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The title compound displays isolated [SiS4]4- tetrahedra and a chain of I atoms along [001]. Iodine, which lies on a twofold axis, is coordinated by three lanthanum cations, one of which lies on the same twofold axis, forming an isosceles triangle. The compound is isotypic with Ce3I[SiS4]2 [Gauthier et al. (1998). J. Alloys Compd, 275-277, 46-49].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802019256/br6065sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802019256/br6065Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](S-Si) = 0.001 Å
  • R factor = 0.019
  • wR factor = 0.040
  • Data-to-parameter ratio = 25.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

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

Lanthanum(III)-iodide-di-ortho-thiosilicate top
Crystal data top
La3I(SiS4)2F(000) = 1520
Mr = 856.29Dx = 4.119 Mg m3
Monoclinic, C2/cMelting point: not measured K
Hall symbol: -C 2ycMo Kα radiation, λ = 0.71073 Å
a = 16.110 (3) ÅCell parameters from 11586 reflections
b = 7.9175 (12) Åθ = 2.6–28.1°
c = 10.931 (2) ŵ = 12.69 mm1
β = 97.94 (2)°T = 293 K
V = 1380.9 (4) Å3Tabular, white
Z = 40.20 × 0.13 × 0.09 mm
Data collection top
Stoe IPDS
diffractometer
1671 independent reflections
Radiation source: fine-focus sealed tube1467 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
Detector resolution: 60 pixels mm-1θmax = 28.1°, θmin = 2.6°
240 exposures, Δφ 1.2° scansh = 2121
Absorption correction: gaussian
(X-RED; Stoe & Cie, 1998)
k = 1010
Tmin = 0.120, Tmax = 0.256l = 1414
11586 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.019 w = 1/[σ2(Fo2) + (0.0253P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.040(Δ/σ)max = 0.001
S = 0.95Δρmax = 0.89 e Å3
1671 reflectionsΔρmin = 1.22 e Å3
66 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00359 (8)
Special details top

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
La10.196475 (12)0.11952 (3)0.67991 (2)0.00871 (7)
La20.50000.09471 (4)0.75000.01084 (9)
I0.00000.98426 (5)0.25000.02214 (11)
Si0.15969 (6)0.46257 (13)0.02948 (9)0.00768 (19)
S10.14499 (5)0.25682 (12)0.14650 (9)0.01085 (19)
S20.28056 (5)0.56896 (12)0.08540 (8)0.00946 (17)
S30.06842 (5)0.65210 (12)0.04226 (9)0.01100 (18)
S40.15039 (5)0.39868 (12)0.15905 (9)0.01027 (18)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La10.00974 (11)0.00804 (11)0.00825 (11)0.00132 (7)0.00092 (7)0.00064 (8)
La20.00740 (13)0.01163 (16)0.01343 (16)0.0000.00126 (10)0.000
I0.01317 (17)0.01203 (19)0.0432 (3)0.0000.01081 (15)0.000
Si0.0079 (4)0.0079 (5)0.0071 (4)0.0007 (3)0.0004 (3)0.0003 (4)
S10.0114 (4)0.0093 (4)0.0122 (4)0.0015 (3)0.0030 (3)0.0032 (3)
S20.0090 (4)0.0108 (4)0.0083 (4)0.0019 (3)0.0002 (3)0.0007 (3)
S30.0087 (4)0.0103 (4)0.0134 (5)0.0005 (3)0.0008 (3)0.0023 (3)
S40.0105 (4)0.0117 (4)0.0083 (4)0.0015 (3)0.0001 (3)0.0016 (3)
Geometric parameters (Å, º) top
La1—S2i2.9467 (10)La2—S1i2.9747 (10)
La1—S4ii2.9828 (10)La2—S1viii2.9747 (11)
La1—S3iii2.9885 (11)La2—S3vii3.2640 (12)
La1—S2iv3.0006 (11)La2—S3iv3.2640 (12)
La1—S4iv3.0580 (10)La2—S3viii3.2988 (11)
La1—S2iii3.0614 (10)La2—S3i3.2988 (11)
La1—S1v3.1009 (10)La2—Iix3.3335 (7)
La1—S1i3.1213 (12)Si—S12.1048 (14)
La1—Ivi3.4571 (7)Si—S42.1070 (14)
La2—S4iv2.9328 (10)Si—S32.1189 (14)
La2—S4vii2.9328 (10)Si—S22.1322 (13)
S2i—La1—S4ii82.70 (3)S1i—La2—S3viii148.27 (3)
S2i—La1—S3iii137.70 (3)S1viii—La2—S3viii67.52 (3)
S4ii—La1—S3iii68.78 (3)S3vii—La2—S3viii131.03 (3)
S2i—La1—S2iv139.152 (17)S3iv—La2—S3viii60.56 (3)
S4ii—La1—S2iv138.01 (3)S4iv—La2—S3i65.22 (3)
S3iii—La1—S2iv76.28 (3)S4vii—La2—S3i78.00 (3)
S2i—La1—S4iv76.69 (3)S1i—La2—S3i67.52 (3)
S4ii—La1—S4iv137.469 (19)S1viii—La2—S3i148.27 (3)
S3iii—La1—S4iv144.72 (3)S3vii—La2—S3i60.56 (3)
S2iv—La1—S4iv69.09 (3)S3iv—La2—S3i131.03 (3)
S2i—La1—S2iii133.92 (2)S3viii—La2—S3i107.35 (4)
S4ii—La1—S2iii76.11 (3)S4iv—La2—Iix121.95 (2)
S3iii—La1—S2iii69.48 (3)S4vii—La2—Iix121.95 (2)
S2iv—La1—S2iii70.24 (3)S1i—La2—Iix66.72 (2)
S4iv—La1—S2iii92.08 (3)S1viii—La2—Iix66.722 (19)
S2i—La1—S1v67.37 (3)S3vii—La2—Iix81.997 (18)
S4ii—La1—S1v134.20 (3)S3iv—La2—Iix81.997 (18)
S3iii—La1—S1v111.55 (3)S3viii—La2—Iix126.324 (19)
S2iv—La1—S1v79.90 (3)S3i—La2—Iix126.324 (19)
S4iv—La1—S1v69.34 (3)La2ix—I—La1vi103.750 (8)
S2iii—La1—S1v149.10 (3)La2ix—I—La1x103.750 (8)
S2i—La1—S1i68.65 (3)La1vi—I—La1x152.500 (16)
S4ii—La1—S1i70.02 (3)S1—Si—S4114.19 (6)
S3iii—La1—S1i124.48 (3)S1—Si—S3111.76 (6)
S2iv—La1—S1i115.44 (3)S4—Si—S3106.16 (6)
S4iv—La1—S1i67.91 (3)S1—Si—S2107.85 (5)
S2iii—La1—S1i65.76 (3)S4—Si—S2108.30 (6)
S1v—La1—S1i123.78 (2)S3—Si—S2108.42 (6)
S2i—La1—Ivi72.26 (3)Si—S1—La2i94.90 (4)
S4ii—La1—Ivi74.64 (2)Si—S1—La1xi139.87 (5)
S3iii—La1—Ivi70.48 (2)La2i—S1—La1xi123.11 (3)
S2iv—La1—Ivi114.93 (3)Si—S1—La1i88.59 (4)
S4iv—La1—Ivi130.80 (2)La2i—S1—La1i105.33 (3)
S2iii—La1—Ivi136.692 (19)La1xi—S1—La1i92.68 (3)
S1v—La1—Ivi63.866 (18)Si—S2—La1i92.83 (5)
S1i—La1—Ivi129.58 (2)Si—S2—La1xii90.31 (4)
S4iv—La2—S4vii116.10 (4)La1i—S2—La1xii153.07 (4)
S4iv—La2—S1i71.50 (3)Si—S2—La1x89.19 (4)
S4vii—La2—S1i137.35 (3)La1i—S2—La1x97.03 (3)
S4iv—La2—S1viii137.35 (3)La1xii—S2—La1x109.76 (3)
S4vii—La2—S1viii71.50 (3)Si—S3—La1x91.41 (4)
S1i—La2—S1viii133.44 (4)Si—S3—La2xiii88.88 (4)
S4iv—La2—S3vii123.84 (3)La1x—S3—La2xiii133.89 (4)
S4vii—La2—S3vii65.83 (3)Si—S3—La2i85.80 (4)
S1i—La2—S3vii75.49 (3)La1x—S3—La2i106.55 (3)
S1viii—La2—S3vii98.08 (3)La2xiii—S3—La2i119.44 (3)
S4iv—La2—S3iv65.83 (3)Si—S4—La2xiii98.52 (5)
S4vii—La2—S3iv123.84 (3)Si—S4—La1xiv139.93 (5)
S1i—La2—S3iv98.08 (3)La2xiii—S4—La1xiv116.96 (3)
S1viii—La2—S3iv75.49 (3)Si—S4—La1xii89.23 (4)
S3vii—La2—S3iv163.99 (4)La2xiii—S4—La1xii108.02 (3)
S4iv—La2—S3viii78.00 (3)La1xiv—S4—La1xii96.34 (3)
S4vii—La2—S3viii65.22 (3)
Symmetry codes: (i) x+1/2, y+1/2, z+1; (ii) x, y, z+1; (iii) x, y+1, z+1/2; (iv) x+1/2, y1/2, z+1/2; (v) x, y, z+1/2; (vi) x, y+1, z+1; (vii) x+1/2, y1/2, z+1; (viii) x+1/2, y+1/2, z+1/2; (ix) x+1/2, y+3/2, z+1; (x) x, y+1, z1/2; (xi) x, y, z1/2; (xii) x+1/2, y+1/2, z+1/2; (xiii) x1/2, y+1/2, z1; (xiv) x, y, z1.
 

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