The title structures of KScS2 (potassium scandium sulfide), RbScS2 (rubidium scandium sulfide) and KLnS2 [Ln = Nd (potassium neodymium sufide), Sm (potassium samarium sulfide), Tb (potassium terbium sulfide), Dy (potassium dysprosium sulfide), Ho (potassium holmium sulfide), Er (potassium erbium sulfide), Tm (potassium thulium sulfide) and Yb (potassium ytterbium sulfide)] are either newly determined (KScS2, RbScS2 and KTbS2) or redetermined. All of them belong to the α-NaFeO2 structure type in agreement with the ratio of the ionic radii r3+/r+. KScS2, the member of this structural family with the smallest trivalent cation, is an extreme representative of these structures with rare earth trivalent cations. The title structures are compared with isostructural alkali rare earth sulfides in plots showing the dependence of several relevant parameters on the trivalent cation crystal radius; the parameters thus compared are c, a and c/a, the thicknesses of the S—S layers which contain the respective constituent cations, the sulfur fractional coordinates z(S2−) and the bond-valence sums.
Supporting information
| Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229615011833/fa3364sup1.cif Contains datablocks global, I, II, III, IV, V, VI, VII, VIII, IX, X |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364Isup2.hkl Contains datablock I |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364IIsup3.hkl Contains datablock II |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364IIIsup4.hkl Contains datablock III |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364IVsup5.hkl Contains datablock IV |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364Vsup6.hkl Contains datablock V |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364VIsup7.hkl Contains datablock VI |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364VIIsup8.hkl Contains datablock VII |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364VIIIsup9.hkl Contains datablock VIII |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364IXsup10.hkl Contains datablock IX |
| Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011833/fa3364Xsup11.hkl Contains datablock X |
| Portable Document Format (PDF) file https://doi.org/10.1107/S2053229615011833/fa3364sup12.pdf Overview of known determinations |
| Portable Document Format (PDF) file https://doi.org/10.1107/S2053229615011833/fa3364sup13.pdf Extra tables |
| Portable Document Format (PDF) file https://doi.org/10.1107/S2053229615011833/fa3364sup14.pdf Extra figures |
CCDC references: 1407927; 1407926; 1407925; 1407924; 1407923; 1407922; 1407921; 1407920; 1407919; 1407918
For all compounds, data collection: CrysAlis PRO (Agilent, 2014); cell refinement: CrysAlis PRO (Agilent, 2014); data reduction: CrysAlis PRO (Agilent, 2014); program(s) used to solve structure: SUPERFLIP (Palatinus & Chapuis, 2007); program(s) used to refine structure: JANA2006 (Petříček et al., 2014). Molecular graphics: Brandenburg & Putz (2005) for (II). For all compounds, software used to prepare material for publication: JANA2006 (Petříček et al., 2014).
(I) Potassium scandium sulfide
top
Crystal data top
KScS2 | Dx = 2.703 Mg m−3 |
Mr = 148.2 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 936 reflections |
Hall symbol: -R 3 2" | θ = 5.6–28.8° |
a = 3.8106 (3) Å | µ = 4.04 mm−1 |
c = 21.719 (2) Å | T = 292 K |
V = 273.12 (4) Å3 | Plate, yellow |
Z = 3 | 0.46 × 0.27 × 0.05 mm |
F(000) = 216 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 119 independent reflections |
Radiation source: X-ray tube | 106 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.052 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 29.2°, θmin = 5.6° |
ω scans | h = −5→5 |
Absorption correction: gaussian JANA2006 (Petříček et al., 2014) | k = −5→5 |
Tmin = 0.347, Tmax = 0.832 | l = −28→29 |
1277 measured reflections | |
Refinement top
Refinement on F2 | 0 restraints |
R[F > 3σ(F)] = 0.025 | 0 constraints |
wR(F) = 0.064 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
S = 1.92 | (Δ/σ)max = 0.002 |
119 reflections | Δρmax = 0.48 e Å−3 |
8 parameters | Δρmin = −0.53 e Å−3 |
Special details top
Refinement. Refinement of a model with obverse–reverse twinning turned out to be
insignificant. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K | 0 | 0 | 0 | 0.0124 (5) | |
Sc | 0.333333 | 0.666667 | 0.166667 | 0.0062 (4) | |
S | 0 | 0 | 0.23113 (6) | 0.0067 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.0139 (6) | 0.0139 (6) | 0.0094 (9) | 0.0069 (3) | 0 | 0 |
Sc | 0.0058 (5) | 0.0058 (5) | 0.0068 (7) | 0.0029 (2) | 0 | 0 |
S | 0.0066 (4) | 0.0066 (4) | 0.0068 (7) | 0.0033 (2) | 0 | 0 |
Geometric parameters (Å, º) top
K—Ki | 3.8106 (9) | Sc—Scvi | 3.8106 (9) |
K—Kii | 3.8106 (6) | Sc—S | 2.6078 (8) |
K—Kiii | 3.8106 (6) | Sc—Siv | 2.6078 (8) |
K—Kiv | 3.8106 (6) | Sc—Svi | 2.6078 (8) |
K—Kv | 3.8106 (6) | Sc—Sxi | 2.6078 (8) |
K—Kvi | 3.8106 (9) | Sc—Sxii | 2.6078 (8) |
K—Svii | 3.1253 (11) | Sc—Sxiii | 2.6078 (8) |
K—Sviii | 3.1253 (10) | S—Si | 3.8106 (9) |
K—Six | 3.1253 (11) | S—Sii | 3.8106 (6) |
K—Sx | 3.1253 (11) | S—Siii | 3.8106 (6) |
K—Sxi | 3.1253 (10) | S—Siv | 3.8106 (6) |
K—Sxii | 3.1253 (11) | S—Sv | 3.8106 (6) |
Sc—Sci | 3.8106 (9) | S—Svi | 3.8106 (9) |
Sc—Scii | 3.8106 (6) | S—Sx | 3.5611 (16) |
Sc—Sciii | 3.8106 (6) | S—Sxi | 3.5611 (16) |
Sc—Sciv | 3.8106 (6) | S—Sxii | 3.5611 (16) |
Sc—Scv | 3.8106 (6) | | |
| | | |
S—Sc—Siv | 93.88 (2) | Svi—Sc—Sxiii | 86.12 (3) |
S—Sc—Svi | 93.88 (3) | Sxi—Sc—Sxii | 93.88 (2) |
S—Sc—Sxi | 86.12 (3) | Sxi—Sc—Sxiii | 93.88 (3) |
S—Sc—Sxii | 86.12 (2) | Sxii—Sc—Sxiii | 93.88 (2) |
S—Sc—Sxiii | 180.0 (5) | Kxiv—S—Kxv | 75.13 (3) |
Siv—Sc—Svi | 93.88 (2) | Kxiv—S—Kxvi | 75.13 (3) |
Siv—Sc—Sxi | 86.12 (2) | Kxv—S—Kxvi | 75.13 (3) |
Siv—Sc—Sxii | 180.0 (5) | Sci—S—Sciii | 93.88 (3) |
Siv—Sc—Sxiii | 86.12 (2) | Sci—S—Sc | 93.88 (3) |
Svi—Sc—Sxi | 180.0 (5) | Sciii—S—Sc | 93.88 (3) |
Svi—Sc—Sxii | 86.12 (2) | | |
Symmetry codes: (i) x−1, y−1, z; (ii) x−1, y, z; (iii) x, y−1, z; (iv) x, y+1, z; (v) x+1, y, z; (vi) x+1, y+1, z; (vii) x−2/3, y−1/3, z−1/3; (viii) x+1/3, y−1/3, z−1/3; (ix) x+1/3, y+2/3, z−1/3; (x) y−1/3, x−2/3, −z+1/3; (xi) y−1/3, x+1/3, −z+1/3; (xii) y+2/3, x+1/3, −z+1/3; (xiii) y+2/3, x+4/3, −z+1/3; (xiv) x−1/3, y−2/3, z+1/3; (xv) x−1/3, y+1/3, z+1/3; (xvi) x+2/3, y+1/3, z+1/3. |
(II) Rubidium scandium sulfide
top
Crystal data top
RbScS2 | Dx = 3.367 Mg m−3 |
Mr = 194.5 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 539 reflections |
Hall symbol: -R 3 2" | θ = 5.4–28.9° |
a = 3.8299 (6) Å | µ = 15.35 mm−1 |
c = 22.656 (3) Å | T = 293 K |
V = 287.80 (7) Å3 | Plate, yellow–green |
Z = 3 | 0.17 × 0.14 × 0.04 mm |
F(000) = 270 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 120 independent reflections |
Radiation source: X-ray tube | 118 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.069 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 28.9°, θmin = 5.4° |
ω scans | h = −5→3 |
Absorption correction: gaussian JANA2006 (Petříček et al., 2014) | k = −3→5 |
Tmin = 0.173, Tmax = 0.609 | l = −25→30 |
611 measured reflections | |
Refinement top
Refinement on F2 | 0 restraints |
R[F > 3σ(F)] = 0.033 | 0 constraints |
wR(F) = 0.068 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
S = 1.86 | (Δ/σ)max = 0.004 |
120 reflections | Δρmax = 0.82 e Å−3 |
8 parameters | Δρmin = −0.97 e Å−3 |
Special details top
Refinement. Refinement of a model with obverse–reverse twinning turned out to be
insignificant. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Rb | 0 | 0 | 0 | 0.0145 (4) | |
Sc | 0.333333 | 0.666667 | 0.166667 | 0.0070 (6) | |
S | 0 | 0 | 0.22811 (10) | 0.0073 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rb | 0.0155 (5) | 0.0155 (5) | 0.0125 (7) | 0.0078 (2) | 0 | 0 |
Sc | 0.0065 (6) | 0.0065 (6) | 0.0080 (11) | 0.0032 (3) | 0 | 0 |
S | 0.0072 (6) | 0.0072 (6) | 0.0075 (10) | 0.0036 (3) | 0 | 0 |
Geometric parameters (Å, º) top
Rb—Si | 3.2515 (18) | Sc—Six | 2.6129 (14) |
Rb—Sii | 3.2515 (17) | S—Sx | 3.8299 (18) |
Rb—Siii | 3.2515 (18) | S—Sxi | 3.8299 (12) |
Rb—Siv | 3.2515 (18) | S—Sxii | 3.8299 (12) |
Rb—Sv | 3.2515 (17) | S—Svii | 3.8299 (12) |
Rb—Svi | 3.2515 (18) | S—Sxiii | 3.8299 (12) |
Sc—S | 2.6129 (14) | S—Sviii | 3.8299 (18) |
Sc—Svii | 2.6129 (12) | S—Siv | 3.555 (3) |
Sc—Sviii | 2.6129 (14) | S—Sv | 3.555 (3) |
Sc—Sv | 2.6129 (14) | S—Svi | 3.555 (3) |
Sc—Svi | 2.6129 (12) | | |
| | | |
Si—Rb—Sii | 72.16 (3) | S—Sc—Svi | 85.74 (4) |
Si—Rb—Siii | 72.16 (3) | S—Sc—Six | 180.0 (5) |
Si—Rb—Siv | 107.84 (3) | Svii—Sc—Sviii | 94.26 (4) |
Si—Rb—Sv | 107.84 (3) | Svii—Sc—Sv | 85.74 (4) |
Si—Rb—Svi | 180.0 (5) | Svii—Sc—Svi | 180.0 (5) |
Sii—Rb—Siii | 72.16 (3) | Svii—Sc—Six | 85.74 (4) |
Sii—Rb—Siv | 107.84 (3) | Sviii—Sc—Sv | 180.0 (5) |
Sii—Rb—Sv | 180.0 (5) | Sviii—Sc—Svi | 85.74 (4) |
Sii—Rb—Svi | 107.84 (3) | Sviii—Sc—Six | 85.74 (4) |
Siii—Rb—Siv | 180.0 (5) | Sv—Sc—Svi | 94.26 (4) |
Siii—Rb—Sv | 107.84 (3) | Sv—Sc—Six | 94.26 (4) |
Siii—Rb—Svi | 107.84 (3) | Svi—Sc—Six | 94.26 (4) |
Siv—Rb—Sv | 72.16 (3) | Rbxiv—S—Rbxv | 72.16 (4) |
Siv—Rb—Svi | 72.16 (3) | Rbxiv—S—Rbxvi | 72.16 (4) |
Sv—Rb—Svi | 72.16 (3) | Rbxv—S—Rbxvi | 72.16 (4) |
S—Sc—Svii | 94.26 (4) | Scx—S—Scxii | 94.26 (6) |
S—Sc—Sviii | 94.26 (4) | Scx—S—Sc | 94.26 (6) |
S—Sc—Sv | 85.74 (4) | | |
Symmetry codes: (i) x−2/3, y−1/3, z−1/3; (ii) x+1/3, y−1/3, z−1/3; (iii) x+1/3, y+2/3, z−1/3; (iv) y−1/3, x−2/3, −z+1/3; (v) y−1/3, x+1/3, −z+1/3; (vi) y+2/3, x+1/3, −z+1/3; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) y+2/3, x+4/3, −z+1/3; (x) x−1, y−1, z; (xi) x−1, y, z; (xii) x, y−1, z; (xiii) x+1, y, z; (xiv) x−1/3, y−2/3, z+1/3; (xv) x−1/3, y+1/3, z+1/3; (xvi) x+2/3, y+1/3, z+1/3. |
(III) Potassium neodymium sufide
top
Crystal data top
KNdS2 | Dx = 3.75 Mg m−3 |
Mr = 247.5 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 1587 reflections |
Hall symbol: -R 3 2" | θ = 5.6–29.4° |
a = 4.1626 (3) Å | µ = 13.52 mm−1 |
c = 21.8996 (19) Å | T = 301 K |
V = 328.62 (5) Å3 | Plate, blue |
Z = 3 | 0.14 × 0.13 × 0.05 mm |
F(000) = 333 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 140 independent reflections |
Radiation source: X-ray tube | 140 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.036 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 29.5°, θmin = 5.6° |
w/2q scans | h = −5→5 |
Absorption correction: gaussian JANA2006 (Petříček et al., 2014) | k = −5→5 |
Tmin = 0.258, Tmax = 0.544 | l = −29→27 |
1538 measured reflections | |
Refinement top
Refinement on F2 | 0 constraints |
R[F > 3σ(F)] = 0.010 | Weighting scheme based on measured s.u.'s w = 1/[σ2(F) + 0.0001F2] |
wR(F) = 0.010 | (Δ/σ)max = 0.002 |
S = 0.60 | Δρmax = 0.17 e Å−3 |
140 reflections | Δρmin = −0.09 e Å−3 |
9 parameters | Extinction correction: B-C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147] |
0 restraints | Extinction coefficient: 160 (40) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K | 0 | 0 | 0 | 0.0150 (3) | |
Nd | 0.333333 | 0.666667 | 0.166667 | 0.00774 (10) | |
S | 0 | 0 | 0.23595 (4) | 0.0088 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.0160 (3) | 0.0160 (3) | 0.0131 (5) | 0.00800 (17) | 0 | 0 |
Nd | 0.00639 (13) | 0.00639 (13) | 0.01047 (16) | 0.00320 (6) | 0 | 0 |
S | 0.0082 (2) | 0.0082 (2) | 0.0101 (4) | 0.00409 (13) | 0 | 0 |
Geometric parameters (Å, º) top
K—Si | 3.2132 (8) | Nd—Sviii | 2.8421 (7) |
K—Sii | 3.2132 (7) | Nd—Sv | 2.8421 (7) |
K—Siii | 3.2132 (8) | Nd—Svi | 2.8421 (5) |
K—Siv | 3.2132 (8) | Nd—Six | 2.8421 (7) |
K—Sv | 3.2132 (7) | S—Siv | 3.8708 (12) |
K—Svi | 3.2132 (8) | S—Sv | 3.8708 (11) |
Nd—S | 2.8421 (7) | S—Svi | 3.8708 (12) |
Nd—Svii | 2.8421 (5) | | |
| | | |
Si—K—Sii | 80.743 (14) | Svii—Nd—Sviii | 94.161 (16) |
Si—K—Siii | 80.743 (16) | Svii—Nd—Sv | 85.839 (16) |
Si—K—Siv | 99.257 (16) | Svii—Nd—Svi | 180 |
Si—K—Sv | 99.257 (14) | Svii—Nd—Six | 85.839 (16) |
Si—K—Svi | 180 | Sviii—Nd—Sv | 180 |
Sii—K—Siii | 80.743 (14) | Sviii—Nd—Svi | 85.839 (16) |
Sii—K—Siv | 99.257 (14) | Sviii—Nd—Six | 85.839 (17) |
Sii—K—Sv | 180 | Sv—Nd—Svi | 94.161 (16) |
Sii—K—Svi | 99.257 (14) | Sv—Nd—Six | 94.161 (17) |
Siii—K—Siv | 180 | Svi—Nd—Six | 94.161 (16) |
Siii—K—Sv | 99.257 (14) | Kx—S—Kxi | 80.743 (19) |
Siii—K—Svi | 99.257 (16) | Kx—S—Kxii | 80.74 (2) |
Siv—K—Sv | 80.743 (14) | Kxi—S—Kxii | 80.743 (19) |
Siv—K—Svi | 80.743 (16) | Kxi—S—Ndxiii | 92.183 (7) |
Sv—K—Svi | 80.743 (14) | Kxi—S—Ndxiv | 170.68 (3) |
S—Nd—Svii | 94.161 (16) | Kxi—S—Nd | 92.183 (7) |
S—Nd—Sviii | 94.161 (17) | Ndxiii—S—Ndxiv | 94.16 (2) |
S—Nd—Sv | 85.839 (17) | Ndxiii—S—Nd | 94.16 (2) |
S—Nd—Svi | 85.839 (16) | Ndxiv—S—Nd | 94.16 (2) |
S—Nd—Six | 180 | | |
Symmetry codes: (i) x−2/3, y−1/3, z−1/3; (ii) x+1/3, y−1/3, z−1/3; (iii) x+1/3, y+2/3, z−1/3; (iv) y−1/3, x−2/3, −z+1/3; (v) y−1/3, x+1/3, −z+1/3; (vi) y+2/3, x+1/3, −z+1/3; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) y+2/3, x+4/3, −z+1/3; (x) x−1/3, y−2/3, z+1/3; (xi) x−1/3, y+1/3, z+1/3; (xii) x+2/3, y+1/3, z+1/3; (xiii) x−1, y−1, z; (xiv) x, y−1, z. |
(IV) Potassium samarium sulfide
top
Crystal data top
KSmS2 | Dx = 3.931 Mg m−3 |
Mr = 253.6 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 646 reflections |
Hall symbol: -R 3 2" | θ = 5.6–28.9° |
a = 4.1174 (6) Å | µ = 15.42 mm−1 |
c = 21.888 (3) Å | T = 293 K |
V = 321.35 (8) Å3 | Plate, yellow |
Z = 3 | 0.20 × 0.14 × 0.03 mm |
F(000) = 339 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 135 independent reflections |
Radiation source: X-ray tube | 135 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.086 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 29.0°, θmin = 5.6° |
ω scans | h = −5→5 |
Absorption correction: gaussian JANA2006 (Petříček et al., 2014) | k = −4→5 |
Tmin = 0.227, Tmax = 0.672 | l = −28→25 |
721 measured reflections | |
Refinement top
Refinement on F2 | 0 constraints |
R[F > 3σ(F)] = 0.031 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
wR(F) = 0.069 | (Δ/σ)max = 0.001 |
S = 1.86 | Δρmax = 1.48 e Å−3 |
135 reflections | Δρmin = −1.79 e Å−3 |
9 parameters | Extinction correction: B-C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147] |
0 restraints | Extinction coefficient: 470 (150) |
Special details top
Refinement. Refinement of a model with obverse-reverse twinning turned out to be
insignificant. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K | 0 | 0 | 0 | 0.0153 (11) | |
Sm | 0.333333 | 0.666667 | 0.166667 | 0.0073 (4) | |
S | 0 | 0 | 0.23520 (16) | 0.0087 (8) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.0174 (13) | 0.0174 (13) | 0.011 (2) | 0.0087 (7) | 0 | 0 |
Sm | 0.0062 (5) | 0.0062 (5) | 0.0096 (6) | 0.0031 (2) | 0 | 0 |
S | 0.0092 (10) | 0.0092 (10) | 0.0076 (15) | 0.0046 (5) | 0 | 0 |
Geometric parameters (Å, º) top
K—Si | 3.204 (2) | Sm—S | 2.811 (2) |
K—Sii | 3.204 (2) | Sm—Svii | 2.8109 (18) |
K—Siii | 3.204 (2) | Sm—Sviii | 2.811 (2) |
K—Siv | 3.204 (2) | Sm—Sv | 2.811 (2) |
K—Sv | 3.204 (2) | Sm—Svi | 2.8109 (18) |
K—Svi | 3.204 (2) | Sm—Six | 2.811 (2) |
| | | |
Si—K—Sii | 79.97 (5) | S—Sm—Svi | 85.82 (6) |
Si—K—Siii | 79.97 (5) | S—Sm—Six | 180.0 (5) |
Si—K—Siv | 100.03 (5) | Svii—Sm—Sviii | 94.18 (6) |
Si—K—Sv | 100.03 (5) | Svii—Sm—Sv | 85.82 (6) |
Si—K—Svi | 180.0 (5) | Svii—Sm—Svi | 180.0 (5) |
Sii—K—Siii | 79.97 (5) | Svii—Sm—Six | 85.82 (6) |
Sii—K—Siv | 100.03 (5) | Sviii—Sm—Sv | 180.0 (5) |
Sii—K—Sv | 180.0 (5) | Sviii—Sm—Svi | 85.82 (6) |
Sii—K—Svi | 100.03 (5) | Sviii—Sm—Six | 85.82 (6) |
Siii—K—Siv | 180.0 (5) | Sv—Sm—Svi | 94.17 (6) |
Siii—K—Sv | 100.03 (5) | Sv—Sm—Six | 94.18 (6) |
Siii—K—Svi | 100.03 (5) | Svi—Sm—Six | 94.17 (6) |
Siv—K—Sv | 79.97 (5) | Kx—S—Kxi | 79.97 (7) |
Siv—K—Svi | 79.97 (5) | Kx—S—Kxii | 79.97 (7) |
Sv—K—Svi | 79.97 (5) | Kxi—S—Kxii | 79.97 (7) |
S—Sm—Svii | 94.18 (6) | Smxiii—S—Smxiv | 94.18 (8) |
S—Sm—Sviii | 94.18 (6) | Smxiii—S—Sm | 94.18 (8) |
S—Sm—Sv | 85.82 (6) | Smxiv—S—Sm | 94.18 (8) |
Symmetry codes: (i) x−2/3, y−1/3, z−1/3; (ii) x+1/3, y−1/3, z−1/3; (iii) x+1/3, y+2/3, z−1/3; (iv) y−1/3, x−2/3, −z+1/3; (v) y−1/3, x+1/3, −z+1/3; (vi) y+2/3, x+1/3, −z+1/3; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) y+2/3, x+4/3, −z+1/3; (x) x−1/3, y−2/3, z+1/3; (xi) x−1/3, y+1/3, z+1/3; (xii) x+2/3, y+1/3, z+1/3; (xiii) x−1, y−1, z; (xiv) x, y−1, z. |
(V) Potassium terbium sulfide
top
Crystal data top
KTbS2 | Dx = 4.196 Mg m−3 |
Mr = 262.1 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 597 reflections |
Hall symbol: -R 3 2" | θ = 5.6–28.7° |
a = 4.0523 (7) Å | µ = 18.81 mm−1 |
c = 21.885 (3) Å | T = 295 K |
V = 311.23 (9) Å3 | Prism, white |
Z = 3 | 0.20 × 0.08 × 0.05 mm |
F(000) = 348 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 129 independent reflections |
Radiation source: X-ray tube | 129 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.061 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 29.3°, θmin = 5.6° |
ω scans | h = −5→4 |
Absorption correction: gaussian JANA2006 (Petříček et al., 2014) | k = −5→5 |
Tmin = 0.238, Tmax = 0.447 | l = −26→27 |
674 measured reflections | |
Refinement top
Refinement on F2 | 0 constraints |
R[F > 3σ(F)] = 0.017 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
wR(F) = 0.035 | (Δ/σ)max = 0.003 |
S = 0.97 | Δρmax = 0.45 e Å−3 |
129 reflections | Δρmin = −0.64 e Å−3 |
9 parameters | Extinction correction: B-C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147] |
0 restraints | Extinction coefficient: 1570 (120) |
Special details top
Refinement. Refinement of a model with obverse–reverse twinning turned out to be
insignificant. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K | 0 | 0 | 0 | 0.0149 (6) | |
Tb | 0.333333 | 0.666667 | 0.166667 | 0.0076 (2) | |
S | 0 | 0 | 0.23463 (9) | 0.0086 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.0172 (7) | 0.0172 (7) | 0.0103 (11) | 0.0086 (4) | 0 | 0 |
Tb | 0.0067 (3) | 0.0067 (3) | 0.0094 (3) | 0.00334 (14) | 0 | 0 |
S | 0.0084 (5) | 0.0084 (5) | 0.0091 (8) | 0.0042 (3) | 0 | 0 |
Geometric parameters (Å, º) top
K—Si | 3.1844 (16) | Tb—S | 2.7723 (14) |
K—Sii | 3.1844 (14) | Tb—Svii | 2.7723 (11) |
K—Siii | 3.1844 (16) | Tb—Sviii | 2.7723 (14) |
K—Siv | 3.1844 (16) | Tb—Sv | 2.7723 (14) |
K—Sv | 3.1844 (14) | Tb—Svi | 2.7723 (11) |
K—Svi | 3.1844 (16) | Tb—Six | 2.7723 (14) |
| | | |
Si—K—Sii | 79.03 (3) | S—Tb—Svi | 86.08 (3) |
Si—K—Siii | 79.03 (3) | S—Tb—Six | 180.0 (5) |
Si—K—Siv | 100.97 (3) | Svii—Tb—Sviii | 93.92 (3) |
Si—K—Sv | 100.97 (3) | Svii—Tb—Sv | 86.08 (3) |
Si—K—Svi | 180.0 (5) | Svii—Tb—Svi | 180.0 (5) |
Sii—K—Siii | 79.03 (3) | Svii—Tb—Six | 86.08 (3) |
Sii—K—Siv | 100.97 (3) | Sviii—Tb—Sv | 180.0 (5) |
Sii—K—Sv | 180.0 (5) | Sviii—Tb—Svi | 86.08 (3) |
Sii—K—Svi | 100.97 (3) | Sviii—Tb—Six | 86.08 (4) |
Siii—K—Siv | 180.0 (5) | Sv—Tb—Svi | 93.92 (3) |
Siii—K—Sv | 100.97 (3) | Sv—Tb—Six | 93.92 (4) |
Siii—K—Svi | 100.97 (3) | Svi—Tb—Six | 93.92 (3) |
Siv—K—Sv | 79.03 (3) | Kx—S—Kxi | 79.03 (4) |
Siv—K—Svi | 79.03 (3) | Kx—S—Kxii | 79.03 (4) |
Sv—K—Svi | 79.03 (3) | Kxi—S—Kxii | 79.03 (4) |
S—Tb—Svii | 93.92 (3) | Tbxiii—S—Tbxiv | 93.92 (5) |
S—Tb—Sviii | 93.92 (4) | Tbxiii—S—Tb | 93.92 (5) |
S—Tb—Sv | 86.08 (4) | Tbxiv—S—Tb | 93.92 (5) |
Symmetry codes: (i) x−2/3, y−1/3, z−1/3; (ii) x+1/3, y−1/3, z−1/3; (iii) x+1/3, y+2/3, z−1/3; (iv) y−1/3, x−2/3, −z+1/3; (v) y−1/3, x+1/3, −z+1/3; (vi) y+2/3, x+1/3, −z+1/3; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) y+2/3, x+4/3, −z+1/3; (x) x−1/3, y−2/3, z+1/3; (xi) x−1/3, y+1/3, z+1/3; (xii) x+2/3, y+1/3, z+1/3; (xiii) x−1, y−1, z; (xiv) x, y−1, z. |
(VI) Potassium dysprosium sulfide
top
Crystal data top
KDyS2 | Dx = 4.296 Mg m−3 |
Mr = 265.7 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 386 reflections |
Hall symbol: -R 3 2" | θ = 5.9–28.6° |
a = 4.0315 (11) Å | µ = 19.97 mm−1 |
c = 21.890 (5) Å | T = 294 K |
V = 308.11 (14) Å3 | Block, white |
Z = 3 | 0.21 × 0.09 × 0.03 mm |
F(000) = 351 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 126 independent reflections |
Radiation source: X-ray tube | 124 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.100 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 29.3°, θmin = 5.6° |
ω scans | h = −5→4 |
Absorption correction: gaussian JANA2006 (Petříček et al., 2014) | k = −3→5 |
Tmin = 0.201, Tmax = 0.703 | l = −25→27 |
658 measured reflections | |
Refinement top
Refinement on F2 | 0 constraints |
R[F > 3σ(F)] = 0.052 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
wR(F) = 0.105 | (Δ/σ)max = 0.001 |
S = 2.32 | Δρmax = 4.44 e Å−3 |
126 reflections | Δρmin = −2.46 e Å−3 |
9 parameters | Extinction correction: B-C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147] |
0 restraints | Extinction coefficient: 1900 (400) |
Special details top
Refinement. A model with inclusion of obverse–reverse twinning turned out to be
insignificant. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K | 0 | 0 | 0 | 0.022 (3) | |
Dy | 0.333333 | 0.666667 | 0.166667 | 0.0137 (8) | |
S | 0 | 0 | 0.2345 (3) | 0.0138 (19) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.020 (3) | 0.020 (3) | 0.025 (5) | 0.0099 (14) | 0 | 0 |
Dy | 0.0106 (9) | 0.0106 (9) | 0.0199 (13) | 0.0053 (5) | 0 | 0 |
S | 0.011 (2) | 0.011 (2) | 0.019 (4) | 0.0057 (10) | 0 | 0 |
Geometric parameters (Å, º) top
K—Si | 3.179 (5) | Dy—Sviii | 2.760 (4) |
K—Sii | 3.179 (5) | Dy—Sv | 2.760 (4) |
K—Siii | 3.179 (5) | Dy—Svi | 2.760 (4) |
K—Siv | 3.179 (5) | Dy—Six | 2.760 (4) |
K—Sv | 3.179 (5) | S—Siv | 3.772 (8) |
K—Svi | 3.179 (5) | S—Sv | 3.772 (8) |
Dy—S | 2.760 (4) | S—Svi | 3.772 (8) |
Dy—Svii | 2.760 (4) | | |
| | | |
Si—K—Sii | 78.72 (11) | S—Dy—Svi | 86.18 (13) |
Si—K—Siii | 78.72 (11) | S—Dy—Six | 180.0 (5) |
Si—K—Siv | 101.28 (11) | Svii—Dy—Sviii | 93.82 (13) |
Si—K—Sv | 101.28 (11) | Svii—Dy—Sv | 86.18 (13) |
Si—K—Svi | 180.0 (5) | Svii—Dy—Svi | 180.0 (5) |
Sii—K—Siii | 78.72 (11) | Svii—Dy—Six | 86.18 (13) |
Sii—K—Siv | 101.28 (11) | Sviii—Dy—Sv | 180.0 (5) |
Sii—K—Sv | 180.0 (5) | Sviii—Dy—Svi | 86.18 (13) |
Sii—K—Svi | 101.28 (11) | Sviii—Dy—Six | 86.18 (13) |
Siii—K—Siv | 180.0 (5) | Sv—Dy—Svi | 93.82 (13) |
Siii—K—Sv | 101.28 (11) | Sv—Dy—Six | 93.82 (13) |
Siii—K—Svi | 101.28 (11) | Svi—Dy—Six | 93.82 (13) |
Siv—K—Sv | 78.72 (11) | Kx—S—Kxi | 78.72 (15) |
Siv—K—Svi | 78.72 (11) | Kx—S—Kxii | 78.72 (15) |
Sv—K—Svi | 78.72 (11) | Dyxiii—S—Dyxiv | 93.82 (18) |
S—Dy—Svii | 93.82 (13) | Dyxiii—S—Dy | 93.82 (18) |
S—Dy—Sviii | 93.82 (13) | Dyxiv—S—Dy | 93.82 (18) |
S—Dy—Sv | 86.18 (13) | | |
Symmetry codes: (i) x−2/3, y−1/3, z−1/3; (ii) x+1/3, y−1/3, z−1/3; (iii) x+1/3, y+2/3, z−1/3; (iv) y−1/3, x−2/3, −z+1/3; (v) y−1/3, x+1/3, −z+1/3; (vi) y+2/3, x+1/3, −z+1/3; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) y+2/3, x+4/3, −z+1/3; (x) x−1/3, y−2/3, z+1/3; (xi) x−1/3, y+1/3, z+1/3; (xii) x+2/3, y+1/3, z+1/3; (xiii) x−1, y−1, z; (xiv) x, y−1, z. |
(VII) Potassium holmium sulfide
top
Crystal data top
KHoS2 | Dx = 4.385 Mg m−3 |
Mr = 268.1 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 1327 reflections |
Hall symbol: -R 3 2" | θ = 5.6–28.8° |
a = 4.0098 (4) Å | µ = 21.29 mm−1 |
c = 21.878 (2) Å | T = 303 K |
V = 304.64 (5) Å3 | Prism, yellow |
Z = 3 | 0.19 × 0.14 × 0.07 mm |
F(000) = 354 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 216 independent reflections |
Radiation source: X-ray tube | 139 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.058 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 29.2°, θmin = 5.6° |
ω scans | h = −5→5 |
Absorption correction: gaussian JANA2006 (Petříček et al., 2014) | k = −5→5 |
Tmin = 0.090, Tmax = 0.243 | l = −29→29 |
2289 measured reflections | |
Refinement top
Refinement on F2 | 0 constraints |
R[F > 3σ(F)] = 0.020 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
wR(F) = 0.060 | (Δ/σ)max = 0.002 |
S = 1.56 | Δρmax = 0.77 e Å−3 |
216 reflections | Δρmin = −1.00 e Å−3 |
10 parameters | Extinction correction: B-C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147] |
0 restraints | Extinction coefficient: 1410 (130) |
Special details top
Refinement. Obverse–reverse twinning has been applied, with the twinning matrix
(-1 0 0 / 0 - 1 0 / 0 0 1).
The domain-state proportions are 0.99986 (3) and 0.00014 (3). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K | 0 | 0 | 0 | 0.0156 (8) | |
Ho | 0.333333 | 0.666667 | 0.166667 | 0.0077 (3) | |
S | 0 | 0 | 0.23430 (11) | 0.0091 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.0180 (10) | 0.0180 (10) | 0.0108 (13) | 0.0090 (5) | 0 | 0 |
Ho | 0.0078 (4) | 0.0078 (4) | 0.0074 (4) | 0.00390 (18) | 0 | 0 |
S | 0.0105 (7) | 0.0105 (7) | 0.0063 (10) | 0.0053 (4) | 0 | 0 |
Geometric parameters (Å, º) top
K—Si | 3.1708 (17) | Ho—S | 2.7475 (14) |
K—Sii | 3.1708 (17) | Ho—Svii | 2.7475 (13) |
K—Siii | 3.1708 (17) | Ho—Sviii | 2.7475 (14) |
K—Siv | 3.1708 (17) | Ho—Sv | 2.7475 (14) |
K—Sv | 3.1708 (17) | Ho—Svi | 2.7475 (13) |
K—Svi | 3.1708 (17) | Ho—Six | 2.7475 (14) |
| | | |
Si—K—Sii | 78.44 (3) | S—Ho—Svi | 86.28 (4) |
Si—K—Siii | 78.44 (4) | S—Ho—Six | 180.0 (5) |
Si—K—Siv | 101.56 (4) | Svii—Ho—Sviii | 93.73 (4) |
Si—K—Sv | 101.56 (3) | Svii—Ho—Sv | 86.28 (4) |
Si—K—Svi | 180.0 (5) | Svii—Ho—Svi | 180.0 (5) |
Sii—K—Siii | 78.44 (3) | Svii—Ho—Six | 86.28 (4) |
Sii—K—Siv | 101.56 (3) | Sviii—Ho—Sv | 180.0 (5) |
Sii—K—Sv | 180.0 (5) | Sviii—Ho—Svi | 86.28 (4) |
Sii—K—Svi | 101.56 (3) | Sviii—Ho—Six | 86.28 (4) |
Siii—K—Siv | 180.0 (5) | Sv—Ho—Svi | 93.72 (4) |
Siii—K—Sv | 101.56 (3) | Sv—Ho—Six | 93.72 (4) |
Siii—K—Svi | 101.56 (4) | Svi—Ho—Six | 93.72 (4) |
Siv—K—Sv | 78.44 (3) | Kx—S—Kxi | 78.44 (5) |
Siv—K—Svi | 78.44 (4) | Kx—S—Kxii | 78.44 (5) |
Sv—K—Svi | 78.44 (3) | Kxi—S—Kxii | 78.44 (5) |
S—Ho—Svii | 93.73 (4) | Hoxiii—S—Hoxiv | 93.73 (6) |
S—Ho—Sviii | 93.73 (4) | Hoxiii—S—Ho | 93.73 (6) |
S—Ho—Sv | 86.28 (4) | Hoxiv—S—Ho | 93.73 (6) |
Symmetry codes: (i) x−2/3, y−1/3, z−1/3; (ii) x+1/3, y−1/3, z−1/3; (iii) x+1/3, y+2/3, z−1/3; (iv) y−1/3, x−2/3, −z+1/3; (v) y−1/3, x+1/3, −z+1/3; (vi) y+2/3, x+1/3, −z+1/3; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) y+2/3, x+4/3, −z+1/3; (x) x−1/3, y−2/3, z+1/3; (xi) x−1/3, y+1/3, z+1/3; (xii) x+2/3, y+1/3, z+1/3; (xiii) x−1, y−1, z; (xiv) x, y−1, z. |
(VIII) Potassium erbium sulfide
top
Crystal data top
KErS2 | Dx = 4.462 Mg m−3 |
Mr = 270.5 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 1188 reflections |
Hall symbol: -R 3 2" | θ = 5.6–28.9° |
a = 3.9935 (4) Å | µ = 22.66 mm−1 |
c = 21.866 (2) Å | T = 296 K |
V = 302.00 (5) Å3 | Block, pink |
Z = 3 | 0.08 × 0.07 × 0.05 mm |
F(000) = 357 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 132 independent reflections |
Radiation source: X-ray tube | 132 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.070 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 29.1°, θmin = 2.8° |
ω scans | h = −5→5 |
Absorption correction: gaussian JANA2006 (Petříček et al., 2014) | k = −5→5 |
Tmin = 0.255, Tmax = 0.434 | l = −29→28 |
1405 measured reflections | |
Refinement top
Refinement on F2 | 0 constraints |
R[F > 3σ(F)] = 0.027 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
wR(F) = 0.064 | (Δ/σ)max = 0.001 |
S = 1.81 | Δρmax = 1.54 e Å−3 |
132 reflections | Δρmin = −1.01 e Å−3 |
9 parameters | Extinction correction: B-C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147] |
0 restraints | Extinction coefficient: 770 (160) |
Special details top
Refinement. The refinement of a model with obverse–reverse twinning turned out to be
insignificant |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K | 0 | 0 | 0 | 0.0144 (13) | |
Er | 0.333333 | 0.666667 | 0.166667 | 0.0074 (4) | |
S | 0 | 0 | 0.23407 (17) | 0.0078 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.0138 (14) | 0.0138 (14) | 0.015 (2) | 0.0069 (7) | 0 | 0 |
Er | 0.0058 (5) | 0.0058 (5) | 0.0105 (6) | 0.0029 (2) | 0 | 0 |
S | 0.0075 (11) | 0.0075 (11) | 0.0082 (17) | 0.0038 (5) | 0 | 0 |
Geometric parameters (Å, º) top
K—Si | 3.166 (3) | Er—Sviii | 2.737 (2) |
K—Sii | 3.166 (3) | Er—Sv | 2.737 (2) |
K—Siii | 3.166 (3) | Er—Svi | 2.737 (2) |
K—Siv | 3.166 (3) | Er—Six | 2.737 (2) |
K—Sv | 3.166 (3) | S—Siv | 3.742 (4) |
K—Svi | 3.166 (3) | S—Sv | 3.742 (4) |
Er—S | 2.737 (2) | S—Svi | 3.742 (4) |
Er—Svii | 2.737 (2) | | |
| | | |
Si—K—Sii | 78.19 (5) | S—Er—Svi | 86.28 (6) |
Si—K—Siii | 78.19 (5) | S—Er—Six | 180.0 (5) |
Si—K—Siv | 101.81 (5) | Svii—Er—Sviii | 93.72 (6) |
Si—K—Sv | 101.81 (5) | Svii—Er—Sv | 86.28 (6) |
Si—K—Svi | 180.0 (5) | Svii—Er—Svi | 180.0 (5) |
Sii—K—Siii | 78.19 (5) | Svii—Er—Six | 86.28 (6) |
Sii—K—Siv | 101.81 (5) | Sviii—Er—Sv | 180.0 (5) |
Sii—K—Sv | 180.0 (5) | Sviii—Er—Svi | 86.28 (6) |
Sii—K—Svi | 101.81 (5) | Sviii—Er—Six | 86.28 (6) |
Siii—K—Siv | 180.0 (5) | Sv—Er—Svi | 93.72 (6) |
Siii—K—Sv | 101.81 (5) | Sv—Er—Six | 93.72 (6) |
Siii—K—Svi | 101.81 (5) | Svi—Er—Six | 93.72 (6) |
Siv—K—Sv | 78.19 (5) | Kx—S—Kxi | 78.19 (8) |
Siv—K—Svi | 78.19 (5) | Kx—S—Kxii | 78.19 (8) |
Sv—K—Svi | 78.19 (5) | Kxi—S—Kxii | 78.19 (8) |
S—Er—Svii | 93.72 (6) | Erxiii—S—Erxiv | 93.72 (9) |
S—Er—Sviii | 93.72 (6) | Erxiii—S—Er | 93.72 (9) |
S—Er—Sv | 86.28 (6) | Erxiv—S—Er | 93.72 (9) |
Symmetry codes: (i) x−2/3, y−1/3, z−1/3; (ii) x+1/3, y−1/3, z−1/3; (iii) x+1/3, y+2/3, z−1/3; (iv) y−1/3, x−2/3, −z+1/3; (v) y−1/3, x+1/3, −z+1/3; (vi) y+2/3, x+1/3, −z+1/3; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) y+2/3, x+4/3, −z+1/3; (x) x−1/3, y−2/3, z+1/3; (xi) x−1/3, y+1/3, z+1/3; (xii) x+2/3, y+1/3, z+1/3; (xiii) x−1, y−1, z; (xiv) x, y−1, z. |
(IX) Potassium thulium sulfide
top
Crystal data top
KTmS2 | Dx = 4.534 Mg m−3 |
Mr = 272.2 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 595 reflections |
Hall symbol: -R 3 2" | θ = 5.6–29.1° |
a = 3.9761 (5) Å | µ = 24.09 mm−1 |
c = 21.841 (3) Å | T = 293 K |
V = 299.03 (7) Å3 | Plate, yellow |
Z = 3 | 0.17 × 0.11 × 0.06 mm |
F(000) = 360 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 124 independent reflections |
Radiation source: X-ray tube | 124 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.048 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 29.2°, θmin = 5.6° |
ω scans | h = −5→3 |
Absorption correction: gaussian JANA2006 (Petříček et al., 2014) | k = −4→5 |
Tmin = 0.111, Tmax = 0.291 | l = −28→20 |
637 measured reflections | |
Refinement top
Refinement on F2 | 0 constraints |
R[F > 3σ(F)] = 0.016 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
wR(F) = 0.040 | (Δ/σ)max = 0.001 |
S = 1.12 | Δρmax = 0.48 e Å−3 |
124 reflections | Δρmin = −1.00 e Å−3 |
9 parameters | Extinction correction: B-C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147] |
0 restraints | Extinction coefficient: 2710 (180) |
Special details top
Refinement. The refinement of a model with obverse–reverse twinning turned out to be
insignificant. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K | 0 | 0 | 0 | 0.0143 (8) | |
Tm | 0.333333 | 0.666667 | 0.166667 | 0.0067 (3) | |
S | 0 | 0 | 0.23376 (11) | 0.0083 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.0158 (10) | 0.0158 (10) | 0.0113 (15) | 0.0079 (5) | 0 | 0 |
Tm | 0.0061 (4) | 0.0061 (4) | 0.0079 (4) | 0.00307 (19) | 0 | 0 |
S | 0.0082 (7) | 0.0082 (7) | 0.0085 (11) | 0.0041 (4) | 0 | 0 |
Geometric parameters (Å, º) top
K—Si | 3.1622 (19) | Tm—S | 2.7235 (15) |
K—Sii | 3.1622 (18) | Tm—Svii | 2.7234 (14) |
K—Siii | 3.1622 (19) | Tm—Sviii | 2.7235 (15) |
K—Siv | 3.1622 (19) | Tm—Sv | 2.7235 (15) |
K—Sv | 3.1622 (18) | Tm—Svi | 2.7235 (14) |
K—Svi | 3.1622 (19) | Tm—Six | 2.7235 (15) |
| | | |
Si—K—Sii | 77.91 (4) | S—Tm—Svi | 86.23 (4) |
Si—K—Siii | 77.91 (4) | S—Tm—Six | 180.0 (5) |
Si—K—Siv | 102.09 (4) | Svii—Tm—Sviii | 93.77 (4) |
Si—K—Sv | 102.09 (4) | Svii—Tm—Sv | 86.23 (4) |
Si—K—Svi | 180.0 (5) | Svii—Tm—Svi | 180.0 (5) |
Sii—K—Siii | 77.91 (4) | Svii—Tm—Six | 86.23 (4) |
Sii—K—Siv | 102.09 (4) | Sviii—Tm—Sv | 180.0 (5) |
Sii—K—Sv | 180.0 (5) | Sviii—Tm—Svi | 86.23 (4) |
Sii—K—Svi | 102.09 (4) | Sviii—Tm—Six | 86.23 (4) |
Siii—K—Siv | 180.0 (5) | Sv—Tm—Svi | 93.77 (4) |
Siii—K—Sv | 102.09 (4) | Sv—Tm—Six | 93.77 (4) |
Siii—K—Svi | 102.09 (4) | Svi—Tm—Six | 93.77 (4) |
Siv—K—Sv | 77.91 (4) | Kx—S—Kxi | 77.91 (5) |
Siv—K—Svi | 77.91 (4) | Kx—S—Kxii | 77.91 (5) |
Sv—K—Svi | 77.91 (4) | Kxi—S—Kxii | 77.91 (5) |
S—Tm—Svii | 93.77 (4) | Tmxiii—S—Tmxiv | 93.77 (6) |
S—Tm—Sviii | 93.77 (4) | Tmxiii—S—Tm | 93.77 (6) |
S—Tm—Sv | 86.23 (4) | Tmxiv—S—Tm | 93.77 (6) |
Symmetry codes: (i) x−2/3, y−1/3, z−1/3; (ii) x+1/3, y−1/3, z−1/3; (iii) x+1/3, y+2/3, z−1/3; (iv) y−1/3, x−2/3, −z+1/3; (v) y−1/3, x+1/3, −z+1/3; (vi) y+2/3, x+1/3, −z+1/3; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) y+2/3, x+4/3, −z+1/3; (x) x−1/3, y−2/3, z+1/3; (xi) x−1/3, y+1/3, z+1/3; (xii) x+2/3, y+1/3, z+1/3; (xiii) x−1, y−1, z; (xiv) x, y−1, z. |
(X) Potassium ytterbium sulfide
top
Crystal data top
KYbS2 | Dx = 4.643 Mg m−3 |
Mr = 276.3 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m | Cell parameters from 582 reflections |
Hall symbol: -R 3 2" | θ = 5.6–28.9° |
a = 3.9615 (8) Å | µ = 25.52 mm−1 |
c = 21.810 (3) Å | T = 301 K |
V = 296.42 (9) Å3 | Plate, yellow |
Z = 3 | 0.13 × 0.11 × 0.09 mm |
F(000) = 363 | |
Data collection top
Xcalibur Gemini Ultra diffractometer with Atlas detector | 124 independent reflections |
Radiation source: X-ray tube | 124 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.069 |
Detector resolution: 5.1873 pixels mm-1 | θmax = 29.0°, θmin = 5.6° |
ω scans | h = −2→5 |
Absorption correction: gaussian (JANA2006; Petříček et al., 2014) | k = −5→4 |
Tmin = 0.099, Tmax = 0.193 | l = −29→29 |
444 measured reflections | |
Refinement top
Refinement on F2 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
R[F > 3σ(F)] = 0.029 | (Δ/σ)max = 0.003 |
wR(F) = 0.069 | Δρmax = 1.42 e Å−3 |
S = 1.65 | Δρmin = −2.15 e Å−3 |
124 reflections | Extinction correction: B-C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147] |
9 parameters | Extinction coefficient: 3900 (400) |
0 restraints | Absolute structure: Refinement of a model with
obverse–reverse twinning turned out to be insignificant |
0 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K | 0 | 0 | 0 | 0.0133 (13) | |
Yb | 0.333333 | 0.666667 | 0.166667 | 0.0063 (5) | |
S | 0 | 0 | 0.23346 (19) | 0.0072 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.0146 (16) | 0.0146 (16) | 0.011 (2) | 0.0073 (8) | 0 | 0 |
Yb | 0.0054 (6) | 0.0054 (6) | 0.0081 (7) | 0.0027 (3) | 0 | 0 |
S | 0.0077 (12) | 0.0077 (12) | 0.0062 (16) | 0.0039 (6) | 0 | 0 |
Geometric parameters (Å, º) top
K—Si | 3.159 (3) | Yb—Six | 2.712 (2) |
K—Sii | 3.159 (3) | S—Sx | 3.961 (2) |
K—Siii | 3.159 (3) | S—Sxi | 3.9615 (16) |
K—Siv | 3.159 (3) | S—Sxii | 3.9615 (16) |
K—Sv | 3.159 (3) | S—Svii | 3.9615 (16) |
K—Svi | 3.159 (3) | S—Sxiii | 3.9615 (16) |
Yb—S | 2.712 (2) | S—Sviii | 3.961 (2) |
Yb—Svii | 2.712 (2) | S—Siv | 3.704 (5) |
Yb—Sviii | 2.712 (2) | S—Sv | 3.704 (5) |
Yb—Sv | 2.712 (2) | S—Svi | 3.704 (5) |
Yb—Svi | 2.712 (2) | | |
| | | |
Si—K—Sii | 77.67 (6) | S—Yb—Sviii | 93.85 (7) |
Si—K—Siii | 77.67 (6) | S—Yb—Sv | 86.15 (7) |
Si—K—Siv | 102.33 (6) | S—Yb—Svi | 86.15 (7) |
Si—K—Sv | 102.33 (6) | S—Yb—Six | 180.0 (5) |
Si—K—Svi | 180.0 (5) | Svii—Yb—Sviii | 93.85 (7) |
Sii—K—Siii | 77.67 (6) | Svii—Yb—Sv | 86.15 (7) |
Sii—K—Siv | 102.33 (6) | Svii—Yb—Svi | 180.0 (5) |
Sii—K—Sv | 180.0 (5) | Svii—Yb—Six | 86.15 (7) |
Sii—K—Svi | 102.33 (6) | Sviii—Yb—Sv | 180.0 (5) |
Siii—K—Siv | 180.0 (5) | Sviii—Yb—Svi | 86.15 (7) |
Siii—K—Sv | 102.33 (6) | Sviii—Yb—Six | 86.15 (7) |
Siii—K—Svi | 102.33 (6) | Sv—Yb—Svi | 93.85 (7) |
Siv—K—Sv | 77.67 (6) | Sv—Yb—Six | 93.85 (7) |
Siv—K—Svi | 77.67 (6) | Svi—Yb—Six | 93.85 (7) |
Sv—K—Svi | 77.67 (6) | Kxiv—S—Kxv | 77.67 (8) |
S—Yb—Svii | 93.85 (7) | Kxiv—S—Kxvi | 77.67 (9) |
Symmetry codes: (i) x−2/3, y−1/3, z−1/3; (ii) x+1/3, y−1/3, z−1/3; (iii) x+1/3, y+2/3, z−1/3; (iv) y−1/3, x−2/3, −z+1/3; (v) y−1/3, x+1/3, −z+1/3; (vi) y+2/3, x+1/3, −z+1/3; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) y+2/3, x+4/3, −z+1/3; (x) x−1, y−1, z; (xi) x−1, y, z; (xii) x, y−1, z; (xiii) x+1, y, z; (xiv) x−1/3, y−2/3, z+1/3; (xv) x−1/3, y+1/3, z+1/3; (xvi) x+2/3, y+1/3, z+1/3. |