A High-Nuclearity "Celtic-Ring" Isopolyoxotungstate, [H12W36O120]12-, That Captures Trace Potassium Ions
De-Liang Long; Hamera Abbas; Paul Kögerler; Leroy Cronin; Journal of the American Chemical Society 126 (2004) 13880–13881; doi:10.1021/ja046410v

data_4113120
_publ_section_title
;
 A High-Nuclearity "Celtic-Ring" Isopolyoxotungstate, [H12W36O120]12-,
 That Captures Trace Potassium Ions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13880
_journal_page_last               13881
_journal_paper_doi               10.1021/ja046410v
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety
'9(C6 H16 N O3 +), 2(Na +), (H12 K W36 O120 11-), 21(H2 O)'
_chemical_formula_sum            'C54 H198 K N9 Na2 O168 W36'
_chemical_formula_weight         10365.9
_chemical_name_common            'Compound DL098'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.6536(12)
_cell_length_b                   35.0945(13)
_cell_length_c                   20.6000(8)
_cell_measurement_reflns_used    7277
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     19992.1(14)
_computing_cell_refinement       'POSTREF (CCP4 1994)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'EVAL-14 (Duisenberg, Kroon-Batenburg & Schreurs 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1297
_diffrn_reflns_av_sigmaI/netI    0.1458
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            50472
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    20.753
_exptl_absorpt_correction_T_max  0.3690
_exptl_absorpt_correction_T_min  0.0625
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.444
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             18536
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.76
_refine_diff_density_min         -1.45
_refine_diff_density_rms         0.34
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1147
_refine_ls_number_reflns         17472
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1475
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0439P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                9165
_reflns_number_total             17472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046410vsi20040830_042555.cif
_cod_data_source_block           dl098
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4113120