scholarly journals Synthesis, structural and conformational study of selected N-substituted phthalimides

2005 ◽  
Vol 3 (4) ◽  
pp. 683-704 ◽  
Author(s):  
Isabel Iriepa ◽  
F. Javier Villasante ◽  
Enrique Gálvez ◽  
Antonio Herrera ◽  
Angel Sánchez ◽  
...  
Keyword(s):  
Double Resonance ◽  
13C Nmr Spectroscopy ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
1H And 13C Nmr ◽  
Conformational Studies ◽  
One Dimensional ◽  
X Ray ◽  
Nmr Techniques ◽  
New Compounds

AbstractThis paper synthesizes N-substituted phthalimides derived from nitrogen heterocycles as potential 5-HT4 ligands by using the Mitsunobu reaction. Conformational studies of some of the new compounds have been conducted using 1H and 13C-NMR spectroscopy. Proton and carbon resonances were achieved through the application of one-dimensional selective NOE, two-dimensional NMR techniques-homonuclear COSY-45, NOESY and heteronuclear 1H-13C HMQC correlated spectroscopy- and double resonance experiments. The crystal structure of compound 1 was determined by X-ray diffraction.

scholarly journals The Solvent Effect on Composition and Dimensionality of Mercury(II) Complexes with Picolinic Acid

Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 5002
Author(s):  
Željka Soldin ◽  
Boris-Marko Kukovec ◽  
Dubravka Matković-Čalogović ◽  
Zora Popović
Keyword(s):  
Coordination Compounds ◽  
Picolinic Acid ◽  
Chloride Ion ◽  
13C Nmr Spectroscopy ◽  
Thermal Methods ◽  
1H And 13C Nmr ◽  
Coordination Environment ◽  
One Dimensional ◽  
X Ray ◽  
Different Types

Three new mercury(II) coordination compounds, {[HgCl(pic)]}n (1), [HgCl(pic)(picH)] (2), and [HgBr(pic)(picH)] (3) (picH = pyridine-2-carboxylic acid, picolinic acid) were prepared by reactions of the corresponding mercury(II) halides and picolinic acid in an aqueous (1) or alcohol–methanol or ethanol (2 and 3) solutions. Two different types of coordination compounds were obtained depending on the solvent used. The crystal structures were determined by the single-crystal X-ray structural analysis. Compound 1 is a one-dimensional (1-D) coordination polymer with mercury(II) ions bridged by chelating and bridging N,O,O′-picolinate ions. Each mercury(II) ion is four-coordinated with a bidentate picolinate ion, a carboxylate O atom from the symmetry-related picolinate ion and with a chloride ion; the resulting coordination environment can be described as a highly distorted tetrahedron. Compounds 2 and 3 are isostructural mononuclear coordination compounds, each mercury(II) ion being coordinated with the respective halide ion, N,O-bidentate picolinate ion, and N,O-bidentate picolinic acid in a highly distorted square-pyramidal coordination environment. Compounds 1–3 were characterized by IR spectroscopy, PXRD, and thermal methods (TGA/DSC) in the solid state and by 1H and 13C NMR spectroscopy in the DMSO solution.

scholarly journals SOLVENT-FREE SYNTHESIS AND CRYSTAL STRUCTURE OF rac-2-THIOHYDANTOIN-VALINE

2019 ◽  
Vol 16 (31) ◽  
pp. 347-352
Author(s):  
G. E. DELGADO ◽  
Asiloé J. MORA ◽  
T. GONZÁLEZ ◽  
I. SANTOS ◽  
P. RIVAS ◽  
...  
Keyword(s):  
Heterocyclic Ring ◽  
Solvent Free ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
One Dimensional ◽  
X Ray ◽  
Dimensional Network ◽  
Nmr Techniques ◽  
Solvent Free Synthesis

Thiohydantoins have been used in the manufacture of medicines and in industrial processes. Depending on the nature and type of substitution on the heterocyclic ring, these compounds may display pharmaceutical and biological activity with a variety of applications as antiepileptic, antitumoral, antiinflammatory, and principally for the treatment of prostate cancer. In this study, a new thiohydantoin was synthetized from the valine amino acid and structurally characterized. The title compound, C6H10N2O2S, with systematic name rac-5-isopropyl-2-tioxoimidazolidin-4-one, has been synthetized by a solvent-free synthesis. The heterocyclic compound was characterized by spectroscopic infrared (FTIR) and nuclear magnetic resonance (NMR) techniques, powder and single-crystal X-ray diffraction analysis (XRD). This material crystallizes in the monoclinic space group P21/c. In the supramolecular structure, the molecules are joined by N- --H···O and N---H···S hydrogen bonds, forming centrosymmetric R2 2(8) dimers and C2 2(9) chains that run along the [001] direction in an infinite one-dimensional network.

scholarly journals A new one-dimensional NiIIcoordination polymer with a two-dimensional supramolecular architecture

2017 ◽  
Vol 73 (2) ◽  
pp. 192-195
Author(s):  
Kai-Long Zhong
Keyword(s):  
Hydrogen Bonds ◽  
Water Molecule ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Sulfate Ions ◽  
Sulfate Anion ◽  
One Dimensional ◽  
X Ray ◽  
Distorted Octahedral ◽  
Metal Organic

A new one-dimensional NiIIcoordination polymer of 1,3,5-tris(imidazol-1-ylmethyl)benzene, namelycatena-poly[[aqua(sulfato-κO)hemi(μ-ethane-1,2-diol-κ2O:O′)[μ3-1,3,5-tris(1H-imidazol-1-ylmethyl)benzene-κ3N3,N3′,N3′′]nickel(II)] ethane-1,2-diol monosolvate monohydrate], {[Ni(SO4)(C18H18N6)(C2H6O2)0.5(H2O)]·C2H6O2·H2O}n, was synthesized and characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The NiIIcation is coordinated by three N atoms of three different 1,3,5-tris(imidazol-1-ylmethyl)benzene ligands, one O atom of an ethane-1,2-diol molecule, by a sulfate anion and a water molecule, forming a distorted octahedral NiN3O3coordination geometry. The tripodal 1,3,5-tris(imidazol-1-ylmethyl)benzene ligands link the NiIIcations, generating metal–organic chains running along the [100] direction. Adjacent chains are further connected by O—H...O hydrogen bonds, resulting in a two-dimensional supermolecular architecture running parallel to the (001) plane. Another water molecule and a second ethane-1,2-diol molecule are non-coordinating and are linked to the coordinating sulfate ionsviaO—H...O hydrogen bonds.

Synthesis, Characterization, and Catalytic Activity of a Series of Aluminium–Amidate Complexes

2015 ◽  
Vol 68 (3) ◽  
pp. 357 ◽  
Author(s):  
Kevin P. Yeagle ◽  
Darryl Hester ◽  
Nicholas A. Piro ◽  
William G. Dougherty ◽  
W. Scott Kassel ◽  
...  
Keyword(s):  
Catalytic Activity ◽  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
13C Nmr ◽  
13C Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
Metathesis Reaction ◽  
Chloride Complexes ◽  
1H And 13C Nmr ◽  
X Ray

The aluminium complexes {[κ2-N,O-(t-BuNCOPh)]AlMe2}2 (2), [κ2-N,O-(t-BuNCOPh)]2AlMe (3), and [κ2-N,O-(t-BuNCOPh)]3Al (4) were prepared through the protonolysis reaction between trimethylaluminium and one, two, or three equivalents, respectively, of N-tert-butylbenzamide. Complex 2 was also prepared via a salt metathesis reaction between K(t-BuNCOPh) and dimethylaluminium chloride. Complexes 2–4 were characterized using 1H and 13C NMR spectroscopy. Single-crystal X-ray diffraction analysis of the complexes corroborated ligand : metal stoichiometries and revealed that all the amidate ligands coordinate to the aluminium ion in a κ2 fashion. The Al–amidate complexes 2–4 were viable catalyst precursors for the Meerwein–Ponndorf–Verley–Oppenauer reduction–oxidation manifold, successfully interconverting several classes of carbonyl and alcohol substrates.

Two-Dimensional Neutral Framework Generated from Mixed Organic Ligands: Structure and Magnetic Properties

2012 ◽  
Vol 455-456 ◽  
pp. 735-739
Author(s):  
Rui Xin Chen ◽  
Ling Yan Xu ◽  
Chang Feng Sun
Keyword(s):  
Magnetic Properties ◽  
Hydrothermal Condition ◽  
Organic Ligands ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Magnetic Susceptibilities ◽  
One Dimensional ◽  
X Ray ◽  
Ferromagnetic Interactions ◽  
Cu Ions

A new two-dimensional neutral framework generated from mixed organic ligands [Cu3(1,2,4-BTC)2(4,4/-bipy)(H2O)4] (where1,2,4-BTC = 1,2,4-benzenetricarboxylate), has been prepared under hydrothermal condition and characterized by single crystal X-ray diffraction and magnetic susceptibilities. Its structure contains two different one-dimensional chains for the Cu ions, namely [Cu2(1,2,4-BTC)2]n2n-and [Cu (4,4/-bipy)]n2n+, respectively; the carboxylate of 1,2,4-BTC ligands links the two different 1-D chains into a interesting steplike supramolecular neutral framework, which exists ferromagnetic interactions between the copper centers.

A one-dimensional cobalt(II) coordination polymer based on 2,4′-oxydibenzoic acid: poly[[[diaquabis[2-(4-carboxyphenoxy)benzoato-κO1]cobalt(II)]-μ-4,4′-bipyridine-κ2N:N′] dihydrate]

2014 ◽  
Vol 70 (7) ◽  
pp. 654-658 ◽  
Author(s):  
Long Tang ◽  
Feng Fu ◽  
Ji-Jiang Wang ◽  
Qi-Rui Liu ◽  
Hang-Hang Zhao
Keyword(s):  
Coordination Polymer ◽  
Hydrothermal Condition ◽  
Dimensional Chain ◽  
Supramolecular Architecture ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
The One ◽  
Two Sides

The reaction of CoSO4with 2,4-oxydibenzoic acid (H2oba) and 4,4′-bipyridine (bipy) under hydrothermal condition yielded a new one-dimensional cobalt(II) coordination polymer, {[Co(C14H9O5)2(C10H8N2)(H2O)2]·2H2O}n, which was characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, magnetic properties and single-crystal X-ray diffraction. The CoIIions are connected by bipy ligands into infinite one-dimensional chains. The Hoba−ligands extend out from the two sides of the one-dimensional chain. O—H...O hydrogen bonding extends these chains into a two-dimensional supramolecular architecture.

scholarly journals Synthesis, Crystal Structure, and Luminescence of Cadmium(II) and Silver(I) Coordination Polymers Based on 1,3-Bis(1,2,4-triazol-1-yl)adamantane

Molecules ◽  
2021 ◽  
Vol 26 (17) ◽  
pp. 5400
Author(s):  
Roman D. Marchenko ◽  
Taisiya S. Sukhikh ◽  
Alexey A. Ryadun ◽  
Andrei S. Potapov
Keyword(s):  
Crystal Structure ◽  
Coordination Polymer ◽  
Metal Ions ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Coordination Polymers ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray

Coordination polymers with a new rigid ligand 1,3-bis(1,2,4-triazol-1-yl)adamantane (L) were prepared by its reaction with cadmium(II) or silver(I) nitrates. Crystal structure of the coordination polymers was determined using single-crystal X-ray diffraction analysis. Silver formed two-dimensional coordination polymer [Ag(L)NO3]n, in which metal ions are linked by 1,3-bis(1,2,4-triazol-1-yl)adamantane ligands, coordinated by nitrogen atoms at positions 2 and 4 of 1,2,4-triazole rings. Layers of the coordination polymer consist of rare 18- and 30-membered {Ag2L2} and {Ag4L4} metallocycles. Cadmium(II) nitrate formed two kinds of one-dimensional coordination polymers depending on the metal-to-ligand ratio used in the synthesis. Coordination polymer [Cd(L)2(NO3)2]n was obtained in case of a 1:2 M:L ratio, while for M:L = 2:1 product {[Cd(L)(NO3)2(CH3OH)]·0.5CH3OH}n was isolated. All coordination polymers demonstrated ligand-centered emission near 450 nm upon excitation at 370 nm.

One- and two-dimensional PbII compounds resulting from reaction of PbBr2 and Pb(SCN)2 with pyrimidine-2-thione

2021 ◽  
Vol 77 (7) ◽  
Author(s):  
Vânia Denise Schwade ◽  
Bárbara Tirloni
Keyword(s):  
Structural Characterization ◽  
Diffuse Reflectance ◽  
Tautomeric Form ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Ft Ir ◽  
Compound Ii

Pyrimidine-2-thione (HSpym) reacts with lead(II) thiocyanate and lead(II) bromide in N,N-dimethylformamide (DMF) to form poly[(μ-isothiocyanato-κ2 N:S)(μ4-pyrimidine-2-thiolato-κ6 N 1,S:S:S:S,N 3)lead(II)], [Pb(C4H3N2S)(NCS)] n or [Pb(Spym)(NCS)] n , (I), and the polymeric one-dimensional (1D) compound catena-poly[[μ4-bromido-di-μ-bromido-(μ-pyrimidine-2-thiolato-κ3 N 1,S:S)(μ-pyrimidine-2-thione-κ3 N 1,S:S)dilead(II)] N,N-dimethylformamide monosolvate], {[Pb2Br3(C4H3N2S)(C4H4N2S)]·C3H7NO} n or {[Pb2Br3(Spym)(HSpym)]·DMF} n , (IIa), respectively. Poly[μ4-bromido-di-μ3-bromido-(μ-pyrimidine-2-thiolato-κ3 N 1,S:S)(μ-pyrimidine-2-thione-κ3 N 1,S:S)dilead(II)], [Pb2Br3(C4H3N2S)(C4H4N2S)] n or [Pb2Br3(Spym)(HSpym)] n , (IIb), could be obtained as a mixture with (IIa) when using a lesser amount of solvent. In the crystal structures of the pseudohalide/halide PbII stable compounds, coordination of anionic and neutral HSpym has been observed. Both Spym− (in the thiolate tautomeric form) and NCS− ligands were responsible for the two-dimensional (2D) arrangement in (I). The Br− ligands establish the 1D polymeric arrangement in (IIa). Eight-coordinated metal centres have been observed in both compounds, when considering the Pb...S and Pb...Br interactions. Both compounds were characterized by FT–IR and diffuse reflectance spectroscopies, as well as by powder X-ray diffraction. Compound (IIa) and its desolvated version (IIb) represent the first structurally characterized PbII compounds containing neutral HSpym and anionic Spym− ligands. After a prolonged time in solution, (IIa) is converted to another compound due to complete deprotonation of HSpym. The structural characterization of (I) and (II) suggests HSpym as a good candidate for the removal of PbII ions from solutions containing thiocyanate or bromide ions.

Analysis the Actual Nanostructure of α Phase Polyoctylfluorene Thin Film via Synchrotron Grazing-Incidence X-Ray Diffraction

2013 ◽  
Vol 333-335 ◽  
pp. 1832-1835
Author(s):  
Liu Ran Chen ◽  
Xi Chen ◽  
Ji Cai Liang ◽  
Ji Dong Zhang
Keyword(s):  
Thin Film ◽  
Grazing Incidence ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Α Phase ◽  
Out Of Plane ◽  
Diffraction Signal

The nanostructure of α phase polyoctylfluorene thin film was characterized using normal X-ray diffraction, one-dimensional out-of-plane grazing incidence X-ray diffraction and two-dimensional grazing incidence X-ray diffraction with lab diffractometer and synchrotron diffractometer. The results show that using grazing incidence X-ray diffraction the weak diffraction signal of thin film can be observed after the elimination of background signals. Incorrect (h10) diffraction signals can be collected by lab diffractometer due to its low collimation and resolution, which can be overcome by using synchrotron diffractometer with high collimation and resolution that reveal the actual microstructure of polyoctylfluorene thin film.

scholarly journals Structural Variations in Manganese Halide Chain Compounds Mediated by Methylimidazolium Isomers

Crystals ◽  
2020 ◽  
Vol 10 (10) ◽  
pp. 930
Author(s):  
Ceng Han ◽  
David B. Cordes ◽  
Alexandra M. Z. Slawin ◽  
Philip Lightfoot
Keyword(s):  
Hydrogen Bonding ◽  
Ambient Temperature ◽  
X Ray Diffraction ◽  
Structural Variations ◽  
One Dimensional ◽  
X Ray ◽  
Chain Compounds ◽  
Red Luminescence ◽  
New Compounds ◽  
Related Compounds

The structures of two new hybrid organic–inorganic manganese halide compounds [1MiH]MnCl3(H2O) and [4MiH]MnCl3(H2O) ([1MiH] = 1-methylimidazolium, [4MiH] = 4-methylimidazolium) have been determined by single crystal X-ray diffraction. Both are composed of one dimensional [MnCl3(H2O)]n− edge-sharing octahedral chains. The structures are compared to the previously reported isomeric analogue [2MiH]MnCl3(H2O) ([2MiH] = 2-methylimidazolium), and three closely related compounds. The variations in packing of the inorganic chains are shown to be influenced by hydrogen bonding abilities of the imidazolium or related moieties. Both new compounds show intense red luminescence at ambient temperature under UV irradiation.

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