Cation-controlled assembly of Na±linked lacunary alpha-Keggin tungstosilicates.
Chiba, Hirokazu; Wada, Akihide; Ozeki, Tomoji; Dalton transactions (Cambridge, England : 2003)  (2006) 1213–1217; doi:10.1039/b514169a

data_7006802
_publ_section_title
;
 Cation-controlled assembly of Na+-linked lacunary alpha-Keggin
 tungstosilicates.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1213
_journal_page_last               1217
_journal_paper_doi               10.1039/b514169a
_journal_year                    2006
_chemical_formula_moiety
'(C H6 N3 1+), (K 1+)6, (Na O39 Si W11 7-), 11.5(H2 O)'
_chemical_formula_sum            'C H29 K6 N3 Na O50.5 Si W11'
_chemical_formula_weight         3199.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           40
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2a'
_symmetry_space_group_name_H-M   'A m a 2'
_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                   19.457(1)
_cell_length_b                   22.581(1)
_cell_length_c                   11.069(1)
_cell_measurement_reflns_used    19065
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      13.53
_cell_measurement_theta_min      1.28
_cell_volume                     4863.3(5)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'DIP Xpress (MAC Science, 1999)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'MAC Science DIP LABO'
_diffrn_measurement_method       'Weissenberg 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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33873
_diffrn_reflns_theta_full        13.53
_diffrn_reflns_theta_max         13.53
_diffrn_reflns_theta_min         1.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.516
_exptl_absorpt_correction_T_max  0.70018
_exptl_absorpt_correction_T_min  0.68385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON MULABS (Spek, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             5652
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.458
_refine_diff_density_min         -1.875
_refine_diff_density_rms         0.248
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         7281
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0287P)^2^+107.2638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                7023
_reflns_number_total             7281
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b514169a.txt
_cod_data_source_block           compound_2
_cod_original_sg_symbol_H-M      Ama2
_cod_original_formula_sum        'C H29 K6 N3 Na O50.50 Si W11'
_cod_database_code               7006802