Synthesis and X-ray Crystal Structure of trans-Mo(CO)4{Ph2P(CH2CH2O)4CH2CH2PPh2-P,P'}, a Molecular Gyroscope Formed by Trans Coordination of a Bis(phosphine) Ligand in an Octahedral Metal Complex

Gray, Gary M.; Duffey, Christina H.

doi:10.1021/om00017a002

Cited by 32 publications

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“…This observation is consistent with rapid rotation about the Os−Sn bonds in 1 so as to render the inner and outer carbonyl ligands equivalent. (A similar low-energy barrier to rotation is observed for the P−Mo−P bonds in trans -Mo(CO) 4 [Ph 2 P(CH 2 CH 2 O) 4 CH 2 CH 2 PPh 2 - P , P‘ ] …”

Section: Resultssupporting

confidence: 57%

Synthesis and Structure of [Os(CO)₄(SnPh₂)]₆: A Compound with an Unprecedented 12-Membered Ring of Metal Atoms

et al. 1997

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The compound [Os(CO)4(SnPh2)]6 (1) has been isolated as one product from the reaction of Na2[Os(CO)4] and Ph2SnCl2 in THF. The X-ray structure of 1 reveals it possesses an approximately planar 12-membered ring of alternating tin and osmium atoms. Carbon-13 NMR spectroscopy indicates there is free rotation about the Os−Sn bonds in 1 in solution so as to render all the carbonyl ligands equivalent.

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Section: Resultssupporting

confidence: 57%

Synthesis and Structure of [Os(CO)₄(SnPh₂)]₆: A Compound with an Unprecedented 12-Membered Ring of Metal Atoms

et al. 1997

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“…The crude product was characterized by its 1 H NMR spectrum and its successful use in the next step of the ligand synthesis. 6).…”

Section: Methodsmentioning

confidence: 99%

“…(ii) Preparation of 1,2-(Ph2P(CH2CH2O)2)2C6H4 (6). A solution of 50 mL of THF and 9.3 g (0.021 mol) of 1,2-(MsO-(CH2CH2O)2)2C6H4 in a 200 mL Schlenk flask was cooled to -78 °C in dry ice/acetone and then titrated to a persistent rose color with a 0.5 M solution of potassium diphenylphosphide in THF.…”

Section: Methodsmentioning

confidence: 99%

“…[1][2][3][4][5][6][7][8][9] Metallacrown ethers that contain the conformationally mobile Ph 2 P(CH 2 CH 2 O) 4 CH 2 CH 2 PPh 2 (1) ligand exhibit a variety of phosphine coordination geometries. These geometries include cis-octahedral (cis-Mo(CO) 4 {Ph 2 P(CH 2 CH 2 O) 4 CH 2 CH 2 PPh 2 -P,P′} (2) 4 ), trans-octahedral (trans-Mo(CO) 4 {Ph 2 P(CH 2 CH 2 O) 4 CH 2 -CH 2 PPh 2 -P,P′} (3) 6 and cis,cis,trans-RuCl 2 (CO) 2 {Ph 2 P-(CH 2 CH 2 O) 4 CH 2 CH 2 PPh 2 -P,P′} (4) 7 ), and cis-square planar (cis-PtCl 2 {Ph 2 P(CH 2 CH 2 O) 4 CH 2 CH 2 PPh 2 -P,P′} (5) 5 ). Complex 2 binds alkali metal cations, methanol, and water 9 and also rapidly isomerizes into 3 in the presence of HgCl 2 .…”

Section: Introductionmentioning

confidence: 99%

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Conformationally Restrained Octahedral Metallacrown Ethers with 1,2-(Ph₂P(CH₂CH₂O)₂)₂C₆H₄ Ligands. X-ray Crystal Structure of cis-Mo(CO)₄{1,2-(Ph₂P(CH₂CH₂O)₂)₂C₆H₄-P,P‘}

1998

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A new R,ω-bis(phosphine)-polyether ligand, 1,2-(Ph 2 P(CH 2 CH 2 O) 2 ) 2 C 6 H 4 , has been synthesized and used to prepare a number of conformationally restrained metallacrown ethers. The reaction of 1,2-(Ph 2 P(CH 2 CH 2 O) 2 ) 2 C 6 H 4 and Mo(CO) 4 (nbd) gives a good yield of cis-Mo-(CO) 4 {1,2-(Ph 2 P(CH 2 CH 2 O) 2 ) 2 C 6 H 4 -P,P′}. This complex has been isomerized to trans-Mo-(CO) 4 {1,2-(Ph 2 P(CH 2 CH 2 O) 2 ) 2 C 6 H 4 -P,P′} using both UV light and HgCl 2 catalysis. The reaction of 1,2-(Ph 2 P(CH 2 CH 2 O) 2 ) 2 C 6 H 4 with fac-RuCl 2 (CO) 3 (THF) initially yields a mixture of monomeric and oligomeric cis,cis,trans-[RuCl 2 (CO) 2 {1,2-(Ph 2 P(CH 2 CH 2 O) 2 ) 2 C 6 H 4 -P,P′}] n metallacrown ethers. Surprisingly, the oligomeric metallacrown ethers slowly convert into the monomeric metallacrown ether at ambient temperature in a chloroform-d solution. This does not occur with the conformationally mobile [cis,cis,trans-RuCl 2 (CO) 2 {Ph 2 P(CH 2 CH 2 O) 4 -CH 2 CH 2 PPh 2 -P,P′}] n metallacrown ethers. The X-ray crystal structure of cis-Mo(CO) 4 {1,2-(Ph 2 P(CH 2 CH 2 O) 2 ) 2 C 6 H 4 -P,P′} has also been determined. The four ether oxygens lie in a plane, and the average cross-ring oxygen-oxygen distance is slightly larger than those in metallacrown ethers containing Ph 2 P(CH 2 CH 2 O) 4 CH 2 CH 2 PPh 2 ligands.

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“…[96][97][98] Metallacrown ethers [99][100][101][102][103] and metallacalixarenes [104][105][106][107][108][109][110] are interesting transition-metal analogues to crown ethers and calixarenes that preserve their guest-binding functionality. Since crown ethers are excellent hosts for hard metal cations and calixarenes have a high affinity for neutral guests, they are expected to extend the functionality of molecular squares when combined into a single supramolecular assembly.…”

Section: Scheme 33mentioning

confidence: 99%

Self-Assembly of Discrete Cyclic Nanostructures Mediated by Transition Metals

2000

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Synthesis and X-ray Crystal Structure of trans-Mo(CO)4{Ph2P(CH2CH2O)4CH2CH2PPh2-P,P'}, a Molecular Gyroscope Formed by Trans Coordination of a Bis(phosphine) Ligand in an Octahedral Metal Complex

Cited by 32 publications

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Synthesis and Structure of [Os(CO)₄(SnPh₂)]₆: A Compound with an Unprecedented 12-Membered Ring of Metal Atoms

Synthesis and Structure of [Os(CO)₄(SnPh₂)]₆: A Compound with an Unprecedented 12-Membered Ring of Metal Atoms

Conformationally Restrained Octahedral Metallacrown Ethers with 1,2-(Ph₂P(CH₂CH₂O)₂)₂C₆H₄ Ligands. X-ray Crystal Structure of cis-Mo(CO)₄{1,2-(Ph₂P(CH₂CH₂O)₂)₂C₆H₄-P,P‘}

Self-Assembly of Discrete Cyclic Nanostructures Mediated by Transition Metals

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Synthesis and X-ray Crystal Structure of trans-Mo(CO)4{Ph2P(CH2CH2O)4CH2CH2PPh2-P,P'}, a Molecular Gyroscope Formed by Trans Coordination of a Bis(phosphine) Ligand in an Octahedral Metal Complex

Cited by 32 publications

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Synthesis and Structure of [Os(CO)4(SnPh2)]6: A Compound with an Unprecedented 12-Membered Ring of Metal Atoms

Synthesis and Structure of [Os(CO)4(SnPh2)]6: A Compound with an Unprecedented 12-Membered Ring of Metal Atoms

Conformationally Restrained Octahedral Metallacrown Ethers with 1,2-(Ph2P(CH2CH2O)2)2C6H4 Ligands. X-ray Crystal Structure of cis-Mo(CO)4{1,2-(Ph2P(CH2CH2O)2)2C6H4-P,P‘}

Self-Assembly of Discrete Cyclic Nanostructures Mediated by Transition Metals

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Synthesis and Structure of [Os(CO)₄(SnPh₂)]₆: A Compound with an Unprecedented 12-Membered Ring of Metal Atoms

Synthesis and Structure of [Os(CO)₄(SnPh₂)]₆: A Compound with an Unprecedented 12-Membered Ring of Metal Atoms

Conformationally Restrained Octahedral Metallacrown Ethers with 1,2-(Ph₂P(CH₂CH₂O)₂)₂C₆H₄ Ligands. X-ray Crystal Structure of cis-Mo(CO)₄{1,2-(Ph₂P(CH₂CH₂O)₂)₂C₆H₄-P,P‘}