Dimorphism of [Bi₂O₂(OH)](NO₃) – the ordered Pna2₁ structure at 100 K

A structural phase transition occurs for [Bi₂O₂(OH)](NO₃) between 173 K (space group Cmc2₁; previous single-crystal X-ray data) and 100 K (space group Pna2₁; current single-crystal X-ray data).

Computing details

Dioxidodibismuth(III) hydroxide nitrate

Crystal data

[Bi2O2(OH)](NO3)	Dx = 7.129 Mg m^−3
Mr = 528.98	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pna21	Cell parameters from 3403 reflections
a = 5.3854 (13) Å	θ = 2.9–36.3°
b = 5.3676 (13) Å	µ = 71.27 mm^−1
c = 17.051 (4) Å	T = 100 K
V = 492.9 (2) Å^3	Plate, light yellow
Z = 4	0.09 × 0.08 × 0.01 mm
F(000) = 888

Data collection

Bruker APEXII CCD diffractometer	2407 reflections with I > 2σ(I)
ω–scans	Rint = 0.062
Absorption correction: numerical (HABITUS; Herrendorf, 1997)	θmax = 38.8°, θmin = 1.2°
Tmin = 0.017, Tmax = 0.524	h = −8→9
9853 measured reflections	k = −9→8
2798 independent reflections	l = −29→29

Refinement

Refinement on F^2	1 restraint
Least-squares matrix: full	H-atom parameters not defined
R[F^2 > 2σ(F^2)] = 0.030	w = 1/[σ^2(Fo^2) + (0.0213P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.057	(Δ/σ)max < 0.001
S = 0.98	Δρmax = 3.13 e Å^−3
2798 reflections	Δρmin = −3.61 e Å^−3
48 parameters	Absolute structure: Twinning involves inversion, so Flack parameter cannot be determined

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 2-component inversion twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Bi1	0.04362 (7)	−0.00785 (7)	0.23658 (3)	0.00299 (7)
Bi2	0.08217 (8)	0.48199 (6)	0.08442 (4)	0.00432 (8)
O1A	0.2866 (15)	0.2468 (15)	0.1678 (5)	0.0041 (15)*
O1B	0.2840 (15)	0.7394 (15)	0.1683 (5)	0.0053 (15)*
O2	0.4937 (17)	0.4539 (16)	0.0423 (6)	0.0097 (15)*
N1	0.021 (2)	0.4969 (18)	0.3759 (6)	0.0091 (19)*
O3	0.0363 (16)	0.4977 (15)	0.3004 (5)	0.0089 (14)*
O4	0.8650 (17)	0.6351 (17)	0.4084 (6)	0.0148 (19)*
O5	0.1626 (17)	0.3604 (16)	0.4153 (6)	0.0145 (18)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Bi1	0.00314 (12)	0.00303 (15)	0.00279 (14)	−0.00018 (11)	0.00001 (12)	0.0001 (2)
Bi2	0.00461 (13)	0.00439 (16)	0.00395 (15)	−0.00002 (11)	−0.00086 (14)	0.0010 (3)

Geometric parameters (Å, º)

Bi1—O1B^i	2.203 (8)	Bi2—O1B	2.267 (8)
Bi1—O1B^ii	2.207 (8)	Bi2—O2	2.334 (9)
Bi1—O1A	2.226 (8)	Bi2—O1A^i	2.462 (8)
Bi1—O1A^i	2.292 (8)	Bi2—O2^i	2.493 (9)
Bi1—O3^iii	2.868 (9)	Bi2—O1B^iv	2.619 (8)
Bi1—O3^ii	2.868 (8)	N1—O5	1.251 (14)
Bi1—O3	2.924 (8)	N1—O4^v	1.251 (13)
Bi1—O3^i	2.941 (9)	N1—O3	1.291 (14)
Bi2—O1A	2.197 (8)
O1B^i—Bi1—O1B^ii	75.34 (18)	O1A^i—Bi2—O1B^iv	64.7 (3)
O1B^i—Bi1—O1A	116.2 (3)	O2^i—Bi2—O1B^iv	125.2 (3)
O1B^ii—Bi1—O1A	75.8 (3)	Bi2—O1A—Bi1	113.5 (3)
O1B^i—Bi1—O1A^i	72.0 (3)	Bi2—O1A—Bi1^iii	106.4 (3)
O1B^ii—Bi1—O1A^i	117.4 (3)	Bi1—O1A—Bi1^iii	117.4 (4)
O1A—Bi1—O1A^i	73.15 (16)	Bi2—O1A—Bi2^iii	103.7 (3)
O1A—Bi2—O1B	72.6 (3)	Bi1—O1A—Bi2^iii	112.2 (3)
O1A—Bi2—O2	71.7 (3)	Bi1^iii—O1A—Bi2^iii	102.1 (3)
O1B—Bi2—O2	77.2 (3)	Bi1^iii—O1B—Bi1^vi	116.1 (4)
O1A—Bi2—O1A^i	70.34 (18)	Bi1^iii—O1B—Bi2	107.1 (3)
O1B—Bi2—O1A^i	104.4 (3)	Bi1^vi—O1B—Bi2	115.2 (4)
O2—Bi2—O1A^i	139.4 (3)	Bi1^iii—O1B—Bi2^vii	102.8 (3)
O1A—Bi2—O2^i	75.1 (3)	Bi1^vi—O1B—Bi2^vii	107.3 (3)
O1B—Bi2—O2^i	147.7 (3)	Bi2—O1B—Bi2^vii	107.3 (3)
O2—Bi2—O2^i	91.8 (3)	Bi2—O2—Bi2^iii	98.8 (3)
O1A^i—Bi2—O2^i	64.8 (3)	O5—N1—O4^v	121.3 (11)
O1A—Bi2—O1B^iv	106.4 (3)	O5—N1—O3	120.0 (10)
O1B—Bi2—O1B^iv	66.50 (16)	O4^v—N1—O3	118.7 (10)
O2—Bi2—O1B^iv	141.9 (3)

Symmetry codes: (i) x−1/2, −y+1/2, z; (ii) x, y−1, z; (iii) x+1/2, −y+1/2, z; (iv) x−1/2, −y+3/2, z; (v) x−1, y, z; (vi) x, y+1, z; (vii) x+1/2, −y+3/2, z.