(Benzoylacetone 4-methoxybenzoylhydrazonato-κ^3^<i>O,N,O</i>')(<i>N</i>-benzoylhydroxylaminato-κ^2^<i>O,O</i>')oxovanadium(IV)
Gao, Shan; Huo, Li-Hua; Zhao, Hui; Ng, Seik Weng; Acta Crystallographica Section E 61 (2005) m325–m326; doi:10.1107/S1600536805000929

data_2205102
_publ_section_title
;(Benzoylacetone
 4-methoxybenzoylhydrazonato-\k^3^<i>O,N,O</i>')(<i>N</i>-benzoylhydroxylaminato-\k^2^<i>O,O</i>')oxovanadium(IV)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m325
_journal_page_last               m326
_journal_paper_doi               10.1107/S1600536805000929
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[V (C13 H10 N O2) (C18 H16 N2 O3) O]'
_chemical_formula_moiety         'C31 H26 N3 O6 V'
_chemical_formula_sum            'C31 H26 N3 O6 V'
_chemical_formula_weight         587.49
_chemical_name_systematic
;
(Benzoylacetone 4-methoxybenzoylhydrazonato-\k^3^O,N,O')(N-
benzoylhydroxylaminato-\k^2^O,O')oxovanadium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.247(2)
_cell_length_b                   12.387(3)
_cell_length_c                   21.858(2)
_cell_measurement_reflns_used    24313
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     2774.3(9)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.016
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26700
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         6307
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.047
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0701P)^2^+0.1309P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.105
_refine_ls_wR_factor_ref         0.110
_reflns_number_gt                4958
_reflns_number_total             6307
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp6031.cif
_cod_data_source_block           I
_cod_original_cell_volume        2774.3(8)
_cod_original_sg_symbol_Hall     '-P 2yc'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2205102
_cod_database_fobs_code          2205102