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Issue 7, 2012
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Investigation of the crystal structure of a basic bismuth(iii) nitrate with the composition [Bi6O4(OH)4]0.54(1)[Bi6O5(OH)3]0.46(1)(NO3)5.54(1)

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Abstract

A basic bismuth(III) nitrate with the composition [Bi6O4(OH)4]0.5[Bi6O5(OH)3]0.5(NO3)5.5 formed in a slow crystal growth mode has an ordered crystal structure with the monoclinic space group P21 and lattice parameters a = 15.850(3), b = 14.986(3), c = 18.230(4) Å, β = 107.329(17)° and volume V = 4133.6 Å3 (Henry et al. 2003). In a very fast crystal growth mode the complex ions disorder in another P21 cell with slightly different lattice parameters a = 15.8404(1), b = 15.1982(1), c = 18.3122(1) Å, β = 106.829(1)° and V = 4219.8 Å3. This cell can be related to two smaller cells: a monoclinic C2/m cell with a = 13.7161(1), b = 15.1943(1), c = 10.2399(1) Å, β = 98.586(1)° and V = 2110.1 Å3 and a trigonal R[3 with combining macron] cell with a = 15.18650(6), c = 15.8416(1) Å (hexagonal setting) and V = 3164.1 Å3. These smaller cells correspond to average structures and hence the X-ray data do not account for the difference in the structures of the two different complex ions. However, when analysing neutron powder diffraction data, it is possible to distinguish between the two complex ions using a trigonal R[3 with combining macron] cell with a = 15.1865(1) and c = 15.8416(1) Å (hexagonal setting). In a Rietveld type structure model refinement with a total of 28 atom sites (4 Bi, 3 N, 15 O and 6 H), the composition of this sample is determined to be [Bi6O4(OH)4]0.54(1)[Bi6O5(OH)3]0.46(1)(NO3)5.54(1).

Graphical abstract: Investigation of the crystal structure of a basic bismuth(iii) nitrate with the composition [Bi6O4(OH)4]0.54(1)[Bi6O5(OH)3]0.46(1)(NO3)5.54(1)

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Article information


Submitted
31 Aug 2011
Accepted
18 Oct 2011
First published
16 Dec 2011

Dalton Trans., 2012,41, 1971-1980
Article type
Paper

Investigation of the crystal structure of a basic bismuth(III) nitrate with the composition [Bi6O4(OH)4]0.54(1)[Bi6O5(OH)3]0.46(1)(NO3)5.54(1)

A. Nørlund Christensen and B. Lebech, Dalton Trans., 2012, 41, 1971
DOI: 10.1039/C1DT11646K

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