#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011633.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_2011633 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first e542 _journal_page_last e542 _publ_section_title ; The titanium--thiolate complex [Ti~2~(SC~6~H~5~)~9~][Li(C~4~H~8~O)~4~] ; loop_ _publ_author_name 'Puke, Carsten' 'Schmengler, Kai' 'Kirschbaum, Kristin' 'Conrad, Olaf' 'Giolando, Dean M.' _chemical_formula_moiety 'C16 H32 Li1 O4 1+, C54 H45 S9 Ti2 1-' _chemical_formula_sum 'C70 H77 Li1 O4 S9 Ti2' _chemical_formula_structural '[Li(C4H8O1)4][Ti2(C6H5S1)9]' _chemical_formula_iupac '[Li (C4 H8 O)4] [Ti2 (C6 H5 S)9]' _chemical_formula_weight 1372.91 _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P 21 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 19.096(3) _cell_length_b 19.096(3) _cell_length_c 19.096(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6963.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _exptl_crystal_density_diffrn 1.300 _diffrn_ambient_temperature 120(2) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ti1 .38661(5) .11339(5) .88661(5) .0477(4) Uani d S 1 . . Ti Ti2 .49381(4) .00619(4) .99381(4) .0413(3) Uani d S 1 . . Ti S1 .28124(8) .07822(9) .83549(8) .0618(4) Uani d . 1 . . S S2 .50131(7) .13194(6) .95058(7) .0461(3) Uani d . 1 . . S S3 .59641(7) -.03528(7) .94316(7) .0525(3) Uani d . 1 . . S C1 .2171(3) .0403(3) .8905(3) .0574(14) Uani d . 1 . . C C2 .2016(3) .0655(3) .9556(4) .0632(15) Uani d . 1 . . C H2A .2257 .1040 .9730 .076 Uiso calc R 1 . . H C3 .1509(3) .0343(4) .9952(4) .0772(19) Uani d . 1 . . C H3A .1412 .0516 1.0397 .093 Uiso calc R 1 . . H C4 .1136(4) -.0229(4) .9699(5) .084(2) Uani d . 1 . . C H4A .0798 -.0445 .9976 .101 Uiso calc R 1 . . H C5 .1275(4) -.0475(4) .9026(4) .0769(19) Uani d . 1 . . C H5A .1019 -.0846 .8841 .092 Uiso calc R 1 . . H C6 .1797(3) -.0163(3) .8638(4) .0685(16) Uani d . 1 . . C H6A .1901 -.0332 .8193 .082 Uiso calc R 1 . . H C7 .5771(3) .1514(3) .9002(3) .0493(12) Uani d . 1 . . C C8 .6192(3) .2057(3) .9230(3) .0608(14) Uani d . 1 . . C H8A .6056 .2320 .9617 .073 Uiso calc R 1 . . H C9 .6816(3) .2216(3) .8890(4) .0696(17) Uani d . 1 . . C H9A .7094 .2583 .9049 .083 Uiso calc R 1 . . H C10 .7017(3) .1834(4) .8328(4) .0700(18) Uani d . 1 . . C H10A .7440 .1928 .8105 .084 Uiso calc R 1 . . H C11 .6592(3) .1310(4) .8094(3) .0640(16) Uani d . 1 . . C H11A .6729 .1053 .7704 .077 Uiso calc R 1 . . H C12 .5967(3) .1150(3) .8414(3) .0578(14) Uani d . 1 . . C H12A .5681 .0800 .8234 .069 Uiso calc R 1 . . H C13 .6659(3) -.0333(3) 1.0036(3) .0587(14) Uani d . 1 . . C C14 .6881(4) -.0919(5) 1.0352(4) .091(2) Uani d . 1 . . C H14A .6668 -.1346 1.0257 .109 Uiso calc R 1 . . H C15 .7462(5) -.0878(6) 1.0848(5) .110(3) Uani d . 1 . . C H15A .7610 -.1272 1.1093 .132 Uiso calc R 1 . . H C16 .7774(4) -.0265(6) 1.0940(5) .104(3) Uani d . 1 . . C H16A .8150 -.0239 1.1248 .125 Uiso calc R 1 . . H C17 .7577(4) .0301(5) 1.0620(4) .086(2) Uani d . 1 . . C H17A .7813 .0720 1.0703 .104 Uiso calc R 1 . . H C18 .7024(3) .0289(4) 1.0159(4) .0703(17) Uani d . 1 . . C H18A .6893 .0697 .9928 .084 Uiso calc R 1 . . H Li1 .8070(7) -.1930(7) .8070(7) .078(5) Uiso d S 1 . . Li O1 .7208(6) -.1396(6) .7979(7) .082(4) Uiso d PD .50 A 1 O C21 .6628(10) -.1808(10) .7719(14) .121(7) Uiso d PD .50 A 1 C H21A .6706 -.1921 .7230 .145 Uiso calc PR .50 A 1 H H21B .6598 -.2243 .7980 .145 Uiso calc PR .50 A 1 H C22 .6049(9) -.1463(9) .7784(9) .176(6) Uiso d PD .50 A 1 C H22A .5908 -.1404 .8268 .211 Uiso calc PR .50 A 1 H H22B .5669 -.1664 .7513 .211 Uiso calc PR .50 A 1 H C23 .6347(7) -.0778(7) .7453(8) .076(4) Uiso d PD .50 A 1 C H23A .6409 -.0829 .6951 .091 Uiso calc PR .50 A 1 H H23B .6039 -.0384 .7542 .091 Uiso calc PR .50 A 1 H C24 .7055(7) -.0681(7) .7823(8) .079(4) Uiso d PD .50 A 1 C H24A .7403 -.0476 .7516 .094 Uiso calc PR .50 A 1 H H24B .7011 -.0400 .8244 .094 Uiso calc PR .50 A 1 H O1A .7204(7) -.1589(8) .7790(8) .098(5) Uiso d PD .50 A 2 O C21A .6583(7) -.1818(8) .8163(9) .079(4) Uiso d PD .50 A 2 C H21C .6526 -.2322 .8139 .095 Uiso calc PR .50 A 2 H H21D .6594 -.1674 .8650 .095 Uiso calc PR .50 A 2 H C22A .6049(9) -.1463(9) .7784(9) .176(6) Uiso d PD .50 A 2 C H22C .5676 -.1794 .7688 .211 Uiso calc PR .50 A 2 H H22D .5857 -.1100 .8082 .211 Uiso calc PR .50 A 2 H C23A .6235(9) -.1180(10) .7198(9) .095(5) Uiso d PD .50 A 2 C H23C .6115 -.0686 .7194 .114 Uiso calc PR .50 A 2 H H23D .6003 -.1408 .6808 .114 Uiso calc PR .50 A 2 H C24A .6963(12) -.1267(16) .7151(14) .160(10) Uiso d PD .50 A 2 C H24C .7189 -.0816 .7088 .192 Uiso calc PR .50 A 2 H H24D .7078 -.1561 .6754 .192 Uiso calc PR .50 A 2 H O2A .8842(7) -.1439(10) .8539(10) .082(5) Uiso d PD .33 A -3 O C31 .9383(19) -.118(3) .901(2) .265(18) Uiso d PD .33 A -3 C H31A .9194 -.0909 .9391 .318 Uiso calc PR .33 A -3 H H31B .9676 -.1556 .9187 .318 Uiso calc PR .33 A -3 H C32 .972(3) -.078(3) .853(3) .265(18) Uiso d PD .33 A -3 C H32A 1.0143 -.0572 .8721 .318 Uiso calc PR .33 A -3 H H32B .9422 -.0414 .8344 .318 Uiso calc PR .33 A -3 H C33 .989(2) -.134(4) .797(3) .265(18) Uiso d PD .33 A -3 C H33A .9994 -.1126 .7518 .318 Uiso calc PR .33 A -3 H H33B 1.0277 -.1634 .8110 .318 Uiso calc PR .33 A -3 H C34 .930(2) -.167(3) .796(2) .265(18) Uiso d PD .33 A -3 C H34A .9384 -.2172 .8009 .318 Uiso calc PR .33 A -3 H H34B .9062 -.1596 .7519 .318 Uiso calc PR .33 A -3 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti1 .0477(4) .0477(4) .0477(4) .0015(4) -.0015(4) .0015(4) Ti2 .0413(3) .0413(3) .0413(3) -.0006(4) .0006(4) -.0006(4) S1 .0502(8) .0751(10) .0602(9) .0004(7) -.0082(7) .0007(7) S2 .0480(7) .0435(6) .0469(6) -.0024(6) .0007(6) .0013(5) S3 .0489(7) .0551(8) .0536(8) .0033(6) .0045(6) -.0030(6) C1 .042(3) .064(3) .066(3) .005(3) -.006(3) -.001(3) C2 .043(3) .071(4) .076(4) .011(3) -.004(3) -.001(3) C3 .053(3) .092(5) .086(5) .017(3) .014(4) -.002(4) C4 .053(4) .086(5) .114(6) .002(3) .012(4) .018(4) C5 .068(4) .059(4) .104(5) -.007(3) -.007(4) .003(4) C6 .058(3) .067(4) .081(4) .008(3) -.007(3) -.013(3) C7 .050(3) .050(3) .049(3) -.004(2) -.003(2) .011(2) C8 .057(3) .056(3) .070(4) -.006(3) -.002(3) -.002(3) C9 .061(4) .064(4) .084(4) -.017(3) -.010(3) .013(4) C10 .053(3) .082(4) .075(4) -.004(3) .010(3) .028(4) C11 .064(4) .073(4) .056(3) -.005(3) .003(3) .013(3) C12 .059(3) .065(3) .050(3) -.003(3) .000(3) .012(3) C13 .044(3) .070(4) .062(3) .011(3) .004(3) .000(3) C14 .074(4) .105(6) .093(6) .012(4) -.001(4) .021(5) C15 .079(5) .135(8) .117(7) .042(6) -.004(5) .045(6) C16 .061(5) .130(8) .120(7) .008(5) -.018(5) -.012(6) C17 .058(4) .110(6) .090(5) -.003(4) -.014(4) -.002(5) C18 .053(3) .085(4) .074(4) -.009(3) -.003(3) -.008(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 S1 12_565 2.3351(17) yes Ti1 S1 6_456 2.3351(17) no Ti1 S1 . 2.3351(17) no Ti1 S2 . 2.5329(17) yes Ti1 S2 6_456 2.5330(17) no Ti1 S2 12_565 2.5330(17) no Ti2 S3 12_565 2.3240(15) yes Ti2 S3 . 2.3240(15) no Ti2 S3 6_456 2.3241(15) no Ti2 S2 6_456 2.5434(16) yes Ti2 S2 . 2.5435(16) no Ti2 S2 12_565 2.5435(16) no S1 C1 . 1.770(6) no S2 C7 . 1.778(5) no S3 C13 . 1.759(6) no C1 C2 . 1.365(9) no C1 C6 . 1.392(9) no C2 C3 . 1.365(9) no C3 C4 . 1.392(11) no C4 C5 . 1.394(11) no C5 C6 . 1.378(10) no C7 C12 . 1.373(8) no C7 C8 . 1.382(8) no C8 C9 . 1.391(9) no C9 C10 . 1.353(10) no C10 C11 . 1.365(10) no C11 C12 . 1.375(8) no C13 C14 . 1.341(10) no C13 C18 . 1.397(9) no C14 C15 . 1.462(13) no C15 C16 . 1.325(14) no C16 C17 . 1.298(13) no C17 C18 . 1.374(10) no Li1 O1A . 1.856(17) no Li1 O1A 9_645 1.856(17) no Li1 O1A 5_546 1.856(17) no Li1 O1 9_645 1.944(13) no Li1 O1 . 1.944(13) no Li1 O1 5_546 1.944(13) no Li1 O2A 5_546 1.96(3) no Li1 O2A . 1.96(3) no Li1 O2A 9_645 1.96(3) no Li1 C34 5_546 2.40(4) no Li1 C34 . 2.40(4) no Li1 C34 9_645 2.40(4) no O1 C24 . 1.428(14) no O1 C21 . 1.446(16) no C21 C22 . 1.29(2) no C22 C23 . 1.56(2) no C23 C24 . 1.536(19) no O1A C24A . 1.44(2) no O1A C21A . 1.452(18) no C23A C24A . 1.40(2) no O2A C31 . 1.452(19) no O2A C34 . 1.471(19) no C31 C32 . 1.36(4) no C32 C33 . 1.54(4) no C33 C34 . 1.31(4) no