Crystal structure of di-μ-methanolato-bis[<i>N</i>'-(1-benzoylprop-1-en-2-yl)thiophene-2-carbohydrazidato-κ^3^<i>O</i>,<i>N</i>',<i>O</i>']oxidovanadium(V)]
Carroccia, Murilo C.; Pesci, Rafaela B. P.; da Maia, Pedro Ivo; Deflon, Victor M.; Acta Crystallographica Section E 70 (2014) m353–m354; doi:10.1107/S1600536814020327

data_2240011
_publ_section_title
;
 Crystal structure of
 di-\m-methanolato-bis[<i>N</i>'-(1-benzoylprop-1-en-2-yl)thiophene-2-carbohydrazidato-\k^3^<i>O</i>,<i>N</i>',<i>O</i>']oxidovanadium(V)]
;
_journal_coeditor_code           WM5059
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m353
_journal_page_last               m354
_journal_paper_doi               10.1107/S1600536814020327
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[V2 (C15 H12 N2 O2 S)2 (C H3 O)2 O2]'
_chemical_formula_moiety         'C32 H30 N4 O8 S2 V2'
_chemical_formula_sum            'C32 H30 N4 O8 S2 V2'
_chemical_formula_weight         764.60
_chemical_melting_point          451
_chemical_name_common            {(VOLaOME)2}
_chemical_name_systematic
Di-\m-methanolato-\k^4^<i>O</i>:<i>O</i>-bis[<i>N</i>'-(1-benzoylprop-1-en-2-yl)thiophene-2-carbohydrazidato-\k^3^<i>O</i>,<i>N</i>',<i>O</i>']oxidovanadium(V)]
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 119.8840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9900(2)
_cell_length_b                   15.9297(3)
_cell_length_c                   11.0178(3)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.49
_cell_volume                     1672.39(7)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 2012) and PLATON (Spek, 2009)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20108
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         2.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.9297
_exptl_absorpt_correction_T_min  0.8601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0427P)^2^+0.7671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                2718
_reflns_number_total             3067
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5059sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1672.39(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2240011
_cod_database_fobs_code          2240011