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The title compound, dicaesium sulfate selenate-telluric acid adduct, Cs2(SO4)0.57(SeO4)0.43·Te(OH)6, is a solid solution in the series Cs2(SO4)·Te(OH)6/Cs2(SeO4)·Te(OH)6. It crystallizes in the same structure as the end member Cs2(SeO4)·Te(OH)6 in space group P21/c, whereas the corresponding sulfate adopts another structure type and crystallizes in space group R3. The structure contains planes of statistically distributed SO4/SeO4 tetrahedra alternating with planes of Te(OH)6 octahedra, and with Cs+ cations situated between the planes. Both Te atoms lie on centres of symmetry.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (Te-O) = 0.009 Å
- H-atom completeness 1%
- R factor = 0.037
- wR factor = 0.035
- Data-to-parameter ratio = 10.7
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O8 .. 2.59 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O7 .. 2.72 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O3 .. O7 .. 2.78 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O4 .. O10 .. 2.77 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O5 .. O10 .. 2.79 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O6 .. O9 .. 2.62 Ang.
Alert level C
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.92
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ?
PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc.
Alert level G
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:H6 Cs2 O10 S0.57 Se0.43 Te1
Atom count from the _atom_site data: Cs2 O10 S0.566 Se0.434 Te1
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_sum Cs2 H6 O10 S0.57 Se0.43 Te1
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
Cs 8.00 8.00 0.00
H 24.00 0.00 24.00
O 40.00 40.00 0.00
S 2.28 2.26 0.02
Se 1.72 1.74 -0.02
Te 4.00 4.00 0.00
0 ALERT level A = In general: serious problem
6 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
7 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 2001); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: CRYSTALS.
Dicesium sulfate-selenate tellurate
top
Crystal data top
Cs2(SO4)0.57(SeO4)0.43·Te(OH)6 | F(000) = 1063.2 |
Mr = 611.68 | Dx = 3.765 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 986 reflections |
a = 12.2646 (4) Å | θ = 1.8–25.8° |
b = 7.3926 (4) Å | µ = 11.12 mm−1 |
c = 12.6354 (6) Å | T = 298 K |
β = 111.095 (3)° | Prism, colourless |
V = 1068.84 (9) Å3 | 0.10 × 0.05 × 0.05 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 1216 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.042 |
φ scans | θmax = 25.8°, θmin = 1.8° |
Absorption correction: empirical (using intensity measurements) MULABS in PLATON (Spek, 2003) | h = −14→14 |
Tmin = 0.541, Tmax = 0.573 | k = −8→0 |
2044 measured reflections | l = 0→14 |
1881 independent reflections | |
Refinement top
Refinement on F | Primary atom site location: heavy-atom method |
Least-squares matrix: full | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.037 | Weighting scheme: Chebychev polynomial (Watkin, 1994; Prince,
1982) w = 1/[2.38T0(x)-2.95T1(x) + 2.50T2-1.02T3 + 0.340Tn-1(x)],
where x = F /Fmax; robust weighting (Prince, 1982): W =
w[1-(δF/6σF)2]2 |
wR(F2) = 0.035 | (Δ/σ)max = 0.000204 |
S = 0.94 | Δρmax = 2.43 e Å−3 |
1216 reflections | Δρmin = −2.54 e Å−3 |
114 parameters | Extinction correction: Larson (1970) |
1 restraint | Extinction coefficient: 17.2 (14) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Te1 | 0.0000 | 0.0000 | 0.5000 | 0.0126 | |
Te2 | 0.5000 | 0.5000 | 0.5000 | 0.0125 | |
Cs1 | 0.86573 (7) | 0.03842 (10) | 0.10885 (7) | 0.0157 | |
Cs2 | 0.63706 (7) | 0.99099 (11) | 0.35694 (6) | 0.0147 | |
S1 | 0.24815 (10) | −0.00046 (10) | 0.24890 (10) | 0.0182 | 0.566 (7) |
Se1 | 0.24815 (10) | −0.00046 (10) | 0.24890 (10) | 0.0182 | 0.434 (7) |
O1 | −0.0176 (8) | 0.2415 (11) | 0.4370 (7) | 0.0224 | |
O2 | −0.1109 (8) | −0.0746 (11) | 0.3562 (7) | 0.0198 | |
O3 | 0.1211 (7) | −0.0524 (12) | 0.4446 (7) | 0.0218 | |
O4 | 0.4726 (8) | 0.6954 (10) | 0.3913 (7) | 0.0173 | |
O5 | 0.3627 (8) | 0.3851 (11) | 0.3997 (7) | 0.0177 | |
O6 | 0.5857 (8) | 0.3786 (11) | 0.4197 (7) | 0.0169 | |
O7 | 0.1425 (8) | 0.1012 (11) | 0.2521 (7) | 0.0222 | |
O8 | 0.2189 (9) | −0.1993 (11) | 0.2202 (8) | 0.0203 | |
O9 | 0.2838 (8) | 0.0861 (11) | 0.1537 (8) | 0.0240 | |
O10 | 0.3449 (8) | 0.0117 (12) | 0.3679 (7) | 0.0236 | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Te1 | 0.01131 (16) | 0.01085 (16) | 0.01222 (16) | 0.00000 (16) | 0.00004 (16) | 0.00000 (16) |
Te2 | 0.01232 (16) | 0.01082 (16) | 0.01294 (16) | 0.00030 (16) | 0.00275 (16) | 0.00025 (16) |
Cs1 | 0.0132 (4) | 0.0164 (3) | 0.0178 (3) | 0.0005 (3) | 0.0058 (3) | 0.0013 (3) |
Cs2 | 0.0129 (4) | 0.0147 (3) | 0.0162 (3) | −0.0007 (3) | 0.0049 (3) | 0.0002 (3) |
S1 | 0.01767 (10) | 0.01767 (10) | 0.01767 (10) | −0.00276 (10) | 0.00445 (10) | −0.00276 (10) |
Se1 | 0.01767 (10) | 0.01767 (10) | 0.01767 (10) | −0.00276 (10) | 0.00445 (10) | −0.00276 (10) |
O1 | 0.023 (6) | 0.017 (4) | 0.026 (5) | 0.002 (4) | 0.008 (4) | 0.004 (3) |
O2 | 0.014 (5) | 0.017 (4) | 0.024 (5) | 0.001 (3) | 0.002 (4) | 0.000 (3) |
O3 | 0.013 (5) | 0.023 (4) | 0.032 (5) | 0.001 (4) | 0.011 (4) | 0.003 (4) |
O4 | 0.017 (5) | 0.017 (4) | 0.018 (4) | −0.004 (3) | 0.006 (4) | −0.001 (3) |
O5 | 0.014 (5) | 0.021 (4) | 0.016 (4) | −0.005 (3) | 0.004 (4) | −0.001 (3) |
O6 | 0.018 (5) | 0.018 (4) | 0.017 (4) | 0.002 (3) | 0.009 (4) | 0.000 (3) |
O7 | 0.025 (6) | 0.015 (4) | 0.026 (5) | 0.001 (3) | 0.008 (4) | 0.008 (3) |
O8 | 0.017 (5) | 0.015 (4) | 0.028 (5) | 0.000 (4) | 0.007 (4) | 0.001 (3) |
O9 | 0.018 (5) | 0.021 (4) | 0.031 (5) | 0.003 (4) | 0.007 (4) | 0.000 (4) |
O10 | 0.026 (5) | 0.019 (4) | 0.022 (4) | 0.002 (4) | 0.004 (4) | 0.005 (4) |
Geometric parameters (Å, º) top
Te1—O1i | 1.935 (8) | Cs1—O1iii | 3.065 (9) |
Te1—O2i | 1.917 (8) | Cs1—O3iv | 3.116 (9) |
Te1—O3i | 1.896 (8) | Cs1—O2v | 3.147 (9) |
Te1—O1 | 1.935 (8) | Cs1—O7v | 3.255 (9) |
Te1—O2 | 1.917 (8) | Cs1—O9vi | 3.292 (9) |
Te1—O3 | 1.896 (8) | Cs1—O8iv | 3.334 (9) |
Te2—O4ii | 1.937 (8) | Cs1—O1vii | 3.413 (9) |
Te2—O6ii | 1.925 (8) | Cs1—O6viii | 3.460 (9) |
Te2—O5ii | 1.905 (8) | Cs1—O7iii | 3.698 (8) |
Te2—O4 | 1.937 (8) | Cs2—O6ix | 3.098 (8) |
Te2—O5 | 1.905 (8) | Cs2—O4 | 3.109 (8) |
Te2—O6 | 1.925 (8) | Cs2—O2x | 3.133 (9) |
S1—O7 | 1.511 (9) | Cs2—O3ii | 3.153 (9) |
S1—O8 | 1.526 (8) | Cs2—O9iv | 3.165 (9) |
S1—O9 | 1.558 (9) | Cs2—O8xi | 3.248 (9) |
S1—O10 | 1.546 (8) | Cs2—O4iv | 3.301 (8) |
Se1—O7 | 1.511 (9) | Cs2—O5iv | 3.337 (8) |
Se1—O8 | 1.526 (8) | Cs2—O10ii | 3.404 (8) |
Se1—O9 | 1.558 (9) | Cs2—O10ix | 3.639 (10) |
Se1—O10 | 1.546 (8) | Cs2—O6iv | 3.675 (9) |
Cs1—O5iii | 2.988 (9) | | |
| | | |
O1i—Te1—O2i | 86.5 (4) | O4ii—Te2—O5 | 91.5 (3) |
O1i—Te1—O3i | 91.3 (4) | O6ii—Te2—O5 | 92.2 (4) |
O2i—Te1—O3i | 88.5 (4) | O5ii—Te2—O5 | 179.994 |
O1i—Te1—O1 | 179.994 | O4—Te2—O5 | 88.5 (3) |
O2i—Te1—O1 | 93.5 (4) | O4ii—Te2—O6 | 92.1 (4) |
O3i—Te1—O1 | 88.7 (4) | O6ii—Te2—O6 | 179.994 |
O1i—Te1—O2 | 93.5 (4) | O5ii—Te2—O6 | 92.2 (4) |
O2i—Te1—O2 | 179.994 | O4—Te2—O6 | 87.9 (4) |
O3i—Te1—O2 | 91.5 (4) | O5—Te2—O6 | 87.8 (4) |
O1—Te1—O2 | 86.5 (4) | O7—S1—O8 | 110.8 (5) |
O1i—Te1—O3 | 88.7 (4) | O7—S1—O9 | 107.3 (4) |
O2i—Te1—O3 | 91.5 (4) | O8—S1—O9 | 108.6 (5) |
O3i—Te1—O3 | 179.994 | O7—S1—O10 | 108.1 (5) |
O1—Te1—O3 | 91.3 (4) | O8—S1—O10 | 108.6 (5) |
O2—Te1—O3 | 88.5 (4) | O9—S1—O10 | 113.4 (5) |
O4ii—Te2—O6ii | 87.9 (4) | O7—Se1—O8 | 110.8 (5) |
O4ii—Te2—O5ii | 88.5 (3) | O7—Se1—O9 | 107.3 (4) |
O6ii—Te2—O5ii | 87.8 (4) | O8—Se1—O9 | 108.6 (5) |
O4ii—Te2—O4 | 179.994 | O7—Se1—O10 | 108.1 (5) |
O6ii—Te2—O4 | 92.1 (4) | O8—Se1—O10 | 108.6 (5) |
O5ii—Te2—O4 | 91.5 (3) | O9—Se1—O10 | 113.4 (5) |
Symmetry codes: (i) −x, −y, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, y−1/2, −z+1/2; (iv) −x+1, y+1/2, −z+1/2; (v) x+1, y, z; (vi) −x+1, −y, −z; (vii) x+1, −y+1/2, z−1/2; (viii) x, −y+1/2, z−1/2; (ix) x, y+1, z; (x) x+1, y+1, z; (xi) −x+1, y+3/2, −z+1/2. |
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