Hexakis(dimethylammonium) di-μ~6~-oxido-tetra-μ~3~-oxido-tetradeca-μ~2~-oxido-octaoxidodecavanadate(V) monohydrate
Wang, Sulian; Lu, Liping; Feng, Sisi; Zhu, Miaoli; Acta Crystallographica Section E 66 (2010) m632–; doi:10.1107/S1600536810016442

data_2226169
_publ_section_title
;
 Hexakis(dimethylammonium)
 di-\m~6~-oxido-tetra-\m~3~-oxido-tetradeca-\m~2~-oxido-octaoxidodecavanadate(V)
 monohydrate
;
_journal_coeditor_code           HY2304
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m632
_journal_paper_doi               10.1107/S1600536810016442
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C2 H8 N)6 [V10 O28], H2 O'
_chemical_formula_moiety         '6(C2 H8 N +), O28 V10 6-, H2 O'
_chemical_formula_sum            'C12 H50 N6 O29 V10'
_chemical_formula_weight         1251.98
_chemical_name_systematic
;
Hexakis(dimethylammonium) di-\m~6~-oxido-tetra-\m~3~-oxido-
tetradeca-\m~2~-oxido-octaoxidodecavanadate(V) monohydrate
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.6149(18)
_cell_length_b                   18.629(3)
_cell_length_c                   30.235(2)
_cell_measurement_reflns_used    1649
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.03
_cell_measurement_theta_min      2.25
_cell_volume                     7668.6(17)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_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      203(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_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  0.0778
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            18064
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    2.423
_exptl_absorpt_correction_T_max  0.8884
_exptl_absorpt_correction_T_min  0.4842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.700
_refine_diff_density_min         -0.825
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3464
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0964
_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^)+(0.0331P)^2^+151.3848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1766
_reflns_number_gt                2951
_reflns_number_total             3464
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2304.cif
_cod_data_source_block           I
_cod_original_cell_volume        7668.5(16)
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2226169
_cod_database_fobs_code          2226169