TY - JOUR
T1 - Syntheses of low coordination number divalent lanthanoid organoamide complexes, and the x-ray crystal structures of Bis[(N-2,6-diisopropylphenyl)(N-trimethylsiIyl)amido]bis(tetrahydrofuran) samarium(II) and -ytterbium(II)
AU - Deacon, Glen B.
AU - Fallen, Gary D.
AU - Forsyth, Craig M.
AU - Schumann, Herbert
AU - Weimann, Roman
PY - 1997/1/1
Y1 - 1997/1/1
N2 - The mercury(II) amide complex Hg[N(SiMe3)(2,6-iPr2C6H3)] 2 (1) was prepared by reaction of HgBr2 with Li[N(SiMe3)(2,6-iPr2C6H3)] in diethyl ether solvent. Redox transmetallation reactions of 1 with elemental samarium, europium or ytterbium in THF solvent (THF = tetrahydrofuran), generated the novel divalent complexes Ln[N(SiMe3)(2,6-iPr2C6H3)] 2(THF)2 with Ln = Sm (2), Eu (3) and Yb (4). 4 was also synthesized by reaction of elemental ytterbium, HgPh2 and HN(SiMe3)(2,6-]Pr2C6H3) in THF solvent. This generally more convenient approach has also been applied to the preparation of Ln[N(Si-Me3)2]2(THF)2 [Ln = Sm (5), Yb (6)] by reaction of the metals with HgPh2 and HN(SiMe3)2. Thermal desolvation of 4 under high vacuum gave Yb[N(SiMe3)(2,6-jPr2C6H3)]2(THF) (7), whereas under identical conditions 6 yielded the solvent-free complex (Yb[N(SiMe3)2]2}2 (8). The new compounds 1-4 and 7 are hydrocarbon soluble and 171Yb-NMR spectra were recorded for 4, 6, 7 and 8. X-ray crystal structure determinations of 2 and 4 revealed four-coordinate, distorted tetrahedral metal environments augmented by weak Ln⋯ipso-C(aryl) interactions.
AB - The mercury(II) amide complex Hg[N(SiMe3)(2,6-iPr2C6H3)] 2 (1) was prepared by reaction of HgBr2 with Li[N(SiMe3)(2,6-iPr2C6H3)] in diethyl ether solvent. Redox transmetallation reactions of 1 with elemental samarium, europium or ytterbium in THF solvent (THF = tetrahydrofuran), generated the novel divalent complexes Ln[N(SiMe3)(2,6-iPr2C6H3)] 2(THF)2 with Ln = Sm (2), Eu (3) and Yb (4). 4 was also synthesized by reaction of elemental ytterbium, HgPh2 and HN(SiMe3)(2,6-]Pr2C6H3) in THF solvent. This generally more convenient approach has also been applied to the preparation of Ln[N(Si-Me3)2]2(THF)2 [Ln = Sm (5), Yb (6)] by reaction of the metals with HgPh2 and HN(SiMe3)2. Thermal desolvation of 4 under high vacuum gave Yb[N(SiMe3)(2,6-jPr2C6H3)]2(THF) (7), whereas under identical conditions 6 yielded the solvent-free complex (Yb[N(SiMe3)2]2}2 (8). The new compounds 1-4 and 7 are hydrocarbon soluble and 171Yb-NMR spectra were recorded for 4, 6, 7 and 8. X-ray crystal structure determinations of 2 and 4 revealed four-coordinate, distorted tetrahedral metal environments augmented by weak Ln⋯ipso-C(aryl) interactions.
KW - (n-2,6-diisopropylphenyl)(n-trimethylsilyl)amide complexes
KW - Bis(trimethylsilyl)amide complexes
KW - Lanthanides
KW - Lanthanoid(ii) complexes
KW - Mercury
UR - http://www.scopus.com/inward/record.url?scp=0000252395&partnerID=8YFLogxK
U2 - 10.1002/cber.19971300316
DO - 10.1002/cber.19971300316
M3 - Article
AN - SCOPUS:0000252395
VL - 130
SP - 409
EP - 415
JO - Chemische Berichte
JF - Chemische Berichte
SN - 0009-2940
IS - 3
ER -