LaTe1.82(1): modulated crystal structure and chemical bonding of a chalcogen-deficient rare earth metal polytelluride
Authors:Poddig, Hagen; Finzel, Kati; Doert, Thomas
Journal:Acta Crystallographica, Section C 76 530-540 (2020)
DOI:https://doi.org/10.1107/S2053229620005094
B-IncStrDB ID: RL0UQ53fdsS Entry date: 2022-01-20 Last revision: 2022-01-21
I
Chemical data
Full Name: Lanthanum telluride (1/1.8) [ Help ]
Formula moiety: La Te1.81 [ Help ]
Structural Formula Sum: La Te1.81 [ Help ]
Formula weight: 370.50 Da [ Help ]
Crystallographic data and experimental details
Crystal system: tetragonal [ Help ]
Space group name (H-M): P 4/n m m [ Help ]
Space group name (Hall): P 4ab 2ab -1ab [ Help ]
Symmetry operations of the space group: (Show/hide table) [ Help ]
| Operation code | Operation in algebraic form |
|---|---|
| 1 | x, y, z |
| 2 | -x+1/2, -y+1/2, -z |
| 3 | -y+1/2, x+1/2, z |
| 4 | -x, -y, z |
| 5 | y+1/2, -x+1/2, z |
| 6 | y, -x, -z |
| 7 | -y, x, -z |
| 8 | x+1/2, -y+1/2, -z |
| 9 | -x+1/2, y+1/2, -z |
| 10 | y, x, -z |
| 11 | -y, -x, -z |
| 12 | x+1/2, y+1/2, -z |
| 13 | -x, y, z |
| 14 | x, -y, z |
| 15 | -y+1/2, -x+1/2, z |
| 16 | y+1/2, x+1/2, z |
a: 4.4996(5) Å [ Help ]
b: 4.4996 Å [ Help ]
c: 9.1794(12) Å [ Help ]
α: 90 ° [ Help ]
β: 90 ° [ Help ]
γ: 90 ° [ Help ]
Volume: 185.85(3) Å3 [ Help ]
Z: 2 [ Help ]
Cell determination reflection Nb.: 872 [ Help ]
θ(min) for cell determination: 4.44 ° [ Help ]
θ(max) for cell determination: 34.72 ° [ Help ]
Cell measurement temperature: 296.0(10) K [ Help ]
μ: 25.177 mm-1 [ Help ]
Absorption correction type: multi-scan [ Help ]
Absorption correction remarks: (SADABS; Krause et al., 2015) [ Help ]
Minimum transmission factor: 0.6405 [ Help ]
Maximum transmission factor: 0.7476 [ Help ]
Refinement details
Refinement remarks: Single-crystal X-ray diffraction was performed with the four-circle diffractometer Kappa Apex2 (Bruker) equipped with a CCD-detector using graphite-monochromated Mo-Kα radiation (λ= 0.71073 °A) at 296(1) K. Data for the average structure was corrected for Lorentz and polarization factors, and multi-scan absorption corrections was applied (Krause et al., 2015). The structure was solved using the dual space approach of the program package SHELXT (Sheldrick, 2015a). Structure refinement was performed with the program package SHELXL against F2 including anisotropic displacement parameters for all atoms (Sheldrick, 2015b). Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3–10. Sheldrick, G. M. (2015a). Acta Cryst. A71, 3–8. Sheldrick, G. M. (2015b). Acta Cryst. C71, 3–8. [ Help ]
Total nb. of reflections: 351 [ Help ]
Nb. of observed reflections: 289 [ Help ]
Intense reflections threshold: I > 2σ(I) [ Help ]
Refinement based on: Fsqd [ Help ]
Matrix type used for the least-squares: full [ Help ]
R(all): 0.0378 [ Help ]
R(obs): 0.0244 [ Help ]
wR(obs): 0.0530 [ Help ]
wR(all): 0.0571 [ Help ]
S(all): 1.074 [ Help ]
Restrained S(all): 1.074 [ Help ]
Nb. of reflections: 351 [ Help ]
Nb. of parameters: 11 [ Help ]
Number of restraints: 0 [ Help ]
Refinement of hydrogen atoms: undef [ Help ]
Weighting scheme: calc [ Help ]
Weighting scheme remarks: w=1/[σ2(Fo2)+(0.0248P)2+0.9467P] where P=(Fo2+2Fc2)/3 [ Help ]
Δ/σ(max): 0.000 [ Help ]
Δ/σ(mean): 0.000 [ Help ]
Δρ(max): 3.153 e_Å-3 [ Help ]
Δρ(min): -2.349 e_Å-3 [ Help ]
Extinction method: SHELXL2019 (Sheldrick, 2015b) [ Help ]
Extinction coefficient: 0.0266(18) [ Help ]
Extinction expression: Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 [ Help ]
Absolute structure remarks: No quotients, so Flack parameter determined by classical intensity fit [ Help ]
Structural Information
Average Structure: (Show/hide table) [ Help ]
| Atom symbol | Atom site label | x | y | z | Uiso/equiv | ADP type | Coords from (d)iffraction or (c)alculated | Occupancy | Disordered cluster | Disordered group |
|---|---|---|---|---|---|---|---|---|---|---|
| La | La1 | 0.000000 | 0.500000 | 0.27121(7) | 0.01498(15) | Uani | d | 1 | . | . |
| Te | Te1 | 0.000000 | 0.500000 | 0.63329(7) | 0.01164(15) | Uani | d | 1 | . | . |
| Te | Te2 | 0.000000 | 0.000000 | 0.000000 | 0.0408(4) | Uani | d | 0.813(4) | . | . |
ADP components: (Show/hide table) [ Help ]
| Atom site label | U11 | U22 | U33 | U12 | U13 | U23 |
|---|---|---|---|---|---|---|
| La1 | 0.00971(16) | 0.00971(16) | 0.0255(3) | 0.000 | 0.000 | 0.000 |
| Te1 | 0.00909(17) | 0.00909(17) | 0.0167(3) | 0.000 | 0.000 | 0.000 |
| Te2 | 0.0568(6) | 0.0568(6) | 0.0088(4) | 0.000 | 0.000 | 0.000 |
II
Chemical data
Structural Formula Sum: La Te1.811 [ Help ]
Formula weight: 370 Da [ Help ]
Absolute configuration: . [ Help ]
Crystallographic data and experimental details
Crystal system: orthorhombic [ Help ]
Space group name (H-M): P m m n [ Help ]
Superspace group name: Pmmn(αβ1/2)000(-αβ1/2)000 [ Help ]
Symmetry operations of the superspace group: (Show/hide table) [ Help ]
| Operation code | Operation in algebraic form |
|---|---|
| 1 | x1,x2,x3,x4,x5 |
| 2 | -x1,-x2,x3,x3-x4,x3-x5 |
| 3 | -x1+1/2,x2+1/2,-x3,-x3+x5,-x3+x4 |
| 4 | x1+1/2,-x2+1/2,-x3,-x5,-x4 |
| 5 | -x1+1/2,-x2+1/2,-x3,-x4,-x5 |
| 6 | x1+1/2,x2+1/2,-x3,-x3+x4,-x3+x5 |
| 7 | x1,-x2,x3,x3-x5,x3-x4 |
| 8 | -x1,x2,x3,x5,x4 |
a: 4.4861(5) Å [ Help ]
b: 4.5030(5) Å [ Help ]
c: 9.1806(11) Å [ Help ]
α: 90 ° [ Help ]
β: 90 ° [ Help ]
γ: 90 ° [ Help ]
Volume: 185.46(4) Å3 [ Help ]
Z: 2 [ Help ]
Cell determination reflection Nb.: 872 [ Help ]
θ(min) for cell determination: 4.44 ° [ Help ]
θ(max) for cell determination: 34.72 ° [ Help ]
Cell measurement temperature: 296.0(10) K [ Help ]
Modulation dimension: 2 [ Help ]
Measured independent wave vectors: (Show/hide table) [ Help ]
| Wave vector id | q_x | q_y | q_z |
|---|---|---|---|
| 1 | 0.272(1) | 0.314(1) | 0.500000 |
| 2 | -0.272(1) | 0.314(1) | 0.500000 |
μ: 25.199 mm-1 [ Help ]
Absorption correction type: gaussian [ Help ]
Absorption correction remarks: Jana2006 [ Help ]
Minimum transmission factor: 0.3929 [ Help ]
Maximum transmission factor: 0.4983 [ Help ]
Refinement details
Total nb. of reflections: 1757 [ Help ]
Nb. of observed reflections: 738 [ Help ]
Intense reflections threshold: I>3σ(I) [ Help ]
Refinement based on: Fsqd [ Help ]
R(all): 0.1300 [ Help ]
R(obs): 0.0495 [ Help ]
wR(obs): 0.0872 [ Help ]
wR(all): 0.1111 [ Help ]
S(all): 1.26 [ Help ]
S(obs): 1.53 [ Help ]
Nb. of reflections: 1757 [ Help ]
Nb. of parameters: 24 [ Help ]
Number of restraints: 0 [ Help ]
Number of constraints: 1 [ Help ]
Weighting scheme: sigma [ Help ]
Weighting scheme remarks: w=1/(σ2(I)+0.0004I2) [ Help ]
Δ/σ(max): 0.0451 [ Help ]
Δ/σ(mean): 0.0099 [ Help ]
Δρ(max): 15.11 e_Å-3 [ Help ]
Δρ(min): -17.25 e_Å-3 [ Help ]
Extinction method: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) [ Help ]
Extinction coefficient: 150E1(8) [ Help ]
Structural Information
Average Structure: (Show/hide table) [ Help ]
| Atom symbol | Atom site label | x | y | z | Uiso/equiv | ADP type | Coords from (d)iffraction or (c)alculated | Coords restraints or constraints | Occupancy | Symmetry multiplicity | Disordered cluster | Disordered group |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| La | La1 | 0 | 0.5 | 0.27147(8) | 0.01052(18) | Uani | d | . | 1 | 2 | . | . |
| Te | Te1 | 0 | 0.5 | 0.63322(8) | 0.01043(19) | Uani | d | . | 1 | 2 | . | . |
| Te | Te2 | 0 | 0 | 0 | 0.0204(4) | Uani | d | . | 0.811(4) | 2 | . | . |
ADP components: (Show/hide table) [ Help ]
| Atom site label | U11 | U22 | U33 | U12 | U13 | U23 | Atom site symbol |
|---|---|---|---|---|---|---|---|
| La1 | 0.0099(3) | 0.0090(3) | 0.0127(4) | 0 | 0 | 0 | La |
| Te1 | 0.0096(3) | 0.0095(3) | 0.0121(4) | 0 | 0 | 0 | Te |
| Te2 | 0.0258(7) | 0.0266(8) | 0.0088(5) | 0 | 0 | 0 | Te |
Fourier Wave Vectors (explicit: q_x,q_y,q_z or coefficients: q_1,q_2,...): (Show/hide table) [ Help ]
| Wave vector code | q_1 | q_2 |
|---|---|---|
| 1 | 1 | 0 |
| 2 | 0 | 1 |
Table: (Show/hide table) [ Help ]
| _jana_atom_site_occ_Fourier_absolute_site_label | _jana_atom_site_occ_Fourier_absolute |
|---|---|
| Te2 | 0.811(4) |
Definition of the occupation Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Wave vector code |
|---|---|---|
| Te2o1 | Te2 | 1 |
| Te2o2 | Te2 | 2 |
Occupation Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| Te2o1 | -0.262(3) | 0 |
| Te2o2 | -0.262(3) | 0 |
Definition of the displacive (translational) Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Displacement axis | Wave vector code |
|---|---|---|---|
| La1x1 | La1 | x | 1 |
| La1y1 | La1 | y | 1 |
| La1z1 | La1 | z | 1 |
| La1x2 | La1 | x | 2 |
| La1y2 | La1 | y | 2 |
| La1z2 | La1 | z | 2 |
| Te1x1 | Te1 | x | 1 |
| Te1y1 | Te1 | y | 1 |
| Te1z1 | Te1 | z | 1 |
| Te1x2 | Te1 | x | 2 |
| Te1y2 | Te1 | y | 2 |
| Te1z2 | Te1 | z | 2 |
| Te2x1 | Te2 | x | 1 |
| Te2y1 | Te2 | y | 1 |
| Te2z1 | Te2 | z | 1 |
| Te2x2 | Te2 | x | 2 |
| Te2y2 | Te2 | y | 2 |
| Te2z2 | Te2 | z | 2 |
Displacive (translational) Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| La1x1 | 0.00394(18) | -0.00344(15) |
| La1y1 | 0.00325(19) | -0.00284(16) |
| La1z1 | 0.00809(6) | 0.00926(7) |
| La1x2 | -0.00394(18) | 0.00344(15) |
| La1y2 | 0.00325(19) | -0.00284(16) |
| La1z2 | 0.00809(6) | 0.00926(7) |
| Te1x1 | -0.0012(2) | -0.00053(10) |
| Te1y1 | -0.0006(2) | -0.00026(10) |
| Te1z1 | -0.00307(4) | 0.00691(10) |
| Te1x2 | 0.0012(2) | 0.00053(10) |
| Te1y2 | -0.0006(2) | -0.00026(10) |
| Te1z2 | -0.00307(4) | 0.00691(10) |
| Te2x1 | 0 | -0.0364(4) |
| Te2y1 | 0 | -0.0385(4) |
| Te2z1 | -0.00026(14) | 0 |
| Te2x2 | 0 | 0.0364(4) |
| Te2y2 | 0 | -0.0385(4) |
| Te2z2 | -0.00026(14) | 0 |