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Volume 64 
Part 10 
Pages m1280-m1281  
October 2008  

Received 9 June 2008
Accepted 11 September 2008
Online 20 September 2008

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Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.010 Å
H completeness 37%
Disorder in main residue
R = 0.025
wR = 0.063
Data-to-parameter ratio = 16.9
Details
Open access

Tricaesium tris(pyridine-2,6-dicarboxylato-[kappa]3O2,N,O6)lutetium(III) octahydrate

Vincent Legrand,a* Flavien Aubert,b Anthony D'Aléo,c Philippe Rabillerb and Olivier Mauryc

aInstitut Laue Langevin, 6 rue Jules Horowitz, B.P.156, 38042 Grenoble Cedex 9, France,bGroupe Matiere Condensee et Materiaux, UMR CNRS 6626, Universite de Rennes 1, Campus de Beaulieu, 35042 Rennes cedex, France, and cLaboratoire de Chimie, UMR CNRS 5182, ENS Lyon, 46 allee d'Italie, 69364 Lyon cedex 07, France
Correspondence e-mail: legrand@ill.fr

Colourless block crystals of the title compound, Cs3[Lu(dipic)3]·8H2O [dipic is dipicolinate or pyridine-2,6-dicarboxylate, C7H3NO4] were synthesized by slow evaporation of the solvent. The crystal structure of this LuIII-complex, isostructural with the DyIII and EuIII complexes, was determined from a crystal twinned by inversion and consists of discrete [Lu(dipic)3]3- anions, Cs+ cations and water molecules involving hydrogen bonding. The Lu atom lies on a twofold rotation axis and is coordinated by six O atoms and three N atoms of three dipicolinate ligands. One Cs atom is also on a twofold axis. The unit cell can be regarded as successive layers along the crystallographic c-axis formed by [Lu(dipic)3]3- anionic planes and [Cs+, H2O] cationic planes. In the crystal structure, although the H atoms attached to water molecules could not be located, short O-O contacts clearly indicate the occurrence of an intricate hydrogen-bonded network through contacts with other water molecules, Cs cations or with the O atoms of the dipicolinate ligands.

Related literature

For potential applications of lanthanide complexes as second-order non-linear optical materials, see: Tancrez et al. (2005[Tancrez, N., Feuvrie, C., Ledoux, I., Zyss, J., Toupet, L., Le Bozec, H. & Maury, O. (2005). J. Am. Chem. Soc. 127, 13474-13475.]); Sénéchal et al. (2004[Sénéchal, K., Toupet, L., Ledoux, I., Zyss, J., Le Bozec, H. & Maury, O. (2004). Chem. Commun. pp. 2180-2181.]). For the isostructural EuIII complex, see: Brayshaw et al. (1995[Brayshaw, P. A., Bünzli, J.-C. G., Foidevaux, P., Harrowfield, J. M., Kim, Y. & Sobolev, A. N. (1995). Inorg. Chem. 34, 2068-2076.]). For other related complexes, see: Murray et al. (1990[Murray, G. M., Sarrio, R. M. & Peterson, J. R. (1990). Inorg. Chim. Acta, 176, 233-240.]). For related literature, see: Flack & Bernardinelli (1999[Flack, H. D. & Bernardinelli, G. (1999). Acta Cryst. A55, 908-915.], 2000[Flack, H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148.]).

[Scheme 1]

Experimental

Crystal data

  • Cs3[Lu(C7H3NO4)3]·8H2O

  • Mr = 1213.14

  • Orthorhombic, C 2221

  • a = 10.0406 (2) Å

  • b = 17.8109 (6) Å

  • c = 18.4221 (5) Å

  • V = 3294.46 (16) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 6.36 mm-1

  • T = 100 (2) K

  • 0.20 × 0.19 × 0.19 mm
Data collection

  • Oxford Diffraction Xcalibur-Sapphire3 diffractometer

  • Absorption correction: Gaussian (ABSORB; DeTitta, 1985[DeTitta, G. T. (1985). J. Appl. Cryst. 18, 75-79.]) Tmin = 0.307, Tmax = 0.425

  • 51066 measured reflections

  • 3520 independent reflections

  • 3491 reflections with I > 2[sigma](I)

  • Rint = 0.045
Refinement

  • R[F2 > 2[sigma](F2)] = 0.025

  • wR(F2) = 0.063

  • S = 1.46

  • 3520 reflections

  • 208 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 3.00 e Å-3

  • [Delta][rho]min = -0.94 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1501 Friedel pairs

  • Flack parameter: 0.270 (12)

Data collection: CrysAlis CCD (Oxford Diffraction 2006[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.]); cell refinement: CrysAlis RED (Oxford Diffraction 2006[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.]); data reduction: SORTAV (Blessing, 1989[Blessing, R. H. (1989). J. Appl. Cryst. 22, 396-397.]); program(s) used to solve structure: SIR97 (Altomare et al., 1999[Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: DN2357 ).

References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.  [CrossRef] [details]
Blessing, R. H. (1989). J. Appl. Cryst. 22, 396-397.  [CrossRef] [details]
Brayshaw, P. A., Bünzli, J.-C. G., Foidevaux, P., Harrowfield, J. M., Kim, Y. & Sobolev, A. N. (1995). Inorg. Chem. 34, 2068-2076.  [CrossRef] [ChemPort]
DeTitta, G. T. (1985). J. Appl. Cryst. 18, 75-79.  [CrossRef] [details]
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  [CrossRef] [details]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [details]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Flack, H. D. & Bernardinelli, G. (1999). Acta Cryst. A55, 908-915.  [CrossRef] [details]
Flack, H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148.  [CrossRef] [details]
Murray, G. M., Sarrio, R. M. & Peterson, J. R. (1990). Inorg. Chim. Acta, 176, 233-240.  [CrossRef] [ChemPort]
Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.
Sénéchal, K., Toupet, L., Ledoux, I., Zyss, J., Le Bozec, H. & Maury, O. (2004). Chem. Commun. pp. 2180-2181.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Tancrez, N., Feuvrie, C., Ledoux, I., Zyss, J., Toupet, L., Le Bozec, H. & Maury, O. (2005). J. Am. Chem. Soc. 127, 13474-13475.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]

Acta Cryst (2008). E64, m1280-m1281   [ doi:10.1107/S1600536808029243 ]

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