#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200349.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2200349 loop_ _publ_author_name 'Urs, Usha K.' 'Anitha, K. C.' 'Raghunathan, K. Lakshmi' 'Shivashankar, S. A.' 'Robinson, W. T.' 'Row, T. N. Guru' _publ_section_title ; Low-temperature oxobis(2,2,6,6-tetramethyl-3,5-heptanedionato)vanadium(IV) ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m242 _journal_page_last m243 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[V O (C11 H19 O2)2]' _chemical_formula_moiety 'C22 H38 O5 V' _chemical_formula_sum 'C22 H38 O5 V' _chemical_formula_weight 433.46 _chemical_name_systematic ; oxobis(2,2,6,6-tetramethyl-3,5-heptadionato)vanadium(IV) ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 109.0250(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.4515(2) _cell_length_b 10.7953(3) _cell_length_c 12.7494(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 149(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 8 _cell_volume 1229.79(6) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Fait, 1991)' _computing_data_reduction XSCANS _computing_molecular_graphics ' ORTEP-3 (Johnson, 1976; Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_measured_fraction_theta_full .982 _diffrn_measured_fraction_theta_max .982 _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .093 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7897 _diffrn_reflns_theta_full 26.5 _diffrn_reflns_theta_max 26.5 _diffrn_reflns_theta_min 1.7 _diffrn_standards_decay_% 'no decay' _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .429 _exptl_absorpt_correction_type none _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 466 _exptl_crystal_size_max .50 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .40 _refine_diff_density_max .95 _refine_diff_density_min -1.01 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack .03(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .92 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 4217 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all .92 _refine_ls_R_factor_gt .074 _refine_ls_shift/su_max <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0898P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .187 _reflns_number_gt 2751 _reflns_number_total 4217 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file tk6017.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21' _cod_database_code 2200349 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 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_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V .3005 .5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O5 V1 O1 107.5(2) yes O5 V1 O4 106.2(2) yes O1 V1 O4 83.59(16) yes O5 V1 O2 106.4(2) yes O1 V1 O2 86.81(16) yes O4 V1 O2 147.4(2) yes O5 V1 O3 106.6(2) yes O1 V1 O3 145.88(18) yes O4 V1 O3 85.92(18) yes O2 V1 O3 84.78(17) yes C3 O2 V1 129.5(4) no C12 O4 V1 129.5(3) no C1 O1 V1 130.2(4) no C14 O3 V1 131.0(4) no O1 C1 C2 121.9(6) no O1 C1 C8 115.9(5) no C2 C1 C8 122.1(5) no C14 C15 C16 108.5(5) no C14 C15 C17 109.6(5) no C16 C15 C17 109.4(6) no C14 C15 C18 110.9(5) no C16 C15 C18 109.8(5) no C17 C15 C18 108.6(6) no C21 C19 C22 112.0(7) no C21 C19 C12 108.7(6) no C22 C19 C12 113.4(5) no C21 C19 C20 107.5(6) no C22 C19 C20 108.6(8) no C12 C19 C20 106.3(5) no O4 C12 C13 124.7(5) no O4 C12 C19 114.1(5) no C13 C12 C19 121.1(5) no O2 C3 C2 123.3(5) no O2 C3 C4 115.1(5) no C2 C3 C4 121.4(5) no C12 C13 C14 123.6(5) no C11B C8 C11A 130.5(12) no C11B C8 C10A 36.5(10) no C11A C8 C10A 114.5(10) no C11B C8 C1 115.4(10) no C11A C8 C1 112.8(8) no C10A C8 C1 109.9(7) no C11B C8 C10B 112.8(12) no C11A C8 C10B 62.3(11) no C10A C8 C10B 141.3(10) no C1 C8 C10B 105.8(8) no C11B C8 C9B 109.7(14) no C11A C8 C9B 45.0(9) no C10A C8 C9B 77.4(10) no C1 C8 C9B 105.5(9) no C10B C8 C9B 107.2(12) no C11B C8 C9A 68.8(11) no C11A C8 C9A 106.7(9) no C10A C8 C9A 104.9(9) no C1 C8 C9A 107.4(7) no C10B C8 C9A 48.9(8) no C9B C8 C9A 143.8(10) no C7 C4 C5 109.4(6) no C7 C4 C6 108.5(6) no C5 C4 C6 110.4(7) no C7 C4 C3 110.2(5) no C5 C4 C3 111.9(5) no C6 C4 C3 106.4(5) no C3 C2 C1 124.7(5) no O3 C14 C13 121.6(5) no O3 C14 C15 116.8(5) no C13 C14 C15 121.6(5) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_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