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_4116534
_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            'H94 N14 O91 P2 U2 W18'
_chemical_formula_weight         5594.19
_chemical_name_systematic
; 
 ? 
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.056(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6010(17)
_cell_length_b                   20.175(3)
_cell_length_c                   35.124(8)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      1.17
_cell_volume                     8818(3)
_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 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0758
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            86503
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.17
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    27.194
_exptl_absorpt_correction_T_max  0.04197
_exptl_absorpt_correction_T_min  0.00944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, R. (1995)'
_exptl_crystal_colour            'greenish yellow'
_exptl_crystal_density_diffrn    4.214
_exptl_crystal_description       plate
_exptl_crystal_F_000             9864
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         6.381
_refine_diff_density_min         -4.218
_refine_diff_density_rms         0.547
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         21246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0620P)^2^+195.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1449
_reflns_number_gt                15442
_reflns_number_total             21246
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9909125_2.cif
_cod_data_source_block           npu
_cod_database_code               4116534