Uranium tris­ulfide, US₃

Uranium tris­ulfide, US₃, is isostructural with USe₃, which has the ZrSe₃ structure type. In the asymmetric unit, the site symmetries of the U atom and the three S atoms are m. The structure consists of two-dimensional layers that stack perpendicular to the [001] direction. Each layer comprises US₈ bicapped trigonal prisms that edge share in the [100] direction and face share in the [010] direction. The compound may be described as U⁴⁺(S²⁻)(S₂²⁻).

Key indicators

• Single-crystal X-ray study
• T = 153 K
• Mean [sigma](S-S) = 0.004 Å
• R factor = 0.031
• wR factor = 0.085
• Data-to-parameter ratio = 20.8

checkCIF/PLATON results

No syntax errors found



Alert level C
DIFMX01_ALERT_2_C  The maximum difference density is > 0.1*ZMAX*0.75
            _refine_diff_density_max given =      7.920
            Test value =      6.900
DIFMX02_ALERT_1_C  The maximum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.78
PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............       7.92 e/A   3

   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

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: SMART (Bruker, 2003); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: CrystalMaker (CrystalMaker Software, 2005); software used to prepare material for publication: SHELXTL.

uranium trisulfide

Crystal data

US3	F(000) = 280
Mr = 334.21	Dx = 5.822 Mg m^−3
Monoclinic, P21/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yb	Cell parameters from 2131 reflections
a = 5.3738 (14) Å	θ = 2.3–28.8°
b = 3.9598 (10) Å	µ = 43.95 mm^−1
c = 9.032 (2) Å	T = 153 K
β = 97.258 (3)°	Plate-like needle, black
V = 190.66 (8) Å^3	0.35 × 0.06 × 0.01 mm
Z = 2

Data collection

Bruker SMART 1000 CCD diffractometer	521 independent reflections
Radiation source: fine-focus sealed tube	510 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.035
ω scans	θmax = 28.8°, θmin = 2.3°
Absorption correction: numerical face indexed	h = −6→7
Tmin = 0.049, Tmax = 0.542	k = −5→5
2232 measured reflections	l = −11→11

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.031	Secondary atom site location: difference Fourier map
wR(F^2) = 0.085	w = 1/[σ^2(Fo^2) + (0.0643P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.16	(Δ/σ)max < 0.001
521 reflections	Δρmax = 7.92 e Å^−3
25 parameters	Δρmin = −2.09 e Å^−3

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
U1	0.28292 (5)	0.2500	0.15671 (3)	0.0064 (2)
S1	0.4794 (5)	0.2500	0.6668 (3)	0.0092 (5)
S2	0.7634 (4)	0.2500	0.0609 (3)	0.0071 (5)
S3	0.8656 (5)	0.2500	0.6584 (3)	0.0100 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
U1	0.0057 (3)	0.0033 (3)	0.0100 (3)	0.000	0.00029 (18)	0.000
S1	0.0090 (12)	0.0066 (10)	0.0109 (12)	0.000	−0.0024 (9)	0.000
S2	0.0051 (11)	0.0072 (11)	0.0089 (11)	0.000	0.0002 (8)	0.000
S3	0.0104 (13)	0.0073 (12)	0.0125 (12)	0.000	0.0028 (9)	0.000

Geometric parameters (Å, º)

U1—S1^i	2.7530 (18)	U1—U1^vii	3.9598 (10)
U1—S1^ii	2.7530 (18)	S1—S3	2.086 (4)
U1—S3^i	2.7716 (19)	S1—U1^i	2.7529 (18)
U1—S3^ii	2.7716 (19)	S1—U1^ii	2.7529 (18)
U1—S2^iii	2.7787 (18)	S2—U1^iii	2.7787 (18)
U1—S2^iv	2.7787 (18)	S2—U1^iv	2.7787 (18)
U1—S2^v	2.817 (2)	S2—U1^viii	2.817 (2)
U1—S2	2.825 (2)	S3—U1^i	2.7716 (19)
U1—U1^vi	3.9598 (10)	S3—U1^ii	2.7716 (19)
S1^i—U1—S1^ii	91.98 (8)	S1^ii—U1—U1^vi	135.99 (4)
S1^i—U1—S3^i	44.37 (8)	S3^i—U1—U1^vi	44.41 (4)
S1^ii—U1—S3^i	108.22 (7)	S3^ii—U1—U1^vi	135.59 (4)
S1^i—U1—S3^ii	108.22 (7)	S2^iii—U1—U1^vi	135.44 (4)
S1^ii—U1—S3^ii	44.37 (8)	S2^iv—U1—U1^vi	44.56 (4)
S3^i—U1—S3^ii	91.18 (8)	S2^v—U1—U1^vi	90.0
S1^i—U1—S2^iii	156.30 (7)	S2—U1—U1^vi	90.0
S1^ii—U1—S2^iii	83.73 (6)	S1^i—U1—U1^vii	135.99 (4)
S3^i—U1—S2^iii	158.16 (7)	S1^ii—U1—U1^vii	44.01 (4)
S3^ii—U1—S2^iii	84.85 (6)	S3^i—U1—U1^vii	135.59 (4)
S1^i—U1—S2^iv	83.73 (6)	S3^ii—U1—U1^vii	44.41 (4)
S1^ii—U1—S2^iv	156.30 (7)	S2^iii—U1—U1^vii	44.56 (4)
S3^i—U1—S2^iv	84.85 (6)	S2^iv—U1—U1^vii	135.44 (4)
S3^ii—U1—S2^iv	158.16 (7)	S2^v—U1—U1^vii	90.0
S2^iii—U1—S2^iv	90.88 (7)	S2—U1—U1^vii	90.0
S1^i—U1—S2^v	123.18 (5)	U1^vi—U1—U1^vii	180.000 (15)
S1^ii—U1—S2^v	123.18 (5)	S3—S1—U1^i	68.29 (7)
S3^i—U1—S2^v	80.53 (7)	S3—S1—U1^ii	68.29 (7)
S3^ii—U1—S2^v	80.53 (7)	U1^i—S1—U1^ii	91.98 (8)
S2^iii—U1—S2^v	77.64 (6)	U1^iii—S2—U1^iv	90.88 (7)
S2^iv—U1—S2^v	77.64 (6)	U1^iii—S2—U1^viii	102.36 (6)
S1^i—U1—S2	78.60 (6)	U1^iv—S2—U1^viii	102.36 (6)
S1^ii—U1—S2	78.60 (6)	U1^iii—S2—U1	102.30 (6)
S3^i—U1—S2	121.90 (6)	U1^iv—S2—U1	102.30 (6)
S3^ii—U1—S2	121.90 (6)	U1^viii—S2—U1	144.56 (10)
S2^iii—U1—S2	77.70 (6)	S1—S3—U1^i	67.34 (8)
S2^iv—U1—S2	77.70 (6)	S1—S3—U1^ii	67.34 (8)
S2^v—U1—S2	144.56 (10)	U1^i—S3—U1^ii	91.18 (8)
S1^i—U1—U1^vi	44.01 (4)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) −x+1, −y, −z; (iv) −x+1, −y+1, −z; (v) x−1, y, z; (vi) x, y+1, z; (vii) x, y−1, z; (viii) x+1, y, z.