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Volume 69 
Part 6 
Page m346  
June 2013  

Received 21 May 2013
Accepted 22 May 2013
Online 31 May 2013

Key indicators
Single-crystal X-ray study
T = 150 K
Mean [sigma](C-C) = 0.003 Å
R = 0.031
wR = 0.079
Data-to-parameter ratio = 17.9
Details
Open access

{N,N-Bis[bis(2,2,2-trifluoroethoxy)phosphanyl]methylamine-[kappa]2P,P'}bis([eta]5-cyclopentadienyl)titanium(II)

aLeibniz-Institut für Katalyse e. V. an der Universität Rostock, Albert-Einstein-Strasse 29a, 18059 Rostock, Germany
Correspondence e-mail: torsten.beweries@catalysis.de

The title compound, [Ti(C5H5)2(C9H11F12NO4P2)], is a four-membered titanacycle obtained from the reaction of Cp2Ti([eta]2-Me3SiC2SiMe3) and CH3N[P(OCH2CF3)2]2 {N,N-bis[bis(trifluoroethoxy)phosphanyl]methylamine, tfepma}. The TiII atom is coordinated by two cyclopentadienyl (Cp) ligands and the chelating tfepma ligand in a strongly distorted tetrahedral geometry. The molecule is located on a mirror plane.

Related literature

For other titanocene complexes with four-membered metallacycles [TiPNP], see: Haehnel et al. (2012[Haehnel, M., Hansen, S., Spannenberg, A., Arndt, P., Beweries, T. & Rosenthal, U. (2012). Chem. Eur. J. 18, 10546-10553.]). For selected examples of four-membered metallacycles with a chelating tfepma ligand, see: M = Rh, Esswein et al. (2005[Esswein, A. J., Veige, A. S. & Nocera, D. G. (2005). J. Am. Chem. Soc. 127, 16641-16651.], 2007[Esswein, A. J., Dempsey, J. L. & Nocera, D. G. (2007). Inorg. Chem. 46, 2362-2364.]); M = Ir, Heyduk & Nocera (1999[Heyduk, A. F. & Nocera, D. G. (1999). Chem. Commun. pp. 1519-1520.], 2000[Heyduk, A. F. & Nocera, D. G. (2000). J. Am. Chem. Soc. 122, 9415-9426.]); Gray et al. (2004[Gray, T. G., Veige, A. S. & Nocera, D. G. (2004). J. Am. Chem. Soc. 126, 9760-9768.]); Veige et al. (2005[Veige, A. S., Gray, T. G. & Nocera, D. G. (2005). Inorg. Chem. 44, 17-26.]); Esswein et al. (2008[Esswein, A. J., Veige, A. S., Piccoli, P. M. B., Schultz, A. J. & Nocera, D. G. (2008). Organometallics, 27, 1073-1083.]). The starting alkyne complex Cp2Ti([eta]2-Me3SiC2SiMe3) is described by Burlakov et al. (1988[Burlakov, V. V., Rosenthal, U., Petrovskii, P. V., Shur, V. B. & Vol'pin, M. E. (1988). Organomet. Chem. USSR, 1, 526-528.]).

[Scheme 1]

Experimental

Crystal data
  • [Ti(C5H5)2(C9H11F12NO4P2)]

  • Mr = 665.21

  • Orthorhombic, P n m a

  • a = 14.6494 (2) Å

  • b = 20.0535 (3) Å

  • c = 8.7694 (1) Å

  • V = 2576.20 (6) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.57 mm-1

  • T = 150 K

  • 0.42 × 0.41 × 0.16 mm

Data collection
  • Bruker Kappa APEXII DUO diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.90, Tmax = 1.00

  • 60903 measured reflections

  • 3420 independent reflections

  • 2988 reflections with I > 2[sigma](I)

  • Rint = 0.033

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

  • wR(F2) = 0.079

  • S = 1.06

  • 3420 reflections

  • 191 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.51 e Å-3

  • [Delta][rho]min = -0.40 e Å-3

Data collection: APEX2 (Bruker, 2011[Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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: XP in 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: BT6910 ).


Acknowledgements

Financial support by the DFG (grant code RO 1269/8-1) and the BMBF (project "Light2Hydrogen") is gratefully acknowledged.

References

Bruker (2008). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2009). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Burlakov, V. V., Rosenthal, U., Petrovskii, P. V., Shur, V. B. & Vol'pin, M. E. (1988). Organomet. Chem. USSR, 1, 526-528.
Esswein, A. J., Dempsey, J. L. & Nocera, D. G. (2007). Inorg. Chem. 46, 2362-2364.  [CrossRef] [PubMed] [ChemPort]
Esswein, A. J., Veige, A. S. & Nocera, D. G. (2005). J. Am. Chem. Soc. 127, 16641-16651.  [CrossRef] [PubMed] [ChemPort]
Esswein, A. J., Veige, A. S., Piccoli, P. M. B., Schultz, A. J. & Nocera, D. G. (2008). Organometallics, 27, 1073-1083.  [CrossRef] [ChemPort]
Gray, T. G., Veige, A. S. & Nocera, D. G. (2004). J. Am. Chem. Soc. 126, 9760-9768.  [CrossRef] [PubMed] [ChemPort]
Haehnel, M., Hansen, S., Spannenberg, A., Arndt, P., Beweries, T. & Rosenthal, U. (2012). Chem. Eur. J. 18, 10546-10553.  [CrossRef] [ChemPort] [PubMed]
Heyduk, A. F. & Nocera, D. G. (1999). Chem. Commun. pp. 1519-1520.  [CrossRef]
Heyduk, A. F. & Nocera, D. G. (2000). J. Am. Chem. Soc. 122, 9415-9426.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]
Veige, A. S., Gray, T. G. & Nocera, D. G. (2005). Inorg. Chem. 44, 17-26.  [CrossRef] [PubMed] [ChemPort]


Acta Cryst (2013). E69, m346  [ doi:10.1107/S1600536813014244 ]

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