Neutral and cationic carbonyl complexes of manganese with tetramethylthiourea. Crystal structure of cis-{Mn(CO)4(SC[N(CH3)2]2)2} CIO4

Carriedo, C.; Sanchez, M.; Carriedo, Gabino A.; Soláns, Xavier; Valín, M. Luz

doi:10.1016/s0022-328x(00)98913-7

Cited by 10 publications

(2 citation statements)

References 33 publications

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“…Interestingly, however, the bis-TMTU complexes feature a rather acute S–M–S angle of ca. 78° similar to that observed for the cationic manganese analogue, cis -[Mn(CO) 4 (TMTU) 2 ](ClO 4 ) …”

Section: Resultssupporting

confidence: 76%

“…78°similar to that observed for the cationic manganese analogue, cis-[Mn(CO) 4 -(TMTU) 2 ](ClO 4 ). 67 The solution dynamics of the bis-TMTU complexes were found to be quite different from those of related [M(CO) 4 L 2 ] compounds (e.g., L = PR 3 ). 68 In no instance was any evidence found for isomerization of the cis isomers to the sterically lessencumbered trans isomers.…”

Section: ■ Introductionmentioning

confidence: 86%

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Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS₂ and WS₂

et al. 2014

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The molybdenum(0) and tungsten(0) carbonyl complexes, [M(CO) n (TMTU) 6−n ] (M = Mo and W; TMTU = tetramethylthiourea; n = 4 and 5), have been prepared by addition of TMTU to the appropriate carbonyl precursors. In the solid state, the compounds are monomeric and feature octahedral coordination geometries about the metal. In the case of [M(CO) 4 (TMTU) 2 ], the TMTU ligands are bound in a cis fashion. Dissolution of cis-[M(CO) 4 (TMTU) 2 ] produces an equilibrium mixture of cis-[M(CO) 4 (TMTU) 2 ], free TMTU, and the putative dimeric species, cis,cis-[M 2 (CO) 8 -(μ-TMTU) 2 ]. Attempts to prepare the tricarbonyl complex, [Mo(CO) 3 (TMTU) 3 ], by addition of TMTU to fac-[Mo-(CO) 3 (η 6 -cycloheptatriene)] results in isolation of cis-[Mo-(CO) 4 (TMTU) 2 ], demonstrating that exchange of CO and TMTU ligands is facile in these compounds. Each of the compounds decomposes readily in the solid state above 110 °C, ultimately forming the tetravalent metal disulfide. Thermolysis reactions of [M(CO) n (TMTU) 6−n ] complexes at 300 °C under an argon atmosphere produces amorphous MS 2 , establishing the utility of these compounds as precursors to molybdenum and tungsten disulfide materials under relatively mild conditions.

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Section: Resultssupporting

confidence: 76%

Section: ■ Introductionmentioning

confidence: 86%

Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS₂ and WS₂

et al. 2014

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Formation of the Salt‐like Complexes [Co{S₂CC(PPh₃)₂}₃][Co(CO)₄]₃ and [(CO)₄Mn{S₂CC(PPh₃)₂}][Mn(CO)₅] from the Reaction of the Related Carbonyl Compounds with S₂CC(PPh₃)₂

Petz

Neumüller

Hehl

2006

Zeitschrift anorg allge chemie

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The betain-like compound S 2 CC(PPh 3 ) 2 (1), which is obtained from CS 2 and the double ylide C(PPh 3 ) 2 , reacts with [Co 2 (CO) 8 ] and [Mn 2 (CO) 10 ] in THF to afford the salt-like complexes [Co{S 2 CC(PPh 3 ) 2 } 3 ][Co(CO) 4 ] 3 (2) a n d [(CO) 4 Mn{S 2 CC(PPh 3 ) 2 }][Mn(CO) 5 ] (3), respectively, in good yields. At both d 6 cations 1 acts as a chelating ligand. Disproportionation reactions from formal Co 0 into Co III and Co ϪI and from Mn 0 into Mn I and Mn ϪI occurred with the removal of four or one carbonyl groups, respectively. The crystal structures of 2·5.5THF and 3·2THF are reported, which show a shortening of the CϪC bond in the ligand upon complex formation. The compounds are further characterized by 31 P NMR and IR spectroscopy.

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The Ylide Adduct SOC₂(PPh₃)₂ as Complex Ligand. Reaction with [Mn₂(CO)₁₀] and InCl₃; Crystal Structures of [(CO)₄Mn(SOC₂{PPh₃}₂)₂][Mn(CO)₅] and (H₂C{PPh₃}₂)[InCl₄]₂

Petz

Fahlbusch

Gromm

et al. 2008

Zeitschrift anorg allge chemie

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The betain-like SOC 2 (PPh 3 ) 2 (1a) reacts with [Mn 2 (CO) 10 ] in THF to produce the salt-like complex [(CO) 4 Mn(SOC 2 {PPh 3 } 2 ) 2 ][Mn(CO) 5 ] (2). 1a is bonded via the sulfur atoms which are arranged in trans position in the octahedral environment of the manganese atom. With InCl 3 from CH 2 Cl 2 solution the addition product [Cl 3 In(SOC 2 {PPh 3 } 2 )] (3) is obtained along with the salt (H 2 C{PPh 3 } 2 )[InCl 4 ] 2 (4), which is the result of proton abstraction from the solvent. The crystal structures of 2 · 0.5THF and 4 · CH 2 Cl 2 are reported. The compounds are further characterized by IR and 31 P NMR spectroscopy.

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Neutral and cationic carbonyl complexes of manganese with tetramethylthiourea. Crystal structure of cis-{Mn(CO)4(SC[N(CH3)2]2)2} CIO4

Cited by 10 publications

References 33 publications

Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS₂ and WS₂

Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS₂ and WS₂

Formation of the Salt‐like Complexes [Co{S₂CC(PPh₃)₂}₃][Co(CO)₄]₃ and [(CO)₄Mn{S₂CC(PPh₃)₂}][Mn(CO)₅] from the Reaction of the Related Carbonyl Compounds with S₂CC(PPh₃)₂

The Ylide Adduct SOC₂(PPh₃)₂ as Complex Ligand. Reaction with [Mn₂(CO)₁₀] and InCl₃; Crystal Structures of [(CO)₄Mn(SOC₂{PPh₃}₂)₂][Mn(CO)₅] and (H₂C{PPh₃}₂)[InCl₄]₂

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Neutral and cationic carbonyl complexes of manganese with tetramethylthiourea. Crystal structure of cis-{Mn(CO)4(SC[N(CH3)2]2)2} CIO4

Cited by 10 publications

References 33 publications

Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS2 and WS2

Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS2 and WS2

Formation of the Salt‐like Complexes [Co{S2CC(PPh3)2}3][Co(CO)4]3 and [(CO)4Mn{S2CC(PPh3)2}][Mn(CO)5] from the Reaction of the Related Carbonyl Compounds with S2CC(PPh3)2

The Ylide Adduct SOC2(PPh3)2 as Complex Ligand. Reaction with [Mn2(CO)10] and InCl3; Crystal Structures of [(CO)4Mn(SOC2{PPh3}2)2][Mn(CO)5] and (H2C{PPh3}2)[InCl4]2

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Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS₂ and WS₂

Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS₂ and WS₂

Formation of the Salt‐like Complexes [Co{S₂CC(PPh₃)₂}₃][Co(CO)₄]₃ and [(CO)₄Mn{S₂CC(PPh₃)₂}][Mn(CO)₅] from the Reaction of the Related Carbonyl Compounds with S₂CC(PPh₃)₂

The Ylide Adduct SOC₂(PPh₃)₂ as Complex Ligand. Reaction with [Mn₂(CO)₁₀] and InCl₃; Crystal Structures of [(CO)₄Mn(SOC₂{PPh₃}₂)₂][Mn(CO)₅] and (H₂C{PPh₃}₂)[InCl₄]₂