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Volume 69 
Part 12 
Pages m686-m687  
December 2013  

Received 20 November 2013
Accepted 25 November 2013
Online 30 November 2013

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.002 Å
Disorder in main residue
R = 0.020
wR = 0.057
Data-to-parameter ratio = 17.0
Details
Open access

Di-[mu]-oxido-bis­[bis­(diiso­propyl­aceta­midinato)-[kappa]N;[kappa]2N,N'-germanium(IV)]

aChemisches Institut, Otto-von-Guericke-Universität Magdeburg, Universitätsplatz 2, D-39106 Magdeburg, Germany,bInstitut für Mikro- und Sensorsysteme, Otto-von-Guericke-Universität Magdeburg, Universitätsplatz 2, D-39106 Magdeburg, Germany, and cInstitut für Anorganische und Analytische Chemie, Technische Universität Braunschweig, Hagenring 30, D-38106 Braunschweig, Germany
Correspondence e-mail: frank.edelmann@ovgu.de

The title compound, [Ge2(C8H17N2)4O2], crystallizes with imposed twofold symmetry, which allows the monodentate amidinate ligands to be arranged in a cisoid fashion. The independent Ge-O distances within the central Ge2O2 ring, which is essentially planar (r.m.s. deviation = 0.039 Å), are 1.7797 (8) and 1.8568 (8) Å. The germanium centres adopt a distorted trigonal-bipyramidal geometry, being coordinated by the two O atoms and by one bidentate and one monodentate amidinate ligand (three N atoms). One N-isopropyl group is disordered over two positions; these are mutually exclusive because of `collisions' between symmetry-equivalent methyl groups and thus each has 0.5 occupancy.

Related literature

For comprehensive reviews on metal amidinates and guanidinates, see: Edelmann (2008[Edelmann, F. T. (2008). Adv. Organomet. Chem. 57, 183-352.], 2013[Edelmann, F. T. (2013). Adv. Organomet. Chem. 61, 55-374.]). For information on germanium precursors for CVD or ALD production of GST thin layers, see: Chen et al. (2007[Chen, T., Xu, C., Hunks, W., Stender, M., Stauf, G. T., Chen, P. S. & Roeder, J. F. (2007). ECS Trans. 11, 269-278.], 2009[Chen, T., Hunks, W., Chen, P. S., Stauf, G. T., Cameron, T. M., Xu, C., DiPasquale, A. G. & Rheingold, A. L. (2009). Eur. J. Inorg. Chem. pp. 2047-2049.], 2010[Chen, T., Hunks, W., Chen, P. S., Xu, C., DiPasquale, A. G. & Rheingold, A. L. (2010). Organometallics, 29, 501-504.]); Lee et al. (2007[Lee, J., Choi, S., Lee, C., Kang, Y. & Lim, D. (2007). Appl. Surf. Sci. 253, 3969-3976.]). For previous literature on related germanium amidinates, see: Brück et al. (2012[Brück, A., Gallego, D., Wang, W., Irran, E., Driess, M. & Hartwig, J. F. (2012). Angew. Chem. Int. Ed. 51, 11478-11482.]); Cabeza et al. (2013[Cabeza, J. A., García-Álvarez, P. & Polo, D. (2013). Dalton Trans. 42, 1329-1332.]); Foley et al. (1997[Foley, S. R., Bensimon, C. & Richeson, D. S. (1997). J. Am. Chem. Soc. 119, 10359-10363.], 2000[Foley, S. R., Yap, G. P. A. & Richeson, D. S. (2000). Dalton Trans. pp. 1663-1668.]); Jones et al. (2008[Jones, C., Rose, R. P. & Stasch, A. (2008). Dalton Trans. pp. 2871-2878.]); Jutzi et al. (1999[Jutzi, P., Keitemeyer, S., Neumann, B. & Stammler, H.-G. (1999). Organometallics, 18, 4778-4784.]); Karsch et al. (1998[Karsch, H. H., Schlüter, P. A. & Reisky, M. (1998). Eur. J. Inorg. Chem. pp. 433-436.]); Kühl (2004[Kühl, O. (2004). Coord. Chem. Rev. 248, 411-427.]); Matioszek et al. (2012[Matioszek, D., Saffon, N., Sotiropoulos, J.-M., Miqueu, K., Castel, A. & Escudié, J. (2012). Inorg. Chem. 51, 11716-11721.]); Yeong et al. (2012[Yeong, H.-X., Zhang, S.-H., Xi, W.-W., Guo, J.-D., Lim, K. H., Nagase, S. & So, C.-W. (2012). Chem. Eur. J. 18, 2685-2691.]); Zhang & So (2011[Zhang, S.-H. & So, C.-W. (2011). Organometallics, 30, 2059-2062.]).

[Scheme 1]

Experimental

Crystal data
  • [Ge2(C8H17N2)4O2]

  • Mr = 742.12

  • Monoclinic, C 2/c

  • a = 20.1934 (2) Å

  • b = 12.7424 (1) Å

  • c = 15.9008 (1) Å

  • [beta] = 100.038 (1)°

  • V = 4028.84 (6) Å3

  • Z = 4

  • Cu K[alpha] radiation

  • [mu] = 2.11 mm-1

  • T = 100 K

  • 0.08 × 0.08 × 0.04 mm

Data collection
  • Oxford Diffraction Xcalibur (Atlas, Nova) diffractometer

  • Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012[Agilent (2012). CrysAlis PRO. Agilent Technologies Ltd, Yarnton, Oxfordshire, England.]) Tmin = 0.837, Tmax = 1.000

  • 35712 measured reflections

  • 4173 independent reflections

  • 4014 reflections with I > 2[sigma](I)

  • Rint = 0.021

Refinement
  • R[F2 > 2[sigma](F2)] = 0.020

  • wR(F2) = 0.057

  • S = 1.08

  • 4173 reflections

  • 245 parameters

  • 28 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.27 e Å-3

  • [Delta][rho]min = -0.29 e Å-3

Data collection: CrysAlis PRO (Agilent, 2012[Agilent (2012). CrysAlis PRO. Agilent Technologies Ltd, Yarnton, Oxfordshire, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; 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 (Siemens, 1994[Siemens (1994). XP. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]); 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: ZL2570 ).


Acknowledgements

Financial support of this work by the Deutsche Forschungsgemeinschaft (DFG), grants Nos. ED 29/22-1 and BU 978/50-1, is gratefully acknowledged.

References

Agilent (2012). CrysAlis PRO. Agilent Technologies Ltd, Yarnton, Oxfordshire, England.
Brück, A., Gallego, D., Wang, W., Irran, E., Driess, M. & Hartwig, J. F. (2012). Angew. Chem. Int. Ed. 51, 11478-11482.
Cabeza, J. A., García-Álvarez, P. & Polo, D. (2013). Dalton Trans. 42, 1329-1332.  [CrossRef] [ChemPort] [PubMed]
Chen, T., Hunks, W., Chen, P. S., Stauf, G. T., Cameron, T. M., Xu, C., DiPasquale, A. G. & Rheingold, A. L. (2009). Eur. J. Inorg. Chem. pp. 2047-2049.  [CrossRef]
Chen, T., Hunks, W., Chen, P. S., Xu, C., DiPasquale, A. G. & Rheingold, A. L. (2010). Organometallics, 29, 501-504.  [CrossRef] [ChemPort]
Chen, T., Xu, C., Hunks, W., Stender, M., Stauf, G. T., Chen, P. S. & Roeder, J. F. (2007). ECS Trans. 11, 269-278.  [ChemPort]
Edelmann, F. T. (2008). Adv. Organomet. Chem. 57, 183-352.  [ChemPort]
Edelmann, F. T. (2013). Adv. Organomet. Chem. 61, 55-374.
Foley, S. R., Bensimon, C. & Richeson, D. S. (1997). J. Am. Chem. Soc. 119, 10359-10363.  [CrossRef] [ChemPort]
Foley, S. R., Yap, G. P. A. & Richeson, D. S. (2000). Dalton Trans. pp. 1663-1668.
Jones, C., Rose, R. P. & Stasch, A. (2008). Dalton Trans. pp. 2871-2878.  [CrossRef]
Jutzi, P., Keitemeyer, S., Neumann, B. & Stammler, H.-G. (1999). Organometallics, 18, 4778-4784.  [CrossRef] [ChemPort]
Karsch, H. H., Schlüter, P. A. & Reisky, M. (1998). Eur. J. Inorg. Chem. pp. 433-436.  [CrossRef]
Kühl, O. (2004). Coord. Chem. Rev. 248, 411-427.
Lee, J., Choi, S., Lee, C., Kang, Y. & Lim, D. (2007). Appl. Surf. Sci. 253, 3969-3976.  [CrossRef] [ChemPort]
Matioszek, D., Saffon, N., Sotiropoulos, J.-M., Miqueu, K., Castel, A. & Escudié, J. (2012). Inorg. Chem. 51, 11716-11721.  [CrossRef] [ChemPort] [PubMed]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Siemens (1994). XP. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Yeong, H.-X., Zhang, S.-H., Xi, W.-W., Guo, J.-D., Lim, K. H., Nagase, S. & So, C.-W. (2012). Chem. Eur. J. 18, 2685-2691.  [CrossRef] [ChemPort] [PubMed]
Zhang, S.-H. & So, C.-W. (2011). Organometallics, 30, 2059-2062.  [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m686-m687   [ doi:10.1107/S1600536813032133 ]

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