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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

cif

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

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043100sup2.hkl
Contains datablock 100

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043200sup3.hkl
Contains datablock 200

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043275sup4.hkl
Contains datablock 275

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043300sup5.hkl
Contains datablock 300

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043370sup6.hkl
Contains datablock 370

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043380sup7.hkl
Contains datablock 380

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043465sup8.hkl
Contains datablock 465

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043560sup9.hkl
Contains datablock 560

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043655sup10.hkl
Contains datablock 655

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043705sup11.hkl
Contains datablock 705

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043755sup12.hkl
Contains datablock 755

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043805sup13.hkl
Contains datablock 805

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Structure factor file (CIF format) https://doi.org/10.1107/S2052520616003334/gw5043855sup14.hkl
Contains datablock 855

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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

Computing details top

For all compounds, program(s) used to refine structure: Jana2006, (Petricek,2014).

(100) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.176 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.44220 (9) ŵ = 11.31 mm1
b = 4.13054 (4) ÅT = 100 K
c = 4.44900 (5) Åmetallic_grey
V = 210.27 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.38°, 2θmax = 62.2°, 2θstep = 0.01°
Refinement top
Rp = 0.01532 parameters
Rwp = 0.0220 restraints
Rexp = 0.0100 constraints
R(F) = 0.012Weighting 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 78.078Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.11797 (3)0.250.10576 (7)0.00474 (11)0.9816
Se0.85523 (4)0.250.48229 (9)0.00499 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.00419 (16)0.0047 (2)0.0053 (2)00.00112 (18)0
Se0.0052 (2)0.0048 (3)0.0050 (3)00.0004 (2)0
Geometric parameters (Å, º) top
Sn—Sei2.743Sn—Seiv3.442
Sn—Seii2.778Sn—Snv3.527
Sn—Seiii3.347Sn—Sevi4.090
Sei—Sn—Seii89.140Seii—Sn—Seiii92.685
Sei—Sn—Seiii78.329Sei—Sn—Seiv159.083
Sevii—Sn—Seiii76.195Sei—Sn—Snv136.012
Seviii—Sn—Seii96.042
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(200) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.155 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.46438 (10) ŵ = 11.27 mm1
b = 4.13865 (4) ÅT = 200 K
c = 4.44651 (6) Åmetallic_grey
V = 210.97 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 3.41°, 2θmax = 54.73°, 2θstep = 0.01°
Refinement top
Rp = 0.01632 parameters
Rwp = 0.0230 restraints
Rexp = 0.0100 constraints
R(F) = 0.013Weighting 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 78.078Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.11818 (3)0.250.10454 (8)0.00911 (14)0.9816
Se0.85513 (4)0.250.48226 (10)0.00852 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0084 (2)0.0087 (3)0.0102 (3)00.0025 (2)0
Se0.0091 (3)0.0080 (3)0.0084 (3)00.0008 (3)0
Geometric parameters (Å, º) top
Sn—Sei2.744Sn—Seiv3.452
Sn—Seii2.784Sn—Snv3.534
Sn—Seiii3.344Sn—Sevi4.093
Sei—Sn—Seii89.086Seii—Sn—Seiii92.574
Sei—Sn—Seiii78.444Sei—Sn—Seiv158.972
Sevii—Sn—Seiii76.454Sei—Sn—Snv136.232
Seviii—Sn—Seii96.020
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(275) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.134 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.48933 (12) ŵ = 11.23 mm1
b = 4.14894 (5) ÅT = 275 K
c = 4.44118 (7) Åmetallic_grey
V = 211.71 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.02°, 2θmax = 53.18°, 2θstep = 0.01°
Refinement top
Rp = 0.01732 parameters
Rwp = 0.0230 restraints
Rexp = 0.0090 constraints
R(F) = 0.021Weighting 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 78.088Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.11846 (3)0.250.10274 (9)0.01406 (17)0.9816
Se0.85505 (4)0.250.48208 (11)0.0122 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0132 (3)0.0129 (3)0.0161 (3)00.0040 (3)0
Se0.0128 (3)0.0123 (4)0.0116 (4)00.0015 (3)0
Geometric parameters (Å, º) top
Sn—Sei2.744Sn—Seiv3.464
Sn—Seii2.792Sn—Snv3.542
Sn—Seiii3.338Sn—Sevi4.094
Sei—Sn—Seii89.009Seii—Sn—Seiii92.417
Sei—Sn—Seiii78.632Sei—Sn—Seiv158.786
Sevii—Sn—Seiii76.848Sei—Sn—Snv136.541
Seviii—Sn—Seii95.971
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(300) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.127 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.49417 (12) ŵ = 11.22 mm1
b = 4.15096 (5) ÅT = 300 K
c = 4.44175 (7) Åmetallic_grey
V = 211.92 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 3.31°, 2θmax = 48.15°, 2θstep = 0.01°
Refinement top
Rp = 0.01632 parameters
Rwp = 0.0220 restraints
Rexp = 0.0140 constraints
R(F) = 0.018Weighting 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 78.048Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.11849 (4)0.250.10297 (9)0.01313 (18)0.9816
Se0.85523 (5)0.250.48204 (11)0.0115 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0125 (3)0.0129 (3)0.0140 (3)00.0034 (3)0
Se0.0120 (4)0.0116 (4)0.0111 (4)00.0013 (3)0
Geometric parameters (Å, º) top
Sn—Sei2.747Sn—Seiv3.463
Sn—Seii2.792Sn—Snv3.545
Sn—Seiii3.339Sn—Sevi4.094
Sei—Sn—Seii89.059Seii—Sn—Seiii92.402
Sei—Sn—Seiii78.664Sei—Sn—Seiv158.808
Sevii—Sn—Seiii76.856Sei—Sn—Snv136.527
Seviii—Sn—Seii96.028
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(370) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.111 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.51746 (14) ŵ = 11.19 mm1
b = 4.16192 (6) ÅT = 370 K
c = 4.43267 (8) Åmetallic_grey
V = 212.48 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 3.89°, 2θmax = 38.28°, 2θstep = 0.01°
Refinement top
Rp = 0.01832 parameters
Rwp = 0.0240 restraints
Rexp = 0.0090 constraints
R(F) = 0.015Weighting 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 78.088Background function: 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.11879 (4)0.250.10015 (10)0.0201 (2)0.9816
Se0.85505 (5)0.250.48222 (13)0.0165 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0197 (4)0.0189 (4)0.0218 (4)00.0055 (4)0
Se0.0172 (5)0.0160 (5)0.0162 (5)00.0023 (4)0
Geometric parameters (Å, º) top
Sn—Sei2.745Sn—Seiv3.478
Sn—Seii2.801Sn—Snv3.551
Sn—Seiii3.329Sn—Sevi4.090
Sei—Sn—Seii88.928Seii—Sn—Seiii92.198
Sei—Sn—Seiii78.884Sei—Sn—Seiv158.501
Sevii—Sn—Seiii77.368Sei—Sn—Snv136.936
Seviii—Sn—Seii95.943
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(380) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.107 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.51965 (14) ŵ = 11.18 mm1
b = 4.16265 (6) ÅT = 380 K
c = 4.43427 (8) Åmetallic_grey
V = 212.63 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.02°, 2θmax = 38.28°, 2θstep = 0.01°
Refinement top
Rp = 0.01732 parameters
Rwp = 0.0220 restraints
Rexp = 0.0130 constraints
R(F) = 0.017Weighting 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 78.048Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.11883 (4)0.250.10051 (10)0.0186 (2)0.9816
Se0.85524 (5)0.250.48217 (12)0.0150 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0183 (3)0.0183 (4)0.0192 (4)00.0048 (3)0
Se0.0153 (4)0.0149 (5)0.0149 (5)00.0016 (4)0
Geometric parameters (Å, º) top
Sn—Sei2.748Sn—Seiv3.476
Sn—Seii2.801Sn—Snv3.553
Sn—Seiii3.331Sn—Sevi4.091
Sei—Sn—Seii88.994Seii—Sn—Seiii92.212
Sei—Sn—Seiii78.910Sei—Sn—Seiv158.533
Sevii—Sn—Seiii77.335Sei—Sn—Snv136.908
Seviii—Sn—Seii95.986
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(465) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.088 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.54547 (15) ŵ = 11.14 mm1
b = 4.17619 (6) ÅT = 465 K
c = 4.42402 (9) Åmetallic_grey
V = 213.31 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.02°, 2θmax = 38.28°, 2θstep = 0.01°
Refinement top
Rp = 0.01732 parameters
Rwp = 0.0230 restraints
Rexp = 0.0130 constraints
R(F) = 0.024Weighting 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 78.048Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.11923 (4)0.250.09733 (11)0.0237 (2)0.9816
Se0.85523 (6)0.250.48242 (13)0.0185 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0239 (4)0.0229 (5)0.0241 (4)00.0058 (4)0
Se0.0183 (5)0.0190 (5)0.0184 (5)00.0024 (4)0
Geometric parameters (Å, º) top
Sn—Sei2.748Sn—Seiv3.492
Sn—Seii2.811Sn—Snv3.561
Sn—Seiii3.320Sn—Sevi4.085
Sei—Sn—Seii88.906Seii—Sn—Seiii91.973
Sei—Sn—Seiii79.208Sei—Sn—Seiv158.175
Sevii—Sn—Seiii77.932Sei—Sn—Snv137.362
Seviii—Sn—Seii95.930
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(560) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.063 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.57949 (14) ŵ = 11.10 mm1
b = 4.19611 (5) ÅT = 560 K
c = 4.40769 (8) Åmetallic_grey
V = 214.16 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.02°, 2θmax = 37.82°, 2θstep = 0.01°
Refinement top
Rp = 0.01732 parameters
Rwp = 0.0220 restraints
Rexp = 0.0130 constraints
R(F) = 0.028Weighting 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 78.048Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.11982 (5)0.250.09182 (11)0.0301 (3)0.9816
Se0.85529 (6)0.250.48266 (13)0.0233 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0300 (4)0.0291 (5)0.0313 (4)00.0079 (4)0
Se0.0227 (5)0.0241 (5)0.0231 (6)00.0025 (4)0
Geometric parameters (Å, º) top
Sn—Sei2.746Sn—Seiv3.514
Sn—Seii2.829Sn—Snv3.572
Sn—Seiii3.301Sn—Sevi4.073
Sei—Sn—Seii88.744Seii—Sn—Seiii91.621
Sei—Sn—Seiii79.723Sei—Sn—Seiv157.512
Sevii—Sn—Seiii78.926Sei—Sn—Snv138.094
Seviii—Sn—Seii95.744
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(655) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.036 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.62000 (13) ŵ = 11.05 mm1
b = 4.22357 (6) ÅT = 655 K
c = 4.38333 (7) Åmetallic_grey
V = 215.13 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.02°, 2θmax = 37.82°, 2θstep = 0.01°
Refinement top
Rp = 0.01732 parameters
Rwp = 0.0230 restraints
Rexp = 0.0130 constraints
R(F) = 0.035Weighting 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 78.048Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.12084 (5)0.250.08170 (12)0.0371 (3)0.9816
Se0.85555 (6)0.250.48400 (14)0.0295 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0352 (5)0.0359 (6)0.0403 (5)00.0083 (5)0
Se0.0274 (6)0.0306 (6)0.0304 (7)00.0011 (5)0
Geometric parameters (Å, º) top
Sn—Sei2.742Sn—Seiv3.551
Sn—Seii2.856Sn—Snv3.586
Sn—Seiii3.269Sn—Sevi4.046
Sei—Sn—Seii88.539Seii—Sn—Seiii91.139
Sei—Sn—Seiii80.612Sei—Sn—Seiv156.257
Sevii—Sn—Seiii80.494Sei—Sn—Snv139.274
Seviii—Sn—Seii95.348
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(705) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.022 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.64398 (13) ŵ = 11.02 mm1
b = 4.24224 (5) ÅT = 705 K
c = 4.36522 (7) Åmetallic_grey
V = 215.63 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.02°, 2θmax = 34.48°, 2θstep = 0.01°
Refinement top
Rp = 0.01832 parameters
Rwp = 0.0240 restraints
Rexp = 0.0130 constraints
R(F) = 0.031Weighting 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 78.048Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.12148 (6)0.250.07350 (13)0.0416 (3)0.9816
Se0.85571 (7)0.250.48517 (16)0.0326 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0386 (5)0.0417 (7)0.0446 (6)00.0088 (5)0
Se0.0299 (6)0.0330 (7)0.0348 (7)00.0007 (6)0
Geometric parameters (Å, º) top
Sn—Sei2.739Sn—Seiv3.579
Sn—Seii2.878Sn—Snv3.594
Sn—Seiii3.243Sn—Sevi4.021
Sei—Sn—Seii88.321Seii—Sn—Seiii90.789
Sei—Sn—Seiii81.266Sei—Sn—Seiv155.221
Sevii—Sn—Seiii81.697Sei—Sn—Snv140.094
Seviii—Sn—Seii94.968
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(755) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 6.007 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.67175 (14) ŵ = 11.00 mm1
b = 4.26761 (6) ÅT = 755 K
c = 4.33976 (7) Åmetallic_grey
V = 216.17 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.02°, 2θmax = 34.48°, 2θstep = 0.01°
Refinement top
Rp = 0.02027 parameters
Rwp = 0.0260 restraints
Rexp = 0.0130 constraints
R(F) = 0.042Weighting 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 78.048Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.12231 (6)0.250.05985 (16)0.0475 (4)0.9816
Se0.85591 (7)0.250.4881 (2)0.0351 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0419 (6)0.0498 (8)0.0508 (7)00.0100 (7)0
Se0.0339 (7)0.0331 (9)0.0383 (9)00.0028 (7)0
Geometric parameters (Å, º) top
Sn—Sei2.734Sn—Seiv3.622
Sn—Seii2.910Sn—Snv3.602
Sn—Seiii3.205Sn—Sevi3.978
Sei—Sn—Seii87.948Seii—Sn—Seiii90.291
Sei—Sn—Seiii82.211Sei—Sn—Seiv153.496
Sevii—Sn—Seiii83.482Sei—Sn—Snv141.203
Seviii—Sn—Seii94.334
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(805) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, PnmaDx = 5.991 Mg m3
Hall symbol: -P 2ac 2nSynchrotron,monochromatic radiation
a = 11.70577 (16) ŵ = 10.97 mm1
b = 4.30722 (16) ÅT = 805 K
c = 4.29911 (16) Åmetallic_grey
V = 216.76 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.02°, 2θmax = 34.48°, 2θstep = 0.01°
Refinement top
Rp = 0.02232 parameters
Rwp = 0.0300 restraints
Rexp = 0.0130 constraints
R(F) = 0.058Weighting 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 78.048Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn0.12399 (7)0.250.0192 (6)0.0577 (9)0.9816
Se0.85663 (9)0.250.4968 (8)0.0396 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0479 (7)0.062 (2)0.0627 (16)00.0181 (19)0
Se0.0402 (10)0.038 (2)0.0406 (18)00.000 (2)0
Geometric parameters (Å, º) top
Sn—Sei2.724Sn—Seiv3.743
Sn—Seii3.003Sn—Snv3.618
Sn—Seiii3.100Sn—Sevi3.852
Sei—Sn—Seii86.677Seii—Sn—Seiii89.547
Sei—Sn—Seiii84.766Sei—Sn—Seiv148.185
Sevii—Sn—Seiii88.003Sei—Sn—Snv143.213
Seviii—Sn—Seii91.636
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1, y+1/2, z+1; (iii) x+1, y+1/2, z; (iv) x1, y, z; (v) x, y1/2, z; (vi) x1, y, z1; (vii) x+1, y1/2, z; (viii) x+1, y1/2, z+1.
(855) top
Crystal data top
SeSn0.9816Z = 4
Mr = 195.50F(000) = 332.3
Orthorhombic, CmcmDx = 5.973 Mg m3
Hall symbol: -C 2c 2Synchrotron,monochromatic radiation
a = 4.29978 (8) ŵ = 10.93 mm1
b = 11.71878 (17) ÅT = 855 K
c = 4.31479 (8) Åmetallic_grey
V = 217.41 (1) Å3
Data collection top
BL44B2
diffractometer
Data collection mode: transmission
Specimen mounting: capillary2θmin = 4.02°, 2θmax = 32.22°, 2θstep = 0.01°
Refinement top
Rp = 0.02228 parameters
Rwp = 0.0300 restraints
Rexp = 0.0130 constraints
R(F) = 0.032Weighting 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 78.058Background function: Manual background combined with 8 Chebyshev polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn00.12424 (7)0.250.0634 (6)0.9816
Se0.50.85654 (8)0.250.0422 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0804 (13)0.0492 (8)0.0606 (11)000
Se0.0490 (14)0.0400 (10)0.0375 (13)000
Geometric parameters (Å, º) top
Sn—Sei2.722Sn—Seiv3.803
Sn—Seii3.054Sn—Snv3.624
Sn—Seiii3.054Sn—Sevi3.803
Sei—Sn—Seii85.771Seii—Sn—Seiii89.490
Sei—Sn—Seiii85.771Sei—Sn—Seiv145.577
Sevii—Sn—Seiii89.887Sei—Sn—Snv143.465
Seviii—Sn—Seii89.887
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+1, y+1, z+1/2; (iii) x, y+1, z+1/2; (iv) x, y1, z; (v) x, y, z1/2; (vi) x1, y1, z; (vii) x, y+1, z1/2; (viii) x+1, y+1, z1/2.
 

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