Oxido{<i>N</i>-[(2-oxido-1-naphthyl-κ<i>O</i>)methylidene]asparaginato-κ^2^<i>O</i>^1^,<i>N</i>^2^}(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')vanadium(IV) <i>N</i>,<i>N</i>-dimethylformamide monosolvate
Bian, Lin; Li, Lianzhi; Zhang, Qingfu; Wang, Daqi; Acta Crystallographica Section E 66 (2010) m1051–; doi:10.1107/S1600536810030126

data_2227906
_publ_section_title
;
 Oxido{<i>N</i>-[(2-oxido-1-naphthyl-\k<i>O</i>)methylidene]asparaginato-\k^2^<i>O</i>^1^,<i>N</i>^2^}(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')vanadium(IV)
 <i>N</i>,<i>N</i>-dimethylformamide monosolvate
;
_journal_coeditor_code           PV2309
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1051
_journal_paper_doi               10.1107/S1600536810030126
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[V (C15 H12 N2 O4) O (C12 H8 N2)], C3 H7 N O'
_chemical_formula_moiety         'C27 H20 N4 O5 V, C3 H7 N O'
_chemical_formula_sum            'C30 H27 N5 O6 V'
_chemical_formula_weight         604.51
_chemical_name_systematic
;
Oxido{<i>N</i>-[(2-oxido-1-naphthyl-\k<i>O</i>)methylidene]asparaginato-
\k^2^<i>O</i>^1^,<i>N</i>^2^}(1,10-phenanthroline-
\k^2^<i>N</i>,<i>N</i>')vanadium(IV) <i>N</i>,<i>N</i>-dimethylformamide
monosolvate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.396(2)
_cell_angle_beta                 104.196(2)
_cell_angle_gamma                91.0100(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3570(10)
_cell_length_b                   11.1021(12)
_cell_length_c                   12.9119(14)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.694
_cell_measurement_theta_min      2.238
_cell_volume                     1407.5(3)
_computing_cell_refinement       'SAINT (Bruker, 1996)'
_computing_data_collection       'SMART (Bruker, 1996)'
_computing_data_reduction        'SAINT (Bruker, 1996)'
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7387
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  0.9054
_exptl_absorpt_correction_T_min  0.8677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             626
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.404
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         4892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0745
_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^)+(0.130P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                3123
_reflns_number_total             4892
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2309.cif
_cod_data_source_block           I
_cod_database_code               2227906
_cod_database_fobs_code          2227906