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Paek ,Cheolki,Ko, Jaejung,Kang, Sangook,Patrick J.Carrol Korean Chemical Society 1994 Bulletin of the Korean Chemical Society Vol.15 No.6
Monomeric rhodium and iridium-diaryltetrazene complexes $Cp^*$M(RNN=NNR)($Cp^*$=1,2,3,4,5-pentamethylcyclope ntadienyl; M=Rh, Ir; R=Ph, 4-tolyl) have been synthesized from [$Cp^*MCl_2]_2$(M=Rh, Ir) and 2 equiv. of $[Li(THF)_x]_2(RN_4$R) in benzene. We have determined the crystal structure of (${\eta}^5$-pentamethylcyclopentadienyl)diphenyltetrazene iridium by using graphite-monochromated Mo-$K_a$ radiation. The compound was crystallized in the monoclinic space group $P2_{1/c}$ with a=13.781(3), b=9.035(l), c=17.699(3) ${\AA}$, and ${\beta}=111.93(l)^{\circ}$. An X-ray crystal structure of complex 1 showed a short N(2)-N(3) distance ($1.265 {\AA}$) consistent with the valence tautomer A with Ir(III) rather than Ir(I). All complexes are highly colored and decompose on irradiation at 254 nm. Electrochemical studies show that complex 1 displays a quasi-reversible reduction.
Paek Cheolki,Ko Jaejung,Kong Youngkun,Kim, Chang Hwan,Lee Myong Euy Korean Chemical Society 1994 Bulletin of the Korean Chemical Society Vol.15 No.6
New silicon-monosubstituted (${\eta}^4$-2,3,4,5-tetraphenyl-l-silacyclopentadiene)transi tion metal complexes are described. (7-Alkyl-7-silanorbornadienyl)MLn(Alkyl=Methyl: MLn=CpRu$(CO)_2$: Alkyl=Methyl: MLn=CpNi(CO): Alkyl=Ethyl: MLn=CpNi(CO)) complexes were prepared from the corresponding silole-transition metal complexes with dimethylacetylenedicarboxylate. Cycloaddition products were obtained with 2,3-dimethyl-1,3-butadiene, 2,3-butanedione, and 1,4-benzoquinone through the ruthenium-substituted silylene. We have determined the crystal structure of (1-methyl-2,3,4,5-tetraphenyl-l-silacyclopentadien yl)cyclopentadienyldicarbonylruthenium by using graphite monochromated Mo-Ka radiation. The compound was crystallized in the monoclinic space group $P2_{1/c}$ with a = 9.838(l), b = 15.972(3), c = 18.327(3) ${\AA}$, and ${\beta}= 94.28(l)^{circ}$. The ruthenium moiety CpRu$(CO)_2$ on silicon is in an axial position.