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_7010331
_publ_section_title
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 Hydrogen-bonded aggregates of protonated decavanadate anions in their
 tetraalkylammonium salts&#x200A;&#x2020;&#x200A;&#x2021;
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_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-)'
_chemical_formula_sum            'C36 H87 N3 O28 V10'
_chemical_formula_weight         1519.49
_chemical_name_common
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Tris(tetra-n-propylammonium) trihydrogendecavanadate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.996(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.3026(13)
_cell_length_b                   14.0097(13)
_cell_length_c                   21.9911(18)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    298
_cell_measurement_theta_max      14.96
_cell_measurement_theta_min      14.88
_cell_volume                     5839.7(8)
_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-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC 7R'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13743
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        2.20
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         13371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.9482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                9478
_reflns_number_total             13371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008128k.txt
_cod_data_source_block           TPAv
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7010331