A three-dimensional supramolecular vanadium hydroxylamide complex: poly[di-μ~2~-aqua-bis(hydroxylamido)-μ~3~-malonato-oxidosodiumvanadium(V)]
Zhang, Qi-Ying; Zhang, Heng-Qiang; Kong, Ai-Guo; Yang, Qian; Shan, Yong-Kui; Acta Crystallographica Section C 65 (2009) m401–m403; doi:10.1107/S0108270109036300

data_2017319
_publ_section_title
;
 A three-dimensional supramolecular vanadium hydroxylamide complex:
 poly[di-\m~2~-aqua-bis(hydroxylamido)-\m~3~-malonato-oxidosodiumvanadium(V)]
;
_journal_coeditor_code           DN3120
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m401
_journal_page_last               m403
_journal_paper_doi               10.1107/S0108270109036300
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Na V (C3 H2 O4) (N H2 O)2 O (H2 O)2]'
_chemical_formula_moiety         'C3 H10 N2 Na O9 V'
_chemical_formula_sum            'C3 H10 N2 Na O9 V'
_chemical_formula_weight         292.06
_chemical_name_systematic
;
poly[di-\m~2~-aqua-bis(hydroxylamido)-\m~3~-malonato-oxidosodiumvanadium(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                 111.9840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6393(2)
_cell_length_b                   15.4265(4)
_cell_length_c                   7.4346(2)
_cell_measurement_reflns_used    8964
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.28
_cell_volume                     1025.15(4)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13757
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0352P)^2^+0.4548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                2306
_reflns_number_total             2529
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn3120.cif
_cod_data_source_block           I
_cod_original_cell_volume        1025.14(4)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017319
_cod_database_fobs_code          2017319