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Volume 64 
Part 7 
Pages i43-i44  
July 2008  

Received 8 March 2008
Accepted 21 April 2008
Online 7 June 2008

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Key indicators
Single-crystal X-ray study
T = 150 K
Mean [sigma](S-O) = 0.002 Å
R = 0.018
wR = 0.040
Data-to-parameter ratio = 13.9
Details
Open access

Cadmium sulfite hexahydrate revisited

Sergio Baggio,a Andrés Ibáñezb and Ricardo Baggioc*

aUniversidad Nacional de la Patagonia, Sede Puerto Madryn, and, CenPat, CONICET, 9120 Puerto Madryn, Chubut, Argentina,bDepartamento de Física, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile and CIMAT, Casilla 487-3, Santiago de Chile, Chile, and cDepartamento de Física, Comisión Nacional de Energía Atómica, Buenos Aires, Argentina
Correspondence e-mail: unbaggio@cenpat.edu.ar

The present structural revision of the title compound, tetracadmium tetrasulfite hexahydrate, [Cd4(SO3)4(H2O)5]·H2O, is a low-temperature upgrade (T = 100 K and R = 0.017) of the original room-temperature structure reported by Kiers & Vos [Cryst. Struct. Commun. (1978). 7, 399-403; T = 293 K and R = 0.080). The compound is a three-dimensional polymer with four independent cadmium centres, four sulfite anions and six water molecules, five of them coordinated to two cadmium centres and the remaining one an unbound solvent molecule which completes the asymmetric unit. There are two types of cadmium environment: CdO8 (through four chelating sulfite ligands) and CdO6 (by way of six monocoordinated ligands). The former groups form planar arrays [parallel to (001) and separated by half a unit cell translation along c], made up of chains running along [110] and [[\overline{1}]10], respectively. These chains are, in turn, interconnected both in an intraplanar as well as in an interplanar fashion by the latter CdO6 polyhedra into a tight three-dimensional framework. There is, in addition, an extensive network of hydrogen bonds, in which all 12 water H atoms act as donors and eight O atoms from all four sulfite groups and two water molecules act as acceptors.

Related literature

For related literature, see: Agre et al. (1981[Agre, V. M., Kozlova, N. P., TrunovV, K. & Ershova, S. D. (1981). Zh. Strukt. Khim. 22, 138-146.]); Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]); Elder et al. (1978[Elder, R. C., Heeg, M. J., Payne, M. D., Trkula, M. & Deutsch, E. (1978). Inorg. Chem. 17, 431-440.]); Harvey et al. (2006[Harvey, M. A., Baggio, S. & Baggio, R. (2006). Acta Cryst. B62, 1038-1042.]); Kiers & Vos (1978[Kiers, C. Th. & Vos, A. (1978). Cryst. Struct. Commun. 7, 399-403.]); Larsson & Kierkegaard (1969[Larsson, L. O. & Kierkegaard, P. (1969). Acta Chem. Scand. 23, 2253-2260.]).

Experimental

Crystal data

  • [Cd4(SO3)4(H2O)5]·H2O

  • Mr = 877.94

  • Monoclinic, P 21 /c

  • a = 12.1406 (3) Å

  • b = 10.5485 (3) Å

  • c = 13.9329 (4) Å

  • [beta] = 103.93 (1)°

  • V = 1731.82 (11) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 5.41 mm-1

  • T = 150 (2) K

  • 0.24 × 0.12 × 0.08 mm
Data collection

  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2001[Sheldrick, G. M. (2001). SADABS. University of Göttingen, Germany.]) Tmin = 0.40, Tmax = 0.64

  • 31336 measured reflections

  • 3959 independent reflections

  • 3922 reflections with I > 2[sigma](I)

  • Rint = 0.021
Refinement

  • R[F2 > 2[sigma](F2)] = 0.017

  • wR(F2) = 0.040

  • S = 1.26

  • 3959 reflections

  • 284 parameters

  • 18 restraints

  • All H-atom parameters refined

  • [Delta][rho]max = 0.70 e Å-3

  • [Delta][rho]min = -0.56 e Å-3

Table 1
Selected bond lengths (Å)

Cd1-O13 2.2452 (18)
Cd1-O32i 2.2839 (18)
Cd1-O22 2.3065 (18)
Cd1-O21 2.4078 (17)
Cd1-O12 2.4542 (18)
Cd1-O31 2.4752 (18)
Cd1-O23 2.6544 (18)
Cd1-O12i 2.7665 (19)
Cd2-O34 2.3311 (18)
Cd2-O14ii 2.3365 (18)
Cd2-O33 2.3440 (18)
Cd2-O11 2.3545 (18)
Cd2-O24ii 2.4074 (18)
Cd2-O23 2.4446 (18)
Cd2-O14 2.6091 (18)
Cd2-O21 2.8126 (18)
Cd3-O2W 2.215 (2)
Cd3-O1W 2.2272 (19)
Cd3-O3W 2.278 (2)
Cd3-O31 2.3201 (17)
Cd3-O12 2.3482 (18)
Cd3-O11iii 2.3518 (18)
Cd4-O34 2.2412 (18)
Cd4-O4W 2.2599 (18)
Cd4-O5W 2.2601 (19)
Cd4-O32iv 2.2816 (18)
Cd4-O23v 2.3203 (17)
Cd4-O21 2.3571 (17)
Symmetry codes: (i) -x+1, -y, -z+1; (ii) -x, -y+1, -z+1; (iii) -x+1, -y+1, -z+1; (iv) [-x+1, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]; (v) [x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}].

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1W-H1WA...O13i 0.82 (3) 1.88 (2) 2.693 (3) 170 (4)
O1W-H1WB...O14vi 0.82 (3) 1.93 (2) 2.679 (3) 151 (3)
O2W-H2WA...O4Wiv 0.82 (3) 1.93 (2) 2.719 (3) 162 (4)
O2W-H2WB...O6W 0.82 (3) 1.95 (2) 2.681 (3) 149 (4)
O3W-H3WA...O6Wvii 0.82 (3) 2.02 (2) 2.833 (3) 172 (4)
O3W-H3WB...O22i 0.82 (3) 2.29 (2) 3.092 (3) 168 (4)
O4W-H4WA...O22 0.82 (3) 1.87 (2) 2.651 (3) 159 (3)
O4W-H4WB...O31v 0.82 (3) 1.98 (2) 2.780 (3) 167 (3)
O5W-H5WA...O33 0.82 (3) 2.05 (2) 2.848 (3) 167 (4)
O5W-H5WB...O24viii 0.82 (3) 1.92 (2) 2.708 (3) 162 (4)
O6W-H6WA...O24ix 0.82 (3) 2.16 (2) 2.876 (3) 146 (4)
O6W-H6WB...O33x 0.82 (3) 2.18 (2) 2.948 (3) 157 (4)
Symmetry codes: (i) -x+1, -y, -z+1; (iv) [-x+1, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]; (v) [x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]; (vi) x+1, y, z; (vii) [x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]; (viii) [-x, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]; (ix) [-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]; (x) [x+1, -y+{\script{1\over 2}}, z+{\script{1\over 2}}].

Data collection: SMART (Bruker, 2001[Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2003[Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.]).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BR2070 ).

Acknowledgements

We acknowledge the Spanish Research Council (CSIC) for providing us with a free-of-charge licence for the CSD system (Allen, 2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]).

References

Agre, V. M., Kozlova, N. P., TrunovV, K. & Ershova, S. D. (1981). Zh. Strukt. Khim. 22, 138-146.  [ChemPort]
Allen, F. H. (2002). Acta Cryst. B58, 380-388.  [ISI] [CrossRef] [details]
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.  [CrossRef] [details]
Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Elder, R. C., Heeg, M. J., Payne, M. D., Trkula, M. & Deutsch, E. (1978). Inorg. Chem. 17, 431-440.  [CrossRef] [ChemPort]
Harvey, M. A., Baggio, S. & Baggio, R. (2006). Acta Cryst. B62, 1038-1042.  [CrossRef] [details]
Kiers, C. Th. & Vos, A. (1978). Cryst. Struct. Commun. 7, 399-403.  [ChemPort]
Larsson, L. O. & Kierkegaard, P. (1969). Acta Chem. Scand. 23, 2253-2260.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2001). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.  [CrossRef] [details]

Acta Cryst (2008). E64, i43-i44   [ doi:10.1107/S1600536808011409 ]

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