Na~8.5~H~1.5~[GeW~9~O~34~]·20H~2~O containing trivacant A-α- and A-β-Keggin anions
Xiaoou Cao; Haruo Naruke; Toshihiro Yamase; Acta Crystallographica Section E 59 (2003) i116–i118; doi:10.1107/S1600536803015344

data_2202294
_publ_section_title
;
 Na~8.5~H~1.5~[GeW~9~O~34~]&#x00B7;20H~2~O containing trivacant A-\a-
 and A-\b-Keggin anions
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i116
_journal_page_last               i118
_journal_paper_doi               10.1107/S1600536803015344
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'Na8.5 H1.5 [Ge W9 O~4], 20H2 O'
_chemical_formula_structural     'Na8.5 H1.5 (Ge W9 O34) (H2 O)20'
_chemical_formula_sum            'Ge H41.5 Na8.5 O54 W9'
_chemical_formula_weight         2828.45
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                72.576(3)
_cell_angle_beta                 70.078(3)
_cell_angle_gamma                62.848(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6563(9)
_cell_length_b                   13.2600(10)
_cell_length_c                   18.491(2)
_cell_measurement_reflns_used    11591
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.3
_cell_volume                     2557.3(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction
'teXsan Ver. 1.11 (Molecular Structure Corporation, 2000)'
_computing_publication_material  'teXsan Ver. 1.11, ORTEP II (Johnson, 1976)'
_computing_structure_refinement  'teXsan Ver. 1.11'
_computing_structure_solution    'SYSTEM90 (Yonggeng et al, 1994)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9685
_diffrn_measured_fraction_theta_max 0.9685
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18682
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_exptl_absorpt_coefficient_mu    20.948
_exptl_absorpt_correction_T_max  0.173
_exptl_absorpt_correction_T_min  0.041
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         4.29
_refine_diff_density_min         -3.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.559
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     586
_refine_ls_number_reflns         14383
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1631
_reflns_number_gt                9852
_reflns_number_total             14391
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            br6108.cif
_cod_data_source_block           I
_cod_original_cell_volume        2557.3(3)
_cod_original_formula_sum        'Ge H41.50 Na8.50 O54 W9 '
_cod_database_code               2202294