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The structural behaviour of both low-temperature β- and high-temperature α-Ba(OD)2, barium dihydroxide-d, was investigated at temperatures between 10 and 552 K by neutron powder diffraction. While the β phase (P21/n) remains stable to the lowest temperature investigated, the quenchable α phase (Pnma) shows a reversible orthorhombic-to-monoclinic phase transition between 100 and 150 K. The structure of the new αm phase (P21/n) is quite similar to that of the α phase. This behaviour is unusual as a metastable phase transforms to another metastable phase. The PnmaP21/n low-temperature phase transition is driven by an order–disorder mechanism, mainly caused by one of the D atoms, which is disordered on positions off the mirror plane, mimicking a special position on the mirror plane in the orthorhombic phase. Refinements of the α phase above the phase transition indicate this disorder across the mirror plane through a conspicuously high isotropic displacement parameter if compared to the other D atoms. At low temperature the energy of the vibration is lowered and the D atom is frozen at a general position in a correlated way, thus violating the mirror plane and reducing the space-group symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768101013647/os0074sup1.cif
Contains datablocks global, 480, a10, a50, a100, a150, a200, a552, b10, brt, b50, b100, b150, b200, b250, b300, b420, b480

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a10sup2.rtv
Contains datablock a10

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a10sup3.hkl
Contains datablock a10

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a50sup4.rtv
Contains datablock a50

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a50sup5.hkl
Contains datablock a50

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074100sup6.rtv
Contains datablock a100

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a150sup7.rtv
Contains datablock a150

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a200sup8.rtv
Contains datablock a200

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a200sup9.hkl
Contains datablock a200

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a480sup10.rtv
Contains datablock a480

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a552sup11.rtv
Contains datablock a552

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a552sup12.hkl
Contains datablock 552

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b10sup13.rtv
Contains datablock b10

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074brtsup14.rtv
Contains datablock brt

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074brtsup15.hkl
Contains datablock brt

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b50sup16.rtv
Contains datablock b50

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b100sup17.rtv
Contains datablock b100

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b150sup18.rtv
Contains datablock b150

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b200sup19.rtv
Contains datablock b200

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b250sup20.rtv
Contains datablock b250

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b250sup21.hkl
Contains datablock b250

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b300sup22.rtv
Contains datablock b300

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b420sup23.rtv
Contains datablock b420

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b480sup24.rtv
Contains datablock b480

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b480sup25.hkl
Contains datablock b480

txt

Text file https://doi.org/10.1107/S0108768101013647/os0074a10sup26.txt
Supplementary material

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Text file https://doi.org/10.1107/S0108768101013647/os0074a50sup27.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074a150sup28.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074a200sup29.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074a480sup30.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074a552sup31.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074b10sup32.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074brtsup33.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074b50sup34.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074b100sup35.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074b150sup36.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074b200sup37.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074b250sup38.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074b300sup39.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074b420sup40.txt
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Text file https://doi.org/10.1107/S0108768101013647/os0074b480sup41.txt
Supplementary material

Computing details top

For all compounds, cell refinement: GSAS (Larson and Von Dreele, 1994); data reduction: GSAS; program(s) used to refine structure: GSAS; molecular graphics: Crystal Maker, version 4.0.1 (Palmer, D.C., 1994-99); software used to prepare material for publication: GSAS.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(a10) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 1264.94 (5) Å3
Mr = 3467.32Z = 20
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 7.08251 (17) ÅT = 10 K
b = 10.8701 (3) Åwhite
c = 16.4349 (4) Åcylinder, ? × ? × ? mm
β = 91.3334 (15)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 10.141°, 2θmax = 159.991°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2998 data points
Rp = 0.021Profile function: pseudo-Voigt
Rwp = 0.0311 parameters
Rexp = ?(Δ/σ)max = 0.013
χ2 = 1.904Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 91.3334 (15)°
Mr = 3467.32V = 1264.94 (5) Å3
Monoclinic, P21/nZ = 20
a = 7.08251 (17) ÅNeutron radiation, λ = 1.59432 Å
b = 10.8701 (3) ÅT = 10 K
c = 16.4349 (4) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 10.141°, 2θmax = 159.991°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.021χ2 = 1.904
Rwp = 0.0312998 data points
Rexp = ?1 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.4333 (9)0.3245 (6)0.2463 (4)0.00505*
Ba20.9095 (9)0.4744 (6)0.3745 (4)0.00146*
Ba30.4322 (9)0.3292 (7)0.4879 (4)0.00108*
O10.3744 (8)0.0754 (5)0.2484 (4)0.00549*
O20.8147 (8)0.3241 (5)0.2483 (4)0.00764*
O30.5075 (8)0.5092 (6)0.3587 (3)0.00048*
O40.1586 (9)0.2910 (7)0.3727 (4)0.00343*
O50.6580 (8)0.2260 (6)0.3925 (4)0.00399*
O60.2902 (8)0.0579 (6)0.4765 (4)0.00117*
D10.2584 (10)0.0645 (6)0.2200 (4)0.02488*
D20.9405 (9)0.2877 (6)0.2562 (4)0.02828*
D30.5451 (10)0.5851 (7)0.3330 (4)0.02731*
D40.1842 (9)0.2075 (7)0.3581 (4)0.02172*
D50.7360 (8)0.2406 (6)0.3435 (4)0.01863*
D60.2173 (9)0.0461 (6)0.4278 (4)0.02051*
Ba2A0.4220 (10)0.0198 (6)0.6247 (4)0.00315*
Ba3A0.9258 (10)0.1709 (7)0.5070 (4)0.00063*
O3A0.0316 (9)0.0028 (7)0.6311 (4)0.00795*
O4A0.6671 (8)0.2075 (6)0.6172 (4)0.00442*
O5A0.1652 (8)0.2885 (7)0.6059 (4)0.00609*
O6A0.7935 (9)0.4499 (6)0.5233 (4)0.00353*
D3A0.0109 (10)0.9358 (7)0.6643 (4)0.02283*
D4A0.6539 (10)0.2875 (7)0.6367 (4)0.0278*
D5A0.2394 (9)0.2567 (6)0.6523 (4)0.01951*
D6A0.7205 (8)0.4482 (6)0.5723 (4)0.02206*
(a50) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 1265.22 (5) Å3
Mr = 3467.32Z = 20
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 7.08260 (18) ÅT = 50 K
b = 10.8730 (3) Åwhite
c = 16.4338 (4) Åcylinder, ? × ? × ? mm
β = 91.3091 (15)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 10.091°, 2θmax = 159.991°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2999 data points
Rp = 0.022Profile function: pseudo-Voigt
Rwp = 0.0291 parameters
Rexp = ?(Δ/σ)max = 0.013
χ2 = 1.664Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 91.3091 (15)°
Mr = 3467.32V = 1265.22 (5) Å3
Monoclinic, P21/nZ = 20
a = 7.08260 (18) ÅNeutron radiation, λ = 1.59432 Å
b = 10.8730 (3) ÅT = 50 K
c = 16.4338 (4) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 10.091°, 2θmax = 159.991°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.022χ2 = 1.664
Rwp = 0.0292999 data points
Rexp = ?1 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.4323 (9)0.3244 (6)0.2461 (4)0.00607*
Ba20.9097 (10)0.4743 (6)0.3742 (4)0.00438*
Ba30.4331 (9)0.3287 (7)0.4869 (4)0.00183*
O10.3737 (9)0.0752 (5)0.2484 (4)0.01048*
O20.8150 (8)0.3260 (5)0.2484 (4)0.01178*
O30.5077 (9)0.5099 (7)0.3599 (3)0.00614*
O40.1577 (9)0.2909 (7)0.3729 (4)0.00804*
O50.6584 (8)0.2253 (6)0.3916 (4)0.00269*
O60.2917 (9)0.0581 (6)0.4769 (4)0.00472*
D10.2587 (12)0.0647 (6)0.2211 (4)0.03267*
D20.9360 (9)0.2876 (6)0.2565 (4)0.02834*
D30.5457 (10)0.5844 (7)0.3321 (4)0.03339*
D40.1826 (10)0.2077 (7)0.3590 (4)0.0263*
D50.7358 (9)0.2400 (6)0.3431 (4)0.02227*
D60.2186 (9)0.0486 (6)0.4284 (4)0.02014*
Ba2A0.4201 (9)0.0190 (6)0.6248 (4)0.00136*
Ba3A0.9321 (9)0.1701 (7)0.5079 (4)0.00137*
O3A0.0305 (8)0.0006 (6)0.6307 (4)0.00308*
O4A0.6669 (8)0.2073 (6)0.6165 (4)0.00285*
O5A0.1661 (9)0.2869 (7)0.6055 (4)0.00738*
O6A0.7918 (9)0.4509 (6)0.5240 (4)0.00544*
D3A0.0125 (11)0.9352 (8)0.6650 (5)0.0326*
D4A0.6537 (10)0.2871 (8)0.6365 (4)0.03146*
D5A0.2407 (9)0.2577 (6)0.6514 (4)0.02178*
D6A0.7201 (9)0.4487 (6)0.5718 (4)0.02461*
(a100) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 1267.96 (6) Å3
Mr = 3467.32Z = 20
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 7.0832 (2) ÅT = 100 K
b = 10.8967 (3) Åwhite
c = 16.4306 (5) Åcylinder, ? × ? × ? mm
β = 91.0598 (19)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.141°, 2θmax = 160.041°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2999 data points
Rp = 0.030Profile function: pseudo-Voigt
Rwp = 0.033109 parameters
Rexp = ?
χ2 = 2.310Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 91.0598 (19)°
Mr = 3467.32V = 1267.96 (6) Å3
Monoclinic, P21/nZ = 20
a = 7.0832 (2) ÅNeutron radiation, λ = 1.59432 Å
b = 10.8967 (3) ÅT = 100 K
c = 16.4306 (5) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.141°, 2θmax = 160.041°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.030χ2 = 2.310
Rwp = 0.0332999 data points
Rexp = ?109 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.4313 (11)0.3223 (7)0.2472 (6)0.00686*
Ba20.9113 (12)0.4744 (9)0.3759 (5)0.00676*
Ba30.4357 (11)0.3288 (8)0.4880 (5)0.00076*
O10.3777 (10)0.0747 (7)0.2479 (6)0.01514*
O20.8096 (11)0.3254 (7)0.2519 (6)0.01935*
O30.5095 (10)0.5073 (8)0.3618 (4)0.00806*
O40.1572 (12)0.2900 (9)0.3733 (5)0.01114*
O50.1572 (12)0.2900 (9)0.3733 (5)0.01386*
O60.2894 (11)0.0584 (8)0.4753 (5)0.00456*
D10.2626 (15)0.0615 (9)0.2291 (6)0.04944*
D20.9401 (12)0.2870 (7)0.2532 (6)0.03545*
D30.5413 (13)0.5789 (10)0.3308 (6)0.04106*
D40.1797 (14)0.2101 (11)0.3596 (6)0.03841*
D50.7363 (11)0.2388 (8)0.3460 (5)0.02667*
D60.2209 (11)0.0474 (8)0.4273 (5)0.02784*
Ba2A0.4211 (11)0.0199 (8)0.6241 (5)0.00524*
Ba3A0.9276 (11)0.1683 (8)0.5082 (5)0.002*
O3A0.0312 (11)0.0016 (9)0.6328 (5)0.01063*
O4A0.6663 (11)0.2076 (8)0.6185 (5)0.01067*
O5A0.1621 (11)0.2832 (8)0.6050 (5)0.00995*
O6A0.7980 (10)0.4476 (7)0.5227 (4)0.00227*
D3A0.0136 (13)0.9326 (10)0.6651 (6)0.03574*
D4A0.6531 (14)0.2892 (11)0.6381 (6)0.04458*
D5A0.2393 (11)0.2586 (8)0.6517 (5)0.0245*
D6A0.7248 (12)0.4472 (9)0.5709 (5)0.03927*
(a150) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 1272.26 (6) Å3
Mr = 3467.32Z = 20
Orthorhombic, PnmaNeutron radiation, λ = 1.59432 Å
a = 10.9577 (3) ÅT = 150 K
b = 16.4138 (5) Åwhite
c = 7.07374 (18) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.091°, 2θmax = 160.041°, 2θstep = 0.05°
Refinement top
Refinement on rietveld3000 data points
Rp = 0.052Profile function: pseudo-Voigt
Rwp = 0.03977 parameters
Rexp = ?
χ2 = 3.240Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2V = 1272.26 (6) Å3
Mr = 3467.32Z = 20
Orthorhombic, PnmaNeutron radiation, λ = 1.59432 Å
a = 10.9577 (3) ÅT = 150 K
b = 16.4138 (5) Åcylinder, ? × ? × ? mm
c = 7.07374 (18) Å
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.091°, 2θmax = 160.041°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.052χ2 = 3.240
Rwp = 0.0393000 data points
Rexp = ?77 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.3187 (6)0.250.4353 (9)0.002*
Ba20.4771 (4)0.3764 (3)0.9167 (6)0.00562*
Ba30.3324 (4)0.4890 (3)0.4305 (7)0.00134*
O10.0762 (6)0.250.3738 (9)0.00914*
O20.3216 (7)0.250.8151 (11)0.02342*
O30.4992 (4)0.3650 (3)0.5213 (7)0.01015*
O40.2872 (4)0.3788 (3)0.1619 (7)0.00865*
O50.2188 (5)0.3942 (3)0.6573 (7)0.00788*
O60.0562 (5)0.4759 (3)0.2922 (7)0.0116*
D10.0551 (13)0.250.2589 (18)0.09487*
D20.2808 (8)0.250.9393 (14)0.05533*
D30.5663 (6)0.3333 (4)0.5155 (10)0.05763*
D40.2129 (6)0.3616 (5)0.1566 (10)0.0663*
D50.2379 (4)0.3469 (3)0.7417 (7)0.02435*
D60.0579 (6)0.4279 (3)0.2274 (8)0.04106*
(a200) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 1276.96 (6) Å3
Mr = 3467.32Z = 20
Orthorhombic, PnmaNeutron radiation, λ = 1.59432 Å
a = 10.9789 (3) ÅT = 200 K
b = 16.4317 (4) Åwhite
c = 7.07840 (18) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.091°, 2θmax = 160.041°, 2θstep = 0.05°
Refinement top
Refinement on rietveld3000 data points
Rp = 0.060Profile function: pseudo-Voigt
Rwp = 0.0391 parameters
Rexp = ?(Δ/σ)max = 0.009
χ2 = 3.098Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2V = 1276.96 (6) Å3
Mr = 3467.32Z = 20
Orthorhombic, PnmaNeutron radiation, λ = 1.59432 Å
a = 10.9789 (3) ÅT = 200 K
b = 16.4317 (4) Åcylinder, ? × ? × ? mm
c = 7.07840 (18) Å
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.091°, 2θmax = 160.041°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.060χ2 = 3.098
Rwp = 0.0393000 data points
Rexp = ?1 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.3185 (6)0.250.4382 (9)0.00065*
Ba20.4771 (4)0.3766 (3)0.9157 (6)0.00671*
Ba30.3323 (4)0.4893 (3)0.4292 (7)0.00508*
O10.0758 (7)0.250.3717 (10)0.01192*
O20.3212 (8)0.250.8150 (12)0.03108*
O30.4975 (5)0.3646 (3)0.5226 (7)0.01384*
O40.2855 (4)0.3787 (3)0.1598 (7)0.01078*
O50.2180 (5)0.3941 (3)0.6573 (7)0.00919*
O60.0567 (5)0.4763 (3)0.2922 (7)0.01252*
D10.0547 (13)0.250.255 (2)0.10467*
D20.2784 (8)0.250.9350 (15)0.05741*
D30.5644 (7)0.3349 (4)0.5119 (11)0.06318*
D40.2152 (6)0.3597 (5)0.1506 (10)0.07645*
D50.2377 (4)0.3474 (3)0.7409 (7)0.02781*
D60.0609 (6)0.4282 (3)0.2308 (9)0.04575*
(480) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 1310.99 (7) Å3
Mr = 3467.32Z = 20
Orthorhombic, PnmaNeutron radiation, λ = 1.59432 Å
a = 11.0818 (4) ÅT = 480 K
b = 16.6025 (5) Åwhite
c = 7.1255 (2) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.091°, 2θmax = 159.991°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2999 data points
Rp = 0.094Profile function: pseudo-Voigt
Rwp = 0.03278 parameters
Rexp = ?
χ2 = 2.341Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2V = 1310.99 (7) Å3
Mr = 3467.32Z = 20
Orthorhombic, PnmaNeutron radiation, λ = 1.59432 Å
a = 11.0818 (4) ÅT = 480 K
b = 16.6025 (5) Åcylinder, ? × ? × ? mm
c = 7.1255 (2) Å
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.091°, 2θmax = 159.991°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.094χ2 = 2.341
Rwp = 0.0322999 data points
Rexp = ?78 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.3171 (8)0.250.4408 (12)0.02123*
Ba20.4737 (4)0.3764 (4)0.9180 (7)0.01903*
Ba30.3338 (5)0.4883 (3)0.4249 (9)0.02065*
O10.0775 (9)0.250.3760 (14)0.0415*
O20.3257 (9)0.250.8140 (13)0.04299*
O30.4930 (7)0.3654 (5)0.5294 (10)0.04643*
O40.2809 (6)0.3803 (4)0.1639 (10)0.03464*
O50.2141 (5)0.3950 (3)0.6572 (8)0.02691*
O60.0574 (7)0.4756 (4)0.2984 (10)0.03786*
D10.0551 (13)0.250.261 (2)0.13132*
D20.2683 (9)0.250.9128 (15)0.07645*
D30.5542 (8)0.3390 (5)0.4957 (12)0.10137*
D40.2252 (7)0.3516 (5)0.1270 (12)0.1021*
D50.2372 (5)0.3527 (4)0.7382 (8)0.04792*
D60.0779 (7)0.4303 (4)0.2460 (11)0.08113*
(a552) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 1323.9 (1) Å3
Mr = 3467.32Z = 20
Orthorhombic, PnmaNeutron radiation, λ = 1.59432 Å
a = 11.1191 (5) ÅT = 552 K
b = 16.6694 (9) Åwhite
c = 7.1420 (4) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.091°, 2θmax = 159.941°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2998 data points
Rp = 0.064Profile function: pseudo-Voigt
Rwp = 0.0321 parameters
Rexp = ?(Δ/σ)max = 0.005
χ2 = 1.716Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2V = 1323.9 (1) Å3
Mr = 3467.32Z = 20
Orthorhombic, PnmaNeutron radiation, λ = 1.59432 Å
a = 11.1191 (5) ÅT = 552 K
b = 16.6694 (9) Åcylinder, ? × ? × ? mm
c = 7.1420 (4) Å
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.2θmin = 10.091°, 2θmax = 159.941°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.064χ2 = 1.716
Rwp = 0.0322998 data points
Rexp = ?1 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.3186 (10)0.250.4441 (14)0.02583*
Ba20.4731 (5)0.3772 (5)0.9170 (9)0.0226*
Ba30.3330 (6)0.4883 (4)0.4223 (11)0.02376*
O10.0788 (11)0.250.3729 (17)0.04015*
O20.3270 (11)0.250.8121 (16)0.05235*
O30.4925 (9)0.3668 (7)0.5284 (13)0.06051*
O40.2814 (8)0.3804 (5)0.1610 (13)0.04731*
O50.2130 (6)0.3963 (4)0.6550 (10)0.03306*
O60.0570 (8)0.4746 (5)0.2988 (13)0.04214*
D10.0538 (14)0.250.265 (3)0.12645*
D20.2675 (10)0.250.9054 (17)0.08068*
D30.5529 (10)0.3388 (6)0.4950 (14)0.11191*
D40.2277 (8)0.3515 (6)0.1297 (15)0.10892*
D50.2356 (6)0.3556 (5)0.7362 (10)0.05153*
D60.0807 (9)0.4316 (5)0.2457 (14)0.09593*
(b10) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 494.08 (1) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.34892 (14) ÅT = 10 K
b = 7.86485 (12) Åwhite
c = 6.75254 (10) Åcylinder, ? × ? × ? mm
β = 95.6551 (8)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2900 data points
Rp = 0.023Profile function: pseudo-Voigt
Rwp = 0.02766 parameters
Rexp = ?
χ2 = 2.103Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.6551 (8)°
Mr = 1386.93V = 494.08 (1) Å3
Monoclinic, P21/nZ = 8
a = 9.34892 (14) ÅNeutron radiation, λ = 1.59432 Å
b = 7.86485 (12) ÅT = 10 K
c = 6.75254 (10) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.023χ2 = 2.103
Rwp = 0.0272900 data points
Rexp = ?66 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.6031 (2)0.6413 (2)0.2504 (3)0.00044*
Ba20.1815 (2)0.5489 (2)0.2163 (3)0.00132*
O10.8821 (2)0.4890 (2)0.1763 (3)0.00337*
O20.4125 (2)0.3604 (2)0.1457 (3)0.00333*
O30.6064 (2)0.3467 (2)0.4934 (3)0.00173*
O40.1641 (2)0.2961 (2)0.4655 (3)0.00516*
D10.8848 (2)0.5319 (2)0.3105 (3)0.01984*
D20.4714 (2)0.3500 (2)0.2734 (3)0.01545*
D30.6245 (2)0.2355 (2)0.4424 (3)0.01748*
D40.1007 (2)0.2425 (3)0.5521 (3)0.02005*
(brt) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 501.80 (3) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.4098 (3) ÅT = RT K
b = 7.9101 (3) Åwhite
c = 6.7759 (2) Åcylinder, ? × ? × ? mm
β = 95.7651 (18)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 159.991°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2899 data points
Rp = 0.052Profile function: pseudo-Voigt
Rwp = 0.0431 parameters
Rexp = ?(Δ/σ)max = 0.001
χ2 = 3.725Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.7651 (18)°
Mr = 1386.93V = 501.80 (3) Å3
Monoclinic, P21/nZ = 8
a = 9.4098 (3) ÅNeutron radiation, λ = 1.59432 Å
b = 7.9101 (3) ÅT = RT K
c = 6.7759 (2) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 159.991°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.052χ2 = 3.725
Rwp = 0.0432899 data points
Rexp = ?1 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.5990 (5)0.6394 (6)0.2505 (7)0.01237*
Ba20.1793 (4)0.5499 (5)0.2170 (7)0.00905*
O10.8802 (4)0.4871 (5)0.1769 (7)0.01342*
O20.4108 (4)0.3595 (6)0.1439 (6)0.01401*
O30.6052 (4)0.3451 (6)0.4916 (7)0.01625*
O40.1659 (5)0.2949 (5)0.4662 (7)0.02071*
D10.8828 (5)0.5298 (6)0.3094 (7)0.03607*
D20.4702 (4)0.3484 (5)0.2682 (7)0.02775*
D30.6258 (5)0.2365 (6)0.4394 (7)0.03138*
D40.1029 (5)0.2462 (6)0.5475 (9)0.03682*
(b50) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 494.25 (1) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.35056 (15) ÅT = 50 K
b = 7.86586 (12) Åwhite
c = 6.75282 (10) Åcylinder, ? × ? × ? mm
β = 95.6551 (8)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2900 data points
Rp = 0.022Profile function: pseudo-Voigt
Rwp = 0.02766 parameters
Rexp = ?
χ2 = 1.850Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.6551 (8)°
Mr = 1386.93V = 494.25 (1) Å3
Monoclinic, P21/nZ = 8
a = 9.35056 (15) ÅNeutron radiation, λ = 1.59432 Å
b = 7.86586 (12) ÅT = 50 K
c = 6.75282 (10) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.022χ2 = 1.850
Rwp = 0.0272900 data points
Rexp = ?66 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.6032 (2)0.6411 (2)0.2509 (3)0.00069*
Ba20.1817 (2)0.5495 (3)0.2158 (3)0.00187*
O10.8822 (2)0.4887 (2)0.1764 (3)0.00396*
O20.4122 (2)0.3605 (2)0.1457 (3)0.00415*
O30.6065 (2)0.3463 (3)0.4933 (3)0.00312*
O40.1643 (2)0.2964 (2)0.4656 (3)0.00531*
D10.8847 (2)0.5315 (3)0.3106 (3)0.02*
D20.4712 (2)0.3503 (2)0.2727 (3)0.01575*
D30.6245 (2)0.2353 (3)0.4418 (3)0.01909*
D40.1010 (2)0.2431 (3)0.5521 (4)0.02111*
(b100) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 494.92 (1) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.35611 (15) ÅT = 100 K
b = 7.86963 (12) Åwhite
c = 6.75469 (10) Åcylinder, ? × ? × ? mm
β = 95.6564 (9)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2900 data points
Rp = 0.022Profile function: pseudo-Voigt
Rwp = 0.02766 parameters
Rexp = ?
χ2 = 1.796Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.6564 (9)°
Mr = 1386.93V = 494.92 (1) Å3
Monoclinic, P21/nZ = 8
a = 9.35611 (15) ÅNeutron radiation, λ = 1.59432 Å
b = 7.86963 (12) ÅT = 100 K
c = 6.75469 (10) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.022χ2 = 1.796
Rwp = 0.0272900 data points
Rexp = ?66 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.6032 (2)0.6408 (3)0.2505 (3)0.00241*
Ba20.1814 (2)0.5488 (3)0.2162 (3)0.00343*
O10.8819 (2)0.4886 (2)0.1767 (3)0.00535*
O20.4119 (2)0.3604 (2)0.1458 (3)0.0058*
O30.6064 (2)0.3464 (3)0.4937 (3)0.00469*
O40.1646 (2)0.2960 (2)0.4655 (3)0.00624*
D10.8847 (2)0.5317 (3)0.3106 (3)0.0221*
D20.4711 (2)0.3502 (2)0.2733 (3)0.01744*
D30.6246 (2)0.2356 (3)0.4412 (3)0.02043*
D40.1012 (2)0.2427 (3)0.5514 (4)0.0231*
(b150) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 496.06 (1) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.36521 (16) ÅT = 150 K
b = 7.87628 (13) Åwhite
c = 6.75813 (10) Åcylinder, ? × ? × ? mm
β = 95.6670 (9)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2900 data points
Rp = 0.024Profile function: pseudo-Voigt
Rwp = 0.02766 parameters
Rexp = ?
χ2 = 1.796Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.6670 (9)°
Mr = 1386.93V = 496.06 (1) Å3
Monoclinic, P21/nZ = 8
a = 9.36521 (16) ÅNeutron radiation, λ = 1.59432 Å
b = 7.87628 (13) ÅT = 150 K
c = 6.75813 (10) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.024χ2 = 1.796
Rwp = 0.0272900 data points
Rexp = ?66 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.6027 (2)0.6408 (3)0.2506 (3)0.00511*
Ba20.1813 (2)0.5489 (3)0.2161 (3)0.00486*
O10.8819 (2)0.4886 (2)0.1761 (3)0.00656*
O20.4124 (2)0.3605 (3)0.1460 (3)0.00712*
O30.6068 (2)0.3462 (3)0.4937 (3)0.00676*
O40.1649 (2)0.2964 (2)0.4653 (3)0.00896*
D10.8847 (2)0.5311 (3)0.3106 (3)0.02416*
D20.4711 (2)0.3502 (3)0.2725 (3)0.01823*
D30.6246 (2)0.2359 (3)0.4422 (3)0.02263*
D40.1017 (2)0.2429 (3)0.5517 (4)0.02548*
(b200) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 497.58 (1) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.37718 (16) ÅT = 200 K
b = 7.88503 (13) Åwhite
c = 6.76289 (10) Åcylinder, ? × ? × ? mm
β = 95.6888 (9)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2900 data points
Rp = 0.024Profile function: pseudo-Voigt
Rwp = 0.02666 parameters
Rexp = ?
χ2 = 1.690Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.6888 (9)°
Mr = 1386.93V = 497.58 (1) Å3
Monoclinic, P21/nZ = 8
a = 9.37718 (16) ÅNeutron radiation, λ = 1.59432 Å
b = 7.88503 (13) ÅT = 200 K
c = 6.76289 (10) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.024χ2 = 1.690
Rwp = 0.0262900 data points
Rexp = ?66 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.6029 (2)0.6406 (3)0.2503 (3)0.00657*
Ba20.1816 (2)0.5482 (3)0.2158 (4)0.00712*
O10.8823 (2)0.4878 (3)0.1763 (3)0.00948*
O20.4119 (2)0.3604 (3)0.1452 (3)0.00929*
O30.6067 (2)0.3462 (3)0.4942 (3)0.00972*
O40.1649 (2)0.2964 (3)0.4651 (3)0.01181*
D10.8846 (2)0.5308 (3)0.3104 (4)0.02725*
D20.4708 (2)0.3494 (3)0.2721 (3)0.02113*
D30.6246 (2)0.2362 (3)0.4423 (3)0.02596*
D40.1022 (2)0.2431 (3)0.5514 (4)0.02748*
(b250) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 499.37 (2) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.39124 (17) ÅT = 250 K
b = 7.89581 (14) Åwhite
c = 6.76818 (11) Åcylinder, ? × ? × ? mm
β = 95.7195 (10)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 159.991°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2899 data points
Rp = 0.028Profile function: pseudo-Voigt
Rwp = 0.0271 parameters
Rexp = ?(Δ/σ)max = 0.00020
χ2 = 1.742Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.7195 (10)°
Mr = 1386.93V = 499.37 (2) Å3
Monoclinic, P21/nZ = 8
a = 9.39124 (17) ÅNeutron radiation, λ = 1.59432 Å
b = 7.89581 (14) ÅT = 250 K
c = 6.76818 (11) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 159.991°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.028χ2 = 1.742
Rwp = 0.0272899 data points
Rexp = ?1 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.6027 (3)0.6400 (3)0.2512 (4)0.00853*
Ba20.1813 (2)0.5483 (3)0.2160 (4)0.0092*
O10.8824 (2)0.4870 (3)0.1766 (4)0.01139*
O20.4114 (2)0.3601 (3)0.1452 (3)0.0126*
O30.6066 (2)0.3464 (3)0.4947 (4)0.01315*
O40.1654 (2)0.2962 (3)0.4656 (4)0.01404*
D10.8847 (2)0.5304 (3)0.3104 (4)0.03018*
D20.4702 (2)0.3494 (3)0.2709 (3)0.02332*
D30.6249 (2)0.2370 (3)0.4426 (3)0.02823*
D40.1028 (3)0.2434 (3)0.5507 (4)0.03088*
(b300) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 501.55 (1) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.40841 (16) ÅT = 300 K
b = 7.90854 (13) Åwhite
c = 6.77476 (10) Åcylinder, ? × ? × ? mm
β = 95.7570 (9)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2900 data points
Rp = 0.032Profile function: pseudo-Voigt
Rwp = 0.02466 parameters
Rexp = ?
χ2 = 2.465Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.7570 (9)°
Mr = 1386.93V = 501.55 (1) Å3
Monoclinic, P21/nZ = 8
a = 9.40841 (16) ÅNeutron radiation, λ = 1.59432 Å
b = 7.90854 (13) ÅT = 300 K
c = 6.77476 (10) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 160.041°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.032χ2 = 2.465
Rwp = 0.0242900 data points
Rexp = ?66 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.6018 (2)0.6396 (3)0.2519 (3)0.01118*
Ba20.1810 (2)0.5475 (3)0.2158 (3)0.01107*
O10.8825 (2)0.4866 (3)0.1772 (3)0.01412*
O20.4108 (2)0.3594 (3)0.1444 (3)0.01489*
O30.6068 (2)0.3462 (3)0.4953 (3)0.01646*
O40.1662 (2)0.2960 (3)0.4646 (3)0.01832*
D10.8844 (2)0.5299 (3)0.3101 (4)0.03572*
D20.4697 (2)0.3494 (3)0.2702 (3)0.02604*
D30.6249 (2)0.2383 (3)0.4424 (3)0.03261*
D40.1041 (3)0.2444 (3)0.5505 (4)0.03568*
(b420) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 507.09 (2) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.4576 (3) ÅT = 420 K
b = 7.9390 (2) Åwhite
c = 6.78930 (19) Åcylinder, ? × ? × ? mm
β = 95.8690 (15)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 159.941°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2898 data points
Rp = 0.055Profile function: pseudo-Voigt
Rwp = 0.03466 parameters
Rexp = ?
χ2 = 2.465Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.8690 (15)°
Mr = 1386.93V = 507.09 (2) Å3
Monoclinic, P21/nZ = 8
a = 9.4576 (3) ÅNeutron radiation, λ = 1.59432 Å
b = 7.9390 (2) ÅT = 420 K
c = 6.78930 (19) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 159.941°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.055χ2 = 2.465
Rwp = 0.0342898 data points
Rexp = ?66 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.5996 (4)0.6382 (5)0.2519 (6)0.01782*
Ba20.1802 (4)0.5474 (4)0.2158 (6)0.01287*
O10.8827 (4)0.4857 (5)0.1783 (6)0.02265*
O20.4096 (4)0.3578 (5)0.1430 (5)0.01951*
O30.6075 (4)0.3451 (5)0.4952 (6)0.02553*
O40.1675 (4)0.2933 (5)0.4642 (6)0.02521*
D10.8832 (4)0.5279 (5)0.3099 (7)0.04819*
D20.4684 (4)0.3480 (5)0.2650 (6)0.03738*
D30.6256 (4)0.2398 (5)0.4409 (6)0.04359*
D40.1058 (4)0.2470 (5)0.5474 (8)0.04907*
(b480) deuterated barium hydroxide top
Crystal data top
Ba(OD)2V = 510.26 (2) Å3
Mr = 1386.93Z = 8
Monoclinic, P21/nNeutron radiation, λ = 1.59432 Å
a = 9.4881 (2) ÅT = 480 K
b = 7.95273 (19) Åwhite
c = 6.79846 (17) Åcylinder, ? × ? × ? mm
β = 95.9117 (13)°
Data collection top
Diffractometer D 2B, ILLData collection mode: transmission
Radiation source: high-flux isotope reactorScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 159.941°, 2θstep = 0.05°
Refinement top
Refinement on rietveld2898 data points
Rp = 0.058Profile function: pseudo-Voigt
Rwp = 0.0281 parameters
Rexp = ?(Δ/σ)max = 0.001
χ2 = 1.690Background function: shifted Chebyshev background function
Crystal data top
Ba(OD)2β = 95.9117 (13)°
Mr = 1386.93V = 510.26 (2) Å3
Monoclinic, P21/nZ = 8
a = 9.4881 (2) ÅNeutron radiation, λ = 1.59432 Å
b = 7.95273 (19) ÅT = 480 K
c = 6.79846 (17) Åcylinder, ? × ? × ? mm
Data collection top
Diffractometer D 2B, ILLScan method: step
Specimen mounting: the powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.2θmin = 15.091°, 2θmax = 159.941°, 2θstep = 0.05°
Data collection mode: transmission
Refinement top
Rp = 0.058χ2 = 1.690
Rwp = 0.0282898 data points
Rexp = ?1 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.5999 (3)0.6371 (4)0.2534 (5)0.02082*
Ba20.1810 (3)0.5446 (4)0.2139 (5)0.01553*
O10.8851 (3)0.4842 (4)0.1797 (6)0.02888*
O20.4086 (3)0.3568 (4)0.1418 (5)0.02452*
O30.6092 (3)0.3466 (5)0.4979 (6)0.03385*
O40.1693 (3)0.2920 (4)0.4643 (5)0.02796*
D10.8840 (4)0.5279 (5)0.3092 (6)0.05974*
D20.4681 (3)0.3476 (4)0.2636 (5)0.0452*
D30.6266 (4)0.2432 (5)0.4446 (6)0.05567*
D40.1080 (4)0.2474 (5)0.5479 (7)0.05723*

Experimental details

(a10)(a50)(a100)(a150)
Crystal data
Chemical formulaBa(OD)2Ba(OD)2Ba(OD)2Ba(OD)2
Mr3467.323467.323467.323467.32
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/nOrthorhombic, Pnma
Temperature (K)1050100150
a, b, c (Å)7.08251 (17), 10.8701 (3), 16.4349 (4)7.08260 (18), 10.8730 (3), 16.4338 (4)7.0832 (2), 10.8967 (3), 16.4306 (5)10.9577 (3), 16.4138 (5), 7.07374 (18)
α, β, γ (°)90, 91.3334 (15), 9090, 91.3091 (15), 9090, 91.0598 (19), 9090, 90, 90
V3)1264.94 (5)1265.22 (5)1267.96 (6)1272.26 (6)
Z20202020
Radiation typeNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 Å
µ (mm1)????
Specimen shape, size (mm)Cylinder, ? × ? × ?Cylinder, ? × ? × ?Cylinder, ? × ? × ?Cylinder, ? × ? × ?
Data collection
DiffractometerDiffractometer D 2B, ILLDiffractometer D 2B, ILLDiffractometer D 2B, ILLDiffractometer D 2B, ILL
Specimen mountingThe powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.
Data collection modeTransmissionTransmissionTransmissionTransmission
Scan methodStepStepStepStep
2θ values (°)2θmin = 10.141 2θmax = 159.991 2θstep = 0.052θmin = 10.091 2θmax = 159.991 2θstep = 0.052θmin = 10.141 2θmax = 160.041 2θstep = 0.052θmin = 10.091 2θmax = 160.041 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.021, Rwp = 0.031, Rexp = ?, χ2 = 1.904Rp = 0.022, Rwp = 0.029, Rexp = ?, χ2 = 1.664Rp = 0.030, Rwp = 0.033, Rexp = ?, χ2 = 2.310Rp = 0.052, Rwp = 0.039, Rexp = ?, χ2 = 3.240
No. of data points2998299929993000
No. of parameters1110977
No. of restraints????


(a200)(480)(a552)(b10)
Crystal data
Chemical formulaBa(OD)2Ba(OD)2Ba(OD)2Ba(OD)2
Mr3467.323467.323467.321386.93
Crystal system, space groupOrthorhombic, PnmaOrthorhombic, PnmaOrthorhombic, PnmaMonoclinic, P21/n
Temperature (K)20048055210
a, b, c (Å)10.9789 (3), 16.4317 (4), 7.07840 (18)11.0818 (4), 16.6025 (5), 7.1255 (2)11.1191 (5), 16.6694 (9), 7.1420 (4)9.34892 (14), 7.86485 (12), 6.75254 (10)
α, β, γ (°)90, 90, 9090, 90, 9090, 90, 9090, 95.6551 (8), 90
V3)1276.96 (6)1310.99 (7)1323.9 (1)494.08 (1)
Z2020208
Radiation typeNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 Å
µ (mm1)????
Specimen shape, size (mm)Cylinder, ? × ? × ?Cylinder, ? × ? × ?Cylinder, ? × ? × ?Cylinder, ? × ? × ?
Data collection
DiffractometerDiffractometer D 2B, ILLDiffractometer D 2B, ILLDiffractometer D 2B, ILLDiffractometer D 2B, ILL
Specimen mountingThe powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryostat.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.
Data collection modeTransmissionTransmissionTransmissionTransmission
Scan methodStepStepStepStep
2θ values (°)2θmin = 10.091 2θmax = 160.041 2θstep = 0.052θmin = 10.091 2θmax = 159.991 2θstep = 0.052θmin = 10.091 2θmax = 159.941 2θstep = 0.052θmin = 15.091 2θmax = 160.041 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.060, Rwp = 0.039, Rexp = ?, χ2 = 3.098Rp = 0.094, Rwp = 0.032, Rexp = ?, χ2 = 2.341Rp = 0.064, Rwp = 0.032, Rexp = ?, χ2 = 1.716Rp = 0.023, Rwp = 0.027, Rexp = ?, χ2 = 2.103
No. of data points3000299929982900
No. of parameters178166
No. of restraints????


(brt)(b50)(b100)(b150)
Crystal data
Chemical formulaBa(OD)2Ba(OD)2Ba(OD)2Ba(OD)2
Mr1386.931386.931386.931386.93
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)RT50100150
a, b, c (Å)9.4098 (3), 7.9101 (3), 6.7759 (2)9.35056 (15), 7.86586 (12), 6.75282 (10)9.35611 (15), 7.86963 (12), 6.75469 (10)9.36521 (16), 7.87628 (13), 6.75813 (10)
α, β, γ (°)90, 95.7651 (18), 9090, 95.6551 (8), 9090, 95.6564 (9), 9090, 95.6670 (9), 90
V3)501.80 (3)494.25 (1)494.92 (1)496.06 (1)
Z8888
Radiation typeNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 Å
µ (mm1)????
Specimen shape, size (mm)Cylinder, ? × ? × ?Cylinder, ? × ? × ?Cylinder, ? × ? × ?Cylinder, ? × ? × ?
Data collection
DiffractometerDiffractometer D 2B, ILLDiffractometer D 2B, ILLDiffractometer D 2B, ILLDiffractometer D 2B, ILL
Specimen mountingThe powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.
Data collection modeTransmissionTransmissionTransmissionTransmission
Scan methodStepStepStepStep
2θ values (°)2θmin = 15.091 2θmax = 159.991 2θstep = 0.052θmin = 15.091 2θmax = 160.041 2θstep = 0.052θmin = 15.091 2θmax = 160.041 2θstep = 0.052θmin = 15.091 2θmax = 160.041 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.052, Rwp = 0.043, Rexp = ?, χ2 = 3.725Rp = 0.022, Rwp = 0.027, Rexp = ?, χ2 = 1.850Rp = 0.022, Rwp = 0.027, Rexp = ?, χ2 = 1.796Rp = 0.024, Rwp = 0.027, Rexp = ?, χ2 = 1.796
No. of data points2899290029002900
No. of parameters1666666
No. of restraints????


(b200)(b250)(b300)(b420)
Crystal data
Chemical formulaBa(OD)2Ba(OD)2Ba(OD)2Ba(OD)2
Mr1386.931386.931386.931386.93
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)200250300420
a, b, c (Å)9.37718 (16), 7.88503 (13), 6.76289 (10)9.39124 (17), 7.89581 (14), 6.76818 (11)9.40841 (16), 7.90854 (13), 6.77476 (10)9.4576 (3), 7.9390 (2), 6.78930 (19)
α, β, γ (°)90, 95.6888 (9), 9090, 95.7195 (10), 9090, 95.7570 (9), 9090, 95.8690 (15), 90
V3)497.58 (1)499.37 (2)501.55 (1)507.09 (2)
Z8888
Radiation typeNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 ÅNeutron, λ = 1.59432 Å
µ (mm1)????
Specimen shape, size (mm)Cylinder, ? × ? × ?Cylinder, ? × ? × ?Cylinder, ? × ? × ?Cylinder, ? × ? × ?
Data collection
DiffractometerDiffractometer D 2B, ILLDiffractometer D 2B, ILLDiffractometer D 2B, ILLDiffractometer D 2B, ILL
Specimen mountingThe powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.The powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.
Data collection modeTransmissionTransmissionTransmissionTransmission
Scan methodStepStepStepStep
2θ values (°)2θmin = 15.091 2θmax = 160.041 2θstep = 0.052θmin = 15.091 2θmax = 159.991 2θstep = 0.052θmin = 15.091 2θmax = 160.041 2θstep = 0.052θmin = 15.091 2θmax = 159.941 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.024, Rwp = 0.026, Rexp = ?, χ2 = 1.690Rp = 0.028, Rwp = 0.027, Rexp = ?, χ2 = 1.742Rp = 0.032, Rwp = 0.024, Rexp = ?, χ2 = 2.465Rp = 0.055, Rwp = 0.034, Rexp = ?, χ2 = 2.465
No. of data points2900289929002898
No. of parameters6616666
No. of restraints????


(b480)
Crystal data
Chemical formulaBa(OD)2
Mr1386.93
Crystal system, space groupMonoclinic, P21/n
Temperature (K)480
a, b, c (Å)9.4881 (2), 7.95273 (19), 6.79846 (17)
α, β, γ (°)90, 95.9117 (13), 90
V3)510.26 (2)
Z8
Radiation typeNeutron, λ = 1.59432 Å
µ (mm1)?
Specimen shape, size (mm)Cylinder, ? × ? × ?
Data collection
DiffractometerDiffractometer D 2B, ILL
Specimen mountingThe powder was filled in a vanadium can with a diameter of 14 mm and a height of 55 mm. The vanadium can was then mounted within an aluminium-cryofurnace.
Data collection modeTransmission
Scan methodStep
2θ values (°)2θmin = 15.091 2θmax = 159.941 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.058, Rwp = 0.028, Rexp = ?, χ2 = 1.690
No. of data points2898
No. of parameters1
No. of restraints?

Computer programs: GSAS (Larson and Von Dreele, 1994), GSAS, Crystal Maker, version 4.0.1 (Palmer, D.C., 1994-99).

 

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