Synthesis and Crystal Structure of Lead(II) Thenoyltrifluoroacetonate Complexes with Substituted 2,2' -Bipyridines: Interplay of Intermolecular Interactions in Crystals

2010 ◽  
Vol 65 (2) ◽  
pp. 128-134 ◽  
Author(s):  
Farzin Marandi ◽  
Zahra Nikpey ◽  
Jia Hao Goh ◽  
Hoong-Kun Fun
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Nmr Spectroscopy ◽  
Intermolecular Interactions ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
C Nmr

Three substituted 2,2'-bipyridine adducts of lead(II) thenoyltrifluoroacetonate, [Pb(4,4'-dm-2,2’- bpy)(ttfa)2]2, 1, [Pb(5,5' -dm-2,2’-bpy)(ttfa)2]2, 2, and [Pb(4,4'-dmo-2,2’-bpy)(ttfa)2], 3, (4,4’ -dm- 2,2’-bpy, 5,5’-dm-2,2’-bpy, 4,4’-dmo-2,2’-bpy and ttfa are the abbreviations for 4,4’-dimethyl-, 5,5’-dimethyl-, and 4,4’-dimethoxy-2,2’-bipyridine, and thenoyltrifluoroacetonate, respectively) have been synthesized, characterized by elemental and thermal analysis, IR and 1H- and 13C-NMR spectroscopy, and studied by X-ray crystallography. The supramolecular features in these complexes are guided/controlled by weak directional intermolecular interactions.

Synthesis and crystal structure of a new homoleptic tetraarylruthenium(IV) complex Ru(2,4,5-Me3C6H2)4

2017 ◽  
Vol 72 (7) ◽  
pp. 523-525
Author(s):  
Chang-Jiu Wang ◽  
Xiu-Li Wu ◽  
Xiu-Fang Ma ◽  
Ai-Quan Jia ◽  
Qian-Feng Zhang
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Column Chromatography ◽  
Proton Nmr ◽  
Proton Nmr Spectroscopy ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Moderate Yield

AbstractTreatment of [Ru(acac)3] (acac−=acetylacetonate) with (2,4,5-Me3C6H2)MgBr, followed by column chromatography in air, afforded the homoleptic tetraaryl-ruthenium(IV) complex [Ru(2,4,5-Me3C6H2)4] (1) in moderate yield. The product was characterized by proton NMR spectroscopy and microanalyses. Its crystal structure has also been established by X-ray crystallography.

2,2'-Bipyridine Mercury(II) Complexes [Hg(bpy)(NO2)X] (X = NO2 –, SCN– , CH3COO–); Π-Π Stacking In The Crystal Structure Of [Hg(bpy)(NO2)2]

2005 ◽  
Vol 60 (3) ◽  
pp. 289-293 ◽  
Author(s):  
Ali Ramazani ◽  
Ali Morsali ◽  
Leila Dolatyari ◽  
Bijan Ganjeie
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Aromatic Rings ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
Coordinate Geometry ◽  
C Nmr

The mercury(II) complexes of 2,2′-bipyridine (bpy), [Hg(bpy)(NO2)2], [Hg(bpy)(NO2) (CH3COO)], and [Hg(bpy)(NO2)(NCS)] have been synthesized and characterized by elemental analysis, IR, 1H NMR and 13C NMR spectroscopy. The structure of [Hg(bpy)(NO2)2] has been confirmed by X-ray crystallography. The complex is a monomer and the Hg atom has an unsymmetrical six-coordinate geometry, formed by two nitrogen atoms of the bpy ligand and four oxygen atoms of the two nitrite anions. There is a short intermolecular π-π stacking interaction between parallel aromatic rings

Structural and spectral study of coordination of 4,4′-dimethoxy-2,2′-bipyridine toward Zn(II) and Cd(II) containing thiocyanato or azido ligands

2016 ◽  
Vol 71 (9) ◽  
pp. 959-965 ◽  
Author(s):  
Farzin Marandi ◽  
Keyvan Moeini ◽  
Hadi Amiri Rudbari
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
Ft Ir ◽  
New Compounds ◽  
C Nmr

AbstractThree new compounds of zinc(II) and cadmium(II) with the ligand 4,4′-dimethoxy-2,2′-bipyridine (4,4′-dmo-2,2′-bpy), including cis-[Zn(4,4′-dmo-2,2′-bpy)2(SCN)2] (1), cis-[Cd(4,4′-dmo-2,2′-bpy)2(SCN)2] (2), and [Cd3(4,4′-dmo-2,2′-bpy)3(N3)5(OAc)]n (3), have been obtained as white single crystals by the branched tube method and characterized by elemental analysis, FT-IR and 1H, 13C NMR spectroscopy, and X-ray crystallography. Single-crystal structure analyses of the isostructural complexes 1 and 2 showed distorted octahedral geometry for zinc(II) and cadmium(II) with ZnN6 and CdN6 environments. Complex 3 reveals a rare coordination polymer containing octahedrally coordinated cadmium(II) expanding to chains by two different bridging modes, including Cd‒O‒C‒O‒Cd and Cd‒N‒Cd.

The first example of the stereoselective synthesis and crystal structure of a spirobicycloquinazolinone based on (–)-fenchone and anthranilamide

2019 ◽  
Vol 75 (12) ◽  
pp. 1675-1680 ◽  
Author(s):  
Vladimir V. Chernyshov ◽  
Yuri V. Gatilov ◽  
Olga I. Yarovaya ◽  
Igor P. Koskin ◽  
Spartak S. Yarovoy ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Unit Cell Volume ◽  
Stereoselective Synthesis ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
First Time ◽  
C Nmr

The possibility of a single-stage solvent-free stereoselective synthesis of a spirocyclic compound from the natural bicyclic monoterpenoid (−)-fenchone and anthranilamide has been shown for the first time. The molecular and crystal structure of (1R,2S,4S)-1,3,3-trimethyl-1′H-spiro[bicyclo[2.2.1]heptane-2,2′-quinazolin]-4′(3′H)-one, C17H22N2O, was established by X-ray diffraction though the chirality was assumed via the known reactant connectivity and 1H and 13C NMR spectroscopy. It has shown that in the molecule, for steric reasons, there is an elongation of the Me2C—C(N)N bond to 1.603 (5) Å. The formation of dimers via N—H...O=C hydrogen bonds with an interaction energy of 93.30 kJ mol−1 and through cavities (33.7% of the unit-cell volume) was established in the packing of the molecules. There are no π-stacking interactions in the structure.

Synthesis and crystal structure of a homoleptic diruthenium complex containing tetra-2-pyridyl-1,4-pyrazine (tppz)

2017 ◽  
Vol 72 (10) ◽  
pp. 759-762 ◽  
Author(s):  
Marion Graf ◽  
Peter Mayer ◽  
Hans-Christian Böttcher
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Title Complex ◽  
Dinuclear Complex ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diruthenium Complex

AbstractTreatment of hydrated ruthenium(III) chloride with tetra-2-pyridyl-1,4-pyrazine (tppz) in refluxing ethoxyethanol afforded the homoleptic dinuclear complex [(tppz)Ru(μ-tppz)Ru(tppz)]4+ (1) besides small amounts of the species [Ru(tppz)2]2+. The title complex 1 was obtained as purple crystals and characterized as its hexafluoridophosphate salt by NMR spectroscopy, mass spectrometry and microanalyses. The molecular structure of 1(PF6)4 has been established by X-ray crystallography.

Triazene derivatives of (1,x-)diazacycloalkanes. Part VI. 3-({5,5-Dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines — Synthesis, characterization, and X-ray crystal structure

2006 ◽  
Vol 84 (10) ◽  
pp. 1294-1300 ◽  
Author(s):  
Keith Vaughan ◽  
Shasta Lee Moser ◽  
Reid Tingley ◽  
M Brad Peori ◽  
Valerio Bertolasi
Keyword(s):  
Crystal Structure ◽  
Significant Degree ◽  
Ion Trapping ◽  
Published Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diazonium Ion ◽  
Derivatives Of ◽  
C Nmr

Reaction of a series of diazonium salts with a mixture of formaldehyde and 1,2-diamino-2-methylpropane affords the 3-({5,5-dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines (1a–1f) in excellent yield. The products have been characterized by IR and NMR spectroscopic analysis, elemental analysis, and X-ray crystallography. The X-ray crystal structure of the p-methoxycarbonyl derivative (1c) establishes without question the connectivity of these novel molecules, which can be described as linear bicyclic oligomers with two imidazolidinyl groups linked together by a one-carbon spacer. This is indeed a rare molecular building block. The molecular structure is corroborated by 1H and 13C NMR data, which correlates with the previously published data of compounds of types 5 and 6 derived from 1,3-propanediamine. The triazene moieties in the crystal of 1c display significant π conjugation, which gives the N—N bond a significant degree of double-bond character. This in turn causes restricted rotation around the N—N bond, which leads to considerable broadening of signals in both the 1H and 13C NMR spectra. The molecular ion of the p-cyanophenyl derivative (1b) was observed using electrospray mass spectrometry (ES + Na). The mechanism of formation of molecules of type 1 is proposed to involve diazonium ion trapping of the previously unreported bisimidazolidinyl methane (13).Key words: triazene, bistriazene, imidazolidine, synthesis, X-ray crystallography, NMR spectroscopy.

[Zn(phen)2(CX3COO)]+, X = H orCl; Influence of X on the Coordination Mode of the Carboxylate Group (phen = 1,10-Phenanthroline)

2005 ◽  
Vol 60 (10) ◽  
pp. 1049-1053 ◽  
Author(s):  
Zeanab Talaei ◽  
Ali Morsali ◽  
Ali R. Mahjoub
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Mode ◽  
Bidentate Ligand ◽  
Carboxylate Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Coordinate Geometry ◽  
C Nmr

Two new ZnII(phen)2 complexes with trichloroacetate and acetate anions, [Zn(phen)2(CCl3COO)- (H2O)](ClO4) and [Zn(phen)2(CH3COO)](ClO4), have been synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR spectroscopy. The single crystal X-ray data of these compounds show the Zn atoms to have six-coordinate geometry. From IR spectra and X-ray crystallography it is established that the coordination of the COO− group is different for trichloroacetate and acetate. The former acts as a monodentate whereas the latter acts as a bidentate ligand.

A Zinc(II)-Silver(I) Bimetallic Coordination Polymer Assembled Through Argentophilic and π-π Interactions, f[Zn(phen)2(H2O) {Ag(CN)2g][Ag(CN)2]·MeOH}n (phen=1,10-Phenanthroline)

2013 ◽  
Vol 68 (2) ◽  
pp. 161-167 ◽  
Author(s):  
Muhammad Monim-ul-Mehbooba ◽  
Muhammad Ramzan ◽  
Tobias Rüffe ◽  
Heinrich Lang ◽  
Shafqat Naddem ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Ir Spectroscopy ◽  
Coordination Polymer ◽  
Hydrogen Bonds ◽  
X Ray ◽  
Π Interactions ◽  
X Ray Crystallography ◽  
3D Network ◽  
Argentophilic Interactions

A cyanido-bridged Zn(II)-Ag(I) bimetallic coordination polymer, {[Zn(phen)2(H2O){Ag(CN)2}] [Ag(CN)2]·MeOH}n (1), was prepared using ZnCl2, 1,10-phenanthroline (phen) and K[Ag(CN)2] and characterized by IR spectroscopy, thermal analysis and X-ray crystallography. The crystal structure of 1 consists of dinuclear [Zn(phen)2(H2O){Ag(CN)2}]+ cations, [Ag(CN)2]- anions and a methanol molecule. The non-coordinated [Ag(CN)2]- anions are linked to the [Zn(phen)2(H2O){Ag(CN)2}]+ complex cations through argentophilic interactions leading to the formation of chains. The chains are connected by hydrogen bonds and π-π interactions to give a 3D network.

scholarly journals Synthesis and Crystal Structure of Unexpected (1S,4R,5R,6S)-4-Cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonan-6-yl Acetate

2017 ◽  
Vol 70 (12) ◽  
pp. 1269
Author(s):  
Steven Gareth Williams ◽  
Mohan Bhadbhade ◽  
Roger Bishop ◽  
Alison Thavary Ung
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
High Resolution Mass Spectrometry ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Ir And Nmr Spectroscopy ◽  
Resolution Mass

The reaction of (–)-β-pinene with KCN under a mild bridged Ritter reaction gave (1S,5R,6S)-2,2,6-trimethyl-3-aza-bicyclo[3.3.1]non-3-en-6-yl acetate that subsequently reacted to provide an unexpected (1S,4R,5R,6S)-4-cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonane-6-yl acetate. The structure of the compound was determined by high-resolution mass spectrometry, and IR and NMR spectroscopy and confirmed by single crystal X-ray crystallography. The compound crystallises in the monoclinic P21 space group, with unit cell parameters a 8.6120 (17), b 7.4570 (15), c 11.189 (2) Å, and β 110.16 (3)°.

scholarly journals Synthesis and Crystal Structure of C1-Symmetric 3,3′-Bi(1,1′-dinaphthyl-camphopyrazole)

2016 ◽  
Vol 2016 ◽  
pp. 1-5
Author(s):  
Jannis Barrera ◽  
Victoria A. Smolenski ◽  
Jerry P. Jasinski ◽  
Jesús Pastrán
Keyword(s):  
Crystal Structure ◽  
Crystal Packing ◽  
Pyrazole Ring ◽  
Stacking Interactions ◽  
Naphthalene Ring ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Group Form ◽  
C Nmr

The compound 3,3′-bi(1,1′-dinaphthyl-camphopyrazole) 1, C42H42O4, was obtained in good yield and structurally characterized by 1H and 13C NMR spectroscopy, elemental analysis, and X-ray diffraction. It consists of a 3,3′-bipyrazole group with each pyrazole ring containing a fused camphor group and a naphthalene ring bonded to the adjacent nitrogen atom in the ring. Both of the trimethyl, 5-membered rings of the fused camphor group form an envelope with the apex carbon atom as the flap in each case. In the crystal, weak π–π stacking interactions are observed between nearby 6-carbon rings of the two naphthalene rings linking the molecules into extended chains. Weak π–ring intermolecular interactions are also observed between naphthalene atoms and pyrazole rings from each of the groups helping to stabilize the crystal packing. No classical hydrogen interactions are formed.

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