Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768109026986/ck5035sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768109026986/ck5035Isup2.hkl |
Data collection: X-AREA, STOE, 2006; cell refinement: X-AREA, STOE, 2006; data reduction: X-AREA, STOE, 2002; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: Jana2000 (Petricek, Dusek & Palatinus, 2000); molecular graphics: DIAMOND-Visuelles Informationssystem für Kristallstrukturen (G. Bergerhoff, Bonn, 1999); software used to prepare material for publication: Jana2000 (Petricek, Dusek & Palatinus, 2000).
As2AuCe | Z = 4 |
Mr = 486.93 | F(000) = 808 |
Monoclinic, P21/m(α0γ)00† | Dx = 9.41 Mg m−3 |
q = 0.08000a* + -0.38890c* | Mo Kα radiation, λ = 0.71073 Å |
a = 5.8040 (1) Å | µ = 74.55 mm−1 |
b = 5.8140 (1) Å | T = 293 K |
c = 10.1790 (1) Å | , black |
β = 90.09 (8)° | 0.14 × 0.14 × 0.004 mm |
V = 343.48 (9) Å3 |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, 1/2+x2, −x3, −x4; (3) −x1, −x2, −x3, −x4; (4) x1, 1/2−x2, x3, x4. |
STOE IPDS 2 diffractometer | 4210 independent reflections |
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus | 1422 reflections with I > 3σ(I) |
Plane graphite monochromator | Rint = 0.068 |
Detector resolution: 6.67 pixels mm-1 | θmax = 33.5°, θmin = 2.8° |
ω scans | h = −9→9 |
Absorption correction: numerical (Jana2000; Petricek, Dusek & Palatinus, 2000) | k = −8→8 |
Tmin = 0.015, Tmax = 0.306 | l = −16→14 |
20909 measured reflections |
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
R[F2 > 2σ(F2)] = 0.034 | (Δ/σ)max = 0.041 |
wR(F2) = 0.040 | Δρmax = 2.49 e Å−3 |
S = 1.25 | Δρmin = −2.29 e Å−3 |
4210 reflections | Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) |
134 parameters | Extinction coefficient: 0.53 (2) |
As2AuCe | β = 90.09 (8)° |
Mr = 486.93 | V = 343.48 (9) Å3 |
Monoclinic, P21/m(α0γ)00† | Z = 4 |
q = 0.08000a* + -0.38890c* | Mo Kα radiation |
a = 5.8040 (1) Å | µ = 74.55 mm−1 |
b = 5.8140 (1) Å | T = 293 K |
c = 10.1790 (1) Å | 0.14 × 0.14 × 0.004 mm |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, 1/2+x2, −x3, −x4; (3) −x1, −x2, −x3, −x4; (4) x1, 1/2−x2, x3, x4. |
STOE IPDS 2 diffractometer | 4210 independent reflections |
Absorption correction: numerical (Jana2000; Petricek, Dusek & Palatinus, 2000) | 1422 reflections with I > 3σ(I) |
Tmin = 0.015, Tmax = 0.306 | Rint = 0.068 |
20909 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | 134 parameters |
wR(F2) = 0.040 | Δρmax = 2.49 e Å−3 |
S = 1.25 | Δρmin = −2.29 e Å−3 |
4210 reflections |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ce1 | 0.0005 (4) | 0.25 | 0.23003 (4) | 0.01262 (12) | |
Ce2 | 0.5001 (4) | 0.75 | 0.24019 (4) | 0.01220 (13) | |
Au1 | 0.24822 (4) | −0.0005 (2) | 0.49929 (10) | 0.01869 (7) | 0.9858 (17) |
As1 | 0.9978 (6) | 0.25 | 0.68044 (9) | 0.0142 (2) | |
As2 | 0.4991 (6) | 0.75 | 0.67811 (8) | 0.0141 (2) | |
As3 | 0.27901 (14) | −0.0038 (6) | 0.0001 (3) | 0.02084 (18) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ce1 | 0.0136 (2) | 0.0104 (2) | 0.0139 (2) | 0 | 0.0004 (8) | 0 |
Ce2 | 0.0142 (2) | 0.0101 (2) | 0.0122 (2) | 0 | −0.0019 (9) | 0 |
Au1 | 0.02132 (13) | 0.01698 (10) | 0.01778 (11) | −0.0024 (3) | −0.0011 (7) | −0.00082 (10) |
As1 | 0.0140 (4) | 0.0106 (3) | 0.0179 (4) | 0 | −0.0090 (12) | 0 |
As2 | 0.0142 (4) | 0.0111 (3) | 0.0169 (4) | 0 | −0.0079 (12) | 0 |
As3 | 0.0148 (3) | 0.0352 (4) | 0.0124 (2) | 0.0049 (9) | −0.0025 (11) | −0.0019 (3) |
Average | Minimum | Maximum | |
Ce1—Au1 | 3.419 (3) | 3.389 (3) | 3.449 (3) |
Ce1—Au1i | 3.434 (3) | 3.418 (3) | 3.450 (3) |
Ce1—Au1ii | 3.434 (3) | 3.418 (3) | 3.450 (3) |
Ce1—Au1iii | 3.419 (3) | 3.389 (3) | 3.449 (3) |
Ce1—As1iv | 3.0465 (14) | 3.0416 (14) | 3.0515 (14) |
Ce1—As1v | 3.0465 (14) | 3.0416 (14) | 3.0515 (14) |
Ce1—As2vi | 3.048 (5) | 3.024 (5) | 3.071 (5) |
Ce1—As2v | 3.050 (5) | 3.040 (5) | 3.060 (5) |
Ce1—As3 | 3.207 (4) | 3.177 (5) | 3.237 (5) |
Ce1—As3vii | 3.187 (4) | 3.159 (5) | 3.217 (5) |
Ce1—As3viii | 3.187 (4) | 3.159 (5) | 3.217 (5) |
Ce1—As3iii | 3.207 (4) | 3.177 (5) | 3.237 (5) |
Ce2—Au1ix | 3.348 (3) | 3.312 (3) | 3.385 (3) |
Ce2—Au1v | 3.358 (3) | 3.344 (3) | 3.373 (3) |
Ce2—Au1x | 3.358 (3) | 3.344 (3) | 3.373 (3) |
Ce2—Au1iii | 3.348 (3) | 3.312 (3) | 3.385 (3) |
Ce2—As1v | 3.002 (5) | 2.974 (5) | 3.029 (5) |
Ce2—As1xi | 3.023 (5) | 3.012 (5) | 3.034 (5) |
Ce2—As2v | 3.0237 (13) | 3.0186 (12) | 3.0287 (13) |
Ce2—As2xii | 3.0237 (13) | 3.0186 (12) | 3.0287 (13) |
Ce2—As3ix | 3.107 (4) | 3.065 (5) | 3.151 (5) |
Ce2—As3xiii | 3.134 (4) | 3.080 (5) | 3.188 (5) |
Ce2—As3xiv | 3.134 (4) | 3.080 (5) | 3.188 (5) |
Ce2—As3iii | 3.107 (4) | 3.065 (5) | 3.151 (5) |
Au1—Au1i | 2.8815 (18) | 2.870 (3) | 2.893 (3) |
Au1—Au1iv | 2.9227 (18) | 2.913 (3) | 2.932 (3) |
Au1—Au1xv | 2.901 (2) | 2.889 (2) | 2.914 (2) |
Au1—Au1iii | 2.913 (2) | 2.900 (2) | 2.925 (2) |
Au1—As1xvi | 2.765 (4) | 2.735 (4) | 2.795 (4) |
Au1—As1iv | 2.735 (4) | 2.718 (4) | 2.753 (4) |
Au1—As2xvii | 2.744 (4) | 2.720 (4) | 2.767 (4) |
Au1—As2v | 2.747 (4) | 2.719 (4) | 2.773 (4) |
As3—As3vii | 3.241 (5) | 3.211 (6) | 3.275 (6) |
As3—As3xviii | 2.569 (5) | 2.519 (6) | 2.623 (6) |
As3—As3xv | 2.861 (6) | 2.699 (5) | 3.026 (5) |
As3—As3iii | 2.953 (6) | 2.788 (5) | 3.115 (5) |
Symmetry codes: (i) −x1, −x2, −x3+1, −x4; (ii) −x1, x2+1/2, −x3+1, −x4; (iii) x1, −x2+1/2, x3, x4; (iv) −x1+1, −x2, −x3+1, −x4; (v) −x1+1, −x2+1, −x3+1, −x4; (vi) −x1, −x2+1, −x3+1, −x4; (vii) −x1, −x2, −x3, −x4; (viii) −x1, x2+1/2, −x3, −x4; (ix) x1, x2+1, x3, x4; (x) −x1+1, x2+1/2, −x3+1, −x4; (xi) −x1+2, −x2+1, −x3+1, −x4; (xii) −x1+1, −x2+2, −x3+1, −x4; (xiii) −x1+1, −x2+1, −x3, −x4; (xiv) −x1+1, x2+1/2, −x3, −x4; (xv) x1, −x2−1/2, x3, x4; (xvi) x1−1, x2, x3, x4; (xvii) x1, x2−1, x3, x4; (xviii) −x1+1, −x2, −x3, −x4. |
Experimental details
Crystal data | |
Chemical formula | As2AuCe |
Mr | 486.93 |
Crystal system, space group | Monoclinic, P21/m(α0γ)00† |
Temperature (K) | 293 |
Wave vectors | q = 0.08000a* + -0.38890c* |
a, b, c (Å) | 5.8040 (1), 5.8140 (1), 10.1790 (1) |
β (°) | 90.09 (8) |
V (Å3) | 343.48 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 74.55 |
Crystal size (mm) | 0.14 × 0.14 × 0.004 |
Data collection | |
Diffractometer | STOE IPDS 2 diffractometer |
Absorption correction | Numerical (Jana2000; Petricek, Dusek & Palatinus, 2000) |
Tmin, Tmax | 0.015, 0.306 |
No. of measured, independent and observed [I > 3σ(I)] reflections | 20909, 4210, 1422 |
Rint | 0.068 |
(sin θ/λ)max (Å−1) | 0.776 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.040, 1.25 |
No. of reflections | 4210 |
No. of parameters | 134 |
No. of restraints | ? |
Δρmax, Δρmin (e Å−3) | 2.49, −2.29 |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, 1/2+x2, −x3, −x4; (3) −x1, −x2, −x3, −x4; (4) x1, 1/2−x2, x3, x4.
Computer programs: X-AREA, STOE, 2006, X-AREA, STOE, 2002, SHELXS97 (Sheldrick, 1997), Jana2000 (Petricek, Dusek & Palatinus, 2000), DIAMOND-Visuelles Informationssystem für Kristallstrukturen (G. Bergerhoff, Bonn, 1999).
Average | Minimum | Maximum | |
Ce1—Au1 | 3.419 (3) | 3.389 (3) | 3.449 (3) |
Ce1—Au1i | 3.434 (3) | 3.418 (3) | 3.450 (3) |
Ce1—Au1ii | 3.434 (3) | 3.418 (3) | 3.450 (3) |
Ce1—Au1iii | 3.419 (3) | 3.389 (3) | 3.449 (3) |
Ce1—As1iv | 3.0465 (14) | 3.0416 (14) | 3.0515 (14) |
Ce1—As1v | 3.0465 (14) | 3.0416 (14) | 3.0515 (14) |
Ce1—As2vi | 3.048 (5) | 3.024 (5) | 3.071 (5) |
Ce1—As2v | 3.050 (5) | 3.040 (5) | 3.060 (5) |
Ce1—As3 | 3.207 (4) | 3.177 (5) | 3.237 (5) |
Ce1—As3vii | 3.187 (4) | 3.159 (5) | 3.217 (5) |
Ce1—As3viii | 3.187 (4) | 3.159 (5) | 3.217 (5) |
Ce1—As3iii | 3.207 (4) | 3.177 (5) | 3.237 (5) |
Ce2—Au1ix | 3.348 (3) | 3.312 (3) | 3.385 (3) |
Ce2—Au1v | 3.358 (3) | 3.344 (3) | 3.373 (3) |
Ce2—Au1x | 3.358 (3) | 3.344 (3) | 3.373 (3) |
Ce2—Au1iii | 3.348 (3) | 3.312 (3) | 3.385 (3) |
Ce2—As1v | 3.002 (5) | 2.974 (5) | 3.029 (5) |
Ce2—As1xi | 3.023 (5) | 3.012 (5) | 3.034 (5) |
Ce2—As2v | 3.0237 (13) | 3.0186 (12) | 3.0287 (13) |
Ce2—As2xii | 3.0237 (13) | 3.0186 (12) | 3.0287 (13) |
Ce2—As3ix | 3.107 (4) | 3.065 (5) | 3.151 (5) |
Ce2—As3xiii | 3.134 (4) | 3.080 (5) | 3.188 (5) |
Ce2—As3xiv | 3.134 (4) | 3.080 (5) | 3.188 (5) |
Ce2—As3iii | 3.107 (4) | 3.065 (5) | 3.151 (5) |
Au1—Au1i | 2.8815 (18) | 2.870 (3) | 2.893 (3) |
Au1—Au1iv | 2.9227 (18) | 2.913 (3) | 2.932 (3) |
Au1—Au1xv | 2.901 (2) | 2.889 (2) | 2.914 (2) |
Au1—Au1iii | 2.913 (2) | 2.900 (2) | 2.925 (2) |
Au1—As1xvi | 2.765 (4) | 2.735 (4) | 2.795 (4) |
Au1—As1iv | 2.735 (4) | 2.718 (4) | 2.753 (4) |
Au1—As2xvii | 2.744 (4) | 2.720 (4) | 2.767 (4) |
Au1—As2v | 2.747 (4) | 2.719 (4) | 2.773 (4) |
As3—As3vii | 3.241 (5) | 3.211 (6) | 3.275 (6) |
As3—As3xviii | 2.569 (5) | 2.519 (6) | 2.623 (6) |
As3—As3xv | 2.861 (6) | 2.699 (5) | 3.026 (5) |
As3—As3iii | 2.953 (6) | 2.788 (5) | 3.115 (5) |
Symmetry codes: (i) −x1, −x2, −x3+1, −x4; (ii) −x1, x2+1/2, −x3+1, −x4; (iii) x1, −x2+1/2, x3, x4; (iv) −x1+1, −x2, −x3+1, −x4; (v) −x1+1, −x2+1, −x3+1, −x4; (vi) −x1, −x2+1, −x3+1, −x4; (vii) −x1, −x2, −x3, −x4; (viii) −x1, x2+1/2, −x3, −x4; (ix) x1, x2+1, x3, x4; (x) −x1+1, x2+1/2, −x3+1, −x4; (xi) −x1+2, −x2+1, −x3+1, −x4; (xii) −x1+1, −x2+2, −x3+1, −x4; (xiii) −x1+1, −x2+1, −x3, −x4; (xiv) −x1+1, x2+1/2, −x3, −x4; (xv) x1, −x2−1/2, x3, x4; (xvi) x1−1, x2, x3, x4; (xvii) x1, x2−1, x3, x4; (xviii) −x1+1, −x2, −x3, −x4. |