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_4116616
_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            'H96 N12 O134 P5 W30 Y'
_chemical_formula_weight         8168.15
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.1420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.52550(10)
_cell_length_b                   21.0554(2)
_cell_length_c                   35.5201(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      1.13
_cell_volume                     12709.91(19)
_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 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0967
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            136241
_diffrn_reflns_theta_full        28.54
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    27.663
_exptl_absorpt_correction_T_max  0.027388
_exptl_absorpt_correction_T_min  0.003960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'empirical (Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.269
_exptl_crystal_description       Block
_exptl_crystal_F_000             14344
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.223
_refine_diff_density_min         -8.081
_refine_diff_density_rms         0.570
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         31070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+735.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                22400
_reflns_number_total             31070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992105b_s6.cif
_cod_data_source_block           nyp
_cod_original_cell_volume        12709.91(18)
_cod_database_code               4116616