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
Key indicators
- Powder synchrotron study
- T = 293 K
- Mean (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
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
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
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).
Crystal data top
Pr4Ge3S12 | Dx = 4.52 Mg m−3 |
Mr = 1166.18 | Synchrotron radiation, λ = 0.65296 Å |
Trigonal, R3c | µ = 12.86 mm−1 |
Hall symbol: R 3 -2"C | T = 293 K |
a = 19.2856 (1) Å | green |
c = 7.98049 (3) Å | cylinder, × 0.3 mm |
V = 2570.55 (2) Å3 | Specimen preparation: Prepared at 1273 K and 0.05(5) kPa |
Z = 6 | |
Data collection top
ESRF BM16 diffractometer | Scan method: continuous |
Radiation source: synchrotron | Absorption correction: for a cylinder mounted on the φ axis |
Si(111) monochromator | Tmin = 0.012, Tmax = 0.023 |
Specimen mounting: glass capillary | 2θmin = 3.0°, 2θmax = 40.0°, 2θstep = 0.002° |
Data collection mode: transmission | |
Refinement top
Rp = 0.084 | 63 parameters |
Rwp = 0.108 | 0 restraints |
Rexp = 0.031 | 2 constraints |
18500 data points | σ |
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 - 21.952 | Background function: polynomial |
Profile function: pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pr1 | 0.0000 (1) | 0.0000 (1) | 0.0000 (1) | 0.0233 (5)* | |
Pr2 | 0.0038 (1) | 0.2316 (1) | 0.2033 (4) | 0.0233 (5)* | |
Ge | 0.1991 (2) | 0.1862 (2) | 0.1553 (5) | 0.0130 (10)* | |
S1 | 0.1536 (4) | 0.3788 (4) | 0.1601 (10) | 0.0253 (12)* | |
S2 | 0.1228 (4) | 0.0643 (5) | 0.2452 (8) | 0.0253 (12)* | |
S3 | 0.1177 (5) | 0.2032 (4) | 0.9923 (9) | 0.0253 (12)* | |
S4 | 0.3954 (4) | 0.0592 (4) | 0.1843 (10) | 0.0253 (12)* | |
Geometric parameters (Å, º) top
Pr1i—S2ii | 2.836 (7) | Pr2i—S2ii | 2.932 (7) |
Pr1i—S2i | 2.836 (7) | Pr2i—S4 | 2.933 (8) |
Pr1i—S2iii | 2.836 (7) | Pr2i—S1iv | 2.976 (8) |
Pr1i—S2 | 2.889 (7) | Pr2i—S3 | 2.995 (8) |
Pr1i—S2 | 2.889 (7) | Pr2i—S3 | 3.028 (8) |
Pr1i—S2 | 2.889 (7) | Pr2i—S1v | 3.546 (8) |
Pr1i—S3 | 3.409 (7) | Pr2i—S4vi | 3.702 (8) |
Pr1i—S3 | 3.409 (7) | Geii—S2ii | 2.178 (9) |
Pr1i—S3 | 3.409 (8) | Geii—S3 | 2.186 (8) |
Pr2i—S4ii | 2.830 (7) | Geii—S1v | 2.196 (8) |
Pr2i—S1i | 2.884 (7) | Geii—S4vii | 2.203 (8) |
| | | |
S2ii—Pr1i—S2i | 77.6 (3) | S4ii—Pr2i—S1iv | 77.5 (2) |
S2ii—Pr1i—S2iii | 77.6 (2) | S4ii—Pr2i—S3 | 128.6 (2) |
S2ii—Pr1i—S2 | 88.4 (3) | S4ii—Pr2i—S3 | 135.1 (2) |
S2ii—Pr1i—S2 | 135.9 (2) | S4ii—Pr2i—S1v | 79.3 (2) |
S2ii—Pr1i—S2 | 140.1 (2) | S4ii—Pr2i—S4vi | 59.8 (2) |
S2ii—Pr1i—S3 | 65.1 (2) | S1i—Pr2i—S2ii | 142.4 (3) |
S2ii—Pr1i—S3 | 74.2 (2) | S1i—Pr2i—S4 | 77.4 (2) |
S2ii—Pr1i—S3 | 137.0 (2) | S1i—Pr2i—S1iv | 128.7 (2) |
S2i—Pr1i—S2iii | 77.6 (2) | S1i—Pr2i—S3 | 85.0 (2) |
S2i—Pr1i—S2 | 135.9 (2) | S1i—Pr2i—S3 | 69.6 (2) |
S2i—Pr1i—S2 | 140.1 (3) | S1i—Pr2i—S1v | 141.0 (2) |
S2i—Pr1i—S2 | 88.4 (2) | S1i—Pr2i—S4vi | 61.4 (2) |
S2i—Pr1i—S3 | 137.0 (2) | S2ii—Pr2i—S4 | 110.7 (2) |
S2i—Pr1i—S3 | 65.1 (2) | S2ii—Pr2i—S1iv | 72.1 (2) |
S2i—Pr1i—S3 | 74.2 (2) | S2ii—Pr2i—S3 | 71.4 (2) |
S2iii—Pr1i—S2 | 140.1 (2) | S2ii—Pr2i—S3 | 79.0 (2) |
S2iii—Pr1i—S2 | 88.4 (2) | S2ii—Pr2i—S1v | 63.9 (2) |
S2iii—Pr1i—S2 | 135.9 (3) | S2ii—Pr2i—S4vi | 130.7 (2) |
S2iii—Pr1i—S3 | 74.2 (2) | S4—Pr2i—S1iv | 135.6 (2) |
S2iii—Pr1i—S3 | 136.97 (18) | S4—Pr2i—S3 | 151.8 (2) |
S2iii—Pr1i—S3 | 65.1 (2) | S4—Pr2i—S3 | 69.2 (2) |
S2—Pr1i—S2 | 75.9 (3) | S4—Pr2i—S1v | 64.14 (17) |
S2—Pr1i—S2 | 75.9 (2) | S4—Pr2i—S4vi | 117.8 (2) |
S2—Pr1i—S3 | 66.03 (19) | S1iv—Pr2i—S3 | 72.5 (2) |
S2—Pr1i—S3 | 70.9 (2) | S1iv—Pr2i—S3 | 147.3 (3) |
S2—Pr1i—S3 | 134.1 (2) | S1iv—Pr2i—S1v | 80.17 (19) |
S2—Pr1i—S2 | 75.9 (2) | S1iv—Pr2i—S4vi | 67.64 (17) |
S2—Pr1i—S3 | 70.9 (2) | S3—Pr2i—S3 | 84.2 (2) |
S2—Pr1i—S3 | 134.13 (18) | S3—Pr2i—S1v | 132.90 (18) |
S2—Pr1i—S3 | 66.0 (2) | S3—Pr2i—S4vi | 70.4 (2) |
S2—Pr1i—S3 | 134.1 (2) | S3—Pr2i—S1v | 100.8 (2) |
S2—Pr1i—S3 | 66.0 (2) | S3—Pr2i—S4vi | 125.80 (18) |
S2—Pr1i—S3 | 70.9 (2) | S1v—Pr2i—S4vi | 131.8 (2) |
S3—Pr1i—S3 | 120.0 (2) | S2ii—Geii—S3 | 102.1 (4) |
S3—Pr1i—S3 | 119.97 (18) | S2ii—Geii—S1v | 105.0 (3) |
S3—Pr1i—S3 | 120.0 (2) | S2ii—Geii—S4vii | 114.1 (3) |
S4ii—Pr2i—S1i | 82.4 (2) | S3—Geii—S1v | 107.3 (3) |
S4ii—Pr2i—S2ii | 135.2 (2) | S3—Geii—S4vii | 124.2 (3) |
S4ii—Pr2i—S4 | 70.9 (2) | S1v—Geii—S4vii | 102.7 (4) |
Symmetry codes: (i) x+2/3, y+1/3, z+1/3; (ii) −y+2/3, x−y+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, x−y+2/3, z+1/6; (vi) x+1/3, y+2/3, z+2/3; (vii) x, x−y, z+1/2. |
Full Pattern Decomposition results for different models top | A | B | C | D |
Rp | 0.094 | 0.073 | 0.075 | 0.097 |
Rwp | 0.149 | 0.094 | 0.100 | 0.157 |
GOF | 5.5 | 3.5 | 3.9 | 6.1 |
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 | A | B | C | D |
Rp | 0.099 | 0.084 | 0.099 | 0.100 |
Rwp | 0.148 | 0.108 | 0.147 | 0.148 |
GOF | 4.8 | 3.5 | 4.8 | 4.8 |
Pr4Ge3S12(%) | 100.0 | 100.0 | 97.9 | 98.6 |
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) |