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The stable structures of deuterated thiophene C4D4S were investigated at 155 (phase III), 115 (phase IV), 100 and 1.5 K (phase V) by neutron powder diffraction. At 155 K, thiophene is orthorhombic with space group Pbnm. Although there is some degree of in-plane orientational disorder, molecules begin to order along two symmetrically equivalent main orientations. At 115 K the structure is incommensurate, with a wavevector q ≃ 0.55a*. At 100 K and below, there is a doubling of the a cell parameter and the structure space group is P21. For the first time, it is shown that, unlike C4H4S, phase V of C4D4S is not an orientational glass: thiophene molecules are perfectly ordered and are oriented within the molecular plane along two alternating directions, corresponding to the two main orientations observed at 155 K. This ordering probably originates in the slowing down of the in-plane reorientational dynamics upon deuteration.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768108015103/kd5024sup1.cif
Contains datablocks global, 100K, 1.5K, 155K, 115K

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768108015103/kd5024100Ksup2.rtv
Contains datablock 100K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108015103/kd5024100Ksup3.hkl
Contains datablock 100K

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768108015103/kd50241point5Ksup4.rtv
Contains datablock 1point5K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108015103/kd50241point5Ksup5.hkl
Contains datablock 1point5K

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768108015103/kd5024155Ksup6.rtv
Contains datablock 155K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108015103/kd5024155Ksup7.hkl
Contains datablock 155K

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768108015103/kd5024115Ksup8.rtv
Contains datablock 115K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108015103/kd5024115Ksup9.hkl
Contains datablock 115K

CCDC references: 705588; 705589; 705590

Experimental top

The synthesis of deuterated thiophene was performed as described in Dunstetter et al. Chem. Phys. 175, 475 (1993)

Computing details top

Program(s) used to refine structure: FULLPROF for 100K, 1point5K, 155K; (Jana2000; Petricek and Dusek, 2000) for 115K. Molecular graphics: Diamond for 100K, 1point5K, 155K. Software used to prepare material for publication: (Jana2000; Petricek and Dusek, 2000) for 115K.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
(100K) deuterated thiophene top
Crystal data top
C4D4SV = 842.93 (2) Å3
Mr = 88Z = 8
Monoclinic, P21vanadium sample holder
Hall symbol: P 2ybNeutron radiation, λ = 2.450000 Å
a = 11.05278 (19) ÅT = 100 K
b = 7.50396 (9) Åcolourless
c = 10.1632 (2) Å?, ? × ? × ? mm
β = 89.996 (6)°
Data collection top
Powder
diffractometer
2θmin = 1.952°, 2θmax = 159.852°, 2θstep = 0.100°
Radiation source: nuclear reactor, G41, Saclay
Refinement top
Rp = 3.706Excluded region(s): 32.40 33.75
Rwp = 4.731Profile function: manual
Rexp = 1.82740 parameters
RBragg = 5.5920 restraints
χ2 = NOT FOUND
1580 data pointsPreferred orientation correction: no
Crystal data top
C4D4Sβ = 89.996 (6)°
Mr = 88V = 842.93 (2) Å3
Monoclinic, P21Z = 8
a = 11.05278 (19) ÅNeutron radiation, λ = 2.450000 Å
b = 7.50396 (9) ÅT = 100 K
c = 10.1632 (2) Å?, ? × ? × ? mm
Data collection top
Powder
diffractometer
2θmin = 1.952°, 2θmax = 159.852°, 2θstep = 0.100°
Refinement top
Rp = 3.706χ2 = NOT FOUND
Rwp = 4.7311580 data points
Rexp = 1.82740 parameters
RBragg = 5.5920 restraints
Special details top

Experimental. Sample was first cooled quickly down to 1.5 K (metastable phase sequence), then heated up to 160 K, at which temperature it was kept for a few hours until the transformation from metastable phase II to stable phase III was complete

Geometry. rigid body group non refined

Refinement. Rigid-body Rietvelt refinement of powder data using TLS matrices (4 molecules)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PI10.168820.184530.118880.00000
PI20.049770.090720.078760.00000
PI30.217960.245080.016460.00000
PI40.036060.099000.058620.00000
PI50.137290.191910.115930.00000
PI60.015470.027370.139860.00000
PI70.298920.315910.038110.00000
PI80.036950.045890.113930.00000
PI90.147450.215130.218320.00000
PJ10.094990.236150.407130.00000
PJ20.206340.118180.437440.00000
PJ30.034160.247370.543980.00000
PJ40.206160.071850.571460.00000
PJ50.102530.149600.635580.00000
PJ60.275500.074040.372350.00000
PJ70.046360.315520.571490.00000
PJ80.271440.008070.620250.00000
PJ90.082670.133570.737040.00000
PO10.320420.193980.121890.00000
PO20.438300.089760.093310.00000
PO30.284950.257840.017620.00000
PO40.463400.095980.042200.00000
PO50.371100.197140.108970.00000
PO60.495670.021260.160430.00000
PO70.209050.335410.046930.00000
PO80.538350.036290.090320.00000
PO90.370230.220550.211930.00000
PP10.417290.215850.606700.00000
PP20.301330.113900.566670.00000
PP30.477090.248390.471180.00000
PP40.298410.093830.429190.00000
PP50.404190.174770.371720.00000
PP60.231260.063260.627920.00000
PP70.559800.314630.449420.00000
PP80.229720.029400.373910.00000
PP90.422410.176830.269220.00000
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
PI10.002390.005710.009090.001460.000710.00001
PI20.001720.006190.010340.000870.000830.00025
PI30.001480.006250.010610.000810.000630.00017
PI40.002240.007730.010840.000680.001450.00023
PI50.004140.007280.008790.001120.000110.00035
PI60.004550.013480.013980.001840.003120.00097
PI70.003040.013840.015610.002200.001890.00051
PI80.005060.016830.015320.002040.004300.00070
PI90.011000.015420.008920.000650.000560.00112
PJ10.002470.005290.009060.001350.000390.00048
PJ20.001670.006480.010390.001020.000970.00015
PJ30.001470.006420.010610.000900.000750.00015
PJ40.002500.006790.010640.000340.001060.00056
PJ50.004060.007310.008930.001260.000650.00057
PJ60.004310.014660.014190.001230.003650.00050
PJ70.003070.014240.015560.001960.002280.00051
PJ80.005840.013980.014710.003060.003180.00163
PJ90.010740.015600.009360.000180.002200.00167
PO10.002270.005750.009220.001450.000810.00002
PO20.001950.005950.010120.000850.000820.00036
PO30.001690.006000.010400.000770.000690.00027
PO40.002080.007660.011010.000570.001310.00026
PO50.004140.007280.008800.001170.000240.00043
PO60.005380.012660.013160.001880.003020.00136
PO70.003740.012960.014920.002350.002170.00081
PO80.004600.016570.015820.002370.003870.00079
PO90.011050.015390.008910.000500.000500.00139
PP10.002480.005540.009000.001390.000520.00026
PP20.001610.006450.010460.000970.000900.00016
PP30.001390.006440.010690.000890.000660.00013
PP40.002410.007330.010660.000510.001300.00041
PP50.004090.007370.008830.001160.000510.00017
PP60.004120.014470.014420.001450.003430.00060
PP70.002770.014420.015870.001960.001970.00041
PP80.005590.015620.014780.002530.003910.00120
PP90.010820.015770.009060.000510.001780.00046
Geometric parameters (Å, º) top
PI1—PI21.717PI4—PI51.442
PI2—PI41.368PI2—PI61.072
PI3—PI1—PI291.90PI1—PI2—PI6121.0
PI1—PI2—PI4112.0PI2—PI4—PI5120.0
(1point5K) deuterated thiophene top
Crystal data top
C4D4Sβ = 89.989 (5)°
Mr = 88V = 826.85 (2) Å3
Monoclinic, P21Z = 8
Hall symbol: P 2ybNeutron radiation, λ = 2.450000 Å
a = 11.02171 (18) ÅT = 2 K
b = 7.42951 (10) Åcolourless
c = 10.09755 (18) Å?, ? × ? × ? mm
Data collection top
Powder
diffractometer
Scan method: step
Radiation source: nuclear reactor, G41, Saclay2θmin = 1.955°, 2θmax = 159.855°, 2θstep = 0.100°
Refinement top
Rp = 4.542Excluded region(s): 32.6 33.75
Rwp = 5.758Profile function: manual
Rexp = 1.83841 parameters
RBragg = 5.0510 restraints
χ2 = NOT FOUND
1580 data pointsPreferred orientation correction: no
Crystal data top
C4D4Sβ = 89.989 (5)°
Mr = 88V = 826.85 (2) Å3
Monoclinic, P21Z = 8
a = 11.02171 (18) ÅNeutron radiation, λ = 2.450000 Å
b = 7.42951 (10) ÅT = 2 K
c = 10.09755 (18) Å?, ? × ? × ? mm
Data collection top
Powder
diffractometer
2θmin = 1.955°, 2θmax = 159.855°, 2θstep = 0.100°
Scan method: step
Refinement top
Rp = 4.542χ2 = NOT FOUND
Rwp = 5.7581580 data points
Rexp = 1.83841 parameters
RBragg = 5.0510 restraints
Special details top

Experimental. Sample was first cooled quickly down to 1.5 K (metastable phase sequence), then heated up to 160 K, at which temperature it was kept for a few hours until the transformation from metastable phase II to stable phase III was complete

Refinement. Rigid-body Rietvelt refinement of powder data using TLS matrices (4 molecules)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PI10.179510.184770.131710.00000
PI20.060550.086790.094090.00000
PI30.224650.249050.005440.00000
PI40.043400.096350.043670.00000
PI50.142160.194010.103580.00000
PI60.002470.020050.157000.00000
PI70.304270.323360.029050.00000
PI80.030350.041090.097610.00000
PI90.149560.218990.206740.00000
PJ10.085080.229480.406280.00000
PJ20.199500.116490.437330.00000
PJ30.029070.251480.545850.00000
PJ40.204990.081960.574070.00000
PJ50.102430.163200.639390.00000
PJ60.266990.068050.370980.00000
PJ70.051560.320380.573830.00000
PJ80.273380.007690.623910.00000
PJ90.086540.155690.742890.00000
PO10.328390.178700.112590.00000
PO20.450910.086240.081550.00000
PO30.288300.241060.026880.00000
PO40.474180.096750.055110.00000
PO50.376310.189940.120380.00000
PO60.512300.022350.147850.00000
PO70.208370.311720.054830.00000
PO80.551430.044960.104940.00000
PO90.373170.214690.223810.00000
PP10.407970.253330.585970.00000
PP20.296910.134150.552910.00000
PP30.471660.264500.449700.00000
PP40.299740.087210.418090.00000
PP50.404910.165660.355960.00000
PP60.226300.089640.616810.00000
PP70.552930.333310.423890.00000
PP80.235250.006440.367500.00000
PP90.426820.149350.254350.00000
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
PI10.000850.001000.003690.000410.000310.00003
PI20.000680.001150.004220.000040.000330.00021
PI30.000590.001160.004330.000000.000260.00015
PI40.000830.002120.004450.000060.000580.00020
PI50.001590.002010.003560.000260.000010.00026
PI60.002090.005340.005790.001490.001240.00081
PI70.001490.005430.006500.001750.000790.00045
PI80.002080.007460.006430.001600.001710.00061
PI90.004450.007120.003630.000610.000070.00083
PJ10.000900.000820.003680.000340.000200.00025
PJ20.000620.001340.004220.000120.000390.00015
PJ30.000550.001300.004330.000060.000300.00013
PJ40.000960.001730.004430.000210.000470.00034
PJ50.001570.002050.003570.000290.000200.00021
PJ60.001860.006070.005800.001170.001460.00052
PJ70.001380.005820.006490.001570.000930.00042
PJ80.002480.006310.006370.002060.001390.00101
PJ90.004380.007310.003660.000490.000690.00059
PO10.000810.001020.003720.000420.000340.00000
PO20.000700.001180.004190.000060.000350.00021
PO30.000590.001200.004310.000020.000290.00016
PO40.000750.002200.004530.000040.000570.00015
PO50.001590.002010.003560.000270.000080.00028
PO60.002150.005430.005670.001420.001300.00082
PO70.001480.005590.006440.001660.000900.00047
PO80.001830.007720.006660.001520.001690.00047
PO90.004460.007120.003630.000560.000140.00089
PP10.000940.000740.003690.000350.000140.00033
PP20.000590.001390.004250.000140.000390.00012
PP30.000520.001320.004350.000060.000290.00012
PP40.001050.001550.004400.000240.000430.00041
PP50.001540.002020.003630.000340.000310.00035
PP60.001710.006260.005930.001110.001480.00043
PP70.001310.005870.006550.001560.000880.00038
PP80.002730.005770.006280.002130.001280.00119
PP90.004280.007240.003860.000340.001020.00101
Geometric parameters (Å, º) top
PI1—PI21.717PI4—PI51.442
PI2—PI41.368PI2—PI61.072
PI3—PI1—PI291.90PI1—PI2—PI6121.0
PI1—PI2—PI4112.0PI2—PI4—PI5120.0
(155K) deuterated thiophene top
Crystal data top
C4D4SV = 432.13 (1) Å3
Mr = 88Z = 4
Orthorhombic, PBNMNeutron radiation, λ = 2.450000 Å
Hall symbol: -P 2c 2abT = 155 K
a = 5.5226 (1) Åcolourless
b = 7.62000 (9) Å?, ? × ? × ? mm
c = 10.2688 (2) Å
Data collection top
Powder
diffractometer
2θmin = 1.949°, 2θmax = 159.849°, 2θstep = 0.100°
Radiation source: nuclear reactor, G41, Saclay
Refinement top
Rp = 2.788Excluded region(s): 32.30 33.75 and 58.05 58.75
Rwp = 3.756Profile function: manual
Rexp = 1.75631 parameters
RBragg = 3.9190 restraints
χ2 = NOT FOUND
1580 data pointsPreferred orientation correction: no
Crystal data top
C4D4SV = 432.13 (1) Å3
Mr = 88Z = 4
Orthorhombic, PBNMNeutron radiation, λ = 2.450000 Å
a = 5.5226 (1) ÅT = 155 K
b = 7.62000 (9) Å?, ? × ? × ? mm
c = 10.2688 (2) Å
Data collection top
Powder
diffractometer
2θmin = 1.949°, 2θmax = 159.849°, 2θstep = 0.100°
Refinement top
Rp = 2.788χ2 = NOT FOUND
Rwp = 3.7561580 data points
Rexp = 1.75631 parameters
RBragg = 3.9190 restraints
Special details top

Experimental. Sample was first cooled quickly down to 1.5 K (metastable phase sequence), then heated up to 160 K, at which temperature it was kept for a few hours until the transformation from metastable phase II to stable phase III was complete

Refinement. Rigid-body Rietvelt refinement of powder data using TLS matrices (3 molecules on the same site with different orientations and different occupations)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
PI10.059100.196530.142360.000001.000 (6)
PI20.165480.093780.190290.000001.000 (6)
PI30.180830.246680.272850.000001.000 (6)
PI40.165950.088720.327130.000001.000 (6)
PI50.042480.180740.376820.000001.000 (6)
PI60.304430.033250.134340.000001.000 (6)
PI70.342910.319040.288680.000001.000 (6)
PI80.297790.027270.386900.000001.000 (6)
PI90.081880.194890.477420.000001.000 (6)
PJ10.111230.280020.264370.000000.057 (5)
PJ20.008760.223020.130680.000000.057 (5)
PJ30.015730.132090.353870.000000.057 (5)
PJ40.123450.066610.145290.000000.057 (5)
PJ50.119250.011880.279620.000000.057 (5)
PJ60.027990.285580.038650.000000.057 (5)
PJ70.041020.115610.455830.000000.057 (5)
PJ80.214140.003010.070250.000000.057 (5)
PJ90.206490.102700.314940.000000.057 (5)
PK10.106770.107930.165970.000000.086 (5)
PK20.175440.159480.306930.000000.086 (5)
PK30.161690.165430.160350.000000.086 (5)
PK40.026510.234260.369100.000000.086 (5)
PK50.229410.237840.280880.000000.086 (5)
PK60.344430.144630.355420.000000.086 (5)
PK70.285750.155760.081430.000000.086 (5)
PK80.032940.281800.466160.000000.086 (5)
PK90.402550.288320.305470.000000.086 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
PI10.025910.008590.014740.005050.005130.00000
PI20.026950.010060.015010.003000.001300.00175
PI30.017350.009370.020400.001610.003080.00059
PI40.032450.011570.015220.001780.002340.00313
PI50.035250.011110.014310.007620.006200.00054
PI60.044340.021030.022080.009450.007840.00596
PI70.021960.019760.034300.004260.007300.00209
PI80.055330.023550.022170.006640.010730.00833
PI90.070830.022650.015470.018540.013890.00037
PJ10.017860.006910.017560.000950.001940.00043
PJ20.027740.009020.013360.005350.004670.00001
PJ30.032960.009300.014200.005730.003450.00159
PJ40.036850.010360.015530.000660.001760.00342
PJ50.039050.008040.017910.004280.001020.00176
PJ60.056540.017460.014330.013260.011640.00238
PJ70.066780.019270.014940.015980.007500.00315
PJ80.068270.020210.020940.002170.009280.00930
PJ90.071140.012960.027530.013440.005100.00525
PK10.028210.008820.013950.000130.000560.00208
PK20.022750.011080.012960.000110.001230.00169
PK30.024220.010170.018500.006060.006070.00027
PK40.032180.010410.013850.006660.006360.00044
PK50.017830.011860.023030.002050.004320.00084
PK60.032260.024940.017720.001440.007810.00479
PK70.042900.022190.025060.013930.017300.00190
PK80.066420.020560.014450.016200.013230.00262
PK90.021790.025630.038240.002140.010590.00281
Geometric parameters (Å, º) top
PI1—PI21.717PI4—PI51.442
PI2—PI41.368PI2—PI61.072
PI3—PI1—PI291.90PI1—PI2—PI6121.0
PI1—PI2—PI4112.0PI2—PI4—PI5120.0
(115K) top
Crystal data top
C4D4SV = 423.17 Å3
Mr = 84.1Z = 4
Monoclinic, P21(α0γ)0†F(000) = 135
q = 0.55243a*Dx = 1.320 Mg m3
a = 5.5169 ÅNeutron radiation, λ = 2.45 Å
b = 7.5335 ÅT = 115 K
c = 10.1817 Å?, ? × ? × ? mm
β = 89.996°
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, 1/2+x2, −x3, −x4.

Data collection top
2θmin = 1.8°, 2θmax = 159.7°, 2θstep = 0.1°
Refinement top
Rp = 0.071Excluded region(s): from 32.3 to 33.750
Rwp = 0.090Profile function: Pseudo-Voigt
Rexp = 0.0634 parameters
R(F) = 0.050Weighting scheme based on measured s.u.'s
χ2 = NOT FOUND(Δ/σ)max = 0.003
1580 data pointsPreferred orientation correction: none
Crystal data top
C4D4Sβ = 89.996°
Mr = 84.1V = 423.17 Å3
Monoclinic, P21(α0γ)0†Z = 4
q = 0.55243a*Neutron radiation, λ = 2.45 Å
a = 5.5169 ÅT = 115 K
b = 7.5335 Å?, ? × ? × ? mm
c = 10.1817 Å
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, 1/2+x2, −x3, −x4.

Data collection top
2θmin = 1.8°, 2θmax = 159.7°, 2θstep = 0.1°
Refinement top
Rp = 0.071χ2 = NOT FOUND
Rwp = 0.0901580 data points
Rexp = 0.0634 parameters
R(F) = 0.050
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C2aa0.4174180.2600570.019750.0981*0.25
C3aa0.0911830.075460.0678420.0233*0.25
C4aa0.2704950.1928890.121150.0273*0.25
D1aa0.0017160.0169690.1276710.0549*0.25
D2aa0.5619560.3499340.038890.08*0.25
D3aa0.0404880.0086430.1256350.0795*0.25
D4aa0.2862410.2226250.2227760.0166*0.25
C2ab0.4475590.2396970.0284770.0981*0.25
C3ab0.0694060.1123340.0652290.0233*0.25
C4ab0.2879610.1757310.1252830.0273*0.25
D1ab0.0623410.0947030.1347370.0549*0.25
D2ab0.6205210.2927780.0529010.08*0.25
D3ab0.0780630.0577480.1186920.0795*0.25
D4ab0.3201860.1732610.2281250.0166*0.25
C1ca0.4248620.086980.4524080.0416*0.25
C2ca0.0817230.243080.5388290.0349*0.25
C3ca0.4367470.0913180.5904370.013*0.25
C4ca0.2309870.1849060.6422490.0137*0.25
D1ca0.5607310.0235690.3949140.0557*0.25
D2ca0.0807520.3153760.5564620.076*0.25
D3ca0.5750850.0348830.6497090.0871*0.25
D4ca0.20020.2054120.7441150.0023*0.25
C1cb0.424 (2)0.0826 (14)0.5226 (16)0.0416*0.25
C2cb0.075 (2)0.2381 (14)0.6031 (16)0.0349*0.25
C3cb0.407 (2)0.0625 (14)0.6597 (16)0.013*0.25
C4cb0.198 (2)0.1558 (14)0.7079 (16)0.0137*0.25
D1cb0.567 (2)0.0235 (14)0.4676 (16)0.0557*0.25
D2cb0.085 (2)0.3142 (14)0.6181 (16)0.076*0.25
D3cb0.527 (2)0.0100 (14)0.7205 (16)0.0871*0.25
D4cb0.147 (2)0.1599 (14)0.8085 (16)0.0023*0.25

Experimental details

(100K)(1point5K)(155K)(115K)
Crystal data
Chemical formulaC4D4SC4D4SC4D4SC4D4S
Mr88888884.1
Crystal system, space groupMonoclinic, P21Monoclinic, P21Orthorhombic, PBNMMonoclinic, P21(α0γ)0†
Temperature (K)1002155115
a, b, c (Å)11.05278 (19), 7.50396 (9), 10.1632 (2)11.02171 (18), 7.42951 (10), 10.09755 (18)5.5226 (1), 7.62000 (9), 10.2688 (2)?
α, β, γ (°)90, 89.996 (6), 9090, 89.989 (5), 9090, 90, 905.5169, 7.5335, 10.1817
V3)842.93 (2)826.85 (2)432.13 (1)90, 89.996, 90
Z884423.17
Radiation typeNeutron, λ = 2.450000 ÅNeutron, λ = 2.450000 ÅNeutron, λ = 2.450000 Å?
Specimen shape, size (mm)?, ? × ? × ??, ? × ? × ??, ? × ? × ??
Data collection
DiffractometerPowder
diffractometer
Powder
diffractometer
Powder
diffractometer
?
Specimen mounting????
Data collection mode????
Scan method?Step??
2θ values (°)2θmin = 1.952 2θmax = 159.852 2θstep = 0.1002θmin = 1.955 2θmax = 159.855 2θstep = 0.1002θmin = 1.949 2θmax = 159.849 2θstep = 0.1002θmin = 1.8 2θmax = 159.7 2θstep = 0.1
Refinement
R factors and goodness of fitRp = 3.706, Rwp = 4.731, Rexp = 1.827, RBragg = 5.592, χ2 = NOT FOUNDRp = 4.542, Rwp = 5.758, Rexp = 1.838, RBragg = 5.051, χ2 = NOT FOUNDRp = 2.788, Rwp = 3.756, Rexp = 1.756, RBragg = 3.919, χ2 = NOT FOUNDRp = 0.071, Rwp = 0.090, Rexp = 0.063, R(F) = 0.050, χ2 = NOT FOUND
No. of data points1580158015801580
No. of parameters4041314
No. of restraints000?

† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, 1/2+x2, −x3, −x4.

Computer programs: FULLPROF, (Jana2000; Petricek and Dusek, 2000), Diamond.

Selected geometric parameters (Å, º) for (100K) top
PI1—PI21.717PI4—PI51.442
PI2—PI41.368PI2—PI61.072
PI3—PI1—PI291.90PI1—PI2—PI6121.0
PI1—PI2—PI4112.0PI2—PI4—PI5120.0
Selected geometric parameters (Å, º) for (1point5K) top
PI1—PI21.717PI4—PI51.442
PI2—PI41.368PI2—PI61.072
PI3—PI1—PI291.90PI1—PI2—PI6121.0
PI1—PI2—PI4112.0PI2—PI4—PI5120.0
Selected geometric parameters (Å, º) for (155K) top
PI1—PI21.717PI4—PI51.442
PI2—PI41.368PI2—PI61.072
PI3—PI1—PI291.90PI1—PI2—PI6121.0
PI1—PI2—PI4112.0PI2—PI4—PI5120.0
 

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