#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2014403.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_2014403 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2006 _journal_volume 62 _journal_page_first m116 _journal_page_last m118 _publ_section_title ; Racemic cis-methoxobis(2-methyl-3-oxo-4H-pyran-4-olato)oxovanadium(V) redetermined at 120 K: hydrogen-bonded ribbons containing R~2~^2^(7), R~2~^2^(14) and R~4~^4^(18) rings ; _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_ _publ_author_name 'Kavitha, Savaridasson Jose' 'Panchanatheswaran, Krishnaswamy ' 'Low, John N.' 'Glidewell, Christopher' _chemical_formula_moiety 'C13 H13 O8 V' _chemical_formula_sum 'C13 H13 O8 V' _chemical_formula_iupac '[V (C H3 O) (C6 H5 O3)2 O]' _chemical_formula_weight 348.17 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -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' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 28.007(2) _cell_length_b 7.6637(6) _cell_length_c 13.3083(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.937(4) _cell_angle_gamma 90.00 _cell_volume 2849.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _exptl_crystal_density_diffrn 1.623 _diffrn_ambient_temperature 120(2) loop_ _atom_site_type_symbol _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 V V1 0.37224(3) 0.17205(10) 0.36110(5) 0.0282(2) Uani d . 1 . . O O11 0.54468(12) 0.4003(6) 0.3918(2) 0.0473(10) Uani d . 1 . . C C12 0.51825(16) 0.2490(7) 0.3870(3) 0.0411(12) Uani d . 1 . . C C121 0.54684(18) 0.0873(8) 0.3974(4) 0.0523(15) Uani d . 1 . . C C13 0.46975(16) 0.2619(7) 0.3751(3) 0.0351(11) Uani d . 1 . . O O13 0.44055(10) 0.1220(4) 0.3727(2) 0.0336(8) Uani d . 1 . . C C14 0.44647(16) 0.4263(6) 0.3609(3) 0.0330(11) Uani d . 1 . . O O14 0.40143(10) 0.4243(4) 0.3447(2) 0.0298(7) Uani d . 1 . . C C15 0.47552(17) 0.5791(7) 0.3678(3) 0.0412(13) Uani d . 1 . . C C16 0.52349(19) 0.5554(8) 0.3828(3) 0.0474(14) Uani d . 1 . . O O21 0.26444(10) 0.5505(4) 0.5724(2) 0.0313(7) Uani d . 1 . . C C22 0.26864(15) 0.4695(5) 0.4816(3) 0.0266(10) Uani d . 1 . . C C221 0.22651(15) 0.4982(6) 0.4090(3) 0.0313(10) Uani d . 1 . . C C23 0.30830(14) 0.3761(5) 0.4646(3) 0.0224(9) Uani d . 1 . . O O23 0.31374(9) 0.2955(4) 0.3766(2) 0.0261(7) Uani d . 1 . . C C24 0.34654(15) 0.3577(5) 0.5412(3) 0.0251(9) Uani d . 1 . . O O24 0.38196(10) 0.2650(4) 0.5213(2) 0.0278(7) Uani d . 1 . . C C25 0.34060(16) 0.4485(5) 0.6335(3) 0.0273(10) Uani d . 1 . . C C26 0.30033(17) 0.5371(6) 0.6438(3) 0.0316(10) Uani d . 1 . . O O31 0.35924(10) -0.0332(4) 0.4134(2) 0.0325(7) Uani d . 1 . . C C31 0.3448(2) -0.1890(7) 0.3612(5) 0.0543(15) Uani d . 1 . . O O41 0.35987(10) 0.1349(4) 0.2444(2) 0.0343(8) Uani d . 1 . . H H12A 0.5582 0.0713 0.4681 0.078 Uiso calc R 1 . . H H12B 0.5743 0.0958 0.3558 0.078 Uiso calc R 1 . . H H12C 0.5269 -0.0125 0.3751 0.078 Uiso calc R 1 . . H H15 0.4619 0.6925 0.3622 0.049 Uiso calc R 1 . . H H16 0.5433 0.6563 0.3873 0.057 Uiso calc R 1 . . H H22A 0.2314 0.6045 0.3700 0.047 Uiso calc R 1 . . H H22B 0.1976 0.5108 0.4460 0.047 Uiso calc R 1 . . H H22C 0.2228 0.3982 0.3632 0.047 Uiso calc R 1 . . H H25 0.3650 0.4457 0.6866 0.033 Uiso calc R 1 . . H H26 0.2968 0.5946 0.7061 0.038 Uiso calc R 1 . . H H31A 0.3128 -0.2229 0.3798 0.081 Uiso calc R 1 . . H H31B 0.3676 -0.2826 0.3796 0.081 Uiso calc R 1 . . H H31C 0.3441 -0.1685 0.2885 0.081 Uiso calc R 1 . . 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 0.0238(4) 0.0334(4) 0.0273(4) 0.0011(3) 0.0008(3) -0.0054(3) O11 0.0266(18) 0.087(3) 0.0279(18) -0.0104(19) -0.0018(14) 0.0070(19) C12 0.026(2) 0.074(4) 0.024(2) -0.006(3) 0.0023(19) 0.007(2) C121 0.029(3) 0.088(4) 0.041(3) 0.012(3) 0.009(2) 0.007(3) C13 0.026(2) 0.060(3) 0.020(2) -0.005(2) 0.0007(18) -0.003(2) O13 0.0240(16) 0.0435(19) 0.0331(17) 0.0014(14) 0.0002(13) -0.0016(15) C14 0.031(3) 0.055(3) 0.013(2) -0.008(2) 0.0033(18) 0.001(2) O14 0.0255(17) 0.0385(18) 0.0248(15) -0.0041(13) -0.0013(13) 0.0032(13) C15 0.033(3) 0.068(4) 0.022(2) -0.015(2) -0.002(2) 0.008(2) C16 0.042(3) 0.078(4) 0.022(2) -0.021(3) -0.002(2) 0.009(3) O21 0.0327(17) 0.0312(17) 0.0307(17) 0.0017(14) 0.0072(14) -0.0062(14) C22 0.031(2) 0.024(2) 0.026(2) -0.0057(19) 0.0059(19) -0.0040(18) C221 0.028(2) 0.028(2) 0.038(3) -0.0026(19) 0.002(2) -0.003(2) C23 0.025(2) 0.020(2) 0.021(2) -0.0020(17) 0.0005(17) -0.0002(17) O23 0.0218(14) 0.0332(17) 0.0230(15) -0.0006(12) 0.0003(12) -0.0077(12) C24 0.026(2) 0.026(2) 0.024(2) -0.0048(19) -0.0008(17) 0.0065(18) O24 0.0251(15) 0.0311(16) 0.0267(15) -0.0009(13) -0.0018(12) 0.0003(13) C25 0.034(2) 0.025(2) 0.022(2) -0.007(2) -0.0023(19) 0.0006(18) C26 0.043(3) 0.029(2) 0.023(2) -0.001(2) 0.004(2) -0.0045(19) O31 0.0288(16) 0.0281(17) 0.0411(18) -0.0006(13) 0.0054(14) -0.0040(14) C31 0.049(3) 0.037(3) 0.078(4) -0.004(3) 0.011(3) -0.016(3) O41 0.0267(16) 0.049(2) 0.0272(16) -0.0005(14) 0.0009(13) -0.0102(15) 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 O13 . 1.947(3) y V1 O14 . 2.116(3) y V1 O31 . 1.768(3) y C13 O13 . 1.347(5) y C14 O14 . 1.265(5) y C12 C13 . 1.360(6) y C13 C14 . 1.425(7) y C14 C15 . 1.425(7) y C15 C16 . 1.357(7) y O11 C12 . 1.375(6) y O11 C16 . 1.331(7) y C12 C121 . 1.476(7) no C121 H12A . 0.98 no C121 H12B . 0.98 no C121 H12C . 0.98 no C15 H15 . 0.95 no C16 H16 . 0.95 no V1 O23 . 1.915(3) y V1 O24 . 2.246(3) y V1 O41 . 1.593(3) y C23 O23 . 1.342(5) y C24 O24 . 1.263(5) y C22 C23 . 1.354(6) y C23 C24 . 1.433(5) y C24 C25 . 1.432(6) y C25 C26 . 1.331(6) y O21 C22 . 1.370(5) y O21 C26 . 1.339(5) y C22 C221 . 1.489(6) no C221 H22A . 0.98 no C221 H22B . 0.98 no C221 H22C . 0.98 no C25 H25 . 0.95 no C26 H26 . 0.95 no O31 C31 . 1.426(5) no C31 H31A . 0.98 no C31 H31B . 0.98 no C31 H31C . 0.98 no _cod_database_code 2014403