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_4116612
_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 H94 K5 O153 P5 W30'
_chemical_formula_weight         8448.68
_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                 104.8080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.4987(2)
_cell_length_b                   21.5054(3)
_cell_length_c                   17.54970(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      1.20
_cell_volume                     6384.90(12)
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0880
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70566
_diffrn_reflns_theta_full        28.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    27.303
_exptl_absorpt_correction_T_max  0.065688
_exptl_absorpt_correction_T_min  0.019394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'empirical (Blessing, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    4.395
_exptl_crystal_description       Block
_exptl_crystal_F_000             7456
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         5.688
_refine_diff_density_min         -7.767
_refine_diff_density_rms         0.590
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         15933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0707P)^2^+313.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1632
_reflns_number_gt                11706
_reflns_number_total             15933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992105b_s2.cif
_cod_data_source_block           hca
_cod_original_formula_sum        'H94 Ca K5 O153 P5 W30'
_cod_database_code               4116612