Synthesis and Single-crystal X-Ray Structure Determination of trans-PF6 (tmc=1,4,8,11-tetramethyl-1,4,8,11-tetra-azacyclotetradecane)

DOI: 10.1039/DT9880001561

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 1561 - 1564 (1988)

Update date:2022-07-29

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Authors:

Blake, Alexander J.

Reid, Gillian

Schroeder, Martin

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Article abstract of DOI:10.1039/DT9880001561

Reaction of RhCl3*3H2O with one molar equivalent of tmc (1,4,8,11-tetramethyl-1,4,8,11-tetra-azacyclotetradecane) in refluxing MeOH affords the complex cation (1+).The complex PF6 crystallises in the orthorhombic space group Pnma, with each anion and each cation lying on a crystallographic mirror plane.The single-crystal X-ray structure of the octahedral complex shows the chloride ions mutually trans to one another, Rh-Cl 2.355(3) and 2.362(3) Angstroem, with the tetra-aza macrocycle adopting an RRSS conformation with two methyl groups lying above, and two methyl groups lying below the RhN4 plane . trans-(1+) shows a quasi-reversible Rh^III-Rh^II redox couple at E_1/2=-0.99 V vs. -(1+) in MeCN; slow loss of chloride occurs on electrochemical reduction of the complex.

Full text of DOI:10.1039/DT9880001561

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