ISSN:
1572-8862
Keywords:
Iron
;
ynamine
;
aminoalkyne
;
diazoalkane
;
carbene
;
C-N coupling
;
insertion
;
structure
Source:
Springer Online Journal Archives 1860-2000
Topics:
Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
,
Physics
Notes:
Abstract The diiron ynamine complex [Fe2(CO)7{μ-CR)C(NEt2)}] (1:R=Me,2:R = C3H5.3:R=SiMe3.4:R = Ph) reacts at room temperature with diphenyldiazomethane Ph2CN2, in hexane to yield complexes [Fe2(CO)6{C(R)C(NEt2)N (NCPh2)] (5a:R=Me,6a:R=C3H5.7a R=SiMe3.8a:R=Ph) resulting from the insertion of the terminal nitrogen atom into the Fe=C carbene bond. Insertion the second nitrogen atom and formation of compounds [Fe2(CO)6zμ-C(R)C(NEt2)NN(CPh2)}] (5b:R=Me,6b:R=C3H5,7b:R=SiMe3,8b:R=Ph) is observed when compounds5a-5a are treated in refluxing hexane. Transformation of compoundsa tob is also obtained at room temperature within a few days. All compounds were identified by their1H NMR spectra. Compounds6a, 7a, 8a, and8b were characterized by single crystal X-ray diffraction analyses. Crystal data: for6a: space group = P21/n,a=12.853(1) A,b=24.800(7) A,c=8.947(6) A,β=99.29(3)°,Z=4, 2227 rellectionsR=0,038; for7a: space group=Pl,a=ll.483(4) A,b=14.975(4) A,c = 17.890(8) A,α = 82.80(3)°,β=94.29(7)°,γ=85.42(2),Z = 4, 5888 reflectionR = 0.035: for8a: space group = Pcab.a = 31.023(8) A.b=20.137(1) A.c=9.686(2) A.Z=8. 1651 reflections,R=0.071; for8b: space group=P21/n,a=21.459(4),b=10,100(3) A,c=28,439(8) A,ß=103.86(4)°,Z=8. 2431 reflections.R=0.057.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1007/BF01165799
