{2-[(η5-Cyclo­penta­dien­yl)diphenyl­meth­yl]-1H-imidazolido-κN}bis­(N,N-diethyl­amido)­titanium(IV)

Cai, X.; Xu, Y.; Nie, W.; Borzov, M.V.

doi:10.1107/S1600536811012396

Volume 67
Part 5
Pages m549-m550
May 2011

Received 23 March 2011
Accepted 3 April 2011
Online 7 April 2011

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.005 Å
R = 0.040
wR = 0.102
Data-to-parameter ratio = 15.8
Details

{2-[(⁵-Cyclopentadienyl)diphenylmethyl]-1H-imidazolido-N}bis(N,N-diethylamido)titanium(IV)

Xianfeng Cai,^a ⁺ Yingying Xu,^a Wanli Nie ^a ^* and Maxim V. Borzov ^a

^aKey Laboratory of Synthetic and Natural Chemistry of the Ministry of Education, College of Chemistry and Material Science, The North-West University of Xi'an, Taibai Bei Avenue 229, Xi'an 710069, Shaanxi Province, People's Republic of China
Correspondence e-mail: niewl126@126.com

The chemically achiral title molecule, [Ti(C₄H₁₀N)₂(C₂₁H₁₆N₂)], crystallizes in the chiral space group P2₁. All three N atoms coordinating to the Ti^IV atom adopt planar environments [sums of valence angles = 359.5 (6), 360.0 (7) and 360.0 (6)°], which is indicative of p [pi] -d [pi] donation from all of these N atoms to the metal and, thus, of the formal 18 e^- nature of the complex. The overall coordination about the Ti^IV atom is distorted tetrahedral, assuming the cyclopentadienyl ring occupies one coordination site. The Ti-N_imidazole amide-type bond is longer by approximately 0.16 Å than the other two Ti-N_amide bonds.

Related literature

For structural parameters of [eta] ⁵-CpTi-tris(sec-amido)-type complexes, see: Rhodes et al. (2002); Li et al. (2003); Seo et al. (2001); Kunz et al. (2001, 2002); Carpenetti et al. (1996); Bertolasi et al. (2007); Wu et al. (2006); Cano et al. (2005); Martin et al. (1994). For two related Ti^IV complexes, see: Wang et al. (2009). For the structural parameters of 1H-imidazol(in)-2-yl side-chain functionalized cyclopentadienes and their Li, Ti, and Zr complexes, see: Krut'ko et al. (2006); Nie et al. (2008); Sun et al. (2009, 2010); Ge et al. (2010). For synthetic details, see: Curtis & Brown (1980); Bürger & Dämmen (1974); Bradley & Thomas (1960); Chajara & Ottosson (2004); Armarego & Perrin (1997). For a description of the Cambridge Structural Database, see: Allen (2002).

Experimental

Crystal data

[Ti(C₄H₁₀N)₂(C₂₁H₁₆N₂)]
M_r = 488.52
Monoclinic, P 2₁
a = 8.6495 (6) Å
b = 17.9486 (12) Å
c = 9.1130 (6) Å
= 110.603 (1)°
V = 1324.27 (15) Å³
Z = 2
Mo K radiation
= 0.35 mm^-1
T = 296 K
0.35 × 0.23 × 0.08 mm

Data collection

Bruker SMART APEXII diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.888, T_max = 0.973
7145 measured reflections
4906 independent reflections
4031 reflections with I > 2(I)
R_int = 0.022

Refinement

R[F² > 2(F²)] = 0.040
wR(F²) = 0.102
S = 0.99
4906 reflections
311 parameters
1 restraint
H-atom parameters constrained
_max = 0.21 e Å^-3
_min = -0.21 e Å^-3
Absolute structure: Flack (1983), 2209 Friedel pairs
Flack parameter: 0.02 (3)

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; 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: SHELXTL (Sheldrick, 2008) and OLEX2.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2469 ).

Acknowledgements

Financial support from the National Natural Science Foundation of China (project Nos. 20702041 and 21072157) and the Shaanxi Province Administration of Foreign Experts Bureau Foundation (grant No. 20106100079) is gratefully acknowledged. The authors are grateful to Mr Wang Minchang and Mr Su Pengfei (Xi'an Modern Chemistry Research Institute) for their help in carrying out the NMR spectroscopy and X-ray diffraction experiments.

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