Synlett 2008(20): 3106-3110  
DOI: 10.1055/s-0028-1087418
LETTER
© Georg Thieme Verlag Stuttgart ˙ New York

Preparation and Catalytic Performance of Novel Dimeric Tetranuclear Zinc Complexes in Hydroamination of Alkenes at Room Temperature

Mustafa Biyikal, Karolin Löhnwitz, Peter W. Roesky*a, Siegfried Blechert*b
a Institut für Anorganische Chemie, Universität Karlsruhe, Engesserstr. 15, 76128 Karlsruhe, Germany
Fax: +49(721)6084854; e-Mail: roesky@chemie.uni-karlsruhe.de;
b Institut für Chemie, Technische Universität Berlin, Strasse des 17. Juni 135, 10623 Berlin, Germany
Fax: +49(30)31423619; e-Mail: blechert@chem.tu-berlin.de;
Further Information

Publication History

Received 10 August 2008
Publication Date:
27 November 2008 (online)

Abstract

The synthesis of two novel dimeric tetranuclear zinc complexes has been described. The application of these complexes in hydroamination of unactivated alkenes showed at room temperature high catalytic activity.

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Single-Crystal X-ray Diffraction Data of Compound 4
C34H52Br4N4O2Zn4˙0.5 (toluene) (1175.98): Stoe IPDS 2T, space group C2/c (No. 15) with a = 29.1063 (12) Å, b = 17.2017 (7) Å, c = 22.2739 (9) Å, β = 126.790 (2)˚ at 200 K, Z = 8, V = 8931.0(6) ų, ρ = 1.749 g cm, 2θ max = 50˚, 7865 reflections collected, 6354 unique reflections (R int = 0.0860). The structure was solved by Patterson methods (SHELXS-97 and SHELXL-97) and refined by full-matrix least-square techniques with I > 2σ(I) to R 1 = 0.0483 and wR 2 = 0.1190.
Single-Crystal X-ray Diffraction Data of Compound 9
C34H56N4O2Zn4 (814.31): Oxford Diffraction Xcalibur S Sapphire, space group P61 (No. 169) with a = 11.21070 (10) Å, c = 50.8375 (12) Å, at 150 K, Z = 6, V = 5533.25 (15) ų, ρ = 1.466 g cm, 2θ max = 50˚, 41505 reflections collected, 6515 unique reflections (R int = 0.0898). The structure was solved by Patterson methods (SHELXS-97 and SHELXL-97) and refined by full-matrix least-square techniques with I > 2σ(I) to R 1 = 0.0605 and wR 2 = 0.0812.
Positional parameters, hydrogen-atom parameters, thermal parameters, bond lengths and angles have been deposited as Supporting Information; CCDC-689633 (4) and 689634 (9).