Bis(μ-methanolato-κ^2^<i>O</i>:<i>O</i>)bis{[4-bromo-<i>N</i>'-(1-methyl-3-oxidobut-2-en-1-ylidene-κ<i>O</i>)benzohydrazidato-κ^2^<i>N</i>',<i>O</i>]oxidovanadium(V)}
Wong, Hon Wee; Lo, Kong Mun; Ng, Seik Weng; Acta Crystallographica Section E 67 (2011) m902–; doi:10.1107/S1600536811021647

data_2230926
_publ_section_title
;
 Bis(\m-methanolato-\k^2^<i>O</i>:<i>O</i>)bis{[4-bromo-<i>N</i>'-(1-methyl-3-oxidobut-2-en-1-ylidene-\k<i>O</i>)benzohydrazidato-\k^2^<i>N</i>',<i>O</i>]oxidovanadium(V)}
;
_journal_coeditor_code           XU5231
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m902
_journal_paper_doi               10.1107/S1600536811021647
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[V2 (C12 H11 Br N2 O2)2 (C H3 O)2 O2]'
_chemical_formula_moiety         'C26 H28 Br2 N4 O8 V2'
_chemical_formula_sum            'C26 H28 Br2 N4 O8 V2'
_chemical_formula_weight         786.22
_chemical_name_systematic
;
Bis(\m-methanolato-\k^2^<i>O</i>:<i>O</i>)bis{[4-bromo-<i>N</i>'-(1-
methyl-3-oxidobut-2-en-1-ylidene-\k<i>O</i>)benzohydrazidato-
\k^2^<i>N</i>',<i>O</i>]oxidovanadium(V)}
;
_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                 101.8782(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7517(5)
_cell_length_b                   12.3409(7)
_cell_length_c                   13.9952(8)
_cell_measurement_reflns_used    8361
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.22
_cell_volume                     1479.17(15)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       '\w scans'
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18572
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.388
_exptl_absorpt_correction_T_max  0.5506
_exptl_absorpt_correction_T_min  0.4297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3400
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+1.3638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                3106
_reflns_number_total             3400
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5231.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2230926
_cod_database_fobs_code          2230926