scholarly journals Tetrathiafulvalene-based azine ligands for anion and metal cation coordination

2015 ◽  
Vol 11 ◽  
pp. 1379-1391 ◽  
Author(s):  
Awatef Ayadi ◽  
Aziz El Alamy ◽  
Olivier Alévêque ◽  
Magali Allain ◽  
Nabil Zouari ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Tricarbonyl Complex ◽  
Full Characterization ◽  
Rhenium Complex ◽  
Radical Cation Salts ◽  
Cation Coordination ◽  
Rhenium Tricarbonyl ◽  
Methyl Pyridine

The synthesis and full characterization of two tetrathiafulvalene-appended azine ligands, namely 2-([2,2’-bi(1,3-dithiolylidene)]-4-yl)-6-((2,4-dinitrophenyl)hydrazono)methyl)pyridine (L1) and 5-([2,2’-bi(1,3-dithiolylidene)]-4-yl)-2-((2,4-dinitrophenyl)hydrazono)methyl)pyridine (L2) are described. The crystal structure of ligand L1 indicates that the ligand is completely planar with the presence of a strong intramolecular N3–H3···O1 hydrogen bonding. Titration experiments with inorganic anions showed that both ligands are suitable candidates for the sensing of fluoride anions. Ligand L2 was reacted with a Re(I) cation to yield the corresponding rhenium tricarbonyl complex 3. In the crystal structure of the newly prepared electroactive rhenium complex the TTF is neutral and the rhenium cation is hexacoordinated. The electrochemical behavior of the three compounds indicates that they are promising for the construction of crystalline radical cation salts.

scholarly journals Etazene (N,N-diethyl-2-{[(4-ethoxyphenyl)methyl]-1H-benzimidazol-1-yl}-ethan-1-amine (dihydrochloride)): a novel benzimidazole opioid NPS identified in seized material: crystal structure and spectroscopic characterization

2020 ◽  
Author(s):  
Marta Siczek ◽  
Marcin Zawadzki ◽  
Miłosz Siczek ◽  
Agnieszka Chłopaś-Konowałek ◽  
Paweł Szpot
Keyword(s):  
Crystal Structure ◽  
Analytical Data ◽  
Chemical Characterization ◽  
Drug Market ◽  
Spectroscopic Characterization ◽  
Illegal Drug ◽  
Spectroscopic Techniques ◽  
X Ray ◽  
Full Characterization

Abstract Purpose The aim of the study was to present the spectroscopic characteristics and crystal structure of the etazene—a benzimidazole opioid, which appeared on the illegal drug market in Poland in the last weeks. Methods The title compound was analyzed by X-ray crystallography as well as gas and liquid chromatography combined with mass spectrometry. Spectroscopic techniques have also been used, such as nuclear magnetic resonance, infrared and ultraviolet-visible spectroscopies. Results We presented the identification and the broad chemical characterization of etazene, a synthetic opioid that has recently been introduced on the illegal drug market. Conclusions In this paper, we described single-crystal X-ray, chromatographic and spectroscopic characterization of a synthetic opioid that emerged on the new psychoactive substance (NPS) market in Poland. To the best of our knowledge, this is the first full characterization of etazene. Analytical data presented in the work can be helpful in identification and detection of the NPS in forensic and clinical laboratories.

A halide-free pyridinium-substituted η3-cycloheptatrienide–Pd complex

2017 ◽  
Vol 73 (9) ◽  
pp. 754-759
Author(s):  
C. Jandl ◽  
S. Stegbauer ◽  
A. Pöthig
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Synthesis And Characterization ◽  
Dimeric Complex ◽  
Coordination Sites ◽  
Internal Hydrogen ◽  
Halide Ligands

We report the synthesis and characterization of a novel 4-(dimethylamino)pyridinium-substituted η3-cycloheptatrienide–Pd complex which is free of halide ligands. Diacetonitrile{η3-[4-(dimethylamino)pyridinium-1-yl]cycloheptatrienido}palladium(II) bis(tetrafluoroborate), [Pd(C2H3N)2(C14H16N2)](BF4)2, was prepared by the exchange of two bromide ligands for noncoordinating anions, which results in the empty coordination sites being occupied by acetonitrile ligands. As described previously, exchange of only one bromide leads to a dimeric complex, di-μ-bromido-bis({η3-[4-(dimethylamino)pyridinium-1-yl]cycloheptatrienido}palladium(II)) bis(tetrafluoroborate) acetonitrile disolvate, [Pd2Br2(C14H16N2)2](BF4)2·2CH3CN, with bridging bromide ligands, and the crystal structure of this compound is also reported here. The structures of the cycloheptatrienide ligands of both complexes are analogous to the dibromide derivative, showing the allyl bond in the β-position with respect to the pyridinium substituent. This indicates that, unlike a previous interpretation, the main reason for the formation of the β-isomer cannot be internal hydrogen bonding between the cationic substituents and bromide ligands.

Hydrothermal Synthesis and Structure Characterization of a Bi-Capped Keggin Heteropoly Molybdovanadated Derivative

2014 ◽  
Vol 1004-1005 ◽  
pp. 542-545
Author(s):  
Ya Bing Liu ◽  
Li Guang Xiao
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Building Blocks ◽  
Crystal Structure Analysis ◽  
Structure Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Supramolecular Networks

A new bi-capped Keggin heteropoly molybdovanadated derivative, [Co (en)3]2[SiMo8V6O42]∙6H2O (1) (en = ethylendiamine) has been hydrothermally synthesized and structurally characterized by the elemental analysis, IR, XPS and single crystal X-ray diffraction. The crystal structure analysis reveals that compound 1 consists of [Co (en)3]2+transition metal coordination fragment and the [SiMo8V6O42]4-building blocks, which are linked together via hydrogen-bonding interactions to form a new 3-D supramolecular networks.

Improved syntheses, and structural and electronic characterization of carboxamide-substituted TpCONHPh,Meand TpCONHt-Bu,Meligands

2013 ◽  
Vol 69 (9) ◽  
pp. 947-953 ◽  
Author(s):  
Eric R. Sirianni ◽  
Glenn P. A. Yap ◽  
Eser S. Akturk ◽  
Klaus H. Theopold
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Spectroscopic Properties ◽  
Carbonyl Complexes ◽  
Strong Electron ◽  
Complex Molecules ◽  
Solvent Molecules ◽  
Related Compounds

Improvements in the syntheses of the carboxamide-substituted tris(pyrazolyl)borate ligands TpCONHPh,Me[tris(3-anilinocarbonyl-5-methylpyrazol-1-yl)borate] and TpCONHt-Bu,Me[tris(3-tert-butylaminocarbonyl-5-methylpyrazol-1-yl)borate] are reported. Their TlIsalts, namely [tris(3-anilinocarbonyl-5-methylpyrazol-1-yl-κN2)borato]thallium(I), [Tl(C33H31BN9O3)], (II), and [tris(3-tert-butylaminocarbonyl-5-methylpyrazol-1-yl-κN2)borato]thallium(I), [Tl(C27H43BN9O3)], (III), as well as the CuIcarbonyl complexes (TpCONHPh,Me)Cu(CO), namely carbonyl[tris(3-anilinocarbonyl-5-methylpyrazol-1-yl-κN2)borato]copper(I) tetrahydrofuran trisolvate, [Cu(C33H31BN9O3)(CO)]·3C4H8O, (IV), and (TpCONHt-Bu,Me)Cu(CO), namely carbonyl[tris(3-tert-butylaminocarbonyl-5-methylpyrazol-1-yl-κN2)borato]copper(I) tetrahydrofuran hemisolvate, [Cu(C27H43BN9O3)(CO)]·0.5C4H8O, (V), have been prepared. Their spectroscopic properties and structures are compared with those of related compounds. The molecules of (II)–(V) show hydrogen bonding to either solvent molecules or neighboring complex moleculesviaamide groups. The title compounds feature the ability to engage other ligands in hydrogen bonding and they show strong electron-withdrawing character. Compound (V) displays voids ofca800 Å3in the crystal structure.

Preparation, Crystal Structure and Spectroscopic Characterization of [Ga(OH)(SO4)(terpy)(H2O)] · H2O (terpy=2,2’:6’,2-Terpyridine): The First Characterized Gallium(III) Sulfato Complex

2004 ◽  
Vol 59 (3) ◽  
pp. 291-297 ◽  
Author(s):  
Andreas Sofetis ◽  
Giannis S. Papaefstathiou ◽  
Aris Terzis ◽  
Catherine P. Raptopoulou ◽  
Theodoros F. Zafiropoulos
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Good Yield ◽  
Spectroscopic Data ◽  
Spectroscopic Characterization ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr

The reaction of Ga2(SO4)3·18H2O and excess 2,2′:6′,2″-terpyridine (terpy) in MeOH / H2O leads to [Ga(OH)(SO4)(terpy)(H2O)]·H2O (1·H2O] in good yield. The structure of the complex has been determined by single-crystal X-ray crystallography. The GaIII atom in 1·H2O is 6-coordinate and ligation is provided by one terdentate terpy molecule, one monodentate sulfate, one terminal hydroxide and one terminal H2O molecule; the coodination polyhedron about the metal is described as a distorted octahedron. There is an extensive hydrogen-bonding network in the crystal structure which generates corrugated layers parallel to bc. The new complex was characterized by IR and 1H NMR spectroscopy. The spectroscopic data are discussed in terms of the nature of bonding

Crystal Structure of and ab initio Calculations on [(C6H5)(CH3)CH-NH]- P(O)(p-OC6H4CH3)2, Syntheses and Spectroscopic Characterization of N-Benzyl Phosphoramidic Acid (4-Methylphenyl)ester Derivatives

2005 ◽  
Vol 60 (1) ◽  
pp. 67-74 ◽  
Author(s):  
Khodayar Gholivand ◽  
Zahra Shariatinia ◽  
Mehrdad Pourayoubi
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Ab Initio Calculations ◽  
Ab Initio ◽  
Spectroscopic Characterization ◽  
Crystalline Lattice ◽  
Independent Molecule ◽  
Nmr Data ◽  
Independent Molecules

Some new N-benzyl phosphoramidic acid (4-methylphenyl)ester derivatives were synthesized and characterized by 1H, 13C, 31P NMR and IR spectroscopy and elemental analysis. The structure of [(C6H5)(CH3)CH-NH]P(O)(p-OC6H4CH3)2 (2) was investigated. This compound exists in polymeric zigzag chains in the crystalline lattice produced by hydrogen bonding built from two alternating independent molecules. NMR data indicate two diastereotopic p-cresol groups as confirmed by Xray crystallography. Ab initio calculations were performed on the geometry of compound 2 at the UHF/6-311G** and B3LYP/6-311G** levels. The optimized structure of each independent molecule contains two different p-cresol groups, in agreement with the experimental results.

scholarly journals Synthesis and Crystal Structure Characterization of Zinc (II) Tetronic Acid Complexes

2010 ◽  
Vol 2010 ◽  
pp. 1-7 ◽  
Author(s):  
K. C. Prousis ◽  
G. Athanasellis ◽  
V. Stefanou ◽  
D. Matiadis ◽  
E. Kokalari ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Structure Characterization ◽  
Synthesis And Characterization ◽  
Zinc Ions ◽  
Carbonyl Groups ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Tetronic Acid

The synthesis and characterization of two new tetronic acid zinc (II) complexes of the empirical formulae [Zn(L–H)2(H2O)2] (1) and [Zn(L–H)2(H2O)(MeOH)]H2O(2) found within the same crystal are reported. The zinc ions bind through alkoxide and carbonyl groups of the ligand 3-methoxycarbonyl-5-phenyl tetronic acid (LH) as indicated byHNMR and X-ray crystallographic studies. These complexes promote intra- and intermolecular interactions, such as hydrogen bonding andπstacking, giving place to the formation of molecular aggregates.

Synthesis, Reactivity and Structural Chemistry of 5,10,15,20-Tetraalkylporphyrins

1999 ◽  
Vol 03 (02) ◽  
pp. 99-116 ◽  
Author(s):  
MATHIAS O. SENGE ◽  
INES BISCHOFF ◽  
NORA Y. NELSON ◽  
KEVIN M. SMITH
Keyword(s):  
Crystal Structure ◽  
Experimental Evidence ◽  
Conformational Flexibility ◽  
Variable Degree ◽  
Free Base ◽  
Absorption Bands ◽  
Tert Butyl ◽  
Full Characterization ◽  
Derivatives Of

The synthesis, reactivity and full characterization of a series of meso-tetraalkyl porphyrins and metalloporphyrins with R ≡ n-butyl (6), 2-methyl-propyl (7), isopropyl (8), l-ethyl-propyl (10) and tert-butyl (11) groups are reported. Derivatives of the last of these show considerably bathochromically shifted absorption bands and the crystal structure of Zn ( II )11(pyr) exhibits a severely ruffled macrocycle conformation. Systematic crystallographic studies of the porphyrins showed that the free base porphyrins with R ≡ n-butyl ( H 26), 2-methyl-propyl ( H 27) and 1-ethyl-propyl ( H 210) are planar. A larger conformational variety was found for the metal complexes. While most Ni ( II ) derivatives and Pd ( II )8 showed a ruffled macrocycle conformation with a degree of ruffling exceeding that of meso-unsubstituted porphyrins, both planar and non-planar forms were found for the related Cu ( II ) derivatives. The Zn ( II ) complexes of porphyrins with isopropyl or 1-ethyl-propyl exhibited conformations with variable degree of distortion. Together with comparative structures from the literature, this study provides experimental evidence that considerable conformational flexibility exists for meso-alkylporphyrins with substituents less bulky than tert-butyl groups.

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