data_1100800 _publ_requested_journal 'Organometallics' _publ_section_title ; Crystal structure of compounds 6, 9 and 13 ; loop_ _publ_author_name 'Marta E. G. Mosquera' 'Maria Sudupe' _chemical_formula_moiety 'C36 H54 N4 Si2 Ti1' _chemical_formula_sum 'C36 H54 N4 Si2 Ti' _chemical_formula_weight 646.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7722(10) _cell_length_b 11.3369(4) _cell_length_c 17.0066(16) _cell_angle_alpha 98.372(6) _cell_angle_beta 102.866(10) _cell_angle_gamma 99.863(7) _cell_volume 1776.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 120 _cell_measurement_theta_min 5.123 _cell_measurement_theta_max 21.149 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.412 _exptl_crystal_size_mid 0.396 _exptl_crystal_size_min 0.194 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.338 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 1.242 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 15135 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0986 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8058 _reflns_number_gt 5192 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+1.4230P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8058 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C10 C 0.2452(3) 0.2792(3) 0.1986(2) 0.0265(7) Uani 1 1 d . . . H10A H 0.1793 0.2011 0.1928 0.040 Uiso 1 1 calc R . . H10B H 0.2140 0.3167 0.1511 0.040 Uiso 1 1 calc R . . H10C H 0.2452 0.3336 0.2490 0.040 Uiso 1 1 calc R . . C6 C 0.6224(4) 0.6787(3) 0.3835(2) 0.0356(8) Uani 1 1 d . . . H6A H 0.5913 0.7424 0.3550 0.053 Uiso 1 1 calc R . . H6B H 0.7201 0.6739 0.3799 0.053 Uiso 1 1 calc R . . H6C H 0.6211 0.6985 0.4413 0.053 Uiso 1 1 calc R . . Ti1 Ti 0.59675(6) 0.23075(5) 0.30176(3) 0.01901(15) Uani 1 1 d . . . Si1 Si 0.49779(10) 0.52856(8) 0.33424(6) 0.0236(2) Uani 1 1 d . . . Si2 Si 0.81571(12) 0.16891(9) 0.42846(6) 0.0337(2) Uani 1 1 d . . . N3 N 0.6500(3) 0.3256(2) 0.22320(15) 0.0171(5) Uani 1 1 d . . . N1 N 0.4972(3) 0.4790(2) 0.23103(16) 0.0200(5) Uani 1 1 d . . . N4 N 0.4210(3) 0.1426(2) 0.21100(16) 0.0222(6) Uani 1 1 d . . . N2 N 0.7401(3) 0.1270(2) 0.32307(16) 0.0233(6) Uani 1 1 d . . . C31 C 0.7562(3) 0.3754(3) 0.18271(19) 0.0185(6) Uani 1 1 d . . . C36 C 0.7407(3) 0.3244(3) 0.0997(2) 0.0224(7) Uani 1 1 d . . . C37 C 0.6184(4) 0.2214(3) 0.0530(2) 0.0273(7) Uani 1 1 d . . . H37A H 0.6269 0.1990 -0.0034 0.041 Uiso 1 1 calc R . . H37B H 0.5272 0.2470 0.0517 0.041 Uiso 1 1 calc R . . H37C H 0.6212 0.1509 0.0800 0.041 Uiso 1 1 calc R . . C11 C 0.4762(3) 0.5526(3) 0.1639(2) 0.0229(7) Uani 1 1 d . . . C30 C 0.5130(3) 0.3544(3) 0.21154(18) 0.0184(6) Uani 1 1 d . . . C32 C 0.8778(3) 0.4677(3) 0.2246(2) 0.0234(7) Uani 1 1 d . . . C41 C 0.3067(3) 0.0371(3) 0.1773(2) 0.0249(7) Uani 1 1 d . . . C22 C 0.7935(4) 0.0448(3) 0.2651(2) 0.0260(7) Uani 1 1 d . . . C5 C 0.6969(4) 0.3870(3) 0.41899(19) 0.0279(7) Uani 1 1 d . . . H5 H 0.7825 0.4433 0.4215 0.034 Uiso 1 1 calc R . . C13 C 0.3992(4) 0.4693(3) 0.0806(2) 0.0336(8) Uani 1 1 d . . . H13A H 0.3080 0.4218 0.0845 0.050 Uiso 1 1 calc R . . H13B H 0.4599 0.4137 0.0658 0.050 Uiso 1 1 calc R . . H13C H 0.3806 0.5191 0.0385 0.050 Uiso 1 1 calc R . . C2 C 0.4616(4) 0.3005(3) 0.3997(2) 0.0309(8) Uani 1 1 d . . . H2 H 0.3597 0.2864 0.3856 0.037 Uiso 1 1 calc R . . C33 C 0.9768(3) 0.5090(3) 0.1818(2) 0.0299(8) Uani 1 1 d . . . H33 H 1.0574 0.5723 0.2097 0.036 Uiso 1 1 calc R . . C25 C 0.6681(4) -0.0236(3) 0.1928(2) 0.0391(9) Uani 1 1 d . . . H25A H 0.5950 -0.0714 0.2134 0.059 Uiso 1 1 calc R . . H25B H 0.7028 -0.0783 0.1553 0.059 Uiso 1 1 calc R . . H25C H 0.6260 0.0352 0.1635 0.059 Uiso 1 1 calc R . . C35 C 0.8438(4) 0.3693(3) 0.0596(2) 0.0289(7) Uani 1 1 d . . . H35 H 0.8324 0.3360 0.0034 0.035 Uiso 1 1 calc R . . C43 C 0.1562(4) -0.1463(3) 0.1933(3) 0.0400(10) Uani 1 1 d . . . H43 H 0.1316 -0.2020 0.2271 0.048 Uiso 1 1 calc R . . C7 C 0.3205(4) 0.5450(3) 0.3556(2) 0.0350(8) Uani 1 1 d . . . H7A H 0.2492 0.4691 0.3311 0.053 Uiso 1 1 calc R . . H7B H 0.2883 0.6123 0.3318 0.053 Uiso 1 1 calc R . . H7C H 0.3316 0.5621 0.4151 0.053 Uiso 1 1 calc R . . C1 C 0.5555(4) 0.4047(3) 0.3880(2) 0.0261(7) Uani 1 1 d . . . C4 C 0.6922(4) 0.2726(3) 0.4459(2) 0.0309(8) Uani 1 1 d . . . C34 C 0.9612(4) 0.4607(3) 0.1003(2) 0.0332(8) Uani 1 1 d . . . H34 H 1.0305 0.4901 0.0725 0.040 Uiso 1 1 calc R . . C46 C 0.2307(4) 0.0150(3) 0.0938(2) 0.0303(8) Uani 1 1 d . . . C3 C 0.5436(4) 0.2232(3) 0.4349(2) 0.0316(8) Uani 1 1 d . . . H3 H 0.5059 0.1488 0.4494 0.038 Uiso 1 1 calc R . . C42 C 0.2716(4) -0.0475(3) 0.2267(2) 0.0336(8) Uani 1 1 d . . . C14 C 0.3807(4) 0.6419(3) 0.1829(2) 0.0336(8) Uani 1 1 d . . . H14A H 0.2889 0.5961 0.1871 0.050 Uiso 1 1 calc R . . H14B H 0.3635 0.6882 0.1386 0.050 Uiso 1 1 calc R . . H14C H 0.4289 0.6982 0.2349 0.050 Uiso 1 1 calc R . . C12 C 0.6189(4) 0.6260(3) 0.1577(2) 0.0327(8) Uani 1 1 d . . . H12A H 0.6685 0.6792 0.2108 0.049 Uiso 1 1 calc R . . H12B H 0.6005 0.6758 0.1155 0.049 Uiso 1 1 calc R . . H12C H 0.6790 0.5700 0.1428 0.049 Uiso 1 1 calc R . . C47 C 0.2707(4) 0.0898(3) 0.0320(2) 0.0383(9) Uani 1 1 d . . . H47A H 0.3510 0.1580 0.0601 0.057 Uiso 1 1 calc R . . H47B H 0.1879 0.1213 0.0064 0.057 Uiso 1 1 calc R . . H47C H 0.2990 0.0381 -0.0104 0.057 Uiso 1 1 calc R . . C48 C 0.3511(5) -0.0343(4) 0.3149(3) 0.0460(10) Uani 1 1 d . . . H48A H 0.4287 0.0385 0.3303 0.069 Uiso 1 1 calc R . . H48B H 0.3917 -0.1065 0.3221 0.069 Uiso 1 1 calc R . . H48C H 0.2848 -0.0265 0.3500 0.069 Uiso 1 1 calc R . . C9 C 0.7926(6) 0.0453(4) 0.4897(3) 0.0568(12) Uani 1 1 d . . . H9A H 0.8572 -0.0097 0.4810 0.085 Uiso 1 1 calc R . . H9B H 0.6930 -0.0008 0.4720 0.085 Uiso 1 1 calc R . . H9C H 0.8154 0.0819 0.5482 0.085 Uiso 1 1 calc R . . C45 C 0.1167(4) -0.0866(3) 0.0634(3) 0.0417(10) Uani 1 1 d . . . H45 H 0.0652 -0.1018 0.0073 0.050 Uiso 1 1 calc R . . C23 C 0.8607(4) -0.0493(3) 0.3078(3) 0.0392(9) Uani 1 1 d . . . H23A H 0.7889 -0.0986 0.3284 0.059 Uiso 1 1 calc R . . H23B H 0.9423 -0.0070 0.3538 0.059 Uiso 1 1 calc R . . H23C H 0.8939 -0.1024 0.2685 0.059 Uiso 1 1 calc R . . C38 C 0.9023(4) 0.5273(4) 0.3128(2) 0.0439(10) Uani 1 1 d . . . H38A H 0.8250 0.4895 0.3350 0.066 Uiso 1 1 calc R . . H38B H 0.9032 0.6145 0.3163 0.066 Uiso 1 1 calc R . . H38C H 0.9947 0.5168 0.3446 0.066 Uiso 1 1 calc R . . C44 C 0.0775(4) -0.1656(3) 0.1138(3) 0.0471(11) Uani 1 1 d . . . H44 H -0.0029 -0.2318 0.0931 0.057 Uiso 1 1 calc R . . C8 C 1.0076(5) 0.2521(4) 0.4596(3) 0.0576(12) Uani 1 1 d . . . H8A H 1.0692 0.1948 0.4497 0.086 Uiso 1 1 calc R . . H8B H 1.0338 0.2891 0.5181 0.086 Uiso 1 1 calc R . . H8C H 1.0205 0.3161 0.4273 0.086 Uiso 1 1 calc R . . C24 C 0.9079(4) 0.1204(3) 0.2331(3) 0.0427(10) Uani 1 1 d . . . H24A H 0.8667 0.1812 0.2057 0.064 Uiso 1 1 calc R . . H24B H 0.9404 0.0664 0.1940 0.064 Uiso 1 1 calc R . . H24C H 0.9896 0.1618 0.2793 0.064 Uiso 1 1 calc R . . C40 C 0.3949(3) 0.2582(3) 0.20313(19) 0.0213(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C10 0.0189(16) 0.0292(17) 0.0325(19) 0.0034(14) 0.0097(14) 0.0064(13) C6 0.038(2) 0.0329(18) 0.033(2) -0.0022(15) 0.0080(17) 0.0081(15) Ti1 0.0198(3) 0.0217(3) 0.0173(3) 0.0044(2) 0.0074(2) 0.0051(2) Si1 0.0254(5) 0.0251(4) 0.0207(5) 0.0000(3) 0.0076(4) 0.0075(4) Si2 0.0388(6) 0.0399(6) 0.0244(5) 0.0097(4) 0.0032(4) 0.0166(4) N3 0.0165(12) 0.0192(12) 0.0164(13) 0.0034(10) 0.0061(10) 0.0040(9) N1 0.0231(14) 0.0182(12) 0.0192(13) 0.0020(10) 0.0061(11) 0.0058(10) N4 0.0192(14) 0.0230(13) 0.0256(15) 0.0032(11) 0.0094(11) 0.0041(10) N2 0.0244(14) 0.0259(13) 0.0248(15) 0.0103(11) 0.0106(12) 0.0090(11) C31 0.0168(15) 0.0220(15) 0.0219(16) 0.0096(12) 0.0087(12) 0.0083(12) C36 0.0232(16) 0.0254(16) 0.0235(17) 0.0091(13) 0.0098(13) 0.0097(13) C37 0.0286(18) 0.0293(17) 0.0235(17) 0.0005(13) 0.0091(14) 0.0053(14) C11 0.0248(17) 0.0223(15) 0.0258(17) 0.0088(13) 0.0092(14) 0.0089(12) C30 0.0193(15) 0.0212(14) 0.0158(15) 0.0032(11) 0.0062(12) 0.0056(12) C32 0.0175(16) 0.0273(16) 0.0265(17) 0.0077(13) 0.0061(13) 0.0046(12) C41 0.0185(16) 0.0207(15) 0.0365(19) 0.0000(13) 0.0129(14) 0.0037(12) C22 0.0295(18) 0.0250(16) 0.0308(18) 0.0112(13) 0.0134(15) 0.0131(13) C5 0.0344(19) 0.0322(18) 0.0155(16) -0.0012(13) 0.0057(14) 0.0079(14) C13 0.043(2) 0.0340(19) 0.0251(18) 0.0085(15) 0.0067(16) 0.0128(16) C2 0.036(2) 0.0371(19) 0.0243(18) 0.0049(14) 0.0172(15) 0.0090(15) C33 0.0167(16) 0.0348(18) 0.038(2) 0.0123(15) 0.0074(15) 0.0004(13) C25 0.043(2) 0.040(2) 0.035(2) 0.0016(16) 0.0104(18) 0.0179(17) C35 0.0305(19) 0.0391(19) 0.0238(18) 0.0107(14) 0.0140(15) 0.0126(15) C43 0.034(2) 0.0218(17) 0.070(3) 0.0076(17) 0.026(2) 0.0053(15) C7 0.037(2) 0.040(2) 0.032(2) 0.0013(16) 0.0163(17) 0.0153(16) C1 0.0319(19) 0.0307(17) 0.0173(16) 0.0008(13) 0.0096(14) 0.0095(14) C4 0.041(2) 0.0374(19) 0.0156(16) 0.0039(14) 0.0072(15) 0.0136(16) C34 0.0239(18) 0.045(2) 0.036(2) 0.0159(16) 0.0161(16) 0.0040(15) C46 0.0216(17) 0.0263(17) 0.039(2) -0.0036(14) 0.0073(15) 0.0028(13) C3 0.048(2) 0.0323(18) 0.0215(18) 0.0087(14) 0.0181(16) 0.0118(16) C42 0.0301(19) 0.0248(17) 0.049(2) 0.0028(15) 0.0203(17) 0.0049(14) C14 0.038(2) 0.0351(19) 0.035(2) 0.0114(15) 0.0139(17) 0.0199(16) C12 0.0319(19) 0.0326(18) 0.041(2) 0.0168(16) 0.0150(17) 0.0105(15) C47 0.029(2) 0.043(2) 0.035(2) 0.0009(17) 0.0030(16) -0.0021(16) C48 0.059(3) 0.033(2) 0.053(3) 0.0209(18) 0.026(2) 0.0023(18) C9 0.085(4) 0.065(3) 0.038(2) 0.028(2) 0.020(2) 0.041(3) C45 0.028(2) 0.034(2) 0.053(3) -0.0088(17) 0.0059(18) 0.0010(15) C23 0.043(2) 0.034(2) 0.050(2) 0.0175(17) 0.0177(19) 0.0204(17) C38 0.031(2) 0.054(2) 0.034(2) -0.0088(18) 0.0109(17) -0.0122(17) C44 0.028(2) 0.0246(19) 0.082(3) -0.0041(19) 0.015(2) -0.0027(15) C8 0.042(3) 0.062(3) 0.055(3) -0.004(2) -0.011(2) 0.018(2) C24 0.045(2) 0.039(2) 0.060(3) 0.0208(19) 0.033(2) 0.0168(18) C40 0.0224(16) 0.0227(15) 0.0205(16) 0.0020(12) 0.0095(13) 0.0061(12)