Development of a Novel Method for Quantitative Determination of Indomethacin

A new green analytical chemistry method using a Ultraviolet–visible (UV-Vis) Spectroscopy is proposed to measure Indomethacin (as cuprous complex); Designate, sophisticated, and proved for determination pure mode of indomethacin, and at dosage forms respective. The present study was prepared quantitatively of the Indomethacin complex, and the molar ratio between the cuprous and indomethacin (1:1) is measured by UV-Vis spectroscopy, the maximum absorbance peak of cuprous complex was measured at (319 nm) in wavelength range (190‐900 nm), at range of the concentration (10–60μg.mL-1) the linear calibration curve was painted and show regression equation (Y = 0.0036X – 0.0054) and correlation Coefficient (R2 = 0.9999). This study was validated and applied to the estimation of indomethacin in tablets from one company in Iraqi markets, when the wavelength and the analysis conditions were determined, no interference was found. It was concluded that the advanced method was accurate, sensitive, precise, and repeatable.

A new heteroleptic phosphorescent cuprous complex supported by a BINAP ligand: synthesis, structure, luminescence properties and theoretical analyses

Luminescent cuprous complexes are an important class of coordination compounds due to their relative abundance, low cost and ability to display excellent luminescence. The heteroleptic cuprous complex solvate rac-(acetonitrile-κN)(3-aminopyridine-κN)[2,2′-bis(diphenylphosphanyl)-1,1′-binaphthyl-κ2 P,P′]copper(I) hexafluoridophosphate dichloromethane monosolvate, [Cu(C5H6N2)(C2H3N)(C44H32P2)]PF6·CH2Cl2, conventionally abbreviated as [Cu(3-PyNH2)(CH3CN)(BINAP)]PF6·CH2Cl2, (I), where BINAP and 3-PyNH2 represent 2,2′-bis(diphenylphosphanyl)-1,1′-binaphthyl and 3-aminopyridine, respectively, is described. In this complex solvate, the asymmetric unit consists of a cocrystallized dichloromethane molecule, a hexafluoridophosphate anion and a complete racemic heteroleptic cuprous complex cation in which the cuprous centre, in a tetrahedral CuP2N2 coordination, is coordinated by two P atoms from the BINAP ligand, one N atom from the 3-PyNH2 ligand and another N atom from a coordinated acetonitrile molecule. The UV–Vis absorption and photoluminescence properties of this heteroleptic cuprous complex have been studied on polycrystalline powder samples, which had been verified by powder X-ray diffraction before recording the spectra. Time-dependent density functional theory (TD-DFT) calculations and a wavefunction analysis reveal that the orange–yellow phosphorescence emission should originate from intra-ligand (BINAP) charge transfer mixed with a little of the metal-to-ligand charge transfer 3(IL+ML)CT excited state.

Comparative Analysis of Crystal Structures between 2,2′-Bipyridine and 6,6′-Dimethyl-2,2′-Bipyridine Supported CuSCF3 Complexes: An Unusual Coordination Transition from Mononuclear to Binuclear Mode

We report herein the synthesis of CuSCF3 complex supported by 6,6′-dimethyl-2,2′-bipyridine via the strategy of triphenylphosphine-mediated deoxygenation of CF3SO2Na in the presence of cuprous chloride. The molecular structure of this new cuprous complex was characterized by elemental analysis, 1H (13C, 19F) NMR spectra and verified by X-ray crystallography. Unlike the classical [(2,2′- bipyridine)Cu(SCF3)] complex, 6,6′-dimethyl-2,2′-bipyridine supported cuprous trifluoromethylthiolate complex was dimerized in the form of [{(6,6′-dimethyl-2,2′-bipyridine)Cu(SCF3)}2]. The X-ray crystal structure revealed the Cu2S2 cyclic pattern and sulfur atoms serving as the bridge. The Cu-Cu distance was equal to 3.083 Å which was remarkably longer than the analogous [{(1,10-phenanthroline)Cu(SCF3)}2] (2.5781(9) Å). This interesting phenomenon demonstrated that the substituents on the ligand scaffolds have profound influence on the coordination modes of these N,N-ligand coordinated CuSCF3 complexes.

Synthesis and X-Ray Crystal Structure of 1,1'-Bis(diphenyphosphino)ferrocene Supported CuSCF3 Complex

We report herein the synthesis of CuSCF3 complex supported by 1,1'-bis(diphenyphosphino)ferrocene via deoxygenative reduction of Langlois reagent (CF3SO2Na). This cuprous complex [(dppf)Cu(SCF3)] was fully characterized by elemental analysis and 1H (13C, 19F, 31P) NMR spectra. In addition, the molecular structure of [(dppf)Cu(SCF3)] was established by X-ray crystallography. The crystal of compound 1 crystallizes in monoclinic, space group P21/n with a = 11.4366(9), b = 19.1340(16), c = 14.0625(11) Å, V = 3072.62(2) Å3, Z = 4, Z’ = 0, C35H28CuF3FeP2S, Mr = 719.00 and R-factor = 3.69. The short contacts between the two fluorine atoms of CF3S moiety and aromatic hydrogen of Cp/(Ph) rings were observed with leaving the sterically-congested fluorine untouched which highly resembled to the sibling [(PPh3)2CuSCF3]. These interesting secondary interactions in the crystal lattice were explained by the electrostatic forces in terms of the strong dipole of C-F bonds.

A new phosphorescent heteroleptic cuprous complex with a neutral 2-methylquinolin-8-ol ligand: synthesis, structure characterization, properties and TD–DFT calculations

Luminescent CuI complexes have emerged as promising substitutes for phosphorescent emitters based on Ir, Pt and Os due to their abundance and low cost. The title heteroleptic cuprous complex, [9,9-dimethyl-4,5-bis(diphenylphosphanyl)-9H-xanthene-κ2 P,P](2-methylquinolin-8-ol-κ2 N,O)copper(I) hexafluorophosphate, [Cu(C10H9NO)(C39H32OP2)]PF6, conventionally abbreviated as [Cu(Xantphos)(8-HOXQ)]PF6, where Xantphos is the chelating diphosphine ligand 9,9-dimethyl-4,5-bis(diphenylphosphanyl)-9H-xanthene and 8-HOXQ is the N,O-chelating ligand 2-methylquinolin-8-ol that remains protonated at the hydroxy O atom, is described. In this complex, the asymmetric unit consists of a hexafluorophosphate anion and a whole mononuclear cation, where the CuI atom is coordinated by two P atoms from the Xantphos ligand and by the N and O atoms from the 8-HOXQ ligand, giving rise to a tetrahedral CuP2NO coordination geometry. The electronic absorption and photoluminescence properties of this complex have been studied on as-synthesized samples, whose purity had been determined by powder X-ray diffraction. In the detailed TD–DFT (time-dependent density functional theory) studies, the yellow emission appears to be derived from the inter-ligand charge transfer and metal-to-ligand charge transfer (M+L′)→LCT excited state (LCT is ligand charge transfer).