Redetermination of hepta-potassium nona-hydrogen bis-[α-hexa-molybdoplatinate(IV)] undeca-hydrate.

Previously reported at a temperature of 298 (2) K [Lee & Joo (2007 ▶). Acta Cryst. E63, i11-i13], the title compound, K(7)[H(9)α-Pt(2)Mo(12)O(48)]·11H(2)O or K(7)[H(4.5)α-PtMo(6)O(24)](2)·11H(2)O, 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 ▶). For related structures, see: Lee & Sasaki (1994 ▶); Joo et al. (1994 ▶); Lee & Joo (2006a ▶,b ▶).

Experimental

Crystal data

K7[H4.5PtMo6O24]2·11H2O

M = 2790.39

Triclinic,

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

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

K7[H4.5PtMo6O24]2·11H2O	Z = 1
Mr = 2790.39	F(000) = 1296.0
Triclinic, P1	Dx = 3.541 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.0430 (3) Å	Cell parameters from 9000 reflections
b = 12.1512 (4) Å	θ = 2.5–28.3°
c = 12.4498 (4) Å	µ = 8.78 mm−1
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

Bruker SMART APEXII CCD diffractometer	5699 independent reflections
Radiation source: Rotating Anode	5599 reflections with I > 2σ(I)
Bruker HELIOS graded multilayer optics	Rint = 0.031
Detector resolution: 10.0 pixels mm-1	θmax = 27.0°, θmin = 1.8°
φ and ω scans	h = −12→12
Absorption correction: multi-scan (SADABS; Bruker, 2009)	k = −15→15
Tmin = 0.353, Tmax = 0.621	l = −15→15
22108 measured reflections

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)] = 0.021	Hydrogen site location: difference Fourier map
wR(F2) = 0.056	H atoms treated by a mixture of independent and constrained refinement
S = 1.23	w = 1/[σ2(Fo2) + (0.0236P)2 + 1.1372P] where P = (Fo2 + 2Fc2)/3
5699 reflections	(Δ/σ)max = 0.001
430 parameters	Δρmax = 0.88 e Å−3
20 restraints	Δρmin = −2.50 e Å−3

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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pt	0.370508 (12)	0.214544 (10)	0.496464 (11)	0.00637 (5)
Mo1	0.70622 (3)	0.22945 (2)	0.32045 (3)	0.00847 (7)
Mo2	0.47058 (3)	0.32387 (3)	0.19019 (3)	0.00951 (7)
Mo3	0.12269 (3)	0.31421 (2)	0.35851 (3)	0.00933 (7)
Mo4	0.01778 (3)	0.22408 (2)	0.66624 (3)	0.00926 (7)
Mo5	0.26446 (3)	0.14143 (3)	0.79903 (3)	0.00971 (7)
Mo6	0.61144 (3)	0.14446 (2)	0.62239 (3)	0.00808 (7)
K1	0.07055 (10)	0.42124 (8)	0.85759 (9)	0.0273 (2)
K2	0.0000	0.0000	0.5000	0.0355 (4)
K3	0.59498 (11)	0.36460 (8)	0.82891 (9)	0.0313 (2)
K4	0.26045 (10)	0.09021 (8)	0.12674 (8)	0.0281 (2)
O1C	0.5151 (2)	0.3258 (2)	0.3496 (2)	0.0090 (5)
O2C	0.3163 (3)	0.1907 (2)	0.3667 (2)	0.0097 (5)
H2	0.316 (5)	0.118 (3)	0.370 (4)	0.039 (14)*
O3C	0.2066 (3)	0.3296 (2)	0.4991 (2)	0.0100 (5)
H3	0.239 (5)	0.401 (3)	0.484 (5)	0.051 (16)*
O4C	0.2191 (2)	0.1077 (2)	0.6475 (2)	0.0088 (5)
H4	0.206 (5)	0.034 (4)	0.652 (4)	0.036 (13)*
O5C	0.4239 (2)	0.2395 (2)	0.6249 (2)	0.0095 (5)
O6C	0.5309 (3)	0.1025 (2)	0.4921 (2)	0.0098 (5)
H6	0.5000	0.0000	0.5000	0.07 (3)*
O7B	0.6133 (3)	0.1997 (2)	0.2207 (2)	0.0122 (5)
O8B	0.2979 (2)	0.4051 (2)	0.2462 (2)	0.0114 (5)
O9B	0.0238 (2)	0.1989 (2)	0.5211 (2)	0.0119 (5)
O10B	0.1262 (3)	0.2514 (2)	0.7562 (2)	0.0127 (5)
O11B	0.4359 (3)	0.0325 (2)	0.7600 (2)	0.0124 (5)
H11	0.429 (5)	−0.044 (4)	0.767 (5)	0.042 (14)*
O12B	0.7099 (2)	0.2530 (2)	0.4686 (2)	0.0116 (5)
O13T	0.8149 (3)	0.1062 (2)	0.3315 (2)	0.0139 (5)
O14T	0.8155 (3)	0.3469 (2)	0.2130 (2)	0.0145 (5)
O15T	0.5792 (3)	0.4457 (2)	0.0911 (2)	0.0168 (5)
O16T	0.4268 (3)	0.2674 (2)	0.0998 (2)	0.0168 (6)
O17T	0.0066 (3)	0.4276 (2)	0.3516 (3)	0.0170 (6)
O18T	0.0983 (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)
O21T	0.1625 (3)	0.0179 (2)	0.9083 (2)	0.0194 (6)
O22T	0.3249 (3)	0.2023 (2)	0.8760 (2)	0.0160 (5)
O23T	0.6388 (3)	0.1967 (2)	0.7219 (2)	0.0146 (5)
O24T	0.7139 (2)	0.0163 (2)	0.6320 (2)	0.0122 (5)
O1W	0.0212 (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)*
O2W	0.7580 (6)	0.2330 (4)	0.9609 (4)	0.0773 (17)
H2A	0.738 (8)	0.214 (7)	1.039 (3)	0.13 (3)*
H2B	0.812 (5)	0.181 (4)	0.942 (5)	0.065 (19)*
O3W	0.3643 (3)	0.4685 (3)	0.6662 (3)	0.0297 (7)
H3A	0.421 (4)	0.528 (3)	0.642 (5)	0.046 (15)*
H3B	0.415 (5)	0.413 (3)	0.652 (5)	0.052 (17)*
O4W	0.1450 (3)	0.4420 (3)	1.0368 (3)	0.0232 (6)
H4A	0.226 (3)	0.470 (4)	1.000 (4)	0.043 (15)*
H4B	0.145 (5)	0.382 (3)	1.100 (3)	0.037 (14)*
O5W	0.7096 (3)	0.4622 (2)	0.5447 (3)	0.0199 (6)
H5A	0.782 (4)	0.418 (4)	0.548 (4)	0.046 (15)*
H5B	0.707 (4)	0.478 (4)	0.474 (3)	0.023 (13)*
O6W	0.4612 (8)	−0.0364 (7)	0.0153 (7)	0.044 (2)	0.50
H6A	0.534 (8)	−0.080 (9)	0.005 (11)	0.066*	0.50
H6B	0.410 (11)	−0.064 (11)	−0.010 (11)	0.066*	0.50

	U11	U22	U33	U12	U13	U23
Pt	0.00609 (7)	0.00591 (7)	0.00734 (8)	0.00024 (5)	−0.00257 (6)	−0.00247 (6)
Mo1	0.00692 (14)	0.00822 (13)	0.01040 (15)	0.00071 (10)	−0.00275 (11)	−0.00396 (12)
Mo2	0.00948 (14)	0.01008 (14)	0.00836 (15)	−0.00072 (10)	−0.00320 (12)	−0.00235 (12)
Mo3	0.00878 (14)	0.00899 (14)	0.01138 (16)	0.00063 (10)	−0.00517 (12)	−0.00346 (12)
Mo4	0.00725 (14)	0.00911 (14)	0.01092 (15)	0.00039 (10)	−0.00240 (12)	−0.00391 (12)
Mo5	0.00970 (14)	0.01067 (14)	0.00813 (15)	0.00112 (11)	−0.00255 (12)	−0.00355 (12)
Mo6	0.00793 (14)	0.00677 (13)	0.01079 (15)	0.00094 (10)	−0.00482 (12)	−0.00325 (12)
K1	0.0422 (5)	0.0217 (4)	0.0297 (5)	0.0106 (4)	−0.0209 (4)	−0.0167 (4)
K2	0.0150 (6)	0.0269 (7)	0.0648 (10)	−0.0064 (5)	0.0054 (6)	−0.0334 (7)
K3	0.0470 (6)	0.0201 (4)	0.0281 (5)	0.0015 (4)	−0.0120 (5)	−0.0114 (4)
K4	0.0356 (5)	0.0302 (5)	0.0164 (4)	−0.0166 (4)	−0.0084 (4)	−0.0022 (4)
O1C	0.0081 (11)	0.0091 (11)	0.0080 (12)	−0.0020 (9)	−0.0016 (9)	−0.0017 (10)
O2C	0.0123 (12)	0.0082 (11)	0.0106 (13)	0.0000 (9)	−0.0056 (10)	−0.0041 (10)
O3C	0.0088 (12)	0.0089 (11)	0.0130 (13)	−0.0002 (9)	−0.0051 (10)	−0.0033 (10)
O4C	0.0078 (11)	0.0066 (11)	0.0089 (12)	−0.0021 (9)	−0.0010 (10)	−0.0007 (10)
O5C	0.0097 (11)	0.0120 (11)	0.0097 (12)	0.0009 (9)	−0.0050 (10)	−0.0057 (10)
O6C	0.0080 (11)	0.0093 (11)	0.0123 (13)	0.0008 (9)	−0.0037 (10)	−0.0042 (10)
O7B	0.0110 (12)	0.0144 (12)	0.0137 (13)	0.0009 (9)	−0.0044 (10)	−0.0077 (11)
O8B	0.0111 (12)	0.0107 (11)	0.0127 (13)	0.0000 (9)	−0.0058 (10)	−0.0030 (10)
O9B	0.0109 (12)	0.0119 (11)	0.0117 (13)	−0.0029 (9)	−0.0027 (10)	−0.0035 (10)
O10B	0.0117 (12)	0.0141 (12)	0.0144 (13)	0.0036 (9)	−0.0056 (10)	−0.0075 (11)
O11B	0.0114 (12)	0.0088 (11)	0.0143 (13)	−0.0008 (9)	−0.0031 (10)	−0.0023 (10)
O12B	0.0120 (12)	0.0093 (11)	0.0131 (13)	−0.0008 (9)	−0.0048 (10)	−0.0031 (10)
O13T	0.0094 (12)	0.0129 (12)	0.0203 (14)	0.0008 (9)	−0.0046 (11)	−0.0078 (11)
O14T	0.0130 (12)	0.0136 (12)	0.0145 (13)	−0.0021 (9)	−0.0032 (11)	−0.0035 (11)
O15T	0.0126 (12)	0.0166 (13)	0.0163 (14)	−0.0034 (10)	−0.0034 (11)	−0.0011 (11)
O16T	0.0163 (13)	0.0204 (13)	0.0151 (14)	0.0005 (10)	−0.0063 (11)	−0.0073 (12)
O17T	0.0141 (13)	0.0159 (13)	0.0213 (15)	0.0034 (10)	−0.0081 (11)	−0.0062 (12)
O18T	0.0148 (12)	0.0164 (12)	0.0152 (13)	−0.0002 (10)	−0.0073 (11)	−0.0070 (11)
O19T	0.0142 (13)	0.0168 (13)	0.0248 (15)	0.0045 (10)	−0.0078 (12)	−0.0104 (12)
O20T	0.0145 (13)	0.0157 (13)	0.0159 (14)	−0.0030 (10)	−0.0029 (11)	−0.0017 (11)
O21T	0.0166 (14)	0.0163 (13)	0.0166 (15)	0.0011 (10)	−0.0012 (12)	−0.0012 (12)
O22T	0.0201 (13)	0.0196 (13)	0.0138 (13)	0.0042 (10)	−0.0092 (11)	−0.0097 (11)
O23T	0.0171 (13)	0.0144 (12)	0.0156 (14)	−0.0006 (10)	−0.0069 (11)	−0.0076 (11)
O24T	0.0108 (12)	0.0106 (11)	0.0152 (13)	0.0011 (9)	−0.0050 (10)	−0.0044 (10)
O1W	0.0324 (18)	0.041 (2)	0.0307 (19)	−0.0046 (15)	0.0027 (15)	−0.0203 (17)
O2W	0.099 (4)	0.088 (3)	0.026 (2)	0.072 (3)	−0.019 (2)	−0.023 (2)
O3W	0.0254 (16)	0.0216 (15)	0.044 (2)	−0.0014 (13)	−0.0079 (15)	−0.0178 (15)
O4W	0.0189 (14)	0.0273 (16)	0.0163 (15)	−0.0046 (12)	−0.0062 (12)	0.0009 (13)
O5W	0.0227 (15)	0.0132 (13)	0.0284 (17)	0.0015 (11)	−0.0129 (13)	−0.0091 (13)
O6W	0.051 (6)	0.054 (6)	0.037 (4)	0.030 (4)	−0.032 (4)	−0.018 (4)

Pt—O1C	1.979 (2)	Mo6—O5C	2.091 (2)
Pt—O2C	2.006 (2)	Mo6—O6C	2.286 (2)
Pt—O3C	2.034 (2)	Mo6—O11B	2.114 (2)
Pt—O4C	2.011 (2)	Mo6—O12B	1.840 (2)
Pt—O5C	1.992 (2)	Mo6—O23T	1.701 (2)
Pt—O6C	1.986 (2)	Mo6—O24T	1.756 (2)
Pt—Mo6	3.2149 (3)	K1—O10B	2.713 (3)
Mo1—Mo2	3.2140 (4)	K1—O14Ti	2.854 (3)
Mo1—O1C	2.118 (2)	K1—O17Tii	2.880 (3)
Mo1—O6C	2.329 (2)	K1—O1W	3.039 (4)
Mo1—O7B	1.951 (2)	K1—O3W	2.986 (3)
Mo1—O12B	1.984 (2)	K1—O4W	2.700 (3)
Mo1—O13T	1.742 (2)	K1—O4Wiii	2.815 (3)
Mo1—O14T	1.694 (2)	K2—O9Biv	2.574 (2)
Mo2—O1C	2.196 (2)	K2—O9B	2.574 (2)
Mo2—O2C	2.289 (2)	K2—O13Tv	3.128 (3)
Mo2—O7B	1.987 (2)	K2—O13Tvi	3.128 (3)
Mo2—O8B	1.927 (2)	K2—O18Tiv	3.149 (3)
Mo2—O15T	1.704 (2)	K2—O18T	3.149 (3)
Mo2—O16T	1.716 (3)	K2—O24Tvi	2.767 (2)
Mo3—O2C	2.326 (2)	K2—O24Tv	2.767 (2)
Mo3—O3C	2.273 (3)	K3—O8Bi	2.799 (2)
Mo3—O8B	1.936 (2)	K3—O15Ti	2.985 (3)
Mo3—O9B	1.936 (2)	K3—O16Tvii	2.983 (3)
Mo3—O17T	1.698 (2)	K3—O19Tviii	3.105 (3)
Mo3—O18T	1.721 (2)	K3—O22T	3.282 (3)
Mo4—O3C	2.285 (2)	K3—O23T	2.749 (3)
Mo4—O4C	2.323 (2)	K3—O2W	2.706 (4)
Mo4—O9B	1.923 (3)	K3—O5W	3.068 (3)
Mo4—O10B	1.950 (2)	K4—O16T	2.720 (3)
Mo4—O19T	1.697 (2)	K4—O18T	2.995 (3)
Mo4—O20T	1.707 (2)	K4—O20Tiv	2.702 (3)
Mo5—O4C	2.278 (3)	K4—O22Tix	2.744 (3)
Mo5—O5C	2.151 (2)	K4—O24Tv	2.883 (3)
Mo5—O10B	1.892 (2)	K4—O1Wix	2.756 (4)
Mo5—O11B	2.076 (2)	K4—O6Wx	2.866 (8)
Mo5—O21T	1.715 (2)	K4—O6W	2.687 (8)
Mo5—O22T	1.702 (2)	O6C—H6	1.28 (0)
O1C—Pt—O6C	83.77 (10)	O4W—K1—O3W	95.82 (9)
O1C—Pt—O5C	97.36 (10)	O10B—K1—O3W	71.65 (8)
O6C—Pt—O5C	83.63 (10)	O4Wiii—K1—O3W	136.06 (9)
O1C—Pt—O2C	82.44 (10)	O14Ti—K1—O3W	66.24 (8)
O6C—Pt—O2C	96.73 (10)	O17Tii—K1—O3W	82.07 (9)
O5C—Pt—O2C	179.57 (9)	O4W—K1—O1W	71.71 (9)
O1C—Pt—O4C	177.47 (9)	O10B—K1—O1W	72.44 (8)
O6C—Pt—O4C	98.47 (10)	O4Wiii—K1—O1W	102.34 (9)
O5C—Pt—O4C	81.74 (10)	O14Ti—K1—O1W	139.77 (9)
O2C—Pt—O4C	98.44 (10)	O17Tii—K1—O1W	145.67 (9)
O1C—Pt—O3C	95.90 (10)	O3W—K1—O1W	115.70 (9)
O6C—Pt—O3C	179.41 (9)	O9Biv—K2—O9B	180.000 (17)
O5C—Pt—O3C	96.90 (10)	O9B—K2—O24Tvi	83.34 (7)
O2C—Pt—O3C	82.74 (10)	O9B—K2—O24Tv	96.66 (7)
O4C—Pt—O3C	81.88 (10)	O9B—K2—O13Tvi	93.58 (7)
O14T—Mo1—O13T	105.35 (12)	O9B—K2—O18Tiv	123.48 (7)
O14T—Mo1—O7B	100.55 (11)	O9Biv—K2—O18T	123.48 (7)
O13T—Mo1—O7B	96.64 (11)	O9B—K2—O18T	56.52 (7)
O14T—Mo1—O12B	96.89 (11)	O24Tvi—K2—O18T	107.85 (7)
O13T—Mo1—O12B	96.56 (11)	O24Tv—K2—O18T	72.15 (7)
O7B—Mo1—O12B	154.46 (10)	O13Tv—K2—O18T	119.67 (6)
O14T—Mo1—O1C	96.38 (10)	O13Tvi—K2—O18T	60.33 (6)
O13T—Mo1—O1C	158.00 (10)	O18Tiv—K2—O18T	180.00 (14)
O7B—Mo1—O1C	75.67 (9)	O2W—K3—O23T	87.40 (12)
O12B—Mo1—O1C	84.01 (10)	O2W—K3—O8Bi	101.70 (15)
O14T—Mo1—O6C	165.54 (10)	O23T—K3—O8Bi	135.26 (8)
O13T—Mo1—O6C	86.23 (10)	O2W—K3—O16Tvii	68.29 (11)
O7B—Mo1—O6C	86.39 (10)	O23T—K3—O16Tvii	112.47 (8)
O12B—Mo1—O6C	72.78 (9)	O2W—K3—O15Ti	117.98 (11)
O1C—Mo1—O6C	72.89 (9)	O23T—K3—O15Ti	151.29 (8)
O15T—Mo2—O16T	106.40 (12)	O2W—K3—O5W	121.75 (11)
O15T—Mo2—O8B	98.22 (11)	O23T—K3—O5W	64.76 (7)
O16T—Mo2—O8B	100.68 (11)	O8Bi—K3—O5W	73.57 (7)
O15T—Mo2—O7B	101.30 (11)	O16Tvii—K3—O5W	168.39 (8)
O16T—Mo2—O7B	92.82 (11)	O15Ti—K3—O5W	107.09 (7)
O8B—Mo2—O7B	152.03 (10)	O2W—K3—O19Tviii	66.76 (11)
O15T—Mo2—O1C	92.44 (11)	O23T—K3—O19Tviii	63.34 (7)
O16T—Mo2—O1C	158.60 (10)	O5W—K3—O19Tviii	55.12 (7)
O8B—Mo2—O1C	86.22 (9)	O2W—K3—O22T	110.14 (14)
O7B—Mo2—O1C	73.19 (9)	O23T—K3—O22T	59.79 (7)
O15T—Mo2—O2C	161.42 (11)	O8Bi—K3—O22T	145.97 (7)
O16T—Mo2—O2C	91.12 (11)	O16Tvii—K3—O22T	71.25 (7)
O8B—Mo2—O2C	71.88 (9)	O15Ti—K3—O22T	96.63 (7)
O7B—Mo2—O2C	83.57 (9)	O5W—K3—O22T	98.56 (7)
O1C—Mo2—O2C	71.63 (9)	O19Tviii—K3—O22T	123.13 (7)
O17T—Mo3—O18T	106.56 (12)	O6W—K4—O20Tiv	86.85 (17)
O17T—Mo3—O8B	98.83 (11)	O6W—K4—O16T	100.30 (17)
O18T—Mo3—O8B	101.53 (11)	O20Tiv—K4—O16T	163.39 (9)
O17T—Mo3—O9B	101.37 (11)	O6W—K4—O22Tix	72.57 (17)
O18T—Mo3—O9B	97.67 (11)	O20Tiv—K4—O22Tix	112.52 (8)
O8B—Mo3—O9B	146.75 (10)	O16T—K4—O22Tix	84.01 (8)
O17T—Mo3—O3C	99.47 (11)	O6W—K4—O1Wix	125.74 (17)
O18T—Mo3—O3C	153.10 (10)	O20Tiv—K4—O1Wix	75.80 (9)
O8B—Mo3—O3C	80.67 (10)	O16T—K4—O1Wix	110.80 (9)
O9B—Mo3—O3C	70.18 (9)	O22Tix—K4—O1Wix	68.01 (9)
O17T—Mo3—O2C	166.65 (11)	O6W—K4—O6Wx	22.7 (3)
O18T—Mo3—O2C	84.31 (10)	O20Tiv—K4—O6Wx	109.37 (17)
O8B—Mo3—O2C	70.90 (9)	O16T—K4—O6Wx	77.87 (16)
O9B—Mo3—O2C	84.41 (10)	O22Tix—K4—O6Wx	66.98 (16)
O3C—Mo3—O2C	70.96 (9)	O1Wix—K4—O6Wx	132.79 (17)
O19T—Mo4—O20T	106.07 (13)	O6W—K4—O24Tv	97.28 (17)
O19T—Mo4—O9B	101.28 (12)	O20Tiv—K4—O24Tv	80.55 (8)
O20T—Mo4—O9B	98.83 (12)	O16T—K4—O24Tv	83.66 (8)
O19T—Mo4—O10B	98.77 (11)	O22Tix—K4—O24Tv	162.32 (8)
O20T—Mo4—O10B	100.44 (12)	O1Wix—K4—O24Tv	128.57 (9)
O9B—Mo4—O10B	147.02 (10)	O6Wx—K4—O24Tv	98.00 (16)
O19T—Mo4—O3C	95.89 (11)	O6W—K4—O18T	164.77 (16)
O20T—Mo4—O3C	157.14 (10)	O20Tiv—K4—O18T	102.64 (8)
O9B—Mo4—O3C	70.14 (9)	O16T—K4—O18T	67.51 (7)
O10B—Mo4—O3C	82.01 (10)	O22Tix—K4—O18T	113.50 (8)
O19T—Mo4—O4C	163.39 (11)	O1Wix—K4—O18T	68.76 (9)
O20T—Mo4—O4C	88.94 (11)	O6Wx—K4—O18T	144.85 (16)
O9B—Mo4—O4C	82.95 (10)	O24Tv—K4—O18T	72.99 (7)
O10B—Mo4—O4C	70.94 (9)	Pt—O1C—Mo1	105.46 (10)
O3C—Mo4—O4C	70.23 (9)	Pt—O1C—Mo2	104.98 (10)
O22T—Mo5—O21T	106.70 (13)	Mo1—O1C—Mo2	96.30 (9)
O22T—Mo5—O10B	101.84 (11)	Pt—O2C—Mo2	100.81 (10)
O21T—Mo5—O10B	102.99 (11)	Pt—O2C—Mo3	102.68 (10)
O22T—Mo5—O11B	97.58 (11)	Mo2—O2C—Mo3	92.77 (9)
O21T—Mo5—O11B	89.09 (11)	Pt—O3C—Mo3	103.60 (10)
O10B—Mo5—O11B	152.95 (10)	Pt—O3C—Mo4	104.25 (10)
O22T—Mo5—O5C	91.56 (11)	Mo3—O3C—Mo4	94.06 (9)
O21T—Mo5—O5C	154.90 (10)	Pt—O4C—Mo5	100.24 (10)
O10B—Mo5—O5C	89.52 (10)	Pt—O4C—Mo4	103.64 (10)
O11B—Mo5—O5C	71.17 (9)	Mo5—O4C—Mo4	92.53 (9)
O22T—Mo5—O4C	162.98 (11)	Pt—O5C—Mo6	103.86 (10)
O21T—Mo5—O4C	90.31 (11)	Pt—O5C—Mo5	105.34 (10)
O10B—Mo5—O4C	72.93 (9)	Mo6—O5C—Mo5	105.12 (10)
O11B—Mo5—O4C	83.03 (9)	Pt—O6C—Mo6	97.38 (10)
O5C—Mo5—O4C	72.45 (9)	Pt—O6C—Mo1	97.89 (10)
O23T—Mo6—O24T	104.61 (11)	Mo6—O6C—Mo1	90.69 (8)
O23T—Mo6—O12B	103.60 (11)	Mo1—O7B—Mo2	109.41 (11)
O24T—Mo6—O12B	103.93 (11)	Mo2—O8B—Mo3	119.78 (12)
O23T—Mo6—O5C	92.37 (11)	Mo2—O8B—K3i	101.44 (9)
O24T—Mo6—O5C	154.05 (10)	Mo3—O8B—K3i	137.03 (11)
O12B—Mo6—O5C	90.63 (10)	Mo4—O9B—Mo3	119.62 (12)
O23T—Mo6—O11B	93.94 (11)	Mo5—O10B—Mo4	119.84 (12)
O24T—Mo6—O11B	87.50 (10)	Mo5—O11B—Mo6	107.00 (11)
O12B—Mo6—O11B	155.64 (10)	Mo6—O12B—Mo1	118.20 (12)
O5C—Mo6—O11B	71.63 (9)	H1A—O1W—H1B	103 (4)
O23T—Mo6—O6C	166.81 (10)	H2A—O2W—H2B	105 (4)
O24T—Mo6—O6C	88.05 (10)	H3A—O3W—H3B	107 (3)
O12B—Mo6—O6C	76.34 (10)	H4A—O4W—H4B	109 (4)
O5C—Mo6—O6C	74.46 (9)	H5A—O5W—H5B	105 (3)
O11B—Mo6—O6C	82.73 (9)	H6A—O6W—H6B	101 (10)
O4W—K1—O10B	131.27 (9)

D—H···A	D—H	H···A	D···A	D—H···A
O2C—H2···O24Tv	0.87 (3)	1.70 (3)	2.561 (3)	168 (5)
O3C—H3···O5Wi	0.89 (3)	1.67 (3)	2.552 (4)	177 (5)
O4C—H4···O13Tv	0.89 (5)	1.67 (5)	2.562 (3)	176 (5)
O6C—H6···O6Cv	1.28	1.28	2.553 (3)	180
O11B—H11···O7Bv	0.90 (5)	1.93 (5)	2.826 (3)	172 (4)
O1W—H1A···O13Txi	0.84 (3)	2.27 (4)	3.014 (4)	149 (5)
O1W—H1B···O21Txii	0.89 (3)	2.22 (4)	3.067 (4)	159 (6)
O2W—H2A···O7Bvii	0.86 (3)	2.10 (4)	2.906 (5)	157 (7)
O2W—H2B···O21Txiii	0.83 (3)	2.49 (5)	3.038 (5)	125 (5)
O3W—H3A···O1Ci	0.86 (3)	2.01 (3)	2.811 (4)	154 (5)
O3W—H3B···O5C	0.83 (3)	2.24 (3)	2.973 (4)	147 (4)
O4W—H4A···O15Ti	0.81 (3)	2.03 (3)	2.839 (4)	175 (5)
O4W—H4B···O18Tvii	0.84 (3)	2.11 (3)	2.938 (4)	168 (4)
O5W—H5A···O19Tviii	0.86 (3)	2.14 (3)	2.856 (4)	141 (4)
O5W—H5B···O3Wi	0.83 (2)	1.99 (3)	2.787 (4)	160 (4)
O6W—H6A···O22Tv	0.85 (3)	2.41 (8)	3.097 (7)	138 (11)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2C—H2⋯O24Ti	0.87 (3)	1.70 (3)	2.561 (3)	168 (5)
O3C—H3⋯O5Wii	0.89 (3)	1.67 (3)	2.552 (4)	177 (5)
O4C—H4⋯O13Ti	0.89 (5)	1.67 (5)	2.562 (3)	176 (5)
O6C—H6⋯O6Ci	1.28	1.28	2.553 (3)	180
O11B—H11⋯O7Bi	0.90 (5)	1.93 (5)	2.826 (3)	172 (4)

Symmetry codes: (i) ; (ii) .