bis‐cyclometalated compound [Rh2(C8H4S)P(C8H5S)2}2(CH3CO2H)2(O2CCH3)2] (2 a) have been isolated from the reaction of dirhodiumtetraacetate and tris(2‐benzo[b]thienyl)phosphine (2 BTP) using low acidic solutions. By contrast, in pure acetic acid the reaction of Rh2(O2CCH3)4 with 2 BTP and tris(2‐thienyl)phosphine (2 TP), followed by replacement of the axial acetate ligands by chlorides, led to [Rh2(2‐C8H5S
单环金属化化合物[Rh 2 (C 8 H 4 S)P(C 8 H 5 S)2 }(CH 3 CO 2 H)2(O 2 CCH 3)3 ](1 a)和双环金属化化合物[Rh 2 ((C 8 H 4 S)P(C 8 H 5 S)2 } 2(CH 3 CO 2 H)2(O 2 CCH 3)2 ](2 a)已从低乙酸溶液中的四乙酸二钠和三(2-苯并[ b ]噻吩基)膦(2 BTP)的反应中分离得到。相比之下,在纯乙酸中,Rh 2(O 2 CCH 3)4与2 BTP和三(2-噻吩基)膦(2 TP)的反应,然后用氯化物替换轴向乙酸盐配体,导致[Rh 2 (2-C 8 H 5 S)P(2-C 8 H 5 S)2 } 2 Cl 2(O 2 CCH 3)2 ](3 b)和[Rh 2 (2-C 4 H 3 S)P(C 4 H 3 S)2 } 2 Cl 2(O 2 CCH 3)2 ](5 b)。这些新的