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

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

doi:10.1107/S2056989015009135

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ISSN: 2056-9890

Volume 71| Part 6| June 2015| Pages 647-649

doi:10.1107/S2056989015009135

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

Hea-Chung Joo ^a and Uk Lee ^a ^*

^aDepartment of Chemistry, Pukyong National University, 599-1 Daeyeon 3-dong, Nam-gu, Busan 608-737, Republic of Korea
^*Correspondence e-mail: uklee@pknu.ac.kr

Edited by A. Van der Lee, Université de Montpellier II, France (Received 8 May 2015; accepted 13 May 2015; online 20 May 2015)

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.

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

CCDC reference: 1400654

1. Structural commentary

Two heteropolyanions that belong to the decavanadate structure system (Lee, 2006 ) have recently been reported: the tellurium derivative [H_nTeV₉O₂₈]⁽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 [H_nTeV₉O₂₈]⁽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), OC (μ₃-O), and OD (μ₄-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).

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7B—H7⋯O19Bⁱ	0.90 (8)	1.86 (8)	2.738 (4)	164 (8)
O8B—H8⋯O4Cⁱ	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⋯O11Bⁱⁱ	0.86 (3)	2.23 (5)	2.975 (6)	145 (8)
O3W—H3A⋯O3Cⁱⁱⁱ	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⋯O13Bⁱ	0.83 (3)	1.88 (3)	2.680 (5)	162 (7)
O4W—H4B⋯O14B^iv	0.83 (3)	2.10 (4)	2.850 (5)	151 (7)
O5W—H5A⋯O2W^v	0.87 (3)	1.84 (3)	2.710 (8)	175 (8)
O5W—H5B⋯O24T^vi	0.84 (3)	2.26 (5)	2.972 (6)	142 (7)
O6W—H6A⋯O5C^iv	0.97	1.81	2.755 (5)	163
O6W—H6B⋯O10B^v	0.97	2.04	2.755 (5)	129
O7W—H7A⋯O7Bⁱⁱⁱ	0.85 (3)	2.07 (4)	2.891 (5)	163 (8)
O7W—H7B⋯O6C^v	0.84 (3)	2.27 (6)	2.885 (5)	130 (6)
O8W—H8A⋯O5W^v	0.86 (3)	1.98 (5)	2.795 (7)	159 (10)
O8W—H8B⋯O19B^vii	0.86 (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, y-1, z; (v) -x+1, -y+1, -z+1; (vi) -x+1, -y+1, -z; (vii) x, y, z+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
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.]

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).

2. 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.

3. 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-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.

Table 2
Experimental details

Crystal data
Chemical formula	K₅[H₂PtV₉O₂₈]·9H₂O
M_r	1461.21
Crystal system, space group	Triclinic, P $[\overline{1}]$
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)
V (Å³)	1645.8 (3)
Z	2
Radiation type	Mo Kα
μ (mm⁻¹)	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 > 2σ(I)] reflections	6797, 6797, 6242
(sin θ/λ)_max (Å⁻¹)	0.628

Refinement
R[F² > 2σ(F²)], wR(F²), 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
Δρ_max, Δρ_min (e Å⁻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 ).

Supporting information

CCDC reference: 1400654

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

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

checkCIF report

Structural commentary top

Two heteropolyanions that belong to the decavanadate structure system (Lee, 2006) have recently been reported: the tellurium derivative [H_nTeV₉O₂₈]^(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 [H_nTeV₉O₂₈]^(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, Mo═O), OB (bridging, µ₂-O), OC (µ₃-O), and OD (µ₄-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 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 the SHELXL2014 command DFIX, and were included in the refinement with U_iso(H) = 1.5 U_eq(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

	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.
	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]·9H₂O	Z = 2
M_r = 1461.21	F(000) = 1392
Triclinic, P1	D_x = 2.949 Mg m⁻³
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 mm⁻¹
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 top

Stoe Stadi4 diffractometer	R_int = 0.0000
Radiation source: fine-focus sealed tube	θ_max = 26.5°, θ_min = 1.6°
ω/2–θ scans	h = −12→12
Absorption correction: empirical (using intensity measurements) (X-SHAPE; Stoe & Cie,1996)	k = −16→15
T_min = 0.301, T_max = 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 top

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(F_o²) + (0.0277P)² + 4.5476P] where P = (F_o² + 2F_c²)/3
S = 1.10	(Δ/σ)_max < 0.001
6797 reflections	Δρ_max = 1.30 e Å⁻³
526 parameters	Δρ_min = −1.46 e Å⁻³
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)

Crystal data top

K₅[H₂PtV₉O₂₈]·9H₂O	γ = 92.480 (4)°
M_r = 1461.21	V = 1645.8 (3) Å³
Triclinic, P1	Z = 2
a = 10.1663 (7) Å	Mo Kα radiation
b = 12.8350 (7) Å	µ = 7.42 mm⁻¹
c = 13.615 (2) Å	T = 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)	R_int = 0.0000
T_min = 0.301, T_max = 0.378	3 standard reflections every 60 min
6797 measured reflections	intensity decay: 2.5%
6797 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	25 restraints
wR(F²) = 0.066	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	Δρ_max = 1.30 e Å⁻³
6797 reflections	Δρ_min = −1.46 e Å⁻³
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

	x	y	z	U_iso*/U_eq
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) top

	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) top

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—O25T^iv	2.924 (4)
V4—V7	3.2078 (11)	K1—O24T^v	3.267 (4)
V4—V8	3.2162 (10)	K1—O5W^vi	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—O20B^vi	2.772 (3)
Pt1—O1D	1.985 (3)	K2—O8B^vii	2.917 (3)
Pt1—O2D	1.986 (3)	K2—O3W	2.936 (7)
Pt1—O4C	2.015 (3)	K2—O24T^vi	3.069 (4)
Pt1—O3C	2.017 (3)	K2—O5Wⁱⁱ	3.156 (5)
Pt1—O8B	2.027 (3)	K3—O23T^vi	2.844 (4)
Pt1—O7B	2.036 (3)	K3—O25T^viii	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—O21T^ix	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—O14B^viii	3.151 (3)
V2—O9B	1.862 (3)	K4—O6W	2.733 (5)
V2—O16B	1.863 (3)	K4—O16B^vii	2.806 (4)
V2—O17B	1.885 (3)	K4—O26T^viii	2.841 (4)
V2—O7B	2.067 (3)	K4—O9W	2.904 (5)
V2—O2D	2.374 (3)	K4—O26T^vii	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—O18B^vi	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—O22T^vii	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—O25T^iv	82.50 (12)
O1D—Pt1—V2	133.30 (9)	O2W—K1—O25T^iv	129.92 (16)
O2D—Pt1—V2	48.70 (9)	O1W—K1—O25T^iv	85.91 (13)
O4C—Pt1—V2	90.75 (9)	O12Bⁱⁱ—K1—O25T^iv	106.98 (11)
O3C—Pt1—V2	88.98 (9)	O4Wⁱⁱⁱ—K1—O25T^iv	84.34 (11)
O8B—Pt1—V2	138.14 (9)	O3Wⁱ—K1—O24T^v	65.13 (14)
O7B—Pt1—V2	40.05 (9)	O2W—K1—O24T^v	65.37 (12)
V6—Pt1—V2	119.45 (2)	O1W—K1—O24T^v	133.36 (13)
V8—Pt1—V2	60.73 (2)	O12Bⁱⁱ—K1—O24T^v	88.44 (10)
V9—Pt1—V2	121.27 (2)	O4Wⁱⁱⁱ—K1—O24T^v	64.45 (10)
V7—Pt1—V2	60.08 (2)	O25T^iv—K1—O24T^v	138.04 (10)
V4—Pt1—V2	90.86 (2)	O3Wⁱ—K1—O5W^vi	110.45 (14)
O21T—V1—O12B	102.27 (17)	O2W—K1—O5W^vi	51.31 (16)
O21T—V1—O13B	102.73 (17)	O1W—K1—O5W^vi	79.54 (14)
O12B—V1—O13B	90.13 (14)	O12Bⁱⁱ—K1—O5W^vi	67.77 (12)
O21T—V1—O19B	105.72 (16)	O4Wⁱⁱⁱ—K1—O5W^vi	106.58 (12)
O12B—V1—O19B	91.05 (14)	O25T^iv—K1—O5W^vi	164.20 (12)
O13B—V1—O19B	150.57 (14)	O24T^v—K1—O5W^vi	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—O20B^vi	124.36 (11)
O21T—V1—O1D	176.60 (16)	O27Tⁱⁱ—K2—O20B^vi	110.65 (11)
O12B—V1—O1D	80.42 (12)	O28Tⁱⁱ—K2—O20B^vi	77.91 (10)
O13B—V1—O1D	75.06 (12)	O4Wⁱⁱ—K2—O8B^vii	82.79 (11)
O19B—V1—O1D	76.16 (12)	O27Tⁱⁱ—K2—O8B^vii	73.02 (10)
O8B—V1—O1D	77.79 (12)	O28Tⁱⁱ—K2—O8B^vii	75.73 (10)
O22T—V2—O9B	103.62 (17)	O20B^vi—K2—O8B^vii	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)	O20B^vi—K2—O3W	85.81 (12)
O16B—V2—O17B	150.56 (14)	O8B^vii—K2—O3W	89.37 (12)
O22T—V2—O7B	97.56 (16)	O4Wⁱⁱ—K2—O24T^vi	69.29 (11)
O9B—V2—O7B	158.78 (14)	O27Tⁱⁱ—K2—O24T^vi	128.86 (11)
O16B—V2—O7B	84.50 (14)	O28Tⁱⁱ—K2—O24T^vi	132.88 (10)
O17B—V2—O7B	84.59 (13)	O20B^vi—K2—O24T^vi	55.63 (9)
O22T—V2—O2D	175.77 (15)	O8B^vii—K2—O24T^vi	145.32 (10)
O9B—V2—O2D	80.53 (13)	O3W—K2—O24T^vi	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)	O20B^vi—K2—O5Wⁱⁱ	79.90 (12)
O23T—V3—O18B	104.12 (17)	O8B^vii—K2—O5Wⁱⁱ	127.23 (12)
O9B—V3—O18B	92.55 (15)	O3W—K2—O5Wⁱⁱ	118.55 (13)
O23T—V3—O15B	103.56 (18)	O24T^vi—K2—O5Wⁱⁱ	57.03 (11)
O9B—V3—O15B	90.80 (15)	O23T^vi—K3—O25T^viii	136.47 (11)
O18B—V3—O15B	150.37 (14)	O23T^vi—K3—O5W	75.77 (13)
O23T—V3—O10B	101.92 (16)	O25T^viii—K3—O5W	120.42 (12)
O9B—V3—O10B	153.94 (14)	O23T^vi—K3—O6W	72.84 (12)
O18B—V3—O10B	82.41 (14)	O25T^viii—K3—O6W	64.17 (12)
O15B—V3—O10B	81.76 (14)	O5W—K3—O6W	104.30 (15)
O23T—V3—O2D	174.90 (16)	O23T^vi—K3—O9W	76.16 (15)
O9B—V3—O2D	80.92 (13)	O25T^viii—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)	O23T^vi—K3—O21T^ix	133.79 (11)
O10B—V4—O11B	108.05 (16)	O25T^viii—K3—O21T^ix	74.44 (10)
O10B—V4—O6C	98.10 (15)	O5W—K3—O21T^ix	123.14 (14)
O11B—V4—O6C	99.13 (15)	O6W—K3—O21T^ix	128.44 (13)
O10B—V4—O5C	98.12 (15)	O9W—K3—O21T^ix	71.85 (14)
O11B—V4—O5C	96.71 (15)	O23T^vi—K3—O27T	74.05 (10)
O6C—V4—O5C	152.55 (13)	O25T^viii—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)	O21T^ix—K3—O27T	72.77 (10)
O10B—V4—O1D	164.37 (14)	O23T^vi—K3—O4W	136.36 (11)
O11B—V4—O1D	87.58 (14)	O25T^viii—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)	O21T^ix—K3—O4W	70.07 (10)
O24T—V5—O20B	103.26 (16)	O27T—K3—O4W	84.26 (10)
O12B—V5—O20B	91.36 (15)	O23T^vi—K3—O14B^viii	119.30 (11)
O24T—V5—O14B	103.76 (16)	O25T^viii—K3—O14B^viii	53.38 (9)
O12B—V5—O14B	91.43 (15)	O5W—K3—O14B^viii	67.26 (11)
O20B—V5—O14B	151.11 (14)	O6W—K3—O14B^viii	72.00 (11)
O24T—V5—O11B	100.00 (16)	O9W—K3—O14B^viii	137.58 (13)
O12B—V5—O11B	155.07 (14)	O21T^ix—K3—O14B^viii	106.80 (10)
O20B—V5—O11B	82.61 (14)	O27T—K3—O14B^viii	132.52 (10)
O14B—V5—O11B	82.82 (14)	O4W—K3—O14B^viii	53.88 (9)
O24T—V5—O1D	173.91 (15)	O6W—K4—O16B^vii	162.73 (15)
O12B—V5—O1D	81.14 (13)	O6W—K4—O26T^viii	73.88 (13)
O20B—V5—O1D	75.91 (12)	O16B^vii—K4—O26T^viii	118.24 (13)
O14B—V5—O1D	76.13 (12)	O6W—K4—O9W	78.81 (17)
O11B—V5—O1D	73.92 (11)	O16B^vii—K4—O9W	83.95 (15)
O25T—V6—O13B	103.58 (16)	O26T^viii—K4—O9W	126.27 (17)
O25T—V6—O14B	103.90 (16)	O6W—K4—O26T^vii	138.56 (13)
O13B—V6—O14B	94.04 (15)	O16B^vii—K4—O26T^vii	54.50 (10)
O25T—V6—O3C	97.90 (16)	O26T^viii—K4—O26T^vii	64.75 (12)
O13B—V6—O3C	91.22 (14)	O9W—K4—O26T^vii	124.14 (16)
O14B—V6—O3C	155.66 (14)	O6W—K4—O7W	111.55 (14)
O25T—V6—O5C	102.60 (16)	O16B^vii—K4—O7W	65.92 (11)
O13B—V6—O5C	152.25 (14)	O26T^viii—K4—O7W	146.61 (15)
O14B—V6—O5C	88.47 (14)	O9W—K4—O7W	86.49 (16)
O3C—V6—O5C	76.20 (13)	O26T^vii—K4—O7W	104.46 (12)
O25T—V6—O1D	175.51 (15)	O6W—K4—O3W	118.81 (16)
O13B—V6—O1D	78.63 (13)	O16B^vii—K4—O3W	74.21 (12)
O14B—V6—O1D	79.71 (12)	O26T^viii—K4—O3W	95.01 (14)
O3C—V6—O1D	78.07 (12)	O9W—K4—O3W	138.71 (17)
O5C—V6—O1D	74.63 (12)	O26T^vii—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—O18B^vi	116.68 (16)
O15B—V7—O16B	95.34 (16)	O8W—K5—O9B	88.96 (16)
O26T—V7—O5C	102.03 (17)	O18B^vi—K5—O9B	115.20 (11)
O15B—V7—O5C	89.99 (14)	O8W—K5—O7W	86.37 (17)
O16B—V7—O5C	152.57 (14)	O18B^vi—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—O22T^vii	67.49 (15)
O16B—V7—O3C	89.04 (14)	O18B^vi—K5—O22T^vii	170.27 (11)
O5C—V7—O3C	75.93 (13)	O9B—K5—O22T^vii	72.81 (10)
O26T—V7—O2D	175.00 (16)	O7W—K5—O22T^vii	76.63 (12)
O15B—V7—O2D	80.25 (13)	O8W—K5—O9W	142.73 (18)
O16B—V7—O2D	79.42 (13)	O18B^vi—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)	O22T^vii—K5—O9W	75.98 (14)
O27T—V8—O18B	102.86 (16)	O8W—K5—O23T	78.72 (14)
O17B—V8—O18B	94.12 (15)	O18B^vi—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)	O22T^vii—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) top

D—H···A	D—H	H···A	D···A	D—H···A
O7B—H7···O19B^ix	0.90 (8)	1.86 (8)	2.738 (4)	164 (8)
O8B—H8···O4C^ix	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···O11B^v	0.86 (3)	2.23 (5)	2.975 (6)	145 (8)
O3W—H3A···O3C^vii	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···O13B^ix	0.83 (3)	1.88 (3)	2.680 (5)	162 (7)
O4W—H4B···O14B^viii	0.83 (3)	2.10 (4)	2.850 (5)	151 (7)
O5W—H5A···O2W^vi	0.87 (3)	1.84 (3)	2.710 (8)	175 (8)
O5W—H5B···O24T^x	0.84 (3)	2.26 (5)	2.972 (6)	142 (7)
O6W—H6A···O5C^viii	0.97	1.81	2.755 (5)	163
O6W—H6B···O10B^vi	0.97	2.04	2.755 (5)	129
O7W—H7A···O7B^vii	0.85 (3)	2.07 (4)	2.891 (5)	163 (8)
O7W—H7B···O6C^vi	0.84 (3)	2.27 (6)	2.885 (5)	130 (6)
O8W—H8A···O5W^vi	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.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7B—H7···O19Bⁱ	0.90 (8)	1.86 (8)	2.738 (4)	164 (8)
O8B—H8···O4Cⁱ	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···O11Bⁱⁱ	0.86 (3)	2.23 (5)	2.975 (6)	145 (8)
O3W—H3A···O3Cⁱⁱⁱ	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···O13Bⁱ	0.83 (3)	1.88 (3)	2.680 (5)	162 (7)
O4W—H4B···O14B^iv	0.83 (3)	2.10 (4)	2.850 (5)	151 (7)
O5W—H5A···O2W^v	0.87 (3)	1.84 (3)	2.710 (8)	175 (8)
O5W—H5B···O24T^vi	0.84 (3)	2.26 (5)	2.972 (6)	142 (7)
O6W—H6A···O5C^iv	0.97	1.81	2.755 (5)	162.7
O6W—H6B···O10B^v	0.97	2.04	2.755 (5)	129.0
O7W—H7A···O7Bⁱⁱⁱ	0.85 (3)	2.07 (4)	2.891 (5)	163 (8)
O7W—H7B···O6C^v	0.84 (3)	2.27 (6)	2.885 (5)	130 (6)
O8W—H8A···O5W^v	0.86 (3)	1.98 (5)	2.795 (7)	159 (10)
O8W—H8B···O19B^vii	0.86 (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, y−1, z; (v) −x+1, −y+1, −z+1; (vi) −x+1, −y+1, −z; (vii) x, y, z+1.

Experimental details

Crystal data
Chemical formula	K₅[H₂PtV₉O₂₈]·9H₂O
M_r	1461.21
Crystal system, space group	Triclinic, 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)
V (Å³)	1645.8 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	7.42
Crystal size (mm)	0.21 × 0.19 × 0.17

Data collection
Diffractometer	Stoe Stadi4 diffractometer
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 > 2σ(I)] reflections	6797, 6797, 6242
R_int	0.0000
(sin θ/λ)_max (Å⁻¹)	0.628

Refinement
R[F² > 2σ(F²)], wR(F²), 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
Δρ_max, Δρ_min (e Å⁻³)	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).

References

Brandenburg, K. (1998). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Brese, N. E. & O'Keeffe, M. (1991). Acta Cryst. B47, 192–197. CrossRef CAS Web of Science IUCr Journals Google Scholar
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244–247. CrossRef CAS Web of Science IUCr Journals Google Scholar
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849–854. Web of Science CrossRef CAS IUCr Journals Google Scholar
Joo, H.-C., Park, K.-M. & Lee, U. (2011). Acta Cryst. E67, m1801–m1802. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
Konaka, S., Ozawa, Y., Shonaka, T., Watanabe, S. & Yagasaki, A. (2011). Inorg. Chem. 50, 6183–6188. Web of Science CSD CrossRef CAS PubMed Google Scholar
Lee, U. (2006). Acta Cryst. E62, i176–i178. Web of Science CrossRef IUCr Journals Google Scholar
Lee, U., Joo, H.-C., Park, K.-M., Mal, S. S., Kortz, U., Keita, B. & Nadjo, L. (2008). Angew. Chem. Int. Ed. 47, 793–796. CrossRef CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sheldrick, G. M. (2015). Acta Cryst. C71, 3–8. Web of Science CrossRef IUCr Journals Google Scholar
Stoe & Cie (1996). STADI4, X-RED and X-SHAPE. Stoe & Cie Gmbh, Darmstadt, Germany. Google Scholar

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Volume 71| Part 6| June 2015| Pages 647-649

doi:10.1107/S2056989015009135

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research communications\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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

1. Structural commentary

2. Synthesis and crystallization

3. Refinement

Supporting information

References

research communications

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