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The novel protonated hemiundecasodium hemipenta­hydrogen hexatungstoplatinate(IV) heptadecahydrate, Na5.5[H2.5PtW6O24]·17H2O, crystallizes in the triclinic system in space group P\overline 1. The protonated O atoms were identified by considering three factors: inter-polyanion hydrogen bonds, elongation of W-O(H) bond distances, and bond angles of W-O(H)-W. The [H2.5(PtW6O24)]5.5- polyanion has no inversion symmetry, and it forms a dimer, viz. [H5(PtW6O24)2]11-, via five strong hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804002302/wm6009sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804002302/wm6009Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](W-O) = 0.008 Å
  • H-atom completeness 1%
  • R factor = 0.039
  • wR factor = 0.098
  • Data-to-parameter ratio = 17.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O25
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O26
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O27
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O28
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O29
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O30
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O31
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O32
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O33
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O34
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O35
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O36
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O37
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O38
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O39
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O40
Author Response: Explained in _publ_section_exptl_refinement
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O41
Author Response: Explained in _publ_section_exptl_refinement

Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O1 = 2.60 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O2     ..  O32      =       2.80 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O3     ..  O14      =       2.56 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O4     ..  O33      =       2.82 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O5     ..  O15      =       2.60 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O6     ..  O30      =       2.73 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O7     ..  O28      =       2.83 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O8     ..  O25      =       2.82 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O9     ..  O34      =       2.82 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O10    ..  O35      =       2.81 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O10    ..  O36      =       2.83 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O11    ..  O41      =       2.77 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O13    ..  O27      =       2.69 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O21    ..  O26      =       2.84 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O24    ..  O41      =       2.80 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O26    ..  O31      =       2.80 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O27    ..  O41      =       2.76 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O27    ..  O37      =       2.80 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O30    ..  O41      =       2.83 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O32    ..  O36      =       2.81 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_B Short Inter D...A Contact  O33    ..  O34      =       2.80 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.

Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 2117.43 TEST: Calculate formula weight from _atom_site_* atom mass num sum H 1.01 0.00 0.00 Na 22.99 5.50 126.44 Pt 195.08 1.00 195.08 W 183.85 6.00 1103.10 O 16.00 41.00 655.96 Calculated formula weight 2080.58 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
Author Response: Because H atoms of H2O were not included.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
Author Response: Because H atoms of H2O were not included.:
PLAT043_ALERT_1_C Check Reported Molecular Weight ................    2117.43
Author Response: Because H atoms of H2O were not included.
PLAT044_ALERT_1_C Calculated and Reported Dx Differ ..............          ?
Author Response: Because H atoms of H2O were not included.
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
Author Response: Because H atoms of H2O were not included.
PLAT430_ALERT_2_C Short Inter D...A Contact  O19    ..  O26      =       2.89 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT430_ALERT_2_C Short Inter D...A Contact  O24    ..  O31      =       2.90 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          4
              O
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          7
              O
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          8
              O
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          9
              O
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         10
              O
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         11
              O
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         15
              O
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         17
              O
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         20
              Na
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         21
              Na
Author Response: Because of groupping to related atoms.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         22
              Na
Author Response: Because of groupping to related atoms.

Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: H36.5 Na5.5 O41 Pt1 W6 Atom count from _chemical_formula_moiety:H36.5 Na5.5 O41 Pt1 W65 FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:H36.5 Na5.5 O41 Pt1 W6 Atom count from the _atom_site data: Na5.5 O41 Pt1 W6 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum H36.50 Na5.50 O41 Pt W6 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff H 73.00 0.00 73.00 Na 11.00 11.00 0.00 O 82.00 82.00 0.00 Pt 2.00 2.00 0.00 W 12.00 12.00 0.00
17 ALERT level A = In general: serious problem 21 ALERT level B = Potentially serious problem 20 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 42 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 11 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: STADI4 (Stoe & Coe, 1996); cell refinement: STADI4; data reduction: X-RED (STOE, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
Na5.5[H2.5PtW6O24](H2O)17]Z = 2
Mr = 2117.43F(000) = 1967
Triclinic, P1Dx = 3.785 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 10.736 (2) ÅCell parameters from 30 reflections
b = 12.803 (3) Åθ = 9.5–10.5°
c = 14.877 (3) ŵ = 22.43 mm1
α = 105.50 (3)°T = 298 K
β = 105.13 (3)°Triclinic, pale yellow
γ = 97.43 (3)°0.30 × 0.25 × 0.24 mm
V = 1858.1 (9) Å3
Data collection top
Stoe Stadi-4
diffractometer
7210 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 27.5°, θmin = 1.7°
ω/2θ scansh = 013
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1996)
k = 1616
Tmin = 0.005, Tmax = 0.010l = 1918
8526 measured reflections3 standard reflections every 60 min
8526 independent reflections intensity decay: 3.5%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullH-atom parameters not refined
R[F2 > 2σ(F2)] = 0.039 w = 1/[σ2(Fo2) + (0.042P)2 + 22.4365P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.098(Δ/σ)max = 0.001
S = 1.13Δρmax = 1.89 e Å3
8526 reflectionsΔρmin = 2.38 e Å3
485 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00196 (5)
Primary atom site location: structure-invariant direct methods
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pt0.53177 (3)0.63934 (3)0.19396 (2)0.01129 (9)
W10.36598 (4)0.38366 (3)0.12171 (3)0.01673 (10)
W20.23581 (4)0.57111 (3)0.03140 (3)0.01545 (10)
W30.39646 (4)0.82623 (3)0.11042 (3)0.01574 (10)
W40.68999 (4)0.90412 (3)0.29045 (3)0.01498 (10)
W50.81131 (4)0.72228 (3)0.38136 (3)0.01662 (10)
W60.64513 (4)0.45429 (3)0.29557 (3)0.01810 (10)
Na10.9679 (7)0.3308 (6)0.2866 (5)0.0588 (17)
Na21.1374 (5)0.6005 (4)0.3672 (4)0.0339 (11)
Na31.2834 (5)0.8758 (4)0.4486 (3)0.0347 (11)
Na41.1614 (8)0.9366 (10)0.2435 (5)0.092 (3)
Na51.00001.00000.00000.102 (5)
Na60.6471 (5)1.0511 (4)0.0975 (4)0.0415 (13)
O10.4369 (7)0.5191 (6)0.0644 (5)0.0152 (13)
O20.3617 (6)0.6889 (6)0.1682 (5)0.0140 (13)
O30.5885 (7)0.7630 (6)0.1426 (5)0.0162 (14)
O40.6228 (7)0.7577 (6)0.3235 (5)0.0150 (13)
O50.7028 (7)0.5885 (5)0.2258 (5)0.0141 (13)
O60.4734 (7)0.5227 (6)0.2484 (5)0.0178 (14)
O70.2291 (7)0.4688 (6)0.1056 (5)0.0177 (14)
O80.3245 (8)0.6930 (6)0.0012 (5)0.0230 (16)
O90.5065 (7)0.9080 (6)0.2446 (5)0.0182 (14)
O100.8360 (7)0.8270 (6)0.3089 (5)0.0185 (15)
O110.7105 (7)0.5968 (6)0.3980 (5)0.0178 (14)
O120.5452 (8)0.3609 (6)0.1633 (6)0.0242 (16)
O130.2935 (9)0.3086 (7)0.1839 (6)0.0286 (18)
O140.3209 (8)0.2907 (7)0.0023 (6)0.0265 (17)
O150.1908 (8)0.4777 (6)0.0885 (5)0.0236 (16)
O160.0945 (7)0.6179 (7)0.0403 (6)0.0258 (17)
O170.2549 (8)0.8732 (6)0.1204 (6)0.0238 (16)
O180.4644 (8)0.9031 (6)0.0468 (6)0.0254 (17)
O190.7564 (8)0.9812 (7)0.2249 (6)0.0276 (17)
O200.7245 (8)0.9943 (6)0.4067 (6)0.0274 (17)
O210.8523 (9)0.8128 (7)0.4990 (6)0.0289 (18)
O220.9538 (8)0.6742 (7)0.3755 (7)0.0315 (19)
O230.7940 (9)0.4162 (7)0.2964 (7)0.034 (2)
O240.5830 (9)0.3808 (7)0.3637 (6)0.0323 (19)
O250.8137 (10)0.2156 (8)0.1400 (8)0.048 (3)
O260.9144 (9)0.1930 (7)0.3596 (7)0.037 (2)
O271.1494 (16)0.2316 (14)0.2846 (11)0.092 (5)
O281.0415 (9)0.4652 (8)0.2085 (7)0.038 (2)
O291.0884 (12)0.4576 (9)0.4445 (8)0.054 (3)
O301.3557 (9)0.5721 (8)0.3922 (7)0.038 (2)
O311.2492 (10)0.7337 (8)0.5287 (7)0.038 (2)
O321.2049 (9)0.7390 (8)0.2911 (6)0.035 (2)
O331.4869 (10)0.8070 (8)0.4632 (7)0.041 (2)
O341.3742 (10)1.0077 (9)0.3741 (9)0.052 (3)
O351.0953 (8)0.9555 (7)0.3831 (6)0.0329 (19)
O360.9662 (10)0.7575 (9)0.1681 (8)0.049 (3)
O371.0069 (15)1.0182 (14)0.1657 (11)0.083 (4)
O381.0083 (13)1.1993 (12)0.0359 (10)0.073 (4)
O390.7485 (12)0.9397 (9)0.0179 (8)0.054 (3)
O400.5149 (16)1.1390 (10)0.1937 (11)0.089 (5)
O410.3661 (12)0.3701 (10)0.4343 (8)0.055 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt0.01289 (17)0.01005 (16)0.00966 (16)0.00129 (13)0.00292 (13)0.00215 (12)
W10.0203 (2)0.01261 (18)0.01477 (19)0.00064 (15)0.00584 (15)0.00185 (15)
W20.01495 (19)0.01546 (19)0.01234 (18)0.00012 (14)0.00307 (14)0.00125 (14)
W30.0167 (2)0.01366 (19)0.01556 (19)0.00221 (15)0.00228 (15)0.00568 (15)
W40.0170 (2)0.01145 (18)0.01356 (18)0.00074 (14)0.00223 (14)0.00275 (14)
W50.0157 (2)0.01604 (19)0.01526 (19)0.00286 (15)0.00078 (15)0.00449 (15)
W60.0203 (2)0.01458 (19)0.0190 (2)0.00452 (15)0.00367 (16)0.00663 (15)
Na10.054 (4)0.054 (4)0.060 (4)0.003 (3)0.011 (3)0.015 (3)
Na20.029 (3)0.036 (3)0.034 (3)0.009 (2)0.009 (2)0.007 (2)
Na30.044 (3)0.036 (3)0.021 (2)0.011 (2)0.011 (2)0.003 (2)
Na40.068 (5)0.190 (10)0.047 (4)0.068 (6)0.031 (4)0.052 (5)
Na50.149 (13)0.068 (8)0.074 (8)0.017 (8)0.052 (9)0.000 (6)
Na60.039 (3)0.039 (3)0.039 (3)0.007 (2)0.004 (2)0.025 (2)
O10.014 (3)0.016 (3)0.012 (3)0.000 (3)0.002 (3)0.002 (3)
O20.008 (3)0.017 (3)0.013 (3)0.001 (3)0.001 (2)0.004 (3)
O30.025 (4)0.017 (3)0.010 (3)0.004 (3)0.009 (3)0.006 (3)
O40.017 (3)0.017 (3)0.008 (3)0.002 (3)0.004 (3)0.001 (3)
O50.019 (3)0.013 (3)0.010 (3)0.003 (3)0.005 (3)0.003 (3)
O60.019 (4)0.019 (3)0.017 (3)0.003 (3)0.007 (3)0.007 (3)
O70.017 (3)0.021 (4)0.015 (3)0.001 (3)0.006 (3)0.007 (3)
O80.027 (4)0.019 (4)0.020 (4)0.003 (3)0.006 (3)0.005 (3)
O90.016 (3)0.015 (3)0.021 (4)0.003 (3)0.005 (3)0.002 (3)
O100.010 (3)0.018 (3)0.021 (4)0.004 (3)0.004 (3)0.007 (3)
O110.017 (3)0.017 (3)0.014 (3)0.001 (3)0.001 (3)0.004 (3)
O120.031 (4)0.011 (3)0.024 (4)0.007 (3)0.005 (3)0.002 (3)
O130.034 (5)0.023 (4)0.036 (5)0.004 (3)0.017 (4)0.017 (4)
O140.028 (4)0.028 (4)0.024 (4)0.003 (3)0.007 (3)0.010 (3)
O150.023 (4)0.023 (4)0.016 (4)0.000 (3)0.002 (3)0.001 (3)
O160.020 (4)0.029 (4)0.031 (4)0.006 (3)0.007 (3)0.014 (4)
O170.020 (4)0.024 (4)0.027 (4)0.008 (3)0.003 (3)0.010 (3)
O180.027 (4)0.019 (4)0.028 (4)0.001 (3)0.007 (3)0.007 (3)
O190.031 (4)0.030 (4)0.026 (4)0.001 (3)0.013 (3)0.012 (3)
O200.035 (5)0.021 (4)0.018 (4)0.009 (3)0.001 (3)0.000 (3)
O210.035 (5)0.025 (4)0.022 (4)0.008 (4)0.002 (3)0.005 (3)
O220.021 (4)0.035 (5)0.043 (5)0.011 (4)0.009 (4)0.019 (4)
O230.030 (5)0.031 (5)0.043 (5)0.015 (4)0.011 (4)0.013 (4)
O240.037 (5)0.031 (5)0.035 (5)0.006 (4)0.010 (4)0.021 (4)
O250.045 (6)0.042 (6)0.047 (6)0.004 (5)0.006 (5)0.022 (5)
O260.039 (5)0.031 (5)0.036 (5)0.008 (4)0.002 (4)0.010 (4)
O270.086 (11)0.099 (12)0.077 (10)0.021 (9)0.044 (9)0.005 (9)
O280.039 (5)0.046 (6)0.035 (5)0.011 (4)0.017 (4)0.017 (4)
O290.075 (8)0.051 (6)0.036 (6)0.005 (6)0.015 (5)0.019 (5)
O300.035 (5)0.053 (6)0.040 (5)0.021 (4)0.022 (4)0.021 (5)
O310.048 (6)0.044 (5)0.033 (5)0.022 (5)0.021 (4)0.018 (4)
O320.041 (5)0.039 (5)0.027 (4)0.013 (4)0.018 (4)0.005 (4)
O330.039 (5)0.048 (6)0.036 (5)0.008 (5)0.021 (4)0.006 (4)
O340.036 (6)0.056 (7)0.061 (7)0.004 (5)0.025 (5)0.008 (5)
O350.020 (4)0.034 (5)0.034 (5)0.000 (4)0.003 (3)0.002 (4)
O360.043 (6)0.046 (6)0.047 (6)0.007 (5)0.007 (5)0.004 (5)
O370.075 (9)0.126 (13)0.075 (9)0.046 (9)0.031 (8)0.056 (9)
O380.061 (8)0.092 (10)0.077 (9)0.014 (7)0.020 (7)0.047 (8)
O390.068 (8)0.037 (6)0.048 (6)0.015 (5)0.003 (6)0.013 (5)
O400.120 (13)0.030 (6)0.091 (11)0.024 (7)0.007 (10)0.001 (7)
O410.058 (7)0.068 (8)0.040 (6)0.007 (6)0.020 (5)0.017 (5)
Geometric parameters (Å, º) top
Pt—W13.264 (1)W6—O62.174 (7)
Pt—W23.2939 (9)W6—O111.942 (7)
Pt—W33.305 (1)W6—O121.939 (8)
Pt—W43.328 (2)W6—O231.729 (8)
Pt—W53.3366 (9)W6—O241.749 (8)
Pt—W63.329 (1)Na1—Na23.420 (8)
W1—W23.336 (1)Na1—Na6i4.355 (9)
W1—W63.239 (2)Na2—Na33.412 (7)
W2—W33.234 (1)Na3—Na43.328 (9)
W3—W43.384 (2)Na4—Na53.931 (8)
W4—W53.239 (1)Na5—Na64.460 (6)
W5—W63.387 (2)Na6—Na6ii3.50 (1)
Pt—O12.026 (7)Na1—O232.30 (1)
Pt—O21.987 (7)Na1—O252.33 (1)
Pt—O32.025 (7)Na1—O262.39 (1)
Pt—O42.009 (6)Na1—O272.46 (2)
Pt—O52.010 (7)Na1—O282.48 (1)
Pt—O61.988 (7)Na1—O292.38 (1)
W1—O12.259 (7)Na2—O222.31 (1)
W1—O62.143 (7)Na2—O282.39 (1)
W1—O71.943 (7)Na2—O292.48 (1)
W1—O121.946 (8)Na2—O302.37 (1)
W1—O131.745 (7)Na2—O312.43 (1)
W1—O141.755 (8)Na2—O322.47 (1)
W2—O12.311 (7)Na3—O20iii2.372 (9)
W2—O22.154 (7)Na3—O312.47 (1)
W2—O71.931 (7)Na3—O322.38 (1)
W2—O81.959 (7)Na3—O332.44 (1)
W2—O151.763 (7)Na3—O352.47 (1)
W2—O161.725 (8)Na3—O342.48 (1)
W3—O22.185 (7)Na4—O17iv2.32 (1)
W3—O32.293 (7)Na4—O322.86 (1)
W3—O81.933 (7)Na4—O342.45 (2)
W3—O91.952 (7)Na4—O352.33 (1)
W3—O171.733 (8)Na4—O362.66 (2)
W3—O181.751 (8)Na4—O372.30 (2)
W4—O32.325 (7)Na5—O37v2.39 (1)
W4—O42.145 (7)Na5—O372.39 (1)
W4—O91.921 (7)Na5—O382.45 (2)
W4—O101.956 (7)Na5—O38v2.45 (2)
W4—O191.769 (8)Na5—O39v2.63 (1)
W4—O201.717 (7)Na5—O392.63 (1)
W5—O42.140 (7)Na6—O182.348 (9)
W5—O52.368 (7)Na6—O18ii2.43 (1)
W5—O101.965 (7)Na6—O192.41 (1)
W5—O111.928 (7)Na6—O25vi2.40 (1)
W5—O211.726 (8)Na6—O402.44 (2)
W5—O221.735 (8)Na6—O392.50 (1)
W6—O52.330 (7)
W1—O1—W293.8 (2)O23—W6—O1296.9 (4)
W2—O2—W396.4 (3)O24—W6—O12100.5 (4)
W3—O3—W494.3 (3)O23—W6—O1199.1 (4)
W5—O4—W498.2 (3)O24—W6—O1197.2 (4)
W6—O5—W592.3 (2)O12—W6—O11152.4 (3)
W1—O6—W697.2 (3)O23—W6—O6157.6 (4)
W2—O7—W1118.9 (3)O24—W6—O697.6 (3)
W3—O8—W2112.4 (4)O12—W6—O672.9 (3)
W4—O9—W3121.8 (4)O11—W6—O684.1 (3)
W4—O10—W5111.4 (3)O23—W6—O588.4 (4)
W5—O11—W6122.2 (4)O24—W6—O5164.7 (3)
W6—O12—W1113.0 (4)O12—W6—O586.7 (3)
W1—Pt—W261.15 (3)O11—W6—O571.5 (3)
W1—Pt—W3119.79 (3)O6—W6—O571.5 (2)
W2—Pt—W358.68 (3)Na2—Na1—Na6i154.7 (2)
W1—Pt—W4173.46 (2)Na3—Na2—Na1175.4 (2)
W2—Pt—W4119.86 (4)Na4—Na3—Na298.7 (3)
W3—Pt—W461.35 (3)Na3—Na4—Na5177.2 (3)
W1—Pt—W658.85 (3)Na4v—Na5—Na690.7 (1)
W2—Pt—W6119.78 (3)Na4—Na5—Na689.3 (1)
W3—Pt—W6173.11 (2)Na6ii—Na6—Na5112.1 (2)
W4—Pt—W6119.14 (3)O23—Na1—O2582.1 (4)
W1—Pt—W5119.84 (4)O23—Na1—O2987.3 (5)
W2—Pt—W5172.14 (2)O25—Na1—O29168.8 (5)
W3—Pt—W5119.39 (3)O23—Na1—O2697.7 (4)
W4—Pt—W558.16 (3)O25—Na1—O2687.6 (4)
W6—Pt—W561.08 (3)O29—Na1—O2690.2 (4)
W6—W1—W2121.21 (3)O23—Na1—O27175.6 (5)
W3—W2—W1119.77 (3)O25—Na1—O2798.4 (5)
W2—W3—W4119.95 (4)O29—Na1—O2791.8 (5)
W5—W4—W3119.93 (3)O26—Na1—O2777.9 (5)
W4—W5—W6120.02 (3)O23—Na1—O2887.8 (4)
W1—W6—W5119.06 (4)O25—Na1—O2892.9 (4)
O2—Pt—O695.6 (3)O29—Na1—O2890.4 (4)
O2—Pt—O496.3 (3)O26—Na1—O28174.5 (5)
O6—Pt—O496.5 (3)O27—Na1—O2896.6 (5)
O2—Pt—O5177.4 (3)O23—Na1—Na281.5 (3)
O6—Pt—O582.4 (3)O22—Na2—O30164.2 (4)
O4—Pt—O582.3 (3)O22—Na2—O2897.7 (4)
O2—Pt—O382.9 (3)O30—Na2—O2897.1 (4)
O6—Pt—O3177.5 (3)O22—Na2—O3186.3 (4)
O4—Pt—O381.7 (3)O30—Na2—O3178.9 (4)
O5—Pt—O399.1 (3)O28—Na2—O31176.0 (4)
O2—Pt—O183.0 (3)O22—Na2—O3289.1 (3)
O6—Pt—O182.6 (3)O30—Na2—O3285.5 (4)
O4—Pt—O1178.8 (3)O28—Na2—O3290.1 (3)
O5—Pt—O198.3 (3)O31—Na2—O3289.9 (3)
O3—Pt—O199.1 (3)O22—Na2—O2995.7 (4)
O13—W1—O14103.4 (4)O30—Na2—O2989.7 (4)
O13—W1—O793.8 (3)O28—Na2—O2990.0 (4)
O14—W1—O799.9 (3)O31—Na2—O2989.7 (4)
O13—W1—O1299.2 (4)O32—Na2—O29175.1 (4)
O14—W1—O1296.3 (3)O20iii—Na3—O32158.5 (4)
O7—W1—O12156.2 (3)O20iii—Na3—O33115.3 (4)
O13—W1—O696.0 (3)O32—Na3—O3384.8 (4)
O14—W1—O6159.3 (3)O20iii—Na3—O3186.3 (3)
O7—W1—O685.5 (3)O32—Na3—O3191.2 (4)
O12—W1—O673.4 (3)O33—Na3—O3177.9 (4)
O13—W1—O1163.8 (3)O20iii—Na3—O3578.4 (3)
O14—W1—O188.5 (3)O32—Na3—O3584.3 (3)
O7—W1—O173.1 (3)O33—Na3—O35159.9 (4)
O12—W1—O190.2 (3)O31—Na3—O35119.1 (4)
O6—W1—O174.0 (2)O20iii—Na3—O3498.8 (4)
O16—W2—O15104.8 (4)O32—Na3—O3488.9 (4)
O16—W2—O798.1 (3)O33—Na3—O3487.6 (4)
O15—W2—O7100.6 (3)O31—Na3—O34165.5 (4)
O16—W2—O899.2 (3)O35—Na3—O3475.3 (4)
O15—W2—O894.1 (3)O37—Na4—O17iv100.0 (5)
O7—W2—O8153.5 (3)O37—Na4—O3597.0 (5)
O16—W2—O294.8 (3)O17iv—Na4—O35161.7 (6)
O15—W2—O2158.3 (3)O37—Na4—O34134.2 (7)
O7—W2—O285.4 (3)O17iv—Na4—O3494.3 (4)
O8—W2—O273.4 (3)O35—Na4—O3478.5 (4)
O16—W2—O1164.6 (3)O37—Na4—O3683.8 (6)
O15—W2—O188.9 (3)O17iv—Na4—O3691.7 (5)
O7—W2—O172.1 (3)O35—Na4—O3683.2 (4)
O8—W2—O186.4 (3)O34—Na4—O36139.2 (5)
O2—W2—O173.0 (2)O37—Na4—O32144.8 (7)
O17—W3—O18105.5 (4)O17iv—Na4—O3285.2 (4)
O17—W3—O8101.5 (4)O35—Na4—O3276.9 (4)
O18—W3—O894.8 (3)O34—Na4—O3279.3 (4)
O17—W3—O996.3 (3)O36—Na4—O3261.1 (4)
O18—W3—O9100.0 (3)O37v—Na5—O37180.00 (7)
O8—W3—O9152.9 (3)O37v—Na5—O3891.1 (5)
O17—W3—O296.0 (3)O37—Na5—O3888.9 (5)
O18—W3—O2157.2 (3)O37v—Na5—O38v88.9 (5)
O8—W3—O273.1 (3)O37—Na5—O38v91.1 (5)
O9—W3—O284.9 (3)O38—Na5—O38v180.000 (1)
O17—W3—O3163.2 (3)O37v—Na5—O39v77.9 (4)
O18—W3—O387.8 (3)O37—Na5—O39v102.1 (4)
O8—W3—O387.2 (3)O38—Na5—O39v83.0 (4)
O9—W3—O370.9 (3)O38v—Na5—O39v97.0 (4)
O2—W3—O372.7 (2)O37v—Na5—O39102.1 (4)
O20—W4—O19105.7 (4)O37—Na5—O3977.9 (4)
O20—W4—O997.3 (4)O38—Na5—O3997.0 (4)
O19—W4—O9100.6 (4)O38v—Na5—O3983.0 (4)
O20—W4—O10100.9 (3)O39v—Na5—O39180.0 (5)
O19—W4—O1093.6 (4)O18—Na6—O25vi172.4 (4)
O9—W4—O10153.0 (3)O18—Na6—O1989.9 (3)
O20—W4—O496.1 (3)O25vi—Na6—O1996.9 (4)
O19—W4—O4156.2 (3)O18—Na6—O18ii85.9 (3)
O9—W4—O485.9 (3)O25vi—Na6—O18ii87.6 (3)
O10—W4—O472.5 (3)O19—Na6—O18ii172.0 (4)
O20—W4—O3163.4 (3)O18—Na6—O4080.8 (4)
O19—W4—O388.2 (3)O25vi—Na6—O4095.6 (5)
O9—W4—O370.7 (3)O19—Na6—O4092.6 (4)
O10—W4—O387.1 (3)O18ii—Na6—O4093.5 (4)
O4—W4—O372.2 (2)O18—Na6—O3990.5 (4)
O21—W5—O22104.7 (4)O25vi—Na6—O3992.7 (4)
O21—W5—O1198.8 (4)O19—Na6—O3990.5 (4)
O22—W5—O11100.0 (4)O18ii—Na6—O3982.7 (4)
O21—W5—O10100.6 (4)O40—Na6—O39170.8 (5)
O22—W5—O1094.7 (4)Pt—O1—W199.1 (3)
O11—W5—O10151.8 (3)Pt—O1—W298.6 (3)
O21—W5—O498.0 (3)Pt—O2—W2105.3 (3)
O22—W5—O4155.7 (4)Pt—O2—W3104.7 (3)
O11—W5—O484.7 (3)Pt—O3—W399.7 (3)
O10—W5—O472.5 (3)Pt—O3—W499.6 (3)
O21—W5—O5165.6 (3)Pt—O4—W5107.0 (3)
O22—W5—O587.3 (4)Pt—O4—W4106.4 (3)
O11—W5—O570.8 (3)Pt—O5—W699.9 (3)
O10—W5—O586.1 (3)Pt—O5—W599.0 (3)
O4—W5—O571.6 (2)Pt—O6—W1104.4 (3)
O23—W6—O24103.9 (4)Pt—O6—W6106.1 (3)
Symmetry codes: (i) x, y1, z; (ii) x+1, y+2, z; (iii) x+2, y+2, z+1; (iv) x+1, y, z; (v) x+2, y+2, z; (vi) x, y+1, z.
Hydrogen-bond geometry (Å) top
D—H···AD···A
O1···O1vii2.60 (1)
O3···O14vii2.56 (1)
O5···O15vii2.60 (1)
O25···O8vii2.82 (1)
O25···O233.04 (2)
O25···O38i2.90 (2)
O26···O19i2.90 (1)
O26···O21viii2.84 (1)
O26···O273.05 (2)
O26···O31viii2.80 (1)
O27···O13iv2.68 (2)
O27···O37i2.80 (2)
O27···O41iv2.76 (2)
O28···O7iv2.83 (1)
O28···O15vii2.96 (1)
O29···O11viii3.04 (1)
O29···O29viii2.95 (2)
O30···O6iv2.73 (1)
O30···O313.05 (1)
O30···O332.93 (1)
O30···O41iv2.83 (1)
O31···O24viii2.90 (1)
O31···O333.08 (1)
O32···O2iv2.80 (1)
O32···O362.81 (2)
O33···O4iv2.82 (1)
O33···O34ix2.80 (2)
O34···O9iv2.82 (1)
O34···O353.03 (1)
O35···O102.81 (1)
O35···O20iii3.06 (1)
O35···O21iii2.91 (1)
O36···O102.83 (1)
O36···O15vii3.01 (1)
O36···O16iv2.98 (1)
O37···O193.06 (2)
O38···O16ii3.07 (2)
O38···O17ii3.00 (2)
O39···O14vii3.03 (1)
O40···O12vi2.98 (2)
Symmetry codes: (i) x, y1, z; (ii) x+1, y+2, z; (iii) x+2, y+2, z+1; (iv) x+1, y, z; (vi) x, y+1, z; (vii) x+1, y+1, z; (viii) x+2, y+1, z+1; (ix) x+3, y+2, z+1.
 

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