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The title compound, NaV3(SO4)2(OH)6, was synthesized and found to crystallize in the trigonal space group R\overline 3m with the Na atom at a site with 3m symmetry, the V atom at a site with 2/m symmetry, and the S and a terminal O atom at sites with 3m symmetry; the remaining two O atoms and the H atom are at sites with m symmetry. Octahedrally coordinated vanadium and tetrahedral sulfate ions share corners to form layers that are held together by hydrogen bonds and by sodium ions, which are located between the layers.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100011239/iz1003sup1.cif
Contains datablocks NaVOHSO4_comments, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100011239/iz1003Isup2.hkl
Contains datablock I

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and ATOMS (Dowty, 1999); software used to prepare material for publication: SHELXL97.

Sodium trivanadium disulfate hexahydroxide top
Crystal data top
NaV3(SO4)2(OH)6Dx = 3.018 Mg m3
Mr = 470Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3mCell parameters from 1353 reflections
Hall symbol: -R 3 2"θ = 6.9–56.9°
a = 7.2821 (6) ŵ = 3.19 mm1
c = 16.889 (2) ÅT = 293 K
V = 775.6 (2) Å3Octahedron, brown
Z = 30.13 × 0.12 × 0.06 mm
F(000) = 690
Data collection top
CCD Smart Apex
diffractometer
272 independent reflections
Radiation source: fine-focus sealed tube265 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
ω scansθmax = 28.5°, θmin = 3.5°
Absorption correction: ψ scan
(SADABS; Sheldrick, 1996)
h = 99
Tmin = 0.583, Tmax = 0.790k = 98
1643 measured reflectionsl = 2211
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026Hydrogen site location: difference Fourier map
wR(F2) = 0.072All H-atom parameters refined
S = 1.31 w = 1/[σ2(Fo2) + (0.0325P)2 + 3.007P]
where P = (Fo2 + 2Fc2)/3
272 reflections(Δ/σ)max < 0.001
27 parametersΔρmax = 0.67 e Å3
0 restraintsΔρmin = 0.50 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
Na10.00000.00000.00000.0715 (19)
V10.83330.16670.16670.0081 (3)
S10.66670.33330.02351 (7)0.0076 (3)
O11.12675 (18)0.2535 (4)0.13318 (13)0.0117 (5)
O20.77717 (17)0.22283 (17)0.05270 (12)0.0131 (5)
O30.66670.33330.0627 (2)0.0121 (8)
H11.167 (3)0.334 (6)0.114 (3)0.015*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.094 (3)0.094 (3)0.027 (2)0.0469 (16)0.0000.000
V10.0076 (3)0.0076 (3)0.0102 (4)0.0046 (3)0.00007 (12)0.00007 (12)
S10.0084 (4)0.0084 (4)0.0061 (5)0.00418 (19)0.0000.000
O10.0086 (7)0.0101 (11)0.0168 (10)0.0050 (6)0.0030 (4)0.0060 (9)
O20.0170 (8)0.0170 (8)0.0109 (9)0.0127 (9)0.0006 (4)0.0006 (4)
O30.0153 (11)0.0153 (11)0.0057 (15)0.0077 (6)0.0000.000
Geometric parameters (Å, º) top
Na1—O1i2.760 (2)V1—O1viii1.9835 (9)
Na1—O1ii2.760 (2)V1—O1ix1.9835 (9)
Na1—O1iii2.760 (2)V1—O22.051 (2)
Na1—O1iv2.760 (2)V1—O2ix2.051 (2)
Na1—O1v2.760 (2)V1—Na1x3.5132 (3)
Na1—O1vi2.760 (2)V1—Na1xi3.5133 (3)
Na1—O2iii2.948 (2)S1—O31.457 (4)
Na1—O2iv2.948 (2)S1—O21.478 (2)
Na1—O2vi2.948 (2)S1—O2xii1.478 (2)
Na1—O2v2.948 (2)S1—O2iii1.478 (2)
Na1—O2i2.948 (2)O1—V1xiii1.9835 (9)
Na1—O2ii2.948 (2)O1—Na1x2.760 (2)
V1—O1vii1.9835 (9)O2—Na1x2.948 (2)
V1—O11.9835 (9)
O1i—Na1—O1ii180.00 (5)O2vi—Na1—O2i68.70 (4)
O1i—Na1—O1iii60.23 (8)O2v—Na1—O2i111.30 (4)
O1ii—Na1—O1iii119.77 (8)O1i—Na1—O2ii121.48 (3)
O1i—Na1—O1iv119.77 (8)O1ii—Na1—O2ii58.52 (3)
O1ii—Na1—O1iv60.23 (8)O1iii—Na1—O2ii72.17 (6)
O1iii—Na1—O1iv180.00 (7)O1iv—Na1—O2ii107.83 (6)
O1i—Na1—O1v60.23 (8)O1v—Na1—O2ii121.48 (3)
O1ii—Na1—O1v119.77 (8)O1vi—Na1—O2ii58.52 (3)
O1iii—Na1—O1v60.23 (8)O2iii—Na1—O2ii68.70 (4)
O1iv—Na1—O1v119.77 (8)O2iv—Na1—O2ii111.30 (4)
O1i—Na1—O1vi119.77 (8)O2vi—Na1—O2ii111.30 (4)
O1ii—Na1—O1vi60.23 (8)O2v—Na1—O2ii68.70 (4)
O1iii—Na1—O1vi119.77 (8)O2i—Na1—O2ii180.00 (3)
O1iv—Na1—O1vi60.23 (8)O1vii—V1—O188.55 (13)
O1v—Na1—O1vi180.00 (5)O1vii—V1—O1viii180.0
O1i—Na1—O2iii58.52 (3)O1—V1—O1viii91.45 (13)
O1ii—Na1—O2iii121.48 (3)O1vii—V1—O1ix91.45 (13)
O1iii—Na1—O2iii58.52 (3)O1—V1—O1ix180.0
O1iv—Na1—O2iii121.48 (3)O1viii—V1—O1ix88.55 (13)
O1v—Na1—O2iii107.83 (6)O1vii—V1—O287.67 (7)
O1vi—Na1—O2iii72.17 (6)O1—V1—O287.67 (7)
O1i—Na1—O2iv121.48 (3)O1viii—V1—O292.33 (7)
O1ii—Na1—O2iv58.52 (3)O1ix—V1—O292.33 (7)
O1iii—Na1—O2iv121.48 (3)O1vii—V1—O2ix92.33 (7)
O1iv—Na1—O2iv58.52 (3)O1—V1—O2ix92.33 (7)
O1v—Na1—O2iv72.17 (6)O1viii—V1—O2ix87.66 (7)
O1vi—Na1—O2iv107.83 (6)O1ix—V1—O2ix87.66 (7)
O2iii—Na1—O2iv180.00 (9)O2—V1—O2ix180.0
O1i—Na1—O2vi72.17 (6)O1vii—V1—Na1x51.58 (7)
O1ii—Na1—O2vi107.83 (6)O1—V1—Na1x51.58 (7)
O1iii—Na1—O2vi121.48 (3)O1viii—V1—Na1x128.42 (7)
O1iv—Na1—O2vi58.52 (3)O1ix—V1—Na1x128.42 (7)
O1v—Na1—O2vi121.48 (3)O2—V1—Na1x56.96 (6)
O1vi—Na1—O2vi58.52 (3)O2ix—V1—Na1x123.04 (6)
O2iii—Na1—O2vi68.70 (4)O1vii—V1—Na1xi128.42 (7)
O2iv—Na1—O2vi111.30 (4)O1—V1—Na1xi128.42 (7)
O1i—Na1—O2v107.83 (6)O1viii—V1—Na1xi51.58 (7)
O1ii—Na1—O2v72.17 (6)O1ix—V1—Na1xi51.58 (7)
O1iii—Na1—O2v58.52 (3)O2—V1—Na1xi123.04 (6)
O1iv—Na1—O2v121.48 (3)O2ix—V1—Na1xi56.96 (6)
O1v—Na1—O2v58.52 (3)Na1x—V1—Na1xi180.0
O1vi—Na1—O2v121.48 (3)O3—S1—O2109.48 (9)
O2iii—Na1—O2v111.30 (4)O3—S1—O2xii109.48 (9)
O2iv—Na1—O2v68.70 (4)O2—S1—O2xii109.46 (9)
O2vi—Na1—O2v180.0O3—S1—O2iii109.48 (9)
O1i—Na1—O2i58.52 (3)O2—S1—O2iii109.46 (9)
O1ii—Na1—O2i121.48 (3)O2xii—S1—O2iii109.46 (9)
O1iii—Na1—O2i107.83 (6)V1xiii—O1—V1133.23 (12)
O1iv—Na1—O2i72.17 (6)V1xiii—O1—Na1x94.15 (7)
O1v—Na1—O2i58.52 (3)V1—O1—Na1x94.15 (7)
O1vi—Na1—O2i121.48 (3)S1—O2—V1129.68 (13)
O2iii—Na1—O2i111.30 (4)S1—O2—Na1x142.95 (11)
O2iv—Na1—O2i68.70 (4)V1—O2—Na1x87.37 (7)
Symmetry codes: (i) x1, y, z; (ii) x+1, y, z; (iii) x+y+1, x+1, z; (iv) xy1, x1, z; (v) y, xy1, z; (vi) y, x+y+1, z; (vii) y+1, xy1, z; (viii) y+2/3, x+y+4/3, z+1/3; (ix) x+5/3, y+1/3, z+1/3; (x) x+1, y, z; (xi) x+2/3, y+1/3, z+1/3; (xii) y+1, xy, z; (xiii) x+y+2, x+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O3xiv0.62 (4)2.25 (4)2.865 (3)171 (6)
Symmetry code: (xiv) y+1, x, z.
 

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