Hydrogen-bonded aggregates of protonated decavanadate anions in their tetraalkylammonium salts † ‡
Nakamura, Setsuko; Ozeki, Tomoji; Journal of the Chemical Society, Dalton Transactions  (2001) 472–; doi:10.1039/b008128k

data_7010329
_publ_section_title
;
 Hydrogen-bonded aggregates of protonated decavanadate anions in their
 tetraalkylammonium salts&#x200A;&#x2020;&#x200A;&#x2021;
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              472
_journal_paper_doi               10.1039/b008128k
_journal_year                    2001
_chemical_formula_moiety         '(C8 H20 N +)3, (H3 V10 O28 3-), 2(H2 O)'
_chemical_formula_sum            'C24 H67 N3 O30 V10'
_chemical_formula_weight         1387.21
_chemical_name_common
;
Tris(tetraethylammonium) trihydrogendecavanadate dihydrate
;
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 98.5520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.4919(9)
_cell_length_b                   21.5128(5)
_cell_length_c                   13.9059(4)
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      1.13
_cell_volume                     9907.9(5)
_computing_cell_refinement       'Siemens SAINT program'
_computing_data_collection       'Siemens SMART program'
_computing_data_reduction        'Siemens SAINT program'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Siemens CCD SMART Area Detector System'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'UltraX18 Rigaku Denki rotating Mo anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39819
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        0.005
_exptl_absorpt_coefficient_mu    1.886
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997b)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         12329
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0587
_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^)+(0.1037P)^2^+1.1961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1976
_reflns_number_gt                6615
_reflns_number_total             12329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008128k.txt
_cod_data_source_block           TEAh
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7010329