(Methanol-κ<i>O</i>)(methanolato-κ<i>O</i>)oxido[<i>N</i>-(2-oxidobenzylidene)isoleucinato-κ^3^<i>O</i>,<i>N</i>,<i>O</i>']vanadium(V)
Wang, Chengyuan; Guo, Zhenghua; Dong, Jianfang; Li, Lianzhi; Acta Crystallographica Section E 68 (2012) m982–; doi:10.1107/S1600536812028231

data_2235504
_publ_section_title
;
 (Methanol-\k<i>O</i>)(methanolato-\k<i>O</i>)oxido[<i>N</i>-(2-oxidobenzylidene)isoleucinato-\k^3^<i>O</i>,<i>N</i>,<i>O</i>']vanadium(V)
;
_journal_coeditor_code           HY2555
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m982
_journal_paper_doi               10.1107/S1600536812028231
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[V (C13 H15 N O3) O (C H3 O) (C H4 O)]'
_chemical_formula_moiety         'C15 H22 N O6 V'
_chemical_formula_sum            'C15 H22 N O6 V'
_chemical_formula_weight         363.28
_chemical_name_systematic
;
(Methanol-\k<i>O</i>)(methanolato-\k<i>O</i>)oxido[<i>N</i>-(2-
oxidobenzylidene)isoleucinato-\k^3^<i>O</i>,<i>N</i>,<i>O</i>']vanadium(V)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.6148(9)
_cell_length_b                   18.463(2)
_cell_length_c                   29.286(3)
_cell_measurement_reflns_used    2166
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.6
_cell_volume                     3576.7(7)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.1738
_diffrn_reflns_av_sigmaI/netI    0.1798
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            18864
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.9549
_exptl_absorpt_correction_T_min  0.8635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.405
_refine_ls_abs_structure_details 'Flack (1983), 2690 Friedel pairs'
_refine_ls_abs_structure_Flack   0.09(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6295
_refine_ls_number_restraints     1046
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1630
_refine_ls_R_factor_gt           0.0922
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2151
_reflns_number_gt                3229
_reflns_number_total             6295
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2555.cif
_cod_data_source_block           I
_cod_database_code               2235504
_cod_database_fobs_code          2235504