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_4113122
_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         '6(C6 H16 N O3 +), (H2 O40 W12 6-)'
_chemical_formula_sum            'C36 H98 N6 O58 W12'
_chemical_formula_weight         3749.40
_chemical_name_common            'Compound HA162'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                   22.9618(3)
_cell_length_b                   14.7301(2)
_cell_length_c                   22.6265(4)
_cell_measurement_reflns_used    4583
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.62
_cell_volume                     7653.0(2)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\w scan'
_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  0.0778
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34923
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    18.068
_exptl_absorpt_correction_T_max  0.1394
_exptl_absorpt_correction_T_min  0.1228
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS: Bruker Nonius area detector scaling and absorption
 correction - V2.10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.254
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6832
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.44
_refine_diff_density_min         -1.25
_refine_diff_density_rms         0.23
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(12)
_refine_ls_extinction_coef       0.000019(4)
_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   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         7266
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0296P)^2^+71.2389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                6720
_reflns_number_total             7266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046410vsi20040830_042631.cif
_cod_data_source_block           HA162
_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               4113122