Mono-, di- and tetra-nuclear p-cymeneruthenium complexes containing oxalato ligands

Yan, Hong; Süß‐Fink, Georg; Neels, Antonia; Stœckli-Evans, Helen

doi:10.1039/a704658h

Cited by 165 publications

(126 citation statements)

References 29 publications

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“…The IR spectra of 2, 5, 9, and 10, as well as the already reported metalla-cubes 1, 3, 4, and 6, are dominated by absorptions of the coordinated porphyrin panels with, in particular, a strong in-plane N-H deformation at ,1220 cm À1 observed in 1, 4, 9, and 10, [18] and the bands assigned to the C¼C and C¼N skeletal modes of the porphyrins located between 1620 and 1400 cm À1 . [19] Moreover, the bands associated with the OO\OO bridges, including the strong C¼O stretching vibration (at ,1530 cm À1 ), are only slightly shifted compared with the corresponding vibrations observed in the dinuclear complexes [Ru 2 (p-cymene) 2 (C 2 O 4 )Cl 2 ] [20] and [Ru 2 (arene) 2 (C 6 H 2 O 4 ) Cl 2 ]. [12] In addition to the porphyrin and OO\OO absorptions, strong stretching vibrations due to the triflate anions (1260(s), 1030(s), 638(m) cm À1 ) are also observed in the IR spectra of the salts [1][2][3][4][5][6] Under the conditions of ESI-MS, all the metalla-cubes 1-6, 9, and 10 are remarkably stable.…”

Section: Characterizationmentioning

confidence: 94%

Synthesis, Characterization and Anticancer Activity of Porphyrin-Containing Organometallic Cubes

et al. 2010

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Self-assembly of 5,10,15,20-tetra(4-pyridyl)porphyrin (tpp-H 2 ) and 5,10,15,20-tetra(4-pyridyl) (10) respectively. All cationic metalla-cubes were isolated as triflate salts and characterized by NMR, infrared, electro-spray mass spectrometry and UV-visible spectroscopy. Moreover, the formation of unsymmetrical metalla-cubes built using a mixture of the different porphyrin panels during the self-assembly of the 2,5-dioxydo-1,4-benzoquinonato metalla-cubes, 8

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Section: Characterizationmentioning

confidence: 94%

Synthesis, Characterization and Anticancer Activity of Porphyrin-Containing Organometallic Cubes

et al. 2010

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“…{ From a structural point of view, the two tpt subunits are expected to be around 5.5 Å apart, based on the Ru-Ru separation observed in 3 (mean 5.503(6) Å ). 8 Indeed, the single-crystal X-ray structure analyses of 1 and 2 reveal an average Ru-Ru separation of 5.49 Å . Surprisingly, the two central triazine units in 2 are very close.…”

mentioning

confidence: 97%

“…Compounds 1 and 2 were prepared following a two-step strategy in which the known dinuclear oxalato complex [Ru 2 (p-Pr i C 6 H 4 Me) 2 (C 2 O 4 )Cl 2 ] (3) 8 and the new oxalato dinuclear complex [Ru 2 (C 6 Me 6 ) 2 (C 2 O 4 )Cl 2 ] (4) are used as metal ''clips'' (Scheme 1). The coordinatively unsaturated intermediate formed upon addition of AgOSO 2 CF 3 presumably allows the Ru 2 (arene) 2 (C 2 O 4 ) 2+ moities to adopt a syn geometry upon coordination to the tpt unit.…”

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confidence: 99%

Self-assembled hexanuclear arene ruthenium metallo-prisms with unexpected double helical chirality

et al. 2006

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Self-assembly of 2,4,6-tripyridyl-1,3,5-triazine (tpt) subunits with arene ruthenium building blocks and oxalato bridges affords cationic triangular metallo-prisms of the type [Ru 6 (arene) 6 (tpt) 2 (C 2 O 4 ) 3 ] 6+ (arene = C 6 Me 6 and p-Pr i C 6 -H 4 Me); the unexpected double helical chirality of the metalloprisms observed in the solid state persists in solution giving rise to two different stereodynamic processes as demonstrated by NMR enantiodifferentiation experiments.The self-assembly of transition metal complexes to give discrete supramolecular architectures has been studied by several groups and is the subject of some extensive reviews. 1 Both, two-and threedimensional architectures are known, in which the metal centres or the branched ligands or a combination of both control the shape of the resulting assemblies. The simplest three-dimensional construction which involves the fewest components is the triangular prism: only five building blocks are necessary to obtain a triangular prism; two trigonal subunits, and three linear connecting units. 2 However, metal-based triangular prisms including more components 3 are known as well. If no stereogenic elements are introduced within the components of the prism and the two planar triangular subunits perfectly eclipsed, the triangular prism possesses a D 3h symmetry, and is therefore achiral. However, a slight deviation from the eclipsed conformation reduces the achiral point group D 3h to the chiral D 3 symmetry group and therefore generates ''double-rosette'' type helicity with P or M configuration. 4 Moreover, concerted rotation of some aromatic rings of the tritopic subunits creates three-bladed propeller chirality with D (clockwise) or L (counterclockwise) configuration. Whereas either or both of these stereogenic elements can easily be detected in the solid state, so far, it has been hardly observed in solution, 5 the complexes being too configurationally labile or the system being achiral in solution.Herein we report the synthesis and characterisation of two cationic triangular metallo-prisms incorporating arene ruthenium building blocks, bridged by oxalato ligands, and connected by two 2,4,6-tripyridyl-1,3,5-triazine (tpt) subunits (Scheme 1). (1) and [Ru 6 (C 6 Me 6 ) 6 (tpt) 2 (C 2 O 4 ) 3 ] 6+ (2), which turned out to be quite soluble in (CH 3 ) 2 CO, CH 3 CN and MeOH, and only sparingly soluble in CH 2 Cl 2 and CHCl 3 .The molecular structures of 1 and 2 have been solved by singlecrystal X-ray analysis of the triflate salts, for the IR and NMR data see supporting information.{ From a structural point of view, the two tpt subunits are expected to be around 5.5 Å apart, based on the Ru-Ru separation observed in 3 (mean 5.503(6) Å ). 8 Indeed, the single-crystal X-ray structure analyses of 1 and 2 reveal an average Ru-Ru separation of 5.49 Å . Surprisingly, the two central triazine units in 2 are very close. The centroid … centroid distance between the two triazine moieties is only 3.42 Å as compared to 3.83 Å in 1, where the tpt ligands adopt an...

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“…The synthesis was modi ed from a procedure reported by Yan and co-workers [1]. To a solution of [Os(η 6 -p-cymene)Br] 2 (2.348 g, 2.33 mmol) in CH 2 Cl 2 -CH 3 OH (1:1, 40 mL) was added an excess of (NH4) 2 C 2 O4·H 2 O (4.180 g, 29.53 mmol).…”

Section: Source Of Materialsmentioning

confidence: 99%

Crystal structure of dibromido μ-oxalato-κ² O,O′:κ² O′′,O′′′−η⁶-p-cymenediosmium(II), C₂₂H₂₈Br₂O₄Os₂

Clayton

Tapala

Lemmerer

2016

Zeitschrift Für Kristallographie - New Crystal Structures

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CCDC no.: 1500900The title structure is shown in the gure. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters. Source of materialThe synthesis was modi ed from a procedure reported by Yan and co-workers [1]. To a solution of [Os(η 6 -p-cymene)Br] 2 (2.348 g, 2.33 mmol) in CH 2 Cl 2 -CH 3 OH (1:1, 40 mL) was added an excess of (NH4) 2 C 2 O4·H 2 O (4.180 g, 29.53 mmol). The mixture was stirred at room temperature overnight and

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Mono-, di- and tetra-nuclear p-cymeneruthenium complexes containing oxalato ligands

Cited by 165 publications

References 29 publications

Synthesis, Characterization and Anticancer Activity of Porphyrin-Containing Organometallic Cubes

Synthesis, Characterization and Anticancer Activity of Porphyrin-Containing Organometallic Cubes

Self-assembled hexanuclear arene ruthenium metallo-prisms with unexpected double helical chirality

Crystal structure of dibromido μ-oxalato-κ² O,O′:κ² O′′,O′′′−η⁶-p-cymenediosmium(II), C₂₂H₂₈Br₂O₄Os₂

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Mono-, di- and tetra-nuclear p-cymeneruthenium complexes containing oxalato ligands

Cited by 165 publications

References 29 publications

Synthesis, Characterization and Anticancer Activity of Porphyrin-Containing Organometallic Cubes

Synthesis, Characterization and Anticancer Activity of Porphyrin-Containing Organometallic Cubes

Self-assembled hexanuclear arene ruthenium metallo-prisms with unexpected double helical chirality

Crystal structure of dibromido μ-oxalato-κ2 O,O′:κ2 O′′,O′′′−η6-p-cymenediosmium(II), C22H28Br2O4Os2

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Crystal structure of dibromido μ-oxalato-κ² O,O′:κ² O′′,O′′′−η⁶-p-cymenediosmium(II), C₂₂H₂₈Br₂O₄Os₂