Tricesium tantalum tetrasulfide, Cs3TaS4, crystallizes in space group Pnma of the orthorhombic system. It is isostructural with K3VS4. In the asymmetric unit, the site symmetries of one of the Cs atoms, the Ta atom, and two of the S atoms are m. The structure consists of the packing of discrete Cs+ cations and nearly regular tetrahedral TaS43- anions.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean (Ta-S) = 0.001 Å
- R factor = 0.025
- wR factor = 0.071
- Data-to-parameter ratio = 33.7
checkCIF/PLATON results
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Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2003); program(s) used to refine structure: SHELXL97 in SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL.
Tricesium tantalum tetrasulfide
top
Crystal data top
Cs3TaS4 | F(000) = 1208 |
Mr = 707.92 | Dx = 4.144 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 5650 reflections |
a = 9.9205 (8) Å | θ = 2.7–28.8° |
b = 11.507 (1) Å | µ = 19.83 mm−1 |
c = 9.9406 (9) Å | T = 153 K |
V = 1134.77 (17) Å3 | Flat plate, colorless |
Z = 4 | 0.43 × 0.12 × 0.05 mm |
Data collection top
'Bruker SMART 1000 CCD' diffractometer | 1482 independent reflections |
Radiation source: fine-focus sealed tube | 1462 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
0.3° ω scans | θmax = 28.8°, θmin = 2.7° |
Absorption correction: numerical face indexed (SHELXTL, Sheldrick, 2003)' | h = −13→13 |
Tmin = 0.037, Tmax = 0.396 | k = −15→15 |
12415 measured reflections | l = −13→13 |
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)] = 0.026 | w = 1/[σ2(Fo2) + (0.0478P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.071 | (Δ/σ)max = 0.002 |
S = 1.20 | Δρmax = 3.16 e Å−3 |
1482 reflections | Δρmin = −3.04 e Å−3 |
44 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00075 (13) |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cs1 | 0.04691 (2) | 0.540192 (18) | 0.29120 (2) | 0.01540 (12) | |
Cs2 | 0.14991 (3) | 0.2500 | 0.08566 (4) | 0.02268 (13) | |
Ta | 0.222204 (19) | 0.2500 | 0.51653 (2) | 0.01070 (11) | |
S1 | 0.33203 (9) | 0.08637 (9) | 0.45161 (11) | 0.0202 (2) | |
S2 | 0.01011 (13) | 0.2500 | 0.42884 (13) | 0.0143 (3) | |
S3 | 0.20718 (12) | 0.2500 | 0.74462 (13) | 0.0141 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cs1 | 0.01669 (18) | 0.01083 (17) | 0.01869 (18) | 0.00041 (7) | −0.00036 (8) | 0.00079 (8) |
Cs2 | 0.0172 (2) | 0.0345 (2) | 0.0164 (2) | 0.000 | 0.00236 (12) | 0.000 |
Ta | 0.01025 (16) | 0.01044 (16) | 0.01141 (16) | 0.000 | 0.00022 (6) | 0.000 |
S1 | 0.0168 (5) | 0.0201 (5) | 0.0237 (5) | 0.0056 (4) | −0.0010 (4) | −0.0071 (4) |
S2 | 0.0112 (5) | 0.0153 (6) | 0.0164 (6) | 0.000 | −0.0014 (4) | 0.000 |
S3 | 0.0161 (6) | 0.0143 (6) | 0.0118 (6) | 0.000 | 0.0001 (5) | 0.000 |
Geometric parameters (Å, º) top
Cs1—S3i | 3.4632 (9) | Ta—S1 | 2.2691 (9) |
Cs1—S3ii | 3.5085 (9) | Ta—S3 | 2.2723 (14) |
Cs1—S1iii | 3.5343 (10) | Ta—S2 | 2.2775 (13) |
Cs1—S1iv | 3.5588 (10) | Ta—Cs1ii | 4.0754 (3) |
Cs1—S1v | 3.6221 (11) | Ta—Cs1x | 4.0755 (3) |
Cs1—S2 | 3.6271 (6) | Ta—Cs1xi | 4.3047 (3) |
Cs1—S2ii | 3.7274 (11) | Ta—Cs1xii | 4.3047 (3) |
Cs1—Cs2 | 4.0459 (4) | Ta—Cs2vii | 4.3628 (5) |
Cs1—Taii | 4.0754 (3) | Ta—Cs1iv | 4.3809 (4) |
Cs1—Tai | 4.3046 (3) | S1—Cs1xiii | 3.5342 (10) |
Cs1—Cs1ii | 4.3537 (6) | S1—Cs1iv | 3.5588 (10) |
Cs1—Ta | 4.3809 (4) | S1—Cs1xii | 3.6222 (11) |
Cs2—S3vi | 3.4374 (14) | S1—Cs2vii | 3.6914 (10) |
Cs2—S2vii | 3.5763 (14) | S1—Cs2xiv | 4.0975 (11) |
Cs2—S2 | 3.6825 (14) | S2—Cs2viii | 3.5764 (14) |
Cs2—S1iii | 3.6915 (10) | S2—Cs1iv | 3.6271 (6) |
Cs2—S1viii | 3.6915 (10) | S2—Cs1ii | 3.7274 (11) |
Cs2—Cs1iv | 4.0459 (4) | S2—Cs1x | 3.7275 (11) |
Cs2—S1v | 4.0974 (11) | S3—Cs2xv | 3.4374 (14) |
Cs2—S1ix | 4.0975 (11) | S3—Cs1xi | 3.4633 (9) |
Cs2—Ta | 4.3428 (6) | S3—Cs1xii | 3.4633 (9) |
Cs2—Taviii | 4.3629 (5) | S3—Cs1ii | 3.5085 (9) |
Cs2—Cs1i | 4.8418 (4) | S3—Cs1x | 3.5085 (9) |
Ta—S1iv | 2.2690 (9) | | |
| | | |
S3i—Cs1—S3ii | 90.736 (8) | Ta—S1—Cs1xiii | 145.67 (4) |
S3i—Cs1—S1iii | 128.38 (3) | Ta—S1—Cs1iv | 94.90 (3) |
S3ii—Cs1—S1iii | 77.34 (2) | Cs1xiii—S1—Cs1iv | 90.27 (2) |
S3i—Cs1—S1iv | 77.60 (2) | Ta—S1—Cs1xii | 90.91 (3) |
S3ii—Cs1—S1iv | 153.91 (3) | Cs1xiii—S1—Cs1xii | 112.09 (3) |
S1iii—Cs1—S1iv | 128.08 (3) | Cs1iv—S1—Cs1xii | 128.40 (3) |
S3i—Cs1—S1v | 62.59 (3) | Ta—S1—Cs2vii | 90.89 (3) |
S3ii—Cs1—S1v | 92.45 (3) | Cs1xiii—S1—Cs2vii | 68.063 (19) |
S1iii—Cs1—S1v | 67.91 (3) | Cs1iv—S1—Cs2vii | 147.43 (3) |
S1iv—Cs1—S1v | 102.363 (15) | Cs1xii—S1—Cs2vii | 83.40 (2) |
S3i—Cs1—S2 | 139.74 (3) | Ta—S1—Cs2xiv | 135.43 (4) |
S3ii—Cs1—S2 | 126.83 (3) | Cs1xiii—S1—Cs2xiv | 78.840 (19) |
S1iii—Cs1—S2 | 79.49 (3) | Cs1iv—S1—Cs2xiv | 78.11 (2) |
S1iv—Cs1—S2 | 62.24 (2) | Cs1xii—S1—Cs2xiv | 62.861 (18) |
S1v—Cs1—S2 | 121.33 (3) | Cs2vii—S1—Cs2xiv | 118.50 (2) |
S3i—Cs1—S2ii | 75.83 (3) | Ta—S2—Cs2viii | 159.80 (5) |
S3ii—Cs1—S2ii | 61.38 (3) | Ta—S2—Cs1 | 92.95 (2) |
S1iii—Cs1—S2ii | 133.26 (3) | Cs2viii—S2—Cs1 | 94.90 (2) |
S1iv—Cs1—S2ii | 92.93 (3) | Ta—S2—Cs1iv | 92.95 (2) |
S1v—Cs1—S2ii | 130.63 (2) | Cs2viii—S2—Cs1iv | 94.90 (2) |
S2—Cs1—S2ii | 107.420 (11) | Cs1—S2—Cs1iv | 134.04 (4) |
S3vi—Cs2—S2vii | 78.18 (3) | Ta—S2—Cs2 | 90.38 (4) |
S3vi—Cs2—S2 | 167.39 (3) | Cs2viii—S2—Cs2 | 109.81 (3) |
S2vii—Cs2—S2 | 114.43 (3) | Cs1—S2—Cs2 | 67.21 (2) |
S3vi—Cs2—S1iii | 92.42 (3) | Cs1iv—S2—Cs2 | 67.21 (2) |
S2vii—Cs2—S1iii | 148.161 (17) | Ta—S2—Cs1ii | 81.63 (3) |
S2—Cs2—S1iii | 76.78 (2) | Cs2viii—S2—Cs1ii | 83.02 (3) |
S3vi—Cs2—S1viii | 92.42 (3) | Cs1—S2—Cs1ii | 72.580 (10) |
S2vii—Cs2—S1viii | 148.160 (17) | Cs1iv—S2—Cs1ii | 153.28 (3) |
S2—Cs2—S1viii | 76.78 (2) | Cs2—S2—Cs1ii | 138.488 (16) |
S1iii—Cs2—S1viii | 61.34 (3) | Ta—S2—Cs1x | 81.63 (3) |
S3vi—Cs2—S1v | 70.857 (15) | Cs2viii—S2—Cs1x | 83.02 (3) |
S2vii—Cs2—S1v | 86.745 (16) | Cs1—S2—Cs1x | 153.28 (3) |
S2—Cs2—S1v | 108.525 (15) | Cs1iv—S2—Cs1x | 72.579 (10) |
S1iii—Cs2—S1v | 61.50 (2) | Cs2—S2—Cs1x | 138.487 (16) |
S1viii—Cs2—S1v | 119.113 (16) | Cs1ii—S2—Cs1x | 80.74 (3) |
Cs1—Cs2—S1v | 52.815 (16) | Ta—S3—Cs2xv | 174.24 (5) |
Cs1iv—Cs2—S1v | 162.729 (16) | Ta—S3—Cs1xi | 95.00 (3) |
S3vi—Cs2—S1ix | 70.856 (15) | Cs2xv—S3—Cs1xi | 89.12 (3) |
S2vii—Cs2—S1ix | 86.744 (16) | Ta—S3—Cs1xii | 95.00 (3) |
S2—Cs2—S1ix | 108.525 (15) | Cs2xv—S3—Cs1xii | 89.12 (3) |
S1iii—Cs2—S1ix | 119.113 (16) | Cs1xi—S3—Cs1xii | 88.39 (3) |
S1viii—Cs2—S1ix | 61.50 (2) | Ta—S3—Cs1ii | 86.90 (3) |
Cs1—Cs2—S1ix | 162.729 (16) | Cs2xv—S3—Cs1ii | 88.93 (3) |
Cs1iv—Cs2—S1ix | 52.816 (16) | Cs1xi—S3—Cs1ii | 92.291 (9) |
S1v—Cs2—S1ix | 141.69 (3) | Cs1xii—S3—Cs1ii | 177.92 (4) |
S1iv—Ta—S1 | 112.16 (5) | Ta—S3—Cs1x | 86.90 (3) |
S1iv—Ta—S3 | 108.38 (3) | Cs2xv—S3—Cs1x | 88.93 (3) |
S1—Ta—S3 | 108.38 (3) | Cs1xi—S3—Cs1x | 177.92 (4) |
S1iv—Ta—S2 | 109.56 (3) | Cs1xii—S3—Cs1x | 92.290 (9) |
S1—Ta—S2 | 109.56 (3) | Cs1ii—S3—Cs1x | 86.96 (3) |
S3—Ta—S2 | 108.74 (4) | | |
Symmetry codes: (i) −x+1/2, −y+1, z−1/2; (ii) −x, −y+1, −z+1; (iii) x−1/2, −y+1/2, −z+1/2; (iv) x, −y+1/2, z; (v) −x+1/2, y+1/2, z−1/2; (vi) x, y, z−1; (vii) x+1/2, y, −z+1/2; (viii) x−1/2, y, −z+1/2; (ix) −x+1/2, −y, z−1/2; (x) −x, y−1/2, −z+1; (xi) −x+1/2, −y+1, z+1/2; (xii) −x+1/2, y−1/2, z+1/2; (xiii) x+1/2, −y+1/2, −z+1/2; (xiv) −x+1/2, −y, z+1/2; (xv) x, y, z+1. |