Synthesis and coordination chemistry of pyrimidine-substituted phosphine ligands

T.D. Nixon; A.J. Gamble; R.J. Thatcher; A.C. Whitwood; J.M. Lynam

doi:10.1016/j.ica.2011.10.058

Synthesis and coordination chemistry of pyrimidine-substituted phosphine ligands

T.D. Nixon, A.J. Gamble, R.J. Thatcher, A.C. Whitwood, J.M. Lynam

Research output: Contribution to journal › Article › peer-review

Abstract

Reaction of PPh2H with UrI (Ur = uracil) in the presence of Pd(OAc)2 affords PPh2Ur. In the solid state, PPh2Ur crystallises as a methanol solvate in the monoclinic space group P21/c. Reaction of PPh2Ur with CuI in dry and deoxygenated THF solution results in the formation of [Cu4(μ3-I)4(PPh2Ur)4]. A single crystal X-ray diffraction study demonstrated that this species contains a distorted tetrahedral core of copper atoms, with facially-capping iodides. The uracil groups in the clusters are engaged in hydrogen bonding to groups on neighbouring molecules to form an extended array. A similar reaction between PPh2Ur and CuI in unpurified THF allows for the isolation of the phosphine oxide P(O)PPh2Ur. The synthesis of the benzyl-protected phosphine PPh2UrP is also described [UrP = 2,4-bis(benzyloxy)pyrimidine]. Reaction of PPh2UrP with [Ru(η5-C5H5)(NCMe)3]PF6 allows for isolation of [Ru(η5-C5H5)(NCMe)(PPh2UrP)2]PF6.

Original language	English
Pages (from-to)	252-260
Journal	INORGANICA CHIMICA ACTA
Volume	380
Issue number	1
DOIs	https://doi.org/10.1016/j.ica.2011.10.058
Publication status	Published - 15 Jan 2012

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title = "Synthesis and coordination chemistry of pyrimidine-substituted phosphine ligands",

abstract = "Reaction of PPh2H with UrI (Ur = uracil) in the presence of Pd(OAc)2 affords PPh2Ur. In the solid state, PPh2Ur crystallises as a methanol solvate in the monoclinic space group P21/c. Reaction of PPh2Ur with CuI in dry and deoxygenated THF solution results in the formation of [Cu4(μ3-I)4(PPh2Ur)4]. A single crystal X-ray diffraction study demonstrated that this species contains a distorted tetrahedral core of copper atoms, with facially-capping iodides. The uracil groups in the clusters are engaged in hydrogen bonding to groups on neighbouring molecules to form an extended array. A similar reaction between PPh2Ur and CuI in unpurified THF allows for the isolation of the phosphine oxide P(O)PPh2Ur. The synthesis of the benzyl-protected phosphine PPh2UrP is also described [UrP = 2,4-bis(benzyloxy)pyrimidine]. Reaction of PPh2UrP with [Ru(η5-C5H5)(NCMe)3]PF6 allows for isolation of [Ru(η5-C5H5)(NCMe)(PPh2UrP)2]PF6.",

author = "T.D. Nixon and A.J. Gamble and R.J. Thatcher and A.C. Whitwood and J.M. Lynam",

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T1 - Synthesis and coordination chemistry of pyrimidine-substituted phosphine ligands

AU - Nixon, T.D.

AU - Gamble, A.J.

AU - Thatcher, R.J.

AU - Whitwood, A.C.

AU - Lynam, J.M.

PY - 2012/1/15

Y1 - 2012/1/15

N2 - Reaction of PPh2H with UrI (Ur = uracil) in the presence of Pd(OAc)2 affords PPh2Ur. In the solid state, PPh2Ur crystallises as a methanol solvate in the monoclinic space group P21/c. Reaction of PPh2Ur with CuI in dry and deoxygenated THF solution results in the formation of [Cu4(μ3-I)4(PPh2Ur)4]. A single crystal X-ray diffraction study demonstrated that this species contains a distorted tetrahedral core of copper atoms, with facially-capping iodides. The uracil groups in the clusters are engaged in hydrogen bonding to groups on neighbouring molecules to form an extended array. A similar reaction between PPh2Ur and CuI in unpurified THF allows for the isolation of the phosphine oxide P(O)PPh2Ur. The synthesis of the benzyl-protected phosphine PPh2UrP is also described [UrP = 2,4-bis(benzyloxy)pyrimidine]. Reaction of PPh2UrP with [Ru(η5-C5H5)(NCMe)3]PF6 allows for isolation of [Ru(η5-C5H5)(NCMe)(PPh2UrP)2]PF6.

AB - Reaction of PPh2H with UrI (Ur = uracil) in the presence of Pd(OAc)2 affords PPh2Ur. In the solid state, PPh2Ur crystallises as a methanol solvate in the monoclinic space group P21/c. Reaction of PPh2Ur with CuI in dry and deoxygenated THF solution results in the formation of [Cu4(μ3-I)4(PPh2Ur)4]. A single crystal X-ray diffraction study demonstrated that this species contains a distorted tetrahedral core of copper atoms, with facially-capping iodides. The uracil groups in the clusters are engaged in hydrogen bonding to groups on neighbouring molecules to form an extended array. A similar reaction between PPh2Ur and CuI in unpurified THF allows for the isolation of the phosphine oxide P(O)PPh2Ur. The synthesis of the benzyl-protected phosphine PPh2UrP is also described [UrP = 2,4-bis(benzyloxy)pyrimidine]. Reaction of PPh2UrP with [Ru(η5-C5H5)(NCMe)3]PF6 allows for isolation of [Ru(η5-C5H5)(NCMe)(PPh2UrP)2]PF6.

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Synthesis and coordination chemistry of pyrimidine-substituted phosphine ligands

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