Proton and carbon-13 nuclear magnetic resonance reinvestigation of the dibenzo[a,c]cyclononatetraenyl anion and its 5,9-diphenyl derivative. Planarity vs nonplanarity

ansa-Zirconocene Complexes with Modified Benzindenyl Ligands: Syntheses, Crystal Structure, and Properties as Propene Polymerization Catalysts1,2

“…MS (EI): m / z 216 (M + , 100%). These NMR data are in agreement with those previously obtained by others. , …”

“…For the preparation of cyclopenta[ l ]phenanthrene 14a-H , we applied a strategy (Scheme ), similar to a procedure used by Katz and co-workers, which proved to be more convenient than the syntheses previously described in the literature. , The corresponding 2-methyl derivative 14b-H was synthesized by the addition of MeMgBr to the keto group of 15 10,11 and subsequent dehydration (Scheme ).

2

3

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“…3-Hydro-2-hydroxy-2-methyl-1 H -cyclopenta[ l ]phenanthrene (16). To 5 g (21.19 mmol) of 2,3-dihydro-2-oxo-1 H -cyclopenta[ l ]phenanthrene ( 15 ), , suspended in 20 mL of ether, was added 8.83 mL (26.49 mmol) of a 3 M solution of MeMgBr in ether and the mixture refluxed for 3 h. The mixture was hydrolyzed with 10 mL of an aqueous 2 N solution of HCl and extracted three times with ether (200 mL). The combined organic fractions were washed successively with saturated aqueous solutions of NaHSO 3 (50 mL), NaHCO 3 (50 mL), and water (50 mL).…”

Charge Transfer Properties in Cyclopenta[l]phenanthrene Ferrocenyl Complexes

“…The synthesis of the bimetallic (2-ferrocenyl)(η 5 -cyclopenta[ l ]phenanthrenyl)FeCp compound ( 2 ) was achieved through a sequence which proceeds through an initial step providing the η 1 -[Fe(CO) 2 Cp] adduct, a revised approach to the preparation of CpFe(CO) 2 (η 1 -indenyl), initially described by Cotton and co-workers, followed by η 1 → η 5 conversion with concurrent elimination of two molecules of CO (Scheme ). The same procedure, starting from cyclopenta[ l ]phenanthrene, was adopted for the preparation of the reference complex (η 5 -cyclopenta[ l ]phenanthrenyl)FeCp ( 1b ).…”

“…Ferrocene and n -butyllithium solution were Sigma-Aldrich products. Ferrocenium(BF 4 ) and acetylferrocenium(BF 4 ), 1,3-dihydrocyclopenta[ l ]phenanthren-2-one, cyclopenta[ l ]phenanthrene, and (η 5 -cyclopenta[ l ]phenanthrenyl)FeCp were synthesized according to published procedures.…”