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_7004496
_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
'(C24 H52 N +)2, (H4 O28 V10 2-), 4(C4 H8 O2)'
_chemical_formula_sum            'C64 H140 N2 O36 V10'
_chemical_formula_weight         2023.18
_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                 133.093(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   53.8043(8)
_cell_length_b                   12.3166(2)
_cell_length_c                   36.8334(8)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      1.51
_cell_volume                     17824.6(8)
_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      93(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -71
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            71084
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.8998
_exptl_absorpt_correction_T_min  0.6830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs (Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.388
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         22147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.1286
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+1506.4004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3188
_refine_ls_wR_factor_ref         0.3273
_reflns_number_gt                17334
_reflns_number_total             22147
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b807880g.txt
_cod_data_source_block           THA-dioxane
_cod_original_cell_volume        17824.5(6)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7004496