Synthetic, structural and biochemical approach of the macro cyclic complexes of manganese (II) and tin (II)

2021 ◽  
Vol 25 (7) ◽  
pp. 161-166
Author(s):  
Nidhi Bansal ◽  
Saurabh Dave ◽  
Ruchi Seth
Keyword(s):  
Metal Ion ◽  
Biological Properties ◽  
Molar Ratio ◽  
High Yield ◽  
Spectral Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Elemental Analyses ◽  
Biochemical Approach ◽  
Formation Of Complexes

This study presents a brief account of the synthesis, spectroscopic and biochemical aspects of tetraazamacrocyclic complexes of managenese (II) and tin (II). The complexes of manganese (II) and tin (II) were prepared by the template condensation of metal salts with phthalic acid and diamines (1,3-diaminobutane and 1,4- diaminobutane) in 1:2:2 molar ratio. All the complexes are soluble in polar solvent. The structures were investigated using elemental analyses, molecular weight determinations, conductivity measurements, electronic, infrared and X-Ray diffraction spectral studies. The elemental analyses are consistent with the formation of complexes of the type [M(Macn)Cl2] (where, n=1-2, M=Mn(II), Sn (II)). An octahedral geometry around the metal ion is suggested for these complexes. All the complexes were screened against several fungi and bacteria to assess its biological properties and results are discussed.The importance of this method includes shorter reaction time and high yield.

scholarly journals Synthesis and spectroscopic characterization of some lanthanide(III) nitrate complexes of 3-[3-carboxyethyl-4,5- dimethylthiophene-2-yl)azo]pent-2,4-dione

2011 ◽  
Vol 76 (2) ◽  
pp. 249-261 ◽  
Author(s):  
Janardhanan Athira ◽  
Yesodharan Sindhu ◽  
Susamma Sujamol ◽  
Kochukittan Mohanan
Keyword(s):  
Elemental Analysis ◽  
Metal Ion ◽  
Spectroscopic Characterization ◽  
Molar Conductance ◽  
Spectral Studies ◽  
Structural Form ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nitrate Complexes

3-[3-Carboxyethyl-4,5-dimethylthiophene-2-yl)azo]pent-2,4-dione was synthesized by coupling diazotized 2-amino-3-carboxyethyl- 4,5-dimethylthiophene with acetylacetone. Based on various spectral studies and elemental analysis, an intramolecularly hydrogen bonded azoenol structural form was assigned for the ligand. This ligand is versatile in forming a series of lanthanide(III) complexes viz, lanthanum(III), cerium(III), praseodymium(III), neodymium(III), samarium(III) and gadolinium(III), which were characterized through various spectral studies, elemental analysis, magnetic susceptibility measurements, molar conductance and thermal analysis. The spectral data revealed that the ligand acted as a neutral tridentate, coordinating to the metal ion through one of the azo nitrogen atoms, the ester carbonyl and the enolic oxygen of the acetylacetone moiety, without deprotonation. Molar conductance values adequately supported their non-electrolytic nature. The ligand and lanthanum(III) complexes were subjected to X-ray diffraction studies. In addition, the lanthanum(III) complex underwent a facile transesterification reaction on refluxing with methanol for a long period. The thermal behavior of the lanthanum(III) complex was also examined.

Darstellung und Kristallstrukturbestimmung von 1,2-Di-t-butyl-1,2-diiodo- diarsan (t-C4H9AsI)2 und Synthese von 1,2,3,4-Tetrakis(t-butyl)tetraarsetan (t-C4H9As)4 über selektive Reduktion von t-Butylarsendiiodid t-C4H9AsI2 Synthesis and Crystal Structure of 1,2-Di-t-butyl-1,2-diiododiarsane (t-C4H9AsI)2 and Synthesis of 1,2,3,4-Tetrakis(t-butyl)tetraarsetane (t-C4H9As)4 via Selective Reduction of t-Butylarsenic Diiodide t-C4H9AsI2

1997 ◽  
Vol 52 (7) ◽  
pp. 790-794 ◽  
Author(s):  
Klaus Megges ◽  
Evgeni V. Avtomonov ◽  
Jörg Lorberth
Keyword(s):  
Crystal Structure ◽  
Low Temperatures ◽  
Selective Reduction ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Elemental Analyses ◽  
High Yields ◽  
C Nmr

Abstract 1,2,3,4-Tetrakis(t-butyl)tetraarsetane (t-C4H9As)4(4) has been synthesized by reduction of t-butylarsenic (III) diiodide (1) with equivalent quantities of either Mg, Ca, Zn, Li, or CoCp2 in THF at low temperatures in high yields. Treatment of 1 with CoCp2 in a molar ratio 1:1 in n-pentane at -78 °C leads to the formation of 1,2-di-t-butyl-1,2-diiododiarsine (2) (t-C4H9AsI)2 in 69 % yield. The products have been characterized by spectroscopic methods (H, 13C-NMR, EI-MS) and elemental analyses. The crystal structure of 2 has been determined by X-ray diffraction methods.

Gold Clustering at Dimethylsulfoximine Me2S(O)NH

2000 ◽  
Vol 55 (10) ◽  
pp. 889-894 ◽  
Author(s):  
Armin Hamel ◽  
Christian Hollatz ◽  
Annette Schier ◽  
Hubert Schmidbaur
Keyword(s):  
Nitrogen Atom ◽  
Dinuclear Complex ◽  
Trinuclear Complex ◽  
Molar Ratio ◽  
High Yield ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molar Ratios ◽  
Pyramidal Configuration ◽  
Unknown Structure

Abstract Gold Clustering, Dimethylsulfoximine Polyaurated complexes of the dimethylsulfoximide anion [Me2S(O)N]- have been prepared by reacting N-trimethylsilyl-dimethylsulfoximide with [(Ph3P)Au]BF4 in various molar ratios. With one or two equivalents of the gold(I) reagent only the dinuclear complex is obtained in high yield: {[(Ph3P)Au]2NS(O)Me2}+ BF4- . With three or four equivalents only the trinuclear complex is produced: {[(Ph3P)Au]3NS(O)Me2}2+ 2 BF4- . No mono- or tetra-auration was observed, respectively. The composition of the compounds has been confirmed by analytical and spectroscopic data, and the crystal structure of the dinuclear compound has been determined by single crystal X-ray diffraction of the dichloromethane solvate. The two gold atoms are found to be coordinated to the nitrogen atom with a small Au-N-Au angle of only 92.3(3)° and a short Au-Au distance of 2.9900(5) Å. The nitrogen atom is in a distorted trigonal pyramidal configuration which allows an intramolecular SO-Au contact. For the trinuclear complex a structure with a tetracoordinate nitrogen atom [SNAU3] is proposed which is analogous to the corresponding complexes of phosphinimines R3P=NH. With the ditertiary phosphine Ph2PCH2Ch2PPh2 (dppe) a cyclic dinuclear complex (dppe)Au2[NS(0 )Me2]BF4 can be synthesized starting from (dppe)Au2Cl2. The reaction of the phosphine-rich precursor [(Ph3P)2Au]BF4 with Me3SiNS(0 )Me2 in the molar ratio 2:1 affords a binuclear complex {[(Ph3P)2Au]2NS(0 )Me2}BF4 of an as yet unknown structure

scholarly journals Bacterial Cellulose-Hydroxyapatite Nanocomposites for Bone Regeneration

2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
S. Saska ◽  
H. S. Barud ◽  
A. M. M. Gaspar ◽  
R. Marchetto ◽  
S. J. L. Ribeiro ◽  
...  
Keyword(s):  
Bone Regeneration ◽  
Bacterial Cellulose ◽  
Biological Properties ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Spectroscopy Analysis ◽  
X Ray ◽  
Fourier Transformed Infrared Spectroscopy ◽  
Cellulose Membranes

The aim of this study was to develop and to evaluate the biological properties of bacterial cellulose-hydroxyapatite (BC-HA) nanocomposite membranes for bone regeneration. Nanocomposites were prepared from bacterial cellulose membranes sequentially incubated in solutions of CaCl2followed by Na2HPO4. BC-HA membranes were evaluated in noncritical bone defects in rat tibiae at 1, 4, and 16 weeks. Thermogravimetric analyses showed that the amount of the mineral phase was 40%–50% of the total weight. Spectroscopy, electronic microscopy/energy dispersive X-ray analyses, and X-ray diffraction showed formation of HA crystals on BC nanofibres. Low crystallinity HA crystals presented Ca/P a molar ratio of 1.5 (calcium-deficient HA), similar to physiological bone. Fourier transformed infrared spectroscopy analysis showed bands assigned to phosphate and carbonate ions.In vivotests showed no inflammatory reaction after 1 week. After 4 weeks, defects were observed to be completely filled in by new bone tissue. The BC-HA membranes were effective for bone regeneration.

Formation of the Complexes [Fe(H2BDI)3]X2 and [CpCr(H2BDI)2]X2 (X =OTf) fromthe Unusual Reactions of Benzil-bis(trimethylsilyl)diimine with CpML2Cl (M = Fe, L = CO; M = Cr, L = NO)

2010 ◽  
Vol 65 (2) ◽  
pp. 101-106 ◽  
Author(s):  
Nadera Haque ◽  
Bernd Neumann ◽  
Ingo-Peter Lorenz
Keyword(s):  
Molecular Structures ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
First Case ◽  
Distorted Octahedral ◽  
Elemental Analyses ◽  
Diimine Ligand ◽  
Tetragonal Pyramidal ◽  
C Nmr ◽  
Formation Of Complexes

The reaction of CpML2Cl (M = Fe, L = CO; M = Cr, L = NO) with benzil diimine (H2BDI) (2) derived from benzil-bis(trimethylsilyl)diimine (Si2BDI) (1) in a 1 : 3 and 1 : 2 molar ratio in the presence of excess AgO3SCF3 (= AgOTf) resulted in the formation of the new cationic tris- and bisbenzildiimine complexes [Fe(H2BDI)3]X2 (3) and [CpCr(H2BDI)2]X2 (X = OTf) (4), respectively. The addition of AgO3SCF3 is necessary in both cases to abstract chloride. Unusual in the first case is the total replacement of ligands of CpFe(CO)2Cl and in the second case the oxidation of Cr(0) to Cr(III) leading to the formation of complexes 3 and 4, respectively, with the neutral bidentate diimine ligand 2. Complexes 3 and 4 were fully characterized by their IR, mass, 1H- and 13C-NMR spectra, as well as elemental analyses. The molecular structures determined by X-ray diffraction studies reveal a distorted octahedral tris-chelate configuration in 3 and a pseudo-tetragonal pyramidal one in 4.

Bis(silylation) of Tris(dimethylamino)phosphonium Methylide

1997 ◽  
Vol 52 (6) ◽  
pp. 674-678 ◽  
Author(s):  
Karl-Heinz Dreihäupl ◽  
Andreas Bauer ◽  
Hubert Schmidbaur
Keyword(s):  
Carbon Atom ◽  
Quantum Chemical ◽  
Phosphonium Salt ◽  
Molar Ratio ◽  
High Yield ◽  
X Ray Diffraction ◽  
X Ray ◽  
Planar Configuration ◽  
Internal Motions ◽  
Energy Profiles

Abstract Treatment of (Me2N)3PCHSiMe3 with Me3SiOTf (OTf = triflate) affords the phosphonium salt [(Me2N)3PCH(SiMe3)2]OTf (2a), which can be converted into the correspond­ing ylide (Me2N)3PC(SiMe3)2 (3a) in high yield using NaN(SiMe3)2. The compounds with SiMe2Ph substituents (2, 3b) are obtained following an analogous procedure. The ylide (Me2N)3PC[Si(OMe)3]2 (3c) is available in 50% yield by direct transylidation of (MeO)3SiOTf with (Me2N)3PCH2 in the molar ratio 2:3, with [(Me2N)3PMe]OTf as the by-product. Com­pound 3c is a distillable liquid, but 3a,b are crystalline solids the structure of which has been determined by single crystal X-ray diffraction. Both compounds feature a trigonal planar ylidic carbon atom and short ylidic P-C and Si-C bonds. The nitrogen atoms are also in a planar configuration with non-standard orientations of the NMe2 groups at the phosphorus atoms. These data are in agreement with the results of recent quantum chemical calculations of simple prototypes which show very flat energy profiles for internal motions (rotation, inversion) of dimethylamino groups at the phosphorus atoms in phosphines and phosphoranes.

scholarly journals Formation and structural characterization of a europium(II) mono(scorpionate) complex and a sterically crowded pyrazabole

2017 ◽  
Vol 73 (12) ◽  
pp. 1921-1925 ◽  
Author(s):  
Phil Liebing ◽  
Marcel Kühling ◽  
Josef Takats ◽  
Liane Hilfert ◽  
Frank T. Edelmann
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Molar Ratio ◽  
High Yield ◽  
X Ray Diffraction ◽  
Isopropyl Group ◽  
X Ray

The reaction of EuI2(THF)2with potassium hydrotris(3,5-diisopropylpyrazolyl)borate (K[HB(3,5-iPr2pz)3] (= KTpiPr2, pz = pyrazolyl) in a molar ratio of 1:1.5 resulted in extensive ligand fragmentation and formation of the europium(II) mono(scorpionate) complex bis(3,5-diisopropyl-1H-pyrazole)[hydrotris(3,5-diisopropylpyrazolyl)borato]iodidoeuropium(II), [Eu(C27H46BN6)I(C9H16N2)2] or (TpiPr2)(3,5-iPr2pzH)2EuIII,1, in high yield (78%). As a typical by-product, small amounts of the sterically crowded pyrazabole derivativetrans-4,8-bis(3,5-diisopropylpyrazol-1-yl)-1,3,5,7-tetraisopropylpyrazabole, C36H62B2H8ortrans-{(3,5-iPr2pz)HB(μ-3,5-iPr2pz)}2,2, were formed. Both title compounds have been structurally characterized through single-crystal X-ray diffraction. In1, two isopropyl groups are each disordered over two orientations with occupancy ratios of 0.574 (10):0.426 (10) and 0.719 (16):0.281 (16). In2, one isopropyl group is similarly disordered, occupancy ratio 0.649 (9):0.351 (9).

scholarly journals Synthesis of Ni(II), Cu (II) and Zn(II) coumarin-3-carboxilic acid derivates and their and their physical-chemical properties

2021 ◽  
Vol 10 (3) ◽  
pp. e47910313430
Author(s):  
Dirceu Aparecido Gonçalves de Souza ◽  
Ricardo Luis Tranquilin ◽  
Marcio Luiz dos Santos ◽  
Regina Mara Silva Pereira
Keyword(s):  
Metal Ion ◽  
Chemical Properties ◽  
Biological Properties ◽  
New Drugs ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dpph Method ◽  
The Degree Of Crystallinity ◽  
Transition Complexes

In the search for new drugs, coumarins are an important class of compounds due to their chemical and biological properties, such as their potential to reduce cancer, diabetes, and cardiovascular diseases. They are heterocyclic compounds that contain oxygen in their structure and are found in plants.To improve the chemical and biological properties of the coumarin-3-carboxilic acid, were prepared metal transition complexes of Cu(II), Ni(II) and Zn(II) of coumarin-3-carboxilic acid by a new synthetic route. All complexes were characterized by ultraviolet, Infrared (FTIR), and Raman spectroscopy; Scanning electronic microscopy (SEM); X-Ray diffraction (XRD), as well as conductivity and elemental analysis. Electron microscopy and X-ray analysis showed that the degree of crystallinity of the complexes changes when compared with the precursor, 3-carboxy-coumarin acid, and the degree of crystallinity depends on the nature of the metal ion attached to coumarin. In addition, the antioxidant action of the complexes was evaluated by the DPPH method, and the results showed a higher activity of the complexes when compared with the precursor, suggesting that these complexes may present biological properties of interest.

Effect of Hydrated Metal Salts on the Coordination Product of Cobalt(II) halide and PNP Type Ligand, 2,6-bis(di-tertbutylphosphinomethyl) pyridine

2018 ◽  
Author(s):  
Tasneem Siddiquee ◽  
Abdul Goni
Keyword(s):  
Metal Salts ◽  
Molar Ratio ◽  
Pincer Complexes ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Pincer Ligand ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Distorted Tetrahedral Geometry ◽  
Cobalt Center

Chemical treatment of CoX<sub>2</sub><b><sup>. </sup></b>6H<sub>2</sub>O (X = Cl, Br, I) with the potentially tridentate PNP pincer ligand 2,6-bis(di-<i>tert</i>-butylphosphinomethyl)pyridine in 1:1 molar ratio results in cobalt(II) halide-PNP pincer complexes. The effect of the hydrated metal source on molecular structure and geometry of the complexes was studied by single crystal X-ray diffraction analysis. The complexes are neutral and the cobalt center adopts a penta-coordinate system with potential atropisomerization. Within the unit cell there are two distinct molecules per asymmetric unit. One of the two phosphorus atoms in the PNP ligand was observed to be partially oxidized to phosphinoxide. Disorder in the structure reflects a mixture of square pyramidal and distorted tetrahedral geometry.

Ten-Vertex Polyhedral Monocarbaborane Chemistry. The Novel High-Yield Formation of the Ten-Vertex closo Compound [6-(PMe2Ph)-closo-1-CB9H9] from the Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11]

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
High Yield ◽  
Monoclinic Space Group ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
X Ray ◽  
Yield Formation ◽  
Boiling Toluene

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.

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