Premium
Reaction of SiCl 2 ·dipp with K[Ge 9 {Si(SiMe 3 ) 3 } 3 ] – Synthesis and Characterization of [K(dipp) 2 ][Ge 9 {Si(SiMe 3 ) 3 } 3 ]·tol and [dipp‐H][Ge 9 {Si(SiMe 3 ) 3 } 3 ]·2acn [dipp = 1,3‐Bis(2,6‐Diisopropylphenyl)imidazol‐2‐ylidene]
Author(s) -
Fischer Christina,
Klein Wilhelm,
Jantke LauraAlice,
Schiegerl Lorenz J.,
Fässler Thomas F.
Publication year - 2016
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201600296
Subject(s) - monoclinic crystal system , orthorhombic crystal system , toluene , acetonitrile , crystallography , chemistry , raman spectroscopy , crystal structure , nuclear magnetic resonance spectroscopy , stereochemistry , physics , organic chemistry , optics
From solutions of K[Ge 9 {Si(SiMe 3 ) 3 } 3 ] with 1,3‐bis(2,6‐diisopropylphenyl‐)imidazol‐2‐ylidene (dipp) two new compounds were obtained. From toluene, single crystals of [K(dipp) 2 ][Ge 9 {Si(SiMe 3 ) 3 } 3 ] · tol ( 1 ) (tol = toluene) were isolated and the crystal structure was determined [monoclinic, P 2 1 / c , a = 16.8386(3), b = 24.6597(5), c = 30.2988(6) Å, β = 101.813(2)°, V = 12314.7(4) Å 3 , Z = 4, 24192 independent reflections, R 1 = 0.046, wR 2 = 0.084]. The investigation of single crystals from acetonitrile solution revealed the formation of [dipp‐H][Ge 9 {Si(SiMe 3 ) 3 } 3 ] · 2 acn ( 2 ) (acn = acetonitrile) [orthorhombic, P 2 1 2 1 2 1 , a = 13.4484(4), b = 25.8775(7), c = 26.4390(9) Å, V = 9201.1(5) Å 3 , Z = 4, 18065 independent reflections, R 1 = 0.031, wR 2 = 0.052]. The two [Ge 9 {Si(SiMe 3 ) 3 } 3 ] – entities show the minimal and maximal distortion of the central tricapped prism that have been reported to date. All compounds were characterized by ESI‐MS, NMR and Raman spectroscopy, and DFT calculations.