Terpyridine - Ruthenium Complexes as Building Blocks for New Metallo-Supramolecular Architectures

2004 ◽  
Vol 57 (5) ◽  
pp. 419 ◽  
Author(s):  
Harald Hofmeier ◽  
Philip R. Andres ◽  
Richard Hoogenboom ◽  
Eberhardt Herdtweck ◽  
Ulrich S. Schubert
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Functional Groups ◽  
Building Blocks ◽  
Two Dimensional ◽  
X Ray ◽  
Supramolecular Architectures ◽  
Directed Synthesis ◽  
Materials Research ◽  
Terpyridine Ligands

Supramolecular architectures are of great interest in modern materials research. The directed synthesis of asym-metric 2,2′:6′,2′′-terpyridine ruthenium(II) complexes is an important tool towards such systems. In this contribution, we report the synthesis of asymmetric terpyridine ruthenium(II) complexes as models for supramolecular architectures and polymers. Terpyridines, bearing different functional groups in the 4′-position, were complexed with unfunctionalized terpyridine ligands using Ru(III)/Ru(II) chemistry. The resulting compounds were characterized by UV-vis, one- and two-dimensional NMR spectroscopy as well as MALDI-TOF mass spectrometry. In addition, X-ray structure analysis was performed for one selected example.

scholarly journals Bathyptilones: Terpenoids from an Antarctic Sea Pen, Anthoptilum grandiflorum (Verrill, 1879)

Marine Drugs ◽  
2019 ◽  
Vol 17 (9) ◽  
pp. 513 ◽  
Author(s):  
Santana A.L. Thomas ◽  
Anthony Sanchez ◽  
Younghoon Kee ◽  
Nerida G. Wilson ◽  
Bill J. Baker
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Cell Line ◽  
Structure Elucidation ◽  
Two Dimensional ◽  
Mammalian Cell Line ◽  
X Ray ◽  
X Ray Crystallography ◽  
Austral Autumn ◽  
Skeleton Structure

An Antarctic coral belonging to the order Pennatulacea, collected during the 2013 austral autumn by trawl from 662 to 944 m depth, has yielded three new briarane diterpenes, bathyptilone A-C (1–3) along with a trinorditerpene, enbepeanone A (4), which bears a new carbon skeleton. Structure elucidation was facilitated by one- and two-dimensional NMR spectroscopy, mass spectrometry and confirmed by X-ray crystallography. The three compounds were screened in four cancer cell lines. Bathyptilone A displayed selective nanomolar cytotoxicity against the neurogenic mammalian cell line Ntera-2.

Unusual Terpyridines as Ligands for Novel Light-Emitting Iridium(III) Complexes: Synthesis and Characterization

2006 ◽  
Vol 59 (11) ◽  
pp. 773 ◽  
Author(s):  
Andreas Winter ◽  
Christoph Ulbricht ◽  
Elisabeth Holder ◽  
Nikolaus Risch ◽  
Ulrich S. Schubert
Keyword(s):  
Mass Spectrometry ◽  
Optical Properties ◽  
Nmr Spectroscopy ◽  
Splitting Method ◽  
Synthesis And Characterization ◽  
Two Dimensional ◽  
Photoluminescence Spectra ◽  
Light Emitting ◽  
Yellow Orange ◽  
Terpyridine Ligands

Based on S-shaped terpyridines, a series of yellow, orange, and red-orange light-emitting iridium(iii) complexes has been synthesized. The respective compounds have been prepared by the bridge-splitting method starting from the dimeric precursor complexes [(ppy)2Ir-μ-Cl]2, [(ppy-CHO)2Ir-μ-Cl]2, and [(c6)2Ir-μ-Cl]2. The products have been fully characterized by one- and two-dimensional (1H–1H correlation) NMR spectroscopy, elemental analysis, and MALDI-TOF mass spectrometry revealing the successful coordination of the iridium(iii) centres to the S-shaped terpyridine ligands. Furthermore, the quantitative coordination has been verified by the photophysical and electrochemical properties of the mononuclear iridium(iii) complexes. The photoluminescence spectra have shown strong emissions with maxima between 538 and 600 nm. The study of the optical properties of these novel complexes has indicated that the colour shifts are mainly depending on the nature of the cyclometallating ligands.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

Neue Cyclophosphazene mit Metallen der III. Hauptgruppe als Ringbausteine / New Cyclophosphazenes with Metals of Main Group III as Building Blocks

1994 ◽  
Vol 49 (1) ◽  
pp. 43-49 ◽  
Author(s):  
Reinhard Hasselbring ◽  
Herbert W. Roesky ◽  
Andreas Heine ◽  
Dietmar Stalke ◽  
George M. Sheldrick
Keyword(s):  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Building Blocks ◽  
Main Group ◽  
Ring Formation ◽  
Lewis Acidity ◽  
X Ray ◽  
Group Iii ◽  
Space Groups ◽  
Ring Compounds

Abstract Acylic silylated phosphazenes of the type HN(PR2NSiMe3)2 (1) react quantitatively with molecules MMe3 (M = Al, Ga, In) under ring formation and CH4 evolution. The ring compounds N(PPh2NSiMe3)2AlMe2 (2 a) and N(PPh2NSiMe3)2InMe2 (4 a) have been investiga­ ted by X-ray structure determination. 2a and 4a crystallize in the space groups P 1̄ and P 31, respectively; they show different conformations regarding the cyclohexane framework. NMR spectroscopy of the nuclei in the chelating phosphazene ligand indicates decreasing Lewis acidity of the metal containing fragments in the series AlMe2 ≥ GaMe2 > InMe2.

Synthesis and characterization of new tetra-substituted porphyrins with exo-donor carboxylic groups as building blocks for supramolecular architectures: Catalytic and structural studies of their metalated derivatives

2010 ◽  
Vol 14 (09) ◽  
pp. 804-814 ◽  
Author(s):  
Lucia Carlucci ◽  
Gianfranco Ciani ◽  
Simona Maggini ◽  
Davide M. Proserpio ◽  
Fabio Ragaini ◽  
...  
Keyword(s):  
Building Blocks ◽  
Supramolecular Organization ◽  
Silver Complexes ◽  
Structural Studies ◽  
Polymeric Compound ◽  
X Ray ◽  
X Ray Crystallography ◽  
Supramolecular Architectures ◽  
Carboxylic Groups

We report herein the synthesis of the porphyrins 5,10,15,20-tetrakis(4-carboxybiphenyl)-porphyrin (H2TCBP) and 5,10,15,20-tetrakis(4-carboxy-2,6-dimethylbiphenyl)porphyrin (H2TCDMBP) bearing diphenyl units on meso-positions, and of their cobalt and silver derivatives. The silver complexes of H2TCDMBP and of H2TCPP ( H2TCPP = 5 ,10,15,20-tetrakis(4-carboxyphenyl)porphyrin) were investigated by X-ray crystallography and their supramolecular organization elucidated. Co(TCBP) was reacted with copper formate, yielding a polymeric compound that showed a catalytic activity in the benzylic amination of hydrocarbons using arylazide as aminating agent.

scholarly journals Ircinal E, a New Manzamine Derivative from the Indonesian Marine Sponge Acanthostrongylophora ingens

2015 ◽  
Vol 10 (11) ◽  
pp. 1934578X1501001 ◽  
Author(s):  
Mousa AlTarabeen ◽  
Georgios Daletos ◽  
Weaam Ebrahim ◽  
Werner E. G. Müller ◽  
Rudolf Hartmann ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
High Resolution ◽  
Cell Line ◽  
Marine Sponge ◽  
High Resolution Mass Spectrometry ◽  
Two Dimensional ◽  
Meoh Extract ◽  
L5178y Cell ◽  
Resolution Mass

Chemical investigation of the MeOH extract of the sponge Acanthostrongylophora ingens afforded the new manzamine derivative ircinal E (1), in addition to six known metabolites (2–7). The structure of the new compound was unequivocally elucidated using one- and two-dimensional NMR spectroscopy, as well as high-resolution mass spectrometry. Compounds 1–6 exhibited strong to moderate cytotoxicity against the murine lymphoma L5178Y cell line with IC50 values ranging from 2.8 to 21.7 μM.

Thiocarbonyl Complexes of Rhenium. Part I.

1993 ◽  
Vol 48 (6) ◽  
pp. 771-777 ◽  
Author(s):  
Ulrich Abram ◽  
Bernd Lorenz
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Space Group ◽  
X Ray ◽  
Monomeric Complex ◽  
Structure Solution ◽  
R Value

Novel rhenium complexes with terminal thiocarbonyl groups have been synthesized from ReCl3(Me2PhP)3 and sodium diethyldithiocarbamate. mer-(Diethyldithiocarbamato)tris-(dimethylphenylphosphine)(thiocarbonyl)rhenium(I), mer-[Re(CS)(Me2PhP)3(Et2dtc)], and tris(diethyldithiocarbamato)(thiocarbonyl)rhenium(III), [Re(CS)(Et2dtc)3] have been studied by infrared and NMR spectroscopy, mass spectrometry and X-ray diffraction.mer-[Re(CS)(Me2PhP)3(Et2dtc)] crystallizes orthorhombic in the space group Pna21 with a = 1516.1(2), b = 2189.8(2) and c = 1035.6(1) pm. Structure solution and refinement converged at R = 0.042. The coordination geometry is a distorted octahedron. The Re—C bond length is found to be 184(2) pm.[Re(CS)(Et2dtc)3] crystallizes monoclinic in the space group P21/c with a = 962.2(6), b = 1744.0(2), c = 1537.4(6) pm and β = 96.21(1)°. The final R value is 0.028. In the monomeric complex the rhenium atom is seven-coordinate with an approximate pentagonal-bipyramidal coordination sphere and a rhenium-carbon distance of 181(1) pm.

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