The α polymorph of racemic tris(2,4-pentanedionato-κ^2^<i>O</i>,<i>O</i>')vanadium(III), redetermined at 120 K
Kavitha, S. Jose; Panchanatheswaran, Krishnaswamy; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section E 61 (2005) m1326–m1328; doi:10.1107/S1600536805018441

data_2206240
_publ_section_title
;
 The \a polymorph of racemic
 tris(2,4-pentanedionato-\k^2^<i>O</i>,<i>O</i>')vanadium(III),
 redetermined at 120 K
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1326
_journal_page_last               m1328
_journal_paper_doi               10.1107/S1600536805018441
_journal_volume                  61
_journal_year                    2005
_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_name_systematic
;
\a-Tris(2,4-pentanedionato-\k^2^O,O')vanadium(III)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.3920(7)
_cell_length_b                   16.4043(6)
_cell_length_c                   15.1901(10)
_cell_measurement_reflns_used    3824
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.21
_cell_volume                     3337.1(3)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) and COLLECT'
_computing_data_collection       'COLLECT (Hooft, 1999)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'OSCAIL and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker--Nonius 95mm CCD camera on \k goniostat'
_diffrn_measurement_method       '\p and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR91 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1744
_diffrn_reflns_av_sigmaI/netI    0.1218
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30601
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.470
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1560
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.2837P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1347
_reflns_number_gt                1876
_reflns_number_total             3824
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6448.cif
_cod_data_source_block           I
_cod_database_code               2206240
_cod_database_fobs_code          2206240