This work is a correction of our earlier structural study where the structure of K2SeO4Te(OH)6 (KSeTe) was published in the non-centrosymmetric space group Cc [Dammak et al. (1999). J. Solid State Chem. 145, 612-618]. The present X-ray structure determination, using remeasured intensities, shows that KSeTe is monoclinic in space group C2/c. In this structure, the Te atom lies on a centre of symmetry and the Se atom on a twofold axis.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Se-O) = 0.002 Å
- R factor = 0.019
- wR factor = 0.021
- Data-to-parameter ratio = 11.2
checkCIF/PLATON results
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PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
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Data collection: DENZO (Otwinowski & Minor, 1997); cell refinement: DENZO; data reduction: DENZO; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: CRYSTALS (Watkin et al., 2001); molecular graphics: DIAMOND (Brandenburg & Brendt, 1999); software used to prepare material for publication: CRYSTALS.
potassium selenate tellurate
top
Crystal data top
K2SeO4Te(OH)6 | F(000) = 840.0 |
Mr = 450.81 | Dx = 3.022 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3431 reflections |
a = 11.536 (2) Å | θ = 2–25° |
b = 6.427 (1) Å | µ = 7.55 mm−1 |
c = 13.898 (3) Å | T = 293 K |
β = 105.95 (3)° | Prism, white |
V = 990.8 (3) Å3 | 0.1 × 0.05 × 0.05 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 883 reflections with I > 3.00σ(I) |
Graphite monochromator | Rint = 0.042 |
φ rotation scans with 2°steps | θmax = 25.7°, θmin = 3.1° |
Absorption correction: empirical (using intensity measurements) (MULABS in PLATON; Spek, 1998) | h = 0→13 |
Tmin = 0.641, Tmax = 0.680 | k = 0→7 |
3431 measured reflections | l = −16→16 |
918 independent reflections | |
Refinement top
Refinement on F | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | All H-atom parameters refined |
R[F2 > 2σ(F2)] = 0.019 | Robust Weighting (Prince, 1982); W = [weight][1-(δF/6σF)2]2,
where [weight] is from the Chebychev polynomial:
[weight] = 1.0/[A0T0(x) + A1T1(x) ··· + An-1]*Tn-1(x)]
where Ai are the Chebychev coefficients = 1.85 -0.632 1.40, respectively,
and x = F /Fmax |
wR(F2) = 0.021 | (Δ/σ)max = 0.002 |
S = 1.04 | Δρmax = 0.87 e Å−3 |
883 reflections | Δρmin = −0.56 e Å−3 |
79 parameters | Extinction correction: Larson 1970 Crystallographic Computing eq 22 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 87.3 (32) |
Special details top
Experimental. Unit-cell dimensions were determined from more than a thousand reflections in
all the angular range, taken from ten frames with φ steps of 2°·A 180°
range in φ was scanned during data collection with 2°φ steps and 8 s
exposure by frame·The crystal to detector distance was 28 mm. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Te1 | 0.2500 | 0.2500 | 0.0000 | 0.0147 | |
Se1 | 0.0000 | 0.28752 (6) | 0.2500 | 0.0155 | |
K1 | 0.64897 (6) | 0.6996 (1) | 0.64109 (5) | 0.0320 | |
O1 | 0.23268 (19) | 0.2153 (3) | 0.13253 (14) | 0.0245 | |
O2 | 0.09939 (16) | 0.1107 (3) | −0.05302 (14) | 0.0259 | |
O3 | 0.16966 (17) | 0.5130 (3) | −0.01024 (13) | 0.0254 | |
O4 | 0.11687 (17) | 0.1409 (3) | 0.29889 (14) | 0.0313 | |
O5 | −0.03331 (16) | 0.4322 (3) | 0.33604 (13) | 0.0279 | |
H1 | 0.167 (4) | 0.275 (5) | 0.135 (2) | 0.033 (9)* | |
H2 | 0.112 (3) | 0.027 (6) | −0.095 (3) | 0.05 (1)* | |
H3 | 0.100 (4) | 0.514 (6) | −0.059 (3) | 0.055 (11)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Te1 | 0.01564 (18) | 0.01477 (17) | 0.01401 (16) | −0.00066 (7) | 0.0044 (1) | 0.00009 (6) |
Se1 | 0.0155 (2) | 0.01606 (19) | 0.0148 (2) | 0.0000 | 0.00393 (14) | 0.0000 |
K1 | 0.0268 (3) | 0.0235 (3) | 0.0447 (4) | 0.0011 (3) | 0.0083 (3) | −0.0007 (3) |
O1 | 0.0279 (11) | 0.0287 (9) | 0.0184 (8) | 0.0028 (8) | 0.0091 (7) | 0.0019 (7) |
O2 | 0.0212 (9) | 0.0276 (9) | 0.0301 (9) | −0.0050 (7) | 0.0091 (7) | −0.0095 (8) |
O3 | 0.029 (1) | 0.0182 (9) | 0.0265 (9) | 0.0069 (7) | 0.0029 (8) | −0.0007 (7) |
O4 | 0.028 (1) | 0.034 (1) | 0.033 (1) | 0.0107 (8) | 0.0104 (8) | 0.0126 (8) |
O5 | 0.030 (1) | 0.0278 (9) | 0.0284 (9) | −0.0003 (7) | 0.0115 (7) | −0.0114 (7) |
Geometric parameters (Å, º) top
Te1—O1 | 1.9195 (18) | K1—O5vii | 2.7775 (19) |
Te1—O1i | 1.9195 (18) | O1—O2 | 2.699 (3) |
Te1—O2 | 1.9131 (18) | O1—O2i | 2.721 (3) |
Te1—O2i | 1.9131 (18) | O1—O3 | 2.708 (3) |
Te1—O3 | 1.9141 (17) | O1—O3i | 2.713 (3) |
Te1—O3i | 1.9141 (17) | O1—O5ii | 2.824 (3) |
Se1—O4 | 1.6322 (18) | O2—O3 | 2.726 (3) |
Se1—O4ii | 1.6322 (18) | O2—O3i | 2.686 (3) |
Se1—O5 | 1.6416 (16) | O2—O4viii | 2.668 (3) |
Se1—O5ii | 1.6416 (16) | O3—O5ix | 2.724 (3) |
K1—O1iii | 2.849 (2) | O4—O4ii | 2.665 (4) |
K1—O2iv | 2.847 (2) | O4—O5 | 2.695 (2) |
K1—O3v | 2.8580 (18) | O4—O5ii | 2.638 (2) |
K1—O4vi | 2.794 (2) | O5—O5ii | 2.706 (3) |
| | | |
O1—Te1—O1i | 179.994 | O1—O2—O3i | 60.50 (7) |
O1—Te1—O2 | 89.55 (8) | O1i—O2—O3i | 60.11 (7) |
O1i—Te1—O2 | 90.45 (8) | O3—O2—O3i | 90.03 (7) |
O1—Te1—O2i | 90.45 (8) | Te1—O2—O4viii | 109.12 (8) |
O1i—Te1—O2i | 89.55 (8) | K1xi—O2—O4viii | 94.04 (7) |
O2—Te1—O2i | 179.994 | O1—O2—O4viii | 138.1 (1) |
O1—Te1—O3 | 89.89 (8) | O1i—O2—O4viii | 73.90 (7) |
O1i—Te1—O3 | 90.11 (8) | O3—O2—O4viii | 131.45 (9) |
O2—Te1—O3 | 90.85 (8) | O3i—O2—O4viii | 78.16 (8) |
O2i—Te1—O3 | 89.15 (8) | Te1—O3—K1xii | 130.74 (8) |
O1—Te1—O3i | 90.11 (8) | Te1—O3—O1 | 45.13 (5) |
O1i—Te1—O3i | 89.89 (8) | K1xii—O3—O1 | 88.70 (7) |
O2—Te1—O3i | 89.15 (8) | Te1—O3—O1i | 45.02 (5) |
O2i—Te1—O3i | 90.85 (8) | K1xii—O3—O1i | 160.63 (9) |
O3—Te1—O3i | 179.994 | O1—O3—O1i | 90.16 (7) |
O4—Se1—O4ii | 109.47 (15) | K1xii—O3—O2 | 133.91 (8) |
O4—Se1—O5 | 110.84 (9) | O1—O3—O2 | 59.57 (7) |
O4ii—Se1—O5 | 107.36 (9) | O1i—O3—O2 | 60.02 (6) |
O4—Se1—O5ii | 107.36 (9) | Te1—O3—O2i | 45.41 (5) |
O4ii—Se1—O5ii | 110.84 (9) | K1xii—O3—O2i | 103.08 (7) |
O5—Se1—O5ii | 110.99 (14) | O1—O3—O2i | 60.57 (7) |
O1iii—K1—O2iv | 96.13 (6) | O1i—O3—O2i | 59.99 (7) |
O1iii—K1—O3v | 118.44 (5) | O2—O3—O2i | 89.97 (7) |
O2iv—K1—O3v | 95.22 (6) | Te1—O3—O5ix | 117.82 (9) |
O1iii—K1—O4vi | 92.57 (6) | K1xii—O3—O5ix | 105.42 (7) |
O2iv—K1—O4vi | 168.01 (6) | O1—O3—O5ix | 131.74 (9) |
O3v—K1—O4vi | 73.33 (5) | O1i—O3—O5ix | 89.66 (8) |
O1iii—K1—O5vii | 168.82 (6) | O2—O3—O5ix | 79.14 (8) |
O2iv—K1—O5vii | 76.22 (5) | O2i—O3—O5ix | 148.91 (9) |
O3v—K1—O5vii | 70.94 (5) | Se1—O4—K1vi | 122.2 (1) |
O4vi—K1—O5vii | 96.23 (6) | Se1—O4—O2xiii | 116.24 (9) |
Te1—O1—K1x | 105.94 (8) | K1vi—O4—O2xiii | 105.30 (8) |
Te1—O1—O2 | 45.13 (6) | K1vi—O4—O4ii | 155.78 (6) |
K1x—O1—O2 | 72.31 (6) | O2xiii—O4—O4ii | 96.49 (8) |
K1x—O1—O2i | 133.55 (8) | K1vi—O4—O5 | 107.91 (8) |
O2—O1—O2i | 89.81 (7) | O2xiii—O4—O5 | 94.84 (8) |
K1x—O1—O3 | 131.75 (9) | O4ii—O4—O5 | 58.95 (6) |
O2—O1—O3 | 60.55 (7) | K1vi—O4—O5ii | 94.95 (7) |
O2i—O1—O3 | 59.31 (7) | O2xiii—O4—O5ii | 152.65 (9) |
K1x—O1—O3i | 73.97 (6) | O4ii—O4—O5ii | 61.10 (7) |
O2—O1—O3i | 59.51 (7) | O5—O4—O5ii | 60.96 (9) |
O2i—O1—O3i | 60.22 (7) | Se1—O5—K1vii | 141.4 (1) |
O3—O1—O3i | 89.84 (7) | Se1—O5—O1ii | 101.34 (9) |
Te1—O1—O5ii | 113.26 (9) | K1vii—O5—O1ii | 88.03 (6) |
K1x—O1—O5ii | 98.96 (7) | Se1—O5—O3xiv | 108.76 (9) |
O2—O1—O5ii | 89.79 (8) | K1vii—O5—O3xiv | 97.85 (7) |
O2i—O1—O5ii | 124.12 (9) | O1ii—O5—O3xiv | 120.23 (8) |
O3—O1—O5ii | 72.45 (7) | K1vii—O5—O4 | 165.47 (9) |
O3i—O1—O5ii | 149.29 (9) | O1ii—O5—O4 | 106.28 (8) |
Te1—O2—K1xi | 140.51 (9) | O3xiv—O5—O4 | 77.34 (7) |
Te1—O2—O1 | 45.32 (6) | K1vii—O5—O4ii | 126.36 (8) |
K1xi—O2—O1 | 127.05 (8) | O1ii—O5—O4ii | 66.77 (7) |
K1xi—O2—O1i | 119.18 (8) | O3xiv—O5—O4ii | 135.78 (9) |
O1—O2—O1i | 90.19 (7) | O4—O5—O4ii | 59.96 (9) |
K1xi—O2—O3 | 96.16 (7) | K1vii—O5—O5ii | 111.30 (5) |
O1—O2—O3 | 59.88 (7) | O1ii—O5—O5ii | 125.30 (9) |
O1i—O2—O3 | 59.76 (7) | O3xiv—O5—O5ii | 107.5 (1) |
Te1—O2—O3i | 45.44 (5) | O4—O5—O5ii | 58.47 (6) |
K1xi—O2—O3i | 172.10 (8) | O4ii—O5—O5ii | 60.57 (6) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z; (ii) −x, y, −z+1/2; (iii) x+1/2, −y+1/2, z+1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) x+1/2, −y+3/2, z+1/2; (vi) −x+1, −y+1, −z+1; (vii) −x+1/2, −y+3/2, −z+1; (viii) x, −y, z−1/2; (ix) x, −y+1, z−1/2; (x) x−1/2, −y+1/2, z−1/2; (xi) −x+1/2, y−1/2, −z+1/2; (xii) x−1/2, −y+3/2, z−1/2; (xiii) x, −y, z+1/2; (xiv) x, −y+1, z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O5ii | 0.85 (4) | 1.98 (4) | 2.824 (3) | 170 (4) |
O2—H2···O4viii | 0.84 (4) | 1.83 (4) | 2.668 (3) | 171 (3) |
O3—H3···O5ix | 0.90 (4) | 1.84 (4) | 2.724 (3) | 169 (4) |
Symmetry codes: (ii) −x, y, −z+1/2; (viii) x, −y, z−1/2; (ix) x, −y+1, z−1/2. |