Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827011103589X/fn3086sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827011103589X/fn3086ScTesup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827011103589X/fn3086Y3Au2sup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827011103589X/fn3086Y2Ausup4.hkl |
The formation of all three phases was in fact first noted in powder pattern data from nearby ternary systems. β-ScTe was synthesized from a mixture of Sc and Sc2Te3. The latter was obtained from a prereaction of Sc and Te in a 2:3 ratio, sealed in a silica tube under vacuum, heated at 723 K for 12 h and then at 1173 K for 72 h. Y3Au2 and Y2Au were prepared from mixtures of high-purity elements. The three combinations were each pelletized and arc-melted under an argon atmosphere in a glovebox. The pellets were then sealed in tantalum containers and annealed in a graphite-heated vacuum furnace at 1573 K for 200 h for β-ScTe, and at 1323 K for one week for Y3Au2 and Y2Au.
For all compounds, data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2000); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
ScTe | Dx = 5.797 Mg m−3 Dm = 5.797 Mg m−3 Dm measured by not measured |
Mr = 172.56 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63/mmc | Cell parameters from 983 reflections |
a = 4.0969 (6) Å | θ = 5.9–28.1° |
c = 13.602 (3) Å | µ = 17.64 mm−1 |
V = 197.71 (6) Å3 | T = 293 K |
Z = 4 | Irregularly shaped, black |
F(000) = 292 | 0.15 × 0.08 × 0.07 mm |
Bruker SMART CCD area-detector diffractometer | 92 independent reflections |
Radiation source: fine-focus sealed tube | 90 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ϕ and ω scans | θmax = 25.0°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −4→4 |
Tmin = 0.177, Tmax = 0.372 | k = −4→4 |
1274 measured reflections | l = −15→16 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.036 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.081 | w = 1/[σ2(Fo2) + (0.0179P)2 + 7.5992P] where P = (Fo2 + 2Fc2)/3 |
S = 1.57 | (Δ/σ)max < 0.001 |
92 reflections | Δρmax = 1.21 e Å−3 |
8 parameters | Δρmin = −1.65 e Å−3 |
ScTe | Z = 4 |
Mr = 172.56 | Mo Kα radiation |
Hexagonal, P63/mmc | µ = 17.64 mm−1 |
a = 4.0969 (6) Å | T = 293 K |
c = 13.602 (3) Å | 0.15 × 0.08 × 0.07 mm |
V = 197.71 (6) Å3 |
Bruker SMART CCD area-detector diffractometer | 92 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 90 reflections with I > 2σ(I) |
Tmin = 0.177, Tmax = 0.372 | Rint = 0.020 |
1274 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 8 parameters |
wR(F2) = 0.081 | 0 restraints |
S = 1.57 | Δρmax = 1.21 e Å−3 |
92 reflections | Δρmin = −1.65 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Te1 | 0.3333 | 0.6667 | 0.2500 | 0.0078 (7) | |
Te2 | 0.0000 | 0.0000 | 0.0000 | 0.0110 (7) | |
Sc1 | 0.3333 | 0.6667 | 0.6183 (3) | 0.0241 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Te1 | 0.0079 (8) | 0.0079 (8) | 0.0077 (10) | 0.0039 (4) | 0.000 | 0.000 |
Te2 | 0.0100 (8) | 0.0100 (8) | 0.0130 (11) | 0.0050 (4) | 0.000 | 0.000 |
Sc1 | 0.0276 (19) | 0.0276 (19) | 0.017 (2) | 0.0138 (10) | 0.000 | 0.000 |
Te1—Sc1i | 2.967 (3) | Te2—Sc1ix | 2.861 (3) |
Te1—Sc1ii | 2.967 (3) | Te2—Sc1iii | 2.861 (3) |
Te1—Sc1iii | 2.967 (3) | Te2—Sc1x | 2.861 (3) |
Te1—Sc1iv | 2.967 (3) | Sc1—Te2xi | 2.861 (3) |
Te1—Sc1v | 2.967 (3) | Sc1—Te2xii | 2.861 (3) |
Te1—Sc1vi | 2.967 (3) | Sc1—Te2xiii | 2.861 (3) |
Te2—Sc1vii | 2.861 (3) | Sc1—Te1ii | 2.967 (3) |
Te2—Sc1i | 2.861 (3) | Sc1—Te1iv | 2.967 (3) |
Te2—Sc1viii | 2.861 (3) | Sc1—Te1vi | 2.967 (3) |
Sc1i—Te1—Sc1ii | 74.27 (15) | Sc1i—Te2—Sc1x | 88.55 (11) |
Sc1i—Te1—Sc1iii | 87.33 (11) | Sc1viii—Te2—Sc1x | 91.45 (11) |
Sc1ii—Te1—Sc1iii | 133.02 (5) | Sc1ix—Te2—Sc1x | 88.55 (11) |
Sc1i—Te1—Sc1iv | 133.02 (5) | Sc1iii—Te2—Sc1x | 180.00 (16) |
Sc1ii—Te1—Sc1iv | 87.33 (11) | Te2xi—Sc1—Te2xii | 91.45 (11) |
Sc1iii—Te1—Sc1iv | 133.02 (5) | Te2xi—Sc1—Te2xiii | 91.45 (11) |
Sc1i—Te1—Sc1v | 87.33 (11) | Te2xii—Sc1—Te2xiii | 91.45 (11) |
Sc1ii—Te1—Sc1v | 133.02 (5) | Te2xi—Sc1—Te1ii | 90.574 (11) |
Sc1iii—Te1—Sc1v | 87.33 (11) | Te2xii—Sc1—Te1ii | 177.10 (15) |
Sc1iv—Te1—Sc1v | 74.26 (15) | Te2xiii—Sc1—Te1ii | 90.574 (11) |
Sc1i—Te1—Sc1vi | 133.02 (5) | Te2xi—Sc1—Te1iv | 177.10 (15) |
Sc1ii—Te1—Sc1vi | 87.33 (11) | Te2xii—Sc1—Te1iv | 90.574 (11) |
Sc1iii—Te1—Sc1vi | 74.26 (15) | Te2xiii—Sc1—Te1iv | 90.574 (11) |
Sc1iv—Te1—Sc1vi | 87.33 (11) | Te1ii—Sc1—Te1iv | 87.33 (10) |
Sc1v—Te1—Sc1vi | 133.02 (5) | Te2xi—Sc1—Te1vi | 90.574 (11) |
Sc1vii—Te2—Sc1i | 180.00 (16) | Te2xii—Sc1—Te1vi | 90.573 (11) |
Sc1vii—Te2—Sc1viii | 91.45 (11) | Te2xiii—Sc1—Te1vi | 177.10 (15) |
Sc1i—Te2—Sc1viii | 88.55 (11) | Te1ii—Sc1—Te1vi | 87.33 (10) |
Sc1vii—Te2—Sc1ix | 88.55 (11) | Te1iv—Sc1—Te1vi | 87.33 (10) |
Sc1i—Te2—Sc1ix | 91.45 (11) | Te2xi—Sc1—Sc1xiv | 124.23 (8) |
Sc1viii—Te2—Sc1ix | 180.00 (16) | Te2xii—Sc1—Sc1xiv | 124.23 (8) |
Sc1vii—Te2—Sc1iii | 88.55 (11) | Te2xiii—Sc1—Sc1xiv | 124.23 (8) |
Sc1i—Te2—Sc1iii | 91.45 (11) | Te1ii—Sc1—Sc1xiv | 52.87 (7) |
Sc1viii—Te2—Sc1iii | 88.55 (11) | Te1iv—Sc1—Sc1xiv | 52.87 (7) |
Sc1ix—Te2—Sc1iii | 91.45 (11) | Te1vi—Sc1—Sc1xiv | 52.87 (7) |
Sc1vii—Te2—Sc1x | 91.45 (11) |
Symmetry codes: (i) −x+1, −y+1, z−1/2; (ii) −x+1, −y+1, −z+1; (iii) −x, −y+1, z−1/2; (iv) −x+1, −y+2, −z+1; (v) −x+1, −y+2, z−1/2; (vi) −x, −y+1, −z+1; (vii) x−1, y−1, −z+1/2; (viii) x, y, −z+1/2; (ix) −x, −y, z−1/2; (x) x, y−1, −z+1/2; (xi) −x, −y, z+1/2; (xii) −x, −y+1, z+1/2; (xiii) −x+1, −y+1, z+1/2; (xiv) x, y, −z+3/2. |
Y3Au2 | Dx = 8.647 Mg m−3 Dm = 8.647 Mg m−3 Dm measured by not measured |
Mr = 660.66 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P4/mbm | Cell parameters from 497 reflections |
a = 8.059 (3) Å | θ = 3.6–26.5° |
c = 3.907 (3) Å | µ = 91.35 mm−1 |
V = 253.7 (3) Å3 | T = 293 K |
Z = 2 | Irregularly shaped, metallic silver |
F(000) = 550 | 0.05 × 0.04 × 0.02 mm |
Bruker SMART CCD area-detector diffractometer | 194 independent reflections |
Radiation source: fine-focus sealed tube | 156 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.093 |
ϕ and ω scans | θmax = 28.1°, θmin = 3.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→10 |
Tmin = 0.092, Tmax = 0.262 | k = −9→10 |
1866 measured reflections | l = −5→5 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.030 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.069 | w = 1/[σ2(Fo2) + (0.P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.93 | (Δ/σ)max < 0.001 |
194 reflections | Δρmax = 1.46 e Å−3 |
11 parameters | Δρmin = −1.40 e Å−3 |
Y3Au2 | Z = 2 |
Mr = 660.66 | Mo Kα radiation |
Tetragonal, P4/mbm | µ = 91.35 mm−1 |
a = 8.059 (3) Å | T = 293 K |
c = 3.907 (3) Å | 0.05 × 0.04 × 0.02 mm |
V = 253.7 (3) Å3 |
Bruker SMART CCD area-detector diffractometer | 194 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 156 reflections with I > 2σ(I) |
Tmin = 0.092, Tmax = 0.262 | Rint = 0.093 |
1866 measured reflections |
R[F2 > 2σ(F2)] = 0.030 | 11 parameters |
wR(F2) = 0.069 | 0 restraints |
S = 0.93 | Δρmax = 1.46 e Å−3 |
194 reflections | Δρmin = −1.40 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Au1 | 0.63399 (7) | 0.13399 (7) | 0.0000 | 0.0213 (3) | |
Y1 | 0.0000 | 0.0000 | 0.0000 | 0.0221 (7) | |
Y2 | 0.16226 (19) | 0.66226 (19) | 0.5000 | 0.0241 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Au1 | 0.0227 (4) | 0.0227 (4) | 0.0184 (5) | −0.0018 (3) | 0.000 | 0.000 |
Y1 | 0.0261 (10) | 0.0261 (10) | 0.0141 (13) | 0.000 | 0.000 | 0.000 |
Y2 | 0.0294 (7) | 0.0294 (7) | 0.0135 (11) | −0.0039 (8) | 0.000 | 0.000 |
Au1—Y2i | 3.035 (2) | Y1—Au1xi | 3.1409 (13) |
Au1—Y2ii | 3.035 (2) | Y1—Au1xii | 3.1409 (13) |
Au1—Au1iii | 3.0539 (19) | Y1—Au1iii | 3.1409 (13) |
Au1—Y2iv | 3.0932 (19) | Y2—Au1i | 3.035 (2) |
Au1—Y2v | 3.0932 (19) | Y2—Au1ii | 3.035 (2) |
Au1—Y2vi | 3.0932 (19) | Y2—Au1xiii | 3.0932 (19) |
Au1—Y2vii | 3.0932 (19) | Y2—Au1xiv | 3.0932 (19) |
Au1—Y1viii | 3.1409 (13) | Y2—Au1x | 3.0932 (19) |
Au1—Y1ix | 3.1409 (13) | Y2—Au1xv | 3.0932 (19) |
Y1—Au1x | 3.1409 (13) | ||
Y2i—Au1—Y2ii | 80.15 (8) | Au1iii—Y1—Y2xx | 126.98 (3) |
Y2i—Au1—Au1iii | 139.92 (4) | Y2xvi—Y1—Y2xx | 72.84 (2) |
Y2ii—Au1—Au1iii | 139.92 (4) | Y2vii—Y1—Y2xx | 107.16 (2) |
Y2i—Au1—Y2iv | 141.66 (3) | Y2xvii—Y1—Y2xx | 65.81 (5) |
Y2ii—Au1—Y2iv | 88.34 (5) | Y2xviii—Y1—Y2xx | 114.19 (5) |
Au1iii—Au1—Y2iv | 60.42 (2) | Y2xix—Y1—Y2xx | 107.16 (2) |
Y2i—Au1—Y2v | 141.66 (3) | Y2v—Y1—Y2xx | 72.84 (2) |
Y2ii—Au1—Y2v | 88.34 (5) | Au1x—Y1—Y2xxi | 125.85 (4) |
Au1iii—Au1—Y2v | 60.42 (2) | Au1xi—Y1—Y2xxi | 54.15 (4) |
Y2iv—Au1—Y2v | 73.43 (7) | Au1xii—Y1—Y2xxi | 126.98 (3) |
Y2i—Au1—Y2vi | 88.34 (5) | Au1iii—Y1—Y2xxi | 53.02 (3) |
Y2ii—Au1—Y2vi | 141.66 (3) | Y2xvi—Y1—Y2xxi | 107.16 (2) |
Au1iii—Au1—Y2vi | 60.42 (2) | Y2vii—Y1—Y2xxi | 72.84 (2) |
Y2iv—Au1—Y2vi | 78.34 (7) | Y2xvii—Y1—Y2xxi | 114.19 (5) |
Y2v—Au1—Y2vi | 120.84 (4) | Y2xviii—Y1—Y2xxi | 65.81 (5) |
Y2i—Au1—Y2vii | 88.34 (5) | Y2xix—Y1—Y2xxi | 72.84 (2) |
Y2ii—Au1—Y2vii | 141.66 (3) | Y2v—Y1—Y2xxi | 107.16 (2) |
Au1iii—Au1—Y2vii | 60.42 (2) | Y2xx—Y1—Y2xxi | 180.00 (3) |
Y2iv—Au1—Y2vii | 120.84 (4) | Au1i—Y2—Au1ii | 80.15 (8) |
Y2v—Au1—Y2vii | 78.34 (7) | Au1i—Y2—Au1xiii | 149.78 (3) |
Y2vi—Au1—Y2vii | 73.43 (7) | Au1ii—Y2—Au1xiii | 92.91 (5) |
Y2i—Au1—Y1viii | 71.210 (16) | Au1i—Y2—Au1xiv | 92.91 (5) |
Y2ii—Au1—Y1viii | 71.210 (16) | Au1ii—Y2—Au1xiv | 149.78 (3) |
Au1iii—Au1—Y1viii | 114.894 (12) | Au1xiii—Y2—Au1xiv | 78.34 (7) |
Y2iv—Au1—Y1viii | 138.60 (4) | Au1i—Y2—Au1x | 149.78 (3) |
Y2v—Au1—Y1viii | 70.46 (3) | Au1ii—Y2—Au1x | 92.91 (5) |
Y2vi—Au1—Y1viii | 138.60 (4) | Au1xiii—Y2—Au1x | 59.16 (4) |
Y2vii—Au1—Y1viii | 70.46 (3) | Au1xiv—Y2—Au1x | 106.57 (7) |
Y2i—Au1—Y1ix | 71.210 (16) | Au1i—Y2—Au1xv | 92.91 (5) |
Y2ii—Au1—Y1ix | 71.210 (16) | Au1ii—Y2—Au1xv | 149.78 (3) |
Au1iii—Au1—Y1ix | 114.894 (12) | Au1xiii—Y2—Au1xv | 106.57 (7) |
Y2iv—Au1—Y1ix | 70.46 (3) | Au1xiv—Y2—Au1xv | 59.16 (4) |
Y2v—Au1—Y1ix | 138.60 (4) | Au1x—Y2—Au1xv | 78.34 (7) |
Y2vi—Au1—Y1ix | 70.46 (3) | Au1i—Y2—Y1xxii | 55.77 (3) |
Y2vii—Au1—Y1ix | 138.60 (4) | Au1ii—Y2—Y1xxii | 97.87 (6) |
Y1viii—Au1—Y1ix | 130.21 (2) | Au1xiii—Y2—Y1xxii | 96.79 (4) |
Au1x—Y1—Au1xi | 180.000 (7) | Au1xiv—Y2—Y1xxii | 55.39 (2) |
Au1x—Y1—Au1xii | 90.0 | Au1x—Y2—Y1xxii | 154.21 (5) |
Au1xi—Y1—Au1xii | 90.0 | Au1xv—Y2—Y1xxii | 102.37 (5) |
Au1x—Y1—Au1iii | 90.0 | Au1i—Y2—Y1xxiii | 97.87 (6) |
Au1xi—Y1—Au1iii | 90.0 | Au1ii—Y2—Y1xxiii | 55.77 (3) |
Au1xii—Y1—Au1iii | 180.0 | Au1xiii—Y2—Y1xxiii | 55.39 (2) |
Au1x—Y1—Y2xvi | 126.98 (3) | Au1xiv—Y2—Y1xxiii | 96.79 (4) |
Au1xi—Y1—Y2xvi | 53.02 (3) | Au1x—Y2—Y1xxiii | 102.37 (5) |
Au1xii—Y1—Y2xvi | 54.15 (4) | Au1xv—Y2—Y1xxiii | 154.21 (5) |
Au1iii—Y1—Y2xvi | 125.85 (4) | Y1xxii—Y2—Y1xxiii | 65.81 (5) |
Au1x—Y1—Y2vii | 53.02 (3) | Au1i—Y2—Y1xxiv | 55.77 (3) |
Au1xi—Y1—Y2vii | 126.98 (3) | Au1ii—Y2—Y1xxiv | 97.87 (6) |
Au1xii—Y1—Y2vii | 125.85 (4) | Au1xiii—Y2—Y1xxiv | 154.21 (5) |
Au1iii—Y1—Y2vii | 54.15 (4) | Au1xiv—Y2—Y1xxiv | 102.37 (5) |
Y2xvi—Y1—Y2vii | 180.00 (3) | Au1x—Y2—Y1xxiv | 96.79 (4) |
Au1x—Y1—Y2xvii | 54.15 (4) | Au1xv—Y2—Y1xxiv | 55.39 (2) |
Au1xi—Y1—Y2xvii | 125.85 (4) | Y1xxii—Y2—Y1xxiv | 104.78 (5) |
Au1xii—Y1—Y2xvii | 53.02 (3) | Y1xxiii—Y2—Y1xxiv | 147.71 (7) |
Au1iii—Y1—Y2xvii | 126.98 (3) | Au1i—Y2—Y1viii | 97.87 (6) |
Y2xvi—Y1—Y2xvii | 107.16 (2) | Au1ii—Y2—Y1viii | 55.77 (3) |
Y2vii—Y1—Y2xvii | 72.84 (2) | Au1xiii—Y2—Y1viii | 102.37 (5) |
Au1x—Y1—Y2xviii | 125.85 (4) | Au1xiv—Y2—Y1viii | 154.21 (5) |
Au1xi—Y1—Y2xviii | 54.15 (4) | Au1x—Y2—Y1viii | 55.39 (2) |
Au1xii—Y1—Y2xviii | 126.98 (3) | Au1xv—Y2—Y1viii | 96.79 (4) |
Au1iii—Y1—Y2xviii | 53.02 (3) | Y1xxii—Y2—Y1viii | 147.71 (7) |
Y2xvi—Y1—Y2xviii | 72.84 (2) | Y1xxiii—Y2—Y1viii | 104.78 (5) |
Y2vii—Y1—Y2xviii | 107.16 (2) | Y1xxiv—Y2—Y1viii | 65.81 (5) |
Y2xvii—Y1—Y2xviii | 180.0 | Au1i—Y2—Y2xvii | 139.92 (4) |
Au1x—Y1—Y2xix | 126.98 (3) | Au1ii—Y2—Y2xvii | 139.92 (4) |
Au1xi—Y1—Y2xix | 53.02 (3) | Au1xiii—Y2—Y2xvii | 53.29 (4) |
Au1xii—Y1—Y2xix | 54.15 (4) | Au1xiv—Y2—Y2xvii | 53.29 (4) |
Au1iii—Y1—Y2xix | 125.85 (4) | Au1x—Y2—Y2xvii | 53.29 (4) |
Y2xvi—Y1—Y2xix | 65.81 (5) | Au1xv—Y2—Y2xvii | 53.29 (4) |
Y2vii—Y1—Y2xix | 114.19 (5) | Y1xxii—Y2—Y2xvii | 106.14 (3) |
Y2xvii—Y1—Y2xix | 72.84 (2) | Y1xxiii—Y2—Y2xvii | 106.14 (3) |
Y2xviii—Y1—Y2xix | 107.16 (2) | Y1xxiv—Y2—Y2xvii | 106.14 (3) |
Au1x—Y1—Y2v | 53.02 (3) | Y1viii—Y2—Y2xvii | 106.14 (3) |
Au1xi—Y1—Y2v | 126.98 (3) | Au1i—Y2—Y2xxv | 130.08 (4) |
Au1xii—Y1—Y2v | 125.85 (4) | Au1ii—Y2—Y2xxv | 49.92 (4) |
Au1iii—Y1—Y2v | 54.15 (4) | Au1xiii—Y2—Y2xxv | 50.83 (3) |
Y2xvi—Y1—Y2v | 114.19 (5) | Au1xiv—Y2—Y2xxv | 129.17 (3) |
Y2vii—Y1—Y2v | 65.81 (5) | Au1x—Y2—Y2xxv | 50.83 (3) |
Y2xvii—Y1—Y2v | 107.16 (2) | Au1xv—Y2—Y2xxv | 129.17 (3) |
Y2xviii—Y1—Y2v | 72.84 (2) | Y1xxii—Y2—Y2xxv | 122.90 (2) |
Y2xix—Y1—Y2v | 180.0 | Y1xxiii—Y2—Y2xxv | 57.10 (3) |
Au1x—Y1—Y2xx | 54.15 (4) | Y1xxiv—Y2—Y2xxv | 122.90 (3) |
Au1xi—Y1—Y2xx | 125.85 (4) | Y1viii—Y2—Y2xxv | 57.10 (2) |
Au1xii—Y1—Y2xx | 53.02 (3) | Y2xvii—Y2—Y2xxv | 90.0 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+1, −z; (iii) −x+1, −y, −z; (iv) y, −x, −z; (v) −y+1, x, z−1; (vi) y, −x, −z+1; (vii) −y+1, x, z; (viii) −x+1/2, y+1/2, −z; (ix) x+1, y, z; (x) y, −x+1, −z; (xi) −y, x−1, z; (xii) x−1, y, z; (xiii) −y, x, z; (xiv) −y, x, z+1; (xv) y, −x+1, −z+1; (xvi) y−1, −x, −z; (xvii) −x, −y+1, −z+1; (xviii) x, y−1, z−1; (xix) y−1, −x, −z+1; (xx) −x, −y+1, −z; (xxi) x, y−1, z; (xxii) x, y+1, z+1; (xxiii) x, y+1, z; (xxiv) −x+1/2, y+1/2, −z+1; (xxv) x, y, z−1. |
Y2Au | Dx = 7.962 Mg m−3 Dm = 7.962 Mg m−3 Dm measured by not measured |
Mr = 374.79 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pnma | Cell parameters from 584 reflections |
a = 7.115 (3) Å | θ = 4.6–27.7° |
b = 4.933 (2) Å | µ = 83.29 mm−1 |
c = 8.908 (4) Å | T = 293 K |
V = 312.7 (2) Å3 | Irregularly shaped, metallic silver |
Z = 4 | 0.12 × 0.08 × 0.04 mm |
F(000) = 628 |
Bruker SMART CCD area-detector diffractometer | 345 independent reflections |
Radiation source: fine-focus sealed tube | 299 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
ϕ and ω scans | θmax = 26.0°, θmin = 3.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→8 |
Tmin = 0.036, Tmax = 0.135 | k = −6→5 |
1619 measured reflections | l = −7→10 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.026 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.058 | w = 1/[σ2(Fo2) + (0.0321P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max < 0.001 |
345 reflections | Δρmax = 1.76 e Å−3 |
20 parameters | Δρmin = −2.14 e Å−3 |
Y2Au | V = 312.7 (2) Å3 |
Mr = 374.79 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 7.115 (3) Å | µ = 83.29 mm−1 |
b = 4.933 (2) Å | T = 293 K |
c = 8.908 (4) Å | 0.12 × 0.08 × 0.04 mm |
Bruker SMART CCD area-detector diffractometer | 345 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 299 reflections with I > 2σ(I) |
Tmin = 0.036, Tmax = 0.135 | Rint = 0.039 |
1619 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 20 parameters |
wR(F2) = 0.058 | 0 restraints |
S = 1.07 | Δρmax = 1.76 e Å−3 |
345 reflections | Δρmin = −2.14 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Au1 | 0.24296 (8) | 0.2500 | 0.39987 (6) | 0.0107 (2) | |
Y1 | 0.1474 (2) | 0.2500 | 0.08075 (15) | 0.0100 (3) | |
Y2 | 0.01605 (19) | 0.2500 | 0.67592 (15) | 0.0104 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Au1 | 0.0135 (3) | 0.0082 (3) | 0.0105 (3) | 0.000 | −0.0005 (2) | 0.000 |
Y1 | 0.0135 (8) | 0.0059 (7) | 0.0107 (6) | 0.000 | 0.0001 (6) | 0.000 |
Y2 | 0.0113 (7) | 0.0088 (7) | 0.0111 (7) | 0.000 | 0.0007 (5) | 0.000 |
Au1—Y1i | 2.883 (2) | Y1—Au1viii | 3.0477 (12) |
Au1—Y1 | 2.9228 (18) | Y1—Y2i | 3.480 (2) |
Au1—Y2 | 2.9417 (18) | Y1—Y2v | 3.4833 (17) |
Au1—Y1ii | 3.0478 (13) | Y1—Y2iv | 3.4833 (17) |
Au1—Y1iii | 3.0478 (13) | Y2—Au1iv | 3.1521 (13) |
Au1—Y2iv | 3.1521 (13) | Y2—Au1v | 3.1521 (13) |
Au1—Y2v | 3.1521 (13) | Y2—Y1vi | 3.480 (2) |
Y1—Au1vi | 2.883 (2) | Y2—Y1v | 3.4833 (17) |
Y1—Au1vii | 3.0477 (13) | Y2—Y1iv | 3.4833 (17) |
Y1i—Au1—Y1 | 106.89 (4) | Au1viii—Y1—Y1x | 51.20 (3) |
Y1i—Au1—Y2 | 119.86 (5) | Y2i—Y1—Y1x | 100.34 (6) |
Y1—Au1—Y2 | 133.25 (5) | Y2v—Y1—Y1x | 64.03 (4) |
Y1i—Au1—Y1ii | 73.31 (4) | Y2iv—Y1—Y1x | 123.23 (7) |
Y1—Au1—Y1ii | 125.01 (3) | Y2viii—Y1—Y1x | 90.72 (4) |
Y2—Au1—Y1ii | 72.46 (4) | Y2vii—Y1—Y1x | 169.28 (7) |
Y1i—Au1—Y1iii | 73.31 (4) | Y1ix—Y1—Y1x | 88.25 (7) |
Y1—Au1—Y1iii | 125.01 (3) | Au1vi—Y1—Y2xi | 78.91 (4) |
Y2—Au1—Y1iii | 72.46 (4) | Au1—Y1—Y2xi | 178.93 (6) |
Y1ii—Au1—Y1iii | 108.05 (5) | Au1vii—Y1—Y2xi | 63.41 (3) |
Y1i—Au1—Y2iv | 126.62 (3) | Au1viii—Y1—Y2xi | 63.41 (3) |
Y1—Au1—Y2iv | 69.86 (3) | Y2i—Y1—Y2xi | 63.45 (4) |
Y2—Au1—Y2iv | 81.84 (4) | Y2v—Y1—Y2xi | 121.24 (4) |
Y1ii—Au1—Y2iv | 153.66 (4) | Y2iv—Y1—Y2xi | 121.24 (4) |
Y1iii—Au1—Y2iv | 68.26 (4) | Y2viii—Y1—Y2xi | 113.67 (4) |
Y1i—Au1—Y2v | 126.62 (3) | Y2vii—Y1—Y2xi | 113.67 (4) |
Y1—Au1—Y2v | 69.86 (3) | Y1ix—Y1—Y2xi | 57.21 (4) |
Y2—Au1—Y2v | 81.84 (4) | Y1x—Y1—Y2xi | 57.21 (4) |
Y1ii—Au1—Y2v | 68.26 (4) | Au1—Y2—Au1iv | 98.16 (4) |
Y1iii—Au1—Y2v | 153.66 (4) | Au1—Y2—Au1v | 98.16 (4) |
Y2iv—Au1—Y2v | 102.98 (5) | Au1iv—Y2—Au1v | 102.98 (5) |
Y1i—Au1—Y2vii | 63.80 (3) | Au1—Y2—Y1vi | 82.21 (5) |
Y1—Au1—Y2vii | 64.70 (4) | Au1iv—Y2—Y1vi | 54.45 (3) |
Y2—Au1—Y2vii | 136.34 (2) | Au1v—Y2—Y1vi | 54.45 (3) |
Y1ii—Au1—Y2vii | 136.41 (4) | Au1—Y2—Y1v | 134.70 (3) |
Y1iii—Au1—Y2vii | 67.49 (4) | Au1iv—Y2—Y1v | 119.48 (5) |
Y2iv—Au1—Y2vii | 67.93 (3) | Au1v—Y2—Y1v | 51.98 (3) |
Y2v—Au1—Y2vii | 134.01 (3) | Y1vi—Y2—Y1v | 99.04 (4) |
Y1i—Au1—Y2viii | 63.80 (3) | Au1—Y2—Y1iv | 134.70 (3) |
Y1—Au1—Y2viii | 64.70 (3) | Au1iv—Y2—Y1iv | 51.98 (3) |
Y2—Au1—Y2viii | 136.34 (2) | Au1v—Y2—Y1iv | 119.48 (5) |
Y1ii—Au1—Y2viii | 67.49 (4) | Y1vi—Y2—Y1iv | 99.04 (4) |
Y1iii—Au1—Y2viii | 136.41 (4) | Y1v—Y2—Y1iv | 90.16 (6) |
Y2iv—Au1—Y2viii | 134.01 (3) | Au1—Y2—Y1ii | 55.16 (3) |
Y2v—Au1—Y2viii | 67.93 (3) | Au1iv—Y2—Y1ii | 152.78 (5) |
Y2vii—Au1—Y2viii | 86.31 (4) | Au1v—Y2—Y1ii | 78.41 (4) |
Au1vi—Y1—Au1 | 100.02 (4) | Y1vi—Y2—Y1ii | 110.64 (4) |
Au1vi—Y1—Au1vii | 106.69 (4) | Y1v—Y2—Y1ii | 83.19 (3) |
Au1—Y1—Au1vii | 117.04 (3) | Y1iv—Y2—Y1ii | 150.23 (5) |
Au1vi—Y1—Au1viii | 106.69 (4) | Au1—Y2—Y1iii | 55.16 (3) |
Au1—Y1—Au1viii | 117.04 (3) | Au1iv—Y2—Y1iii | 78.41 (4) |
Au1vii—Y1—Au1viii | 108.05 (5) | Au1v—Y2—Y1iii | 152.78 (5) |
Au1vi—Y1—Y2i | 142.36 (5) | Y1vi—Y2—Y1iii | 110.64 (4) |
Au1—Y1—Y2i | 117.62 (6) | Y1v—Y2—Y1iii | 150.23 (5) |
Au1vii—Y1—Y2i | 57.29 (3) | Y1iv—Y2—Y1iii | 83.19 (3) |
Au1viii—Y1—Y2i | 57.29 (3) | Y1ii—Y2—Y1iii | 88.31 (5) |
Au1vi—Y1—Y2v | 68.25 (3) | Au1—Y2—Au1ii | 101.62 (4) |
Au1—Y1—Y2v | 58.17 (3) | Au1iv—Y2—Au1ii | 158.71 (5) |
Au1vii—Y1—Y2v | 170.92 (4) | Au1v—Y2—Au1ii | 82.03 (3) |
Au1viii—Y1—Y2v | 80.87 (4) | Y1vi—Y2—Au1ii | 136.22 (2) |
Y2i—Y1—Y2v | 131.34 (3) | Y1v—Y2—Au1ii | 47.95 (3) |
Au1vi—Y1—Y2iv | 68.25 (3) | Y1iv—Y2—Au1ii | 107.39 (5) |
Au1—Y1—Y2iv | 58.17 (3) | Y1ii—Y2—Au1ii | 48.27 (3) |
Au1vii—Y1—Y2iv | 80.87 (4) | Y1iii—Y2—Au1ii | 106.69 (5) |
Au1viii—Y1—Y2iv | 170.92 (4) | Au1—Y2—Au1iii | 101.62 (4) |
Y2i—Y1—Y2iv | 131.34 (3) | Au1iv—Y2—Au1iii | 82.03 (3) |
Y2v—Y1—Y2iv | 90.16 (5) | Au1v—Y2—Au1iii | 158.71 (5) |
Au1vi—Y1—Y2viii | 131.36 (3) | Y1vi—Y2—Au1iii | 136.22 (2) |
Au1—Y1—Y2viii | 67.03 (3) | Y1v—Y2—Au1iii | 107.39 (5) |
Au1vii—Y1—Y2viii | 121.14 (5) | Y1iv—Y2—Au1iii | 47.95 (3) |
Au1viii—Y1—Y2viii | 52.39 (3) | Y1ii—Y2—Au1iii | 106.69 (5) |
Y2i—Y1—Y2viii | 69.36 (4) | Y1iii—Y2—Au1iii | 48.27 (3) |
Y2v—Y1—Y2viii | 65.39 (3) | Au1ii—Y2—Au1iii | 86.31 (4) |
Y2iv—Y1—Y2viii | 124.75 (5) | Au1—Y2—Y1xii | 132.18 (6) |
Au1vi—Y1—Y2vii | 131.36 (3) | Au1iv—Y2—Y1xii | 110.73 (3) |
Au1—Y1—Y2vii | 67.03 (3) | Au1v—Y2—Y1xii | 110.73 (3) |
Au1vii—Y1—Y2vii | 52.39 (3) | Y1vi—Y2—Y1xii | 145.60 (6) |
Au1viii—Y1—Y2vii | 121.14 (5) | Y1v—Y2—Y1xii | 58.76 (4) |
Y2i—Y1—Y2vii | 69.36 (4) | Y1iv—Y2—Y1xii | 58.76 (4) |
Y2v—Y1—Y2vii | 124.75 (5) | Y1ii—Y2—Y1xii | 93.56 (4) |
Y2iv—Y1—Y2vii | 65.39 (3) | Y1iii—Y2—Y1xii | 93.56 (4) |
Y2viii—Y1—Y2vii | 88.31 (5) | Au1ii—Y2—Y1xii | 49.10 (3) |
Au1vi—Y1—Y1ix | 55.49 (4) | Au1iii—Y2—Y1xii | 49.10 (3) |
Au1—Y1—Y1ix | 122.19 (5) | Au1—Y2—Y2xiii | 77.06 (4) |
Au1vii—Y1—Y1ix | 51.20 (3) | Au1iv—Y2—Y2xiii | 128.51 (3) |
Au1viii—Y1—Y1ix | 120.02 (6) | Au1v—Y2—Y2xiii | 128.51 (3) |
Y2i—Y1—Y1ix | 100.34 (6) | Y1vi—Y2—Y2xiii | 159.28 (6) |
Y2v—Y1—Y1ix | 123.23 (7) | Y1v—Y2—Y2xiii | 95.54 (5) |
Y2iv—Y1—Y1ix | 64.03 (4) | Y1iv—Y2—Y2xiii | 95.54 (5) |
Y2viii—Y1—Y1ix | 169.28 (7) | Y1ii—Y2—Y2xiii | 56.57 (3) |
Y2vii—Y1—Y1ix | 90.72 (4) | Y1iii—Y2—Y2xiii | 56.57 (3) |
Au1vi—Y1—Y1x | 55.49 (4) | Au1ii—Y2—Y2xiii | 50.34 (3) |
Au1—Y1—Y1x | 122.19 (5) | Au1iii—Y2—Y2xiii | 50.34 (3) |
Au1vii—Y1—Y1x | 120.02 (6) | Y1xii—Y2—Y2xiii | 55.12 (5) |
Symmetry codes: (i) x+1/2, y, −z+1/2; (ii) −x+1/2, −y+1, z+1/2; (iii) −x+1/2, −y, z+1/2; (iv) −x, −y, −z+1; (v) −x, −y+1, −z+1; (vi) x−1/2, y, −z+1/2; (vii) −x+1/2, −y, z−1/2; (viii) −x+1/2, −y+1, z−1/2; (ix) −x, −y, −z; (x) −x, −y+1, −z; (xi) x, y, z−1; (xii) x, y, z+1; (xiii) x+1/2, y, −z+3/2. |
Experimental details
(ScTe) | (Y3Au2) | (Y2Au) | |
Crystal data | |||
Chemical formula | ScTe | Y3Au2 | Y2Au |
Mr | 172.56 | 660.66 | 374.79 |
Crystal system, space group | Hexagonal, P63/mmc | Tetragonal, P4/mbm | Orthorhombic, Pnma |
Temperature (K) | 293 | 293 | 293 |
a, b, c (Å) | 4.0969 (6), 4.0969 (6), 13.602 (3) | 8.059 (3), 8.059 (3), 3.907 (3) | 7.115 (3), 4.933 (2), 8.908 (4) |
α, β, γ (°) | 90, 90, 120 | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 197.71 (6) | 253.7 (3) | 312.7 (2) |
Z | 4 | 2 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 17.64 | 91.35 | 83.29 |
Crystal size (mm) | 0.15 × 0.08 × 0.07 | 0.05 × 0.04 × 0.02 | 0.12 × 0.08 × 0.04 |
Data collection | |||
Diffractometer | Bruker SMART CCD area-detector diffractometer | Bruker SMART CCD area-detector diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) | Multi-scan (SADABS; Sheldrick, 1996) | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.177, 0.372 | 0.092, 0.262 | 0.036, 0.135 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1274, 92, 90 | 1866, 194, 156 | 1619, 345, 299 |
Rint | 0.020 | 0.093 | 0.039 |
(sin θ/λ)max (Å−1) | 0.595 | 0.662 | 0.617 |
Refinement | |||
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.081, 1.57 | 0.030, 0.069, 0.93 | 0.026, 0.058, 1.07 |
No. of reflections | 92 | 194 | 345 |
No. of parameters | 8 | 11 | 20 |
Δρmax, Δρmin (e Å−3) | 1.21, −1.65 | 1.46, −1.40 | 1.76, −2.14 |
Computer programs: SMART (Bruker, 2002), SAINT-Plus (Bruker, 2003), SHELXTL (Sheldrick, 2008), DIAMOND (Brandenburg, 2000).
Research within solid-state chemistry on ternary and polynary compounds has attracted much attention during the past few decades because of their interesting structures, bonding and physical properties. Knowledge of binary compounds can provide significant references during the exploratory synthesis of polynary compounds, and their identification is therefore valued. Although many binary combinations of elements are covered by binary phase diagrams and the crystal databases, some have been missed because of the limitations of the earlier experiments. For instance, only two compounds, ScTe and Sc2Te3, were in the Sc–Te phase diagram reported in 1990 (Reference?), missing several examples, Sc2Te, Sc8Te3 and Sc9Te2, which were discovered later during the study of ternary systems (Maggard & Corbett, 1997, 1998, 2000). We discovered that the structure of β-ScTe was still missing, with an inverse Li2O2-type structure, a double hexagonal close-packed (dhcp) version of ScTe (NiAs-type) (Men kov et al., 1961). Y3Au2 was missed in the investigation of the Y–Au phase diagram (Saccone et al., 1997), whereas Y2Au was identified as Co2Si-type (Yakinthos et al., 1978) from lattice parameters only; no refinement of powder diffraction intensities was carried out. The crystal structures of these three phases are described here.
β-ScTe is presumably a high-temperature phase with an inverse Li2O2-type structure. A view of one unit cell approximately along [001] is shown in Fig. 1(a) and a section approximately along [100] is shown in Fig. 1(b), in which Te atoms form hexagonal close-packed (hcp) layers with ABAC··· stacking, leaving all nominal octahedral cavities filled by Sc atoms. Note that ScTe (NiAs-type) crystallizes in the same space group, P63/mmc, with a = 4.130 (5) Å and c = 6.749 (5) Å, and contains simple hcp Te atoms of ABAB··· ordering with Sc atoms occupying the octahedral cavities (Men kov et al., 1961). Therefore, β-ScTe is a stacking variant of ScTe, with a c axis twice as large.
Y3Au2 crystallizes in the U3Si2-type structure in space group P4/mbm (No. 127). An approximately [001] projection along the short 3.907 (3) Å c axis is shown in Fig. 2. The basic building units are an Au2-centered bitrigonal prism (BTP) of Y2 and a Y1-centered Y2 cube. The Au2 unit is an unusual dimer 3.0539 (19) Å long. The two-dimensional motif is created in such a way that each Y2 cube, with the centered Y1 atom on a fourfold axis, interconnects with four identical units through shared Y2–Y2 edges, leaving the cavities filled by the BTPs. The centered Y1 and Au atoms lie on a mirror plane at c = 0. The two-dimensional motif repeats along c to form a three-dimensional network, sharing bitriangular and square faces.
The structure of Y2Au in space group Pnma projected along [010] is shown in Fig. 3, in which each Au atom forms the center of a trigonal prism (TP) of Y1 or Y2 atoms that shares trigonal faces with identical units to generate an infinite one-dimensional column along b. The TPs interconnect with shared Y2–Y2 edges and lead to the formation of puckered sheets along a. Adjoining sheets stack along c, with displacements of b/2, to create a three-dimensional structural network. As a result, each TP is tricapped by two Y1 atoms and one Y2 atom so that each Au atom has nine neighbors. Y2Au is better described as an inverse PbCl2-type structure rather than the earlier reported Co2Si-type, in which the Si atom would have ten neighbors (Flahaut & Thévet, 1980; Liu & Corbett, 2006).