Slow Proton Exchange in Aqueous Solution. Consequences of Protonation and Hydration within the Central Cavity of Preyssler Anion Derivatives, [|M(H2O)|@P5W30O110]n-
Kee-Chan Kim; Michael T. Pope; Gennaro J. Gama; Michael H. Dickman; Journal of the American Chemical Society 121 (1999) 11164–11170; doi:10.1021/ja992105b

data_4116611
_publ_section_title
;
 Slow Proton Exchange in Aqueous Solution. Consequences of Protonation and
 Hydration within the Central Cavity of Preyssler Anion Derivatives,
 [|M(H2O)|@P5W30O110]n-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11164
_journal_page_last               11170
_journal_paper_doi               10.1021/ja992105b
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'Ca H100 N13 O134 P5 W30'
_chemical_formula_weight         8137.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 104.5050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.7526(3)
_cell_length_b                   21.1054(4)
_cell_length_c                   17.8629(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.18
_cell_volume                     6479.47(18)
_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  0.1232
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            68656
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    26.731
_exptl_absorpt_correction_T_max  0.067774
_exptl_absorpt_correction_T_min  0.011168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'empirical (Blessing, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    4.171
_exptl_crystal_description       Plate
_exptl_crystal_F_000             7156
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.16
_refine_diff_density_max         10.059
_refine_diff_density_min         -9.714
_refine_diff_density_rms         0.761
_refine_ls_extinction_coef       0.000227(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         15877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0840
_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^)+(0.1073P)^2^+533.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2382
_reflns_number_gt                11398
_reflns_number_total             15877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992105b_s1.cif
_cod_data_source_block           ncp
_cod_original_formula_sum        'H100 Ca N13 O134 P5 W30'
_cod_database_code               4116611