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A series of trinuclear carbonylmetal complexes of tri(1-cyclohepta-2,4,6-trienyl)phosphane, P(C 7 H 7 ) 3  (1), has been prepared by the reaction of P(SiMe 3 ) 3  with η 7 -tropylium halfsandwich salts, [(η 7 -C 7 H 7 )M(CO) 3 ]BF 4 , (M = Cr, Mo, W). While phosphorus remains uncoordinated in the chromium complex P[(η 6 -C 7 H 7 )Cr(CO) 3 ] 3  (2a), the molybdenum and tungsten analogues,(M = Mo (2b), W (2c)), contain a coordinated phosphorus atom together with a η 4 -norcaradienyl substituent. Reaction of 2a with pentacarbonylmetal fragments, [M(CO) 5 ], leads to trinuclear products,- (CO) 4 ][(η-C 7 H 7 )M(CO) 3 ] 2  (M = Cr (5a), W (5c)), in which phosphorus is coordinated next to an η 2 -cycloheptatrienyl substituent. Several alkyl- and arylphosphanes containing [(η 6 -C 7 H 7 )Cr(CO) 3 ] substituents (X), e. g. Ph 2 P(X) (6a), RP(X) 2  (R = Me (7a), CH 2 Ph (8a), Ph (9a)) and (X) 2 P(R')P(X) 2  (R' = methylene (10a) or ο-phenylene (11a)), have also been synthesized. The chromium complexes 6a - 11a contain an uncoordinated phosphorus center, but in contrast to 9a, the corresponding tungsten compound PhP(9c) has again a structure similar to 2c. The arsenic complexes, As[(η 6 -C 7 H 7 )M(CO) 3 ] 3  (M = Cr (12a), W (12c)) both contain an uncoordinated arsenic center, analogous to 2a. The molecular structures of all new complexes in solution at room temperature were deduced from a consistent set of  1 H,  13 C and  31 P NMR data, and X-ray structure determinations were carried out for 2a and 5c.

zeitschrift für naturforschung b

Oligonuclear Tricarbonylchromium- and Tricarbonyltungsten Derivatives of Tris(1-cyclohepta-2,4,6-trienyl)phosphane, P(C 7 H 7 ) 3 , and Related Ligands