Synthesis and Characterization of the GeO4Al12(OH)24(OH2)128+ Polyoxocation
Alasdair P. Lee; Brian L. Phillips; Marilyn M. Olmstead; William H. Casey; Inorganic Chemistry 40 (2001) 4485–4487; doi:10.1021/ic010146e

data_4320073
_publ_section_title
;
 Synthesis and Characterization of the GeO4Al12(OH)24(OH2)128+
 Polyoxocation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4485
_journal_page_last               4487
_journal_paper_doi               10.1021/ic010146e
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'Al12 Ge H62 O70 Se4'
_chemical_formula_weight         1894.69
_chemical_name_common            '[GeO4Al12(OH)24(H2O)12](SeO4)4.14H2O'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           119
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 -2'
_symmetry_space_group_name_H-M   'I -4 m 2'
_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            2
_cell_length_a                   13.0322(7)
_cell_length_b                   13.0322(7)
_cell_length_c                   17.2087(13)
_cell_measurement_reflns_used    2639
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.21
_cell_volume                     2922.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27190
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames measured at beginning and end'
_exptl_absorpt_coefficient_mu    3.345
_exptl_absorpt_correction_T_max  0.9673
_exptl_absorpt_correction_T_min  0.9673
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2.0 (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tetrahedron
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.387
_refine_diff_density_min         -1.734
_refine_diff_density_rms         0.209
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_coef       0.00029(15)
_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   1.299
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.299
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+75.6718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                1764
_reflns_number_total             1829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010146e.cif
_cod_data_source_block           mn1158
_cod_original_formula_sum        'H62 Al12 Ge O70 Se4'
_cod_database_code               4320073