Temperature-dependent neutron powder diffraction study of the Ba(OD)2 polymorphs: a new low-temperature phase

Friedrich, A.; Kunz, M.; Suard, E.

doi:10.1107/S0108768101013647

Temperature-dependent neutron powder diffraction study of the Ba(OD)₂ polymorphs: a new low-temperature phase

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 α_m 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 Pnma ↔ P2₁/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.

Keywords: polymorphism; low-temperature; phase transitions; deuterium.

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Supporting information

	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
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a10sup2.rtv Contains datablock a10
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a10sup3.hkl Contains datablock a10
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a50sup4.rtv Contains datablock a50
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a50sup5.hkl Contains datablock a50
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074100sup6.rtv Contains datablock a100
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a150sup7.rtv Contains datablock a150
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a200sup8.rtv Contains datablock a200
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a200sup9.hkl Contains datablock a200
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a480sup10.rtv Contains datablock a480
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a552sup11.rtv Contains datablock a552
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074a552sup12.hkl Contains datablock 552
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b10sup13.rtv Contains datablock b10
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074brtsup14.rtv Contains datablock brt
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074brtsup15.hkl Contains datablock brt
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b50sup16.rtv Contains datablock b50
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b100sup17.rtv Contains datablock b100
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b150sup18.rtv Contains datablock b150
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b200sup19.rtv Contains datablock b200
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b250sup20.rtv Contains datablock b250
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b250sup21.hkl Contains datablock b250
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b300sup22.rtv Contains datablock b300
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b420sup23.rtv Contains datablock b420
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b480sup24.rtv Contains datablock b480
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768101013647/os0074b480sup25.hkl Contains datablock b480
	Text file https://doi.org/10.1107/S0108768101013647/os0074a10sup26.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074a50sup27.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074a150sup28.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074a200sup29.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074a480sup30.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074a552sup31.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074b10sup32.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074brtsup33.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074b50sup34.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074b100sup35.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074b150sup36.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074b200sup37.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074b250sup38.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074b300sup39.txt Supplementary material
	Text file https://doi.org/10.1107/S0108768101013647/os0074b420sup40.txt Supplementary material
	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

(a10) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 1264.94 (5) Å³
M_r = 3467.32	Z = 20
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 7.08251 (17) Å	T = 10 K
b = 10.8701 (3) Å	white
c = 16.4349 (4) Å	cylinder, ? × ? × ? mm
β = 91.3334 (15)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 10.141°, 2θ_max = 159.991°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2998 data points
R_p = 0.021	Profile function: pseudo-Voigt
R_wp = 0.031	1 parameters
R_exp = ?	(Δ/σ)_max = 0.013
χ² = 1.904	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 91.3334 (15)°
M_r = 3467.32	V = 1264.94 (5) Å³
Monoclinic, P2₁/n	Z = 20
a = 7.08251 (17) Å	Neutron radiation, λ = 1.59432 Å
b = 10.8701 (3) Å	T = 10 K
c = 16.4349 (4) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 10.141°, 2θ_max = 159.991°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.021	χ² = 1.904
R_wp = 0.031	2998 data points
R_exp = ?	1 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.4333 (9)	0.3245 (6)	0.2463 (4)	0.00505*
Ba2	0.9095 (9)	0.4744 (6)	0.3745 (4)	0.00146*
Ba3	0.4322 (9)	0.3292 (7)	0.4879 (4)	0.00108*
O1	0.3744 (8)	0.0754 (5)	0.2484 (4)	0.00549*
O2	0.8147 (8)	0.3241 (5)	0.2483 (4)	0.00764*
O3	0.5075 (8)	0.5092 (6)	0.3587 (3)	0.00048*
O4	0.1586 (9)	0.2910 (7)	0.3727 (4)	0.00343*
O5	0.6580 (8)	0.2260 (6)	0.3925 (4)	0.00399*
O6	0.2902 (8)	0.0579 (6)	0.4765 (4)	0.00117*
D1	0.2584 (10)	0.0645 (6)	0.2200 (4)	0.02488*
D2	0.9405 (9)	0.2877 (6)	0.2562 (4)	0.02828*
D3	0.5451 (10)	0.5851 (7)	0.3330 (4)	0.02731*
D4	0.1842 (9)	0.2075 (7)	0.3581 (4)	0.02172*
D5	0.7360 (8)	0.2406 (6)	0.3435 (4)	0.01863*
D6	0.2173 (9)	0.0461 (6)	0.4278 (4)	0.02051*
Ba2A	0.4220 (10)	0.0198 (6)	0.6247 (4)	0.00315*
Ba3A	0.9258 (10)	0.1709 (7)	0.5070 (4)	0.00063*
O3A	0.0316 (9)	0.0028 (7)	0.6311 (4)	0.00795*
O4A	0.6671 (8)	0.2075 (6)	0.6172 (4)	0.00442*
O5A	0.1652 (8)	0.2885 (7)	0.6059 (4)	0.00609*
O6A	0.7935 (9)	0.4499 (6)	0.5233 (4)	0.00353*
D3A	0.0109 (10)	0.9358 (7)	0.6643 (4)	0.02283*
D4A	0.6539 (10)	0.2875 (7)	0.6367 (4)	0.0278*
D5A	0.2394 (9)	0.2567 (6)	0.6523 (4)	0.01951*
D6A	0.7205 (8)	0.4482 (6)	0.5723 (4)	0.02206*

(a50) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 1265.22 (5) Å³
M_r = 3467.32	Z = 20
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 7.08260 (18) Å	T = 50 K
b = 10.8730 (3) Å	white
c = 16.4338 (4) Å	cylinder, ? × ? × ? mm
β = 91.3091 (15)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 10.091°, 2θ_max = 159.991°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2999 data points
R_p = 0.022	Profile function: pseudo-Voigt
R_wp = 0.029	1 parameters
R_exp = ?	(Δ/σ)_max = 0.013
χ² = 1.664	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 91.3091 (15)°
M_r = 3467.32	V = 1265.22 (5) Å³
Monoclinic, P2₁/n	Z = 20
a = 7.08260 (18) Å	Neutron radiation, λ = 1.59432 Å
b = 10.8730 (3) Å	T = 50 K
c = 16.4338 (4) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 10.091°, 2θ_max = 159.991°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.022	χ² = 1.664
R_wp = 0.029	2999 data points
R_exp = ?	1 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.4323 (9)	0.3244 (6)	0.2461 (4)	0.00607*
Ba2	0.9097 (10)	0.4743 (6)	0.3742 (4)	0.00438*
Ba3	0.4331 (9)	0.3287 (7)	0.4869 (4)	0.00183*
O1	0.3737 (9)	0.0752 (5)	0.2484 (4)	0.01048*
O2	0.8150 (8)	0.3260 (5)	0.2484 (4)	0.01178*
O3	0.5077 (9)	0.5099 (7)	0.3599 (3)	0.00614*
O4	0.1577 (9)	0.2909 (7)	0.3729 (4)	0.00804*
O5	0.6584 (8)	0.2253 (6)	0.3916 (4)	0.00269*
O6	0.2917 (9)	0.0581 (6)	0.4769 (4)	0.00472*
D1	0.2587 (12)	0.0647 (6)	0.2211 (4)	0.03267*
D2	0.9360 (9)	0.2876 (6)	0.2565 (4)	0.02834*
D3	0.5457 (10)	0.5844 (7)	0.3321 (4)	0.03339*
D4	0.1826 (10)	0.2077 (7)	0.3590 (4)	0.0263*
D5	0.7358 (9)	0.2400 (6)	0.3431 (4)	0.02227*
D6	0.2186 (9)	0.0486 (6)	0.4284 (4)	0.02014*
Ba2A	0.4201 (9)	0.0190 (6)	0.6248 (4)	0.00136*
Ba3A	0.9321 (9)	0.1701 (7)	0.5079 (4)	0.00137*
O3A	0.0305 (8)	0.0006 (6)	0.6307 (4)	0.00308*
O4A	0.6669 (8)	0.2073 (6)	0.6165 (4)	0.00285*
O5A	0.1661 (9)	0.2869 (7)	0.6055 (4)	0.00738*
O6A	0.7918 (9)	0.4509 (6)	0.5240 (4)	0.00544*
D3A	0.0125 (11)	0.9352 (8)	0.6650 (5)	0.0326*
D4A	0.6537 (10)	0.2871 (8)	0.6365 (4)	0.03146*
D5A	0.2407 (9)	0.2577 (6)	0.6514 (4)	0.02178*
D6A	0.7201 (9)	0.4487 (6)	0.5718 (4)	0.02461*

(a100) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 1267.96 (6) Å³
M_r = 3467.32	Z = 20
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 7.0832 (2) Å	T = 100 K
b = 10.8967 (3) Å	white
c = 16.4306 (5) Å	cylinder, ? × ? × ? mm
β = 91.0598 (19)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 10.141°, 2θ_max = 160.041°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2999 data points
R_p = 0.030	Profile function: pseudo-Voigt
R_wp = 0.033	109 parameters
R_exp = ?
χ² = 2.310	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 91.0598 (19)°
M_r = 3467.32	V = 1267.96 (6) Å³
Monoclinic, P2₁/n	Z = 20
a = 7.0832 (2) Å	Neutron radiation, λ = 1.59432 Å
b = 10.8967 (3) Å	T = 100 K
c = 16.4306 (5) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 10.141°, 2θ_max = 160.041°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.030	χ² = 2.310
R_wp = 0.033	2999 data points
R_exp = ?	109 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.4313 (11)	0.3223 (7)	0.2472 (6)	0.00686*
Ba2	0.9113 (12)	0.4744 (9)	0.3759 (5)	0.00676*
Ba3	0.4357 (11)	0.3288 (8)	0.4880 (5)	0.00076*
O1	0.3777 (10)	0.0747 (7)	0.2479 (6)	0.01514*
O2	0.8096 (11)	0.3254 (7)	0.2519 (6)	0.01935*
O3	0.5095 (10)	0.5073 (8)	0.3618 (4)	0.00806*
O4	0.1572 (12)	0.2900 (9)	0.3733 (5)	0.01114*
O5	0.1572 (12)	0.2900 (9)	0.3733 (5)	0.01386*
O6	0.2894 (11)	0.0584 (8)	0.4753 (5)	0.00456*
D1	0.2626 (15)	0.0615 (9)	0.2291 (6)	0.04944*
D2	0.9401 (12)	0.2870 (7)	0.2532 (6)	0.03545*
D3	0.5413 (13)	0.5789 (10)	0.3308 (6)	0.04106*
D4	0.1797 (14)	0.2101 (11)	0.3596 (6)	0.03841*
D5	0.7363 (11)	0.2388 (8)	0.3460 (5)	0.02667*
D6	0.2209 (11)	0.0474 (8)	0.4273 (5)	0.02784*
Ba2A	0.4211 (11)	0.0199 (8)	0.6241 (5)	0.00524*
Ba3A	0.9276 (11)	0.1683 (8)	0.5082 (5)	0.002*
O3A	0.0312 (11)	0.0016 (9)	0.6328 (5)	0.01063*
O4A	0.6663 (11)	0.2076 (8)	0.6185 (5)	0.01067*
O5A	0.1621 (11)	0.2832 (8)	0.6050 (5)	0.00995*
O6A	0.7980 (10)	0.4476 (7)	0.5227 (4)	0.00227*
D3A	0.0136 (13)	0.9326 (10)	0.6651 (6)	0.03574*
D4A	0.6531 (14)	0.2892 (11)	0.6381 (6)	0.04458*
D5A	0.2393 (11)	0.2586 (8)	0.6517 (5)	0.0245*
D6A	0.7248 (12)	0.4472 (9)	0.5709 (5)	0.03927*

(a150) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 1272.26 (6) Å³
M_r = 3467.32	Z = 20
Orthorhombic, Pnma	Neutron radiation, λ = 1.59432 Å
a = 10.9577 (3) Å	T = 150 K
b = 16.4138 (5) Å	white
c = 7.07374 (18) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 10.091°, 2θ_max = 160.041°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	3000 data points
R_p = 0.052	Profile function: pseudo-Voigt
R_wp = 0.039	77 parameters
R_exp = ?
χ² = 3.240	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	V = 1272.26 (6) Å³
M_r = 3467.32	Z = 20
Orthorhombic, Pnma	Neutron radiation, λ = 1.59432 Å
a = 10.9577 (3) Å	T = 150 K
b = 16.4138 (5) Å	cylinder, ? × ? × ? mm
c = 7.07374 (18) Å

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 10.091°, 2θ_max = 160.041°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.052	χ² = 3.240
R_wp = 0.039	3000 data points
R_exp = ?	77 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.3187 (6)	0.25	0.4353 (9)	0.002*
Ba2	0.4771 (4)	0.3764 (3)	0.9167 (6)	0.00562*
Ba3	0.3324 (4)	0.4890 (3)	0.4305 (7)	0.00134*
O1	0.0762 (6)	0.25	0.3738 (9)	0.00914*
O2	0.3216 (7)	0.25	0.8151 (11)	0.02342*
O3	0.4992 (4)	0.3650 (3)	0.5213 (7)	0.01015*
O4	0.2872 (4)	0.3788 (3)	0.1619 (7)	0.00865*
O5	0.2188 (5)	0.3942 (3)	0.6573 (7)	0.00788*
O6	0.0562 (5)	0.4759 (3)	0.2922 (7)	0.0116*
D1	0.0551 (13)	0.25	0.2589 (18)	0.09487*
D2	0.2808 (8)	0.25	0.9393 (14)	0.05533*
D3	0.5663 (6)	0.3333 (4)	0.5155 (10)	0.05763*
D4	0.2129 (6)	0.3616 (5)	0.1566 (10)	0.0663*
D5	0.2379 (4)	0.3469 (3)	0.7417 (7)	0.02435*
D6	0.0579 (6)	0.4279 (3)	0.2274 (8)	0.04106*

(a200) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 1276.96 (6) Å³
M_r = 3467.32	Z = 20
Orthorhombic, Pnma	Neutron radiation, λ = 1.59432 Å
a = 10.9789 (3) Å	T = 200 K
b = 16.4317 (4) Å	white
c = 7.07840 (18) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 10.091°, 2θ_max = 160.041°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	3000 data points
R_p = 0.060	Profile function: pseudo-Voigt
R_wp = 0.039	1 parameters
R_exp = ?	(Δ/σ)_max = 0.009
χ² = 3.098	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	V = 1276.96 (6) Å³
M_r = 3467.32	Z = 20
Orthorhombic, Pnma	Neutron radiation, λ = 1.59432 Å
a = 10.9789 (3) Å	T = 200 K
b = 16.4317 (4) Å	cylinder, ? × ? × ? mm
c = 7.07840 (18) Å

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 10.091°, 2θ_max = 160.041°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.060	χ² = 3.098
R_wp = 0.039	3000 data points
R_exp = ?	1 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.3185 (6)	0.25	0.4382 (9)	0.00065*
Ba2	0.4771 (4)	0.3766 (3)	0.9157 (6)	0.00671*
Ba3	0.3323 (4)	0.4893 (3)	0.4292 (7)	0.00508*
O1	0.0758 (7)	0.25	0.3717 (10)	0.01192*
O2	0.3212 (8)	0.25	0.8150 (12)	0.03108*
O3	0.4975 (5)	0.3646 (3)	0.5226 (7)	0.01384*
O4	0.2855 (4)	0.3787 (3)	0.1598 (7)	0.01078*
O5	0.2180 (5)	0.3941 (3)	0.6573 (7)	0.00919*
O6	0.0567 (5)	0.4763 (3)	0.2922 (7)	0.01252*
D1	0.0547 (13)	0.25	0.255 (2)	0.10467*
D2	0.2784 (8)	0.25	0.9350 (15)	0.05741*
D3	0.5644 (7)	0.3349 (4)	0.5119 (11)	0.06318*
D4	0.2152 (6)	0.3597 (5)	0.1506 (10)	0.07645*
D5	0.2377 (4)	0.3474 (3)	0.7409 (7)	0.02781*
D6	0.0609 (6)	0.4282 (3)	0.2308 (9)	0.04575*

(480) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 1310.99 (7) Å³
M_r = 3467.32	Z = 20
Orthorhombic, Pnma	Neutron radiation, λ = 1.59432 Å
a = 11.0818 (4) Å	T = 480 K
b = 16.6025 (5) Å	white
c = 7.1255 (2) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 10.091°, 2θ_max = 159.991°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2999 data points
R_p = 0.094	Profile function: pseudo-Voigt
R_wp = 0.032	78 parameters
R_exp = ?
χ² = 2.341	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	V = 1310.99 (7) Å³
M_r = 3467.32	Z = 20
Orthorhombic, Pnma	Neutron radiation, λ = 1.59432 Å
a = 11.0818 (4) Å	T = 480 K
b = 16.6025 (5) Å	cylinder, ? × ? × ? mm
c = 7.1255 (2) Å

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 10.091°, 2θ_max = 159.991°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.094	χ² = 2.341
R_wp = 0.032	2999 data points
R_exp = ?	78 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.3171 (8)	0.25	0.4408 (12)	0.02123*
Ba2	0.4737 (4)	0.3764 (4)	0.9180 (7)	0.01903*
Ba3	0.3338 (5)	0.4883 (3)	0.4249 (9)	0.02065*
O1	0.0775 (9)	0.25	0.3760 (14)	0.0415*
O2	0.3257 (9)	0.25	0.8140 (13)	0.04299*
O3	0.4930 (7)	0.3654 (5)	0.5294 (10)	0.04643*
O4	0.2809 (6)	0.3803 (4)	0.1639 (10)	0.03464*
O5	0.2141 (5)	0.3950 (3)	0.6572 (8)	0.02691*
O6	0.0574 (7)	0.4756 (4)	0.2984 (10)	0.03786*
D1	0.0551 (13)	0.25	0.261 (2)	0.13132*
D2	0.2683 (9)	0.25	0.9128 (15)	0.07645*
D3	0.5542 (8)	0.3390 (5)	0.4957 (12)	0.10137*
D4	0.2252 (7)	0.3516 (5)	0.1270 (12)	0.1021*
D5	0.2372 (5)	0.3527 (4)	0.7382 (8)	0.04792*
D6	0.0779 (7)	0.4303 (4)	0.2460 (11)	0.08113*

(a552) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 1323.9 (1) Å³
M_r = 3467.32	Z = 20
Orthorhombic, Pnma	Neutron radiation, λ = 1.59432 Å
a = 11.1191 (5) Å	T = 552 K
b = 16.6694 (9) Å	white
c = 7.1420 (4) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 10.091°, 2θ_max = 159.941°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2998 data points
R_p = 0.064	Profile function: pseudo-Voigt
R_wp = 0.032	1 parameters
R_exp = ?	(Δ/σ)_max = 0.005
χ² = 1.716	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	V = 1323.9 (1) Å³
M_r = 3467.32	Z = 20
Orthorhombic, Pnma	Neutron radiation, λ = 1.59432 Å
a = 11.1191 (5) Å	T = 552 K
b = 16.6694 (9) Å	cylinder, ? × ? × ? mm
c = 7.1420 (4) Å

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 10.091°, 2θ_max = 159.941°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.064	χ² = 1.716
R_wp = 0.032	2998 data points
R_exp = ?	1 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.3186 (10)	0.25	0.4441 (14)	0.02583*
Ba2	0.4731 (5)	0.3772 (5)	0.9170 (9)	0.0226*
Ba3	0.3330 (6)	0.4883 (4)	0.4223 (11)	0.02376*
O1	0.0788 (11)	0.25	0.3729 (17)	0.04015*
O2	0.3270 (11)	0.25	0.8121 (16)	0.05235*
O3	0.4925 (9)	0.3668 (7)	0.5284 (13)	0.06051*
O4	0.2814 (8)	0.3804 (5)	0.1610 (13)	0.04731*
O5	0.2130 (6)	0.3963 (4)	0.6550 (10)	0.03306*
O6	0.0570 (8)	0.4746 (5)	0.2988 (13)	0.04214*
D1	0.0538 (14)	0.25	0.265 (3)	0.12645*
D2	0.2675 (10)	0.25	0.9054 (17)	0.08068*
D3	0.5529 (10)	0.3388 (6)	0.4950 (14)	0.11191*
D4	0.2277 (8)	0.3515 (6)	0.1297 (15)	0.10892*
D5	0.2356 (6)	0.3556 (5)	0.7362 (10)	0.05153*
D6	0.0807 (9)	0.4316 (5)	0.2457 (14)	0.09593*

(b10) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 494.08 (1) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.34892 (14) Å	T = 10 K
b = 7.86485 (12) Å	white
c = 6.75254 (10) Å	cylinder, ? × ? × ? mm
β = 95.6551 (8)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2900 data points
R_p = 0.023	Profile function: pseudo-Voigt
R_wp = 0.027	66 parameters
R_exp = ?
χ² = 2.103	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.6551 (8)°
M_r = 1386.93	V = 494.08 (1) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.34892 (14) Å	Neutron radiation, λ = 1.59432 Å
b = 7.86485 (12) Å	T = 10 K
c = 6.75254 (10) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.023	χ² = 2.103
R_wp = 0.027	2900 data points
R_exp = ?	66 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.6031 (2)	0.6413 (2)	0.2504 (3)	0.00044*
Ba2	0.1815 (2)	0.5489 (2)	0.2163 (3)	0.00132*
O1	0.8821 (2)	0.4890 (2)	0.1763 (3)	0.00337*
O2	0.4125 (2)	0.3604 (2)	0.1457 (3)	0.00333*
O3	0.6064 (2)	0.3467 (2)	0.4934 (3)	0.00173*
O4	0.1641 (2)	0.2961 (2)	0.4655 (3)	0.00516*
D1	0.8848 (2)	0.5319 (2)	0.3105 (3)	0.01984*
D2	0.4714 (2)	0.3500 (2)	0.2734 (3)	0.01545*
D3	0.6245 (2)	0.2355 (2)	0.4424 (3)	0.01748*
D4	0.1007 (2)	0.2425 (3)	0.5521 (3)	0.02005*

(brt) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 501.80 (3) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.4098 (3) Å	T = RT K
b = 7.9101 (3) Å	white
c = 6.7759 (2) Å	cylinder, ? × ? × ? mm
β = 95.7651 (18)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 159.991°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2899 data points
R_p = 0.052	Profile function: pseudo-Voigt
R_wp = 0.043	1 parameters
R_exp = ?	(Δ/σ)_max = 0.001
χ² = 3.725	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.7651 (18)°
M_r = 1386.93	V = 501.80 (3) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.4098 (3) Å	Neutron radiation, λ = 1.59432 Å
b = 7.9101 (3) Å	T = RT K
c = 6.7759 (2) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 159.991°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.052	χ² = 3.725
R_wp = 0.043	2899 data points
R_exp = ?	1 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.5990 (5)	0.6394 (6)	0.2505 (7)	0.01237*
Ba2	0.1793 (4)	0.5499 (5)	0.2170 (7)	0.00905*
O1	0.8802 (4)	0.4871 (5)	0.1769 (7)	0.01342*
O2	0.4108 (4)	0.3595 (6)	0.1439 (6)	0.01401*
O3	0.6052 (4)	0.3451 (6)	0.4916 (7)	0.01625*
O4	0.1659 (5)	0.2949 (5)	0.4662 (7)	0.02071*
D1	0.8828 (5)	0.5298 (6)	0.3094 (7)	0.03607*
D2	0.4702 (4)	0.3484 (5)	0.2682 (7)	0.02775*
D3	0.6258 (5)	0.2365 (6)	0.4394 (7)	0.03138*
D4	0.1029 (5)	0.2462 (6)	0.5475 (9)	0.03682*

(b50) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 494.25 (1) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.35056 (15) Å	T = 50 K
b = 7.86586 (12) Å	white
c = 6.75282 (10) Å	cylinder, ? × ? × ? mm
β = 95.6551 (8)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2900 data points
R_p = 0.022	Profile function: pseudo-Voigt
R_wp = 0.027	66 parameters
R_exp = ?
χ² = 1.850	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.6551 (8)°
M_r = 1386.93	V = 494.25 (1) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.35056 (15) Å	Neutron radiation, λ = 1.59432 Å
b = 7.86586 (12) Å	T = 50 K
c = 6.75282 (10) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.022	χ² = 1.850
R_wp = 0.027	2900 data points
R_exp = ?	66 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.6032 (2)	0.6411 (2)	0.2509 (3)	0.00069*
Ba2	0.1817 (2)	0.5495 (3)	0.2158 (3)	0.00187*
O1	0.8822 (2)	0.4887 (2)	0.1764 (3)	0.00396*
O2	0.4122 (2)	0.3605 (2)	0.1457 (3)	0.00415*
O3	0.6065 (2)	0.3463 (3)	0.4933 (3)	0.00312*
O4	0.1643 (2)	0.2964 (2)	0.4656 (3)	0.00531*
D1	0.8847 (2)	0.5315 (3)	0.3106 (3)	0.02*
D2	0.4712 (2)	0.3503 (2)	0.2727 (3)	0.01575*
D3	0.6245 (2)	0.2353 (3)	0.4418 (3)	0.01909*
D4	0.1010 (2)	0.2431 (3)	0.5521 (4)	0.02111*

(b100) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 494.92 (1) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.35611 (15) Å	T = 100 K
b = 7.86963 (12) Å	white
c = 6.75469 (10) Å	cylinder, ? × ? × ? mm
β = 95.6564 (9)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2900 data points
R_p = 0.022	Profile function: pseudo-Voigt
R_wp = 0.027	66 parameters
R_exp = ?
χ² = 1.796	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.6564 (9)°
M_r = 1386.93	V = 494.92 (1) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.35611 (15) Å	Neutron radiation, λ = 1.59432 Å
b = 7.86963 (12) Å	T = 100 K
c = 6.75469 (10) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.022	χ² = 1.796
R_wp = 0.027	2900 data points
R_exp = ?	66 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.6032 (2)	0.6408 (3)	0.2505 (3)	0.00241*
Ba2	0.1814 (2)	0.5488 (3)	0.2162 (3)	0.00343*
O1	0.8819 (2)	0.4886 (2)	0.1767 (3)	0.00535*
O2	0.4119 (2)	0.3604 (2)	0.1458 (3)	0.0058*
O3	0.6064 (2)	0.3464 (3)	0.4937 (3)	0.00469*
O4	0.1646 (2)	0.2960 (2)	0.4655 (3)	0.00624*
D1	0.8847 (2)	0.5317 (3)	0.3106 (3)	0.0221*
D2	0.4711 (2)	0.3502 (2)	0.2733 (3)	0.01744*
D3	0.6246 (2)	0.2356 (3)	0.4412 (3)	0.02043*
D4	0.1012 (2)	0.2427 (3)	0.5514 (4)	0.0231*

(b150) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 496.06 (1) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.36521 (16) Å	T = 150 K
b = 7.87628 (13) Å	white
c = 6.75813 (10) Å	cylinder, ? × ? × ? mm
β = 95.6670 (9)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2900 data points
R_p = 0.024	Profile function: pseudo-Voigt
R_wp = 0.027	66 parameters
R_exp = ?
χ² = 1.796	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.6670 (9)°
M_r = 1386.93	V = 496.06 (1) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.36521 (16) Å	Neutron radiation, λ = 1.59432 Å
b = 7.87628 (13) Å	T = 150 K
c = 6.75813 (10) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.024	χ² = 1.796
R_wp = 0.027	2900 data points
R_exp = ?	66 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.6027 (2)	0.6408 (3)	0.2506 (3)	0.00511*
Ba2	0.1813 (2)	0.5489 (3)	0.2161 (3)	0.00486*
O1	0.8819 (2)	0.4886 (2)	0.1761 (3)	0.00656*
O2	0.4124 (2)	0.3605 (3)	0.1460 (3)	0.00712*
O3	0.6068 (2)	0.3462 (3)	0.4937 (3)	0.00676*
O4	0.1649 (2)	0.2964 (2)	0.4653 (3)	0.00896*
D1	0.8847 (2)	0.5311 (3)	0.3106 (3)	0.02416*
D2	0.4711 (2)	0.3502 (3)	0.2725 (3)	0.01823*
D3	0.6246 (2)	0.2359 (3)	0.4422 (3)	0.02263*
D4	0.1017 (2)	0.2429 (3)	0.5517 (4)	0.02548*

(b200) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 497.58 (1) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.37718 (16) Å	T = 200 K
b = 7.88503 (13) Å	white
c = 6.76289 (10) Å	cylinder, ? × ? × ? mm
β = 95.6888 (9)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2900 data points
R_p = 0.024	Profile function: pseudo-Voigt
R_wp = 0.026	66 parameters
R_exp = ?
χ² = 1.690	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.6888 (9)°
M_r = 1386.93	V = 497.58 (1) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.37718 (16) Å	Neutron radiation, λ = 1.59432 Å
b = 7.88503 (13) Å	T = 200 K
c = 6.76289 (10) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.024	χ² = 1.690
R_wp = 0.026	2900 data points
R_exp = ?	66 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.6029 (2)	0.6406 (3)	0.2503 (3)	0.00657*
Ba2	0.1816 (2)	0.5482 (3)	0.2158 (4)	0.00712*
O1	0.8823 (2)	0.4878 (3)	0.1763 (3)	0.00948*
O2	0.4119 (2)	0.3604 (3)	0.1452 (3)	0.00929*
O3	0.6067 (2)	0.3462 (3)	0.4942 (3)	0.00972*
O4	0.1649 (2)	0.2964 (3)	0.4651 (3)	0.01181*
D1	0.8846 (2)	0.5308 (3)	0.3104 (4)	0.02725*
D2	0.4708 (2)	0.3494 (3)	0.2721 (3)	0.02113*
D3	0.6246 (2)	0.2362 (3)	0.4423 (3)	0.02596*
D4	0.1022 (2)	0.2431 (3)	0.5514 (4)	0.02748*

(b250) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 499.37 (2) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.39124 (17) Å	T = 250 K
b = 7.89581 (14) Å	white
c = 6.76818 (11) Å	cylinder, ? × ? × ? mm
β = 95.7195 (10)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 159.991°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2899 data points
R_p = 0.028	Profile function: pseudo-Voigt
R_wp = 0.027	1 parameters
R_exp = ?	(Δ/σ)_max = 0.00020
χ² = 1.742	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.7195 (10)°
M_r = 1386.93	V = 499.37 (2) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.39124 (17) Å	Neutron radiation, λ = 1.59432 Å
b = 7.89581 (14) Å	T = 250 K
c = 6.76818 (11) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 159.991°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.028	χ² = 1.742
R_wp = 0.027	2899 data points
R_exp = ?	1 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.6027 (3)	0.6400 (3)	0.2512 (4)	0.00853*
Ba2	0.1813 (2)	0.5483 (3)	0.2160 (4)	0.0092*
O1	0.8824 (2)	0.4870 (3)	0.1766 (4)	0.01139*
O2	0.4114 (2)	0.3601 (3)	0.1452 (3)	0.0126*
O3	0.6066 (2)	0.3464 (3)	0.4947 (4)	0.01315*
O4	0.1654 (2)	0.2962 (3)	0.4656 (4)	0.01404*
D1	0.8847 (2)	0.5304 (3)	0.3104 (4)	0.03018*
D2	0.4702 (2)	0.3494 (3)	0.2709 (3)	0.02332*
D3	0.6249 (2)	0.2370 (3)	0.4426 (3)	0.02823*
D4	0.1028 (3)	0.2434 (3)	0.5507 (4)	0.03088*

(b300) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 501.55 (1) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.40841 (16) Å	T = 300 K
b = 7.90854 (13) Å	white
c = 6.77476 (10) Å	cylinder, ? × ? × ? mm
β = 95.7570 (9)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2900 data points
R_p = 0.032	Profile function: pseudo-Voigt
R_wp = 0.024	66 parameters
R_exp = ?
χ² = 2.465	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.7570 (9)°
M_r = 1386.93	V = 501.55 (1) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.40841 (16) Å	Neutron radiation, λ = 1.59432 Å
b = 7.90854 (13) Å	T = 300 K
c = 6.77476 (10) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 160.041°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.032	χ² = 2.465
R_wp = 0.024	2900 data points
R_exp = ?	66 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.6018 (2)	0.6396 (3)	0.2519 (3)	0.01118*
Ba2	0.1810 (2)	0.5475 (3)	0.2158 (3)	0.01107*
O1	0.8825 (2)	0.4866 (3)	0.1772 (3)	0.01412*
O2	0.4108 (2)	0.3594 (3)	0.1444 (3)	0.01489*
O3	0.6068 (2)	0.3462 (3)	0.4953 (3)	0.01646*
O4	0.1662 (2)	0.2960 (3)	0.4646 (3)	0.01832*
D1	0.8844 (2)	0.5299 (3)	0.3101 (4)	0.03572*
D2	0.4697 (2)	0.3494 (3)	0.2702 (3)	0.02604*
D3	0.6249 (2)	0.2383 (3)	0.4424 (3)	0.03261*
D4	0.1041 (3)	0.2444 (3)	0.5505 (4)	0.03568*

(b420) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 507.09 (2) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.4576 (3) Å	T = 420 K
b = 7.9390 (2) Å	white
c = 6.78930 (19) Å	cylinder, ? × ? × ? mm
β = 95.8690 (15)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 159.941°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2898 data points
R_p = 0.055	Profile function: pseudo-Voigt
R_wp = 0.034	66 parameters
R_exp = ?
χ² = 2.465	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.8690 (15)°
M_r = 1386.93	V = 507.09 (2) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.4576 (3) Å	Neutron radiation, λ = 1.59432 Å
b = 7.9390 (2) Å	T = 420 K
c = 6.78930 (19) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 159.941°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.055	χ² = 2.465
R_wp = 0.034	2898 data points
R_exp = ?	66 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.5996 (4)	0.6382 (5)	0.2519 (6)	0.01782*
Ba2	0.1802 (4)	0.5474 (4)	0.2158 (6)	0.01287*
O1	0.8827 (4)	0.4857 (5)	0.1783 (6)	0.02265*
O2	0.4096 (4)	0.3578 (5)	0.1430 (5)	0.01951*
O3	0.6075 (4)	0.3451 (5)	0.4952 (6)	0.02553*
O4	0.1675 (4)	0.2933 (5)	0.4642 (6)	0.02521*
D1	0.8832 (4)	0.5279 (5)	0.3099 (7)	0.04819*
D2	0.4684 (4)	0.3480 (5)	0.2650 (6)	0.03738*
D3	0.6256 (4)	0.2398 (5)	0.4409 (6)	0.04359*
D4	0.1058 (4)	0.2470 (5)	0.5474 (8)	0.04907*

(b480) deuterated barium hydroxide top

Crystal data top

Ba(OD)₂	V = 510.26 (2) Å³
M_r = 1386.93	Z = 8
Monoclinic, P2₁/n	Neutron radiation, λ = 1.59432 Å
a = 9.4881 (2) Å	T = 480 K
b = 7.95273 (19) Å	white
c = 6.79846 (17) Å	cylinder, ? × ? × ? mm
β = 95.9117 (13)°

Data collection top

Diffractometer D 2B, ILL	Data collection mode: transmission
Radiation source: high-flux isotope reactor	Scan 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.	2θ_min = 15.091°, 2θ_max = 159.941°, 2θ_step = 0.05°

Refinement top

Refinement on rietveld	2898 data points
R_p = 0.058	Profile function: pseudo-Voigt
R_wp = 0.028	1 parameters
R_exp = ?	(Δ/σ)_max = 0.001
χ² = 1.690	Background function: shifted Chebyshev background function

Crystal data top

Ba(OD)₂	β = 95.9117 (13)°
M_r = 1386.93	V = 510.26 (2) Å³
Monoclinic, P2₁/n	Z = 8
a = 9.4881 (2) Å	Neutron radiation, λ = 1.59432 Å
b = 7.95273 (19) Å	T = 480 K
c = 6.79846 (17) Å	cylinder, ? × ? × ? mm

Data collection top

Diffractometer D 2B, ILL	Scan 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.	2θ_min = 15.091°, 2θ_max = 159.941°, 2θ_step = 0.05°
Data collection mode: transmission

Refinement top

R_p = 0.058	χ² = 1.690
R_wp = 0.028	2898 data points
R_exp = ?	1 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.5999 (3)	0.6371 (4)	0.2534 (5)	0.02082*
Ba2	0.1810 (3)	0.5446 (4)	0.2139 (5)	0.01553*
O1	0.8851 (3)	0.4842 (4)	0.1797 (6)	0.02888*
O2	0.4086 (3)	0.3568 (4)	0.1418 (5)	0.02452*
O3	0.6092 (3)	0.3466 (5)	0.4979 (6)	0.03385*
O4	0.1693 (3)	0.2920 (4)	0.4643 (5)	0.02796*
D1	0.8840 (4)	0.5279 (5)	0.3092 (6)	0.05974*
D2	0.4681 (3)	0.3476 (4)	0.2636 (5)	0.0452*
D3	0.6266 (4)	0.2432 (5)	0.4446 (6)	0.05567*
D4	0.1080 (4)	0.2474 (5)	0.5479 (7)	0.05723*

Experimental details

	(a10)	(a50)	(a100)	(a150)
Crystal data
Chemical formula	Ba(OD)₂	Ba(OD)₂	Ba(OD)₂	Ba(OD)₂
M_r	3467.32	3467.32	3467.32	3467.32
Crystal system, space group	Monoclinic, P2₁/n	Monoclinic, P2₁/n	Monoclinic, P2₁/n	Orthorhombic, Pnma
Temperature (K)	10	50	100	150
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), 90	90, 91.3091 (15), 90	90, 91.0598 (19), 90	90, 90, 90
V (Å³)	1264.94 (5)	1265.22 (5)	1267.96 (6)	1272.26 (6)
Z	20	20	20	20
Radiation type	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å
µ (mm⁻¹)	?	?	?	?
Specimen shape, size (mm)	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?

Data collection
Diffractometer	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL
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.	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 mode	Transmission	Transmission	Transmission	Transmission
Scan method	Step	Step	Step	Step
2θ values (°)	2θ_min = 10.141 2θ_max = 159.991 2θ_step = 0.05	2θ_min = 10.091 2θ_max = 159.991 2θ_step = 0.05	2θ_min = 10.141 2θ_max = 160.041 2θ_step = 0.05	2θ_min = 10.091 2θ_max = 160.041 2θ_step = 0.05

Refinement
R factors and goodness of fit	R_p = 0.021, R_wp = 0.031, R_exp = ?, χ² = 1.904	R_p = 0.022, R_wp = 0.029, R_exp = ?, χ² = 1.664	R_p = 0.030, R_wp = 0.033, R_exp = ?, χ² = 2.310	R_p = 0.052, R_wp = 0.039, R_exp = ?, χ² = 3.240
No. of data points	2998	2999	2999	3000
No. of parameters	1	1	109	77
No. of restraints	?	?	?	?

	(a200)	(480)	(a552)	(b10)
Crystal data
Chemical formula	Ba(OD)₂	Ba(OD)₂	Ba(OD)₂	Ba(OD)₂
M_r	3467.32	3467.32	3467.32	1386.93
Crystal system, space group	Orthorhombic, Pnma	Orthorhombic, Pnma	Orthorhombic, Pnma	Monoclinic, P2₁/n
Temperature (K)	200	480	552	10
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, 90	90, 90, 90	90, 90, 90	90, 95.6551 (8), 90
V (Å³)	1276.96 (6)	1310.99 (7)	1323.9 (1)	494.08 (1)
Z	20	20	20	8
Radiation type	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å
µ (mm⁻¹)	?	?	?	?
Specimen shape, size (mm)	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?

Data collection
Diffractometer	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL
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.	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 mode	Transmission	Transmission	Transmission	Transmission
Scan method	Step	Step	Step	Step
2θ values (°)	2θ_min = 10.091 2θ_max = 160.041 2θ_step = 0.05	2θ_min = 10.091 2θ_max = 159.991 2θ_step = 0.05	2θ_min = 10.091 2θ_max = 159.941 2θ_step = 0.05	2θ_min = 15.091 2θ_max = 160.041 2θ_step = 0.05

Refinement
R factors and goodness of fit	R_p = 0.060, R_wp = 0.039, R_exp = ?, χ² = 3.098	R_p = 0.094, R_wp = 0.032, R_exp = ?, χ² = 2.341	R_p = 0.064, R_wp = 0.032, R_exp = ?, χ² = 1.716	R_p = 0.023, R_wp = 0.027, R_exp = ?, χ² = 2.103
No. of data points	3000	2999	2998	2900
No. of parameters	1	78	1	66
No. of restraints	?	?	?	?

	(brt)	(b50)	(b100)	(b150)
Crystal data
Chemical formula	Ba(OD)₂	Ba(OD)₂	Ba(OD)₂	Ba(OD)₂
M_r	1386.93	1386.93	1386.93	1386.93
Crystal system, space group	Monoclinic, P2₁/n	Monoclinic, P2₁/n	Monoclinic, P2₁/n	Monoclinic, P2₁/n
Temperature (K)	RT	50	100	150
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), 90	90, 95.6551 (8), 90	90, 95.6564 (9), 90	90, 95.6670 (9), 90
V (Å³)	501.80 (3)	494.25 (1)	494.92 (1)	496.06 (1)
Z	8	8	8	8
Radiation type	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å
µ (mm⁻¹)	?	?	?	?
Specimen shape, size (mm)	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?

Data collection
Diffractometer	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL
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.	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 mode	Transmission	Transmission	Transmission	Transmission
Scan method	Step	Step	Step	Step
2θ values (°)	2θ_min = 15.091 2θ_max = 159.991 2θ_step = 0.05	2θ_min = 15.091 2θ_max = 160.041 2θ_step = 0.05	2θ_min = 15.091 2θ_max = 160.041 2θ_step = 0.05	2θ_min = 15.091 2θ_max = 160.041 2θ_step = 0.05

Refinement
R factors and goodness of fit	R_p = 0.052, R_wp = 0.043, R_exp = ?, χ² = 3.725	R_p = 0.022, R_wp = 0.027, R_exp = ?, χ² = 1.850	R_p = 0.022, R_wp = 0.027, R_exp = ?, χ² = 1.796	R_p = 0.024, R_wp = 0.027, R_exp = ?, χ² = 1.796
No. of data points	2899	2900	2900	2900
No. of parameters	1	66	66	66
No. of restraints	?	?	?	?

	(b200)	(b250)	(b300)	(b420)
Crystal data
Chemical formula	Ba(OD)₂	Ba(OD)₂	Ba(OD)₂	Ba(OD)₂
M_r	1386.93	1386.93	1386.93	1386.93
Crystal system, space group	Monoclinic, P2₁/n	Monoclinic, P2₁/n	Monoclinic, P2₁/n	Monoclinic, P2₁/n
Temperature (K)	200	250	300	420
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), 90	90, 95.7195 (10), 90	90, 95.7570 (9), 90	90, 95.8690 (15), 90
V (Å³)	497.58 (1)	499.37 (2)	501.55 (1)	507.09 (2)
Z	8	8	8	8
Radiation type	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å	Neutron, λ = 1.59432 Å
µ (mm⁻¹)	?	?	?	?
Specimen shape, size (mm)	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?	Cylinder, ? × ? × ?

Data collection
Diffractometer	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL	Diffractometer D 2B, ILL
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.	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 mode	Transmission	Transmission	Transmission	Transmission
Scan method	Step	Step	Step	Step
2θ values (°)	2θ_min = 15.091 2θ_max = 160.041 2θ_step = 0.05	2θ_min = 15.091 2θ_max = 159.991 2θ_step = 0.05	2θ_min = 15.091 2θ_max = 160.041 2θ_step = 0.05	2θ_min = 15.091 2θ_max = 159.941 2θ_step = 0.05

Refinement
R factors and goodness of fit	R_p = 0.024, R_wp = 0.026, R_exp = ?, χ² = 1.690	R_p = 0.028, R_wp = 0.027, R_exp = ?, χ² = 1.742	R_p = 0.032, R_wp = 0.024, R_exp = ?, χ² = 2.465	R_p = 0.055, R_wp = 0.034, R_exp = ?, χ² = 2.465
No. of data points	2900	2899	2900	2898
No. of parameters	66	1	66	66
No. of restraints	?	?	?	?

	(b480)
Crystal data
Chemical formula	Ba(OD)₂
M_r	1386.93
Crystal system, space group	Monoclinic, 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
V (Å³)	510.26 (2)
Z	8
Radiation type	Neutron, λ = 1.59432 Å
µ (mm⁻¹)	?
Specimen shape, size (mm)	Cylinder, ? × ? × ?

Data collection
Diffractometer	Diffractometer D 2B, ILL
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.
Data collection mode	Transmission
Scan method	Step
2θ values (°)	2θ_min = 15.091 2θ_max = 159.941 2θ_step = 0.05

Refinement
R factors and goodness of fit	R_p = 0.058, R_wp = 0.028, R_exp = ?, χ² = 1.690
No. of data points	2898
No. of parameters	1
No. of restraints	?

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

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
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Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text