Dipotassium hexa­hydrogen hexa­molybdoplatinate(IV) hexa­hydrate

Lee, U.; Joo, H.-C.

doi:10.1107/S1600536806046125

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Dipotassium hexahydrogen hexamolybdoplatinate(IV) hexahydrate

U. Lee and H.-C. Joo

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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806046125/wm2064sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806046125/wm2064Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (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]·6H₂O	F(000) = 2504
M_r = 1347.07	D_x = 3.356 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2yc	Cell parameters from 30 reflections
a = 21.178 (3) Å	θ = 9.5–10.4°
b = 12.940 (2) Å	µ = 8.38 mm⁻¹
c = 10.110 (2) Å	T = 298 K
β = 105.77 (1)°	Hexagonal block, pale yellow
V = 2666.3 (8) Å³	0.42 × 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 tube	R_int = 0.010
Graphite monochromator	θ_max = 27.5°, θ_min = 1.9°
ω/2θ scans	h = −27→26
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996)	k = 0→16
T_min = 0.229, T_max = 0.376	l = 0→13
3078 measured reflections	3 standard reflections every 60 min
3056 independent reflections	intensity decay: 3.2%

Refinement top

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)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.081	H atoms treated by a mixture of independent and constrained refinement
S = 1.16	w = 1/[σ²(F_o²) + (0.0368P)² + 9.1413P] where P = (F_o² + 2F_c²)/3
3056 reflections	(Δ/σ)_max < 0.001
210 parameters	Δρ_max = 0.97 e Å⁻³
8 restraints	Δρ_min = −1.27 e Å⁻³

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	0.2500	0.2500	0.0000	0.01349 (9)
Mo1	0.40336 (3)	0.34274 (4)	0.06449 (6)	0.02157 (14)
Mo2	0.34798 (3)	0.26249 (4)	0.32760 (6)	0.01849 (13)
Mo3	0.19606 (3)	0.16989 (4)	0.26248 (6)	0.01903 (13)
K1	0.5000	0.62888 (19)	0.2500	0.0426 (6)
K2	0.4913 (2)	0.0638 (3)	0.5596 (5)	0.0566 (12)	0.50
O1C	0.3295 (2)	0.2475 (3)	−0.0723 (5)	0.0187 (9)
O2C	0.3026 (2)	0.3565 (3)	0.1270 (5)	0.0186 (9)
H2	0.284 (4)	0.416 (5)	0.131 (9)	0.03 (2)*
O3C	0.2827 (2)	0.1571 (3)	0.1616 (4)	0.0160 (9)
H3	0.298 (4)	0.096 (5)	0.130 (8)	0.03 (2)*
O4B	0.3522 (3)	0.4257 (4)	−0.1024 (5)	0.0261 (11)
H4	0.361 (7)	0.486 (7)	−0.103 (14)	0.11 (5)*
O5B	0.4045 (2)	0.2459 (3)	0.2076 (5)	0.0216 (10)
O6B	0.2581 (2)	0.2735 (4)	0.3417 (5)	0.0231 (10)
O7T	0.4670 (3)	0.3023 (5)	0.0061 (6)	0.0430 (14)
O8T	0.4277 (3)	0.4548 (4)	0.1523 (6)	0.0377 (14)
O9T	0.3787 (3)	0.3731 (4)	0.4121 (5)	0.0281 (11)
O10T	0.3775 (3)	0.1636 (4)	0.4370 (5)	0.0298 (12)
O11T	0.2256 (3)	0.0603 (4)	0.3558 (5)	0.0305 (12)
O12T	0.1295 (3)	0.2088 (4)	0.3103 (5)	0.0313 (12)
O13W	0.5000	0.0853 (8)	0.2500	0.064 (3)
H13	0.477 (5)	0.120 (7)	0.273 (12)	0.05 (3)*
O14W	0.6168 (5)	0.0610 (6)	0.5963 (9)	0.068 (2)
H14A	0.626 (7)	0.131 (7)	0.575 (13)	0.098*
H14B	0.587 (5)	0.086 (8)	0.616 (12)	0.050*
O15W	0.4892 (7)	0.1583 (9)	0.6918 (13)	0.055 (4)	0.50
H15A	0.5064	0.2208	0.6617	0.082*	0.50
H15B	0.4428	0.1713	0.6790	0.082*	0.50
O16W	0.3233 (3)	−0.0263 (4)	0.1255 (6)	0.0439 (15)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt	0.01563 (16)	0.01233 (15)	0.01243 (16)	−0.00035 (12)	0.00369 (12)	0.00013 (11)
Mo1	0.0183 (3)	0.0239 (3)	0.0210 (3)	−0.0040 (2)	0.0028 (2)	0.0030 (2)
Mo2	0.0229 (3)	0.0161 (3)	0.0147 (3)	−0.0011 (2)	0.0021 (2)	0.00053 (19)
Mo3	0.0220 (3)	0.0196 (3)	0.0166 (3)	−0.0013 (2)	0.0072 (2)	0.0029 (2)
K1	0.0304 (13)	0.0294 (12)	0.072 (2)	0.000	0.0213 (13)	0.000
K2	0.042 (2)	0.053 (2)	0.064 (3)	−0.0027 (19)	−0.004 (2)	0.007 (2)
O1C	0.016 (2)	0.019 (2)	0.021 (2)	−0.0012 (17)	0.0055 (18)	0.0020 (17)
O2C	0.021 (2)	0.0119 (19)	0.021 (2)	−0.0014 (17)	0.0015 (19)	−0.0028 (17)
O3C	0.021 (2)	0.014 (2)	0.012 (2)	−0.0010 (17)	0.0030 (17)	0.0017 (16)
O4B	0.032 (3)	0.022 (2)	0.019 (2)	−0.009 (2)	−0.001 (2)	0.0025 (19)
O5B	0.019 (2)	0.021 (2)	0.023 (2)	0.0008 (18)	0.0020 (19)	0.0019 (18)
O6B	0.028 (3)	0.024 (2)	0.018 (2)	−0.0044 (19)	0.008 (2)	−0.0049 (18)
O7T	0.026 (3)	0.058 (4)	0.047 (4)	0.001 (3)	0.014 (3)	0.010 (3)
O8T	0.040 (3)	0.028 (3)	0.037 (3)	−0.016 (2)	−0.004 (3)	0.006 (2)
O9T	0.030 (3)	0.022 (2)	0.027 (3)	−0.002 (2)	−0.002 (2)	−0.004 (2)
O10T	0.036 (3)	0.026 (2)	0.024 (3)	0.005 (2)	0.003 (2)	0.005 (2)
O11T	0.037 (3)	0.024 (2)	0.029 (3)	−0.006 (2)	0.007 (2)	0.009 (2)
O12T	0.030 (3)	0.038 (3)	0.028 (3)	−0.001 (2)	0.012 (2)	0.000 (2)
O13W	0.040 (6)	0.033 (5)	0.109 (10)	0.000	0.001 (6)	0.000
O14W	0.094 (7)	0.037 (4)	0.071 (5)	−0.019 (4)	0.022 (5)	0.006 (4)
O15W	0.056 (9)	0.048 (7)	0.050 (8)	0.017 (6)	−0.004 (7)	0.002 (6)
O16W	0.057 (4)	0.035 (3)	0.035 (3)	0.011 (3)	0.004 (3)	−0.004 (2)

Geometric parameters (Å, º) top

Mo1—Mo2	3.3503 (10)	Mo3—O12T	1.688 (5)
Mo1—Mo3ⁱ	3.4065 (10)	K1—O7Tⁱⁱ	2.994 (6)
Mo2—Mo3	3.3269 (9)	K1—O7Tⁱⁱⁱ	2.994 (6)
Pt—O1C	2.010 (4)	K1—O8T	2.751 (5)
Pt—O2C	2.003 (4)	K1—O8T^iv	2.751 (5)
Pt—O3C	1.995 (4)	K1—O15W^v	2.813 (13)
Pt—O3Cⁱ	1.995 (4)	K1—O15W^vi	2.813 (13)
Pt—O2Cⁱ	2.003 (4)	K1—O12T^vii	2.837 (5)
Pt—O1Cⁱ	2.010 (4)	K1—O12T^viii	2.837 (5)
Mo1—O1C	2.169 (4)	K2—O10T	2.719 (7)
Mo1—O2C	2.391 (5)	K2—O7T^iv	3.325 (8)
Mo1—O4B	2.044 (5)	K2—O13W	3.198 (5)
Mo1—O5B	1.909 (5)	K2—O13W^ix	2.696 (9)
Mo1—O7T	1.696 (6)	K2—O14W	2.583 (11)
Mo1—O8T	1.706 (5)	K2—O14W^ix	2.894 (10)
Mo2—O2C	2.336 (5)	K2—O15W	1.820 (14)
Mo2—O3C	2.308 (4)	K2—O15W^x	2.723 (14)
Mo2—O5B	1.934 (5)	O2C—H2	0.86 (7)
Mo2—O6B	1.953 (5)	O3C—H3	0.93 (6)
Mo2—O9T	1.702 (5)	O4B—H4	0.81 (8)
Mo2—O10T	1.695 (5)	O13W—H13	0.75 (7)
Mo3—O1Cⁱ	2.137 (4)	O14W—H14A	0.96 (8)
Mo3—O3C	2.335 (5)	O14W—H14B	0.78 (7)
Mo3—O4Bⁱ	2.073 (5)	O15W—H15A	0.9700
Mo3—O6B	1.895 (5)	O15W—H15B	0.9700
Mo3—O11T	1.724 (5)

Mo3ⁱ—O1C—Mo1	104.58 (18)	O6B—Mo2—O2C	81.16 (18)
Mo2—O2C—Mo1	90.27 (16)	O3C—Mo2—O2C	69.69 (15)
Mo2—O3C—Mo3	91.55 (15)	O12T—Mo3—O11T	107.2 (3)
Mo1—O4B—Mo3ⁱ	111.7 (2)	O12T—Mo3—O6B	101.8 (2)
Mo1—O5B—Mo2	121.3 (2)	O11T—Mo3—O6B	104.1 (2)
Mo3—O6B—Mo2	119.7 (2)	O12T—Mo3—O4Bⁱ	97.4 (2)
Pt—O1C—Mo3ⁱ	106.7 (2)	O11T—Mo3—O4Bⁱ	88.0 (2)
Pt—O1C—Mo1	106.8 (2)	O6B—Mo3—O4Bⁱ	152.9 (2)
Pt—O2C—Mo2	102.93 (18)	O12T—Mo3—O1Cⁱ	94.7 (2)
Pt—O2C—Mo1	99.22 (18)	O11T—Mo3—O1Cⁱ	150.4 (2)
Pt—O3C—Mo2	104.20 (17)	O6B—Mo3—O1Cⁱ	90.18 (19)
Pt—O3C—Mo3	100.13 (19)	O4Bⁱ—Mo3—O1Cⁱ	69.25 (18)
H14A—O14W—H14B	83 (10)	O12T—Mo3—O3C	164.5 (2)
O15W^x—O15W—H15B	104.1	O11T—Mo3—O3C	88.2 (2)
H15A—O15W—H15B	105.5	O6B—Mo3—O3C	72.43 (18)
Mo3—Mo2—Mo1	118.87 (2)	O4Bⁱ—Mo3—O3C	84.05 (19)
Mo2—Mo1—Mo3ⁱ	119.88 (2)	O1Cⁱ—Mo3—O3C	71.31 (16)
O3C—Pt—O3Cⁱ	180.0 (3)	O8T—K1—O8T^iv	70.1 (2)
O3C—Pt—O2Cⁱ	96.84 (18)	O8T—K1—O15W^v	151.9 (3)
O3Cⁱ—Pt—O2Cⁱ	83.16 (18)	O8T^iv—K1—O15W^v	136.1 (3)
O3C—Pt—O2C	83.16 (18)	O8T—K1—O15W^vi	136.1 (3)
O3Cⁱ—Pt—O2C	96.84 (18)	O8T^iv—K1—O15W^vi	151.9 (3)
O2Cⁱ—Pt—O2C	180.0 (4)	O15W^v—K1—O15W^vi	23.4 (5)
O3C—Pt—O1C	98.60 (18)	O8T—K1—O12T^vii	141.86 (18)
O3Cⁱ—Pt—O1C	81.40 (18)	O8T^iv—K1—O12T^vii	79.05 (17)
O2Cⁱ—Pt—O1C	97.51 (19)	O15W^v—K1—O12T^vii	65.1 (3)
O2C—Pt—O1C	82.49 (19)	O8T—K1—O7Tⁱⁱ	99.85 (18)
O3C—Pt—O1Cⁱ	81.40 (18)	O8T^iv—K1—O7Tⁱⁱ	108.43 (18)
O3Cⁱ—Pt—O1Cⁱ	98.60 (18)	O15W^v—K1—O7Tⁱⁱ	82.2 (3)
O2Cⁱ—Pt—O1Cⁱ	82.49 (19)	O15W^vi—K1—O7Tⁱⁱ	63.4 (3)
O2C—Pt—O1Cⁱ	97.51 (19)	O15W^v—K1—O7Tⁱⁱⁱ	63.4 (3)
O1C—Pt—O1Cⁱ	180.00 (9)	O15W^vi—K1—O7Tⁱⁱⁱ	82.2 (3)
O7T—Mo1—O8T	106.7 (3)	O15W—K2—O14W	97.7 (6)
O7T—Mo1—O5B	102.3 (3)	K2^ix—K2—O14W	75.0 (3)
O8T—Mo1—O5B	102.9 (2)	O15W—K2—O13W^ix	88.1 (5)
O7T—Mo1—O4B	99.6 (3)	O14W—K2—O13W^ix	91.1 (2)
O8T—Mo1—O4B	90.0 (2)	O15W—K2—O10T	79.7 (5)
O5B—Mo1—O4B	149.9 (2)	O14W—K2—O10T	145.4 (3)
O7T—Mo1—O1C	96.1 (2)	O13W^ix—K2—O10T	123.1 (2)
O8T—Mo1—O1C	151.5 (2)	O15W—K2—O15W^x	18.0 (5)
O5B—Mo1—O1C	88.19 (18)	O14W—K2—O15W^x	89.0 (4)
O4B—Mo1—O1C	69.13 (18)	O13W^ix—K2—O15W^x	72.5 (3)
O7T—Mo1—O2C	165.1 (2)	O10T—K2—O15W^x	95.8 (4)
O8T—Mo1—O2C	87.9 (2)	O15W—K2—O14W^ix	127.0 (6)
O5B—Mo1—O2C	71.16 (18)	O14W—K2—O14W^ix	134.5 (2)
O4B—Mo1—O2C	82.45 (19)	O15W—K2—O13W	132.8 (5)
O1C—Mo1—O2C	70.74 (16)	O14W—K2—O13W	79.1 (2)
O10T—Mo2—O9T	106.5 (2)	O13W^ix—K2—O13W	138.60 (18)
O10T—Mo2—O5B	98.3 (2)	O10T—K2—O13W	78.00 (18)
O9T—Mo2—O5B	101.0 (2)	O15W^x—K2—O13W	146.1 (4)
O10T—Mo2—O6B	101.6 (2)	O14W^ix—K2—O13W	76.3 (2)
O9T—Mo2—O6B	98.6 (2)	O15W—K2—O7T^iv	65.4 (5)
O5B—Mo2—O6B	146.69 (19)	K2^ix—K2—O7T^iv	120.6 (3)
O10T—Mo2—O3C	94.0 (2)	O14W—K2—O7T^iv	73.9 (2)
O9T—Mo2—O3C	159.0 (2)	O13W^ix—K2—O7T^iv	146.8 (2)
O5B—Mo2—O3C	80.14 (18)	O10T—K2—O7T^iv	73.66 (18)
O6B—Mo2—O3C	72.11 (18)	O15W^x—K2—O7T^iv	77.6 (3)
O10T—Mo2—O2C	162.0 (2)	O14W^ix—K2—O7T^iv	128.5 (2)
O9T—Mo2—O2C	90.5 (2)	O13W—K2—O7T^iv	68.6 (2)
O5B—Mo2—O2C	72.04 (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, z−1/2; (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···A	D—H	H···A	D···A	D—H···A
O2C—H2···O11T^viii	0.86 (7)	1.89 (7)	2.720 (6)	160 (8)
O4B—H4···O9T^vi	0.81 (8)	1.86 (9)	2.659 (7)	174 (14)
O13W—H13···O5B	0.75 (7)	2.21 (8)	2.850 (9)	144 (11)
O14W—H14A···O1C^iv	0.96 (8)	1.79 (9)	2.707 (8)	159 (12)
O15W—H15B···O12T^xi	0.97	2.20	3.041 (15)	144
O15W—H15B···O10T	0.97	2.46	2.988 (14)	114
O15W—H15A···O7T^iv	0.97	2.20	3.056 (16)	147

Symmetry codes: (iv) −x+1, y, −z+1/2; (vi) x, −y+1, z−1/2; (viii) −x+1/2, y+1/2, −z+1/2; (xi) −x+1/2, −y+1/2, −z+1.

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Dipotassium hexa­hydrogen hexa­molybdoplatinate(IV) hexa­hydrate

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Dipotassium hexahydrogen hexamolybdoplatinate(IV) hexahydrate