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Acta Crystallographica Section E: Crystallographic Communications logoLink to Acta Crystallographica Section E: Crystallographic Communications
. 2015 May 20;71(Pt 6):647–649. doi: 10.1107/S2056989015009135

Crystal structure of penta­potassium di­hydrogen nona­vanadato(V)platinate(IV) nona­hydrate

Hea-Chung Joo a, Uk Lee a,*
PMCID: PMC4459313  PMID: 26090141

The polyanion in K5[H2PtV9O28]·9H2O has approximate mm2 (C 2v) 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.

Keywords: crystal structure, nona­vanadoplatinate(IV) polyanion, heteropolyanions, hydrogen bonding

Abstract

The title compound, K5[H2PtV9O28]·9H2O, containing the nona­vanado­platinate(IV) polyanion, was obtained by hydro­thermal reaction at pH = 4.2. The polyanion has approximate mm2 (C 2v) 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. All K+ cations are located on general positions of the space group P-1.

Structural commentary  

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 heteropoly­oxido­vanadate, [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 heteropolyanion in the title compound. The O atoms of the clusters were designated as OT (terminal, V=O), OB (bridging, μ2-O), OC3-O), and OD4-O). All atoms in the polyanions are 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).

Figure 1.

Figure 1

The mol­ecular structure of the heteropolyanion in 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.

Figure 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.]

Table 1. Hydrogen-bond geometry (, ).

DHA DH HA D A DHA
O7BH7O19B i 0.90(8) 1.86(8) 2.738(4) 164(8)
O8BH8O4C i 0.77(6) 1.90(6) 2.645(5) 161(6)
O1WH1BO9B 0.83(3) 2.50(6) 3.127(6) 133(7)
O1WH1AO8W 0.84(3) 2.10(3) 2.930(9) 170(8)
O2WH2AO15B 0.87(3) 1.88(3) 2.728(6) 166(8)
O2WH2BO11B ii 0.86(3) 2.23(5) 2.975(6) 145(8)
O3WH3AO3C iii 0.84(3) 1.83(3) 2.673(5) 177(10)
O3WH3BO7W 0.83(3) 2.09(5) 2.875(7) 158(8)
O4WH4AO13B i 0.83(3) 1.88(3) 2.680(5) 162(7)
O4WH4BO14B iv 0.83(3) 2.10(4) 2.850(5) 151(7)
O5WH5AO2W v 0.87(3) 1.84(3) 2.710(8) 175(8)
O5WH5BO24T vi 0.84(3) 2.26(5) 2.972(6) 142(7)
O6WH6AO5C iv 0.97 1.81 2.755(5) 163
O6WH6BO10B v 0.97 2.04 2.755(5) 129
O7WH7AO7B iii 0.85(3) 2.07(4) 2.891(5) 163(8)
O7WH7BO6C v 0.84(3) 2.27(6) 2.885(5) 130(6)
O8WH8AO5W v 0.86(3) 1.98(5) 2.795(7) 159(10)
O8WH8BO19B vii 0.86(3) 2.22(4) 3.031(6) 156(8)

Symmetry codes: (i) Inline graphic; (ii) Inline graphic; (iii) Inline graphic; (iv) Inline graphic; (v) Inline graphic; (vi) Inline graphic; (vii) Inline graphic.

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 cations 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 O9W water mol­ecule (Table 1).

Synthesis and crystallization  

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  

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 (SHELXL2014 command HFIX 23), with O—H = 0.97 Å and U iso(H) = 1.5 U eq(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 DFIX, and were included in the refinement with U iso(H) = 1.5U eq(O). The unusually short μ2-O17B⋯terminal-O21T i 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.

Table 2. Experimental details.

Crystal data
Chemical formula K5[H2PtV9O28]9H2O
M r 1461.21
Crystal system, space group Triclinic, P Inline graphic
Temperature (K) 298
a, b, c () 10.1663(7), 12.8350(7), 13.615(2)
, , () 103.734(5), 106.193(6), 92.480(4)
V (3) 1645.8(3)
Z 2
Radiation type Mo K
(mm1) 7.42
Crystal size (mm) 0.21 0.19 0.17
 
Data collection
Diffractometer Stoe Stadi4
Absorption correction Empirical (using intensity measurements) (X-SHAPE; Stoe Cie,1996)
T min, T max 0.301, 0.378
No. of measured, independent and observed [I > 2(I)] reflections 6797, 6797, 6242
(sin /)max (1) 0.628
 
Refinement
R[F 2 > 2(F 2)], wR(F 2), S 0.028, 0.066, 1.10
No. of reflections 6797
No. of parameters 526
No. of restraints 25
H-atom treatment H atoms treated by a mixture of independent and constrained refinement
max, min (e 3) 1.30, 1.46

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

Supplementary Material

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989015009135/vn2093sup1.cif

e-71-00647-sup1.cif (271.5KB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989015009135/vn2093Isup2.hkl

e-71-00647-Isup2.hkl (372.4KB, hkl)

CCDC reference: 1400654

Additional supporting information: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Crystal data

K5[H2PtV9O28]·9H2O Z = 2
Mr = 1461.21 F(000) = 1392
Triclinic, P1 Dx = 2.949 Mg m3
a = 10.1663 (7) Å Mo Kα radiation, λ = 0.71069 Å
b = 12.8350 (7) Å Cell parameters from 30 reflections
c = 13.615 (2) Å θ = 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) Å3 0.21 × 0.19 × 0.17 mm

Data collection

Stoe Stadi4 diffractometer Rint = 0.0000
Radiation source: fine-focus sealed tube θmax = 26.5°, θmin = 1.6°
ω/2–θ scans h = −12→12
Absorption correction: empirical (using intensity measurements) (X-SHAPE; Stoe & Cie,1996) k = −16→15
Tmin = 0.301, Tmax = 0.378 l = 0→17
6797 measured reflections 3 standard reflections every 60 min
6797 independent reflections intensity decay: 2.5%
6242 reflections with I > 2σ(I)

Refinement

Refinement on F2 Secondary atom site location: difference Fourier map
Least-squares matrix: full Hydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028 H 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 reflections Δρmax = 1.30 e Å3
526 parameters Δρmin = −1.46 e Å3
25 restraints Extinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods Extinction coefficient: 0.00505 (13)

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

x y z Uiso*/Ueq
Pt1 0.07476 (2) 0.66204 (2) 0.15945 (2) 0.01102 (6)
V1 0.08091 (8) 0.74803 (6) −0.03864 (6) 0.01675 (16)
V2 0.05610 (8) 0.57644 (6) 0.35482 (6) 0.01798 (16)
V3 0.36393 (8) 0.67118 (6) 0.46862 (6) 0.01860 (17)
V4 0.38427 (7) 0.76066 (6) 0.27828 (6) 0.01375 (15)
V5 0.38558 (8) 0.84633 (6) 0.08300 (6) 0.01680 (16)
V6 0.15181 (8) 0.90837 (6) 0.19135 (6) 0.01625 (16)
V7 0.14522 (8) 0.82358 (6) 0.38572 (6) 0.01838 (17)
V8 0.28571 (8) 0.50931 (6) 0.24210 (6) 0.01521 (16)
V9 0.30124 (8) 0.59746 (6) 0.04752 (6) 0.01441 (15)
K1 0.19325 (16) 0.94505 (11) 0.81002 (11) 0.0433 (3)
K2 0.32640 (13) 0.27185 (9) 0.99666 (11) 0.0329 (3)
K3 0.29033 (13) 0.19821 (10) 0.25987 (10) 0.0353 (3)
K4 0.1688 (2) 0.15936 (14) 0.5300 (2) 0.0819 (7)
K5 0.33393 (14) 0.48579 (12) 0.61615 (13) 0.0439 (3)
O1D 0.2234 (3) 0.7454 (2) 0.1318 (2) 0.0148 (6)
O2D 0.2133 (3) 0.6723 (2) 0.2981 (2) 0.0148 (6)
O3C 0.0321 (3) 0.8071 (2) 0.2320 (2) 0.0156 (6)
O4C 0.1590 (3) 0.5298 (2) 0.1039 (2) 0.0137 (6)
O5C 0.2793 (3) 0.8770 (2) 0.3209 (2) 0.0165 (6)
O6C 0.3986 (3) 0.6174 (2) 0.2014 (2) 0.0147 (6)
O7B −0.0627 (3) 0.5793 (3) 0.2053 (3) 0.0159 (6)
H7 −0.086 (8) 0.519 (6) 0.152 (6) 0.07 (2)*
O8B −0.0508 (3) 0.6659 (3) 0.0160 (3) 0.0168 (7)
H8 −0.067 (6) 0.609 (5) −0.023 (5) 0.021 (15)*
O9B 0.2105 (3) 0.5994 (3) 0.4730 (3) 0.0202 (7)
O10B 0.4757 (3) 0.7538 (3) 0.3997 (3) 0.0207 (7)
O11B 0.4856 (3) 0.8317 (3) 0.2321 (3) 0.0179 (7)
O12B 0.2409 (3) 0.8257 (3) −0.0358 (3) 0.0197 (7)
O13B 0.0439 (3) 0.8680 (2) 0.0548 (3) 0.0182 (7)
O14B 0.3033 (3) 0.9526 (2) 0.1585 (3) 0.0174 (6)
O15B 0.2871 (3) 0.8035 (3) 0.4919 (3) 0.0215 (7)
O16B 0.0221 (3) 0.7196 (3) 0.3937 (3) 0.0204 (7)
O17B 0.1402 (3) 0.4691 (2) 0.2815 (3) 0.0176 (6)
O18B 0.4015 (3) 0.5523 (3) 0.3774 (3) 0.0184 (7)
O19B 0.1590 (3) 0.6178 (2) −0.0635 (2) 0.0158 (6)
O20B 0.4224 (3) 0.7028 (3) 0.0424 (3) 0.0179 (7)
O21T −0.0224 (4) 0.7505 (3) −0.1503 (3) 0.0270 (8)
O22T −0.0570 (4) 0.5099 (3) 0.3842 (3) 0.0257 (8)
O23T 0.4743 (4) 0.6778 (3) 0.5812 (3) 0.0287 (8)
O24T 0.5067 (3) 0.9142 (3) 0.0618 (3) 0.0238 (7)
O25T 0.0976 (4) 1.0199 (3) 0.2403 (3) 0.0245 (7)
O26T 0.0934 (4) 0.9340 (3) 0.4384 (3) 0.0301 (8)
O27T 0.3379 (4) 0.3970 (3) 0.1941 (3) 0.0237 (7)
O28T 0.3493 (4) 0.4863 (3) −0.0055 (3) 0.0234 (7)
O1W 0.1060 (6) 0.7552 (4) 0.6420 (4) 0.0514 (12)
H1A 0.154 (8) 0.721 (6) 0.681 (5) 0.077*
H1B 0.133 (8) 0.750 (7) 0.589 (4) 0.077*
O2W 0.3763 (6) 0.9426 (4) 0.6891 (4) 0.0618 (15)
H2A 0.347 (9) 0.908 (6) 0.623 (3) 0.093*
H2B 0.428 (8) 0.997 (5) 0.688 (6) 0.093*
O3W 0.2228 (5) 0.1440 (4) 0.7752 (6) 0.0660 (17)
H3A 0.143 (5) 0.161 (7) 0.775 (8) 0.099*
H3B 0.268 (7) 0.197 (5) 0.770 (8) 0.099*
O4W 0.2138 (4) 0.0846 (3) 0.0168 (4) 0.0356 (9)
H4A 0.132 (4) 0.097 (5) 0.007 (6) 0.053*
H4B 0.224 (6) 0.029 (4) 0.038 (6) 0.053*
O5W 0.5107 (5) 0.1657 (4) 0.1656 (4) 0.0495 (12)
H5A 0.550 (8) 0.130 (5) 0.210 (4) 0.074*
H5B 0.481 (8) 0.120 (5) 0.106 (3) 0.074*
O6W 0.3583 (5) 0.0913 (4) 0.4279 (4) 0.0552 (13)
H6A 0.3463 0.0134 0.4006 0.083*
H6B 0.4520 0.1148 0.4737 0.083*
O7W 0.3045 (5) 0.3465 (4) 0.7411 (4) 0.0471 (12)
H7A 0.242 (5) 0.367 (6) 0.769 (6) 0.071*
H7B 0.373 (5) 0.394 (5) 0.774 (6) 0.071*
O8W 0.3022 (6) 0.6482 (5) 0.7759 (4) 0.0634 (15)
H8A 0.375 (6) 0.694 (6) 0.797 (6) 0.095*
H8B 0.287 (9) 0.645 (7) 0.834 (4) 0.095*
O9W 0.1770 (7) 0.3233 (4) 0.4164 (5) 0.0629 (15)
H9A 0.265 (3) 0.341 (8) 0.444 (7) 0.094*
H9B 0.159 (8) 0.357 (7) 0.368 (5) 0.094*

Atomic displacement parameters (Å2)

U11 U22 U33 U12 U13 U23
Pt1 0.00977 (9) 0.00941 (9) 0.01224 (9) −0.00006 (5) 0.00238 (6) 0.00097 (6)
V1 0.0165 (4) 0.0157 (4) 0.0161 (4) 0.0005 (3) 0.0017 (3) 0.0046 (3)
V2 0.0159 (4) 0.0202 (4) 0.0177 (4) −0.0023 (3) 0.0051 (3) 0.0053 (3)
V3 0.0183 (4) 0.0199 (4) 0.0148 (4) −0.0021 (3) 0.0010 (3) 0.0047 (3)
V4 0.0120 (3) 0.0126 (3) 0.0144 (4) −0.0016 (3) 0.0020 (3) 0.0019 (3)
V5 0.0162 (4) 0.0151 (4) 0.0194 (4) −0.0013 (3) 0.0058 (3) 0.0050 (3)
V6 0.0182 (4) 0.0106 (3) 0.0187 (4) 0.0017 (3) 0.0048 (3) 0.0022 (3)
V7 0.0231 (4) 0.0151 (4) 0.0160 (4) 0.0024 (3) 0.0076 (3) 0.0000 (3)
V8 0.0168 (4) 0.0121 (3) 0.0162 (4) 0.0025 (3) 0.0041 (3) 0.0036 (3)
V9 0.0158 (4) 0.0120 (3) 0.0157 (4) 0.0015 (3) 0.0060 (3) 0.0026 (3)
K1 0.0556 (9) 0.0407 (7) 0.0386 (7) 0.0112 (6) 0.0207 (7) 0.0109 (6)
K2 0.0380 (7) 0.0222 (6) 0.0465 (7) 0.0055 (5) 0.0257 (6) 0.0078 (5)
K3 0.0327 (6) 0.0355 (7) 0.0352 (7) −0.0054 (5) 0.0075 (5) 0.0090 (5)
K4 0.1103 (16) 0.0426 (9) 0.1207 (18) 0.0171 (10) 0.0879 (15) 0.0091 (10)
K5 0.0328 (7) 0.0496 (8) 0.0667 (10) 0.0148 (6) 0.0246 (7) 0.0346 (7)
O1D 0.0146 (15) 0.0120 (14) 0.0172 (16) −0.0012 (12) 0.0047 (12) 0.0033 (12)
O2D 0.0153 (15) 0.0137 (15) 0.0126 (15) −0.0033 (12) 0.0026 (12) 0.0010 (12)
O3C 0.0157 (15) 0.0128 (15) 0.0167 (16) 0.0019 (12) 0.0059 (12) −0.0007 (12)
O4C 0.0136 (14) 0.0106 (14) 0.0153 (15) 0.0004 (11) 0.0036 (12) 0.0017 (12)
O5C 0.0169 (15) 0.0136 (15) 0.0161 (15) 0.0002 (12) 0.0028 (12) 0.0012 (12)
O6C 0.0128 (14) 0.0135 (15) 0.0153 (15) −0.0002 (12) 0.0012 (12) 0.0030 (12)
O7B 0.0159 (15) 0.0150 (16) 0.0159 (16) 0.0004 (12) 0.0051 (13) 0.0022 (13)
O8B 0.0147 (15) 0.0162 (17) 0.0156 (16) −0.0006 (13) −0.0005 (13) 0.0031 (14)
O9B 0.0221 (17) 0.0206 (17) 0.0169 (16) −0.0022 (13) 0.0055 (13) 0.0040 (13)
O10B 0.0194 (16) 0.0191 (16) 0.0205 (17) −0.0027 (13) 0.0026 (13) 0.0044 (13)
O11B 0.0142 (15) 0.0180 (16) 0.0204 (17) −0.0025 (12) 0.0038 (13) 0.0049 (13)
O12B 0.0243 (17) 0.0174 (16) 0.0179 (16) −0.0010 (13) 0.0055 (14) 0.0069 (13)
O13B 0.0162 (15) 0.0129 (15) 0.0236 (17) 0.0007 (12) 0.0031 (13) 0.0050 (13)
O14B 0.0187 (16) 0.0124 (15) 0.0210 (17) −0.0007 (12) 0.0061 (13) 0.0041 (13)
O15B 0.0273 (18) 0.0197 (17) 0.0141 (16) −0.0007 (14) 0.0062 (14) −0.0017 (13)
O16B 0.0226 (17) 0.0192 (16) 0.0204 (17) 0.0025 (13) 0.0107 (14) 0.0018 (13)
O17B 0.0190 (16) 0.0142 (15) 0.0185 (16) −0.0015 (12) 0.0049 (13) 0.0039 (13)
O18B 0.0169 (15) 0.0173 (16) 0.0185 (16) 0.0016 (12) 0.0009 (13) 0.0052 (13)
O19B 0.0167 (15) 0.0144 (15) 0.0138 (15) 0.0029 (12) 0.0022 (12) 0.0014 (12)
O20B 0.0180 (16) 0.0178 (16) 0.0200 (17) 0.0031 (13) 0.0085 (13) 0.0054 (13)
O21T 0.0298 (19) 0.0255 (18) 0.0220 (18) 0.0016 (15) 0.0007 (15) 0.0075 (15)
O22T 0.0233 (18) 0.0306 (19) 0.0266 (19) −0.0029 (15) 0.0109 (15) 0.0106 (15)
O23T 0.0287 (19) 0.033 (2) 0.0186 (18) −0.0072 (16) −0.0024 (15) 0.0079 (15)
O24T 0.0224 (17) 0.0224 (17) 0.0281 (19) −0.0033 (14) 0.0091 (15) 0.0086 (15)
O25T 0.0245 (18) 0.0164 (16) 0.032 (2) 0.0048 (14) 0.0081 (15) 0.0041 (14)
O26T 0.039 (2) 0.0213 (18) 0.029 (2) 0.0061 (16) 0.0154 (17) −0.0020 (15)
O27T 0.0264 (18) 0.0180 (17) 0.0283 (19) 0.0074 (14) 0.0085 (15) 0.0077 (14)
O28T 0.0278 (18) 0.0164 (16) 0.0277 (19) 0.0037 (14) 0.0130 (15) 0.0034 (14)
O1W 0.066 (3) 0.050 (3) 0.041 (3) 0.008 (2) 0.025 (3) 0.007 (2)
O2W 0.080 (4) 0.056 (3) 0.035 (3) −0.024 (3) 0.017 (3) −0.010 (2)
O3W 0.028 (2) 0.058 (3) 0.126 (5) 0.013 (2) 0.028 (3) 0.044 (4)
O4W 0.028 (2) 0.035 (2) 0.054 (3) 0.0107 (17) 0.0133 (19) 0.027 (2)
O5W 0.052 (3) 0.041 (3) 0.049 (3) −0.008 (2) 0.013 (2) 0.004 (2)
O6W 0.051 (3) 0.034 (2) 0.056 (3) −0.011 (2) 0.003 (2) −0.014 (2)
O7W 0.030 (2) 0.043 (3) 0.078 (4) 0.0107 (19) 0.023 (2) 0.025 (2)
O8W 0.080 (4) 0.066 (4) 0.042 (3) −0.016 (3) 0.028 (3) 0.002 (3)
O9W 0.095 (4) 0.051 (3) 0.056 (3) 0.025 (3) 0.029 (3) 0.028 (3)

Geometric parameters (Å, º)

Pt1—V6 3.1213 (8) V8—O27T 1.612 (3)
Pt1—V8 3.1262 (8) V8—O17B 1.803 (3)
Pt1—V9 3.1359 (8) V8—O18B 1.826 (3)
Pt1—V7 3.1480 (9) V8—O6C 2.033 (3)
Pt1—V4 3.1566 (8) V8—O4C 2.045 (3)
Pt1—V2 3.1574 (9) V8—O2D 2.278 (3)
V1—V5 3.1204 (11) V9—O28T 1.601 (3)
V1—V6 3.1801 (11) V9—O20B 1.816 (3)
V1—V9 3.1802 (11) V9—O19B 1.856 (3)
V2—V3 3.1217 (11) V9—O6C 2.001 (3)
V2—V7 3.1566 (11) V9—O4C 2.064 (3)
V2—V8 3.1767 (11) V9—O1D 2.270 (3)
V2—V4 4.4982 (11) K1—O3Wi 2.725 (5)
V3—V4 3.1255 (11) K1—O2W 2.804 (6)
V3—V8 3.1476 (11) K1—O1W 2.827 (5)
V3—V7 3.1731 (11) K1—O12Bii 2.830 (3)
V4—V5 3.1120 (11) K1—O4Wiii 2.903 (5)
V4—V9 3.1960 (11) K1—O25Tiv 2.924 (4)
V4—V7 3.2078 (11) K1—O24Tv 3.267 (4)
V4—V8 3.2162 (10) K1—O5Wvi 3.351 (6)
V5—V9 3.1578 (10) K2—O4Wii 2.722 (4)
V5—V6 3.1654 (11) K2—O27Tii 2.753 (4)
V6—V7 3.1068 (12) K2—O28Tii 2.760 (3)
V8—V9 3.1566 (11) K2—O20Bvi 2.772 (3)
Pt1—O1D 1.985 (3) K2—O8Bvii 2.917 (3)
Pt1—O2D 1.986 (3) K2—O3W 2.936 (7)
Pt1—O4C 2.015 (3) K2—O24Tvi 3.069 (4)
Pt1—O3C 2.017 (3) K2—O5Wii 3.156 (5)
Pt1—O8B 2.027 (3) K3—O23Tvi 2.844 (4)
Pt1—O7B 2.036 (3) K3—O25Tviii 2.860 (4)
V1—O21T 1.598 (3) K3—O5W 2.876 (5)
V1—O12B 1.857 (3) K3—O6W 2.878 (6)
V1—O13B 1.876 (3) K3—O9W 2.890 (6)
V1—O19B 1.880 (3) K3—O21Tix 2.904 (4)
V1—O8B 2.064 (3) K3—O27T 2.960 (4)
V1—O1D 2.377 (3) K3—O4W 3.139 (5)
V2—O22T 1.596 (3) K3—O14Bviii 3.151 (3)
V2—O9B 1.862 (3) K4—O6W 2.733 (5)
V2—O16B 1.863 (3) K4—O16Bvii 2.806 (4)
V2—O17B 1.885 (3) K4—O26Tviii 2.841 (4)
V2—O7B 2.067 (3) K4—O9W 2.904 (5)
V2—O2D 2.374 (3) K4—O26Tvii 3.055 (4)
V3—O23T 1.608 (3) K4—O7W 3.187 (6)
V3—O9B 1.800 (3) K4—O3W 3.284 (7)
V3—O18B 1.853 (3) K5—O8W 2.734 (6)
V3—O15B 1.895 (3) K5—O18Bvi 2.736 (3)
V3—O10B 2.064 (3) K5—O9B 2.764 (4)
V3—O2D 2.403 (3) K5—O7W 2.803 (5)
V4—O10B 1.681 (3) K5—O22Tvii 2.817 (4)
V4—O11B 1.685 (3) K5—O9W 2.982 (7)
V4—O6C 1.921 (3) K5—O23T 2.996 (4)
V4—O5C 1.943 (3) O7B—H7 0.90 (8)
V4—O2D 2.148 (3) O8B—H8 0.77 (6)
V4—O1D 2.158 (3) O1W—H1A 0.84 (3)
V5—O24T 1.607 (3) O1W—H1B 0.83 (3)
V5—O12B 1.813 (3) O2W—H2A 0.87 (3)
V5—O20B 1.878 (3) O2W—H2B 0.86 (3)
V5—O14B 1.879 (3) O3W—H3A 0.84 (3)
V5—O11B 2.058 (3) O3W—H3B 0.83 (3)
V5—O1D 2.381 (3) O4W—H4A 0.83 (3)
V6—O25T 1.617 (3) O4W—H4B 0.83 (3)
V6—O13B 1.812 (3) O5W—H5A 0.87 (3)
V6—O14B 1.824 (3) O5W—H5B 0.84 (3)
V6—O3C 2.014 (3) O6W—H6A 0.9700
V6—O5C 2.015 (3) O6W—H6B 0.9700
V6—O1D 2.284 (3) O7W—H7A 0.85 (3)
V7—O26T 1.610 (3) O7W—H7B 0.84 (3)
V7—O15B 1.812 (3) O8W—H8A 0.86 (3)
V7—O16B 1.832 (3) O8W—H8B 0.86 (3)
V7—O5C 1.997 (3) O9W—H9A 0.87 (3)
V7—O3C 2.043 (3) O9W—H9B 0.85 (3)
V7—O2D 2.269 (3)
O1D—Pt1—O2D 84.61 (12) Pt1—V4—V8 58.745 (19)
O1D—Pt1—O4C 85.94 (12) V9—V4—V8 58.98 (2)
O2D—Pt1—O4C 85.94 (12) V7—V4—V8 89.47 (3)
O1D—Pt1—O3C 85.44 (12) V4—V5—V1 92.76 (3)
O2D—Pt1—O3C 84.79 (12) V4—V5—V9 61.29 (2)
O4C—Pt1—O3C 167.89 (12) V1—V5—V9 60.86 (2)
O1D—Pt1—O8B 88.49 (13) V4—V5—V6 62.06 (2)
O2D—Pt1—O8B 172.89 (13) V1—V5—V6 60.78 (3)
O4C—Pt1—O8B 95.27 (13) V9—V5—V6 91.58 (3)
O3C—Pt1—O8B 92.99 (13) V4—V5—Pt1 46.338 (17)
O1D—Pt1—O7B 173.32 (13) V1—V5—Pt1 46.428 (18)
O2D—Pt1—O7B 88.75 (12) V9—V5—Pt1 45.928 (17)
O4C—Pt1—O7B 94.36 (12) V6—V5—Pt1 45.659 (17)
O3C—Pt1—O7B 93.22 (13) V7—V6—Pt1 60.72 (2)
O8B—Pt1—O7B 98.12 (13) V7—V6—V5 118.88 (3)
O1D—Pt1—V6 46.91 (9) Pt1—V6—V5 87.85 (2)
O2D—Pt1—V6 88.79 (9) V7—V6—V1 120.95 (3)
O4C—Pt1—V6 132.85 (9) Pt1—V6—V1 60.23 (2)
O3C—Pt1—V6 39.21 (9) V5—V6—V1 58.91 (2)
O8B—Pt1—V6 85.25 (10) V6—V7—V3 120.25 (3)
O7B—Pt1—V6 132.36 (9) Pt1—V7—V3 87.79 (2)
O1D—Pt1—V8 89.65 (9) V2—V7—V3 59.10 (2)
O2D—Pt1—V8 46.63 (9) V6—V7—V4 61.64 (2)
O4C—Pt1—V8 40.00 (9) Pt1—V7—V4 59.55 (2)
O3C—Pt1—V8 131.42 (9) V2—V7—V4 89.94 (3)
O8B—Pt1—V8 135.22 (10) V3—V7—V4 58.66 (2)
O7B—Pt1—V8 86.34 (9) Pt1—V8—V3 88.63 (2)
V6—Pt1—V8 123.63 (2) Pt1—V8—V9 59.88 (2)
O1D—Pt1—V9 46.16 (9) V3—V8—V9 119.00 (3)
O2D—Pt1—V9 89.07 (9) V3—V8—V2 59.15 (2)
O4C—Pt1—V9 40.35 (9) V9—V8—V2 120.00 (3)
O3C—Pt1—V9 131.59 (9) V3—V8—V4 58.82 (2)
O8B—Pt1—V9 87.36 (10) V9—V8—V4 60.19 (2)
O7B—Pt1—V9 134.69 (9) V2—V8—V4 89.43 (3)
V6—Pt1—V9 92.83 (2) Pt1—V9—V8 59.58 (2)
V8—Pt1—V9 60.54 (2) Pt1—V9—V5 87.73 (2)
O1D—Pt1—V7 88.61 (9) V8—V9—V5 119.42 (3)
O2D—Pt1—V7 45.87 (9) Pt1—V9—V1 60.07 (2)
O4C—Pt1—V7 131.81 (9) V8—V9—V1 119.64 (3)
O3C—Pt1—V7 39.46 (9) V5—V9—V1 58.99 (2)
O8B—Pt1—V7 132.43 (10) Pt1—V9—V4 59.80 (2)
O7B—Pt1—V7 86.22 (9) V8—V9—V4 60.83 (2)
V6—Pt1—V7 59.41 (2) V5—V9—V4 58.65 (2)
V8—Pt1—V7 92.22 (2) V1—V9—V4 90.08 (3)
V9—Pt1—V7 122.21 (2) O3Wi—K1—O2W 71.45 (18)
O1D—Pt1—V4 42.45 (9) O3Wi—K1—O1W 122.0 (2)
O2D—Pt1—V4 42.16 (9) O2W—K1—O1W 73.89 (15)
O4C—Pt1—V4 84.02 (8) O3Wi—K1—O12Bii 145.45 (18)
O3C—Pt1—V4 83.88 (9) O2W—K1—O12Bii 118.85 (16)
O8B—Pt1—V4 130.94 (9) O1W—K1—O12Bii 92.12 (13)
O7B—Pt1—V4 130.91 (9) O3Wi—K1—O4Wiii 78.75 (18)
V6—Pt1—V4 62.06 (2) O2W—K1—O4Wiii 128.72 (14)
V8—Pt1—V4 61.58 (2) O1W—K1—O4Wiii 155.55 (14)
V9—Pt1—V4 61.05 (2) O12Bii—K1—O4Wiii 69.55 (10)
V7—Pt1—V4 61.17 (2) O3Wi—K1—O25Tiv 82.50 (12)
O1D—Pt1—V2 133.30 (9) O2W—K1—O25Tiv 129.92 (16)
O2D—Pt1—V2 48.70 (9) O1W—K1—O25Tiv 85.91 (13)
O4C—Pt1—V2 90.75 (9) O12Bii—K1—O25Tiv 106.98 (11)
O3C—Pt1—V2 88.98 (9) O4Wiii—K1—O25Tiv 84.34 (11)
O8B—Pt1—V2 138.14 (9) O3Wi—K1—O24Tv 65.13 (14)
O7B—Pt1—V2 40.05 (9) O2W—K1—O24Tv 65.37 (12)
V6—Pt1—V2 119.45 (2) O1W—K1—O24Tv 133.36 (13)
V8—Pt1—V2 60.73 (2) O12Bii—K1—O24Tv 88.44 (10)
V9—Pt1—V2 121.27 (2) O4Wiii—K1—O24Tv 64.45 (10)
V7—Pt1—V2 60.08 (2) O25Tiv—K1—O24Tv 138.04 (10)
V4—Pt1—V2 90.86 (2) O3Wi—K1—O5Wvi 110.45 (14)
O21T—V1—O12B 102.27 (17) O2W—K1—O5Wvi 51.31 (16)
O21T—V1—O13B 102.73 (17) O1W—K1—O5Wvi 79.54 (14)
O12B—V1—O13B 90.13 (14) O12Bii—K1—O5Wvi 67.77 (12)
O21T—V1—O19B 105.72 (16) O4Wiii—K1—O5Wvi 106.58 (12)
O12B—V1—O19B 91.05 (14) O25Tiv—K1—O5Wvi 164.20 (12)
O13B—V1—O19B 150.57 (14) O24Tv—K1—O5Wvi 57.73 (10)
O21T—V1—O8B 99.44 (16) O4Wii—K2—O27Tii 96.79 (13)
O12B—V1—O8B 158.14 (14) O4Wii—K2—O28Tii 157.70 (12)
O13B—V1—O8B 82.64 (14) O27Tii—K2—O28Tii 71.43 (10)
O19B—V1—O8B 85.45 (14) O4Wii—K2—O20Bvi 124.36 (11)
O21T—V1—O1D 176.60 (16) O27Tii—K2—O20Bvi 110.65 (11)
O12B—V1—O1D 80.42 (12) O28Tii—K2—O20Bvi 77.91 (10)
O13B—V1—O1D 75.06 (12) O4Wii—K2—O8Bvii 82.79 (11)
O19B—V1—O1D 76.16 (12) O27Tii—K2—O8Bvii 73.02 (10)
O8B—V1—O1D 77.79 (12) O28Tii—K2—O8Bvii 75.73 (10)
O22T—V2—O9B 103.62 (17) O20Bvi—K2—O8Bvii 150.46 (10)
O22T—V2—O16B 104.45 (17) O4Wii—K2—O3W 78.19 (15)
O9B—V2—O16B 91.43 (15) O27Tii—K2—O3W 162.23 (13)
O22T—V2—O17B 104.04 (17) O28Tii—K2—O3W 107.12 (13)
O9B—V2—O17B 88.97 (14) O20Bvi—K2—O3W 85.81 (12)
O16B—V2—O17B 150.56 (14) O8Bvii—K2—O3W 89.37 (12)
O22T—V2—O7B 97.56 (16) O4Wii—K2—O24Tvi 69.29 (11)
O9B—V2—O7B 158.78 (14) O27Tii—K2—O24Tvi 128.86 (11)
O16B—V2—O7B 84.50 (14) O28Tii—K2—O24Tvi 132.88 (10)
O17B—V2—O7B 84.59 (13) O20Bvi—K2—O24Tvi 55.63 (9)
O22T—V2—O2D 175.77 (15) O8Bvii—K2—O24Tvi 145.32 (10)
O9B—V2—O2D 80.53 (13) O3W—K2—O24Tvi 65.65 (11)
O16B—V2—O2D 76.07 (13) O4Wii—K2—O5Wii 63.16 (12)
O17B—V2—O2D 74.97 (12) O27Tii—K2—O5Wii 72.57 (12)
O7B—V2—O2D 78.27 (11) O28Tii—K2—O5Wii 126.96 (12)
O23T—V3—O9B 104.10 (17) O20Bvi—K2—O5Wii 79.90 (12)
O23T—V3—O18B 104.12 (17) O8Bvii—K2—O5Wii 127.23 (12)
O9B—V3—O18B 92.55 (15) O3W—K2—O5Wii 118.55 (13)
O23T—V3—O15B 103.56 (18) O24Tvi—K2—O5Wii 57.03 (11)
O9B—V3—O15B 90.80 (15) O23Tvi—K3—O25Tviii 136.47 (11)
O18B—V3—O15B 150.37 (14) O23Tvi—K3—O5W 75.77 (13)
O23T—V3—O10B 101.92 (16) O25Tviii—K3—O5W 120.42 (12)
O9B—V3—O10B 153.94 (14) O23Tvi—K3—O6W 72.84 (12)
O18B—V3—O10B 82.41 (14) O25Tviii—K3—O6W 64.17 (12)
O15B—V3—O10B 81.76 (14) O5W—K3—O6W 104.30 (15)
O23T—V3—O2D 174.90 (16) O23Tvi—K3—O9W 76.16 (15)
O9B—V3—O2D 80.92 (13) O25Tviii—K3—O9W 87.40 (14)
O18B—V3—O2D 76.28 (12) O5W—K3—O9W 150.12 (16)
O15B—V3—O2D 75.21 (12) O6W—K3—O9W 76.75 (14)
O10B—V3—O2D 73.04 (12) O23Tvi—K3—O21Tix 133.79 (11)
O10B—V4—O11B 108.05 (16) O25Tviii—K3—O21Tix 74.44 (10)
O10B—V4—O6C 98.10 (15) O5W—K3—O21Tix 123.14 (14)
O11B—V4—O6C 99.13 (15) O6W—K3—O21Tix 128.44 (13)
O10B—V4—O5C 98.12 (15) O9W—K3—O21Tix 71.85 (14)
O11B—V4—O5C 96.71 (15) O23Tvi—K3—O27T 74.05 (10)
O6C—V4—O5C 152.55 (13) O25Tviii—K3—O27T 146.54 (11)
O10B—V4—O2D 87.63 (14) O5W—K3—O27T 73.96 (12)
O11B—V4—O2D 164.23 (14) O6W—K3—O27T 146.13 (12)
O6C—V4—O2D 79.74 (12) O9W—K3—O27T 88.67 (13)
O5C—V4—O2D 78.95 (12) O21Tix—K3—O27T 72.77 (10)
O10B—V4—O1D 164.37 (14) O23Tvi—K3—O4W 136.36 (11)
O11B—V4—O1D 87.58 (14) O25Tviii—K3—O4W 78.53 (11)
O6C—V4—O1D 79.38 (12) O5W—K3—O4W 61.86 (12)
O5C—V4—O1D 79.03 (12) O6W—K3—O4W 125.62 (12)
O2D—V4—O1D 76.74 (12) O9W—K3—O4W 141.67 (15)
O24T—V5—O12B 104.93 (17) O21Tix—K3—O4W 70.07 (10)
O24T—V5—O20B 103.26 (16) O27T—K3—O4W 84.26 (10)
O12B—V5—O20B 91.36 (15) O23Tvi—K3—O14Bviii 119.30 (11)
O24T—V5—O14B 103.76 (16) O25Tviii—K3—O14Bviii 53.38 (9)
O12B—V5—O14B 91.43 (15) O5W—K3—O14Bviii 67.26 (11)
O20B—V5—O14B 151.11 (14) O6W—K3—O14Bviii 72.00 (11)
O24T—V5—O11B 100.00 (16) O9W—K3—O14Bviii 137.58 (13)
O12B—V5—O11B 155.07 (14) O21Tix—K3—O14Bviii 106.80 (10)
O20B—V5—O11B 82.61 (14) O27T—K3—O14Bviii 132.52 (10)
O14B—V5—O11B 82.82 (14) O4W—K3—O14Bviii 53.88 (9)
O24T—V5—O1D 173.91 (15) O6W—K4—O16Bvii 162.73 (15)
O12B—V5—O1D 81.14 (13) O6W—K4—O26Tviii 73.88 (13)
O20B—V5—O1D 75.91 (12) O16Bvii—K4—O26Tviii 118.24 (13)
O14B—V5—O1D 76.13 (12) O6W—K4—O9W 78.81 (17)
O11B—V5—O1D 73.92 (11) O16Bvii—K4—O9W 83.95 (15)
O25T—V6—O13B 103.58 (16) O26Tviii—K4—O9W 126.27 (17)
O25T—V6—O14B 103.90 (16) O6W—K4—O26Tvii 138.56 (13)
O13B—V6—O14B 94.04 (15) O16Bvii—K4—O26Tvii 54.50 (10)
O25T—V6—O3C 97.90 (16) O26Tviii—K4—O26Tvii 64.75 (12)
O13B—V6—O3C 91.22 (14) O9W—K4—O26Tvii 124.14 (16)
O14B—V6—O3C 155.66 (14) O6W—K4—O7W 111.55 (14)
O25T—V6—O5C 102.60 (16) O16Bvii—K4—O7W 65.92 (11)
O13B—V6—O5C 152.25 (14) O26Tviii—K4—O7W 146.61 (15)
O14B—V6—O5C 88.47 (14) O9W—K4—O7W 86.49 (16)
O3C—V6—O5C 76.20 (13) O26Tvii—K4—O7W 104.46 (12)
O25T—V6—O1D 175.51 (15) O6W—K4—O3W 118.81 (16)
O13B—V6—O1D 78.63 (13) O16Bvii—K4—O3W 74.21 (12)
O14B—V6—O1D 79.71 (12) O26Tviii—K4—O3W 95.01 (14)
O3C—V6—O1D 78.07 (12) O9W—K4—O3W 138.71 (17)
O5C—V6—O1D 74.63 (12) O26Tvii—K4—O3W 68.97 (12)
O26T—V7—O15B 103.92 (18) O7W—K4—O3W 52.73 (14)
O26T—V7—O16B 102.74 (18) O8W—K5—O18Bvi 116.68 (16)
O15B—V7—O16B 95.34 (16) O8W—K5—O9B 88.96 (16)
O26T—V7—O5C 102.03 (17) O18Bvi—K5—O9B 115.20 (11)
O15B—V7—O5C 89.99 (14) O8W—K5—O7W 86.37 (17)
O16B—V7—O5C 152.57 (14) O18Bvi—K5—O7W 94.58 (12)
O26T—V7—O3C 98.14 (17) O9B—K5—O7W 148.49 (12)
O15B—V7—O3C 155.92 (14) O8W—K5—O22Tvii 67.49 (15)
O16B—V7—O3C 89.04 (14) O18Bvi—K5—O22Tvii 170.27 (11)
O5C—V7—O3C 75.93 (13) O9B—K5—O22Tvii 72.81 (10)
O26T—V7—O2D 175.00 (16) O7W—K5—O22Tvii 76.63 (12)
O15B—V7—O2D 80.25 (13) O8W—K5—O9W 142.73 (18)
O16B—V7—O2D 79.42 (13) O18Bvi—K5—O9W 100.56 (14)
O5C—V7—O2D 75.00 (12) O9B—K5—O9W 73.02 (12)
O3C—V7—O2D 77.31 (12) O7W—K5—O9W 92.42 (15)
O27T—V8—O17B 104.28 (16) O22Tvii—K5—O9W 75.98 (14)
O27T—V8—O18B 102.86 (16) O8W—K5—O23T 78.72 (14)
O17B—V8—O18B 94.12 (15) O18Bvi—K5—O23T 71.86 (10)
O27T—V8—O6C 101.85 (16) O9B—K5—O23T 55.51 (10)
O17B—V8—O6C 152.21 (14) O7W—K5—O23T 152.01 (14)
O18B—V8—O6C 89.12 (14) O22Tvii—K5—O23T 117.87 (11)
O27T—V8—O4C 98.38 (15) O9W—K5—O23T 113.75 (13)
O17B—V8—O4C 91.54 (13) Pt1—O1D—V4 99.17 (13)
O18B—V8—O4C 155.90 (13) Pt1—O1D—V9 94.73 (12)
O6C—V8—O4C 75.36 (12) V4—O1D—V9 92.37 (12)
O27T—V8—O2D 175.32 (15) Pt1—O1D—V6 93.70 (12)
O17B—V8—O2D 78.97 (13) V4—O1D—V6 93.47 (12)
O18B—V8—O2D 80.09 (13) V9—O1D—V6 168.86 (15)
O6C—V8—O2D 74.42 (12) Pt1—O1D—V1 92.47 (12)
O4C—V8—O2D 78.04 (11) V4—O1D—V1 168.36 (15)
O28T—V9—O20B 105.26 (16) V9—O1D—V1 86.35 (11)
O28T—V9—O19B 102.34 (16) V6—O1D—V1 86.01 (10)
O20B—V9—O19B 94.63 (14) Pt1—O1D—V5 174.40 (16)
O28T—V9—O6C 102.11 (16) V4—O1D—V5 86.40 (11)
O20B—V9—O6C 90.31 (14) V9—O1D—V5 85.49 (10)
O19B—V9—O6C 152.78 (13) V6—O1D—V5 85.42 (10)
O28T—V9—O4C 96.57 (15) V1—O1D—V5 81.96 (10)
O20B—V9—O4C 156.16 (14) Pt1—O2D—V4 99.47 (13)
O19B—V9—O4C 89.88 (13) Pt1—O2D—V7 95.20 (12)
O6C—V9—O4C 75.62 (12) V4—O2D—V7 93.10 (11)
O28T—V9—O1D 174.17 (15) Pt1—O2D—V8 94.04 (12)
O20B—V9—O1D 80.02 (13) V4—O2D—V8 93.16 (12)
O19B—V9—O1D 79.42 (12) V7—O2D—V8 167.84 (15)
O6C—V9—O1D 75.11 (12) Pt1—O2D—V2 92.35 (11)
O4C—V9—O1D 77.82 (11) V4—O2D—V2 168.17 (15)
V5—V1—Pt1 87.93 (2) V7—O2D—V2 85.63 (11)
V5—V1—V6 60.31 (2) V8—O2D—V2 86.10 (10)
Pt1—V1—V6 58.97 (2) Pt1—O2D—V3 173.86 (16)
V5—V1—V9 60.15 (2) V4—O2D—V3 86.57 (10)
Pt1—V1—V9 59.27 (2) V7—O2D—V3 85.52 (10)
V6—V1—V9 90.89 (3) V8—O2D—V3 84.47 (10)
V5—V1—V4 43.54 (2) V2—O2D—V3 81.61 (10)
Pt1—V1—V4 44.385 (15) V6—O3C—Pt1 101.52 (13)
V6—V1—V4 45.82 (2) V6—O3C—V7 99.96 (13)
V9—V1—V4 45.099 (19) Pt1—O3C—V7 101.69 (14)
V3—V2—V7 60.71 (3) Pt1—O4C—V8 100.70 (13)
V3—V2—Pt1 88.53 (3) Pt1—O4C—V9 100.45 (13)
V7—V2—Pt1 59.81 (2) V8—O4C—V9 100.37 (13)
V3—V2—V8 59.96 (3) V4—O5C—V7 109.01 (15)
V7—V2—V8 91.11 (3) V4—O5C—V6 109.70 (15)
Pt1—V2—V8 59.15 (2) V7—O5C—V6 101.51 (14)
V3—V2—V4 43.98 (2) V4—O6C—V9 109.15 (14)
V7—V2—V4 45.49 (2) V4—O6C—V8 108.85 (15)
Pt1—V2—V4 44.562 (14) V9—O6C—V8 103.00 (13)
V8—V2—V4 45.641 (19) Pt1—O7B—V2 100.62 (13)
V3—V2—V1 89.54 (2) Pt1—O8B—V1 101.22 (14)
V7—V2—V1 59.98 (2) V4—O10B—V3 112.76 (17)
Pt1—V2—V1 1.113 (10) V4—O11B—V5 112.09 (16)
V8—V2—V1 60.11 (2) V5—O12B—V1 116.48 (17)
V4—V2—V1 45.564 (14) V6—O13B—V1 119.14 (17)
V2—V3—V4 92.11 (3) V6—O14B—V5 117.51 (16)
V2—V3—V8 60.89 (3) V7—O15B—V3 117.70 (17)
V4—V3—V8 61.69 (3) V7—O16B—V2 117.32 (17)
V2—V3—V7 60.19 (3) V8—O17B—V2 118.96 (16)
V4—V3—V7 61.23 (2) V8—O18B—V3 117.66 (17)
V8—V3—V7 91.34 (3) V9—O19B—V1 116.70 (16)
V5—V4—Pt1 88.17 (2) V9—O20B—V5 117.45 (17)
V3—V4—Pt1 88.48 (2) H1A—O1W—H1B 109 (5)
V5—V4—V9 60.06 (2) H2A—O2W—H2B 102 (4)
V3—V4—V9 118.47 (3) H3A—O3W—H3B 107 (5)
Pt1—V4—V9 59.155 (19) H4A—O4W—H4B 109 (4)
V5—V4—V7 117.42 (3) H5A—O5W—H5B 106 (4)
V3—V4—V7 60.12 (3) H6A—O6W—H6B 109.4
Pt1—V4—V7 59.28 (2) H7A—O7W—H7B 105 (4)
V9—V4—V7 118.44 (3) H8A—O8W—H8B 103 (4)
V5—V4—V8 118.99 (3) H9A—O9W—H9B 101 (4)
V3—V4—V8 59.49 (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, y−1, z; (ix) −x, −y+1, −z.

Hydrogen-bond geometry (Å, º)

D—H···A D—H H···A D···A D—H···A
O7B—H7···O19Bix 0.90 (8) 1.86 (8) 2.738 (4) 164 (8)
O8B—H8···O4Cix 0.77 (6) 1.90 (6) 2.645 (5) 161 (6)
O1W—H1B···O9B 0.83 (3) 2.50 (6) 3.127 (6) 133 (7)
O1W—H1A···O8W 0.84 (3) 2.10 (3) 2.930 (9) 170 (8)
O2W—H2A···O15B 0.87 (3) 1.88 (3) 2.728 (6) 166 (8)
O2W—H2B···O11Bv 0.86 (3) 2.23 (5) 2.975 (6) 145 (8)
O3W—H3A···O3Cvii 0.84 (3) 1.83 (3) 2.673 (5) 177 (10)
O3W—H3B···O7W 0.83 (3) 2.09 (5) 2.875 (7) 158 (8)
O4W—H4A···O13Bix 0.83 (3) 1.88 (3) 2.680 (5) 162 (7)
O4W—H4B···O14Bviii 0.83 (3) 2.10 (4) 2.850 (5) 151 (7)
O5W—H5A···O2Wvi 0.87 (3) 1.84 (3) 2.710 (8) 175 (8)
O5W—H5B···O24Tx 0.84 (3) 2.26 (5) 2.972 (6) 142 (7)
O6W—H6A···O5Cviii 0.97 1.81 2.755 (5) 163
O6W—H6B···O10Bvi 0.97 2.04 2.755 (5) 129
O7W—H7A···O7Bvii 0.85 (3) 2.07 (4) 2.891 (5) 163 (8)
O7W—H7B···O6Cvi 0.84 (3) 2.27 (6) 2.885 (5) 130 (6)
O8W—H8A···O5Wvi 0.86 (3) 1.98 (5) 2.795 (7) 159 (10)
O8W—H8B···O19Bii 0.86 (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, y−1, z; (ix) −x, −y+1, −z; (x) −x+1, −y+1, −z.

References

  1. Brandenburg, K. (1998). DIAMOND. Crystal Impact GbR, Bonn, Germany.
  2. Brese, N. E. & O’Keeffe, M. (1991). Acta Cryst. B47, 192–197.
  3. Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244–247.
  4. Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849–854.
  5. Joo, H.-C., Park, K.-M. & Lee, U. (2011). Acta Cryst. E67, m1801–m1802. [DOI] [PMC free article] [PubMed]
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  11. Stoe & Cie (1996). STADI4, X-RED and X-SHAPE. Stoe & Cie Gmbh, Darmstadt, Germany.

Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989015009135/vn2093sup1.cif

e-71-00647-sup1.cif (271.5KB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989015009135/vn2093Isup2.hkl

e-71-00647-Isup2.hkl (372.4KB, hkl)

CCDC reference: 1400654

Additional supporting information: crystallographic information; 3D view; checkCIF report


Articles from Acta Crystallographica Section E: Crystallographic Communications are provided here courtesy of International Union of Crystallography

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