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

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ISSN: 2056-9890

The synthetic cobalt vanadium selenite, Co2V2Se2O11

aDepartment of Materials and Environmental Chemistry, Stockholm University, SE-106 91 Stockholm, Sweden
*Correspondence e-mail: mats.johnsson@mmk.su.se

(Received 4 June 2012; accepted 15 June 2012; online 30 June 2012)

The crystal structure of dicobalt(II) divanadium(V) disel­enium(IV) undeca­oxide, Co2V2Se2O11, exhibits a three-dimensional framework, the building units being distorted CoO6 octa­hedra and VO5 square pyramids arranged so as to form alternate chains along [010]. The framework has channels along [100] and [010] in which the two Ψ-SeO3E (site symmetries m; E being the 4s2 lone electron pair of SeIV) tetra­hedra reside and connect to the other building blocks. The structure contains corner- and edge-sharing CoO6 octa­hedra, corner- and edge-sharing VO5 square pyramids and edge-sharing Ψ-SeO3E tetra­hedra. Co2V2Se2O11 is the first oxide containing all the cations CoII, VV and SeIV.

Related literature

For general background, including bond-valence-sum calculations, see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]). For related structures, see: Allen et al. (2004[Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.]); Becker et al. (2007a[Becker, R., Berger, H. & Johnsson, M. (2007a). Acta Cryst. C63, i4-i6.],b[Becker, R., Prester, M., Berger, H., Hui Lin, P., Johnsson, M., Drobac, D. & Zivkovic, I. (2007b). J. Solid State Chem. 180, 1051-1059.]); Jiang et al. (2008[Jiang, H., Kong, F., Fan, Y. & Mao, J. G. (2008). Inorg. Chem. 47, 7430-7437.]); Millet et al. (1999[Millet, P., Enjalbert, R. & Galy, J. (1999). J. Solid State Chem. 147, 296-303.]); Pitzschenke & Jansen (2007[Pitzschenke, D. & Jansen, M. (2007). Z. Anorg. Allg. Chem. 633, 1563-1567.]); Sauerbrei et al. (1974[Sauerbrei, E. E., Faggiani, R. & Calvo, C. (1974). Acta Cryst. B30, 2907-2909.]).

Experimental

Crystal data
  • Co2V2Se2O11

  • Mr = 553.66

  • Monoclinic, P 21 /m

  • a = 4.7913 (2) Å

  • b = 8.8680 (4) Å

  • c = 10.6156 (5) Å

  • β = 101.115 (5)°

  • V = 442.59 (3) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 14.01 mm−1

  • T = 292 K

  • 0.05 × 0.03 × 0.02 mm

Data collection
  • Oxford Diffraction Xcalibur Sapphire3 diffractometer

  • Absorption correction: analytical [CrysAlis RED (Oxford Diffraction, 2007[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]), based on expressions derived by Clark & Reid (1995[Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.])] Tmin = 0.659, Tmax = 0.756

  • 4219 measured reflections

  • 1534 independent reflections

  • 1023 reflections with I > 2σ(I)

  • Rint = 0.051

Refinement
  • R[F2 > 2σ(F2)] = 0.032

  • wR(F2) = 0.048

  • S = 0.76

  • 1534 reflections

  • 85 parameters

  • Δρmax = 1.28 e Å−3

  • Δρmin = −0.98 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2007[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2007[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]); data reduction: CrysAlis RED; 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: DIAMOND (Brandenburg, 2001[Brandenburg, K. (2001). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: enCIFer (Allen et al., 2004[Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.]).

Supporting information


Comment top

The synthesis and crystal structure determination of the new compound Co2V2Se2O11 is a result of an ongoing investigation of the structural chemistry of selenium and tellurium oxides and oxohalides. Transition metal oxides and oxohalides containing p-block cations, such as SeIV and TeIV, with stereochemically active lone pairs frequently show a low-dimensional arrangement of the metal ions. The SeIV lone pairs act as 'chemical scissors' and help to reduce the dimensionality of the atomic arrangements in the crystal structure (Becker et al., 2007a,b). The aim of the present study was to test the synthesis concept in a system containing two transition metals taking different coordination polyhedra: CoO-V2O5—SeO2. The present compound is, to the best of our knowledge, the first oxide to contain all the cations CoII, VV and SeIV. A few selenites containing vanadium plus another transition metal have previously been described; Cd6V2Se5O21 (Jiang et al., 2008), α-CuVSe2O7 and β-CuVSe2O7 (Millet et al., 1999), AgVSeO5 and ZnVSe2O7 (Pitzschenke & Jansen, 2007). The stereochemically active lone electron pairs open up the crystal structures by creating non-bonding volumes and occupy space similar to that taken by an oxygen anion in the crystal structure. α-CuVSe2O7 is a layered compound with only weak van der Waals interactions in between the layers while the others are three-dimensional framework structures where the lone pairs on SeIV are located in voids in the crystal structure.

Co2V2Se2O11 crystallizes in the centrosymmetric monoclinic space group P21/m. The CoII ions are in a slightly distorted octahedral environment. The CoO6 octahedra are connected via O2iii···O2v and O1···O3iii edge sharing [symmetry code: (iii) x + 1,y,z; (v) -x + 1,y + 1/2,-z + 1] to form zigzag chains having the formula [CoO4]n along [100]. The Co···O bonds are in the range 2.074 (3) Å to 2.123 (3) Å which is comparable to what is found in e.g. Co2V2O7 (Sauerbrei et al., 1974). There are two Co—Co distances within a chain; 3.160 (1) Å and 3.179 (2) Å. The VV atoms are surrounded by five O atoms forming a very distorted square pyramid comprising two V1=O vanadyl double bonds of 1.627 (3) Å and 1.635 (3) Å and two long V1–O bonds 2.038 (3) Å and 2.087 (3) Å (Fig. 1). As a consequence, the V atom is located above the square plane. Bond valence sum analysis (Brown & Altermatt, 1985) confirms the coordination, with the calculated valence (VV, the bond valence parameter Ro = 1.803) equal to 5.15. The VO5 square pyramids are connected via O5···O5ii edge sharing and O7 corner sharing [symmetry code: (ii) -x + 1,-y + 1,z - 2] to form chains having the formula [V2O7]n along [010]. The V···V distances in a chain are 3.328 (1) Å and 3.443 (2) Å. The chains of CoO6 and VO5 bridge by corner sharing at O4 and O6. The SeIV ions have both one sided SeO3 coordination owing to the presence of the 4s2 stereochemically active lone pair, E, and they do not polymerize. The crystal structure can be described as being a three-dimensional framework structure made up of [CoO4]n– and [V2O7]n chains (Fig. 2 and 3). The SeO3 groups connect to the metal-oxide framework by corner sharing (Fig. 3). The stereochemically active SeIV lone pairs are located in voids in the structure. Those voids are present as tunnels along (100) and (010) respectively.

Bond valence sum analysis (Brown & Altermatt, 1985) confirms the coordination for all the ions and give 2.04 for Co1, 5.15 for V1, 4.01 for Se1, 3.84 for Se2, 2.07 for O1, 2.02 for O2, 2.11 for O3, 1.92 for O4 and 2.36 for O5.

Related literature top

For general background, including bond-valence-sum calculations, see: Brown & Altermatt (1985). For related structures, see: Allen et al. (2004); Becker et al. (2007a,b); Jiang et al. (2008); Millet et al. (1999); Pitzschenke & Jansen (2007); Sauerbrei et al. (1974).

Experimental top

Single crystals of Co2V2Se2O11 are non-hygroscopic and were synthesized via chemical vapour transport reactions in sealed evacuated silica tubes. The starting materials were 0.150 g (2 mmol) CoO (ABCR GmbH 97.999%), 0.182 g (1 mmol) V2O5 (ABCR GmbH 99.9%), and 0.222 g (2 mmol) SeO2, (Alfa Aesar 99.4%) mixed in a stoichiometric 2:1:2 molar ratio and placed in a 5 cm long silica tube which was first dried for 1 h at 100°C and subsequently evacuated and sealed. The silica tube was treated in a muffle furnace at 500°C for 100 h followed by slow cooling at a rate of 10°C/h to room temperature. The synthesis products were a mixture of red single crystals of Co2V2Se2O11 and a brown-red powder of undetermined composition.

Refinement top

The structure was solved using SHELXS97 (Sheldrick, 2008), and refined by full-matrix least-squares using SHELXL97 (Sheldrick, 2008).

Structure description top

The synthesis and crystal structure determination of the new compound Co2V2Se2O11 is a result of an ongoing investigation of the structural chemistry of selenium and tellurium oxides and oxohalides. Transition metal oxides and oxohalides containing p-block cations, such as SeIV and TeIV, with stereochemically active lone pairs frequently show a low-dimensional arrangement of the metal ions. The SeIV lone pairs act as 'chemical scissors' and help to reduce the dimensionality of the atomic arrangements in the crystal structure (Becker et al., 2007a,b). The aim of the present study was to test the synthesis concept in a system containing two transition metals taking different coordination polyhedra: CoO-V2O5—SeO2. The present compound is, to the best of our knowledge, the first oxide to contain all the cations CoII, VV and SeIV. A few selenites containing vanadium plus another transition metal have previously been described; Cd6V2Se5O21 (Jiang et al., 2008), α-CuVSe2O7 and β-CuVSe2O7 (Millet et al., 1999), AgVSeO5 and ZnVSe2O7 (Pitzschenke & Jansen, 2007). The stereochemically active lone electron pairs open up the crystal structures by creating non-bonding volumes and occupy space similar to that taken by an oxygen anion in the crystal structure. α-CuVSe2O7 is a layered compound with only weak van der Waals interactions in between the layers while the others are three-dimensional framework structures where the lone pairs on SeIV are located in voids in the crystal structure.

Co2V2Se2O11 crystallizes in the centrosymmetric monoclinic space group P21/m. The CoII ions are in a slightly distorted octahedral environment. The CoO6 octahedra are connected via O2iii···O2v and O1···O3iii edge sharing [symmetry code: (iii) x + 1,y,z; (v) -x + 1,y + 1/2,-z + 1] to form zigzag chains having the formula [CoO4]n along [100]. The Co···O bonds are in the range 2.074 (3) Å to 2.123 (3) Å which is comparable to what is found in e.g. Co2V2O7 (Sauerbrei et al., 1974). There are two Co—Co distances within a chain; 3.160 (1) Å and 3.179 (2) Å. The VV atoms are surrounded by five O atoms forming a very distorted square pyramid comprising two V1=O vanadyl double bonds of 1.627 (3) Å and 1.635 (3) Å and two long V1–O bonds 2.038 (3) Å and 2.087 (3) Å (Fig. 1). As a consequence, the V atom is located above the square plane. Bond valence sum analysis (Brown & Altermatt, 1985) confirms the coordination, with the calculated valence (VV, the bond valence parameter Ro = 1.803) equal to 5.15. The VO5 square pyramids are connected via O5···O5ii edge sharing and O7 corner sharing [symmetry code: (ii) -x + 1,-y + 1,z - 2] to form chains having the formula [V2O7]n along [010]. The V···V distances in a chain are 3.328 (1) Å and 3.443 (2) Å. The chains of CoO6 and VO5 bridge by corner sharing at O4 and O6. The SeIV ions have both one sided SeO3 coordination owing to the presence of the 4s2 stereochemically active lone pair, E, and they do not polymerize. The crystal structure can be described as being a three-dimensional framework structure made up of [CoO4]n– and [V2O7]n chains (Fig. 2 and 3). The SeO3 groups connect to the metal-oxide framework by corner sharing (Fig. 3). The stereochemically active SeIV lone pairs are located in voids in the structure. Those voids are present as tunnels along (100) and (010) respectively.

Bond valence sum analysis (Brown & Altermatt, 1985) confirms the coordination for all the ions and give 2.04 for Co1, 5.15 for V1, 4.01 for Se1, 3.84 for Se2, 2.07 for O1, 2.02 for O2, 2.11 for O3, 1.92 for O4 and 2.36 for O5.

For general background, including bond-valence-sum calculations, see: Brown & Altermatt (1985). For related structures, see: Allen et al. (2004); Becker et al. (2007a,b); Jiang et al. (2008); Millet et al. (1999); Pitzschenke & Jansen (2007); Sauerbrei et al. (1974).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2007); cell refinement: CrysAlis RED (Oxford Diffraction, 2007); data reduction: CrysAlis RED (Oxford Diffraction, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: enCIFer (Allen et al. 2004).

Figures top
[Figure 1] Fig. 1. A displacement ellipsoid diagram showing the coordination around the cations. Atomic displacement parameters are given at the 50% probability level [Symmetry codes: (i) x,-y + 1/2,z; (ii) -x + 1,-y - 1,z - 2; (iii) x + 1,y,z; (iv) x + 1,-y + 1/2,z; (v) -x + 1,y + 1/2,-z + 1].
[Figure 2] Fig. 2. A view of the structure of Co2V2Se2O11 along (100).
[Figure 3] Fig. 3. A view of the structure of Co2V2Se2O11 along (010).
dicobalt(II) divanadium(V) diselenium(IV) undecaoxide top
Crystal data top
Co2V2Se2O11F(000) = 512
Mr = 553.66Dx = 4.155 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 1387 reflections
a = 4.7913 (2) Åθ = 3.9–32.2°
b = 8.8680 (4) ŵ = 14.01 mm1
c = 10.6156 (5) ÅT = 292 K
β = 101.115 (5)°Block, red
V = 442.59 (3) Å30.05 × 0.03 × 0.02 mm
Z = 2
Data collection top
Oxford Diffraction Xcalibur Sapphire3
diffractometer
1534 independent reflections
Radiation source: fine-focus sealed tube1023 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
Detector resolution: 16.5 pixels mm-1θmax = 32.3°, θmin = 3.9°
ω scansh = 77
Absorption correction: analytical
[CrysAlis RED (Oxford Diffraction, 2007), based on expressions derived by Clark & Reid (1995)]
k = 1112
Tmin = 0.659, Tmax = 0.756l = 1513
4219 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.032Secondary atom site location: difference Fourier map
wR(F2) = 0.048 w = 1/[σ2(Fo2) + (0.0114P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.76(Δ/σ)max = 0.001
1534 reflectionsΔρmax = 1.28 e Å3
85 parametersΔρmin = 0.98 e Å3
Crystal data top
Co2V2Se2O11V = 442.59 (3) Å3
Mr = 553.66Z = 2
Monoclinic, P21/mMo Kα radiation
a = 4.7913 (2) ŵ = 14.01 mm1
b = 8.8680 (4) ÅT = 292 K
c = 10.6156 (5) Å0.05 × 0.03 × 0.02 mm
β = 101.115 (5)°
Data collection top
Oxford Diffraction Xcalibur Sapphire3
diffractometer
1534 independent reflections
Absorption correction: analytical
[CrysAlis RED (Oxford Diffraction, 2007), based on expressions derived by Clark & Reid (1995)]
1023 reflections with I > 2σ(I)
Tmin = 0.659, Tmax = 0.756Rint = 0.051
4219 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03285 parameters
wR(F2) = 0.0480 restraints
S = 0.76Δρmax = 1.28 e Å3
1534 reflectionsΔρmin = 0.98 e Å3
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
Se10.38839 (12)0.25000.45047 (6)0.00668 (13)
Se20.14374 (12)0.25000.89926 (5)0.00653 (13)
Co10.95757 (12)0.42816 (6)0.63219 (5)0.00751 (13)
V10.53298 (15)0.56239 (8)0.85002 (6)0.00660 (15)
O10.6860 (8)0.25000.5658 (4)0.0105 (9)
O60.7568 (6)0.4597 (3)0.7887 (3)0.0118 (6)
O50.3738 (6)0.4001 (3)0.9523 (3)0.0107 (6)
O20.2107 (6)0.0989 (3)0.4958 (3)0.0093 (6)
O30.1701 (8)0.25000.7454 (4)0.0088 (9)
O40.2448 (6)0.5786 (3)0.7407 (3)0.0132 (7)
O70.6843 (8)0.75000.8501 (4)0.0077 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Se10.0068 (3)0.0069 (3)0.0064 (3)0.0000.0014 (2)0.000
Se20.0080 (3)0.0051 (3)0.0063 (3)0.0000.0008 (2)0.000
Co10.0080 (3)0.0063 (3)0.0082 (3)0.0001 (2)0.0016 (2)0.0001 (2)
V10.0078 (3)0.0063 (3)0.0058 (3)0.0003 (3)0.0017 (3)0.0000 (3)
O10.008 (2)0.005 (2)0.017 (2)0.0000.0012 (18)0.000
O60.0140 (16)0.0077 (15)0.0148 (16)0.0010 (12)0.0059 (13)0.0014 (12)
O50.0153 (16)0.0113 (15)0.0045 (14)0.0088 (12)0.0003 (12)0.0024 (11)
O20.0106 (15)0.0103 (16)0.0071 (15)0.0021 (12)0.0021 (12)0.0024 (11)
O30.012 (2)0.006 (2)0.007 (2)0.0000.0022 (17)0.000
O40.0139 (16)0.0101 (16)0.0132 (16)0.0020 (12)0.0031 (13)0.0025 (12)
O70.009 (2)0.005 (2)0.010 (2)0.0000.0024 (17)0.000
Geometric parameters (Å, º) top
Se1—O11.691 (4)Co1—O62.093 (3)
Se1—O21.706 (3)Co1—O4iv2.095 (3)
Se1—O2i1.706 (3)Co1—O3iv2.122 (3)
Se2—O31.663 (4)V1—O41.630 (3)
Se2—O51.750 (3)V1—O61.635 (3)
Se2—O5i1.750 (3)V1—O71.8147 (17)
Co1—O2ii2.074 (3)V1—O52.038 (3)
Co1—O12.081 (3)V1—O5v2.086 (3)
Co1—O2iii2.090 (3)
O1—Se1—O2101.12 (13)O2ii—Co1—O3iv91.59 (13)
O1—Se1—O2i101.12 (13)O1—Co1—O3iv80.04 (12)
O2—Se1—O2i103.52 (19)O2iii—Co1—O3iv172.01 (14)
O3—Se2—O598.85 (13)O6—Co1—O3iv83.90 (13)
O3—Se2—O5i98.85 (13)O4iv—Co1—O3iv88.29 (11)
O5—Se2—O5i98.97 (19)O4—V1—O6107.24 (15)
O2ii—Co1—O195.00 (14)O4—V1—O7101.71 (16)
O2ii—Co1—O2iii80.44 (12)O6—V1—O7102.62 (15)
O1—Co1—O2iii101.07 (12)O4—V1—O595.11 (13)
O2ii—Co1—O6171.78 (11)O6—V1—O599.22 (13)
O1—Co1—O690.99 (14)O7—V1—O5146.92 (14)
O2iii—Co1—O6103.94 (11)O4—V1—O5v133.61 (14)
O2ii—Co1—O4iv92.69 (12)O6—V1—O5v117.38 (13)
O1—Co1—O4iv166.17 (13)O7—V1—O5v81.09 (14)
O2iii—Co1—O4iv91.51 (11)O5—V1—O5v66.81 (12)
O6—Co1—O4iv80.34 (11)
Symmetry codes: (i) x, y+1/2, z; (ii) x+1, y+1/2, z; (iii) x+1, y+1/2, z+1; (iv) x+1, y, z; (v) x+1, y+1, z+2.

Experimental details

Crystal data
Chemical formulaCo2V2Se2O11
Mr553.66
Crystal system, space groupMonoclinic, P21/m
Temperature (K)292
a, b, c (Å)4.7913 (2), 8.8680 (4), 10.6156 (5)
β (°) 101.115 (5)
V3)442.59 (3)
Z2
Radiation typeMo Kα
µ (mm1)14.01
Crystal size (mm)0.05 × 0.03 × 0.02
Data collection
DiffractometerOxford Diffraction Xcalibur Sapphire3
Absorption correctionAnalytical
[CrysAlis RED (Oxford Diffraction, 2007), based on expressions derived by Clark & Reid (1995)]
Tmin, Tmax0.659, 0.756
No. of measured, independent and
observed [I > 2σ(I)] reflections
4219, 1534, 1023
Rint0.051
(sin θ/λ)max1)0.751
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.048, 0.76
No. of reflections1534
No. of parameters85
Δρmax, Δρmin (e Å3)1.28, 0.98

Computer programs: CrysAlis CCD (Oxford Diffraction, 2007), CrysAlis RED (Oxford Diffraction, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2001), enCIFer (Allen et al. 2004).

 

Footnotes

Permanent address: Department of Chemistry, University of Engineering and Technology, Lahore 54890, Pakistan.

Acknowledgements

This work was carried out with financial support from the Swedish Research Council. FR would like to thank the Higher Education Commission (HEC), Pakistan for a research scholarship during the time this work was performed.

References

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