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Volume 66 
Part 6 
Page i46  
June 2010  

Received 28 April 2010
Accepted 4 May 2010
Online 8 May 2010

Key indicators
Single-crystal X-ray study
T = 296 K
Mean [sigma](Lu-O) = 0.003 Å
R = 0.020
wR = 0.038
Data-to-parameter ratio = 17.5
Details
Open access

Lutetium(III) cyclotetraphosphate

aLaboratoire de Chimie Industrielle, Département de Génie des Matériaux, Ecole Nationale d'Ingénieurs de Sfax, Université de Sfax, BP W 3038, Sfax, Tunisia, and bLaboratoire des Matériaux Inorganiques, UMR CNRS 6002, Université Blaise Pascal, 24 Avenue des Landais, 63177 Aubière, France
Correspondence e-mail: daniel.avignant@univ-bpclermont.fr

Single crystals of the title compound, tetralutetium(III) tris(cyclotetraphosphate), Lu4(P4O12)3, were obtained by solid-state reaction. The cubic structure is isotypic with its AlIII and ScIII analogues and is built up from four-membered (P4O12)4- phosphate ring anions ([\overline{4}] symmetry), isolated from each other and further linked through isolated LuO6 octahedra (.3. symmetry) via corner sharing. Each LuO6 octahedron is linked to six (P4O12)4- rings, while each (P4O12)4- ring is linked to eight LuO6 octahedra.

Related literature

The title compound belongs to a structural type discovered a long time ago through the Al4(P4O12)3 member, the structure of which was first investigated by Hendricks & Wyckoff (1927[Hendricks, S. B. & Wyckoff, R. W. G. (1927). Am. J. Sci. 13, 491-496.]) and then described by Pauling & Sherman (1937[Pauling, L. & Sherman, J. S. (1937). Z. Kristallogr. 96, 481-487.]). Since then, five isotypic compounds have been characterized: Cr4(P4O12)3 (Rémy & Boullé, 1964[Rémy, P. & Boullé, A. (1964). C. R. Acad. Sci. 258, 927-929.]); Ti4(P4O12)3 (Liebau & Williams, 1964[Liebau, F. & Williams, H. P. (1964). Angew. Chem. 76, 303-304.]); Fe4(P4O12)3 (d'Yvoire et al., 1962[d'Yvoire, F. (1962). Bull. Soc. Chim. pp. 1237-1243.]); Sc4(P4O12)3 (Bagieu-Beucher, 1976[Bagieu-Beucher, M. (1976). J. Appl. Cryst. 9, 368-369.]; Mezentseva et al., 1977[Mezentseva, L. P., Domanskii, A. I. & Bondar, I. A. (1977). Russ. J. Inorg. Chem. 22, 43-45.]; Bagieu-Beucher & Guitel, 1978[Bagieu-Beucher, M. & Guitel, J. C. (1978). Acta Cryst. B34, 1439-1442.]; Smolin et al. 1978[Smolin, Y. I., Shepelev, Y. F., Domanskii, A. I. & Belov, N. V. (1978). Kristallografiya, 23, 187-188.]) and Yb4(P4O12)3 (Chudinova, 1979[Chudinova, N. N. (1979). Izv. Akad. Nauk SSSR Neorg. Mater. 15, 833-837.]). For a review of the crystal chemistry of cyclotetraphosphates, see: Durif (1995[Durif, A. (1995). In Crystal Chemistry of Condensed Phosphates. New York and London: Plenum Press.]). For other polymorphs of composition Lu(PO3)3, see: Höppe & Sedlmaier (2007[Höppe, H. A. & Sedlmaier, S. J. (2007). Inorg. Chem. 46, 3467-3474.]); Yuan et al. (2008[Yuan, J. L., Zhang, H., Zhao, J. T., Chen, H. H., Yang, X. X. & Zhang, G. B. (2008). Opt. Mater. 30, 1369-1374.]); Bejaoui et al. (2008[Bejaoui, A., Horchani-Naifer, K. & Férid, M. (2008). Acta Cryst. E64, i48.]).

Experimental

Crystal data
  • Lu4(P4O12)3

  • Mr = 1647.52

  • Cubic, [I \overline 43d ]

  • a = 14.6920 (6) Å

  • V = 3171.3 (2) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 13.08 mm-1

  • T = 296 K

  • 0.18 × 0.10 × 0.08 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.534, Tmax = 0.746

  • 3088 measured reflections

  • 717 independent reflections

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

  • Rint = 0.034

Refinement
  • R[F2 > 2[sigma](F2)] = 0.020

  • wR(F2) = 0.038

  • S = 1.03

  • 717 reflections

  • 41 parameters

  • [Delta][rho]max = 0.90 e Å-3

  • [Delta][rho]min = -0.67 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 272 Friedel pairs

  • Flack parameter: 0.000 (15)

Table 1
Selected bond lengths (Å)

Lu-O3i 2.182 (3)
Lu-O3ii 2.182 (3)
Lu-O3 2.182 (3)
Lu-O2i 2.185 (4)
Lu-O2ii 2.185 (4)
Lu-O2 2.185 (4)
P-O2iii 1.464 (4)
P-O3 1.481 (4)
P-O1iv 1.583 (3)
P-O1 1.594 (3)
Symmetry codes: (i) [-z+1, x-{\script{1\over 2}}, -y+{\script{1\over 2}}]; (ii) [y+{\script{1\over 2}}, -z+{\script{1\over 2}}, -x+1]; (iii) [-z+1, -x+{\script{3\over 2}}, y]; (iv) [-y+{\script{5\over 4}}, x-{\script{3\over 4}}, -z+{\script{3\over 4}}].

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. 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: CaRine (Boudias & Monceau, 1998[Boudias, C. & Monceau, D. (1998). CaRine. CaRine Crystallography, DIVERGENT S.A., Compiègne, France.]) and ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2342 ).


References

Bagieu-Beucher, M. (1976). J. Appl. Cryst. 9, 368-369.  [CrossRef] [details] [ISI]
Bagieu-Beucher, M. & Guitel, J. C. (1978). Acta Cryst. B34, 1439-1442.  [CrossRef] [details] [ISI]
Bejaoui, A., Horchani-Naifer, K. & Férid, M. (2008). Acta Cryst. E64, i48.  [CrossRef] [details]
Boudias, C. & Monceau, D. (1998). CaRine. CaRine Crystallography, DIVERGENT S.A., Compiègne, France.
Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Chudinova, N. N. (1979). Izv. Akad. Nauk SSSR Neorg. Mater. 15, 833-837.  [ChemPort]
Durif, A. (1995). In Crystal Chemistry of Condensed Phosphates. New York and London: Plenum Press.
d'Yvoire, F. (1962). Bull. Soc. Chim. pp. 1237-1243.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  [CrossRef] [details]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Hendricks, S. B. & Wyckoff, R. W. G. (1927). Am. J. Sci. 13, 491-496.  [ChemPort]
Höppe, H. A. & Sedlmaier, S. J. (2007). Inorg. Chem. 46, 3467-3474.  [ISI] [PubMed]
Liebau, F. & Williams, H. P. (1964). Angew. Chem. 76, 303-304.  [CrossRef] [ChemPort]
Mezentseva, L. P., Domanskii, A. I. & Bondar, I. A. (1977). Russ. J. Inorg. Chem. 22, 43-45.
Pauling, L. & Sherman, J. S. (1937). Z. Kristallogr. 96, 481-487.  [ChemPort]
Rémy, P. & Boullé, A. (1964). C. R. Acad. Sci. 258, 927-929.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Smolin, Y. I., Shepelev, Y. F., Domanskii, A. I. & Belov, N. V. (1978). Kristallografiya, 23, 187-188.  [ChemPort]
Yuan, J. L., Zhang, H., Zhao, J. T., Chen, H. H., Yang, X. X. & Zhang, G. B. (2008). Opt. Mater. 30, 1369-1374.  [ISI] [CrossRef] [ChemPort]


Acta Cryst (2010). E66, i46  [ doi:10.1107/S1600536810016363 ]

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