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Volume 67 
Part 4 
Page m487  
April 2011  

Received 14 March 2011
Accepted 15 March 2011
Online 26 March 2011

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Key indicators
Single-crystal X-ray study
T = 150 K
Mean [sigma](C-C) = 0.014 Å
R = 0.037
wR = 0.089
Data-to-parameter ratio = 19.2
Details
Open access

Tris(tetrabutylammonium) tris(nitrato-[kappa]2O,O')tetrakis(thiocyanato-[kappa]N)thorium(IV)

M. Janeth Lozano-Rodriguez,a,b Pierre Thuéry,c Sébastien Petit,a Roy Copping,a Jose Mustre de Leonb and Christophe Den Auwera*

aCEA, Nuclear Energy Division, Radio Chemistry and Processes Department, F-30207 Bagnols sur Cèze, France,bDepartamento de Fisica Aplicada, Cinvestav-Merida, Merida, Yuc. 97310, Mexico, and cCEA, IRAMIS, UMR 3299 CEA/CNRS, SIS2M, LCCEf, Bat. 125, F-91191 Gif-sur-Yvette, France
Correspondence e-mail: christophe.denauwer@cea.fr

The title compound, (C16H36N)3[Th(NCS)4(NO3)3], was obtained from the reaction of Th(NO3)4·5H2O with (Bu4N)(NCS). The ThIV atom is in a ten-coordinate environment of irregular geometry, being bound to the N atoms of the four thiocyanate ions and to three bidentate nitrate ions. The average Th-N and Th-O bond lengths are 2.481 (10) and 2.57 (3) Å, respectively.

Related literature

For the structures of the parent lanthanide complexes, see: Mullica et al. (1997[Mullica, D., Farmer, J. M. & Sappenfield, E. L. (1997). Inorg. Chim. Acta, 256, 115-119.], 1998[Mullica, D., Farmer, J. M. & Kautz, J. A. (1998). Inorg. Chem. Commun. 1, 217-221.]); Farmer et al. (2000[Farmer, J. M., Kautz, J. A., Kwon, H. S. & Mullica, D. F. (2000). J. Chem. Crystallogr. 30, 301-309.]). For the structures of related actinide thiocyanate complexes, see: Countryman & McDonald (1971[Countryman, R. & McDonald, W. S. (1971). J. Inorg. Nucl. Chem. 33, 2213-2220.]); Al-Kazzaz et al. (1972[Al-Kazzaz, Z. M. S., Bagnall, K. W., Brown, D. & Whittaker, B. (1972). J. Chem. Soc. Dalton Trans. pp. 2273-2277.]); Charpin et al. (1983[Charpin, P., Lance, M. & Navaza, A. (1983). Acta Cryst. C39, 190-192.]); Budantseva et al. (2003[Budantseva, N. A., Andreev, G. B., Fedoseev, A. M. & Antipin, M. Y. (2003). Radiochemistry, 45, 335-338.]). For a description of the Cambridge Structural Database, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]).

[Scheme 1]

Experimental

Crystal data

  • (C16H36N)3[Th(NCS)4(NO3)3]

  • Mr = 1377.76

  • Monoclinic, P 21

  • a = 12.1057 (7) Å

  • b = 17.5943 (8) Å

  • c = 16.7084 (8) Å

  • [beta] = 95.946 (3)°

  • V = 3539.6 (3) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 2.28 mm-1

  • T = 150 K

  • 0.12 × 0.12 × 0.07 mm
Data collection

  • Nonius KappaCCD area-detector diffractometer

  • Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]) Tmin = 0.703, Tmax = 0.853

  • 170199 measured reflections

  • 13392 independent reflections

  • 11074 reflections with I > 2[sigma](I)

  • Rint = 0.046
Refinement

  • R[F2 > 2[sigma](F2)] = 0.037

  • wR(F2) = 0.089

  • S = 1.04

  • 13392 reflections

  • 698 parameters

  • 6 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.98 e Å-3

  • [Delta][rho]min = -0.76 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 6435 Friedel pairs

  • Flack parameter: -0.008 (5)

Table 1
Selected geometric parameters (Å, °)

Th-N1 2.480 (5)
Th-N2 2.465 (7)
Th-N3 2.488 (5)
Th-N4 2.490 (7)
Th-O1 2.618 (5)
Th-O2 2.563 (4)
Th-O4 2.557 (4)
Th-O5 2.570 (4)
Th-O7 2.615 (6)
Th-O8 2.524 (5)
O1-Th-O2 49.51 (14)
O4-Th-O5 49.30 (13)
O7-Th-O8 49.44 (15)

Data collection: COLLECT (Nonius, 1998[Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: HKL-2000 (Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]); data reduction: HKL-2000; 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.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2728 ).

Acknowledgements

Financial support by the CEA Basic Research Program (RBPCH), Groupement National de Recherche PARIS and the International Research Staff Exchange Scheme of the European Community (HEXANE) is acknowledged.

References

Al-Kazzaz, Z. M. S., Bagnall, K. W., Brown, D. & Whittaker, B. (1972). J. Chem. Soc. Dalton Trans. pp. 2273-2277.
Allen, F. H. (2002). Acta Cryst. B58, 380-388.  [ISI] [CrossRef] [details]
Budantseva, N. A., Andreev, G. B., Fedoseev, A. M. & Antipin, M. Y. (2003). Radiochemistry, 45, 335-338.  [ChemPort]
Charpin, P., Lance, M. & Navaza, A. (1983). Acta Cryst. C39, 190-192.  [CrossRef] [details]
Countryman, R. & McDonald, W. S. (1971). J. Inorg. Nucl. Chem. 33, 2213-2220.  [ChemPort]
Farmer, J. M., Kautz, J. A., Kwon, H. S. & Mullica, D. F. (2000). J. Chem. Crystallogr. 30, 301-309.  [ISI] [CSD] [CrossRef] [ChemPort]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Mullica, D., Farmer, J. M. & Kautz, J. A. (1998). Inorg. Chem. Commun. 1, 217-221.  [ChemPort]
Mullica, D., Farmer, J. M. & Sappenfield, E. L. (1997). Inorg. Chim. Acta, 256, 115-119.  [ChemPort]
Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]

Acta Cryst (2011). E67, m487  [ doi:10.1107/S1600536811009792 ]

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