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Acta Cryst. (2009). E65, i46-i47    [ doi:10.1107/S1600536809019126 ]

Sr5(VIVOF5)3F(H2O)3 refined from a non-merohedrally twinned crystal

A. Le Bail, A.-M. Mercier and I. Dix

Abstract top

The title compound, pentastrontium tris[pentafluoridooxidovanadate(IV)] fluoride trihydrate, was obtained under hydrothermal conditions. Its crystal structure has been refined from intensity data of a non-merohedrally twinned crystal. Two domains in almost equal proportions are related by a -180° rotation along the reciprocal [101]* vector. The structure may be considered as a derivative of the fluorite structure type, adopted here by SrF2. In the title compound, fluorite-like large rods are recognized, built up from a group of 16 Sr atoms of which 6 are substituted by V atoms, leading to [Sr10V6][infinity] units. These rods extend infinitely along the b axis and are interconnected by the three water molecules. Each of the water molecules is shared by two different Sr atoms belonging to two different rods. The rods are also interconnected by an `independent' F atom in a distorted triangular [FSr3] coordination and by hydrogen-bonding interactions via donor water molecules. The acceptors are either F atoms or the O atoms of the vanadyl ion, VO2+, that is part of the [VOF5] isolated octahedron.

Comment top

The title compound is the first hydrated strontium vanadium oxy-fluoride characterized crystallographically. It is built up from a network of SrOxFy polyhedra (x + y = 9 — 12), connected by faces, edges and vertices. Isolated (VIVOF5)3- octahedra with a short VIV═O bond (1.596 (4)—1.691 (4) Å) characteristic of a vanadyl ion, VO2+, (Crosnier-Lopez et al., 1994) are inserted into this network (Fig. 1). One of the fluorine atoms (F1) is shared exclusively by three strontium atoms (Sr1, Sr2, Sr3) in a triangular [FSr3] coordination, and will be named 'independent' according to previous descriptions (such a structure unit is also present in Sr5Zr3F22 (Le Bail, 1996); it shows the same A5B3X22 formula as the title compound). The three water molecules coordinate to these three (Sr1, Sr2, Sr3) strontium atoms, all of which have an overall ninefold coordination (Fig. 2), that is best described by a distorted tri-capped trigonal prism. The two remaining strontium atoms are exclusively coordinated by F atoms. The distorted [Sr(5)F12] cuboctahedron is connected to the [Sr(4)F11] polyhedra (best described as a defect cuboctahedron, lacking one vertex) by a square face (Fig. 3).

Any strong relation with the fluorite structure (adopted by SrF2) seems to be ruled out by the absence of F atoms in tetrahedral coordination [FSr4]. However, most F atoms are forming [FSr3V] distorted tetrahedra. One may consider that four strontium atoms (two Sr(4)F11 and two Sr(5)12 polyhedra sharing faces) represent a small fluorite structure relic around which half of the expected 12 Sr atoms are replaced by V atoms (forming [Sr10V6] blocks), which leads to the [FSr3V] distorted tetrahedra. Indeed, these blocks form infinite rods along the b axis, with formulation [Sr5V3]∞. The oxygen atoms of the six [VOF5] octahedra are part of the vanadyl VIV═O double bond and are all directed externally to these rods. This is well seen on the crystal structure projection (Fig. 4) where the water molecules are also placed in the rod interstices together with the F1 atom. Both types of ligands play a role in the interconnections between the rods. The relation of Sr5(VIVOF5)3F(H2O)3 with the SrF2 fluorite structure is provided in Fig. 5.

The hydrogen bonding involves both O and F atoms through Ow—H···O/F interactions (Table 1), participating in the interconnection of the [Sr10V6]∞ rods. One of these hydrogen bonds is clearly bifurcated (O1—H11···O4/O5). The distinction between F and O atoms was evident from the valence bond analysis (Table 2) according to the empirical expression given by Brown & Altermatt (1985), using parameters from Brese & O'Keeffe (1991). The valence bond analysis allows also to recognize the water molecules. The short vanadium-oxygen bond is characteristic of a vanadyl VIV═O double bond.

Thermal analysis (TGA) measurement from selected crystals shows a mass loss starting close to 573 K, without any clear stop for the expected 3H2O release; the corresponding 5.42% mass loss is attained at 693 K, then the mass loss accelerates and attains 17% up to 873 K. The X-ray powder diffraction pattern of the final product is similar to fluorite-type SrF2, but the real composition is more probably corresponding to a fluorite solid solution with formula close to Sr5V3IIIO3F13, i.e. (Sr/V)(O/F)2 which may be topotactically rebuilt from the title compound arrangement by re-aligning the fluorite-like [Sr10V6]∞ rods.

Related literature top

For VIV in [VOF5] coordination, see: Crosnier-Lopez et al. (1994). Sr2V2IIIF10.H2O which was also synthesized during this study is isostructural with Sr2Fe2F10.H2O (Le Meins et al., 1997). For a description of similar 'independent' F atoms in the crystal structure of Sr5Zr3F22, see: Le Bail (1996). For bond-valence analysis, see: Brown & Altermatt (1985); Brese & O'Keeffe (1991).

Experimental top

Hydrothermal growth at 493 K from (SrF2/VF3) in HF 5M or 1M solutions produced mixtures of pale-blue-green needle-like crystals (dominant in 5M solution), accompanied with polycrystalline Sr2V2IIIF10.H2O (dominant in 1M solution). The latter compound is orthorhombic, with cell parameters a = 7.8653 (4) Å, b = 19.9298 (7) Å, c = 10.7322 (6) Å (from X-ray powder data), space group Cmca, and is isostructural with Sr2Fe2F10.H2O (Le Meins et al., 1997). All crystals of the title compound were found to be systematically affected by non-merohedral twinning (see Refinement section).

Refinement top

From a first data collection on a conventional four-circle diffractometer, the structure could be solved in spite of the twinning, removing a lot of reflections that belong to two domains, or that were partly overlapping. However, the final data/parameter ratio was so poor that a second data collection was performed (years later), using a Bruker SMART APEX system.

24642 single reflections were attributed to domain 1 (4436 unique), 24601 to domain 2 (4416 unique), and there were 11156 overlapping reflections attributed to both domains.

The reflections were integrated and processed into a HKLF5 file used for the refinement. The final refinement was based on the data set of domain 1. The SHELXL BASF parameter refined to 0.511. A view of the reflection spots of domains 1 and 2 is shown in Fig. 6.

The H atoms were located in Fourier difference maps and their positions could be refined freely. Because of the large spread of O—H and H—H distances, they were finally refined applying soft constraints (0.90 (2) Å for O—H). Their thermal parameters were fixed at 1.2 times that of the corresponding water oxygen atom.

The distinction between F and O atoms was clear from the valence bond analysis, allowing also to recognize the water molecules. The short vanadium-oxygen bond is characteristic of a vanadyl VIV=O double bond.

In the final Fourier map the highest peak is 0.85 Å from atom Sr1 and the deepest hole is 0.82 Å from atom Sr2.

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: publCIF (Westrip, 2009).

Figures top
[Figure 1] Fig. 1. ORTEP-3 view of the [VIVOF5]3- octahedra showing the off-centered V position with short V=O distances (1.596–1.691 Å) and long opposite V—F distances (2.056–2.105 Å). Displacement ellipsoids are drawn at the 50% probability level.
[Figure 2] Fig. 2. ORTEP-3 view of the three SrX9 (X = F,O,H2O) tri-capped trigonal prisms, sharing the F1 atom and two of the three water molecules. This shows how three different fluorite-like [Sr10V6] infinite rods are mainly interconnected. Displacement ellipsoids are drawn at the 50% probability level.
[Figure 3] Fig. 3. ORTEP-3 view of the Sr(5)F12 cuboctahedron and Sr(4)F11 truncated cuboctahedron associated by a face. This situation is like in the fluorite-type structure of SrF2. Displacement ellipsoids are drawn at the 50% probability level.
[Figure 4] Fig. 4. Crystal packing with view along [010] showing the isolated [VOF5] octahedra inside of fluorite-related [Sr10V6]∞ rods running along the b axis and delimited by the oxygen atoms of the vanadyl group, F1 atoms and the water molecules. Hydrogen bonds are indicated with dotted lines.
[Figure 5] Fig. 5. Comparison between the [Sr10V6]∞ rods in the title compound (bottom) and the corresponding Sr16 block in the SrF2 fluorite-type structure (top), obtained by doubling its c axis and reversely replacing V by Sr atoms. The heights of the z coordinates are indicated by the fractions×100.
[Figure 6] Fig. 6. The two lattices of the two component crystal are visible. The SHELXL BASF parameter refines to 0.511 for this non-merohedral twin. The two domains are related by a rotation of -180° along the reciprocal [1 0 1]* vector.
pentastrontium tris[pentafluoridooxidovanadate(IV)] fluoride trihydrate top
Crystal data top
Sr5(VOF5)3F(H2O)3F000 = 1828
Mr = 996.97Dx = 3.776 Mg m−3
Monoclinic, P21/nMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 323 reflections
a = 11.217 (2) Åθ = 2.0–30.0º
b = 8.1775 (15) ŵ = 16.79 mm−1
c = 19.887 (4) ÅT = 298 K
β = 105.999 (4)ºCell measurement pressure: ambient kPa
V = 1753.5 (6) Å3Needle, pale blue-green
Z = 40.36 × 0.08 × 0.04 mm
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer		6596 measured reflections
Radiation source: normal-focus sealed tube6596 independent reflections
Monochromator: graphite4299 reflections with I > 2σ(I)
Detector resolution: 8.366 pixels mm-1Rint = 0.0000
T = 298 Kθmax = 30.0º
P = ambient kPaθmin = 1.9º
ω scansh = −15→15
Absorption correction: multi-scan
(TWINABS; Bruker, 2003)		k = 0→11
Tmin = 0.065, Tmax = 0.553l = 0→27
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038H atoms treated by a mixture of
independent and constrained refinement
wR(F2) = 0.083  w = 1/[σ2(Fo2) + (0.0355P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.93(Δ/σ)max = 0.008
6596 reflectionsΔρmax = 1.28 e Å−3
290 parametersΔρmin = −1.11 e Å−3
9 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
Sr5(VOF5)3F(H2O)3V = 1753.5 (6) Å3
Mr = 996.97Z = 4
Monoclinic, P21/nMo Kα
a = 11.217 (2) ŵ = 16.79 mm−1
b = 8.1775 (15) ÅT = 298 K
c = 19.887 (4) Å0.36 × 0.08 × 0.04 mm
β = 105.999 (4)º
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer		6596 independent reflections
Absorption correction: multi-scan
(TWINABS; Bruker, 2003)		4299 reflections with I > 2σ(I)
Tmin = 0.065, Tmax = 0.553Rint = 0.0000
6596 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0389 restraints
wR(F2) = 0.083H atoms treated by a mixture of
independent and constrained refinement
S = 0.93Δρmax = 1.28 e Å−3
6596 reflectionsΔρmin = −1.11 e Å−3
290 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
Sr10.49725 (5)0.91553 (6)0.14704 (3)0.01037 (10)
Sr20.13869 (5)0.91614 (7)0.14686 (3)0.01133 (11)
Sr30.25819 (5)0.58877 (7)0.01760 (3)0.01119 (11)
Sr40.83170 (5)1.15579 (6)0.17512 (3)0.01218 (12)
Sr50.66417 (5)1.16611 (6)0.32847 (3)0.01202 (12)
V10.57273 (8)0.41800 (11)0.17307 (5)0.00985 (18)
V20.08398 (9)0.41537 (12)0.15922 (5)0.01143 (19)
V30.75847 (9)0.92212 (12)0.02341 (5)0.0121 (2)
F10.3050 (3)0.7747 (4)0.11547 (16)0.0152 (7)
F20.6850 (3)0.9235 (4)0.10740 (17)0.0184 (7)
F30.6078 (3)0.6508 (3)0.18699 (18)0.0162 (7)
F40.0792 (3)0.6462 (4)0.18369 (17)0.0151 (7)
F50.9049 (3)0.8968 (4)0.10573 (16)0.0148 (7)
F60.7705 (3)1.1521 (4)0.04540 (16)0.0171 (8)
F70.7368 (3)0.6882 (4)0.03245 (17)0.0199 (8)
F80.6052 (3)0.1825 (3)0.18916 (18)0.0176 (7)
F90.6924 (3)0.4171 (4)0.11824 (18)0.0201 (7)
F100.7406 (3)0.4169 (4)0.25298 (19)0.0279 (8)
F110.5154 (3)0.4220 (4)0.25564 (17)0.0219 (8)
F12−0.0364 (3)0.4062 (4)0.22370 (17)0.0157 (7)
F13−0.0774 (3)0.4719 (4)0.09201 (17)0.0186 (8)
F140.0383 (3)0.1884 (4)0.14929 (17)0.0169 (8)
F150.2141 (3)0.3756 (4)0.23846 (18)0.0249 (9)
F160.5983 (3)0.9396 (4)−0.03641 (17)0.0211 (8)
O10.3311 (4)1.1241 (5)0.1708 (2)0.0156 (9)
H110.314 (5)1.207 (5)0.1416 (19)0.019*
H120.339 (6)1.144 (6)0.2154 (11)0.019*
O20.4763 (4)0.7121 (5)0.0279 (2)0.0202 (9)
H210.482 (5)0.790 (5)−0.003 (2)0.024*
H220.547 (3)0.650 (6)0.038 (3)0.024*
O30.0503 (4)0.7198 (5)0.0304 (2)0.0201 (10)
H31−0.002 (4)0.653 (6)0.044 (3)0.024*
H320.012 (4)0.782 (6)−0.006 (2)0.024*
O40.4460 (4)0.4223 (5)0.1120 (2)0.0182 (9)
O50.1632 (4)0.4248 (5)0.0991 (2)0.0163 (9)
O60.8434 (4)0.9263 (5)−0.03483 (19)0.0145 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0106 (3)0.0085 (2)0.0121 (3)−0.0001 (2)0.00308 (19)−0.0003 (2)
Sr20.0092 (3)0.0090 (2)0.0150 (3)0.0001 (2)0.0020 (2)0.0004 (2)
Sr30.0125 (3)0.0076 (2)0.0129 (3)−0.0005 (2)0.0026 (2)−0.0011 (2)
Sr40.0118 (3)0.0119 (3)0.0125 (3)−0.0007 (2)0.0029 (2)0.0001 (2)
Sr50.0119 (3)0.0112 (3)0.0129 (3)−0.0004 (2)0.0032 (2)−0.0001 (2)
V10.0104 (5)0.0067 (4)0.0117 (5)0.0003 (4)0.0019 (4)0.0005 (4)
V20.0095 (5)0.0078 (4)0.0166 (5)0.0005 (4)0.0030 (4)−0.0012 (4)
V30.0165 (5)0.0084 (4)0.0101 (5)0.0001 (4)0.0017 (4)0.0012 (4)
F10.0122 (17)0.0094 (17)0.0229 (18)−0.0031 (13)0.0030 (14)−0.0049 (14)
F20.0170 (19)0.0228 (18)0.0194 (18)−0.0064 (16)0.0119 (15)−0.0065 (16)
F30.0176 (19)0.0070 (14)0.023 (2)−0.0006 (13)0.0046 (15)−0.0006 (14)
F40.0139 (19)0.0122 (16)0.0189 (19)−0.0032 (14)0.0037 (15)−0.0027 (14)
F50.0097 (17)0.0175 (17)0.0132 (16)−0.0003 (14)−0.0037 (13)0.0020 (14)
F60.031 (2)0.0050 (15)0.0157 (18)0.0005 (15)0.0078 (16)0.0026 (13)
F70.028 (2)0.0085 (16)0.0213 (19)0.0012 (14)0.0038 (16)0.0002 (14)
F80.018 (2)0.0066 (15)0.026 (2)0.0014 (13)0.0024 (15)−0.0005 (14)
F90.0153 (18)0.0225 (18)0.0255 (19)−0.0043 (16)0.0105 (15)−0.0083 (17)
F100.0141 (19)0.037 (2)0.024 (2)0.0041 (18)−0.0099 (15)−0.0102 (18)
F110.026 (2)0.0264 (19)0.0156 (18)−0.0051 (17)0.0094 (15)−0.0014 (16)
F120.0193 (19)0.0149 (16)0.0160 (17)−0.0017 (15)0.0100 (14)0.0001 (15)
F130.0116 (19)0.0253 (19)0.0156 (18)0.0044 (15)−0.0017 (15)−0.0046 (15)
F140.017 (2)0.0093 (16)0.027 (2)−0.0020 (14)0.0101 (16)−0.0010 (14)
F150.025 (2)0.025 (2)0.020 (2)0.0053 (16)−0.0027 (17)−0.0023 (15)
F160.021 (2)0.021 (2)0.0180 (18)−0.0017 (15)0.0009 (15)0.0003 (15)
O10.017 (2)0.016 (2)0.013 (2)−0.0004 (17)0.0042 (18)0.0000 (16)
O20.014 (2)0.022 (2)0.023 (2)−0.0010 (18)0.0036 (19)0.0018 (19)
O30.017 (2)0.019 (3)0.023 (2)0.0015 (18)0.0039 (19)0.0065 (19)
O40.016 (2)0.017 (2)0.018 (2)0.0031 (19)−0.0015 (17)0.0026 (18)
O50.016 (2)0.013 (2)0.022 (2)−0.0003 (18)0.0098 (18)0.0031 (18)
O60.019 (2)0.013 (2)0.014 (2)0.0074 (18)0.0085 (17)0.0023 (17)
Geometric parameters (Å, °) top
V1—O41.596 (4)Sr2—O32.768 (4)
V1—F111.921 (3)Sr2—F11ii2.932 (3)
V1—F91.949 (3)Sr3—F12.411 (3)
V1—F31.948 (3)Sr3—F6i2.438 (3)
V1—F81.970 (3)Sr3—F7vi2.481 (3)
V1—F102.103 (3)Sr3—O52.552 (4)
V2—O51.676 (4)Sr3—F13vii2.583 (3)
V2—F151.858 (4)Sr3—O22.602 (4)
V2—F141.921 (3)Sr3—O32.642 (4)
V2—F41.954 (3)Sr3—O42.763 (4)
V2—F131.986 (3)Sr3—F9vi2.904 (3)
V2—F122.105 (3)Sr4—F62.480 (3)
V3—O61.691 (4)Sr4—F14viii2.522 (3)
V3—F161.867 (4)Sr4—F12viii2.554 (3)
V3—F61.927 (3)Sr4—F22.629 (3)
V3—F71.943 (3)Sr4—F3iv2.637 (3)
V3—F51.985 (3)Sr4—F8iii2.640 (3)
V3—F22.056 (3)Sr4—F10iv2.676 (4)
Sr1—F12.372 (3)Sr4—F11iv2.681 (3)
Sr1—F22.444 (3)Sr4—F9iii2.704 (4)
Sr1—F16i2.468 (3)Sr4—F52.773 (3)
Sr1—F12ii2.487 (3)Sr4—F10iii2.978 (4)
Sr1—F32.513 (3)Sr5—F5iv2.536 (3)
Sr1—F8iii2.525 (3)Sr5—F13ii2.611 (3)
Sr1—O12.663 (4)Sr5—F12ii2.613 (3)
Sr1—O22.851 (4)Sr5—F9iv2.630 (3)
Sr1—F10iv3.062 (3)Sr5—F3iv2.662 (3)
Sr2—F12.418 (3)Sr5—F8iii2.668 (4)
Sr2—F15ii2.441 (3)Sr5—F4ii2.678 (3)
Sr2—F42.475 (3)Sr5—F7iv2.688 (3)
Sr2—F14iii2.501 (3)Sr5—F2iv2.780 (4)
Sr2—F5v2.527 (3)Sr5—F10iii2.811 (4)
Sr2—O6i2.629 (4)Sr5—F11iii2.816 (4)
Sr2—O12.685 (4)Sr5—F10iv2.978 (4)
O4—V1—F11102.29 (18)F4—V2—F1381.95 (14)
O4—V1—F9100.39 (18)O5—V2—F12172.52 (17)
F11—V1—F9157.28 (15)F15—V2—F1287.89 (15)
O4—V1—F3100.91 (18)F14—V2—F1280.22 (13)
F11—V1—F387.93 (15)F4—V2—F1279.42 (13)
F9—V1—F386.56 (15)F13—V2—F1278.43 (13)
O4—V1—F8103.38 (18)O6—V3—F16100.78 (18)
F11—V1—F888.19 (15)O6—V3—F696.80 (17)
F9—V1—F887.82 (15)F16—V3—F693.72 (15)
F3—V1—F8155.68 (13)O6—V3—F7101.05 (17)
O4—V1—F10178.88 (19)F16—V3—F790.65 (15)
F11—V1—F1078.18 (15)F6—V3—F7160.49 (14)
F9—V1—F1079.12 (15)O6—V3—F594.15 (16)
F3—V1—F1078.06 (14)F16—V3—F5165.02 (15)
F8—V1—F1077.64 (14)F6—V3—F585.67 (14)
O5—V2—F1599.56 (18)F7—V3—F585.24 (14)
O5—V2—F1498.63 (17)O6—V3—F2169.75 (17)
F15—V2—F1492.46 (15)F16—V3—F289.22 (15)
O5—V2—F4100.93 (17)F6—V3—F280.15 (14)
F15—V2—F491.55 (15)F7—V3—F280.90 (14)
F14—V2—F4159.08 (14)F5—V3—F275.92 (14)
O5—V2—F1394.19 (17)H11—O1—H12118 (3)
F15—V2—F13165.70 (15)H21—O2—H22109 (3)
F14—V2—F1389.31 (15)H31—O3—H32113 (3)
Symmetry codes: (i) −x+1, −y+2, −z; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x, y+1, z; (iv) −x+3/2, y+1/2, −z+1/2; (v) x−1, y, z; (vi) −x+1, −y+1, −z; (vii) −x, −y+1, −z; (viii) x+1, y+1, z.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4iii0.88 (4)2.48 (5)3.131 (6)132 (5)
O1—H11···O5iii0.88 (4)2.44 (4)3.185 (6)143 (5)
O1—H12···F4ii0.882 (18)1.96 (3)2.796 (5)157 (5)
O2—H21···F160.90 (4)2.03 (4)2.817 (5)146 (5)
O2—H22···F70.92 (4)2.18 (4)2.905 (5)135 (4)
O3—H31···F130.90 (5)2.07 (5)2.937 (5)164 (5)
O3—H32···O6v0.89 (4)2.17 (4)2.873 (5)135 (5)
Symmetry codes: (iii) x, y+1, z; (ii) −x+1/2, y+1/2, −z+1/2; (v) x−1, y, z.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1—H11···O4i0.88 (4)2.48 (5)3.131 (6)132 (5)
O1—H11···O5i0.88 (4)2.44 (4)3.185 (6)143 (5)
O1—H12···F4ii0.882 (18)1.96 (3)2.796 (5)157 (5)
O2—H21···F160.90 (4)2.03 (4)2.817 (5)146 (5)
O2—H22···F70.92 (4)2.18 (4)2.905 (5)135 (4)
O3—H31···F130.90 (5)2.07 (5)2.937 (5)164 (5)
O3—H32···O6iii0.89 (4)2.17 (4)2.873 (5)135 (5)
Symmetry codes: (i) x, y+1, z; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x−1, y, z.
Table 2
Valence-bond analysis of Sr5(VIVOF5)3F(H2O)3 top
V1V2V3Sr1Sr2Sr3Sr4Sr5ΣΣexpected
F10.380.340.351.071
F20.380.320.190.131.021
F30.510.260.190.181.141
F40.500.290.170.961
F50.460.250.130.251.091
F60.540.320.291.151
F70.520.290.160.971
F80.480.250.190.171.091
F90.510.090.160.190.951
F100.340.060.17;0.070.12;0.070.831
F110.550.080.170.120.921
F120.340.280.230.201.051
F130.460.220.200.881
F140.550.270.261.081
F150.650.320.971
F160.640.300.941
O10.220.212.03*2
O20.140.272.01*2
O30.170.242.01*2
O41.660.171.832
O51.340.311.652
O61.290.251.542
Σ4.053.843.832.212.182.262.051.94
Σexpected44422222
Note: (*) adding a bond valence of 1.6 units, corresponding to the two H atoms linked to O1, O2 and O3, forming water molecules. The valence deficit observed on O4, O5 and O6, as well as on F4, F7, F13 and F16, is expected to be compensated by hydrogen bonding, since they behave as acceptors.
references
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