Abstract: | Summary 6,6,8,8-Tetramethyl-7-oxa-6,8-disila3]ferrocenophane2 was obtained from the di(alkoxysilyl) ferrocene (H4C5SiMe2OR)2Fe (R=CH2CH2OCH2CH2OCH2CH2OMe) by hydrolysis and subsequent intramolecular disiloxane formation. 2,2,3,3,4,4,5,5,6,6,8,8-Dodecamethyl-7-oxa-6,8-disila-3]ferrocenophane3 was formed by air oxidation of 2,23,3,4,4,5,5,6,6,7,7-dodecamethyl-6,7-disila2]ferrocenophane. The crystal structures of both compounds were determined by single-crystal X-ray diffraction (2:a=8.5330(10),b=15.610(3),c=18.774(5)Å, =70.68(2), =77.94(2), =75.150(10)°,V=2259.8(8)Å3,Z=6, space group P
,R=0.045,R
w
=0.044;3:a=12.388(3),b=9.924(3),c=19.136(10)Å, =105.11(3)°,V=2271.2(15)Å3,Z=4, space group P21/c,R=0.076,R
w
=0.060). Owing to the flexibility of the disiloxane bridge,2 and3 are unstrained molecules.
3]Ferrocenophane mit Tetramethyldisiloxan-Brücke: Synthese und Molekülstruktur Zusammenfassung 6,6,8,8-Tetramethyl-7-oxa-6,8-disila3]-ferrocenophan2 entsteht aus dem Di(alkoxysilyl)ferrocen (H4C5SiMe2OR)2Fe (R=CH2CH2OCH2CH2OCH2CH2OMe) durch Hydrolyse und anschließende intramolekulare Disiloxan-Bildung. 2,2,3,3,4,4,5,5,6,6,8,8-Dodecamethyl-7-oxa-6,8-disila3]ferrocenophan3 wurde durch Luftoxidation von 2,2,3,3,4,4,5,5,6,6,7,7-Dodecamethyl-6,7-disila2]ferrocenophan erhaeten. Die Kristallstrukturen beider Verbindungen wurden durch Einkristall-Röntgenstrukturanalyse bestimmt (2:a=8.5330(10),b=15.610(3),c=18.774(5)Å, =70.68(2), =77.94(2), =75.150(10)°,V=2259.8(8)Å3,Z=6, Raumgruppe P
,R=0.045,R
w
=0.044;3:a=12.388(3),b=9.924(3),c=19.136(10)Å, =105.11(3)°,V=2271.2(15)Å3,Z=4, Raumgruppe P21/c,R=0.076,R
w
=0.060). Wegen der Flexibilität der Disiloxan-Brücke sind2 und3 ungespannte Moleküle. |