Redetermination of μ-oxido-bis[bis(<i>N</i>,<i>N</i>-diethylhydroxylaminato)oxidovanadium(V)]
Zhang, Heng-Qiang; Jin, Zhong-Min; Fan, Xin; Zhang, Qi-Ying; Acta Crystallographica Section E 67 (2011) m860–m861; doi:10.1107/S1600536811020551

data_2230903
_publ_section_title
;
 Redetermination of
 \m-oxido-bis[bis(<i>N</i>,<i>N</i>-diethylhydroxylaminato)oxidovanadium(V)]
;
_journal_coeditor_code           WM2493
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m860
_journal_page_last               m861
_journal_paper_doi               10.1107/S1600536811020551
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[V2 (C4 H10 N O)4 O3]'
_chemical_formula_moiety         'C16 H40 N4 O7 V2'
_chemical_formula_sum            'C16 H40 N4 O7 V2'
_chemical_formula_weight         502.40
_chemical_name_systematic
;
\m-oxido-bis[bis(<i>N</i>,<i>N</i>-diethylhydroxylaminato)oxidovanadium(V)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.7440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6106(3)
_cell_length_b                   10.2624(2)
_cell_length_c                   19.4547(3)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.33
_cell_volume                     2507.07(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28459
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064.0
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0563P)^2^+0.3492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                3767
_reflns_number_total             4419
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2493.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P 2y b c'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2230903
_cod_database_fobs_code          2230903