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The crystal structure of a new potassium/hydro­nium tungstophosphate, potassium hydro­nium phosphate tungstate, K2.4(H3O)0.6PO4W12O36, obtained by hydro­thermal synthesis at low pH, has been determined by single-crystal X-ray diffraction. Regular PO4 tetrahedra are located on sites of \overline 43m symmetry. 12 W atoms are in a shell around the phosphate anion and are surrounded by O atoms in a distorted octahedral coordination. The close packing of the heteropoly­anionic units forms orthogonally intersecting channels where the statistically distributed potassium/hydro­nium ions are situated.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680401551X/wm6022sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680401551X/wm6022Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](P-O) = 0.010 Å
  • H-atom completeness 1%
  • Disorder in solvent or counterion
  • R factor = 0.038
  • wR factor = 0.091
  • Data-to-parameter ratio = 12.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O3 .. 2.65 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O3 .. 2.65 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O2 .. 2.82 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O2 .. 2.82 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O3 .. 2.81 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O3 .. 2.81 Ang.
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.124 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT127_ALERT_1_C Implicit Hall Symbol Inconsistent with Expl .... -P 4bc 2bc PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O5 PLAT430_ALERT_2_C Short Inter D...A Contact O1 .. O4 .. 2.89 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact O1 .. O4 .. 2.89 Ang. PLAT731_ALERT_1_C Bond Calc 1.897(7), Rep 1.897(3) ...... 2.33 su-Rat W1 -O1 1.555 35.665 PLAT731_ALERT_1_C Bond Calc 1.897(7), Rep 1.897(3) ...... 2.33 su-Rat W1 -O1 1.555 32.665 PLAT731_ALERT_1_C Bond Calc 1.897(7), Rep 1.897(3) ...... 2.33 su-Rat O1 -W1 1.555 35.665 PLAT731_ALERT_1_C Bond Calc 1.897(7), Rep 1.897(3) ...... 2.33 su-Rat O1 -W1 1.555 32.665
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:H1.62 K2.46 O40.54 P1 W12 Atom count from the _atom_site data: K2.46 O40.54 P1 W12 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 H1.62 K2.46 O40.54 P W12 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff H 3.24 0.00 3.24 K 4.92 4.92 0.00 O 81.08 81.08 0.00 P 2.00 2.00 0.00 W 24.00 24.00 0.00
0 ALERT level A = In general: serious problem 6 ALERT level B = Potentially serious problem 15 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 10 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996-2001); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
K2.4(H3O)0.6PO4W12O36Dx = 6.410 Mg m3
Mr = 2983.48Mo Kα radiation, λ = 0.71073 Å
Cubic, Pn3mCell parameters from 390 reflections
Hall symbol: -P 4bc 2bcθ = 3.6–27.9°
a = 11.5621 (8) ŵ = 44.97 mm1
V = 1545.65 (19) Å3T = 293 K
Z = 2Prism, colorless
F(000) = 25510.04 × 0.04 × 0.03 mm
Data collection top
Bruker SMART APEX 2000
diffractometer
390 independent reflections
Radiation source: fine-focus sealed tube360 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.125
φ and ω scansθmax = 28.3°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1414
Tmin = 0.173, Tmax = 0.217k = 1515
12441 measured reflectionsl = 1415
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038H-atom parameters not refined
wR(F2) = 0.092 w = 1/[σ2(Fo2) + (0.0408P)2 + 49.5098P]
where P = (Fo2 + 2Fc2)/3
S = 1.15(Δ/σ)max < 0.001
390 reflectionsΔρmax = 2.22 e Å3
31 parametersΔρmin = 2.74 e Å3
0 restraints
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*/UeqOcc. (<1)
W10.46708 (4)0.46708 (4)0.25851 (5)0.0101 (3)
P10.25000.25000.25000.016 (3)
O10.6521 (6)0.6521 (6)0.0044 (10)0.015 (2)
O20.0690 (7)0.0690 (7)0.7681 (9)0.015 (2)
O30.1228 (6)0.1228 (6)0.5380 (9)0.014 (2)
O40.3268 (9)0.3268 (9)0.3268 (9)0.010 (4)*
K10.25000.75000.75000.035 (4)0.82 (7)
O50.25000.75000.75000.035 (4)0.18 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.0103 (3)0.0103 (3)0.0098 (4)0.0021 (2)0.00013 (14)0.00013 (14)
P10.016 (3)0.016 (3)0.016 (3)0.0000.0000.000
O10.015 (3)0.015 (3)0.014 (5)0.004 (4)0.005 (3)0.005 (3)
O20.014 (3)0.014 (3)0.016 (6)0.008 (4)0.002 (3)0.002 (3)
O30.018 (3)0.018 (3)0.007 (5)0.007 (5)0.000 (3)0.000 (3)
K10.035 (7)0.036 (5)0.036 (5)0.0000.0000.000
O50.035 (7)0.036 (5)0.036 (5)0.0000.0000.000
Geometric parameters (Å, º) top
W1—O2i1.695 (11)O3—W1xiv1.907 (4)
W1—O1ii1.897 (3)O3—W1xv1.907 (4)
W1—O1iii1.897 (3)O3—K1xiii3.215 (10)
W1—O3iv1.907 (4)O4—W1xi2.426 (10)
W1—O3v1.907 (4)O4—W1xvi2.426 (10)
W1—O42.426 (10)K1—O2xvii2.966 (11)
W1—K1vi4.1243 (3)K1—O2vi2.966 (11)
W1—K1vii4.1243 (3)K1—O2xviii2.966 (11)
P1—O41.537 (18)K1—O2xix2.966 (11)
P1—O4viii1.537 (18)K1—O3vi3.215 (11)
P1—O4ix1.537 (18)K1—O3xvii3.215 (11)
P1—O4x1.537 (18)K1—O3xviii3.215 (11)
O1—W1ii1.897 (3)K1—O3xix3.215 (11)
O1—W1iii1.897 (3)K1—O1xvi3.260 (11)
O1—K1xi3.260 (11)K1—O1xx3.260 (11)
O2—W1xii1.695 (11)K1—O1xxi3.260 (11)
O2—K1xiii2.966 (11)K1—O1xxii3.260 (11)
O2i—W1—O1ii103.2 (4)O2xvii—K1—O3xvii53.7 (3)
O2i—W1—O1iii103.2 (4)O2vi—K1—O3xvii134.4 (3)
O1ii—W1—O1iii84.8 (7)O2xviii—K1—O3xvii86.91 (15)
O2i—W1—O3iv102.2 (4)O2xix—K1—O3xvii86.91 (15)
O1ii—W1—O3iv154.6 (4)O3vi—K1—O3xvii80.6 (3)
O1iii—W1—O3iv88.5 (5)O2xvii—K1—O3xviii86.91 (15)
O2i—W1—O3v102.2 (4)O2vi—K1—O3xviii86.91 (15)
O1ii—W1—O3v88.5 (5)O2xviii—K1—O3xviii53.7 (3)
O1iii—W1—O3v154.6 (4)O2xix—K1—O3xviii134.4 (3)
O3iv—W1—O3v87.2 (6)O3vi—K1—O3xviii125.5 (2)
O2i—W1—O4171.5 (5)O3xvii—K1—O3xviii125.5 (2)
O1ii—W1—O483.0 (4)O2xvii—K1—O3xix86.91 (15)
O1iii—W1—O483.0 (4)O2vi—K1—O3xix86.91 (15)
O3iv—W1—O471.9 (3)O2xviii—K1—O3xix134.4 (3)
O3v—W1—O471.9 (3)O2xix—K1—O3xix53.7 (3)
O2i—W1—K1vi82.375 (8)O3vi—K1—O3xix125.5 (2)
O1ii—W1—K1vi50.4 (3)O3xvii—K1—O3xix125.5 (2)
O1iii—W1—K1vi134.3 (3)O3xviii—K1—O3xix80.6 (3)
O3iv—W1—K1vi135.3 (3)O2xvii—K1—O1xvi56.5 (3)
O3v—W1—K1vi49.0 (3)O2vi—K1—O1xvi115.4 (3)
O4—W1—K1vi97.538 (11)O2xviii—K1—O1xvi93.53 (18)
O2i—W1—K1vii82.375 (8)O2xix—K1—O1xvi93.53 (18)
O1ii—W1—K1vii134.3 (3)O3vi—K1—O1xvi169.1 (3)
O1iii—W1—K1vii50.4 (3)O3xvii—K1—O1xvi110.3 (2)
O3iv—W1—K1vii49.0 (3)O3xviii—K1—O1xvi48.38 (15)
O3v—W1—K1vii135.3 (3)O3xix—K1—O1xvi48.38 (15)
O4—W1—K1vii97.538 (11)O2xvii—K1—O1xx93.53 (18)
K1vi—W1—K1vii164.750 (17)O2vi—K1—O1xx93.53 (18)
O4—P1—O4viii109.471 (2)O2xviii—K1—O1xx56.5 (3)
O4—P1—O4ix109.471 (3)O2xix—K1—O1xx115.4 (3)
O4viii—P1—O4ix109.471 (1)O3vi—K1—O1xx48.38 (15)
O4—P1—O4x109.5O3xvii—K1—O1xx48.38 (15)
O4viii—P1—O4x109.5O3xviii—K1—O1xx110.3 (2)
O4ix—P1—O4x109.471 (1)O3xix—K1—O1xx169.1 (3)
W1ii—O1—W1iii152.9 (7)O1xvi—K1—O1xx139.4 (2)
W1ii—O1—K1xi103.0 (3)O2xvii—K1—O1xxi93.53 (18)
W1iii—O1—K1xi103.0 (3)O2vi—K1—O1xxi93.53 (18)
W1xii—O2—K1xiii165.5 (5)O2xviii—K1—O1xxi115.4 (3)
W1xiv—O3—W1xv126.8 (5)O2xix—K1—O1xxi56.5 (3)
W1xiv—O3—K1xiii104.4 (3)O3vi—K1—O1xxi48.38 (15)
W1xv—O3—K1xiii104.4 (3)O3xvii—K1—O1xxi48.38 (15)
P1—O4—W1125.8 (3)O3xviii—K1—O1xxi169.1 (3)
P1—O4—W1xi125.8 (3)O3xix—K1—O1xxi110.3 (2)
W1—O4—W1xi89.3 (5)O1xvi—K1—O1xxi139.4 (2)
P1—O4—W1xvi125.8 (3)O1xx—K1—O1xxi58.8 (4)
W1—O4—W1xvi89.3 (5)O2xvii—K1—O1xxii115.4 (3)
W1xi—O4—W1xvi89.3 (5)O2vi—K1—O1xxii56.5 (3)
O2xvii—K1—O2vi171.9 (4)O2xviii—K1—O1xxii93.53 (18)
O2xvii—K1—O2xviii90.29 (3)O2xix—K1—O1xxii93.53 (18)
O2vi—K1—O2xviii90.29 (3)O3vi—K1—O1xxii110.3 (2)
O2xvii—K1—O2xix90.29 (3)O3xvii—K1—O1xxii169.1 (3)
O2vi—K1—O2xix90.29 (3)O3xviii—K1—O1xxii48.38 (15)
O2xviii—K1—O2xix171.9 (4)O3xix—K1—O1xxii48.38 (15)
O2xvii—K1—O3vi134.4 (3)O1xvi—K1—O1xxii58.8 (4)
O2vi—K1—O3vi53.7 (3)O1xx—K1—O1xxii139.4 (2)
O2xviii—K1—O3vi86.91 (15)O1xxi—K1—O1xxii139.4 (2)
O2xix—K1—O3vi86.91 (15)
Symmetry codes: (i) x+1/2, y+1/2, z+1; (ii) y+1, z+1/2, x1/2; (iii) z+1/2, x+1, y1/2; (iv) z, x+1/2, y+1/2; (v) y+1/2, z, x+1/2; (vi) z+1, x+1, y+1; (vii) x+1, y+1, z+1; (viii) x+1/2, y, z+1/2; (ix) x, y+1/2, z+1/2; (x) x+1/2, y+1/2, z; (xi) y, z, x; (xii) x1/2, y1/2, z+1; (xiii) y+1, z+1, x+1; (xiv) y+1/2, z+1/2, x; (xv) z+1/2, x+1/2, y; (xvi) z, x, y; (xvii) z+1, x+1/2, y+1/2; (xviii) z1/2, x+1, y+1/2; (xix) z1/2, x+1/2, y+1; (xx) z+1/2, x+3/2, y; (xxi) z+1/2, x, y+3/2; (xxii) z, x+3/2, y+3/2.
 

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