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Single crystals of dicerium trialuminium tetragermanide, Ce2Al3Ge4, have been synthesized from a high-temperature reaction using an eutectic mixture of Al and Ge as a metal flux. Through single-crystal X-ray diffraction it was established that Ce2Al3Ge4 crystallizes in the centrosymmetric space group Cmce (No. 64) with the Ba2Cd3Bi4 structure type (Pearson code oC36). Five atoms compose the asymmetric unit, i.e. one Ce, two Al, and two Ge atoms, all in special positions with Wyckoff symbols 8f (Ce), 4a and 8e (Al), and 8e and 8f (Ge). The structure can be described as a three-dimensional network of Al and Ge atoms, with Ce atoms occupying the cavities of the framework.
Supporting information
CCDC reference: 2055324
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXTL (Bruker, 2002); program(s) used to refine structure: SHELXTL (Bruker, 2002); molecular graphics: XP in SHELXTL (Bruker, 2002); software used to prepare material for publication: SHELXTL (Bruker, 2002).
Dicerium trialuminium tetragermanide
top
Crystal data top
Ce2Al3Ge4 | F(000) = 1132 |
Mr = 651.54 | Dx = 5.980 Mg m−3 |
Orthorhombic, Cmce | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2bc 2 | Cell parameters from 402 reflections |
a = 6.0581 (17) Å | θ = 2.7–26.3° |
b = 15.045 (4) Å | µ = 28.97 mm−1 |
c = 7.940 (2) Å | T = 120 K |
V = 723.7 (4) Å3 | Plate, silver |
Z = 4 | 0.05 × 0.05 × 0.04 mm |
Data collection top
Bruker SMART CCD area detector diffractometer | 402 independent reflections |
Radiation source: fine-focus sealed tube | 371 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
phi and ω scans | θmax = 26.3°, θmin = 2.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | h = −7→7 |
Tmin = 0.259, Tmax = 0.316 | k = −18→18 |
1830 measured reflections | l = −9→9 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.022 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.050 | w = 1/[σ2(Fo2) + (0.026P)2 + 1.7964P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max < 0.001 |
402 reflections | Δρmax = 1.00 e Å−3 |
27 parameters | Δρmin = −0.99 e Å−3 |
Special details top
Experimental. Crystals were selected in the glove box and cut in a Paratone N
oil bath to the desired dimensions. A suitable crystal was
then chosen mounted on the tip of a glass fiber and quickly
placed under the cold nitrogen stream (ca. 120 K) in a Bruker SMART
CCD-based diffractometer. Data collection is performed with four batch runs at
φ = 0.00 ° (450 frames), at φ = 90.00 °
(450 frames), at φ = 180.00 ° (450 frames),
and at φ = 270.00 (450 frames). Frame width
= 0.40 ° in ω. Data are merged, corrected for decay,
and treated with multi-scan absorption corrections. |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds 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 > 2sigma(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ce | 0.0000 | 0.11385 (3) | 0.41715 (6) | 0.00871 (17) | |
Ge1 | 0.0000 | 0.18655 (5) | 0.05260 (11) | 0.0093 (2) | |
Ge2 | 0.2500 | 0.45123 (5) | 0.2500 | 0.0109 (2) | |
Al1 | 0.2500 | 0.28384 (14) | 0.2500 | 0.0074 (5) | |
Al2 | 0.0000 | 0.0000 | 0.0000 | 0.0140 (8) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ce | 0.0076 (3) | 0.0091 (2) | 0.0094 (3) | 0.000 | 0.000 | 0.00012 (15) |
Ge1 | 0.0082 (5) | 0.0097 (4) | 0.0100 (4) | 0.000 | 0.000 | 0.0003 (3) |
Ge2 | 0.0122 (5) | 0.0099 (4) | 0.0107 (5) | 0.000 | −0.0012 (4) | 0.000 |
Al1 | 0.0090 (13) | 0.0045 (10) | 0.0087 (12) | 0.000 | −0.0047 (10) | 0.000 |
Al2 | 0.0065 (18) | 0.0226 (18) | 0.0129 (19) | 0.000 | 0.000 | 0.0083 (14) |
Geometric parameters (Å, º) top
Ce—Ge1 | 3.0944 (12) | Ge2—Al2iii | 2.6025 (5) |
Ce—Ge2i | 3.1688 (9) | Ge2—Al2ix | 2.6025 (6) |
Ce—Ge2ii | 3.1688 (9) | Ge2—Ceix | 3.1688 (9) |
Ce—Ge1iii | 3.1897 (12) | Ge2—Cex | 3.1688 (9) |
Ce—Ge2iv | 3.1996 (8) | Ge2—Cevii | 3.1996 (8) |
Ce—Ge2iii | 3.1996 (8) | Ge2—Ceiv | 3.1996 (8) |
Ce—Ge1v | 3.2294 (9) | Al1—Ge1v | 2.6254 (14) |
Ce—Ge1vi | 3.2294 (9) | Al1—Ge1iii | 2.8750 (10) |
Ce—Al1vi | 3.2551 (18) | Al1—Ge1viii | 2.8750 (10) |
Ce—Al1 | 3.2551 (18) | Al1—Cev | 3.2551 (18) |
Ce—Al1iv | 3.4129 (12) | Al1—Ceiv | 3.4129 (12) |
Ce—Al1iii | 3.4129 (12) | Al1—Cevii | 3.4129 (12) |
Ge1—Al1vi | 2.6254 (14) | Al2—Ge2ii | 2.6025 (5) |
Ge1—Al1 | 2.6254 (14) | Al2—Ge2vii | 2.6025 (5) |
Ge1—Al2 | 2.8375 (11) | Al2—Ge2viii | 2.6025 (5) |
Ge1—Al1vii | 2.8750 (10) | Al2—Ge2i | 2.6025 (5) |
Ge1—Al1viii | 2.8750 (10) | Al2—Ge1xi | 2.8375 (11) |
Ge1—Cevii | 3.1897 (12) | Al2—Cev | 3.5414 (8) |
Ge1—Cevi | 3.2294 (9) | Al2—Cexii | 3.5414 (8) |
Ge1—Cev | 3.2294 (9) | Al2—Cevi | 3.5414 (8) |
Ge2—Al1 | 2.518 (2) | Al2—Cexiii | 3.5414 (8) |
| | | |
Ge1—Ce—Ge2i | 83.17 (2) | Al1—Ge2—Al2iii | 106.377 (17) |
Ge1—Ce—Ge2ii | 83.17 (2) | Al1—Ge2—Al2ix | 106.377 (17) |
Ge2i—Ce—Ge2ii | 57.10 (2) | Al2iii—Ge2—Al2ix | 147.25 (3) |
Ge1—Ce—Ge1iii | 89.01 (2) | Al1—Ge2—Ceix | 140.542 (15) |
Ge2i—Ce—Ge1iii | 150.240 (13) | Al2iii—Ge2—Ceix | 74.99 (2) |
Ge2ii—Ce—Ge1iii | 150.240 (13) | Al2ix—Ge2—Ceix | 79.84 (2) |
Ge1—Ce—Ge2iv | 151.745 (10) | Al1—Ge2—Cex | 140.542 (14) |
Ge2i—Ce—Ge2iv | 109.63 (2) | Al2iii—Ge2—Cex | 79.84 (2) |
Ge2ii—Ce—Ge2iv | 83.309 (19) | Al2ix—Ge2—Cex | 74.99 (2) |
Ge1iii—Ce—Ge2iv | 90.55 (3) | Ceix—Ge2—Cex | 78.92 (3) |
Ge1—Ce—Ge2iii | 151.745 (10) | Al1—Ge2—Cevii | 72.182 (16) |
Ge2i—Ce—Ge2iii | 83.309 (19) | Al2iii—Ge2—Cevii | 116.16 (2) |
Ge2ii—Ce—Ge2iii | 109.63 (2) | Al2ix—Ge2—Cevii | 74.44 (2) |
Ge1iii—Ce—Ge2iii | 90.55 (3) | Ceix—Ge2—Cevii | 143.95 (2) |
Ge2iv—Ce—Ge2iii | 56.50 (2) | Cex—Ge2—Cevii | 70.37 (2) |
Ge1—Ce—Ge1v | 87.12 (2) | Al1—Ge2—Ceiv | 72.182 (16) |
Ge2i—Ce—Ge1v | 137.811 (18) | Al2iii—Ge2—Ceiv | 74.44 (2) |
Ge2ii—Ce—Ge1v | 81.05 (2) | Al2ix—Ge2—Ceiv | 116.16 (2) |
Ge1iii—Ce—Ge1v | 69.884 (17) | Ceix—Ge2—Ceiv | 70.37 (2) |
Ge2iv—Ce—Ge1v | 66.311 (19) | Cex—Ge2—Ceiv | 143.95 (2) |
Ge2iii—Ce—Ge1v | 119.09 (2) | Cevii—Ge2—Ceiv | 144.36 (3) |
Ge1—Ce—Ge1vi | 87.12 (2) | Ge2—Al1—Ge1 | 123.88 (4) |
Ge2i—Ce—Ge1vi | 81.05 (2) | Ge2—Al1—Ge1v | 123.88 (4) |
Ge2ii—Ce—Ge1vi | 137.811 (18) | Ge1—Al1—Ge1v | 112.23 (9) |
Ge1iii—Ce—Ge1vi | 69.884 (17) | Ge2—Al1—Ge1iii | 81.09 (4) |
Ge2iv—Ce—Ge1vi | 119.09 (2) | Ge1—Al1—Ge1iii | 106.35 (3) |
Ge2iii—Ce—Ge1vi | 66.311 (19) | Ge1v—Al1—Ge1iii | 83.76 (3) |
Ge1v—Ce—Ge1vi | 139.42 (3) | Ge2—Al1—Ge1viii | 81.09 (4) |
Ge1—Ce—Al1vi | 48.766 (16) | Ge1—Al1—Ge1viii | 83.76 (3) |
Ge2i—Ce—Al1vi | 102.32 (3) | Ge1v—Al1—Ge1viii | 106.35 (3) |
Ge2ii—Ce—Al1vi | 131.16 (3) | Ge1iii—Al1—Ge1viii | 162.17 (9) |
Ge1iii—Ce—Al1vi | 52.97 (3) | Ge2—Al1—Cev | 141.78 (3) |
Ge2iv—Ce—Al1vi | 142.89 (3) | Ge1—Al1—Cev | 65.61 (4) |
Ge2iii—Ce—Al1vi | 110.914 (18) | Ge1v—Al1—Cev | 62.42 (4) |
Ge1v—Ce—Al1vi | 101.57 (3) | Ge1iii—Al1—Cev | 135.04 (6) |
Ge1vi—Ce—Al1vi | 47.764 (18) | Ge1viii—Al1—Cev | 62.35 (3) |
Ge1—Ce—Al1 | 48.766 (16) | Ge2—Al1—Ce | 141.78 (3) |
Ge2i—Ce—Al1 | 131.16 (3) | Ge1—Al1—Ce | 62.42 (4) |
Ge2ii—Ce—Al1 | 102.32 (3) | Ge1v—Al1—Ce | 65.60 (4) |
Ge1iii—Ce—Al1 | 52.97 (3) | Ge1iii—Al1—Ce | 62.35 (3) |
Ge2iv—Ce—Al1 | 110.914 (18) | Ge1viii—Al1—Ce | 135.04 (6) |
Ge2iii—Ce—Al1 | 142.89 (3) | Cev—Al1—Ce | 76.44 (5) |
Ge1v—Ce—Al1 | 47.764 (18) | Ge2—Al1—Ceiv | 63.19 (3) |
Ge1vi—Ce—Al1 | 101.57 (3) | Ge1—Al1—Ceiv | 165.87 (4) |
Al1vi—Ce—Al1 | 55.46 (4) | Ge1v—Al1—Ceiv | 62.17 (3) |
Ge1—Ce—Al1iv | 124.40 (4) | Ge1iii—Al1—Ceiv | 61.10 (3) |
Ge2i—Ce—Al1iv | 152.21 (3) | Ge1viii—Al1—Ceiv | 110.09 (4) |
Ge2ii—Ce—Al1iv | 117.42 (3) | Cev—Al1—Ceiv | 117.62 (3) |
Ge1iii—Ce—Al1iv | 46.71 (3) | Ce—Al1—Ceiv | 104.19 (2) |
Ge2iv—Ce—Al1iv | 44.63 (4) | Ge2—Al1—Cevii | 63.19 (3) |
Ge2iii—Ce—Al1iv | 73.05 (3) | Ge1—Al1—Cevii | 62.17 (3) |
Ge1v—Ce—Al1iv | 51.203 (17) | Ge1v—Al1—Cevii | 165.87 (4) |
Ge1vi—Ce—Al1iv | 101.88 (3) | Ge1iii—Al1—Cevii | 110.09 (4) |
Al1vi—Ce—Al1iv | 99.66 (2) | Ge1viii—Al1—Cevii | 61.10 (3) |
Al1—Ce—Al1iv | 75.81 (2) | Cev—Al1—Cevii | 104.19 (2) |
Ge1—Ce—Al1iii | 124.40 (4) | Ce—Al1—Cevii | 117.62 (3) |
Ge2i—Ce—Al1iii | 117.42 (3) | Ceiv—Al1—Cevii | 126.38 (7) |
Ge2ii—Ce—Al1iii | 152.21 (3) | Ge2ii—Al2—Ge2vii | 180.00 (3) |
Ge1iii—Ce—Al1iii | 46.71 (3) | Ge2ii—Al2—Ge2viii | 108.82 (2) |
Ge2iv—Ce—Al1iii | 73.05 (3) | Ge2vii—Al2—Ge2viii | 71.18 (2) |
Ge2iii—Ce—Al1iii | 44.63 (4) | Ge2ii—Al2—Ge2i | 71.18 (2) |
Ge1v—Ce—Al1iii | 101.88 (3) | Ge2vii—Al2—Ge2i | 108.82 (2) |
Ge1vi—Ce—Al1iii | 51.203 (17) | Ge2viii—Al2—Ge2i | 180.00 (3) |
Al1vi—Ce—Al1iii | 75.81 (2) | Ge2ii—Al2—Ge1xi | 80.41 (2) |
Al1—Ce—Al1iii | 99.66 (2) | Ge2vii—Al2—Ge1xi | 99.59 (2) |
Al1iv—Ce—Al1iii | 52.69 (2) | Ge2viii—Al2—Ge1xi | 99.59 (2) |
Al1vi—Ge1—Al1 | 70.46 (5) | Ge2i—Al2—Ge1xi | 80.41 (2) |
Al1vi—Ge1—Al2 | 129.74 (5) | Ge2ii—Al2—Ge1 | 99.59 (2) |
Al1—Ge1—Al2 | 129.74 (5) | Ge2vii—Al2—Ge1 | 80.41 (2) |
Al1vi—Ge1—Al1vii | 96.24 (3) | Ge2viii—Al2—Ge1 | 80.41 (2) |
Al1—Ge1—Al1vii | 135.76 (3) | Ge2i—Al2—Ge1 | 99.59 (2) |
Al2—Ge1—Al1vii | 91.73 (5) | Ge1xi—Al2—Ge1 | 180.0 |
Al1vi—Ge1—Al1viii | 135.76 (3) | Ge2ii—Al2—Cev | 59.797 (18) |
Al1—Ge1—Al1viii | 96.24 (3) | Ge2vii—Al2—Cev | 120.203 (19) |
Al2—Ge1—Al1viii | 91.73 (5) | Ge2viii—Al2—Cev | 60.498 (18) |
Al1vii—Ge1—Al1viii | 63.58 (3) | Ge2i—Al2—Cev | 119.502 (18) |
Al1vi—Ge1—Ce | 68.81 (4) | Ge1xi—Al2—Cev | 120.380 (11) |
Al1—Ge1—Ce | 68.81 (4) | Ge1—Al2—Cev | 59.620 (11) |
Al2—Ge1—Ce | 77.76 (2) | Ge2ii—Al2—Cexii | 120.203 (19) |
Al1vii—Ge1—Ce | 146.78 (2) | Ge2vii—Al2—Cexii | 59.797 (18) |
Al1viii—Ge1—Ce | 146.78 (2) | Ge2viii—Al2—Cexii | 119.502 (18) |
Al1vi—Ge1—Cevii | 71.12 (4) | Ge2i—Al2—Cexii | 60.498 (18) |
Al1—Ge1—Cevii | 71.12 (4) | Ge1xi—Al2—Cexii | 59.620 (11) |
Al2—Ge1—Cevii | 151.83 (3) | Ge1—Al2—Cexii | 120.380 (11) |
Al1vii—Ge1—Cevii | 64.68 (4) | Cev—Al2—Cexii | 180.000 (11) |
Al1viii—Ge1—Cevii | 64.68 (4) | Ge2ii—Al2—Cevi | 119.502 (18) |
Ce—Ge1—Cevii | 130.41 (3) | Ge2vii—Al2—Cevi | 60.498 (18) |
Al1vi—Ge1—Cevi | 66.63 (3) | Ge2viii—Al2—Cevi | 120.203 (18) |
Al1—Ge1—Cevi | 133.28 (3) | Ge2i—Al2—Cevi | 59.797 (18) |
Al2—Ge1—Cevi | 71.091 (17) | Ge1xi—Al2—Cevi | 120.380 (11) |
Al1vii—Ge1—Cevi | 67.70 (2) | Ge1—Al2—Cevi | 59.620 (11) |
Al1viii—Ge1—Cevi | 127.50 (3) | Cev—Al2—Cevi | 117.59 (2) |
Ce—Ge1—Cevi | 79.089 (18) | Cexii—Al2—Cevi | 62.41 (2) |
Cevii—Ge1—Cevi | 110.117 (17) | Ge2ii—Al2—Cexiii | 60.498 (18) |
Al1vi—Ge1—Cev | 133.28 (3) | Ge2vii—Al2—Cexiii | 119.502 (18) |
Al1—Ge1—Cev | 66.63 (3) | Ge2viii—Al2—Cexiii | 59.797 (18) |
Al2—Ge1—Cev | 71.091 (16) | Ge2i—Al2—Cexiii | 120.203 (18) |
Al1vii—Ge1—Cev | 127.50 (3) | Ge1xi—Al2—Cexiii | 59.620 (11) |
Al1viii—Ge1—Cev | 67.70 (2) | Ge1—Al2—Cexiii | 120.380 (11) |
Ce—Ge1—Cev | 79.089 (18) | Cev—Al2—Cexiii | 62.41 (2) |
Cevii—Ge1—Cev | 110.117 (17) | Cexii—Al2—Cexiii | 117.59 (2) |
Cevi—Ge1—Cev | 139.42 (3) | Cevi—Al2—Cexiii | 180.0 |
Symmetry codes: (i) x−1/2, y−1/2, z; (ii) x, y−1/2, −z+1/2; (iii) −x, −y+1/2, z+1/2; (iv) −x+1/2, −y+1/2, −z+1; (v) x+1/2, y, −z+1/2; (vi) x−1/2, y, −z+1/2; (vii) −x, −y+1/2, z−1/2; (viii) −x+1/2, −y+1/2, −z; (ix) x+1/2, y+1/2, z; (x) x, y+1/2, −z+1/2; (xi) −x, −y, −z; (xii) −x−1/2, −y, z−1/2; (xiii) −x+1/2, −y, z−1/2. |
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