#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2200252.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_2200252 loop_ _publ_author_name 'Filgueiras, Carlos A. L.' 'Horn, Jr, Adolfo' 'Howie, R. Alan' 'Skakle, Janet M. S.' 'Wardell, James L.' _publ_section_title ; \a-Form of tris(2,4-pentanedionato-O,O')vanadium(III), re-refinement against new intensity data ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m157 _journal_page_last m158 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[V (C5 H7 O2)3]' _chemical_formula_moiety 'C15 H21 O6 V' _chemical_formula_sum 'C15 H21 O6 V' _chemical_formula_weight 348.26 _chemical_melting_point 460.5(5) _chemical_name_common 'tris(acetylacetonato)-vanadium(III) (alpha form)' _chemical_name_systematic ; Tris(2,4-pentanedionato-O,O')-vanadium(III) (alpha form) ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2bc 2ac' _symmetry_space_group_name_H-M 'P c a b' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 15.4466(7) _cell_length_b 16.6228(8) _cell_length_c 13.5016(6) _cell_measurement_reflns_used 4494 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 26.4 _cell_measurement_theta_min 2.4 _cell_volume 3466.7(3) _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _diffrn_ambient_temperature 297(2) _diffrn_measured_fraction_theta_full .898 _diffrn_measured_fraction_theta_max .898 _diffrn_measurement_device_type 'Bruker SMART 1000 area-detector' _diffrn_measurement_method '\f and \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 .055 _diffrn_reflns_av_sigmaI/netI .0477 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 28129 _diffrn_reflns_theta_full 31.0 _diffrn_reflns_theta_max 31.0 _diffrn_reflns_theta_min 2.3 _diffrn_standards_decay_% none _exptl_absorpt_coefficient_mu .60 _exptl_absorpt_correction_T_max .928 _exptl_absorpt_correction_T_min .445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_crystal_colour 'dark orange--brown' _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_meas 1.33 _exptl_crystal_density_method 'flotation in CCl~4~/EtOH (Morosin & Montgomery, 1969)' _exptl_crystal_description block _exptl_crystal_F_000 1456 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _refine_diff_density_max .29 _refine_diff_density_min -.56 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .94 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 205 _refine_ls_number_reflns 5155 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .94 _refine_ls_R_factor_all .126 _refine_ls_R_factor_gt .044 _refine_ls_shift/su_max .003 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0658P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .139 _reflns_number_gt 2251 _reflns_number_total 5155 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya6013.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '460-461' was changed to '460.5(5)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200252 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, -z+1/2' 'x+1/2, -y+1/2, z' 'x, y+1/2, -z+1/2' '-x, -y, -z' '-x-1/2, y, z-1/2' '-x-1/2, y-1/2, -z' '-x, -y-1/2, z-1/2' 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_type_symbol C1 .0027(2) .35220(15) .33680(19) .0682(7) Uani d . 1 C C10 -.0267(3) .40889(19) .4181(2) .1098(13) Uani d . 1 C H10A -.0192 .3834 .4813 .165 Uiso calc R 1 H H10B -.0867 .4219 .4087 .165 Uiso calc R 1 H H10C .0072 .4573 .4157 .165 Uiso calc R 1 H C12 -.04869(19) .33732(18) .2556(2) .0772(9) Uani d . 1 C H12 -.1024 .3626 .2533 .093 Uiso calc R 1 H C2 -.02683(18) .28758(18) .17693(19) .0631(7) Uani d . 1 C C20 -.08692(19) .2776(2) .0909(2) .0928(11) Uani d . 1 C H20A -.0720 .3155 .0400 .139 Uiso calc R 1 H H20B -.1454 .2869 .1121 .139 Uiso calc R 1 H H20C -.0819 .2239 .0652 .139 Uiso calc R 1 H C3 .09410(19) .07824(17) .3143(2) .0713(8) Uani d . 1 C C30 .0465(3) .0223(2) .3825(3) .1097(13) Uani d . 1 C H30A .0279 .0513 .4402 .165 Uiso calc R 1 H H30B .0842 -.0207 .4021 .165 Uiso calc R 1 H H30C -.0031 .0006 .3489 .165 Uiso calc R 1 H C34 .1382(2) .04789(18) .2328(2) .0874(10) Uani d . 1 C H34 .1323 -.0067 .2191 .105 Uiso calc R 1 H C4 .1899(2) .09232(18) .1710(2) .0687(8) Uani d . 1 C C40 .2398(2) .0525(2) .0882(2) .1090(12) Uani d . 1 C H40A .2351 .0843 .0292 .163 Uiso calc R 1 H H40B .2165 -.0001 .0762 .163 Uiso calc R 1 H H40C .2996 .0479 .1067 .163 Uiso calc R 1 H C5 .30280(18) .29429(18) .36737(18) .0641(7) Uani d . 1 C C50 .3605(2) .2859(2) .4569(2) .0983(11) Uani d . 1 C H50A .3440 .3249 .5059 .147 Uiso calc R 1 H H50B .4196 .2948 .4378 .147 Uiso calc R 1 H H50C .3546 .2328 .4839 .147 Uiso calc R 1 H C56 .3225(2) .34965(19) .2937(2) .0848(9) Uani d . 1 C H56 .3735 .3789 .3006 .102 Uiso calc R 1 H C6 .2732(2) .36462(16) .2120(2) .0715(8) Uani d . 1 C C60 .3030(3) .4242(2) .1347(3) .1221(15) Uani d . 1 C H60A .2960 .4012 .0699 .183 Uiso calc R 1 H H60B .3629 .4368 .1454 .183 Uiso calc R 1 H H60C .2691 .4724 .1395 .183 Uiso calc R 1 H O1 .07705(12) .32206(10) .35069(12) .0639(5) Uani d . 1 O O2 .04379(11) .24907(11) .17215(12) .0639(5) Uani d . 1 O O3 .09151(13) .15212(11) .33728(13) .0676(5) Uani d . 1 O O4 .20162(11) .16752(11) .17940(12) .0628(5) Uani d . 1 O O5 .23767(12) .24903(11) .36504(11) .0629(4) Uani d . 1 O O6 .20096(12) .33224(10) .19387(12) .0627(5) Uani d . 1 O V1 .14153(3) .24589(2) .26686(3) .04841(14) Uani d . 1 V 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 C1 .089(2) .0534(15) .0618(16) .0145(15) .0148(15) .0007(13) C10 .145(3) .089(2) .095(2) .049(2) .016(2) -.026(2) C12 .070(2) .092(2) .0691(18) .0257(17) .0046(14) .0003(16) C2 .0541(16) .0823(18) .0528(15) -.0015(14) .0057(12) .0116(14) C20 .0601(18) .156(3) .0627(18) .0012(19) -.0039(14) .0033(19) C3 .075(2) .0570(16) .082(2) -.0139(14) -.0026(15) .0083(15) C30 .124(3) .076(2) .128(3) -.030(2) .018(2) .029(2) C34 .106(3) .0528(16) .103(3) -.0063(18) .004(2) -.0144(17) C4 .0735(19) .0649(18) .0677(18) .0122(15) -.0068(14) -.0160(14) C40 .122(3) .110(3) .095(2) .027(2) .010(2) -.045(2) C5 .0614(17) .0791(19) .0518(14) .0041(15) -.0030(12) -.0080(14) C50 .087(2) .147(3) .0603(18) -.002(2) -.0179(16) -.012(2) C56 .079(2) .096(2) .0796(19) -.0326(19) -.0105(17) .0092(18) C6 .079(2) .0649(17) .0703(18) -.0147(15) .0067(15) .0115(14) C60 .129(3) .119(3) .119(3) -.044(3) .008(2) .054(3) O1 .0699(12) .0649(11) .0570(10) .0080(10) .0041(9) -.0123(9) O2 .0572(10) .0844(13) .0502(10) .0034(10) .0023(7) -.0079(9) O3 .0838(13) .0585(11) .0606(11) -.0119(10) .0159(9) .0029(9) O4 .0683(12) .0633(11) .0568(10) .0062(9) .0126(8) -.0058(9) O5 .0677(11) .0739(11) .0471(9) -.0018(10) -.0016(8) .0092(9) O6 .0695(12) .0643(11) .0545(9) -.0074(9) -.0014(9) .0149(9) V1 .0532(2) .0484(2) .0436(2) -.0010(2) .00513(16) -.00006(18) 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 .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 '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 O1 C1 C12 124.7(2) O1 C1 C10 114.2(3) C12 C1 C10 121.0(3) C1 C10 H10A 109.5 C1 C10 H10B 109.5 H10A C10 H10B 109.5 C1 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C1 C12 C2 125.2(3) C1 C12 H12 117.4 C2 C12 H12 117.4 O2 C2 C12 123.3(3) O2 C2 C20 116.0(2) C12 C2 C20 120.7(3) C2 C20 H20A 109.5 C2 C20 H20B 109.5 H20A C20 H20B 109.5 C2 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 O3 C3 C34 124.1(3) O3 C3 C30 115.7(3) C34 C3 C30 120.1(3) C3 C30 H30A 109.5 C3 C30 H30B 109.5 H30A C30 H30B 109.5 C3 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C4 C34 C3 124.9(3) C4 C34 H34 117.5 C3 C34 H34 117.5 O4 C4 C34 124.0(3) O4 C4 C40 115.2(3) C34 C4 C40 120.7(3) C4 C40 H40A 109.5 C4 C40 H40B 109.5 H40A C40 H40B 109.5 C4 C40 H40C 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 O5 C5 C56 123.7(3) O5 C5 C50 116.0(3) C56 C5 C50 120.4(3) C5 C50 H50A 109.5 C5 C50 H50B 109.5 H50A C50 H50B 109.5 C5 C50 H50C 109.5 H50A C50 H50C 109.5 H50B C50 H50C 109.5 C6 C56 C5 125.3(3) C6 C56 H56 117.3 C5 C56 H56 117.3 O6 C6 C56 125.0(3) O6 C6 C60 114.5(3) C56 C6 C60 120.6(3) C6 C60 H60A 109.5 C6 C60 H60B 109.5 H60A C60 H60B 109.5 C6 C60 H60C 109.5 H60A C60 H60C 109.5 H60B C60 H60C 109.5 C1 O1 V1 128.90(17) C2 O2 V1 129.61(17) C3 O3 V1 129.20(18) C4 O4 V1 129.24(18) C5 O5 V1 129.00(17) C6 O6 V1 128.74(17) O6 V1 O1 93.14(8) O6 V1 O2 90.73(7) O1 V1 O2 88.18(7) O6 V1 O3 174.40(8) O1 V1 O3 91.87(8) O2 V1 O3 91.92(8) O6 V1 O4 87.87(7) O1 V1 O4 177.41(8) O2 V1 O4 89.42(7) O3 V1 O4 87.23(8) O6 V1 O5 88.07(7) O1 V1 O5 88.73(7) O2 V1 O5 176.62(7) O3 V1 O5 89.54(8) O4 V1 O5 93.69(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 O1 1.267(3) C1 C12 1.376(4) C1 C10 1.516(3) C10 H10A .9600 C10 H10B .9600 C10 H10C .9600 C12 C2 1.388(4) C12 H12 .9300 C2 O2 1.266(3) C2 C20 1.497(4) C20 H20A .9600 C20 H20B .9600 C20 H20C .9600 C3 O3 1.267(3) C3 C34 1.390(4) C3 C30 1.501(4) C30 H30A .9600 C30 H30B .9600 C30 H30C .9600 C34 C4 1.370(4) C34 H34 .9300 C4 O4 1.268(3) C4 C40 1.510(4) C40 H40A .9600 C40 H40B .9600 C40 H40C .9600 C5 O5 1.257(3) C5 C56 1.389(4) C5 C50 1.508(4) C50 H50A .9600 C50 H50B .9600 C50 H50C .9600 C56 C6 1.363(4) C56 H56 .9300 C6 O6 1.263(3) C6 C60 1.511(4) C60 H60A .9600 C60 H60B .9600 C60 H60C .9600 O1 V1 1.9688(17) O2 V1 1.9793(17) O3 V1 1.9825(17) O4 V1 1.9881(16) O5 V1 1.9912(18) O6 V1 1.9683(17) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O1 C1 C12 C2 -.3(5) C10 C1 C12 C2 178.9(3) C1 C12 C2 O2 1.0(5) C1 C12 C2 C20 -178.3(3) O3 C3 C34 C4 5.2(5) C30 C3 C34 C4 -173.9(3) C3 C34 C4 O4 -2.2(5) C3 C34 C4 C40 175.9(3) O5 C5 C56 C6 2.7(5) C50 C5 C56 C6 -177.1(3) C5 C56 C6 O6 2.8(5) C5 C56 C6 C60 -177.7(3) C12 C1 O1 V1 -1.0(4) C10 C1 O1 V1 179.73(19) C12 C2 O2 V1 -.2(4) C20 C2 O2 V1 179.01(19) C34 C3 O3 V1 2.9(5) C30 C3 O3 V1 -177.9(2) C34 C4 O4 V1 -8.8(4) C40 C4 O4 V1 173.02(19) C56 C5 O5 V1 -4.6(4) C50 C5 O5 V1 175.20(19) C56 C6 O6 V1 -5.8(4) C60 C6 O6 V1 174.6(2) C6 O6 V1 O1 92.0(2) C6 O6 V1 O2 -179.8(2) C6 O6 V1 O4 -90.4(2) C6 O6 V1 O5 3.4(2) C1 O1 V1 O6 91.9(2) C1 O1 V1 O2 1.3(2) C1 O1 V1 O3 -90.6(2) C1 O1 V1 O5 179.9(2) C2 O2 V1 O6 -93.8(2) C2 O2 V1 O1 -.6(2) C2 O2 V1 O3 91.2(2) C2 O2 V1 O4 178.4(2) C3 O3 V1 O1 168.6(2) C3 O3 V1 O2 80.4(2) C3 O3 V1 O4 -9.0(2) C3 O3 V1 O5 -102.7(2) C4 O4 V1 O6 -170.8(2) C4 O4 V1 O2 -80.1(2) C4 O4 V1 O3 11.9(2) C4 O4 V1 O5 101.2(2) C5 O5 V1 O6 1.7(2) C5 O5 V1 O1 -91.4(2) C5 O5 V1 O3 176.7(2) C5 O5 V1 O4 89.5(2)