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inorganic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 10| October 2011| Page i60
https://doi.org/10.1107/S1600536811039584

Thorium divanadate dihydrate, Th(V2O7)(H2O)2

Said Yagoubi,a Lahcen El Ammari,b Abderrazzak Assanib* and Mohamed Saadib

aGroupe de Radiochimie, Institut de Physique Nucléaire d'Orsay UMR 8608, Université de Paris-Sud-11, Bât. 100, 91406 Orsay, France, and bLaboratoire de Chimie du Solide Appliquée, Faculté des Sciences, Université Mohammed V-Agdal, Avenue Ibn Battouta, BP 1014, Rabat, Morocco
*Correspondence e-mail: abder_assani@yahoo.fr

(Received 19 September 2011; accepted 26 September 2011; online 30 September 2011)

The title compound, Th(V2O7)(H2O)2, was synthesized by a hydro­thermal reaction. The crystal structure consists of ThO7(OH2)2 tricapped trigonal prisms that share edges, forming [ThO5(OH2)2]n chains along [010]. The edge-sharing ThO7(OH2)2 polyhedra share one edge and five vertices with the V2O7 divanadate anions having a nearly ecliptic conformation parallel to [001]. This results in an open framework with the water mol­ecules located in channels. O—H⋯O hydrogen bonding between water molecules and framework O atoms is observed. Bond-valence-sum calculations are in good agreement with the chemical formula of the title compound.

Related literature

For thorium compounds with ninefold coordination of the metal, see: Matkovic et al. (1968[Matkovic, B., Prodic, B. & Sljukic, M. (1968). Croat. Chem. Acta, 40, 147-161.]); Boatner (2002[Boatner, L. A. (2002). Rev. Mineral. Geochem. 48, 87-121.]); Sullens & Albrecht-Schmitt (2005[Sullens, T. A. & Albrecht-Schmitt, T. E. (2005). Inorg. Chem. 44, 2282-2286.]); Sullens et al. (2006[Sullens, T. A., Almond, P. M., Byrd, J. A., Beitz, J. V., Bray, T. H. & Albrecht- Schmitt, T. E. (2006). J. Solid State Chem. 179, 1192-1201.]); Calestani & Andreetti (1984[Calestani, G. & Andreetti, G. D. (1984). Z. Kristallogr. 168, 41-51.]); Kojić-Prodić et al. (1982[Kojić-Prodić, B., Šljukić, M. & Rużić-Toroš, Ž. (1982). Acta Cryst. B38, 67-71.]). For bond-valence sums, see: Brese & O'Keeffe (1991[Brese, N. E. & O'Keeffe, M. (1991). Acta Cryst. B47, 192-197.]).

Experimental

Crystal data

  • Th(V2O7)(H2O)2

  • Mr = 481.95

  • Triclinic, [P \overline 1]

  • a = 7.0432 (4) Å

  • b = 7.3702 (4) Å

  • c = 7.7204 (4) Å

  • α = 77.849 (2)°

  • β = 74.831 (2)°

  • γ = 85.934 (2)°

  • V = 378.08 (4) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 22.06 mm−1

  • T = 296 K

  • 0.19 × 0.12 × 0.10 mm
Data collection

  • Bruker X8 APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.052, Tmax = 0.110

  • 15216 measured reflections

  • 3576 independent reflections

  • 3506 reflections with I > 2σ(I)

  • Rint = 0.031
Refinement

  • R[F2 > 2σ(F2)] = 0.014

  • wR(F2) = 0.033

  • S = 1.15

  • 3576 reflections

  • 110 parameters

  • H-atom parameters constrained

  • Δρmax = 1.60 e Å−3

  • Δρmin = −1.26 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O8—H8A⋯O4i 0.86 2.47 3.114 (3) 133
O8—H8B⋯O5ii 0.86 1.92 2.779 (3) 175
O9—H9A⋯O1iii 0.86 1.77 2.594 (3) 160
O9—H9B⋯O5iv 0.86 1.90 2.741 (3) 166
Symmetry codes: (i) x, y, z+1; (ii) x-1, y, z+1; (iii) -x+1, -y, -z+1; (iv) x-1, y, z.

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]) and DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536811039584/fj2454sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811039584/fj2454Isup2.hkl

checkCIF report


Comment top

As reported in the literature, a few structures with ninefold coordination of thorium have been observed. In the case of orthophosphates and orthoarsenates, only two structure-types exist: the monoclinic KTh2(PO4)3 (space group C2/c) (Matkovic et al. 1968) and the monazite CePO4 (space group P21/n) structures (Boatner, 2002). The KTh2(PO4)3 structure is built from corrugated sheets parallel to (100) face of thorium polyhedra ThO9 sharing edges. Phosphate tetrahedral share vertices and edges with the thorium polyhedra to define a framework with channels occupied by K atoms. For the monazite compound, the structure shows a parallel chains to [010] direction, formed by CeO9 polyhedra that share edges. These infinite chains are connected together by edge-sharing with phosphate tetrahedra to form sheets parallel to the (100) face. The stacking of these layers along [100] direction by further edge-sharing of the CeO9 polyhedra forms a three-dimensional framework. These two structure-types (KTh2(PO4)3 and CePO4) are amongst the most important as they show the widest range of chemical composition. Dimers of edges-shared ThO9 are found in Na6[Th(PO4)(P2O7)]2 (space group P-1) (Kojić-Prodić, et al., 1982). These dimmers are connected together by sharing edges with phosphate tetrahedral into double chains along [100] direction. Pyrophosphate groups share vertices with the double chains and define a framework with channels occupied by Na atoms. Five other Th(IV) compounds with ninefold coordination and heavy oxoanions were cited in the literature: four structures containing mixed geometry anions were published by Sullens & Albrecht-Schmitt (2005); Sullens et al. (2006), Th(VO2)2(TeO6)(H2O)2, Th(SeO3)(SeO4), Th(IO3)2(SeO4)(H2O)3 H2O and Th(CrO4)(IO3)2 and one compound with mixed site Pb0.5Th0.5VO4 was published by Calestani & Andreetti (1984). For all these compounds, each ThO9 (or ThPbO9) polyhedra is bounded by the oxoanions groups.

In an effort to understand the structural chemistry of vanadate with actinides, we obtained the following compound of formula Th(V2O7)(H2O)2 under mild hydrothermal conditions. The structure of this compound consists of ThO7(OH2)2 tricapped trigonal prisms that share edges to form chains [ThO5(OH2)2]∞ along the [010] direction. The edge-sharing ThO7(OH2)2 polyhedra share one edge and five vertices with the V2O7 divanadate anions parallel to [001] direction. That builds an open framework with water molecules pointing towards the tunnels. The bond-valence sums were calculated using the coordination-independent parameters given by Brese and O'Keeffe (1991). The obtained value are as follows: Th1, 4.06; V1, 5.10 and V2, 5.18. The two oxygen atoms (O8 and O9) are concluded to be water molecules on the basis of their high isotropic displacement parameters, their bond valence sums of 0.34 (O8) and 0.47(O9), charge balance requirements. That gives the structural formula Th(V2O7)(H2O)2 for the studied compound.

Related literature top

For thorium compounds with ninefold coordination, see: Matkovic et al. (1968); Boatner (2002); Sullens & Albrecht-Schmitt (2005); Sullens et al. (2006); Calestani & Andreetti (1984); Kojić-Prodić, Šljukić & Rużić-Toroš (1982). For bond-valence sums, see: Brese & O'Keeffe (1991).

Experimental top

Crystals of Th(V2O7)(H2O)2, were hydrothermally synthesized in a 25 ml Teflon-lined steel autoclave from two mixtures: Th(NO3)4(H2O)4, NH4VO3 and V2O5 in the equimolar ratio or Th(NO3)4(H2O)4 and V2O5 in the molar ratio 4:3. Ten ml of distilled water was added in each mixture with pH = 4.5. The autoclaves were heated 7 days at 403 K then 2 days at 483 K followed by slow cooling to room temperature. The resulting product was recovered by filtration, washed with deionized water and finally air dried. The reaction product consists of orange powder and some yellow-colored crystals corresponding to the title compound which they can be isolated using ultrasonic.

Refinement top

The O-bound H atoms were initially located in a difference map and refined with O—H distance restraints of 0.86 (1). In a the last cycle they were refined in the riding model approximation with Uiso(H) set to 1.2Ueq(O). The highest and deepest hole residual peak in the final difference Fourier map are located at 0.67 Å and 0.88 Å, from Th1. The non significant distances and angles are removed from the cif file.

Structure description top

As reported in the literature, a few structures with ninefold coordination of thorium have been observed. In the case of orthophosphates and orthoarsenates, only two structure-types exist: the monoclinic KTh2(PO4)3 (space group C2/c) (Matkovic et al. 1968) and the monazite CePO4 (space group P21/n) structures (Boatner, 2002). The KTh2(PO4)3 structure is built from corrugated sheets parallel to (100) face of thorium polyhedra ThO9 sharing edges. Phosphate tetrahedral share vertices and edges with the thorium polyhedra to define a framework with channels occupied by K atoms. For the monazite compound, the structure shows a parallel chains to [010] direction, formed by CeO9 polyhedra that share edges. These infinite chains are connected together by edge-sharing with phosphate tetrahedra to form sheets parallel to the (100) face. The stacking of these layers along [100] direction by further edge-sharing of the CeO9 polyhedra forms a three-dimensional framework. These two structure-types (KTh2(PO4)3 and CePO4) are amongst the most important as they show the widest range of chemical composition. Dimers of edges-shared ThO9 are found in Na6[Th(PO4)(P2O7)]2 (space group P-1) (Kojić-Prodić, et al., 1982). These dimmers are connected together by sharing edges with phosphate tetrahedral into double chains along [100] direction. Pyrophosphate groups share vertices with the double chains and define a framework with channels occupied by Na atoms. Five other Th(IV) compounds with ninefold coordination and heavy oxoanions were cited in the literature: four structures containing mixed geometry anions were published by Sullens & Albrecht-Schmitt (2005); Sullens et al. (2006), Th(VO2)2(TeO6)(H2O)2, Th(SeO3)(SeO4), Th(IO3)2(SeO4)(H2O)3 H2O and Th(CrO4)(IO3)2 and one compound with mixed site Pb0.5Th0.5VO4 was published by Calestani & Andreetti (1984). For all these compounds, each ThO9 (or ThPbO9) polyhedra is bounded by the oxoanions groups.

In an effort to understand the structural chemistry of vanadate with actinides, we obtained the following compound of formula Th(V2O7)(H2O)2 under mild hydrothermal conditions. The structure of this compound consists of ThO7(OH2)2 tricapped trigonal prisms that share edges to form chains [ThO5(OH2)2]∞ along the [010] direction. The edge-sharing ThO7(OH2)2 polyhedra share one edge and five vertices with the V2O7 divanadate anions parallel to [001] direction. That builds an open framework with water molecules pointing towards the tunnels. The bond-valence sums were calculated using the coordination-independent parameters given by Brese and O'Keeffe (1991). The obtained value are as follows: Th1, 4.06; V1, 5.10 and V2, 5.18. The two oxygen atoms (O8 and O9) are concluded to be water molecules on the basis of their high isotropic displacement parameters, their bond valence sums of 0.34 (O8) and 0.47(O9), charge balance requirements. That gives the structural formula Th(V2O7)(H2O)2 for the studied compound.

For thorium compounds with ninefold coordination, see: Matkovic et al. (1968); Boatner (2002); Sullens & Albrecht-Schmitt (2005); Sullens et al. (2006); Calestani & Andreetti (1984); Kojić-Prodić, Šljukić & Rużić-Toroš (1982). For bond-valence sums, see: Brese & O'Keeffe (1991).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. Partial plot of Th(V2O7)(H2O)2 crystal structure. Displacement ellipsoids are drawn at the 50% probability level. Symmetry codes: (i) x - 1, y, z + 1; (ii) x, y, z + 1; (iii) -x + 1, -y + 1, -z + 1; (iv) -x + 1, -y + 1, -z + 2; (v) -x + 1, -y, -z + 2; (vi) -x + 1, -y, -z + 1; (vii) x - 1, y, z.
[Figure 2] Fig. 2. A three-dimensional polyhedral view of the crystal structure of the Th(V2O7)(H2O)2 showing polyhedra linkage.
Thorium divanadate dihydrate top
Crystal data top
Th(V2O7)(H2O)2Z = 2
Mr = 481.95F(000) = 424
Triclinic, P1Dx = 4.233 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.0432 (4) ÅCell parameters from 3576 reflections
b = 7.3702 (4) Åθ = 2.8–36.0°
c = 7.7204 (4) ŵ = 22.06 mm−1
α = 77.849 (2)°T = 296 K
β = 74.831 (2)°Prism, yellow
γ = 85.934 (2)°0.19 × 0.12 × 0.10 mm
V = 378.08 (4) Å3
Data collection top
Bruker X8 APEXII
diffractometer		3576 independent reflections
Radiation source: fine-focus sealed tube3506 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
φ and ω scansθmax = 36.0°, θmin = 2.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2005)		h = −11→11
Tmin = 0.052, Tmax = 0.110k = −12→12
15216 measured reflectionsl = −12→12
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.014H-atom parameters constrained
wR(F2) = 0.033 w = 1/[σ2(Fo2) + (0.0019P)2 + 0.3878P]
where P = (Fo2 + 2Fc2)/3
S = 1.15(Δ/σ)max = 0.003
3576 reflectionsΔρmax = 1.60 e Å−3
110 parametersΔρmin = −1.26 e Å−3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0083 (3)
Crystal data top
Th(V2O7)(H2O)2γ = 85.934 (2)°
Mr = 481.95V = 378.08 (4) Å3
Triclinic, P1Z = 2
a = 7.0432 (4) ÅMo Kα radiation
b = 7.3702 (4) ŵ = 22.06 mm−1
c = 7.7204 (4) ÅT = 296 K
α = 77.849 (2)°0.19 × 0.12 × 0.10 mm
β = 74.831 (2)°
Data collection top
Bruker X8 APEXII
diffractometer		3576 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2005)		3506 reflections with I > 2σ(I)
Tmin = 0.052, Tmax = 0.110Rint = 0.031
15216 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0140 restraints
wR(F2) = 0.033H-atom parameters constrained
S = 1.15Δρmax = 1.60 e Å−3
3576 reflectionsΔρmin = −1.26 e Å−3
110 parameters
Special details top

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

Refinement. Refinement of F2 against all reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on all data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Th10.358260 (9)0.244262 (9)1.084559 (8)0.00611 (3)
V10.79469 (5)0.33646 (5)0.25516 (4)0.00702 (6)
V20.72488 (5)0.29521 (5)0.70555 (4)0.00705 (6)
O70.6164 (2)0.4536 (2)0.8411 (2)0.0112 (3)
O10.6561 (2)0.2001 (2)0.1850 (2)0.0122 (3)
O60.6084 (3)0.0958 (2)0.8397 (2)0.0137 (3)
O31.0237 (2)0.2469 (2)0.2411 (2)0.0153 (3)
O20.7983 (3)0.5430 (2)0.1207 (2)0.0162 (3)
O40.6682 (3)0.3462 (2)0.4897 (2)0.0151 (3)
O50.9622 (3)0.2782 (3)0.6782 (2)0.0191 (3)
O80.2995 (3)0.1801 (3)1.4332 (2)0.0250 (4)
H8A0.38360.16441.49840.030*
H8B0.19080.20631.50610.030*
O90.1870 (4)0.1056 (3)0.9082 (4)0.0366 (6)
H9A0.22110.00970.85940.044*
H9B0.10360.16420.85190.044*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Th10.00668 (4)0.00456 (3)0.00738 (3)0.00008 (2)−0.00182 (2)−0.00181 (2)
V10.00677 (13)0.00767 (13)0.00671 (12)−0.00029 (10)−0.00215 (10)−0.00106 (10)
V20.00842 (13)0.00610 (13)0.00644 (12)0.00028 (10)−0.00092 (10)−0.00219 (10)
O70.0146 (7)0.0082 (6)0.0112 (6)0.0006 (5)−0.0021 (5)−0.0050 (5)
O10.0109 (6)0.0117 (7)0.0160 (6)0.0013 (5)−0.0050 (5)−0.0054 (5)
O60.0204 (8)0.0070 (6)0.0129 (6)−0.0018 (6)−0.0026 (6)−0.0016 (5)
O30.0097 (6)0.0200 (8)0.0139 (6)0.0018 (6)−0.0020 (5)−0.0006 (6)
O20.0186 (8)0.0122 (7)0.0176 (7)−0.0045 (6)−0.0092 (6)0.0049 (6)
O40.0159 (7)0.0211 (8)0.0084 (6)0.0043 (6)−0.0033 (5)−0.0046 (5)
O50.0100 (7)0.0303 (10)0.0163 (7)0.0025 (7)−0.0016 (6)−0.0063 (7)
O80.0151 (8)0.0467 (13)0.0123 (7)0.0038 (8)−0.0024 (6)−0.0066 (7)
O90.0460 (13)0.0252 (10)0.0645 (15)0.0236 (10)−0.0464 (13)−0.0327 (11)
Geometric parameters (Å, º) top
Th1—O3i2.3508 (16)V1—O11.7037 (16)
Th1—O1ii2.3988 (15)V1—O41.8109 (16)
Th1—O2iii2.4104 (15)V2—O51.6285 (17)
Th1—O7iv2.4430 (16)V2—O61.7296 (16)
Th1—O92.4440 (19)V2—O71.7351 (16)
Th1—O6v2.4598 (16)V2—O41.7722 (15)
Th1—O82.5593 (17)O8—H8A0.8599
Th1—O72.5706 (16)O8—H8B0.8599
Th1—O62.5937 (17)O9—H9A0.8600
V1—O21.6498 (16)O9—H9B0.8600
V1—O31.6845 (16)
O3i—Th1—O1ii133.04 (5)O6v—Th1—O7123.52 (5)
O3i—Th1—O2iii74.96 (6)O8—Th1—O7128.58 (6)
O1ii—Th1—O2iii141.47 (6)O3i—Th1—O6142.46 (6)
O3i—Th1—O7iv87.85 (6)O1ii—Th1—O674.59 (5)
O1ii—Th1—O7iv79.21 (5)O2iii—Th1—O697.58 (6)
O2iii—Th1—O7iv75.88 (6)O7iv—Th1—O6126.68 (5)
O3i—Th1—O974.46 (8)O9—Th1—O669.48 (7)
O1ii—Th1—O9139.27 (6)O6v—Th1—O664.61 (6)
O2iii—Th1—O963.63 (7)O8—Th1—O6130.52 (6)
O7iv—Th1—O9138.65 (6)O7—Th1—O661.59 (5)
O3i—Th1—O6v93.95 (6)O2—V1—O3111.26 (9)
O1ii—Th1—O6v77.24 (6)O2—V1—O1106.38 (8)
O2iii—Th1—O6v134.16 (6)O3—V1—O1110.92 (8)
O7iv—Th1—O6v149.25 (5)O2—V1—O4110.99 (9)
O9—Th1—O6v70.53 (6)O3—V1—O4111.03 (8)
O3i—Th1—O866.51 (6)O1—V1—O4106.04 (8)
O1ii—Th1—O866.54 (6)O5—V2—O6111.61 (9)
O2iii—Th1—O8131.90 (7)O5—V2—O7112.45 (9)
O7iv—Th1—O875.03 (6)O6—V2—O799.47 (8)
O9—Th1—O8126.93 (8)O5—V2—O4110.14 (8)
O6v—Th1—O877.61 (6)O6—V2—O4110.71 (8)
O3i—Th1—O7140.50 (5)O7—V2—O4112.08 (8)
O1ii—Th1—O773.42 (5)V2—O4—V1136.90 (10)
O2iii—Th1—O769.92 (5)H8A—O8—H8B104.5
O7iv—Th1—O766.76 (6)H9A—O9—H9B104.5
O9—Th1—O7104.44 (8)
Symmetry codes: (i) x−1, y, z+1; (ii) x, y, z+1; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y+1, −z+2; (v) −x+1, −y, −z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8A···O4ii0.862.473.114 (3)133
O8—H8B···O5i0.861.922.779 (3)175
O9—H9A···O1vi0.861.772.594 (3)160
O9—H9B···O5vii0.861.902.741 (3)166
Symmetry codes: (i) x−1, y, z+1; (ii) x, y, z+1; (vi) −x+1, −y, −z+1; (vii) x−1, y, z.

Experimental details

Crystal data
Chemical formulaTh(V2O7)(H2O)2
Mr481.95
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)7.0432 (4), 7.3702 (4), 7.7204 (4)
α, β, γ (°)77.849 (2), 74.831 (2), 85.934 (2)
V (Å3)378.08 (4)
Z2
Radiation typeMo Kα
µ (mm−1)22.06
Crystal size (mm)0.19 × 0.12 × 0.10
Data collection
DiffractometerBruker X8 APEXII
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2005)
Tmin, Tmax0.052, 0.110
No. of measured, independent and
observed [I > 2σ(I)] reflections		15216, 3576, 3506
Rint0.031
(sin θ/λ)max (Å−1)0.827
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.014, 0.033, 1.15
No. of reflections3576
No. of parameters110
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)1.60, −1.26

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2006), WinGX (Farrugia, 1999).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8A···O4i0.862.473.114 (3)133
O8—H8B···O5ii0.861.922.779 (3)175
O9—H9A···O1iii0.861.772.594 (3)160
O9—H9B···O5iv0.861.902.741 (3)166
Symmetry codes: (i) x, y, z+1; (ii) x−1, y, z+1; (iii) −x+1, −y, −z+1; (iv) x−1, y, z.
 

Acknowledgements

The authors thank the Unit of Support for Technical and Scientific Research (UATRS, CNRST) for the X-ray measurements.

References

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ISSN: 2056-9890
Volume 67| Part 10| October 2011| Page i60
https://doi.org/10.1107/S1600536811039584
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