Guest driven rearrangements of protonation and hydrogen bonding in decavanadate anions as their tetraalkylammonium salts
Nakamura, Setsuko; Ozeki, Tomoji; Dalton Transactions  (2008) 6135–6140; doi:10.1039/b807880g

data_7004493
_publ_section_title
;
 Guest driven rearrangements of protonation and hydrogen bonding in
 decavanadate anions as their tetraalkylammonium salts
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              6135
_journal_page_last               6140
_journal_paper_doi               10.1039/b807880g
_journal_year                    2008
_chemical_formula_moiety         '(C20 H44 N +)3, (H3 O28 V10 3-), 2(C3 H6 O)'
_chemical_formula_sum            'C66 H147 N3 O30 V10'
_chemical_formula_weight         1972.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   other
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.046(1)
_cell_angle_beta                 83.492(1)
_cell_angle_gamma                64.872(1)
_cell_formula_units_Z            4
_cell_length_a                   15.6398(2)
_cell_length_b                   17.3162(3)
_cell_length_c                   36.3096(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      1.47
_cell_volume                     8800.8(2)
_computing_cell_refinement       'SMART (Bruker AXS)'
_computing_data_collection       'SMART (Bruker AXS)'
_computing_data_reduction        'SAINT (Bruker AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART CCD area detector system'
_diffrn_measurement_method       'oscillation method, \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Ultrax Rotating Mo Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            81535
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         1.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.8992
_exptl_absorpt_correction_T_min  0.7607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs (Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4136
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1942
_refine_ls_number_reflns         42975
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0514P)^2^+17.9283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                24400
_reflns_number_total             42975
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b807880g.txt
_cod_data_source_block           TAA-acetone
_cod_original_cell_volume        8800.81(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004493