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A low-temperature structure determination of the title compound, (NH4)2[WS4], indicates several short N—H...S contacts between the two crystallographically independent ammonium cations and the tetrahedral [WS4]2− anions, which are all located on crystallographic mirror planes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804023761/wm6034sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804023761/wm6034Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](W-S) = 0.001 Å
  • R factor = 0.018
  • wR factor = 0.048
  • Data-to-parameter ratio = 25.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT420_ALERT_2_C D-H Without Acceptor N2 - H1N2 ... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H3# .. S1 .. 2.93 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H4# .. S1 .. 2.89 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H5# .. S1 .. 3.03 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 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 1 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 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: IPDS (Stoe & Cie, 1998); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXTL.

(I) top
Crystal data top
(NH4)2[WS4]F(000) = 640
Mr = 348.17Dx = 2.812 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 7250 reflections
a = 9.6054 (6) Åθ = 10–25°
b = 6.9863 (5) ŵ = 14.97 mm1
c = 12.2557 (10) ÅT = 150 K
V = 822.43 (10) Å3Block, yellow
Z = 40.10 × 0.09 × 0.08 mm
Data collection top
Stoe IPDS
diffractometer
1054 independent reflections
Radiation source: fine-focus sealed tube962 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
φ scansθmax = 27.9°, θmin = 2.7°
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)
h = 1212
Tmin = 0.238, Tmax = 0.297k = 99
7433 measured reflectionsl = 1616
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.018H-atom parameters constrained
wR(F2) = 0.048 w = 1/[σ2(Fo2) + (0.0285P)2 + 1.1841P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.001
1054 reflectionsΔρmax = 0.74 e Å3
41 parametersΔρmin = 1.36 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0029 (3)
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
W10.752691 (13)0.75000.571606 (12)0.00719 (10)
S10.52833 (10)0.75000.61117 (8)0.0151 (2)
S20.78299 (12)0.75000.39486 (8)0.0180 (2)
S30.85205 (8)0.49637 (11)0.64144 (6)0.01860 (17)
N10.4537 (4)0.75000.3368 (3)0.0144 (7)
H1N10.48200.75000.27020.022*
H2N10.51570.75000.38730.022*
H3N10.40180.65090.34590.022*
N20.1658 (4)0.75000.6127 (3)0.0168 (7)
H1N20.23350.75000.65850.025*
H2N20.08720.75000.64630.025*
H3N20.16890.64970.57210.025*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.00843 (13)0.00605 (13)0.00708 (12)0.0000.00001 (4)0.000
S10.0111 (4)0.0202 (5)0.0140 (5)0.0000.0034 (3)0.000
S20.0164 (5)0.0294 (6)0.0081 (5)0.0000.0028 (4)0.000
S30.0172 (3)0.0105 (3)0.0282 (4)0.0007 (3)0.0062 (3)0.0082 (3)
N10.0136 (16)0.0153 (17)0.0143 (16)0.0000.0026 (12)0.000
N20.0156 (17)0.0173 (19)0.0173 (17)0.0000.0027 (13)0.000
Geometric parameters (Å, º) top
W1—S22.1856 (11)N1—H2N10.8601
W1—S3i2.1870 (8)N1—H3N10.8600
W1—S32.1870 (7)N2—H1N20.8599
W1—S12.2090 (10)N2—H2N20.8601
N1—H1N10.8600N2—H3N20.8600
S2—W1—S3i109.25 (3)H1N1—N1—H2N1117.6
S2—W1—S3109.25 (3)H1N1—N1—H3N1107.9
S3i—W1—S3108.23 (4)H2N1—N1—H3N1107.9
S2—W1—S1110.33 (4)H1N2—N2—H2N2110.6
S3i—W1—S1109.87 (2)H1N2—N2—H3N2110.6
S3—W1—S1109.87 (2)H2N2—N2—H3N2107.9
Symmetry code: (i) x, y+3/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N1···S2ii0.862.783.278 (3)118
N1—H1N1···S3iii0.862.833.489 (3)135
N1—H1N1···S3iv0.862.833.489 (3)135
N1—H2N1···S20.862.573.242 (4)136
N1—H2N1···S10.862.753.439 (3)139
N1—H3N1···S3v0.862.653.414 (3)149
N1—H3N1···S1v0.862.933.5552 (7)131
N2—H1N2···S10.862.893.483 (4)128
N2—H2N2···S3vi0.862.873.513 (3)133
N2—H2N2···S3vii0.862.873.513 (3)133
N2—H2N2···S1viii0.863.033.633 (4)129
N2—H3N2···S3v0.862.823.563 (3)146
N2—H3N2···S2v0.862.863.5289 (6)136
Symmetry codes: (ii) x1/2, y, z+1/2; (iii) x+3/2, y+1, z1/2; (iv) x+3/2, y+1/2, z1/2; (v) x+1, y+1, z+1; (vi) x1, y, z; (vii) x1, y+3/2, z; (viii) x1/2, y, z+3/2.
 

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