Structures and Dynamic Behavior of Large Polyhedral Coordination Cages: An Unusual Cage-to-Cage Interconversion
The bis-bidentate bridging ligand L {α,α′-bis[3-(2-pyridyl)pyrazol-1-yl]-1,4-dimethylbenzene}, which contains two chelating pyrazolyl-pyridine units connected to a 1,4-phenylene spacer via flexible methylene units, reacts with transition metal dications to form a range of polyhedral coordination cag...
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Published in | Journal of the American Chemical Society Vol. 133; no. 4; pp. 858 - 870 |
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Main Authors | , , , , |
Format | Journal Article |
Language | English |
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United States
American Chemical Society
02.02.2011
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Abstract | The bis-bidentate bridging ligand L {α,α′-bis[3-(2-pyridyl)pyrazol-1-yl]-1,4-dimethylbenzene}, which contains two chelating pyrazolyl-pyridine units connected to a 1,4-phenylene spacer via flexible methylene units, reacts with transition metal dications to form a range of polyhedral coordination cages based on a 2M:3 L ratio in which a metal ion occupies each vertex of a polyhedron, a bridging ligand lies along every edge, and all metal ions are octahedrally coordinated. Whereas the Ni(II) complex [Ni8L12](BF4)12(SiF6)2 is an octanuclear cubic cage of a type we have seen before, the Cu(II), Zn(II), and Cd(II) complexes form new structural types. [Cu6L9](BF4)12 is an unusual example of a trigonal prismatic cage, and both Zn(II) and Cd(II) form unprecedented hexadecanuclear cages [M16L24]X32(X = ClO4 or BF4) whose core is a skewed tetracapped truncated tetrahedron. Both Cu6L9 and M16L24 cages are based on a cyclic helical M3L3 subunit that can be considered as a triangular “panel”, with the cages being constructed by interconnection of these (homochiral) panels with additional bridging ligands in different ways. Whereas [Cu6L9](BF4)12 is stable in solution (by electrospray mass spectrometry, ES-MS) and is rapidly formed by combination of Cu(BF4)2 and L in the correct proportions in solution, the hexadecanuclear cage [Cd16L24](BF4)32 formed on crystallization slowly rearranges in solution over a period of several weeks to the trigonal prism [Cd6L9](BF4)12, which was unequivocally identified on the basis of its 1H NMR spectrum. Similarly, combination of Cd(BF4)2 and L in a 2:3 ratio generates a mixture whose main component is the trigonal prism [Cd6L9](BF4)12. Thus the hexanuclear trigonal prism is the thermodynamic product arising from combination of Cd(II) and L in a 2:3 ratio in solution, and arises from both assembly of metal and ligand (minutes) and rearrangement of the Cd16 cage (weeks); the large cage [Cd16L24](BF4)32 is present as a minor component of a mixture of species in solution but crystallizes preferentially. |
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AbstractList | The bis-bidentate bridging ligand L {α,α'-bis[3-(2-pyridyl)pyrazol-1-yl]-1,4-dimethylbenzene}, which contains two chelating pyrazolyl-pyridine units connected to a 1,4-phenylene spacer via flexible methylene units, reacts with transition metal dications to form a range of polyhedral coordination cages based on a 2M:3 L ratio in which a metal ion occupies each vertex of a polyhedron, a bridging ligand lies along every edge, and all metal ions are octahedrally coordinated. Whereas the Ni(II) complex [Ni(8)L(12)](BF(4))(12)(SiF(6))(2) is an octanuclear cubic cage of a type we have seen before, the Cu(II), Zn(II), and Cd(II) complexes form new structural types. [Cu(6)L(9)](BF(4))(12) is an unusual example of a trigonal prismatic cage, and both Zn(II) and Cd(II) form unprecedented hexadecanuclear cages [M(16)L(24)]X(32)(X = ClO(4) or BF(4)) whose core is a skewed tetracapped truncated tetrahedron. Both Cu(6)L(9) and M(16)L(24) cages are based on a cyclic helical M(3)L(3) subunit that can be considered as a triangular "panel", with the cages being constructed by interconnection of these (homochiral) panels with additional bridging ligands in different ways. Whereas [Cu(6)L(9)](BF(4))(12) is stable in solution (by electrospray mass spectrometry, ES-MS) and is rapidly formed by combination of Cu(BF(4))(2) and L in the correct proportions in solution, the hexadecanuclear cage [Cd(16)L(24)](BF(4))(32) formed on crystallization slowly rearranges in solution over a period of several weeks to the trigonal prism [Cd(6)L(9)](BF(4))(12), which was unequivocally identified on the basis of its (1)H NMR spectrum. Similarly, combination of Cd(BF(4))(2) and L in a 2:3 ratio generates a mixture whose main component is the trigonal prism [Cd(6)L(9)](BF(4))(12). Thus the hexanuclear trigonal prism is the thermodynamic product arising from combination of Cd(II) and L in a 2:3 ratio in solution, and arises from both assembly of metal and ligand (minutes) and rearrangement of the Cd(16) cage (weeks); the large cage [Cd(16)L(24)](BF(4))(32) is present as a minor component of a mixture of species in solution but crystallizes preferentially. The bis-bidentate bridging ligand L {α,α′-bis[3-(2-pyridyl)pyrazol-1-yl]-1,4-dimethylbenzene}, which contains two chelating pyrazolyl-pyridine units connected to a 1,4-phenylene spacer via flexible methylene units, reacts with transition metal dications to form a range of polyhedral coordination cages based on a 2M:3 L ratio in which a metal ion occupies each vertex of a polyhedron, a bridging ligand lies along every edge, and all metal ions are octahedrally coordinated. Whereas the Ni(II) complex [Ni8L12](BF4)12(SiF6)2 is an octanuclear cubic cage of a type we have seen before, the Cu(II), Zn(II), and Cd(II) complexes form new structural types. [Cu6L9](BF4)12 is an unusual example of a trigonal prismatic cage, and both Zn(II) and Cd(II) form unprecedented hexadecanuclear cages [M16L24]X32(X = ClO4 or BF4) whose core is a skewed tetracapped truncated tetrahedron. Both Cu6L9 and M16L24 cages are based on a cyclic helical M3L3 subunit that can be considered as a triangular “panel”, with the cages being constructed by interconnection of these (homochiral) panels with additional bridging ligands in different ways. Whereas [Cu6L9](BF4)12 is stable in solution (by electrospray mass spectrometry, ES-MS) and is rapidly formed by combination of Cu(BF4)2 and L in the correct proportions in solution, the hexadecanuclear cage [Cd16L24](BF4)32 formed on crystallization slowly rearranges in solution over a period of several weeks to the trigonal prism [Cd6L9](BF4)12, which was unequivocally identified on the basis of its 1H NMR spectrum. Similarly, combination of Cd(BF4)2 and L in a 2:3 ratio generates a mixture whose main component is the trigonal prism [Cd6L9](BF4)12. Thus the hexanuclear trigonal prism is the thermodynamic product arising from combination of Cd(II) and L in a 2:3 ratio in solution, and arises from both assembly of metal and ligand (minutes) and rearrangement of the Cd16 cage (weeks); the large cage [Cd16L24](BF4)32 is present as a minor component of a mixture of species in solution but crystallizes preferentially. |
Author | Argent, Stephen P Stephenson, Andrew Tidmarsh, Ian S Ward, Michael D Riis-Johannessen, Thomas |
AuthorAffiliation | University of Bristol University of Sheffield |
AuthorAffiliation_xml | – name: University of Bristol – name: University of Sheffield |
Author_xml | – sequence: 1 givenname: Andrew surname: Stephenson fullname: Stephenson, Andrew – sequence: 2 givenname: Stephen P surname: Argent fullname: Argent, Stephen P – sequence: 3 givenname: Thomas surname: Riis-Johannessen fullname: Riis-Johannessen, Thomas – sequence: 4 givenname: Ian S surname: Tidmarsh fullname: Tidmarsh, Ian S – sequence: 5 givenname: Michael D surname: Ward fullname: Ward, Michael D email: m.d.ward@sheffield.ac.uk |
BackLink | https://www.ncbi.nlm.nih.gov/pubmed/21175180$$D View this record in MEDLINE/PubMed |
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Snippet | The bis-bidentate bridging ligand L {α,α′-bis[3-(2-pyridyl)pyrazol-1-yl]-1,4-dimethylbenzene}, which contains two chelating pyrazolyl-pyridine units connected... The bis-bidentate bridging ligand L {α,α'-bis[3-(2-pyridyl)pyrazol-1-yl]-1,4-dimethylbenzene}, which contains two chelating pyrazolyl-pyridine units connected... |
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Title | Structures and Dynamic Behavior of Large Polyhedral Coordination Cages: An Unusual Cage-to-Cage Interconversion |
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