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The polyanion in K5[H2PtV9O28]·9H2O has approximate mm2 (C2v) symmetry. The two platinum-bound μ2-O atoms are protonated in the polyanion. The heteropolyanions form inversion-generated dimers, {[H2PtV9O28]2}10−, held together by μ2-O—H...μ2-O and μ2-O—H...μ3-O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989015009135/vn2093sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989015009135/vn2093Isup2.hkl
Contains datablock I

CCDC reference: 1400654

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](V-O) = 0.004 Å
  • R factor = 0.028
  • wR factor = 0.066
  • Data-to-parameter ratio = 12.9

checkCIF/PLATON results

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Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O9W - H9A .. Please Check
Author Response: : Because O9W cooordinated by three K+ ions.

Alert level C PLAT975_ALERT_2_C Check Calcd Residual Density 0.91A From O3W 0.53 eA-3 PLAT976_ALERT_2_C Check Calcd Residual Density 0.74A From O6W -0.49 eA-3
Alert level G PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 26 Note PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 2 Report PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 7 Report PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 25 Note PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 3 Note
0 ALERT level A = Most likely a serious problem - resolve or explain 1 ALERT level B = A potentially serious problem, consider carefully 2 ALERT level C = Check. Ensure it is not caused by an omission or oversight 5 ALERT level G = General information/check it is not something unexpected 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Structural commentary top

Two heteropolyanions that belong to the decavanadate structure system (Lee, 2006) have recently been reported: the tellurium derivative [HnTeV9O28](5-n) (n = 1 and 2), described by Konaka et al. (2011), and the platinum heteropolyoxovanadate, [H2PtV9O28]5-, reported by our group in the form of its sodium salt, Na5[H2PtV9O28]·21H2O (Lee et al., 2008) and a guanidinium salt, (CH6N3)5 [H2PtV9O28] (Joo et al., 2011). The Te heteroatom of the [HnTeV9O28](5-n) polyanion was located on two sites (corresponding to the Pt1 and V4 sites in the title compound) by disorder. However, the Pt atom does not show any disorder in three [H2PtV9O28]5- polyanions. We herein report the structure of the title compound because it could contribute to our knowledge of the structural characteristics of the [H2PtV9O28]5- polyanion.

Fig. 1 shows the structure of the title compound. The O atoms of the clusters were designated as OT (terminal, MoO), OB (bridging, µ2-O), OC3-O), and OD4-O). All atoms in the polyanions were located in general positions. The protonated OB atoms in the polyanions were identified by the locations in the difference Fourier maps of the H atoms bound to atoms O7B and O8B and local structural features, as seen previously in sodium and guanidinium salts, respectively. The geometry of the anion agrees well with that in sodium and guanidinium salts. The nine [VO6] o­cta­hedra in the polyanion are distorted [range of V—O distances = 1.596 (3)–2.403 (3) Å], while the [PtO6] o­cta­hedron is relatively regular [Pt—O = 1.985 (3)–2.036 (3) Å]. The two platinum bound µ2-O atoms are protonated in the polyanion. These protons are particularly important in the solid state as they lead to the formation of a dimeric assembly, {[H2PtV9O28]2}10-, through each of the two µ2-O7B–H7···µ2-O19B and µ2-O8B–H8···µ3-O4C inter­anion hydrogen bonds (Fig. 2 and Table 1).

The K+ ions are variously coordinated by O atoms as [K1(OB)(OT)2(OW)5]+ in the range 2.725 (5)–3.351 (6) Å, [K2(OB)2(OT)3(OW)3]+ in the range 2.722 (4)–3.156 (5) Å, [K3(OB)(OT)4(OW)4]+ in the range 2.844 (4)–3.151 (3) Å, [K4(OB)(OT)2(OW)4]+ in the range 2.733 (5)–3.284 (7) Å, and [K5(OB)2(OT)2(OW)3]+ in the range 2.734 (6)–2.996 (4) Å. The bond-valence sums (BVS; Brown & Altermatt, 1985; Brese & O'Keeffe, 1991) for the K1, K2, K3, K4, and K5 ions are 0.99, 1.12,1.04, 0.81, and 1.10 v.u, respectively (total v.u. = 5.06).

The polyanion dimers are three dimensionally linked via K···OT and K···OB inter­actions. All water molecules form hydrogen bonds with polyanions except for the O3W and O9W water molecules. (Table 1).

Synthesis and crystallization top

Single crystals of the title compound were obtained in the same way as the sodium salt reported by Lee et al. (2008) using K2Pt(OH)6 and KVO3.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 2. Atoms H7 and H8, bound to µ2-O7B and µ2-O8B, respectively, of the polyanion were found in a difference Fourier map and were freely refined. The H atoms of the O6W molecule were positioned geometrically and refined using a riding model (HFIX 23), with O—H = 0.97 Å and Uiso(H) = 1.5 Ueq(O). All other water H atoms were refined with distance restraints of O—H = 0.85 (3) Å and HA···HB = 1.35 (3) Å using the SHELXL2014 command DFIX, and were included in the refinement with Uiso(H) = 1.5 Ueq(O). The unusually short µ2-O17B···terminal-O21Ti distance of 2.949 (5) Å (symmetry code as in Fig. 2.) is caused by the neighboring hydrogen bonds between the polyanions of the dimer as shown in Fig. 2. The highest peak in the difference map is 0.95 Å from K4 and the largest hole is 0.92 Å from Pt1.

Related literature top

For a structural study of decavanadate, see: Lee (2006). For the structure of the sodium and guanidinium salts of the title compound, see: (Lee et al., 2008) & (Joo et al., 2011). For the related heteropolyoxometalate TBA4[HTeV9O28].2CH3CN, see: Konaka et al. (2011).

Computing details top

Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4 (Stoe & Cie, 1996); data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS2014 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms are presented as small spheres of arbitrary radius.
[Figure 2] Fig. 2. Polyhedral view of the inter-anion hydrogen bonds (dotted lines) in the crystal structure of the title compound. [Symmetry code: (i) -x, -y + 1, -z.]
Pentapotassium dihydrogen nonavanadato(V)platinate(IV) nonahydrate top
Crystal data top
K5[H2PtV9O28]·9H2OZ = 2
Mr = 1461.21F(000) = 1392
Triclinic, P1Dx = 2.949 Mg m3
a = 10.1663 (7) ÅMo Kα radiation, λ = 0.71069 Å
b = 12.8350 (7) ÅCell parameters from 30 reflections
c = 13.615 (2) Åθ = 9.6–10.5°
α = 103.734 (5)°µ = 7.42 mm1
β = 106.193 (6)°T = 298 K
γ = 92.480 (4)°Block, dark brown
V = 1645.8 (3) Å30.21 × 0.19 × 0.17 mm
Data collection top
Stoe Stadi4
diffractometer
Rint = 0.0000
Radiation source: fine-focus sealed tubeθmax = 26.5°, θmin = 1.6°
ω/2–θ scansh = 1212
Absorption correction: empirical (using intensity measurements)
(X-SHAPE; Stoe & Cie,1996)
k = 1615
Tmin = 0.301, Tmax = 0.378l = 017
6797 measured reflections3 standard reflections every 60 min
6797 independent reflections intensity decay: 2.5%
6242 reflections with I > 2σ(I)
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.066 w = 1/[σ2(Fo2) + (0.0277P)2 + 4.5476P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
6797 reflectionsΔρmax = 1.30 e Å3
526 parametersΔρmin = 1.46 e Å3
25 restraintsExtinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00505 (13)
Crystal data top
K5[H2PtV9O28]·9H2Oγ = 92.480 (4)°
Mr = 1461.21V = 1645.8 (3) Å3
Triclinic, P1Z = 2
a = 10.1663 (7) ÅMo Kα radiation
b = 12.8350 (7) ŵ = 7.42 mm1
c = 13.615 (2) ÅT = 298 K
α = 103.734 (5)°0.21 × 0.19 × 0.17 mm
β = 106.193 (6)°
Data collection top
Stoe Stadi4
diffractometer
6242 reflections with I > 2σ(I)
Absorption correction: empirical (using intensity measurements)
(X-SHAPE; Stoe & Cie,1996)
Rint = 0.0000
Tmin = 0.301, Tmax = 0.3783 standard reflections every 60 min
6797 measured reflections intensity decay: 2.5%
6797 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02825 restraints
wR(F2) = 0.066H atoms treated by a mixture of independent and constrained refinement
S = 1.10Δρmax = 1.30 e Å3
6797 reflectionsΔρmin = 1.46 e Å3
526 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pt10.07476 (2)0.66204 (2)0.15945 (2)0.01102 (6)
V10.08091 (8)0.74803 (6)0.03864 (6)0.01675 (16)
V20.05610 (8)0.57644 (6)0.35482 (6)0.01798 (16)
V30.36393 (8)0.67118 (6)0.46862 (6)0.01860 (17)
V40.38427 (7)0.76066 (6)0.27828 (6)0.01375 (15)
V50.38558 (8)0.84633 (6)0.08300 (6)0.01680 (16)
V60.15181 (8)0.90837 (6)0.19135 (6)0.01625 (16)
V70.14522 (8)0.82358 (6)0.38572 (6)0.01838 (17)
V80.28571 (8)0.50931 (6)0.24210 (6)0.01521 (16)
V90.30124 (8)0.59746 (6)0.04752 (6)0.01441 (15)
K10.19325 (16)0.94505 (11)0.81002 (11)0.0433 (3)
K20.32640 (13)0.27185 (9)0.99666 (11)0.0329 (3)
K30.29033 (13)0.19821 (10)0.25987 (10)0.0353 (3)
K40.1688 (2)0.15936 (14)0.5300 (2)0.0819 (7)
K50.33393 (14)0.48579 (12)0.61615 (13)0.0439 (3)
O1D0.2234 (3)0.7454 (2)0.1318 (2)0.0148 (6)
O2D0.2133 (3)0.6723 (2)0.2981 (2)0.0148 (6)
O3C0.0321 (3)0.8071 (2)0.2320 (2)0.0156 (6)
O4C0.1590 (3)0.5298 (2)0.1039 (2)0.0137 (6)
O5C0.2793 (3)0.8770 (2)0.3209 (2)0.0165 (6)
O6C0.3986 (3)0.6174 (2)0.2014 (2)0.0147 (6)
O7B0.0627 (3)0.5793 (3)0.2053 (3)0.0159 (6)
H70.086 (8)0.519 (6)0.152 (6)0.07 (2)*
O8B0.0508 (3)0.6659 (3)0.0160 (3)0.0168 (7)
H80.067 (6)0.609 (5)0.023 (5)0.021 (15)*
O9B0.2105 (3)0.5994 (3)0.4730 (3)0.0202 (7)
O10B0.4757 (3)0.7538 (3)0.3997 (3)0.0207 (7)
O11B0.4856 (3)0.8317 (3)0.2321 (3)0.0179 (7)
O12B0.2409 (3)0.8257 (3)0.0358 (3)0.0197 (7)
O13B0.0439 (3)0.8680 (2)0.0548 (3)0.0182 (7)
O14B0.3033 (3)0.9526 (2)0.1585 (3)0.0174 (6)
O15B0.2871 (3)0.8035 (3)0.4919 (3)0.0215 (7)
O16B0.0221 (3)0.7196 (3)0.3937 (3)0.0204 (7)
O17B0.1402 (3)0.4691 (2)0.2815 (3)0.0176 (6)
O18B0.4015 (3)0.5523 (3)0.3774 (3)0.0184 (7)
O19B0.1590 (3)0.6178 (2)0.0635 (2)0.0158 (6)
O20B0.4224 (3)0.7028 (3)0.0424 (3)0.0179 (7)
O21T0.0224 (4)0.7505 (3)0.1503 (3)0.0270 (8)
O22T0.0570 (4)0.5099 (3)0.3842 (3)0.0257 (8)
O23T0.4743 (4)0.6778 (3)0.5812 (3)0.0287 (8)
O24T0.5067 (3)0.9142 (3)0.0618 (3)0.0238 (7)
O25T0.0976 (4)1.0199 (3)0.2403 (3)0.0245 (7)
O26T0.0934 (4)0.9340 (3)0.4384 (3)0.0301 (8)
O27T0.3379 (4)0.3970 (3)0.1941 (3)0.0237 (7)
O28T0.3493 (4)0.4863 (3)0.0055 (3)0.0234 (7)
O1W0.1060 (6)0.7552 (4)0.6420 (4)0.0514 (12)
H1A0.154 (8)0.721 (6)0.681 (5)0.077*
H1B0.133 (8)0.750 (7)0.589 (4)0.077*
O2W0.3763 (6)0.9426 (4)0.6891 (4)0.0618 (15)
H2A0.347 (9)0.908 (6)0.623 (3)0.093*
H2B0.428 (8)0.997 (5)0.688 (6)0.093*
O3W0.2228 (5)0.1440 (4)0.7752 (6)0.0660 (17)
H3A0.143 (5)0.161 (7)0.775 (8)0.099*
H3B0.268 (7)0.197 (5)0.770 (8)0.099*
O4W0.2138 (4)0.0846 (3)0.0168 (4)0.0356 (9)
H4A0.132 (4)0.097 (5)0.007 (6)0.053*
H4B0.224 (6)0.029 (4)0.038 (6)0.053*
O5W0.5107 (5)0.1657 (4)0.1656 (4)0.0495 (12)
H5A0.550 (8)0.130 (5)0.210 (4)0.074*
H5B0.481 (8)0.120 (5)0.106 (3)0.074*
O6W0.3583 (5)0.0913 (4)0.4279 (4)0.0552 (13)
H6A0.34630.01340.40060.083*
H6B0.45200.11480.47370.083*
O7W0.3045 (5)0.3465 (4)0.7411 (4)0.0471 (12)
H7A0.242 (5)0.367 (6)0.769 (6)0.071*
H7B0.373 (5)0.394 (5)0.774 (6)0.071*
O8W0.3022 (6)0.6482 (5)0.7759 (4)0.0634 (15)
H8A0.375 (6)0.694 (6)0.797 (6)0.095*
H8B0.287 (9)0.645 (7)0.834 (4)0.095*
O9W0.1770 (7)0.3233 (4)0.4164 (5)0.0629 (15)
H9A0.265 (3)0.341 (8)0.444 (7)0.094*
H9B0.159 (8)0.357 (7)0.368 (5)0.094*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.00977 (9)0.00941 (9)0.01224 (9)0.00006 (5)0.00238 (6)0.00097 (6)
V10.0165 (4)0.0157 (4)0.0161 (4)0.0005 (3)0.0017 (3)0.0046 (3)
V20.0159 (4)0.0202 (4)0.0177 (4)0.0023 (3)0.0051 (3)0.0053 (3)
V30.0183 (4)0.0199 (4)0.0148 (4)0.0021 (3)0.0010 (3)0.0047 (3)
V40.0120 (3)0.0126 (3)0.0144 (4)0.0016 (3)0.0020 (3)0.0019 (3)
V50.0162 (4)0.0151 (4)0.0194 (4)0.0013 (3)0.0058 (3)0.0050 (3)
V60.0182 (4)0.0106 (3)0.0187 (4)0.0017 (3)0.0048 (3)0.0022 (3)
V70.0231 (4)0.0151 (4)0.0160 (4)0.0024 (3)0.0076 (3)0.0000 (3)
V80.0168 (4)0.0121 (3)0.0162 (4)0.0025 (3)0.0041 (3)0.0036 (3)
V90.0158 (4)0.0120 (3)0.0157 (4)0.0015 (3)0.0060 (3)0.0026 (3)
K10.0556 (9)0.0407 (7)0.0386 (7)0.0112 (6)0.0207 (7)0.0109 (6)
K20.0380 (7)0.0222 (6)0.0465 (7)0.0055 (5)0.0257 (6)0.0078 (5)
K30.0327 (6)0.0355 (7)0.0352 (7)0.0054 (5)0.0075 (5)0.0090 (5)
K40.1103 (16)0.0426 (9)0.1207 (18)0.0171 (10)0.0879 (15)0.0091 (10)
K50.0328 (7)0.0496 (8)0.0667 (10)0.0148 (6)0.0246 (7)0.0346 (7)
O1D0.0146 (15)0.0120 (14)0.0172 (16)0.0012 (12)0.0047 (12)0.0033 (12)
O2D0.0153 (15)0.0137 (15)0.0126 (15)0.0033 (12)0.0026 (12)0.0010 (12)
O3C0.0157 (15)0.0128 (15)0.0167 (16)0.0019 (12)0.0059 (12)0.0007 (12)
O4C0.0136 (14)0.0106 (14)0.0153 (15)0.0004 (11)0.0036 (12)0.0017 (12)
O5C0.0169 (15)0.0136 (15)0.0161 (15)0.0002 (12)0.0028 (12)0.0012 (12)
O6C0.0128 (14)0.0135 (15)0.0153 (15)0.0002 (12)0.0012 (12)0.0030 (12)
O7B0.0159 (15)0.0150 (16)0.0159 (16)0.0004 (12)0.0051 (13)0.0022 (13)
O8B0.0147 (15)0.0162 (17)0.0156 (16)0.0006 (13)0.0005 (13)0.0031 (14)
O9B0.0221 (17)0.0206 (17)0.0169 (16)0.0022 (13)0.0055 (13)0.0040 (13)
O10B0.0194 (16)0.0191 (16)0.0205 (17)0.0027 (13)0.0026 (13)0.0044 (13)
O11B0.0142 (15)0.0180 (16)0.0204 (17)0.0025 (12)0.0038 (13)0.0049 (13)
O12B0.0243 (17)0.0174 (16)0.0179 (16)0.0010 (13)0.0055 (14)0.0069 (13)
O13B0.0162 (15)0.0129 (15)0.0236 (17)0.0007 (12)0.0031 (13)0.0050 (13)
O14B0.0187 (16)0.0124 (15)0.0210 (17)0.0007 (12)0.0061 (13)0.0041 (13)
O15B0.0273 (18)0.0197 (17)0.0141 (16)0.0007 (14)0.0062 (14)0.0017 (13)
O16B0.0226 (17)0.0192 (16)0.0204 (17)0.0025 (13)0.0107 (14)0.0018 (13)
O17B0.0190 (16)0.0142 (15)0.0185 (16)0.0015 (12)0.0049 (13)0.0039 (13)
O18B0.0169 (15)0.0173 (16)0.0185 (16)0.0016 (12)0.0009 (13)0.0052 (13)
O19B0.0167 (15)0.0144 (15)0.0138 (15)0.0029 (12)0.0022 (12)0.0014 (12)
O20B0.0180 (16)0.0178 (16)0.0200 (17)0.0031 (13)0.0085 (13)0.0054 (13)
O21T0.0298 (19)0.0255 (18)0.0220 (18)0.0016 (15)0.0007 (15)0.0075 (15)
O22T0.0233 (18)0.0306 (19)0.0266 (19)0.0029 (15)0.0109 (15)0.0106 (15)
O23T0.0287 (19)0.033 (2)0.0186 (18)0.0072 (16)0.0024 (15)0.0079 (15)
O24T0.0224 (17)0.0224 (17)0.0281 (19)0.0033 (14)0.0091 (15)0.0086 (15)
O25T0.0245 (18)0.0164 (16)0.032 (2)0.0048 (14)0.0081 (15)0.0041 (14)
O26T0.039 (2)0.0213 (18)0.029 (2)0.0061 (16)0.0154 (17)0.0020 (15)
O27T0.0264 (18)0.0180 (17)0.0283 (19)0.0074 (14)0.0085 (15)0.0077 (14)
O28T0.0278 (18)0.0164 (16)0.0277 (19)0.0037 (14)0.0130 (15)0.0034 (14)
O1W0.066 (3)0.050 (3)0.041 (3)0.008 (2)0.025 (3)0.007 (2)
O2W0.080 (4)0.056 (3)0.035 (3)0.024 (3)0.017 (3)0.010 (2)
O3W0.028 (2)0.058 (3)0.126 (5)0.013 (2)0.028 (3)0.044 (4)
O4W0.028 (2)0.035 (2)0.054 (3)0.0107 (17)0.0133 (19)0.027 (2)
O5W0.052 (3)0.041 (3)0.049 (3)0.008 (2)0.013 (2)0.004 (2)
O6W0.051 (3)0.034 (2)0.056 (3)0.011 (2)0.003 (2)0.014 (2)
O7W0.030 (2)0.043 (3)0.078 (4)0.0107 (19)0.023 (2)0.025 (2)
O8W0.080 (4)0.066 (4)0.042 (3)0.016 (3)0.028 (3)0.002 (3)
O9W0.095 (4)0.051 (3)0.056 (3)0.025 (3)0.029 (3)0.028 (3)
Geometric parameters (Å, º) top
Pt1—V63.1213 (8)V8—O27T1.612 (3)
Pt1—V83.1262 (8)V8—O17B1.803 (3)
Pt1—V93.1359 (8)V8—O18B1.826 (3)
Pt1—V73.1480 (9)V8—O6C2.033 (3)
Pt1—V43.1566 (8)V8—O4C2.045 (3)
Pt1—V23.1574 (9)V8—O2D2.278 (3)
V1—V53.1204 (11)V9—O28T1.601 (3)
V1—V63.1801 (11)V9—O20B1.816 (3)
V1—V93.1802 (11)V9—O19B1.856 (3)
V2—V33.1217 (11)V9—O6C2.001 (3)
V2—V73.1566 (11)V9—O4C2.064 (3)
V2—V83.1767 (11)V9—O1D2.270 (3)
V2—V44.4982 (11)K1—O3Wi2.725 (5)
V3—V43.1255 (11)K1—O2W2.804 (6)
V3—V83.1476 (11)K1—O1W2.827 (5)
V3—V73.1731 (11)K1—O12Bii2.830 (3)
V4—V53.1120 (11)K1—O4Wiii2.903 (5)
V4—V93.1960 (11)K1—O25Tiv2.924 (4)
V4—V73.2078 (11)K1—O24Tv3.267 (4)
V4—V83.2162 (10)K1—O5Wvi3.351 (6)
V5—V93.1578 (10)K2—O4Wii2.722 (4)
V5—V63.1654 (11)K2—O27Tii2.753 (4)
V6—V73.1068 (12)K2—O28Tii2.760 (3)
V8—V93.1566 (11)K2—O20Bvi2.772 (3)
Pt1—O1D1.985 (3)K2—O8Bvii2.917 (3)
Pt1—O2D1.986 (3)K2—O3W2.936 (7)
Pt1—O4C2.015 (3)K2—O24Tvi3.069 (4)
Pt1—O3C2.017 (3)K2—O5Wii3.156 (5)
Pt1—O8B2.027 (3)K3—O23Tvi2.844 (4)
Pt1—O7B2.036 (3)K3—O25Tviii2.860 (4)
V1—O21T1.598 (3)K3—O5W2.876 (5)
V1—O12B1.857 (3)K3—O6W2.878 (6)
V1—O13B1.876 (3)K3—O9W2.890 (6)
V1—O19B1.880 (3)K3—O21Tix2.904 (4)
V1—O8B2.064 (3)K3—O27T2.960 (4)
V1—O1D2.377 (3)K3—O4W3.139 (5)
V2—O22T1.596 (3)K3—O14Bviii3.151 (3)
V2—O9B1.862 (3)K4—O6W2.733 (5)
V2—O16B1.863 (3)K4—O16Bvii2.806 (4)
V2—O17B1.885 (3)K4—O26Tviii2.841 (4)
V2—O7B2.067 (3)K4—O9W2.904 (5)
V2—O2D2.374 (3)K4—O26Tvii3.055 (4)
V3—O23T1.608 (3)K4—O7W3.187 (6)
V3—O9B1.800 (3)K4—O3W3.284 (7)
V3—O18B1.853 (3)K5—O8W2.734 (6)
V3—O15B1.895 (3)K5—O18Bvi2.736 (3)
V3—O10B2.064 (3)K5—O9B2.764 (4)
V3—O2D2.403 (3)K5—O7W2.803 (5)
V4—O10B1.681 (3)K5—O22Tvii2.817 (4)
V4—O11B1.685 (3)K5—O9W2.982 (7)
V4—O6C1.921 (3)K5—O23T2.996 (4)
V4—O5C1.943 (3)O7B—H70.90 (8)
V4—O2D2.148 (3)O8B—H80.77 (6)
V4—O1D2.158 (3)O1W—H1A0.84 (3)
V5—O24T1.607 (3)O1W—H1B0.83 (3)
V5—O12B1.813 (3)O2W—H2A0.87 (3)
V5—O20B1.878 (3)O2W—H2B0.86 (3)
V5—O14B1.879 (3)O3W—H3A0.84 (3)
V5—O11B2.058 (3)O3W—H3B0.83 (3)
V5—O1D2.381 (3)O4W—H4A0.83 (3)
V6—O25T1.617 (3)O4W—H4B0.83 (3)
V6—O13B1.812 (3)O5W—H5A0.87 (3)
V6—O14B1.824 (3)O5W—H5B0.84 (3)
V6—O3C2.014 (3)O6W—H6A0.9700
V6—O5C2.015 (3)O6W—H6B0.9700
V6—O1D2.284 (3)O7W—H7A0.85 (3)
V7—O26T1.610 (3)O7W—H7B0.84 (3)
V7—O15B1.812 (3)O8W—H8A0.86 (3)
V7—O16B1.832 (3)O8W—H8B0.86 (3)
V7—O5C1.997 (3)O9W—H9A0.87 (3)
V7—O3C2.043 (3)O9W—H9B0.85 (3)
V7—O2D2.269 (3)
O1D—Pt1—O2D84.61 (12)Pt1—V4—V858.745 (19)
O1D—Pt1—O4C85.94 (12)V9—V4—V858.98 (2)
O2D—Pt1—O4C85.94 (12)V7—V4—V889.47 (3)
O1D—Pt1—O3C85.44 (12)V4—V5—V192.76 (3)
O2D—Pt1—O3C84.79 (12)V4—V5—V961.29 (2)
O4C—Pt1—O3C167.89 (12)V1—V5—V960.86 (2)
O1D—Pt1—O8B88.49 (13)V4—V5—V662.06 (2)
O2D—Pt1—O8B172.89 (13)V1—V5—V660.78 (3)
O4C—Pt1—O8B95.27 (13)V9—V5—V691.58 (3)
O3C—Pt1—O8B92.99 (13)V4—V5—Pt146.338 (17)
O1D—Pt1—O7B173.32 (13)V1—V5—Pt146.428 (18)
O2D—Pt1—O7B88.75 (12)V9—V5—Pt145.928 (17)
O4C—Pt1—O7B94.36 (12)V6—V5—Pt145.659 (17)
O3C—Pt1—O7B93.22 (13)V7—V6—Pt160.72 (2)
O8B—Pt1—O7B98.12 (13)V7—V6—V5118.88 (3)
O1D—Pt1—V646.91 (9)Pt1—V6—V587.85 (2)
O2D—Pt1—V688.79 (9)V7—V6—V1120.95 (3)
O4C—Pt1—V6132.85 (9)Pt1—V6—V160.23 (2)
O3C—Pt1—V639.21 (9)V5—V6—V158.91 (2)
O8B—Pt1—V685.25 (10)V6—V7—V3120.25 (3)
O7B—Pt1—V6132.36 (9)Pt1—V7—V387.79 (2)
O1D—Pt1—V889.65 (9)V2—V7—V359.10 (2)
O2D—Pt1—V846.63 (9)V6—V7—V461.64 (2)
O4C—Pt1—V840.00 (9)Pt1—V7—V459.55 (2)
O3C—Pt1—V8131.42 (9)V2—V7—V489.94 (3)
O8B—Pt1—V8135.22 (10)V3—V7—V458.66 (2)
O7B—Pt1—V886.34 (9)Pt1—V8—V388.63 (2)
V6—Pt1—V8123.63 (2)Pt1—V8—V959.88 (2)
O1D—Pt1—V946.16 (9)V3—V8—V9119.00 (3)
O2D—Pt1—V989.07 (9)V3—V8—V259.15 (2)
O4C—Pt1—V940.35 (9)V9—V8—V2120.00 (3)
O3C—Pt1—V9131.59 (9)V3—V8—V458.82 (2)
O8B—Pt1—V987.36 (10)V9—V8—V460.19 (2)
O7B—Pt1—V9134.69 (9)V2—V8—V489.43 (3)
V6—Pt1—V992.83 (2)Pt1—V9—V859.58 (2)
V8—Pt1—V960.54 (2)Pt1—V9—V587.73 (2)
O1D—Pt1—V788.61 (9)V8—V9—V5119.42 (3)
O2D—Pt1—V745.87 (9)Pt1—V9—V160.07 (2)
O4C—Pt1—V7131.81 (9)V8—V9—V1119.64 (3)
O3C—Pt1—V739.46 (9)V5—V9—V158.99 (2)
O8B—Pt1—V7132.43 (10)Pt1—V9—V459.80 (2)
O7B—Pt1—V786.22 (9)V8—V9—V460.83 (2)
V6—Pt1—V759.41 (2)V5—V9—V458.65 (2)
V8—Pt1—V792.22 (2)V1—V9—V490.08 (3)
V9—Pt1—V7122.21 (2)O3Wi—K1—O2W71.45 (18)
O1D—Pt1—V442.45 (9)O3Wi—K1—O1W122.0 (2)
O2D—Pt1—V442.16 (9)O2W—K1—O1W73.89 (15)
O4C—Pt1—V484.02 (8)O3Wi—K1—O12Bii145.45 (18)
O3C—Pt1—V483.88 (9)O2W—K1—O12Bii118.85 (16)
O8B—Pt1—V4130.94 (9)O1W—K1—O12Bii92.12 (13)
O7B—Pt1—V4130.91 (9)O3Wi—K1—O4Wiii78.75 (18)
V6—Pt1—V462.06 (2)O2W—K1—O4Wiii128.72 (14)
V8—Pt1—V461.58 (2)O1W—K1—O4Wiii155.55 (14)
V9—Pt1—V461.05 (2)O12Bii—K1—O4Wiii69.55 (10)
V7—Pt1—V461.17 (2)O3Wi—K1—O25Tiv82.50 (12)
O1D—Pt1—V2133.30 (9)O2W—K1—O25Tiv129.92 (16)
O2D—Pt1—V248.70 (9)O1W—K1—O25Tiv85.91 (13)
O4C—Pt1—V290.75 (9)O12Bii—K1—O25Tiv106.98 (11)
O3C—Pt1—V288.98 (9)O4Wiii—K1—O25Tiv84.34 (11)
O8B—Pt1—V2138.14 (9)O3Wi—K1—O24Tv65.13 (14)
O7B—Pt1—V240.05 (9)O2W—K1—O24Tv65.37 (12)
V6—Pt1—V2119.45 (2)O1W—K1—O24Tv133.36 (13)
V8—Pt1—V260.73 (2)O12Bii—K1—O24Tv88.44 (10)
V9—Pt1—V2121.27 (2)O4Wiii—K1—O24Tv64.45 (10)
V7—Pt1—V260.08 (2)O25Tiv—K1—O24Tv138.04 (10)
V4—Pt1—V290.86 (2)O3Wi—K1—O5Wvi110.45 (14)
O21T—V1—O12B102.27 (17)O2W—K1—O5Wvi51.31 (16)
O21T—V1—O13B102.73 (17)O1W—K1—O5Wvi79.54 (14)
O12B—V1—O13B90.13 (14)O12Bii—K1—O5Wvi67.77 (12)
O21T—V1—O19B105.72 (16)O4Wiii—K1—O5Wvi106.58 (12)
O12B—V1—O19B91.05 (14)O25Tiv—K1—O5Wvi164.20 (12)
O13B—V1—O19B150.57 (14)O24Tv—K1—O5Wvi57.73 (10)
O21T—V1—O8B99.44 (16)O4Wii—K2—O27Tii96.79 (13)
O12B—V1—O8B158.14 (14)O4Wii—K2—O28Tii157.70 (12)
O13B—V1—O8B82.64 (14)O27Tii—K2—O28Tii71.43 (10)
O19B—V1—O8B85.45 (14)O4Wii—K2—O20Bvi124.36 (11)
O21T—V1—O1D176.60 (16)O27Tii—K2—O20Bvi110.65 (11)
O12B—V1—O1D80.42 (12)O28Tii—K2—O20Bvi77.91 (10)
O13B—V1—O1D75.06 (12)O4Wii—K2—O8Bvii82.79 (11)
O19B—V1—O1D76.16 (12)O27Tii—K2—O8Bvii73.02 (10)
O8B—V1—O1D77.79 (12)O28Tii—K2—O8Bvii75.73 (10)
O22T—V2—O9B103.62 (17)O20Bvi—K2—O8Bvii150.46 (10)
O22T—V2—O16B104.45 (17)O4Wii—K2—O3W78.19 (15)
O9B—V2—O16B91.43 (15)O27Tii—K2—O3W162.23 (13)
O22T—V2—O17B104.04 (17)O28Tii—K2—O3W107.12 (13)
O9B—V2—O17B88.97 (14)O20Bvi—K2—O3W85.81 (12)
O16B—V2—O17B150.56 (14)O8Bvii—K2—O3W89.37 (12)
O22T—V2—O7B97.56 (16)O4Wii—K2—O24Tvi69.29 (11)
O9B—V2—O7B158.78 (14)O27Tii—K2—O24Tvi128.86 (11)
O16B—V2—O7B84.50 (14)O28Tii—K2—O24Tvi132.88 (10)
O17B—V2—O7B84.59 (13)O20Bvi—K2—O24Tvi55.63 (9)
O22T—V2—O2D175.77 (15)O8Bvii—K2—O24Tvi145.32 (10)
O9B—V2—O2D80.53 (13)O3W—K2—O24Tvi65.65 (11)
O16B—V2—O2D76.07 (13)O4Wii—K2—O5Wii63.16 (12)
O17B—V2—O2D74.97 (12)O27Tii—K2—O5Wii72.57 (12)
O7B—V2—O2D78.27 (11)O28Tii—K2—O5Wii126.96 (12)
O23T—V3—O9B104.10 (17)O20Bvi—K2—O5Wii79.90 (12)
O23T—V3—O18B104.12 (17)O8Bvii—K2—O5Wii127.23 (12)
O9B—V3—O18B92.55 (15)O3W—K2—O5Wii118.55 (13)
O23T—V3—O15B103.56 (18)O24Tvi—K2—O5Wii57.03 (11)
O9B—V3—O15B90.80 (15)O23Tvi—K3—O25Tviii136.47 (11)
O18B—V3—O15B150.37 (14)O23Tvi—K3—O5W75.77 (13)
O23T—V3—O10B101.92 (16)O25Tviii—K3—O5W120.42 (12)
O9B—V3—O10B153.94 (14)O23Tvi—K3—O6W72.84 (12)
O18B—V3—O10B82.41 (14)O25Tviii—K3—O6W64.17 (12)
O15B—V3—O10B81.76 (14)O5W—K3—O6W104.30 (15)
O23T—V3—O2D174.90 (16)O23Tvi—K3—O9W76.16 (15)
O9B—V3—O2D80.92 (13)O25Tviii—K3—O9W87.40 (14)
O18B—V3—O2D76.28 (12)O5W—K3—O9W150.12 (16)
O15B—V3—O2D75.21 (12)O6W—K3—O9W76.75 (14)
O10B—V3—O2D73.04 (12)O23Tvi—K3—O21Tix133.79 (11)
O10B—V4—O11B108.05 (16)O25Tviii—K3—O21Tix74.44 (10)
O10B—V4—O6C98.10 (15)O5W—K3—O21Tix123.14 (14)
O11B—V4—O6C99.13 (15)O6W—K3—O21Tix128.44 (13)
O10B—V4—O5C98.12 (15)O9W—K3—O21Tix71.85 (14)
O11B—V4—O5C96.71 (15)O23Tvi—K3—O27T74.05 (10)
O6C—V4—O5C152.55 (13)O25Tviii—K3—O27T146.54 (11)
O10B—V4—O2D87.63 (14)O5W—K3—O27T73.96 (12)
O11B—V4—O2D164.23 (14)O6W—K3—O27T146.13 (12)
O6C—V4—O2D79.74 (12)O9W—K3—O27T88.67 (13)
O5C—V4—O2D78.95 (12)O21Tix—K3—O27T72.77 (10)
O10B—V4—O1D164.37 (14)O23Tvi—K3—O4W136.36 (11)
O11B—V4—O1D87.58 (14)O25Tviii—K3—O4W78.53 (11)
O6C—V4—O1D79.38 (12)O5W—K3—O4W61.86 (12)
O5C—V4—O1D79.03 (12)O6W—K3—O4W125.62 (12)
O2D—V4—O1D76.74 (12)O9W—K3—O4W141.67 (15)
O24T—V5—O12B104.93 (17)O21Tix—K3—O4W70.07 (10)
O24T—V5—O20B103.26 (16)O27T—K3—O4W84.26 (10)
O12B—V5—O20B91.36 (15)O23Tvi—K3—O14Bviii119.30 (11)
O24T—V5—O14B103.76 (16)O25Tviii—K3—O14Bviii53.38 (9)
O12B—V5—O14B91.43 (15)O5W—K3—O14Bviii67.26 (11)
O20B—V5—O14B151.11 (14)O6W—K3—O14Bviii72.00 (11)
O24T—V5—O11B100.00 (16)O9W—K3—O14Bviii137.58 (13)
O12B—V5—O11B155.07 (14)O21Tix—K3—O14Bviii106.80 (10)
O20B—V5—O11B82.61 (14)O27T—K3—O14Bviii132.52 (10)
O14B—V5—O11B82.82 (14)O4W—K3—O14Bviii53.88 (9)
O24T—V5—O1D173.91 (15)O6W—K4—O16Bvii162.73 (15)
O12B—V5—O1D81.14 (13)O6W—K4—O26Tviii73.88 (13)
O20B—V5—O1D75.91 (12)O16Bvii—K4—O26Tviii118.24 (13)
O14B—V5—O1D76.13 (12)O6W—K4—O9W78.81 (17)
O11B—V5—O1D73.92 (11)O16Bvii—K4—O9W83.95 (15)
O25T—V6—O13B103.58 (16)O26Tviii—K4—O9W126.27 (17)
O25T—V6—O14B103.90 (16)O6W—K4—O26Tvii138.56 (13)
O13B—V6—O14B94.04 (15)O16Bvii—K4—O26Tvii54.50 (10)
O25T—V6—O3C97.90 (16)O26Tviii—K4—O26Tvii64.75 (12)
O13B—V6—O3C91.22 (14)O9W—K4—O26Tvii124.14 (16)
O14B—V6—O3C155.66 (14)O6W—K4—O7W111.55 (14)
O25T—V6—O5C102.60 (16)O16Bvii—K4—O7W65.92 (11)
O13B—V6—O5C152.25 (14)O26Tviii—K4—O7W146.61 (15)
O14B—V6—O5C88.47 (14)O9W—K4—O7W86.49 (16)
O3C—V6—O5C76.20 (13)O26Tvii—K4—O7W104.46 (12)
O25T—V6—O1D175.51 (15)O6W—K4—O3W118.81 (16)
O13B—V6—O1D78.63 (13)O16Bvii—K4—O3W74.21 (12)
O14B—V6—O1D79.71 (12)O26Tviii—K4—O3W95.01 (14)
O3C—V6—O1D78.07 (12)O9W—K4—O3W138.71 (17)
O5C—V6—O1D74.63 (12)O26Tvii—K4—O3W68.97 (12)
O26T—V7—O15B103.92 (18)O7W—K4—O3W52.73 (14)
O26T—V7—O16B102.74 (18)O8W—K5—O18Bvi116.68 (16)
O15B—V7—O16B95.34 (16)O8W—K5—O9B88.96 (16)
O26T—V7—O5C102.03 (17)O18Bvi—K5—O9B115.20 (11)
O15B—V7—O5C89.99 (14)O8W—K5—O7W86.37 (17)
O16B—V7—O5C152.57 (14)O18Bvi—K5—O7W94.58 (12)
O26T—V7—O3C98.14 (17)O9B—K5—O7W148.49 (12)
O15B—V7—O3C155.92 (14)O8W—K5—O22Tvii67.49 (15)
O16B—V7—O3C89.04 (14)O18Bvi—K5—O22Tvii170.27 (11)
O5C—V7—O3C75.93 (13)O9B—K5—O22Tvii72.81 (10)
O26T—V7—O2D175.00 (16)O7W—K5—O22Tvii76.63 (12)
O15B—V7—O2D80.25 (13)O8W—K5—O9W142.73 (18)
O16B—V7—O2D79.42 (13)O18Bvi—K5—O9W100.56 (14)
O5C—V7—O2D75.00 (12)O9B—K5—O9W73.02 (12)
O3C—V7—O2D77.31 (12)O7W—K5—O9W92.42 (15)
O27T—V8—O17B104.28 (16)O22Tvii—K5—O9W75.98 (14)
O27T—V8—O18B102.86 (16)O8W—K5—O23T78.72 (14)
O17B—V8—O18B94.12 (15)O18Bvi—K5—O23T71.86 (10)
O27T—V8—O6C101.85 (16)O9B—K5—O23T55.51 (10)
O17B—V8—O6C152.21 (14)O7W—K5—O23T152.01 (14)
O18B—V8—O6C89.12 (14)O22Tvii—K5—O23T117.87 (11)
O27T—V8—O4C98.38 (15)O9W—K5—O23T113.75 (13)
O17B—V8—O4C91.54 (13)Pt1—O1D—V499.17 (13)
O18B—V8—O4C155.90 (13)Pt1—O1D—V994.73 (12)
O6C—V8—O4C75.36 (12)V4—O1D—V992.37 (12)
O27T—V8—O2D175.32 (15)Pt1—O1D—V693.70 (12)
O17B—V8—O2D78.97 (13)V4—O1D—V693.47 (12)
O18B—V8—O2D80.09 (13)V9—O1D—V6168.86 (15)
O6C—V8—O2D74.42 (12)Pt1—O1D—V192.47 (12)
O4C—V8—O2D78.04 (11)V4—O1D—V1168.36 (15)
O28T—V9—O20B105.26 (16)V9—O1D—V186.35 (11)
O28T—V9—O19B102.34 (16)V6—O1D—V186.01 (10)
O20B—V9—O19B94.63 (14)Pt1—O1D—V5174.40 (16)
O28T—V9—O6C102.11 (16)V4—O1D—V586.40 (11)
O20B—V9—O6C90.31 (14)V9—O1D—V585.49 (10)
O19B—V9—O6C152.78 (13)V6—O1D—V585.42 (10)
O28T—V9—O4C96.57 (15)V1—O1D—V581.96 (10)
O20B—V9—O4C156.16 (14)Pt1—O2D—V499.47 (13)
O19B—V9—O4C89.88 (13)Pt1—O2D—V795.20 (12)
O6C—V9—O4C75.62 (12)V4—O2D—V793.10 (11)
O28T—V9—O1D174.17 (15)Pt1—O2D—V894.04 (12)
O20B—V9—O1D80.02 (13)V4—O2D—V893.16 (12)
O19B—V9—O1D79.42 (12)V7—O2D—V8167.84 (15)
O6C—V9—O1D75.11 (12)Pt1—O2D—V292.35 (11)
O4C—V9—O1D77.82 (11)V4—O2D—V2168.17 (15)
V5—V1—Pt187.93 (2)V7—O2D—V285.63 (11)
V5—V1—V660.31 (2)V8—O2D—V286.10 (10)
Pt1—V1—V658.97 (2)Pt1—O2D—V3173.86 (16)
V5—V1—V960.15 (2)V4—O2D—V386.57 (10)
Pt1—V1—V959.27 (2)V7—O2D—V385.52 (10)
V6—V1—V990.89 (3)V8—O2D—V384.47 (10)
V5—V1—V443.54 (2)V2—O2D—V381.61 (10)
Pt1—V1—V444.385 (15)V6—O3C—Pt1101.52 (13)
V6—V1—V445.82 (2)V6—O3C—V799.96 (13)
V9—V1—V445.099 (19)Pt1—O3C—V7101.69 (14)
V3—V2—V760.71 (3)Pt1—O4C—V8100.70 (13)
V3—V2—Pt188.53 (3)Pt1—O4C—V9100.45 (13)
V7—V2—Pt159.81 (2)V8—O4C—V9100.37 (13)
V3—V2—V859.96 (3)V4—O5C—V7109.01 (15)
V7—V2—V891.11 (3)V4—O5C—V6109.70 (15)
Pt1—V2—V859.15 (2)V7—O5C—V6101.51 (14)
V3—V2—V443.98 (2)V4—O6C—V9109.15 (14)
V7—V2—V445.49 (2)V4—O6C—V8108.85 (15)
Pt1—V2—V444.562 (14)V9—O6C—V8103.00 (13)
V8—V2—V445.641 (19)Pt1—O7B—V2100.62 (13)
V3—V2—V189.54 (2)Pt1—O8B—V1101.22 (14)
V7—V2—V159.98 (2)V4—O10B—V3112.76 (17)
Pt1—V2—V11.113 (10)V4—O11B—V5112.09 (16)
V8—V2—V160.11 (2)V5—O12B—V1116.48 (17)
V4—V2—V145.564 (14)V6—O13B—V1119.14 (17)
V2—V3—V492.11 (3)V6—O14B—V5117.51 (16)
V2—V3—V860.89 (3)V7—O15B—V3117.70 (17)
V4—V3—V861.69 (3)V7—O16B—V2117.32 (17)
V2—V3—V760.19 (3)V8—O17B—V2118.96 (16)
V4—V3—V761.23 (2)V8—O18B—V3117.66 (17)
V8—V3—V791.34 (3)V9—O19B—V1116.70 (16)
V5—V4—Pt188.17 (2)V9—O20B—V5117.45 (17)
V3—V4—Pt188.48 (2)H1A—O1W—H1B109 (5)
V5—V4—V960.06 (2)H2A—O2W—H2B102 (4)
V3—V4—V9118.47 (3)H3A—O3W—H3B107 (5)
Pt1—V4—V959.155 (19)H4A—O4W—H4B109 (4)
V5—V4—V7117.42 (3)H5A—O5W—H5B106 (4)
V3—V4—V760.12 (3)H6A—O6W—H6B109.4
Pt1—V4—V759.28 (2)H7A—O7W—H7B105 (4)
V9—V4—V7118.44 (3)H8A—O8W—H8B103 (4)
V5—V4—V8118.99 (3)H9A—O9W—H9B101 (4)
V3—V4—V859.49 (2)
Symmetry codes: (i) x, y+1, z; (ii) x, y, z+1; (iii) x, y+1, z+1; (iv) x, y+2, z+1; (v) x+1, y+2, z+1; (vi) x+1, y+1, z+1; (vii) x, y+1, z+1; (viii) x, y1, z; (ix) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7B—H7···O19Bix0.90 (8)1.86 (8)2.738 (4)164 (8)
O8B—H8···O4Cix0.77 (6)1.90 (6)2.645 (5)161 (6)
O1W—H1B···O9B0.83 (3)2.50 (6)3.127 (6)133 (7)
O1W—H1A···O8W0.84 (3)2.10 (3)2.930 (9)170 (8)
O2W—H2A···O15B0.87 (3)1.88 (3)2.728 (6)166 (8)
O2W—H2B···O11Bv0.86 (3)2.23 (5)2.975 (6)145 (8)
O3W—H3A···O3Cvii0.84 (3)1.83 (3)2.673 (5)177 (10)
O3W—H3B···O7W0.83 (3)2.09 (5)2.875 (7)158 (8)
O4W—H4A···O13Bix0.83 (3)1.88 (3)2.680 (5)162 (7)
O4W—H4B···O14Bviii0.83 (3)2.10 (4)2.850 (5)151 (7)
O5W—H5A···O2Wvi0.87 (3)1.84 (3)2.710 (8)175 (8)
O5W—H5B···O24Tx0.84 (3)2.26 (5)2.972 (6)142 (7)
O6W—H6A···O5Cviii0.971.812.755 (5)163
O6W—H6B···O10Bvi0.972.042.755 (5)129
O7W—H7A···O7Bvii0.85 (3)2.07 (4)2.891 (5)163 (8)
O7W—H7B···O6Cvi0.84 (3)2.27 (6)2.885 (5)130 (6)
O8W—H8A···O5Wvi0.86 (3)1.98 (5)2.795 (7)159 (10)
O8W—H8B···O19Bii0.86 (3)2.22 (4)3.031 (6)156 (8)
Symmetry codes: (ii) x, y, z+1; (v) x+1, y+2, z+1; (vi) x+1, y+1, z+1; (vii) x, y+1, z+1; (viii) x, y1, z; (ix) x, y+1, z; (x) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7B—H7···O19Bi0.90 (8)1.86 (8)2.738 (4)164 (8)
O8B—H8···O4Ci0.77 (6)1.90 (6)2.645 (5)161 (6)
O1W—H1B···O9B0.83 (3)2.50 (6)3.127 (6)133 (7)
O1W—H1A···O8W0.84 (3)2.10 (3)2.930 (9)170 (8)
O2W—H2A···O15B0.87 (3)1.88 (3)2.728 (6)166 (8)
O2W—H2B···O11Bii0.86 (3)2.23 (5)2.975 (6)145 (8)
O3W—H3A···O3Ciii0.84 (3)1.83 (3)2.673 (5)177 (10)
O3W—H3B···O7W0.83 (3)2.09 (5)2.875 (7)158 (8)
O4W—H4A···O13Bi0.83 (3)1.88 (3)2.680 (5)162 (7)
O4W—H4B···O14Biv0.83 (3)2.10 (4)2.850 (5)151 (7)
O5W—H5A···O2Wv0.87 (3)1.84 (3)2.710 (8)175 (8)
O5W—H5B···O24Tvi0.84 (3)2.26 (5)2.972 (6)142 (7)
O6W—H6A···O5Civ0.971.812.755 (5)162.7
O6W—H6B···O10Bv0.972.042.755 (5)129.0
O7W—H7A···O7Biii0.85 (3)2.07 (4)2.891 (5)163 (8)
O7W—H7B···O6Cv0.84 (3)2.27 (6)2.885 (5)130 (6)
O8W—H8A···O5Wv0.86 (3)1.98 (5)2.795 (7)159 (10)
O8W—H8B···O19Bvii0.86 (3)2.22 (4)3.031 (6)156 (8)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+2, z+1; (iii) x, y+1, z+1; (iv) x, y1, z; (v) x+1, y+1, z+1; (vi) x+1, y+1, z; (vii) x, y, z+1.

Experimental details

Crystal data
Chemical formulaK5[H2PtV9O28]·9H2O
Mr1461.21
Crystal system, space groupTriclinic, P1
Temperature (K)298
a, b, c (Å)10.1663 (7), 12.8350 (7), 13.615 (2)
α, β, γ (°)103.734 (5), 106.193 (6), 92.480 (4)
V3)1645.8 (3)
Z2
Radiation typeMo Kα
µ (mm1)7.42
Crystal size (mm)0.21 × 0.19 × 0.17
Data collection
DiffractometerStoe Stadi4
diffractometer
Absorption correctionEmpirical (using intensity measurements)
(X-SHAPE; Stoe & Cie,1996)
Tmin, Tmax0.301, 0.378
No. of measured, independent and
observed [I > 2σ(I)] reflections
6797, 6797, 6242
Rint0.0000
(sin θ/λ)max1)0.628
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.066, 1.10
No. of reflections6797
No. of parameters526
No. of restraints25
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.30, 1.46

Computer programs: STADI4 (Stoe & Cie, 1996), X-RED (Stoe & Cie, 1996), SHELXS2014 (Sheldrick, 2008), SHELXL2014 (Sheldrick, 2015), ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 1998).

 

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