A new Schiff base oxovanadium (IV) complex: [<i>N</i>,<i>N</i>'-bis(4-hydroxysalicylidene)-<i>o</i>-phenylenediamine]oxovanadium(IV) bis(dimethyl sulfoxide) dihydrate
Xie, Ming-Jin; Yan, Shi-Ping; Liao, Dai-Zheng; Jian, Zhong-Hui; Chen, Peng; Acta Crystallographica Section E 60 (2004) m1530–m1532; doi:10.1107/S160053680402210X

data_2204328
_publ_section_title
;A new Schiff base oxovanadium (IV) complex:
 [<i>N</i>,<i>N</i>'-bis(4-hydroxysalicylidene)-<i>o</i>-phenylenediamine]oxovanadium(IV)
 bis(dimethyl sulfoxide) dihydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1530
_journal_page_last               m1532
_journal_paper_doi               10.1107/S160053680402210X
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[V (C20 H14 N2 O4) O] , 2C2 H6 O S , 2H2 O'
_chemical_formula_moiety         'C20 H14 N2 O5 V, 2C2 H6 O S, 2H2 O'
_chemical_formula_sum            'C24 H30 N2 O9 S2 V'
_chemical_formula_weight         605.56
_chemical_name_systematic
;
[N,N'-bis(4-hydroxysalicylidene)-o-phenylenediamine]oxovanadium(IV)
bis(dimethyl sulfoxide) dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                78.464(5)
_cell_angle_beta                 72.067(6)
_cell_angle_gamma                85.072(6)
_cell_formula_units_Z            2
_cell_length_a                   9.325(3)
_cell_length_b                   12.312(4)
_cell_length_c                   12.829(4)
_cell_measurement_reflns_used    729
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.75
_cell_measurement_theta_min      2.60
_cell_volume                     1372.6(8)
_computing_cell_refinement       'SAINT (Bruker, 1994)'
_computing_data_collection       'SMART (Bruker, 1994)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8035
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0557P)^2^+0.0346P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                3146
_reflns_number_total             5595
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6157.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P  1'
_cod_database_code               2204328
_cod_database_fobs_code          2204328