15) 0.37952(8) 0.0302 1.0000 Uani . . . . . . . C5 C 1.08065(17) 1.01080(15) 0.39282(8) 0.0286 1.0000 Uani . . . . . . . C6 C 1.20375(16) 0.93410(15) 0.44532(7) 0.0258 1.0000 Uani . . . . . . . C7 C 1.20471(18) 0.80108(16) 0.48438(8) 0.0294 1.0000 Uani . . . . . . . C8 C 1.08415(18) 0.74332(16) 0.47066(8) 0.0294 1.0000 Uani . . . . . . . C9 C 1.3411(2) 1.11146(17) 0.42238(9) 0.0367 1.0000 Uani . . . . . . . C10 C 0.97006(15) 0.59632(14) 0.11433(7) 0.0208 1.0000 Uani . . . . . . . C11 C 1.10806(17) 0.60680(16) 0.06099(8) 0.0287 1.0000 Uani . . . . . . . C12 C 0.85665(17) 0.85794(14) 0.10913(8) 0.0260 1.0000 Uani . . . . . . . C13 C 0.74962(19) 0.96022(15) 0.15929(9) 0.0329 1.0000 Uani . . . . . . . C14 C 0.7991(2) 0.91491(17) 0.02812(9) 0.0364 1.0000 Uani . . . . . . . C15 C 1.07959(15) 0.33434(14) 0.13910(7) 0.0241 1.0000 Uani . . . . . . . C16 C 1.00492(18) 0.21241(15) 0.15325(9) 0.0315 1.0000 Uani . . . . . . . C17 C 1.22768(18) 0.29687(16) 0.19125(9) 0.0332 1.0000 Uani . . . . . . . C18 C 0.58786(14) 0.45330(14) 0.25247(7) 0.0216 1.0000 Uani . . . . . . . C19 C 0.54245(14) 0.56711(14) 0.29563(7) 0.0220 1.0000 Uani . . . . . . . C20 C 0.49898(15) 0.70083(14) 0.24625(8) 0.0244 1.0000 Uani . . . . . . . C21 C 0.51823(15) 0.66925(14) 0.17283(8) 0.0248 1.0000 Uani . . . . . . . C22 C 0.57360(15) 0.51714(14) 0.17618(7) 0.0224 1.0000 Uani . . . . . . . C23 C 0.61730(17) 0.29657(14) 0.28332(8) 0.0278 1.0000 Uani . . . . . . . C24 C 0.53012(17) 0.54455(17) 0.37914(8) 0.0301 1.0000 Uani . . . . . . . C25 C 0.42333(17) 0.84850(15) 0.26762(9) 0.0329 1.0000 Uani . . . . . . . C26 C 0.46720(19) 0.77473(17) 0.10218(9) 0.0370 1.0000 Uani . . . . . . . C27 C 0.59574(17) 0.44174(17) 0.10970(8) 0.0307 1.0000 Uani . . . . . . . H1 H 0.856(2) 0.409(2) 0.2752(11) 0.040(5) 1.0000 Uiso . . . . . . . H2 H 0.648(3) 0.832(2) 0.3905(11) 0.045(5) 1.0000 Uiso . . . . . . . H3 H 0.810(3) 0.621(2) 0.4573(12) 0.050(6) 1.0000 Uiso . . . . . . . H11 H 1.0477 0.7520 0.2243 0.0342 1.0000 Uiso R . . . . . . H12 H 1.1330 0.7174 0.3015 0.0342 1.0000 Uiso R . . . . . . H13 H 1.2057 0.6197 0.2418 0.0342 1.0000 Uiso R . . . . . . H21 H 1.0302 0.4098 0.3672 0.0351 1.0000 Uiso R . . . . . . H22 H 1.1224 0.5093 0.3884 0.0351 1.0000 Uiso R . . . . . . H23 H 1.1951 0.4116 0.3286 0.0351 1.0000 Uiso R . . . . . . H41 H 0.8770 1.0017 0.3435 0.0366 1.0000 Uiso R . . . . . . H51 H 1.0784 1.1029 0.3668 0.0350 1.0000 Uiso R . . . . . . H71 H 1.2882 0.7501 0.5206 0.0351 1.0000 Uiso R . . . . . . H81 H 1.0857 0.6524 0.4980 0.0361 1.0000 Uiso R . . . . . . H91 H 1.4343 1.1300 0.4392 0.0458 1.0000 Uiso R . . . . . . H92 H 1.2439 1.1875 0.4304 0.0458 1.0000 Uiso R . . . . . . H93 H 1.3519 1.1057 0.3707 0.0458 1.0000 Uiso R . . . . . . H111 H 1.0995 0.7053 0.0451 0.0359 1.0000 Uiso R . . . . . . H112 H 1.2117 0.5568 0.0848 0.0359 1.0000 Uiso R . . . . . . H113 H 1.1000 0.5642 0.0189 0.0359 1.0000 Uiso R . . . . . . H121 H 0.9668 0.8581 0.1127 0.0317 1.0000 Uiso R . . . . . . H131 H 0.7854 0.9255 0.2095 0.0408 1.0000 Uiso R . . . . . . H132 H 0.7583 1.0541 0.1446 0.0408 1.0000 Uiso R . . . . . . H133 H 0.6381 0.9644 0.1550 0.0408 1.0000 Uiso R . . . . . . H141 H 0.8659 0.8518 -0.0033 0.0453 1.0000 Uiso R . . . . . . H142 H 0.8077 1.0089 0.0136 0.0453 1.0000 Uiso R . . . . . . H143 H 0.6875 0.9191 0.0239 0.0453 1.0000 Uiso R . . . . . . H151 H 1.1179 0.3411 0.0892 0.0295 1.0000 Uiso R . . . . . . H161 H 0.9131 0.2346 0.1209 0.0395 1.0000 Uiso R . . . . . . H162 H 1.0851 0.1247 0.1444 0.0395 1.0000 Uiso R . . . . . . H163 H 0.9697 0.2020 0.2035 0.0395 1.0000 Uiso R . . . . . . H171 H 1.2757 0.3721 0.1826 0.0416 1.0000 Uiso R . . . . . . H172 H 1.3072 0.2089 0.1823 0.0416 1.0000 Uiso R . . . . . . H173 H 1.1917 0.2862 0.2414 0.0416 1.0000 Uiso R . . . . . . H231 H 0.6387 0.2779 0.3354 0.0354 1.0000 Uiso R . . . . . . H232 H 0.7066 0.2358 0.2590 0.0354 1.0000 Uiso R . . . . . . H233 H 0.5207 0.2738 0.2752 0.0354 1.0000 Uiso R . . . . . . H241 H 0.4982 0.6354 0.3959 0.0376 1.0000 Uiso R . . . . . . H242 H 0.6342 0.4861 0.4002 0.0376 1.0000 Uiso R . . . . . . H243 H 0.4503 0.4978 0.3941 0.0376 1.0000 Uiso R . . . . . . H251 H 0.4953 0.9041 0.2543 0.0404 1.0000 Uiso R . . . . . . H252 H 0.4046 0.8399 0.3198 0.0404 1.0000 Uiso R . . . . . . H253 H 0.3213 0.8957 0.2420 0.0404 1.0000 Uiso R . . . . . . H261 H 0.4327 0.8709 0.1125 0.0447 1.0000 Uiso R . . . . . . H262 H 0.5563 0.7621 0.0681 0.0447 1.0000 Uiso R . . . . . . H263 H 0.3778 0.7586 0.0802 0.0447 1.0000 Uiso R . . . . . . H271 H 0.6822 0.4613 0.0798 0.0384 1.0000 Uiso R . . . . . . H272 H 0.6240 0.3407 0.1265 0.0384 1.0000 Uiso R . . . . . . H273 H 0.4964 0.4747 0.0815 0.0384 1.0000 Uiso 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 0.01385(10) 0.01872(11) 0.01936(11) -0.00242(8) 0.00034(7) -0.00527(8) N1 0.0162(5) 0.0254(5) 0.0241(5) -0.0066(4) 0.0012(4) -0.0048(4) N2 0.0155(5) 0.0263(5) 0.0234(5) -0.0056(4) -0.0004(4) -0.0054(4) N3 0.0204(5) 0.0206(5) 0.0222(5) -0.0010(4) 0.0010(4) -0.0076(4) N4 0.0177(5) 0.0212(5) 0.0222(5) -0.0040(4) 0.0017(4) -0.0055(4) Si1 0.02574(18) 0.0321(2) 0.02678(18) -0.01183(15) 0.00409(14) -0.01027(15) O1 0.0282(5) 0.0331(5) 0.0366(5) -0.0002(4) -0.0055(4) -0.0109(4) C1 0.0216(6) 0.0378(7) 0.0287(6) -0.0088(5) 0.0018(5) -0.0152(5) C2 0.0237(6) 0.0315(7) 0.0260(6) -0.0053(5) -0.0056(5) -0.0023(5) C3 0.0273(6) 0.0283(6) 0.0258(6) -0.0114(5) 0.0022(5) -0.0073(5) C4 0.0300(7) 0.0264(6) 0.0318(7) -0.0086(5) -0.0044(5) -0.0034(5) C5 0.0304(7) 0.0239(6) 0.0291(7) -0.0045(5) -0.0011(5) -0.0050(5) C6 0.0240(6) 0.0287(6) 0.0237(6) -0.0085(5) 0.0015(5) -0.0051(5) C7 0.0302(7) 0.0315(7) 0.0239(6) -0.0034(5) -0.0034(5) -0.0066(5) C8 0.0352(7) 0.0301(7) 0.0234(6) -0.0060(5) 0.0020(5) -0.0106(6) C9 0.0380(8) 0.0336(8) 0.0407(8) -0.0016(6) -0.0037(6) -0.0160(6) C10 0.0180(5) 0.0262(6) 0.0194(5) -0.0032(4) -0.0005(4) -0.0089(5) C11 0.0246(6) 0.0314(7) 0.0299(7) -0.0034(5) 0.0071(5) -0.0105(5) C12 0.0271(6) 0.0217(6) 0.0297(6) 0.0009(5) 0.0006(5) -0.0113(5) C13 0.0355(7) 0.0215(6) 0.0417(8) -0.0045(6) 0.0039(6) -0.0097(6) C14 0.0424(8) 0.0313(7) 0.0320(7) 0.0078(6) -0.0020(6) -0.0130(6) C15 0.0211(6) 0.0239(6) 0.0263(6) -0.0070(5) 0.0022(5) -0.0050(5) C16 0.0302(7) 0.0234(6) 0.0400(8) -0.0071(6) 0.0029(6) -0.0067(5) C17 0.0250(6) 0.0294(7) 0.0411(8) -0.0085(6) -0.0058(6) -0.0010(5) C18 0.0159(5) 0.0234(6) 0.0256(6) -0.0013(5) 0.0006(4) -0.0077(4) C19 0.0148(5) 0.0246(6) 0.0264(6) -0.0032(5) 0.0023(4) -0.0066(4) C20 0.0142(5) 0.0236(6) 0.0335(7) -0.0023(5) 0.0007(5) -0.0048(4) C21 0.0153(5) 0.0269(6) 0.0298(6) 0.0037(5) -0.0036(5) -0.0073(5) C22 0.0154(5) 0.0283(6) 0.0246(6) -0.0021(5) -0.0004(4) -0.0093(5) C23 0.0251(6) 0.0232(6) 0.0351(7) -0.0005(5) 0.0008(5) -0.0100(5) C24 0.0272(7) 0.0377(7) 0.0275(7) -0.0060(6) 0.0064(5) -0.0139(6) C25 0.0236(6) 0.0247(6) 0.0481(9) -0.0071(6) 0.0034(6) -0.0042(5) C26 0.0310(7) 0.0381(8) 0.0394(8) 0.0136(6) -0.0141(6) -0.0156(6) C27 0.0231(6) 0.0428(8) 0.0292(7) -0.0091(6) -0.0006(5) -0.0127(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.1901(14) 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 . 1.9525(11) yes Ti1 . N2 . 2.2009(10) yes Ti1 . N3 . 2.1937(10) yes Ti1 . N4 . 2.1905(10) yes Ti1 . C18 . 2.3994(12) yes Ti1 . C19 . 2.3846(12) yes Ti1 . C20 . 2.4226(12) yes Ti1 . C21 . 2.4446(12) yes Ti1 . C22 . 2.4300(12) yes Ti1 . H1 . 1.633(19) no N1 . N2 . 1.4446(14) yes N1 . Si1 . 1.7353(11) yes N2 . C1 . 1.4723(16) yes N2 . C2 . 1.4715(17) yes N3 . C10 . 1.3369(16) yes N3 . C12 . 1.4664(16) yes N4 . C10 . 1.3241(16) yes N4 . C15 . 1.4662(16) yes Si1 . C3 . 1.8643(14) yes Si1 . H2 . 1.40(2) no Si1 . H3 . 1.41(2) no O1 . C6 . 1.3688(17) yes O1 . C9 . 1.4151(18) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . C4 . 1.393(2) yes C3 . C8 . 1.403(2) yes C4 . C5 . 1.397(2) yes C4 . H41 . 0.950 no C5 . C6 . 1.3926(19) yes C5 . H51 . 0.950 no C6 . C7 . 1.387(2) yes C7 . C8 . 1.383(2) yes C7 . H71 . 0.950 no C8 . H81 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . C11 . 1.5130(17) yes C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 no C12 . C13 . 1.526(2) yes C12 . C14 . 1.533(2) yes C12 . H121 . 0.950 no C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C15 . C16 . 1.5217(19) yes C15 . C17 . 1.5310(19) yes C15 . H151 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no C17 . H171 . 0.950 no C17 . H172 . 0.950 no C17 . H173 . 0.950 no C18 . C19 . 1.4223(18) yes C18 . C22 . 1.4203(17) yes C18 . C23 . 1.5027(17) yes C19 . C20 . 1.4201(18) yes C19 . C24 . 1.5033(18) yes C20 . C21 . 1.414(2) yes C20 . C25 . 1.5044(19) yes C21 . C22 . 1.4172(19) yes C21 . C26 . 1.4990(18) yes C22 . C27 . 1.4992(19) yes C23 . H231 . 0.950 no C23 . H232 . 0.950 no C23 . H233 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.950 no C24 . H243 . 0.950 no C25 . H251 . 0.950 no C25 . H252 . 0.950 no C25 . H253 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no C27 . H271 . 0.950 no C27 . H272 . 0.950 no C27 . H273 . 0.950 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 N1 . Ti1 . N2 . 40.15(4) yes N1 . Ti1 . N3 . 100.67(4) yes N2 . Ti1 . N3 . 88.12(4) yes N1 . Ti1 . N4 . 129.22(4) yes N2 . Ti1 . N4 . 89.86(4) yes N3 . Ti1 . N4 . 60.55(4) yes N1 . Ti1 . C18 . 119.04(4) yes N2 . Ti1 . C18 . 138.57(4) yes N3 . Ti1 . C18 . 132.90(4) yes N4 . Ti1 . C18 . 104.64(4) yes N1 . Ti1 . C19 . 88.60(4) yes N2 . Ti1 . C19 . 122.42(4) yes N3 . Ti1 . C19 . 135.90(4) yes N4 . Ti1 . C19 . 139.08(4) yes C18 . Ti1 . C19 . 34.59(4) yes N1 . Ti1 . C20 . 89.88(4) yes N2 . Ti1 . C20 . 129.93(4) yes N3 . Ti1 . C20 . 102.06(4) yes N4 . Ti1 . C20 . 137.85(4) yes C18 . Ti1 . C20 . 57.10(4) yes N1 . Ti1 . C21 . 120.66(5) yes N2 . Ti1 . C21 . 156.40(4) yes N3 . Ti1 . C21 . 82.59(4) yes N4 . Ti1 . C21 . 104.12(4) yes C18 . Ti1 . C21 . 56.48(4) yes N1 . Ti1 . C22 . 144.16(4) yes N2 . Ti1 . C22 . 169.45(4) yes N3 . Ti1 . C22 . 98.73(4) yes N4 . Ti1 . C22 . 86.60(4) yes C18 . Ti1 . C22 . 34.20(4) yes N1 . Ti1 . H1 . 96.4(7) no N2 . Ti1 . H1 . 81.2(7) no N3 . Ti1 . H1 . 138.7(7) no N4 . Ti1 . H1 . 79.5(7) no C18 . Ti1 . H1 . 64.3(7) no C19 . Ti1 . C20 . 34.35(4) yes C19 . Ti1 . C21 . 56.46(4) yes C20 . Ti1 . C21 . 33.76(5) yes C19 . Ti1 . C22 . 56.92(4) yes C20 . Ti1 . C22 . 56.60(4) yes C21 . Ti1 . C22 . 33.80(4) yes C19 . Ti1 . H1 . 81.4(7) no C20 . Ti1 . H1 . 115.4(7) no C21 . Ti1 . H1 . 119.6(7) no C22 . Ti1 . H1 . 88.4(7) no Ti1 . N1 . N2 . 79.22(6) yes Ti1 . N1 . Si1 . 155.54(6) yes N2 . N1 . Si1 . 121.36(8) yes N1 . N2 . Ti1 . 60.63(5) yes N1 . N2 . C1 . 115.01(10) yes Ti1 . N2 . C1 . 125.17(8) yes N1 . N2 . C2 . 113.15(10) yes Ti1 . N2 . C2 . 122.44(8) yes C1 . N2 . C2 . 109.43(10) yes Ti1 . N3 . C10 . 91.84(7) yes Ti1 . N3 . C12 . 141.56(9) yes C10 . N3 . C12 . 121.15(11) yes Ti1 . N4 . C10 . 92.33(7) yes Ti1 . N4 . C15 . 140.05(8) yes C10 . N4 . C15 . 120.80(10) yes N1 . Si1 . C3 . 113.71(6) yes N1 . Si1 . H2 . 105.8(8) no C3 . Si1 . H2 . 110.3(8) no N1 . Si1 . H3 . 111.6(9) no C3 . Si1 . H3 . 106.5(9) no H2 . Si1 . H3 . 108.9(12) no C6 . O1 . C9 . 118.00(11) yes N2 . C1 . H11 . 109.4 no N2 . C1 . H12 . 109.4 no H11 . C1 . H12 . 109.5 no N2 . C1 . H13 . 109.5 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no N2 . C2 . H21 . 109.4 no N2 . C2 . H22 . 109.4 no H21 . C2 . H22 . 109.5 no N2 . C2 . H23 . 109.6 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no Si1 . C3 . C4 . 122.38(11) yes Si1 . C3 . C8 . 120.38(11) yes C4 . C3 . C8 . 117.20(13) yes C3 . C4 . C5 . 122.22(13) yes C3 . C4 . H41 . 118.8 no C5 . C4 . H41 . 119.0 no C4 . C5 . C6 . 118.77(13) yes C4 . C5 . H51 . 120.8 no C6 . C5 . H51 . 120.4 no C5 . C6 . O1 . 124.77(13) yes C5 . C6 . C7 . 120.26(13) yes O1 . C6 . C7 . 114.96(12) yes C6 . C7 . C8 . 119.99(13) yes C6 . C7 . H71 . 119.7 no C8 . C7 . H71 . 120.3 no C3 . C8 . C7 . 121.54(13) yes C3 . C8 . H81 . 119.3 no C7 . C8 . H81 . 119.2 no O1 . C9 . H91 . 109.6 no O1 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no O1 . C9 . H93 . 109.3 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N3 . C10 . N4 . 112.31(11) yes N3 . C10 . C11 . 124.18(11) yes N4 . C10 . C11 . 123.47(11) yes C10 . C11 . H111 . 110.0 no C10 . C11 . H112 . 109.9 no H111 . C11 . H112 . 109.5 no C10 . C11 . H113 . 109.1 no H111 . C11 . H113 . 109.2 no H112 . C11 . H113 . 109.2 no N3 . C12 . C13 . 110.01(11) yes N3 . C12 . C14 . 113.31(11) yes C13 . C12 . C14 . 109.29(12) yes N3 . C12 . H121 . 108.1 no C13 . C12 . H121 . 108.0 no C14 . C12 . H121 . 108.0 no C12 . C13 . H131 . 109.5 no C12 . C13 . H132 . 109.8 no H131 . C13 . H132 . 109.5 no C12 . C13 . H133 . 109.2 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no C12 . C14 . H141 . 109.5 no C12 . C14 . H142 . 109.7 no H141 . C14 . H142 . 109.5 no C12 . C14 . H143 . 109.2 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no N4 . C15 . C16 . 110.22(10) yes N4 . C15 . C17 . 112.77(11) yes C16 . C15 . C17 . 109.03(12) yes N4 . C15 . H151 . 108.3 no C16 . C15 . H151 . 108.1 no C17 . C15 . H151 . 108.2 no C15 . C16 . H161 . 109.6 no C15 . C16 . H162 . 109.7 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.1 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no C15 . C17 . H171 . 109.7 no C15 . C17 . H172 . 109.6 no H171 . C17 . H172 . 109.5 no C15 . C17 . H173 . 109.2 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no Ti1 . C18 . C19 . 72.14(7) yes Ti1 . C18 . C22 . 74.08(7) yes C19 . C18 . C22 . 107.66(11) yes Ti1 . C18 . C23 . 127.00(8) yes C19 . C18 . C23 . 124.74(12) yes C22 . C18 . C23 . 126.87(12) yes Ti1 . C19 . C18 . 73.28(7) yes Ti1 . C19 . C20 . 74.29(7) yes C18 . C19 . C20 . 108.36(11) yes Ti1 . C19 . C24 . 122.47(9) yes C18 . C19 . C24 . 124.10(12) yes C20 . C19 . C24 . 127.34(12) yes Ti1 . C20 . C19 . 71.36(7) yes Ti1 . C20 . C21 . 73.97(7) yes C19 . C20 . C21 . 107.47(11) yes Ti1 . C20 . C25 . 126.66(9) yes C19 . C20 . C25 . 126.21(13) yes C21 . C20 . C25 . 125.79(12) yes Ti1 . C21 . C20 . 72.27(7) yes Ti1 . C21 . C22 . 72.54(7) yes C20 . C21 . C22 . 108.72(11) yes Ti1 . C21 . C26 . 127.75(9) yes C20 . C21 . C26 . 126.92(13) yes C22 . C21 . C26 . 123.84(13) yes Ti1 . C22 . C18 . 71.72(7) yes Ti1 . C22 . C21 . 73.66(7) yes C18 . C22 . C21 . 107.79(11) yes Ti1 . C22 . C27 . 124.75(8) yes C18 . C22 . C27 . 127.44(12) yes C21 . C22 . C27 . 124.52(12) yes C18 . C23 . H231 . 111.0 no C18 . C23 . H232 . 111.3 no H231 . C23 . H232 . 109.5 no C18 . C23 . H233 . 108.3 no H231 . C23 . H233 . 108.3 no H232 . C23 . H233 . 108.3 no C19 . C24 . H241 . 109.5 no C19 . C24 . H242 . 109.4 no H241 . C24 . H242 . 109.5 no C19 . C24 . H243 . 109.5 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C20 . C25 . H251 . 109.8 no C20 . C25 . H252 . 109.8 no H251 . C25 . H252 . 109.5 no C20 . C25 . H253 . 109.3 no H251 . C25 . H253 . 109.2 no H252 . C25 . H253 . 109.3 no C21 . C26 . H261 . 110.1 no C21 . C26 . H262 . 110.3 no H261 . C26 . H262 . 109.5 no C21 . C26 . H263 . 109.1 no H261 . C26 . H263 . 108.9 no H262 . C26 . H263 . 108.9 no C22 . C27 . H271 . 109.2 no C22 . C27 . H272 . 108.7 no H271 . C27 . H272 . 109.5 no C22 . C27 . H273 . 109.9 no H271 . C27 . H273 . 109.7 no H272 . C27 . H273 . 109.7 no #===end data_compound_11 _database_code_depnum_ccdc_archive 'CCDC 849351' #TrackingRef '- Mountford Xray SI.CIF' #local code PJT13 _chemical_name_systematic ; Cp*Ti{N(NMe2)SiH(Ph)2N(iPr)CMeNiPr}Cl2 ; _chemical_melting_point ? _publ_section_exptl_refinement ; Si-H hydrogen atoms were located from Fourier maps and positionally and isotropically refined. C-bound H atoms were placed in calculated positions with reference to a Fourier difference map and refined in a riding model. ; _cell_length_a 11.5517(2) _cell_length_b 14.3261(2) _cell_length_c 18.0286(3) _cell_angle_alpha 90 _cell_angle_beta 97.201(1) _cell_angle_gamma 90 _cell_volume 2960.0(1) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C26 H44 Cl2 N4 Si1 Ti1' _chemical_formula_moiety 'C26 H44 Cl2 N4 Si1 Ti1' _chemical_compound_source ? _chemical_formula_weight 559.55 _cell_measurement_reflns_used 6856 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 13030 _reflns_number_total 6704 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_min 5.255 _diffrn_reflns_theta_max 27.451 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.627 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 2.64 _oxford_diffrn_Wilson_scale 7.01 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.44 _refine_diff_density_max 0.92 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 4902 _refine_ls_number_restraints 108 _refine_ls_number_parameters 311 _oxford_refine_ls_R_factor_ref 0.0557 _refine_ls_wR_factor_ref 0.0598 _refine_ls_goodness_of_fit_ref 1.0572 _refine_ls_shift/su_max 0.000847 # The values computed from all data _oxford_reflns_number_all 6704 _refine_ls_R_factor_all 0.0785 _refine_ls_wR_factor_all 0.0743 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5335 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_gt 0.0624 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _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: 1.68 1.71 1.59 0.532 0.364 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # 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_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ti1 Ti 0.86954(4) 0.23543(3) 0.67917(3) 0.0270 1.0000 Uani . . . . . . . Cl1 Cl 0.77944(7) 0.20146(6) 0.78709(4) 0.0436 1.0000 Uani . . . . . . . Cl2 Cl 0.84607(7) 0.39551(5) 0.68063(5) 0.0461 1.0000 Uani . . . . . . . N1 N 1.0359(2) 0.22443(15) 0.67851(12) 0.0278 1.0000 Uani . . . . . . . N2 N 1.0238(2) 0.22784(15) 0.75510(12) 0.0285 1.0000 Uani D . . . . . . N3 N 1.2571(2) 0.32689(16) 0.66426(14) 0.0333 1.0000 Uani D . . . . . . N4 N 1.3253(2) 0.23097(16) 0.75976(13) 0.0320 1.0000 Uani D . . . . . . Si1 Si 1.16107(6) 0.23619(5) 0.63360(4) 0.0273 1.0000 Uani . . . . . . . C1 C 1.0687(3) 0.3109(2) 0.79770(17) 0.0369 1.0000 Uani D . . . . . . C2 C 1.0533(3) 0.1410(2) 0.79707(17) 0.0369 1.0000 Uani D . . . . . . C3 C 1.2366(2) 0.12392(18) 0.61597(15) 0.0286 1.0000 Uani D . . . . . . C4 C 1.2966(2) 0.1206(2) 0.55355(16) 0.0353 1.0000 Uani D . . . . . . C5 C 1.3487(2) 0.0380(2) 0.53282(18) 0.0431 1.0000 Uani D . . . . . . C6 C 1.3399(2) -0.0421(2) 0.57350(18) 0.0414 1.0000 Uani D . . . . . . C7 C 1.2800(2) -0.0406(2) 0.63553(18) 0.0416 1.0000 Uani D . . . . . . C8 C 1.2292(2) 0.0414(2) 0.65616(16) 0.0358 1.0000 Uani D . . . . . . C9 C 1.3423(3) 0.3063(2) 0.72366(16) 0.0337 1.0000 Uani D . . . . . . C10 C 1.4454(3) 0.3709(2) 0.7400(2) 0.0500 1.0000 Uani D . . . . . . C11 C 1.4126(3) 0.1997(2) 0.82074(17) 0.0393 1.0000 Uani D . . . . . . C12 C 1.4075(3) 0.0940(2) 0.8270(2) 0.0519 1.0000 Uani D . . . . . . C13 C 1.3900(4) 0.2457(3) 0.89359(19) 0.0569 1.0000 Uani D . . . . . . C14 C 1.2506(3) 0.4209(2) 0.62846(19) 0.0411 1.0000 Uani D . . . . . . C15 C 1.3011(4) 0.4204(3) 0.5547(2) 0.0615 1.0000 Uani D . . . . . . C16 C 1.1262(3) 0.4592(2) 0.6184(2) 0.0493 1.0000 Uani D . . . . . . C17 C 0.8555(3) 0.1525(3) 0.5651(2) 0.0509 1.0000 Uani D . . . . . . C18 C 0.7851(4) 0.1071(2) 0.6155(2) 0.0552 1.0000 Uani D . . . . . . C19 C 0.6903(3) 0.1658(3) 0.6217(2) 0.0544 1.0000 Uani D . . . . . . C20 C 0.7026(3) 0.2447(3) 0.5830(2) 0.0541 1.0000 Uani D . . . . . . C21 C 0.8031(4) 0.2391(2) 0.54840(17) 0.0498 1.0000 Uani D . . . . . . C22 C 0.9509(4) 0.1047(3) 0.5312(3) 0.0715 1.0000 Uani D . . . . . . C23 C 0.8092(5) 0.0114(3) 0.6486(3) 0.0852 1.0000 Uani D . . . . . . C24 C 0.5860(4) 0.1373(4) 0.6617(3) 0.0861 1.0000 Uani D . . . . . . C25 C 0.6171(5) 0.3252(4) 0.5728(3) 0.0838 1.0000 Uani D . . . . . . C26 C 0.8475(5) 0.3104(3) 0.4961(2) 0.0723 1.0000 Uani D . . . . . . H1 H 1.108(3) 0.267(2) 0.5628(18) 0.038(9) 1.0000 Uiso . . . . . . . H11 H 1.0482 0.3654 0.7690 0.0470 1.0000 Uiso DR . . . . . . H12 H 1.0354 0.3139 0.8432 0.0470 1.0000 Uiso DR . . . . . . H13 H 1.1512 0.3070 0.8083 0.0470 1.0000 Uiso DR . . . . . . H21 H 1.1357 0.1354 0.8077 0.0459 1.0000 Uiso DR . . . . . . H22 H 1.0233 0.0892 0.7679 0.0459 1.0000 Uiso DR . . . . . . H23 H 1.0198 0.1423 0.8426 0.0459 1.0000 Uiso DR . . . . . . H41 H 1.3019 0.1754 0.5245 0.0435 1.0000 Uiso DR . . . . . . H51 H 1.3902 0.0376 0.4906 0.0512 1.0000 Uiso DR . . . . . . H61 H 1.3747 -0.0983 0.5591 0.0510 1.0000 Uiso DR . . . . . . H71 H 1.2732 -0.0960 0.6637 0.0507 1.0000 Uiso DR . . . . . . H81 H 1.1891 0.0420 0.6990 0.0436 1.0000 Uiso DR . . . . . . H101 H 1.4380 0.4215 0.7056 0.0618 1.0000 Uiso DR . . . . . . H102 H 1.5154 0.3378 0.7355 0.0618 1.0000 Uiso DR . . . . . . H103 H 1.4475 0.3943 0.7895 0.0618 1.0000 Uiso DR . . . . . . H111 H 1.4879 0.2174 0.8098 0.0485 1.0000 Uiso DR . . . . . . H121 H 1.4226 0.0663 0.7813 0.0640 1.0000 Uiso DR . . . . . . H122 H 1.3321 0.0762 0.8375 0.0640 1.0000 Uiso DR . . . . . . H123 H 1.4644 0.0735 0.8663 0.0640 1.0000 Uiso DR . . . . . . H131 H 1.4468 0.2258 0.9331 0.0707 1.0000 Uiso DR . . . . . . H132 H 1.3939 0.3116 0.8886 0.0707 1.0000 Uiso DR . . . . . . H133 H 1.3145 0.2284 0.9044 0.0707 1.0000 Uiso DR . . . . . . H141 H 1.2972 0.4624 0.6607 0.0512 1.0000 Uiso DR . . . . . . H151 H 1.2538 0.3806 0.5213 0.0782 1.0000 Uiso DR . . . . . . H152 H 1.3788 0.3973 0.5616 0.0782 1.0000 Uiso DR . . . . . . H153 H 1.3004 0.4816 0.5344 0.0782 1.0000 Uiso DR . . . . . . H161 H 1.0962 0.4609 0.6651 0.0612 1.0000 Uiso DR . . . . . . H162 H 1.1256 0.5204 0.5981 0.0612 1.0000 Uiso DR . . . . . . H163 H 1.0790 0.4194 0.5850 0.0612 1.0000 Uiso DR . . . . . . H221 H 1.0090 0.0835 0.5694 0.1018 1.0000 Uiso DR . . . . . . H222 H 0.9202 0.0530 0.5020 0.1018 1.0000 Uiso DR . . . . . . H223 H 0.9844 0.1480 0.5001 0.1018 1.0000 Uiso DR . . . . . . H231 H 0.7521 -0.0041 0.6802 0.1086 1.0000 Uiso DR . . . . . . H232 H 0.8844 0.0110 0.6769 0.1086 1.0000 Uiso DR . . . . . . H233 H 0.8070 -0.0331 0.6094 0.1086 1.0000 Uiso DR . . . . . . H241 H 0.6120 0.1234 0.7126 0.1131 1.0000 Uiso DR . . . . . . H242 H 0.5493 0.0838 0.6381 0.1131 1.0000 Uiso DR . . . . . . H243 H 0.5319 0.1875 0.6591 0.1131 1.0000 Uiso DR . . . . . . H251 H 0.6472 0.3721 0.5432 0.1086 1.0000 Uiso DR . . . . . . H252 H 0.6063 0.3505 0.6202 0.1086 1.0000 Uiso DR . . . . . . H253 H 0.5443 0.3038 0.5484 0.1086 1.0000 Uiso DR . . . . . . H261 H 0.8469 0.2840 0.4477 0.0953 1.0000 Uiso DR . . . . . . H262 H 0.7985 0.3638 0.4932 0.0953 1.0000 Uiso DR . . . . . . H263 H 0.9249 0.3281 0.5150 0.0953 1.0000 Uiso DR . . . . . . 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 0.0310(2) 0.0202(2) 0.0301(3) -0.00168(18) 0.00558(18) 0.00233(18) Cl1 0.0387(4) 0.0598(5) 0.0345(4) -0.0050(3) 0.0127(3) -0.0076(3) Cl2 0.0498(4) 0.0222(3) 0.0678(5) -0.0045(3) 0.0131(4) 0.0068(3) N1 0.0347(11) 0.0228(10) 0.0261(11) -0.0016(8) 0.0050(9) 0.0010(9) N2 0.0346(12) 0.0271(11) 0.0246(11) -0.0010(8) 0.0064(9) -0.0045(9) N3 0.0413(13) 0.0226(11) 0.0376(13) 0.0035(9) 0.0111(10) -0.0004(9) N4 0.0356(12) 0.0289(11) 0.0320(12) -0.0029(9) 0.0058(9) -0.0016(9) Si1 0.0345(4) 0.0218(3) 0.0263(4) 0.0009(3) 0.0074(3) 0.0027(3) C1 0.0458(16) 0.0353(15) 0.0307(14) -0.0107(12) 0.0096(12) -0.0046(12) C2 0.0403(15) 0.0365(15) 0.0342(15) 0.0073(12) 0.0057(12) -0.0007(12) C3 0.0297(12) 0.0265(13) 0.0289(13) -0.0034(10) 0.0007(10) 0.0025(10) C4 0.0353(14) 0.0375(15) 0.0336(15) -0.0040(12) 0.0059(12) 0.0029(12) C5 0.0374(16) 0.0519(19) 0.0405(17) -0.0124(14) 0.0073(13) 0.0094(14) C6 0.0366(15) 0.0362(15) 0.0497(19) -0.0139(13) -0.0019(13) 0.0092(12) C7 0.0442(17) 0.0284(14) 0.0498(18) -0.0005(13) -0.0032(14) 0.0050(12) C8 0.0416(15) 0.0290(14) 0.0370(15) -0.0014(11) 0.0053(12) 0.0039(12) C9 0.0366(15) 0.0297(14) 0.0360(15) -0.0058(11) 0.0098(12) -0.0025(11) C10 0.0502(19) 0.0407(18) 0.059(2) -0.0055(15) 0.0067(16) -0.0154(15) C11 0.0384(15) 0.0419(16) 0.0368(16) -0.0012(12) 0.0014(12) 0.0012(13) C12 0.053(2) 0.0416(18) 0.058(2) 0.0067(15) -0.0068(16) 0.0063(15) C13 0.069(2) 0.065(2) 0.0346(17) -0.0035(16) -0.0038(16) 0.0113(19) C14 0.0476(17) 0.0242(13) 0.0550(19) 0.0091(13) 0.0200(15) -0.0007(12) C15 0.066(2) 0.049(2) 0.077(3) 0.0347(19) 0.042(2) 0.0201(18) C16 0.057(2) 0.0264(14) 0.071(2) 0.0103(15) 0.0297(18) 0.0100(14) C17 0.0359(16) 0.061(2) 0.053(2) -0.0377(17) -0.0044(14) 0.0105(15) C18 0.089(3) 0.0249(14) 0.0426(19) -0.0004(13) -0.0265(18) -0.0101(16) C19 0.0393(17) 0.074(3) 0.049(2) -0.0219(19) 0.0006(15) -0.0115(17) C20 0.052(2) 0.063(2) 0.0425(18) -0.0113(16) -0.0119(15) 0.0230(17) C21 0.084(3) 0.0395(17) 0.0242(14) -0.0027(12) 0.0014(15) 0.0056(16) C22 0.060(2) 0.081(3) 0.070(3) -0.045(2) -0.003(2) 0.018(2) C23 0.123(4) 0.036(2) 0.084(3) -0.001(2) -0.034(3) -0.009(2) C24 0.054(2) 0.121(4) 0.082(3) -0.020(3) 0.007(2) -0.028(3) C25 0.085(3) 0.084(3) 0.076(3) -0.018(3) -0.017(3) 0.044(3) C26 0.110(4) 0.068(3) 0.039(2) 0.0082(19) 0.007(2) 0.003(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3755(7) 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 . Cl1 . 2.3693(9) yes Ti1 . Cl2 . 2.3099(8) yes Ti1 . N1 . 1.929(2) yes Ti1 . N2 . 2.109(2) yes Ti1 . C17 . 2.364(3) yes Ti1 . C18 . 2.317(3) yes Ti1 . C19 . 2.412(3) yes Ti1 . C20 . 2.430(3) yes Ti1 . C21 . 2.387(3) yes N1 . N2 . 1.406(3) yes N1 . Si1 . 1.752(2) yes N2 . C1 . 1.475(3) yes N2 . C2 . 1.473(4) yes N3 . Si1 . 1.752(2) yes N3 . C9 . 1.392(4) yes N3 . C14 . 1.492(4) yes N4 . C9 . 1.288(4) yes N4 . C11 . 1.466(4) yes Si1 . C3 . 1.876(3) yes Si1 . H1 . 1.42(3) no C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . C4 . 1.395(4) yes C3 . C8 . 1.395(4) yes C4 . C5 . 1.398(4) yes C4 . H41 . 0.950 no C5 . C6 . 1.373(5) yes C5 . H51 . 0.950 no C6 . C7 . 1.387(5) yes C6 . H61 . 0.950 no C7 . C8 . 1.384(4) yes C7 . H71 . 0.950 no C8 . H81 . 0.950 no C9 . C10 . 1.508(4) yes C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . C12 . 1.520(5) yes C11 . C13 . 1.521(5) yes C11 . H111 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . C15 . 1.518(5) yes C14 . C16 . 1.527(5) yes C14 . H141 . 0.950 no C15 . H151 . 0.950 no C15 . H152 . 0.950 no C15 . H153 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no C17 . C18 . 1.447(6) yes C17 . C21 . 1.398(5) yes C17 . C22 . 1.491(5) yes C18 . C19 . 1.396(6) yes C18 . C23 . 1.508(5) yes C19 . C20 . 1.345(6) yes C19 . C24 . 1.535(6) yes C20 . C21 . 1.387(6) yes C20 . C25 . 1.515(5) yes C21 . C26 . 1.522(6) yes C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . H231 . 0.950 no C23 . H232 . 0.950 no C23 . H233 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.950 no C24 . H243 . 0.950 no C25 . H251 . 0.950 no C25 . H252 . 0.950 no C25 . H253 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 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 Cl1 . Ti1 . Cl2 . 97.49(3) yes Cl1 . Ti1 . N1 . 121.91(7) yes Cl2 . Ti1 . N1 . 101.51(7) yes Cl1 . Ti1 . N2 . 83.03(6) yes Cl2 . Ti1 . N2 . 97.74(7) yes N1 . Ti1 . N2 . 40.44(9) yes Cl1 . Ti1 . C17 . 128.48(11) yes Cl2 . Ti1 . C17 . 120.92(11) yes N1 . Ti1 . C17 . 85.02(10) yes N2 . Ti1 . C17 . 119.94(10) yes Cl1 . Ti1 . C18 . 92.47(11) yes Cl2 . Ti1 . C18 . 138.65(9) yes N1 . Ti1 . C18 . 106.84(13) yes N2 . Ti1 . C18 . 123.34(11) yes C17 . Ti1 . C18 . 36.01(14) yes Cl1 . Ti1 . C19 . 79.99(10) yes Cl2 . Ti1 . C19 . 108.64(11) yes N1 . Ti1 . C19 . 139.95(11) yes N2 . Ti1 . C19 . 150.15(13) yes C17 . Ti1 . C19 . 57.09(12) yes Cl1 . Ti1 . C20 . 101.90(11) yes Cl2 . Ti1 . C20 . 82.53(10) yes N1 . Ti1 . C20 . 134.58(12) yes N2 . Ti1 . C20 . 175.00(12) yes C17 . Ti1 . C20 . 56.28(11) yes Cl1 . Ti1 . C21 . 134.09(11) yes Cl2 . Ti1 . C21 . 88.02(9) yes N1 . Ti1 . C21 . 101.12(12) yes N2 . Ti1 . C21 . 141.55(12) yes C17 . Ti1 . C21 . 34.22(12) yes C18 . Ti1 . C19 . 34.28(14) yes C18 . Ti1 . C20 . 56.13(13) yes C19 . Ti1 . C20 . 32.26(14) yes C18 . Ti1 . C21 . 57.65(12) yes C19 . Ti1 . C21 . 55.41(14) yes C20 . Ti1 . C21 . 33.46(14) yes Ti1 . N1 . N2 . 76.67(14) yes Ti1 . N1 . Si1 . 151.10(14) yes N2 . N1 . Si1 . 129.78(18) yes N1 . N2 . Ti1 . 62.88(13) yes N1 . N2 . C1 . 117.9(2) yes Ti1 . N2 . C1 . 120.65(18) yes N1 . N2 . C2 . 115.5(2) yes Ti1 . N2 . C2 . 119.95(17) yes C1 . N2 . C2 . 111.7(2) yes Si1 . N3 . C9 . 116.36(18) yes Si1 . N3 . C14 . 122.5(2) yes C9 . N3 . C14 . 121.1(2) yes C9 . N4 . C11 . 120.1(2) yes N3 . Si1 . N1 . 116.88(11) yes N3 . Si1 . C3 . 113.59(12) yes N1 . Si1 . C3 . 115.09(11) yes N3 . Si1 . H1 . 103.9(13) no N1 . Si1 . H1 . 99.0(14) no C3 . Si1 . H1 . 105.8(14) no N2 . C1 . H11 . 109.4 no N2 . C1 . H12 . 109.3 no H11 . C1 . H12 . 109.5 no N2 . C1 . H13 . 109.7 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no N2 . C2 . H21 . 109.6 no N2 . C2 . H22 . 109.2 no H21 . C2 . H22 . 109.5 no N2 . C2 . H23 . 109.5 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no Si1 . C3 . C4 . 117.1(2) yes Si1 . C3 . C8 . 125.4(2) yes C4 . C3 . C8 . 117.3(3) yes C3 . C4 . C5 . 121.2(3) yes C3 . C4 . H41 . 119.2 no C5 . C4 . H41 . 119.5 no C4 . C5 . C6 . 120.1(3) yes C4 . C5 . H51 . 119.8 no C6 . C5 . H51 . 120.1 no C5 . C6 . C7 . 119.7(3) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 120.3 no C6 . C7 . C8 . 120.1(3) yes C6 . C7 . H71 . 120.0 no C8 . C7 . H71 . 119.9 no C3 . C8 . C7 . 121.6(3) yes C3 . C8 . H81 . 118.9 no C7 . C8 . H81 . 119.5 no N3 . C9 . N4 . 115.4(2) yes N3 . C9 . C10 . 119.0(3) yes N4 . C9 . C10 . 125.6(3) yes C9 . C10 . H101 . 109.7 no C9 . C10 . H102 . 109.7 no H101 . C10 . H102 . 109.5 no C9 . C10 . H103 . 109.0 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N4 . C11 . C12 . 109.3(3) yes N4 . C11 . C13 . 109.8(3) yes C12 . C11 . C13 . 110.8(3) yes N4 . C11 . H111 . 108.9 no C12 . C11 . H111 . 109.1 no C13 . C11 . H111 . 108.9 no C11 . C12 . H121 . 109.8 no C11 . C12 . H122 . 109.1 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 109.5 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no C11 . C13 . H131 . 109.9 no C11 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no C11 . C13 . H133 . 109.0 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N3 . C14 . C15 . 111.7(3) yes N3 . C14 . C16 . 111.8(2) yes C15 . C14 . C16 . 110.9(3) yes N3 . C14 . H141 . 107.8 no C15 . C14 . H141 . 106.8 no C16 . C14 . H141 . 107.5 no C14 . C15 . H151 . 107.7 no C14 . C15 . H152 . 110.4 no H151 . C15 . H152 . 109.5 no C14 . C15 . H153 . 110.3 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 109.5 no C14 . C16 . H161 . 110.2 no C14 . C16 . H162 . 109.7 no H161 . C16 . H162 . 109.5 no C14 . C16 . H163 . 108.4 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no Ti1 . C17 . C18 . 70.22(18) yes Ti1 . C17 . C21 . 73.79(17) yes C18 . C17 . C21 . 105.7(3) yes Ti1 . C17 . C22 . 127.9(2) yes C18 . C17 . C22 . 123.6(4) yes C21 . C17 . C22 . 129.9(4) yes Ti1 . C18 . C17 . 73.78(17) yes Ti1 . C18 . C19 . 76.60(19) yes C17 . C18 . C19 . 106.7(3) yes Ti1 . C18 . C23 . 118.7(2) yes C17 . C18 . C23 . 124.5(4) yes C19 . C18 . C23 . 128.6(4) yes Ti1 . C19 . C18 . 69.13(18) yes Ti1 . C19 . C20 . 74.6(2) yes C18 . C19 . C20 . 109.3(3) yes Ti1 . C19 . C24 . 126.1(3) yes C18 . C19 . C24 . 123.2(4) yes C20 . C19 . C24 . 127.4(4) yes Ti1 . C20 . C19 . 73.1(2) yes Ti1 . C20 . C21 . 71.55(19) yes C19 . C20 . C21 . 109.5(3) yes Ti1 . C20 . C25 . 125.1(3) yes C19 . C20 . C25 . 126.4(4) yes C21 . C20 . C25 . 124.0(4) yes Ti1 . C21 . C17 . 71.99(18) yes Ti1 . C21 . C20 . 74.99(19) yes C17 . C21 . C20 . 108.6(3) yes Ti1 . C21 . C26 . 122.3(3) yes C17 . C21 . C26 . 124.0(4) yes C20 . C21 . C26 . 127.3(4) yes C17 . C22 . H221 . 109.9 no C17 . C22 . H222 . 109.9 no H221 . C22 . H222 . 109.5 no C17 . C22 . H223 . 108.6 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no C18 . C23 . H231 . 110.0 no C18 . C23 . H232 . 109.2 no H231 . C23 . H232 . 109.5 no C18 . C23 . H233 . 109.2 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C19 . C24 . H241 . 109.8 no C19 . C24 . H242 . 109.7 no H241 . C24 . H242 . 109.5 no C19 . C24 . H243 . 109.0 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C20 . C25 . H251 . 109.0 no C20 . C25 . H252 . 109.8 no H251 . C25 . H252 . 109.5 no C20 . C25 . H253 . 109.6 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no C21 . C26 . H261 . 109.7 no C21 . C26 . H262 . 109.2 no H261 . C26 . H262 . 109.5 no C21 . C26 . H263 . 109.4 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no #===end data_compound_12 _database_code_depnum_ccdc_archive 'CCDC 849352' #TrackingRef '- Mountford Xray SI.CIF' # local code PJT7 _chemical_name_systematic ; Cp*Ti{N(NMe2)SiMe2N(iPr)CMeNiPr}Cl2 ; _chemical_melting_point ? _publ_section_exptl_refinement ; H atoms were placed in calculated positions with reference to a Fourier difference map and refined in a riding model. ; _cell_length_a 11.5599(3) _cell_length_b 16.9818(4) _cell_length_c 13.9465(3) _cell_angle_alpha 90 _cell_angle_beta 91.892(1) _cell_angle_gamma 90 _cell_volume 2736.32(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C22 H44 Cl2 N4 Si1 Ti1' _chemical_formula_moiety 'C22 H44 Cl2 N4 Si1 Ti1' _chemical_compound_source ? _chemical_formula_weight 511.51 _cell_measurement_reflns_used 11903 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 22397 _reflns_number_total 6225 _diffrn_reflns_av_R_equivalents 0.105 _diffrn_reflns_theta_min 5.109 _diffrn_reflns_theta_max 27.517 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.966 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -14 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 2.38 _oxford_diffrn_Wilson_scale 39.04 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.42 _refine_diff_density_max 0.51 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 3145 _refine_ls_number_restraints 0 _refine_ls_number_parameters 271 _oxford_refine_ls_R_factor_ref 0.0482 _refine_ls_wR_factor_ref 0.0511 _refine_ls_goodness_of_fit_ref 1.1157 _refine_ls_shift/su_max 0.000513 # The values computed from all data _oxford_reflns_number_all 6225 _refine_ls_R_factor_all 0.1251 _refine_ls_wR_factor_all 0.0852 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3643 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_gt 0.0552 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _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: 0.730 0.479 0.536 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # 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_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ti1 Ti 0.63342(5) 0.65927(4) 0.30875(4) 0.0260 1.0000 Uani . . . . . . . Cl1 Cl 0.69341(8) 0.59110(6) 0.44543(7) 0.0417 1.0000 Uani . . . . . . . Cl2 Cl 0.64449(9) 0.78479(6) 0.38074(7) 0.0427 1.0000 Uani . . . . . . . N1 N 0.7533(2) 0.61849(17) 0.2303(2) 0.0277 1.0000 Uani . . . . . . . N2 N 0.7659(2) 0.70094(17) 0.2211(2) 0.0300 1.0000 Uani . . . . . . . N3 N 0.9866(2) 0.54854(17) 0.2331(2) 0.0308 1.0000 Uani . . . . . . . N4 N 1.0286(3) 0.63857(19) 0.1184(2) 0.0357 1.0000 Uani . . . . . . . Si1 Si 0.84285(8) 0.54357(6) 0.18890(7) 0.0307 1.0000 Uani . . . . . . . C1 C 0.7529(4) 0.7333(3) 0.1234(3) 0.0419 1.0000 Uani . . . . . . . C2 C 0.8674(3) 0.7346(2) 0.2731(3) 0.0392 1.0000 Uani . . . . . . . C3 C 0.7809(3) 0.4524(2) 0.2415(4) 0.0471 1.0000 Uani . . . . . . . C4 C 0.8344(3) 0.5338(3) 0.0563(3) 0.0435 1.0000 Uani . . . . . . . C5 C 1.0686(3) 0.5881(2) 0.1782(3) 0.0305 1.0000 Uani . . . . . . . C6 C 1.1945(3) 0.5644(3) 0.1895(3) 0.0424 1.0000 Uani . . . . . . . C7 C 1.0145(3) 0.5208(2) 0.3328(3) 0.0389 1.0000 Uani . . . . . . . C8 C 1.0694(4) 0.5832(3) 0.3962(3) 0.0507 1.0000 Uani . . . . . . . C9 C 1.0790(4) 0.4422(3) 0.3375(4) 0.0520 1.0000 Uani . . . . . . . C10 C 1.1034(4) 0.6789(3) 0.0502(3) 0.0443 1.0000 Uani . . . . . . . C11 C 1.1300(4) 0.7607(3) 0.0877(4) 0.0580 1.0000 Uani . . . . . . . C12 C 1.0392(4) 0.6825(3) -0.0466(3) 0.0586 1.0000 Uani . . . . . . . C13 C 0.4788(3) 0.5671(2) 0.2815(3) 0.0297 1.0000 Uani . . . . . . . C14 C 0.4372(3) 0.6217(2) 0.3500(2) 0.0285 1.0000 Uani . . . . . . . C15 C 0.4291(3) 0.6958(2) 0.3056(3) 0.0323 1.0000 Uani . . . . . . . C16 C 0.4681(3) 0.6886(2) 0.2101(2) 0.0325 1.0000 Uani . . . . . . . C17 C 0.4952(3) 0.6082(2) 0.1938(3) 0.0324 1.0000 Uani . . . . . . . C18 C 0.4847(3) 0.4800(2) 0.2967(3) 0.0380 1.0000 Uani . . . . . . . C19 C 0.4041(3) 0.6007(2) 0.4498(3) 0.0365 1.0000 Uani . . . . . . . C20 C 0.3759(4) 0.7682(2) 0.3468(3) 0.0437 1.0000 Uani . . . . . . . C21 C 0.4634(4) 0.7546(3) 0.1380(3) 0.0449 1.0000 Uani . . . . . . . C22 C 0.5208(3) 0.5724(3) 0.0995(3) 0.0410 1.0000 Uani . . . . . . . H11 H 0.7277 0.7865 0.1262 0.0505 1.0000 Uiso R . . . . . . H12 H 0.8248 0.7309 0.0924 0.0505 1.0000 Uiso R . . . . . . H13 H 0.6971 0.7032 0.0878 0.0505 1.0000 Uiso R . . . . . . H21 H 0.8692 0.7899 0.2628 0.0462 1.0000 Uiso R . . . . . . H22 H 0.9361 0.7117 0.2501 0.0462 1.0000 Uiso R . . . . . . H23 H 0.8623 0.7242 0.3398 0.0462 1.0000 Uiso R . . . . . . H31 H 0.8246 0.4080 0.2226 0.0564 1.0000 Uiso R . . . . . . H32 H 0.7833 0.4563 0.3095 0.0564 1.0000 Uiso R . . . . . . H33 H 0.7029 0.4465 0.2191 0.0564 1.0000 Uiso R . . . . . . H41 H 0.8843 0.4926 0.0370 0.0523 1.0000 Uiso R . . . . . . H42 H 0.8573 0.5819 0.0278 0.0523 1.0000 Uiso R . . . . . . H43 H 0.7571 0.5217 0.0363 0.0523 1.0000 Uiso R . . . . . . H61 H 1.2398 0.5957 0.1487 0.0509 1.0000 Uiso R . . . . . . H62 H 1.2204 0.5717 0.2542 0.0509 1.0000 Uiso R . . . . . . H63 H 1.2021 0.5105 0.1726 0.0509 1.0000 Uiso R . . . . . . H71 H 0.9416 0.5106 0.3596 0.0456 1.0000 Uiso R . . . . . . H81 H 1.0849 0.5618 0.4583 0.0589 1.0000 Uiso R . . . . . . H82 H 1.1398 0.6002 0.3697 0.0589 1.0000 Uiso R . . . . . . H83 H 1.0182 0.6266 0.4009 0.0589 1.0000 Uiso R . . . . . . H91 H 1.0938 0.4284 0.4028 0.0609 1.0000 Uiso R . . . . . . H92 H 1.1502 0.4467 0.3059 0.0609 1.0000 Uiso R . . . . . . H93 H 1.0328 0.4025 0.3072 0.0609 1.0000 Uiso R . . . . . . H101 H 1.1734 0.6502 0.0445 0.0531 1.0000 Uiso R . . . . . . H111 H 1.1782 0.7872 0.0442 0.0693 1.0000 Uiso R . . . . . . H112 H 1.1686 0.7572 0.1488 0.0688 1.0000 Uiso R . . . . . . H113 H 1.0598 0.7892 0.0934 0.0688 1.0000 Uiso R . . . . . . H121 H 1.0861 0.7081 -0.0918 0.0697 1.0000 Uiso R . . . . . . H122 H 0.9691 0.7109 -0.0405 0.0697 1.0000 Uiso R . . . . . . H123 H 1.0222 0.6305 -0.0681 0.0697 1.0000 Uiso R . . . . . . H181 H 0.5151 0.4557 0.2416 0.0465 1.0000 Uiso R . . . . . . H182 H 0.5335 0.4689 0.3511 0.0465 1.0000 Uiso R . . . . . . H183 H 0.4093 0.4602 0.3069 0.0465 1.0000 Uiso R . . . . . . H191 H 0.3791 0.6466 0.4819 0.0435 1.0000 Uiso R . . . . . . H192 H 0.4693 0.5790 0.4836 0.0435 1.0000 Uiso R . . . . . . H193 H 0.3433 0.5631 0.4471 0.0435 1.0000 Uiso R . . . . . . H201 H 0.3816 0.8106 0.3029 0.0529 1.0000 Uiso R . . . . . . H202 H 0.4149 0.7816 0.4056 0.0529 1.0000 Uiso R . . . . . . H203 H 0.2966 0.7580 0.3581 0.0529 1.0000 Uiso R . . . . . . H211 H 0.4933 0.7367 0.0792 0.0553 1.0000 Uiso R . . . . . . H212 H 0.5088 0.7974 0.1618 0.0553 1.0000 Uiso R . . . . . . H213 H 0.3856 0.7713 0.1276 0.0553 1.0000 Uiso R . . . . . . H221 H 0.5714 0.6056 0.0655 0.0493 1.0000 Uiso R . . . . . . H222 H 0.5559 0.5223 0.1091 0.0493 1.0000 Uiso R . . . . . . H223 H 0.4506 0.5661 0.0628 0.0493 1.0000 Uiso 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 0.0273(3) 0.0264(3) 0.0242(3) 0.0004(3) -0.0011(2) 0.0006(3) Cl1 0.0394(5) 0.0510(6) 0.0340(5) 0.0142(4) -0.0072(4) -0.0019(4) Cl2 0.0485(5) 0.0375(5) 0.0423(5) -0.0138(4) 0.0049(4) -0.0042(4) N1 0.0259(14) 0.0232(15) 0.0339(15) -0.0015(12) 0.0013(12) -0.0028(11) N2 0.0307(15) 0.0253(16) 0.0340(15) 0.0022(12) 0.0009(12) -0.0042(12) N3 0.0273(14) 0.0301(16) 0.0349(16) 0.0031(13) 0.0009(12) 0.0023(12) N4 0.0300(15) 0.0423(19) 0.0349(17) 0.0035(14) 0.0040(13) 0.0009(13) Si1 0.0266(5) 0.0267(5) 0.0387(5) -0.0061(4) 0.0005(4) -0.0007(4) C1 0.046(2) 0.044(2) 0.036(2) 0.0133(18) 0.0092(17) 0.0057(18) C2 0.0340(19) 0.030(2) 0.054(2) -0.0079(17) 0.0050(17) -0.0035(15) C3 0.038(2) 0.027(2) 0.076(3) -0.005(2) 0.009(2) -0.0015(17) C4 0.0319(18) 0.054(3) 0.044(2) -0.017(2) 0.0015(16) 0.0031(18) C5 0.0288(17) 0.0290(18) 0.0337(18) -0.0037(15) 0.0014(14) 0.0023(14) C6 0.0341(19) 0.053(3) 0.040(2) 0.0051(19) -0.0002(16) 0.0062(17) C7 0.0344(19) 0.041(2) 0.041(2) 0.0080(18) 0.0006(16) 0.0044(16) C8 0.061(3) 0.053(3) 0.038(2) -0.005(2) -0.0071(19) 0.009(2) C9 0.054(3) 0.042(3) 0.059(3) 0.010(2) -0.004(2) 0.009(2) C10 0.041(2) 0.047(3) 0.045(2) 0.0143(19) 0.0085(17) 0.0076(18) C11 0.053(3) 0.057(3) 0.065(3) 0.015(2) 0.014(2) -0.005(2) C12 0.068(3) 0.068(3) 0.041(2) 0.012(2) 0.012(2) 0.011(2) C13 0.0218(15) 0.0332(19) 0.0343(19) -0.0027(15) 0.0037(13) 0.0021(13) C14 0.0266(16) 0.0310(18) 0.0278(17) -0.0009(14) 0.0006(13) 0.0010(14) C15 0.0292(17) 0.039(2) 0.0289(17) 0.0009(16) 0.0009(14) 0.0006(15) C16 0.0285(17) 0.038(2) 0.0304(18) 0.0037(15) -0.0052(14) 0.0038(15) C17 0.0272(17) 0.039(2) 0.0310(18) -0.0086(15) -0.0023(14) -0.0027(15) C18 0.0322(19) 0.033(2) 0.049(2) -0.0031(17) 0.0013(16) -0.0054(16) C19 0.0403(19) 0.040(2) 0.0303(18) 0.0066(17) 0.0102(15) 0.0015(17) C20 0.043(2) 0.040(2) 0.048(2) 0.0014(19) 0.0022(18) 0.0140(18) C21 0.041(2) 0.057(3) 0.037(2) 0.0156(19) -0.0009(17) 0.0109(19) C22 0.038(2) 0.061(3) 0.0241(18) -0.0075(17) 0.0024(15) -0.0014(18) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1649(4) 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 . Cl1 . 2.3167(12) yes Ti1 . Cl2 . 2.3579(12) yes Ti1 . N1 . 1.923(3) yes Ti1 . N2 . 2.112(3) yes Ti1 . C13 . 2.397(3) yes Ti1 . C14 . 2.444(3) yes Ti1 . C15 . 2.441(4) yes Ti1 . C16 . 2.371(3) yes Ti1 . C17 . 2.388(3) yes N1 . N2 . 1.414(4) yes N1 . Si1 . 1.750(3) yes N2 . C1 . 1.473(5) yes N2 . C2 . 1.475(5) yes N3 . Si1 . 1.755(3) yes N3 . C5 . 1.409(4) yes N3 . C7 . 1.492(5) yes N4 . C5 . 1.273(5) yes N4 . C10 . 1.475(5) yes Si1 . C3 . 1.867(4) yes Si1 . C4 . 1.856(4) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . H31 . 0.950 no C3 . H32 . 0.950 no C3 . H33 . 0.950 no C4 . H41 . 0.950 no C4 . H42 . 0.950 no C4 . H43 . 0.950 no C5 . C6 . 1.513(5) yes C6 . H61 . 0.950 no C6 . H62 . 0.950 no C6 . H63 . 0.950 no C7 . C8 . 1.507(6) yes C7 . C9 . 1.530(6) yes C7 . H71 . 0.950 no C8 . H81 . 0.950 no C8 . H82 . 0.950 no C8 . H83 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . C11 . 1.513(7) yes C10 . C12 . 1.521(6) yes C10 . H101 . 0.950 no C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . C14 . 1.426(5) yes C13 . C17 . 1.427(5) yes C13 . C18 . 1.495(5) yes C14 . C15 . 1.405(5) yes C14 . C19 . 1.498(5) yes C15 . C16 . 1.426(5) yes C15 . C20 . 1.497(5) yes C16 . C17 . 1.421(5) yes C16 . C21 . 1.504(5) yes C17 . C22 . 1.488(5) yes C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no C19 . H191 . 0.950 no C19 . H192 . 0.950 no C19 . H193 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no C21 . H211 . 0.950 no C21 . H212 . 0.950 no C21 . H213 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 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 Cl1 . Ti1 . Cl2 . 95.21(5) yes Cl1 . Ti1 . N1 . 94.98(10) yes Cl2 . Ti1 . N1 . 122.55(9) yes Cl1 . Ti1 . N2 . 116.13(9) yes Cl2 . Ti1 . N2 . 85.03(9) yes N1 . Ti1 . N2 . 40.68(12) yes Cl1 . Ti1 . C13 . 90.33(9) yes Cl2 . Ti1 . C13 . 133.43(9) yes N1 . Ti1 . C13 . 102.84(12) yes N2 . Ti1 . C13 . 132.69(12) yes Cl1 . Ti1 . C14 . 86.03(9) yes Cl2 . Ti1 . C14 . 99.99(9) yes N1 . Ti1 . C14 . 137.05(12) yes N2 . Ti1 . C14 . 156.93(12) yes C13 . Ti1 . C14 . 34.25(11) yes Cl1 . Ti1 . C15 . 113.89(9) yes Cl2 . Ti1 . C15 . 79.42(9) yes N1 . Ti1 . C15 . 142.78(12) yes N2 . Ti1 . C15 . 128.59(12) yes C13 . Ti1 . C15 . 56.43(12) yes Cl1 . Ti1 . C16 . 142.78(10) yes Cl2 . Ti1 . C16 . 95.07(10) yes N1 . Ti1 . C16 . 109.11(13) yes N2 . Ti1 . C16 . 100.34(12) yes C13 . Ti1 . C16 . 57.49(13) yes Cl1 . Ti1 . C17 . 123.12(10) yes Cl2 . Ti1 . C17 . 129.77(10) yes N1 . Ti1 . C17 . 88.03(12) yes N2 . Ti1 . C17 . 102.39(12) yes C13 . Ti1 . C17 . 34.69(13) yes C14 . Ti1 . C15 . 33.43(12) yes C14 . Ti1 . C16 . 56.96(12) yes C15 . Ti1 . C16 . 34.44(12) yes C14 . Ti1 . C17 . 57.17(12) yes C15 . Ti1 . C17 . 56.98(12) yes C16 . Ti1 . C17 . 34.74(13) yes Ti1 . N1 . N2 . 76.87(18) yes Ti1 . N1 . Si1 . 153.46(18) yes N2 . N1 . Si1 . 128.8(2) yes N1 . N2 . Ti1 . 62.45(16) yes N1 . N2 . C1 . 116.4(3) yes Ti1 . N2 . C1 . 127.4(2) yes N1 . N2 . C2 . 115.0(3) yes Ti1 . N2 . C2 . 115.2(2) yes C1 . N2 . C2 . 111.4(3) yes Si1 . N3 . C5 . 118.5(2) yes Si1 . N3 . C7 . 119.0(2) yes C5 . N3 . C7 . 121.9(3) yes C5 . N4 . C10 . 121.8(3) yes N3 . Si1 . N1 . 114.38(14) yes N3 . Si1 . C3 . 105.84(18) yes N1 . Si1 . C3 . 103.56(17) yes N3 . Si1 . C4 . 111.87(16) yes N1 . Si1 . C4 . 112.42(17) yes C3 . Si1 . C4 . 108.0(2) yes N2 . C1 . H11 . 109.8 no N2 . C1 . H12 . 110.0 no H11 . C1 . H12 . 109.5 no N2 . C1 . H13 . 109.2 no H11 . C1 . H13 . 109.2 no H12 . C1 . H13 . 109.2 no N2 . C2 . H21 . 109.3 no N2 . C2 . H22 . 109.6 no H21 . C2 . H22 . 109.5 no N2 . C2 . H23 . 109.5 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no Si1 . C3 . H31 . 109.5 no Si1 . C3 . H32 . 109.6 no H31 . C3 . H32 . 109.5 no Si1 . C3 . H33 . 109.2 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no Si1 . C4 . H41 . 109.6 no Si1 . C4 . H42 . 109.5 no H41 . C4 . H42 . 109.5 no Si1 . C4 . H43 . 109.3 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no N3 . C5 . N4 . 116.2(3) yes N3 . C5 . C6 . 118.6(3) yes N4 . C5 . C6 . 125.2(3) yes C5 . C6 . H61 . 109.6 no C5 . C6 . H62 . 109.7 no H61 . C6 . H62 . 109.5 no C5 . C6 . H63 . 109.1 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no N3 . C7 . C8 . 113.5(3) yes N3 . C7 . C9 . 114.0(3) yes C8 . C7 . C9 . 113.1(3) yes N3 . C7 . H71 . 104.9 no C8 . C7 . H71 . 105.0 no C9 . C7 . H71 . 105.1 no C7 . C8 . H81 . 109.3 no C7 . C8 . H82 . 109.6 no H81 . C8 . H82 . 109.5 no C7 . C8 . H83 . 109.6 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no C7 . C9 . H91 . 109.2 no C7 . C9 . H92 . 109.7 no H91 . C9 . H92 . 109.5 no C7 . C9 . H93 . 109.5 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N4 . C10 . C11 . 108.7(3) yes N4 . C10 . C12 . 108.1(3) yes C11 . C10 . C12 . 111.0(4) yes N4 . C10 . H101 . 109.6 no C11 . C10 . H101 . 109.7 no C12 . C10 . H101 . 109.7 no C10 . C11 . H111 . 109.3 no C10 . C11 . H112 . 109.6 no H111 . C11 . H112 . 109.5 no C10 . C11 . H113 . 109.4 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no C10 . C12 . H121 . 109.5 no C10 . C12 . H122 . 109.4 no H121 . C12 . H122 . 109.5 no C10 . C12 . H123 . 109.4 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no Ti1 . C13 . C14 . 74.7(2) yes Ti1 . C13 . C17 . 72.32(19) yes C14 . C13 . C17 . 108.3(3) yes Ti1 . C13 . C18 . 126.3(2) yes C14 . C13 . C18 . 124.2(3) yes C17 . C13 . C18 . 126.8(3) yes Ti1 . C14 . C13 . 71.08(19) yes Ti1 . C14 . C15 . 73.2(2) yes C13 . C14 . C15 . 107.8(3) yes Ti1 . C14 . C19 . 123.2(2) yes C13 . C14 . C19 . 124.7(3) yes C15 . C14 . C19 . 127.4(3) yes Ti1 . C15 . C14 . 73.4(2) yes Ti1 . C15 . C16 . 70.10(19) yes C14 . C15 . C16 . 108.5(3) yes Ti1 . C15 . C20 . 127.7(3) yes C14 . C15 . C20 . 126.0(3) yes C16 . C15 . C20 . 125.1(3) yes Ti1 . C16 . C15 . 75.5(2) yes Ti1 . C16 . C17 . 73.29(19) yes C15 . C16 . C17 . 108.1(3) yes Ti1 . C16 . C21 . 123.7(3) yes C15 . C16 . C21 . 123.7(3) yes C17 . C16 . C21 . 127.7(3) yes Ti1 . C17 . C13 . 73.0(2) yes Ti1 . C17 . C16 . 71.97(19) yes C13 . C17 . C16 . 107.3(3) yes Ti1 . C17 . C22 . 126.5(2) yes C13 . C17 . C22 . 126.4(3) yes C16 . C17 . C22 . 125.8(4) yes C13 . C18 . H181 . 109.4 no C13 . C18 . H182 . 109.5 no H181 . C18 . H182 . 109.5 no C13 . C18 . H183 . 109.5 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no C14 . C19 . H191 . 109.5 no C14 . C19 . H192 . 109.4 no H191 . C19 . H192 . 109.5 no C14 . C19 . H193 . 109.5 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C15 . C20 . H201 . 109.7 no C15 . C20 . H202 . 109.8 no H201 . C20 . H202 . 109.5 no C15 . C20 . H203 . 109.0 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C16 . C21 . H211 . 109.5 no C16 . C21 . H212 . 109.2 no H211 . C21 . H212 . 109.5 no C16 . C21 . H213 . 109.8 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C17 . C22 . H221 . 110.0 no C17 . C22 . H222 . 109.7 no H221 . C22 . H222 . 109.5 no C17 . C22 . H223 . 109.3 no H221 . C22 . H223 . 109.2 no H222 . C22 . H223 . 109.2 no #===end data_compound_15 _database_code_depnum_ccdc_archive 'CCDC 849353' #TrackingRef '- Mountford Xray SI.CIF' # local code PJT19 _chemical_name_systematic ; Cp*Ti{N(NPh2)SiH(Me)Ph}Cl2 ; _chemical_melting_point ? _publ_section_exptl_refinement ; Si-H hydrogen atoms were located from Fourier maps and positionally and isotropically refined. C-bound H atoms were placed in calculated positions with reference to a Fourier difference map and refined in a riding model. The largest peak in the final Fourier difference map was located 1.20 A away from Si(1). ; _cell_length_a 8.4930(2) _cell_length_b 11.6230(3) _cell_length_c 14.6209(3) _cell_angle_alpha 95.5060(10) _cell_angle_beta 96.0935(9) _cell_angle_gamma 98.8666(12) _cell_volume 1408.69(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C29 H34 Cl2 N2 Si1 Ti1' _chemical_formula_moiety 'C29 H34 Cl2 N2 Si1 Ti1' _chemical_compound_source ? _chemical_formula_weight 557.49 _cell_measurement_reflns_used 5663 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.080 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.100 _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 10551 _reflns_number_total 6319 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_theta_min 5.146 _diffrn_reflns_theta_max 27.500 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.025 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -11 _reflns_limit_h_max 10 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 2.51 _oxford_diffrn_Wilson_scale 2.86 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.61 _refine_diff_density_max 1.31 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 4490 _refine_ls_number_restraints 0 _refine_ls_number_parameters 320 _oxford_refine_ls_R_factor_ref 0.0525 _refine_ls_wR_factor_ref 0.0562 _refine_ls_goodness_of_fit_ref 1.1107 _refine_ls_shift/su_max 0.0008873 _refine_ls_shift/su_mean 0.0000338 # The values computed from all data _oxford_reflns_number_all 6319 _refine_ls_R_factor_all 0.0775 _refine_ls_wR_factor_all 0.0756 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4866 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_gt 0.0587 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _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: 1.03 0.468 0.706 0.103 0.167 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # 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_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.96513(6) 0.29460(5) 0.75343(3) 0.0249 1.0000 Uani . . . . . . N1 N 0.7523(3) 0.2340(2) 0.69087(16) 0.0241 1.0000 Uani . . . . . . N2 N 0.8118(3) 0.3104(2) 0.62601(16) 0.0239 1.0000 Uani . . . . . . Cl1 Cl 1.04240(9) 0.11326(7) 0.76046(5) 0.0356 1.0000 Uani . . . . . . Cl2 Cl 1.17859(9) 0.37321(8) 0.67880(6) 0.0385 1.0000 Uani . . . . . . Si1 Si 0.61598(10) 0.10197(8) 0.65343(6) 0.0313 1.0000 Uani . . . . . . C1 C 0.8308(3) 0.2543(3) 0.53458(19) 0.0255 1.0000 Uani . . . . . . C2 C 0.7434(4) 0.2826(3) 0.4562(2) 0.0340 1.0000 Uani . . . . . . C3 C 0.7576(4) 0.2271(3) 0.3692(2) 0.0376 1.0000 Uani . . . . . . C4 C 0.8570(4) 0.1451(3) 0.3602(2) 0.0348 1.0000 Uani . . . . . . C5 C 0.9451(4) 0.1176(3) 0.4382(2) 0.0327 1.0000 Uani . . . . . . C6 C 0.9320(4) 0.1717(3) 0.5257(2) 0.0298 1.0000 Uani . . . . . . C7 C 0.7500(3) 0.4203(3) 0.62347(19) 0.0259 1.0000 Uani . . . . . . C8 C 0.5999(3) 0.4333(3) 0.6465(2) 0.0288 1.0000 Uani . . . . . . C9 C 0.5482(4) 0.5399(3) 0.6409(2) 0.0340 1.0000 Uani . . . . . . C10 C 0.6448(4) 0.6326(3) 0.6107(2) 0.0379 1.0000 Uani . . . . . . C11 C 0.7945(4) 0.6177(3) 0.5856(2) 0.0380 1.0000 Uani . . . . . . C12 C 0.8485(4) 0.5125(3) 0.5929(2) 0.0320 1.0000 Uani . . . . . . C13 C 0.4272(4) 0.1318(3) 0.5917(2) 0.0410 1.0000 Uani . . . . . . C14 C 0.5762(3) 0.0214(3) 0.7547(2) 0.0279 1.0000 Uani . . . . . . C15 C 0.6614(4) -0.0701(3) 0.7730(3) 0.0439 1.0000 Uani . . . . . . C16 C 0.6211(5) -0.1419(4) 0.8419(3) 0.0524 1.0000 Uani . . . . . . C17 C 0.4994(6) -0.1209(4) 0.8919(3) 0.0567 1.0000 Uani . . . . . . C18 C 0.4147(5) -0.0338(4) 0.8754(3) 0.0513 1.0000 Uani . . . . . . C19 C 0.4517(4) 0.0356(3) 0.8073(2) 0.0379 1.0000 Uani . . . . . . C20 C 0.9361(4) 0.4635(3) 0.8535(2) 0.0369 1.0000 Uani . . . . . . C21 C 0.8353(4) 0.3650(3) 0.8791(2) 0.0372 1.0000 Uani . . . . . . C22 C 0.9337(4) 0.2879(3) 0.9134(2) 0.0328 1.0000 Uani . . . . . . C23 C 1.0968(3) 0.3392(3) 0.9101(2) 0.0313 1.0000 Uani . . . . . . C24 C 1.0983(4) 0.4473(3) 0.8753(2) 0.0328 1.0000 Uani . . . . . . C25 C 0.8889(6) 0.5755(4) 0.8265(3) 0.0536 1.0000 Uani . . . . . . C26 C 0.6560(4) 0.3518(4) 0.8776(3) 0.0500 1.0000 Uani . . . . . . C27 C 0.8774(5) 0.1770(3) 0.9532(2) 0.0441 1.0000 Uani . . . . . . C28 C 1.2430(4) 0.2896(4) 0.9425(2) 0.0424 1.0000 Uani . . . . . . C29 C 1.2433(5) 0.5364(3) 0.8683(3) 0.0491 1.0000 Uani . . . . . . H1 H 0.695(5) 0.024(4) 0.594(3) 0.052(11) 1.0000 Uiso . . . . . . H21 H 0.6748 0.3395 0.4623 0.0412 1.0000 Uiso R . . . . . H31 H 0.6976 0.2461 0.3157 0.0459 1.0000 Uiso R . . . . . H41 H 0.8652 0.1073 0.3008 0.0421 1.0000 Uiso R . . . . . H51 H 1.0149 0.0616 0.4320 0.0400 1.0000 Uiso R . . . . . H61 H 0.9918 0.1525 0.5791 0.0360 1.0000 Uiso R . . . . . H81 H 0.5329 0.3693 0.6660 0.0349 1.0000 Uiso R . . . . . H91 H 0.4458 0.5498 0.6578 0.0409 1.0000 Uiso R . . . . . H101 H 0.6087 0.7056 0.6068 0.0454 1.0000 Uiso R . . . . . H111 H 0.8602 0.6803 0.5635 0.0456 1.0000 Uiso R . . . . . H121 H 0.9519 0.5027 0.5774 0.0388 1.0000 Uiso R . . . . . H131 H 0.4510 0.1730 0.5405 0.0507 1.0000 Uiso R . . . . . H132 H 0.3757 0.1779 0.6326 0.0507 1.0000 Uiso R . . . . . H133 H 0.3581 0.0598 0.5703 0.0507 1.0000 Uiso R . . . . . H151 H 0.7471 -0.0829 0.7386 0.0542 1.0000 Uiso R . . . . . H161 H 0.6774 -0.2046 0.8534 0.0632 1.0000 Uiso R . . . . . H171 H 0.4741 -0.1682 0.9395 0.0664 1.0000 Uiso R . . . . . H181 H 0.3299 -0.0209 0.9105 0.0632 1.0000 Uiso R . . . . . H191 H 0.3905 0.0956 0.7955 0.0465 1.0000 Uiso R . . . . . H261 H 0.6172 0.2784 0.8975 0.0623 1.0000 Uiso R . . . . . H262 H 0.6301 0.4133 0.9180 0.0623 1.0000 Uiso R . . . . . H263 H 0.6075 0.3549 0.8164 0.0623 1.0000 Uiso R . . . . . H271 H 0.9673 0.1413 0.9715 0.0546 1.0000 Uiso R . . . . . H272 H 0.8240 0.1942 1.0055 0.0546 1.0000 Uiso R . . . . . H273 H 0.8055 0.1251 0.9077 0.0546 1.0000 Uiso R . . . . . H281 H 1.2986 0.3336 0.9978 0.0531 1.0000 Uiso R . . . . . H282 H 1.2144 0.2100 0.9530 0.0531 1.0000 Uiso R . . . . . H283 H 1.3126 0.2930 0.8958 0.0531 1.0000 Uiso R . . . . . H291 H 1.3377 0.5056 0.8863 0.0609 1.0000 Uiso R . . . . . H292 H 1.2412 0.6058 0.9079 0.0609 1.0000 Uiso R . . . . . H293 H 1.2429 0.5542 0.8062 0.0609 1.0000 Uiso R . . . . . H251 H 0.9296 0.5941 0.7707 0.0638 1.0000 Uiso R . . . . . H252 H 0.7753 0.5693 0.8186 0.0638 1.0000 Uiso R . . . . . H253 H 0.9324 0.6370 0.8742 0.0638 1.0000 Uiso 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 0.0182(2) 0.0335(3) 0.0222(3) -0.0009(2) 0.00254(18) 0.0041(2) N1 0.0218(11) 0.0289(12) 0.0220(11) 0.0079(9) 0.0046(9) 0.0015(9) N2 0.0232(11) 0.0256(12) 0.0218(11) 0.0029(9) 0.0047(9) -0.0006(9) Cl1 0.0334(4) 0.0431(5) 0.0327(4) 0.0013(3) 0.0016(3) 0.0174(3) Cl2 0.0231(3) 0.0504(5) 0.0375(4) -0.0059(3) 0.0107(3) -0.0056(3) Si1 0.0328(4) 0.0303(4) 0.0289(4) 0.0015(3) 0.0046(3) -0.0001(3) C1 0.0263(13) 0.0261(14) 0.0217(13) 0.0016(11) 0.0033(11) -0.0026(11) C2 0.0312(15) 0.0432(18) 0.0273(15) 0.0031(13) 0.0011(12) 0.0077(13) C3 0.0419(18) 0.0451(19) 0.0242(15) 0.0035(13) -0.0017(13) 0.0062(15) C4 0.0436(18) 0.0315(16) 0.0252(15) -0.0015(12) 0.0053(13) -0.0043(13) C5 0.0436(17) 0.0231(14) 0.0297(15) 0.0010(12) 0.0061(13) 0.0004(13) C6 0.0363(16) 0.0254(15) 0.0261(14) 0.0031(12) 0.0027(12) 0.0010(12) C7 0.0259(13) 0.0262(14) 0.0240(13) 0.0033(11) 0.0021(11) -0.0004(11) C8 0.0272(14) 0.0290(15) 0.0292(15) 0.0066(12) 0.0025(11) 0.0002(12) C9 0.0268(15) 0.0353(17) 0.0409(17) 0.0084(14) 0.0045(13) 0.0055(12) C10 0.0401(17) 0.0299(16) 0.0415(18) 0.0078(14) -0.0008(14) 0.0009(13) C11 0.0396(17) 0.0299(17) 0.0420(18) 0.0085(14) 0.0059(14) -0.0055(13) C12 0.0298(15) 0.0320(16) 0.0321(16) 0.0031(13) 0.0079(12) -0.0040(12) C13 0.0375(17) 0.0373(18) 0.0404(18) 0.0068(14) -0.0094(14) -0.0094(14) C14 0.0278(14) 0.0284(15) 0.0257(14) 0.0021(11) 0.0013(11) 0.0012(11) C15 0.0411(19) 0.0410(19) 0.049(2) 0.0027(16) 0.0042(16) 0.0094(15) C16 0.061(2) 0.049(2) 0.051(2) 0.0209(18) 0.0003(19) 0.0159(19) C17 0.070(3) 0.052(2) 0.048(2) 0.0182(19) 0.010(2) -0.001(2) C18 0.047(2) 0.063(3) 0.044(2) 0.0120(19) 0.0142(17) -0.0004(19) C19 0.0314(16) 0.0435(19) 0.0371(17) 0.0018(15) 0.0087(13) -0.0004(14) C20 0.0400(17) 0.0464(19) 0.0240(14) -0.0074(13) -0.0019(13) 0.0178(15) C21 0.0269(15) 0.061(2) 0.0244(15) -0.0048(14) 0.0047(12) 0.0140(15) C22 0.0270(14) 0.0478(19) 0.0227(14) -0.0007(13) 0.0057(11) 0.0047(13) C23 0.0252(14) 0.0469(19) 0.0212(13) -0.0019(13) 0.0021(11) 0.0083(13) C24 0.0316(15) 0.0408(18) 0.0234(14) -0.0052(13) 0.0014(12) 0.0048(13) C25 0.074(3) 0.048(2) 0.039(2) -0.0101(16) -0.0085(19) 0.027(2) C26 0.0273(16) 0.087(3) 0.0356(18) -0.0069(19) 0.0067(14) 0.0162(18) C27 0.046(2) 0.054(2) 0.0308(17) 0.0023(15) 0.0112(15) 0.0008(17) C28 0.0313(16) 0.064(2) 0.0326(17) 0.0017(16) -0.0037(13) 0.0166(16) C29 0.053(2) 0.047(2) 0.0373(19) -0.0076(16) -0.0022(16) -0.0100(17) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5790(10) 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 . 1.932(2) yes Ti1 . N2 . 2.197(2) yes Ti1 . Cl1 . 2.3103(10) yes Ti1 . Cl2 . 2.3265(9) yes Ti1 . C20 . 2.393(3) yes Ti1 . C21 . 2.384(3) yes Ti1 . C22 . 2.389(3) yes Ti1 . C23 . 2.412(3) yes Ti1 . C24 . 2.439(3) yes N1 . N2 . 1.438(3) yes N1 . Si1 . 1.775(2) yes N2 . C1 . 1.466(4) yes N2 . C7 . 1.456(4) yes Si1 . C13 . 1.852(3) yes Si1 . C14 . 1.859(3) yes Si1 . H1 . 1.48(4) no C1 . C2 . 1.393(4) yes C1 . C6 . 1.390(4) yes C2 . C3 . 1.396(5) yes C2 . H21 . 0.950 no C3 . C4 . 1.372(5) yes C3 . H31 . 0.950 no C4 . C5 . 1.388(5) yes C4 . H41 . 0.950 no C5 . C6 . 1.393(4) yes C5 . H51 . 0.950 no C6 . H61 . 0.950 no C7 . C8 . 1.379(4) yes C7 . C12 . 1.395(4) yes C8 . C9 . 1.385(5) yes C8 . H81 . 0.950 no C9 . C10 . 1.387(5) yes C9 . H91 . 0.950 no C10 . C11 . 1.391(5) yes C10 . H101 . 0.950 no C11 . C12 . 1.380(5) yes C11 . H111 . 0.950 no C12 . H121 . 0.950 no C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . C15 . 1.406(5) yes C14 . C19 . 1.393(4) yes C15 . C16 . 1.405(6) yes C15 . H151 . 0.950 no C16 . C17 . 1.366(6) yes C16 . H161 . 0.950 no C17 . C18 . 1.355(6) yes C17 . H171 . 0.950 no C18 . C19 . 1.371(5) yes C18 . H181 . 0.950 no C19 . H191 . 0.950 no C20 . C21 . 1.425(5) yes C20 . C24 . 1.426(4) yes C20 . C25 . 1.495(5) yes C21 . C22 . 1.407(5) yes C21 . C26 . 1.505(4) yes C22 . C23 . 1.429(4) yes C22 . C27 . 1.498(5) yes C23 . C24 . 1.399(5) yes C23 . C28 . 1.499(4) yes C24 . C29 . 1.501(5) yes C25 . H251 . 0.950 no C25 . H252 . 0.950 no C25 . H253 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no C27 . H271 . 0.950 no C27 . H272 . 0.950 no C27 . H273 . 0.950 no C28 . H281 . 0.950 no C28 . H282 . 0.950 no C28 . H283 . 0.950 no C29 . H291 . 0.950 no C29 . H292 . 0.950 no C29 . H293 . 0.950 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 N1 . Ti1 . N2 . 40.13(9) yes N1 . Ti1 . Cl1 . 95.22(8) yes N2 . Ti1 . Cl1 . 114.56(7) yes N1 . Ti1 . Cl2 . 123.76(7) yes N2 . Ti1 . Cl2 . 85.94(6) yes Cl1 . Ti1 . Cl2 . 95.60(4) yes N1 . Ti1 . C20 . 105.40(11) yes N2 . Ti1 . C20 . 102.79(10) yes Cl1 . Ti1 . C20 . 140.24(9) yes Cl2 . Ti1 . C20 . 100.29(9) yes N1 . Ti1 . C21 . 86.46(10) yes N2 . Ti1 . C21 . 106.56(10) yes Cl1 . Ti1 . C21 . 116.46(10) yes Cl2 . Ti1 . C21 . 134.48(10) yes C20 . Ti1 . C21 . 34.72(13) yes N1 . Ti1 . C22 . 103.51(10) yes N2 . Ti1 . C22 . 136.65(10) yes Cl1 . Ti1 . C22 . 85.18(9) yes Cl2 . Ti1 . C22 . 132.31(8) yes C20 . Ti1 . C22 . 57.36(12) yes N1 . Ti1 . C23 . 138.10(10) yes N2 . Ti1 . C23 . 159.64(10) yes Cl1 . Ti1 . C23 . 85.13(8) yes Cl2 . Ti1 . C23 . 97.75(8) yes C20 . Ti1 . C23 . 56.86(11) yes N1 . Ti1 . C24 . 139.42(11) yes N2 . Ti1 . C24 . 129.19(10) yes Cl1 . Ti1 . C24 . 115.45(8) yes Cl2 . Ti1 . C24 . 80.96(8) yes C20 . Ti1 . C24 . 34.30(11) yes C21 . Ti1 . C22 . 34.30(12) yes C21 . Ti1 . C23 . 57.06(10) yes C22 . Ti1 . C23 . 34.64(10) yes C21 . Ti1 . C24 . 56.92(11) yes C22 . Ti1 . C24 . 56.72(11) yes C23 . Ti1 . C24 . 33.52(11) yes Ti1 . N1 . N2 . 79.89(14) yes Ti1 . N1 . Si1 . 142.81(15) yes N2 . N1 . Si1 . 121.41(17) yes N1 . N2 . Ti1 . 59.99(12) yes N1 . N2 . C1 . 116.5(2) yes Ti1 . N2 . C1 . 123.52(18) yes N1 . N2 . C7 . 116.8(2) yes Ti1 . N2 . C7 . 115.52(17) yes C1 . N2 . C7 . 113.9(2) yes N1 . Si1 . C13 . 111.07(14) yes N1 . Si1 . C14 . 109.51(12) yes C13 . Si1 . C14 . 111.16(15) yes N1 . Si1 . H1 . 108.7(16) no C13 . Si1 . H1 . 111.5(16) no C14 . Si1 . H1 . 104.6(16) no N2 . C1 . C2 . 119.3(3) yes N2 . C1 . C6 . 120.8(2) yes C2 . C1 . C6 . 119.9(3) yes C1 . C2 . C3 . 119.5(3) yes C1 . C2 . H21 . 119.9 no C3 . C2 . H21 . 120.5 no C2 . C3 . C4 . 120.6(3) yes C2 . C3 . H31 . 119.6 no C4 . C3 . H31 . 119.8 no C3 . C4 . C5 . 119.8(3) yes C3 . C4 . H41 . 120.1 no C5 . C4 . H41 . 120.1 no C4 . C5 . C6 . 120.4(3) yes C4 . C5 . H51 . 119.9 no C6 . C5 . H51 . 119.8 no C5 . C6 . C1 . 119.7(3) yes C5 . C6 . H61 . 120.4 no C1 . C6 . H61 . 119.9 no N2 . C7 . C8 . 122.7(3) yes N2 . C7 . C12 . 116.5(3) yes C8 . C7 . C12 . 120.7(3) yes C7 . C8 . C9 . 119.5(3) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 120.5 no C8 . C9 . C10 . 120.5(3) yes C8 . C9 . H91 . 119.8 no C10 . C9 . H91 . 119.7 no C9 . C10 . C11 . 119.5(3) yes C9 . C10 . H101 . 120.2 no C11 . C10 . H101 . 120.3 no C10 . C11 . C12 . 120.4(3) yes C10 . C11 . H111 . 119.9 no C12 . C11 . H111 . 119.7 no C7 . C12 . C11 . 119.4(3) yes C7 . C12 . H121 . 120.0 no C11 . C12 . H121 . 120.6 no Si1 . C13 . H131 . 109.4 no Si1 . C13 . H132 . 109.6 no H131 . C13 . H132 . 109.5 no Si1 . C13 . H133 . 109.4 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no Si1 . C14 . C15 . 119.0(3) yes Si1 . C14 . C19 . 123.7(2) yes C15 . C14 . C19 . 116.7(3) yes C14 . C15 . C16 . 120.5(4) yes C14 . C15 . H151 . 119.4 no C16 . C15 . H151 . 120.1 no C15 . C16 . C17 . 119.3(4) yes C15 . C16 . H161 . 120.4 no C17 . C16 . H161 . 120.4 no C16 . C17 . C18 . 121.5(4) yes C16 . C17 . H171 . 119.2 no C18 . C17 . H171 . 119.3 no C17 . C18 . C19 . 119.6(4) yes C17 . C18 . H181 . 120.3 no C19 . C18 . H181 . 120.1 no C14 . C19 . C18 . 122.4(4) yes C14 . C19 . H191 . 118.5 no C18 . C19 . H191 . 119.1 no Ti1 . C20 . C21 . 72.27(18) yes Ti1 . C20 . C24 . 74.61(18) yes C21 . C20 . C24 . 107.5(3) yes Ti1 . C20 . C25 . 127.8(2) yes C21 . C20 . C25 . 127.7(3) yes C24 . C20 . C25 . 123.8(3) yes Ti1 . C21 . C20 . 73.01(18) yes Ti1 . C21 . C22 . 73.04(17) yes C20 . C21 . C22 . 108.2(3) yes Ti1 . C21 . C26 . 123.9(2) yes C20 . C21 . C26 . 125.5(3) yes C22 . C21 . C26 . 126.1(3) yes Ti1 . C22 . C21 . 72.66(18) yes Ti1 . C22 . C23 . 73.56(17) yes C21 . C22 . C23 . 107.7(3) yes Ti1 . C22 . C27 . 123.2(2) yes C21 . C22 . C27 . 125.8(3) yes C23 . C22 . C27 . 126.3(3) yes Ti1 . C23 . C22 . 71.80(16) yes Ti1 . C23 . C24 . 74.33(17) yes C22 . C23 . C24 . 108.4(3) yes Ti1 . C23 . C28 . 122.1(2) yes C22 . C23 . C28 . 126.3(3) yes C24 . C23 . C28 . 125.2(3) yes Ti1 . C24 . C20 . 71.09(17) yes Ti1 . C24 . C23 . 72.16(17) yes C20 . C24 . C23 . 108.2(3) yes Ti1 . C24 . C29 . 126.0(2) yes C20 . C24 . C29 . 124.9(3) yes C23 . C24 . C29 . 126.8(3) yes C20 . C25 . H251 . 110.5 no C20 . C25 . H252 . 110.4 no H251 . C25 . H252 . 109.5 no C20 . C25 . H253 . 109.0 no H251 . C25 . H253 . 108.7 no H252 . C25 . H253 . 108.7 no C21 . C26 . H261 . 109.1 no C21 . C26 . H262 . 109.6 no H261 . C26 . H262 . 109.5 no C21 . C26 . H263 . 109.7 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no C22 . C27 . H271 . 109.3 no C22 . C27 . H272 . 109.7 no H271 . C27 . H272 . 109.5 no C22 . C27 . H273 . 109.4 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no C23 . C28 . H281 . 111.0 no C23 . C28 . H282 . 110.7 no H281 . C28 . H282 . 109.5 no C23 . C28 . H283 . 108.5 no H281 . C28 . H283 . 108.6 no H282 . C28 . H283 . 108.6 no C24 . C29 . H291 . 109.4 no C24 . C29 . H292 . 109.6 no H291 . C29 . H292 . 109.5 no C24 . C29 . H293 . 109.4 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no #===end #===end data_compound_20-I _database_code_depnum_ccdc_archive 'CCDC 849354' #TrackingRef '- Mountford Xray SI.CIF' # local code ads73 _chemical_name_systematic ; [Cp*Ti{MeC(NiPr)2}{NNMe3)]I ; _publ_section_exptl_refinement ; H atoms were placed in calculated positions based on a preliminary Fourier map ; _chemical_melting_point ? _cell_length_a 10.0805(3) _cell_length_b 16.6347(4) _cell_length_c 17.7081(5) _cell_angle_alpha 116.9766(13) _cell_angle_beta 94.7391(11) _cell_angle_gamma 91.8067(14) _cell_volume 2629.29(13) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C21 H41 I1 N4 Ti1' _chemical_formula_moiety 'C21 H41 N4 Ti1, I1' _chemical_compound_source ? _chemical_formula_weight 524.39 _cell_measurement_reflns_used 9709 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.86 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 18784 _reflns_number_total 11899 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_min 5.116 _diffrn_reflns_theta_max 27.510 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.859 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -21 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 2.92 _oxford_diffrn_Wilson_scale 23.19 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.92 _refine_diff_density_max 0.62 _refine_ls_number_reflns 7660 _refine_ls_number_restraints 0 _refine_ls_number_parameters 487 _refine_ls_wR_factor_ref 0.0385 _refine_ls_goodness_of_fit_ref 1.1424 _refine_ls_R_factor_all 0.0719 _refine_ls_wR_factor_all 0.0546 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 7660 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_gt 0.0385 _refine_ls_shift/su_max 0.001205 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none _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: 1.23 1.15 1.32 0.471 0.383 ; 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_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.74525(6) 0.78867(4) 0.81229(4) 0.0259 1.0000 Uani . . . . . . N1 N 0.7360(3) 0.6823(2) 0.72612(19) 0.0279 1.0000 Uani . . . . . . N2 N 0.7430(3) 0.5977(2) 0.65372(19) 0.0285 1.0000 Uani . . . . . . N3 N 0.5724(3) 0.8008(2) 0.8730(2) 0.0364 1.0000 Uani . . . . . . N4 N 0.5983(3) 0.8570(2) 0.7815(2) 0.0355 1.0000 Uani . . . . . . C1 C 0.7742(4) 0.5263(3) 0.6809(3) 0.0369 1.0000 Uani . . . . . . C2 C 0.8473(4) 0.6047(3) 0.6014(3) 0.0369 1.0000 Uani . . . . . . C3 C 0.6091(4) 0.5717(3) 0.6014(3) 0.0381 1.0000 Uani . . . . . . C4 C 0.9763(3) 0.7921(3) 0.8536(2) 0.0278 1.0000 Uani . . . . . . C5 C 0.9103(4) 0.8240(3) 0.9291(2) 0.0331 1.0000 Uani . . . . . . C6 C 0.8587(4) 0.9080(3) 0.9431(3) 0.0384 1.0000 Uani . . . . . . C7 C 0.8901(4) 0.9260(3) 0.8756(3) 0.0364 1.0000 Uani . . . . . . C8 C 0.9613(4) 0.8548(3) 0.8207(3) 0.0324 1.0000 Uani . . . . . . C9 C 1.0573(4) 0.7109(3) 0.8224(3) 0.0412 1.0000 Uani . . . . . . C10 C 0.9083(5) 0.7788(4) 0.9860(3) 0.0552 1.0000 Uani . . . . . . C11 C 0.7861(5) 0.9696(4) 1.0161(3) 0.0585 1.0000 Uani . . . . . . C12 C 0.8595(5) 1.0100(3) 0.8681(4) 0.0607 1.0000 Uani . . . . . . C13 C 1.0192(4) 0.8493(4) 0.7429(3) 0.0448 1.0000 Uani . . . . . . C14 C 0.5148(4) 0.8336(3) 0.8242(3) 0.0381 1.0000 Uani . . . . . . C15 C 0.3662(4) 0.8405(4) 0.8135(3) 0.0529 1.0000 Uani . . . . . . C16 C 0.4944(5) 0.7583(3) 0.9137(3) 0.0498 1.0000 Uani . . . . . . C17 C 0.4909(9) 0.8219(5) 1.0074(4) 0.0991 1.0000 Uani . . . . . . C18 C 0.5503(6) 0.6706(4) 0.9009(4) 0.0661 1.0000 Uani . . . . . . C19 C 0.5483(5) 0.8734(3) 0.7098(3) 0.0453 1.0000 Uani . . . . . . C20 C 0.5212(6) 0.9718(4) 0.7399(4) 0.0701 1.0000 Uani . . . . . . C21 C 0.6425(6) 0.8429(4) 0.6436(4) 0.0575 1.0000 Uani . . . . . . H11 H 0.7787 0.4669 0.6294 0.0460 1.0000 Uiso R . . . . . H12 H 0.8622 0.5440 0.7170 0.0460 1.0000 Uiso R . . . . . H13 H 0.7028 0.5206 0.7145 0.0460 1.0000 Uiso R . . . . . H21 H 0.8513 0.5447 0.5507 0.0443 1.0000 Uiso R . . . . . H22 H 0.9360 0.6234 0.6367 0.0443 1.0000 Uiso R . . . . . H23 H 0.8244 0.6509 0.5820 0.0443 1.0000 Uiso R . . . . . H31 H 0.6118 0.5120 0.5501 0.0399 1.0000 Uiso R . . . . . H32 H 0.5877 0.6188 0.5829 0.0399 1.0000 Uiso R . . . . . H33 H 0.5389 0.5669 0.6363 0.0399 1.0000 Uiso R . . . . . H55 H 0.4389 0.7325 0.4369 0.0500 1.0000 Uiso R . . . . . H63 H 0.8185 1.0386 1.0485 0.0500 1.0000 Uiso R . . . . . H91 H 1.0934 0.7020 0.7685 0.0471 1.0000 Uiso R . . . . . H92 H 1.1331 0.7206 0.8666 0.0471 1.0000 Uiso R . . . . . H93 H 0.9992 0.6560 0.8114 0.0471 1.0000 Uiso R . . . . . H101 H 0.8560 0.8141 1.0346 0.0732 1.0000 Uiso R . . . . . H102 H 1.0015 0.7764 1.0085 0.0732 1.0000 Uiso R . . . . . H103 H 0.8652 0.7159 0.9525 0.0732 1.0000 Uiso R . . . . . H111 H 0.7929 0.9458 1.0589 0.0590 1.0000 Uiso R . . . . . H112 H 0.6904 0.9652 0.9936 0.0590 1.0000 Uiso R . . . . . H121 H 0.8921 1.0059 0.8147 0.0718 1.0000 Uiso R . . . . . H122 H 0.9057 1.0642 0.9184 0.0718 1.0000 Uiso R . . . . . H123 H 0.7610 1.0157 0.8657 0.0718 1.0000 Uiso R . . . . . H131 H 1.0310 0.9133 0.7525 0.0606 1.0000 Uiso R . . . . . H132 H 0.9755 0.8139 0.6832 0.0606 1.0000 Uiso R . . . . . H133 H 1.1092 0.8255 0.7429 0.0606 1.0000 Uiso . . . . . . H151 H 0.3458 0.8674 0.7738 0.0557 1.0000 Uiso R . . . . . H152 H 0.3354 0.8800 0.8701 0.0557 1.0000 Uiso R . . . . . H153 H 0.3188 0.7789 0.7892 0.0557 1.0000 Uiso R . . . . . H161 H 0.4008 0.7441 0.8852 0.0615 1.0000 Uiso R . . . . . H171 H 0.4365 0.7922 1.0339 0.1143 1.0000 Uiso R . . . . . H172 H 0.5842 0.8371 1.0363 0.1143 1.0000 Uiso R . . . . . H173 H 0.4506 0.8786 1.0139 0.1143 1.0000 Uiso R . . . . . H181 H 0.4963 0.6415 0.9280 0.0834 1.0000 Uiso R . . . . . H182 H 0.6447 0.6839 0.9281 0.0834 1.0000 Uiso R . . . . . H183 H 0.5484 0.6287 0.8386 0.0834 1.0000 Uiso R . . . . . H191 H 0.4614 0.8364 0.6838 0.0562 1.0000 Uiso R . . . . . H201 H 0.4862 0.9813 0.6903 0.0849 1.0000 Uiso R . . . . . H202 H 0.6067 1.0101 0.7675 0.0849 1.0000 Uiso R . . . . . H203 H 0.4542 0.9891 0.7822 0.0849 1.0000 Uiso R . . . . . H211 H 0.6076 0.8538 0.5948 0.0780 1.0000 Uiso R . . . . . H212 H 0.7312 0.8775 0.6691 0.0780 1.0000 Uiso R . . . . . H213 H 0.6528 0.7768 0.6227 0.0780 1.0000 Uiso R . . . . . I1 I 0.24732(3) 0.654644(18) 0.574743(17) 0.0352 1.0000 Uani . . . . . . Ti101 Ti 0.80825(6) 0.74212(4) 0.31689(4) 0.0226 1.0000 Uani . . . . . . N101 N 0.7927(3) 0.6619(2) 0.21106(19) 0.0299 1.0000 Uani . U . . . . N102 N 0.7814(3) 0.6013(2) 0.1224(2) 0.0354 1.0000 Uani . U . . . . N103 N 0.7376(3) 0.6743(2) 0.38023(19) 0.0259 1.0000 Uani . . . . . . N104 N 0.6153(3) 0.7678(2) 0.3500(2) 0.0272 1.0000 Uani . . . . . . C101 C 0.8817(7) 0.5329(5) 0.1061(4) 0.0888 1.0000 Uani . U . . . . C102 C 0.8063(10) 0.6503(5) 0.0741(4) 0.1065 1.0000 Uani . U . . . . C103 C 0.6479(5) 0.5524(4) 0.0962(3) 0.0617 1.0000 Uani . U . . . . C104 C 1.0047(4) 0.8227(3) 0.3139(2) 0.0299 1.0000 Uani . . . . . . C105 C 1.0332(3) 0.7933(3) 0.3769(2) 0.0284 1.0000 Uani . . . . . . C106 C 0.9540(4) 0.8395(3) 0.4441(2) 0.0309 1.0000 Uani . . . . . . C107 C 0.8771(4) 0.8969(3) 0.4229(3) 0.0333 1.0000 Uani . . . . . . C108 C 0.9056(4) 0.8858(3) 0.3411(3) 0.0332 1.0000 Uani . . . . . . C109 C 1.0800(4) 0.8005(3) 0.2381(3) 0.0390 1.0000 Uani . . . . . . C110 C 1.1387(4) 0.7312(3) 0.3762(3) 0.0410 1.0000 Uani . . . . . . C111 C 0.9586(5) 0.8341(4) 0.5272(3) 0.0467 1.0000 Uani . . . . . . C112 C 0.7895(5) 0.9644(3) 0.4818(3) 0.0528 1.0000 Uani . . . . . . C113 C 0.8534(5) 0.9357(3) 0.2945(4) 0.0503 1.0000 Uani . . . . . . C114 C 0.6163(4) 0.7038(2) 0.3757(2) 0.0268 1.0000 Uani . . . . . . C115 C 0.4922(4) 0.6689(3) 0.3971(3) 0.0380 1.0000 Uani . . . . . . C116 C 0.7515(4) 0.5869(3) 0.3816(3) 0.0338 1.0000 Uani . . . . . . C117 C 0.8992(4) 0.5763(3) 0.3963(3) 0.0446 1.0000 Uani . . . . . . C118 C 0.6877(5) 0.5069(3) 0.2992(3) 0.0439 1.0000 Uani . . . . . . C119 C 0.4894(4) 0.7970(3) 0.3254(3) 0.0339 1.0000 Uani . . . . . . C120 C 0.4495(5) 0.8832(3) 0.3968(3) 0.0521 1.0000 Uani . . . . . . C121 C 0.5024(5) 0.8063(4) 0.2446(3) 0.0475 1.0000 Uani . . . . . . I101 I 0.27557(3) 0.55897(2) 0.148434(18) 0.0467 1.0000 Uani . . . . . . H1011 H 0.8749 0.4901 0.0438 0.0902 1.0000 Uiso R . . . . . H1012 H 0.9738 0.5637 0.1257 0.0902 1.0000 Uiso R . . . . . H1013 H 0.8627 0.4986 0.1385 0.0902 1.0000 Uiso R . . . . . H1021 H 0.7984 0.6073 0.0118 0.1194 1.0000 Uiso R . . . . . H1022 H 0.8977 0.6822 0.0925 0.1194 1.0000 Uiso R . . . . . H1023 H 0.7383 0.6957 0.0850 0.1194 1.0000 Uiso R . . . . . H1031 H 0.6390 0.5098 0.0338 0.0646 1.0000 Uiso R . . . . . H1032 H 0.5781 0.5968 0.1082 0.0646 1.0000 Uiso R . . . . . H1033 H 0.6360 0.5175 0.1289 0.0646 1.0000 Uiso R . . . . . H1091 H 1.0397 0.8297 0.2040 0.0510 1.0000 Uiso R . . . . . H1092 H 1.1757 0.8236 0.2575 0.0510 1.0000 Uiso R . . . . . H1093 H 1.0741 0.7334 0.2020 0.0510 1.0000 Uiso R . . . . . H1101 H 1.1380 0.7213 0.4278 0.0544 1.0000 Uiso R . . . . . H1102 H 1.2283 0.7588 0.3763 0.0544 1.0000 Uiso R . . . . . H1103 H 1.1197 0.6719 0.3237 0.0544 1.0000 Uiso R . . . . . H1111 H 0.8920 0.8735 0.5628 0.0548 1.0000 Uiso R . . . . . H1112 H 1.0501 0.8551 0.5586 0.0548 1.0000 Uiso R . . . . . H1113 H 0.9366 0.7701 0.5152 0.0548 1.0000 Uiso R . . . . . H1121 H 0.7453 0.9971 0.4525 0.0543 1.0000 Uiso R . . . . . H1122 H 0.8454 1.0088 0.5348 0.0543 1.0000 Uiso R . . . . . H1123 H 0.7199 0.9319 0.4973 0.0543 1.0000 Uiso R . . . . . H1131 H 0.7844 0.9757 0.3266 0.0664 1.0000 Uiso R . . . . . H1132 H 0.9283 0.9735 0.2898 0.0664 1.0000 Uiso R . . . . . H1133 H 0.8123 0.8916 0.2361 0.0664 1.0000 Uiso R . . . . . H1151 H 0.5165 0.6360 0.4310 0.0484 1.0000 Uiso R . . . . . H1152 H 0.4340 0.6274 0.3439 0.0484 1.0000 Uiso R . . . . . H1161 H 0.7067 0.5882 0.4304 0.0448 1.0000 Uiso R . . . . . H1171 H 0.9106 0.5177 0.3981 0.0606 1.0000 Uiso R . . . . . H1172 H 0.9391 0.6274 0.4516 0.0606 1.0000 Uiso R . . . . . H1173 H 0.9452 0.5767 0.3486 0.0606 1.0000 Uiso R . . . . . H1181 H 0.6987 0.4493 0.3029 0.0524 1.0000 Uiso R . . . . . H1182 H 0.7325 0.5049 0.2500 0.0524 1.0000 Uiso R . . . . . H1183 H 0.5905 0.5145 0.2905 0.0524 1.0000 Uiso R . . . . . H1191 H 0.4176 0.7482 0.3122 0.0371 1.0000 Uiso R . . . . . H1201 H 0.3634 0.9007 0.3784 0.0542 1.0000 Uiso R . . . . . H1202 H 0.5212 0.9326 0.4118 0.0542 1.0000 Uiso R . . . . . H1203 H 0.4389 0.8734 0.4478 0.0542 1.0000 Uiso R . . . . . H1211 H 0.4170 0.8255 0.2272 0.0611 1.0000 Uiso R . . . . . H1212 H 0.5767 0.8529 0.2559 0.0611 1.0000 Uiso R . . . . . H1213 H 0.5223 0.7469 0.1979 0.0611 1.0000 Uiso 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 0.0214(3) 0.0254(3) 0.0248(3) 0.0061(3) 0.0026(3) 0.0015(3) N1 0.0241(15) 0.0255(16) 0.0264(16) 0.0048(13) 0.0047(12) 0.0036(12) N2 0.0227(15) 0.0266(16) 0.0270(16) 0.0042(13) 0.0025(12) 0.0012(12) N3 0.0280(17) 0.0367(19) 0.0354(18) 0.0078(15) 0.0086(14) 0.0032(14) N4 0.0290(17) 0.0308(18) 0.0373(19) 0.0080(15) -0.0012(14) 0.0063(14) C1 0.044(2) 0.027(2) 0.038(2) 0.0136(18) 0.0045(18) 0.0032(18) C2 0.034(2) 0.034(2) 0.037(2) 0.0092(18) 0.0130(17) 0.0036(17) C3 0.0239(19) 0.037(2) 0.037(2) 0.0030(18) -0.0027(16) -0.0007(16) C4 0.0190(17) 0.0285(19) 0.0315(19) 0.0109(16) -0.0028(14) -0.0004(14) C5 0.0273(19) 0.041(2) 0.0277(19) 0.0153(18) -0.0046(15) -0.0076(17) C6 0.028(2) 0.036(2) 0.029(2) -0.0022(17) -0.0048(16) -0.0032(17) C7 0.029(2) 0.028(2) 0.045(2) 0.0133(18) -0.0078(17) -0.0064(16) C8 0.0231(18) 0.034(2) 0.037(2) 0.0148(17) -0.0020(16) -0.0051(16) C9 0.025(2) 0.042(2) 0.049(3) 0.014(2) -0.0043(18) 0.0042(18) C10 0.056(3) 0.074(4) 0.044(3) 0.037(3) -0.006(2) -0.013(3) C11 0.048(3) 0.052(3) 0.040(3) -0.009(2) 0.002(2) 0.002(2) C12 0.052(3) 0.036(3) 0.087(4) 0.027(3) -0.015(3) -0.005(2) C13 0.035(2) 0.063(3) 0.047(3) 0.035(2) 0.0061(19) -0.002(2) C14 0.029(2) 0.032(2) 0.034(2) -0.0019(18) 0.0063(17) 0.0033(17) C15 0.032(2) 0.060(3) 0.047(3) 0.007(2) 0.001(2) 0.007(2) C16 0.040(2) 0.057(3) 0.048(3) 0.019(2) 0.018(2) -0.003(2) C17 0.150(7) 0.082(5) 0.063(4) 0.024(4) 0.061(5) 0.005(5) C18 0.064(4) 0.062(4) 0.079(4) 0.037(3) 0.023(3) -0.008(3) C19 0.043(2) 0.042(3) 0.051(3) 0.022(2) -0.007(2) 0.008(2) C20 0.066(4) 0.058(3) 0.089(4) 0.038(3) -0.011(3) 0.012(3) C21 0.059(3) 0.071(4) 0.060(3) 0.043(3) 0.010(3) 0.013(3) I1 0.03578(15) 0.03262(15) 0.03058(14) 0.00896(11) 0.00266(11) 0.00351(11) Ti101 0.0186(3) 0.0246(3) 0.0230(3) 0.0094(3) 0.0032(2) -0.0001(2) N101 0.0287(16) 0.0337(17) 0.0238(15) 0.0105(13) 0.0029(12) -0.0044(13) N102 0.0387(18) 0.0363(18) 0.0223(15) 0.0058(14) 0.0063(13) -0.0057(15) N103 0.0265(15) 0.0296(16) 0.0238(15) 0.0135(13) 0.0045(12) 0.0074(13) N104 0.0180(14) 0.0255(16) 0.0371(17) 0.0128(14) 0.0063(13) 0.0022(12) C101 0.070(4) 0.103(5) 0.045(3) -0.008(3) -0.002(3) 0.043(4) C102 0.199(8) 0.077(4) 0.031(3) 0.019(3) 0.006(4) -0.056(5) C103 0.046(3) 0.073(4) 0.037(3) 0.002(2) 0.000(2) -0.016(3) C104 0.0214(17) 0.037(2) 0.0308(19) 0.0153(17) 0.0035(15) -0.0040(15) C105 0.0180(16) 0.035(2) 0.0277(18) 0.0113(16) 0.0030(14) -0.0039(15) C106 0.0223(18) 0.036(2) 0.0236(18) 0.0056(16) -0.0012(14) -0.0073(16) C107 0.0242(19) 0.026(2) 0.035(2) 0.0015(16) 0.0044(16) -0.0047(16) C108 0.0267(19) 0.028(2) 0.043(2) 0.0156(18) -0.0016(17) -0.0064(16) C109 0.032(2) 0.051(3) 0.038(2) 0.025(2) 0.0066(17) -0.0073(19) C110 0.0238(19) 0.059(3) 0.049(3) 0.031(2) 0.0078(18) 0.0081(19) C111 0.042(2) 0.061(3) 0.030(2) 0.016(2) 0.0045(19) -0.009(2) C112 0.037(2) 0.035(2) 0.061(3) -0.002(2) 0.016(2) -0.0016(19) C113 0.042(3) 0.040(3) 0.076(3) 0.035(3) -0.002(2) -0.006(2) C114 0.0242(18) 0.0275(19) 0.0239(17) 0.0076(15) 0.0040(14) -0.0022(15) C115 0.028(2) 0.048(3) 0.041(2) 0.023(2) 0.0059(17) -0.0061(18) C116 0.033(2) 0.040(2) 0.039(2) 0.0266(19) 0.0056(17) 0.0048(17) C117 0.035(2) 0.054(3) 0.060(3) 0.038(2) 0.010(2) 0.012(2) C118 0.051(3) 0.031(2) 0.050(3) 0.020(2) 0.003(2) 0.002(2) C119 0.0208(18) 0.026(2) 0.044(2) 0.0070(17) 0.0034(16) 0.0018(15) C120 0.034(2) 0.043(3) 0.059(3) 0.006(2) 0.000(2) 0.016(2) C121 0.037(2) 0.055(3) 0.060(3) 0.035(3) 0.005(2) 0.010(2) I101 0.04476(17) 0.05082(19) 0.03015(15) 0.00606(13) 0.00382(12) 0.00621(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2113(2) 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 . 1.728(3) yes Ti1 . N3 . 2.090(3) yes Ti1 . N4 . 2.078(3) yes Ti1 . C4 . 2.375(3) yes Ti1 . C5 . 2.379(4) yes Ti1 . C6 . 2.421(4) yes Ti1 . C7 . 2.409(4) yes Ti1 . C8 . 2.371(4) yes N1 . N2 . 1.419(4) yes N2 . C1 . 1.502(5) yes N2 . C2 . 1.493(5) yes N2 . C3 . 1.503(5) yes N3 . C14 . 1.322(6) yes N3 . C16 . 1.469(6) yes N4 . C14 . 1.335(6) yes N4 . C19 . 1.469(6) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C3 . H31 . 1.000 no C3 . H32 . 1.000 no C3 . H33 . 1.000 no C4 . C5 . 1.426(5) yes C4 . C8 . 1.414(6) yes C4 . C9 . 1.504(6) yes C5 . C6 . 1.428(6) yes C5 . C10 . 1.507(6) yes C6 . C7 . 1.414(6) yes C6 . C11 . 1.503(6) yes C7 . C8 . 1.411(6) yes C7 . C12 . 1.501(7) yes C8 . C13 . 1.506(6) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . H63 . 1.049 no C11 . H111 . 1.000 no C11 . H112 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.002 no C14 . C15 . 1.510(6) yes C15 . H151 . 1.000 no C15 . H152 . 1.000 no C15 . H153 . 1.000 no C16 . C17 . 1.515(7) yes C16 . C18 . 1.506(8) yes C16 . H161 . 1.000 no C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no C18 . H183 . 1.000 no C19 . C20 . 1.515(7) yes C19 . C21 . 1.486(7) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no H55 . C115 . 1.152 no Ti101 . N101 . 1.728(3) yes Ti101 . N103 . 2.066(3) yes Ti101 . N104 . 2.079(3) yes Ti101 . C104 . 2.374(4) yes Ti101 . C105 . 2.378(3) yes Ti101 . C106 . 2.419(4) yes Ti101 . C107 . 2.434(4) yes Ti101 . C108 . 2.390(4) yes N101 . N102 . 1.422(4) yes N102 . C101 . 1.491(7) yes N102 . C102 . 1.454(7) yes N102 . C103 . 1.474(6) yes N103 . C114 . 1.343(5) yes N103 . C116 . 1.475(5) yes N104 . C114 . 1.333(5) yes N104 . C119 . 1.475(5) yes C101 . H1011 . 1.000 no C101 . H1012 . 1.000 no C101 . H1013 . 1.000 no C102 . H1021 . 1.000 no C102 . H1022 . 1.000 no C102 . H1023 . 1.000 no C103 . H1031 . 1.000 no C103 . H1032 . 1.000 no C103 . H1033 . 1.000 no C104 . C105 . 1.420(6) yes C104 . C108 . 1.420(6) yes C104 . C109 . 1.501(5) yes C105 . C106 . 1.418(5) yes C105 . C110 . 1.503(6) yes C106 . C107 . 1.406(6) yes C106 . C111 . 1.511(6) yes C107 . C108 . 1.430(6) yes C107 . C112 . 1.510(6) yes C108 . C113 . 1.492(6) yes C109 . H1091 . 1.000 no C109 . H1092 . 1.000 no C109 . H1093 . 1.000 no C110 . H1101 . 1.000 no C110 . H1102 . 1.000 no C110 . H1103 . 1.000 no C111 . H1111 . 1.000 no C111 . H1112 . 1.000 no C111 . H1113 . 1.000 no C112 . H1121 . 1.000 no C112 . H1122 . 1.000 no C112 . H1123 . 1.000 no C113 . H1131 . 1.000 no C113 . H1132 . 1.000 no C113 . H1133 . 1.000 no C114 . C115 . 1.510(5) yes C115 . H1151 . 1.000 no C115 . H1152 . 1.000 no C116 . C117 . 1.520(6) yes C116 . C118 . 1.531(6) yes C116 . H1161 . 1.000 no C117 . H1171 . 1.000 no C117 . H1172 . 1.000 no C117 . H1173 . 1.000 no C118 . H1181 . 1.000 no C118 . H1182 . 1.000 no C118 . H1183 . 1.000 no C119 . C120 . 1.514(6) yes C119 . C121 . 1.524(6) yes C119 . H1191 . 1.000 no C120 . H1201 . 1.000 no C120 . H1202 . 1.000 no C120 . H1203 . 1.000 no C121 . H1211 . 1.000 no C121 . H1212 . 1.000 no C121 . H1213 . 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 N1 . Ti1 . N3 . 108.42(14) yes N1 . Ti1 . N4 . 105.55(14) yes N3 . Ti1 . N4 . 64.87(15) yes N1 . Ti1 . C4 . 95.27(14) yes N3 . Ti1 . C4 . 134.34(14) yes N4 . Ti1 . C4 . 144.88(14) yes N1 . Ti1 . C5 . 118.52(15) yes N3 . Ti1 . C5 . 99.99(14) yes N4 . Ti1 . C5 . 135.92(14) yes C4 . Ti1 . C5 . 34.92(13) yes N1 . Ti1 . C6 . 151.87(15) yes N3 . Ti1 . C6 . 89.42(14) yes N4 . Ti1 . C6 . 101.66(14) yes C4 . Ti1 . C6 . 57.48(13) yes C5 . Ti1 . C6 . 34.61(15) yes N1 . Ti1 . C7 . 138.71(15) yes N3 . Ti1 . C7 . 112.74(14) yes N4 . Ti1 . C7 . 89.23(14) yes C4 . Ti1 . C7 . 57.33(14) yes C5 . Ti1 . C7 . 57.29(14) yes N1 . Ti1 . C8 . 105.49(14) yes N3 . Ti1 . C8 . 145.60(14) yes N4 . Ti1 . C8 . 111.10(14) yes C4 . Ti1 . C8 . 34.66(14) yes C5 . Ti1 . C8 . 57.67(14) yes C6 . Ti1 . C7 . 34.03(15) yes C6 . Ti1 . C8 . 57.04(14) yes C7 . Ti1 . C8 . 34.32(14) yes Ti1 . N1 . N2 . 173.5(3) yes N1 . N2 . C1 . 110.3(3) yes N1 . N2 . C2 . 110.3(3) yes C1 . N2 . C2 . 109.7(3) yes N1 . N2 . C3 . 108.1(3) yes C1 . N2 . C3 . 108.9(3) yes C2 . N2 . C3 . 109.5(3) yes Ti1 . N3 . C14 . 89.3(2) yes Ti1 . N3 . C16 . 142.0(3) yes C14 . N3 . C16 . 122.0(4) yes Ti1 . N4 . C14 . 89.4(3) yes Ti1 . N4 . C19 . 139.6(3) yes C14 . N4 . C19 . 121.2(4) yes N2 . C1 . H11 . 109.7 no N2 . C1 . H12 . 109.2 no H11 . C1 . H12 . 109.5 no N2 . C1 . H13 . 109.5 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no N2 . C2 . H21 . 109.6 no N2 . C2 . H22 . 109.4 no H21 . C2 . H22 . 109.5 no N2 . C2 . H23 . 109.4 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no N2 . C3 . H31 . 109.4 no N2 . C3 . H32 . 109.3 no H31 . C3 . H32 . 109.5 no N2 . C3 . H33 . 109.7 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no Ti1 . C4 . C5 . 72.7(2) yes Ti1 . C4 . C8 . 72.5(2) yes C5 . C4 . C8 . 107.5(3) yes Ti1 . C4 . C9 . 124.8(3) yes C5 . C4 . C9 . 124.3(4) yes C8 . C4 . C9 . 127.9(4) yes Ti1 . C5 . C4 . 72.4(2) yes Ti1 . C5 . C6 . 74.3(2) yes C4 . C5 . C6 . 107.8(4) yes Ti1 . C5 . C10 . 122.9(3) yes C4 . C5 . C10 . 124.4(4) yes C6 . C5 . C10 . 127.6(4) yes Ti1 . C6 . C5 . 71.1(2) yes Ti1 . C6 . C7 . 72.5(2) yes C5 . C6 . C7 . 107.7(4) yes Ti1 . C6 . C11 . 122.9(3) yes C5 . C6 . C11 . 127.9(4) yes C7 . C6 . C11 . 124.4(4) yes Ti1 . C7 . C6 . 73.5(2) yes Ti1 . C7 . C8 . 71.4(2) yes C6 . C7 . C8 . 108.3(4) yes Ti1 . C7 . C12 . 124.0(3) yes C6 . C7 . C12 . 125.0(4) yes C8 . C7 . C12 . 126.6(4) yes Ti1 . C8 . C4 . 72.8(2) yes Ti1 . C8 . C7 . 74.3(2) yes C4 . C8 . C7 . 108.7(4) yes Ti1 . C8 . C13 . 121.9(3) yes C4 . C8 . C13 . 125.6(4) yes C7 . C8 . C13 . 125.6(4) yes C4 . C9 . H91 . 109.5 no C4 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no C4 . C9 . H93 . 109.3 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C5 . C10 . H101 . 109.2 no C5 . C10 . H102 . 109.9 no H101 . C10 . H102 . 109.5 no C5 . C10 . H103 . 109.4 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no C6 . C11 . H63 . 118.6 no C6 . C11 . H111 . 106.6 no H63 . C11 . H111 . 107.2 no C6 . C11 . H112 . 107.6 no H63 . C11 . H112 . 107.2 no H111 . C11 . H112 . 109.5 no C7 . C12 . H121 . 109.0 no C7 . C12 . H122 . 109.5 no H121 . C12 . H122 . 109.5 no C7 . C12 . H123 . 109.9 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no C8 . C13 . H131 . 105.3 no C8 . C13 . H132 . 124.4 no H131 . C13 . H132 . 105.7 no C8 . C13 . H133 . 106.7 no H131 . C13 . H133 . 108.9 no H132 . C13 . H133 . 105.3 no N4 . C14 . N3 . 114.5(4) yes N4 . C14 . C15 . 121.9(4) yes N3 . C14 . C15 . 123.5(4) yes C14 . C15 . H151 . 109.3 no C14 . C15 . H152 . 109.6 no H151 . C15 . H152 . 109.5 no C14 . C15 . H153 . 109.5 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 109.5 no N3 . C16 . C17 . 111.0(4) yes N3 . C16 . C18 . 110.0(4) yes C17 . C16 . C18 . 111.4(5) yes N3 . C16 . H161 . 108.1 no C17 . C16 . H161 . 108.2 no C18 . C16 . H161 . 108.0 no C16 . C17 . H171 . 109.9 no C16 . C17 . H172 . 108.8 no H171 . C17 . H172 . 109.5 no C16 . C17 . H173 . 109.7 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no C16 . C18 . H181 . 109.8 no C16 . C18 . H182 . 108.6 no H181 . C18 . H182 . 109.5 no C16 . C18 . H183 . 110.0 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no N4 . C19 . C20 . 111.2(4) yes N4 . C19 . C21 . 110.3(4) yes C20 . C19 . C21 . 112.0(5) yes N4 . C19 . H191 . 107.7 no C20 . C19 . H191 . 107.5 no C21 . C19 . H191 . 107.9 no C19 . C20 . H201 . 109.9 no C19 . C20 . H202 . 108.7 no H201 . C20 . H202 . 109.5 no C19 . C20 . H203 . 109.8 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C19 . C21 . H211 . 109.9 no C19 . C21 . H212 . 109.1 no H211 . C21 . H212 . 109.5 no C19 . C21 . H213 . 109.4 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no N101 . Ti101 . N103 . 104.52(14) yes N101 . Ti101 . N104 . 106.49(14) yes N103 . Ti101 . N104 . 65.25(12) yes N101 . Ti101 . C104 . 96.97(14) yes N103 . Ti101 . C104 . 140.36(13) yes N104 . Ti101 . C104 . 138.64(13) yes N101 . Ti101 . C105 . 113.69(14) yes N103 . Ti101 . C105 . 105.60(13) yes N104 . Ti101 . C105 . 139.73(13) yes C104 . Ti101 . C105 . 34.77(13) yes N101 . Ti101 . C106 . 148.05(14) yes N103 . Ti101 . C106 . 89.23(13) yes N104 . Ti101 . C106 . 105.46(13) yes C104 . Ti101 . C106 . 57.25(13) yes C105 . Ti101 . C106 . 34.38(12) yes N101 . Ti101 . C107 . 147.96(15) yes N103 . Ti101 . C107 . 107.52(13) yes N104 . Ti101 . C107 . 87.52(12) yes C104 . Ti101 . C107 . 56.92(13) yes C105 . Ti101 . C107 . 56.66(13) yes N101 . Ti101 . C108 . 113.50(15) yes N103 . Ti101 . C108 . 141.95(13) yes N104 . Ti101 . C108 . 103.98(13) yes C104 . Ti101 . C108 . 34.69(14) yes C105 . Ti101 . C108 . 57.71(14) yes C106 . Ti101 . C107 . 33.67(14) yes C106 . Ti101 . C108 . 57.24(14) yes C107 . Ti101 . C108 . 34.47(14) yes Ti101 . N101 . N102 . 175.6(3) yes N101 . N102 . C101 . 109.2(3) yes N101 . N102 . C102 . 110.3(4) yes C101 . N102 . C102 . 108.9(6) yes N101 . N102 . C103 . 109.1(3) yes C101 . N102 . C103 . 107.5(5) yes C102 . N102 . C103 . 111.7(5) yes Ti101 . N103 . C114 . 90.2(2) yes Ti101 . N103 . C116 . 138.4(2) yes C114 . N103 . C116 . 120.4(3) yes Ti101 . N104 . C114 . 89.9(2) yes Ti101 . N104 . C119 . 142.0(3) yes C114 . N104 . C119 . 121.6(3) yes N102 . C101 . H1011 . 109.9 no N102 . C101 . H1012 . 110.1 no H1011 . C101 . H1012 . 109.5 no N102 . C101 . H1013 . 108.5 no H1011 . C101 . H1013 . 109.5 no H1012 . C101 . H1013 . 109.5 no N102 . C102 . H1021 . 109.9 no N102 . C102 . H1022 . 110.1 no H1021 . C102 . H1022 . 109.5 no N102 . C102 . H1023 . 108.3 no H1021 . C102 . H1023 . 109.5 no H1022 . C102 . H1023 . 109.5 no N102 . C103 . H1031 . 109.6 no N102 . C103 . H1032 . 109.5 no H1031 . C103 . H1032 . 109.5 no N102 . C103 . H1033 . 109.4 no H1031 . C103 . H1033 . 109.5 no H1032 . C103 . H1033 . 109.5 no Ti101 . C104 . C105 . 72.8(2) yes Ti101 . C104 . C108 . 73.3(2) yes C105 . C104 . C108 . 108.2(3) yes Ti101 . C104 . C109 . 126.1(3) yes C105 . C104 . C109 . 125.4(4) yes C108 . C104 . C109 . 125.9(4) yes Ti101 . C105 . C104 . 72.5(2) yes Ti101 . C105 . C106 . 74.4(2) yes C104 . C105 . C106 . 108.1(3) yes Ti101 . C105 . C110 . 123.5(3) yes C104 . C105 . C110 . 125.7(3) yes C106 . C105 . C110 . 126.0(4) yes Ti101 . C106 . C105 . 71.2(2) yes Ti101 . C106 . C107 . 73.7(2) yes C105 . C106 . C107 . 108.0(3) yes Ti101 . C106 . C111 . 124.3(3) yes C105 . C106 . C111 . 126.3(4) yes C107 . C106 . C111 . 125.5(4) yes Ti101 . C107 . C106 . 72.6(2) yes Ti101 . C107 . C108 . 71.1(2) yes C106 . C107 . C108 . 108.7(3) yes Ti101 . C107 . C112 . 126.5(3) yes C106 . C107 . C112 . 124.3(4) yes C108 . C107 . C112 . 126.8(4) yes Ti101 . C108 . C107 . 74.4(2) yes Ti101 . C108 . C104 . 72.0(2) yes C107 . C108 . C104 . 107.0(4) yes Ti101 . C108 . C113 . 123.1(3) yes C107 . C108 . C113 . 128.0(4) yes C104 . C108 . C113 . 124.7(4) yes C104 . C109 . H1091 . 109.2 no C104 . C109 . H1092 . 109.8 no H1091 . C109 . H1092 . 109.5 no C104 . C109 . H1093 . 109.4 no H1091 . C109 . H1093 . 109.5 no H1092 . C109 . H1093 . 109.5 no C105 . C110 . H1101 . 109.6 no C105 . C110 . H1102 . 109.6 no H1101 . C110 . H1102 . 109.5 no C105 . C110 . H1103 . 109.2 no H1101 . C110 . H1103 . 109.5 no H1102 . C110 . H1103 . 109.5 no C106 . C111 . H1111 . 109.4 no C106 . C111 . H1112 . 109.6 no H1111 . C111 . H1112 . 109.5 no C106 . C111 . H1113 . 109.4 no H1111 . C111 . H1113 . 109.5 no H1112 . C111 . H1113 . 109.5 no C107 . C112 . H1121 . 109.4 no C107 . C112 . H1122 . 109.5 no H1121 . C112 . H1122 . 109.5 no C107 . C112 . H1123 . 109.6 no H1121 . C112 . H1123 . 109.5 no H1122 . C112 . H1123 . 109.5 no C108 . C113 . H1131 . 109.2 no C108 . C113 . H1132 . 109.5 no H1131 . C113 . H1132 . 109.5 no C108 . C113 . H1133 . 109.6 no H1131 . C113 . H1133 . 109.5 no H1132 . C113 . H1133 . 109.5 no N103 . C114 . N104 . 113.3(3) yes N103 . C114 . C115 . 124.0(4) yes N104 . C114 . C115 . 122.7(3) yes C114 . C115 . H55 . 105.0 no C114 . C115 . H1151 . 110.5 no H55 . C115 . H1151 . 110.6 no C114 . C115 . H1152 . 110.6 no H55 . C115 . H1152 . 110.6 no H1151 . C115 . H1152 . 109.5 no N103 . C116 . C117 . 108.4(3) yes N103 . C116 . C118 . 112.3(3) yes C117 . C116 . C118 . 110.4(4) yes N103 . C116 . H1161 . 108.4 no C117 . C116 . H1161 . 108.6 no C118 . C116 . H1161 . 108.7 no C116 . C117 . H1171 . 109.6 no C116 . C117 . H1172 . 109.8 no H1171 . C117 . H1172 . 109.5 no C116 . C117 . H1173 . 109.0 no H1171 . C117 . H1173 . 109.5 no H1172 . C117 . H1173 . 109.5 no C116 . C118 . H1181 . 109.6 no C116 . C118 . H1182 . 109.2 no H1181 . C118 . H1182 . 109.5 no C116 . C118 . H1183 . 109.6 no H1181 . C118 . H1183 . 109.5 no H1182 . C118 . H1183 . 109.5 no N104 . C119 . C120 . 112.2(3) yes N104 . C119 . C121 . 109.1(3) yes C120 . C119 . C121 . 111.9(4) yes N104 . C119 . H1191 . 107.6 no C120 . C119 . H1191 . 107.8 no C121 . C119 . H1191 . 108.0 no C119 . C120 . H1201 . 110.1 no C119 . C120 . H1202 . 109.0 no H1201 . C120 . H1202 . 109.5 no C119 . C120 . H1203 . 109.3 no H1201 . C120 . H1203 . 109.5 no H1202 . C120 . H1203 . 109.5 no C119 . C121 . H1211 . 109.6 no C119 . C121 . H1212 . 109.2 no H1211 . C121 . H1212 . 109.5 no C119 . C121 . H1213 . 109.6 no H1211 . C121 . H1213 . 109.5 no H1212 . C121 . H1213 . 109.5 no #===end data_compound_21-Br _database_code_depnum_ccdc_archive 'CCDC 849355' #TrackingRef '- Mountford Xray SI.CIF' # local code PJT15 _chemical_name_systematic ; [Cp*Ti{MeC(NiPr)2}(NNMe2Et)]Br ; _chemical_melting_point ? _publ_section_exptl_refinement ; One of the NMe2Et groups of (based on N(6)) showed evidence of positional disorder. Attempts to find a reasonable model were unsuccessful and so loose similarity restraints were applied to the APDs and certain N-C bond distances. H atoms were placed in calculated positions and refined in a riding model. The maximum residual electron density in the final Fourier difference map was located close to the disordered NNMe2Et moiety. ; _cell_length_a 10.2911(5) _cell_length_b 16.2599(6) _cell_length_c 18.4540(9) _cell_angle_alpha 69.245(2) _cell_angle_beta 78.120(2) _cell_angle_gamma 86.849(2) _cell_volume 2825.2(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C24 H47 Br1 N4 O0.50 Ti1' _chemical_formula_moiety 'C22 H43 Br1 N4 Ti1, 0.5 (C4 H8 O)' _chemical_compound_source ? _chemical_formula_weight 527.47 _cell_measurement_reflns_used 9780 _cell_measurement_theta_min 5 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description lath _exptl_crystal_colour red _exptl_crystal_size_min 0.010 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_max 0.100 _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 17928 _reflns_number_total 10863 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_min 5.110 _diffrn_reflns_theta_max 26.031 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.251 _diffrn_measured_fraction_theta_full 0.982 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -18 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 3.29 _oxford_diffrn_Wilson_scale 8.46 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.79 _refine_diff_density_max 0.76 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 6564 _refine_ls_number_restraints 37 _refine_ls_number_parameters 550 _oxford_refine_ls_R_factor_ref 0.0780 _refine_ls_wR_factor_ref 0.0737 _refine_ls_goodness_of_fit_ref 1.1080 _refine_ls_shift/su_max 0.0007800 _refine_ls_shift/su_mean 0.0000164 # The values computed from all data _oxford_reflns_number_all 10863 _refine_ls_R_factor_all 0.1474 _refine_ls_wR_factor_all 0.0993 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7621 _refine_ls_R_factor_gt 0.0945 _refine_ls_wR_factor_gt 0.0769 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none _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: 2.40 -0.418E-01 1.84 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # 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_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.58735(11) 0.83240(7) 0.26298(7) 0.0359 1.0000 Uani . . . . . . N1 N 0.5460(5) 0.9141(4) 0.3018(3) 0.0424 1.0000 Uani . . . . . . N2 N 0.5173(5) 0.9834(3) 0.3328(3) 0.0421 1.0000 Uani D . . . . . N3 N 0.6597(5) 0.7300(4) 0.3493(3) 0.0431 1.0000 Uani . . . . . . N4 N 0.7938(5) 0.8253(4) 0.2451(3) 0.0442 1.0000 Uani . . . . . . C1 C 0.4623(8) 1.0601(4) 0.2747(4) 0.0554 1.0000 Uani D . . . . . C2 C 0.4178(6) 0.9519(5) 0.4088(4) 0.0528 1.0000 Uani D . . . . . C3 C 0.6440(6) 1.0115(5) 0.3477(5) 0.0491 1.0000 Uani D . . . . . C4 C 0.7072(7) 0.9407(5) 0.4054(5) 0.0543 1.0000 Uani . . . . . . C5 C 0.7841(7) 0.7648(5) 0.3175(5) 0.0476 1.0000 Uani . . . . . . C6 C 0.8974(7) 0.7398(6) 0.3604(5) 0.0590 1.0000 Uani . . . . . . C7 C 0.6207(7) 0.6768(5) 0.4321(5) 0.0524 1.0000 Uani . . . . . . C8 C 0.4691(8) 0.6835(5) 0.4578(5) 0.0564 1.0000 Uani . . . . . . C9 C 0.6613(8) 0.5823(5) 0.4501(5) 0.0596 1.0000 Uani . . . . . . C10 C 0.9180(7) 0.8758(5) 0.2039(4) 0.0494 1.0000 Uani . . . . . . C11 C 0.8904(9) 0.9710(6) 0.1599(6) 0.0744 1.0000 Uani . . . . . . C12 C 1.0012(9) 0.8361(7) 0.1477(6) 0.0774 1.0000 Uani . . . . . . C13 C 0.3923(6) 0.7855(5) 0.2366(4) 0.0409 1.0000 Uani . . . . . . C14 C 0.4345(6) 0.8677(5) 0.1773(4) 0.0415 1.0000 Uani . . . . . . C15 C 0.5596(6) 0.8562(5) 0.1314(4) 0.0452 1.0000 Uani . . . . . . C16 C 0.5919(6) 0.7655(5) 0.1637(4) 0.0431 1.0000 Uani . . . . . . C17 C 0.4902(6) 0.7232(4) 0.2274(4) 0.0386 1.0000 Uani . . . . . . C18 C 0.2631(6) 0.7682(5) 0.2941(5) 0.0498 1.0000 Uani . . . . . . C19 C 0.3565(7) 0.9512(5) 0.1594(4) 0.0495 1.0000 Uani . . . . . . C20 C 0.6341(7) 0.9228(6) 0.0598(4) 0.0577 1.0000 Uani . . . . . . C21 C 0.7119(7) 0.7218(5) 0.1326(4) 0.0504 1.0000 Uani . . . . . . C22 C 0.4796(8) 0.6254(5) 0.2740(5) 0.0521 1.0000 Uani . . . . . . Br1 Br 0.49813(8) 0.79417(5) 0.60291(5) 0.0542 1.0000 Uani . . . . . . Ti2 Ti 0.96544(11) 0.65597(8) 0.75870(7) 0.0394 1.0000 Uani . . . . . . N5 N 0.9894(7) 0.7315(4) 0.6645(3) 0.0547 1.0000 Uani . U . . . . N6 N 1.0017(7) 0.7953(4) 0.5885(4) 0.0723 1.0000 Uani D U . . . . N7 N 1.0092(5) 0.7235(4) 0.8279(3) 0.0444 1.0000 Uani . . . . . . N8 N 1.1527(5) 0.6332(4) 0.7870(3) 0.0426 1.0000 Uani . . . . . . C27 C 0.8759(10) 0.8492(8) 0.5833(7) 0.1106 1.0000 Uani D U . . . . C28 C 1.1057(9) 0.8617(6) 0.5769(6) 0.0765 1.0000 Uani D U . . . . C29 C 0.9874(11) 0.7587(7) 0.5267(6) 0.0973 1.0000 Uani D U . . . . C30 C 1.0914(11) 0.6868(8) 0.5253(6) 0.1014 1.0000 Uani D U . . . . C31 C 1.1379(7) 0.7013(5) 0.8132(4) 0.0435 1.0000 Uani . . . . . . C32 C 1.2517(8) 0.7481(5) 0.8213(5) 0.0576 1.0000 Uani . . . . . . C33 C 0.9730(8) 0.8033(5) 0.8477(4) 0.0528 1.0000 Uani . . . . . . C34 C 0.8365(8) 0.8308(6) 0.8297(5) 0.0646 1.0000 Uani . . . . . . C35 C 0.9737(9) 0.7878(6) 0.9329(5) 0.0657 1.0000 Uani . . . . . . C36 C 1.2866(7) 0.6061(5) 0.7590(5) 0.0497 1.0000 Uani . . . . . . C37 C 1.2850(8) 0.5698(6) 0.6956(5) 0.0633 1.0000 Uani . . . . . . C38 C 1.3373(8) 0.5383(6) 0.8299(5) 0.0649 1.0000 Uani . . . . . . C39 C 0.7986(7) 0.5718(5) 0.8707(4) 0.0540 1.0000 Uani . . . . . . C40 C 0.7383(7) 0.6103(5) 0.8022(4) 0.0531 1.0000 Uani . . . . . . C41 C 0.7929(7) 0.5720(5) 0.7457(4) 0.0490 1.0000 Uani . . . . . . C42 C 0.8921(7) 0.5128(5) 0.7743(5) 0.0538 1.0000 Uani . . . . . . C43 C 0.8942(8) 0.5109(5) 0.8531(4) 0.0541 1.0000 Uani . . . . . . C44 C 0.7623(9) 0.5854(6) 0.9471(5) 0.0696 1.0000 Uani . . . . . . C45 C 0.6277(7) 0.6755(6) 0.7980(5) 0.0618 1.0000 Uani . . . . . . C46 C 0.7468(8) 0.5908(5) 0.6689(5) 0.0578 1.0000 Uani . . . . . . C47 C 0.9609(9) 0.4512(5) 0.7354(6) 0.0674 1.0000 Uani . . . . . . C48 C 0.9756(9) 0.4533(6) 0.9088(6) 0.0709 1.0000 Uani . . . . . . Br2 Br 1.08251(7) 0.95727(5) 0.34553(4) 0.0471 1.0000 Uani . . . . . . O1 O 0.4371(12) 0.6871(9) -0.0217(7) 0.1436 1.0000 Uani . . . . . . C23 C 0.3873(12) 0.6468(9) 0.0581(8) 0.1014 1.0000 Uani . . . . . . C24 C 0.2928(11) 0.7130(9) 0.0807(7) 0.0932 1.0000 Uani . . . . . . C25 C 0.3353(12) 0.7961(8) 0.0215(7) 0.0930 1.0000 Uani . . . . . . C26 C 0.4522(16) 0.7772(9) -0.0315(8) 0.1149 1.0000 Uani . . . . . . H11 H 0.4446 1.1063 0.2953 0.0683 1.0000 Uiso R . . . . . H12 H 0.5251 1.0801 0.2262 0.0683 1.0000 Uiso R . . . . . H13 H 0.3823 1.0425 0.2657 0.0683 1.0000 Uiso R . . . . . H21 H 0.3380 0.9345 0.3994 0.0682 1.0000 Uiso R . . . . . H22 H 0.4000 0.9984 0.4291 0.0682 1.0000 Uiso R . . . . . H23 H 0.4518 0.9033 0.4460 0.0682 1.0000 Uiso R . . . . . H31 H 0.6240 1.0588 0.3667 0.0692 1.0000 Uiso R . . . . . H32 H 0.7062 1.0311 0.2989 0.0692 1.0000 Uiso R . . . . . H41 H 0.7279 0.8933 0.3866 0.0735 1.0000 Uiso R . . . . . H42 H 0.7860 0.9620 0.4126 0.0735 1.0000 Uiso R . . . . . H43 H 0.6457 0.9210 0.4544 0.0735 1.0000 Uiso R . . . . . H61 H 0.9751 0.7724 0.3279 0.0748 1.0000 Uiso R . . . . . H62 H 0.8762 0.7519 0.4081 0.0748 1.0000 Uiso R . . . . . H63 H 0.9129 0.6788 0.3721 0.0748 1.0000 Uiso R . . . . . H71 H 0.6626 0.7006 0.4617 0.0640 1.0000 Uiso R . . . . . H81 H 0.4466 0.7431 0.4498 0.0682 1.0000 Uiso R . . . . . H82 H 0.4419 0.6489 0.5122 0.0682 1.0000 Uiso R . . . . . H83 H 0.4255 0.6623 0.4270 0.0682 1.0000 Uiso R . . . . . H91 H 0.7551 0.5791 0.4359 0.0765 1.0000 Uiso R . . . . . H92 H 0.6205 0.5573 0.4208 0.0765 1.0000 Uiso R . . . . . H93 H 0.6330 0.5506 0.5051 0.0765 1.0000 Uiso R . . . . . H101 H 0.9676 0.8739 0.2425 0.0625 1.0000 Uiso R . . . . . H111 H 0.9721 1.0022 0.1338 0.0917 1.0000 Uiso R . . . . . H112 H 0.8434 0.9963 0.1965 0.0917 1.0000 Uiso R . . . . . H113 H 0.8386 0.9742 0.1219 0.0917 1.0000 Uiso R . . . . . H121 H 1.0224 0.7773 0.1756 0.0984 1.0000 Uiso R . . . . . H122 H 0.9528 0.8366 0.1089 0.0984 1.0000 Uiso R . . . . . H123 H 1.0808 0.8700 0.1225 0.0984 1.0000 Uiso R . . . . . H181 H 0.2589 0.7080 0.3271 0.0610 1.0000 Uiso R . . . . . H182 H 0.2570 0.8040 0.3256 0.0610 1.0000 Uiso R . . . . . H183 H 0.1916 0.7804 0.2667 0.0610 1.0000 Uiso R . . . . . H191 H 0.2770 0.9415 0.1448 0.0602 1.0000 Uiso R . . . . . H192 H 0.4076 0.9971 0.1171 0.0602 1.0000 Uiso R . . . . . H193 H 0.3353 0.9674 0.2050 0.0602 1.0000 Uiso R . . . . . H201 H 0.7145 0.8989 0.0406 0.0736 1.0000 Uiso R . . . . . H202 H 0.6538 0.9725 0.0717 0.0736 1.0000 Uiso R . . . . . H203 H 0.5811 0.9403 0.0206 0.0736 1.0000 Uiso R . . . . . H211 H 0.7117 0.7274 0.0796 0.0671 1.0000 Uiso R . . . . . H212 H 0.7097 0.6612 0.1645 0.0671 1.0000 Uiso R . . . . . H213 H 0.7900 0.7490 0.1342 0.0671 1.0000 Uiso R . . . . . H221 H 0.5577 0.5974 0.2576 0.0653 1.0000 Uiso R . . . . . H222 H 0.4046 0.6010 0.2656 0.0653 1.0000 Uiso R . . . . . H223 H 0.4695 0.6166 0.3286 0.0653 1.0000 Uiso R . . . . . H231 H 0.4583 0.6384 0.0856 0.1315 1.0000 Uiso R . . . . . H232 H 0.3453 0.5918 0.0697 0.1315 1.0000 Uiso R . . . . . H241 H 0.2939 0.7134 0.1319 0.1238 1.0000 Uiso R . . . . . H242 H 0.2058 0.6986 0.0786 0.1238 1.0000 Uiso R . . . . . H251 H 0.3581 0.8347 0.0455 0.1158 1.0000 Uiso R . . . . . H252 H 0.2669 0.8211 -0.0067 0.1158 1.0000 Uiso R . . . . . H261 H 0.4523 0.8115 -0.0852 0.1490 1.0000 Uiso R . . . . . H262 H 0.5325 0.7880 -0.0183 0.1490 1.0000 Uiso R . . . . . H271 H 0.8666 0.8774 0.6212 0.1178 1.0000 Uiso R . . . . . H272 H 0.8832 0.8925 0.5319 0.1178 1.0000 Uiso R . . . . . H273 H 0.8003 0.8125 0.5945 0.1178 1.0000 Uiso R . . . . . H281 H 1.0811 0.8894 0.6152 0.0967 1.0000 Uiso R . . . . . H282 H 1.1877 0.8330 0.5830 0.0967 1.0000 Uiso R . . . . . H283 H 1.1149 0.9048 0.5254 0.0967 1.0000 Uiso R . . . . . H291 H 1.0005 0.8045 0.4764 0.1209 1.0000 Uiso R . . . . . H292 H 0.9016 0.7327 0.5382 0.1209 1.0000 Uiso R . . . . . H301 H 1.0864 0.6621 0.4864 0.1260 1.0000 Uiso R . . . . . H302 H 1.0777 0.6417 0.5760 0.1260 1.0000 Uiso R . . . . . H303 H 1.1766 0.7135 0.5142 0.1260 1.0000 Uiso R . . . . . H321 H 1.2407 0.7444 0.8748 0.0724 1.0000 Uiso R . . . . . H322 H 1.3324 0.7212 0.8070 0.0724 1.0000 Uiso R . . . . . H323 H 1.2545 0.8082 0.7880 0.0724 1.0000 Uiso R . . . . . H331 H 1.0343 0.8498 0.8155 0.0641 1.0000 Uiso R . . . . . H341 H 0.8379 0.8417 0.7754 0.0794 1.0000 Uiso R . . . . . H342 H 0.8091 0.8822 0.8416 0.0794 1.0000 Uiso R . . . . . H343 H 0.7761 0.7836 0.8615 0.0794 1.0000 Uiso R . . . . . H351 H 0.9505 0.8400 0.9441 0.0772 1.0000 Uiso R . . . . . H352 H 1.0590 0.7699 0.9441 0.0772 1.0000 Uiso R . . . . . H353 H 0.9100 0.7426 0.9647 0.0772 1.0000 Uiso R . . . . . H361 H 1.3447 0.6561 0.7382 0.0634 1.0000 Uiso R . . . . . H371 H 1.2257 0.5205 0.7162 0.0808 1.0000 Uiso R . . . . . H372 H 1.3710 0.5523 0.6765 0.0808 1.0000 Uiso R . . . . . H373 H 1.2544 0.6142 0.6535 0.0808 1.0000 Uiso R . . . . . H381 H 1.4244 0.5202 0.8135 0.0814 1.0000 Uiso R . . . . . H382 H 1.2784 0.4887 0.8513 0.0814 1.0000 Uiso R . . . . . H383 H 1.3378 0.5635 0.8690 0.0814 1.0000 Uiso R . . . . . H441 H 0.7725 0.6459 0.9388 0.0836 1.0000 Uiso R . . . . . H442 H 0.8180 0.5517 0.9817 0.0836 1.0000 Uiso R . . . . . H443 H 0.6724 0.5673 0.9700 0.0836 1.0000 Uiso R . . . . . H451 H 0.6032 0.6930 0.7478 0.0773 1.0000 Uiso R . . . . . H452 H 0.5534 0.6485 0.8383 0.0773 1.0000 Uiso R . . . . . H453 H 0.6562 0.7257 0.8059 0.0773 1.0000 Uiso R . . . . . H461 H 0.7568 0.6517 0.6380 0.0732 1.0000 Uiso R . . . . . H462 H 0.7986 0.5577 0.6404 0.0732 1.0000 Uiso R . . . . . H463 H 0.6560 0.5736 0.6802 0.0732 1.0000 Uiso R . . . . . H471 H 1.0082 0.4848 0.6842 0.0801 1.0000 Uiso R . . . . . H472 H 0.8975 0.4138 0.7309 0.0801 1.0000 Uiso R . . . . . H473 H 1.0213 0.4165 0.7659 0.0801 1.0000 Uiso R . . . . . H481 H 1.0315 0.4188 0.8836 0.0870 1.0000 Uiso R . . . . . H482 H 1.0286 0.4887 0.9233 0.0870 1.0000 Uiso R . . . . . H483 H 0.9188 0.4158 0.9548 0.0870 1.0000 Uiso 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 0.0301(6) 0.0387(6) 0.0403(6) -0.0156(5) -0.0073(5) 0.0026(5) N1 0.040(3) 0.046(3) 0.047(3) -0.023(3) -0.011(2) 0.009(2) N2 0.039(3) 0.039(3) 0.052(3) -0.019(3) -0.013(3) 0.006(2) N3 0.037(3) 0.044(3) 0.047(3) -0.013(3) -0.013(2) 0.002(2) N4 0.030(3) 0.047(3) 0.053(4) -0.017(3) -0.004(2) 0.000(2) C1 0.067(5) 0.044(4) 0.063(5) -0.024(4) -0.025(4) 0.018(4) C2 0.035(4) 0.064(5) 0.065(5) -0.035(4) -0.002(3) 0.004(3) C3 0.038(4) 0.047(4) 0.067(5) -0.026(4) -0.011(3) 0.002(3) C4 0.034(4) 0.069(5) 0.072(5) -0.037(4) -0.017(3) 0.006(3) C5 0.038(4) 0.051(4) 0.060(5) -0.025(4) -0.013(3) 0.008(3) C6 0.047(4) 0.066(5) 0.072(5) -0.029(4) -0.022(4) 0.005(4) C7 0.054(4) 0.046(4) 0.055(4) -0.011(3) -0.016(4) -0.003(3) C8 0.057(4) 0.062(5) 0.047(4) -0.020(4) 0.000(3) -0.005(4) C9 0.061(5) 0.046(4) 0.061(5) -0.004(4) -0.015(4) 0.002(4) C10 0.042(4) 0.059(5) 0.049(4) -0.022(4) -0.006(3) -0.007(3) C11 0.064(5) 0.061(5) 0.088(7) -0.023(5) 0.002(5) -0.007(4) C12 0.049(5) 0.081(6) 0.098(7) -0.040(6) 0.014(5) -0.015(4) C13 0.030(3) 0.054(4) 0.046(4) -0.025(3) -0.008(3) -0.005(3) C14 0.035(3) 0.053(4) 0.039(3) -0.018(3) -0.013(3) 0.008(3) C15 0.035(3) 0.060(4) 0.045(4) -0.021(3) -0.012(3) 0.001(3) C16 0.040(4) 0.046(4) 0.052(4) -0.027(3) -0.013(3) 0.006(3) C17 0.034(3) 0.042(4) 0.046(4) -0.022(3) -0.009(3) 0.002(3) C18 0.033(3) 0.057(4) 0.061(5) -0.024(4) -0.011(3) 0.007(3) C19 0.049(4) 0.051(4) 0.047(4) -0.011(3) -0.019(3) 0.006(3) C20 0.042(4) 0.073(5) 0.048(4) -0.016(4) 0.005(3) -0.008(4) C21 0.036(4) 0.066(5) 0.054(4) -0.031(4) -0.003(3) 0.009(3) C22 0.050(4) 0.042(4) 0.068(5) -0.026(4) -0.007(4) -0.001(3) Br1 0.0695(5) 0.0457(4) 0.0480(4) -0.0173(3) -0.0125(4) 0.0039(4) Ti2 0.0382(6) 0.0388(6) 0.0388(6) -0.0100(5) -0.0086(5) -0.0005(5) N5 0.073(4) 0.051(3) 0.041(3) -0.013(3) -0.016(3) -0.005(3) N6 0.095(4) 0.065(4) 0.053(3) -0.009(3) -0.022(3) -0.018(3) N7 0.044(3) 0.045(3) 0.041(3) -0.014(3) -0.006(2) 0.009(3) N8 0.036(3) 0.044(3) 0.050(3) -0.021(3) -0.008(2) 0.002(2) C27 0.104(7) 0.104(7) 0.090(6) 0.025(5) -0.043(5) -0.028(6) C28 0.071(5) 0.071(5) 0.069(5) 0.006(4) -0.022(4) -0.019(4) C29 0.099(6) 0.107(6) 0.072(5) -0.017(5) -0.013(5) 0.004(5) C30 0.093(6) 0.130(8) 0.063(5) -0.022(5) -0.004(5) 0.029(6) C31 0.040(4) 0.052(4) 0.041(4) -0.017(3) -0.010(3) -0.003(3) C32 0.050(4) 0.060(5) 0.067(5) -0.028(4) -0.009(4) -0.007(4) C33 0.055(4) 0.045(4) 0.051(4) -0.013(3) -0.002(3) 0.000(3) C34 0.064(5) 0.057(5) 0.069(5) -0.021(4) -0.012(4) 0.022(4) C35 0.080(6) 0.063(5) 0.059(5) -0.032(4) -0.009(4) 0.004(4) C36 0.035(4) 0.050(4) 0.063(5) -0.022(4) -0.006(3) 0.005(3) C37 0.053(5) 0.065(5) 0.069(5) -0.025(4) -0.006(4) 0.020(4) C38 0.049(4) 0.069(5) 0.067(5) -0.017(4) -0.008(4) 0.017(4) C39 0.040(4) 0.066(5) 0.045(4) -0.004(3) -0.010(3) -0.008(3) C40 0.031(3) 0.063(5) 0.054(4) -0.008(4) -0.007(3) 0.000(3) C41 0.036(4) 0.050(4) 0.058(4) -0.015(4) -0.009(3) -0.004(3) C42 0.051(4) 0.035(4) 0.065(5) -0.003(3) -0.013(4) -0.008(3) C43 0.053(4) 0.048(4) 0.051(4) 0.002(3) -0.021(3) -0.008(3) C44 0.060(5) 0.080(6) 0.055(5) -0.002(4) -0.015(4) -0.013(4) C45 0.037(4) 0.085(6) 0.061(5) -0.020(4) -0.016(4) 0.006(4) C46 0.061(5) 0.060(5) 0.053(4) -0.016(4) -0.018(4) -0.011(4) C47 0.064(5) 0.047(4) 0.093(6) -0.025(4) -0.020(5) 0.001(4) C48 0.064(5) 0.063(5) 0.076(6) -0.004(4) -0.026(4) -0.008(4) Br2 0.0388(4) 0.0496(4) 0.0517(4) -0.0187(3) -0.0044(3) -0.0004(3) O1 0.152(9) 0.168(10) 0.131(9) -0.079(8) -0.035(7) 0.039(8) C23 0.085(8) 0.116(9) 0.108(10) -0.045(8) -0.012(7) -0.025(7) C24 0.070(6) 0.127(10) 0.099(8) -0.057(8) -0.021(6) 0.000(7) C25 0.097(8) 0.097(8) 0.103(8) -0.052(7) -0.027(7) -0.012(6) C26 0.160(13) 0.099(9) 0.089(8) -0.049(7) 0.005(8) -0.034(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3673(8) 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 . 1.717(5) yes Ti1 . N3 . 2.083(6) yes Ti1 . N4 . 2.085(5) yes Ti1 . C13 . 2.384(6) yes Ti1 . C14 . 2.363(6) yes Ti1 . C15 . 2.395(7) yes Ti1 . C16 . 2.432(7) yes Ti1 . C17 . 2.423(6) yes N1 . N2 . 1.426(7) yes N2 . C1 . 1.500(7) yes N2 . C2 . 1.495(7) yes N2 . C3 . 1.512(7) yes N3 . C5 . 1.356(9) yes N3 . C7 . 1.446(9) yes N4 . C5 . 1.337(9) yes N4 . C10 . 1.470(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . C4 . 1.489(10) yes C3 . H31 . 0.950 no C3 . H32 . 0.950 no C4 . H41 . 0.950 no C4 . H42 . 0.950 no C4 . H43 . 0.950 no C5 . C6 . 1.500(10) yes C6 . H61 . 0.950 no C6 . H62 . 0.950 no C6 . H63 . 0.950 no C7 . C8 . 1.544(11) yes C7 . C9 . 1.507(11) yes C7 . H71 . 0.950 no C8 . H81 . 0.950 no C8 . H82 . 0.950 no C8 . H83 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . C11 . 1.513(12) yes C10 . C12 . 1.508(11) yes C10 . H101 . 0.950 no C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . C14 . 1.415(10) yes C13 . C17 . 1.417(9) yes C13 . C18 . 1.490(9) yes C14 . C15 . 1.431(9) yes C14 . C19 . 1.506(9) yes C15 . C16 . 1.430(10) yes C15 . C20 . 1.472(10) yes C16 . C17 . 1.396(10) yes C16 . C21 . 1.503(9) yes C17 . C22 . 1.514(10) yes C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no C19 . H191 . 0.950 no C19 . H192 . 0.950 no C19 . H193 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no C21 . H211 . 0.950 no C21 . H212 . 0.950 no C21 . H213 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no Ti2 . N5 . 1.712(6) yes Ti2 . N7 . 2.079(6) yes Ti2 . N8 . 2.080(5) yes Ti2 . C39 . 2.426(7) yes Ti2 . C40 . 2.378(7) yes Ti2 . C41 . 2.397(7) yes Ti2 . C42 . 2.388(7) yes Ti2 . C43 . 2.426(7) yes N5 . N6 . 1.404(9) yes N6 . C27 . 1.524(8) yes N6 . C28 . 1.492(7) yes N6 . C29 . 1.496(8) yes N7 . C31 . 1.351(9) yes N7 . C33 . 1.479(9) yes N8 . C31 . 1.347(9) yes N8 . C36 . 1.470(8) yes C27 . H271 . 0.950 no C27 . H272 . 0.950 no C27 . H273 . 0.950 no C28 . H281 . 0.950 no C28 . H282 . 0.950 no C28 . H283 . 0.950 no C29 . C30 . 1.545(8) yes C29 . H291 . 0.950 no C29 . H292 . 0.950 no C30 . H301 . 0.950 no C30 . H302 . 0.950 no C30 . H303 . 0.950 no C31 . C32 . 1.492(10) yes C32 . H321 . 0.950 no C32 . H322 . 0.950 no C32 . H323 . 0.950 no C33 . C34 . 1.517(11) yes C33 . C35 . 1.502(11) yes C33 . H331 . 0.950 no C34 . H341 . 0.950 no C34 . H342 . 0.950 no C34 . H343 . 0.950 no C35 . H351 . 0.950 no C35 . H352 . 0.950 no C35 . H353 . 0.950 no C36 . C37 . 1.490(11) yes C36 . C38 . 1.548(11) yes C36 . H361 . 0.950 no C37 . H371 . 0.950 no C37 . H372 . 0.950 no C37 . H373 . 0.950 no C38 . H381 . 0.950 no C38 . H382 . 0.950 no C38 . H383 . 0.950 no C39 . C40 . 1.446(10) yes C39 . C43 . 1.428(11) yes C39 . C44 . 1.474(12) yes C40 . C41 . 1.404(11) yes C40 . C45 . 1.508(11) yes C41 . C42 . 1.415(10) yes C41 . C46 . 1.510(11) yes C42 . C43 . 1.447(11) yes C42 . C47 . 1.497(12) yes C43 . C48 . 1.491(11) yes C44 . H441 . 0.950 no C44 . H442 . 0.950 no C44 . H443 . 0.950 no C45 . H451 . 0.950 no C45 . H452 . 0.950 no C45 . H453 . 0.950 no C46 . H461 . 0.950 no C46 . H462 . 0.950 no C46 . H463 . 0.950 no C47 . H471 . 0.950 no C47 . H472 . 0.950 no C47 . H473 . 0.950 no C48 . H481 . 0.950 no C48 . H482 . 0.950 no C48 . H483 . 0.950 no O1 . C23 . 1.379(15) yes O1 . C26 . 1.425(16) yes C23 . C24 . 1.520(16) yes C23 . H231 . 0.950 no C23 . H232 . 0.950 no C24 . C25 . 1.425(16) yes C24 . H241 . 0.950 no C24 . H242 . 0.950 no C25 . C26 . 1.478(17) yes C25 . H251 . 0.950 no C25 . H252 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 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 N1 . Ti1 . N3 . 106.2(2) yes N1 . Ti1 . N4 . 105.9(2) yes N3 . Ti1 . N4 . 65.2(2) yes N1 . Ti1 . C13 . 108.7(2) yes N3 . Ti1 . C13 . 110.3(2) yes N4 . Ti1 . C13 . 144.8(2) yes N1 . Ti1 . C14 . 97.4(2) yes N3 . Ti1 . C14 . 143.9(2) yes N4 . Ti1 . C14 . 133.6(2) yes C13 . Ti1 . C14 . 34.7(2) yes N1 . Ti1 . C15 . 119.3(3) yes N3 . Ti1 . C15 . 134.5(2) yes N4 . Ti1 . C15 . 99.1(2) yes C13 . Ti1 . C15 . 57.7(2) yes C14 . Ti1 . C15 . 35.0(2) yes N1 . Ti1 . C16 . 153.0(3) yes N3 . Ti1 . C16 . 100.4(2) yes N4 . Ti1 . C16 . 88.9(2) yes C13 . Ti1 . C16 . 56.7(2) yes C14 . Ti1 . C16 . 57.3(2) yes N1 . Ti1 . C17 . 142.1(2) yes N3 . Ti1 . C17 . 88.4(2) yes N4 . Ti1 . C17 . 112.0(2) yes C13 . Ti1 . C17 . 34.3(2) yes C14 . Ti1 . C17 . 57.1(2) yes C15 . Ti1 . C16 . 34.5(2) yes C15 . Ti1 . C17 . 56.8(2) yes C16 . Ti1 . C17 . 33.4(2) yes Ti1 . N1 . N2 . 177.5(5) yes N1 . N2 . C1 . 109.9(5) yes N1 . N2 . C2 . 109.8(5) yes C1 . N2 . C2 . 109.3(5) yes N1 . N2 . C3 . 108.9(5) yes C1 . N2 . C3 . 109.5(5) yes C2 . N2 . C3 . 109.4(5) yes Ti1 . N3 . C5 . 89.5(4) yes Ti1 . N3 . C7 . 139.5(5) yes C5 . N3 . C7 . 121.9(6) yes Ti1 . N4 . C5 . 90.0(4) yes Ti1 . N4 . C10 . 143.9(5) yes C5 . N4 . C10 . 120.7(6) yes N2 . C1 . H11 . 109.5 no N2 . C1 . H12 . 109.5 no H11 . C1 . H12 . 109.5 no N2 . C1 . H13 . 109.5 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no N2 . C2 . H21 . 109.4 no N2 . C2 . H22 . 109.1 no H21 . C2 . H22 . 109.5 no N2 . C2 . H23 . 109.9 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no N2 . C3 . C4 . 114.4(6) yes N2 . C3 . H31 . 108.1 no C4 . C3 . H31 . 108.7 no N2 . C3 . H32 . 108.3 no C4 . C3 . H32 . 107.7 no H31 . C3 . H32 . 109.5 no C3 . C4 . H41 . 109.3 no C3 . C4 . H42 . 110.9 no H41 . C4 . H42 . 109.5 no C3 . C4 . H43 . 108.2 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no N3 . C5 . N4 . 112.9(6) yes N3 . C5 . C6 . 123.3(7) yes N4 . C5 . C6 . 123.8(6) yes C5 . C6 . H61 . 109.7 no C5 . C6 . H62 . 109.9 no H61 . C6 . H62 . 109.5 no C5 . C6 . H63 . 108.9 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no N3 . C7 . C8 . 108.6(6) yes N3 . C7 . C9 . 113.1(7) yes C8 . C7 . C9 . 111.1(6) yes N3 . C7 . H71 . 108.3 no C8 . C7 . H71 . 107.8 no C9 . C7 . H71 . 107.8 no C7 . C8 . H81 . 109.7 no C7 . C8 . H82 . 109.7 no H81 . C8 . H82 . 109.5 no C7 . C8 . H83 . 109.0 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no C7 . C9 . H91 . 110.1 no C7 . C9 . H92 . 109.0 no H91 . C9 . H92 . 109.5 no C7 . C9 . H93 . 109.3 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N4 . C10 . C11 . 111.0(6) yes N4 . C10 . C12 . 111.5(6) yes C11 . C10 . C12 . 110.0(7) yes N4 . C10 . H101 . 107.9 no C11 . C10 . H101 . 108.5 no C12 . C10 . H101 . 107.8 no C10 . C11 . H111 . 109.5 no C10 . C11 . H112 . 109.1 no H111 . C11 . H112 . 109.5 no C10 . C11 . H113 . 109.8 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no C10 . C12 . H121 . 110.2 no C10 . C12 . H122 . 109.1 no H121 . C12 . H122 . 109.5 no C10 . C12 . H123 . 109.1 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no Ti1 . C13 . C14 . 71.9(3) yes Ti1 . C13 . C17 . 74.4(3) yes C14 . C13 . C17 . 107.7(5) yes Ti1 . C13 . C18 . 122.5(5) yes C14 . C13 . C18 . 125.1(6) yes C17 . C13 . C18 . 127.1(6) yes Ti1 . C14 . C13 . 73.4(4) yes Ti1 . C14 . C15 . 73.7(4) yes C13 . C14 . C15 . 108.2(6) yes Ti1 . C14 . C19 . 123.4(5) yes C13 . C14 . C19 . 126.6(6) yes C15 . C14 . C19 . 125.0(6) yes Ti1 . C15 . C14 . 71.3(4) yes Ti1 . C15 . C16 . 74.2(4) yes C14 . C15 . C16 . 106.9(6) yes Ti1 . C15 . C20 . 124.4(5) yes C14 . C15 . C20 . 126.4(7) yes C16 . C15 . C20 . 126.5(6) yes Ti1 . C16 . C15 . 71.3(4) yes Ti1 . C16 . C17 . 72.9(4) yes C15 . C16 . C17 . 108.4(6) yes Ti1 . C16 . C21 . 123.5(5) yes C15 . C16 . C21 . 126.0(6) yes C17 . C16 . C21 . 125.5(6) yes Ti1 . C17 . C13 . 71.3(3) yes Ti1 . C17 . C16 . 73.7(4) yes C13 . C17 . C16 . 108.8(6) yes Ti1 . C17 . C22 . 125.6(5) yes C13 . C17 . C22 . 125.4(6) yes C16 . C17 . C22 . 125.5(6) yes C13 . C18 . H181 . 108.4 no C13 . C18 . H182 . 109.9 no H181 . C18 . H182 . 109.5 no C13 . C18 . H183 . 110.1 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no C14 . C19 . H191 . 109.1 no C14 . C19 . H192 . 109.9 no H191 . C19 . H192 . 109.5 no C14 . C19 . H193 . 109.5 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C15 . C20 . H201 . 109.9 no C15 . C20 . H202 . 109.7 no H201 . C20 . H202 . 109.5 no C15 . C20 . H203 . 108.7 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C16 . C21 . H211 . 109.6 no C16 . C21 . H212 . 109.3 no H211 . C21 . H212 . 109.5 no C16 . C21 . H213 . 109.4 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C17 . C22 . H221 . 109.9 no C17 . C22 . H222 . 109.8 no H221 . C22 . H222 . 109.5 no C17 . C22 . H223 . 108.7 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no N5 . Ti2 . N7 . 105.2(3) yes N5 . Ti2 . N8 . 105.8(3) yes N7 . Ti2 . N8 . 65.0(2) yes N5 . Ti2 . C39 . 144.2(3) yes N7 . Ti2 . C39 . 88.3(3) yes N8 . Ti2 . C39 . 110.0(2) yes N5 . Ti2 . C40 . 109.6(3) yes N7 . Ti2 . C40 . 108.5(3) yes N8 . Ti2 . C40 . 144.3(2) yes C39 . Ti2 . C40 . 35.0(2) yes N5 . Ti2 . C41 . 96.6(3) yes N7 . Ti2 . C41 . 142.4(2) yes N8 . Ti2 . C41 . 137.2(2) yes C39 . Ti2 . C41 . 57.4(3) yes C40 . Ti2 . C41 . 34.2(3) yes N5 . Ti2 . C42 . 115.9(3) yes N7 . Ti2 . C42 . 139.0(3) yes N8 . Ti2 . C42 . 102.9(2) yes C39 . Ti2 . C42 . 57.8(3) yes C40 . Ti2 . C42 . 57.5(3) yes N5 . Ti2 . C43 . 150.7(3) yes N7 . Ti2 . C43 . 104.0(2) yes N8 . Ti2 . C43 . 89.1(2) yes C39 . Ti2 . C43 . 34.2(3) yes C40 . Ti2 . C43 . 57.4(3) yes C41 . Ti2 . C42 . 34.4(2) yes C41 . Ti2 . C43 . 57.2(2) yes C42 . Ti2 . C43 . 35.0(3) yes Ti2 . N5 . N6 . 176.6(6) yes N5 . N6 . C27 . 109.5(7) yes N5 . N6 . C28 . 109.4(6) yes C27 . N6 . C28 . 103.0(7) yes N5 . N6 . C29 . 113.6(7) yes C27 . N6 . C29 . 95.3(8) yes C28 . N6 . C29 . 123.7(8) yes Ti2 . N7 . C31 . 89.6(4) yes Ti2 . N7 . C33 . 141.3(5) yes C31 . N7 . C33 . 120.4(6) yes Ti2 . N8 . C31 . 89.7(4) yes Ti2 . N8 . C36 . 141.9(5) yes C31 . N8 . C36 . 119.8(6) yes N6 . C27 . H271 . 107.6 no N6 . C27 . H272 . 110.0 no H271 . C27 . H272 . 109.5 no N6 . C27 . H273 . 110.8 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no N6 . C28 . H281 . 109.7 no N6 . C28 . H282 . 109.0 no H281 . C28 . H282 . 109.5 no N6 . C28 . H283 . 109.6 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no N6 . C29 . C30 . 109.4(8) yes N6 . C29 . H291 . 109.6 no C30 . C29 . H291 . 109.6 no N6 . C29 . H292 . 110.6 no C30 . C29 . H292 . 108.1 no H291 . C29 . H292 . 109.5 no C29 . C30 . H301 . 112.2 no C29 . C30 . H302 . 108.8 no H301 . C30 . H302 . 109.5 no C29 . C30 . H303 . 107.3 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no N7 . C31 . N8 . 111.9(6) yes N7 . C31 . C32 . 124.8(6) yes N8 . C31 . C32 . 123.3(6) yes C31 . C32 . H321 . 108.8 no C31 . C32 . H322 . 109.5 no H321 . C32 . H322 . 109.5 no C31 . C32 . H323 . 110.1 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no N7 . C33 . C34 . 108.1(6) yes N7 . C33 . C35 . 111.7(6) yes C34 . C33 . C35 . 110.6(7) yes N7 . C33 . H331 . 109.8 no C34 . C33 . H331 . 108.1 no C35 . C33 . H331 . 108.4 no C33 . C34 . H341 . 109.8 no C33 . C34 . H342 . 111.0 no H341 . C34 . H342 . 109.5 no C33 . C34 . H343 . 107.6 no H341 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no C33 . C35 . H351 . 110.2 no C33 . C35 . H352 . 110.3 no H351 . C35 . H352 . 109.5 no C33 . C35 . H353 . 107.9 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no N8 . C36 . C37 . 110.2(6) yes N8 . C36 . C38 . 109.2(6) yes C37 . C36 . C38 . 111.6(6) yes N8 . C36 . H361 . 108.8 no C37 . C36 . H361 . 108.9 no C38 . C36 . H361 . 108.0 no C36 . C37 . H371 . 108.9 no C36 . C37 . H372 . 111.4 no H371 . C37 . H372 . 109.5 no C36 . C37 . H373 . 108.1 no H371 . C37 . H373 . 109.5 no H372 . C37 . H373 . 109.5 no C36 . C38 . H381 . 110.9 no C36 . C38 . H382 . 108.0 no H381 . C38 . H382 . 109.5 no C36 . C38 . H383 . 109.6 no H381 . C38 . H383 . 109.5 no H382 . C38 . H383 . 109.5 no Ti2 . C39 . C40 . 70.7(4) yes Ti2 . C39 . C43 . 72.9(4) yes C40 . C39 . C43 . 106.7(7) yes Ti2 . C39 . C44 . 125.6(6) yes C40 . C39 . C44 . 127.6(7) yes C43 . C39 . C44 . 125.4(7) yes Ti2 . C40 . C39 . 74.3(4) yes Ti2 . C40 . C41 . 73.7(4) yes C39 . C40 . C41 . 108.8(7) yes Ti2 . C40 . C45 . 121.8(5) yes C39 . C40 . C45 . 123.6(7) yes C41 . C40 . C45 . 127.4(7) yes Ti2 . C41 . C40 . 72.2(4) yes Ti2 . C41 . C42 . 72.5(4) yes C40 . C41 . C42 . 108.7(7) yes Ti2 . C41 . C46 . 123.0(5) yes C40 . C41 . C46 . 124.0(7) yes C42 . C41 . C46 . 127.3(7) yes Ti2 . C42 . C41 . 73.2(4) yes Ti2 . C42 . C43 . 73.9(4) yes C41 . C42 . C43 . 107.7(7) yes Ti2 . C42 . C47 . 127.7(5) yes C41 . C42 . C47 . 124.4(7) yes C43 . C42 . C47 . 126.9(7) yes C42 . C43 . Ti2 . 71.1(4) yes C42 . C43 . C39 . 108.0(6) yes Ti2 . C43 . C39 . 72.9(4) yes C42 . C43 . C48 . 127.0(8) yes Ti2 . C43 . C48 . 124.0(5) yes C39 . C43 . C48 . 125.0(8) yes C39 . C44 . H441 . 109.5 no C39 . C44 . H442 . 109.9 no H441 . C44 . H442 . 109.5 no C39 . C44 . H443 . 109.0 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no C40 . C45 . H451 . 110.1 no C40 . C45 . H452 . 108.7 no H451 . C45 . H452 . 109.5 no C40 . C45 . H453 . 109.6 no H451 . C45 . H453 . 109.5 no H452 . C45 . H453 . 109.5 no C41 . C46 . H461 . 110.6 no C41 . C46 . H462 . 108.7 no H461 . C46 . H462 . 109.5 no C41 . C46 . H463 . 109.1 no H461 . C46 . H463 . 109.5 no H462 . C46 . H463 . 109.5 no C42 . C47 . H471 . 108.7 no C42 . C47 . H472 . 110.0 no H471 . C47 . H472 . 109.5 no C42 . C47 . H473 . 109.7 no H471 . C47 . H473 . 109.5 no H472 . C47 . H473 . 109.5 no C43 . C48 . H481 . 109.2 no C43 . C48 . H482 . 109.5 no H481 . C48 . H482 . 109.5 no C43 . C48 . H483 . 109.6 no H481 . C48 . H483 . 109.5 no H482 . C48 . H483 . 109.5 no C23 . O1 . C26 . 104.1(10) yes O1 . C23 . C24 . 104.9(11) yes O1 . C23 . H231 . 108.6 no C24 . C23 . H231 . 108.7 no O1 . C23 . H232 . 112.1 no C24 . C23 . H232 . 112.9 no H231 . C23 . H232 . 109.5 no C23 . C24 . C25 . 105.2(10) yes C23 . C24 . H241 . 112.9 no C25 . C24 . H241 . 111.0 no C23 . C24 . H242 . 107.9 no C25 . C24 . H242 . 110.2 no H241 . C24 . H242 . 109.5 no C24 . C25 . C26 . 105.2(10) yes C24 . C25 . H251 . 109.7 no C26 . C25 . H251 . 111.3 no C24 . C25 . H252 . 110.5 no C26 . C25 . H252 . 110.6 no H251 . C25 . H252 . 109.5 no C25 . C26 . O1 . 105.3(11) yes C25 . C26 . H261 . 111.1 no O1 . C26 . H261 . 108.0 no C25 . C26 . H262 . 111.2 no O1 . C26 . H262 . 111.7 no H261 . C26 . H262 . 109.5 no #===end data_compound_23-BPh4 _database_code_depnum_ccdc_archive 'CCDC 849356' #TrackingRef '- Mountford Xray SI.CIF' # local code PJT14 _chemical_name_systematic ; [Cp*Ti{MeC(NiPr)2}{N(H)(NMe2)}][BPh4] ; _chemical_melting_point ? _publ_section_exptl_refinement ; H atoms were placed in calculated positions, with reference to a fourier difference map. H(1) was located from a Fourier map and positionally and isotropically refined. Loose similarity restraints were applied to the adps of C(5), C(6) and C(7). ; _cell_length_a 28.0165(4) _cell_length_b 15.8661(2) _cell_length_c 8.97260(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3988.43(9) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,z -x,-y,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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C44 H59 B1 N4 Ti1' _chemical_formula_moiety 'C20 H39 N4 Ti1, C24 H20 B1' _chemical_compound_source ? _chemical_formula_weight 702.69 _cell_measurement_reflns_used 8605 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.250 # Sheldrick geometric approximatio 0.96 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.96 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 26420 _reflns_number_total 8965 _diffrn_reflns_av_R_equivalents 0.039 # Number of reflections with Friedels Law is 4812 # Number of reflections without Friedels Law is 8965 # Theoretical number of reflections is about 4563 _diffrn_reflns_theta_min 5.191 _diffrn_reflns_theta_max 27.460 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.911 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min 0 _reflns_limit_h_max 36 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -11 _reflns_limit_l_max 11 _oxford_diffrn_Wilson_B_factor 2.67 _oxford_diffrn_Wilson_scale 4.58 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.49 _refine_diff_density_max 0.47 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 6840 _refine_ls_number_restraints 19 _refine_ls_number_parameters 456 _oxford_refine_ls_R_factor_ref 0.0519 _refine_ls_wR_factor_ref 0.0576 _refine_ls_goodness_of_fit_ref 1.1289 _refine_ls_shift/su_max 0.001904 # The values computed from all data _oxford_reflns_number_all 8965 _refine_ls_R_factor_all 0.0705 _refine_ls_wR_factor_all 0.0695 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7420 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_gt 0.0601 _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs' _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _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: 1.80 0.960 1.73 0.178 0.351 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # 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_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ti1 Ti 0.384651(15) 0.26483(3) 0.93617(9) 0.0275 1.0000 Uani . . . . . . . N1 N 0.42069(9) 0.31509(15) 1.0903(3) 0.0364 1.0000 Uani . . . . . . . N2 N 0.38510(8) 0.37891(14) 1.0707(3) 0.0316 1.0000 Uani . . . . . . . N3 N 0.31403(10) 0.29168(18) 0.8746(4) 0.0478 1.0000 Uani . U . . . . . N4 N 0.33445(10) 0.19421(17) 1.0396(3) 0.0444 1.0000 Uani . . . . . . . C1 C 0.40417(13) 0.45941(18) 1.0182(4) 0.0449 1.0000 Uani . . . . . . . C2 C 0.35359(14) 0.3881(2) 1.1990(4) 0.0474 1.0000 Uani . . . . . . . C3 C 0.29962(12) 0.2393(2) 0.9817(4) 0.0503 1.0000 Uani . . . . . . . C4 C 0.24844(15) 0.2351(3) 1.0367(8) 0.0857 1.0000 Uani . . . . . . . C5 C 0.28251(14) 0.3562(2) 0.8080(6) 0.0652 1.0000 Uani . U . . . . . C6 C 0.31167(18) 0.4322(3) 0.7577(7) 0.0796 1.0000 Uani . U . . . . . C7 C 0.2565(2) 0.3228(3) 0.6740(8) 0.0958 1.0000 Uani . U . . . . . C8 C 0.32882(18) 0.1410(2) 1.1762(5) 0.0653 1.0000 Uani . . . . . . . C9 C 0.37672(19) 0.1256(3) 1.2467(4) 0.0663 1.0000 Uani . . . . . . . C10 C 0.3049(2) 0.0559(3) 1.1402(7) 0.0866 1.0000 Uani . . . . . . . C11 C 0.41744(10) 0.25747(17) 0.6951(3) 0.0307 1.0000 Uani . . . . . . . C12 C 0.39043(10) 0.18214(16) 0.7181(3) 0.0291 1.0000 Uani . . . . . . . C13 C 0.41304(9) 0.13519(15) 0.8308(3) 0.0284 1.0000 Uani . . . . . . . C14 C 0.45300(10) 0.18227(16) 0.8844(3) 0.0302 1.0000 Uani . . . . . . . C15 C 0.45582(10) 0.25712(16) 0.7972(3) 0.0309 1.0000 Uani . . . . . . . C16 C 0.41037(13) 0.3195(2) 0.5713(4) 0.0437 1.0000 Uani . . . . . . . C17 C 0.34775(11) 0.15346(19) 0.6339(4) 0.0390 1.0000 Uani . . . . . . . C18 C 0.40014(11) 0.04679(17) 0.8701(4) 0.0366 1.0000 Uani . . . . . . . C19 C 0.48801(11) 0.15654(19) 1.0006(4) 0.0419 1.0000 Uani . . . . . . . C20 C 0.49618(11) 0.31938(19) 0.8032(4) 0.0406 1.0000 Uani . . . . . . . C21 C 0.64340(10) 0.30528(16) 0.5005(4) 0.0335 1.0000 Uani . . . . . . . C22 C 0.68617(10) 0.33894(18) 0.4439(5) 0.0432 1.0000 Uani . . . . . . . C23 C 0.71718(12) 0.3864(2) 0.5298(5) 0.0515 1.0000 Uani . . . . . . . C24 C 0.70664(13) 0.40327(19) 0.6767(5) 0.0528 1.0000 Uani . . . . . . . C25 C 0.66465(13) 0.3733(2) 0.7360(4) 0.0478 1.0000 Uani . . . . . . . C26 C 0.63387(11) 0.32542(18) 0.6484(4) 0.0394 1.0000 Uani . . . . . . . C27 C 0.57827(10) 0.32523(16) 0.2977(3) 0.0322 1.0000 Uani . . . . . . . C28 C 0.59581(11) 0.36096(19) 0.1659(4) 0.0416 1.0000 Uani . . . . . . . C29 C 0.57314(12) 0.42663(19) 0.0919(4) 0.0437 1.0000 Uani . . . . . . . C30 C 0.53058(11) 0.45942(18) 0.1476(4) 0.0397 1.0000 Uani . . . . . . . C31 C 0.51236(11) 0.42675(18) 0.2788(4) 0.0376 1.0000 Uani . . . . . . . C32 C 0.53617(10) 0.36152(18) 0.3515(3) 0.0347 1.0000 Uani . . . . . . . C33 C 0.57185(10) 0.18881(17) 0.4824(3) 0.0333 1.0000 Uani . . . . . . . C34 C 0.52615(10) 0.16661(17) 0.4310(4) 0.0385 1.0000 Uani . . . . . . . C35 C 0.49744(11) 0.1078(2) 0.5033(4) 0.0447 1.0000 Uani . . . . . . . C36 C 0.51321(13) 0.06822(19) 0.6308(4) 0.0473 1.0000 Uani . . . . . . . C37 C 0.55807(13) 0.08596(19) 0.6840(4) 0.0444 1.0000 Uani . . . . . . . C38 C 0.58698(11) 0.14525(18) 0.6109(3) 0.0384 1.0000 Uani . . . . . . . C39 C 0.63750(10) 0.18852(17) 0.2808(4) 0.0356 1.0000 Uani . . . . . . . C40 C 0.67871(12) 0.14790(19) 0.3327(4) 0.0439 1.0000 Uani . . . . . . . C41 C 0.70302(14) 0.0881(2) 0.2454(5) 0.0522 1.0000 Uani . . . . . . . C42 C 0.68762(14) 0.06768(19) 0.1080(5) 0.0531 1.0000 Uani . . . . . . . C43 C 0.64722(14) 0.1062(2) 0.0523(5) 0.0558 1.0000 Uani . . . . . . . C44 C 0.62269(12) 0.1654(2) 0.1380(4) 0.0445 1.0000 Uani . . . . . . . B1 B 0.60722(11) 0.25240(19) 0.3905(4) 0.0334 1.0000 Uani . . . . . . . H1 H 0.454(2) 0.335(4) 1.123(7) 0.101(18) 1.0000 Uiso . . . . . . . H11 H 0.3789 0.4991 1.0080 0.0536 1.0000 Uiso R . . . . . . H12 H 0.4267 0.4801 1.0883 0.0536 1.0000 Uiso R . . . . . . H13 H 0.4193 0.4515 0.9246 0.0536 1.0000 Uiso R . . . . . . H21 H 0.3308 0.4311 1.1794 0.0574 1.0000 Uiso R . . . . . . H22 H 0.3718 0.4028 1.2843 0.0574 1.0000 Uiso R . . . . . . H23 H 0.3375 0.3363 1.2167 0.0574 1.0000 Uiso R . . . . . . H41 H 0.2290 0.2721 0.9798 0.1011 1.0000 Uiso R . . . . . . H42 H 0.2368 0.1791 1.0270 0.1011 1.0000 Uiso R . . . . . . H43 H 0.2476 0.2514 1.1386 0.1011 1.0000 Uiso R . . . . . . H51 H 0.2601 0.3741 0.8807 0.0739 1.0000 Uiso R . . . . . . H61 H 0.2910 0.4732 0.7156 0.1022 1.0000 Uiso R . . . . . . H62 H 0.3280 0.4558 0.8406 0.1022 1.0000 Uiso R . . . . . . H63 H 0.3342 0.4146 0.6850 0.1022 1.0000 Uiso R . . . . . . H71 H 0.2366 0.3657 0.6339 0.1215 1.0000 Uiso R . . . . . . H72 H 0.2374 0.2762 0.7035 0.1215 1.0000 Uiso R . . . . . . H73 H 0.2787 0.3052 0.6005 0.1215 1.0000 Uiso R . . . . . . H81 H 0.3094 0.1705 1.2455 0.0802 1.0000 Uiso R . . . . . . H91 H 0.3731 0.0918 1.3333 0.0806 1.0000 Uiso R . . . . . . H92 H 0.3906 0.1781 1.2734 0.0806 1.0000 Uiso R . . . . . . H93 H 0.3969 0.0975 1.1775 0.0806 1.0000 Uiso R . . . . . . H101 H 0.3017 0.0231 1.2281 0.1051 1.0000 Uiso R . . . . . . H102 H 0.2742 0.0667 1.0993 0.1051 1.0000 Uiso R . . . . . . H103 H 0.3237 0.0261 1.0696 0.1051 1.0000 Uiso R . . . . . . H161 H 0.3820 0.3061 0.5186 0.0527 1.0000 Uiso R . . . . . . H162 H 0.4079 0.3746 0.6116 0.0527 1.0000 Uiso R . . . . . . H163 H 0.4368 0.3170 0.5052 0.0527 1.0000 Uiso R . . . . . . H171 H 0.3370 0.1012 0.6730 0.0471 1.0000 Uiso R . . . . . . H172 H 0.3559 0.1467 0.5318 0.0471 1.0000 Uiso R . . . . . . H173 H 0.3231 0.1943 0.6429 0.0471 1.0000 Uiso R . . . . . . H181 H 0.4201 0.0280 0.9490 0.0454 1.0000 Uiso R . . . . . . H182 H 0.3677 0.0445 0.9010 0.0454 1.0000 Uiso R . . . . . . H183 H 0.4045 0.0114 0.7857 0.0454 1.0000 Uiso R . . . . . . H191 H 0.4784 0.1044 1.0432 0.0509 1.0000 Uiso R . . . . . . H192 H 0.4892 0.1985 1.0761 0.0509 1.0000 Uiso R . . . . . . H193 H 0.5187 0.1504 0.9569 0.0509 1.0000 Uiso R . . . . . . H201 H 0.5171 0.3048 0.8823 0.0490 1.0000 Uiso R . . . . . . H202 H 0.4837 0.3743 0.8196 0.0490 1.0000 Uiso R . . . . . . H203 H 0.5132 0.3184 0.7115 0.0490 1.0000 Uiso R . . . . . . H221 H 0.6942 0.3283 0.3428 0.0525 1.0000 Uiso R . . . . . . H231 H 0.7457 0.4079 0.4870 0.0611 1.0000 Uiso R . . . . . . H241 H 0.7282 0.4348 0.7366 0.0637 1.0000 Uiso R . . . . . . H251 H 0.6567 0.3852 0.8367 0.0574 1.0000 Uiso R . . . . . . H261 H 0.6050 0.3058 0.6914 0.0479 1.0000 Uiso R . . . . . . H281 H 0.6247 0.3395 0.1255 0.0491 1.0000 Uiso R . . . . . . H291 H 0.5866 0.4491 0.0032 0.0527 1.0000 Uiso R . . . . . . H301 H 0.5143 0.5032 0.0962 0.0486 1.0000 Uiso R . . . . . . H311 H 0.4837 0.4492 0.3194 0.0452 1.0000 Uiso R . . . . . . H321 H 0.5230 0.3405 0.4417 0.0412 1.0000 Uiso R . . . . . . H341 H 0.5144 0.1929 0.3432 0.0463 1.0000 Uiso R . . . . . . H351 H 0.4667 0.0949 0.4645 0.0537 1.0000 Uiso R . . . . . . H361 H 0.4934 0.0289 0.6812 0.0562 1.0000 Uiso R . . . . . . H371 H 0.5695 0.0584 0.7710 0.0529 1.0000 Uiso R . . . . . . H381 H 0.6179 0.1564 0.6493 0.0461 1.0000 Uiso R . . . . . . H401 H 0.6904 0.1610 0.4293 0.0533 1.0000 Uiso R . . . . . . H411 H 0.7308 0.0617 0.2842 0.0628 1.0000 Uiso R . . . . . . H421 H 0.7044 0.0273 0.0499 0.0641 1.0000 Uiso R . . . . . . H431 H 0.6362 0.0924 -0.0448 0.0658 1.0000 Uiso R . . . . . . H441 H 0.5948 0.1908 0.0978 0.0536 1.0000 Uiso 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 0.02872(19) 0.02240(18) 0.03136(19) -0.0052(2) -0.0001(2) -0.00011(17) N1 0.0411(13) 0.0244(11) 0.0439(13) -0.0032(10) -0.0085(11) 0.0091(10) N2 0.0372(12) 0.0192(10) 0.0383(12) -0.0036(9) 0.0004(10) 0.0013(9) N3 0.0376(13) 0.0395(13) 0.0662(17) -0.0212(13) -0.0156(13) 0.0136(11) N4 0.0447(14) 0.0346(13) 0.0539(16) -0.0078(12) 0.0155(12) -0.0009(12) C1 0.0547(19) 0.0223(13) 0.0578(19) -0.0039(13) -0.0038(15) -0.0060(13) C2 0.066(2) 0.0309(14) 0.0456(17) -0.0099(13) 0.0101(15) 0.0051(15) C3 0.0429(17) 0.0418(16) 0.066(2) -0.0215(16) 0.0171(14) -0.0146(14) C4 0.042(2) 0.062(2) 0.153(5) -0.023(3) 0.035(3) -0.0023(18) C5 0.0507(17) 0.0430(16) 0.102(2) -0.0196(17) -0.0324(17) 0.0176(14) C6 0.069(2) 0.057(2) 0.113(3) 0.003(2) -0.037(2) 0.0154(19) C7 0.094(3) 0.056(2) 0.138(4) -0.019(2) -0.068(3) 0.016(2) C8 0.099(3) 0.0352(17) 0.062(2) -0.0050(16) 0.050(2) -0.0114(19) C9 0.105(4) 0.048(2) 0.0453(19) 0.0050(16) 0.010(2) 0.003(2) C10 0.107(4) 0.047(2) 0.105(4) 0.004(2) 0.049(3) -0.025(2) C11 0.0342(13) 0.0246(12) 0.0334(13) -0.0009(10) 0.0030(10) -0.0016(10) C12 0.0349(14) 0.0253(12) 0.0271(12) -0.0026(9) 0.0005(10) 0.0008(10) C13 0.0341(13) 0.0202(11) 0.0308(12) -0.0057(10) 0.0018(10) 0.0020(9) C14 0.0307(12) 0.0248(12) 0.0350(13) -0.0054(10) 0.0015(10) 0.0032(10) C15 0.0310(12) 0.0263(12) 0.0354(13) 0.0002(10) 0.0052(11) -0.0022(10) C16 0.0511(18) 0.0368(16) 0.0432(16) 0.0086(13) -0.0026(14) -0.0042(13) C17 0.0426(16) 0.0341(14) 0.0404(16) -0.0045(12) -0.0020(13) -0.0062(12) C18 0.0443(15) 0.0218(12) 0.0437(14) -0.0019(12) 0.0013(13) -0.0016(11) C19 0.0410(16) 0.0387(15) 0.0459(16) 0.0002(14) -0.0043(13) 0.0076(13) C20 0.0339(14) 0.0357(14) 0.0523(18) -0.0033(13) 0.0025(13) -0.0094(12) C21 0.0305(13) 0.0224(12) 0.0475(15) -0.0006(12) -0.0050(12) 0.0031(10) C22 0.0398(14) 0.0317(13) 0.0582(18) 0.0004(16) -0.0021(17) -0.0043(11) C23 0.0389(16) 0.0324(15) 0.083(3) 0.0042(16) -0.0107(17) -0.0074(13) C24 0.0469(18) 0.0236(14) 0.088(3) -0.0049(16) -0.0211(18) -0.0008(12) C25 0.0490(18) 0.0322(15) 0.062(2) -0.0117(14) -0.0157(15) 0.0062(13) C26 0.0361(14) 0.0301(14) 0.0520(18) -0.0058(13) -0.0052(13) 0.0030(11) C27 0.0336(13) 0.0240(12) 0.0389(14) -0.0033(11) -0.0036(12) -0.0009(10) C28 0.0389(15) 0.0324(15) 0.0535(18) 0.0052(13) 0.0014(14) 0.0019(12) C29 0.0495(17) 0.0337(15) 0.0479(17) 0.0079(13) -0.0026(14) -0.0028(13) C30 0.0433(16) 0.0266(13) 0.0493(17) -0.0010(12) -0.0130(13) 0.0009(11) C31 0.0417(15) 0.0291(13) 0.0421(15) -0.0071(12) -0.0094(13) 0.0046(11) C32 0.0365(14) 0.0314(13) 0.0362(14) -0.0030(12) -0.0024(11) 0.0017(11) C33 0.0351(13) 0.0249(12) 0.0400(14) -0.0034(10) 0.0016(11) 0.0005(10) C34 0.0380(13) 0.0310(12) 0.0466(14) -0.0028(15) -0.0002(15) -0.0017(10) C35 0.0399(16) 0.0357(15) 0.0586(19) -0.0102(14) 0.0076(14) -0.0060(12) C36 0.0538(19) 0.0291(14) 0.059(2) -0.0077(14) 0.0208(16) -0.0009(13) C37 0.061(2) 0.0286(14) 0.0434(16) 0.0030(13) 0.0089(15) 0.0033(13) C38 0.0419(16) 0.0315(14) 0.0419(16) -0.0016(12) -0.0001(13) 0.0023(12) C39 0.0338(14) 0.0238(12) 0.0492(17) 0.0042(12) 0.0064(13) -0.0019(10) C40 0.0498(18) 0.0286(14) 0.0532(19) 0.0047(13) 0.0045(14) 0.0079(13) C41 0.0536(19) 0.0275(15) 0.075(2) 0.0065(15) 0.0161(18) 0.0106(13) C42 0.059(2) 0.0256(14) 0.075(2) -0.0063(15) 0.0277(19) 0.0000(14) C43 0.064(2) 0.0445(18) 0.059(2) -0.0169(16) 0.0142(18) -0.0133(17) C44 0.0383(15) 0.0367(15) 0.059(2) -0.0096(14) -0.0001(14) -0.0037(12) B1 0.0345(15) 0.0248(14) 0.0409(16) -0.0010(11) -0.0008(12) 0.0022(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4725(8) 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 . 1.889(3) yes Ti1 . N2 . 2.176(2) yes Ti1 . N3 . 2.098(3) yes Ti1 . N4 . 2.024(3) yes Ti1 . C11 . 2.353(3) yes Ti1 . C12 . 2.361(3) yes Ti1 . C13 . 2.400(2) yes Ti1 . C14 . 2.366(3) yes Ti1 . C15 . 2.355(3) yes N1 . N2 . 1.432(3) yes N1 . H1 . 1.02(6) no N2 . C1 . 1.462(4) yes N2 . C2 . 1.458(4) yes N3 . C3 . 1.333(5) yes N3 . C5 . 1.478(4) yes N4 . C3 . 1.317(5) yes N4 . C8 . 1.496(5) yes C1 . H11 . 0.951 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . C4 . 1.518(5) yes C4 . H41 . 0.950 no C4 . H42 . 0.950 no C4 . H43 . 0.950 no C5 . C6 . 1.524(7) yes C5 . C7 . 1.503(6) yes C5 . H51 . 0.950 no C6 . H61 . 0.950 no C6 . H62 . 0.950 no C6 . H63 . 0.950 no C7 . H71 . 0.950 no C7 . H72 . 0.950 no C7 . H73 . 0.950 no C8 . C9 . 1.504(7) yes C8 . C10 . 1.541(6) yes C8 . H81 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . C12 . 1.430(4) yes C11 . C15 . 1.412(4) yes C11 . C16 . 1.497(4) yes C12 . C13 . 1.406(4) yes C12 . C17 . 1.486(4) yes C13 . C14 . 1.429(4) yes C13 . C18 . 1.491(4) yes C14 . C15 . 1.424(4) yes C14 . C19 . 1.488(4) yes C15 . C20 . 1.502(4) yes C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no C17 . H171 . 0.950 no C17 . H172 . 0.950 no C17 . H173 . 0.950 no C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no C19 . H191 . 0.950 no C19 . H192 . 0.950 no C19 . H193 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no C21 . C22 . 1.406(4) yes C21 . C26 . 1.391(5) yes C21 . B1 . 1.644(4) yes C22 . C23 . 1.384(5) yes C22 . H221 . 0.950 no C23 . C24 . 1.377(6) yes C23 . H231 . 0.950 no C24 . C25 . 1.376(5) yes C24 . H241 . 0.950 no C25 . C26 . 1.392(4) yes C25 . H251 . 0.950 no C26 . H261 . 0.950 no C27 . C28 . 1.400(4) yes C27 . C32 . 1.399(4) yes C27 . B1 . 1.639(4) yes C28 . C29 . 1.389(4) yes C28 . H281 . 0.950 no C29 . C30 . 1.394(5) yes C29 . H291 . 0.950 no C30 . C31 . 1.384(5) yes C30 . H301 . 0.950 no C31 . C32 . 1.394(4) yes C31 . H311 . 0.950 no C32 . H321 . 0.950 no C33 . C34 . 1.406(4) yes C33 . C38 . 1.410(4) yes C33 . B1 . 1.637(4) yes C34 . C35 . 1.392(4) yes C34 . H341 . 0.950 no C35 . C36 . 1.378(5) yes C35 . H351 . 0.950 no C36 . C37 . 1.373(5) yes C36 . H361 . 0.950 no C37 . C38 . 1.404(4) yes C37 . H371 . 0.950 no C38 . H381 . 0.950 no C39 . C40 . 1.402(4) yes C39 . C44 . 1.396(5) yes C39 . B1 . 1.648(4) yes C40 . C41 . 1.406(5) yes C40 . H401 . 0.950 no C41 . C42 . 1.346(6) yes C41 . H411 . 0.950 no C42 . C43 . 1.380(6) yes C42 . H421 . 0.950 no C43 . C44 . 1.396(5) yes C43 . H431 . 0.950 no C44 . H441 . 0.950 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 N1 . Ti1 . N2 . 40.49(9) yes N1 . Ti1 . N3 . 127.67(10) yes N2 . Ti1 . N3 . 89.00(10) yes N1 . Ti1 . N4 . 105.63(12) yes N2 . Ti1 . N4 . 102.14(10) yes N3 . Ti1 . N4 . 65.02(13) yes N1 . Ti1 . C11 . 119.03(11) yes N2 . Ti1 . C11 . 123.29(9) yes N3 . Ti1 . C11 . 97.84(12) yes N4 . Ti1 . C11 . 131.73(10) yes N1 . Ti1 . C12 . 143.57(10) yes N2 . Ti1 . C12 . 157.15(9) yes N3 . Ti1 . C12 . 87.67(10) yes N4 . Ti1 . C12 . 96.90(10) yes C11 . Ti1 . C12 . 35.31(9) yes N1 . Ti1 . C13 . 118.25(10) yes N2 . Ti1 . C13 . 158.42(9) yes N3 . Ti1 . C13 . 112.52(10) yes N4 . Ti1 . C13 . 86.36(10) yes C11 . Ti1 . C13 . 57.70(9) yes N1 . Ti1 . C14 . 86.84(10) yes N2 . Ti1 . C14 . 124.39(9) yes N3 . Ti1 . C14 . 145.49(10) yes N4 . Ti1 . C14 . 110.24(10) yes C11 . Ti1 . C14 . 58.40(10) yes N1 . Ti1 . C15 . 87.54(11) yes N2 . Ti1 . C15 . 109.39(9) yes N3 . Ti1 . C15 . 132.04(12) yes N4 . Ti1 . C15 . 143.38(10) yes C11 . Ti1 . C15 . 34.92(10) yes C12 . Ti1 . C13 . 34.35(9) yes C12 . Ti1 . C14 . 58.28(9) yes C13 . Ti1 . C14 . 34.90(9) yes C12 . Ti1 . C15 . 58.28(9) yes C13 . Ti1 . C15 . 57.73(9) yes C14 . Ti1 . C15 . 35.12(9) yes Ti1 . N1 . N2 . 80.59(15) yes Ti1 . N1 . H1 . 146(3) no N2 . N1 . H1 . 117(3) no N1 . N2 . Ti1 . 58.92(13) yes N1 . N2 . C1 . 113.8(2) yes Ti1 . N2 . C1 . 123.4(2) yes N1 . N2 . C2 . 113.3(2) yes Ti1 . N2 . C2 . 121.16(19) yes C1 . N2 . C2 . 112.8(2) yes Ti1 . N3 . C3 . 88.2(2) yes Ti1 . N3 . C5 . 144.1(3) yes C3 . N3 . C5 . 122.8(3) yes Ti1 . N4 . C3 . 91.9(2) yes Ti1 . N4 . C8 . 139.6(3) yes C3 . N4 . C8 . 123.5(3) yes N2 . C1 . H11 . 109.7 no N2 . C1 . H12 . 109.4 no H11 . C1 . H12 . 109.3 no N2 . C1 . H13 . 109.4 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no N2 . C2 . H21 . 109.4 no N2 . C2 . H22 . 109.6 no H21 . C2 . H22 . 109.5 no N2 . C2 . H23 . 109.4 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no N3 . C3 . N4 . 113.5(3) yes N3 . C3 . C4 . 123.2(4) yes N4 . C3 . C4 . 123.2(4) yes C3 . C4 . H41 . 109.8 no C3 . C4 . H42 . 109.6 no H41 . C4 . H42 . 109.5 no C3 . C4 . H43 . 109.0 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no N3 . C5 . C6 . 110.3(3) yes N3 . C5 . C7 . 111.7(3) yes C6 . C5 . C7 . 107.6(5) yes N3 . C5 . H51 . 109.0 no C6 . C5 . H51 . 108.8 no C7 . C5 . H51 . 109.5 no C5 . C6 . H61 . 109.5 no C5 . C6 . H62 . 109.8 no H61 . C6 . H62 . 109.5 no C5 . C6 . H63 . 109.1 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no C5 . C7 . H71 . 109.6 no C5 . C7 . H72 . 108.9 no H71 . C7 . H72 . 109.5 no C5 . C7 . H73 . 109.9 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no N4 . C8 . C9 . 110.0(3) yes N4 . C8 . C10 . 111.6(4) yes C9 . C8 . C10 . 109.5(4) yes N4 . C8 . H81 . 108.5 no C9 . C8 . H81 . 108.4 no C10 . C8 . H81 . 108.7 no C8 . C9 . H91 . 109.9 no C8 . C9 . H92 . 109.2 no H91 . C9 . H92 . 109.5 no C8 . C9 . H93 . 109.3 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 110.4 no C8 . C10 . H102 . 108.4 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.6 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no Ti1 . C11 . C12 . 72.67(15) yes Ti1 . C11 . C15 . 72.62(15) yes C12 . C11 . C15 . 107.8(2) yes Ti1 . C11 . C16 . 126.7(2) yes C12 . C11 . C16 . 125.9(3) yes C15 . C11 . C16 . 125.8(3) yes Ti1 . C12 . C11 . 72.03(15) yes Ti1 . C12 . C13 . 74.31(14) yes C11 . C12 . C13 . 107.9(2) yes Ti1 . C12 . C17 . 122.4(2) yes C11 . C12 . C17 . 127.5(3) yes C13 . C12 . C17 . 124.5(2) yes Ti1 . C13 . C12 . 71.33(14) yes Ti1 . C13 . C14 . 71.27(14) yes C12 . C13 . C14 . 108.5(2) yes Ti1 . C13 . C18 . 129.25(19) yes C12 . C13 . C18 . 124.0(2) yes C14 . C13 . C18 . 127.0(2) yes Ti1 . C14 . C13 . 73.83(14) yes Ti1 . C14 . C15 . 72.01(15) yes C13 . C14 . C15 . 107.1(2) yes Ti1 . C14 . C19 . 123.2(2) yes C13 . C14 . C19 . 127.5(2) yes C15 . C14 . C19 . 125.2(2) yes Ti1 . C15 . C14 . 72.87(15) yes Ti1 . C15 . C11 . 72.46(15) yes C14 . C15 . C11 . 108.5(2) yes Ti1 . C15 . C20 . 125.74(19) yes C14 . C15 . C20 . 124.8(3) yes C11 . C15 . C20 . 126.4(3) yes C11 . C16 . H161 . 109.5 no C11 . C16 . H162 . 109.4 no H161 . C16 . H162 . 109.5 no C11 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no C12 . C17 . H171 . 109.6 no C12 . C17 . H172 . 109.4 no H171 . C17 . H172 . 109.5 no C12 . C17 . H173 . 109.4 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no C13 . C18 . H181 . 109.2 no C13 . C18 . H182 . 109.6 no H181 . C18 . H182 . 109.5 no C13 . C18 . H183 . 109.6 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no C14 . C19 . H191 . 109.5 no C14 . C19 . H192 . 109.3 no H191 . C19 . H192 . 109.5 no C14 . C19 . H193 . 109.6 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C15 . C20 . H201 . 109.4 no C15 . C20 . H202 . 109.4 no H201 . C20 . H202 . 109.5 no C15 . C20 . H203 . 109.6 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C22 . C21 . C26 . 114.9(3) yes C22 . C21 . B1 . 120.2(3) yes C26 . C21 . B1 . 124.8(3) yes C21 . C22 . C23 . 122.7(4) yes C21 . C22 . H221 . 118.6 no C23 . C22 . H221 . 118.7 no C22 . C23 . C24 . 120.3(3) yes C22 . C23 . H231 . 119.9 no C24 . C23 . H231 . 119.9 no C23 . C24 . C25 . 119.1(3) yes C23 . C24 . H241 . 120.4 no C25 . C24 . H241 . 120.5 no C24 . C25 . C26 . 120.0(4) yes C24 . C25 . H251 . 120.0 no C26 . C25 . H251 . 120.0 no C25 . C26 . C21 . 123.1(3) yes C25 . C26 . H261 . 118.5 no C21 . C26 . H261 . 118.4 no C28 . C27 . C32 . 114.9(3) yes C28 . C27 . B1 . 122.7(3) yes C32 . C27 . B1 . 122.1(3) yes C27 . C28 . C29 . 123.2(3) yes C27 . C28 . H281 . 118.4 no C29 . C28 . H281 . 118.4 no C28 . C29 . C30 . 120.0(3) yes C28 . C29 . H291 . 120.0 no C30 . C29 . H291 . 120.0 no C29 . C30 . C31 . 118.7(3) yes C29 . C30 . H301 . 120.6 no C31 . C30 . H301 . 120.6 no C30 . C31 . C32 . 120.0(3) yes C30 . C31 . H311 . 119.8 no C32 . C31 . H311 . 120.2 no C27 . C32 . C31 . 123.2(3) yes C27 . C32 . H321 . 118.5 no C31 . C32 . H321 . 118.3 no C34 . C33 . C38 . 114.8(3) yes C34 . C33 . B1 . 122.7(3) yes C38 . C33 . B1 . 122.1(3) yes C33 . C34 . C35 . 122.8(3) yes C33 . C34 . H341 . 118.6 no C35 . C34 . H341 . 118.6 no C34 . C35 . C36 . 120.5(3) yes C34 . C35 . H351 . 119.8 no C36 . C35 . H351 . 119.7 no C35 . C36 . C37 . 119.3(3) yes C35 . C36 . H361 . 120.4 no C37 . C36 . H361 . 120.3 no C36 . C37 . C38 . 120.2(3) yes C36 . C37 . H371 . 120.0 no C38 . C37 . H371 . 119.8 no C33 . C38 . C37 . 122.5(3) yes C33 . C38 . H381 . 118.7 no C37 . C38 . H381 . 118.8 no C40 . C39 . C44 . 115.4(3) yes C40 . C39 . B1 . 120.6(3) yes C44 . C39 . B1 . 123.8(3) yes C39 . C40 . C41 . 121.6(3) yes C39 . C40 . H401 . 119.1 no C41 . C40 . H401 . 119.2 no C40 . C41 . C42 . 121.2(4) yes C40 . C41 . H411 . 119.4 no C42 . C41 . H411 . 119.5 no C41 . C42 . C43 . 119.2(3) yes C41 . C42 . H421 . 120.4 no C43 . C42 . H421 . 120.4 no C42 . C43 . C44 . 120.2(4) yes C42 . C43 . H431 . 119.8 no C44 . C43 . H431 . 120.0 no C39 . C44 . C43 . 122.4(3) yes C39 . C44 . H441 . 118.8 no C43 . C44 . H441 . 118.8 no C39 . B1 . C21 . 110.8(2) yes C39 . B1 . C27 . 112.6(3) yes C21 . B1 . C27 . 104.5(2) yes C39 . B1 . C33 . 103.5(2) yes C21 . B1 . C33 . 112.7(3) yes C27 . B1 . C33 . 113.0(2) yes #===end