#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4062453.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4062453 _journal_name_full 'Organometallics' _journal_year 2003 _chemical_name_common '[{TiCl(C7H12N3)(NtBu)}2]' _chemical_formula_moiety 'C22 H42 Cl2 N8 Ti2' _chemical_formula_structural 'C22 H42 Cl2 N8 Ti2' _chemical_formula_sum 'C22 H42 Cl2 N8 Ti2' _chemical_formula_weight 585.34 _symmetry_cell_setting monoclinic _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.8443(11) _cell_length_b 9.1562(4) _cell_length_c 19.2712(10) _cell_angle_alpha 90 _cell_angle_beta 115.112(2) _cell_angle_gamma 90 _cell_volume 2851.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _exptl_crystal_density_diffrn 1.364 _diffrn_ambient_temperature 173(2) 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 Ti Ti 0.05010(2) 0.04963(4) 0.07426(2) 0.01981(14) Uani 1 1 d . . . Cl Cl -0.01634(4) 0.21898(6) 0.11917(3) 0.03602(18) Uani 1 1 d . . . N1 N 0.13356(11) -0.0026(2) 0.18525(10) 0.0268(4) Uani 1 1 d . . . N2 N 0.16925(11) 0.0103(2) 0.08936(10) 0.0271(4) Uani 1 1 d . . . N3 N 0.26827(11) -0.0854(2) 0.20744(11) 0.0308(5) Uani 1 1 d . . . N4 N -0.01396(10) -0.11347(18) 0.03255(10) 0.0210(4) Uani 1 1 d . . . C1 C 0.19394(13) -0.0282(2) 0.16261(13) 0.0242(5) Uani 1 1 d . A . C5 C 0.32739(14) -0.1134(3) 0.17466(15) 0.0398(6) Uani 1 1 d . A . H5A H 0.3629 -0.1976 0.201 0.048 Uiso 1 1 calc R . . H5B H 0.3634 -0.0271 0.1822 0.048 Uiso 1 1 calc R . . C6 C 0.28134(15) -0.1457(3) 0.09003(15) 0.0402(6) Uani 1 1 d . . . H6A H 0.2507 -0.2389 0.0828 0.048 Uiso 1 1 calc R A . H6B H 0.3213 -0.1565 0.0672 0.048 Uiso 1 1 calc R . . C7 C 0.22089(15) -0.0230(3) 0.04969(15) 0.0358(6) Uani 1 1 d . A . H7A H 0.2521 0.0654 0.0481 0.043 Uiso 1 1 calc R . . H7B H 0.1853 -0.0522 -0.0037 0.043 Uiso 1 1 calc R . . C8 C -0.03162(13) -0.2497(2) 0.06502(12) 0.0248(5) Uani 1 1 d . A . C9 C -0.09945(15) -0.3363(2) 0.00093(14) 0.0346(6) Uani 1 1 d . . . H9A H -0.0806 -0.3615 -0.0385 0.052 Uiso 1 1 calc R A . H9B H -0.1497 -0.2768 -0.0219 0.052 Uiso 1 1 calc R . . H9C H -0.1114 -0.4259 0.0222 0.052 Uiso 1 1 calc R . . C10 C -0.06051(16) -0.2111(3) 0.12635(14) 0.0369(6) Uani 1 1 d . . . H10A H -0.1114 -0.1531 0.1036 0.055 Uiso 1 1 calc R A . H10B H -0.0174 -0.1544 0.1669 0.055 Uiso 1 1 calc R . . H10C H -0.0714 -0.3009 0.1482 0.055 Uiso 1 1 calc R . . C11 C 0.04767(15) -0.3401(3) 0.09888(16) 0.0400(6) Uani 1 1 d . . . H11A H 0.0654 -0.3638 0.0585 0.06 Uiso 1 1 calc R A . H11B H 0.0374 -0.4305 0.1206 0.06 Uiso 1 1 calc R . . H11C H 0.0912 -0.2839 0.1393 0.06 Uiso 1 1 calc R . . C2 C 0.14878(15) -0.0318(3) 0.26393(13) 0.0341(6) Uani 0.893(7) 1 d P A 1 H2A H 0.1292 -0.1314 0.2676 0.041 Uiso 0.893(7) 1 calc PR A 1 H2B H 0.117 0.0383 0.28 0.041 Uiso 0.893(7) 1 calc PR A 1 C3 C 0.23924(18) -0.0194(3) 0.31703(16) 0.0384(9) Uani 0.893(7) 1 d P A 1 H3A H 0.2485 -0.0506 0.3692 0.046 Uiso 0.893(7) 1 calc PR A 1 H3B H 0.2572 0.0835 0.3196 0.046 Uiso 0.893(7) 1 calc PR A 1 C4 C 0.28979(15) -0.1155(3) 0.28790(14) 0.0370(6) Uani 0.893(7) 1 d P A 1 H4A H 0.3495 -0.0968 0.3186 0.044 Uiso 0.893(7) 1 calc PR A 1 H4B H 0.279 -0.2196 0.2941 0.044 Uiso 0.893(7) 1 calc PR A 1 C2A C 0.14878(15) -0.0318(3) 0.26393(13) 0.0341(6) Uani 0.107(7) 1 d P A 2 H2A1 H 0.0972 -0.0684 0.2653 0.041 Uiso 0.107(7) 1 calc PR A 2 H2A2 H 0.1641 0.0605 0.2934 0.041 Uiso 0.107(7) 1 calc PR A 2 C3A C 0.2173(12) -0.143(3) 0.3019(11) 0.027(7) Uani 0.107(7) 1 d P A 2 H3A1 H 0.2338 -0.1423 0.3578 0.033 Uiso 0.107(7) 1 calc PR A 2 H3A2 H 0.1957 -0.2418 0.2826 0.033 Uiso 0.107(7) 1 calc PR A 2 C4A C 0.28979(15) -0.1155(3) 0.28790(14) 0.0370(6) Uani 0.107(7) 1 d P A 2 H4A1 H 0.3268 -0.2016 0.3042 0.044 Uiso 0.107(7) 1 calc PR A 2 H4A2 H 0.3204 -0.0311 0.3192 0.044 Uiso 0.107(7) 1 calc PR A 2 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 Ti 0.0176(2) 0.0209(2) 0.0200(2) -0.00011(14) 0.00711(17) 0.00150(15) Cl 0.0325(3) 0.0388(3) 0.0386(4) -0.0084(2) 0.0169(3) 0.0077(3) N1 0.0216(10) 0.0338(10) 0.0223(10) 0.0022(8) 0.0066(8) 0.0026(8) N2 0.0194(10) 0.0361(10) 0.0263(11) 0.0053(8) 0.0101(8) 0.0045(8) N3 0.0210(10) 0.0338(10) 0.0312(11) 0.0047(8) 0.0049(8) 0.0054(8) N4 0.0197(9) 0.0204(9) 0.0241(10) 0.0019(7) 0.0103(8) 0.0030(7) C1 0.0193(11) 0.0199(11) 0.0284(13) 0.0001(8) 0.0053(10) -0.0005(9) C5 0.0236(13) 0.0402(14) 0.0521(17) 0.0099(12) 0.0127(12) 0.0093(11) C6 0.0311(14) 0.0473(15) 0.0473(16) 0.0059(12) 0.0216(12) 0.0134(12) C7 0.0283(13) 0.0467(15) 0.0386(15) 0.0089(11) 0.0203(12) 0.0091(11) C8 0.0299(13) 0.0204(10) 0.0261(12) 0.0037(8) 0.0137(10) 0.0002(9) C9 0.0415(14) 0.0253(12) 0.0370(14) -0.0013(10) 0.0167(11) -0.0081(11) C10 0.0470(16) 0.0367(14) 0.0327(14) 0.0019(10) 0.0225(12) -0.0085(11) C11 0.0396(15) 0.0258(12) 0.0507(17) 0.0104(11) 0.0153(13) 0.0058(11) C2 0.0346(14) 0.0386(13) 0.0252(13) 0.0029(10) 0.0089(11) 0.0022(11) C3 0.0395(17) 0.040(2) 0.0246(15) 0.0003(12) 0.0025(13) 0.0022(14) C4 0.0330(13) 0.0345(13) 0.0304(14) 0.0041(10) 0.0009(11) 0.0051(11) C2A 0.0346(14) 0.0386(13) 0.0252(13) 0.0029(10) 0.0089(11) 0.0022(11) C3A 0.016(11) 0.047(16) 0.012(11) 0.014(9) -0.001(8) 0.009(10) C4A 0.0330(13) 0.0345(13) 0.0304(14) 0.0041(10) 0.0009(11) 0.0051(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti N4 1.8447(17) . ? Ti N4 1.9667(17) 5 ? Ti N2 2.0519(18) . ? Ti N1 2.0779(18) . ? Ti Cl 2.3301(7) . ? Ti C1 2.507(2) . ? Ti Ti 2.8056(7) 5 ? N1 C1 1.343(3) . ? N1 C2 1.447(3) . ? N2 C1 1.335(3) . ? N2 C7 1.457(3) . ? N3 C1 1.344(3) . ? N3 C4 1.457(3) . ? N3 C5 1.464(3) . ? N4 C8 1.488(3) . ? N4 Ti 1.9667(17) 5 ? C5 C6 1.512(4) . ? C6 C7 1.523(3) . ? C8 C10 1.518(3) . ? C8 C11 1.526(3) . ? C8 C9 1.533(3) . ? C2 C3 1.505(4) . ? C3 C4 1.527(4) . ?