#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200349.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_2200349 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first m242 _journal_page_last m243 _publ_section_title ; Low-temperature oxobis(2,2,6,6-tetramethyl-3,5-heptadionato)vanadium(IV) ; loop_ _publ_author_name 'Urs, Usha K.' 'Anitha, K. C.' 'Lakshmi Raghunathan, K.' 'Shivashankar, S. A.' 'Robinson, W. T.' 'Guru Row, T. N.' _chemical_formula_moiety 'C22 H38 O5 V' _chemical_formula_sum 'C22 H38 O5 V' _chemical_formula_iupac '[V O (C11 H19 O2)2]' _chemical_formula_weight 433.46 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.4515(2) _cell_length_b 10.7953(3) _cell_length_c 12.7494(4) _cell_angle_alpha 90 _cell_angle_beta 109.0250(10) _cell_angle_gamma 90 _cell_volume 1229.79(6) _cell_formula_units_Z 2 _cell_measurement_temperature 149(2) _exptl_crystal_density_diffrn 1.171 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 V1 .71881(10) .26486(9) .31402(8) .0238(3) Uani d . 1 . . V O2 .6290(4) .1734(4) .4098(3) .0278(10) Uani d . 1 . . O O4 .8731(4) .2700(5) .2425(3) .0295(9) Uani d . 1 . . O O1 .8863(5) .3000(4) .4482(3) .0306(12) Uani d . 1 . . O O3 .6198(4) .1396(4) .2014(3) .0272(11) Uani d . 1 . . O C1 .8940(6) .2958(5) .5501(5) .0230(15) Uani d . 1 A . C C15 .5284(7) .0200(6) .0366(5) .0246(15) Uani d . 1 . . C C19 .9992(6) .2808(8) .1103(5) .0328(16) Uani d . 1 . . C C18 .6081(8) -.0684(6) -.0209(6) .0353(17) Uani d . 1 . . C H18A .6418 -.0227 -.0729 .053 Uiso calc R 1 . . H H18B .5396 -.1318 -.0595 .053 Uiso calc R 1 . . H H18C .6924 -.1058 .0338 .053 Uiso calc R 1 . . H C12 .8661(6) .2364(5) .1459(5) .0196(14) Uani d . 1 . . C C3 .6589(7) .1788(6) .5143(5) .0235(14) Uani d . 1 A . C C13 .7560(6) .1642(6) .0780(5) .0236(14) Uani d . 1 . . C H13 .7579 .1482 .0068 .028 Uiso calc R 1 . . H C8 1.0346(7) .3479(7) .6322(6) .0334(17) Uani d . 1 . . C C4 .5548(7) .1020(6) .5605(5) .0265(15) Uani d . 1 . . C C2 .7811(6) .2412(6) .5838(5) .0296(17) Uani d . 1 . . C H2 .7893 .2474 .6583 .035 Uiso calc R 1 A . H C14 .6381(6) .1118(6) .1100(5) .0206(13) Uani d . 1 . . C C17 .4572(9) -.0566(7) .1066(6) .044(2) Uani d . 1 . . C H17A .5325 -.1066 .1579 .066 Uiso calc R 1 . . H H17B .3812 -.1092 .0591 .066 Uiso calc R 1 . . H H17C .4131 -.0023 .147 .066 Uiso calc R 1 . . H C7 .3971(8) .1048(8) .4806(7) .051(2) Uani d . 1 . . C H7A .3349 .0517 .5074 .077 Uiso calc R 1 . . H H7B .3966 .0765 .4091 .077 Uiso calc R 1 . . H H7C .3594 .188 .4744 .077 Uiso calc R 1 . . H O5 .6249(5) .3889(4) .2791(4) .0401(13) Uani d . 1 . . O C6 .6123(9) -.0323(7) .5697(8) .056(3) Uani d . 1 . . C H6A .554 -.0832 .6019 .084 Uiso calc R 1 . . H H6B .7154 -.0345 .6158 .084 Uiso calc R 1 . . H H6C .6035 -.0629 .4972 .084 Uiso calc R 1 . . H C16 .4075(8) .0918(7) -.0501(6) .045(2) Uani d . 1 . . C H16A .3578 .1464 -.0139 .068 Uiso calc R 1 . . H H16B .3361 .0349 -.0965 .068 Uiso calc R 1 . . H H16C .452 .1394 -.0947 .068 Uiso calc R 1 . . H C5 .5558(9) .1487(8) .6727(6) .051(2) Uani d . 1 . . C H5A .5334 .2357 .668 .077 Uiso calc R 1 . . H H5B .6528 .1351 .7264 .077 Uiso calc R 1 . . H H5C .4817 .1049 .6949 .077 Uiso calc R 1 . . H C21 1.1383(8) .2221(8) .1837(8) .061(3) Uani d . 1 . . C H21A 1.1345 .1345 .1701 .092 Uiso calc R 1 . . H H21B 1.1473 .2371 .2598 .092 Uiso calc R 1 . . H H21C 1.2232 .2567 .1686 .092 Uiso calc R 1 . . H C20 1.0133(9) .4237(7) .1325(8) .058(2) Uani d . 1 . . C H20A 1.0186 .4398 .2077 .087 Uiso calc R 1 . . H H20B .9276 .4649 .0828 .087 Uiso calc R 1 . . H H20C 1.1024 .4539 .1207 .087 Uiso calc R 1 . . H C22 .9772(9) .2583(12) -.0111(6) .072(3) Uani d . 1 . . C H22A 1.0551 .2993 -.0309 .109 Uiso calc R 1 . . H H22B .8817 .2904 -.0555 .109 Uiso calc R 1 . . H H22C .9809 .171 -.0241 .109 Uiso calc R 1 . . H C9A 1.1227(15) .2348(14) .7071(12) .060(3) Uiso d P .580(7) A 1 C H9A1 1.2182 .2632 .7549 .089 Uiso calc PR .580(7) A 1 H H9A2 1.1372 .1701 .66 .089 Uiso calc PR .580(7) A 1 H H9A3 1.0654 .2035 .7511 .089 Uiso calc PR .580(7) A 1 H C10A .9955(15) .4329(15) .7119(12) .048(3) Uiso d P .580(7) A 1 C H10A .9496 .386 .7561 .072 Uiso calc PR .580(7) A 1 H H10B .927 .4952 .6711 .072 Uiso calc PR .580(7) A 1 H H10C 1.0847 .4718 .7593 .072 Uiso calc PR .580(7) A 1 H C11A 1.1368(16) .4022(15) .5784(13) .056(3) Uiso d P .580(7) A 1 C H11A 1.0932 .4765 .5398 .084 Uiso calc PR .580(7) A 1 H H11B 1.1528 .3439 .5265 .084 Uiso calc PR .580(7) A 1 H H11C 1.2307 .4216 .6337 .084 Uiso calc PR .580(7) A 1 H C10B 1.1622(16) .267(2) .6225(14) .048(3) Uiso d P .420(7) A 2 C H10D 1.2551 .2948 .6746 .072 Uiso calc PR .420(7) A 2 H H10E 1.1671 .2729 .5486 .072 Uiso calc PR .420(7) A 2 H H10F 1.1448 .1824 .6381 .072 Uiso calc PR .420(7) A 2 H C11B 1.033(2) .358(2) .7442(17) .056(3) Uiso d P .420(7) A 2 C H11D 1.1244 .397 .7892 .084 Uiso calc PR .420(7) A 2 H H11E 1.0258 .2772 .7728 .084 Uiso calc PR .420(7) A 2 H H11F .9494 .4075 .7454 .084 Uiso calc PR .420(7) A 2 H C9B 1.055(2) .482(2) .5859(18) .060(3) Uiso d P .420(7) A 2 C H9B1 .9805 .5375 .5954 .089 Uiso calc PR .420(7) A 2 H H9B2 1.0442 .4765 .5085 .089 Uiso calc PR .420(7) A 2 H H9B3 1.1528 .5137 .6261 .089 Uiso calc PR .420(7) A 2 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 V1 .0401(5) .0192(5) .0170(5) -.0041(5) .0160(4) -.0037(6) O2 .043(2) .027(3) .018(3) -.011(2) .015(2) -.007(2) O4 .043(2) .032(3) .018(2) -.010(3) .0168(17) -.009(3) O1 .044(2) .031(3) .023(2) -.016(2) .021(2) -.0082(19) O3 .039(2) .028(3) .020(2) -.0117(19) .016(2) -.008(2) C1 .040(3) .018(4) .016(3) .004(3) .015(3) -.001(2) C15 .041(4) .018(4) .017(4) -.002(3) .012(3) -.008(3) C19 .041(3) .036(5) .028(3) -.004(4) .021(3) -.006(4) C18 .059(5) .016(4) .035(4) -.009(3) .021(4) -.020(3) C12 .034(3) .010(4) .015(3) .004(2) .008(2) .000(2) C3 .037(3) .018(3) .021(4) .004(3) .016(3) .006(3) C13 .038(3) .022(4) .014(3) -.003(3) .013(3) -.006(3) C8 .042(4) .035(4) .025(4) -.012(3) .014(3) -.009(3) C4 .043(4) .022(4) .022(4) -.007(3) .020(3) -.002(3) C2 .043(3) .034(5) .015(3) -.006(3) .015(3) -.001(3) C14 .033(3) .015(3) .017(3) .003(2) .012(3) .004(3) C17 .069(5) .030(5) .039(5) -.024(4) .026(4) -.009(4) C7 .054(5) .045(5) .065(6) -.009(4) .035(5) .013(5) O5 .067(3) .025(3) .033(3) .014(2) .023(3) .011(2) C6 .065(5) .032(5) .086(7) .007(4) .046(5) .021(5) C16 .043(4) .032(5) .049(5) .003(3) -.004(4) -.007(4) C5 .074(5) .048(5) .045(5) -.026(4) .038(4) -.004(4) C21 .053(5) .046(6) .093(7) .006(4) .036(5) .022(5) C20 .065(5) .030(5) .095(7) -.005(4) .048(5) .008(5) C22 .082(5) .100(7) .063(5) -.046(7) .061(5) -.035(7) 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 V1 O5 . 1.588(5) yes V1 O1 . 1.952(4) yes V1 O4 . 1.957(3) yes V1 O2 . 1.965(4) yes V1 O3 . 1.972(4) yes O2 C3 . 1.270(7) no O4 C12 . 1.264(6) no O1 C1 . 1.279(7) no O3 C14 . 1.269(7) no C1 C2 . 1.403(8) no C1 C8 . 1.507(8) no C15 C14 . 1.516(8) no C15 C16 . 1.518(9) no C15 C17 . 1.526(8) no C15 C18 . 1.541(8) no C19 C21 . 1.485(10) no C19 C22 . 1.513(9) no C19 C12 . 1.546(7) no C19 C20 . 1.566(11) no C12 C13 . 1.361(8) no C3 C2 . 1.381(8) no C3 C4 . 1.543(8) no C13 C14 . 1.423(8) no C8 C11B . 1.44(2) no C8 C11A . 1.476(15) no C8 C10A . 1.502(15) no C8 C10B . 1.526(19) no C8 C9B . 1.60(2) no C8 C9A . 1.605(16) no C4 C7 . 1.506(10) no C4 C5 . 1.514(9) no C4 C6 . 1.539(10) no