α-Form of tris(2,4-pentanedionato-<i>O</i>,<i>O</i>')vanadium(III), re-refinement against new intensity data
Filgueiras, Carlos A. L.; Horn Jr, Adolfo; Howie, R. Alan; Skakle, Janet M. S.; Wardell, James L.; Acta Crystallographica Section E 57 (2001) m157–m158; doi:10.1107/S1600536801004391

data_2200252
_publ_section_title
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 \a-Form of tris(2,4-pentanedionato-<i>O</i>,<i>O</i>')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_paper_doi               10.1107/S1600536801004391
_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)
_cod_data_source_file            ya6013.cif
_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 1646 2011-03-28 12:23:43Z adriana 

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
_cod_database_fobs_code          2200252