Redetermination of bis(acetylacetonato)oxidopyridinevanadium(IV)
Silva, Rubia M. S. da; Spiazzi, Cristiano C.; Bortolotto, Ricardo; Burrow, Robert A.; Acta Crystallographica Section E 63 (2007) m2422–m2422; doi:10.1107/S1600536807039323

data_2215207
_publ_section_title
;
 Redetermination of bis(acetylacetonato)oxidopyridinevanadium(IV)
;
_journal_coeditor_code           LH2476
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2422
_journal_page_last               m2422
_journal_paper_doi               10.1107/S1600536807039323
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[V (C5 H7 O2)2 O (C5 H5 N)]'
_chemical_formula_moiety         'C15 H19 N O5 V'
_chemical_formula_sum            'C15 H19 N O5 V'
_chemical_formula_weight         344.25
_chemical_name_systematic
;
 bis(acetylacetonato)oxidopyridinevanadium(IV)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.621(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9121(3)
_cell_length_b                   15.5258(7)
_cell_length_c                   14.2523(6)
_cell_measurement_reflns_used    2628
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      2.94
_cell_volume                     1701.54(13)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2, COSMO and BIS (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11650
_diffrn_reflns_theta_full        30.43
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.90281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            blue--green
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.0762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.105
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                1837
_reflns_number_total             2595
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2476.cif
_cod_data_source_block           I
_cod_original_cell_volume        1701.54(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2215207
_cod_database_fobs_code          2215207