Oxido[<i>N</i>-(2-oxidobenzylidene-κ<i>O</i>)leucinato-κ^2^<i>N</i>,<i>O</i>](1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')vanadium(IV)
Wang, Cheng-Yuan; Jing, Bu-Qin; Dong, Jian-Fang; Li, Lian-Zhi; Acta Crystallographica Section E 68 (2012) m907–; doi:10.1107/S1600536812025391

data_2235683
_publ_section_title
;
 Oxido[<i>N</i>-(2-oxidobenzylidene-\k<i>O</i>)leucinato-\k^2^<i>N</i>,<i>O</i>](1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')vanadium(IV)
;
_journal_coeditor_code           XU5555
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m907
_journal_paper_doi               10.1107/S1600536812025391
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[V (C13 H15 N O3) O (C12 H8 N2)]'
_chemical_formula_moiety         'C25 H23 N3 O4 V'
_chemical_formula_sum            'C25 H23 N3 O4 V'
_chemical_formula_weight         480.40
_chemical_name_systematic
;
Oxido[<i>N</i>-(2-oxidobenzylidene-\k<i>O</i>)leucinato-
\k^2^<i>N</i>,<i>O</i>](1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')vanadium(IV)
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   33.675(4)
_cell_length_b                   33.675(4)
_cell_length_c                   10.283(2)
_cell_measurement_reflns_used    3014
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.317
_cell_measurement_theta_min      2.419
_cell_volume                     10099(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1367
_diffrn_reflns_av_sigmaI/netI    0.1340
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17437
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_correction_T_min  0.8977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4482
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.376
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                2020
_reflns_number_total             3962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            xu5555.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2235683
_cod_database_fobs_code          2235683