Self-assembly of a lacunary alpha-Keggin undecatungstophosphate into a three-dimensional network linked by s-block cations.
Honma, Noritaka; Kusaka, Katsuhiro; Ozeki, Tomoji; Chemical communications (Cambridge, England)  (2002) 2896–2897; doi:10.1039/b209076g

data_7125579
_publ_section_title
;
 Self-assembly of a lacunary alpha-Keggin undecatungstophosphate into a
 three-dimensional network linked by s-block cations.
;
_journal_issue                   23
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2896
_journal_page_last               2897
_journal_paper_doi               10.1039/b209076g
_journal_year                    2002
_chemical_formula_moiety
;
(Na 1+)2, (C4 H12 N 1+)4, H 1+, P W11 O39 7-, 8(H2 O)
;
_chemical_formula_sum            'C16 H65 N4 Na2 O47 P W11'
_chemical_formula_weight         3165.02
_chemical_name_common
;
Disodium Tetrakis(tetramethylammonium) hydrogen
undecatungstophosphate octahydrate
;
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 106.206(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   18.494(1)
_cell_length_b                   18.102(1)
_cell_length_c                   19.214(1)
_cell_measurement_reflns_used    6679
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      13.54
_cell_measurement_theta_min      0.934
_cell_volume                     6176.8(6)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'DIP Xpress (MAC Science, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'MAC Science DIP LABO'
_diffrn_measurement_method       'oscillation method'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'SPring-8 BL04B2 bending magnet beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3282
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25266
_diffrn_reflns_theta_full        13.54
_diffrn_reflns_theta_max         13.54
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    2.729
_exptl_absorpt_correction_T_max  0.96072
_exptl_absorpt_correction_T_min  0.87691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON MULABS (Spek, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5664
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         6.275
_refine_diff_density_min         -3.232
_refine_diff_density_rms         0.573
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         14592
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w==1/[\s^2^(Fo^2^)+(0.0747P)^2^+292.0473P] where 
P==(Fo^2^+2Fc^2^)/3=
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                13509
_reflns_number_total             14592
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b209076g.txt
_cod_data_source_block           pw11
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7125579