Phosphororganische Verbindungen, XXVIII. Diarylchlorphosphine aus Aryldichlorphosphinen durch Disproportionierung

Horner, L.; Beck, P.; Toscano, Vicente G.

doi:10.1002/cber.19610940826

Cited by 23 publications

(2 citation statements)

References 12 publications

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“…[Fe 2 (m-S 2 )(CO) 6 ], [20] [Fe 3 (CO) 12 ], [24] HSCH 2 (CH 2 OCH 2 ) n CH 2 SH (n 1 ± 3), [25,26] Ph 2 PCl, [27] 1,3,5-Me(BrCH 2 ) 2 C 6 H 3 , [28] 1,4-(BrCH 2 )C 6 H 4 , [29] I(CH 2 ) 4 I, [30] CpFe(CO) 2 I, [31] and SeCl 2 [32] were prepared according to literature procedures. PhC(O)Cl, CS 2 , MeI, PhCH 2 Br, Et 3 N, and Br(CH 2 ) n Br (n 2 ± 4) were of commercial origin and used without further purification.…”

Section: Resultsmentioning

confidence: 99%

Formation and Chemical Reactivities of a New Type of Double‐Butterfly [{Fe₂(μ‐CO)(CO)₆}₂(μ‐SZS‐μ)]²⁻: Synthetic and Structural Studies on Novel Linear and Macrocyclic Butterfly Fe/E (E=S, Se) Cluster Complexes

Song

Fan

et al. 2002

Chemistry A European J

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A new type of double-butterfly [[Fe(2)(mu-CO)(CO)(6)](2)(mu-SZS-mu)](2-) (3), a dianion that has two mu-CO ligands, has been synthesized from dithiol HSZSH (Z=(CH(2))(4), CH(2)(CH(2)OCH(2))(1-3)CH(2)), [Fe(3)(CO)(12)], and Et(3)N in a molar ratio of 1:2:2 at room temperature. Interestingly, the in situ reactions of dianions 3 with various electrophiles affords a series of novel linear and macrocyclic butterfly Fe/E (E=S, Se) cluster complexes. For instance, while reactions of 3 with PhC(O)Cl and Ph(2)PCl give linear clusters [[Fe(2)(mu-PhCO)(CO)(6)](2)(mu-SZS-mu)] (4 a,b: Z=CH(2)(CH(2)OCH(2))(2,3)CH(2)) and [[Fe(2)(mu-Ph(2)P)(CO)(6)](2)(mu-SZS-mu)] (5 a,b: Z=CH(2)(CH(2)OCH(2))(2,3)CH(2)), reactions with CS(2) followed by treatment with monohalides RX or dihalides X-Y-X give both linear clusters [[Fe(2)(mu-RCS(2))(CO)(6)](2)(mu-SZS-mu)] (6 a-e: Z=CH(2)(CH(2)OCH(2))(1,2)CH(2); R=Me, PhCH(2), FeCp(CO)(2)) and macrocyclic clusters [[Fe(2)(CO)(6)](2)(mu-SZS-mu)(mu-CS(2)YCS(2)-mu)] (7 a-e: Z=(CH(2))(4), CH(2)(CH(2)OCH(2))(1-3)CH(2); Y=(CH(2))(2-4), 1,3,5-Me(CH(2))(2)C(6)H(3), 1,4-(CH(2))(2)C(6)H(4)). In addition, reactions of dianions 3 with [Fe(2)(mu-S(2))(CO)(6)] followed by treatment with RX or X-Y-X give linear clusters [[[Fe(2)(CO)(6)](2)(mu-RS)(mu(4)-S)](2)(mu-SZS-mu)] (8 a-c: Z=CH(2)(CH(2)OCH(2))(1,2)CH(2); R=Me, PhCH(2)) and macrocyclic clusters [[[Fe(2)(CO)(6)](2)(mu(4)-S)](2)(mu-SYS-mu)(mu-SZS-mu)] (9 a,b: Z=CH(2)(CH(2)OCH(2))(2,3)CH(2); Y=(CH(2))(4)), and reactions with SeCl(2) afford macrocycles [[Fe(2)(CO)(6)](2)(mu(4)-Se)(mu-SZS-mu)] (10 d: Z=CH(2)(CH(2)OCH(2))(3)CH(2)) and [[[Fe(2)(CO)(6)](2)(mu(4)-Se)](2)(mu-SZS-mu)(2)] (11 a-d: Z=(CH(2))(4), CH(2)(CH(2)OCH(2))(1-3)CH(2)). Production pathways have been suggested; these involve initial nucleophilic attacks by the Fe-centered dianions 3 at the corresponding electrophiles. All the products are new and have been characterized by combustion analysis and spectroscopy, and by X-ray diffraction techniques for 6 c, 7 d, 9 b, 10 d, and 11 c in particular. X-ray diffraction analyses revealed that the double-butterfly cluster core Fe(4)S(2)Se in 10 d is severely distorted in comparison to that in 11 c. In view of the Z chains in 10 a-c being shorter than the chain in 10 d, the double cluster core Fe(4)S(2)Se in 10 a-c would be expected to be even more severely distorted, a possible reason for why 10 a-c could not be formed.

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Section: Resultsmentioning

confidence: 99%

Formation and Chemical Reactivities of a New Type of Double‐Butterfly [{Fe₂(μ‐CO)(CO)₆}₂(μ‐SZS‐μ)]²⁻: Synthetic and Structural Studies on Novel Linear and Macrocyclic Butterfly Fe/E (E=S, Se) Cluster Complexes

Song

Fan

et al. 2002

Chemistry A European J

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“…Tetrahydrofuran (THF) was distilled from Na/benzophenone ketyl under nitrogen. Fe 3 (CO) 12 , Ph 2 PCl, N(CH 2 CH 2 SH) 3 , 1,3,5-(HSCH 2 ) 3 C 6 H 3 , PhSBr, and PhC(Cl)NPh were prepared according to literature procedures. Et 3 N, CS 2 , MeI, PhCH 2 Br, CH 2 CHCH 2 Br, and PhNCS were of commercial origin and used without further purification.…”

Section: Methodsmentioning

confidence: 99%

Synthesis and Characterization of Starlike Complexes Containing Three Terminal Butterfly Fe/S Cluster Cores Generated via Reactions of the Three-μ-CO-Containing Trianions {[(μ-CO)Fe₂(CO)₆]₃[(μ-SCH₂CH₂)₃N]}³^- and {[(μ-CO)Fe₂(CO)₆]₃[1,3,5-(μ-SCH₂)₃C₆H₃]}³^- with Electrophiles

et al. 2005

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The novel three-µ-CO-containing trianions {[(µ-CO)Fe 2 (CO) 6 ] 3 [(µ-SCH 2 CH 2 ) 3 N]} 3-(4A) and {[(µ-CO)Fe 2 (CO) 6 ] 3 [1,3,5-(µ-SCH 2 ) 3 C 6 H 3 ]} 3-(4B) were prepared by reaction of trithiol N(CH 2 CH 2 SH) 3 or 1,3,5-(HSCH 2 ) 3 C 6 H 3 with Fe 3 (CO) 12 and Et 3 N in 1:3:3 molar ratio in THF at room temperature. Further in situ treatment of 4A with electrophiles Ph 2 PCl, PhSBr, PhC(Cl)dNPh, and CH 2 dCHCH 2 Br afforded starlike complexes [(µ-Y)Fe 2 (CO) 6 ] 3 -[(µ-SCH 2 CH 2 ) 3 N] (5-8: Y ) Ph 2 P, PhS, PhCdNPh, CH 2 dCHCH 2 ), whereas its reaction with CS 2 followed by treatment with organic halides RX produced complexes [(µ-Y)Fe 2 (CO) 6 ] 3 -[(µ-SCH 2 CH 2 ) 3 N] (9-11: Y ) MeSCdS, PhCH 2 SCdS, CH 2 dCHCH 2 SCdS). Similarly, 4B reacted in situ with Ph 2 PCl, PhSBr, PhC(Cl)dNPh, CH 2 dCHCH 2 Br, and PhNCS to give starlike complexes [(µ-Y)Fe 2 (CO) 6 ] 3 [1,3,5-(µ-SCH 2 ) 3 C 6 H 3 ] (12-16: Y ) Ph 2 P, PhS, PhCdNPh, CH 2 dCHCH 2 , PhNHCdS), whereas its reaction with CS 2 followed by treatment with RX yielded complexes [(µ-Y)Fe 2 (CO) 6 ] 3 [1,3,5-(µ-SCH 2 ) 3 C 6 H 3 ] (17-19: Y ) MeSCdS, PhCH 2 SCdS, CH 2 dCHCH 2 SCdS). All the starlike complexes 5-19 contain three terminal butterfly Fe/S cluster cores, which have been fully characterized by elemental analysis and spectroscopy, and particularly by X-ray diffraction techniques for 5, 12, 15, and 17.

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Polydentate Phosphines: Their Syntheses, Structural Aspects, and Selected Applications

Cotton

Hong

1992

Progress in Inorganic Chemistry

103

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Phosphororganische Verbindungen, XXVIII. Diarylchlorphosphine aus Aryldichlorphosphinen durch Disproportionierung

Abstract: Jahrg. 94 4-Hydroxy-cyclohexadien-(2S)-carbonsaure-( I )-essigsaure-(1)-diaihylesier ( I l)

Cited by 23 publications

References 12 publications

Formation and Chemical Reactivities of a New Type of Double‐Butterfly [{Fe₂(μ‐CO)(CO)₆}₂(μ‐SZS‐μ)]²⁻: Synthetic and Structural Studies on Novel Linear and Macrocyclic Butterfly Fe/E (E=S, Se) Cluster Complexes

Formation and Chemical Reactivities of a New Type of Double‐Butterfly [{Fe₂(μ‐CO)(CO)₆}₂(μ‐SZS‐μ)]²⁻: Synthetic and Structural Studies on Novel Linear and Macrocyclic Butterfly Fe/E (E=S, Se) Cluster Complexes

Polydentate Phosphines: Their Syntheses, Structural Aspects, and Selected Applications

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Phosphororganische Verbindungen, XXVIII. Diarylchlorphosphine aus Aryldichlorphosphinen durch Disproportionierung

Abstract: Jahrg. 94 4-Hydroxy-cyclohexadien-(2S)-carbonsaure-( I )-essigsaure-(1)-diaihylesier ( I l)

Cited by 23 publications

References 12 publications

Formation and Chemical Reactivities of a New Type of Double‐Butterfly [{Fe2(μ‐CO)(CO)6}2(μ‐SZS‐μ)]2−: Synthetic and Structural Studies on Novel Linear and Macrocyclic Butterfly Fe/E (E=S, Se) Cluster Complexes

Formation and Chemical Reactivities of a New Type of Double‐Butterfly [{Fe2(μ‐CO)(CO)6}2(μ‐SZS‐μ)]2−: Synthetic and Structural Studies on Novel Linear and Macrocyclic Butterfly Fe/E (E=S, Se) Cluster Complexes

Synthesis and Characterization of Starlike Complexes Containing Three Terminal Butterfly Fe/S Cluster Cores Generated via Reactions of the Three-μ-CO-Containing Trianions {[(μ-CO)Fe2(CO)6]3[(μ-SCH2CH2)3N]}3- and {[(μ-CO)Fe2(CO)6]3[1,3,5-(μ-SCH2)3C6H3]}3- with Electrophiles

Polydentate Phosphines: Their Syntheses, Structural Aspects, and Selected Applications

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Formation and Chemical Reactivities of a New Type of Double‐Butterfly [{Fe₂(μ‐CO)(CO)₆}₂(μ‐SZS‐μ)]²⁻: Synthetic and Structural Studies on Novel Linear and Macrocyclic Butterfly Fe/E (E=S, Se) Cluster Complexes

Formation and Chemical Reactivities of a New Type of Double‐Butterfly [{Fe₂(μ‐CO)(CO)₆}₂(μ‐SZS‐μ)]²⁻: Synthetic and Structural Studies on Novel Linear and Macrocyclic Butterfly Fe/E (E=S, Se) Cluster Complexes