Cs₃TaS₄

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 TaS₄^3- anions.

Key indicators

• Single-crystal X-ray study
• T = 153 K
• Mean [sigma](Ta-S) = 0.001 Å
• R factor = 0.025
• wR factor = 0.071
• Data-to-parameter ratio = 33.7

checkCIF/PLATON results

No syntax errors found


No errors found in this datablock

---

Computing details

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

Crystal data

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) Å^3	Flat plate, colorless
Z = 4	0.43 × 0.12 × 0.05 mm

Data collection

'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

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.026	w = 1/[σ^2(Fo^2) + (0.0478P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00075 (13)

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Cs1—S3^i	3.4632 (9)	Ta—S1	2.2691 (9)
Cs1—S3^ii	3.5085 (9)	Ta—S3	2.2723 (14)
Cs1—S1^iii	3.5343 (10)	Ta—S2	2.2775 (13)
Cs1—S1^iv	3.5588 (10)	Ta—Cs1^ii	4.0754 (3)
Cs1—S1^v	3.6221 (11)	Ta—Cs1^x	4.0755 (3)
Cs1—S2	3.6271 (6)	Ta—Cs1^xi	4.3047 (3)
Cs1—S2^ii	3.7274 (11)	Ta—Cs1^xii	4.3047 (3)
Cs1—Cs2	4.0459 (4)	Ta—Cs2^vii	4.3628 (5)
Cs1—Ta^ii	4.0754 (3)	Ta—Cs1^iv	4.3809 (4)
Cs1—Ta^i	4.3046 (3)	S1—Cs1^xiii	3.5342 (10)
Cs1—Cs1^ii	4.3537 (6)	S1—Cs1^iv	3.5588 (10)
Cs1—Ta	4.3809 (4)	S1—Cs1^xii	3.6222 (11)
Cs2—S3^vi	3.4374 (14)	S1—Cs2^vii	3.6914 (10)
Cs2—S2^vii	3.5763 (14)	S1—Cs2^xiv	4.0975 (11)
Cs2—S2	3.6825 (14)	S2—Cs2^viii	3.5764 (14)
Cs2—S1^iii	3.6915 (10)	S2—Cs1^iv	3.6271 (6)
Cs2—S1^viii	3.6915 (10)	S2—Cs1^ii	3.7274 (11)
Cs2—Cs1^iv	4.0459 (4)	S2—Cs1^x	3.7275 (11)
Cs2—S1^v	4.0974 (11)	S3—Cs2^xv	3.4374 (14)
Cs2—S1^ix	4.0975 (11)	S3—Cs1^xi	3.4633 (9)
Cs2—Ta	4.3428 (6)	S3—Cs1^xii	3.4633 (9)
Cs2—Ta^viii	4.3629 (5)	S3—Cs1^ii	3.5085 (9)
Cs2—Cs1^i	4.8418 (4)	S3—Cs1^x	3.5085 (9)
Ta—S1^iv	2.2690 (9)
S3^i—Cs1—S3^ii	90.736 (8)	Ta—S1—Cs1^xiii	145.67 (4)
S3^i—Cs1—S1^iii	128.38 (3)	Ta—S1—Cs1^iv	94.90 (3)
S3^ii—Cs1—S1^iii	77.34 (2)	Cs1^xiii—S1—Cs1^iv	90.27 (2)
S3^i—Cs1—S1^iv	77.60 (2)	Ta—S1—Cs1^xii	90.91 (3)
S3^ii—Cs1—S1^iv	153.91 (3)	Cs1^xiii—S1—Cs1^xii	112.09 (3)
S1^iii—Cs1—S1^iv	128.08 (3)	Cs1^iv—S1—Cs1^xii	128.40 (3)
S3^i—Cs1—S1^v	62.59 (3)	Ta—S1—Cs2^vii	90.89 (3)
S3^ii—Cs1—S1^v	92.45 (3)	Cs1^xiii—S1—Cs2^vii	68.063 (19)
S1^iii—Cs1—S1^v	67.91 (3)	Cs1^iv—S1—Cs2^vii	147.43 (3)
S1^iv—Cs1—S1^v	102.363 (15)	Cs1^xii—S1—Cs2^vii	83.40 (2)
S3^i—Cs1—S2	139.74 (3)	Ta—S1—Cs2^xiv	135.43 (4)
S3^ii—Cs1—S2	126.83 (3)	Cs1^xiii—S1—Cs2^xiv	78.840 (19)
S1^iii—Cs1—S2	79.49 (3)	Cs1^iv—S1—Cs2^xiv	78.11 (2)
S1^iv—Cs1—S2	62.24 (2)	Cs1^xii—S1—Cs2^xiv	62.861 (18)
S1^v—Cs1—S2	121.33 (3)	Cs2^vii—S1—Cs2^xiv	118.50 (2)
S3^i—Cs1—S2^ii	75.83 (3)	Ta—S2—Cs2^viii	159.80 (5)
S3^ii—Cs1—S2^ii	61.38 (3)	Ta—S2—Cs1	92.95 (2)
S1^iii—Cs1—S2^ii	133.26 (3)	Cs2^viii—S2—Cs1	94.90 (2)
S1^iv—Cs1—S2^ii	92.93 (3)	Ta—S2—Cs1^iv	92.95 (2)
S1^v—Cs1—S2^ii	130.63 (2)	Cs2^viii—S2—Cs1^iv	94.90 (2)
S2—Cs1—S2^ii	107.420 (11)	Cs1—S2—Cs1^iv	134.04 (4)
S3^vi—Cs2—S2^vii	78.18 (3)	Ta—S2—Cs2	90.38 (4)
S3^vi—Cs2—S2	167.39 (3)	Cs2^viii—S2—Cs2	109.81 (3)
S2^vii—Cs2—S2	114.43 (3)	Cs1—S2—Cs2	67.21 (2)
S3^vi—Cs2—S1^iii	92.42 (3)	Cs1^iv—S2—Cs2	67.21 (2)
S2^vii—Cs2—S1^iii	148.161 (17)	Ta—S2—Cs1^ii	81.63 (3)
S2—Cs2—S1^iii	76.78 (2)	Cs2^viii—S2—Cs1^ii	83.02 (3)
S3^vi—Cs2—S1^viii	92.42 (3)	Cs1—S2—Cs1^ii	72.580 (10)
S2^vii—Cs2—S1^viii	148.160 (17)	Cs1^iv—S2—Cs1^ii	153.28 (3)
S2—Cs2—S1^viii	76.78 (2)	Cs2—S2—Cs1^ii	138.488 (16)
S1^iii—Cs2—S1^viii	61.34 (3)	Ta—S2—Cs1^x	81.63 (3)
S3^vi—Cs2—S1^v	70.857 (15)	Cs2^viii—S2—Cs1^x	83.02 (3)
S2^vii—Cs2—S1^v	86.745 (16)	Cs1—S2—Cs1^x	153.28 (3)
S2—Cs2—S1^v	108.525 (15)	Cs1^iv—S2—Cs1^x	72.579 (10)
S1^iii—Cs2—S1^v	61.50 (2)	Cs2—S2—Cs1^x	138.487 (16)
S1^viii—Cs2—S1^v	119.113 (16)	Cs1^ii—S2—Cs1^x	80.74 (3)
Cs1—Cs2—S1^v	52.815 (16)	Ta—S3—Cs2^xv	174.24 (5)
Cs1^iv—Cs2—S1^v	162.729 (16)	Ta—S3—Cs1^xi	95.00 (3)
S3^vi—Cs2—S1^ix	70.856 (15)	Cs2^xv—S3—Cs1^xi	89.12 (3)
S2^vii—Cs2—S1^ix	86.744 (16)	Ta—S3—Cs1^xii	95.00 (3)
S2—Cs2—S1^ix	108.525 (15)	Cs2^xv—S3—Cs1^xii	89.12 (3)
S1^iii—Cs2—S1^ix	119.113 (16)	Cs1^xi—S3—Cs1^xii	88.39 (3)
S1^viii—Cs2—S1^ix	61.50 (2)	Ta—S3—Cs1^ii	86.90 (3)
Cs1—Cs2—S1^ix	162.729 (16)	Cs2^xv—S3—Cs1^ii	88.93 (3)
Cs1^iv—Cs2—S1^ix	52.816 (16)	Cs1^xi—S3—Cs1^ii	92.291 (9)
S1^v—Cs2—S1^ix	141.69 (3)	Cs1^xii—S3—Cs1^ii	177.92 (4)
S1^iv—Ta—S1	112.16 (5)	Ta—S3—Cs1^x	86.90 (3)
S1^iv—Ta—S3	108.38 (3)	Cs2^xv—S3—Cs1^x	88.93 (3)
S1—Ta—S3	108.38 (3)	Cs1^xi—S3—Cs1^x	177.92 (4)
S1^iv—Ta—S2	109.56 (3)	Cs1^xii—S3—Cs1^x	92.290 (9)
S1—Ta—S2	109.56 (3)	Cs1^ii—S3—Cs1^x	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.