Oxidative coupling of cycloalkanones with 3-(pyridin-2-yl)-1,2,4-triazinone coordinated to Pd(II)

2018 ◽  
Vol 73 (8) ◽  
pp. 583-587
Author(s):  
Mustafa M. El-Abadelah ◽  
Firas F. Awwadi ◽  
Hamdallah A. Hodali ◽  
Rasha S. Rawajfeh ◽  
Monther S. Zreid ◽  
...  
Keyword(s):  
Single Crystal ◽  
Spectral Data ◽  
Oxidative Coupling ◽  
Coupling Reaction ◽  
X Ray ◽  
X Ray Crystallography ◽  
Square Planar ◽  
Pd Complexes ◽  
Palladium Ion

AbstractDichloro[3-(pyridin-2-yl)-1,2,4-triazinone]Pd(II) undergoes oxidative C–C coupling reaction with cyclopentanone and cyclohexanone at 110°C to yield the respective Pd complexes, chloro[1-(4-chlorophenyl)-5-(2-hydroxycyclopent-1-enyl)-3-(pyridin-2-yl)-1,2,4-triazin-6(1H)-one]palladium(II) (3) and chloro[1-(4-chlorophenyl)-5-(2-hydroxycyclohex-1-enyl)-3-(pyridin-2-yl)-1,2,4-triazin-6(1H)-one]palladium(II) (4). The structures of both complexes are supported by spectral data and confirmed by single-crystal X-ray crystallography. The molecules 3 and 4 stack to form tunnel structures, whilst the geometry around the palladium ion is square planar.

The reaction of imidazo[1,5-a]pyridines with ninhydrin revisited

2020 ◽  
Vol 75 (6-7) ◽  
pp. 559-565
Author(s):  
Mustafa M. El-Abadelah ◽  
Firas F. Awwadi ◽  
Ahmad H. Abdullah ◽  
Wolfgang Voelter
Keyword(s):  
Single Crystal ◽  
Spectral Data ◽  
Room Temperature ◽  
X Ray ◽  
X Ray Crystallography

AbstractThe synthesis of 2,2′-(Imidazo[1,5-a]pyridine-1,3-diyl)bis(2-hydroxy-1H-indene-1,3(2H)-dione) (11) is achieved by reaction of imidazo[1,5-a]pyridine (7) with two equivalents of ninhydrin (1) at room temperature. The structure of this new 1,3-bis-adduct 11 is evidenced from HRMS and NMR spectral data and confirmed by single-crystal X-ray crystallography. Employment of equimolar amounts of 1 and 7 gave a separable mixture of the respective 1- and 3-monomeric adducts (9, 10).

Facile synthesis of model 2,4-diaryl-1,3,4-thiadiazino[5,6-h]fluoroquinolones

2019 ◽  
Vol 74 (6) ◽  
pp. 507-512
Author(s):  
Mohammed M. Abadleh ◽  
Tawfiq Arafat ◽  
Luay Abu-Qatouseh ◽  
Mustafa M. El-Abadelah ◽  
Firas F. Awwadi ◽  
...  
Keyword(s):  
Single Crystal ◽  
Spectral Data ◽  
Carboxylic Acids ◽  
Facile Synthesis ◽  
X Ray ◽  
X Ray Crystallography

AbstractA Selected set of 2,4-diaryl-7-oxo-1,2,4-thiadiazino[5,6-h]quinoline-8-carboxylic acids 6a–e has been prepared via reaction of the parent 7-chloro-8-nitro-10-cyclopropyl-6-fluoroquinolone 4 with the appropriate N′-(aryl)benzothiohydrazide 5a–e in presence of triethylamine. Structures of the new heterocyclics 6a–e are supported by spectral data and confirmed by single-crystal X-ray crystallography for 6a.

scholarly journals Utilization of 1-phenylimidazo[1,5-a]quinoline as partner in 1,4-dipolar cycloaddition reactions

2020 ◽  
Vol 75 (3) ◽  
pp. 259-267
Author(s):  
Areej M. Jaber ◽  
Jalal A. Zahra ◽  
Mustafa M. El-Abadelah ◽  
Salim S. Sabri ◽  
Monther A. Khanfar ◽  
...  
Keyword(s):  
Single Crystal ◽  
Spectral Data ◽  
Cycloaddition Reaction ◽  
Dipolar Cycloaddition ◽  
Cycloaddition Reactions ◽  
Dimethyl Acetylenedicarboxylate ◽  
X Ray ◽  
X Ray Crystallography

AbstractA Selected set of 2-(quinolin-2-yl)-1,3-oxazepino[7,6-b]indoles 4a–d and dihydroacenaphtho[1,2-f][1,3]oxazepine 5 have been prepared via 1,4-dipolar cycloaddition reaction involving 1-phenylimidazo[1,5-a]quinoline, dimethyl acetylenedicarboxylate, and N-(substituted)isatins or acenaphthoquinone. Structures of the new heterocycles 4a–d and 5 are supported by NMR and HRMS spectral data, and confirmed by single-crystal X-ray crystallography for 4c and 5.

Verfeinerung der Kristallstruktur von Tripalladium-di-tetrathiophospliat Pd3(PS4)2 Refinement of the Crystal Structure of Tripalladium-di-tetrathiophosphate Pda3(PS4)2

1983 ◽  
Vol 38 (4) ◽  
pp. 426-427 ◽  
Author(s):  
Arndt Simon ◽  
Karl Peters ◽  
Harry Hahn
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Type Structure ◽  
Tetrahedral Symmetry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Planar Environment

Abstract The structure of the title compound has been determined by X-ray crystallography. The title compound is synthesized from the elements at 600 °C. Its crystal structure, derived from powder data [3] is refined by single crystal diffractometer data. The structure is trigonal (P3̅ml, α = 684.1(1), c = 724.4(1) pm); Pd2+ cations and PS43- anions form a network with an anti-Claudetite (AS2O3) type structure. The PS4 units are distinctly distorted from ideal tetrahedral symmetry. The Pd atoms have a planar environment of 4 S atoms.

scholarly journals Stereoselective Convergent Synthesis of Carbon Skeleton of Cotylenin A Aglycone

Synthesis ◽  
2021 ◽  
Author(s):  
Kazuyuki Sugita ◽  
Motoi Kuwabara ◽  
Ami Matsuo ◽  
Shogo Kamo ◽  
Akinobu Matsuzawa
Keyword(s):  
Single Crystal ◽  
Aldol Reaction ◽  
Coupling Reaction ◽  
Carbon Skeleton ◽  
Convergent Synthesis ◽  
X Ray ◽  
Related Compounds

AbstractIn this paper, the synthesis of the carbon skeleton of cotylenin A aglycone is described. The key reactions, including an intramolecular aldol reaction, an aldol coupling reaction, and a ring-closing meta­thesis, allow for the effective and stereoselective access to the carbon skeleton of cotylenin A aglycone. The stereochemistry was confirmed by single-crystal X-ray crystallographic analyses of related compounds.

Synthesis of 4-(3-coumarinyl)-3-benzyl-4-thiazolin-2-one 4-methylbenzylidenehydrazone and determination of the isomeric structure by X-ray analysis

2003 ◽  
Vol 218 (12) ◽  
Author(s):  
Süheyla Özbey ◽  
Nilgün Karalı ◽  
Aysel Gürsoy
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Spectral Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Isomeric Structure ◽  
Elemental Analyses

AbstractIn this study 4-(3-coumarinyl)-3-benzyl-4-thi azolin-2-one 4-methylbenzylidenehydrazone 3 was synthesised. An independent proof of the thiazolylhydrazone structure of 3 was achieved by single crystal X-ray diffraction analysis. Elemental analyses and spectral data (IR,

scholarly journals Synthesis, Structure, and Antiproliferative Activity of Three Gallium(III) Azole Complexes

2010 ◽  
Vol 2010 ◽  
pp. 1-10 ◽  
Author(s):  
Stergios Zanias ◽  
Giannis S. Papaefstathiou ◽  
Catherine P. Raptopoulou ◽  
Konstantinos T. Papazisis ◽  
Vasiliki Vala ◽  
...  
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystal ◽  
Antiproliferative Activity ◽  
Bioinorganic Chemistry ◽  
Anionic Complex ◽  
X Ray ◽  
X Ray Crystallography ◽  
Mononuclear Complexes ◽  
Human And Mouse ◽  
Antiproliferative Activities

As part of our interest into the bioinorganic chemistry of gallium, gallium(III) complexes of the azole ligands 2,1,3-benzothiadiazole (btd), 1,2,3-benzotriazole (btaH), and 1-methyl-4,5-diphenylimidazole (L) have been isolated. Reaction of btaH or btd withGaBr3orGaCl3resulted in the mononuclear complexes[GaBr3(btaH)2](1) and[GaCl3(btd)2](2), respectively, while treatment ofGaCl3with L resulted in the anionic complex(LH)2[GaCl4](3). All three complexes were characterized by single-crystal X-ray crystallography and IR spectroscopy, while their antiproliferative activities were investigated against a series of human and mouse cancer cell lines.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

scholarly journals Crystal and molecular structure and 31P and 195Pt nmr spectroscopy of [Pt3S2(PMe2Ph)6][BEt4]2; a trinuclear complex containing triply-bridging sulphide ligands

1984 ◽  
Vol 62 (4) ◽  
pp. 696-702 ◽  
Author(s):  
Gordon William Bushnell ◽  
Keith Roger Dixon ◽  
Reiko Ono ◽  
Alan Pidcock
Keyword(s):  
Trinuclear Complex ◽  
Complete Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Interactions ◽  
Nuclear Magnetic Resonance Spectra ◽  
Square Planar ◽  
Metal Metal ◽  
Pd Complexes

An X-ray diffraction study of [Pt3S2(PMe2Ph)6][BEt4]2 shows that it crystallises in the monoclinic space group, C2/c, with a = 15.447(2), b = 18.033(3), c = 26.505(5) Å, β = 96.73(2)°. The cation consists of three, distorted, square-planar cis-PtS2(PMe2Ph)2 moieties combined by sharing of the two sulphur atoms to produce a central Pt3S2 unit with C2 symmetry and Pt—Pt distances of 3.182(1) Å (one edge) and 3.108(1) Å (two edges). Complete analysis and computer simulation of 31P{1H} and 195Pt{1H} nuclear magnetic resonance spectra give values for 1J(Pt—P), 3202 Hz; 3J(Pt—P), −25 Hz; and 2J(Pt—Pt), 476 Hz. The structure is compared with previous results for analogous Ni and Pd complexes and the structural and nmr parameters are discussed with reference to the possibility of metal–metal interactions.

Crystal Structure, Spectroscopic and Redox Properties of Copper(II) Bis{2-[(2,6-dimethylphenyl)iminomethyl-3-methoxyphenolate]}

2007 ◽  
Vol 62 (9) ◽  
pp. 1133-1138 ◽  
Author(s):  
Veli T. Kasumov ◽  
Ibrahim Uçar ◽  
Ahmet Bulut ◽  
Fevzi Kösal
Keyword(s):  
Crystal Structure ◽  
Title Complex ◽  
Redox Properties ◽  
Orthorhombic Space Group ◽  
Long Distance ◽  
X Ray ◽  
X Ray Crystallography ◽  
Square Planar ◽  
Planar Molecules ◽  
Exchange Interaction Parameter

The coordination chemistry of N-(2,6-di-methylphenyl)-2-hydroxy-3-methoxybenzaldimine (1) with Cu(II) has been investigated by X-ray crystallography, electronic and EPR spectroscopies, as well as by electro- and magnetochemistry. The title complex 2 crystallizes in the orthorhombic space group P212121 (a = 8.1538, b = 17.7466, c =19.8507 Å). The mononuclear square-planar molecules 2 featuring trans-N2O2 coordination are connected via weak intermolecular C-H· · ·π interactions into infinite chains parallel to the a axis. Although the intermolecular Cu· · ·Cu separations within individual chains and between chains are very long (8.154 and 9.726 Å ), the exchange interaction parameter G = 2.03 < 4, estimated from solid state EPR spectra, suggests the existence of long-distance superexchange pathways between adjacent Cu(II) centers. The electronic and electrochemical features of the compound are also discussed.

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