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The title compound, K2[H6PtMo6O24]·6H2O, containing the hexa­molybdoplatinate(IV) polyanion with the highest level of protonation, was isolated at pH 1.60. The anion has the Pt atom at an inversion center and exhibits a local symmetry close to \overline{3}m. Four O atoms of the central PtO6 octa­hedron and two O atoms of the edge-shared MoO6 octa­hedron are protonated. One K+ ion and one O atom of a water mol­ecule are located on twofold axes; the positions of a second K+ ion and one water mol­ecule, both on general sites, are half-occupied.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806046125/wm2064sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806046125/wm2064Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](o-O) = 0.005 Å
  • H-atom completeness 78%
  • Disorder in solvent or counterion
  • R factor = 0.033
  • wR factor = 0.081
  • Data-to-parameter ratio = 14.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O16W
Author Response: Explained in _publ_section_exptl_refinement

Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
Author Response: Because H atoms of H2O(O16w) were not included.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
Author Response: Because H atoms of H2O(O16w) were not included.
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
Author Response: Because H atoms of H2O(O16w) were not included.
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       2.69 Ratio
Author Response: Explained in _publ_section_exptl_refinement.
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.67 Ratio
Author Response: Explained in _publ_section_exptl_refinement.
PLAT245_ALERT_2_C U(iso) H14B    Smaller than U(eq) O14W    by ...       0.02 AngSq
Author Response: Explained in _publ_section_exptl_refinement.
PLAT245_ALERT_2_C U(iso) H13     Smaller than U(eq) O13W    by ...       0.01 AngSq
Author Response: Explained in _publ_section_exptl_refinement.
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      17.00 Perc.
Author Response: I think no problem. Explained in the comment.

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:H18 K2 Mo6 O30 Pt1 Atom count from the _atom_site data: H14 K2 Mo6 O30 Pt1 ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR) is > 2.00 Tmin and Tmax reported: 0.229 0.376 Tmin and Tmax expected: 0.042 0.366 RR = 5.354 Please check that your absorption correction is appropriate. 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 4 From the CIF: _chemical_formula_sum H18 K2 Mo6 O30 Pt TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff H 72.00 56.00 16.00 K 8.00 8.00 0.00 Mo 24.00 24.00 0.00 O 120.00 120.00 0.00 Pt 4.00 4.00 0.00
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); 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.

Dipotassium hexahydrogen hexamolybdoplatinate(IV) hexahydrate top
Crystal data top
K2[H6PtMo6O24]·6H2OF(000) = 2504
Mr = 1347.07Dx = 3.356 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2ycCell parameters from 30 reflections
a = 21.178 (3) Åθ = 9.5–10.4°
b = 12.940 (2) ŵ = 8.38 mm1
c = 10.110 (2) ÅT = 298 K
β = 105.77 (1)°Hexagonal block, pale yellow
V = 2666.3 (8) Å30.42 × 0.36 × 0.12 mm
Z = 4
Data collection top
Stoe Stadi-4
diffractometer
2608 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.010
Graphite monochromatorθmax = 27.5°, θmin = 1.9°
ω/2θ scansh = 2726
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1996)
k = 016
Tmin = 0.229, Tmax = 0.376l = 013
3078 measured reflections3 standard reflections every 60 min
3056 independent reflections intensity decay: 3.2%
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)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H atoms treated by a mixture of independent and constrained refinement
S = 1.16 w = 1/[σ2(Fo2) + (0.0368P)2 + 9.1413P]
where P = (Fo2 + 2Fc2)/3
3056 reflections(Δ/σ)max < 0.001
210 parametersΔρmax = 0.97 e Å3
8 restraintsΔρmin = 1.27 e Å3
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)
Pt0.25000.25000.00000.01349 (9)
Mo10.40336 (3)0.34274 (4)0.06449 (6)0.02157 (14)
Mo20.34798 (3)0.26249 (4)0.32760 (6)0.01849 (13)
Mo30.19606 (3)0.16989 (4)0.26248 (6)0.01903 (13)
K10.50000.62888 (19)0.25000.0426 (6)
K20.4913 (2)0.0638 (3)0.5596 (5)0.0566 (12)0.50
O1C0.3295 (2)0.2475 (3)0.0723 (5)0.0187 (9)
O2C0.3026 (2)0.3565 (3)0.1270 (5)0.0186 (9)
H20.284 (4)0.416 (5)0.131 (9)0.03 (2)*
O3C0.2827 (2)0.1571 (3)0.1616 (4)0.0160 (9)
H30.298 (4)0.096 (5)0.130 (8)0.03 (2)*
O4B0.3522 (3)0.4257 (4)0.1024 (5)0.0261 (11)
H40.361 (7)0.486 (7)0.103 (14)0.11 (5)*
O5B0.4045 (2)0.2459 (3)0.2076 (5)0.0216 (10)
O6B0.2581 (2)0.2735 (4)0.3417 (5)0.0231 (10)
O7T0.4670 (3)0.3023 (5)0.0061 (6)0.0430 (14)
O8T0.4277 (3)0.4548 (4)0.1523 (6)0.0377 (14)
O9T0.3787 (3)0.3731 (4)0.4121 (5)0.0281 (11)
O10T0.3775 (3)0.1636 (4)0.4370 (5)0.0298 (12)
O11T0.2256 (3)0.0603 (4)0.3558 (5)0.0305 (12)
O12T0.1295 (3)0.2088 (4)0.3103 (5)0.0313 (12)
O13W0.50000.0853 (8)0.25000.064 (3)
H130.477 (5)0.120 (7)0.273 (12)0.05 (3)*
O14W0.6168 (5)0.0610 (6)0.5963 (9)0.068 (2)
H14A0.626 (7)0.131 (7)0.575 (13)0.098*
H14B0.587 (5)0.086 (8)0.616 (12)0.050*
O15W0.4892 (7)0.1583 (9)0.6918 (13)0.055 (4)0.50
H15A0.50640.22080.66170.082*0.50
H15B0.44280.17130.67900.082*0.50
O16W0.3233 (3)0.0263 (4)0.1255 (6)0.0439 (15)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt0.01563 (16)0.01233 (15)0.01243 (16)0.00035 (12)0.00369 (12)0.00013 (11)
Mo10.0183 (3)0.0239 (3)0.0210 (3)0.0040 (2)0.0028 (2)0.0030 (2)
Mo20.0229 (3)0.0161 (3)0.0147 (3)0.0011 (2)0.0021 (2)0.00053 (19)
Mo30.0220 (3)0.0196 (3)0.0166 (3)0.0013 (2)0.0072 (2)0.0029 (2)
K10.0304 (13)0.0294 (12)0.072 (2)0.0000.0213 (13)0.000
K20.042 (2)0.053 (2)0.064 (3)0.0027 (19)0.004 (2)0.007 (2)
O1C0.016 (2)0.019 (2)0.021 (2)0.0012 (17)0.0055 (18)0.0020 (17)
O2C0.021 (2)0.0119 (19)0.021 (2)0.0014 (17)0.0015 (19)0.0028 (17)
O3C0.021 (2)0.014 (2)0.012 (2)0.0010 (17)0.0030 (17)0.0017 (16)
O4B0.032 (3)0.022 (2)0.019 (2)0.009 (2)0.001 (2)0.0025 (19)
O5B0.019 (2)0.021 (2)0.023 (2)0.0008 (18)0.0020 (19)0.0019 (18)
O6B0.028 (3)0.024 (2)0.018 (2)0.0044 (19)0.008 (2)0.0049 (18)
O7T0.026 (3)0.058 (4)0.047 (4)0.001 (3)0.014 (3)0.010 (3)
O8T0.040 (3)0.028 (3)0.037 (3)0.016 (2)0.004 (3)0.006 (2)
O9T0.030 (3)0.022 (2)0.027 (3)0.002 (2)0.002 (2)0.004 (2)
O10T0.036 (3)0.026 (2)0.024 (3)0.005 (2)0.003 (2)0.005 (2)
O11T0.037 (3)0.024 (2)0.029 (3)0.006 (2)0.007 (2)0.009 (2)
O12T0.030 (3)0.038 (3)0.028 (3)0.001 (2)0.012 (2)0.000 (2)
O13W0.040 (6)0.033 (5)0.109 (10)0.0000.001 (6)0.000
O14W0.094 (7)0.037 (4)0.071 (5)0.019 (4)0.022 (5)0.006 (4)
O15W0.056 (9)0.048 (7)0.050 (8)0.017 (6)0.004 (7)0.002 (6)
O16W0.057 (4)0.035 (3)0.035 (3)0.011 (3)0.004 (3)0.004 (2)
Geometric parameters (Å, º) top
Mo1—Mo23.3503 (10)Mo3—O12T1.688 (5)
Mo1—Mo3i3.4065 (10)K1—O7Tii2.994 (6)
Mo2—Mo33.3269 (9)K1—O7Tiii2.994 (6)
Pt—O1C2.010 (4)K1—O8T2.751 (5)
Pt—O2C2.003 (4)K1—O8Tiv2.751 (5)
Pt—O3C1.995 (4)K1—O15Wv2.813 (13)
Pt—O3Ci1.995 (4)K1—O15Wvi2.813 (13)
Pt—O2Ci2.003 (4)K1—O12Tvii2.837 (5)
Pt—O1Ci2.010 (4)K1—O12Tviii2.837 (5)
Mo1—O1C2.169 (4)K2—O10T2.719 (7)
Mo1—O2C2.391 (5)K2—O7Tiv3.325 (8)
Mo1—O4B2.044 (5)K2—O13W3.198 (5)
Mo1—O5B1.909 (5)K2—O13Wix2.696 (9)
Mo1—O7T1.696 (6)K2—O14W2.583 (11)
Mo1—O8T1.706 (5)K2—O14Wix2.894 (10)
Mo2—O2C2.336 (5)K2—O15W1.820 (14)
Mo2—O3C2.308 (4)K2—O15Wx2.723 (14)
Mo2—O5B1.934 (5)O2C—H20.86 (7)
Mo2—O6B1.953 (5)O3C—H30.93 (6)
Mo2—O9T1.702 (5)O4B—H40.81 (8)
Mo2—O10T1.695 (5)O13W—H130.75 (7)
Mo3—O1Ci2.137 (4)O14W—H14A0.96 (8)
Mo3—O3C2.335 (5)O14W—H14B0.78 (7)
Mo3—O4Bi2.073 (5)O15W—H15A0.9700
Mo3—O6B1.895 (5)O15W—H15B0.9700
Mo3—O11T1.724 (5)
Mo3i—O1C—Mo1104.58 (18)O6B—Mo2—O2C81.16 (18)
Mo2—O2C—Mo190.27 (16)O3C—Mo2—O2C69.69 (15)
Mo2—O3C—Mo391.55 (15)O12T—Mo3—O11T107.2 (3)
Mo1—O4B—Mo3i111.7 (2)O12T—Mo3—O6B101.8 (2)
Mo1—O5B—Mo2121.3 (2)O11T—Mo3—O6B104.1 (2)
Mo3—O6B—Mo2119.7 (2)O12T—Mo3—O4Bi97.4 (2)
Pt—O1C—Mo3i106.7 (2)O11T—Mo3—O4Bi88.0 (2)
Pt—O1C—Mo1106.8 (2)O6B—Mo3—O4Bi152.9 (2)
Pt—O2C—Mo2102.93 (18)O12T—Mo3—O1Ci94.7 (2)
Pt—O2C—Mo199.22 (18)O11T—Mo3—O1Ci150.4 (2)
Pt—O3C—Mo2104.20 (17)O6B—Mo3—O1Ci90.18 (19)
Pt—O3C—Mo3100.13 (19)O4Bi—Mo3—O1Ci69.25 (18)
H14A—O14W—H14B83 (10)O12T—Mo3—O3C164.5 (2)
O15Wx—O15W—H15B104.1O11T—Mo3—O3C88.2 (2)
H15A—O15W—H15B105.5O6B—Mo3—O3C72.43 (18)
Mo3—Mo2—Mo1118.87 (2)O4Bi—Mo3—O3C84.05 (19)
Mo2—Mo1—Mo3i119.88 (2)O1Ci—Mo3—O3C71.31 (16)
O3C—Pt—O3Ci180.0 (3)O8T—K1—O8Tiv70.1 (2)
O3C—Pt—O2Ci96.84 (18)O8T—K1—O15Wv151.9 (3)
O3Ci—Pt—O2Ci83.16 (18)O8Tiv—K1—O15Wv136.1 (3)
O3C—Pt—O2C83.16 (18)O8T—K1—O15Wvi136.1 (3)
O3Ci—Pt—O2C96.84 (18)O8Tiv—K1—O15Wvi151.9 (3)
O2Ci—Pt—O2C180.0 (4)O15Wv—K1—O15Wvi23.4 (5)
O3C—Pt—O1C98.60 (18)O8T—K1—O12Tvii141.86 (18)
O3Ci—Pt—O1C81.40 (18)O8Tiv—K1—O12Tvii79.05 (17)
O2Ci—Pt—O1C97.51 (19)O15Wv—K1—O12Tvii65.1 (3)
O2C—Pt—O1C82.49 (19)O8T—K1—O7Tii99.85 (18)
O3C—Pt—O1Ci81.40 (18)O8Tiv—K1—O7Tii108.43 (18)
O3Ci—Pt—O1Ci98.60 (18)O15Wv—K1—O7Tii82.2 (3)
O2Ci—Pt—O1Ci82.49 (19)O15Wvi—K1—O7Tii63.4 (3)
O2C—Pt—O1Ci97.51 (19)O15Wv—K1—O7Tiii63.4 (3)
O1C—Pt—O1Ci180.00 (9)O15Wvi—K1—O7Tiii82.2 (3)
O7T—Mo1—O8T106.7 (3)O15W—K2—O14W97.7 (6)
O7T—Mo1—O5B102.3 (3)K2ix—K2—O14W75.0 (3)
O8T—Mo1—O5B102.9 (2)O15W—K2—O13Wix88.1 (5)
O7T—Mo1—O4B99.6 (3)O14W—K2—O13Wix91.1 (2)
O8T—Mo1—O4B90.0 (2)O15W—K2—O10T79.7 (5)
O5B—Mo1—O4B149.9 (2)O14W—K2—O10T145.4 (3)
O7T—Mo1—O1C96.1 (2)O13Wix—K2—O10T123.1 (2)
O8T—Mo1—O1C151.5 (2)O15W—K2—O15Wx18.0 (5)
O5B—Mo1—O1C88.19 (18)O14W—K2—O15Wx89.0 (4)
O4B—Mo1—O1C69.13 (18)O13Wix—K2—O15Wx72.5 (3)
O7T—Mo1—O2C165.1 (2)O10T—K2—O15Wx95.8 (4)
O8T—Mo1—O2C87.9 (2)O15W—K2—O14Wix127.0 (6)
O5B—Mo1—O2C71.16 (18)O14W—K2—O14Wix134.5 (2)
O4B—Mo1—O2C82.45 (19)O15W—K2—O13W132.8 (5)
O1C—Mo1—O2C70.74 (16)O14W—K2—O13W79.1 (2)
O10T—Mo2—O9T106.5 (2)O13Wix—K2—O13W138.60 (18)
O10T—Mo2—O5B98.3 (2)O10T—K2—O13W78.00 (18)
O9T—Mo2—O5B101.0 (2)O15Wx—K2—O13W146.1 (4)
O10T—Mo2—O6B101.6 (2)O14Wix—K2—O13W76.3 (2)
O9T—Mo2—O6B98.6 (2)O15W—K2—O7Tiv65.4 (5)
O5B—Mo2—O6B146.69 (19)K2ix—K2—O7Tiv120.6 (3)
O10T—Mo2—O3C94.0 (2)O14W—K2—O7Tiv73.9 (2)
O9T—Mo2—O3C159.0 (2)O13Wix—K2—O7Tiv146.8 (2)
O5B—Mo2—O3C80.14 (18)O10T—K2—O7Tiv73.66 (18)
O6B—Mo2—O3C72.11 (18)O15Wx—K2—O7Tiv77.6 (3)
O10T—Mo2—O2C162.0 (2)O14Wix—K2—O7Tiv128.5 (2)
O9T—Mo2—O2C90.5 (2)O13W—K2—O7Tiv68.6 (2)
O5B—Mo2—O2C72.04 (18)
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x+1, y+1, z; (iii) x, y+1, z+1/2; (iv) x+1, y, z+1/2; (v) x+1, y+1, z+1; (vi) x, y+1, z1/2; (vii) x+1/2, y+1/2, z; (viii) x+1/2, y+1/2, z+1/2; (ix) x+1, y, z+1; (x) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2C—H2···O11Tviii0.86 (7)1.89 (7)2.720 (6)160 (8)
O4B—H4···O9Tvi0.81 (8)1.86 (9)2.659 (7)174 (14)
O13W—H13···O5B0.75 (7)2.21 (8)2.850 (9)144 (11)
O14W—H14A···O1Civ0.96 (8)1.79 (9)2.707 (8)159 (12)
O15W—H15B···O12Txi0.972.203.041 (15)144
O15W—H15B···O10T0.972.462.988 (14)114
O15W—H15A···O7Tiv0.972.203.056 (16)147
Symmetry codes: (iv) x+1, y, z+1/2; (vi) x, y+1, z1/2; (viii) x+1/2, y+1/2, z+1/2; (xi) x+1/2, y+1/2, z+1.
 

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