#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/08/2210807.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2210807
loop_
_publ_author_name
'Han, Qiu-Xia'
'Wang, Jing-Ping'
'Song, Li-Hua'
_publ_section_title
;
 K₂NaH[GeW₁₂O₄₀]·7H₂O, with a Keggin-type
 heteropolyoxoanion
;
_journal_coeditor_code           WM2028
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i201
_journal_page_last               i203
_journal_paper_doi               10.1107/S1600536806034362
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'K2 Na H [Ge W12 O40] , 7H2 O'
_chemical_formula_structural     'Ge H1 K2 Na1 O40 W12 , 7H2 O'
_chemical_formula_sum            'Ge H15 K2 Na O47 W12'
_chemical_formula_weight         3147.12
_chemical_name_systematic
;
Dipotassium sodium hydrogen dodecatungstogermanate heptahydrate
;
_space_group_IT_number           180
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 62 2 (0 0 4)'
_symmetry_space_group_name_H-M   'P 62 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   19.057(3)
_cell_length_b                   19.057(3)
_cell_length_c                   12.557(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     3949.3(13)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics
;
XP in SHELXTL (Bruker, 2000) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ω
_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  0.0910
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12980
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    26.916
_exptl_absorpt_correction_T_max  0.2950
_exptl_absorpt_correction_T_min  0.1738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.973
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4087
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.730
_refine_diff_density_min         -1.248
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs'
_refine_ls_abs_structure_Flack   0.61(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2318
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0394P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                2165
_reflns_number_total             2318
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2028.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'P62 2c'
_cod_original_sg_symbol_H-M      'P62 2 2'
_cod_original_formula_sum        'Ge H15 K2 Na1 O47 W12'
_cod_database_code               2210807
_cod_database_fobs_code          2210807
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/3'
'-y, x-y, z+2/3'
'-x, -y, z'
'-x+y, -x, z+1/3'
'y, -x+y, z+2/3'
'-y, -x, -z+2/3'
'x-y, -y, -z'
'x, x-y, -z+1/3'
'y, x, -z+2/3'
'-x+y, y, -z'
'-x, -x+y, -z+1/3'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
K K1 -1.62856(13) -0.2571(3) 0.5000 0.0152(10) Uani d S 1
Ge Ge1 -1.5000 -0.5000 0.3333 0.0065(6) Uani d S 1
W W1 -1.62679(4) -0.63466(4) 0.53271(4) 0.01136(15) Uani d . 1
W W2 -1.70650(3) -0.55520(4) 0.32408(5) 0.01000(15) Uani d . 1
W W3 -1.56860(4) -0.41735(4) 0.53160(4) 0.00986(15) Uani d . 1
O O1 -1.6984(7) -0.6857(6) 0.6270(7) 0.015(2) Uani d U 1
O O2 -1.8049(7) -0.5831(7) 0.3523(8) 0.017(2) Uani d U 1
O O3 -1.6228(6) -0.3971(6) 0.6223(7) 0.012(2) Uani d U 1
O O4 -1.6861(7) -0.6205(6) 0.4210(8) 0.016(2) Uani d U 1
O O5 -1.5913(7) -0.5254(6) 0.5683(8) 0.015(2) Uani d U 1
O O6 -1.7240(7) -0.6318(7) 0.2112(7) 0.015(2) Uani d U 1
O O7 -1.6819(6) -0.4755(7) 0.2140(7) 0.014(2) Uani d U 1
O O8 -1.6473(6) -0.4696(6) 0.4214(7) 0.009(2) Uani d U 1
O O9 -1.4674(6) -0.3744(7) 0.6046(7) 0.015(2) Uani d U 1
O O10 -1.5822(6) -0.5216(6) 0.2524(7) 0.007(2) Uani d U 1
O O1W -1.6527(9) -0.1231(9) 0.5176(11) 0.039(3) Uani d DU 1
O O2W -1.5000 -0.5000 -0.1192(11) 0.021(4) Uani d S 1
Na Na1 -1.790(2) -0.131(2) 0.435(3) 0.039(8) Uiso d P 0.25
O O3W -1.757(3) 0.0000 0.5000 0.083(16) Uiso d SP 0.50
H H1WA -1.661(12) -0.082(8) 0.526(15) 0.039(3) Uiso d DU 1
H H1WB -1.699(6) -0.138(12) 0.487(13) 0.039(3) Uiso d DU 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 K1 O3 9_566 3_364 157.9(5) ?
O3 K1 O7 9_566 7_335 109.8(3) ?
O3 K1 O7 3_364 7_335 78.3(3) ?
O3 K1 O7 9_566 5_235 78.3(3) ?
O3 K1 O7 3_364 5_235 109.8(3) ?
O7 K1 O7 7_335 5_235 138.1(5) ?
O3 K1 O1W 9_566 11_256 88.3(4) ?
O3 K1 O1W 3_364 11_256 74.3(4) ?
O7 K1 O1W 7_335 11_256 72.7(4) ?
O7 K1 O1W 5_235 11_256 149.0(4) ?
O3 K1 O1W 9_566 . 74.3(4) ?
O3 K1 O1W 3_364 . 88.3(4) ?
O7 K1 O1W 7_335 . 149.0(4) ?
O7 K1 O1W 5_235 . 72.7(4) ?
O1W K1 O1W 11_256 . 76.8(6) ?
O3 K1 O3 9_566 11_256 126.1(2) ?
O3 K1 O3 3_364 11_256 72.2(3) ?
O7 K1 O3 7_335 11_256 93.0(3) ?
O7 K1 O3 5_235 11_256 54.5(3) ?
O1W K1 O3 11_256 11_256 145.6(3) ?
O1W K1 O3 . 11_256 109.5(3) ?
O3 K1 O3 9_566 . 72.2(3) ?
O3 K1 O3 3_364 . 126.1(2) ?
O7 K1 O3 7_335 . 54.5(3) ?
O7 K1 O3 5_235 . 93.0(3) ?
O1W K1 O3 11_256 . 109.5(3) ?
O1W K1 O3 . . 145.6(3) ?
O3 K1 O3 11_256 . 84.7(4) ?
O3 K1 W3 9_566 11_256 100.8(2) ?
O3 K1 W3 3_364 11_256 94.6(2) ?
O7 K1 W3 7_335 11_256 111.8(2) ?
O7 K1 W3 5_235 11_256 29.5(2) ?
O1W K1 W3 11_256 11_256 167.3(3) ?
O1W K1 W3 . 11_256 97.0(3) ?
O3 K1 W3 11_256 11_256 26.52(17) ?
O3 K1 W3 . 11_256 82.0(2) ?
O3 K1 W3 9_566 . 94.6(2) ?
O3 K1 W3 3_364 . 100.8(2) ?
O7 K1 W3 7_335 . 29.5(2) ?
O7 K1 W3 5_235 . 111.8(2) ?
O1W K1 W3 11_256 . 97.0(3) ?
O1W K1 W3 . . 167.3(3) ?
O3 K1 W3 11_256 . 82.0(2) ?
O3 K1 W3 . . 26.52(17) ?
W3 K1 W3 11_256 . 91.16(10) ?
O3 K1 K1 9_566 3_364 158.2(3) ?
O3 K1 K1 3_364 3_364 39.1(2) ?
O7 K1 K1 7_335 3_364 83.1(2) ?
O7 K1 K1 5_235 3_364 80.5(2) ?
O1W K1 K1 11_256 3_364 112.7(3) ?
O1W K1 K1 . 3_364 103.9(3) ?
O3 K1 K1 11_256 3_364 33.13(17) ?
O3 K1 K1 . 3_364 104.3(2) ?
W3 K1 K1 11_256 3_364 57.58(8) ?
W3 K1 K1 . 3_364 88.65(5) ?
O3 K1 K1 9_566 5_235 39.1(2) ?
O3 K1 K1 3_364 5_235 158.2(3) ?
O7 K1 K1 7_335 5_235 80.5(2) ?
O7 K1 K1 5_235 5_235 83.1(2) ?
O1W K1 K1 11_256 5_235 103.9(3) ?
O1W K1 K1 . 5_235 112.7(3) ?
O3 K1 K1 11_256 5_235 104.3(2) ?
O3 K1 K1 . 5_235 33.13(17) ?
W3 K1 K1 11_256 5_235 88.65(5) ?
W3 K1 K1 . 5_235 57.58(8) ?
K1 K1 K1 3_364 5_235 132.86(14) ?
O10 Ge1 O10 4_245 . 108.3(6) yes
O10 Ge1 O10 4_245 10_465 109.6(7) y
O10 Ge1 O10 . 10_465 110.5(6) yes
O10 Ge1 O10 4_245 7_335 110.5(6) ?
O10 Ge1 O10 . 7_335 109.6(7) ?
O10 Ge1 O10 10_465 7_335 108.3(6) ?
O1 W1 O5 . . 102.0(5) ?
O1 W1 O4 . . 103.4(5) ?
O5 W1 O4 . . 86.0(4) ?
O1 W1 O6 . 10_465 100.0(5) ?
O5 W1 O6 . 10_465 157.9(4) ?
O4 W1 O6 . 10_465 89.1(4) ?
O1 W1 O9 . 4_245 99.7(4) ?
O5 W1 O9 . 4_245 89.2(5) ?
O4 W1 O9 . 4_245 156.9(4) ?
O6 W1 O9 10_465 4_245 87.0(5) ?
O1 W1 O10 . 10_465 169.1(4) ?
O5 W1 O10 . 10_465 85.4(4) ?
O4 W1 O10 . 10_465 84.9(4) ?
O6 W1 O10 10_465 10_465 72.7(4) ?
O9 W1 O10 4_245 10_465 72.2(4) ?
O2 W2 O8 . . 102.8(5) ?
O2 W2 O4 . . 102.3(5) ?
O8 W2 O4 . . 85.6(4) ?
O2 W2 O7 . . 101.0(5) ?
O8 W2 O7 . . 88.8(4) ?
O4 W2 O7 . . 156.7(5) ?
O2 W2 O6 . . 99.6(5) ?
O8 W2 O6 . . 157.5(4) ?
O4 W2 O6 . . 89.4(4) ?
O7 W2 O6 . . 87.2(4) ?
O2 W2 O10 . . 169.0(4) ?
O8 W2 O10 . . 85.8(4) ?
O4 W2 O10 . . 85.0(4) ?
O7 W2 O10 . . 72.0(4) ?
O6 W2 O10 . . 72.0(4) ?
O3 W3 O9 . . 100.3(4) ?
O3 W3 O8 . . 101.2(4) ?
O9 W3 O8 . . 158.5(4) ?
O3 W3 O7 . 7_335 98.0(4) ?
O9 W3 O7 . 7_335 88.6(5) ?
O8 W3 O7 . 7_335 89.0(4) ?
O3 W3 O5 . . 104.1(4) ?
O9 W3 O5 . . 89.0(5) ?
O8 W3 O5 . . 85.3(4) ?
O7 W3 O5 7_335 . 157.9(4) ?
O3 W3 O10 . 7_335 168.7(4) ?
O9 W3 O10 . 7_335 73.1(4) ?
O8 W3 O10 . 7_335 85.8(4) ?
O7 W3 O10 7_335 7_335 73.0(4) ?
O5 W3 O10 . 7_335 85.2(4) ?
O3 W3 K1 . . 54.9(3) ?
O9 W3 K1 . . 110.7(4) ?
O8 W3 K1 . . 82.5(3) ?
O7 W3 K1 7_335 . 46.3(3) ?
O5 W3 K1 . . 152.6(3) ?
O10 W3 K1 7_335 . 118.1(3) ?
W3 O3 K1 . 5_235 141.1(5) ?
W3 O3 K1 . . 98.5(4) ?
K1 O3 K1 5_235 . 107.7(3) ?
W1 O4 W2 . . 152.7(6) ?
W1 O5 W3 . . 151.7(6) ?
W1 O6 W2 10_465 . 121.1(6) ?
W1 O6 Na1 10_465 3_364 120.8(8) ?
W2 O6 Na1 . 3_364 106.0(8) ?
W3 O7 W2 7_335 . 120.9(5) ?
W3 O7 K1 7_335 3_364 104.2(4) ?
W2 O7 K1 . 3_364 132.9(5) ?
W2 O8 W3 . . 152.8(6) ?
W3 O9 W1 . 4_245 120.4(5) ?
Ge1 O10 W3 . 7_335 123.1(5) ?
Ge1 O10 W1 . 10_465 122.5(5) ?
W3 O10 W1 7_335 10_465 94.3(3) ?
Ge1 O10 W2 . . 121.2(5) ?
W3 O10 W2 7_335 . 94.1(4) ?
W1 O10 W2 10_465 . 94.1(4) ?
Na1 O1W K1 . . 120.3(9) ?
Na1 O1W H1WA . . 60(10) ?
K1 O1W H1WA . . 178(10) ?
Na1 O1W H1WB . . 15(10) ?
K1 O1W H1WB . . 105(10) ?
H1WA O1W H1WB . . 75(10) ?
O3W Na1 O1W . . 93.7(17) ?
O3W Na1 O6 . 5_235 120.6(14) ?
O1W Na1 O6 . 5_235 97.5(11) ?
O3W Na1 Na1 . 7_335 129.0(14) ?
O1W Na1 Na1 . 7_335 125.5(9) ?
O6 Na1 Na1 5_235 7_335 88.3(15) ?
O3W Na1 H1WA . . 76(2) ?
O1W Na1 H1WA . . 18.0(16) ?
O6 Na1 H1WA 5_235 . 107(4) ?
Na1 Na1 H1WA 7_335 . 139(4) ?
O3W Na1 H1WB . . 100(6) ?
O1W Na1 H1WB . . 7(6) ?
O6 Na1 H1WB 5_235 . 94(6) ?
Na1 Na1 H1WB 7_335 . 120(6) ?
H1WA Na1 H1WB . . 25(6) ?
Na1 O3W Na1 8_556 . 150(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
K1 O3 9_566 2.708(9) y
K1 O3 3_364 2.708(9) ?
K1 O7 7_335 2.819(11) y
K1 O7 5_235 2.819(11) ?
K1 O1W 11_256 2.822(15) ?
K1 O1W . 2.822(15) y
K1 O3 11_256 3.127(10) y
K1 O3 . 3.127(10) ?
K1 W3 11_256 3.778(3) ?
K1 W3 . 3.778(3) ?
K1 K1 3_364 4.719(4) ?
K1 K1 5_235 4.719(4) ?
Ge1 O10 4_245 1.734(10) ?
Ge1 O10 . 1.734(10) y
Ge1 O10 10_465 1.734(10) ?
Ge1 O10 7_335 1.734(10) ?
W1 O1 . 1.697(10) yes
W1 O5 . 1.893(11) yes
W1 O4 . 1.903(10) yes
W1 O6 10_465 1.921(10) yes
W1 O9 4_245 1.938(10) yes
W1 O10 10_465 2.286(10) yes
W2 O2 . 1.711(11) yes
W2 O8 . 1.893(9) yes
W2 O4 . 1.915(10) yes
W2 O7 . 1.929(10) yes
W2 O6 . 1.940(10) yes
W2 O10 . 2.306(10) yes
W3 O3 . 1.706(10) yes
W3 O9 . 1.911(10) yes
W3 O8 . 1.914(9) yes
W3 O7 7_335 1.917(10) yes
W3 O5 . 1.937(11) yes
W3 O10 7_335 2.268(10) yes
O3 K1 5_235 2.708(9) ?
O6 W1 10_465 1.921(10) ?
O6 Na1 3_364 2.89(4) ?
O7 W3 7_335 1.917(10) ?
O7 K1 3_364 2.819(11) ?
O9 W1 4_245 1.938(10) ?
O10 W3 7_335 2.268(10) ?
O10 W1 10_465 2.286(10) ?
O1W Na1 . 2.76(4) ?
O1W H1WA . 0.87(5) ?
O1W H1WB . 0.87(5) ?
O2W O2W 7_334 1.19(3) ?
Na1 O3W . 2.39(4) y
Na1 O6 5_235 2.89(4) y
Na1 Na1 7_335 2.96(6) ?
Na1 H1WA . 2.4(2) ?
Na1 H1WB . 1.93(10) ?
O3W Na1 8_556 2.39(4) ?
