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_7010330
_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_sum            'C24 H60 N2 O28 V10'
_chemical_formula_weight         1334.14
_chemical_name_common
;
Bis(tetra-n-propylammonium) tetrahydrogendecavanadate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.6530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.55680(10)
_cell_length_b                   13.1873(2)
_cell_length_c                   20.1901(3)
_cell_measurement_reflns_used    4769
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.84
_cell_volume                     2275.83(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16898
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0.001
_diffrn_standards_number         135
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997b)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5664
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0559P)^2^+0.2174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                3395
_reflns_number_total             5664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008128k.txt
_cod_data_source_block           TPAc
_cod_depositor_comments
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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/n'
_cod_database_code               7010330