Bis(diethyl­amido-κN)(diethyl­amine-κN)bis­(2,6-diisopropyl­phenyl­amido-κN)zirconium(IV)

Zauliczny, M.; Grubba, R.; Ponikiewski, Ł.; Pikies, J.

doi:10.1107/S160053681205115X

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 (C-C) = 0.007 Å
R = 0.073
wR = 0.188
Data-to-parameter ratio = 18.4
Details

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

Mateusz Zauliczny,^a Rafal Grubba,^a Lukasz Ponikiewski ^a ^* and Jerzy Pikies ^a

^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 Zr^IV 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-HN contact occurs. There are two independent molecules in the asymmetric unit.

Related literature

For related zirconium(IV) structures, see: Profilet et al. (1990); Blake et al. (1997); Porter & Danopoulos (2004); Ghesner et al. (2006). For related syntheses, see: Kempe (2000).

Experimental

Crystal data

[Zr(C₁₂H₁₈N)₂(C₄H₁₀N)₂(C₄H₁₁N)]
M_r = 661.17
Triclinic, $[P \overline 1]$
a = 11.2079 (3) Å
b = 13.1612 (5) Å
c = 14.3443 (6) Å
= 86.578 (3)°
= 70.484 (3)°
= 71.232 (3)°
V = 1885.61 (12) Å³
Z = 2
Mo K radiation
= 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) T_min = 0.889, T_max = 0.928
11493 measured reflections
7412 independent reflections
5867 reflections with I > 2(I)
R_int = 0.035

Refinement

R[F² > 2(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
_max = 1.82 e Å^-3
_min = -2.13 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N3-H3AN1	0.84 (5)	2.56 (5)	2.983 (5)	112 (4)

Data collection: CrysAlis PRO (Agilent, 2010); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SUPERFLIP (Palatinus & Chapuis, 2007); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: WinGX (Farrugia, 2012).

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.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
Ghesner, I., Fenwick, A. & Stephen, D. W. (2006). Organometallics, 25, 4985-4995.
Kempe, R. (2000). Angew. Chem. Int. Ed. 39, 468-493.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Porter, R. M. & Danopoulos, A. A. (2004). Dalton Trans. pp. 2556-2562.
Profilet, R. D., Zabrano, C. H., Fanwick, P. E., Nash, J. J. & Rothwell, I. P. (1990). Inorg. Chem. 29, 4362-4364.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds