Synthesis and structural studies on Ni(II) dithiocarbamates: Exploring intramolecular Ni⋯H–C interactions

Abstract[Ni(dtc)2] (dtc = N‐(pyrrole‐2‐ylmethyl)‐N‐thiophenemethyldithiocarbamate (1), N‐methylferrocenyl‐N‐(2‐phenylethyl)dithiocarbamate (2), N‐furfuryl‐N‐methylferrocenyldithiocarbamate (3), and (N‐[pyrrole‐2‐ylmethyl]‐N‐thiophenemethyldithiocarbamato‐S,S′)(thiocyanato‐N)(triphenylphosphine)nickel(II) (4) complexes were prepared and characterized by elemental analysis, infrared, ultraviolet–visible, and nuclear magnetic resonance (1H and 13C) spectroscopies. The data were consistent with the formation of square planar nickel(II) complexes, which was confirmed by single‐crystal X‐ray diffraction studies on 2 and 4. Fe···Fe interactions exhibited by complex 2 led to supramolecular aggregation. The structure of 4 reveals intermolecular and intramolecular C‐H···Ni anagostic interactions. The anion‐sensing properties of 2 were studied with halide ions by cyclic voltammetry. It was observed that 2 acts as sensor for bromide. Complexes 1, 2, and 3, were utilized to prepare nickel sulfide, nickel–iron sulfide‐1, and nickel–iron sulfide‐2, respectively. The composition, structure, morphology, and optical properties of nickel sulfide and nickel–iron sulfides were examined using powder X‐ray diffraction, transmission electron microscopy, energy‐dispersive X‐ray spectroscopy, ultraviolet–visible, fluorescence, and infrared spectroscopy. Powder X‐ray diffraction patterns of nickel sulfide, nickel–iron sulfide‐1, and nickel–iron sulfide‐2 indicate the formation of orthorhombic Ni9S8, cubic NiFeS2, and cubic Ni2FeS4, respectively. The photocatalytic activities of as‐prepared nickel sulfide and nickel–iron sulfide‐1 nanoparticles were investigated for photodegradation of methylene blue and rhodamine‐B under ultraviolet irradiation. Nickel–iron sulfide‐1 nanoparticles show slightly higher photodegradation efficiency compared with the nickel sulfide nanoparticles.

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Synthesis of nickel sulfide and nickel–iron sulfide nanoparticles from nickel dithiocarbamate complexes and their photocatalytic activities

Thirumaran

Gurumoorthy

Arulmozhi

et al. 2020

Applied Organom Chemis

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Regiospecific Remote Pt–H Interactions in Oligomethylene‐Vaulted (N^{^}C^{^}N)‐Pincer Pt^II Complexes

et al. 2018

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(N^C^N)‐Pincer type bis(iminomethyl)phenylPtII complexes 1 and 2 having a macrocyclic vaulting structure consisting of deca‐ undeca‐, and dodecamethylene bridges were synthesized and subsequently characterized by NMR, IR spectroscopy, mass spectrometry, and single‐crystal XRD. Unprecedented remote intramolecular Pt–H interactions were observed on the linker hydrogen atoms at β‐and ζ‐positions in a highly regiospecific manner both in the crystal and solution states. The hydrogen bonding nature, originating from overlap between Pt dz² and σ* of the specific C–H bonds, was revealed by NBO analysis of 1 on the basis of dispersion‐corrected DFT calculations.

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Novel dithiocarbamate–Hg(II) complexes containing mixed ligands: Synthesis, spectroscopic characterization, and H₂ storage capacity

Al-Nassiry

Al‐Janabi

Al-Janabi

et al. 2019

J Chinese Chemical Soc

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A tetrahedral Hg(II) diethyl dithiocarbamate (Et 2 Dt) complex containing triphenylphosphine (PPh 3 ) of the composition [HgCl(κ 2 -Et 2 Dt) 2 (PPh 3 )] (1) is prepared. Furthermore, complex (1) is used as a synthone to prepare a novel series of complexes of the following composition [Hg(Et 2 Dt)L(PPh 3 )] {L = saccharinate (2), thiosaccharinate (3), benzisothiazolinate (4), benzothiozole-2-thiolate (5), and benzooxazole-2-thiolate (6) anions}. The resulted complexes(1)-(6) are characterized by elemental analysis, molar conductivity, powder X-ray diffraction, fourier transform Infrared, and NMR ( 1 H and 31 P) spectroscopic techniques. The Et 2 Dt ligand is coordinated as bidentate chelate through the sulfur atoms, whereas the L ligands are bonded as monodentate ligands to afford a tetrahedral geometry around the Hg(II) ion. Nitrogen adsorptiondesorption isotherm for two of as-prepared complexes (2) and (3) are measured first to get their Brunauer-Emmett-Teller surface area. Moreover, the mentioned two complexes are evaluated for their ability to store hydrogen gas at 77 K. However, the results of the hydrogen storage tests proved that the selected complexes are all capable of storing hydrogen, but in varying degrees, where complex (2) exhibited a storage capacity of 4.22 wt% under 88 bar. K E Y W O R D Sbidentate chelate, complexes, diethyl dithiocarbamate, Hg(II), hydrogen storage

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Synthesis and structural studies on Ni(II) dithiocarbamates: Exploring intramolecular Ni⋯H–C interactions

Cited by 15 publications

References 43 publications

Synthesis of nickel sulfide and nickel–iron sulfide nanoparticles from nickel dithiocarbamate complexes and their photocatalytic activities

Synthesis of nickel sulfide and nickel–iron sulfide nanoparticles from nickel dithiocarbamate complexes and their photocatalytic activities

Regiospecific Remote Pt–H Interactions in Oligomethylene‐Vaulted (N^{^}C^{^}N)‐Pincer Pt^II Complexes

Novel dithiocarbamate–Hg(II) complexes containing mixed ligands: Synthesis, spectroscopic characterization, and H₂ storage capacity

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Synthesis and structural studies on Ni(II) dithiocarbamates: Exploring intramolecular Ni⋯H–C interactions

Cited by 15 publications

References 43 publications

Synthesis of nickel sulfide and nickel–iron sulfide nanoparticles from nickel dithiocarbamate complexes and their photocatalytic activities

Synthesis of nickel sulfide and nickel–iron sulfide nanoparticles from nickel dithiocarbamate complexes and their photocatalytic activities

Regiospecific Remote Pt–H Interactions in Oligomethylene‐Vaulted (N^C^N)‐Pincer PtII Complexes

Novel dithiocarbamate–Hg(II) complexes containing mixed ligands: Synthesis, spectroscopic characterization, and H2 storage capacity

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Product

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Regiospecific Remote Pt–H Interactions in Oligomethylene‐Vaulted (N^{^}C^{^}N)‐Pincer Pt^II Complexes

Novel dithiocarbamate–Hg(II) complexes containing mixed ligands: Synthesis, spectroscopic characterization, and H₂ storage capacity