Tin selenide-based functional materials are extensively studied in the field of optoelectronic, photovoltaic and thermoelectric devices. Specifically, SnSe has been reported to have an ultrahigh thermoelectric figure of merit of 2.6 ± 0.3 in the high-temperature phase. Here we report the evolution of lattice constants, fractional coordinates, site occupancy factors and atomic displacement factors with temperature by means of high-resolution synchrotron powder X-ray diffraction measured from 100 to 855 K. The structure is shown to be cation defective with a Sn content of 0.982 (4). The anisotropy of the thermal parameters of Sn becomes more pronounced approaching the high-temperature phase transition (∼ 810 K). Anharmonic Gram–Charlier parameters have been refined, but data from single-crystal diffraction appear to be needed to firmly quantify anharmonic features. Based on modelling of the atomic displacement parameters the Debye temperature is found to be 175 (4) K. Conflicting reports concerning the different coordinate system settings in the low-temperature and high-temperature phases are discussed. It is also shown that the high-temperature Cmcm phase is not pseudo-tetragonal as commonly assumed.
Supporting information
| Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520616003334/gw5043sup1.cif Contains datablocks global, 100, 200, 275, 300, 370, 380, 465, 560, 655, 705, 755, 805, 855 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043100sup2.hkl Contains datablock 100 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043200sup3.hkl Contains datablock 200 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043275sup4.hkl Contains datablock 275 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043300sup5.hkl Contains datablock 300 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043370sup6.hkl Contains datablock 370 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043380sup7.hkl Contains datablock 380 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043465sup8.hkl Contains datablock 465 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043560sup9.hkl Contains datablock 560 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043655sup10.hkl Contains datablock 655 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043705sup11.hkl Contains datablock 705 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043755sup12.hkl Contains datablock 755 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043805sup13.hkl Contains datablock 805 |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043855sup14.hkl Contains datablock 855 |
| Portable Document Format (PDF) file https://doi.org/10.1107/S2052520616003334/gw5043sup15.pdf Supporting figures |
CCDC references: 1455949; 1455950; 1455951; 1455952; 1455953; 1455954; 1455955; 1455956; 1455957; 1455958; 1455959; 1455960; 1455961
For all compounds, program(s) used to refine structure: Jana2006, (Petricek,2014).
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.176 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.44220 (9) Å | µ = 11.31 mm−1 |
b = 4.13054 (4) Å | T = 100 K |
c = 4.44900 (5) Å | metallic_grey |
V = 210.27 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.38°, 2θmax = 62.2°, 2θstep = 0.01° |
Refinement top
Rp = 0.015 | 32 parameters |
Rwp = 0.022 | 0 restraints |
Rexp = 0.010 | 0 constraints |
R(F) = 0.012 | Weighting scheme based on measured s.u.'s |
7800 data points | (Δ/σ)max = 0.035 |
Excluded region(s): from 0.01 to 4.370, from 62.21 to 78.078 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.11797 (3) | 0.25 | 0.10576 (7) | 0.00474 (11) | 0.9816 |
Se | 0.85523 (4) | 0.25 | 0.48229 (9) | 0.00499 (16) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.00419 (16) | 0.0047 (2) | 0.0053 (2) | 0 | −0.00112 (18) | 0 |
Se | 0.0052 (2) | 0.0048 (3) | 0.0050 (3) | 0 | −0.0004 (2) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.743 | Sn—Seiv | 3.442 |
Sn—Seii | 2.778 | Sn—Snv | 3.527 |
Sn—Seiii | 3.347 | Sn—Sevi | 4.090 |
| | | |
Sei—Sn—Seii | 89.140 | Seii—Sn—Seiii | 92.685 |
Sei—Sn—Seiii | 78.329 | Sei—Sn—Seiv | 159.083 |
Sevii—Sn—Seiii | 76.195 | Sei—Sn—Snv | 136.012 |
Seviii—Sn—Seii | 96.042 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.155 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.46438 (10) Å | µ = 11.27 mm−1 |
b = 4.13865 (4) Å | T = 200 K |
c = 4.44651 (6) Å | metallic_grey |
V = 210.97 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 3.41°, 2θmax = 54.73°, 2θstep = 0.01° |
Refinement top
Rp = 0.016 | 32 parameters |
Rwp = 0.023 | 0 restraints |
Rexp = 0.010 | 0 constraints |
R(F) = 0.013 | Weighting scheme based on measured s.u.'s |
7800 data points | (Δ/σ)max = 0.013 |
Excluded region(s): from 0.01 to 3.400, from 54.74 to 78.078 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.11818 (3) | 0.25 | 0.10454 (8) | 0.00911 (14) | 0.9816 |
Se | 0.85513 (4) | 0.25 | 0.48226 (10) | 0.00852 (19) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0084 (2) | 0.0087 (3) | 0.0102 (3) | 0 | −0.0025 (2) | 0 |
Se | 0.0091 (3) | 0.0080 (3) | 0.0084 (3) | 0 | −0.0008 (3) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.744 | Sn—Seiv | 3.452 |
Sn—Seii | 2.784 | Sn—Snv | 3.534 |
Sn—Seiii | 3.344 | Sn—Sevi | 4.093 |
| | | |
Sei—Sn—Seii | 89.086 | Seii—Sn—Seiii | 92.574 |
Sei—Sn—Seiii | 78.444 | Sei—Sn—Seiv | 158.972 |
Sevii—Sn—Seiii | 76.454 | Sei—Sn—Snv | 136.232 |
Seviii—Sn—Seii | 96.020 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.134 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.48933 (12) Å | µ = 11.23 mm−1 |
b = 4.14894 (5) Å | T = 275 K |
c = 4.44118 (7) Å | metallic_grey |
V = 211.71 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.02°, 2θmax = 53.18°, 2θstep = 0.01° |
Refinement top
Rp = 0.017 | 32 parameters |
Rwp = 0.023 | 0 restraints |
Rexp = 0.009 | 0 constraints |
R(F) = 0.021 | Weighting scheme based on measured s.u.'s |
7801 data points | (Δ/σ)max = 0.024 |
Excluded region(s): from 0.01 to 4.010, from 53.19 to 78.088 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.11846 (3) | 0.25 | 0.10274 (9) | 0.01406 (17) | 0.9816 |
Se | 0.85505 (4) | 0.25 | 0.48208 (11) | 0.0122 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0132 (3) | 0.0129 (3) | 0.0161 (3) | 0 | −0.0040 (3) | 0 |
Se | 0.0128 (3) | 0.0123 (4) | 0.0116 (4) | 0 | −0.0015 (3) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.744 | Sn—Seiv | 3.464 |
Sn—Seii | 2.792 | Sn—Snv | 3.542 |
Sn—Seiii | 3.338 | Sn—Sevi | 4.094 |
| | | |
Sei—Sn—Seii | 89.009 | Seii—Sn—Seiii | 92.417 |
Sei—Sn—Seiii | 78.632 | Sei—Sn—Seiv | 158.786 |
Sevii—Sn—Seiii | 76.848 | Sei—Sn—Snv | 136.541 |
Seviii—Sn—Seii | 95.971 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.127 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.49417 (12) Å | µ = 11.22 mm−1 |
b = 4.15096 (5) Å | T = 300 K |
c = 4.44175 (7) Å | metallic_grey |
V = 211.92 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 3.31°, 2θmax = 48.15°, 2θstep = 0.01° |
Refinement top
Rp = 0.016 | 32 parameters |
Rwp = 0.022 | 0 restraints |
Rexp = 0.014 | 0 constraints |
R(F) = 0.018 | Weighting scheme based on measured s.u.'s |
7797 data points | (Δ/σ)max = 0.016 |
Excluded region(s): from 0.01 to 3.300, from 48.16 to 78.048 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.11849 (4) | 0.25 | 0.10297 (9) | 0.01313 (18) | 0.9816 |
Se | 0.85523 (5) | 0.25 | 0.48204 (11) | 0.0115 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0125 (3) | 0.0129 (3) | 0.0140 (3) | 0 | −0.0034 (3) | 0 |
Se | 0.0120 (4) | 0.0116 (4) | 0.0111 (4) | 0 | −0.0013 (3) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.747 | Sn—Seiv | 3.463 |
Sn—Seii | 2.792 | Sn—Snv | 3.545 |
Sn—Seiii | 3.339 | Sn—Sevi | 4.094 |
| | | |
Sei—Sn—Seii | 89.059 | Seii—Sn—Seiii | 92.402 |
Sei—Sn—Seiii | 78.664 | Sei—Sn—Seiv | 158.808 |
Sevii—Sn—Seiii | 76.856 | Sei—Sn—Snv | 136.527 |
Seviii—Sn—Seii | 96.028 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.111 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.51746 (14) Å | µ = 11.19 mm−1 |
b = 4.16192 (6) Å | T = 370 K |
c = 4.43267 (8) Å | metallic_grey |
V = 212.48 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 3.89°, 2θmax = 38.28°, 2θstep = 0.01° |
Refinement top
Rp = 0.018 | 32 parameters |
Rwp = 0.024 | 0 restraints |
Rexp = 0.009 | 0 constraints |
R(F) = 0.015 | Weighting scheme based on measured s.u.'s |
7801 data points | (Δ/σ)max = 0.017 |
Excluded region(s): from 0.01 to 3.880, from 38.29 to 78.088 | Background function: 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.11879 (4) | 0.25 | 0.10015 (10) | 0.0201 (2) | 0.9816 |
Se | 0.85505 (5) | 0.25 | 0.48222 (13) | 0.0165 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0197 (4) | 0.0189 (4) | 0.0218 (4) | 0 | −0.0055 (4) | 0 |
Se | 0.0172 (5) | 0.0160 (5) | 0.0162 (5) | 0 | −0.0023 (4) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.745 | Sn—Seiv | 3.478 |
Sn—Seii | 2.801 | Sn—Snv | 3.551 |
Sn—Seiii | 3.329 | Sn—Sevi | 4.090 |
| | | |
Sei—Sn—Seii | 88.928 | Seii—Sn—Seiii | 92.198 |
Sei—Sn—Seiii | 78.884 | Sei—Sn—Seiv | 158.501 |
Sevii—Sn—Seiii | 77.368 | Sei—Sn—Snv | 136.936 |
Seviii—Sn—Seii | 95.943 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.107 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.51965 (14) Å | µ = 11.18 mm−1 |
b = 4.16265 (6) Å | T = 380 K |
c = 4.43427 (8) Å | metallic_grey |
V = 212.63 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.02°, 2θmax = 38.28°, 2θstep = 0.01° |
Refinement top
Rp = 0.017 | 32 parameters |
Rwp = 0.022 | 0 restraints |
Rexp = 0.013 | 0 constraints |
R(F) = 0.017 | Weighting scheme based on measured s.u.'s |
7797 data points | (Δ/σ)max = 0.015 |
Excluded region(s): from 0.01 to 4.010, from 38.29 to 78.048 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.11883 (4) | 0.25 | 0.10051 (10) | 0.0186 (2) | 0.9816 |
Se | 0.85524 (5) | 0.25 | 0.48217 (12) | 0.0150 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0183 (3) | 0.0183 (4) | 0.0192 (4) | 0 | −0.0048 (3) | 0 |
Se | 0.0153 (4) | 0.0149 (5) | 0.0149 (5) | 0 | −0.0016 (4) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.748 | Sn—Seiv | 3.476 |
Sn—Seii | 2.801 | Sn—Snv | 3.553 |
Sn—Seiii | 3.331 | Sn—Sevi | 4.091 |
| | | |
Sei—Sn—Seii | 88.994 | Seii—Sn—Seiii | 92.212 |
Sei—Sn—Seiii | 78.910 | Sei—Sn—Seiv | 158.533 |
Sevii—Sn—Seiii | 77.335 | Sei—Sn—Snv | 136.908 |
Seviii—Sn—Seii | 95.986 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.088 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.54547 (15) Å | µ = 11.14 mm−1 |
b = 4.17619 (6) Å | T = 465 K |
c = 4.42402 (9) Å | metallic_grey |
V = 213.31 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.02°, 2θmax = 38.28°, 2θstep = 0.01° |
Refinement top
Rp = 0.017 | 32 parameters |
Rwp = 0.023 | 0 restraints |
Rexp = 0.013 | 0 constraints |
R(F) = 0.024 | Weighting scheme based on measured s.u.'s |
7797 data points | (Δ/σ)max = 0.020 |
Excluded region(s): from 0.01 to 4.010, from 38.29 to 78.048 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.11923 (4) | 0.25 | 0.09733 (11) | 0.0237 (2) | 0.9816 |
Se | 0.85523 (6) | 0.25 | 0.48242 (13) | 0.0185 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0239 (4) | 0.0229 (5) | 0.0241 (4) | 0 | −0.0058 (4) | 0 |
Se | 0.0183 (5) | 0.0190 (5) | 0.0184 (5) | 0 | −0.0024 (4) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.748 | Sn—Seiv | 3.492 |
Sn—Seii | 2.811 | Sn—Snv | 3.561 |
Sn—Seiii | 3.320 | Sn—Sevi | 4.085 |
| | | |
Sei—Sn—Seii | 88.906 | Seii—Sn—Seiii | 91.973 |
Sei—Sn—Seiii | 79.208 | Sei—Sn—Seiv | 158.175 |
Sevii—Sn—Seiii | 77.932 | Sei—Sn—Snv | 137.362 |
Seviii—Sn—Seii | 95.930 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.063 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.57949 (14) Å | µ = 11.10 mm−1 |
b = 4.19611 (5) Å | T = 560 K |
c = 4.40769 (8) Å | metallic_grey |
V = 214.16 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.02°, 2θmax = 37.82°, 2θstep = 0.01° |
Refinement top
Rp = 0.017 | 32 parameters |
Rwp = 0.022 | 0 restraints |
Rexp = 0.013 | 0 constraints |
R(F) = 0.028 | Weighting scheme based on measured s.u.'s |
7797 data points | (Δ/σ)max = 0.035 |
Excluded region(s): from 0.01 to 4.010, from 37.83 to 78.048 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.11982 (5) | 0.25 | 0.09182 (11) | 0.0301 (3) | 0.9816 |
Se | 0.85529 (6) | 0.25 | 0.48266 (13) | 0.0233 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0300 (4) | 0.0291 (5) | 0.0313 (4) | 0 | −0.0079 (4) | 0 |
Se | 0.0227 (5) | 0.0241 (5) | 0.0231 (6) | 0 | −0.0025 (4) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.746 | Sn—Seiv | 3.514 |
Sn—Seii | 2.829 | Sn—Snv | 3.572 |
Sn—Seiii | 3.301 | Sn—Sevi | 4.073 |
| | | |
Sei—Sn—Seii | 88.744 | Seii—Sn—Seiii | 91.621 |
Sei—Sn—Seiii | 79.723 | Sei—Sn—Seiv | 157.512 |
Sevii—Sn—Seiii | 78.926 | Sei—Sn—Snv | 138.094 |
Seviii—Sn—Seii | 95.744 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.036 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.62000 (13) Å | µ = 11.05 mm−1 |
b = 4.22357 (6) Å | T = 655 K |
c = 4.38333 (7) Å | metallic_grey |
V = 215.13 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.02°, 2θmax = 37.82°, 2θstep = 0.01° |
Refinement top
Rp = 0.017 | 32 parameters |
Rwp = 0.023 | 0 restraints |
Rexp = 0.013 | 0 constraints |
R(F) = 0.035 | Weighting scheme based on measured s.u.'s |
7797 data points | (Δ/σ)max = 0.041 |
Excluded region(s): from 0.01 to 4.010, from 37.83 to 78.048 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.12084 (5) | 0.25 | 0.08170 (12) | 0.0371 (3) | 0.9816 |
Se | 0.85555 (6) | 0.25 | 0.48400 (14) | 0.0295 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0352 (5) | 0.0359 (6) | 0.0403 (5) | 0 | −0.0083 (5) | 0 |
Se | 0.0274 (6) | 0.0306 (6) | 0.0304 (7) | 0 | −0.0011 (5) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.742 | Sn—Seiv | 3.551 |
Sn—Seii | 2.856 | Sn—Snv | 3.586 |
Sn—Seiii | 3.269 | Sn—Sevi | 4.046 |
| | | |
Sei—Sn—Seii | 88.539 | Seii—Sn—Seiii | 91.139 |
Sei—Sn—Seiii | 80.612 | Sei—Sn—Seiv | 156.257 |
Sevii—Sn—Seiii | 80.494 | Sei—Sn—Snv | 139.274 |
Seviii—Sn—Seii | 95.348 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.022 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.64398 (13) Å | µ = 11.02 mm−1 |
b = 4.24224 (5) Å | T = 705 K |
c = 4.36522 (7) Å | metallic_grey |
V = 215.63 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.02°, 2θmax = 34.48°, 2θstep = 0.01° |
Refinement top
Rp = 0.018 | 32 parameters |
Rwp = 0.024 | 0 restraints |
Rexp = 0.013 | 0 constraints |
R(F) = 0.031 | Weighting scheme based on measured s.u.'s |
7797 data points | (Δ/σ)max = 0.011 |
Excluded region(s): from 0.01 to 4.010, from 34.49 to 78.048 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.12148 (6) | 0.25 | 0.07350 (13) | 0.0416 (3) | 0.9816 |
Se | 0.85571 (7) | 0.25 | 0.48517 (16) | 0.0326 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0386 (5) | 0.0417 (7) | 0.0446 (6) | 0 | −0.0088 (5) | 0 |
Se | 0.0299 (6) | 0.0330 (7) | 0.0348 (7) | 0 | −0.0007 (6) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.739 | Sn—Seiv | 3.579 |
Sn—Seii | 2.878 | Sn—Snv | 3.594 |
Sn—Seiii | 3.243 | Sn—Sevi | 4.021 |
| | | |
Sei—Sn—Seii | 88.321 | Seii—Sn—Seiii | 90.789 |
Sei—Sn—Seiii | 81.266 | Sei—Sn—Seiv | 155.221 |
Sevii—Sn—Seiii | 81.697 | Sei—Sn—Snv | 140.094 |
Seviii—Sn—Seii | 94.968 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 6.007 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.67175 (14) Å | µ = 11.00 mm−1 |
b = 4.26761 (6) Å | T = 755 K |
c = 4.33976 (7) Å | metallic_grey |
V = 216.17 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.02°, 2θmax = 34.48°, 2θstep = 0.01° |
Refinement top
Rp = 0.020 | 27 parameters |
Rwp = 0.026 | 0 restraints |
Rexp = 0.013 | 0 constraints |
R(F) = 0.042 | Weighting scheme based on measured s.u.'s |
7797 data points | (Δ/σ)max = 0.046 |
Excluded region(s): from 0.01 to 4.010, from 34.49 to 78.048 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.12231 (6) | 0.25 | 0.05985 (16) | 0.0475 (4) | 0.9816 |
Se | 0.85591 (7) | 0.25 | 0.4881 (2) | 0.0351 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0419 (6) | 0.0498 (8) | 0.0508 (7) | 0 | −0.0100 (7) | 0 |
Se | 0.0339 (7) | 0.0331 (9) | 0.0383 (9) | 0 | −0.0028 (7) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.734 | Sn—Seiv | 3.622 |
Sn—Seii | 2.910 | Sn—Snv | 3.602 |
Sn—Seiii | 3.205 | Sn—Sevi | 3.978 |
| | | |
Sei—Sn—Seii | 87.948 | Seii—Sn—Seiii | 90.291 |
Sei—Sn—Seiii | 82.211 | Sei—Sn—Seiv | 153.496 |
Sevii—Sn—Seiii | 83.482 | Sei—Sn—Snv | 141.203 |
Seviii—Sn—Seii | 94.334 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Pnma | Dx = 5.991 Mg m−3 |
Hall symbol: -P 2ac 2n | Synchrotron,monochromatic radiation |
a = 11.70577 (16) Å | µ = 10.97 mm−1 |
b = 4.30722 (16) Å | T = 805 K |
c = 4.29911 (16) Å | metallic_grey |
V = 216.76 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.02°, 2θmax = 34.48°, 2θstep = 0.01° |
Refinement top
Rp = 0.022 | 32 parameters |
Rwp = 0.030 | 0 restraints |
Rexp = 0.013 | 0 constraints |
R(F) = 0.058 | Weighting scheme based on measured s.u.'s |
7797 data points | (Δ/σ)max = 0.040 |
Excluded region(s): from 0.01 to 4.010, from 34.49 to 78.048 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0.12399 (7) | 0.25 | 0.0192 (6) | 0.0577 (9) | 0.9816 |
Se | 0.85663 (9) | 0.25 | 0.4968 (8) | 0.0396 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0479 (7) | 0.062 (2) | 0.0627 (16) | 0 | −0.0181 (19) | 0 |
Se | 0.0402 (10) | 0.038 (2) | 0.0406 (18) | 0 | 0.000 (2) | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.724 | Sn—Seiv | 3.743 |
Sn—Seii | 3.003 | Sn—Snv | 3.618 |
Sn—Seiii | 3.100 | Sn—Sevi | 3.852 |
| | | |
Sei—Sn—Seii | 86.677 | Seii—Sn—Seiii | 89.547 |
Sei—Sn—Seiii | 84.766 | Sei—Sn—Seiv | 148.185 |
Sevii—Sn—Seiii | 88.003 | Sei—Sn—Snv | 143.213 |
Seviii—Sn—Seii | 91.636 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1/2; (ii) −x+1, y+1/2, −z+1; (iii) −x+1, y+1/2, −z; (iv) x−1, y, z; (v) −x, y−1/2, −z; (vi) x−1, y, z−1; (vii) −x+1, y−1/2, −z; (viii) −x+1, y−1/2, −z+1. |
Crystal data top
SeSn0.9816 | Z = 4 |
Mr = 195.50 | F(000) = 332.3 |
Orthorhombic, Cmcm | Dx = 5.973 Mg m−3 |
Hall symbol: -C 2c 2 | Synchrotron,monochromatic radiation |
a = 4.29978 (8) Å | µ = 10.93 mm−1 |
b = 11.71878 (17) Å | T = 855 K |
c = 4.31479 (8) Å | metallic_grey |
V = 217.41 (1) Å3 | |
Data collection top
BL44B2 diffractometer | Data collection mode: transmission |
Specimen mounting: capillary | 2θmin = 4.02°, 2θmax = 32.22°, 2θstep = 0.01° |
Refinement top
Rp = 0.022 | 28 parameters |
Rwp = 0.030 | 0 restraints |
Rexp = 0.013 | 0 constraints |
R(F) = 0.032 | Weighting scheme based on measured s.u.'s |
7798 data points | (Δ/σ)max = 0.013 |
Excluded region(s): from 0.01 to 4.010, from 32.23 to 78.058 | Background function: Manual background combined with 8 Chebyshev polynoms |
Profile function: Pseudo-Voigt | Preferred orientation correction: none |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn | 0 | 0.12424 (7) | 0.25 | 0.0634 (6) | 0.9816 |
Se | 0.5 | 0.85654 (8) | 0.25 | 0.0422 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0804 (13) | 0.0492 (8) | 0.0606 (11) | 0 | 0 | 0 |
Se | 0.0490 (14) | 0.0400 (10) | 0.0375 (13) | 0 | 0 | 0 |
Geometric parameters (Å, º) top
Sn—Sei | 2.722 | Sn—Seiv | 3.803 |
Sn—Seii | 3.054 | Sn—Snv | 3.624 |
Sn—Seiii | 3.054 | Sn—Sevi | 3.803 |
| | | |
Sei—Sn—Seii | 85.771 | Seii—Sn—Seiii | 89.490 |
Sei—Sn—Seiii | 85.771 | Sei—Sn—Seiv | 145.577 |
Sevii—Sn—Seiii | 89.887 | Sei—Sn—Snv | 143.465 |
Seviii—Sn—Seii | 89.887 | | |
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) −x+1, −y+1, z+1/2; (iii) −x, −y+1, z+1/2; (iv) x, y−1, z; (v) −x, −y, z−1/2; (vi) x−1, y−1, z; (vii) −x, −y+1, z−1/2; (viii) −x+1, −y+1, z−1/2. |