“…Nucleophilic attack of the organometallic enolate anions [(η 5 -C 5 H 4 Ac)Fe(η 5 -C 5 H 4 COCH 2 )] - and [CpFe(COCH 2 )(CO)(PPh 3 )] - on the tropylium ring of [(η 7 -C 7 H 7 )M(CO) 3 ] + (M = Cr, Mo) gives the heterobimetallic complexes [(CO) 3 M(μ-C 7 H 7 CH 2 COC 5 H 4 - κ M C 7 H 7 (η 7 ), κ Fe C 5 H 4 (η 5 ))Fe(C 5 H 4 Ac)] and [(CO) 3 M(μ-C 7 H 7 CH 2 CO- κ M C 7 H 7 (η 7 ), κ Fe C )FeCp(CO)(PPh 3 )]. The X-ray crystal structure of the former molybdenum−iron complex has been determined (see Figure ) 24 Crystal structure of [(OC) 3 Mo(μ-C 7 H 7 CH 2 COC 5 H 4 )Fe(C 5 H 4 COMe)].…”
Section: Lx-type Bridgesmentioning
confidence: 99%
“… 24 Crystal structure of [(OC) 3 Mo(μ-C 7 H 7 CH 2 COC 5 H 4 )Fe(C 5 H 4 COMe)]. Reprinted from ref . Copyright 1991 Elsevier Science Ltd.…”
Section: Lx-type Bridgesmentioning
confidence: 99%
“…The X-ray crystal structure of the former molybdenumiron complex has been determined (see Figure 24). 140 The labile molybdenum precursor [Mo(CO) 4 (nbd)] reacts with the nickel phosphinothiolate complex [Ni-(SCH 2 CH 2 PPh 2 ) 2 ] to form the sulfur-bridged bimetallic species [(CO) 4 Mo(µ-SCH 2 CH 2 PPh 2 -κ Mo S,κ Ni S,κ Ni P) 2 -Ni], the X-ray crystal structure of which has been obtained. 141 The longer chain phosphinothiol Ph 2 P-(CH 2 ) 3 SH has also been used as a bridging ligand in heterobimetallic complexes: its titanocene derivative [Cp 2 Ti{S(CH 2 ) 3 PPh 2 -S} 2 ] acts as a metalloligand for nickel(0), and the resulting compound, [Cp 2 Ti{µ-S(CH 2 ) 3 PPh 2 -κ Ti S,κ Ni S,κ Ni P}Ni], has been crystallographically characterized.…”
“…Nucleophilic attack of the organometallic enolate anions [(η 5 -C 5 H 4 Ac)Fe(η 5 -C 5 H 4 COCH 2 )] - and [CpFe(COCH 2 )(CO)(PPh 3 )] - on the tropylium ring of [(η 7 -C 7 H 7 )M(CO) 3 ] + (M = Cr, Mo) gives the heterobimetallic complexes [(CO) 3 M(μ-C 7 H 7 CH 2 COC 5 H 4 - κ M C 7 H 7 (η 7 ), κ Fe C 5 H 4 (η 5 ))Fe(C 5 H 4 Ac)] and [(CO) 3 M(μ-C 7 H 7 CH 2 CO- κ M C 7 H 7 (η 7 ), κ Fe C )FeCp(CO)(PPh 3 )]. The X-ray crystal structure of the former molybdenum−iron complex has been determined (see Figure ) 24 Crystal structure of [(OC) 3 Mo(μ-C 7 H 7 CH 2 COC 5 H 4 )Fe(C 5 H 4 COMe)].…”
Section: Lx-type Bridgesmentioning
confidence: 99%
“… 24 Crystal structure of [(OC) 3 Mo(μ-C 7 H 7 CH 2 COC 5 H 4 )Fe(C 5 H 4 COMe)]. Reprinted from ref . Copyright 1991 Elsevier Science Ltd.…”
Section: Lx-type Bridgesmentioning
confidence: 99%
“…The X-ray crystal structure of the former molybdenumiron complex has been determined (see Figure 24). 140 The labile molybdenum precursor [Mo(CO) 4 (nbd)] reacts with the nickel phosphinothiolate complex [Ni-(SCH 2 CH 2 PPh 2 ) 2 ] to form the sulfur-bridged bimetallic species [(CO) 4 Mo(µ-SCH 2 CH 2 PPh 2 -κ Mo S,κ Ni S,κ Ni P) 2 -Ni], the X-ray crystal structure of which has been obtained. 141 The longer chain phosphinothiol Ph 2 P-(CH 2 ) 3 SH has also been used as a bridging ligand in heterobimetallic complexes: its titanocene derivative [Cp 2 Ti{S(CH 2 ) 3 PPh 2 -S} 2 ] acts as a metalloligand for nickel(0), and the resulting compound, [Cp 2 Ti{µ-S(CH 2 ) 3 PPh 2 -κ Ti S,κ Ni S,κ Ni P}Ni], has been crystallographically characterized.…”
“…Complex 7 , shown in Scheme , was identified as the acyl compound [Re(CO) 5 {C(O)Fc}], where the CO chemical shift presents at 234.8 ppm, obtained from the reaction shown in Scheme . It has been previously synthesized by Beck et al by the reaction of FcCOCl and [Re(CO) 5 ] − and was structurally characterized. The formation of C (Scheme ) in the reaction mixture is seen as a potential precursor to 7 , which is formed after the displacement of the coordinated solvent molecule by CO.…”
Fischer carbene complexes of the group VII transition metals (Mn and Re) containing at least two or three different transition metal substituents, all in electronic contact with the carbene carbon atom, were synthesized. The structural features and their relevance to bonding in the carbene multimetal compounds were investigated, as they represent indicators of possible reactivity sites in polymetallic carbene assemblies. For complexes of the type [ML(x){C(OR)R'}] (ML(x) = MnCp(CO)(2) or Re(2)(CO)(9)), ferrocenyl (Fc) was chosen as the R' substituent, while the OR substituent was systematically varied between an ethoxy or a titanoxy group, to yield the complexes 1a (ML(x) = MnCp(CO)(2), R = Et, R' = Fc), 2a (ML(x) = MnCp(CO)(2), R = TiCp(2)Cl, R' = Fc), 3a (ML(x) = Re(2)(CO)(9), R = Et, R' = Fc), and 4a (ML(x) = Re(2)(CO)(9), R = TiCp(2)Cl, R' = Fc). Direct lithiation of the ferrocene with n-BuLi/TMEDA at elevated temperatures, followed by the Fischer method of carbene preparation, resulted in formation of the novel biscarbene complexes with bridging ferrocen-1,1'-diyl (Fc') substituents [{π-Fe(C(5)H(4))(2)-C,C'}{C(OEt)ML(x)}(2)] (1b, ML(x) = MnCp(CO)(2); 3b, ML(x) = Re(2)(CO)(9)) or the unusual bimetallacyclic bridged biscarbene complexes [{π-TiCp(2)O(2)-O,O'}{π-Fe(C(5)H(4))(2)-C,C'}{CML(x)}(2)] (2b, ML(x) = MnCp(CO)(2); 4b, ML(x) = Re(2)(CO)(9)). The target compounds that were isolated displayed a variety of different geometric isomers and conformations. The greater reactivity of the binary dirhenium acylates in solution, compared to that of the cyclopentadienyl manganese acylate, resulted in a complex reaction mixture. Although the stabilization of hydroxycarbene or hydrido-acyl intermediates of dirhenium carbonyls could not be achieved, their existence in solution was confirmed by the isolation of [(π-H)(2)-(Re(CO)(4){C(O)Fc})(2)] (8), the unique dichloro-bridged biscarbene complex fac-[(π-Cl)(2)-(Re(CO)(3){C(OEt)Fc})(2)] (6), the known hydrido complex [Re(3)(CO)(14)H] (5), the acyl complex [Re(CO)(5){C(O)Fc}] (7), and the aldehyde-functionalized eq-[Re(2)(CO)(9){C(OTiCp(2)Cl)(Fc'CHO)}] (9).
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