scholarly journals Synthesis of thiadiazolobenzamide via cyclization of thioxothiourea and its Ni and Pd complexes

2012 ◽  
Vol 77 (9) ◽  
pp. 1211-1222 ◽  
Author(s):  
Forogh Adhami ◽  
Nasim Nabilzadeh ◽  
Franziska Emmerling ◽  
Mina Ghiasi ◽  
Majid Heravi
Keyword(s):  
Mass Spectrometry ◽  
Hydrogen Sulfide ◽  
Membered Ring ◽  
X Ray ◽  
X Ray Crystallography ◽  
Thermal Gravimetry ◽  
Pd Complexes ◽  
Benzoyl Isothiocyanate ◽  
Shed Light

In this study, the new compound, N-(3-methyl-4- oxo[1,3,4]thiadiazolo[2,3-c][1,2,4]triazin-7-yl) benzamide, could be obtained via two different reactions: 1) reaction of 4-amino-6-Methyl-3- (Methylsulfanyl)-1,2,4-triazin-5-one with benzoyl isothiocyanate under removal of methylmercaptane, 2) reaction of 4-amino-6-Methyl-3-thioxo- 1,2,4-triazin-5-one with benzoyl isothiocyanate under elimination of hydrogen sulfide. In both reactions a new bond between sulfur and nitrogen atoms was formed and a five-membered ring was created. The oxo thiadiazolo benzamide was characterized by IR-, 1HNMR- and 13CNMR spectroscopy as well as by Mass spectrometry. X-ray crystallography was used to shed light on the structure of this new compound. Two new complexes could be generated by coordination of oxo thiadiazolo benzamide to Pd(II) and Ni(II) ions. These complexes have been analyzed by IR-, 1HNMR- and 13CNMR spectroscopy, conductometry and Thermal gravimetry (TGA). Theoretical QM Calculation GIAO has also been applied to predict the structure of the Pd complex.

scholarly journals 4-vinylpyridine derivatives: Protonation, methylation and silver(I) coordination chemistry

2021 ◽  
pp. 174751982198965
Author(s):  
Guoqi Zhang
Keyword(s):  
Mass Spectrometry ◽  
Schiff Base ◽  
Coordination Chemistry ◽  
Elemental Analysis ◽  
Silver Complex ◽  
Spectroscopic Techniques ◽  
X Ray ◽  
X Ray Crystallography ◽  
Pyridine Moiety ◽  
New Compounds

( E)-4-[2-(Pyridin-4-yl)vinyl]benzaldehyde, containing both a 4-vinylpyridine and an aldehyde functionality, is utilized to develop new, highly conjugated chalcone compounds and a bis-Schiff base azine compound. The chalcone-containing compounds are further explored for their protonation, methylation and silver(I) coordination chemistry using the pyridine moiety. In parallel, a cyano-containing analogue, ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile is also synthesized and studied for its silver(I) coordination chemistry. These new compounds are fully characterized by mass spectrometry, elemental analysis and spectroscopic techniques. The methylated product of ( E)-1-(9-anthryl)-3-{4-[2-(pyridin-4-yl)vinyl]phenyl}prop-2-en-1-one and a silver complex of ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile are structurally determined by X-ray crystallography.

Structural determination and characterization of copper and zinc bis-glycinates with X-ray crystallography and mass spectrometry

2010 ◽  
Vol 63 (19) ◽  
pp. 3335-3347 ◽  
Author(s):  
Sanjit Konar ◽  
Kevin Gagnon ◽  
Abraham Clearfield ◽  
Charles Thompson ◽  
Jennifer Hartle ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Structural Determination ◽  
X Ray ◽  
X Ray Crystallography ◽  
Copper And Zinc

scholarly journals Silylated gallium and indium chalcogenide ring systems as potential precursors to ME (E=O, S) materials

2013 ◽  
Vol 11 (7) ◽  
pp. 1225-1238
Author(s):  
Iliana Medina-Ramírez ◽  
Cynthia Floyd ◽  
Joel Mague ◽  
Mark Fink
Keyword(s):  
Thermal Decomposition ◽  
Room Temperature ◽  
Membered Ring ◽  
Molecular Structures ◽  
Nmr Studies ◽  
X Ray ◽  
X Ray Crystallography ◽  
High Yields ◽  
Vt Nmr ◽  
State 1

AbstractThe reaction of R3M (M=Ga, In) with HESiR′3 (E=O, S; R′3=Ph3, iPr3, Et3, tBuMe2) leads to the formation of (Me2GaOSiPh3)2(1); (Me2GaOSitBuMe2)2(2); (Me2GaOSiEt3)2(3); (Me2InOSiPh3)2(4); (Me2InOSitBuMe2)2(5); (Me2InOSiEt3)2(6); (Me2GaSSiPh3)2(7); (Et2GaSSiPh3)2(8); (Me2GaSSiiPr3)2(9); (Et2GaSSiiPr3)2(10); (Me2InSSiPh3)3(11); (Me2InSSiiPr3)n(12), in high yields at room temperature. The compounds have been characterized by multinuclear NMR and in most cases by X-ray crystallography. The molecular structures of (1), (4), (7) and (8) have been determined. Compounds (3), (6) and (10) are liquids at room temperature. In the solid state, (1), (4), (7) and (9) are dimers with central core of the dimer being composed of a M2E2 four-membered ring. VT-NMR studies of (7) show facile redistribution between four- and six-membered rings in solution. The thermal decomposition of (1)–(12) was examined by TGA and range from 200 to 350°C. Bulk pyrolysis of (1) and (2) led to the formation of Ga2O3; (4) and (5) In metal; (7)–(10) GaS and (11)–(12) InS powders, respectively.

scholarly journals Simple Methylcadmium Alkoxides

2007 ◽  
Vol 62 (10) ◽  
pp. 1339-1342 ◽  
Author(s):  
Surajit Jana ◽  
Tania Pape ◽  
Norbert W. Mitzel
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Molecular Formula ◽  
Equimolar Ratio ◽  
X Ray ◽  
X Ray Crystallography ◽  
Elemental Analyses ◽  
Solid State Structures ◽  
Structural Aspects ◽  
C Nmr

The reaction of dimethylcadmium with alcohols R-OH in equimolar ratio leads to the formation of tetrameric methylcadmium alkoxides with molecular formula [(MeCd)4 (OR)4] [R = Me (1), Et (2) and iPr (3)]. These compounds have been characterised by 1H, 13C NMR and IR spectroscopy, by mass spectrometry, elemental analyses and by X-ray crystallography (for 2 and 3). The solid state structures show distorted cubane-type aggregates with Cd4O4 cores. The structural aspects and the spectroscopic characterisations of these compounds are discussed.

Mapping the protein-binding sites for iridium(iii)-based CO-releasing molecules

2016 ◽  
Vol 45 (30) ◽  
pp. 12206-12214 ◽  
Author(s):  
Marco Caterino ◽  
Ariel A. Petruk ◽  
Alessandro Vergara ◽  
Giarita Ferraro ◽  
Daniela Marasco ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Protein Binding ◽  
Binding Sites ◽  
Raman Microspectroscopy ◽  
Rnase A ◽  
Protein Binding Sites ◽  
X Ray ◽  
X Ray Crystallography ◽  
Model Protein ◽  
Circular Dichroïsm

Mass spectrometry, Raman microspectroscopy, circular dichroism and X-ray crystallography have been used to investigate the reaction of CO-releasing molecule Cs2IrCl5CO with the model protein RNase A.

scholarly journals The grease trap: uncovering the mechanism of the hydrophobic lid in Cutibacterium acnes lipase

2020 ◽  
Vol 61 (5) ◽  
pp. 722-733
Author(s):  
Hyo Jung Kim ◽  
Bong-Jin Lee ◽  
Ae-Ran Kwon
Keyword(s):  
Lipase Activity ◽  
Current Management ◽  
X Ray ◽  
X Ray Crystallography ◽  
Cutibacterium Acnes ◽  
Open Structures ◽  
Type Ia ◽  
Future Drug ◽  
Lid Domain ◽  
Shed Light

Acne is one of the most common dermatological conditions, but the details of its pathology are unclear, and current management regimens often have adverse effects. Cutibacterium acnes is known as a major acne-associated bacterium that derives energy from lipase-mediated sebum lipid degradation. C. acnes is commensal, but lipase activity has been observed to differ among C. acnes types. For example, higher populations of the type IA strains are present in acne lesions with higher lipase activity. In the present study, we examined a conserved lipase in types IB and II that was truncated in type IA C. acnes strains. Closed, blocked, and open structures of C. acnes ATCC11828 lipases were elucidated by X-ray crystallography at 1.6–2.4 Å. The closed crystal structure, which is the most common form in aqueous solution, revealed that a hydrophobic lid domain shields the active site. By comparing closed, blocked, and open structures, we found that the lid domain-opening mechanisms of C. acnes lipases (CAlipases) involve the lid-opening residues, Phe-179 and Phe-211. To the best of our knowledge, this is the first structure-function study of CAlipases, which may help to shed light on the mechanisms involved in acne development and may aid in future drug design.

scholarly journals Reaction with Proteins of a Five-Coordinate Platinum(II) Compound

2019 ◽  
Vol 20 (3) ◽  
pp. 520 ◽  
Author(s):  
Giarita Ferraro ◽  
Tiziano Marzo ◽  
Maria Cucciolito ◽  
Francesco Ruffo ◽  
Luigi Messori ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Platinum Complexes ◽  
Rnase A ◽  
Side Chain ◽  
Planar Geometry ◽  
Ionization Mass ◽  
X Ray ◽  
X Ray Crystallography ◽  
Egg White Lysozyme ◽  
Square Planar

Stable five-coordinate Pt(II) complexes have been highlighted as a promising and original platform for the development of new cytotoxic drugs. Their interaction with proteins has been scarcely studied. Here, the reactivity of the five-coordinate Pt(II) compound [Pt(I)(Me) (dmphen)(olefin)] (Me = methyl, dmphen = 2,9-dimethyl-1,10-phenanthroline, olefin = dimethylfumarate) with the model proteins hen egg white lysozyme (HEWL) and bovine pancreatic ribonuclease (RNase A) has been investigated by X-ray crystallography and electrospray ionization mass spectrometry. The X-ray structures of the adducts of RNase A and HEWL with [Pt(I)(Me)(dmphen)(olefin)] are not of very high quality, but overall data indicate that, upon reaction with RNase A, the compound coordinates the side chain of His105 upon releasing the iodide ligand, but retains the pentacoordination. On the contrary, upon reaction with HEWL, the trigonal bi-pyramidal Pt geometry is lost, the iodide and the olefin ligands are released, and the metal center coordinates the side chain of His15 probably adopting a nearly square-planar geometry. This work underlines the importance of the combined use of crystallographic and mass spectrometry techniques to characterize, in detail, the protein–metallodrug recognition process. Our findings also suggest that five-coordinate Pt(II) complexes can act either retaining their uncommon structure or functioning as prodrugs, i.e., releasing square-planar platinum complexes as bioactive species.

Synthesis and crystal structures of three novel benzimidazole/benzoindolizine hybrids

2016 ◽  
Vol 71 (3) ◽  
pp. 231-239 ◽  
Author(s):  
Roumaissa Belguedj ◽  
Sofiane Bouacida ◽  
Hocine Merazig ◽  
Ali Belfaitah ◽  
Aissa Chibani ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Dipolar Cycloaddition ◽  
Dimethyl Acetylenedicarboxylate ◽  
X Ray ◽  
X Ray Crystallography ◽  
Dimethyl Maleate

AbstractThree benzoindolizine derivatives, 1, 2, and 3, were obtained via 1,3-dipolar cycloaddition. The reaction of 1-(2′-benzimidazolylmethyl)isoquinolinium ylides with dimethyl acetylenedicarboxylate gave a mixture of pyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (1) and 1,10b-dihydropyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (2) derivatives containing a benzimidazole moiety. The reaction of this isoquinolinium N-ylide with dimethyl maleate gave an unexpected 2,3-dihydropyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (3). The structures of all reported compounds have been examined by X-ray crystallography, mass spectrometry, and NMR spectroscopy.

Mononuclear and Binuclear Complexes of Platinum(0) Containing (Alkynyl)phenylsilanes

1999 ◽  
Vol 52 (1) ◽  
pp. 51 ◽  
Author(s):  
Martin A. Bennett ◽  
Christopher J. Cobley ◽  
David C. R. Hockless ◽  
Thomas Klettke
Keyword(s):  
Spectroscopic Data ◽  
Chair Conformation ◽  
Membered Ring ◽  
Binuclear Complexes ◽  
Nickel Compound ◽  
X Ray ◽  
X Ray Crystallography

Reaction of bis(cycloocta-1,5-diene)platinum(0) with the (alkynyl)phenylsilanes Ph3SiC2But, Ph2Si(C2But)2 and PhSi(C2But)3 gives, respectively, [Pt (Ph3SiC2But)2] (1b), [Pt {Ph2Si(C2But)}]2 (2b), and [Pt {PhSi(C2But)3}]2 (4b), which contain zerovalent platinum atoms coordinated by two alkyne units. Spectroscopic data indicate that (2b) and (4b) contain two PtC4 and two SiC4 tetrahedra joined at the corners. X-Ray crystallography shows that complex (4b) is isostructural and isomorphous with the known nickel analogue, two of the alkyne units being uncoordinated; the central eight-membered ring comprising two silicon, four alkyne carbon and two platinum atoms has an approximate chair conformation. In contrast, the monomer (1b) is isostructural but not isomorphous with the analogous nickel compound (1a); in the crystal there is evidence for a weak intramolecular phenyl-phenyl interaction.

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