A diprotonated hexatungstoplatinate(IV), Na6[H2PtW6O24]·22H2O

Lee, U.; Joo, H.-C.; Park, K.-M.

doi:10.1107/S1600536804004970

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A diprotonated hexatungstoplatinate(IV), Na₆[H₂PtW₆O₂₄]·22H₂O

U. Lee, H.-C. Joo and K.-M. Park

The novel protonated hexasodium dihydrogen hexatungstoplatinate(IV) doicosahydrate, Na₆[H₂PtW₆O₂₄]·22H₂O, was crystallized in the triclinic system in space group P $\overline 1$ . The [H₂PtW₆O₂₄]^6- polyanion has C_i ( $\overline 1$ ) symmetry. The identification of the protonated O atom in the polyanion is difficult because it does not form interpolyanion hydrogen bonds, and a clear difference was not found in the W-O(H) bond lengths or the W-O(H)-W bond angles to indicate protonation of the O atom.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804004970/br6139sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536804004970/br6139Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (W-O) = 0.007 Å
H-atom completeness 1%
Disorder in solvent or counterion
R factor = 0.035
wR factor = 0.096
Data-to-parameter ratio = 17.8

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O13

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O14

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O15

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O16

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O17

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O18

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O19

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O20

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O21

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O22

Author Response: Explained in _publ_section_exptl_refinement

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O23

Author Response: Explained in _publ_section_exptl_refinement


Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact  O1     ..  O16     ..       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  O2     ..  O14     ..       2.67 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     ..  O23     ..       2.66 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     ..  O19     ..       2.67 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     ..  O13     ..       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  O6     ..  O20     ..       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  O7     ..  O19     ..       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  O7     ..  O16     ..       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  O11    ..  O21     ..       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  O13    ..  O20     ..       2.79 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  O14    ..  O23     ..       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  O15    ..  O17     ..       2.79 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  O17    ..  O18     ..       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  O18    ..  O18     ..       2.79 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                    1
           From the CIF: _chemical_formula_weight          2218.50
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           W       183.85    6.00 1103.10
           O        16.00   46.00  735.95
           H         1.01    0.00    0.00
           Pt      195.08    1.00  195.08
           Na       22.99    6.00  137.94
           Calculated formula weight             2172.07

Author Response: Because H atoms of H2O were not included.

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 ................    2218.50

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.

PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?

Author Response: Because H atoms of H2O were not included.

PLAT302_ALERT_4_C Anion/Solvent Disorder .........................       3.00 Perc.
PLAT430_ALERT_2_C Short Inter D...A Contact  O5     ..  O18     ..       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  O10    ..  O22     ..       2.85 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  O12    ..  O18     ..       2.88 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.  #          9
              O

Author Response: Because of groupping to related atoms.

PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #         12
              O

Author Response: Because of groupping to related atoms.


Alert level G
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:H46 Na6 O46 Pt1 W6
            Atom count from the _atom_site data:  Na6 O46 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    1
           From the CIF: _chemical_formula_sum  H46 Na6 O46 Pt W6
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           H         46.00      0.00   46.00
           Na         6.00      6.00    0.00
           O         46.00     46.00    0.00
           Pt         1.00      1.00    0.00
           W          6.00      6.00    0.00

  11 ALERT level A = In general: serious problem
  14 ALERT level B = Potentially serious problem
  12 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  30 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
   3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4 (Stoe & Cie, 1996); data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97-2 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97-2 (Sheldrick, 1997).

(I) top

Crystal data top

Na₆[H₂PtW₆O₂₄]·22H₂O	Z = 1
M_r = 2218.50	F(000) = 1002
Triclinic, P1	D_x = 3.440 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71069 Å
a = 10.028 (1) Å	Cell parameters from 27 reflections
b = 10.591 (1) Å	θ = 9.6–10.5°
c = 12.109 (3) Å	µ = 19.48 mm⁻¹
α = 113.13 (1)°	T = 298 K
β = 107.17 (1)°	Hexagonal prism, pale yellow
γ = 99.48 (1)°	0.26 × 0.13 × 0.10 mm
V = 1070.8 (3) Å³

Data collection top

Stoe Stadi-4 diffractometer	4223 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.000
Graphite monochromator	θ_max = 27.5°, θ_min = 2.0°
ω/2–θ scans	h = 0→13
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996)	k = −13→13
T_min = 0.051, T_max = 0.156	l = −15→14
4896 measured reflections	3 standard reflections every 60 min
4896 independent reflections	intensity decay: 3.7%

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	H-atom parameters not refined
R[F² > 2σ(F²)] = 0.035	w = 1/[σ2^(F_o2) + (0.0492P)2^{+ 10.2521P] where P = (F_o2} + 2F_c2^)/3
wR(F2^{) = 0.096}	(Δ/^σ^{)_max < 0.001}
S = 1.11	Δ^ρ^{_max = 2.62 e Å}−3
4896 reflections	Δ^ρ^{_min =}⁻^{2.18 e Å}−3
275 parameters	Extinction correction: SHELXL97, Fc*^{=kFc[1+0.001xFc2}λ3^/sin(2^θ^)]-1/4
0 restraints	Extinction coefficient: 0.0073 (2)
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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pt	0.5000	0.5000	0.5000	0.01087 (11)
W1	0.33879 (4)	0.25398 (4)	0.56051 (3)	0.01577 (11)
W2	0.18378 (3)	0.24979 (4)	0.27524 (3)	0.01620 (11)
W3	0.35661 (3)	0.49681 (4)	0.21816 (3)	0.01555 (11)
O1	0.5484 (6)	0.3639 (6)	0.5718 (6)	0.0154 (11)
O2	0.2980 (6)	0.4155 (6)	0.4870 (6)	0.0145 (11)
O3	0.4132 (7)	0.3558 (7)	0.3086 (6)	0.0164 (12)
O4	0.2786 (7)	0.1568 (7)	0.3713 (6)	0.0207 (13)
O5	0.1810 (7)	0.4127 (7)	0.2372 (6)	0.0191 (12)
O6	0.5666 (7)	0.5787 (7)	0.2672 (6)	0.0192 (12)
O7	0.4046 (7)	0.1226 (7)	0.5879 (7)	0.0277 (15)
O8	0.1655 (7)	0.2209 (8)	0.5668 (7)	0.0254 (14)
O9	0.0154 (7)	0.2248 (7)	0.2904 (7)	0.0244 (14)
O10	0.1492 (7)	0.1124 (7)	0.1216 (6)	0.0286 (15)
O11	0.3242 (7)	0.3612 (8)	0.0622 (6)	0.0257 (14)
O12	0.2935 (7)	0.6262 (8)	0.1880 (7)	0.0268 (14)
Na1	0.0692 (4)	0.7606 (5)	0.5278 (4)	0.0343 (9)
Na2	0.1244 (9)	0.7539 (10)	0.2315 (9)	0.0366 (19)	0.50
Na3	0.2998 (5)	0.7366 (5)	0.0474 (4)	0.0365 (10)
Na4	0.5000	1.0000	0.0000	0.0337 (13)
O13	−0.0149 (10)	0.5605 (12)	0.3040 (10)	0.069 (3)
O14	0.1830 (9)	0.6111 (9)	0.6065 (8)	0.0377 (18)
O15	0.1706 (9)	1.0201 (10)	0.6822 (9)	0.046 (2)
O16	0.2762 (11)	0.8203 (10)	0.4749 (12)	0.066 (3)
O17	−0.0453 (16)	0.8666 (14)	0.1383 (15)	0.092 (4)
O18	0.0423 (11)	0.6340 (17)	0.0027 (11)	0.086 (4)
O19	0.3787 (16)	0.9433 (13)	0.2571 (9)	0.083 (4)
O20	0.2839 (8)	0.5013 (9)	−0.1066 (7)	0.0386 (18)
O21	0.5540 (8)	0.8287 (9)	0.0809 (8)	0.0374 (18)
O22	0.2395 (8)	0.8982 (9)	−0.0435 (7)	0.0340 (17)
O23	0.5561 (9)	1.1732 (9)	0.2230 (8)	0.0386 (19)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt	0.0097 (2)	0.0108 (2)	0.0115 (2)	0.00414 (15)	0.00272 (16)	0.00544 (16)
W1	0.01467 (17)	0.01440 (18)	0.01787 (18)	0.00371 (13)	0.00488 (14)	0.00872 (14)
W2	0.01195 (17)	0.01535 (18)	0.01674 (18)	0.00270 (12)	0.00167 (13)	0.00680 (14)
W3	0.01353 (17)	0.01868 (19)	0.01336 (17)	0.00541 (13)	0.00341 (13)	0.00777 (14)
O1	0.015 (3)	0.012 (3)	0.019 (3)	0.007 (2)	0.005 (2)	0.007 (2)
O2	0.013 (3)	0.014 (3)	0.020 (3)	0.007 (2)	0.007 (2)	0.009 (2)
O3	0.018 (3)	0.017 (3)	0.013 (3)	0.004 (2)	0.003 (2)	0.009 (2)
O4	0.023 (3)	0.018 (3)	0.024 (3)	0.013 (3)	0.008 (3)	0.010 (3)
O5	0.017 (3)	0.026 (3)	0.022 (3)	0.011 (3)	0.010 (3)	0.016 (3)
O6	0.015 (3)	0.022 (3)	0.020 (3)	0.005 (2)	0.007 (2)	0.011 (3)
O7	0.025 (3)	0.025 (3)	0.037 (4)	0.010 (3)	0.008 (3)	0.019 (3)
O8	0.014 (3)	0.031 (4)	0.032 (4)	0.006 (3)	0.006 (3)	0.018 (3)
O9	0.013 (3)	0.029 (4)	0.033 (4)	0.007 (3)	0.007 (3)	0.017 (3)
O10	0.029 (4)	0.026 (4)	0.021 (3)	0.009 (3)	0.006 (3)	0.005 (3)
O11	0.024 (3)	0.029 (4)	0.020 (3)	0.007 (3)	0.008 (3)	0.008 (3)
O12	0.025 (3)	0.031 (4)	0.031 (4)	0.014 (3)	0.013 (3)	0.018 (3)
Na1	0.025 (2)	0.034 (2)	0.045 (2)	0.0125 (17)	0.0128 (19)	0.0191 (19)
Na2	0.030 (4)	0.049 (5)	0.034 (5)	0.020 (4)	0.011 (4)	0.021 (4)
Na3	0.034 (2)	0.040 (2)	0.037 (2)	0.0095 (19)	0.0115 (19)	0.023 (2)
Na4	0.032 (3)	0.026 (3)	0.035 (3)	0.007 (2)	0.011 (3)	0.009 (2)
O13	0.035 (5)	0.063 (7)	0.060 (6)	0.032 (5)	−0.006 (4)	−0.005 (5)
O14	0.040 (4)	0.036 (4)	0.039 (4)	0.022 (4)	0.016 (4)	0.016 (4)
O15	0.043 (5)	0.046 (5)	0.047 (5)	0.002 (4)	0.024 (4)	0.021 (4)
O16	0.059 (6)	0.033 (5)	0.121 (10)	0.015 (4)	0.066 (7)	0.027 (5)
O17	0.086 (9)	0.071 (9)	0.102 (10)	0.018 (7)	0.041 (8)	0.023 (7)
O18	0.035 (5)	0.163 (13)	0.062 (7)	0.012 (7)	0.007 (5)	0.070 (8)
O19	0.150 (12)	0.085 (8)	0.030 (5)	0.096 (9)	0.026 (6)	0.026 (5)
O20	0.032 (4)	0.056 (5)	0.033 (4)	0.017 (4)	0.017 (3)	0.022 (4)
O21	0.033 (4)	0.035 (4)	0.041 (4)	0.019 (3)	0.014 (4)	0.011 (3)
O22	0.027 (4)	0.040 (4)	0.033 (4)	0.015 (3)	0.012 (3)	0.014 (3)
O23	0.047 (5)	0.036 (4)	0.034 (4)	0.027 (4)	0.019 (4)	0.011 (3)

Geometric parameters (Å, º) top

Pt—W1	3.2789 (5)	W3—O12	1.718 (7)
Pt—W2	3.3099 (8)	Na1—Na2	3.76 (1)
Pt—W3	3.2730 (9)	Na2—Na3	3.19 (1)
W1—W2	3.3222 (9)	Na3—Na4	3.498 (4)
W1—W3ⁱ	3.2300 (9)	Na1—O8ⁱⁱ	2.372 (8)
W2—W3	3.3107 (6)	Na1—O9ⁱⁱ	2.544 (8)
Pt—O1	2.008 (6)	Na1—O13	2.47 (1)
Pt—O2	2.008 (6)	Na1—O14	2.420 (9)
Pt—O3	2.013 (6)	Na1—O15	2.45 (1)
W1—O1	2.166 (6)	Na1—O16	2.406 (9)
W1—O2	2.257 (6)	Na2—O12	2.388 (11)
W1—O4	1.949 (6)	Na2—O13	2.85 (2)
W1—O6ⁱ	1.940 (6)	Na2—O16	2.62 (2)
W1—O7	1.737 (7)	Na2—O17	2.49 (2)
W1—O8	1.745 (6)	Na2—O18	2.35 (2)
W2—O2	2.244 (6)	Na2—O19	2.83 (2)
W2—O3	2.227 (6)	Na3—O12	2.424 (8)
W2—O4	1.945 (6)	Na3—O18	2.44 (1)
W2—O5	1.955 (6)	Na3—O19	2.40 (1)
W2—O9	1.740 (6)	Na3—O20	2.399 (9)
W2—O10	1.739 (6)	Na3—O21	2.423 (9)
W3—O1ⁱ	2.170 (6)	Na3—O22	2.435 (9)
W3—O3	2.224 (6)	Na4—O21	2.439 (8)
W3—O5	1.958 (6)	Na4—O22	2.465 (7)
W3—O6	1.948 (6)	Na4—O23	2.418 (8)
W3—O11	1.757 (6)

W1—Pt—W3	120.926 (16)	W1—O1—W3ⁱ	96.3 (2)
W2—Pt—W3	60.384 (15)	W2—O2—W1	95.1 (2)
W1—Pt—W2	60.558 (17)	W3—O3—W2	96.1 (2)
W3ⁱ—W1—Pt	60.372 (17)	W2—O4—W1	117.1 (3)
W3ⁱ—W1—W2	120.538 (17)	W2—O5—W3	115.6 (3)
W1ⁱ—W3—Pt	60.554 (15)	W1ⁱ—O6—W3	112.3 (3)
Pt—W1—W2	60.182 (16)	Pt—O1—W1	103.5 (2)
Pt—W2—W3	59.256 (17)	Pt—O1—W3ⁱ	103.0 (2)
O2—Pt—O2ⁱ	180.000 (1)	Pt—O2—W2	102.1 (2)
O2—Pt—O1	82.6 (2)	Pt—O2—W1	100.3 (2)
O2ⁱ—Pt—O1	97.4 (2)	Pt—O2—O14	114.5 (3)
O1—Pt—O1ⁱ	180.000 (1)	Pt—O3—W3	101.0 (3)
O2—Pt—O3ⁱ	97.4 (2)	Pt—O3—W2	102.5 (2)
O2ⁱ—Pt—O3ⁱ	82.6 (2)	O8ⁱⁱ—Na1—O16	124.9 (4)
O1—Pt—O3ⁱ	82.1 (2)	O8ⁱⁱ—Na1—O14	141.2 (3)
O1ⁱ—Pt—O3ⁱ	97.9 (2)	O16—Na1—O14	88.3 (4)
O2—Pt—O3	82.6 (2)	O8ⁱⁱ—Na1—O15	92.3 (3)
O2ⁱ—Pt—O3	97.4 (2)	O16—Na1—O15	81.4 (3)
O1—Pt—O3	97.9 (2)	O14—Na1—O15	114.3 (3)
O1ⁱ—Pt—O3	82.1 (2)	O8ⁱⁱ—Na1—O13	80.5 (3)
O3ⁱ—Pt—O3	180.000 (1)	O16—Na1—O13	79.3 (4)
O7—W1—O8	104.4 (3)	O14—Na1—O13	87.6 (3)
O7—W1—O6ⁱ	102.2 (3)	O15—Na1—O13	150.2 (4)
O8—W1—O6ⁱ	94.5 (3)	O8ⁱⁱ—Na1—O9ⁱⁱ	83.0 (2)
O7—W1—O4	96.2 (3)	O16—Na1—O9ⁱⁱ	145.7 (4)
O8—W1—O4	99.1 (3)	O14—Na1—O9ⁱⁱ	76.4 (3)
O6ⁱ—W1—O4	153.6 (3)	O15—Na1—O9ⁱⁱ	77.5 (3)
O7—W1—O1	92.2 (3)	O13—Na1—O9ⁱⁱ	129.4 (4)
O8—W1—O1	161.7 (3)	O18—Na2—O12	74.8 (4)
O6ⁱ—W1—O1	73.9 (2)	O18—Na2—O17	71.1 (5)
O4—W1—O1	86.7 (3)	O12—Na2—O17	141.8 (5)
O7—W1—O2	161.6 (3)	O18—Na2—O16	157.9 (6)
O8—W1—O2	91.6 (3)	O12—Na2—O16	83.6 (4)
O6ⁱ—W1—O2	85.3 (2)	O17—Na2—O16	130.8 (5)
O4—W1—O2	71.9 (2)	O18—Na2—O19	91.7 (4)
O1—W1—O2	73.6 (2)	O12—Na2—O19	70.3 (3)
O10—W2—O9	105.1 (3)	O17—Na2—O19	94.0 (5)
O10—W2—O4	95.1 (3)	O16—Na2—O19	85.0 (4)
O9—W2—O4	101.0 (3)	O18—Na2—O13	107.2 (5)
O10—W2—O5	100.5 (3)	O12—Na2—O13	93.5 (4)
O9—W2—O5	97.0 (3)	O17—Na2—O13	112.4 (5)
O4—W2—O5	152.2 (3)	O16—Na2—O13	69.2 (3)
O10—W2—O3	93.1 (3)	O19—Na2—O13	151.2 (4)
O9—W2—O3	160.6 (3)	O19—Na3—O20	156.9 (4)
O4—W2—O3	83.5 (2)	O19—Na3—O21	82.0 (4)
O5—W2—O3	72.9 (2)	O20—Na3—O21	89.9 (3)
O10—W2—O2	161.8 (3)	O19—Na3—O12	77.7 (4)
O9—W2—O2	90.5 (3)	O20—Na3—O12	84.6 (3)
O4—W2—O2	72.2 (2)	O21—Na3—O12	108.4 (3)
O5—W2—O2	86.7 (2)	O19—Na3—O18	101.0 (5)
O3—W2—O2	72.8 (2)	O20—Na3—O18	87.4 (4)
O12—W3—O11	103.9 (3)	O21—Na3—O18	177.0 (4)
O12—W3—O6	100.4 (3)	O12—Na3—O18	72.5 (3)
O11—W3—O6	95.0 (3)	O19—Na3—O22	85.9 (3)
O12—W3—O5	94.8 (3)	O20—Na3—O22	115.6 (3)
O11—W3—O5	99.0 (3)	O21—Na3—O22	88.9 (3)
O6—W3—O5	156.2 (3)	O12—Na3—O22	153.9 (3)
O12—W3—O1ⁱ	92.3 (3)	O18—Na3—O22	91.2 (4)
O11—W3—O1ⁱ	161.8 (3)	O23ⁱⁱⁱ—Na4—O23	180.0 (4)
O6—W3—O1ⁱ	73.6 (2)	O23ⁱⁱⁱ—Na4—O21	92.4 (3)
O5—W3—O1ⁱ	87.6 (2)	O23—Na4—O21	87.6 (3)
O12—W3—O3	161.6 (3)	O23ⁱⁱⁱ—Na4—O21ⁱⁱⁱ	87.6 (3)
O11—W3—O3	91.8 (3)	O23—Na4—O21ⁱⁱⁱ	92.4 (3)
O6—W3—O3	87.6 (2)	O21—Na4—O21ⁱⁱⁱ	180.000 (1)
O5—W3—O3	72.9 (2)	O23ⁱⁱⁱ—Na4—O22ⁱⁱⁱ	92.7 (3)
O1ⁱ—W3—O3	73.8 (2)	O23—Na4—O22ⁱⁱⁱ	87.3 (3)
O12—W3—W2	127.0 (2)	O21—Na4—O22ⁱⁱⁱ	92.1 (3)
O11—W3—W2	89.9 (2)	O21ⁱⁱⁱ—Na4—O22ⁱⁱⁱ	87.9 (3)
O6—W3—W2	129.52 (18)	O23ⁱⁱⁱ—Na4—O22	87.3 (3)
O5—W3—W2	32.18 (18)	O23—Na4—O22	92.7 (3)
O1ⁱ—W3—W2	86.81 (16)	O21—Na4—O22	87.9 (3)
O3—W3—W2	41.99 (15)	O21ⁱⁱⁱ—Na4—O22	92.1 (3)
W1ⁱ—W3—W2	120.898 (19)	O22ⁱⁱⁱ—Na4—O22	180.0
Pt—W3—W2	60.360 (16)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+1; (iii) −x+1, −y+2, −z.

Hydrogen-bond geometry (Å) top

D—H···A	D···A
O13···O5	2.81 (1)
O13···O14ⁱⁱ	2.99 (2)
O13···O20^iv	2.79 (1)
O14···O2	2.671 (9)
O14···O9ⁱⁱ	3.07 (1)
O14···O23^v	2.73 (1)
O15···O8^vi	2.97 (1)
O15···O17^vii	2.79 (2)
O15···O21^v	2.95 (1)
O16···O1ⁱ	2.84 (1)
O16···O7^vi	2.82 (1)
O17···O10^vi	3.10 (2)
O17···O11^iv	2.95 (2)
O17···O15^vii	2.79 (2)
O17···O18	2.81 (2)
O18···O5^iv	2.89 (1)
O18···O12	2.88 (1)
O18···O18^iv	2.79 (3)
O19···O4^vi	2.67 (1)
O19···O7ⁱ	2.80 (1)
O19···O12	3.02 (1)
O19···O23	3.01 (2)
O20···O6^viii	2.755 (9)
O20···O11	2.94 (1)
O20···O13^iv	2.79 (1)
O21···O11^viii	2.80 (1)
O21···O15^v	2.95 (1)
O22···O9^iv	2.92 (1)
O22···O10^vi	2.85 (1)
O23···O3^vi	2.661 (9)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+1; (iv) −x, −y+1, −z; (v) −x+1, −y+2, −z+1; (vi) x, y+1, z; (vii) −x, −y+2, −z+1; (viii) −x+1, −y+1, −z.

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