[Journal logo]

Volume 69 
Part 2 
Page m72  
February 2013  

Received 4 December 2012
Accepted 18 December 2012
Online 4 January 2013

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.007 Å
R = 0.073
wR = 0.188
Data-to-parameter ratio = 18.4
Details
Open access

Bis(diethylamido-[kappa]N)(diethylamine-[kappa]N)bis(2,6-diisopropylphenylamido-[kappa]N)zirconium(IV)

aChemical Faculty, Gdansk University of Technology, Gabriela Narutowicza Street 11/12, 80-233 Gdansk, Poland
Correspondence e-mail: lukasz.ponikiewski@pg.gda.pl

In the title compound, [Zr(C12H18N)2(C4H10N)2(C4H11N)] or [Zr(HNC6H3iPr2)2(NEt2)2(HNEt2)], which was obtained by the reaction of Zr(NEt)4 with iPr2C6H3NH2, the ZrIV atom is in a trigonal-bipiramidal geometry in which the N atoms from two iPr2C6H3NH and one NEt2 ligand occupy the equatorial positions, and the N atoms of an NEt2 and an Et2NH ligand occupy the apical positions. An intramolecular N-H...N contact occurs. There are two independent molecules in the asymmetric unit.

Related literature

For related zirconium(IV) structures, see: Profilet et al. (1990[Profilet, R. D., Zabrano, C. H., Fanwick, P. E., Nash, J. J. & Rothwell, I. P. (1990). Inorg. Chem. 29, 4362-4364.]); Blake et al. (1997[Blake, A. J., Nikonov, G. I. & Mountford, P. (1997). Acta Cryst. C53, 874-876.]); Porter & Danopoulos (2004[Porter, R. M. & Danopoulos, A. A. (2004). Dalton Trans. pp. 2556-2562.]); Ghesner et al. (2006[Ghesner, I., Fenwick, A. & Stephen, D. W. (2006). Organometallics, 25, 4985-4995.]). For related syntheses, see: Kempe (2000[Kempe, R. (2000). Angew. Chem. Int. Ed. 39, 468-493.]).

[Scheme 1]

Experimental

Crystal data
  • [Zr(C12H18N)2(C4H10N)2(C4H11N)]

  • Mr = 661.17

  • Triclinic, [P \overline 1]

  • a = 11.2079 (3) Å

  • b = 13.1612 (5) Å

  • c = 14.3443 (6) Å

  • [alpha] = 86.578 (3)°

  • [beta] = 70.484 (3)°

  • [gamma] = 71.232 (3)°

  • V = 1885.61 (12) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.32 mm-1

  • T = 293 K

  • 0.58 × 0.39 × 0.34 mm

Data collection
  • Agilent Xcalibur (Sapphire2 diffractometer

  • Absorption correction: analytical (CrysAlis PRO; Agilent, 2010[Agilent (2010). CrysAlis PRO. Agilent Technologies, Yarnton, England.]) Tmin = 0.889, Tmax = 0.928

  • 11493 measured reflections

  • 7412 independent reflections

  • 5867 reflections with I > 2[sigma](I)

  • Rint = 0.035

Refinement
  • R[F2 > 2[sigma](F2)] = 0.073

  • wR(F2) = 0.188

  • S = 1.12

  • 7412 reflections

  • 402 parameters

  • 1 restraint

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

  • [Delta][rho]max = 1.82 e Å-3

  • [Delta][rho]min = -2.13 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N3-H3A...N1 0.84 (5) 2.56 (5) 2.983 (5) 112 (4)

Data collection: CrysAlis PRO (Agilent, 2010[Agilent (2010). CrysAlis PRO. Agilent Technologies, Yarnton, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SUPERFLIP (Palatinus & Chapuis, 2007[Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.]); program(s) used to refine structure: SHELXL97 (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: WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG5310 ).


References

Agilent (2010). CrysAlis PRO. Agilent Technologies, Yarnton, England.
Blake, A. J., Nikonov, G. I. & Mountford, P. (1997). Acta Cryst. C53, 874-876.  [CSD] [CrossRef] [details]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Ghesner, I., Fenwick, A. & Stephen, D. W. (2006). Organometallics, 25, 4985-4995.  [CSD] [CrossRef] [ChemPort]
Kempe, R. (2000). Angew. Chem. Int. Ed. 39, 468-493.  [CrossRef] [ChemPort]
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.  [ISI] [CrossRef] [ChemPort] [details]
Porter, R. M. & Danopoulos, A. A. (2004). Dalton Trans. pp. 2556-2562.  [CSD] [CrossRef]
Profilet, R. D., Zabrano, C. H., Fanwick, P. E., Nash, J. J. & Rothwell, I. P. (1990). Inorg. Chem. 29, 4362-4364.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]


Acta Cryst (2013). E69, m72  [ doi:10.1107/S160053681205115X ]

This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.