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Volume 69 
Part 10 
Page m566  
October 2013  

Received 20 September 2013
Accepted 22 September 2013
Online 28 September 2013

Key indicators
Single-crystal X-ray study
T = 193 K
Mean [sigma](C-C) = 0.004 Å
R = 0.017
wR = 0.042
Data-to-parameter ratio = 17.1
Details
Open access

Azido([eta]5-pentamethylcyclopentadienyl)[2-(pyridin-2-yl)phenyl]iridium(III)

aDepartment of Chemistry, Faculty of Science, Okayama University, Tsushimanaka 3-1-1, Okayama, 700-8530, Japan
Correspondence e-mail: suzuki@okayama-u.ac.jp

In the title compound, [Ir(C10H15)(C11H8N)(N3)], the IrIII ion is coordinated by three anionic ligands, namely, pentamethylcyclopentadienyl (Cp*-), 2-(pyridin-2-yl)phenyl (ppy-) and azide (N3-), and adopts a three-legged piano-stool geometry The coordination mode of N3- is typical for Cp*IrIII-N3 complexes, with an Ir-N(N3) bond length of 2.125 (2) Å and an Ir-N=N bond angle of 116.5 (2)°. The N3- ligand is almost linear [N=N=N = 176.0 (3)°], and the N=N bond length between the central and coordinating N atom and that between the central and non-coordinating terminal N atom are 1.194 (3) and 1.157 (3) Å, respectively. For the ppy- ligand, the Ir-C and Ir-N bond lengths are 2.066 (3) and 2.079 (3) Å, respectively, which are rather close to each other, compared to the related IrIII- or RhIII-ppy complexes. The Ir-C(Cp*) bond lengths vary in the range 2.163 (2)-2.232 (2) Å, indicating a strong trans influence of the cyclometallated C-donor atom of the ppy- ligand.

Related literature

For crystallographic analyses of [Cp*IrIII(N3)(L-L')] (L-L' = bidentate chelate ligands; e.g., bpy, 2-Spy, etc.) complexes, see: Suzuki et al. (2009[Suzuki, T., Kotera, M., Takayama, A. & Kojima, M. (2009). Polyhedron, 28, 2287-2293.]); Suzuki (2005[Suzuki, T. (2005). Acta Cryst. E61, m488-m490.]). For crystallographic analyses of mononuclear [Cp*Ir(ppy)X] complexes (X = Cl, I, MeCN4, etc.), see: Boutadla et al. (2009[Boutadla, Y., Al-Duaij, O., Davies, D. L., Griffith, G. A. & Singh, K. (2009). Organometallics, 28, 433-440.]); Park-Gehrke et al. (2009[Park-Gehrke, L. S., Freudenthal, J., Kaminsky, W., DiPasquale, A. G. & Mayer, J. M. (2009). Dalton Trans. pp. 1972-1983.]); Takayama et al. (2013[Takayama, A., Suzuki, T., Ikeda, M., Sunatsuki, Y. & Kojima, M. (2013). Dalton Trans. 42, 14556-14567.]). For photochemistry of [Cp*IrIII(N3)(L-L')] complexes, see: Sekioka et al. (2005[Sekioka, Y., Kaizaki, S., Mayer, J. M. & Suzuki, T. (2005). Inorg. Chem. 44, 8173-8175.]); Kotera et al. (2008[Kotera, M., Sekioka, Y. & Suzuki, T. (2008). Inorg. Chem. 47, 3498-3508.]).

[Scheme 1]

Experimental

Crystal data
  • [Ir(C10H15)(C11H8N)(N3)]

  • Mr = 523.63

  • Monoclinic, P 21 /n

  • a = 15.4821 (18) Å

  • b = 7.3938 (9) Å

  • c = 15.7137 (18) Å

  • [beta] = 91.477 (4)°

  • V = 1798.2 (4) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 7.44 mm-1

  • T = 193 K

  • 0.30 × 0.30 × 0.20 mm

Data collection
  • Rigaku R-AXIS RAPIDII diffractometer

  • Absorption correction: numerical (NUMABS; Rigaku, 1999[Rigaku (1999). NUMABS. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.103, Tmax = 0.225

  • 27640 measured reflections

  • 4115 independent reflections

  • 4022 reflections with I > 2[sigma](I)

  • Rint = 0.045

Refinement
  • R[F2 > 2[sigma](F2)] = 0.017

  • wR(F2) = 0.042

  • S = 1.13

  • 4115 reflections

  • 240 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.61 e Å-3

  • [Delta][rho]min = -0.65 e Å-3

Data collection: RAPID-AUTO (Rigaku, 2006[Rigaku (2006). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.]); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: DIRDIF99-PATTY (Beurskens et al., 1999[Beurskens, P. T., Beurskens, G., de Gelder, R., García-Granda, S., Israel, R., Gould, R. O. & Smits, J. M. M. (1999). The DIRDIF99 Program System. Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands.]); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: SHELXL2013.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IS5306 ).


Acknowledgements

This work was partly supported by JSPS KAKENHI grant No. 25410070.

References

Beurskens, P. T., Beurskens, G., de Gelder, R., García-Granda, S., Israel, R., Gould, R. O. & Smits, J. M. M. (1999). The DIRDIF99 Program System. Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands.
Boutadla, Y., Al-Duaij, O., Davies, D. L., Griffith, G. A. & Singh, K. (2009). Organometallics, 28, 433-440.  [CSD] [CrossRef] [ChemPort]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Kotera, M., Sekioka, Y. & Suzuki, T. (2008). Inorg. Chem. 47, 3498-3508.  [Web of Science] [CrossRef] [PubMed] [ChemPort]
Park-Gehrke, L. S., Freudenthal, J., Kaminsky, W., DiPasquale, A. G. & Mayer, J. M. (2009). Dalton Trans. pp. 1972-1983.
Rigaku (1999). NUMABS. Rigaku Corporation, Tokyo, Japan.
Rigaku (2006). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
Sekioka, Y., Kaizaki, S., Mayer, J. M. & Suzuki, T. (2005). Inorg. Chem. 44, 8173-8175.  [Web of Science] [CSD] [CrossRef] [PubMed] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Suzuki, T. (2005). Acta Cryst. E61, m488-m490.  [CrossRef] [IUCr Journals]
Suzuki, T., Kotera, M., Takayama, A. & Kojima, M. (2009). Polyhedron, 28, 2287-2293.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Takayama, A., Suzuki, T., Ikeda, M., Sunatsuki, Y. & Kojima, M. (2013). Dalton Trans. 42, 14556-14567.  [CSD] [CrossRef] [ChemPort] [PubMed]


Acta Cryst (2013). E69, m566  [ doi:10.1107/S1600536813026159 ]

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