13241-47-9Relevant articles and documents
Germanium-containing ferrocenes and ferrocenophanes. Potential precursors for ring-opening polymerizations and 'germaferrocenes'
Zürcher, Stefan,Gramlich, Volker,Togni, Antonio
, p. 355 - 364 (1999)
The new germanium-containing ferrocene and ferrocenophane derivatives (2,3,4,5-tetramethylbuta-1,3-dien-1,4-diyl)-germa-[1]ferrocenophane (2), 2-(2,3,4,5-tetramethylbuta-1,3-dien-1,4-diyl)-1,3-dithia-2-germa-[3] ferrocenophane (3), 1,1′-bis(1-ethoxy-2,3,4,5-tetramethyl-1-germacyclopenta-2,4-dienyl)- ferrocene (6), 1,3-bis(2,3,4,5-tetramethylbuta-1,3-dien-1,4-diyl)-1,3-digerma-2-oxo-[3] ferrocenophane (7), 1,1′-bis(1-hydrido-2,3,4,5-tetramethyl-1-germacyclopenta-2,4-dienyl)- ferrocene (8) and 1,2-bis(2,3,4,5-tetramethylbuta-1,3-dien-1,4-diyl)-digerma-[2]ferrocenophane (9) have been prepared starting from the dichlorogermol 1. The synthesis of the known ferrocenophanes dichloro-(ferrocene-1,1′-dithiolato)-germane (10a) and dichloro-(ferrocene-1,1′-dithiolato)-stannane (10b) was improved. X-ray crystal structural studies of 2 (C18H20FeGe, a=10.907(4), b=11.040(4), c=13.771(5) ?, β=110.87°, monoclinic, C2/c (No. 15), Z=4), 3 (C18H20FeGeS2, a=8.104(3), b=8.593(4), c=13.177(6) ?, α=70.79(4), β=77.56(3), γ=85.80(3) ? triclinic, P1? (No. 2), Z=2), 7 (C26H32FeGe2O, a=18.95(2), b=8.557(6), c=16.69(6) ?, β=110.65(6)°, monoclinic, C2/c (No. 15), Z=4), 9 (C26H32FeGe2, a=11.209(6), b=10.839(5), c=19.819(10) ?, β=92.89(2), γ=90°, monoclinic, P21/n (No. 14), Z=4), 10a (C10H8FeGeS2, a=10.873(5), b=7.417(4), c=16.415(10) ?, orthorhombic, Pca21 (No. 29), Z=4), 12a (C20H16Fe2GeS4, a=7.459(4), b=10.921(5), c=23.552(12) ?, orthorhombic, Pbcn (No. 60), Z=4) and 12b (C20H16Fe2SnS4, a=7.484(4), b=10.953(6), c=23.917(12) ?, orthorhombic, Pbcn (No. 60), Z=4) and cyclovoltammetric characterizations for all ferrocene-containing compounds have been carried out.
A new geometrical form for tin. Synthesis and structure of the spirocyclic complex [(CH3)4N][(C7H6S2) 2SnCl] and the related monocyclic derivative [(C2H5)4N][(C7H6S 2)Ph2SnCl]
Sau, Arjun C.,Day, Roberta O.,Holmes, Robert R.
, p. 3076 - 3081 (2008/10/08)
The synthesis and X-ray structure of the tetramethylammonium chloride adduct of the spirobi(dithiolato)stannate(IV), [(CH3)4N]+[(C7H6S 2)2SnCl]-, (2), provide the first example of a tin compound having a discrete rectangular-pyramidal geometry. The synthesis and X-ray structure of the related monocyclic derivative [(C2H5)4N]+[(C7H 6S2)Ph2SnCl]- (4) shows tin to possess a trigonal-bipyramidal geometry. 2 crystallizes in the monoclinic space group Cc, with a = 14.126 (4), b = 11.485 (6) ?, c = 14.609 (5) ?, β = 100.37 (3)°, and Z = 4. 4 crystallizes in the monoclinic space group P21/c, with a = 12.344 (4) ?, b = 11.975 (5) ?, c = 19.120 (5) ?, β = 96.41 (2)°, and Z = 4. Data for both compounds were collected on an Enraf-Nonius CAD 4 automated diffractometer out to a maximum 2θMo Kα of 50°. The final conventional unweighted residuals were 0.039 and 0.048 for 2 and 4, respectively. It is shown that the 119mSn M?ssbauer quadrupole splitting parameter is useful in distinguishing the square (or rectangular) pyramid from the trigonal bipyramid. Comparison of pentacoordinated tin(IV) with pentacoordinated germanium(IV) and phosphorus shows that the known rectangular pyramids have spirocyclic systems as a common structural feature.
