Cation-Directed Structure Changes in Polyoxometalate Chemistry. Equilibria between Isomers of Bis(9-tungstophosphatodioxouranate(VI)) Complexes
Kee-Chan Kim; Michael T. Pope; Journal of the American Chemical Society 121 (1999) 8512–8517; doi:10.1021/ja9909125

data_4116533
_publ_section_title
;
 Cation-Directed Structure Changes in Polyoxometalate Chemistry.
 Equilibria between Isomers of Bis(9-tungstophosphatodioxouranate(VI))
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8512
_journal_page_last               8517
_journal_paper_doi               10.1021/ja9909125
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'H76 Na14 O110 P2 U2 W18'
_chemical_formula_weight         6005.77
_chemical_name_systematic
; 
 ? 
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.2600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.6797(8)
_cell_length_b                   14.6412(7)
_cell_length_c                   21.2925(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      1.32
_cell_volume                     4812.3(4)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1068
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52355
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    24.997
_exptl_absorpt_correction_T_max  0.01679
_exptl_absorpt_correction_T_min  0.00057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, R. (1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.145
_exptl_crystal_description       trianglular
_exptl_crystal_F_000             5312
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_refine_diff_density_max         3.724
_refine_diff_density_min         -4.218
_refine_diff_density_rms         0.545
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         11682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0591P)^2^+194.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                10575
_reflns_number_total             11682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9909125_1.cif
_cod_data_source_block           upw
_cod_database_code               4116533