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  • 1
    ISSN: 0009-2940
    Keywords: Mercury ; Lanthanides ; Lanthanoid(II) complexes ; (N-2,6-Diisopropylphenyl)(N-trimethylsily)amide complexes ; Bis(trimethylsilyl)amide complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 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-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-iPr2C6H3)]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.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0044-2313
    Keywords: Silicon ; germanium ; tin compounds, phosphanes ; tetramethylcyclopentadienyl ; carbonyl complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimethyl(tetramethylcyclopentadienyl)silyl-, -germyl-, and -stannylphosphanes. X-Ray Structures of Chloro(dimethyl)tetramethylcyclopentadienyl-stannane and Tetracarbonyl[1-dimethyl(tetramethylcyclopentadienyl)germyl-3,4-dimethyl-phospholene]iron(0)Me2Cp′SiCl (1) (Cp′ = C5HMe4) reacts with magnesium and R2PCl (R = Ph, tBu) as well as PCl3 in tetrahydrofurane yielding Me2Cp′SiPPh2 (4), Me2Cp′SiPtBu2 (5) and (Me2Cp′Si)3P (6) respectively. The reaction of Me3SiPPh2 (7) or Me3SiPC4H4Me2 (10) with Me2Cp′GeCl (2) and Me2Cp′SnCl (3) leads to the formation of Me2Cp′EPPh2 (E = Ge (8), Sn (9)) and Me2Cp′EPC4H4Me2 (E = Ge (11), Sn (12)). 11 reacts with Fe(CO)5 with formation of Fe(CO)4[(PC4H4Me2)GeCp′Me2] (13). 3 crystallizes in the space group P21/n with a = 986,7(1), b = 1247,3(2), c = 1028,2(1) pm, β = 92,71(1)°, Z = 4 and V = 1264,1(2) 10-30 m3. The final refinement resulted in R1 = 0,0249 for 2097 observed reflexions with Fo ≥ 4σ(Fo). 13 crystallizes in the space group P21/n with a = 967,7(3), b = 1298,70(16), c = 1832,7(3) pm, β = 95,810(19)°, Z = 4 and V = 2291,4(8) 10-30 m3 (R1 = 0,0444 for 4043 observed reflexions with Fo ≥ 4σ(Fo). 13 forms a trigonal bipyramide with the phosphane ligand 11 in an axial position.
    Notes: Me2Cp′SiCl (1) (Cp′ = C5HMe4) reagiert mit Magnesium und R2PCl (R = Ph, tBu) bzw, PCl3 in Tetrahydrofuran unter Bildung von Me2Cp′SiPPh2 (4) und Me2Cp′SiPtBu2 (5) bzw. (Me2Cp′Si)3P (6). Durch Umsetzung von Me3SiPPh2 (7) oder Me3SiPC4H4Me2 (10) mit Me2Cp′GeCl (2) und Me2Cp′SnCl (3) wurden Me2Cp′EPPh2 (E = Ge (8), Sn (9)) bzw. Me2Cp′EPC4H4Me2 (E = Ge (11), Sn (12)) erhalten. 11 reagiert mit Fe(CO)5 unter Bildung von Fe(CO)4[(PC4H4Me2)GeCp′Me2] (13). 3 kristallisiert in der Raumgruppe P21/n mit a = 986,7(1), b = 1247,3(2), c = 1028,2(1) pm, β = 92,71(1)°, Z = 4 und V = 1264,1(2) 10-30 m3 (R1 = 0,0249 für 2097 beobachtete Reflexe mit Fo ≥ 4σ(Fo). 13 kristallisiert in der Raumgruppe P21/n mit a = 967,7(3), b = 1298,70(16), c = 1832,7(3) pm, β = 95,810(19)°, Z = 4 und V = 2291,4(8) 10-30 m3 (R1 = 0,0444 für 4043 beobachtete Reflexe mit Fo ≤ 4σ(Fo). 13 ist trigonal bipyramidal mit dem Phosphanliganden 11 in axialer Position.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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