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_7010332
_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         '(C12 H28 N +)3, (H3 V10 O28 3-), 0.5(H2 O)'
_chemical_formula_sum            'C36 H88 N3 O28.5 V10'
_chemical_formula_weight         1528.49
_chemical_name_common
;
 Tris(tetra-n-propylammonium) trihydrogendecavanadate monohydrate
;
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 95.448(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.994(4)
_cell_length_b                   24.643(4)
_cell_length_c                   17.9049(15)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    298
_cell_measurement_theta_max      14.995
_cell_measurement_theta_min      14.855
_cell_volume                     12296(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection       'MSC/AFC Diffractometer Control Software'
_computing_data_reduction
'teXsan PROCESS (Molecular Structure Corporation, 1993)'
_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 0.585
_diffrn_measured_fraction_theta_max 0.585
_diffrn_measurement_device_type  'Rigaku AFC7R'
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_sigmaI/netI    0.1189
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16466
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        3.084
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6264
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.09(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         8347
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1972
_reflns_number_gt                3612
_reflns_number_total             8347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008128k.txt
_cod_data_source_block           TPAh
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C36 H88 N3 O28.50 V10'
_cod_database_code               7010332