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Volume 68 
Part 11 
Page m1341  
November 2012  

Received 16 July 2012
Accepted 23 September 2012
Online 10 October 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.005 Å
R = 0.031
wR = 0.071
Data-to-parameter ratio = 12.9
Details
Open access

Bis[4,4,5,5-tetramethyl-2-(pyridin-2-yl-[kappa]2N)imidazoline-1-oxyl 3-oxide-[kappa]O]tris(nitrato-[kappa]2O,O')terbium(III)

aChemical Institute, Linyi University, Linyi Shandong 276005, People's Republic of China
Correspondence e-mail: lidongjiao@lyu.edu.cn

The title compound, [Tb(NO3)3(C12H16N3O2)2], was prepared from the nitroxide radical ligand 4,4,5,5-tetramethyl-2-(pyridin-2-yl)-imidazoline-1-oxyl-3-oxide and TbIII nitrate. The TbIII ion adopts a doubly-capped square-antiprismatic coordination environment defined by three chelating nitrate anions and two N,O-bidentate nitronyl nitroxide radical ligands. Weak C-H...O hydrogen bonds connect the molecules into a three-dimensional framework. The title structure is isotypic with the Ho analogue [Li (2012[Li, D.-J. (2012). Acta Cryst. E68, m550.]). Acta Cryst. E68, 550].

Related literature

For background to the use of rare earth complexes with nitroxide radicals in coordination chemistry, see: Sutter et al. (1998[Sutter, J. P., Kahn, M. L. & Golhen, S. (1998). Chem. Eur. J. 4, 571-576.]); Kahn et al. (2000[Kahn, M. L., Sutter, J. P. & Golhen, S. (2000). J. Am. Chem. Soc. 122, 3413-3421.]); Lescop et al. (2000[Lescop, C., Luneau, D. & Bussière, G. (2000). Inorg. Chem. 39, 3740-3741.]). For the structures of related complexes, see: Li et al. (2004a[Li, D.-J., Liao, D.-Z. & Li, L.-C. (2004a). J. Coord. Chem. 57, 1571-1576.],b[Li, D.-J., Yan, S.-P. & Liao, D.-Z. (2004b). J. Mol. Struct. 698, 103-107.], 2005[Li, D.-J., Liao, D.-Z. & Li, L.-C. (2005). Chin. J. Struct. Chem. 24, 905-908.]); Li (2012[Li, D.-J. (2012). Acta Cryst. E68, m550.]).

[Scheme 1]

Experimental

Crystal data
  • [Tb(NO3)3(C12H16N3O2)2]

  • Mr = 813.51

  • Monoclinic, P 21 /n

  • a = 12.292 (3) Å

  • b = 11.114 (2) Å

  • c = 23.264 (5) Å

  • [beta] = 98.37 (3)°

  • V = 3144.6 (11) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 2.33 mm-1

  • T = 293 K

  • 0.20 × 0.20 × 0.20 mm

Data collection
  • Rigaku Saturn CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2004[Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.]) Tmin = 0.581, Tmax = 1.000

  • 25443 measured reflections

  • 5554 independent reflections

  • 4726 reflections with I > 2[sigma](I)

  • Rint = 0.059

Refinement
  • R[F2 > 2[sigma](F2)] = 0.031

  • wR(F2) = 0.071

  • S = 1.01

  • 5554 reflections

  • 432 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.89 e Å-3

  • [Delta][rho]min = -0.95 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C22-H22...O13i 0.93 2.55 3.440 (5) 161
C17-H17B...O6ii 0.96 2.40 3.327 (5) 161
C6-H6B...O3iii 0.96 2.55 3.473 (5) 161
C24-H24...O9iv 0.93 2.38 3.211 (5) 148
Symmetry codes: (i) [-x-{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (ii) -x, -y+1, -z; (iii) -x+1, -y+2, -z; (iv) [-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}].

Data collection: CrystalClear (Rigaku, 2008[Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; 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: MW2078 ).


Acknowledgements

The author thanks the Chemical Institute of Linyi University for supporting this work.

References

Kahn, M. L., Sutter, J. P. & Golhen, S. (2000). J. Am. Chem. Soc. 122, 3413-3421.  [ISI] [CrossRef] [ChemPort]
Lescop, C., Luneau, D. & Bussière, G. (2000). Inorg. Chem. 39, 3740-3741.  [ISI] [CrossRef] [PubMed] [ChemPort]
Li, D.-J. (2012). Acta Cryst. E68, m550.  [CSD] [CrossRef] [details]
Li, D.-J., Liao, D.-Z. & Li, L.-C. (2004a). J. Coord. Chem. 57, 1571-1576.  [ISI] [CSD] [CrossRef] [ChemPort]
Li, D.-J., Liao, D.-Z. & Li, L.-C. (2005). Chin. J. Struct. Chem. 24, 905-908.
Li, D.-J., Yan, S.-P. & Liao, D.-Z. (2004b). J. Mol. Struct. 698, 103-107.  [ISI] [CrossRef] [ChemPort]
Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Sutter, J. P., Kahn, M. L. & Golhen, S. (1998). Chem. Eur. J. 4, 571-576.  [CrossRef] [ChemPort]


Acta Cryst (2012). E68, m1341  [ doi:10.1107/S1600536812040287 ]

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