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Crystals of lithium niobium di­sulfide [LiyNbS2; y = 0.70 (9)] have been prepared by separated reactants metathesis (SRM) at 1073 K. Single-crystal data collected at reduced temperature [150 (2) K] indicate that the compound is isostructural with Li0.63NbS2 [Salyer, Barker, Blake, Gregory & Wilson (2003). Acta Cryst. C59, i4-i6], crystallizing in the hexagonal space group P63/mmc (No. 194). Li0.7NbS2 shows an expansion of both the a and c lattice parameters when compared with previously reported results on LiyNbS2 intercalation compounds with y < 0.70. This provides the first single-crystal structural evidence of unit cell expansion with increasing lithium content in LiyNbS2, where y > 0.5.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803014855/br6107sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803014855/br6107Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](Nb-S) = 0.001 Å
  • Disorder in solvent or counterion
  • R factor = 0.016
  • wR factor = 0.047
  • Data-to-parameter ratio = 9.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
CRYSC_01 Alert C There is an ordering error in _exptl_crystal_colour. It should be (QUALIFIER) (INTENSITY) (BASE_COLOUR). PLAT_302 Alert C Anion/Solvent Disorder ......................... 3.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT and SHELXTL (Bruker, 1997); program(s) used to solve structure: SIR92 (Altomare, 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS 4.1 (Dowty, 1998); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 1990, 2002).

(I) top
Crystal data top
Li0.70NbS2Dx = 4.260 Mg m3
Mr = 161.89Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmcCell parameters from 778 reflections
Hall symbol: -p 6c 2cθ = 3.2–28.9°
a = 3.3572 (5) ŵ = 6.02 mm1
c = 12.912 (3) ÅT = 150 K
V = 126.03 (4) Å3Hexagonal tablet, metallic grey
Z = 20.10 × 0.10 × 0.04 mm
F(000) = 150
Data collection top
Bruker SMART1000 CCD area-detector
diffractometer
85 independent reflections
Radiation source: normal-focus sealed tube83 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
ω scansθmax = 28.8°, θmin = 3.2°
Absorption correction: integration
(SHELXTL; Bruker, 2001)
h = 44
Tmin = 0.600, Tmax = 0.789k = 44
974 measured reflectionsl = 1717
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.016Secondary atom site location: difference Fourier map
wR(F2) = 0.047 w = 1/[σ2(Fo2) + (0.0212P)2 + 0.2307P]
where P = (Fo2 + 2Fc2)/3
S = 1.58(Δ/σ)max < 0.001
85 reflectionsΔρmax = 0.69 e Å3
9 parametersΔρmin = 0.60 e Å3
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*/UeqOcc. (<1)
Nb10.00000.00000.25000.0050 (3)
S10.33330.66670.12828 (10)0.0061 (4)
Li10.00000.00000.00000.012 (8)0.70 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0041 (3)0.0041 (3)0.0068 (4)0.00207 (16)0.0000.000
S10.0052 (5)0.0052 (5)0.0077 (6)0.0026 (2)0.0000.000
Li10.015 (10)0.015 (10)0.006 (11)0.007 (5)0.0000.000
Geometric parameters (Å, º) top
Nb1—S1i2.4954 (9)S1—Li12.5495 (9)
Nb1—S1ii2.4954 (9)S1—Li1viii2.5495 (9)
Nb1—S1iii2.4954 (9)S1—Li1vii2.5495 (9)
Nb1—S1iv2.4954 (9)Li1—S1x2.5495 (9)
Nb1—S12.4954 (9)Li1—S1xi2.5495 (9)
Nb1—S1v2.4954 (9)Li1—S1iv2.5495 (9)
Nb1—Li1vi3.2279 (6)Li1—S1xii2.5495 (9)
Nb1—Li13.2279 (6)Li1—S1ii2.5495 (9)
Nb1—Nb1ii3.3572 (5)Li1—Nb1x3.2279 (6)
Nb1—Nb1vii3.3572 (5)Li1—Li1vii3.3572 (5)
Nb1—Nb1viii3.3572 (5)Li1—Li1ii3.3572 (5)
Nb1—Nb1ix3.3572 (5)Li1—Li1iv3.3572 (5)
S1—Nb1vii2.4954 (9)Li1—Li1xiii3.3572 (5)
S1—Nb1viii2.4954 (9)
S1i—Nb1—S1ii134.294 (17)Nb1viii—S1—Li1viii79.550 (14)
S1i—Nb1—S1iii84.55 (4)Nb1—S1—Li1viii134.782 (5)
S1ii—Nb1—S1iii134.294 (17)Li1—S1—Li1viii82.36 (4)
S1i—Nb1—S1iv134.294 (17)Nb1vii—S1—Li1vii79.550 (14)
S1ii—Nb1—S1iv84.55 (4)Nb1viii—S1—Li1vii134.782 (5)
S1iii—Nb1—S1iv78.07 (5)Nb1—S1—Li1vii134.782 (5)
S1i—Nb1—S178.07 (5)Li1—S1—Li1vii82.36 (4)
S1ii—Nb1—S184.55 (4)Li1viii—S1—Li1vii82.36 (4)
S1iii—Nb1—S1134.294 (17)S1x—Li1—S1180.00 (5)
S1iv—Nb1—S184.55 (4)S1x—Li1—S1xi82.36 (4)
S1i—Nb1—S1v84.55 (4)S1—Li1—S1xi97.64 (4)
S1ii—Nb1—S1v78.07 (5)S1x—Li1—S1iv97.64 (4)
S1iii—Nb1—S1v84.55 (4)S1—Li1—S1iv82.36 (4)
S1iv—Nb1—S1v134.294 (17)S1xi—Li1—S1iv180.00 (5)
S1—Nb1—S1v134.294 (17)S1x—Li1—S1xii82.36 (4)
Li1vi—Nb1—Li1180.0S1—Li1—S1xii97.64 (4)
Nb1vii—S1—Nb1viii84.55 (4)S1xi—Li1—S1xii82.36 (4)
Nb1vii—S1—Nb184.55 (4)S1iv—Li1—S1xii97.64 (4)
Nb1viii—S1—Nb184.55 (4)S1x—Li1—S1ii97.64 (4)
Nb1vii—S1—Li1134.782 (5)S1—Li1—S1ii82.36 (4)
Nb1viii—S1—Li1134.782 (5)S1xi—Li1—S1ii97.64 (4)
Nb1—S1—Li179.550 (14)S1iv—Li1—S1ii82.36 (4)
Nb1vii—S1—Li1viii134.782 (5)S1xii—Li1—S1ii180.00 (5)
Symmetry codes: (i) x, y, z+1/2; (ii) x1, y1, z; (iii) x, y1, z+1/2; (iv) x, y1, z; (v) x1, y1, z+1/2; (vi) x, y, z+1/2; (vii) x+1, y+1, z; (viii) x, y+1, z; (ix) x+1, y, z; (x) x, y, z; (xi) x, y+1, z; (xii) x+1, y+1, z; (xiii) x1, y, z.
 

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