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The Chemistry of 1,3,5‐Triazacyclohexane Complexes, 3 . High Yield Synthesis of [Cr{N(SiMe 3 ) 2 } 3 ] and Accurate Structure Determination by Cocrystallization with Me 6 Si 2
Author(s) -
Köhn Randolf D.,
KociokKöhn Gabriele,
Haufe Matthias
Publication year - 1996
Publication title -
chemische berichte
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 0009-2940
DOI - 10.1002/cber.19961290107
Subject(s) - chemistry , chromium , yield (engineering) , ligand (biochemistry) , crystal structure , trigonal crystal system , medicinal chemistry , ether , crystallography , petroleum ether , stereochemistry , organic chemistry , metallurgy , biochemistry , materials science , receptor , extraction (chemistry)
The reaction of N,N′,N′′ ‐trimethyl‐1,3,5‐triazacyclohexane chromium trichloride ((Me 3 TAC)CrCl 3 , 1 ) with LiN(SiMe 3 ) 2 or NaN(SiMe 3 ) 2 in petroleum ether yields nearly quantitatively [Cr{N(SiMe 3 ) 2 } 3 ] ( 2 ) with loss of the Me 3 TAC ligand. Compound 2 could be crystallized from hexamethyldisilane as [Cr{N(SiMe 3 ) 2 } 3 ] · (Me 6 Si 2 ) 0,5 which allowed the refinement of the X‐ray crystal structure in the trigonal space group P‐31c (no. 163) ( a = 16.012(3) Å, c = 8.4796(12) Å, V = 1882.8(6) Å 3 , Z = 2) without severe disorder.