research papers
Following the recent determination of the Al3AuIr structure, a new ternary phase has been identified in the Al–Au–Ir phase diagram. It has a chemical composition Al9(Au;Ir)4 with an apparently low gold content. Its crystal structure has been determined with single-crystal X-ray diffraction. The new compound crystallizes in the tetragonal crystal system and has been successfully solved in space group I41/acd (Pearson symbol tI104) with lattice parameters a = 8.6339 (2) and c = 21.8874 (7) Å. Atomic environments are described as well as similarities with the BGa8Ir4 compound.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520618016712/dq5033sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520618016712/dq5033Isup2.hkl |
CCDC reference: 1881225
Computing details top
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXL2014 (Sheldrick, 2014); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2014).
(I) top
Crystal data top
Al72Au2.50Ir29.50 | Dx = 8.249 Mg m−3 |
Mr = 8104.88 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41/acd | Cell parameters from 9909 reflections |
a = 8.6339 (2) Å | θ = 3.7–44.3° |
c = 21.8874 (7) Å | µ = 66.45 mm−1 |
V = 1631.58 (9) Å3 | T = 296 K |
Z = 1 | Platelet, black |
F(000) = 3405 | 0.05 × 0.05 × 0.01 mm |
Data collection top
Bruker APEX-II QUAZAR CCD diffractometer | 1177 reflections with I > 2σ(I) |
Radiation source: micro sources | Rint = 0.064 |
ω scan | θmax = 44.3°, θmin = 3.8° |
Absorption correction: multi-scan SADABS 2014/5 | h = −16→16 |
Tmin = 0.274, Tmax = 0.749 | k = −16→16 |
44132 measured reflections | l = −42→42 |
1629 independent reflections |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0139P)2 + 16.567P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.017 | (Δ/σ)max = 0.002 |
wR(F2) = 0.043 | Δρmax = 4.05 e Å−3 |
S = 1.13 | Δρmin = −1.85 e Å−3 |
1629 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
35 parameters | Extinction coefficient: 0.000130 (10) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ir1 | 0.0000 | 0.2500 | 0.01467 (2) | 0.00316 (4) | 0.923 (4) |
Au1 | 0.0000 | 0.2500 | 0.01467 (2) | 0.00316 (4) | 0.0782 (4) |
Ir2 | 0.19858 (2) | 0.44858 (2) | 0.1250 | 0.00368 (3) | 0.922 (4) |
Au2 | 0.19858 (2) | 0.44858 (2) | 0.1250 | 0.00368 (3) | 0.0781 (3) |
Al1 | 0.04687 (12) | 0.03071 (12) | 0.31109 (4) | 0.0063 (2) | |
Al2 | 0.27779 (12) | 0.19958 (12) | 0.19068 (5) | 0.0068 (2) | |
Al3 | 0.0000 | 0.2500 | 0.1250 | 0.0060 (3) |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Ir1 | 0.00365 (14) | 0.00361 (13) | 0.00224 (5) | 0.00039 (3) | 0.000 | 0.000 |
Au1 | 0.00365 (14) | 0.00361 (13) | 0.00224 (5) | 0.00039 (3) | 0.000 | 0.000 |
Ir2 | 0.00358 (4) | 0.00358 (4) | 0.00390 (5) | 0.00009 (3) | 0.00000 (3) | 0.00000 (3) |
Au2 | 0.00358 (4) | 0.00358 (4) | 0.00390 (5) | 0.00009 (3) | 0.00000 (3) | 0.00000 (3) |
Al1 | 0.0084 (4) | 0.0049 (4) | 0.0057 (4) | 0.0003 (3) | 0.0004 (3) | 0.0012 (3) |
Al2 | 0.0049 (4) | 0.0091 (4) | 0.0064 (4) | 0.0003 (3) | −0.0010 (3) | −0.0015 (3) |
Al3 | 0.0080 (4) | 0.0080 (4) | 0.0020 (6) | −0.0043 (5) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
Ir1—Al3 | 2.4148 (1) | Al1—Ir1xi | 2.6589 (10) |
Ir1—Al2i | 2.5481 (10) | Al1—Au1xi | 2.6589 (10) |
Ir1—Al2ii | 2.5481 (10) | Al1—Al1xii | 2.726 (2) |
Ir1—Al1iii | 2.5491 (10) | Al1—Al2xiii | 2.7431 (15) |
Ir1—Al1iv | 2.5491 (10) | Al1—Al2ix | 2.7778 (15) |
Ir1—Al2iii | 2.6262 (10) | Al1—Al2xii | 2.8160 (14) |
Ir1—Al2iv | 2.6262 (10) | Al2—Au1xiv | 2.5481 (10) |
Ir1—Al1v | 2.6589 (10) | Al2—Ir1xiv | 2.5481 (10) |
Ir1—Al1vi | 2.6589 (10) | Al2—Au2xv | 2.6086 (10) |
Ir2—Al3 | 2.4247 (1) | Al2—Ir2xv | 2.6086 (10) |
Ir2—Al2vii | 2.6086 (10) | Al2—Ir1iii | 2.6262 (10) |
Ir2—Al2viii | 2.6086 (10) | Al2—Au1iii | 2.6262 (10) |
Ir2—Al1ix | 2.6113 (11) | Al2—Al1xvi | 2.7431 (15) |
Ir2—Al1ii | 2.6113 (11) | Al2—Al1ix | 2.7778 (15) |
Ir2—Al1v | 2.6364 (10) | Al2—Al2ix | 2.780 (2) |
Ir2—Al1x | 2.6364 (10) | Al2—Al1xii | 2.8160 (14) |
Ir2—Al2iii | 2.6751 (11) | Al3—Au1iii | 2.4148 (1) |
Ir2—Al2 | 2.6751 (11) | Al3—Ir1iii | 2.4148 (1) |
Al1—Au1iii | 2.5492 (10) | Al3—Au2xvii | 2.4247 (1) |
Al1—Ir1iii | 2.5492 (10) | Al3—Ir2xvii | 2.4247 (1) |
Al1—Au2ix | 2.6113 (11) | Al3—Al1x | 2.8274 (10) |
Al1—Ir2ix | 2.6113 (11) | Al3—Al1vi | 2.8274 (10) |
Al1—Au2xi | 2.6363 (10) | Al3—Al1v | 2.8274 (10) |
Al1—Ir2xi | 2.6363 (10) | Al3—Al1xii | 2.8274 (10) |
Al3—Ir1—Al2i | 129.46 (2) | Au2ix—Al1—Al2ix | 59.43 (3) |
Al3—Ir1—Al2ii | 129.46 (2) | Ir2ix—Al1—Al2ix | 59.43 (3) |
Al2i—Ir1—Al2ii | 101.08 (5) | Au2xi—Al1—Al2ix | 132.14 (5) |
Al3—Ir1—Al1iii | 130.58 (2) | Ir2xi—Al1—Al2ix | 132.14 (5) |
Al2i—Ir1—Al1iii | 65.12 (4) | Ir1xi—Al1—Al2ix | 147.32 (4) |
Al2ii—Ir1—Al1iii | 66.04 (4) | Au1xi—Al1—Al2ix | 147.32 (4) |
Al3—Ir1—Al1iv | 130.58 (2) | Al1xii—Al1—Al2ix | 98.59 (5) |
Al2i—Ir1—Al1iv | 66.04 (4) | Al2xiii—Al1—Al2ix | 90.90 (4) |
Al2ii—Ir1—Al1iv | 65.12 (4) | Au1iii—Al1—Al2xii | 128.89 (5) |
Al1iii—Ir1—Al1iv | 98.84 (5) | Ir1iii—Al1—Al2xii | 128.89 (5) |
Al3—Ir1—Al2iii | 68.16 (2) | Au2ix—Al1—Al2xii | 57.31 (3) |
Al2i—Ir1—Al2iii | 153.61 (4) | Ir2ix—Al1—Al2xii | 57.31 (3) |
Al2ii—Ir1—Al2iii | 64.99 (4) | Au2xi—Al1—Al2xii | 112.74 (4) |
Al1iii—Ir1—Al2iii | 88.51 (3) | Ir2xi—Al1—Al2xii | 112.74 (4) |
Al1iv—Ir1—Al2iii | 120.67 (3) | Ir1xi—Al1—Al2xii | 57.24 (3) |
Al3—Ir1—Al2iv | 68.16 (2) | Au1xi—Al1—Al2xii | 57.24 (3) |
Al2i—Ir1—Al2iv | 64.99 (4) | Al1xii—Al1—Al2xii | 81.32 (4) |
Al2ii—Ir1—Al2iv | 153.61 (4) | Al2xiii—Al1—Al2xii | 167.09 (5) |
Al1iii—Ir1—Al2iv | 120.67 (3) | Al2ix—Al1—Al2xii | 101.88 (3) |
Al1iv—Ir1—Al2iv | 88.51 (3) | Au1xiv—Al2—Ir1xiv | 0.000 (4) |
Al2iii—Ir1—Al2iv | 136.31 (4) | Au1xiv—Al2—Au2xv | 115.68 (4) |
Al3—Ir1—Al1v | 67.54 (2) | Ir1xiv—Al2—Au2xv | 115.68 (4) |
Al2i—Ir1—Al1v | 106.50 (4) | Au1xiv—Al2—Ir2xv | 115.68 (4) |
Al2ii—Ir1—Al1v | 101.64 (3) | Ir1xiv—Al2—Ir2xv | 115.68 (4) |
Al1iii—Ir1—Al1v | 161.75 (2) | Au2xv—Al2—Ir2xv | 0.000 (2) |
Al1iv—Ir1—Al1v | 63.09 (4) | Au1xiv—Al2—Ir1iii | 115.01 (4) |
Al2iii—Ir1—Al1v | 98.51 (3) | Ir1xiv—Al2—Ir1iii | 115.01 (4) |
Al2iv—Ir1—Al1v | 64.39 (3) | Au2xv—Al2—Ir1iii | 114.47 (4) |
Al3—Ir1—Al1vi | 67.54 (2) | Ir2xv—Al2—Ir1iii | 114.47 (4) |
Al2i—Ir1—Al1vi | 101.64 (3) | Au1xiv—Al2—Au1iii | 115.01 (4) |
Al2ii—Ir1—Al1vi | 106.50 (4) | Ir1xiv—Al2—Au1iii | 115.01 (4) |
Al1iii—Ir1—Al1vi | 63.09 (4) | Au2xv—Al2—Au1iii | 114.47 (4) |
Al1iv—Ir1—Al1vi | 161.75 (2) | Ir2xv—Al2—Au1iii | 114.47 (4) |
Al2iii—Ir1—Al1vi | 64.39 (3) | Ir1iii—Al2—Au1iii | 0.000 (5) |
Al2iv—Ir1—Al1vi | 98.51 (3) | Au1xiv—Al2—Ir2 | 113.37 (4) |
Al1v—Ir1—Al1vi | 135.07 (4) | Ir1xiv—Al2—Ir2 | 113.37 (4) |
Al3—Ir2—Al2vii | 130.00 (2) | Au2xv—Al2—Ir2 | 113.04 (4) |
Al3—Ir2—Al2viii | 130.00 (2) | Ir2xv—Al2—Ir2 | 113.04 (4) |
Al2vii—Ir2—Al2viii | 100.01 (5) | Ir1iii—Al2—Ir2 | 80.40 (3) |
Al3—Ir2—Al1ix | 130.06 (2) | Au1iii—Al2—Ir2 | 80.40 (3) |
Al2vii—Ir2—Al1ix | 65.29 (3) | Au1xiv—Al2—Al1xvi | 57.46 (3) |
Al2viii—Ir2—Al1ix | 65.84 (3) | Ir1xiv—Al2—Al1xvi | 57.46 (3) |
Al3—Ir2—Al1ii | 130.06 (2) | Au2xv—Al2—Al1xvi | 58.96 (3) |
Al2vii—Ir2—Al1ii | 65.84 (3) | Ir2xv—Al2—Al1xvi | 58.96 (3) |
Al2viii—Ir2—Al1ii | 65.29 (3) | Ir1iii—Al2—Al1xvi | 150.09 (5) |
Al1ix—Ir2—Al1ii | 99.88 (4) | Au1iii—Al2—Al1xvi | 150.09 (5) |
Al3—Ir2—Al1v | 67.78 (2) | Ir2—Al2—Al1xvi | 129.50 (5) |
Al2vii—Ir2—Al1v | 159.91 (3) | Au1xiv—Al2—Al1ix | 57.00 (3) |
Al2viii—Ir2—Al1v | 63.06 (3) | Ir1xiv—Al2—Al1ix | 57.00 (3) |
Al1ix—Ir2—Al1v | 96.48 (4) | Au2xv—Al2—Al1ix | 130.25 (4) |
Al1ii—Ir2—Al1v | 111.95 (3) | Ir2xv—Al2—Al1ix | 130.25 (4) |
Al3—Ir2—Al1x | 67.78 (2) | Ir1iii—Al2—Al1ix | 111.34 (4) |
Al2vii—Ir2—Al1x | 63.06 (3) | Au1iii—Al2—Al1ix | 111.34 (4) |
Al2viii—Ir2—Al1x | 159.91 (3) | Ir2—Al2—Al1ix | 57.19 (3) |
Al1ix—Ir2—Al1x | 111.95 (3) | Al1xvi—Al2—Al1ix | 89.07 (4) |
Al1ii—Ir2—Al1x | 96.48 (4) | Au1xiv—Al2—Al2ix | 58.86 (4) |
Al1v—Ir2—Al1x | 135.56 (4) | Ir1xiv—Al2—Al2ix | 58.86 (4) |
Al3—Ir2—Al2iii | 67.20 (2) | Au2xv—Al2—Al2ix | 142.03 (6) |
Al2vii—Ir2—Al2iii | 98.43 (4) | Ir2xv—Al2—Al2ix | 142.03 (6) |
Al2viii—Ir2—Al2iii | 110.58 (3) | Ir1iii—Al2—Al2ix | 56.15 (4) |
Al1ix—Ir2—Al2iii | 161.22 (3) | Au1iii—Al2—Al2ix | 56.15 (4) |
Al1ii—Ir2—Al2iii | 63.38 (3) | Ir2—Al2—Al2ix | 101.89 (5) |
Al1v—Ir2—Al2iii | 97.85 (3) | Al1xvi—Al2—Al2ix | 109.01 (6) |
Al1x—Ir2—Al2iii | 64.56 (3) | Al1ix—Al2—Al2ix | 81.06 (5) |
Al3—Ir2—Al2 | 67.20 (2) | Au1xiv—Al2—Al1xii | 131.49 (5) |
Al2vii—Ir2—Al2 | 110.58 (3) | Ir1xiv—Al2—Al1xii | 131.49 (5) |
Al2viii—Ir2—Al2 | 98.43 (4) | Au2xv—Al2—Al1xii | 57.40 (3) |
Al1ix—Ir2—Al2 | 63.38 (3) | Ir2xv—Al2—Al1xii | 57.40 (3) |
Al1ii—Ir2—Al2 | 161.22 (3) | Ir1iii—Al2—Al1xii | 58.37 (3) |
Al1v—Ir2—Al2 | 64.56 (3) | Au1iii—Al2—Al1xii | 58.37 (3) |
Al1x—Ir2—Al2 | 97.85 (3) | Ir2—Al2—Al1xii | 112.27 (4) |
Al2iii—Ir2—Al2 | 134.40 (4) | Al1xvi—Al2—Al1xii | 102.95 (4) |
Au1iii—Al1—Ir1iii | 0.000 (4) | Al1ix—Al2—Al1xii | 167.85 (5) |
Au1iii—Al1—Au2ix | 115.54 (4) | Al2ix—Al2—Al1xii | 96.42 (5) |
Ir1iii—Al1—Au2ix | 115.54 (4) | Ir1—Al3—Au1iii | 180.0 |
Au1iii—Al1—Ir2ix | 115.54 (4) | Ir1—Al3—Ir1iii | 180.0 |
Ir1iii—Al1—Ir2ix | 115.54 (4) | Au1iii—Al3—Ir1iii | 0.0 |
Au2ix—Al1—Ir2ix | 0.000 (6) | Ir1—Al3—Ir2 | 90.0 |
Au1iii—Al1—Au2xi | 114.67 (4) | Au1iii—Al3—Ir2 | 90.0 |
Ir1iii—Al1—Au2xi | 114.67 (4) | Ir1iii—Al3—Ir2 | 90.0 |
Au2ix—Al1—Au2xi | 114.25 (4) | Ir1—Al3—Au2xvii | 90.0 |
Ir2ix—Al1—Au2xi | 114.25 (4) | Au1iii—Al3—Au2xvii | 90.0 |
Au1iii—Al1—Ir2xi | 114.67 (4) | Ir1iii—Al3—Au2xvii | 90.0 |
Ir1iii—Al1—Ir2xi | 114.67 (4) | Ir2—Al3—Au2xvii | 180.0 |
Au2ix—Al1—Ir2xi | 114.25 (4) | Ir1—Al3—Ir2xvii | 90.0 |
Ir2ix—Al1—Ir2xi | 114.25 (4) | Au1iii—Al3—Ir2xvii | 90.0 |
Au2xi—Al1—Ir2xi | 0.000 (1) | Ir1iii—Al3—Ir2xvii | 90.0 |
Au1iii—Al1—Ir1xi | 113.85 (4) | Ir2—Al3—Ir2xvii | 180.0 |
Ir1iii—Al1—Ir1xi | 113.85 (4) | Au2xvii—Al3—Ir2xvii | 0.000 (6) |
Au2ix—Al1—Ir1xi | 113.28 (4) | Ir1—Al3—Al1x | 119.65 (2) |
Ir2ix—Al1—Ir1xi | 113.28 (4) | Au1iii—Al3—Al1x | 60.35 (2) |
Au2xi—Al1—Ir1xi | 80.52 (3) | Ir1iii—Al3—Al1x | 60.35 (2) |
Ir2xi—Al1—Ir1xi | 80.52 (3) | Ir2—Al3—Al1x | 59.67 (2) |
Au1iii—Al1—Au1xi | 113.85 (4) | Au2xvii—Al3—Al1x | 120.33 (2) |
Ir1iii—Al1—Au1xi | 113.85 (4) | Ir2xvii—Al3—Al1x | 120.33 (2) |
Au2ix—Al1—Au1xi | 113.28 (4) | Ir1—Al3—Al1vi | 60.35 (2) |
Ir2ix—Al1—Au1xi | 113.28 (4) | Au1iii—Al3—Al1vi | 119.65 (2) |
Au2xi—Al1—Au1xi | 80.52 (3) | Ir1iii—Al3—Al1vi | 119.65 (2) |
Ir2xi—Al1—Au1xi | 80.52 (3) | Ir2—Al3—Al1vi | 120.33 (2) |
Ir1xi—Al1—Au1xi | 0.000 (5) | Au2xvii—Al3—Al1vi | 59.67 (2) |
Au1iii—Al1—Al1xii | 60.42 (4) | Ir2xvii—Al3—Al1vi | 59.67 (2) |
Ir1iii—Al1—Al1xii | 60.42 (4) | Al1x—Al3—Al1vi | 89.97 (4) |
Au2ix—Al1—Al1xii | 122.60 (2) | Ir1—Al3—Al1v | 60.35 (2) |
Ir2ix—Al1—Al1xii | 122.60 (2) | Au1iii—Al3—Al1v | 119.65 (2) |
Au2xi—Al1—Al1xii | 117.91 (3) | Ir1iii—Al3—Al1v | 119.65 (2) |
Ir2xi—Al1—Al1xii | 117.91 (3) | Ir2—Al3—Al1v | 59.67 (2) |
Ir1xi—Al1—Al1xii | 56.49 (4) | Au2xvii—Al3—Al1v | 120.33 (2) |
Au1xi—Al1—Al1xii | 56.49 (4) | Ir2xvii—Al3—Al1v | 120.33 (2) |
Au1iii—Al1—Al2xiii | 57.42 (3) | Al1x—Al3—Al1v | 119.35 (4) |
Ir1iii—Al1—Al2xiii | 57.42 (3) | Al1vi—Al3—Al1v | 120.69 (4) |
Au2ix—Al1—Al2xiii | 133.16 (5) | Ir1—Al3—Al1xii | 119.65 (2) |
Ir2ix—Al1—Al2xiii | 133.16 (5) | Au1iii—Al3—Al1xii | 60.35 (2) |
Au2xi—Al1—Al2xiii | 57.97 (3) | Ir1iii—Al3—Al1xii | 60.35 (2) |
Ir2xi—Al1—Al2xiii | 57.97 (3) | Ir2—Al3—Al1xii | 120.33 (2) |
Ir1xi—Al1—Al2xiii | 110.50 (4) | Au2xvii—Al3—Al1xii | 59.67 (2) |
Au1xi—Al1—Al2xiii | 110.50 (4) | Ir2xvii—Al3—Al1xii | 59.67 (2) |
Al1xii—Al1—Al2xiii | 95.13 (4) | Al1x—Al3—Al1xii | 120.69 (4) |
Au1iii—Al1—Al2ix | 56.96 (3) | Al1vi—Al3—Al1xii | 119.35 (4) |
Ir1iii—Al1—Al2ix | 56.96 (3) | Al1v—Al3—Al1xii | 89.97 (4) |
Symmetry codes: (i) y−1/4, x−1/4, z−1/4; (ii) −y+1/4, −x+3/4, z−1/4; (iii) y−1/4, x+1/4, −z+1/4; (iv) −y+1/4, −x+1/4, −z+1/4; (v) y+1/4, −x+1/4, z−1/4; (vi) −y−1/4, x+1/4, z−1/4; (vii) −x+1/2, y+1/2, z; (viii) y+1/4, −x+3/4, −z+1/4; (ix) −x+1/2, −y+1/2, −z+1/2; (x) −x, y+1/2, −z+1/2; (xi) −y+1/4, x−1/4, z+1/4; (xii) x, −y, −z+1/2; (xiii) x−1/2, y, −z+1/2; (xiv) −y+3/4, −x+1/4, z+1/4; (xv) −y+3/4, x−1/4, −z+1/4; (xvi) x+1/2, y, −z+1/2; (xvii) −x, −y+1/2, z. |