The thf adduct of FeCl2, FeCl2(thf)1.5, reacts with bidentate aliphatic nitrogen bases in toluene as medium to give the corresponding adducts of FeCl2. X-ray crystallography of Fe(dienMe)Cl2 (dienMe = bis(2-dimethylaminoethyl)methylamine) has shown the compound to be mononuclear with pentacoordinated iron, thus confirming an earlier suggestion by Ciampolini and Speroni based on spectroscopic and magnetic data. Crystal data: C9H23Cl2FeN3; M = 300.06 g mol-1; monoclinic; space group P21/c (No.14); a = 8.396(3); b = 29.556(8); c = 12.108(3) Å ; g= 101.22(4)° ; V = 2947(3) Å 3; Z = 8; dcalc = 1.352 g.cm-3; lAg-Ka = 0.56087 Å ; mu = 7.02 cm-1; F(000) = 1264; T = 293 K. Bromo- and iodo complexes of iron(II) have been prepared by using cis-FeX2(CO)4 (X = Br, I) as precursors. The reaction of cis-Fe(CO)4X2 (X = Br, I) with N,N’-dimethylethylenediamine (dmeda) or N,N,N’,N’-tetramethylethylenediamine (tmeda) in heptane as medium affords adducts of general formula Fe(NN)nX2 - X = Br, I; NN = dmeda, n = 2, NN = tmeda, n = 1. The iodo derivative Fe(tmeda)I2 has been characterized by X-ray crystallography and found to be mononuclear with tetracoordinated iron(II) in a distorted tetrahedral arrangement of two iodo- and two nitrogen atoms of the bidentate amine. Crystal data: C6H16FeI2N2; M = 425.86 gmol-1; orthorhombic; space group Pbca (No. 61); a = 14.724(2); b = 15.151(4); c = 24.173(3) Å ; U = 5392(2) Å 3; Z = 16; dcalc = 2.098 g cm-3; Ag-Ka = 0.56087 Å ; mu = 29.52 cm-1; F(000) = 3168; T = 293 K.
Tetra-, Penta-, and Hexacoordination in Iron(II) Adducts of Aliphatic Bidentate Amines. Crystal and Molecular Structure of the Mononuclear Complexes Fe(dienMe)Cl2 and Fe(tmeda)I2
CALDERAZZO, FAUSTO;PAMPALONI, GUIDO;
1999-01-01
Abstract
The thf adduct of FeCl2, FeCl2(thf)1.5, reacts with bidentate aliphatic nitrogen bases in toluene as medium to give the corresponding adducts of FeCl2. X-ray crystallography of Fe(dienMe)Cl2 (dienMe = bis(2-dimethylaminoethyl)methylamine) has shown the compound to be mononuclear with pentacoordinated iron, thus confirming an earlier suggestion by Ciampolini and Speroni based on spectroscopic and magnetic data. Crystal data: C9H23Cl2FeN3; M = 300.06 g mol-1; monoclinic; space group P21/c (No.14); a = 8.396(3); b = 29.556(8); c = 12.108(3) Å ; g= 101.22(4)° ; V = 2947(3) Å 3; Z = 8; dcalc = 1.352 g.cm-3; lAg-Ka = 0.56087 Å ; mu = 7.02 cm-1; F(000) = 1264; T = 293 K. Bromo- and iodo complexes of iron(II) have been prepared by using cis-FeX2(CO)4 (X = Br, I) as precursors. The reaction of cis-Fe(CO)4X2 (X = Br, I) with N,N’-dimethylethylenediamine (dmeda) or N,N,N’,N’-tetramethylethylenediamine (tmeda) in heptane as medium affords adducts of general formula Fe(NN)nX2 - X = Br, I; NN = dmeda, n = 2, NN = tmeda, n = 1. The iodo derivative Fe(tmeda)I2 has been characterized by X-ray crystallography and found to be mononuclear with tetracoordinated iron(II) in a distorted tetrahedral arrangement of two iodo- and two nitrogen atoms of the bidentate amine. Crystal data: C6H16FeI2N2; M = 425.86 gmol-1; orthorhombic; space group Pbca (No. 61); a = 14.724(2); b = 15.151(4); c = 24.173(3) Å ; U = 5392(2) Å 3; Z = 16; dcalc = 2.098 g cm-3; Ag-Ka = 0.56087 Å ; mu = 29.52 cm-1; F(000) = 3168; T = 293 K.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
