#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/33/2203371.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_2203371
loop_
_publ_author_name
'Lee, Uk'
'Joo, Hea-Chung'
'Park, Ki-Min'
_publ_section_title
;
 A diprotonated hexatungstoplatinate(IV),
 Na₆[H₂PtW₆O₂₄]·22H₂O
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i55
_journal_page_last               i57
_journal_paper_doi               10.1107/S1600536804004970
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'Na6 [H2 Pt W6 O24], 22H2 O'
_chemical_formula_moiety         'H2 O24 Pt W6 6-, 22H2 O, 6Na 1+'
_chemical_formula_structural     'Na6 [H2 Pt W6 O24], 22H2 O'
_chemical_formula_sum            'H46 Na6 O46 Pt W6'
_chemical_formula_weight         2218.50
_chemical_name_systematic        ?
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.130(10)
_cell_angle_beta                 107.170(10)
_cell_angle_gamma                99.480(10)
_cell_formula_units_Z            1
_cell_length_a                   10.0280(10)
_cell_length_b                   10.5910(10)
_cell_length_c                   12.109(3)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      10.5
_cell_measurement_theta_min      9.6
_cell_volume                     1070.8(3)
_computing_cell_refinement       'STADI4 (Stoe & Cie, 1996)'
_computing_data_collection       'STADI4 (Stoe & Cie, 1996)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)'
_computing_publication_material  'SHELXL97-2 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97-2 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       'ω/2-θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4896
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        3.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    19.483
_exptl_absorpt_correction_T_max  0.1556
_exptl_absorpt_correction_T_min  0.0505
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    3.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.618
_refine_diff_density_min         -2.184
_refine_ls_extinction_coef       0.0073(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc2^λ3^/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0354
_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/[σ2^(Fo2^)+(0.0492P)2^+10.2521P] where P=(Fo2+2Fc2)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                4223
_reflns_number_total             4896
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br6139.cif
_cod_data_source_block           I
_cod_database_code               2203371
_cod_database_fobs_code          2203371
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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
_atom_site_type_symbol
Pt 0.5000 0.5000 0.5000 0.01087(11) Uani d S 1 Pt
W1 0.33879(4) 0.25398(4) 0.56051(3) 0.01577(11) Uani d . 1 W
W2 0.18378(3) 0.24979(4) 0.27524(3) 0.01620(11) Uani d . 1 W
W3 0.35661(3) 0.49681(4) 0.21816(3) 0.01555(11) Uani d . 1 W
O1 0.5484(6) 0.3639(6) 0.5718(6) 0.0154(11) Uani d . 1 O
O2 0.2980(6) 0.4155(6) 0.4870(6) 0.0145(11) Uani d . 1 O
O3 0.4132(7) 0.3558(7) 0.3086(6) 0.0164(12) Uani d . 1 O
O4 0.2786(7) 0.1568(7) 0.3713(6) 0.0207(13) Uani d . 1 O
O5 0.1810(7) 0.4127(7) 0.2372(6) 0.0191(12) Uani d . 1 O
O6 0.5666(7) 0.5787(7) 0.2672(6) 0.0192(12) Uani d . 1 O
O7 0.4046(7) 0.1226(7) 0.5879(7) 0.0277(15) Uani d . 1 O
O8 0.1655(7) 0.2209(8) 0.5668(7) 0.0254(14) Uani d . 1 O
O9 0.0154(7) 0.2248(7) 0.2904(7) 0.0244(14) Uani d . 1 O
O10 0.1492(7) 0.1124(7) 0.1216(6) 0.0286(15) Uani d . 1 O
O11 0.3242(7) 0.3612(8) 0.0622(6) 0.0257(14) Uani d . 1 O
O12 0.2935(7) 0.6262(8) 0.1880(7) 0.0268(14) Uani d . 1 O
Na1 0.0692(4) 0.7606(5) 0.5278(4) 0.0343(9) Uani d . 1 Na
Na2 0.1244(9) 0.7539(10) 0.2315(9) 0.0366(19) Uani d P 0.50 Na
Na3 0.2998(5) 0.7366(5) 0.0474(4) 0.0365(10) Uani d . 1 Na
Na4 0.5000 1.0000 0.0000 0.0337(13) Uani d S 1 Na
O13 -0.0149(10) 0.5605(12) 0.3040(10) 0.069(3) Uani d . 1 O
O14 0.1830(9) 0.6111(9) 0.6065(8) 0.0377(18) Uani d . 1 O
O15 0.1706(9) 1.0201(10) 0.6822(9) 0.046(2) Uani d . 1 O
O16 0.2762(11) 0.8203(10) 0.4749(12) 0.066(3) Uani d . 1 O
O17 -0.0453(16) 0.8666(14) 0.1383(15) 0.092(4) Uani d . 1 O
O18 0.0423(11) 0.6340(17) 0.0027(11) 0.086(4) Uani d . 1 O
O19 0.3787(16) 0.9433(13) 0.2571(9) 0.083(4) Uani d . 1 O
O20 0.2839(8) 0.5013(9) -0.1066(7) 0.0386(18) Uani d . 1 O
O21 0.5540(8) 0.8287(9) 0.0809(8) 0.0374(18) Uani d . 1 O
O22 0.2395(8) 0.8982(9) -0.0435(7) 0.0340(17) Uani d . 1 O
O23 0.5561(9) 1.1732(9) 0.2230(8) 0.0386(19) Uani d . 1 O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.8490 6.8722 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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
W1 Pt W3 . . 120.926(16) ?
W2 Pt W3 . . 60.384(15) ?
W1 Pt W2 . . 60.558(17) ?
W3 W1 Pt 2_666 . 60.372(17) ?
W3 W1 W2 2_666 . 120.538(17) ?
W1 W3 Pt 2_666 . 60.554(15) ?
Pt W1 W2 . . 60.182(16) ?
Pt W2 W3 . . 59.256(17) ?
O2 Pt O2 . 2_666 180.0000(10) ?
O2 Pt O1 . . 82.6(2) ?
O2 Pt O1 2_666 . 97.4(2) ?
O1 Pt O1 . 2_666 180.0000(10) ?
O2 Pt O3 . 2_666 97.4(2) ?
O2 Pt O3 2_666 2_666 82.6(2) ?
O1 Pt O3 . 2_666 82.1(2) ?
O1 Pt O3 2_666 2_666 97.9(2) ?
O2 Pt O3 . . 82.6(2) ?
O2 Pt O3 2_666 . 97.4(2) ?
O1 Pt O3 . . 97.9(2) ?
O1 Pt O3 2_666 . 82.1(2) ?
O3 Pt O3 2_666 . 180.0000(10) ?
O7 W1 O8 . . 104.4(3) ?
O7 W1 O6 . 2_666 102.2(3) ?
O8 W1 O6 . 2_666 94.5(3) ?
O7 W1 O4 . . 96.2(3) ?
O8 W1 O4 . . 99.1(3) ?
O6 W1 O4 2_666 . 153.6(3) ?
O7 W1 O1 . . 92.2(3) ?
O8 W1 O1 . . 161.7(3) ?
O6 W1 O1 2_666 . 73.9(2) ?
O4 W1 O1 . . 86.7(3) ?
O7 W1 O2 . . 161.6(3) ?
O8 W1 O2 . . 91.6(3) ?
O6 W1 O2 2_666 . 85.3(2) ?
O4 W1 O2 . . 71.9(2) ?
O1 W1 O2 . . 73.6(2) ?
O10 W2 O9 . . 105.1(3) ?
O10 W2 O4 . . 95.1(3) ?
O9 W2 O4 . . 101.0(3) ?
O10 W2 O5 . . 100.5(3) ?
O9 W2 O5 . . 97.0(3) ?
O4 W2 O5 . . 152.2(3) ?
O10 W2 O3 . . 93.1(3) ?
O9 W2 O3 . . 160.6(3) ?
O4 W2 O3 . . 83.5(2) ?
O5 W2 O3 . . 72.9(2) ?
O10 W2 O2 . . 161.8(3) ?
O9 W2 O2 . . 90.5(3) ?
O4 W2 O2 . . 72.2(2) ?
O5 W2 O2 . . 86.7(2) ?
O3 W2 O2 . . 72.8(2) ?
O12 W3 O11 . . 103.9(3) ?
O12 W3 O6 . . 100.4(3) ?
O11 W3 O6 . . 95.0(3) ?
O12 W3 O5 . . 94.8(3) ?
O11 W3 O5 . . 99.0(3) ?
O6 W3 O5 . . 156.2(3) ?
O12 W3 O1 . 2_666 92.3(3) ?
O11 W3 O1 . 2_666 161.8(3) ?
O6 W3 O1 . 2_666 73.6(2) ?
O5 W3 O1 . 2_666 87.6(2) ?
O12 W3 O3 . . 161.6(3) ?
O11 W3 O3 . . 91.8(3) ?
O6 W3 O3 . . 87.6(2) ?
O5 W3 O3 . . 72.9(2) ?
O1 W3 O3 2_666 . 73.8(2) ?
O12 W3 W2 . . 127.0(2) ?
O11 W3 W2 . . 89.9(2) ?
O6 W3 W2 . . 129.52(18) ?
O5 W3 W2 . . 32.18(18) ?
O1 W3 W2 2_666 . 86.81(16) ?
O3 W3 W2 . . 41.99(15) ?
W1 W3 W2 2_666 . 120.898(19) ?
Pt W3 W2 . . 60.360(16) ?
W1 O1 W3 . 2_666 96.3(2) yes
W2 O2 W1 . . 95.1(2) yes
W3 O3 W2 . . 96.1(2) yes
W2 O4 W1 . . 117.1(3) yes
W2 O5 W3 . . 115.6(3) yes
W1 O6 W3 2_666 . 112.3(3) yes
Pt O1 W1 . . 103.5(2) ?
Pt O1 W3 . 2_666 103.0(2) ?
Pt O2 W2 . . 102.1(2) ?
Pt O2 W1 . . 100.3(2) ?
Pt O2 O14 . . 114.5(3) ?
Pt O3 W3 . . 101.0(3) ?
Pt O3 W2 . . 102.5(2) ?
O8 Na1 O16 2_566 . 124.9(4) ?
O8 Na1 O14 2_566 . 141.2(3) ?
O16 Na1 O14 . . 88.3(4) ?
O8 Na1 O15 2_566 . 92.3(3) ?
O16 Na1 O15 . . 81.4(3) ?
O14 Na1 O15 . . 114.3(3) ?
O8 Na1 O13 2_566 . 80.5(3) ?
O16 Na1 O13 . . 79.3(4) ?
O14 Na1 O13 . . 87.6(3) ?
O15 Na1 O13 . . 150.2(4) ?
O8 Na1 O9 2_566 2_566 83.0(2) ?
O16 Na1 O9 . 2_566 145.7(4) ?
O14 Na1 O9 . 2_566 76.4(3) ?
O15 Na1 O9 . 2_566 77.5(3) ?
O13 Na1 O9 . 2_566 129.4(4) ?
O18 Na2 O12 . . 74.8(4) ?
O18 Na2 O17 . . 71.1(5) ?
O12 Na2 O17 . . 141.8(5) ?
O18 Na2 O16 . . 157.9(6) ?
O12 Na2 O16 . . 83.6(4) ?
O17 Na2 O16 . . 130.8(5) ?
O18 Na2 O19 . . 91.7(4) ?
O12 Na2 O19 . . 70.3(3) ?
O17 Na2 O19 . . 94.0(5) ?
O16 Na2 O19 . . 85.0(4) ?
O18 Na2 O13 . . 107.2(5) ?
O12 Na2 O13 . . 93.5(4) ?
O17 Na2 O13 . . 112.4(5) ?
O16 Na2 O13 . . 69.2(3) ?
O19 Na2 O13 . . 151.2(4) ?
O19 Na3 O20 . . 156.9(4) ?
O19 Na3 O21 . . 82.0(4) ?
O20 Na3 O21 . . 89.9(3) ?
O19 Na3 O12 . . 77.7(4) ?
O20 Na3 O12 . . 84.6(3) ?
O21 Na3 O12 . . 108.4(3) ?
O19 Na3 O18 . . 101.0(5) ?
O20 Na3 O18 . . 87.4(4) ?
O21 Na3 O18 . . 177.0(4) ?
O12 Na3 O18 . . 72.5(3) ?
O19 Na3 O22 . . 85.9(3) ?
O20 Na3 O22 . . 115.6(3) ?
O21 Na3 O22 . . 88.9(3) ?
O12 Na3 O22 . . 153.9(3) ?
O18 Na3 O22 . . 91.2(4) ?
O23 Na4 O23 2_675 . 180.0(4) ?
O23 Na4 O21 2_675 . 92.4(3) ?
O23 Na4 O21 . . 87.6(3) ?
O23 Na4 O21 2_675 2_675 87.6(3) ?
O23 Na4 O21 . 2_675 92.4(3) ?
O21 Na4 O21 . 2_675 180.0000(10) ?
O23 Na4 O22 2_675 2_675 92.7(3) ?
O23 Na4 O22 . 2_675 87.3(3) ?
O21 Na4 O22 . 2_675 92.1(3) ?
O21 Na4 O22 2_675 2_675 87.9(3) ?
O23 Na4 O22 2_675 . 87.3(3) ?
O23 Na4 O22 . . 92.7(3) ?
O21 Na4 O22 . . 87.9(3) ?
O21 Na4 O22 2_675 . 92.1(3) ?
O22 Na4 O22 2_675 . 180.0 ?
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
Pt W1 . 3.2789(5) ?
Pt W2 . 3.3099(8) ?
Pt W3 . 3.2730(9) ?
W1 W2 . 3.3222(9) ?
W1 W3 2_666 3.2300(9) ?
W2 W3 . 3.3107(6) ?
Pt O1 . 2.008(6) yes
Pt O2 . 2.008(6) yes
Pt O3 . 2.013(6) yes
W1 O1 . 2.166(6) yes
W1 O2 . 2.257(6) yes
W1 O4 . 1.949(6) yes
W1 O6 2_666 1.940(6) yes
W1 O7 . 1.737(7) yes
W1 O8 . 1.745(6) yes
W2 O2 . 2.244(6) yes
W2 O3 . 2.227(6) yes
W2 O4 . 1.945(6) yes
W2 O5 . 1.955(6) yes
W2 O9 . 1.740(6) yes
W2 O10 . 1.739(6) yes
W3 O1 2_666 2.170(6) yes
W3 O3 . 2.224(6) yes
W3 O5 . 1.958(6) yes
W3 O6 . 1.948(6) yes
W3 O11 . 1.757(6) yes
W3 O12 . 1.718(7) yes
Na1 Na2 . 3.760(10) yes
Na2 Na3 . 3.190(10) yes
Na3 Na4 . 3.498(4) yes
Na1 O8 2_566 2.372(8) yes
Na1 O9 2_566 2.544(8) yes
Na1 O13 . 2.470(10) yes
Na1 O14 . 2.420(9) yes
Na1 O15 . 2.450(10) yes
Na1 O16 . 2.406(9) yes
Na2 O12 . 2.388(11) yes
Na2 O13 . 2.85(2) yes
Na2 O16 . 2.62(2) yes
Na2 O17 . 2.49(2) yes
Na2 O18 . 2.35(2) yes
Na2 O19 . 2.83(2) yes
Na3 O12 . 2.424(8) yes
Na3 O18 . 2.440(10) yes
Na3 O19 . 2.400(10) yes
Na3 O20 . 2.399(9) yes
Na3 O21 . 2.423(9) yes
Na3 O22 . 2.435(9) yes
Na4 O21 . 2.439(8) yes
Na4 O22 . 2.465(7) yes
Na4 O23 . 2.418(8) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O13 O5 . 2.810(10) yes
O13 O14 2_566 2.99(2) yes
O13 O20 2_565 2.790(10) yes
O14 O2 . 2.671(9) yes
O14 O9 2_566 3.070(10) yes
O14 O23 2_676 2.730(10) yes
O15 O8 1_565 2.970(10) yes
O15 O17 2_576 2.79(2) yes
O15 O21 2_676 2.950(10) yes
O16 O1 2_666 2.840(10) yes
O16 O7 1_565 2.820(10) yes
O17 O10 1_565 3.10(2) yes
O17 O11 2_565 2.95(2) yes
O17 O15 2_576 2.79(2) yes
O17 O18 . 2.81(2) yes
O18 O5 2_565 2.890(10) yes
O18 O12 . 2.880(10) yes
O18 O18 2_565 2.79(3) yes
O19 O4 1_565 2.670(10) yes
O19 O7 2_666 2.800(10) yes
O19 O12 . 3.020(10) yes
O19 O23 . 3.01(2) yes
O20 O6 2_665 2.755(9) yes
O20 O11 . 2.940(10) yes
O20 O13 2_565 2.790(10) yes
O21 O11 2_665 2.800(10) yes
O21 O15 2_676 2.950(10) yes
O22 O9 2_565 2.920(10) yes
O22 O10 1_565 2.850(10) yes
O23 O3 1_565 2.661(9) yes
