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The crystal structures of Nb3Te4 and InxNb3Te4 [x = 0.539 (4)] are reported for a series of pressures between 0 and 40 GPa. Both compounds crystallize in space group P63/m with a = b = 10.671 and c = 3.6468 Å for Nb3Te4, and a = b = 10.677 and c = 3.6566 Å for InxNb3Te4 at ambient conditions. Phase transitions were not observed. High-pressure X-ray powder diffraction was measured using a diamond anvil cell and synchrotron radiation. Full Rietveld refinements provided the values of the lattice parameters and the values of the atomic coordinates at each pressure. The bulk modulus is found as K0 = 70 (5) GPa for Nb3Te4 and as K0 = 73 (4) GPa for InxNb3Te4. The analysis of the pressure dependences of the detailed crystal structures shows that the compression along c involves the folding up of the quasi-one-dimensional zigzag chains of Nb. The compression perpendicular to c is entirely due to the reduction of the diameter of the channels. The presence of intercalated In atoms is found to have hardly any influence on the compression behaviour up to 40 GPa.
Supporting information
Cell refinement: Jana2000; data reduction: FIT2D; program(s) used to refine structure: Jana2000.
Crystal data top
In0.54Nb3Te4 | Synchrotron radiation |
Mr = 851.1 | µ = 14.5 mm−1 |
Hexagonal, P63/m | T = 295 K |
a = 10.6768 (3) Å | Particle morphology: needle-like |
c = 3.6566 (1) Å | metallic dark grey |
V = 360.99 (2) Å3 | cylinder, 0.5 × 0.5 mm |
Z = 2 | Specimen preparation: Prepared at 873 K |
Data collection top
ESRF ID15B diffractometer | Data collection mode: transmission |
Specimen mounting: lithiumborate glass capillary 0.5 mm diameter | Scan method: energy dispersive |
Refinement top
Refinement on Inet | 1707 data points |
Rp = 0.026 | Profile function: pseudo-Voigt |
Rwp = 0.042 | 22 parameters |
Rexp = ? | |
χ2 = 2.592 | Background function: manual and Ledendre Polynomial |
Crystal data top
In0.54Nb3Te4 | Z = 2 |
Mr = 851.1 | Synchrotron radiation |
Hexagonal, P63/m | µ = 14.5 mm−1 |
a = 10.6768 (3) Å | T = 295 K |
c = 3.6566 (1) Å | cylinder, 0.5 × 0.5 mm |
V = 360.99 (2) Å3 | |
Data collection top
ESRF ID15B diffractometer | Data collection mode: transmission |
Specimen mounting: lithiumborate glass capillary 0.5 mm diameter | Scan method: energy dispersive |
Refinement top
Rp = 0.026 | χ2 = 2.592 |
Rwp = 0.042 | 1707 data points |
Rexp = ? | 22 parameters |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Nb1 | 0.4881 (2) | 0.1024 (2) | 0.25 | 0.0054 (3) | |
Te2 | 0.666667 | 0.333333 | 0.75 | 0.0051 (5) | |
Te3 | 0.3356 (2) | 0.27194 (1) | 0.25 | 0.0057 (2) | |
In4 | 0 | 0 | 0 | 0.028 (3) | 0.2696 (17) |
In5 | 0 | 0 | 0.25 | 0.029 (3) | 0.2696 (17) |
Geometric parameters (Å, º) top
Nb1—Nb1i | 3.6566 (1) | Te3—Te3xi | 3.770 (2) |
Nb1—Nb1ii | 3.6566 (1) | Te3—Te3xii | 3.770 (2) |
Nb1—Nb1iii | 2.957 (2) | Te3—Te3vii | 3.770 (2) |
Nb1—Nb1iv | 2.957 (2) | Te3—Te3viii | 3.770 (2) |
Nb1—Nb1v | 3.878 (2) | Te3—In4 | 3.4209 (11) |
Nb1—Nb1vi | 3.8777 (18) | Te3—In4xii | 3.4209 (11) |
Nb1—Te2i | 2.8905 (10) | Te3—In5 | 3.2965 (11) |
Nb1—Te2 | 2.8905 (10) | Te3—In5xiii | 3.7695 (10) |
Nb1—Te3 | 2.979 (2) | Te3—In5xiv | 3.7695 (10) |
Nb1—Te3vi | 2.792 (2) | In4—In4i | 3.6566 (1) |
Nb1—Te3vii | 2.7790 (12) | In4—In4ii | 3.6566 (1) |
Nb1—Te3viii | 2.7790 (12) | In4—In4xi | 1.8283 |
Te2—Te2i | 3.6566 (1) | In4—In4xii | 1.8283 |
Te2—Te2ii | 3.6566 (1) | In4—In5i | 2.7425 |
Te2—Te3 | 3.7346 (15) | In4—In5 | 0.9142 |
Te2—Te3ii | 3.7346 (15) | In4—In5xiii | 0.9142 |
Te2—Te3v | 3.7346 (11) | In4—In5xiv | 2.7425 |
Te2—Te3ix | 3.7346 (11) | In5—In5i | 3.6566 (1) |
Te2—Te3vi | 3.7346 (19) | In5—In5ii | 3.6566 (1) |
Te2—Te3x | 3.7346 (19) | In5—In5xiii | 1.8283 |
Te3—Te3i | 3.6566 (1) | In5—In5xiv | 1.8283 |
Te3—Te3ii | 3.6566 (1) | | |
| | | |
Nb1i—Nb1—Nb1ii | 180 | Te3x—Te2—Te3v | 128.30 (3) |
Nb1i—Nb1—Nb1iii | 51.81 (3) | Te3x—Te2—Te3ix | 98.08 (3) |
Nb1i—Nb1—Nb1iv | 128.19 (6) | Te3x—Te2—Te3vi | 58.62 (2) |
Nb1i—Nb1—Nb1v | 90 | Te3i—Te3—Te3ii | 180 |
Nb1i—Nb1—Nb1vi | 90 | Te3i—Te3—Te3xi | 60.99 (3) |
Nb1i—Nb1—Te2i | 50.76 (2) | Te3i—Te3—Te3xii | 119.01 (5) |
Nb1i—Nb1—Te2 | 129.24 (4) | Te3i—Te3—Te3vii | 60.99 (2) |
Nb1i—Nb1—Te3 | 90 | Te3i—Te3—Te3viii | 119.01 (4) |
Nb1i—Nb1—Te3vi | 90 | Te3i—Te3—In4 | 74.50 (2) |
Nb1i—Nb1—Te3vii | 48.86 (2) | Te3i—Te3—In4xii | 105.50 (2) |
Nb1i—Nb1—Te3viii | 131.14 (4) | Te3i—Te3—In5 | 90 |
Nb1ii—Nb1—Nb1i | 180 | Te3i—Te3—In5xiii | 60.99 (2) |
Nb1ii—Nb1—Nb1iii | 128.19 (6) | Te3i—Te3—In5xiv | 119.01 (3) |
Nb1ii—Nb1—Nb1iv | 51.81 (3) | Te3ii—Te3—Te3i | 180 |
Nb1ii—Nb1—Nb1v | 90 | Te3ii—Te3—Te3xi | 119.01 (5) |
Nb1ii—Nb1—Nb1vi | 90 | Te3ii—Te3—Te3xii | 60.99 (3) |
Nb1ii—Nb1—Te2i | 129.24 (4) | Te3ii—Te3—Te3vii | 119.01 (4) |
Nb1ii—Nb1—Te2 | 50.76 (2) | Te3ii—Te3—Te3viii | 60.99 (2) |
Nb1ii—Nb1—Te3 | 90 | Te3ii—Te3—In4 | 105.50 (2) |
Nb1ii—Nb1—Te3vi | 90 | Te3ii—Te3—In4xii | 74.50 (2) |
Nb1ii—Nb1—Te3vii | 131.14 (4) | Te3ii—Te3—In5 | 90 |
Nb1ii—Nb1—Te3viii | 48.86 (2) | Te3ii—Te3—In5xiii | 119.01 (3) |
Nb1iii—Nb1—Nb1i | 51.81 (3) | Te3ii—Te3—In5xiv | 60.99 (2) |
Nb1iii—Nb1—Nb1ii | 128.19 (6) | Te3xi—Te3—Te3i | 60.99 (3) |
Nb1iii—Nb1—Nb1iv | 76.38 (5) | Te3xi—Te3—Te3ii | 119.01 (5) |
Nb1iii—Nb1—Nb1v | 136.37 (3) | Te3xi—Te3—Te3xii | 58.03 (3) |
Nb1iii—Nb1—Nb1vi | 95.55 (5) | Te3xi—Te3—Te3vii | 98.46 (3) |
Nb1iii—Nb1—Te2i | 88.62 (3) | Te3xi—Te3—Te3viii | 128.14 (4) |
Nb1iii—Nb1—Te2 | 139.29 (7) | Te3xi—Te3—In4 | 56.57 (3) |
Nb1iii—Nb1—Te3 | 136.42 (4) | Te3xi—Te3—In4xii | 73.04 (3) |
Nb1iii—Nb1—Te3vi | 57.73 (5) | Te3xi—Te3—In5 | 64.07 (3) |
Nb1iii—Nb1—Te3vii | 58.14 (5) | Te3xi—Te3—In5xiii | 51.86 (2) |
Nb1iii—Nb1—Te3viii | 106.61 (6) | Te3xi—Te3—In5xiv | 81.54 (3) |
Nb1iv—Nb1—Nb1i | 128.19 (6) | Te3xii—Te3—Te3i | 119.01 (5) |
Nb1iv—Nb1—Nb1ii | 51.81 (3) | Te3xii—Te3—Te3ii | 60.99 (3) |
Nb1iv—Nb1—Nb1iii | 76.38 (5) | Te3xii—Te3—Te3xi | 58.03 (3) |
Nb1iv—Nb1—Nb1v | 136.37 (3) | Te3xii—Te3—Te3vii | 128.14 (4) |
Nb1iv—Nb1—Nb1vi | 95.55 (5) | Te3xii—Te3—Te3viii | 98.46 (3) |
Nb1iv—Nb1—Te2i | 139.29 (7) | Te3xii—Te3—In4 | 73.04 (3) |
Nb1iv—Nb1—Te2 | 88.62 (3) | Te3xii—Te3—In4xii | 56.57 (3) |
Nb1iv—Nb1—Te3 | 136.42 (4) | Te3xii—Te3—In5 | 64.07 (3) |
Nb1iv—Nb1—Te3vi | 57.73 (5) | Te3xii—Te3—In5xiii | 81.54 (3) |
Nb1iv—Nb1—Te3vii | 106.61 (6) | Te3xii—Te3—In5xiv | 51.86 (2) |
Nb1iv—Nb1—Te3viii | 58.14 (5) | Te3vii—Te3—Te3i | 60.99 (2) |
Nb1v—Nb1—Nb1i | 90 | Te3vii—Te3—Te3ii | 119.01 (4) |
Nb1v—Nb1—Nb1ii | 90 | Te3vii—Te3—Te3xi | 98.46 (3) |
Nb1v—Nb1—Nb1iii | 136.37 (3) | Te3vii—Te3—Te3xii | 128.14 (4) |
Nb1v—Nb1—Nb1iv | 136.37 (3) | Te3vii—Te3—Te3viii | 58.03 (3) |
Nb1v—Nb1—Nb1vi | 60.00 (5) | Te3vii—Te3—In4 | 56.57 (2) |
Nb1v—Nb1—Te2i | 47.87 (3) | Te3vii—Te3—In4xii | 73.04 (2) |
Nb1v—Nb1—Te2 | 47.87 (3) | Te3vii—Te3—In5 | 64.07 (2) |
Nb1v—Nb1—Te3 | 45.76 (4) | Te3vii—Te3—In5xiii | 51.86 (2) |
Nb1v—Nb1—Te3vi | 109.86 (6) | Te3vii—Te3—In5xiv | 81.54 (2) |
Nb1v—Nb1—Te3vii | 115.41 (7) | Te3viii—Te3—Te3i | 119.01 (4) |
Nb1v—Nb1—Te3viii | 115.41 (7) | Te3viii—Te3—Te3ii | 60.99 (2) |
Nb1vi—Nb1—Nb1i | 90 | Te3viii—Te3—Te3xi | 128.14 (4) |
Nb1vi—Nb1—Nb1ii | 90 | Te3viii—Te3—Te3xii | 98.46 (3) |
Nb1vi—Nb1—Nb1iii | 95.55 (5) | Te3viii—Te3—Te3vii | 58.03 (3) |
Nb1vi—Nb1—Nb1iv | 95.55 (5) | Te3viii—Te3—In4 | 73.04 (2) |
Nb1vi—Nb1—Nb1v | 60.00 (5) | Te3viii—Te3—In4xii | 56.57 (2) |
Nb1vi—Nb1—Te2i | 47.87 (2) | Te3viii—Te3—In5 | 64.07 (2) |
Nb1vi—Nb1—Te2 | 47.87 (2) | Te3viii—Te3—In5xiii | 81.54 (2) |
Nb1vi—Nb1—Te3 | 105.76 (5) | Te3viii—Te3—In5xiv | 51.86 (2) |
Nb1vi—Nb1—Te3vi | 49.86 (5) | In4—Te3—In4xii | 30.998 (10) |
Nb1vi—Nb1—Te3vii | 138.63 (2) | In4—Te3—In5 | 15.499 (5) |
Nb1vi—Nb1—Te3viii | 138.63 (2) | In4—Te3—In5xiii | 13.514 (3) |
Te2i—Nb1—Te2 | 78.47 (3) | In4—Te3—In5xiv | 44.512 (13) |
Te2i—Nb1—Te3 | 79.02 (4) | In4xii—Te3—In4 | 30.998 (10) |
Te2i—Nb1—Te3vi | 82.16 (4) | In4xii—Te3—In5 | 15.499 (5) |
Te2i—Nb1—Te3vii | 96.39 (2) | In4xii—Te3—In5xiii | 44.512 (13) |
Te2i—Nb1—Te3viii | 160.67 (9) | In4xii—Te3—In5xiv | 13.514 (3) |
Te2—Nb1—Te2i | 78.47 (3) | In5—Te3—In5xiii | 29.013 (8) |
Te2—Nb1—Te3 | 79.02 (4) | In5—Te3—In5xiv | 29.013 (8) |
Te2—Nb1—Te3vi | 82.16 (4) | In5xiii—Te3—In5 | 29.013 (8) |
Te2—Nb1—Te3vii | 160.67 (9) | In5xiii—Te3—In5xiv | 58.026 (16) |
Te2—Nb1—Te3viii | 96.39 (2) | In5xiv—Te3—In5 | 29.013 (8) |
Te3—Nb1—Te3vi | 155.62 (6) | In5xiv—Te3—In5xiii | 58.026 (16) |
Te3—Nb1—Te3vii | 81.72 (6) | In4i—In4—In4ii | 180 |
Te3—Nb1—Te3viii | 81.72 (6) | In4i—In4—In4xi | 0 |
Te3vi—Nb1—Te3 | 155.62 (6) | In4i—In4—In4xii | 180 |
Te3vi—Nb1—Te3vii | 115.87 (7) | In4i—In4—In5i | 0 |
Te3vi—Nb1—Te3viii | 115.87 (7) | In4i—In4—In5 | 180 |
Te3vii—Nb1—Te3 | 81.72 (6) | In4i—In4—In5xiii | 0 |
Te3vii—Nb1—Te3vi | 115.87 (7) | In4i—In4—In5xiv | 180 |
Te3vii—Nb1—Te3viii | 82.29 (3) | In4ii—In4—In4i | 180 |
Te3viii—Nb1—Te3 | 81.72 (6) | In4ii—In4—In4xi | 180 |
Te3viii—Nb1—Te3vi | 115.87 (7) | In4ii—In4—In4xii | 0 |
Te3viii—Nb1—Te3vii | 82.29 (3) | In4ii—In4—In5i | 180 |
Te2i—Te2—Te2ii | 180 | In4ii—In4—In5 | 0 |
Te2i—Te2—Te3 | 60.688 (12) | In4ii—In4—In5xiii | 180 |
Te2i—Te2—Te3ii | 119.312 (12) | In4ii—In4—In5xiv | 0 |
Te2i—Te2—Te3v | 60.688 (9) | In4xi—In4—In4i | 0 |
Te2i—Te2—Te3ix | 119.312 (9) | In4xi—In4—In4ii | 180 |
Te2i—Te2—Te3vi | 60.688 (16) | In4xi—In4—In4xii | 180 |
Te2i—Te2—Te3x | 119.312 (16) | In4xi—In4—In5i | 0 |
Te2ii—Te2—Te2i | 180 | In4xi—In4—In5 | 180 |
Te2ii—Te2—Te3 | 119.312 (12) | In4xi—In4—In5xiii | 0 |
Te2ii—Te2—Te3ii | 60.688 (12) | In4xi—In4—In5xiv | 180 |
Te2ii—Te2—Te3v | 119.312 (9) | In4xii—In4—In4i | 180 |
Te2ii—Te2—Te3ix | 60.688 (9) | In4xii—In4—In4ii | 0 |
Te2ii—Te2—Te3vi | 119.312 (16) | In4xii—In4—In4xi | 180 |
Te2ii—Te2—Te3x | 60.688 (16) | In4xii—In4—In5i | 180 |
Te3—Te2—Te3ii | 58.624 (17) | In4xii—In4—In5 | 0 |
Te3—Te2—Te3v | 98.08 (3) | In4xii—In4—In5xiii | 180 |
Te3—Te2—Te3ix | 128.30 (4) | In4xii—In4—In5xiv | 0 |
Te3—Te2—Te3vi | 98.08 (2) | In5i—In4—In5 | 180 |
Te3—Te2—Te3x | 128.30 (2) | In5i—In4—In5xiii | 0 |
Te3ii—Te2—Te3 | 58.624 (17) | In5i—In4—In5xiv | 180 |
Te3ii—Te2—Te3v | 128.30 (4) | In5—In4—In5i | 180 |
Te3ii—Te2—Te3ix | 98.08 (3) | In5—In4—In5xiii | 180 |
Te3ii—Te2—Te3vi | 128.30 (2) | In5—In4—In5xiv | 0 |
Te3ii—Te2—Te3x | 98.08 (2) | In5xiii—In4—In5i | 0 |
Te3v—Te2—Te3 | 98.08 (3) | In5xiii—In4—In5 | 180 |
Te3v—Te2—Te3ii | 128.30 (4) | In5xiii—In4—In5xiv | 180 |
Te3v—Te2—Te3ix | 58.624 (13) | In5xiv—In4—In5i | 180 |
Te3v—Te2—Te3vi | 98.08 (3) | In5xiv—In4—In5 | 0 |
Te3v—Te2—Te3x | 128.30 (3) | In5xiv—In4—In5xiii | 180 |
Te3ix—Te2—Te3 | 128.30 (4) | In5i—In5—In5ii | 180 |
Te3ix—Te2—Te3ii | 98.08 (3) | In5i—In5—In5xiii | 0 |
Te3ix—Te2—Te3v | 58.624 (13) | In5i—In5—In5xiv | 180 |
Te3ix—Te2—Te3vi | 128.30 (3) | In5ii—In5—In5i | 180 |
Te3ix—Te2—Te3x | 98.08 (3) | In5ii—In5—In5xiii | 180 |
Te3vi—Te2—Te3 | 98.08 (2) | In5ii—In5—In5xiv | 0 |
Te3vi—Te2—Te3ii | 128.30 (2) | In5xiii—In5—In5i | 0 |
Te3vi—Te2—Te3v | 98.08 (3) | In5xiii—In5—In5ii | 180 |
Te3vi—Te2—Te3ix | 128.30 (3) | In5xiii—In5—In5xiv | 180 |
Te3vi—Te2—Te3x | 58.62 (2) | In5xiv—In5—In5i | 180 |
Te3x—Te2—Te3 | 128.30 (2) | In5xiv—In5—In5ii | 0 |
Te3x—Te2—Te3ii | 98.08 (2) | In5xiv—In5—In5xiii | 180 |
Symmetry codes: (i) x, y, z−1; (ii) x, y, z+1; (iii) −x+1, −y, −z; (iv) −x+1, −y, −z+1; (v) −x+y+1, −x+1, −z+1/2; (vi) −y+1, x−y, z; (vii) y, −x+y, −z; (viii) y, −x+y, −z+1; (ix) −x+y+1, −x+1, −z+3/2; (x) −y+1, x−y, z+1; (xi) x−y, x, z−1/2; (xii) x−y, x, z+1/2; (xiii) −x, −y, −z; (xiv) −x, −y, −z+1. |
Experimental details
Crystal data |
Chemical formula | In0.54Nb3Te4 |
Mr | 851.1 |
Crystal system, space group | Hexagonal, P63/m |
Temperature (K) | 295 |
a, c (Å) | 10.6768 (3), 3.6566 (1) |
V (Å3) | 360.99 (2) |
Z | 2 |
Radiation type | Synchrotron |
µ (mm−1) | 14.5 |
Specimen shape, size (mm) | Cylinder, 0.5 × 0.5 |
|
Data collection |
Diffractometer | ESRF ID15B diffractometer |
Specimen mounting | Lithiumborate glass capillary 0.5 mm diameter |
Data collection mode | Transmission |
Scan method | Energy dispersive |
2θ values (°) | 2θfixed = ? |
|
Refinement |
R factors and goodness of fit | Rp = 0.026, Rwp = 0.042, Rexp = ?, χ2 = 2.592 |
No. of data points | 1707 |
No. of parameters | 22 |
No. of restraints | ? |
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