Polyhedral organoiridaazaborane chemistry. The preparation of the eleven-vertex nido compound [9-Cl-8-(η5-C5Me5)-nido-8,7-IrNHB9H10] and its characterization by single-crystal X-ray diffraction analysis and nuclear magnetic resonance spectroscopy

1991 ◽  
Vol 56 (8) ◽  
pp. 1607-1617 ◽  
Author(s):  
Karl Nestor ◽  
Xavier L. R. Fontaine ◽  
John D. Kennedy ◽  
Bohumil Štíbr ◽  
Karel Baše ◽  
...  

Reaction between nido-6-HNB9H11 (from[9-(MeNC)-arachno-6-HNB9H11] and [(η5-C5Me5).IrCl2]2 in the presence of N,N,N’,N’-tetramethylnaphthalene-1,8-diamine) gives [9-Cl-8-(η5-C5Me5)-nido-8,7-IrNHB9H10] as a yellow crystalline solid in 40% yield. Crystals are triclinic, space group P1, Z = 2, with a = 825.5(1), b = 986.4(2), c = 1 158.7(2) pm, α = 95.12(1), β = 91.00(1), γ = 111.90(1)°. The molecular structure is based on an open-faced nido {IrNB9} eleven-vertex polyhedron with the iridium and nitrogen atoms in adjacent positions in the open face. Nuclear magnetic single and multiple resonance spectroscopy assigns the cluster 11B and 1H resonances, and suggests strong electronic similarities to the sulphur-containing analogue [9-Cl-8-(η5-C5Me5)-nido-8,7-IrSB9H10].

1990 ◽  
Vol 68 (12) ◽  
pp. 2192-2197
Author(s):  
Jean-Pierre Reboul ◽  
Pierre Brouant ◽  
Jacques Barbe ◽  
Claude Caranoni ◽  
Catherine Soula ◽  
...  

The solid state configuration of 1-isopropyl-2-phenyl-1,3-diaza-6-one-bicyclo[3.3.0]oct-2-ene was determined from X-ray diffraction data (a = 10.039(3) Å; b = 8.683(3) Å; c = 15.505(6) Å; β = 90.72(9)°; P21/c;R = 0.047). This structure is compared to those of three other related (Δ-2)-imidazolines. Molecular structure in solution was investigated by 1H nuclear magnetic resonance spectroscopy. Results clearly indicate that the title compound has the same structure in the solid state as in solution. On the contrary, this configuration differs appreciably from those of other (Δ-2)-imidazolines considered in this report. Keywords: (Δ-2)-imidazolines, crystal structure, NMR, conformations.


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