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Cyclic and Polycyclic Gallium‐Antimony Compounds: Synthesis and Crystal Structures of [GaCl(P n Pr 2 Ph)(SbSi i Pr 3 )] 2 and [(GaCl) 4 (SbSi i Pr 3 ) 4 (P n Pr 2 Ph) 2 ]
Author(s) -
von Hänisch Carsten,
Scheer Petra,
Rolli Birgit
Publication year - 2002
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/1099-0682(200212)2002:12<3268::aid-ejic3268>3.0.co;2-n
Subject(s) - chemistry , antimony , gallium , thermal decomposition , benzene , single crystal , mass spectrometry , crystal structure , crystallography , nuclear magnetic resonance spectroscopy , ring (chemistry) , stereochemistry , medicinal chemistry , inorganic chemistry , organic chemistry , chromatography
The reaction of [(DME)LiE(SiMe 3 ) 2 ] (E = As, Sb) with i Pr 3 SiCl in DME yields the mixed silylated compounds i Pr 3 SiE(SiMe 3 ) 2 ( 1 : E = As, 2 : E = Sb). Compounds 1 and 2 were characterised by multinuclear NMR spectroscopy and mass spectrometry. The antimony compound 2 reacts with [GaCl 3 P n Pr 2 Ph] to give the cyclic compound [GaCl(P n Pr 2 Ph)(SbSi i Pr 3 )] 2 ( 3 ). The polycyclic Ga‐Sb compound [(GaCl) 4 (SbSi i Pr 3 ) 4 (P n Pr 2 Ph) 2 ] ( 4 ) can be obtained from a solution of 3 in benzene. The central structural motif of 3 is a folded Ga 2 Sb 2 four‐membered ring. Compound 4 consists of a ladder‐like Ga 4 Sb 4 unit and is the first polycyclic Ga‐Sb compound described. Compounds 3 and 4 were characterised by single crystal X‐ray diffraction. The thermal decomposition of both compounds results in the formation of the binary phase GaSb.