Inorganic Chemistry p. 4700 - 4713 (2013)
Update date:2022-07-29
Topics:
Naeem, Saira
Ribes, Angela
White, Andrew J. P.
Haque, Mohammed N.
Holt, Katherine B.
Wilton-Ely, James D. E. T.
The versatile precursors [Ru(CH=CHC6H4Me-4)Cl(CO) (BTD)(PPh3)2] (BTD = 2,1,3-benzothiadiazole) and [Ru(C(Ci - CPh)=CHPh)Cl(CO)(PPh3)2] were treated with isonicotinic acid, 4-cyanobenzoic acid, and 4-(4-pyridyl)benzoic acid under basic conditions to yield [Ru(vinyl)(O2CC5H 4N)(CO)(PPh3)2], [Ru(vinyl)(O 2CC6H4CN-4)(CO)(PPh3)2], and [Ru(vinyl){O2CC6H4(C5H 4N)-4}(CO)(PPh3)2], respectively. The osmium analogue [Os(CH=CHC6H4Me-4)(O2CC 5H4N)(CO)(PPh3)2] was also prepared. cis-[RuCl2(dppm)2] was used to prepare the cationic compounds [Ru(O2CC5H4N)(dppm)2] + and [Ru{O2CC6H4(C 5H4N)-4}(dppm)2]+. The treatment of 2 equiv of [Ru(C(Ci - CPh)=CHPh)(O2CC5H 4N)(CO)(PPh3)2] and [Ru(O2CC 5H4N)(dppm)2]+ with AgOTf led to the trimetallic compounds [{Ru(C(Ci - CPh)=CHPh)(CO)(PPh3) 2(O2CC5H4N)}2Ag] + and [{Ru(dppm)2(O2CC5H 4N)}2Ag]3+. In a similar manner, the reaction of [Ru(O2CC5H4N)(dppm)2]+ with PdCl2 or K2PtCl4 yielded [{Ru(dppm) 2(O2CC5H4N)}2MCl 2]2+ (M = Pd, Pt). The reaction of [RuHCl(CO)(BTD) (PPh3)2] with HCi - CC6H4F-4 provided [Ru(CH=CHC6H4F-4)Cl(CO)(BTD)(PPh 3)2], which was treated with isonicotinic acid and base to yield [Ru(CH=CHC6H4F-4)(O2CC5H 4N)(CO)(PPh3)2]. The addition of [Au(C 6F5)(tht)] (tht = tetrahydrothiophene) resulted in the formation of [Ru(CH=CHC6H4F-4){O2CC 5H4N(AuC6F5)}(CO)(PPh 3)2]. Similarly, [Ru(vinyl)(O2CC 6H4CN-4)(CO)(PPh3)2] reacted with [Au(C6F5)(tht)] to provide [Ru(vinyl){O2CC 6H4(CNAuC6F5)-4}(CO)(PPh 3)2]. The reaction of 4-cyanobenzoic acid with [Au(C 6F5)(tht)] yielded [Au(C6F5) (NCC6H4CO2H-4)]. This compound was used to prepare [Ru(CH=CHC6H4F-4){O2CC 6H4(CNAuC6F5)-4}(CO)(PPh 3)2], which was also formed on treatment of [Ru(CH=CHC6H4F-4)(O2CC6H 4CN-4)(CO)(PPh3)2] with [Au(C6F 5)(tht)]. The known compound [RhCl2(NC5H 4CO2)(NC5H4CO2Na) 3] and the new complex [RhCl2{NC5H 4(C6H4CO2)-4}{NC5H 4(C6H4CO2Na)-4}3] were prepared from RhCl3·3H2O and isonicotinic acid or 4-(4-pyridyl)benzoic acid, respectively. The former was treated with [Ru(CH=CHC6H4Me-4)Cl(CO)(BTD)(PPh3) 2] to yield [RhCl2{NC5H4CO 2(Ru(CH=CHC6H4Me-4)(CO)(PPh3) 2}4]Cl. As an alternative route to pentametallic compounds, the Pd-coordinated porphyrin [(Pd-TPP)(p-CO2H) 4] was treated with 4 equiv of [Ru(CH=CHR)Cl(CO)(BTD)(PPh 3)2] in the presence of a base to yield [(Pd-TPP){p-CO2Ru(CH=CHR)(CO)(PPh3)2} 4] (R = C6H4Me-4, CPh2OH). Where R = CPh2OH, treatment with HBF4 led to the formation of [(Pd-TPP){p-CO2Ru(=CHCH=CPh2)(CO)(PPh3) 2}4](BF4)4. [(Pd-TPP){p-CO 2Ru(dppm)2}4](PF6)4 was prepared from [(Pd-TPP)(p-CO2H)4] and cis-[RuCl 2(dppm)2]. The reaction of AgNO3 with sodium borohydride in the presence of [Ru(O2CC5H 4N)(dppm)2]+ or [RuR{O2CC 6H4(C5H4N)-4}(dppm) 2]+ provided silver nanoparticles Ag[NC5H 4CO2Ru(dppm)2]+ and Ag[NC 5H4{C6H4CO2Ru(dppm) 2}-4]+.
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