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Schaefer J.,Albert Ludwigs University of Freiburg | Steffani A.,Institute For Organische Chemie Und Biochemie | Plattner D.A.,Institute For Organische Chemie Und Biochemie | Krossing I.,Albert Ludwigs University of Freiburg
Angewandte Chemie - International Edition | Year: 2012

Freshly prepared red selenium and the copper(I) reagent [Cu(1,2-F 2C 6H 4) 2][A] are the key to the salts [Cu 2Se 19][A] 2 and [Cu 2Se 19][A] 2â0.5 Na[A] ([A]=[Al(OR F) 4], R F=C(CF 3) 3), which provides the first structurally characterized E 19 ring of any elementE. The unusual [Cu 2Se 19] 2+ ion contains two Cu + ions that stabilize the C 2-symmetric Se 19 ring. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.


Schaefer J.,Albert Ludwigs University of Freiburg | Kraft A.,Albert Ludwigs University of Freiburg | Reininger S.,Albert Ludwigs University of Freiburg | Santiso-Quinones G.,ETH Zurich | And 5 more authors.
Chemistry - A European Journal | Year: 2013

The reaction of CuI, AgI, and AuI salts with carbon monoxide in the presence of weakly coordinating anions led to known and structurally unknown non-classical coinage metal carbonyl complexes [M(CO)n][A] (A=fluorinated alkoxy aluminates). The coinage metal carbonyl complexes [Cu(CO)n(CH2Cl2) m]+[A]- (n=1, 3; m=4-n), [Au 2(CO)2Cl]+[A]-, [(OC) nM(A)] (M=Cu: n=2; Ag: n=1, 2) as well as [(OC) 3Cu×××ClAl(ORF)3] and [(OC)Au×××ClAl(ORF)3] were analyzed with X-ray diffraction and partially IR and Raman spectroscopy. In addition to these structures, crystallographic and spectroscopic evidence for the existence of the tetracarbonyl complex [Cu(CO)4]+[Al(OR F)4]- (RF=C(CF3) 3) is presented; its formation was analyzed with the help of theoretical investigations and Born-Fajans-Haber cycles. We discuss the limits of structure determinations by routine X-ray diffraction methods with respect to the C-O bond lengths and apply the experimental CO stretching frequencies for the prediction of bond lengths within the carbonyl ligand based on a correlation with calculated data. Moreover, we provide a simple explanation for the reported, partly confusing and scattered CO stretching frequencies of [Cu I(CO)n] units. Precious carbonyl complexes: Cu I, AgI, and AuI salts react with carbon monoxide in the presence of weakly coordinating anions to known and structurally new non-classical coinage metal carbonyl complexes [M(CO)n][A] (A=fluorinated alkoxy aluminate anions). The first structurally characterized copper(I) triscarbonyl complexes, for example, [Cu(CO)3(CH 2Cl2)]+, and the A-frame [Au 2(CO)2Cl]+ were prepared (see figure). Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.


Stein M.,Institute For Organische Chemie Und Biochemie | Breit B.,Institute For Organische Chemie Und Biochemie
Angewandte Chemie - International Edition | Year: 2013

Under (not so much) pressure: A general method for the hydrogenation of tertiary and secondary amides to amines with excellent selectivity using a bimetallic Pd-Re catalyst has been developed. The reaction proceeds under low pressure and comparatively low temperature. This method provides organic chemists with a simple and reliable tool for the synthesis of amines. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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