#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2009009.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_2009009 _journal_name_full 'Acta Crystallographica' _journal_year 1999 _journal_volume C55 _journal_page_first 1636 _journal_page_last 1639 _publ_section_title ; The twinned structure of the \m-isopropoxido-diisopropoxido(p-tolylimido)vanadium(V) dimer, twin refinement against CCD area-detector data ; loop_ _publ_author_name 'Lutz, Martin' 'Hagen, Henk' 'Schreurs, Antoine M.M.' 'Spek, Anthony L.' 'van Koten, Gerard' _chemical_formula_moiety 'C32 H56 N2 O6 V2' _chemical_formula_sum 'C32 H56 N2 O6 V2' _chemical_formula_iupac '[V2 (C7 H7 N)2 (C3 H7 O)6]' _chemical_formula_weight 666.67 _chemical_melting_point 316 _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_length_a 9.7491(6) _cell_length_b 10.0291(6) _cell_length_c 11.1681(5) _cell_angle_alpha 85.297(4) _cell_angle_beta 71.869(4) _cell_angle_gamma 61.3013(18) _cell_volume 907.28(9) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.220 _diffrn_ambient_temperature 150(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 V .09634(4) .40966(4) .35830(3) .01771(11) Uani d . 1 . . V O1 .11886(17) .56053(16) .26980(13) .0233(3) Uani d . 1 . . O O2 .12243(15) .39492(15) .51737(12) .0188(3) Uani d . 1 . . O O3 -.06219(16) .37786(16) .33799(13) .0237(3) Uani d . 1 . . O N1 .2636(2) .25189(19) .27968(15) .0213(4) Uani d . 1 . . N C1 .3978(2) .1152(2) .21911(18) .0204(4) Uani d . 1 . . C C2 .5397(3) .1119(3) .1341(2) .0289(5) Uani d . 1 . . C H2 .5437 .2044 .1157 .035 Uiso calc R 1 . . H C3 .6746(3) -.0258(3) .0768(2) .0314(5) Uani d . 1 . . C H3 .7699 -.0257 .0197 .038 Uiso calc R 1 . . H C4 .6744(3) -.1627(2) .10027(19) .0264(5) Uani d . 1 . . C C5 .5327(3) -.1592(3) .1835(2) .0294(5) Uani d . 1 . . C H5 .5294 -.2521 .2007 .035 Uiso calc R 1 . . H C6 .3964(3) -.0236(2) .2420(2) .0257(5) Uani d . 1 . . C H6 .3010 -.0246 .2981 .031 Uiso calc R 1 . . H C7 .8214(3) -.3134(3) .0396(2) .0378(6) Uani d . 1 . . C H7A .9108 -.2958 -.0147 .057 Uiso calc R 1 . . H H7B .7907 -.3633 -.0114 .057 Uiso calc R 1 . . H H7C .8581 -.3789 .1055 .057 Uiso calc R 1 . . H C8 .2469(3) .5673(3) .1709(2) .0267(5) Uani d . 1 . . C H8 .2864 .4885 .1013 .032 Uiso calc R 1 . . H C9 .3888(3) .5357(3) .2173(2) .0379(6) Uani d . 1 . . C H9A .4320 .4333 .2471 .057 Uiso calc R 1 . . H H9B .3506 .6112 .2868 .057 Uiso calc R 1 . . H H9C .4759 .5423 .1479 .057 Uiso calc R 1 . . H C10 .1786(3) .7236(3) .1213(3) .0490(7) Uani d . 1 . . C H10A .0872 .7407 .0915 .073 Uiso calc R 1 . . H H10B .2652 .7295 .0511 .073 Uiso calc R 1 . . H H10C .1389 .8016 .1891 .073 Uiso calc R 1 . . H C11 .2491(2) .2926(2) .57076(19) .0211(5) Uani d . 1 . . C H11 .2156 .3349 .6593 .025 Uiso calc R 1 . . H C12 .4109(3) .2897(3) .5006(2) .0292(5) Uani d . 1 . . C H12A .3950 .3939 .4992 .044 Uiso calc R 1 . . H H12B .4499 .2456 .4137 .044 Uiso calc R 1 . . H H12C .4924 .2277 .5434 .044 Uiso calc R 1 . . H C13 .2592(3) .1368(3) .5789(2) .0297(5) Uani d . 1 . . C H13A .1505 .1476 .6252 .044 Uiso calc R 1 . . H H13B .3378 .0723 .6234 .044 Uiso calc R 1 . . H H13C .2959 .0898 .4935 .044 Uiso calc R 1 . . H C14 -.0588(3) .2464(3) .2957(2) .0275(5) Uani d . 1 . . C H14 .0495 .1835 .2305 .033 Uiso calc R 1 . . H C15 -.1956(3) .2983(3) .2372(3) .0435(7) Uani d . 1 . . C H15A -.1782 .3581 .1658 .065 Uiso calc R 1 . . H H15B -.3017 .3613 .3006 .065 Uiso calc R 1 . . H H15C -.1955 .2090 .2074 .065 Uiso calc R 1 . . H C16 -.0804(4) .1542(3) .4066(3) .0470(7) Uani d . 1 . . C H16A .0095 .1231 .4424 .070 Uiso calc R 1 . . H H16B -.0789 .0634 .3784 .070 Uiso calc R 1 . . H H16C -.1858 .2162 .4711 .070 Uiso calc R 1 . . 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 V .01317(19) .0163(2) .02222(19) -.00647(14) -.00504(14) .00303(13) O1 .0194(8) .0219(8) .0266(8) -.0113(7) -.0035(6) .0056(6) O2 .0133(7) .0167(8) .0208(7) -.0024(6) -.0070(6) .0036(5) O3 .0177(8) .0199(8) .0347(8) -.0100(7) -.0077(6) .0020(6) N1 .0171(9) .0208(10) .0232(9) -.0080(8) -.0046(7) .0020(7) C1 .0170(11) .0178(11) .0220(11) -.0048(9) -.0059(9) -.0009(8) C2 .0231(12) .0217(13) .0347(13) -.0100(10) -.0010(10) .0025(10) C3 .0208(12) .0276(14) .0310(13) -.0072(11) .0041(10) -.0014(10) C4 .0242(12) .0230(13) .0249(11) -.0058(10) -.0061(9) -.0049(9) C5 .0307(13) .0193(12) .0383(13) -.0127(11) -.0088(11) -.0016(10) C6 .0217(12) .0222(13) .0298(12) -.0110(10) -.0027(9) .0000(9) C7 .0301(14) .0285(15) .0379(14) -.0051(11) -.0003(11) -.0118(11) C8 .0271(12) .0309(13) .0246(12) -.0199(11) -.0011(10) .0026(9) C9 .0276(13) .0401(16) .0492(16) -.0220(12) -.0071(11) .0059(12) C10 .0472(17) .0563(19) .0531(17) -.0346(15) -.0185(14) .0326(14) C11 .0171(11) .0171(11) .0245(11) -.0028(9) -.0101(9) .0030(8) C12 .0190(12) .0273(13) .0397(14) -.0070(10) -.0153(10) .0081(10) C13 .0280(13) .0211(13) .0348(13) -.0061(10) -.0138(10) .0063(10) C14 .0240(12) .0261(13) .0366(13) -.0143(10) -.0109(10) .0019(10) C15 .0385(15) .0515(18) .0536(17) -.0265(14) -.0228(13) .0050(13) C16 .0605(19) .0440(17) .0584(17) -.0381(15) -.0288(15) .0212(13) 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 V N1 . 1.6709(16) yes V O3 . 1.8014(14) yes V O1 . 1.8037(14) yes V O2 . 1.8560(13) yes V O2 2_566 2.2151(13) yes O1 C8 . 1.412(2) no O2 C11 . 1.440(2) no O2 V 2_566 2.2151(13) no O3 C14 . 1.419(2) no N1 C1 . 1.389(2) yes C1 C2 . 1.400(3) no C1 C6 . 1.401(3) no C2 C3 . 1.386(3) no C2 H2 . .9500 no C3 C4 . 1.378(3) no C3 H3 . .9500 no C4 C5 . 1.391(3) no C4 C7 . 1.510(3) no C5 C6 . 1.382(3) no C5 H5 . .9500 no C6 H6 . .9500 no C7 H7A . .9800 no C7 H7B . .9800 no C7 H7C . .9800 no C8 C9 . 1.510(3) no C8 C10 . 1.513(3) no C8 H8 . 1.0000 no C9 H9A . .9800 no C9 H9B . .9800 no C9 H9C . .9800 no C10 H10A . .9800 no C10 H10B . .9800 no C10 H10C . .9800 no C11 C13 . 1.514(3) no C11 C12 . 1.514(3) no C11 H11 . 1.0000 no C12 H12A . .9800 no C12 H12B . .9800 no C12 H12C . .9800 no C13 H13A . .9800 no C13 H13B . .9800 no C13 H13C . .9800 no C14 C16 . 1.507(3) no C14 C15 . 1.516(3) no C14 H14 . 1.0000 no C15 H15A . .9800 no C15 H15B . .9800 no C15 H15C . .9800 no C16 H16A . .9800 no C16 H16B . .9800 no C16 H16C . .9800 no