Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680401551X/wm6022sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680401551X/wm6022Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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.
K2.4(H3O)0.6PO4W12O36 | Dx = 6.410 Mg m−3 |
Mr = 2983.48 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, Pn3m | Cell parameters from 390 reflections |
Hall symbol: -P 4bc 2bc | θ = 3.6–27.9° |
a = 11.5621 (8) Å | µ = 44.97 mm−1 |
V = 1545.65 (19) Å3 | T = 293 K |
Z = 2 | Prism, colorless |
F(000) = 2551 | 0.04 × 0.04 × 0.03 mm |
Bruker SMART APEX 2000 diffractometer | 390 independent reflections |
Radiation source: fine-focus sealed tube | 360 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.125 |
φ and ω scans | θmax = 28.3°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→14 |
Tmin = 0.173, Tmax = 0.217 | k = −15→15 |
12441 measured reflections | l = −14→15 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.038 | H-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 reflections | Δρmax = 2.22 e Å−3 |
31 parameters | Δρmin = −2.74 e Å−3 |
0 restraints |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
W1 | 0.46708 (4) | 0.46708 (4) | 0.25851 (5) | 0.0101 (3) | |
P1 | 0.2500 | 0.2500 | 0.2500 | 0.016 (3) | |
O1 | 0.6521 (6) | 0.6521 (6) | 0.0044 (10) | 0.015 (2) | |
O2 | 0.0690 (7) | 0.0690 (7) | 0.7681 (9) | 0.015 (2) | |
O3 | 0.1228 (6) | 0.1228 (6) | 0.5380 (9) | 0.014 (2) | |
O4 | 0.3268 (9) | 0.3268 (9) | 0.3268 (9) | 0.010 (4)* | |
K1 | 0.2500 | 0.7500 | 0.7500 | 0.035 (4) | 0.82 (7) |
O5 | 0.2500 | 0.7500 | 0.7500 | 0.035 (4) | 0.18 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
W1 | 0.0103 (3) | 0.0103 (3) | 0.0098 (4) | −0.0021 (2) | −0.00013 (14) | −0.00013 (14) |
P1 | 0.016 (3) | 0.016 (3) | 0.016 (3) | 0.000 | 0.000 | 0.000 |
O1 | 0.015 (3) | 0.015 (3) | 0.014 (5) | 0.004 (4) | 0.005 (3) | 0.005 (3) |
O2 | 0.014 (3) | 0.014 (3) | 0.016 (6) | −0.008 (4) | 0.002 (3) | 0.002 (3) |
O3 | 0.018 (3) | 0.018 (3) | 0.007 (5) | −0.007 (5) | 0.000 (3) | 0.000 (3) |
K1 | 0.035 (7) | 0.036 (5) | 0.036 (5) | 0.000 | 0.000 | 0.000 |
O5 | 0.035 (7) | 0.036 (5) | 0.036 (5) | 0.000 | 0.000 | 0.000 |
W1—O2i | 1.695 (11) | O3—W1xiv | 1.907 (4) |
W1—O1ii | 1.897 (3) | O3—W1xv | 1.907 (4) |
W1—O1iii | 1.897 (3) | O3—K1xiii | 3.215 (10) |
W1—O3iv | 1.907 (4) | O4—W1xi | 2.426 (10) |
W1—O3v | 1.907 (4) | O4—W1xvi | 2.426 (10) |
W1—O4 | 2.426 (10) | K1—O2xvii | 2.966 (11) |
W1—K1vi | 4.1243 (3) | K1—O2vi | 2.966 (11) |
W1—K1vii | 4.1243 (3) | K1—O2xviii | 2.966 (11) |
P1—O4 | 1.537 (18) | K1—O2xix | 2.966 (11) |
P1—O4viii | 1.537 (18) | K1—O3vi | 3.215 (11) |
P1—O4ix | 1.537 (18) | K1—O3xvii | 3.215 (11) |
P1—O4x | 1.537 (18) | K1—O3xviii | 3.215 (11) |
O1—W1ii | 1.897 (3) | K1—O3xix | 3.215 (11) |
O1—W1iii | 1.897 (3) | K1—O1xvi | 3.260 (11) |
O1—K1xi | 3.260 (11) | K1—O1xx | 3.260 (11) |
O2—W1xii | 1.695 (11) | K1—O1xxi | 3.260 (11) |
O2—K1xiii | 2.966 (11) | K1—O1xxii | 3.260 (11) |
O2i—W1—O1ii | 103.2 (4) | O2xvii—K1—O3xvii | 53.7 (3) |
O2i—W1—O1iii | 103.2 (4) | O2vi—K1—O3xvii | 134.4 (3) |
O1ii—W1—O1iii | 84.8 (7) | O2xviii—K1—O3xvii | 86.91 (15) |
O2i—W1—O3iv | 102.2 (4) | O2xix—K1—O3xvii | 86.91 (15) |
O1ii—W1—O3iv | 154.6 (4) | O3vi—K1—O3xvii | 80.6 (3) |
O1iii—W1—O3iv | 88.5 (5) | O2xvii—K1—O3xviii | 86.91 (15) |
O2i—W1—O3v | 102.2 (4) | O2vi—K1—O3xviii | 86.91 (15) |
O1ii—W1—O3v | 88.5 (5) | O2xviii—K1—O3xviii | 53.7 (3) |
O1iii—W1—O3v | 154.6 (4) | O2xix—K1—O3xviii | 134.4 (3) |
O3iv—W1—O3v | 87.2 (6) | O3vi—K1—O3xviii | 125.5 (2) |
O2i—W1—O4 | 171.5 (5) | O3xvii—K1—O3xviii | 125.5 (2) |
O1ii—W1—O4 | 83.0 (4) | O2xvii—K1—O3xix | 86.91 (15) |
O1iii—W1—O4 | 83.0 (4) | O2vi—K1—O3xix | 86.91 (15) |
O3iv—W1—O4 | 71.9 (3) | O2xviii—K1—O3xix | 134.4 (3) |
O3v—W1—O4 | 71.9 (3) | O2xix—K1—O3xix | 53.7 (3) |
O2i—W1—K1vi | 82.375 (8) | O3vi—K1—O3xix | 125.5 (2) |
O1ii—W1—K1vi | 50.4 (3) | O3xvii—K1—O3xix | 125.5 (2) |
O1iii—W1—K1vi | 134.3 (3) | O3xviii—K1—O3xix | 80.6 (3) |
O3iv—W1—K1vi | 135.3 (3) | O2xvii—K1—O1xvi | 56.5 (3) |
O3v—W1—K1vi | 49.0 (3) | O2vi—K1—O1xvi | 115.4 (3) |
O4—W1—K1vi | 97.538 (11) | O2xviii—K1—O1xvi | 93.53 (18) |
O2i—W1—K1vii | 82.375 (8) | O2xix—K1—O1xvi | 93.53 (18) |
O1ii—W1—K1vii | 134.3 (3) | O3vi—K1—O1xvi | 169.1 (3) |
O1iii—W1—K1vii | 50.4 (3) | O3xvii—K1—O1xvi | 110.3 (2) |
O3iv—W1—K1vii | 49.0 (3) | O3xviii—K1—O1xvi | 48.38 (15) |
O3v—W1—K1vii | 135.3 (3) | O3xix—K1—O1xvi | 48.38 (15) |
O4—W1—K1vii | 97.538 (11) | O2xvii—K1—O1xx | 93.53 (18) |
K1vi—W1—K1vii | 164.750 (17) | O2vi—K1—O1xx | 93.53 (18) |
O4—P1—O4viii | 109.471 (2) | O2xviii—K1—O1xx | 56.5 (3) |
O4—P1—O4ix | 109.471 (3) | O2xix—K1—O1xx | 115.4 (3) |
O4viii—P1—O4ix | 109.471 (1) | O3vi—K1—O1xx | 48.38 (15) |
O4—P1—O4x | 109.5 | O3xvii—K1—O1xx | 48.38 (15) |
O4viii—P1—O4x | 109.5 | O3xviii—K1—O1xx | 110.3 (2) |
O4ix—P1—O4x | 109.471 (1) | O3xix—K1—O1xx | 169.1 (3) |
W1ii—O1—W1iii | 152.9 (7) | O1xvi—K1—O1xx | 139.4 (2) |
W1ii—O1—K1xi | 103.0 (3) | O2xvii—K1—O1xxi | 93.53 (18) |
W1iii—O1—K1xi | 103.0 (3) | O2vi—K1—O1xxi | 93.53 (18) |
W1xii—O2—K1xiii | 165.5 (5) | O2xviii—K1—O1xxi | 115.4 (3) |
W1xiv—O3—W1xv | 126.8 (5) | O2xix—K1—O1xxi | 56.5 (3) |
W1xiv—O3—K1xiii | 104.4 (3) | O3vi—K1—O1xxi | 48.38 (15) |
W1xv—O3—K1xiii | 104.4 (3) | O3xvii—K1—O1xxi | 48.38 (15) |
P1—O4—W1 | 125.8 (3) | O3xviii—K1—O1xxi | 169.1 (3) |
P1—O4—W1xi | 125.8 (3) | O3xix—K1—O1xxi | 110.3 (2) |
W1—O4—W1xi | 89.3 (5) | O1xvi—K1—O1xxi | 139.4 (2) |
P1—O4—W1xvi | 125.8 (3) | O1xx—K1—O1xxi | 58.8 (4) |
W1—O4—W1xvi | 89.3 (5) | O2xvii—K1—O1xxii | 115.4 (3) |
W1xi—O4—W1xvi | 89.3 (5) | O2vi—K1—O1xxii | 56.5 (3) |
O2xvii—K1—O2vi | 171.9 (4) | O2xviii—K1—O1xxii | 93.53 (18) |
O2xvii—K1—O2xviii | 90.29 (3) | O2xix—K1—O1xxii | 93.53 (18) |
O2vi—K1—O2xviii | 90.29 (3) | O3vi—K1—O1xxii | 110.3 (2) |
O2xvii—K1—O2xix | 90.29 (3) | O3xvii—K1—O1xxii | 169.1 (3) |
O2vi—K1—O2xix | 90.29 (3) | O3xviii—K1—O1xxii | 48.38 (15) |
O2xviii—K1—O2xix | 171.9 (4) | O3xix—K1—O1xxii | 48.38 (15) |
O2xvii—K1—O3vi | 134.4 (3) | O1xvi—K1—O1xxii | 58.8 (4) |
O2vi—K1—O3vi | 53.7 (3) | O1xx—K1—O1xxii | 139.4 (2) |
O2xviii—K1—O3vi | 86.91 (15) | O1xxi—K1—O1xxii | 139.4 (2) |
O2xix—K1—O3vi | 86.91 (15) |
Symmetry codes: (i) x+1/2, y+1/2, −z+1; (ii) −y+1, z+1/2, x−1/2; (iii) z+1/2, −x+1, y−1/2; (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) x−1/2, y−1/2, −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) z−1/2, −x+1, y+1/2; (xix) z−1/2, 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. |