[3-Chloro-<i>N</i>'-(2-oxidonaphthalen-1-ylmethylidene)benzohydrazidato]methanol(methanolato)oxidovanadium(V)
Wang, Fu-Ming; Acta Crystallographica Section E 67 (2011) m1254–; doi:10.1107/S1600536811032703

data_2231602
_publ_section_title
;
 [3-Chloro-<i>N</i>'-(2-oxidonaphthalen-1-ylmethylidene)benzohydrazidato]methanol(methanolato)oxidovanadium(V)
;
_journal_coeditor_code           LH5304
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1254
_journal_paper_doi               10.1107/S1600536811032703
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[V (C18 H11 Cl N2 O2) (C H3 O) O (C H4 O)]'
_chemical_formula_moiety         'C20 H18 Cl N2 O5 V'
_chemical_formula_sum            'C20 H18 Cl N2 O5 V'
_chemical_formula_weight         452.75
_chemical_name_systematic
;
[3-Chloro-<i>N</i>'-(2-oxidonaphthalen-1-
ylmethylidene)benzohydrazidato]methanol(methanolato)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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.931(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.872(3)
_cell_length_b                   7.613(2)
_cell_length_c                   20.695(3)
_cell_measurement_reflns_used    3491
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.8
_cell_volume                     2003.4(8)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13592
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.9071
_exptl_absorpt_correction_T_min  0.8900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.428
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4368
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.9229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                3104
_reflns_number_total             4368
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5304.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2231602
_cod_database_fobs_code          2231602