#------------------------------------------------------------------------------ #$Date: 2009-11-18 15:56:34 +0100 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/4/4301058.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_4301058 _journal_name_full 'Inorganic Chemistry' _journal_year 2005 _publ_section_title ; New titanium imido synthons: syntheses and supramolecular structures ; loop_ _publ_author_name 'N. Adams, H. R. Bigmore, T. L. Blundell, ' 'C. L. Boyd, S. R. Dubberley, ' 'A. J. Sealey, A. R. Cowley, ' 'M. E. G. Skinner and P. Mountford' _chemical_formula_sum 'C13 H18 Cl6 N3 Ti' _[local]_cod_chemical_formula_sum_orig ' C13 H18 Cl6 N3 Ti1 ' _chemical_formula_moiety ' C10 H15 Cl6 N3 Ti1 . 0.5 (C6 H6) ' _cell_length_a 7.3945(1) _cell_length_b 12.7544(2) _cell_length_c 12.9622(2) _cell_angle_alpha 115.6105(9) _cell_angle_beta 90.7721(8) _cell_angle_gamma 106.112(1) _cell_volume 1046.45 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _cell_formula_units_Z 2 _chemical_formula_weight 476.92 _cell_measurement_temperature 150 _exptl_crystal_density_diffrn 1.513 _diffrn_ambient_temperature 150 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_attached_hydrogens Ti1 Ti 0.03381(5) 0.02529(3) 0.25870(3) 0.0166 1.0000 Uani . N1 N 0.2427(2) 0.14358(17) 0.30819(16) 0.0217 1.0000 Uani . N2 N 0.1120(3) -0.09902(17) 0.31267(16) 0.0230 1.0000 Uani . N3 N -0.1244(2) 0.10460(17) 0.18304(16) 0.0228 1.0000 Uani . C1 C 0.3980(3) 0.24660(18) 0.35655(18) 0.0190 1.0000 Uani . C2 C 0.5014(3) 0.28360(19) 0.46549(18) 0.0204 1.0000 Uani . C3 C 0.6576(3) 0.3892(2) 0.51454(19) 0.0242 1.0000 Uani . C4 C 0.7136(3) 0.4616(2) 0.4583(2) 0.0257 1.0000 Uani . C5 C 0.6146(3) 0.42616(19) 0.3514(2) 0.0236 1.0000 Uani . C6 C 0.4613(3) 0.31910(19) 0.29918(18) 0.0205 1.0000 Uani . C7 C -0.0380(4) -0.2182(2) 0.2756(2) 0.0353 1.0000 Uani . C8 C 0.2967(3) -0.1192(2) 0.2838(2) 0.0335 1.0000 Uani . C9 C -0.3259(3) 0.0309(3) 0.1322(2) 0.0388 1.0000 Uani . C10 C -0.1112(4) 0.2334(2) 0.2589(2) 0.0321 1.0000 Uani . Cl1 Cl 0.02846(9) -0.11429(5) 0.06822(5) 0.0305 1.0000 Uani . Cl2 Cl -0.16605(8) 0.05330(6) 0.39934(5) 0.0298 1.0000 Uani . Cl3 Cl 0.42852(8) 0.19431(5) 0.53476(5) 0.0291 1.0000 Uani . Cl4 Cl 0.78693(9) 0.43322(6) 0.64620(5) 0.0360 1.0000 Uani . Cl5 Cl 0.68878(9) 0.51610(6) 0.28248(6) 0.0364 1.0000 Uani . Cl6 Cl 0.34607(8) 0.27055(5) 0.16239(5) 0.0285 1.0000 Uani . H1 H 0.1255 -0.05851 0.38769 0.0284 1.0000 Uiso . H2 H -0.0632 0.10313 0.12584 0.0289 1.0000 Uiso . H41 H 0.8244 0.5386 0.4949 0.0279 1.0000 Uiso . H71 H -0.1622 -0.2040 0.2953 0.0433 1.0000 Uiso . H72 H -0.0032 -0.2625 0.3164 0.0433 1.0000 Uiso . H73 H -0.0500 -0.2686 0.1901 0.0433 1.0000 Uiso . H81 H 0.3975 -0.0384 0.3090 0.0433 1.0000 Uiso . H82 H 0.3320 -0.1634 0.3246 0.0433 1.0000 Uiso . H83 H 0.2852 -0.1694 0.1983 0.0433 1.0000 Uiso . H91 H -0.3338 -0.0561 0.0811 0.0449 1.0000 Uiso . H92 H -0.4030 0.0343 0.1957 0.0449 1.0000 Uiso . H93 H -0.3766 0.0646 0.0856 0.0449 1.0000 Uiso . H101 H 0.0250 0.2826 0.2929 0.0414 1.0000 Uiso . H102 H -0.1880 0.2372 0.3226 0.0414 1.0000 Uiso . H103 H -0.1616 0.2675 0.2125 0.0414 1.0000 Uiso . C11 C -0.0390(12) 0.4258(7) 0.0496(7) 0.0584(18) 0.5000 Uiso . C12 C 0.1325(13) 0.4994(11) 0.0446(11) 0.093(3) 0.5000 Uiso . C13 C 0.1293(13) 0.5718(9) -0.013(1) 0.083(3) 0.5000 Uiso . C14 C -0.0484(11) 0.5608(6) -0.0595(6) 0.0498(15) 0.5000 Uiso . C15 C -0.2146(13) 0.4863(11) -0.0568(11) 0.101(4) 0.5000 Uiso . C16 C -0.2119(13) 0.4233(12) 0.0034(12) 0.112(4) 0.5000 Uiso . H111 H -0.0395 0.3720 0.0873 0.0704 0.5000 Uiso . H121 H 0.2552 0.5021 0.0805 0.1116 0.5000 Uiso . H131 H 0.2490 0.6276 -0.019 0.0999 0.5000 Uiso . H141 H -0.0529 0.6129 -0.0985 0.0597 0.5000 Uiso . H151 H -0.3367 0.4778 -0.0984 0.1209 0.5000 Uiso . H161 H -0.3343 0.3749 0.0153 0.1364 0.5000 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 0.01670(15) 0.01784(16) 0.01440(16) 0.00844(13) 0.00084(12) 0.00246(13) N1 0.0202(8) 0.0231(9) 0.0230(9) 0.0129(7) 0.0020(7) 0.0046(7) N2 0.0271(9) 0.0242(9) 0.0196(8) 0.0130(7) 0.0023(7) 0.0056(7) N3 0.0220(8) 0.0298(9) 0.0205(8) 0.0134(8) 0.0043(7) 0.0104(7) C1 0.0158(8) 0.0166(9) 0.022(1) 0.0072(8) 0.0025(7) 0.0040(7) C2 0.0209(9) 0.022(1) 0.0200(9) 0.0098(8) 0.0043(8) 0.0086(8) C3 0.0195(9) 0.023(1) 0.022(1) 0.0040(8) -0.0010(8) 0.0070(8) C4 0.0179(9) 0.019(1) 0.0323(12) 0.0071(9) 0.0017(8) 0.0030(8) C5 0.0206(9) 0.020(1) 0.0317(11) 0.0130(9) 0.0070(8) 0.0060(8) C6 0.0199(9) 0.021(1) 0.022(1) 0.0101(8) 0.0034(7) 0.0065(8) C7 0.0386(13) 0.0273(12) 0.0424(14) 0.0224(11) 0.0082(11) 0.003(1) C8 0.0296(12) 0.0390(13) 0.0396(13) 0.0219(11) 0.004(1) 0.016(1) C9 0.0257(11) 0.0485(16) 0.0381(14) 0.0183(12) -0.007(1) 0.0086(11) C10 0.0381(12) 0.0303(12) 0.0351(13) 0.016(1) 0.012(1) 0.019(1) Cl1 0.0503(3) 0.0269(3) 0.0166(2) 0.0092(2) 0.0045(2) 0.0166(2) Cl2 0.0282(3) 0.0445(3) 0.0242(3) 0.0204(2) 0.0101(2) 0.0141(2) Cl3 0.0315(3) 0.0323(3) 0.0256(3) 0.0178(2) 0.0000(2) 0.0053(2) Cl4 0.0314(3) 0.0347(3) 0.0289(3) 0.0074(2) -0.0104(2) 0.0040(2) Cl5 0.0332(3) 0.0303(3) 0.0503(4) 0.0272(3) 0.0082(3) 0.0016(2) Cl6 0.0317(3) 0.0297(3) 0.0241(3) 0.0156(2) 0.0008(2) 0.0043(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 . 1.7079(18) yes Ti1 . N2 . 2.1894(18) yes Ti1 . N3 . 2.1992(18) yes Ti1 . Cl1 . 2.3293(6) yes Ti1 . Cl2 . 2.3319(6) yes N1 . C1 . 1.367(3) yes N2 . C7 . 1.480(3) yes N2 . C8 . 1.483(3) yes N2 . H1 . 0.870 yes N3 . C9 . 1.483(3) yes N3 . C10 . 1.479(3) yes N3 . H2 . 0.870 yes C1 . C2 . 1.413(3) yes C1 . C6 . 1.411(3) yes C2 . C3 . 1.388(3) yes C2 . Cl3 . 1.718(2) yes C3 . C4 . 1.391(3) yes C3 . Cl4 . 1.724(2) yes C4 . C5 . 1.382(3) yes C5 . C6 . 1.389(3) yes C5 . Cl5 . 1.721(2) yes C6 . Cl6 . 1.724(2) yes Cl1 . H2 2_555 2.5922 yes Cl2 . H1 2_556 2.7428 yes Ti1 . Ti1 2_555 6.4527(7) yes Ti1 . Ti1 2_556 6.5720(7) yes C3 . C5 2_666 3.436(3) yes C11 . C12 . 1.374(8) yes C11 . C16 . 1.390(8) yes C12 . C13 . 1.415(8) yes C13 . C14 . 1.385(8) yes C14 . C15 . 1.341(8) yes C15 . C16 . 1.343(8) yes