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The single-crystal structure of a β′-copper vanadium bronze, Cu0.63V2O5, has been studied at room temperature and 9.6 K, and compared with that of the β-sodium vanadium bronze, Na0.33V2O5, structure. No convincing evidence to oppose an assignment of centrosymmetric C2/m symmetry to the structure was identified using the X-ray data. A subsequent convergent beam electron diffraction (CBED) experiment was performed and confirmed the C2/m space group. The oxygen–vanadium atom framework of Cu0.63V2O5 is close to that of Na0.33V2O5. However, in the copper compound the Cu atoms are located in two positions: Cu1 in the 4(i) position with x = 0.541, y = 0 and z = 0.345, and Cu2 in the 8(j) position with x = 0.529, y = 0.038 and z = 0.357. The crystal structure changes little with temperature. Disorder of the Cu ion over two sites is seen at 9.6 K. This suggests that distribution of the Cu atoms over two sites is of a more static than dynamic nature.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768104027739/av5018sup1.cif
Contains datablocks global, ozcult

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768104027739/av5018sup2.hkl
Supplementary material

Computing details top

Data reduction: Xtal DIFDAT ADDREF ABSORB SORTRF; program(s) used to solve structure: Xtal; program(s) used to refine structure: Xtal CRYLSQ; molecular graphics: Xtal; software used to prepare material for publication: Xtal CIFIO.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
(ozcult) top
Crystal data top
Cu0.63O5V2F(000) = 624.8
Mr = 221.59Dx = 4.147 Mg m3
Monoclinic, C2/mMo Kα radiation, λ = 0.7093 Å
Hall symbol: -c 2yCell parameters from 16 reflections
a = 15.100 (1) Åθ = 2.1–50.1°
b = 3.6382 (2) ŵ = 8.79 mm1
c = 10.0595 (7) ÅT = 10 K
β = 105.585 (6)°Rectangular, black
V = 532.32 (6) Å30.27 × 0.18 × 0.17 mm
Z = 6
Data collection top
HUBER 512
diffractometer
3041 reflections with F > .00 sig(F )
ω/2θ scansRint = 0.021
Absorption correction: analytical
?
θmax = 50.0°, θmin = 2.1°
Tmin = 0.268, Tmax = 0.381h = 3232
11127 measured reflectionsk = 77
3051 independent reflectionsl = 2121
Refinement top
Refinement on F0 constraints
Least-squares matrix: fullWeighting scheme based on measured s.u.'s
R[F2 > 2σ(F2)] = 0.018(Δ/σ)max = 1.956
wR(F2) = 0.019Δρmax = 0.77 (7) e Å3
S = 2.65Δρmin = 1.78 (7) e Å3
3041 reflectionsExtinction correction: Zachariasen, Eq22 p292 "Cryst. Comp." Munksgaard 1970
83 parametersExtinction coefficient: 23300 (300)
0 restraints
Crystal data top
Cu0.63O5V2V = 532.32 (6) Å3
Mr = 221.59Z = 6
Monoclinic, C2/mMo Kα radiation
a = 15.100 (1) ŵ = 8.79 mm1
b = 3.6382 (2) ÅT = 10 K
c = 10.0595 (7) Å0.27 × 0.18 × 0.17 mm
β = 105.585 (6)°
Data collection top
HUBER 512
diffractometer
3051 independent reflections
Absorption correction: analytical
?
3041 reflections with F > .00 sig(F )
Tmin = 0.268, Tmax = 0.381Rint = 0.021
11127 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0180 restraints
wR(F2) = 0.019(Δ/σ)max = 1.956
S = 2.65Δρmax = 0.77 (7) e Å3
3041 reflectionsΔρmin = 1.78 (7) e Å3
83 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
CU10.5412 (3)0.000000.3446 (3)0.0052 (3).429 (14)
CU20.5286 (4)0.0379 (19)0.3575 (4)0.0104 (5).254 (7)
V10.332203 (10)0.000000.089222 (15)0.00281 (4)
V20.113648 (12)0.000000.121234 (17)0.00556 (5)
V30.287002 (10)0.000000.406261 (15)0.00321 (4)
O10.000000.000000.000000.0065 (3)
O20.18862 (5)0.000000.04394 (7)0.00472 (19)
O30.36765 (5)0.000000.08718 (7)0.00475 (19)
O40.43233 (5)0.000000.20060 (7)0.0062 (2)
O50.26029 (5)0.000000.22253 (7)0.0049 (2)
O60.09558 (5)0.000000.27665 (7)0.0058 (2)
O70.24449 (5)0.000000.57618 (7)0.0051 (2)
O80.39945 (5)0.000000.45988 (7)0.0065 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
CU10.0047 (4)0.0070 (3)0.0032 (2)0.000000.0004 (2)0.00000
CU20.0072 (5)0.0181 (9)0.0038 (3)0.0044 (6)0.0019 (3)0.0022 (4)
V10.00296 (4)0.00238 (5)0.00293 (4)0.000000.00054 (3)0.00000
V20.01055 (6)0.00232 (5)0.00586 (5)0.000000.00573 (4)0.00000
V30.00421 (4)0.00255 (5)0.00278 (4)0.000000.00078 (3)0.00000
O10.0036 (3)0.0049 (3)0.0103 (4)0.000000.0007 (3)0.00000
O20.0051 (2)0.0034 (2)0.0054 (2)0.000000.00106 (16)0.00000
O30.0067 (2)0.0031 (2)0.0052 (2)0.000000.00283 (17)0.00000
O40.0045 (2)0.0070 (3)0.0061 (2)0.000000.00027 (17)0.00000
O50.0063 (2)0.0044 (2)0.0041 (2)0.000000.00174 (16)0.00000
O60.0065 (2)0.0070 (3)0.0043 (2)0.000000.00206 (17)0.00000
O70.0076 (2)0.0035 (2)0.0045 (2)0.000000.00242 (17)0.00000
O80.0056 (2)0.0081 (3)0.0049 (2)0.000000.00011 (17)0.00000

Experimental details

Crystal data
Chemical formulaCu0.63O5V2
Mr221.59
Crystal system, space groupMonoclinic, C2/m
Temperature (K)10
a, b, c (Å)15.100 (1), 3.6382 (2), 10.0595 (7)
β (°) 105.585 (6)
V3)532.32 (6)
Z6
Radiation typeMo Kα
µ (mm1)8.79
Crystal size (mm)0.27 × 0.18 × 0.17
Data collection
DiffractometerHUBER 512
diffractometer
Absorption correctionAnalytical
Tmin, Tmax0.268, 0.381
No. of measured, independent and
observed [F > .00 sig(F )] reflections
11127, 3051, 3041
Rint0.021
(sin θ/λ)max1)1.080
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.018, 0.019, 2.65
No. of reflections3041
No. of parameters83
(Δ/σ)max1.956
Δρmax, Δρmin (e Å3)0.77 (7), 1.78 (7)

Computer programs: Xtal DIFDAT ADDREF ABSORB SORTRF, Xtal CRYLSQ, Xtal CIFIO.

 

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