Download citation
Download citation
link to html
The structure of praseodymium germanium sulfide, Pr4Ge3S12, has been determined in the course of the determination of the amount of contamination of the title compound by the starting products. Its structure was assumed to be isostructural with the structure of La4Ge3S12. One Pr atom lies on a threefold axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803015162/br6102sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803015162/br6102Isup2.hkl
Contains datablock I

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S1600536803015162/br6102Isup3.rtv
Contains datablock I

Key indicators

  • Powder synchrotron study
  • T = 293 K
  • Mean [sigma](Ge-S) = 0.009 Å
  • R factor = 0.000
  • wR factor = 0.000
  • Data-to-parameter ratio = 0.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
REFI_001 Alert A _refine_ls_structure_factor_coef is missing The structure factor coefficient should be one of the following * Inet * Fsqd * F The following tests will not be performed FCOEF_01 WEIGH_01 Alert A The weighting scheme should be one of the following * sigma * calc Weighting scheme given as \s
Yellow Alert Alert Level C:
GOODF_01 Alert C The least squares goodness of fit parameter lies outside the range 0.80 <> 2.00 Goodness of fit given = 3.500 General Notes
ABSMU_01 Radiation type not identified. Calculation of _exptl_absorpt_correction_mu not performed.
2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Cell refinement: LSPAID (Visser, 1986); data reduction: MRIA (Zlokazov & Chernysev, 1992); program(s) used to refine structure: GSAS (Larson & Von Dreele (1985-2000)); molecular graphics: ORTEPIII (Burnett & Johnson, 1996)); software used to prepare material for publication: VaList (Wills & Brown, 1999) and Xtal (Hall et al., 1995).

(I) top
Crystal data top
Pr4Ge3S12Dx = 4.52 Mg m3
Mr = 1166.18Synchrotron radiation, λ = 0.65296 Å
Trigonal, R3cµ = 12.86 mm1
Hall symbol: R 3 -2"CT = 293 K
a = 19.2856 (1) Ågreen
c = 7.98049 (3) Åcylinder, × 0.3 mm
V = 2570.55 (2) Å3Specimen preparation: Prepared at 1273 K and 0.05(5) kPa
Z = 6
Data collection top
ESRF BM16
diffractometer
Scan method: continuous
Radiation source: synchrotronAbsorption correction: for a cylinder mounted on the φ axis
Si(111) monochromatorTmin = 0.012, Tmax = 0.023
Specimen mounting: glass capillary2θmin = 3.0°, 2θmax = 40.0°, 2θstep = 0.002°
Data collection mode: transmission
Refinement top
Rp = 0.08463 parameters
Rwp = 0.1080 restraints
Rexp = 0.0312 constraints
18500 data pointsσ
Excluded region(s): The following 12 excluded regions were introduced because some contamination is present. 8.532 - 8.768, 9.682 - 9.750, 10.856 - 10.990, 11.198 - 11.268, 11.992 - 12.216, 13.134 - 13.196, 14.256 - 14.372, 14.952 - 15.094, 15.768 - 15.910, 17.294 - 17.440, 20.016 - 20.154, 21.064 - 21.952Background function: polynomial
Profile function: pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pr10.0000 (1)0.0000 (1)0.0000 (1)0.0233 (5)*
Pr20.0038 (1)0.2316 (1)0.2033 (4)0.0233 (5)*
Ge0.1991 (2)0.1862 (2)0.1553 (5)0.0130 (10)*
S10.1536 (4)0.3788 (4)0.1601 (10)0.0253 (12)*
S20.1228 (4)0.0643 (5)0.2452 (8)0.0253 (12)*
S30.1177 (5)0.2032 (4)0.9923 (9)0.0253 (12)*
S40.3954 (4)0.0592 (4)0.1843 (10)0.0253 (12)*
Geometric parameters (Å, º) top
Pr1i—S2ii2.836 (7)Pr2i—S2ii2.932 (7)
Pr1i—S2i2.836 (7)Pr2i—S42.933 (8)
Pr1i—S2iii2.836 (7)Pr2i—S1iv2.976 (8)
Pr1i—S22.889 (7)Pr2i—S32.995 (8)
Pr1i—S22.889 (7)Pr2i—S33.028 (8)
Pr1i—S22.889 (7)Pr2i—S1v3.546 (8)
Pr1i—S33.409 (7)Pr2i—S4vi3.702 (8)
Pr1i—S33.409 (7)Geii—S2ii2.178 (9)
Pr1i—S33.409 (8)Geii—S32.186 (8)
Pr2i—S4ii2.830 (7)Geii—S1v2.196 (8)
Pr2i—S1i2.884 (7)Geii—S4vii2.203 (8)
S2ii—Pr1i—S2i77.6 (3)S4ii—Pr2i—S1iv77.5 (2)
S2ii—Pr1i—S2iii77.6 (2)S4ii—Pr2i—S3128.6 (2)
S2ii—Pr1i—S288.4 (3)S4ii—Pr2i—S3135.1 (2)
S2ii—Pr1i—S2135.9 (2)S4ii—Pr2i—S1v79.3 (2)
S2ii—Pr1i—S2140.1 (2)S4ii—Pr2i—S4vi59.8 (2)
S2ii—Pr1i—S365.1 (2)S1i—Pr2i—S2ii142.4 (3)
S2ii—Pr1i—S374.2 (2)S1i—Pr2i—S477.4 (2)
S2ii—Pr1i—S3137.0 (2)S1i—Pr2i—S1iv128.7 (2)
S2i—Pr1i—S2iii77.6 (2)S1i—Pr2i—S385.0 (2)
S2i—Pr1i—S2135.9 (2)S1i—Pr2i—S369.6 (2)
S2i—Pr1i—S2140.1 (3)S1i—Pr2i—S1v141.0 (2)
S2i—Pr1i—S288.4 (2)S1i—Pr2i—S4vi61.4 (2)
S2i—Pr1i—S3137.0 (2)S2ii—Pr2i—S4110.7 (2)
S2i—Pr1i—S365.1 (2)S2ii—Pr2i—S1iv72.1 (2)
S2i—Pr1i—S374.2 (2)S2ii—Pr2i—S371.4 (2)
S2iii—Pr1i—S2140.1 (2)S2ii—Pr2i—S379.0 (2)
S2iii—Pr1i—S288.4 (2)S2ii—Pr2i—S1v63.9 (2)
S2iii—Pr1i—S2135.9 (3)S2ii—Pr2i—S4vi130.7 (2)
S2iii—Pr1i—S374.2 (2)S4—Pr2i—S1iv135.6 (2)
S2iii—Pr1i—S3136.97 (18)S4—Pr2i—S3151.8 (2)
S2iii—Pr1i—S365.1 (2)S4—Pr2i—S369.2 (2)
S2—Pr1i—S275.9 (3)S4—Pr2i—S1v64.14 (17)
S2—Pr1i—S275.9 (2)S4—Pr2i—S4vi117.8 (2)
S2—Pr1i—S366.03 (19)S1iv—Pr2i—S372.5 (2)
S2—Pr1i—S370.9 (2)S1iv—Pr2i—S3147.3 (3)
S2—Pr1i—S3134.1 (2)S1iv—Pr2i—S1v80.17 (19)
S2—Pr1i—S275.9 (2)S1iv—Pr2i—S4vi67.64 (17)
S2—Pr1i—S370.9 (2)S3—Pr2i—S384.2 (2)
S2—Pr1i—S3134.13 (18)S3—Pr2i—S1v132.90 (18)
S2—Pr1i—S366.0 (2)S3—Pr2i—S4vi70.4 (2)
S2—Pr1i—S3134.1 (2)S3—Pr2i—S1v100.8 (2)
S2—Pr1i—S366.0 (2)S3—Pr2i—S4vi125.80 (18)
S2—Pr1i—S370.9 (2)S1v—Pr2i—S4vi131.8 (2)
S3—Pr1i—S3120.0 (2)S2ii—Geii—S3102.1 (4)
S3—Pr1i—S3119.97 (18)S2ii—Geii—S1v105.0 (3)
S3—Pr1i—S3120.0 (2)S2ii—Geii—S4vii114.1 (3)
S4ii—Pr2i—S1i82.4 (2)S3—Geii—S1v107.3 (3)
S4ii—Pr2i—S2ii135.2 (2)S3—Geii—S4vii124.2 (3)
S4ii—Pr2i—S470.9 (2)S1v—Geii—S4vii102.7 (4)
Symmetry codes: (i) x+2/3, y+1/3, z+1/3; (ii) y+2/3, xy+1/3, z+1/3; (iii) x+y+2/3, x+1/3, z+1/3; (iv) x+y+1/3, x+2/3, z+2/3; (v) x+1/3, xy+2/3, z+1/6; (vi) x+1/3, y+2/3, z+2/3; (vii) x, xy, z+1/2.
Full Pattern Decomposition results for different models top
ABCD
Rp0.0940.0730.0750.097
Rwp0.1490.0940.1000.157
GOF5.53.53.96.1
2θ range 3–23°; A : only 1 phase (Pr4Ge3S12); B : 1 phase (Pr4Ge3S12 + 12 excluded regions); C : 2 phases (Pr4Ge3S12 + GeS2(HT)); D : 2 phases (Pr4Ge3S12 + Pr2S3)
Rietveld Refinement results for different models top
ABCD
Rp0.0990.0840.0990.100
Rwp0.1480.1080.1470.148
GOF4.83.54.84.8
Pr4Ge3S12(%)100.0100.097.998.6
GeS2/Pr2S3(%)--0.8.0
2θ range 3–40°; A : only 1 phase (Pr4Ge3S12); B : 1 phase (Pr4Ge3S12 + 12 excluded regions); C : 2 phases (Pr4Ge3S12 + GeS2(HT)); D : 2 phases (Pr4Ge3S12 + Pr2S3)
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds