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Volume 69 
Part 5 
Pages m234-m235  
May 2013  

Received 17 March 2013
Accepted 23 March 2013
Online 5 April 2013

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.003 Å
Disorder in main residue
R = 0.017
wR = 0.040
Data-to-parameter ratio = 24.7
Details
Open access

(Butane-1,4-diyl)(trimethylphosphane-[kappa]P)[tris(3,5-dimethylpyrazol-1-yl-[kappa]N2)hydroborato]iridium(III)

aInstituto de Investigaciones Químicas (IIQ) and Departamento de Química Inorgánica, Consejo Superior de Investigaciones Cientificas (CSIC) and Universidad de Sevilla, Avenida Américo Vespucio 49, 41092 Sevilla, Spain, and bInstitute of Chemical Technologies and Analytics, Vienna University of Technology, Getreidemarkt 9/164SC, A-1060 Vienna, Austria
Correspondence e-mail: kurt.mereiter@tuwien.ac.at

In the mononuclear title iridium(III) complex, [Ir(C4H8)(C15H22BN6)(C3H9P)], which is based on the [tris(3,5-dimethylpyrazol-1-yl)hydroborato]iridium moiety, Ir[TpMe2], the IrIII atom is coordinated by a chelating butane-1,4-diyl fragment and a trimethylphosphane ligand in a modestly distorted octahedral coordination environment formed by three facial N, two C and one P atom. The iridium-butane-1,4-diyl ring has an envelope conformation. This ring is disordered because alternately the second or the third C atom of the butane-1,4-diyl fragment function as an envelope flap atom (the occupancy ratio is 1:1). In the crystal, molecules are organized into densely packed columns extending along [101]. Coherence between the molecules is essentially based on van der Waals interactions.

Related literature

For general aspects of hydrogen trispyrazolylborate ligands, see: Pettinari & Trofimenko (2008[Pettinari, C. & Trofimenko, S. (2008). In Scorpionates II: Chelating Borate Ligands. London: Imperial College Press.]). For general information on mechanistic aspects of organometallic reactions, involving oxidative addition and reductive elimination, see: Crabtree (2005[Crabtree, R. H. (2005). The Organometallic Chemistry of the Transition Metals, 4th ed. New Jersey: John Wiley and Sons Inc.]). For information on [sigma]-CAM mechanisms, see: Perutz & Sabo-Etienne (2007[Perutz, R. N. & Sabo-Etienne, S. (2007). Angew. Chem. Int. Ed. 46, 2578-2592.]). For general information on the chemistry and potential of Ir[TpMe2] complexes, see: Conejero et al. (2010[Conejero, S., Paneque, M., Poveda, M. L., Santos, L. L. & Carmona, E. (2010). Acc. Chem. Res. 43, 572-580.]). For selected aspects of the synthesis and the crystal structure of the precursor of the title compound, see: Paneque et al. (2000[Paneque, M., Poveda, M. L., Salazar, V., Gutiérrez-Puebla, E. & Monge, A. (2000). Organometallics, 19, 3120-3126.]). For aspects of the chemistry of a CO- instead of PMe3-containing analogue to the precursor of the title compound, see: Gómez et al. (2007[Gómez, M., Paneque, M., Poveda, M. L. & Alvarez, E. (2007). J. Am. Chem. Soc. 129, 6092-6093.]). For a description of the Cambridge Structural Database, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]).

[Scheme 1]

Experimental

Crystal data
  • [Ir(C4H8)(C15H22BN6)(C3H9P)]

  • Mr = 621.57

  • Monoclinic, P 21 /n

  • a = 11.1865 (5) Å

  • b = 18.1771 (8) Å

  • c = 13.4748 (6) Å

  • [beta] = 112.883 (1)°

  • V = 2524.3 (2) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 5.37 mm-1

  • T = 173 K

  • 0.22 × 0.15 × 0.14 mm

Data collection
  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2003[Bruker (2003). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.36, Tmax = 0.47

  • 37102 measured reflections

  • 7359 independent reflections

  • 6892 reflections with I > 2[sigma](I)

  • Rint = 0.018

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

  • wR(F2) = 0.040

  • S = 1.08

  • 7359 reflections

  • 298 parameters

  • 25 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.86 e Å-3

  • [Delta][rho]min = -0.32 e Å-3

Table 1
Selected bond lengths (Å)

Ir1-C19A 2.0780 (18)
Ir1-C16A 2.0871 (19)
Ir1-N5 2.1781 (14)
Ir1-N3 2.2233 (15)
Ir1-P1 2.2381 (5)
Ir1-N1 2.2590 (15)

Data collection: SMART (Bruker, 2003[Bruker (2003). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2003[Bruker (2003). SMART, SAINT and SADABS. 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: Mercury (Macrae et al., 2006[Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: GK2565 ).


Acknowledgements

Financial support (FEDER) from the Spanish Ministry of Science (projects CTQ2010-17476 and Consolider-Ingenio 2010 CSD2007-00006) and the Junta de Andalucía (grant FQM-119 and project P09-FQM-4832) is acknowledged.

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.  [ISI] [CrossRef] [details]
Bruker (2003). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Conejero, S., Paneque, M., Poveda, M. L., Santos, L. L. & Carmona, E. (2010). Acc. Chem. Res. 43, 572-580.  [ISI] [CrossRef] [ChemPort] [PubMed]
Crabtree, R. H. (2005). The Organometallic Chemistry of the Transition Metals, 4th ed. New Jersey: John Wiley and Sons Inc.
Gómez, M., Paneque, M., Poveda, M. L. & Alvarez, E. (2007). J. Am. Chem. Soc. 129, 6092-6093.  [ISI] [PubMed]
Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457.  [ISI] [CrossRef] [ChemPort] [details]
Paneque, M., Poveda, M. L., Salazar, V., Gutiérrez-Puebla, E. & Monge, A. (2000). Organometallics, 19, 3120-3126.  [CrossRef] [ChemPort]
Perutz, R. N. & Sabo-Etienne, S. (2007). Angew. Chem. Int. Ed. 46, 2578-2592.  [ISI] [CrossRef] [ChemPort]
Pettinari, C. & Trofimenko, S. (2008). In Scorpionates II: Chelating Borate Ligands. London: Imperial College Press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]


Acta Cryst (2013). E69, m234-m235   [ doi:10.1107/S1600536813008040 ]

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