electrospray mass spectrum
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2020 ◽  
Vol 76 (11) ◽  
pp. 1757-1761
Author(s):  
John R. Miecznikowski ◽  
Jerry P. Jasinski ◽  
Tyler J. Ostrowski ◽  
Kendra R. Landy ◽  
Sheila C. Bonitatibus ◽  
...  

The structure of the title compound, [CoCl2(C19H27N7S2)(H2O)], at 173 K has monoclinic (C2/c) symmetry. We report here the synthesis, single-crystal structure, electrospray mass spectrum and NMR spectroscopy of a new six-coordinate cobalt(II) pincer complex. The pincer ligand, in this complex, which is novel, coordinates via three nitrogen atoms (two triazole and one pyridine). The ligand is ambidentate and can coordinate via three nitrogen atoms or two sulfur and one nitrogen atoms. The cobalt(II) metal center has pseudo-octahedral geometry and based on the single-crystal structure, the pincer ligand coordinates in a meridional fashion with the metal and adjacent six-membered ring ligands all in a similar plane and forming two slightly distorted boat configurations. The other two coordinated monodentate ligands are one water molecule and two chloride ions with four cobalt(II) complexes in the unit cell. The asymmetric unit of the complex is comprised of half the pyridine ring and water molecule with the CoII atom at the center of the pincer situated about a twofold axis. The Co—N, Co—O, and Co—Cl bond lengths are consistent with single bonds. In the crystal, the complex forms a three-centre bifurcated weak hydrogen-bonding interaction with a chlorine ion, forming one intermolecular interaction with the pincer group and a water molecule and a second intramolecular interaction with a C—H group within the pincer group. Crystal packing is also highlighted with C 2 2(6)>a<a infinite chains forming along [001] supported by R 2 2(8)>a>a ring motifs, forming a three-dimensional supramolecular network structure. While some stacking of the pyridine rings in the unit cell is observed, there are no relevant π–π interactions in the crystal packing. The 1H and 13C{1H} NMR spectra of the complex are consistent with a plane of symmetry being present. The electrospray mass spectrum, which was collected in positive ion mode, showed the loss of one water molecule and one chloride ligand from the complex. In the future, we plan to screen this cobalt(II) complex for electrocatalysis reactivity.


Author(s):  
Dipta Sarker ◽  
Md. Yeamin Reza ◽  
Md. Masuqul Haque ◽  
Rausan Zamir ◽  
Md. Ali Asraf

Copper (II) complex of the ligand, thiophene-2-aldehyde semicarbazone was synthesized and characterized. Their structures were explored on the basis of CHN analysis, conductance and magnetic susceptibility measurements, spectral studies (FT-infrared and ESI-MS) and thermogravimetric analysis (TGA). It has been observed from spectral and analytical studies, the copper complex have the composition of [CuL(CH3COO)2(H2O)] [where L is thiophene-2-aldehyde semicarbazone]. The electrospray mass spectrum of the ligand and complex exhibited ion at mass-to charge ratio (m/z) of 169.13 and 368.86 matching the calculated values for the molecular ion of the ligand and complex, respectively. One mole of the ligand behaves as bidentate chelating agents around the Cu(II) ion. From conductivity studies, we obtained that the copper complex of the ligand, thiophene-2-aldehyde semicarbazone had no ionic properties. All data confirmed a trigonal bipyramidal geometry of the complex. Antibacterial activity of the compounds against the microbe Enterobacter aerogenes and Bacillus cereus have been screened to reflect that the complex has higher antimicrobial activity than the free ligand.


2010 ◽  
Vol 19 (9) ◽  
pp. 907-913 ◽  
Author(s):  
Hang-Jun Zheng ◽  
Lin-Pei Jin ◽  
Jian-Quan Guo ◽  
Jin-You Zhuang ◽  
Long-Gen Zhu ◽  
...  

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