Unusual slow-exchange cadmium-113 NMR spectra observed at ambient temperature for halide, cyanide, and mercaptide cadmium coordination compounds with benzimidazole ligands. Applications to cadmium-substituted metalloproteins

1986 ◽  
Vol 108 (15) ◽  
pp. 4254-4258 ◽  
Author(s):  
Michael F. Summers ◽  
Jacobus. Van Rijn ◽  
Jan. Reedijk ◽  
Luigi G. Marzilli
Keyword(s):  
Ambient Temperature ◽  
Coordination Compounds ◽  
Nmr Spectra ◽  
Slow Exchange

scholarly journals New 3-(2-pyridyl)-1,2,4-triazole derivatives and their palladium (II) complexes

2015 ◽  
Vol 3 (2) ◽  
pp. 115-118 ◽  
Author(s):  
Borys Zakharchenko ◽  
Dmytro Khomenko ◽  
Roman Doroschuk ◽  
Rostyslav Lampeka
Keyword(s):  
Coordination Compounds ◽  
Nmr Spectra ◽  
Lone Electron Pair ◽  
Electron Pair ◽  
Significant Shift ◽  
Amino Groups ◽  
Triazole Derivatives ◽  
Low Field ◽  
Triazole Ligand ◽  
Field Area

The article is devoted to investigation of coordination compounds of palladium (II) with 3-(2-pyridyl)-1,2,4-triazole derivatives containing amino groups. We syntesized 4 ligands and 4 new coordination compounds. An interesting after removing of BOC-protection, NH2-group is still uncoordinated. In 1H NMR spectra of complexes was a significant shift of the ortho-pyridine proton in a low-field area, which prove proposed structure. This may be due to its closeness to the lone electron pair of the nitrogen cycle of the second triazole ligand.

1.3-Dimethyl-1,3-diaza-2-R-5,6-benzo-2λ3-phosphorinan-4-one (R = F, Me2N, 2-Methylpiperidino, MeC(: 0 )N H -) als Liganden in Übergangsmetallkomplexen; Synthese und Struktur von Dichloro-Platin(II)- und Tetracarbonyl-Metall(O)- Koordinationsverbindungen (Metall = Cr, Mo und W) / 1.3-Dimethyl-1,3-diaza-2-R-5,6-benzo-2λ3-phosphorinan-4-ones (R = F, Me2N, 2-Methylpiperidino, MeC(: 0 )NH-) as Ligands in Transition-Metal Complexes; Synthesis and Structure of Dichloro-Platinum(II)- and Tetracarbonyl-Metal(0) Coordination Compounds (Metal = Cr, Mo and W)

1994 ◽  
Vol 49 (1) ◽  
pp. 100-110 ◽  
Author(s):  
Hans-Jürgen Plinta ◽  
Ion Neda ◽  
Reinhard Schmutzler
Keyword(s):  
Coordination Compounds ◽  
Nmr Spectra ◽  
Coupling Constants ◽  
Trans Isomers ◽  
Phosphorus Ligands ◽  
Tungsten Complexes ◽  
Significant Temperature ◽  
Derivatives Of ◽  
Cis Isomer

Abstract 1,3-Dimethyl-1,3-diaza-2-fluoro-5,6-benzo-1,3,2-phosphorinane-4-one (1) reacted with (COD)PtCl2 (COD = 1,5-cyclooctadiene) or K2PtCl4 to give the cis-dichloro-platinum(II) complex (2). The reactions of 1 with the tetracarbonyl norbornadiene derivatives of Cr, Mo and W furnished the complexes 3 - 6 . In the case of the chromium and tungsten complexes the trans-isomers 3 and 6 were formed, due to a cis-trans-isomerization. Room temperature and low temperature 31P NMR spectra of a mixture of 5 and 6 show no significant temperature dependence of the cis-trans equilibrium. The reaction of 1 with the pentacarbonyl tetrahydrofuran derivative of W led to the product 7. The spirophosphoranes 8 and 9 were obtained in low yields. The analogous reactions of 10, 15 and 20 with (COD)PtCl2 and the tetracarbonyl norbornadiene derivatives of Cr and Mo furnished the coordination compounds 11-14, 16-18, 21 and 23. In the case of all chromium complexes only the trans-isomers 11,16 and 21 were formed, whereas in the case of molybdenum cis-trans-isomer mixtures 12 and 13, as well as 17 and 18 were obtained. An attempt to obtain the cis-isomer of the molybdenum complex 22 failed. In the case of platinum the expected cis-complexes 14 and 23 were formed, while the attempted synthesis of 19 was unsuccessful. All these results are interpreted in terms of both steric and electronic factors. The ligands 1, 10, 15 and 20 coordinate via phosphorus. The validity of the concept of hard and soft acids and bases (HSAB) was confirmed. The characterization of 2 - 7 , 11-14, 16-18, 21 and 23 rests, especially, on their 1H, 13C and 31P NMR spectra, and their mass and infrared spectra. 31P - 31P coupling constants 2J(PP) for the cis-coordinated complexes 4, 5 and 14 involving two equivalent phosphorus ligands are also reported.

Metal Tetrahydroborates and Tetrahydroborato Metalates, 15 [1]. An 11B and 113Cd NMR Study of MBH4–CdCl2 Systems in Dimethylformamide and the X-Ray Structure of CdCl2 · 2 DMF

1990 ◽  
Vol 45 (11) ◽  
pp. 1463-1471 ◽  
Author(s):  
Gerald Linti ◽  
Heinrich Nöth ◽  
Martina Thomann
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Coordination Polymer ◽  
Ambient Temperature ◽  
Nmr Spectra ◽  
Carbonyl Oxygen ◽  
X Ray ◽  
Rapid Exchange ◽  
Nmr Study ◽  
In Cis

CdCl2 dissociates in dimethylformamide into the species Cd(DMF)62+, CdCl(DMF)5+ and CdCl3- as determined by 113Cd NMR spectroscopy. 11B and 113Cd NMR spectra of MBH4/CdCl2 solutions in this solvent show the presence of complexes [CdCl2-n(BH4)n+1]- with rapid exchange of BH4- and Cl- at ambient temperature. There is no evidence that Cd(BH4)2 is formed in a metathetical reaction.The crystal structure of CdCl2 · 2 DMF has been determined. It is a coordination polymer containing hexacoordinated Cd atoms with the DMF molecules in cis-position. Coordination of DMF occurs via the carbonyl oxygen atoms.

Reaktionen koordinierter Liganden, VI [1] Substituenteneinflüsse bei der Bildung von Tri- und Tetraphosphinen in der Koordinationssphäre von Übergangsmetallen / Reactions of Coordinated Ligands, VI [1]. Influence of Substituents on the Formation of Tri- and Tetraphosphines in the Coordination Sphere of Transition Metals

1980 ◽  
Vol 35 (1) ◽  
pp. 74-81 ◽  
Author(s):  
Othmar Stelzer ◽  
Norbert Weferling
Keyword(s):  
Transition Metals ◽  
Coordination Sphere ◽  
Coordination Compounds ◽  
Nmr Spectra ◽  
Influence Of Substituents

Abstract The lithiumphosphido complex cis-Mo(CO)4(Me2PLi)2 reacts with dichlorophosphines RPCl2(R = Ph, But) to give coordination compounds of tetraphosphines Me2P-PR-PR-PMe2, whereas the complex of the triphosphine cis-Mo(CO)4 (Ph2P-PMe-PPh2) is obtained starting with the lithiumphosphido complex cis-Mo(CO)4(Ph2PLi)2. Phenyldilithiumphosphine and the chlorophosphine complexes cis-Mo(CO)4(R2PCl)2 (R = Me, Ph) give in low yield cis-Mo(CO)4(R2P-PPh-PPh-PR2) and cis-Mo(CO)4(R2P-PPh-PR2). The mechanisms of these reactions are discussed. The {31P}1H- and {1H}31P-NMR spectra are analysed and correlated with the structures of these complexes.

Coordination compounds of indium. Part 44. The oxidation of indium(I) halides by tetrahalogeno-ortho-quinones

1988 ◽  
Vol 66 (11) ◽  
pp. 2935-2940 ◽  
Author(s):  
Theodore A. Annan ◽  
Dennis G. Tuck
Keyword(s):  
Coordination Compounds ◽  
Nmr Spectra ◽  
Dynamic Behaviour ◽  
Addition Product ◽  
Donor Ligands ◽  
Chelate Complexes ◽  
H Nmr ◽  
Anionic Complexes ◽  
Derivatives Of ◽  
C Nmr

The reaction of indium(I) halides (InX; X = Cl, Br, I) with tetrahalogeno-ortho-quinones (Y4C6O2; Y = Cl, Br) gives the oxidative addition product Y4C6O2InX, These compounds have been isolated as adducts with neutral bidentate donor ligands (N,N,N′,N′-tetramethylethanediamine (tmen), 1,10-phenanthroline) or as salts of the anionic complexes [Y4C6O2InCl2]− or [Y4C6O2In(Cl)Br]−. The number of coordinated tmen molecules, and hence the structure, depends on the method of preparation. Infrared, 1H NMR, and 13C NMR spectroscopy all confirm that these products are all substituted-catecholato derivatives of indium(III), and the structure of these various neutral or anionic derivatives is discussed. The temperature dependence of the 13C NMR spectra shows that the dynamic behaviour of these compounds (in d6-dmso) is similar to that observed in previous studies of indium(III) chelate complexes.

scholarly journals Die Struktur von Undecacarbonyl-(μ-trifluormethylisocyanid)trieisen Fe3(μ-CNCF3)(CO)11 in Lösung

1987 ◽  
Vol 42 (7) ◽  
pp. 839-842 ◽  
Author(s):  
Dieter Lentz
Keyword(s):  
Ambient Temperature ◽  
Time Scale ◽  
Nmr Spectra ◽  
C Nmr

Abstract According to its 13C NMR spectra, undecacarbonyl-(μ-trifluorom ethylisocyanide)triiron, Fe3(μ-CNCF3)(CO)11 , is only partly nonrigid in solution even at ambient temperature. However, on cooling to -100 °C the molecule is rigid on the NMR time scale.

Über die Reaktion sekundärer Amine mit Lithiumtetrahydridoaluminat

1988 ◽  
Vol 43 (9) ◽  
pp. 1101-1112 ◽  
Author(s):  
Gerald Linti ◽  
Heinrich Nöth ◽  
Peter Rahm
Keyword(s):  
Nmr Spectroscopy ◽  
Ambient Temperature ◽  
Nmr Spectra ◽  
Substitution Product ◽  
X Ray ◽  
Molar Ratios

Abstract Lithium-tris(diethylamino)hydridoaluminate, Lithium-bis(diisopropylamino)dihydridoaluminate. Lithium(tetramethylpiperidino)trihydridoaluminate, NMR Spectra, X-Ray Reactions of diethylamine, diisopropylamine and 2,2,6,6-tetramethylpiperidine with LiAlH4 in various ethers have been studied. Only two well-defined products result from Et2NH, namely LiAlH(NEt2)- and LiAl(NEt2)4 . If molar ratios of Et2NH:LiAlH4 smaller than 3:1 are employed all compounds of the series LiAlH4-n(NEt2)n (n = 0, 1, 2, 3) are present in solutions of tetra-hydrofuran and diglyme. In diethylether insoluble materials consisting predominantly of lithium diethylaminohydridoaluminates and, presumably, small quantities of Li3AlH6 are also formed. At ambient temperature diisopropylamine reacts slowly with LiAlH4 , and LiAlH2(NiPr2)2 can be isolated as a well-defined substitution product. 2,2,6,6-tetramethylpiperidine (tmpH) replaces only a single hydride from LiAlH4 with formation of LiAlH3 (tmp). The reactions have been monitored by 7Li, 13C and 27Al NMR spectroscopy, and the structure of LiAlH(NEt2)3 has been determined by X-ray analysis. The monoclinic compound contains chains of AlHN3 and LiHN3 tetrahedra linked through common edges.

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