Bis[1-(3,5-di-tert-butyl-2-hydroxy­benz­yl)-3-isopropyl­imidazolium] penta­chlorido(tetra­hydro­furan)samarate(III)–tetrahydrofuran–toluene (1/1/1)

Wang, Z.; Liu, S.; Bian, Q.

doi:10.1107/S1600536810017678

Volume 66
Part 6
Page m683
June 2010

Received 2 December 2009
Accepted 13 May 2010
Online 22 May 2010

Key indicators
Single-crystal X-ray study
T = 192 K
Mean (C-C) = 0.006 Å
R = 0.035
wR = 0.099
Data-to-parameter ratio = 21.2
Details

Bis[1-(3,5-di-tert-butyl-2-hydroxybenzyl)-3-isopropylimidazolium] pentachlorido(tetrahydrofuran)samarate(III)-tetrahydrofuran-toluene (1/1/1)

Zhiguo Wang,^a ^* Siman Liu ^a and Qinquan Bian ^a

^aDepartment of Chemistry and Chemical Engineering, Mianyang Normal University, Mianyang 621000, People's Republic of China
Correspondence e-mail: wangzhiguo224865@163.com

The title compound, (C₂₁H₃₃N₂O)₂[SmCl₅(C₄H₈O)]·C₇H₈·C₄H₈O, has a layered structure in which each distorted octahedral [SmCl₅(THF)]^2- unit (THF is tetrahydrofuran) is capped by two cations. The central metal Sm^III atom of the [SmCl₅(THF)]^2- anionic unit is coordinated by five Cl atoms and one THF O atom, forming a distorted octahedral geometry. The crystal structure displays C-HCl and O-HCl hydrogen bonding. The structure exhibits disorder of the solvent.

Related literature

For general background to the use of anionic functionalized N-heterocyclic carbenes (NHCs) as anionic tethers in the field of rare earth metals, see: Arnold & Casely (2009); Arnold & Liddle (2005, 2006); Babai & Mudring (2005); Liddle et al. (2007). For related structures, see: Lu et al. (2001); Wang et al. (2006a,b); Yao et al. (2004, 2007); Li et al. (2005).

Experimental

Crystal data

(C₂₁H₃₃N₂O)₂[SmCl₅(C₄H₈O)]·C₇H₈·C₄H₈O
M_r = 1222.93
Triclinic, $[P \overline 1]$
a = 10.2252 (11) Å
b = 17.6968 (18) Å
c = 18.3806 (19) Å
= 76.954 (5)°
= 86.077 (6)°
= 82.789 (6)°
V = 3211.8 (6) Å³
Z = 2
Mo K radiation
= 1.16 mm^-1
T = 192 K
0.34 × 0.25 × 0.15 mm

Data collection

Rigaku Mercury diffractometer
Absorption correction: multi-scan (REQAB; Jacobson, 1998) T_min = 0.695, T_max = 0.846
32162 measured reflections
11687 independent reflections
10327 reflections with I > 2(I)
R_int = 0.031

Refinement

R[F² > 2(F²)] = 0.035
wR(F²) = 0.099
S = 1.09
11687 reflections
550 parameters
54 restraints
H-atom parameters constrained
_max = 1.03 e Å^-3
_min = -0.52 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O1-H1Cl1	0.84	2.30	3.143 (3)	178
O2-H2Cl3	0.84	2.30	3.136 (3)	174
C29-H29Cl5ⁱ	0.95	2.54	3.486 (3)	173
C10-H10Cl1ⁱⁱ	0.95	2.81	3.681 (4)	153
C9-H9Cl2ⁱⁱⁱ	0.95	2.64	3.476 (4)	146
C8-H8Cl5	0.95	2.73	3.655 (4)	164
C5-H5Cl2ⁱⁱⁱ	0.95	2.84	3.736 (3)	158
Symmetry codes: (i) -x, -y+1, -z+1; (ii) x+1, y, z; (iii) -x+1, -y+1, -z.

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: VM2015 ).

Acknowledgements

The authors thank the Sichuan Province Youth Foundation of Science and Technology (09 J J0088) for financial support.

References

Arnold, P. L. & Casely, I. J. (2009). Chem. Rev. 109, 3599-3611.
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Arnold, P. L. & Liddle, S. T. (2006). Chem. Commun. pp. 3959-3971.
Babai, A. & Mudring, A. V. (2005). Inorg. Chem. 44, 8168-8169.
Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.
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metal-organic compounds