Yb[AsO
4], ytterbium(III) oxoarsenate(V), adopts the xenotime structure type. Single crystals were obtained in an attempt to synthesize a compound with nominal composition Yb
3OCl[AsO
3]
2 by fusing a mixture of Yb
2O
3, YbCl
3 and As
2O
3 in a 4:1:3 molar ratio at 1123 K, owing to air-intrusion during the reaction. The structure is built up by chains of edge-sharing [YbO
8] trigonal dodecahedra and [AsO
4] tetrahedra in a primitive rod packing. Yb and As are situated on positions with
m2 symmetry, whereas O atoms are located on a mirror plane.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (s-O) = 0.002 Å
- R factor = 0.009
- wR factor = 0.023
- Data-to-parameter ratio = 9.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT021_ALERT_1_C Ratio Unique / Expected Reflections too High ... 1.02
PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.50
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXL97.
Ytterbium(III) Oxoarsenate(V)
top
Crystal data top
Yb(AsO4) | Dx = 6.830 Mg m−3 |
Mr = 311.96 | Mo Kα radiation, λ = 0.71069 Å |
Tetragonal, I41/amd | Cell parameters from 1512 reflections |
Hall symbol: -I 4bd 2 | θ = 4.4–28.3° |
a = 6.9712 (4) Å | µ = 41.46 mm−1 |
c = 6.2431 (4) Å | T = 293 K |
V = 303.40 (3) Å3 | Block, colourless |
Z = 4 | 0.07 × 0.06 × 0.04 mm |
F(000) = 540 | |
Data collection top
Nonius KappaCCD diffractometer | 114 independent reflections |
Radiation source: fine-focus sealed tube | 109 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.057 |
Detector resolution: 9 pixels mm-1 | θmax = 28.3°, θmin = 4.4° |
φ and ω scans | h = −9→9 |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1999) | k = −9→9 |
Tmin = 0.082, Tmax = 0.174 | l = −8→8 |
2463 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.009 | w = 1/[σ2(Fo2) + (0.0136P)2 + 0.1746P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.023 | (Δ/σ)max < 0.001 |
S = 1.06 | Δρmax = 1.13 e Å−3 |
114 reflections | Δρmin = −0.56 e Å−3 |
12 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0122 (5) |
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 | x | y | z | Uiso*/Ueq | |
Yb | 0.0000 | 0.7500 | 0.1250 | 0.00581 (15) | |
As | 0.0000 | 0.2500 | 0.3750 | 0.00456 (19) | |
O | 0.0000 | 0.4329 (3) | 0.1990 (3) | 0.0101 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Yb | 0.00622 (16) | 0.00622 (16) | 0.00497 (19) | 0.000 | 0.000 | 0.000 |
As | 0.0049 (3) | 0.0049 (3) | 0.0038 (3) | 0.000 | 0.000 | 0.000 |
O | 0.0149 (10) | 0.0074 (9) | 0.0080 (8) | 0.000 | 0.000 | 0.0031 (8) |
Geometric parameters (Å, º) top
Yb—O | 2.2584 (18) | Yb—Asv | 3.1215 (2) |
Yb—Oi | 2.2584 (18) | Yb—Ybix | 3.8191 (2) |
Yb—Oii | 2.2584 (18) | Yb—Ybv | 3.8191 (2) |
Yb—Oiii | 2.2584 (18) | As—Ox | 1.6831 (17) |
Yb—Oiv | 2.3910 (18) | As—Oxi | 1.6831 (17) |
Yb—Ov | 2.3910 (18) | As—Oxii | 1.6831 (17) |
Yb—Ovi | 2.3910 (18) | As—O | 1.6831 (17) |
Yb—Ovii | 2.3910 (18) | As—Ybviii | 3.1216 (2) |
Yb—Asviii | 3.1215 (2) | As—Ybv | 3.1215 (2) |
| | | |
O—Yb—Oi | 92.398 (18) | Ovi—Yb—Asv | 147.78 (4) |
O—Yb—Oii | 156.39 (9) | Ovii—Yb—Asv | 32.22 (4) |
Oi—Yb—Oii | 92.398 (18) | Asviii—Yb—Asv | 180.0 |
O—Yb—Oiii | 92.398 (18) | O—Yb—Ybix | 85.205 (18) |
Oi—Yb—Oiii | 156.39 (9) | Oi—Yb—Ybix | 167.68 (4) |
Oii—Yb—Oiii | 92.398 (18) | Oii—Yb—Ybix | 85.205 (18) |
O—Yb—Oiv | 80.03 (4) | Oiii—Yb—Ybix | 35.93 (4) |
Oi—Yb—Oiv | 134.03 (5) | Oiv—Yb—Ybix | 33.66 (4) |
Oii—Yb—Oiv | 80.03 (4) | Ov—Yb—Ybix | 110.227 (10) |
Oiii—Yb—Oiv | 69.58 (7) | Ovi—Yb—Ybix | 98.10 (4) |
O—Yb—Ov | 69.58 (7) | Ovii—Yb—Ybix | 110.227 (10) |
Oi—Yb—Ov | 80.03 (4) | Asviii—Yb—Ybix | 65.878 (2) |
Oii—Yb—Ov | 134.03 (5) | Asv—Yb—Ybix | 114.122 (2) |
Oiii—Yb—Ov | 80.03 (4) | O—Yb—Ybv | 35.93 (4) |
Oiv—Yb—Ov | 135.70 (5) | Oi—Yb—Ybv | 85.205 (18) |
O—Yb—Ovi | 80.03 (4) | Oii—Yb—Ybv | 167.68 (4) |
Oi—Yb—Ovi | 69.58 (7) | Oiii—Yb—Ybv | 85.205 (18) |
Oii—Yb—Ovi | 80.03 (4) | Oiv—Yb—Ybv | 110.227 (10) |
Oiii—Yb—Ovi | 134.03 (5) | Ov—Yb—Ybv | 33.66 (4) |
Oiv—Yb—Ovi | 64.45 (8) | Ovi—Yb—Ybv | 110.227 (10) |
Ov—Yb—Ovi | 135.70 (5) | Ovii—Yb—Ybv | 98.10 (4) |
O—Yb—Ovii | 134.03 (5) | Asviii—Yb—Ybv | 114.122 (2) |
Oi—Yb—Ovii | 80.03 (4) | Asv—Yb—Ybv | 65.878 (2) |
Oii—Yb—Ovii | 69.58 (7) | Ybix—Yb—Ybv | 99.614 (1) |
Oiii—Yb—Ovii | 80.03 (4) | Ox—As—Oxi | 115.23 (7) |
Oiv—Yb—Ovii | 135.70 (5) | Ox—As—Oxii | 98.49 (12) |
Ov—Yb—Ovii | 64.45 (8) | Oxi—As—Oxii | 115.23 (7) |
Ovi—Yb—Ovii | 135.70 (5) | Ox—As—O | 115.23 (7) |
O—Yb—Asviii | 78.20 (4) | Oxi—As—O | 98.49 (12) |
Oi—Yb—Asviii | 101.80 (4) | Oxii—As—O | 115.23 (7) |
Oii—Yb—Asviii | 78.20 (4) | Ox—As—Ybviii | 49.24 (6) |
Oiii—Yb—Asviii | 101.80 (4) | Oxi—As—Ybviii | 130.76 (6) |
Oiv—Yb—Asviii | 32.22 (4) | Oxii—As—Ybviii | 49.24 (6) |
Ov—Yb—Asviii | 147.78 (4) | O—As—Ybviii | 130.76 (6) |
Ovi—Yb—Asviii | 32.22 (4) | Ox—As—Ybv | 130.76 (6) |
Ovii—Yb—Asviii | 147.78 (4) | Oxi—As—Ybv | 49.24 (6) |
O—Yb—Asv | 101.80 (4) | Oxii—As—Ybv | 130.76 (6) |
Oi—Yb—Asv | 78.20 (4) | O—As—Ybv | 49.24 (6) |
Oii—Yb—Asv | 101.80 (4) | Ybviii—As—Ybv | 180.0 |
Oiii—Yb—Asv | 78.20 (4) | As—O—Yb | 151.05 (10) |
Oiv—Yb—Asv | 147.78 (4) | As—O—Ybv | 98.53 (8) |
Ov—Yb—Asv | 32.22 (4) | Yb—O—Ybv | 110.42 (7) |
Symmetry codes: (i) y−3/4, x+3/4, −z+1/4; (ii) −x, −y+3/2, z; (iii) −y+3/4, x+3/4, −z+1/4; (iv) y−1/4, −x+3/4, z+1/4; (v) −x, −y+1, −z; (vi) −y+1/4, −x+3/4, z+1/4; (vii) x, y+1/2, −z; (viii) −x, −y+1, −z+1; (ix) −x+1/2, −y+3/2, −z+1/2; (x) y−1/4, x+1/4, −z+3/4; (xi) −x, −y+1/2, z; (xii) −y+1/4, x+1/4, −z+3/4. |