Tris(thio­cyanato-κN)tris­(triphenyl­phosphine oxide-κO)terbium(III)

Pham, L.N.; Thames, A.T.; White, F.D.; Xiang, K.R.; Sykora, R.E.

doi:10.1107/S1600536812047289

Volume 68
Part 12
Page m1531
December 2012

Received 8 November 2012
Accepted 16 November 2012
Online 24 November 2012

Key indicators
Single-crystal X-ray study
T = 180 K
Mean (C-C) = 0.006 Å
R = 0.026
wR = 0.056
Data-to-parameter ratio = 15.5
Details

Tris(thiocyanato-N)tris(triphenylphosphine oxide-O)terbium(III)

Lam N. Pham,^a Anthony T. Thames,^a Frankie D. White,^a Kang Rui Xiang ^a and Richard E. Sykora ^a ^*

^aDepartment of Chemistry, University of South Alabama, Mobile, AL 36688, USA
Correspondence e-mail: rsykora@southalabama.edu

The title compound, [Tb(NCS)₃(C₁₈H₁₅OP)₃], contains a six-coordinate Tb^II cation surrounded by three O-bound triphenylphosphine oxide ligands and three N-bound thiocyanate ligands, each in a fac arrangement. There are two crystallographically unique Tb^III atoms in the asymmetric unit. One Tb^III atom resides on a threefold rotation axis, while the other has no imposed crystallographic symmetry. The thiocyanate ligands are bound through N atoms, illustrating the hard-hard bonding principles of metal complex chemistry.

Related literature

For information on structures of related lanthanide phosphine oxide complexes, see: Bowden et al. (2012); Feazell et al. (2004). For the synthesis and characterization of lanthanide triphenylphosphine oxides with nitrate and thiocyanate anions, see: Cousins & Hart (1967, 1968). For more information on the sizes of lanthanide ions, see: Brown & Altermatt (1985).

Experimental

Crystal data

[Tb(NCS)₃(C₁₈H₁₅OP)₃]
M_r = 1168.01
Trigonal, R 3
a = 38.6774 (5) Å
c = 12.3956 (2) Å
V = 16058.8 (4) Å³
Z = 12
Mo K radiation
= 1.57 mm^-1
T = 180 K
0.17 × 0.12 × 0.05 mm

Data collection

Agilent Xcalibur Eos CCD diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012) T_min = 0.913, T_max = 1.000
79947 measured reflections
13045 independent reflections
11605 reflections with I > 2(I)
R_int = 0.034

Refinement

R[F² > 2(F²)] = 0.026
wR(F²) = 0.056
S = 1.06
13045 reflections
841 parameters
1 restraint
H-atom parameters constrained
_max = 0.46 e Å^-3
_min = -0.51 e Å^-3
Absolute structure: Flack (1983), 6522 Friedel pairs
Flack parameter: -0.028 (4)

Table 1
Selected bond lengths (Å)

Tb1-O1	2.265 (3)
Tb1-O2	2.246 (3)
Tb1-O3	2.243 (3)
Tb1-N1	2.350 (4)
Tb1-N2	2.359 (4)
Tb1-N3	2.356 (4)
Tb2-N4	2.355 (4)
Tb2-O4	2.267 (3)

Data collection: CrysAlis PRO (Agilent, 2012); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: publCIF (Westrip, 2010).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2605 ).

Acknowledgements

The authors acknowledge the National Science Foundation for its generous support (NSF Career grant to RES, No. CHE-0846680).

References

Agilent (2012). CrysAlis PRO. Agilent Technologies, Yarnton, Oxfordshire, England.
Bowden, A., Singh, K. & Platt, A. (2012). Polyhedron, 42, 30-35.
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.
Cousins, D. R. & Hart, F. A. (1967). J. Inorg. Nucl. Chem. 29, 1745-1757.
Cousins, D. R. & Hart, F. A. (1968). J. Inorg. Nucl. Chem. 30, 3009-3015.
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.
Feazell, R. P., Gary, J. B., Kautz, J. A., Klausmeyer, K. K., Wong, C. W. & Zancanella, M. (2004). Acta Cryst. E60, m532-m534.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.

metal-organic compounds