Acta Cryst. (2007). E63, i182 [ doi:10.1107/S1600536807046041 ]
Single crystals of La2CuInSe5 were obtained by sintering a La2Se3-Cu2Se-In2Se3 mixture. The crystal structure is similar to the previously reported La2CuInS5. The coordination polyhedron of the Cu atom is a trigonal bipyramid. In contrast to the La2CuInS5 compound, the position of this atom is fully occupied and ordered.
The sample with the nominal compositions La2CuInSe5 was prepared by sintering the elemental constituents (purchased from Alfa Aesar) of the purity better than 99.9 wt.% in an evacuated quartz ampoule. The synthesis was realised in a tube furnace. The ampoule was heated with a heating rate of 30 K/h to maximal temperature 1420 K. The samples were kept at this temperature during 3 h. Afterwards they were cooled slowly (10 K/h) to 870 K and annealed at this temperature during 240 h. After annealing the ampoule with the sample was quenched in cold water. An EDAX PV9800 microanalyzer was used for the confirmation of the compositions of the crystals. Calculated for La2CuInSe5 (black crystals) % La: 32.65, Cu: 7.47, In: 13.49, Se: 46.39 and found % La: 31.74, Cu: 7.57, In: 13.65, Se: 47.04.
The crystal structure was solved by Patterson methods (Sheldrick, 1997) and refined by full matrix least squares method using SHELXL97 (Sheldrick, 1997). Space group Pnma was confirmed with PLATON (Spek, 2003) and no additional symmetry elements were found. The highest peak and deepest hole in the Fourier map are found 0.94Å and 0.65 Å, respectively, from Cu1.
Data collection: CrysAlis CCD (Mayer, 2006); cell refinement: CrysAlis RED (Mayer, 2006); data reduction: CrysAlis RED (Mayer, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: publCIF (Westrip, 2007).
![[Figure 1]](./fi2045fig1thm.gif)
| Fig. 1. The packing of La2CuInSe5 viewed along the b axis. |
![[Figure 2]](./fi2045fig2thm.gif)
| Fig. 2. Trigonal bi-pyramids around the Cu atom in the structures of La2CuInS5 and La2CuInSe5. |
| La2CuInSe5 | F000 = 1448 |
| Mr = 850.98 | Dx = 6.472 Mg m−3 |
| Orthorhombic, Pnma | Mo Kα radiation λ = 0.71073 Å |
| Hall symbol: -P 2ac 2n | Cell parameters from 1049 reflections |
| a = 12.051 (2) Å | θ = 2.9–27.5º |
| b = 4.1223 (8) Å | µ = 35.34 mm−1 |
| c = 17.580 (4) Å | T = 295 (2) K |
| V = 873.3 (3) Å3 | Prism, black |
| Z = 4 | 0.13 × 0.07 × 0.03 mm |
| Kuma KM-4 diffractometer with CCD detector | 1134 independent reflections |
| Radiation source: fine-focus sealed tube | 1049 reflections with I > 2σ(I) |
| Monochromator: graphite | Rint = 0.039 |
| Detector resolution: 33.133 pixels mm-1 | θmax = 27.5º |
| T = 295(2) K | θmin = 2.9º |
| ω scans | h = −15→15 |
| Absorption correction: numerical (CrysAlis RED; Mayer, 2006) | k = −5→4 |
| Tmin = 0.076, Tmax = 0.396 | l = −22→22 |
| 9371 measured reflections |
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0208P)2] where P = (Fo2 + 2Fc2)/3 |
| R[F2 > 2σ(F2)] = 0.020 | (Δ/σ)max = 0.001 |
| wR(F2) = 0.041 | Δρmax = 2.03 e Å−3 |
| S = 1.12 | Δρmin = −1.68 e Å−3 |
| 1134 reflections | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| 56 parameters | Extinction coefficient: 0.00141 (8) |
| Primary atom site location: structure-invariant direct methods |
| La2CuInSe5 | V = 873.3 (3) Å3 |
| Mr = 850.98 | Z = 4 |
| Orthorhombic, Pnma | Mo Kα |
| a = 12.051 (2) Å | µ = 35.34 mm−1 |
| b = 4.1223 (8) Å | T = 295 (2) K |
| c = 17.580 (4) Å | 0.13 × 0.07 × 0.03 mm |
| Kuma KM-4 diffractometer with CCD detector | 1134 independent reflections |
| Absorption correction: numerical (CrysAlis RED; Mayer, 2006) | 1049 reflections with I > 2σ(I) |
| Tmin = 0.076, Tmax = 0.396 | Rint = 0.039 |
| 9371 measured reflections |
| R[F2 > 2σ(F2)] = 0.020 | 56 parameters |
| wR(F2) = 0.041 | Δρmax = 2.03 e Å−3 |
| S = 1.12 | Δρmin = −1.68 e Å−3 |
| 1134 reflections |
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 > 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. |
| x | y | z | Uiso*/Ueq | ||
| La1 | 0.47993 (3) | 0.2500 | 0.67902 (2) | 0.00840 (10) | |
| La2 | 0.13680 (3) | 0.2500 | 0.59252 (2) | 0.00889 (10) | |
| In1 | 0.19371 (4) | 0.2500 | 0.35994 (3) | 0.01362 (12) | |
| Cu1 | 0.58400 (8) | 0.2500 | 0.50300 (5) | 0.0222 (2) | |
| Se1 | 0.39751 (5) | 0.2500 | 0.42335 (4) | 0.00954 (15) | |
| Se2 | 0.24095 (5) | 0.2500 | 0.77082 (4) | 0.01086 (15) | |
| Se3 | 0.38864 (5) | 0.2500 | 0.96206 (4) | 0.00997 (15) | |
| Se4 | 0.48589 (5) | 0.2500 | 0.19359 (4) | 0.00883 (15) | |
| Se5 | 0.18170 (5) | 0.2500 | 0.11544 (4) | 0.00930 (15) |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| La1 | 0.00886 (19) | 0.00760 (19) | 0.00873 (19) | 0.000 | −0.00046 (13) | 0.000 |
| La2 | 0.00796 (19) | 0.00757 (19) | 0.0111 (2) | 0.000 | 0.00015 (14) | 0.000 |
| In1 | 0.0104 (2) | 0.0147 (2) | 0.0158 (3) | 0.000 | −0.00293 (18) | 0.000 |
| Cu1 | 0.0312 (6) | 0.0196 (5) | 0.0159 (5) | 0.000 | 0.0037 (4) | 0.000 |
| Se1 | 0.0082 (3) | 0.0098 (3) | 0.0106 (3) | 0.000 | −0.0007 (2) | 0.000 |
| Se2 | 0.0107 (3) | 0.0117 (3) | 0.0101 (3) | 0.000 | −0.0002 (2) | 0.000 |
| Se3 | 0.0104 (3) | 0.0102 (3) | 0.0093 (3) | 0.000 | 0.0010 (2) | 0.000 |
| Se4 | 0.0093 (3) | 0.0090 (3) | 0.0082 (3) | 0.000 | −0.0004 (2) | 0.000 |
| Se5 | 0.0074 (3) | 0.0088 (3) | 0.0118 (3) | 0.000 | 0.0009 (2) | 0.000 |
| La1—Se1i | 3.1094 (7) | Cu1—Se1ii | 2.4443 (7) |
| La1—Se1ii | 3.1094 (7) | Cu1—Se1i | 2.4443 (7) |
| La1—Se2 | 3.3013 (9) | Cu1—Se5xii | 2.3920 (12) |
| La1—Se2iii | 3.2669 (10) | Cu1—Cu1i | 2.8911 (14) |
| La1—Se4ii | 3.0714 (7) | Cu1—Cu1ii | 2.8911 (14) |
| La1—Se4i | 3.0714 (7) | Se1—Cu1ii | 2.4443 (7) |
| La1—Se5iv | 3.0482 (7) | Se1—Cu1i | 2.4443 (7) |
| La1—Se5v | 3.0482 (7) | Se1—La1i | 3.1094 (7) |
| La1—Cu1 | 3.3389 (12) | Se1—La1ii | 3.1094 (7) |
| La1—La1vi | 4.1223 (8) | Se2—In1v | 2.7061 (6) |
| La1—La1vii | 4.1223 (8) | Se2—In1iv | 2.7061 (6) |
| La2—Se2 | 3.3763 (9) | Se2—La1x | 3.2669 (10) |
| La2—Se3viii | 3.0988 (7) | Se3—In1iv | 2.9079 (7) |
| La2—Se3ix | 3.0988 (7) | Se3—In1v | 2.9079 (7) |
| La2—Se3x | 3.1407 (9) | Se3—La2v | 3.0988 (7) |
| La2—Se4v | 3.0969 (7) | Se3—La2iv | 3.0988 (7) |
| La2—Se4iv | 3.0969 (6) | Se3—La2iii | 3.1407 (9) |
| La2—Se5v | 3.0323 (7) | Se4—In1xii | 2.6754 (9) |
| La2—Se5iv | 3.0323 (7) | Se4—La1ii | 3.0714 (7) |
| La2—La2vi | 4.1223 (8) | Se4—La1i | 3.0714 (7) |
| La2—La2vii | 4.1223 (8) | Se4—La2viii | 3.0969 (6) |
| In1—Se4xi | 2.6754 (9) | Se4—La2ix | 3.0969 (6) |
| In1—Se1 | 2.6972 (9) | Se5—Cu1xi | 2.3920 (12) |
| In1—Se2viii | 2.7061 (6) | Se5—La2ix | 3.0323 (7) |
| In1—Se2ix | 2.7061 (6) | Se5—La2viii | 3.0323 (7) |
| In1—Se3ix | 2.9079 (7) | Se5—La1viii | 3.0482 (7) |
| In1—Se3viii | 2.9079 (7) | Se5—La1ix | 3.0482 (7) |
| Cu1—Se1 | 2.6479 (13) | ||
| Se5iv—La1—Se5v | 85.09 (2) | Se3ix—La2—La2vii | 131.694 (12) |
| Se5iv—La1—Se4ii | 143.79 (2) | Se3x—La2—La2vii | 90.0 |
| Se5v—La1—Se4ii | 84.221 (18) | Se2—La2—La2vii | 90.0 |
| Se5iv—La1—Se4i | 84.221 (18) | La2vi—La2—La2vii | 180.00 (2) |
| Se5v—La1—Se4i | 143.79 (2) | Se4xi—In1—Se1 | 176.18 (3) |
| Se4ii—La1—Se4i | 84.30 (2) | Se4xi—In1—Se2viii | 93.94 (2) |
| Se5iv—La1—Se1i | 69.09 (2) | Se1—In1—Se2viii | 88.53 (2) |
| Se5v—La1—Se1i | 122.65 (2) | Se4xi—In1—Se2ix | 93.94 (2) |
| Se4ii—La1—Se1i | 143.43 (2) | Se1—In1—Se2ix | 88.53 (2) |
| Se4i—La1—Se1i | 85.03 (2) | Se2viii—In1—Se2ix | 99.22 (3) |
| Se5iv—La1—Se1ii | 122.65 (2) | Se4xi—In1—Se3ix | 84.12 (2) |
| Se5v—La1—Se1ii | 69.09 (2) | Se1—In1—Se3ix | 93.19 (2) |
| Se4ii—La1—Se1ii | 85.03 (2) | Se2viii—In1—Se3ix | 175.27 (2) |
| Se4i—La1—Se1ii | 143.43 (2) | Se2ix—In1—Se3ix | 85.23 (2) |
| Se1i—La1—Se1ii | 83.04 (2) | Se4xi—In1—Se3viii | 84.12 (2) |
| Se5iv—La1—Se2iii | 135.583 (13) | Se1—In1—Se3viii | 93.19 (2) |
| Se5v—La1—Se2iii | 135.583 (13) | Se2viii—In1—Se3viii | 85.23 (2) |
| Se4ii—La1—Se2iii | 70.975 (16) | Se2ix—In1—Se3viii | 175.27 (2) |
| Se4i—La1—Se2iii | 70.975 (16) | Se3ix—In1—Se3viii | 90.28 (3) |
| Se1i—La1—Se2iii | 72.473 (18) | Se5xii—Cu1—Se1ii | 114.60 (3) |
| Se1ii—La1—Se2iii | 72.473 (18) | Se5xii—Cu1—Se1i | 114.60 (3) |
| Se5iv—La1—Se2 | 67.777 (19) | Se1ii—Cu1—Se1i | 114.97 (5) |
| Se5v—La1—Se2 | 67.777 (19) | Se5xii—Cu1—Se1 | 87.56 (4) |
| Se4ii—La1—Se2 | 76.149 (19) | Se1ii—Cu1—Se1 | 110.95 (3) |
| Se4i—La1—Se2 | 76.149 (19) | Se1i—Cu1—Se1 | 110.95 (3) |
| Se1i—La1—Se2 | 134.211 (13) | Se5xii—Cu1—Cu1i | 108.24 (4) |
| Se1ii—La1—Se2 | 134.211 (13) | Se1ii—Cu1—Cu1i | 133.18 (6) |
| Se2iii—La1—Se2 | 135.077 (17) | Se1i—Cu1—Cu1i | 58.80 (2) |
| Se5iv—La1—Cu1 | 84.27 (2) | Se1—Cu1—Cu1i | 52.15 (3) |
| Se5v—La1—Cu1 | 84.27 (2) | Se5xii—Cu1—Cu1ii | 108.24 (4) |
| Se4ii—La1—Cu1 | 128.709 (18) | Se1ii—Cu1—Cu1ii | 58.80 (2) |
| Se4i—La1—Cu1 | 128.709 (18) | Se1i—Cu1—Cu1ii | 133.18 (6) |
| Se1i—La1—Cu1 | 44.373 (13) | Se1—Cu1—Cu1ii | 52.15 (3) |
| Se1ii—La1—Cu1 | 44.373 (13) | Cu1i—Cu1—Cu1ii | 90.95 (6) |
| Se2iii—La1—Cu1 | 83.60 (2) | Se5xii—Cu1—La1 | 172.58 (4) |
| Se2—La1—Cu1 | 141.33 (2) | Se1ii—Cu1—La1 | 62.83 (3) |
| Se5iv—La1—La1vi | 132.546 (12) | Se1i—Cu1—La1 | 62.83 (3) |
| Se5v—La1—La1vi | 47.454 (12) | Se1—Cu1—La1 | 99.86 (4) |
| Se4ii—La1—La1vi | 47.849 (12) | Cu1i—Cu1—La1 | 76.75 (4) |
| Se4i—La1—La1vi | 132.151 (12) | Cu1ii—Cu1—La1 | 76.75 (4) |
| Se1i—La1—La1vi | 131.520 (11) | Cu1ii—Se1—Cu1i | 114.97 (5) |
| Se1ii—La1—La1vi | 48.480 (11) | Cu1ii—Se1—Cu1 | 69.05 (3) |
| Se2iii—La1—La1vi | 90.0 | Cu1i—Se1—Cu1 | 69.05 (3) |
| Se2—La1—La1vi | 90.0 | Cu1ii—Se1—In1 | 107.57 (3) |
| Cu1—La1—La1vi | 90.0 | Cu1i—Se1—In1 | 107.57 (3) |
| Se5iv—La1—La1vii | 47.454 (12) | Cu1—Se1—In1 | 172.49 (4) |
| Se5v—La1—La1vii | 132.546 (12) | Cu1ii—Se1—La1i | 145.31 (3) |
| Se4ii—La1—La1vii | 132.151 (12) | Cu1i—Se1—La1i | 72.80 (3) |
| Se4i—La1—La1vii | 47.849 (12) | Cu1—Se1—La1i | 84.43 (2) |
| Se1i—La1—La1vii | 48.480 (11) | In1—Se1—La1i | 101.15 (2) |
| Se1ii—La1—La1vii | 131.520 (11) | Cu1ii—Se1—La1ii | 72.80 (3) |
| Se2iii—La1—La1vii | 90.0 | Cu1i—Se1—La1ii | 145.31 (3) |
| Se2—La1—La1vii | 90.0 | Cu1—Se1—La1ii | 84.43 (2) |
| Cu1—La1—La1vii | 90.0 | In1—Se1—La1ii | 101.15 (2) |
| La1vi—La1—La1vii | 180.00 (2) | La1i—Se1—La1ii | 83.04 (2) |
| Se5v—La2—Se5iv | 85.65 (2) | In1v—Se2—In1iv | 99.22 (3) |
| Se5v—La2—Se4v | 79.38 (2) | In1v—Se2—La1x | 97.12 (2) |
| Se5iv—La2—Se4v | 136.10 (2) | In1iv—Se2—La1x | 97.12 (2) |
| Se5v—La2—Se4iv | 136.10 (2) | In1v—Se2—La1 | 91.67 (2) |
| Se5iv—La2—Se4iv | 79.382 (19) | In1iv—Se2—La1 | 91.67 (2) |
| Se4v—La2—Se4iv | 83.45 (2) | La1x—Se2—La1 | 166.40 (2) |
| Se5v—La2—Se3viii | 128.45 (2) | In1v—Se2—La2 | 130.213 (15) |
| Se5iv—La2—Se3viii | 73.595 (18) | In1iv—Se2—La2 | 130.213 (15) |
| Se4v—La2—Se3viii | 145.09 (2) | La1x—Se2—La2 | 83.84 (2) |
| Se4iv—La2—Se3viii | 86.26 (2) | La1—Se2—La2 | 82.56 (2) |
| Se5v—La2—Se3ix | 73.595 (18) | In1iv—Se3—In1v | 90.28 (3) |
| Se5iv—La2—Se3ix | 128.45 (2) | In1iv—Se3—La2v | 153.46 (3) |
| Se4v—La2—Se3ix | 86.26 (2) | In1v—Se3—La2v | 87.232 (18) |
| Se4iv—La2—Se3ix | 145.09 (2) | In1iv—Se3—La2iv | 87.232 (18) |
| Se3viii—La2—Se3ix | 83.39 (2) | In1v—Se3—La2iv | 153.46 (3) |
| Se5v—La2—Se3x | 136.672 (12) | La2v—Se3—La2iv | 83.39 (2) |
| Se5iv—La2—Se3x | 136.672 (12) | In1iv—Se3—La2iii | 97.84 (2) |
| Se4v—La2—Se3x | 73.779 (19) | In1v—Se3—La2iii | 97.84 (2) |
| Se4iv—La2—Se3x | 73.779 (19) | La2v—Se3—La2iii | 108.680 (18) |
| Se3viii—La2—Se3x | 71.320 (18) | La2iv—Se3—La2iii | 108.680 (18) |
| Se3ix—La2—Se3x | 71.320 (18) | In1xii—Se4—La1ii | 97.52 (2) |
| Se5v—La2—Se2 | 66.952 (16) | In1xii—Se4—La1i | 97.52 (2) |
| Se5iv—La2—Se2 | 66.952 (16) | La1ii—Se4—La1i | 84.30 (2) |
| Se4v—La2—Se2 | 69.200 (18) | In1xii—Se4—La2viii | 104.19 (2) |
| Se4iv—La2—Se2 | 69.200 (18) | La1ii—Se4—La2viii | 158.28 (3) |
| Se3viii—La2—Se2 | 136.374 (13) | La1i—Se4—La2viii | 92.046 (16) |
| Se3ix—La2—Se2 | 136.374 (13) | In1xii—Se4—La2ix | 104.19 (2) |
| Se3x—La2—Se2 | 129.61 (2) | La1ii—Se4—La2ix | 92.046 (16) |
| Se5v—La2—La2vi | 47.177 (12) | La1i—Se4—La2ix | 158.28 (3) |
| Se5iv—La2—La2vi | 132.823 (12) | La2viii—Se4—La2ix | 83.45 (2) |
| Se4v—La2—La2vi | 48.276 (11) | Cu1xi—Se5—La2ix | 103.85 (3) |
| Se4iv—La2—La2vi | 131.724 (11) | Cu1xi—Se5—La2viii | 103.85 (3) |
| Se3viii—La2—La2vi | 131.694 (12) | La2ix—Se5—La2viii | 85.65 (2) |
| Se3ix—La2—La2vi | 48.306 (12) | Cu1xi—Se5—La1viii | 90.27 (3) |
| Se3x—La2—La2vi | 90.0 | La2ix—Se5—La1viii | 165.76 (3) |
| Se2—La2—La2vi | 90.0 | La2viii—Se5—La1viii | 92.868 (17) |
| Se5v—La2—La2vii | 132.823 (12) | Cu1xi—Se5—La1ix | 90.27 (3) |
| Se5iv—La2—La2vii | 47.177 (12) | La2ix—Se5—La1ix | 92.868 (17) |
| Se4v—La2—La2vii | 131.724 (11) | La2viii—Se5—La1ix | 165.76 (3) |
| Se4iv—La2—La2vii | 48.276 (11) | La1viii—Se5—La1ix | 85.09 (2) |
| Se3viii—La2—La2vii | 48.306 (12) | ||
| Se5iv—La1—Cu1—Se1ii | 151.39 (3) | Se2viii—In1—Se1—La1i | 7.132 (18) |
| Se5v—La1—Cu1—Se1ii | 65.77 (3) | Se2ix—In1—Se1—La1i | −92.14 (2) |
| Se4ii—La1—Cu1—Se1ii | −12.10 (4) | Se3ix—In1—Se1—La1i | −177.276 (16) |
| Se4i—La1—Cu1—Se1ii | −130.74 (3) | Se3viii—In1—Se1—La1i | 92.27 (2) |
| Se1i—La1—Cu1—Se1ii | −142.84 (5) | Se2viii—In1—Se1—La1ii | 92.14 (2) |
| Se2iii—La1—Cu1—Se1ii | −71.42 (2) | Se2ix—In1—Se1—La1ii | −7.132 (18) |
| Se2—La1—Cu1—Se1ii | 108.58 (2) | Se3ix—In1—Se1—La1ii | −92.27 (2) |
| La1vi—La1—Cu1—Se1ii | 18.58 (2) | Se3viii—In1—Se1—La1ii | 177.276 (16) |
| La1vii—La1—Cu1—Se1ii | −161.42 (2) | Se5iv—La1—Se2—In1v | −177.282 (19) |
| Se5iv—La1—Cu1—Se1i | −65.77 (3) | Se5v—La1—Se2—In1v | −83.44 (2) |
| Se5v—La1—Cu1—Se1i | −151.39 (3) | Se4ii—La1—Se2—In1v | 5.917 (15) |
| Se4ii—La1—Cu1—Se1i | 130.74 (3) | Se4i—La1—Se2—In1v | 93.36 (2) |
| Se4i—La1—Cu1—Se1i | 12.10 (4) | Se1i—La1—Se2—In1v | 162.00 (2) |
| Se1ii—La1—Cu1—Se1i | 142.84 (5) | Se1ii—La1—Se2—In1v | −62.72 (3) |
| Se2iii—La1—Cu1—Se1i | 71.42 (2) | Se2iii—La1—Se2—In1v | 49.641 (15) |
| Se2—La1—Cu1—Se1i | −108.58 (2) | Cu1—La1—Se2—In1v | −130.359 (15) |
| La1vi—La1—Cu1—Se1i | 161.42 (2) | La1vi—La1—Se2—In1v | −40.359 (15) |
| La1vii—La1—Cu1—Se1i | −18.58 (2) | La1vii—La1—Se2—In1v | 139.641 (15) |
| Se5iv—La1—Cu1—Se1 | 42.810 (12) | Se5iv—La1—Se2—In1iv | 83.44 (2) |
| Se5v—La1—Cu1—Se1 | −42.810 (12) | Se5v—La1—Se2—In1iv | 177.282 (19) |
| Se4ii—La1—Cu1—Se1 | −120.68 (2) | Se4ii—La1—Se2—In1iv | −93.36 (2) |
| Se4i—La1—Cu1—Se1 | 120.68 (2) | Se4i—La1—Se2—In1iv | −5.917 (15) |
| Se1i—La1—Cu1—Se1 | 108.58 (2) | Se1i—La1—Se2—In1iv | 62.72 (3) |
| Se1ii—La1—Cu1—Se1 | −108.58 (2) | Se1ii—La1—Se2—In1iv | −162.00 (2) |
| Se2iii—La1—Cu1—Se1 | 180.0 | Se2iii—La1—Se2—In1iv | −49.641 (15) |
| Se2—La1—Cu1—Se1 | 0.0 | Cu1—La1—Se2—In1iv | 130.359 (15) |
| Se5iv—La1—Cu1—Cu1i | −4.28 (3) | La1vi—La1—Se2—In1iv | −139.641 (15) |
| Se5v—La1—Cu1—Cu1i | −89.90 (3) | La1vii—La1—Se2—In1iv | 40.359 (15) |
| Se4ii—La1—Cu1—Cu1i | −167.78 (2) | Se5iv—La1—Se2—La1x | −46.923 (13) |
| Se4i—La1—Cu1—Cu1i | 73.59 (4) | Se5v—La1—Se2—La1x | 46.923 (13) |
| Se1i—La1—Cu1—Cu1i | 61.49 (2) | Se4ii—La1—Se2—La1x | 136.276 (12) |
| Se1ii—La1—Cu1—Cu1i | −155.67 (5) | Se4i—La1—Se2—La1x | −136.276 (12) |
| Se2iii—La1—Cu1—Cu1i | 132.91 (3) | Se1i—La1—Se2—La1x | −67.64 (2) |
| Se2—La1—Cu1—Cu1i | −47.09 (3) | Se1ii—La1—Se2—La1x | 67.64 (2) |
| La1vi—La1—Cu1—Cu1i | −137.09 (3) | Se2iii—La1—Se2—La1x | 180.0 |
| La1vii—La1—Cu1—Cu1i | 42.91 (3) | Cu1—La1—Se2—La1x | 0.0 |
| Se5iv—La1—Cu1—Cu1ii | 89.90 (3) | Se5iv—La1—Se2—La2 | −46.923 (13) |
| Se5v—La1—Cu1—Cu1ii | 4.28 (3) | Se5v—La1—Se2—La2 | 46.923 (13) |
| Se4ii—La1—Cu1—Cu1ii | −73.59 (4) | Se4ii—La1—Se2—La2 | 136.276 (12) |
| Se4i—La1—Cu1—Cu1ii | 167.78 (2) | Se4i—La1—Se2—La2 | −136.276 (12) |
| Se1i—La1—Cu1—Cu1ii | 155.67 (5) | Se1i—La1—Se2—La2 | −67.64 (2) |
| Se1ii—La1—Cu1—Cu1ii | −61.49 (2) | Se1ii—La1—Se2—La2 | 67.64 (2) |
| Se2iii—La1—Cu1—Cu1ii | −132.91 (3) | Se2iii—La1—Se2—La2 | 180.0 |
| Se2—La1—Cu1—Cu1ii | 47.09 (3) | Cu1—La1—Se2—La2 | 0.0 |
| La1vi—La1—Cu1—Cu1ii | −42.91 (3) | Se5v—La2—Se2—In1v | 38.26 (3) |
| La1vii—La1—Cu1—Cu1ii | 137.09 (3) | Se5iv—La2—Se2—In1v | 133.50 (4) |
| Se5xii—Cu1—Se1—Cu1ii | −115.45 (3) | Se4v—La2—Se2—In1v | −48.73 (3) |
| Se1ii—Cu1—Se1—Cu1ii | 0.0 | Se4iv—La2—Se2—In1v | −139.52 (4) |
| Se1i—Cu1—Se1—Cu1ii | 129.09 (6) | Se3viii—La2—Se2—In1v | 160.47 (3) |
| Cu1i—Cu1—Se1—Cu1ii | 129.09 (6) | Se3ix—La2—Se2—In1v | 11.28 (5) |
| La1—Cu1—Se1—Cu1ii | 64.55 (3) | Se3x—La2—Se2—In1v | −94.12 (3) |
| Se5xii—Cu1—Se1—Cu1i | 115.45 (3) | La2vi—La2—Se2—In1v | −4.12 (3) |
| Se1ii—Cu1—Se1—Cu1i | −129.09 (6) | La2vii—La2—Se2—In1v | 175.88 (3) |
| Se1i—Cu1—Se1—Cu1i | 0.0 | Se5v—La2—Se2—In1iv | −133.50 (4) |
| Cu1ii—Cu1—Se1—Cu1i | −129.09 (6) | Se5iv—La2—Se2—In1iv | −38.26 (3) |
| La1—Cu1—Se1—Cu1i | −64.55 (3) | Se4v—La2—Se2—In1iv | 139.52 (4) |
| Se5xii—Cu1—Se1—La1i | 41.761 (11) | Se4iv—La2—Se2—In1iv | 48.73 (3) |
| Se1ii—Cu1—Se1—La1i | 157.22 (3) | Se3viii—La2—Se2—In1iv | −11.28 (5) |
| Se1i—Cu1—Se1—La1i | −73.69 (3) | Se3ix—La2—Se2—In1iv | −160.47 (3) |
| Cu1i—Cu1—Se1—La1i | −73.69 (3) | Se3x—La2—Se2—In1iv | 94.12 (3) |
| Cu1ii—Cu1—Se1—La1i | 157.22 (3) | La2vi—La2—Se2—In1iv | −175.88 (3) |
| La1—Cu1—Se1—La1i | −138.239 (11) | La2vii—La2—Se2—In1iv | 4.12 (3) |
| Se5xii—Cu1—Se1—La1ii | −41.761 (11) | Se5v—La2—Se2—La1x | 132.380 (13) |
| Se1ii—Cu1—Se1—La1ii | 73.69 (3) | Se5iv—La2—Se2—La1x | −132.380 (13) |
| Se1i—Cu1—Se1—La1ii | −157.22 (3) | Se4v—La2—Se2—La1x | 45.394 (13) |
| Cu1i—Cu1—Se1—La1ii | −157.22 (3) | Se4iv—La2—Se2—La1x | −45.394 (13) |
| Cu1ii—Cu1—Se1—La1ii | 73.69 (3) | Se3viii—La2—Se2—La1x | −105.41 (3) |
| La1—Cu1—Se1—La1ii | 138.239 (11) | Se3ix—La2—Se2—La1x | 105.41 (3) |
| Se2viii—In1—Se1—Cu1ii | 167.44 (3) | Se3x—La2—Se2—La1x | 0.0 |
| Se2ix—In1—Se1—Cu1ii | 68.17 (3) | Se5v—La2—Se2—La1 | −47.620 (13) |
| Se3ix—In1—Se1—Cu1ii | −16.97 (3) | Se5iv—La2—Se2—La1 | 47.620 (13) |
| Se3viii—In1—Se1—Cu1ii | −107.42 (3) | Se4v—La2—Se2—La1 | −134.606 (13) |
| Se2viii—In1—Se1—Cu1i | −68.17 (3) | Se4iv—La2—Se2—La1 | 134.606 (13) |
| Se2ix—In1—Se1—Cu1i | −167.44 (3) | Se3viii—La2—Se2—La1 | 74.59 (3) |
| Se3ix—In1—Se1—Cu1i | 107.42 (3) | Se3ix—La2—Se2—La1 | −74.59 (3) |
| Se3viii—In1—Se1—Cu1i | 16.97 (3) | Se3x—La2—Se2—La1 | 180.0 |
| Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x+1/2, y, −z+3/2; (iv) −x+1/2, −y, z+1/2; (v) −x+1/2, −y+1, z+1/2; (vi) x, y+1, z; (vii) x, y−1, z; (viii) −x+1/2, −y, z−1/2; (ix) −x+1/2, −y+1, z−1/2; (x) x−1/2, y, −z+3/2; (xi) x−1/2, y, −z+1/2; (xii) x+1/2, y, −z+1/2. |
| La1—Se1i | 3.1094 (7) | La2—Se5iv | 3.0323 (7) |
| La1—Se2 | 3.3013 (9) | In1—Se4vii | 2.6754 (9) |
| La1—Se2ii | 3.2669 (10) | In1—Se1 | 2.6972 (9) |
| La1—Se4iii | 3.0714 (7) | In1—Se2v | 2.7061 (6) |
| La1—Se5iv | 3.0482 (7) | In1—Se3viii | 2.9079 (7) |
| La2—Se2 | 3.3763 (9) | Cu1—Se1 | 2.6479 (13) |
| La2—Se3v | 3.0988 (7) | Cu1—Se1iii | 2.4443 (7) |
| La2—Se3vi | 3.1407 (9) | Cu1—Se1i | 2.4443 (7) |
| La2—Se4iv | 3.0969 (6) | Cu1—Se5ix | 2.3920 (12) |
| Symmetry codes: (i) −x+1, −y, −z+1; (ii) x+1/2, y, −z+3/2; (iii) −x+1, −y+1, −z+1; (iv) −x+1/2, −y, z+1/2; (v) −x+1/2, −y, z−1/2; (vi) x−1/2, y, −z+3/2; (vii) x−1/2, y, −z+1/2; (viii) −x+1/2, −y+1, z−1/2; (ix) x+1/2, y, −z+1/2. |
Brandenburg, K. (2005). DIAMOND. Release 3.0e. Crystal Impact GbR, Bonn, Germany.
Huch, M. R., Gulay, L. D., Olekseyuk, I. D. & Pietraszko, A. (2007). J. Alloys Compd. 425, 230–234.
Huch, M. R., Gulay, L. D. & Olekseyuk, I. D. (2007). J. Alloys Compd. In the press.
Mayer, M. (2006). CrysAlis CCD (Version 1.171.10) and CrysAlis RED (Version 1.171.38.1). Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.
Spek, A. L. (2003). PLATON. University of Utrecht, The Netherlands.
Westrip (2007). PublCIF. In preparation.
The formation of quaternary La2CuInSe5 had been established earlier during the investigation of the phase relations in the La2Se3—Cu2Se—In2Se3 system (Huch, Gulay & Olekseyuk, 2007) and the crystal structure of this compound was investigated using X-ray powder diffraction (space group Pnma). The crystal structure of La2CuInSe5 has been reinvestigated by means of X-ray single-crystal diffraction and presented here. Crystal structure of the title compound is similar to previously reported La2CuInS5 (Huch, Gulay, Olekseyuk & Pietraszko, 2007).
The unit cell and the coordination polyhedra of the La, Cu, In and Se atoms in the structure of the La2CuInSe5 compound are shown in Fig. 1. Selenium atoms create bi-capped trigonal prisms, octahedra and tetrahedra around the La, In and Cu atoms, respectively. The coordination polyhedron of the copper atom can be extended to a trigonal bipyramid. In contrast to La2CuInS5, the position of the Cu atom is fully occupied and ordered (Fig. 2). The single-crystal data for La2CuInSe5 agree well with our previous powder diffraction results (Huch, Gulay & Olekseyuk, 2007).