#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _audit_creation_date 01-03-12 _audit_creation_method CRYSTALS _publ_contact_letter ; These are the CIF format data (three compounds) for the paper Novel double substrate insertion versus isocyanate extrusion in reactions of imidotitanium complexes with CO2: critical dependence on imido N-substituents A. E. Guiducci, A. R. Cowley, M. E. G. Skinner and P. Mountford ; loop_ _publ_author_name 'A. E. Guiducci' 'A. R. Cowley' 'M. E. G. Skinner' 'P. Mountford' _publ_contact_author 'Dr P. Mountford' _publ_contact_author_address ; Dr P. Mountford Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone '+44 1865 272679' _contact_author_fax '+44 1865 272690' _publ_contact_author_email 'Philip.Mountford@chem.ox.ac.uk' data_COMPOUND_1b _database_code_CSD 160966 # Local code ARC30 _chemical_name_systematic ; [Ti(C5Me5)(N-2,6-C6H3Me2){MeC(N-iPr)2}] ; _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _cell_length_a 20.5223(4) _cell_angle_alpha 90 _cell_length_b 20.5223(4) _cell_angle_beta 90 _cell_length_c 24.3873(6) _cell_angle_gamma 90 _cell_volume 10271.1 _symmetry_cell_setting 'Tetragonal ' _symmetry_space_group_name_H-M 'I 41 c d ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,y+1/2,z+1/2' '-y,x+1/2,z+1/4' '-y+1/2,x,z+3/4' '-x+1/2,-y+1/2,z+1/2' '-x,-y,z' 'y+1/2,-x,z+3/4' 'y,-x+1/2,z+5/4' '-x,y,z+1/2' '-x+1/2,y+1/2,z' 'y,x+1/2,z+3/4' 'y+1/2,x,z+5/4' 'x+1/2,-y+1/2,z' 'x,-y,z+1/2' '-y+1/2,-x,z+1/4' '-y,-x+1/2,z+3/4' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C26 H41 N3 Ti1 ' _chemical_formula_moiety ' C26 H41 N3 Ti1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 443.53 _cell_measurement_reflns_used 33295 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150 _cell_formula_units_Z 16 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' greenish-brown ' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3844.33 _exptl_absorpt_coefficient_mu 0.35 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.98 _diffrn_ambient_temperature 150 _diffrn_reflns_number 33295 _reflns_number_total 5910 _diffrn_reflns_av_R_equivalents 0.06 _diffrn_measured_fraction_theta_max 1.000 _reflns_number_gt 4139 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min -31 _reflns_limit_l_max 31 _refine_diff_density_min -0.50 _refine_diff_density_max 0.53 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4139 _refine_ls_number_parameters 272 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0418 _refine_ls_goodness_of_fit_ref 1.0434 _refine_ls_shift/su_max 0.001183 _refine_ls_abs_structure_Flack '0.49(3)' _refine_ls_abs_structure_details 'Flack, 325 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 1.18 0.175 0.386 0.120 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ti1 0.257519(19) -0.04863(2) 0.13767(3) 0.0126 1.0000 Uani N1 0.33015(11) -0.09459(12) 0.18393(9) 0.0206 1.0000 Uani N2 0.2497(1) -0.1504(1) 0.14373(11) 0.0182 1.0000 Uani N3 0.28897(11) -0.02765(11) 0.07388(9) 0.0188 1.0000 Uani C1 0.30573(13) -0.15310(14) 0.17168(11) 0.0210 1.0000 Uani C2 0.33778(17) -0.21587(17) 0.18806(15) 0.0358 1.0000 Uani C3 0.39727(14) -0.08753(18) 0.20314(13) 0.0327 1.0000 Uani C4 0.40512(18) -0.0223(2) 0.23135(18) 0.0545 1.0000 Uani C5 0.44511(17) -0.0938(2) 0.15535(17) 0.0484 1.0000 Uani C6 0.22201(16) -0.20844(14) 0.11818(12) 0.0270 1.0000 Uani C7 0.15175(17) -0.19501(18) 0.10203(15) 0.0385 1.0000 Uani C8 0.2614(2) -0.22942(18) 0.06807(16) 0.0466 1.0000 Uani C9 0.30501(13) -0.00145(13) 0.02346(12) 0.0200 1.0000 Uani C10 0.35736(15) 0.04327(15) 0.01789(13) 0.0279 1.0000 Uani C11 0.37432(17) 0.06525(16) -0.03436(14) 0.0367 1.0000 Uani C12 0.34065(19) 0.04540(17) -0.08023(13) 0.0397 1.0000 Uani C13 0.28893(17) 0.00317(15) -0.07494(13) 0.0321 1.0000 Uani C14 0.26978(14) -0.02083(13) -0.02385(12) 0.0217 1.0000 Uani C15 0.3942(2) 0.0663(2) 0.06683(16) 0.0464 1.0000 Uani C16 0.21314(17) -0.06706(16) -0.01946(14) 0.0345 1.0000 Uani C17 0.19218(12) 0.04599(13) 0.13832(13) 0.0225 1.0000 Uani C18 0.23198(14) 0.04951(14) 0.18567(11) 0.0223 1.0000 Uani C19 0.21283(13) -0.00133(14) 0.22171(12) 0.0209 1.0000 Uani C20 0.16150(13) -0.03637(13) 0.19695(11) 0.0199 1.0000 Uani C21 0.14921(13) -0.00687(14) 0.14470(12) 0.0219 1.0000 Uani C22 0.19365(18) 0.09308(16) 0.09118(14) 0.0361 1.0000 Uani C23 0.28026(19) 0.10353(16) 0.19793(15) 0.0369 1.0000 Uani C24 0.23683(18) -0.01395(18) 0.27893(13) 0.0344 1.0000 Uani C25 0.12450(15) -0.09050(16) 0.22392(14) 0.0321 1.0000 Uani C26 0.09402(15) -0.02384(17) 0.10642(14) 0.0346 1.0000 Uani H21 0.3111 -0.2534 0.1746 0.0430 1.0000 Uiso H22 0.3413 -0.2179 0.2289 0.0430 1.0000 Uiso H23 0.3823 -0.2181 0.1716 0.0430 1.0000 Uiso H31 0.4071 -0.1231 0.2299 0.0392 1.0000 Uiso H41 0.4510 -0.0175 0.2445 0.0654 1.0000 Uiso H42 0.3747 -0.0198 0.2633 0.0654 1.0000 Uiso H43 0.3948 0.0134 0.2049 0.0654 1.0000 Uiso H51 0.4907 -0.0889 0.1693 0.0581 1.0000 Uiso H52 0.4400 -0.1376 0.1379 0.0581 1.0000 Uiso H53 0.4359 -0.0591 0.1277 0.0581 1.0000 Uiso H61 0.2235 -0.2449 0.1453 0.0324 1.0000 Uiso H71 0.1327 -0.2347 0.0845 0.0461 1.0000 Uiso H72 0.1260 -0.1836 0.1355 0.0461 1.0000 Uiso H73 0.1503 -0.1579 0.0755 0.0461 1.0000 Uiso H81 0.2413 -0.2692 0.0516 0.0559 1.0000 Uiso H82 0.3072 -0.2394 0.0794 0.0559 1.0000 Uiso H83 0.2616 -0.1934 0.0404 0.0559 1.0000 Uiso H111 0.4117 0.0961 -0.0386 0.0440 1.0000 Uiso H121 0.3537 0.0616 -0.1173 0.0476 1.0000 Uiso H131 0.2645 -0.0106 -0.1085 0.0385 1.0000 Uiso H151 0.4290 0.0973 0.0550 0.0556 1.0000 Uiso H152 0.4145 0.0281 0.0857 0.0556 1.0000 Uiso H153 0.3637 0.0888 0.0926 0.0556 1.0000 Uiso H161 0.1945 -0.0750 -0.0568 0.0414 1.0000 Uiso H162 0.2283 -0.1093 -0.0034 0.0414 1.0000 Uiso H163 0.1789 -0.0476 0.0047 0.0414 1.0000 Uiso H221 0.1630 0.1299 0.0987 0.0433 1.0000 Uiso H222 0.2388 0.1105 0.0866 0.0433 1.0000 Uiso H223 0.1801 0.0702 0.0568 0.0433 1.0000 Uiso H231 0.2578 0.1393 0.2184 0.0443 1.0000 Uiso H232 0.3167 0.0859 0.2207 0.0443 1.0000 Uiso H233 0.2981 0.1211 0.1627 0.0443 1.0000 Uiso H241 0.2100 0.0115 0.3056 0.0412 1.0000 Uiso H242 0.2835 -0.0003 0.2819 0.0412 1.0000 Uiso H243 0.2330 -0.0615 0.2873 0.0412 1.0000 Uiso H251 0.0876 -0.0719 0.2457 0.0386 1.0000 Uiso H252 0.1543 -0.1152 0.2488 0.0386 1.0000 Uiso H253 0.1069 -0.1205 0.1952 0.0386 1.0000 Uiso H261 0.0537 -0.0001 0.1180 0.0415 1.0000 Uiso H262 0.0859 -0.0719 0.1077 0.0415 1.0000 Uiso H263 0.1058 -0.0108 0.0682 0.0415 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0122(2) 0.01431(19) 0.01125(17) 0.0014(2) 0.00011(18) -0.00200(16) N1 0.0146(11) 0.0263(13) 0.0209(12) 0.004(1) -0.0036(9) -0.0016(9) N2 0.0175(9) 0.0171(9) 0.0201(12) 0.001(1) -0.0020(9) -0.0022(8) N3 0.0193(11) 0.0225(12) 0.0145(11) 0.0023(9) 0.0050(9) 0.0004(9) C1 0.0189(13) 0.0258(14) 0.0184(13) 0.0080(11) 0.002(1) -0.0012(11) C2 0.0343(18) 0.0318(17) 0.041(2) 0.0145(15) -0.0048(15) 0.0106(14) C3 0.0164(14) 0.052(2) 0.0299(16) 0.0162(15) -0.0103(12) -0.0052(13) C4 0.0285(18) 0.080(3) 0.055(3) -0.012(2) -0.0105(17) -0.0241(19) C5 0.0226(16) 0.058(2) 0.064(3) 0.0101(19) 0.0079(16) 0.0030(15) C6 0.0380(17) 0.0140(14) 0.0290(16) 0.0011(11) -0.0040(13) -0.0045(12) C7 0.0291(18) 0.045(2) 0.041(2) -0.0063(16) -0.0049(15) -0.0164(15) C8 0.061(2) 0.0343(19) 0.045(2) -0.0140(16) -0.0027(19) 0.0170(17) C9 0.0254(14) 0.0158(13) 0.0189(14) 0.0048(11) 0.0046(11) 0.007(1) C10 0.0300(15) 0.0253(15) 0.0285(16) 0.0072(12) 0.0096(12) 0.0008(12) C11 0.0382(18) 0.0318(17) 0.040(2) 0.0157(15) 0.0191(15) 0.0016(13) C12 0.055(2) 0.0356(18) 0.0287(18) 0.0171(15) 0.0217(16) 0.0162(16) C13 0.050(2) 0.0278(16) 0.0184(14) 0.0021(12) 0.0046(14) 0.0197(15) C14 0.0289(15) 0.0161(13) 0.0199(14) 0.0007(11) 0.0027(12) 0.0089(11) C15 0.044(2) 0.052(2) 0.043(2) 0.0097(18) -0.0011(17) -0.0218(18) C16 0.0412(19) 0.0329(17) 0.0295(17) -0.0010(14) -0.0073(14) -0.0010(14) C17 0.0275(12) 0.0213(12) 0.0185(12) 0.0014(12) 0.0057(14) 0.006(1) C18 0.0318(15) 0.0157(13) 0.0193(13) -0.0050(11) 0.0063(11) -0.0003(11) C19 0.0250(15) 0.0199(14) 0.0177(14) -0.0026(11) 0.0061(11) -0.0002(11) C20 0.0200(13) 0.0227(14) 0.0170(13) -0.0015(11) 0.0065(11) -0.001(1) C21 0.0191(12) 0.0281(14) 0.0186(16) -0.0004(12) 0.0006(12) 0.006(1) C22 0.050(2) 0.0285(17) 0.0298(18) 0.0148(14) 0.0062(15) 0.0119(14) C23 0.055(2) 0.0224(16) 0.0330(18) -0.0049(14) 0.0028(16) -0.0128(15) C24 0.047(2) 0.0422(19) 0.0141(15) -0.0026(13) 0.0016(14) -0.0042(16) C25 0.0293(16) 0.0358(18) 0.0312(17) 0.0008(14) 0.0120(14) -0.0097(13) C26 0.0175(15) 0.049(2) 0.0374(18) -0.0012(16) -0.0054(13) 0.0063(13) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N1 . 2.094(2) yes Ti1 . N2 . 2.099(2) yes Ti1 . N3 . 1.738(2) yes Ti1 . C1 . 2.503(3) yes Ti1 . C17 . 2.360(3) yes Ti1 . C18 . 2.388(3) yes Ti1 . C19 . 2.446(3) yes Ti1 . C20 . 2.457(3) yes Ti1 . C21 . 2.389(3) yes N1 . C1 . 1.335(4) yes N1 . C3 . 1.462(4) yes N2 . C1 . 1.339(4) yes N2 . C6 . 1.460(4) yes N3 . C9 . 1.382(4) yes C1 . C2 . 1.500(4) yes C2 . H21 . 1.000(4) no C2 . H22 . 1.000(4) no C2 . H23 . 1.000(4) no C3 . C4 . 1.513(6) yes C3 . C5 . 1.529(5) yes C3 . H31 . 1.000(3) no C4 . H41 . 1.000(4) no C4 . H42 . 1.000(4) no C4 . H43 . 1.000(5) no C5 . H51 . 1.000(4) no C5 . H52 . 1.000(4) no C5 . H53 . 1.000(4) no C6 . C7 . 1.520(5) yes C6 . C8 . 1.527(5) yes C6 . H61 . 1.000(3) no C7 . H71 . 1.000(3) no C7 . H72 . 1.000(4) no C7 . H73 . 1.000(4) no C8 . H81 . 1.000(4) no C8 . H82 . 1.000(4) no C8 . H83 . 1.000(4) no C9 . C10 . 1.419(4) yes C9 . C14 . 1.419(4) yes C10 . C11 . 1.396(4) yes C10 . C15 . 1.489(5) yes C11 . C12 . 1.377(5) yes C11 . H111 . 1.000(3) no C12 . C13 . 1.376(5) yes C12 . H121 . 1.000(3) no C13 . C14 . 1.396(4) yes C13 . H131 . 1.000(3) no C14 . C16 . 1.504(5) yes C15 . H151 . 1.000(4) no C15 . H152 . 1.000(4) no C15 . H153 . 1.000(4) no C16 . H161 . 1.000(3) no C16 . H162 . 1.000(3) no C16 . H163 . 1.000(4) no C17 . C18 . 1.416(4) yes C17 . C21 . 1.407(4) yes C17 . C22 . 1.502(4) yes C18 . C19 . 1.420(4) yes C18 . C23 . 1.517(4) yes C19 . C20 . 1.411(4) yes C19 . C24 . 1.502(4) yes C20 . C21 . 1.433(4) yes C20 . C25 . 1.498(4) yes C21 . C26 . 1.509(4) yes C22 . H221 . 1.000(3) no C22 . H222 . 1.000(4) no C22 . H223 . 1.000(4) no C23 . H231 . 1.000(4) no C23 . H232 . 1.000(4) no C23 . H233 . 1.000(4) no C24 . H241 . 1.000(3) no C24 . H242 . 1.000(4) no C24 . H243 . 1.000(4) no C25 . H251 . 1.000(3) no C25 . H252 . 1.000(4) no C25 . H253 . 1.000(3) no C26 . H261 . 1.000(3) no C26 . H262 . 1.000(4) no C26 . H263 . 1.000(4) 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 . 64.45(9) yes N1 . Ti1 . N3 . 109.2(1) yes N2 . Ti1 . N3 . 109.74(11) yes N1 . Ti1 . C1 . 32.23(9) yes N2 . Ti1 . C1 . 32.33(9) yes N3 . Ti1 . C1 . 111.2(1) yes N1 . Ti1 . C17 . 140.5(1) yes N2 . Ti1 . C17 . 140.74(9) yes N3 . Ti1 . C17 . 90.76(11) yes C1 . Ti1 . C17 . 158.0(1) yes N1 . Ti1 . C18 . 105.8(1) yes N2 . Ti1 . C18 . 142.0(1) yes N3 . Ti1 . C18 . 108.1(1) yes C1 . Ti1 . C18 . 130.3(1) yes C17 . Ti1 . C18 . 34.7(1) yes N1 . Ti1 . C19 . 89.7(1) yes N2 . Ti1 . C19 . 107.9(1) yes N3 . Ti1 . C19 . 142.3(1) yes C1 . Ti1 . C19 . 102.2(1) yes C17 . Ti1 . C19 . 57.0(1) yes N1 . Ti1 . C20 . 107.46(9) yes N2 . Ti1 . C20 . 89.93(9) yes N3 . Ti1 . C20 . 143.0(1) yes C1 . Ti1 . C20 . 102.11(9) yes C17 . Ti1 . C20 . 57.05(9) yes N1 . Ti1 . C21 . 141.8(1) yes N2 . Ti1 . C21 . 106.28(9) yes N3 . Ti1 . C21 . 108.71(11) yes C1 . Ti1 . C21 . 130.66(9) yes C17 . Ti1 . C21 . 34.5(1) yes C18 . Ti1 . C19 . 34.13(9) yes C18 . Ti1 . C20 . 56.57(9) yes C19 . Ti1 . C20 . 33.45(9) yes C18 . Ti1 . C21 . 57.2(1) yes C19 . Ti1 . C21 . 56.5(1) yes C20 . Ti1 . C21 . 34.4(1) yes Ti1 . N1 . C1 . 90.99(16) yes Ti1 . N1 . C3 . 143.0(2) yes C1 . N1 . C3 . 121.0(3) yes Ti1 . N2 . C1 . 90.66(17) yes Ti1 . N2 . C6 . 144.3(2) yes C1 . N2 . C6 . 121.2(2) yes Ti1 . N3 . C9 . 168.9(2) yes Ti1 . C1 . N1 . 56.77(14) yes Ti1 . C1 . N2 . 57.01(13) yes N1 . C1 . N2 . 113.5(2) yes Ti1 . C1 . C2 . 175.5(2) yes N1 . C1 . C2 . 123.2(3) yes N2 . C1 . C2 . 123.3(3) yes C1 . C2 . H21 . 109.5(3) no C1 . C2 . H22 . 109.5(3) no H21 . C2 . H22 . 109.5(3) no C1 . C2 . H23 . 109.5(3) no H21 . C2 . H23 . 109.5(3) no H22 . C2 . H23 . 109.5(3) no N1 . C3 . C4 . 109.5(3) yes N1 . C3 . C5 . 110.6(3) yes C4 . C3 . C5 . 110.7(3) yes N1 . C3 . H31 . 109.1(3) no C4 . C3 . H31 . 109.1(3) no C5 . C3 . H31 . 107.9(3) no C3 . C4 . H41 . 109.5(4) no C3 . C4 . H42 . 109.5(3) no H41 . C4 . H42 . 109.5(4) no C3 . C4 . H43 . 109.5(3) no H41 . C4 . H43 . 109.5(4) no H42 . C4 . H43 . 109.5(4) no C3 . C5 . H51 . 109.5(4) no C3 . C5 . H52 . 109.5(3) no H51 . C5 . H52 . 109.5(4) no C3 . C5 . H53 . 109.5(3) no H51 . C5 . H53 . 109.5(4) no H52 . C5 . H53 . 109.5(4) no N2 . C6 . C7 . 109.4(2) yes N2 . C6 . C8 . 111.5(3) yes C7 . C6 . C8 . 110.3(3) yes N2 . C6 . H61 . 108.5(3) no C7 . C6 . H61 . 109.7(3) no C8 . C6 . H61 . 107.5(3) no C6 . C7 . H71 . 109.5(3) no C6 . C7 . H72 . 109.5(3) no H71 . C7 . H72 . 109.5(3) no C6 . C7 . H73 . 109.5(3) no H71 . C7 . H73 . 109.5(3) no H72 . C7 . H73 . 109.5(4) no C6 . C8 . H81 . 109.5(4) no C6 . C8 . H82 . 109.5(3) no H81 . C8 . H82 . 109.5(3) no C6 . C8 . H83 . 109.5(3) no H81 . C8 . H83 . 109.5(4) no H82 . C8 . H83 . 109.5(4) no N3 . C9 . C10 . 121.1(3) yes N3 . C9 . C14 . 119.6(3) yes C10 . C9 . C14 . 119.3(3) yes C9 . C10 . C11 . 119.0(3) yes C9 . C10 . C15 . 120.8(3) yes C11 . C10 . C15 . 120.2(3) yes C10 . C11 . C12 . 121.4(3) yes C10 . C11 . H111 . 119.3(4) no C12 . C11 . H111 . 119.3(3) no C11 . C12 . C13 . 119.8(3) yes C11 . C12 . H121 . 120.1(4) no C13 . C12 . H121 . 120.1(4) no C12 . C13 . C14 . 121.5(3) yes C12 . C13 . H131 . 119.2(3) no C14 . C13 . H131 . 119.2(3) no C9 . C14 . C13 . 118.9(3) yes C9 . C14 . C16 . 120.8(3) yes C13 . C14 . C16 . 120.2(3) yes C10 . C15 . H151 . 109.5(3) no C10 . C15 . H152 . 109.5(3) no H151 . C15 . H152 . 109.5(4) no C10 . C15 . H153 . 109.5(3) no H151 . C15 . H153 . 109.5(4) no H152 . C15 . H153 . 109.5(3) no C14 . C16 . H161 . 109.5(3) no C14 . C16 . H162 . 109.5(3) no H161 . C16 . H162 . 109.5(3) no C14 . C16 . H163 . 109.5(3) no H161 . C16 . H163 . 109.5(3) no H162 . C16 . H163 . 109.5(3) no Ti1 . C17 . C18 . 73.73(15) yes Ti1 . C17 . C21 . 73.89(15) yes C18 . C17 . C21 . 108.1(3) yes Ti1 . C17 . C22 . 120.9(2) yes C18 . C17 . C22 . 125.4(3) yes C21 . C17 . C22 . 126.4(3) yes Ti1 . C18 . C17 . 71.57(15) yes Ti1 . C18 . C19 . 75.19(16) yes C17 . C18 . C19 . 107.9(3) yes Ti1 . C18 . C23 . 124.7(2) yes C17 . C18 . C23 . 125.1(3) yes C19 . C18 . C23 . 126.6(3) yes Ti1 . C19 . C18 . 70.68(16) yes Ti1 . C19 . C20 . 73.69(16) yes C18 . C19 . C20 . 108.4(3) yes Ti1 . C19 . C24 . 125.9(2) yes C18 . C19 . C24 . 127.7(3) yes C20 . C19 . C24 . 123.7(3) yes Ti1 . C20 . C19 . 72.86(15) yes Ti1 . C20 . C21 . 70.21(14) yes C19 . C20 . C21 . 107.3(2) yes Ti1 . C20 . C25 . 126.1(2) yes C19 . C20 . C25 . 124.6(3) yes C21 . C20 . C25 . 127.9(3) yes Ti1 . C21 . C17 . 71.65(15) yes Ti1 . C21 . C20 . 75.42(15) yes C17 . C21 . C20 . 108.3(3) yes Ti1 . C21 . C26 . 124.8(2) yes C17 . C21 . C26 . 125.5(3) yes C20 . C21 . C26 . 125.8(3) yes C17 . C22 . H221 . 109.5(3) no C17 . C22 . H222 . 109.5(3) no H221 . C22 . H222 . 109.5(3) no C17 . C22 . H223 . 109.5(3) no H221 . C22 . H223 . 109.5(3) no H222 . C22 . H223 . 109.5(3) no C18 . C23 . H231 . 109.5(3) no C18 . C23 . H232 . 109.5(3) no H231 . C23 . H232 . 109.5(3) no C18 . C23 . H233 . 109.5(3) no H231 . C23 . H233 . 109.5(3) no H232 . C23 . H233 . 109.5(4) no C19 . C24 . H241 . 109.5(3) no C19 . C24 . H242 . 109.5(3) no H241 . C24 . H242 . 109.5(3) no C19 . C24 . H243 . 109.5(3) no H241 . C24 . H243 . 109.5(3) no H242 . C24 . H243 . 109.5(4) no C20 . C25 . H251 . 109.5(3) no C20 . C25 . H252 . 109.5(3) no H251 . C25 . H252 . 109.5(3) no C20 . C25 . H253 . 109.5(3) no H251 . C25 . H253 . 109.5(3) no H252 . C25 . H253 . 109.5(3) no C21 . C26 . H261 . 109.5(3) no C21 . C26 . H262 . 109.5(3) no H261 . C26 . H262 . 109.5(3) no C21 . C26 . H263 . 109.5(3) no H261 . C26 . H263 . 109.5(3) no H262 . C26 . H263 . 109.5(3) no #===end data_COMPOUND_3 _database_code_CSD 160967 # Local code MEGS21 _chemical_name_systematic ; [Ti2{MeC(N-iPr)2}2(C5Me5)2(mu-O)2] ; _publ_section_exptl_refinement ; No special aspects of the structure determination and refinement ; _cell_length_a 9.7810(4) _cell_angle_alpha 90 _cell_length_b 15.4630(4) _cell_angle_beta 92.625(2) _cell_length_c 12.0930(5) _cell_angle_gamma 90 _cell_volume 1827.07 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C36 H64 N4 O2 Ti2' _chemical_formula_moiety ' C36 H64 N4 O2 Ti2' _chemical_compound_source ; ? ; _chemical_formula_weight 680.71 _cell_measurement_reflns_used 9980 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 175 _cell_formula_units_Z 2 _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_measurement_device-type 'Enraf-nonius DIP2000' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_description block _exptl_crystal_colour amber _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.237 _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.47 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.868 _diffrn_ambient_temperature 175 _diffrn_reflns_number 9980 _reflns_number_total 3890 _diffrn_reflns_av_R_equivalents 0.07 _reflns_number_observed 2403 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.45 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.52 _refine_diff_density_max 0.63 _refine_ls_number_reflns 2403 _refine_ls_number_parameters 199 _refine_ls_R_factor_obs 0.0523 _refine_ls_wR_factor_obs 0.0395 _refine_ls_goodness_of_fit_obs 1.0710 _refine_ls_shift/esd_max 0.0002 _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment 'riding model' _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_extinction_method 'None' _refine_ls_extinction_coef none _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_data_collection 'DIP2000 software 'Xpress' (MAC Science, 1989)' _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Ti1 0.03984(6) -0.03424(3) 0.60476(4) 0.0136 1.0000 Uani O1 -0.1180(2) -0.0185(1) 0.5162(2) 0.0185 1.0000 Uani N1 -0.0649(3) 0.0175(2) 0.7465(2) 0.0210 1.0000 Uani N2 0.1475(3) 0.0548(2) 0.7165(2) 0.0181 1.0000 Uani C1 0.0346(3) 0.0743(2) 0.7680(3) 0.0206 1.0000 Uani C2 0.0190(4) 0.1540(2) 0.8384(3) 0.0287 1.0000 Uani C3 -0.2043(3) 0.0306(2) 0.7830(3) 0.0273 1.0000 Uani C4 -0.2143(4) 0.0227(3) 0.9082(3) 0.0399 1.0000 Uani C5 -0.3014(3) -0.0339(3) 0.7269(3) 0.0343 1.0000 Uani C6 0.2689(3) 0.1118(2) 0.7223(3) 0.0242 1.0000 Uani C7 0.3430(4) 0.1108(2) 0.8371(3) 0.0357 1.0000 Uani C8 0.3665(3) 0.0860(2) 0.6350(3) 0.0313 1.0000 Uani C9 -0.0138(3) -0.1866(2) 0.6239(3) 0.0224 1.0000 Uani C10 0.0852(3) -0.1760(2) 0.5418(3) 0.0200 1.0000 Uani C11 0.2093(3) -0.1493(2) 0.5958(3) 0.0202 1.0000 Uani C12 0.1886(3) -0.1412(2) 0.7092(3) 0.0194 1.0000 Uani C13 0.0508(3) -0.1640(2) 0.7269(3) 0.0225 1.0000 Uani C14 -0.1536(4) -0.2232(2) 0.6028(3) 0.0352 1.0000 Uani C15 0.0684(4) -0.2042(2) 0.4242(3) 0.0336 1.0000 Uani C16 0.3403(3) -0.1369(2) 0.5380(3) 0.0280 1.0000 Uani C17 0.2920(4) -0.1212(2) 0.8007(3) 0.0293 1.0000 Uani C18 -0.0072(4) -0.1715(2) 0.8394(3) 0.0325 1.0000 Uani H21 0.1041(4) 0.1850(2) 0.8424(3) 0.0397 1.0000 Uiso H22 -0.0051(4) 0.1377(2) 0.9116(3) 0.0397 1.0000 Uiso H23 -0.0514(4) 0.1903(2) 0.8055(3) 0.0397 1.0000 Uiso H31 -0.2277(3) 0.0884(2) 0.7603(3) 0.0372 1.0000 Uiso H41 -0.3069(4) 0.0321(3) 0.9286(3) 0.0533 1.0000 Uiso H42 -0.1556(4) 0.0649(3) 0.9440(3) 0.0533 1.0000 Uiso H43 -0.1855(4) -0.0342(3) 0.9309(3) 0.0533 1.0000 Uiso H51 -0.3924(3) -0.0246(3) 0.7508(3) 0.0439 1.0000 Uiso H52 -0.2725(3) -0.0916(3) 0.7460(3) 0.0439 1.0000 Uiso H53 -0.3003(3) -0.0265(3) 0.6481(3) 0.0439 1.0000 Uiso H61 0.2325(3) 0.1688(2) 0.7092(3) 0.0329 1.0000 Uiso H71 0.4200(4) 0.1493(2) 0.8371(3) 0.0479 1.0000 Uiso H72 0.2817(4) 0.1291(2) 0.8923(3) 0.0479 1.0000 Uiso H73 0.3742(4) 0.0531(2) 0.8534(3) 0.0479 1.0000 Uiso H81 0.4450(3) 0.1234(2) 0.6391(3) 0.0374 1.0000 Uiso H82 0.3953(3) 0.0273(2) 0.6478(3) 0.0374 1.0000 Uiso H83 0.3217(3) 0.0905(2) 0.5630(3) 0.0374 1.0000 Uiso H141 -0.2014(4) -0.2238(2) 0.6704(3) 0.0458 1.0000 Uiso H142 -0.1466(4) -0.2812(2) 0.5752(3) 0.0458 1.0000 Uiso H143 -0.2029(4) -0.1881(2) 0.5490(3) 0.0458 1.0000 Uiso H151 0.1497(4) -0.1898(2) 0.3868(3) 0.0430 1.0000 Uiso H152 0.0536(4) -0.2655(2) 0.4207(3) 0.0430 1.0000 Uiso H153 -0.0086(4) -0.1749(2) 0.3893(3) 0.0430 1.0000 Uiso H161 0.4112(3) -0.1184(2) 0.5901(3) 0.0400 1.0000 Uiso H162 0.3661(3) -0.1907(2) 0.5052(3) 0.0400 1.0000 Uiso H163 0.3271(3) -0.0940(2) 0.4811(3) 0.0400 1.0000 Uiso H171 0.2483(4) -0.1200(2) 0.8701(3) 0.0407 1.0000 Uiso H172 0.3619(4) -0.1648(2) 0.8030(3) 0.0407 1.0000 Uiso H173 0.3324(4) -0.0658(2) 0.7873(3) 0.0407 1.0000 Uiso H181 0.0593(4) -0.1518(2) 0.8946(3) 0.0436 1.0000 Uiso H182 -0.0299(4) -0.2308(2) 0.8536(3) 0.0436 1.0000 Uiso H183 -0.0881(4) -0.1366(2) 0.8419(3) 0.0436 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0149(2) 0.0116(2) 0.0144(2) 0.0013(2) 0.0005(2) 0.0006(2) O1 0.016(1) 0.021(1) 0.018(1) 0.0051(9) 0.0001(8) -0.0014(9) N1 0.023(1) 0.021(1) 0.019(1) -0.001(1) 0.006(1) 0.000(1) N2 0.018(1) 0.015(1) 0.021(1) -0.002(1) 0.001(1) -0.002(1) C1 0.027(2) 0.019(2) 0.016(1) 0.003(1) -0.000(1) 0.003(1) C2 0.034(2) 0.027(2) 0.025(2) -0.006(1) 0.002(1) 0.000(2) C3 0.026(2) 0.028(2) 0.028(2) 0.002(2) 0.006(1) 0.006(2) C4 0.036(2) 0.055(3) 0.030(2) -0.002(2) 0.013(2) 0.004(2) C5 0.022(2) 0.046(2) 0.035(2) 0.005(2) 0.007(1) 0.002(2) C6 0.024(2) 0.014(1) 0.034(2) 0.002(1) -0.003(1) -0.002(1) C7 0.038(2) 0.029(2) 0.038(2) 0.000(2) -0.011(2) -0.010(2) C8 0.019(2) 0.033(2) 0.042(2) 0.003(2) -0.003(1) -0.008(1) C9 0.025(2) 0.013(1) 0.029(2) 0.002(1) -0.001(1) 0.001(1) C10 0.024(2) 0.013(1) 0.022(2) 0.003(1) -0.002(1) 0.003(1) C11 0.023(2) 0.011(1) 0.027(2) 0.002(1) 0.001(1) 0.005(1) C12 0.024(2) 0.011(1) 0.023(2) 0.002(1) -0.002(1) 0.004(1) C13 0.031(2) 0.011(1) 0.025(2) 0.003(1) 0.003(1) 0.005(1) C14 0.031(2) 0.024(2) 0.051(2) 0.001(2) -0.001(2) -0.006(2) C15 0.050(2) 0.022(2) 0.029(2) -0.002(1) -0.004(2) 0.008(2) C16 0.025(2) 0.026(2) 0.034(2) 0.002(1) 0.009(1) 0.005(1) C17 0.035(2) 0.021(2) 0.031(2) 0.002(1) -0.012(2) 0.001(1) C18 0.038(2) 0.030(2) 0.031(2) 0.013(2) 0.011(2) 0.007(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 . Ti1 2_556 2.823(1) yes Ti1 . O1 . 1.855(2) yes Ti1 . O1 2_556 1.869(2) yes Ti1 . N1 . 2.188(3) yes Ti1 . N2 . 2.168(3) yes Ti1 . C9 . 2.427(3) yes Ti1 . C10 . 2.369(3) yes Ti1 . C11 . 2.438(3) yes Ti1 . C12 . 2.505(3) yes Ti1 . C13 . 2.491(3) yes N1 . C1 . 1.328(4) yes N1 . C3 . 1.466(4) yes N2 . C1 . 1.327(4) yes N2 . C6 . 1.478(4) yes C1 . C2 . 1.510(4) yes C3 . C4 . 1.527(5) yes C3 . C5 . 1.516(5) yes C6 . C7 . 1.536(5) yes C6 . C8 . 1.510(5) yes C9 . C10 . 1.428(4) yes C9 . C13 . 1.414(5) yes C9 . C14 . 1.491(5) yes C10 . C11 . 1.413(4) yes C10 . C15 . 1.489(5) yes C11 . C12 . 1.400(4) yes C11 . C16 . 1.500(4) yes C12 . C13 . 1.420(5) yes C12 . C17 . 1.497(4) yes C13 . C18 . 1.502(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Ti1 2_556 Ti1 . O1 . 40.90(6) yes Ti1 2_556 Ti1 . O1 2_556 40.52(6) yes O1 . Ti1 . O1 2_556 81.41(9) yes Ti1 2_556 Ti1 . N1 . 116.50(8) yes O1 . Ti1 . N1 . 89.9(1) yes O1 2_556 Ti1 . N1 . 132.56(9) yes Ti1 2_556 Ti1 . N2 . 115.31(7) yes O1 . Ti1 . N2 . 130.1(1) yes O1 2_556 Ti1 . N2 . 90.3(1) yes N1 . Ti1 . N2 . 60.7(1) yes Ti1 2_556 Ti1 . C9 . 113.43(8) yes O1 . Ti1 . C9 . 90.2(1) yes O1 2_556 Ti1 . C9 . 126.6(1) yes N1 . Ti1 . C9 . 99.8(1) yes N2 . Ti1 . C9 . 131.2(1) yes Ti1 2_556 Ti1 . C10 . 96.13(8) yes O1 . Ti1 . C10 . 95.7(1) yes O1 2_556 Ti1 . C10 . 93.6(1) yes N1 . Ti1 . C10 . 133.7(1) yes N2 . Ti1 . C10 . 134.0(1) yes Ti1 2_556 Ti1 . C11 . 113.23(8) yes O1 . Ti1 . C11 . 128.3(1) yes O1 2_556 Ti1 . C11 . 88.9(1) yes N1 . Ti1 . C11 . 130.2(1) yes N2 . Ti1 . C11 . 100.3(1) yes Ti1 2_556 Ti1 . C12 . 146.10(8) yes O1 . Ti1 . C12 . 145.7(1) yes O1 2_556 Ti1 . C12 . 115.7(1) yes N1 . Ti1 . C12 . 97.4(1) yes N2 . Ti1 . C12 . 81.4(1) yes Ti1 2_556 Ti1 . C13 . 146.82(8) yes O1 . Ti1 . C13 . 117.4(1) yes O1 2_556 Ti1 . C13 . 143.9(1) yes N1 . Ti1 . C13 . 80.7(1) yes N2 . Ti1 . C13 . 97.8(1) yes C9 . Ti1 . C10 . 34.6(1) yes C9 . Ti1 . C11 . 56.4(1) yes C10 . Ti1 . C11 . 34.2(1) yes C9 . Ti1 . C12 . 55.6(1) yes C10 . Ti1 . C12 . 55.8(1) yes C11 . Ti1 . C12 . 32.9(1) yes C9 . Ti1 . C13 . 33.4(1) yes C10 . Ti1 . C13 . 56.1(1) yes C11 . Ti1 . C13 . 55.1(1) yes C12 . Ti1 . C13 . 33.0(1) yes Ti1 . O1 . Ti1 2_556 98.59(9) yes Ti1 . N1 . C1 . 91.7(2) yes Ti1 . N1 . C3 . 139.6(2) yes C1 . N1 . C3 . 122.2(3) yes Ti1 . N2 . C1 . 92.6(2) yes Ti1 . N2 . C6 . 140.8(2) yes C1 . N2 . C6 . 121.7(3) yes N1 . C1 . N2 . 112.1(3) yes N1 . C1 . C2 . 123.9(3) yes N2 . C1 . C2 . 123.9(3) yes N1 . C3 . C4 . 113.0(3) yes N1 . C3 . C5 . 110.3(3) yes C4 . C3 . C5 . 108.9(3) yes N2 . C6 . C7 . 112.4(3) yes N2 . C6 . C8 . 109.9(3) yes C7 . C6 . C8 . 110.0(3) yes Ti1 . C9 . C10 . 70.5(2) yes Ti1 . C9 . C13 . 75.8(2) yes C10 . C9 . C13 . 107.1(3) yes Ti1 . C9 . C14 . 123.6(2) yes C10 . C9 . C14 . 124.8(3) yes C13 . C9 . C14 . 127.8(3) yes Ti1 . C10 . C9 . 74.9(2) yes Ti1 . C10 . C11 . 75.6(2) yes C9 . C10 . C11 . 107.9(3) yes Ti1 . C10 . C15 . 124.3(2) yes C9 . C10 . C15 . 125.5(3) yes C11 . C10 . C15 . 125.6(3) yes Ti1 . C11 . C10 . 70.3(2) yes Ti1 . C11 . C12 . 76.2(2) yes C10 . C11 . C12 . 108.6(3) yes Ti1 . C11 . C16 . 121.6(2) yes C10 . C11 . C16 . 123.7(3) yes C12 . C11 . C16 . 127.6(3) yes Ti1 . C12 . C11 . 70.9(2) yes Ti1 . C12 . C13 . 72.9(2) yes C11 . C12 . C13 . 107.8(3) yes Ti1 . C12 . C17 . 126.4(2) yes C11 . C12 . C17 . 128.3(3) yes C13 . C12 . C17 . 123.7(3) yes Ti1 . C13 . C9 . 70.8(2) yes Ti1 . C13 . C12 . 74.0(2) yes C9 . C13 . C12 . 108.5(3) yes Ti1 . C13 . C18 . 126.3(2) yes C9 . C13 . C18 . 127.4(3) yes C12 . C13 . C18 . 123.8(3) yes #===end data_COMPOUND_4 _database_code_CSD 160968 # Local code ARC31 _chemical_name_systematic ; [Ti(C5Me5){MeC(N-i-Pr)2}{O(CO)N(2,6-C6H3Me2)(CO)O}] ; _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _cell_length_a 14.4250(2) _cell_angle_alpha 90 _cell_length_b 17.2619(3) _cell_angle_beta 90 _cell_length_c 24.3318(4) _cell_angle_gamma 90 _cell_volume 6058.7 _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P b c a ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,z' 'x+1/2,-y+1/2,-z' 'x,-y+1/2,z+1/2' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' 'x+1/2,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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C31 H44 N3 O4 Ti1 ' _chemical_formula_moiety ' C31 H44 N3 O4 Ti1 ' _chemical_compound_source ; [Ti(C5Me5){MeC(N-i-Pr)2}(N-2,6-C6H3Me2)] + CO2 ; _chemical_formula_weight 570.61 _cell_measurement_reflns_used 19617 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 8 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2442.45 _exptl_absorpt_coefficient_mu 0.32 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.97 _diffrn_ambient_temperature 150 _diffrn_reflns_number 19617 _reflns_number_total 6916 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_measured_fraction_theta_max 0.990 _reflns_number_gt 4551 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 27.50 _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _refine_diff_density_min -0.54 _refine_diff_density_max 0.58 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4551 _refine_ls_number_parameters 352 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.0534 _refine_ls_goodness_of_fit_ref 0.9955 _refine_ls_shift/su_max 0.000330 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 3.09 0.205 2.27 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ti1 0.36108(2) 0.12217(2) 0.153140(15) 0.0147 1.0000 Uani O1 0.4862(1) 0.12560(9) 0.18127(6) 0.0209 1.0000 Uani O2 0.62797(11) 0.16713(11) 0.19997(7) 0.0296 1.0000 Uani O3 0.41663(11) 0.16946(9) 0.08920(6) 0.0209 1.0000 Uani O4 0.50918(13) 0.23715(11) 0.03472(7) 0.0319 1.0000 Uani N1 0.56273(12) 0.2045(1) 0.11943(7) 0.0190 1.0000 Uani N2 0.31701(13) 0.1763(1) 0.22414(7) 0.0189 1.0000 Uani N3 0.25200(13) 0.1991(1) 0.14425(7) 0.0201 1.0000 Uani C1 0.56103(14) 0.16435(12) 0.16985(9) 0.0179 1.0000 Uani C2 0.49386(15) 0.20480(13) 0.07788(8) 0.0189 1.0000 Uani C3 0.64574(16) 0.24881(13) 0.10830(9) 0.0216 1.0000 Uani C4 0.71945(17) 0.21288(15) 0.0812(1) 0.0270 1.0000 Uani C5 0.79890(18) 0.25683(18) 0.07078(12) 0.0361 1.0000 Uani C6 0.80485(19) 0.33233(18) 0.08836(12) 0.0402 1.0000 Uani C7 0.7311(2) 0.36678(15) 0.11551(11) 0.0363 1.0000 Uani C8 0.64938(18) 0.32548(14) 0.1256(1) 0.0276 1.0000 Uani C9 0.71271(19) 0.12937(17) 0.06457(12) 0.0374 1.0000 Uani C10 0.5675(2) 0.36213(14) 0.15349(11) 0.0362 1.0000 Uani C11 0.26137(15) 0.22312(12) 0.19569(9) 0.0201 1.0000 Uani C12 0.21433(19) 0.29290(14) 0.2197(1) 0.0298 1.0000 Uani C13 0.34921(16) 0.19554(14) 0.28000(9) 0.0244 1.0000 Uani C14 0.3851(2) 0.12381(17) 0.30900(11) 0.0386 1.0000 Uani C15 0.42438(19) 0.25807(17) 0.27859(11) 0.0358 1.0000 Uani C16 0.21335(19) 0.24256(15) 0.0974(1) 0.0311 1.0000 Uani C17 0.2677(2) 0.31654(17) 0.08501(13) 0.0448 1.0000 Uani C18 0.1090(2) 0.2577(2) 0.10182(13) 0.0473 1.0000 Uani C19 0.24151(17) 0.03022(13) 0.13308(11) 0.0274 1.0000 Uani C20 0.28383(16) 0.00744(12) 0.1833(1) 0.0245 1.0000 Uani C21 0.37786(16) -0.01226(12) 0.1716(1) 0.0227 1.0000 Uani C22 0.39284(17) 0.00041(12) 0.1144(1) 0.0235 1.0000 Uani C23 0.30818(17) 0.02604(13) 0.0908(1) 0.0262 1.0000 Uani C24 0.1403(2) 0.04718(17) 0.12647(16) 0.0470 1.0000 Uani C25 0.2329(2) -0.00210(16) 0.23656(12) 0.0389 1.0000 Uani C26 0.4497(2) -0.04157(14) 0.21095(11) 0.0337 1.0000 Uani C27 0.4819(2) -0.01281(16) 0.08434(12) 0.0363 1.0000 Uani C28 0.2946(2) 0.04478(17) 0.03098(12) 0.0419 1.0000 Uani C29 0.57023(19) 0.50110(18) 0.03851(12) 0.0381 1.0000 Uani C30 0.53828(18) 0.43105(16) 0.01859(12) 0.0338 1.0000 Uani C31 0.46794(19) 0.43016(17) -0.01990(12) 0.0376 1.0000 Uani H51 0.8519 0.2331 0.0504 0.0433 1.0000 Uiso H61 0.8628 0.3626 0.0815 0.0483 1.0000 Uiso H71 0.7363 0.4218 0.1280 0.0436 1.0000 Uiso H91 0.7713 0.1134 0.0458 0.0449 1.0000 Uiso H92 0.7031 0.0966 0.0980 0.0449 1.0000 Uiso H93 0.6592 0.1224 0.0389 0.0449 1.0000 Uiso H101 0.5826 0.4171 0.1630 0.0434 1.0000 Uiso H102 0.5527 0.3328 0.1878 0.0434 1.0000 Uiso H103 0.5129 0.3609 0.1283 0.0434 1.0000 Uiso H121 0.1763 0.3189 0.1907 0.0357 1.0000 Uiso H122 0.2622 0.3299 0.2337 0.0357 1.0000 Uiso H123 0.1732 0.2764 0.2506 0.0357 1.0000 Uiso H131 0.2950 0.2163 0.3010 0.0292 1.0000 Uiso H141 0.4066 0.1380 0.3468 0.0463 1.0000 Uiso H142 0.4381 0.1016 0.2877 0.0463 1.0000 Uiso H143 0.3343 0.0846 0.3117 0.0463 1.0000 Uiso H151 0.4449 0.2700 0.3169 0.0430 1.0000 Uiso H152 0.4785 0.2391 0.2567 0.0430 1.0000 Uiso H153 0.3989 0.3061 0.2612 0.0430 1.0000 Uiso H161 0.2211 0.2075 0.0650 0.0373 1.0000 Uiso H171 0.2389 0.3438 0.0530 0.0538 1.0000 Uiso H172 0.2664 0.3512 0.1179 0.0538 1.0000 Uiso H173 0.3333 0.3030 0.0760 0.0538 1.0000 Uiso H181 0.0876 0.2872 0.0688 0.0568 1.0000 Uiso H182 0.0960 0.2885 0.1357 0.0568 1.0000 Uiso H183 0.0752 0.2072 0.1038 0.0568 1.0000 Uiso H241 0.1063 -0.0020 0.1183 0.0564 1.0000 Uiso H242 0.1157 0.0703 0.1612 0.0564 1.0000 Uiso H243 0.1313 0.0846 0.0955 0.0564 1.0000 Uiso H251 0.2071 -0.0558 0.2389 0.0467 1.0000 Uiso H252 0.2765 0.0068 0.2679 0.0467 1.0000 Uiso H253 0.1810 0.0363 0.2384 0.0467 1.0000 Uiso H261 0.4459 -0.0993 0.2132 0.0405 1.0000 Uiso H262 0.5127 -0.0261 0.1977 0.0405 1.0000 Uiso H263 0.4385 -0.0188 0.2482 0.0405 1.0000 Uiso H271 0.4840 -0.0674 0.0706 0.0436 1.0000 Uiso H272 0.5352 -0.0036 0.1098 0.0436 1.0000 Uiso H273 0.4860 0.0237 0.0525 0.0436 1.0000 Uiso H281 0.2722 -0.0024 0.0112 0.0503 1.0000 Uiso H282 0.3548 0.0621 0.0148 0.0503 1.0000 Uiso H283 0.2477 0.0871 0.0273 0.0503 1.0000 Uiso H291 0.6211 0.5021 0.0664 0.0457 1.0000 Uiso H301 0.5659 0.3814 0.0320 0.0406 1.0000 Uiso H311 0.4445 0.3796 -0.0344 0.0451 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01444(17) 0.01296(17) 0.01683(18) 0.00033(14) -0.00035(15) -0.00048(14) O1 0.0169(7) 0.0252(8) 0.0207(7) 0.0077(6) -0.0022(6) -0.0037(6) O2 0.0206(8) 0.040(1) 0.0279(8) 0.0101(7) -0.0064(7) -0.0082(7) O3 0.0192(8) 0.0255(8) 0.0181(7) 0.0038(6) -0.0018(6) -0.0036(6) O4 0.0323(9) 0.042(1) 0.0211(8) 0.0114(7) -0.0027(7) -0.0105(8) N1 0.0174(9) 0.0213(9) 0.0182(9) 0.0021(7) 0.0003(7) -0.0037(7) N2 0.0194(9) 0.0190(8) 0.0183(8) -0.0015(7) -0.0007(7) -0.0008(7) N3 0.0216(9) 0.0188(8) 0.0200(9) 0.0017(7) -0.0005(7) 0.0042(7) C1 0.017(1) 0.0176(9) 0.019(1) 0.0006(8) 0.0001(8) -0.0012(8) C2 0.020(1) 0.020(1) 0.016(1) -0.0004(8) 0.0001(8) 0.0002(8) C3 0.0219(11) 0.023(1) 0.019(1) 0.0053(9) -0.0000(8) -0.0067(9) C4 0.0210(11) 0.0351(13) 0.0249(12) 0.006(1) 0.0009(9) -0.002(1) C5 0.0217(12) 0.0480(16) 0.0386(14) 0.0133(12) 0.0008(11) -0.0046(11) C6 0.0307(14) 0.0507(17) 0.0393(15) 0.0191(13) -0.0088(12) -0.0198(12) C7 0.0442(16) 0.0321(13) 0.0327(13) 0.0080(11) -0.0105(11) -0.0203(12) C8 0.0354(13) 0.0256(11) 0.0218(11) 0.0021(9) -0.004(1) -0.008(1) C9 0.0289(13) 0.0391(15) 0.0442(15) -0.0026(12) 0.0111(12) 0.0021(11) C10 0.0550(17) 0.0228(11) 0.0306(12) -0.003(1) 0.0075(13) -0.0013(11) C11 0.019(1) 0.0170(9) 0.0248(11) 0.0009(8) 0.0064(9) -0.0016(8) C12 0.0345(13) 0.0235(11) 0.0314(13) -0.001(1) 0.0068(11) 0.006(1) C13 0.0231(11) 0.0304(12) 0.020(1) -0.0042(9) 0.0018(9) -0.0048(9) C14 0.0459(16) 0.0454(15) 0.0246(12) 0.0042(11) -0.0070(11) 0.0048(13) C15 0.0334(14) 0.0476(16) 0.0265(12) -0.0083(11) -0.0026(11) -0.0145(12) C16 0.0394(14) 0.0298(12) 0.0239(11) 0.002(1) -0.0041(11) 0.0142(11) C17 0.0582(19) 0.0331(15) 0.0431(16) 0.0195(12) 0.0137(14) 0.0152(14) C18 0.0436(16) 0.0514(18) 0.0470(17) 0.0024(14) -0.0144(14) 0.0175(15) C19 0.0215(11) 0.017(1) 0.0441(14) -0.004(1) -0.005(1) -0.0041(9) C20 0.0268(12) 0.0113(9) 0.0353(13) 0.0008(9) 0.006(1) -0.0048(8) C21 0.0239(12) 0.0119(9) 0.0323(12) 0.0035(8) 0.0016(9) -0.0001(8) C22 0.0266(11) 0.0145(9) 0.0294(12) -0.0031(9) -0.001(1) 0.0014(8) C23 0.0318(13) 0.016(1) 0.0307(12) -0.0048(9) -0.008(1) -0.0028(9) C24 0.0216(13) 0.0331(14) 0.086(2) -0.0007(15) -0.0110(15) -0.0064(11) C25 0.0429(16) 0.0237(12) 0.0502(17) -0.0010(11) 0.0214(13) -0.0080(11) C26 0.0427(15) 0.0212(11) 0.0373(14) 0.010(1) -0.0063(12) 0.0051(11) C27 0.0371(15) 0.0299(13) 0.0420(15) -0.0041(11) 0.0136(12) 0.0062(11) C28 0.0567(18) 0.0369(15) 0.0321(14) -0.0065(11) -0.0160(13) -0.0037(13) C29 0.0275(13) 0.0493(16) 0.0374(14) 0.0057(12) -0.0018(12) -0.0028(12) C30 0.0283(13) 0.0362(14) 0.0369(14) 0.0105(11) 0.0071(11) 0.0008(11) C31 0.0307(14) 0.0382(14) 0.0439(16) 0.0014(12) 0.0028(12) -0.0063(11) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . O1 . 1.9317(15) yes Ti1 . O3 . 1.9310(15) yes Ti1 . N2 . 2.0642(18) yes Ti1 . N3 . 2.0706(18) yes Ti1 . C11 . 2.485(2) yes Ti1 . C19 . 2.394(2) yes Ti1 . C20 . 2.388(2) yes Ti1 . C21 . 2.376(2) yes Ti1 . C22 . 2.349(2) yes Ti1 . C23 . 2.375(2) yes O1 . C1 . 1.299(3) yes O2 . C1 . 1.213(3) yes O3 . C2 . 1.300(3) yes O4 . C2 . 1.210(3) yes N1 . C1 . 1.410(3) yes N1 . C2 . 1.417(3) yes N1 . C3 . 1.446(3) yes N2 . C11 . 1.333(3) yes N2 . C13 . 1.474(3) yes N3 . C11 . 1.325(3) yes N3 . C16 . 1.474(3) yes C3 . C4 . 1.397(3) yes C3 . C8 . 1.390(3) yes C4 . C5 . 1.397(4) yes C4 . C9 . 1.500(4) yes C5 . C6 . 1.374(4) yes C5 . H51 . 1.000(3) no C6 . C7 . 1.387(4) yes C6 . H61 . 1.000(3) no C7 . C8 . 1.399(4) yes C7 . H71 . 1.000(3) no C8 . C10 . 1.502(4) yes C9 . H91 . 1.000(3) no C9 . H92 . 1.000(3) no C9 . H93 . 1.000(3) no C10 . H101 . 1.000(2) no C10 . H102 . 1.000(3) no C10 . H103 . 1.000(3) no C11 . C12 . 1.501(3) yes C12 . H121 . 1.000(3) no C12 . H122 . 1.000(3) no C12 . H123 . 1.000(3) no C13 . C14 . 1.516(4) yes C13 . C15 . 1.530(3) yes C13 . H131 . 1.000(2) no C14 . H141 . 1.000(3) no C14 . H142 . 1.000(3) no C14 . H143 . 1.000(3) no C15 . H151 . 1.000(2) no C15 . H152 . 1.000(3) no C15 . H153 . 1.000(3) no C16 . C17 . 1.528(4) yes C16 . C18 . 1.532(4) yes C16 . H161 . 1.000(2) no C17 . H171 . 1.000(3) no C17 . H172 . 1.000(3) no C17 . H173 . 1.000(3) no C18 . H181 . 1.000(3) no C18 . H182 . 1.000(3) no C18 . H183 . 1.000(4) no C19 . C20 . 1.422(4) yes C19 . C23 . 1.411(4) yes C19 . C24 . 1.498(4) yes C20 . C21 . 1.427(3) yes C20 . C25 . 1.499(4) yes C21 . C22 . 1.427(3) yes C21 . C26 . 1.498(3) yes C22 . C23 . 1.420(3) yes C22 . C27 . 1.495(4) yes C23 . C28 . 1.503(4) yes C24 . H241 . 1.000(3) no C24 . H242 . 1.000(4) no C24 . H243 . 1.000(4) no C25 . H251 . 1.000(3) no C25 . H252 . 1.000(3) no C25 . H253 . 1.000(3) no C26 . H261 . 1.000(2) no C26 . H262 . 1.000(3) no C26 . H263 . 1.000(3) no C27 . H271 . 1.000(3) no C27 . H272 . 1.000(3) no C27 . H273 . 1.000(3) no C28 . H281 . 1.000(3) no C28 . H282 . 1.000(3) no C28 . H283 . 1.000(3) no C29 . C30 . 1.382(4) yes C29 . C31 2_665 1.384(4) yes C29 . H291 . 1.000(3) no C30 . C31 . 1.381(4) yes C30 . H301 . 1.000(3) no C31 . H311 . 1.000(3) 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 O1 . Ti1 . O3 . 83.38(6) yes O1 . Ti1 . N2 . 88.70(7) yes O3 . Ti1 . N2 . 127.65(7) yes O1 . Ti1 . N3 . 136.68(7) yes O3 . Ti1 . N3 . 87.71(7) yes N2 . Ti1 . N3 . 64.09(7) yes O1 . Ti1 . C11 . 111.83(7) yes O3 . Ti1 . C11 . 106.22(7) yes N2 . Ti1 . C11 . 32.43(7) yes N3 . Ti1 . C11 . 32.21(7) yes O1 . Ti1 . C19 . 139.98(8) yes O3 . Ti1 . C19 . 114.52(8) yes N2 . Ti1 . C19 . 104.40(8) yes N3 . Ti1 . C19 . 81.75(8) yes C11 . Ti1 . C19 . 97.63(8) yes O1 . Ti1 . C20 . 110.65(8) yes O3 . Ti1 . C20 . 142.36(8) yes N2 . Ti1 . C20 . 88.52(8) yes N3 . Ti1 . C20 . 102.10(8) yes C11 . Ti1 . C20 . 100.57(8) yes O1 . Ti1 . C21 . 82.39(7) yes O3 . Ti1 . C21 . 121.55(8) yes N2 . Ti1 . C21 . 108.33(8) yes N3 . Ti1 . C21 . 136.36(8) yes C11 . Ti1 . C21 . 131.66(8) yes O1 . Ti1 . C22 . 89.29(8) yes O3 . Ti1 . C22 . 88.49(8) yes N2 . Ti1 . C22 . 143.23(8) yes N3 . Ti1 . C22 . 132.87(8) yes C11 . Ti1 . C22 . 155.16(8) yes O1 . Ti1 . C23 . 123.24(8) yes O3 . Ti1 . C23 . 85.05(8) yes N2 . Ti1 . C23 . 138.77(8) yes N3 . Ti1 . C23 . 97.90(8) yes C11 . Ti1 . C23 . 124.76(8) yes C19 . Ti1 . C20 . 34.58(9) yes C19 . Ti1 . C21 . 57.63(8) yes C20 . Ti1 . C21 . 34.85(8) yes C19 . Ti1 . C22 . 57.68(8) yes C20 . Ti1 . C22 . 58.16(8) yes C21 . Ti1 . C22 . 35.16(8) yes C19 . Ti1 . C23 . 34.41(9) yes C20 . Ti1 . C23 . 57.79(8) yes C21 . Ti1 . C23 . 58.09(8) yes C22 . Ti1 . C23 . 34.98(8) yes Ti1 . O1 . C1 . 135.72(13) yes Ti1 . O3 . C2 . 136.45(14) yes C1 . N1 . C2 . 127.60(18) yes C1 . N1 . C3 . 115.93(17) yes C2 . N1 . C3 . 116.44(17) yes Ti1 . N2 . C11 . 91.44(13) yes Ti1 . N2 . C13 . 140.95(15) yes C11 . N2 . C13 . 122.10(19) yes Ti1 . N3 . C11 . 91.40(13) yes Ti1 . N3 . C16 . 133.98(15) yes C11 . N3 . C16 . 127.60(19) yes O1 . C1 . O2 . 123.51(19) yes O1 . C1 . N1 . 116.99(18) yes O2 . C1 . N1 . 119.50(19) yes O3 . C2 . O4 . 123.9(2) yes O3 . C2 . N1 . 116.63(18) yes O4 . C2 . N1 . 119.5(2) yes N1 . C3 . C4 . 119.0(2) yes N1 . C3 . C8 . 118.6(2) yes C4 . C3 . C8 . 122.5(2) yes C3 . C4 . C5 . 118.0(2) yes C3 . C4 . C9 . 120.3(2) yes C5 . C4 . C9 . 121.7(2) yes C4 . C5 . C6 . 120.6(3) yes C4 . C5 . H51 . 119.7(3) no C6 . C5 . H51 . 119.7(3) no C5 . C6 . C7 . 120.5(2) yes C5 . C6 . H61 . 119.8(3) no C7 . C6 . H61 . 119.8(3) no C6 . C7 . C8 . 120.8(2) yes C6 . C7 . H71 . 119.6(3) no C8 . C7 . H71 . 119.6(3) no C3 . C8 . C7 . 117.7(2) yes C3 . C8 . C10 . 120.6(2) yes C7 . C8 . C10 . 121.8(2) yes C4 . C9 . H91 . 109.5(2) no C4 . C9 . H92 . 109.5(2) no H91 . C9 . H92 . 109.5(3) no C4 . C9 . H93 . 109.5(2) no H91 . C9 . H93 . 109.5(3) no H92 . C9 . H93 . 109.5(3) no C8 . C10 . H101 . 109.5(3) no C8 . C10 . H102 . 109.5(2) no H101 . C10 . H102 . 109.5(2) no C8 . C10 . H103 . 109.5(2) no H101 . C10 . H103 . 109.5(3) no H102 . C10 . H103 . 109.5(3) no Ti1 . C11 . N2 . 56.12(11) yes Ti1 . C11 . N3 . 56.39(11) yes N2 . C11 . N3 . 111.23(19) yes Ti1 . C11 . C12 . 170.56(16) yes N2 . C11 . C12 . 123.9(2) yes N3 . C11 . C12 . 124.9(2) yes C11 . C12 . H121 . 109.5(2) no C11 . C12 . H122 . 109.5(2) no H121 . C12 . H122 . 109.5(2) no C11 . C12 . H123 . 109.5(2) no H121 . C12 . H123 . 109.5(2) no H122 . C12 . H123 . 109.5(2) no N2 . C13 . C14 . 110.63(19) yes N2 . C13 . C15 . 111.20(19) yes C14 . C13 . C15 . 110.1(2) yes N2 . C13 . H131 . 107.7(2) no C14 . C13 . H131 . 108.8(2) no C15 . C13 . H131 . 108.2(2) no C13 . C14 . H141 . 109.5(2) no C13 . C14 . H142 . 109.5(2) no H141 . C14 . H142 . 109.5(3) no C13 . C14 . H143 . 109.5(2) no H141 . C14 . H143 . 109.5(3) no H142 . C14 . H143 . 109.5(3) no C13 . C15 . H151 . 109.5(2) no C13 . C15 . H152 . 109.5(2) no H151 . C15 . H152 . 109.5(3) no C13 . C15 . H153 . 109.5(2) no H151 . C15 . H153 . 109.5(3) no H152 . C15 . H153 . 109.5(3) no N3 . C16 . C17 . 112.5(2) yes N3 . C16 . C18 . 113.8(2) yes C17 . C16 . C18 . 112.1(2) yes N3 . C16 . H161 . 105.0(2) no C17 . C16 . H161 . 107.1(2) no C18 . C16 . H161 . 105.6(2) no C16 . C17 . H171 . 109.5(3) no C16 . C17 . H172 . 109.5(2) no H171 . C17 . H172 . 109.5(3) no C16 . C17 . H173 . 109.5(2) no H171 . C17 . H173 . 109.5(3) no H172 . C17 . H173 . 109.5(3) no C16 . C18 . H181 . 109.5(3) no C16 . C18 . H182 . 109.5(3) no H181 . C18 . H182 . 109.5(3) no C16 . C18 . H183 . 109.5(3) no H181 . C18 . H183 . 109.5(3) no H182 . C18 . H183 . 109.5(3) no Ti1 . C19 . C20 . 72.47(13) yes Ti1 . C19 . C23 . 72.04(13) yes C20 . C19 . C23 . 108.7(2) yes Ti1 . C19 . C24 . 126.48(17) yes C20 . C19 . C24 . 124.4(3) yes C23 . C19 . C24 . 126.6(3) yes Ti1 . C20 . C19 . 72.94(13) yes Ti1 . C20 . C21 . 72.11(12) yes C19 . C20 . C21 . 107.6(2) yes Ti1 . C20 . C25 . 125.85(16) yes C19 . C20 . C25 . 124.3(2) yes C21 . C20 . C25 . 127.7(2) yes Ti1 . C21 . C20 . 73.04(12) yes Ti1 . C21 . C22 . 71.39(12) yes C20 . C21 . C22 . 107.6(2) yes Ti1 . C21 . C26 . 121.41(16) yes C20 . C21 . C26 . 127.7(2) yes C22 . C21 . C26 . 124.8(2) yes Ti1 . C22 . C21 . 73.46(12) yes Ti1 . C22 . C23 . 73.50(13) yes C21 . C22 . C23 . 108.2(2) yes Ti1 . C22 . C27 . 120.02(16) yes C21 . C22 . C27 . 125.7(2) yes C23 . C22 . C27 . 126.1(2) yes Ti1 . C23 . C19 . 73.55(13) yes Ti1 . C23 . C22 . 71.51(13) yes C19 . C23 . C22 . 107.9(2) yes Ti1 . C23 . C28 . 120.66(16) yes C19 . C23 . C28 . 127.3(2) yes C22 . C23 . C28 . 124.8(2) yes C19 . C24 . H241 . 109.5(3) no C19 . C24 . H242 . 109.5(3) no H241 . C24 . H242 . 109.5(3) no C19 . C24 . H243 . 109.5(3) no H241 . C24 . H243 . 109.5(3) no H242 . C24 . H243 . 109.5(3) no C20 . C25 . H251 . 109.5(2) no C20 . C25 . H252 . 109.5(2) no H251 . C25 . H252 . 109.5(3) no C20 . C25 . H253 . 109.5(2) no H251 . C25 . H253 . 109.5(3) no H252 . C25 . H253 . 109.5(3) no C21 . C26 . H261 . 109.5(2) no C21 . C26 . H262 . 109.5(2) no H261 . C26 . H262 . 109.5(3) no C21 . C26 . H263 . 109.5(2) no H261 . C26 . H263 . 109.5(2) no H262 . C26 . H263 . 109.5(3) no C22 . C27 . H271 . 109.5(2) no C22 . C27 . H272 . 109.5(2) no H271 . C27 . H272 . 109.5(3) no C22 . C27 . H273 . 109.5(2) no H271 . C27 . H273 . 109.5(3) no H272 . C27 . H273 . 109.5(3) no C23 . C28 . H281 . 109.5(3) no C23 . C28 . H282 . 109.5(3) no H281 . C28 . H282 . 109.5(3) no C23 . C28 . H283 . 109.5(3) no H281 . C28 . H283 . 109.5(3) no H282 . C28 . H283 . 109.5(3) no C30 . C29 . C31 2_665 120.2(3) yes C30 . C29 . H291 . 119.9(3) no C31 2_665 C29 . H291 . 119.9(3) no C29 . C30 . C31 . 119.5(3) yes C29 . C30 . H301 . 120.2(3) no C31 . C30 . H301 . 120.2(3) no C29 2_665 C31 . C30 . 120.3(3) yes C29 2_665 C31 . H311 . 119.8(3) no C30 . C31 . H311 . 119.8(3) no #===end