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_7004495
_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-)'
_chemical_formula_sum            'C60 H135 N3 O28 V10'
_chemical_formula_weight         1856.11
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                119.342(1)
_cell_angle_beta                 91.881(1)
_cell_angle_gamma                100.598(1)
_cell_formula_units_Z            8
_cell_length_a                   15.5420(2)
_cell_length_b                   34.9806(2)
_cell_length_c                   35.6115(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      1.36
_cell_volume                     16417.5(4)
_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 0.976
_diffrn_measured_fraction_theta_max 0.947
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            159050
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.8456
_exptl_absorpt_correction_T_min  0.7288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs (Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7760
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.551
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2619
_refine_ls_number_reflns         95592
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0722
_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^)+(0.0421P)^2^+85.8530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1832
_reflns_number_gt                56050
_reflns_number_total             95592
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b807880g.txt
_cod_data_source_block           TAAh
_cod_original_cell_volume        16417.5(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004495