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Acta Crystallogr Sect E Struct Rep Online. 2010 April 1; 66(Pt 4): i25.
Published online 2010 March 13. doi:  10.1107/S1600536810008639
PMCID: PMC2984051

Redetermination of hepta­potassium nona­hydrogen bis­[α-hexa­molybdoplatinate(IV)] undeca­hydrate

Abstract

Previously reported at a temperature of 298 (2) K [Lee & Joo (2007 [triangle]). Acta Cryst. E63, i11–i13], the title compound, K7[H9α-Pt2Mo12O48]·11H2O or K7[H4.5α-PtMo6O24]2·11H2O, was redetermined at 146 (2) K in order to determine whether the H atom in the hydrogen bond that crosses the center of symmetry was located at the center of symmetry or disordered around it as assumed in the previous study. During the present low-temperature study it was found on the center of symmetry. One water molecule shows half-occupancy.

Related literature

For the crystal structure of K3.5[H4.5α-PtMo6O24]·5.5H2O, see: Lee & Joo (2007 [triangle]). For related structures, see: Lee & Sasaki (1994 [triangle]); Joo et al. (1994 [triangle]); Lee & Joo (2006a [triangle],b [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-00i25-scheme1.jpg

Experimental

Crystal data

  • K7[H4.5PtMo6O24]2·11H2O
  • M r = 2790.39
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-00i25-efi1.jpg
  • a = 10.0430 (3) Å
  • b = 12.1512 (4) Å
  • c = 12.4498 (4) Å
  • α = 67.792 (1)°
  • β = 68.542 (1)°
  • γ = 83.465 (2)°
  • V = 1308.58 (7) Å3
  • Z = 1
  • Mo Kα radiation
  • μ = 8.78 mm−1
  • T = 148 K
  • 0.15 × 0.09 × 0.06 mm

Data collection

  • Bruker SMART APEXII CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2009 [triangle]) T min = 0.353, T max = 0.621
  • 22108 measured reflections
  • 5699 independent reflections
  • 5599 reflections with I > 2σ(I)
  • R int = 0.031

Refinement

  • R[F 2 > 2σ(F 2)] = 0.021
  • wR(F 2) = 0.056
  • S = 1.23
  • 5699 reflections
  • 430 parameters
  • 20 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.88 e Å−3
  • Δρmin = −2.50 e Å−3

Data collection: APEX2 (Bruker, 2009 [triangle]); cell refinement: SAINT (Bruker, 2009 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: ORTEP-3 (Farrugia, 1997 [triangle]) and DIAMOND (Brandenburg, 1998 [triangle]); software used to prepare material for publication: SHELXL97.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810008639/br2139sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810008639/br2139Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Pukyong National University Research Fund in 2008 (PK-2008-018).

supplementary crystallographic information

Comment

The α-β-α geometrical isomerization according to the stepwise protonation in the [PtMo6O24]8- polyoxometalate species is very unusual phenomenon, viz., ([H3.5α-PtMo6O24]4.5- (Lee & Sasaki, 1994), [H4β-PtMo6O24]4- (Lee & Sasaki, 1994; Joo et al., 1994) and [H4.5α-PtMo6O24]3.5- (Lee & Sasaki, 1994; Lee & Joo, 2007).

This study was carried out to identify the position of the hydrogen atom that lies close to the center of symmetry. The structure of the title compound has been discussed in detail (Lee & Joo, 2007). Fig. 1 shows the structure of the polyanion. The O atoms of the clusters were designated as Ot(terminal Mo═O atom), Ob (O bridged µ2-O atom), and Oc3-O atom). The protonated O atoms in the polyanion were identified by the location in difference Fourier maps of the H atoms bound to O atoms and local structural features as seen previously (Lee & Joo, 2006a,b and Table 1). Fig. 2 shows a symmetrical electron density map around H6 atom. The position of H6 is (1/2, 0, 1/2). The distance of O6c–H6 and O6c···.O6ci are 1.28Å and 2.553 (5) Å, and the bond angle of O6c–H6–O6ci is 180 ° (Table 1 & Fig. 3).

The position of H6 was not found on the diffenence map in the previoius report (Lee & Joo, 2007). Therefore the H atom was considered as having positional disorder. The K2 ion is located on the inversion center. As a result the number of K+ ion is 7 and H+ ion is 9 in the unit cell.

The K+ ions are variously coordinated by O atoms as [K1(Ob)(Ot)2(Ow)4]+, [K2(Ob)2(Ot)6]+, [K3(Ob)(Ot)5(Ow)2]+, and [K4(Ot)5(Ow)2]+, respectively.

Experimental

Crystals of title compound were prepared by the reaction of K2MoO4.2H2O and K2Pt(OH)6 at pH 2.85 as described in a previous report (Lee & Sasaki, 1994).

Refinement

All H atoms in the polyanion were positioned in a difference Fourier maps and refined freely except H2 and H3. H2 and H3 refined with a distances restraint of O–H = 0.85 (3) Å. The H atoms of all Ow water molecules were placed in calculated positions with a distances restraint of O–H = 0.85 (3) Å. Their displacement parameters were freely refined except the O6w water molecule. The reasonable termal ellipsoid of O6w was obtained by half occupancy. The H atoms of O6w were included in the refinement with Uiso(H) = 1.5 Ueq(O).

Figures

Fig. 1.
The polyanion structure in the title compound. Displacement ellipsoids are drawn at the 50 % probability level for non-H atoms. H atoms are presented as a small spheres of arbitrary radius.
Fig. 2.
Difference Fourier map around H6 atom where atom H6 is absent.
Fig. 3.
Polyhedral view of the heteropolyanion in the title compound with O–H···O contacts of the inter-anion hydrogen bonds shown as red dashed lines. [Symmetry code: (i) - x + 1, - y, - z + 1.]

Crystal data

K7[H4.5PtMo6O24]2·11H2OZ = 1
Mr = 2790.39F(000) = 1296.0
Triclinic, P1Dx = 3.541 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.0430 (3) ÅCell parameters from 9000 reflections
b = 12.1512 (4) Åθ = 2.5–28.3°
c = 12.4498 (4) ŵ = 8.78 mm1
α = 67.792 (1)°T = 148 K
β = 68.542 (1)°Block, pale yellow
γ = 83.465 (2)°0.15 × 0.09 × 0.06 mm
V = 1308.58 (7) Å3

Data collection

Bruker SMART APEXII CCD diffractometer5699 independent reflections
Radiation source: Rotating Anode5599 reflections with I > 2σ(I)
Bruker HELIOS graded multilayer opticsRint = 0.031
Detector resolution: 10.0 pixels mm-1θmax = 27.0°, θmin = 1.8°
[var phi] and ω scansh = −12→12
Absorption correction: multi-scan (SADABS; Bruker, 2009)k = −15→15
Tmin = 0.353, Tmax = 0.621l = −15→15
22108 measured reflections

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021Hydrogen site location: difference Fourier map
wR(F2) = 0.056H atoms treated by a mixture of independent and constrained refinement
S = 1.23w = 1/[σ2(Fo2) + (0.0236P)2 + 1.1372P] where P = (Fo2 + 2Fc2)/3
5699 reflections(Δ/σ)max = 0.001
430 parametersΔρmax = 0.88 e Å3
20 restraintsΔρmin = −2.50 e Å3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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)

xyzUiso*/UeqOcc. (<1)
Pt0.370508 (12)0.214544 (10)0.496464 (11)0.00637 (5)
Mo10.70622 (3)0.22945 (2)0.32045 (3)0.00847 (7)
Mo20.47058 (3)0.32387 (3)0.19019 (3)0.00951 (7)
Mo30.12269 (3)0.31421 (2)0.35851 (3)0.00933 (7)
Mo40.01778 (3)0.22408 (2)0.66624 (3)0.00926 (7)
Mo50.26446 (3)0.14143 (3)0.79903 (3)0.00971 (7)
Mo60.61144 (3)0.14446 (2)0.62239 (3)0.00808 (7)
K10.07055 (10)0.42124 (8)0.85759 (9)0.0273 (2)
K20.00000.00000.50000.0355 (4)
K30.59498 (11)0.36460 (8)0.82891 (9)0.0313 (2)
K40.26045 (10)0.09021 (8)0.12674 (8)0.0281 (2)
O1C0.5151 (2)0.3258 (2)0.3496 (2)0.0090 (5)
O2C0.3163 (3)0.1907 (2)0.3667 (2)0.0097 (5)
H20.316 (5)0.118 (3)0.370 (4)0.039 (14)*
O3C0.2066 (3)0.3296 (2)0.4991 (2)0.0100 (5)
H30.239 (5)0.401 (3)0.484 (5)0.051 (16)*
O4C0.2191 (2)0.1077 (2)0.6475 (2)0.0088 (5)
H40.206 (5)0.034 (4)0.652 (4)0.036 (13)*
O5C0.4239 (2)0.2395 (2)0.6249 (2)0.0095 (5)
O6C0.5309 (3)0.1025 (2)0.4921 (2)0.0098 (5)
H60.50000.00000.50000.07 (3)*
O7B0.6133 (3)0.1997 (2)0.2207 (2)0.0122 (5)
O8B0.2979 (2)0.4051 (2)0.2462 (2)0.0114 (5)
O9B0.0238 (2)0.1989 (2)0.5211 (2)0.0119 (5)
O10B0.1262 (3)0.2514 (2)0.7562 (2)0.0127 (5)
O11B0.4359 (3)0.0325 (2)0.7600 (2)0.0124 (5)
H110.429 (5)−0.044 (4)0.767 (5)0.042 (14)*
O12B0.7099 (2)0.2530 (2)0.4686 (2)0.0116 (5)
O13T0.8149 (3)0.1062 (2)0.3315 (2)0.0139 (5)
O14T0.8155 (3)0.3469 (2)0.2130 (2)0.0145 (5)
O15T0.5792 (3)0.4457 (2)0.0911 (2)0.0168 (5)
O16T0.4268 (3)0.2674 (2)0.0998 (2)0.0168 (6)
O17T0.0066 (3)0.4276 (2)0.3516 (3)0.0170 (6)
O18T0.0983 (3)0.2410 (2)0.2724 (2)0.0144 (5)
O19T−0.0931 (3)0.3406 (2)0.6643 (3)0.0178 (6)
O20T−0.0825 (3)0.1011 (2)0.7766 (2)0.0171 (6)
O21T0.1625 (3)0.0179 (2)0.9083 (2)0.0194 (6)
O22T0.3249 (3)0.2023 (2)0.8760 (2)0.0160 (5)
O23T0.6388 (3)0.1967 (2)0.7219 (2)0.0146 (5)
O24T0.7139 (2)0.0163 (2)0.6320 (2)0.0122 (5)
O1W0.0212 (4)0.1809 (3)1.0680 (3)0.0361 (8)
H1A−0.039 (6)0.190 (5)1.132 (4)0.08 (2)*
H1B−0.010 (6)0.114 (4)1.070 (6)0.08 (2)*
O2W0.7580 (6)0.2330 (4)0.9609 (4)0.0773 (17)
H2A0.738 (8)0.214 (7)1.039 (3)0.13 (3)*
H2B0.812 (5)0.181 (4)0.942 (5)0.065 (19)*
O3W0.3643 (3)0.4685 (3)0.6662 (3)0.0297 (7)
H3A0.421 (4)0.528 (3)0.642 (5)0.046 (15)*
H3B0.415 (5)0.413 (3)0.652 (5)0.052 (17)*
O4W0.1450 (3)0.4420 (3)1.0368 (3)0.0232 (6)
H4A0.226 (3)0.470 (4)1.000 (4)0.043 (15)*
H4B0.145 (5)0.382 (3)1.100 (3)0.037 (14)*
O5W0.7096 (3)0.4622 (2)0.5447 (3)0.0199 (6)
H5A0.782 (4)0.418 (4)0.548 (4)0.046 (15)*
H5B0.707 (4)0.478 (4)0.474 (3)0.023 (13)*
O6W0.4612 (8)−0.0364 (7)0.0153 (7)0.044 (2)0.50
H6A0.534 (8)−0.080 (9)0.005 (11)0.066*0.50
H6B0.410 (11)−0.064 (11)−0.010 (11)0.066*0.50

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Pt0.00609 (7)0.00591 (7)0.00734 (8)0.00024 (5)−0.00257 (6)−0.00247 (6)
Mo10.00692 (14)0.00822 (13)0.01040 (15)0.00071 (10)−0.00275 (11)−0.00396 (12)
Mo20.00948 (14)0.01008 (14)0.00836 (15)−0.00072 (10)−0.00320 (12)−0.00235 (12)
Mo30.00878 (14)0.00899 (14)0.01138 (16)0.00063 (10)−0.00517 (12)−0.00346 (12)
Mo40.00725 (14)0.00911 (14)0.01092 (15)0.00039 (10)−0.00240 (12)−0.00391 (12)
Mo50.00970 (14)0.01067 (14)0.00813 (15)0.00112 (11)−0.00255 (12)−0.00355 (12)
Mo60.00793 (14)0.00677 (13)0.01079 (15)0.00094 (10)−0.00482 (12)−0.00325 (12)
K10.0422 (5)0.0217 (4)0.0297 (5)0.0106 (4)−0.0209 (4)−0.0167 (4)
K20.0150 (6)0.0269 (7)0.0648 (10)−0.0064 (5)0.0054 (6)−0.0334 (7)
K30.0470 (6)0.0201 (4)0.0281 (5)0.0015 (4)−0.0120 (5)−0.0114 (4)
K40.0356 (5)0.0302 (5)0.0164 (4)−0.0166 (4)−0.0084 (4)−0.0022 (4)
O1C0.0081 (11)0.0091 (11)0.0080 (12)−0.0020 (9)−0.0016 (9)−0.0017 (10)
O2C0.0123 (12)0.0082 (11)0.0106 (13)0.0000 (9)−0.0056 (10)−0.0041 (10)
O3C0.0088 (12)0.0089 (11)0.0130 (13)−0.0002 (9)−0.0051 (10)−0.0033 (10)
O4C0.0078 (11)0.0066 (11)0.0089 (12)−0.0021 (9)−0.0010 (10)−0.0007 (10)
O5C0.0097 (11)0.0120 (11)0.0097 (12)0.0009 (9)−0.0050 (10)−0.0057 (10)
O6C0.0080 (11)0.0093 (11)0.0123 (13)0.0008 (9)−0.0037 (10)−0.0042 (10)
O7B0.0110 (12)0.0144 (12)0.0137 (13)0.0009 (9)−0.0044 (10)−0.0077 (11)
O8B0.0111 (12)0.0107 (11)0.0127 (13)0.0000 (9)−0.0058 (10)−0.0030 (10)
O9B0.0109 (12)0.0119 (11)0.0117 (13)−0.0029 (9)−0.0027 (10)−0.0035 (10)
O10B0.0117 (12)0.0141 (12)0.0144 (13)0.0036 (9)−0.0056 (10)−0.0075 (11)
O11B0.0114 (12)0.0088 (11)0.0143 (13)−0.0008 (9)−0.0031 (10)−0.0023 (10)
O12B0.0120 (12)0.0093 (11)0.0131 (13)−0.0008 (9)−0.0048 (10)−0.0031 (10)
O13T0.0094 (12)0.0129 (12)0.0203 (14)0.0008 (9)−0.0046 (11)−0.0078 (11)
O14T0.0130 (12)0.0136 (12)0.0145 (13)−0.0021 (9)−0.0032 (11)−0.0035 (11)
O15T0.0126 (12)0.0166 (13)0.0163 (14)−0.0034 (10)−0.0034 (11)−0.0011 (11)
O16T0.0163 (13)0.0204 (13)0.0151 (14)0.0005 (10)−0.0063 (11)−0.0073 (12)
O17T0.0141 (13)0.0159 (13)0.0213 (15)0.0034 (10)−0.0081 (11)−0.0062 (12)
O18T0.0148 (12)0.0164 (12)0.0152 (13)−0.0002 (10)−0.0073 (11)−0.0070 (11)
O19T0.0142 (13)0.0168 (13)0.0248 (15)0.0045 (10)−0.0078 (12)−0.0104 (12)
O20T0.0145 (13)0.0157 (13)0.0159 (14)−0.0030 (10)−0.0029 (11)−0.0017 (11)
O21T0.0166 (14)0.0163 (13)0.0166 (15)0.0011 (10)−0.0012 (12)−0.0012 (12)
O22T0.0201 (13)0.0196 (13)0.0138 (13)0.0042 (10)−0.0092 (11)−0.0097 (11)
O23T0.0171 (13)0.0144 (12)0.0156 (14)−0.0006 (10)−0.0069 (11)−0.0076 (11)
O24T0.0108 (12)0.0106 (11)0.0152 (13)0.0011 (9)−0.0050 (10)−0.0044 (10)
O1W0.0324 (18)0.041 (2)0.0307 (19)−0.0046 (15)0.0027 (15)−0.0203 (17)
O2W0.099 (4)0.088 (3)0.026 (2)0.072 (3)−0.019 (2)−0.023 (2)
O3W0.0254 (16)0.0216 (15)0.044 (2)−0.0014 (13)−0.0079 (15)−0.0178 (15)
O4W0.0189 (14)0.0273 (16)0.0163 (15)−0.0046 (12)−0.0062 (12)0.0009 (13)
O5W0.0227 (15)0.0132 (13)0.0284 (17)0.0015 (11)−0.0129 (13)−0.0091 (13)
O6W0.051 (6)0.054 (6)0.037 (4)0.030 (4)−0.032 (4)−0.018 (4)

Geometric parameters (Å, °)

Pt—O1C1.979 (2)Mo6—O5C2.091 (2)
Pt—O2C2.006 (2)Mo6—O6C2.286 (2)
Pt—O3C2.034 (2)Mo6—O11B2.114 (2)
Pt—O4C2.011 (2)Mo6—O12B1.840 (2)
Pt—O5C1.992 (2)Mo6—O23T1.701 (2)
Pt—O6C1.986 (2)Mo6—O24T1.756 (2)
Pt—Mo63.2149 (3)K1—O10B2.713 (3)
Mo1—Mo23.2140 (4)K1—O14Ti2.854 (3)
Mo1—O1C2.118 (2)K1—O17Tii2.880 (3)
Mo1—O6C2.329 (2)K1—O1W3.039 (4)
Mo1—O7B1.951 (2)K1—O3W2.986 (3)
Mo1—O12B1.984 (2)K1—O4W2.700 (3)
Mo1—O13T1.742 (2)K1—O4Wiii2.815 (3)
Mo1—O14T1.694 (2)K2—O9Biv2.574 (2)
Mo2—O1C2.196 (2)K2—O9B2.574 (2)
Mo2—O2C2.289 (2)K2—O13Tv3.128 (3)
Mo2—O7B1.987 (2)K2—O13Tvi3.128 (3)
Mo2—O8B1.927 (2)K2—O18Tiv3.149 (3)
Mo2—O15T1.704 (2)K2—O18T3.149 (3)
Mo2—O16T1.716 (3)K2—O24Tvi2.767 (2)
Mo3—O2C2.326 (2)K2—O24Tv2.767 (2)
Mo3—O3C2.273 (3)K3—O8Bi2.799 (2)
Mo3—O8B1.936 (2)K3—O15Ti2.985 (3)
Mo3—O9B1.936 (2)K3—O16Tvii2.983 (3)
Mo3—O17T1.698 (2)K3—O19Tviii3.105 (3)
Mo3—O18T1.721 (2)K3—O22T3.282 (3)
Mo4—O3C2.285 (2)K3—O23T2.749 (3)
Mo4—O4C2.323 (2)K3—O2W2.706 (4)
Mo4—O9B1.923 (3)K3—O5W3.068 (3)
Mo4—O10B1.950 (2)K4—O16T2.720 (3)
Mo4—O19T1.697 (2)K4—O18T2.995 (3)
Mo4—O20T1.707 (2)K4—O20Tiv2.702 (3)
Mo5—O4C2.278 (3)K4—O22Tix2.744 (3)
Mo5—O5C2.151 (2)K4—O24Tv2.883 (3)
Mo5—O10B1.892 (2)K4—O1Wix2.756 (4)
Mo5—O11B2.076 (2)K4—O6Wx2.866 (8)
Mo5—O21T1.715 (2)K4—O6W2.687 (8)
Mo5—O22T1.702 (2)O6C—H61.28 (0)
O1C—Pt—O6C83.77 (10)O4W—K1—O3W95.82 (9)
O1C—Pt—O5C97.36 (10)O10B—K1—O3W71.65 (8)
O6C—Pt—O5C83.63 (10)O4Wiii—K1—O3W136.06 (9)
O1C—Pt—O2C82.44 (10)O14Ti—K1—O3W66.24 (8)
O6C—Pt—O2C96.73 (10)O17Tii—K1—O3W82.07 (9)
O5C—Pt—O2C179.57 (9)O4W—K1—O1W71.71 (9)
O1C—Pt—O4C177.47 (9)O10B—K1—O1W72.44 (8)
O6C—Pt—O4C98.47 (10)O4Wiii—K1—O1W102.34 (9)
O5C—Pt—O4C81.74 (10)O14Ti—K1—O1W139.77 (9)
O2C—Pt—O4C98.44 (10)O17Tii—K1—O1W145.67 (9)
O1C—Pt—O3C95.90 (10)O3W—K1—O1W115.70 (9)
O6C—Pt—O3C179.41 (9)O9Biv—K2—O9B180.000 (17)
O5C—Pt—O3C96.90 (10)O9B—K2—O24Tvi83.34 (7)
O2C—Pt—O3C82.74 (10)O9B—K2—O24Tv96.66 (7)
O4C—Pt—O3C81.88 (10)O9B—K2—O13Tvi93.58 (7)
O14T—Mo1—O13T105.35 (12)O9B—K2—O18Tiv123.48 (7)
O14T—Mo1—O7B100.55 (11)O9Biv—K2—O18T123.48 (7)
O13T—Mo1—O7B96.64 (11)O9B—K2—O18T56.52 (7)
O14T—Mo1—O12B96.89 (11)O24Tvi—K2—O18T107.85 (7)
O13T—Mo1—O12B96.56 (11)O24Tv—K2—O18T72.15 (7)
O7B—Mo1—O12B154.46 (10)O13Tv—K2—O18T119.67 (6)
O14T—Mo1—O1C96.38 (10)O13Tvi—K2—O18T60.33 (6)
O13T—Mo1—O1C158.00 (10)O18Tiv—K2—O18T180.00 (14)
O7B—Mo1—O1C75.67 (9)O2W—K3—O23T87.40 (12)
O12B—Mo1—O1C84.01 (10)O2W—K3—O8Bi101.70 (15)
O14T—Mo1—O6C165.54 (10)O23T—K3—O8Bi135.26 (8)
O13T—Mo1—O6C86.23 (10)O2W—K3—O16Tvii68.29 (11)
O7B—Mo1—O6C86.39 (10)O23T—K3—O16Tvii112.47 (8)
O12B—Mo1—O6C72.78 (9)O2W—K3—O15Ti117.98 (11)
O1C—Mo1—O6C72.89 (9)O23T—K3—O15Ti151.29 (8)
O15T—Mo2—O16T106.40 (12)O2W—K3—O5W121.75 (11)
O15T—Mo2—O8B98.22 (11)O23T—K3—O5W64.76 (7)
O16T—Mo2—O8B100.68 (11)O8Bi—K3—O5W73.57 (7)
O15T—Mo2—O7B101.30 (11)O16Tvii—K3—O5W168.39 (8)
O16T—Mo2—O7B92.82 (11)O15Ti—K3—O5W107.09 (7)
O8B—Mo2—O7B152.03 (10)O2W—K3—O19Tviii66.76 (11)
O15T—Mo2—O1C92.44 (11)O23T—K3—O19Tviii63.34 (7)
O16T—Mo2—O1C158.60 (10)O5W—K3—O19Tviii55.12 (7)
O8B—Mo2—O1C86.22 (9)O2W—K3—O22T110.14 (14)
O7B—Mo2—O1C73.19 (9)O23T—K3—O22T59.79 (7)
O15T—Mo2—O2C161.42 (11)O8Bi—K3—O22T145.97 (7)
O16T—Mo2—O2C91.12 (11)O16Tvii—K3—O22T71.25 (7)
O8B—Mo2—O2C71.88 (9)O15Ti—K3—O22T96.63 (7)
O7B—Mo2—O2C83.57 (9)O5W—K3—O22T98.56 (7)
O1C—Mo2—O2C71.63 (9)O19Tviii—K3—O22T123.13 (7)
O17T—Mo3—O18T106.56 (12)O6W—K4—O20Tiv86.85 (17)
O17T—Mo3—O8B98.83 (11)O6W—K4—O16T100.30 (17)
O18T—Mo3—O8B101.53 (11)O20Tiv—K4—O16T163.39 (9)
O17T—Mo3—O9B101.37 (11)O6W—K4—O22Tix72.57 (17)
O18T—Mo3—O9B97.67 (11)O20Tiv—K4—O22Tix112.52 (8)
O8B—Mo3—O9B146.75 (10)O16T—K4—O22Tix84.01 (8)
O17T—Mo3—O3C99.47 (11)O6W—K4—O1Wix125.74 (17)
O18T—Mo3—O3C153.10 (10)O20Tiv—K4—O1Wix75.80 (9)
O8B—Mo3—O3C80.67 (10)O16T—K4—O1Wix110.80 (9)
O9B—Mo3—O3C70.18 (9)O22Tix—K4—O1Wix68.01 (9)
O17T—Mo3—O2C166.65 (11)O6W—K4—O6Wx22.7 (3)
O18T—Mo3—O2C84.31 (10)O20Tiv—K4—O6Wx109.37 (17)
O8B—Mo3—O2C70.90 (9)O16T—K4—O6Wx77.87 (16)
O9B—Mo3—O2C84.41 (10)O22Tix—K4—O6Wx66.98 (16)
O3C—Mo3—O2C70.96 (9)O1Wix—K4—O6Wx132.79 (17)
O19T—Mo4—O20T106.07 (13)O6W—K4—O24Tv97.28 (17)
O19T—Mo4—O9B101.28 (12)O20Tiv—K4—O24Tv80.55 (8)
O20T—Mo4—O9B98.83 (12)O16T—K4—O24Tv83.66 (8)
O19T—Mo4—O10B98.77 (11)O22Tix—K4—O24Tv162.32 (8)
O20T—Mo4—O10B100.44 (12)O1Wix—K4—O24Tv128.57 (9)
O9B—Mo4—O10B147.02 (10)O6Wx—K4—O24Tv98.00 (16)
O19T—Mo4—O3C95.89 (11)O6W—K4—O18T164.77 (16)
O20T—Mo4—O3C157.14 (10)O20Tiv—K4—O18T102.64 (8)
O9B—Mo4—O3C70.14 (9)O16T—K4—O18T67.51 (7)
O10B—Mo4—O3C82.01 (10)O22Tix—K4—O18T113.50 (8)
O19T—Mo4—O4C163.39 (11)O1Wix—K4—O18T68.76 (9)
O20T—Mo4—O4C88.94 (11)O6Wx—K4—O18T144.85 (16)
O9B—Mo4—O4C82.95 (10)O24Tv—K4—O18T72.99 (7)
O10B—Mo4—O4C70.94 (9)Pt—O1C—Mo1105.46 (10)
O3C—Mo4—O4C70.23 (9)Pt—O1C—Mo2104.98 (10)
O22T—Mo5—O21T106.70 (13)Mo1—O1C—Mo296.30 (9)
O22T—Mo5—O10B101.84 (11)Pt—O2C—Mo2100.81 (10)
O21T—Mo5—O10B102.99 (11)Pt—O2C—Mo3102.68 (10)
O22T—Mo5—O11B97.58 (11)Mo2—O2C—Mo392.77 (9)
O21T—Mo5—O11B89.09 (11)Pt—O3C—Mo3103.60 (10)
O10B—Mo5—O11B152.95 (10)Pt—O3C—Mo4104.25 (10)
O22T—Mo5—O5C91.56 (11)Mo3—O3C—Mo494.06 (9)
O21T—Mo5—O5C154.90 (10)Pt—O4C—Mo5100.24 (10)
O10B—Mo5—O5C89.52 (10)Pt—O4C—Mo4103.64 (10)
O11B—Mo5—O5C71.17 (9)Mo5—O4C—Mo492.53 (9)
O22T—Mo5—O4C162.98 (11)Pt—O5C—Mo6103.86 (10)
O21T—Mo5—O4C90.31 (11)Pt—O5C—Mo5105.34 (10)
O10B—Mo5—O4C72.93 (9)Mo6—O5C—Mo5105.12 (10)
O11B—Mo5—O4C83.03 (9)Pt—O6C—Mo697.38 (10)
O5C—Mo5—O4C72.45 (9)Pt—O6C—Mo197.89 (10)
O23T—Mo6—O24T104.61 (11)Mo6—O6C—Mo190.69 (8)
O23T—Mo6—O12B103.60 (11)Mo1—O7B—Mo2109.41 (11)
O24T—Mo6—O12B103.93 (11)Mo2—O8B—Mo3119.78 (12)
O23T—Mo6—O5C92.37 (11)Mo2—O8B—K3i101.44 (9)
O24T—Mo6—O5C154.05 (10)Mo3—O8B—K3i137.03 (11)
O12B—Mo6—O5C90.63 (10)Mo4—O9B—Mo3119.62 (12)
O23T—Mo6—O11B93.94 (11)Mo5—O10B—Mo4119.84 (12)
O24T—Mo6—O11B87.50 (10)Mo5—O11B—Mo6107.00 (11)
O12B—Mo6—O11B155.64 (10)Mo6—O12B—Mo1118.20 (12)
O5C—Mo6—O11B71.63 (9)H1A—O1W—H1B103 (4)
O23T—Mo6—O6C166.81 (10)H2A—O2W—H2B105 (4)
O24T—Mo6—O6C88.05 (10)H3A—O3W—H3B107 (3)
O12B—Mo6—O6C76.34 (10)H4A—O4W—H4B109 (4)
O5C—Mo6—O6C74.46 (9)H5A—O5W—H5B105 (3)
O11B—Mo6—O6C82.73 (9)H6A—O6W—H6B101 (10)
O4W—K1—O10B131.27 (9)

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

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O2C—H2···O24Tv0.87 (3)1.70 (3)2.561 (3)168 (5)
O3C—H3···O5Wi0.89 (3)1.67 (3)2.552 (4)177 (5)
O4C—H4···O13Tv0.89 (5)1.67 (5)2.562 (3)176 (5)
O6C—H6···O6Cv1.281.282.553 (3)180
O11B—H11···O7Bv0.90 (5)1.93 (5)2.826 (3)172 (4)
O1W—H1A···O13Txi0.84 (3)2.27 (4)3.014 (4)149 (5)
O1W—H1B···O21Txii0.89 (3)2.22 (4)3.067 (4)159 (6)
O2W—H2A···O7Bvii0.86 (3)2.10 (4)2.906 (5)157 (7)
O2W—H2B···O21Txiii0.83 (3)2.49 (5)3.038 (5)125 (5)
O3W—H3A···O1Ci0.86 (3)2.01 (3)2.811 (4)154 (5)
O3W—H3B···O5C0.83 (3)2.24 (3)2.973 (4)147 (4)
O4W—H4A···O15Ti0.81 (3)2.03 (3)2.839 (4)175 (5)
O4W—H4B···O18Tvii0.84 (3)2.11 (3)2.938 (4)168 (4)
O5W—H5A···O19Tviii0.86 (3)2.14 (3)2.856 (4)141 (4)
O5W—H5B···O3Wi0.83 (2)1.99 (3)2.787 (4)160 (4)
O6W—H6A···O22Tv0.85 (3)2.41 (8)3.097 (7)138 (11)

Symmetry codes: (v) −x+1, −y, −z+1; (i) −x+1, −y+1, −z+1; (xi) x−1, y, z+1; (xii) −x, −y, −z+2; (vii) x, y, z+1; (xiii) −x+1, −y, −z+2; (viii) x+1, y, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BR2139).

References

  • Brandenburg, K. (1998). DIAMOND Crystal Impact GbR, Bonn, Germany.
  • Bruker (2009). APEX2, SADABS and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Farrugia, L. J. (1997). J. Appl. Cryst.30, 565.
  • Joo, H. C., Park, K. M. & Lee, U. (1994). Acta Cryst. C50, 1659–1661.
  • Lee, U. & Joo, H.-C. (2006a). Acta Cryst. E62, i231–i233.
  • Lee, U. & Joo, H.-C. (2006b). Acta Cryst. E62, i241–i243.
  • Lee, U. & Joo, H.-C. (2007). Acta Cryst. E63, i11–i13.
  • Lee, U. & Sasaki, Y. (1994). Bull. Korean Chem. Soc 15, 37–45.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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