A new series of lanthanoid containing Keggin-type germanotungstates with acetate chelators: [{Ln(CH3COO)GeW11O39(H2O)}2]12− {Ln=EuIII, GdIII, TbIII, DyIII, HoIII, ErIII, TmIII, and YbIII}
Hussain, Firasat; Sandriesser, Stefan; Speldrich, Manfred; Patzke, Greta R.; Journal of Solid State Chemistry 184 (2011) 214–219; doi:10.1016/j.jssc.2010.11.005

data_1563349
_publ_section_title
;
 A new series of lanthanoid containing Keggin-type germanotungstates with
 acetate chelators: [{Ln(CH3COO)GeW11O39(H2O)}2]12&#x2212; {Ln=EuIII,
 GdIII, TbIII, DyIII, HoIII, ErIII, TmIII, and YbIII}
;
_journal_issue                   1
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              214
_journal_page_last               219
_journal_paper_doi               10.1016/j.jssc.2010.11.005
_journal_volume                  184
_journal_year                    2011
_chemical_formula_sum            'C4 H6 Ge2 K8 Na4 O110 Tb2 W22'
_chemical_formula_weight         6726.57
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 110.886(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.1171(5)
_cell_length_b                   12.6768(2)
_cell_length_c                   21.1300(5)
_cell_measurement_reflns_used    8267
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.4139
_cell_measurement_theta_min      2.5268
_cell_volume                     5034.5(2)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_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  0.0953
_diffrn_reflns_av_sigmaI/netI    0.1092
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43134
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    27.460
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamondshape
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         8.890
_refine_diff_density_min         -3.029
_refine_diff_density_rms         0.451
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         9548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0317P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                6099
_reflns_number_total             9548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2011-184-214.cif
_cod_data_source_block           fh124
_cod_original_cell_volume        5034.51(19)
_cod_database_code               1563349