scholarly journals Synthesis, crystal structure, and theoretical studies of a macrocyclic silver(I) complex of imino-pyridyl Schiff base ligand

2021 ◽  
Vol 12 (3) ◽  
pp. 248-255
Author(s):  
Jahangir Mondal ◽  
Meman Sahu ◽  
Bhaskar Sharma ◽  
Rakesh Ganguly ◽  
Shubhamoy Chowdhury ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Complex I ◽  
Average Distance ◽  
Spectroscopic Techniques ◽  
Triclinic Space Group ◽  
X Ray ◽  
Elemental Analyses ◽  
Photophysical Studies ◽  
Pyridyl Ligand

The synthesis and characterization of an imino-pyridyl ligand N,N'-(butane-1,4-diyl)bis(1-(pyridin-2-yl)methanimine) (L) and its Ag(I)ClO4 complex (I) by various spectroscopic techniques and elemental analyses is presented in this study. X-ray single crystal structure of complex I revealed that in complex I, each Ag(I) ion is tetra coordinated with two pyridine N-atoms and two imine N-atoms of the ligand L, forming a macrocyclic dimeric Ag(I) grid. In the macrocyclic dimer complex I, Ag-Ag separation along the chain is 5.318 Å. The Ag-Npy average distance is 2.396 Å and that of the Ag-Nim is 2.257 Å. The macrocyclic dimer complex I is supramolecularly arranged by π-stacking interactions. Computational, Hirshfeld surface analysis and photophysical studies on ligand L and complex I have also been performed. Crystal data for C32H36Ag2Cl2N8O8 (M =947.33 g/mol): Triclinic, space group P-1 (no. 2), a = 9.1714(12) Å, b = 10.4373(14) Å, c = 10.8297(14) Å, α = 112.317(3)°, β = 91.391(3)°, γ = 92.353(3)°, V = 957.3(2) Å3, Z = 1, T = 293.15 K, μ(MoKα) = 1.220 mm-1, Dcalc = 1.643 g/cm3, 10248 reflections measured (4.07° ≤ 2Θ ≤ 53.098°), 3966 unique (Rint = 0.0280, Rsigma = 0.0331) which were used in all calculations. The final R1 was 0.0722 (I > 2σ(I)) and wR2 was 0.2229 (all data).

Structural and IR-spectroscopic characterization of magnesium acesulfamate

2016 ◽  
Vol 71 (1) ◽  
pp. 51-55 ◽  
Author(s):  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Elemental Analysis ◽  
Spectroscopic Characterization ◽  
Magnesium Carbonate ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir Spectroscopic

AbstractMagnesium acesulfamate, Mg(C4H4NO4S)2·6H2O, was prepared by the reaction of acesulfamic acid and magnesium carbonate in aqueous solution, and characterized by elemental analysis. Its crystal structure was determined by single crystal X-ray diffraction methods. The substance crystallizes in the triclinic space group P1̅ with one molecule per unit cell. The FTIR spectrum of the compound was also recorded and is briefly discussed. Some comparisons with other simple acesulfamate and saccharinate salts are also made.

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.

Synthesis and structural characterization of Mn(II) and Cu(II) complexes with bis(4-(1H-imidazol-1-yl)phenyl)methanone ligands

2017 ◽  
Vol 72 (1) ◽  
pp. 83-87 ◽  
Author(s):  
Gao-Feng Wang ◽  
Xiao Zhang ◽  
Zhao-Rong Liu ◽  
Yu-Chun Wang ◽  
Hong-Shi Jiang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Octahedral Geometry ◽  
Helical Chain ◽  
Distorted Octahedral Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bridging Ligand ◽  
Distorted Octahedral ◽  
Elemental Analyses

AbstractTwo complexes, {Mn(hfac)2(BIPMO)}n (1), {Cu(hfac)2(BIPMO)}n (2) [hfac=1,1,1,5,5,5-hexafluoro-pentane-2,4-dionato(–), BIPMO=bis(4-(1H-imidazol-1-yl)phenyl)methanone], with the V-shaped ligands were synthesized and characterized by infrared spectroscopy, elemental analyses, along with single-crystal X-ray diffraction analyses. The X-ray diffraction studies have shown that the metal ions in 1 and 2 are both six-coordinated to two nitrogen atoms of two BIPMO ligands and four oxygen atoms of two hfac ligands to form a distorted octahedral geometry. Each BIPMO ligand acts as a bridging ligand to link two adjacent metal(II) atoms to form a helical chain in the crystal structure.

scholarly journals SYNTHESIS, CRYSTAL STRUCTURE AND SPECTRAL PROPERTIES OF COPPER(II) AND COBALT(II) 3-METHYLTHIOPHENE-2- CARBOXYLATO COMPLEXES WITH FUROPYRIDINES

2013 ◽  
Vol 12 (2) ◽  
pp. 75-82
Author(s):  
Jozef Miklovič ◽  
Miroslava Bašnárová ◽  
Peter Segľa ◽  
Marián Koman
Keyword(s):  
Crystal Structure ◽  
Crystal Structure Analysis ◽  
Carboxylic Group ◽  
X Ray ◽  
Monomeric Complex ◽  
Distorted Octahedral ◽  
Elemental Analyses ◽  
Single Crystal Structure Analysis ◽  
Mode Of Coordination

Abstract The synthesis and characterization of eleven new Cu(II) and Co(II) complexes is reported. The complexes were characterized by elemental analyses, infrared and electronic spectra. Copper(II) with 3- methylthiophene-2-carboxylic acid (HMTK) forms a dinuclear complex of the acetate type [Cu2(MTK)4(H2O)2]. By reaction of this complex with 2-metylfuro[3,2-c]pyridine (MeFP), not only acetate type complexes [Cu2(MTK)4L2] (L= FP, MeFP) were obtained, but also monomeric complex [Cu(MTK)2(FP)2]. In the cases of [1]benzofuro[3,2-c]pyridine (BFP) and 2-(3-trifluoromethylphenyl) furo[3,2-c]pyridine (CF3FP) only monomeric complexes [Cu(MTK)2L2] (L = BFP, CF3FP) were obtained. It is possible to observe, that with increasing amount of the ligand, the yield of monomeric complexes increases too. In monomeric complexes, the carboxylic group of anionic MTK binds to atom Cu(II) by asymmetrically chelating O,O-coordination. The crystal structure of the complex [Cu(MTK)2(MeFP)2] was determined by X-ray single crystal structure analysis. The copper(II) atom lies in the crystallographic centre of symmetry in an distorted tetragonal-bipyramidal arrangement. The structure of this complex confirms an asymmetric chelate coordination of the carboxylic group. HMTK and Cobalt(II) form coordination compound [Co(H2O)6](MTK)2 with assumed ionic mode of coordination of anionic MTK. With furopyridines monomeric complexes [Co(MTK)2L2] (L= FP, MeFP, BFP, CF3FP) with distorted octahedral coordination polyhedron around Co(II), were formed.

scholarly journals Imino-pyridyl and PPh3 mixed ligand complexes of Cu(I)X (X: I, Br, and Cl): Synthesis, structure, DFT and Hirshfeld surface studies

2020 ◽  
Vol 11 (4) ◽  
pp. 334-341
Author(s):  
Jahangir Mondal ◽  
Amit Kumar Manna ◽  
Goutam Kumar Patra
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Room Temperature ◽  
Hirshfeld Surface ◽  
Mixed Ligand ◽  
Crystal Data ◽  
Surface Studies ◽  
Triclinic Space Group ◽  
X Ray ◽  
Pyridyl Ligand

Three new halide bridged copper(I)complexes [Cu2(µ-L)(µ-X)2)(PPh3)2]n {X: I (1), Br (2) and Cl (3)} have been synthesized by the reaction of Cu(I)X (X: I, Br and Cl) with PPh3 and the polydentate imino-pyridyl ligand L. Interestingly, copper(I) forms coordination polymers with the ligand L and the co-ligand PPh3. These complexes 1, 2 and 3 have been characterized by elemental analysis, IR, UV-Vis, and NMR spectroscopy. The crystal structure of the complex 2 has been determined by single-crystal X-ray analysis. Crystal data for complex 2: triclinic, space group P-1 (no. 2), a = 9.471(10) Å, b = 11.043(11) Å, c = 13.215(18) Å, α = 65.853(18)°, β = 69.94(2)°, γ = 67.350(14)°, V = 1135(2) Å3, Z = 2, T = 296.15 K, μ(MoKα) = 2.806 mm-1, Dcalc = 1.535 g/cm3, 4059 reflections measured (3.462° ≤ 2Θ ≤ 44.818°), 2639 unique (Rint = 0.0637, Rsigma = 0.1621) which were used in all calculations. The final R1 was 0.0700 (I > 2σ(I)) and wR2 was 0.2207 (all data). Hirshfeld surface analysis of the complex 2 showed H···H, N···H and Br···H interactions of 55.9, 14.4 and 4.1%, respectively. MEP of ligand L reflects the whole molecule is reddish yellow in color because of equally distributed electron density over the molecule. For this reason, the ligand is supramolecularly arranged via -{CuI2-µ-X2} rhomboid core in the complex 2. The ligand L is non-emissive at room temperature in dichloromethane, whereas the complexes 1, 2 and 3 are photoluminescent. DFT and Hirshfeld surface studies have also been performed for complex 2.

Two-dimensional lanthanide(III) coordination polymers: solvothermal synthesis, crystal structure, and stability

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Runmei Ding ◽  
Zixin He ◽  
Meilin Wang ◽  
Danian Tian ◽  
Peipei Cen
Keyword(s):  
Crystal Structure ◽  
Coordination Polymers ◽  
Solvothermal Synthesis ◽  
Analysis Data ◽  
Water Stability ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Solvothermal Conditions

AbstractBased on 2-(4-pyridyl)-terephthalate (H2pta) and oxalate ligands, two new lanthanide-containing coordination polymers (CPs), [Tb(pta)(C2O4)0.5(H2O)2)]·2H2O (1) and [Sm(pta)(C2O4)0.5(H2O)2)]·2H2O (2), have been synthesized under solvothermal conditions. The structures of both 1 and 2 have been determined by single-crystal X-ray diffraction. Infrared, elemental analysis, powder X-ray diffraction and thermogravimetric analysis data are also presented. The crystals of 1 and 2 exhibit isostructural layer-like networks, crystallizing in the triclinic space group P$‾{1}$. The layers are further stabilized and associated into 3D architectures through hydrogen bonding. Remarkably, the CPs 1 and 2 exhibit excellent water stability and remarkable thermostability with thermal decomposition temperatures of more than 420 °C.

Synthesis and Crystal Structure of the Flexible Ligand Coordination Polymer [Co3(bpd)5.5(NCS)6(NH3)]n⋅2H2O(bpd= 1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene)

2013 ◽  
Vol 803 ◽  
pp. 80-84
Author(s):  
Yu Qi Liu ◽  
Yong Yang ◽  
Rui Yang ◽  
Xiao Jun Xu
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Coordination Polymer ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Elemental Analyses ◽  
Ligand Coordination ◽  
Point Symbol

A novel metalorganic coordination polymer, namely [Co3(bpd)5.5(NCS)6(NH3)]n2H2O (1) (bpd=1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene), has been synthesized and characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. Compound 1 presents 2D[3,4,-connected 3-nodal net with the point symbol (4268210)(4462)(8210). In addition, four identical 2D single nets is interlocked with each other in parallel, thus directly leading to the formation of a polycatenated layer (2D2D).

The preparation and characterization of Pt(Se3PPh)(PR3)2; the X-ray crystal structure of Pt(Se3PPh)(dppe)·CH2Cl2

Polyhedron ◽  
1990 ◽  
Vol 9 (7) ◽  
pp. 987-990 ◽  
Author(s):  
Ivan P. Parkin ◽  
Mark J. Pilkington ◽  
Alexandra M.Z. Slawin ◽  
David J. Williams ◽  
J.Derek Woollins
Keyword(s):  
Crystal Structure ◽  
X Ray

Structural Systematics of Rare Earth Complexes. VII. Crystal Structure of Bis(2,2'/6',2␛-Terpyridinium) Octaaquaterbium(III) Heptachloride Hydrate

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Title Compound ◽  
Room Temperature ◽  
Chloride Ions ◽  
Full Matrix ◽  
X Ray

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.

A 35-year-old mystery solved: a facile synthetic route and structural confirmation of tetrachlorobis(diethyl ether)tungsten(IV)

2021 ◽  
Vol 77 (4) ◽  
Author(s):  
Thomas E. Shaw ◽  
Alfred P. Sattelberger ◽  
Titel Jurca
Keyword(s):  
Crystal Structure ◽  
Diethyl Ether ◽  
Thermal Instability ◽  
Room Temperature ◽  
Surface Characteristics ◽  
Hirshfeld Surface ◽  
Asymmetric Unit ◽  
Synthetic Route ◽  
X Ray ◽  
Elemental Analyses

The true identity of the diethyl ether adduct of tungsten(IV) chloride, WCl4(Et2O) x , has been in doubt since 1985. Initially postulated as the bis-adduct, WCl4(Et2O)2, questions arose when elemental analyses were more in line with a mono-ether adduct, viz. WCl4(Et2O). It was proposed that this was due to the thermal instability of the bis-adduct. Here, we report the room-temperature X-ray crystal structure and Hirshfeld surface characteristics of trans-tetrachloridobis(diethyl ether)tungsten(IV), trans-WCl4(Et2O)2 or trans-[WCl4(C4H10O)2]. The compound crystallizes, with half of the molecule in the asymmetric unit, in the centrosymmetric space group P21/n. The W—O distance is 2.070 (2) Å, while the W—Cl distances are 2.3586 (10) and 2.3554 (10) Å.

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