Preparation, Properties, and Reactions of Metal‐Containing Heterocycles, XCIII . Diosma[5. n .5. n ]ortho‐, ‐meta‐, and ‐paracyclophanes ( n = 0–2)

The reaction of the ortho‐, meta ‐, and para ‐bis(triflates) [(F 3 CSO 2 OCH 2 CH 2 C 6 H 4 ) 2 (CH 2 ) n ] with n = 0 ( ortho : 1a ), n = 0, 1 ( meta : 1b, d ), and n = 0–2 ( para : 1c, e, g ) with [Os(CO) 4 ] 2– results in the formation of the diosma[5. n .5. n ]‐ortho‐, ‐meta‐, and ‐paracyclophanes with n = 0 (ortho: 2a ), n = 0, 1 (meta: 2b, d ), and n = 0–2 (para: 2c, e, g ). On reaction of the bis(triflates) 1a, b with the dianionic [Fe(CO) 4 ] 2– the corresponding ferracyclophanes are formed only in situ. Carbon monoxide insertion into the Fe–C s̀ bonds of the ferracycles affords the ketones 6a, b . The structures of 2a and 2e were investigated by X‐ray structural analysis. Compounds 2a and 2e crystallize in the space group P 2 1 / c with Z = 8 and P 1 with Z = 2, respectively.