scholarly journals Synthesis and Characterization of Novel Copper(II)-Sunitinib Complex: Molecular Docking, DFT Studies, Hirshfeld Analysis and Cytotoxicity Studies

Inorganics ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 3
Author(s):  
Facundo Tarasi ◽  
Priscila Ailín Lanza ◽  
Valeria Ferretti ◽  
Gustavo Alberto Echeverría ◽  
Oscar Enrique Piro ◽  
...  
Keyword(s):  
Molecular Docking ◽  
Solid State ◽  
Free Ligand ◽  
X Ray Diffraction ◽  
Allosteric Site ◽  
Triclinic Space Group ◽  
Atp Binding Site ◽  
Cytotoxicity Studies ◽  
Hirshfeld Analysis

The main goal of this work was to report the synthesis, characterization, and cytotoxicity study of a novel copper(II)-sunitinib complex, CuSun. It has been synthesized and characterized in solid state and in solution by different methods (such as DFT, FTIR, Raman, UV-vis, EPR, NMR, etc.). The solid-state molecular structure of trichlorosunitinibcopper(II), where sunitinib: N-[2-(diethylamino)ethyl]-5-[(Z)-(5-fluoro-2-oxo-1H-indol-3-ylidene)methyl]-2,4-dimethyl-1H-pyrrole-3-carboxamide, for short Cu(Sun)Cl3, was determined by X-ray diffraction. It crystallizes in the triclinic space group P-1 with a = 7.9061(5) Å, b = 12.412(1) Å, c = 13.7005(8) Å, α = 105.021(6)°, β = 106.744(5)°, γ = 91.749(5)°, and Z = 2 molecules per unit cell. Also, we have found π-π interactions and classic and non-classic H-bonds in the crystal structure by using Hirshfeld surface analysis. In the speciation studies, the complex has dissociated in protonated sunitinib and chlorocomplex of copper(II), according to 1HNMR, EPR, UV-vis and conductimetric analysis. Molecular docking of the complex in both, ATP binding site and allosteric site of VEGFR2 have shown no improvement in comparison to the free ligand. Besides, cytotoxicity assay on HepG2 cell line shows similar activity for complex and ligand in the range between 1–25 μM supporting the data obtained from studies in solution.

Synthesis and structural characterization of BaSr2Ge3O9

2016 ◽  
Vol 71 (12) ◽  
pp. 1225-1232
Author(s):  
Sebastian Bräuchle ◽  
Clivia Hejny ◽  
Hubert Huppertz
Keyword(s):  
High Temperature ◽  
Solid State ◽  
Structural Characterization ◽  
Diffraction Data ◽  
Barium Carbonate ◽  
Strontium Carbonate ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray

AbstractBaSr2Ge3O9 was prepared by high-temperature solid-state synthesis at 1100°C in a platinum crucible from barium carbonate, strontium carbonate, and germanium(IV) oxide. The compound crystallizes in the triclinic space group P1̅ (no. 2) isotypically to walstromite BaCa2Si3O9. The structure was refined from single-crystal X-ray diffraction data: a=7.104(5), b=10.060(7), c=7.099(5) Å, α=83.0(2), β=77.0(2), γ=70.2(2)°, V=464.3(6) Å3, R1=0.0230, and wR2=0.0602 for all data. BaSr2Ge3O9 is characterized by three-membered rings of germanate tetrahedra. There are three crystallographically different Ge sites (Ge1, Ge2, and Ge3) in each [Ge3O9]6− ring. The rings occur in layers with the apices of alternating rings pointing in opposite directions. The Sr2+ and Ba2+ ions are located in between. The Sr1 cation is eight-fold coordinated, while Sr2 is octahedrally surrounded by oxide anions, and the Ba cation again eight-fold coordinated.

scholarly journals Synthesis and characterization of Ti(IV), Zr(IV) and Al(III) salen-based complexes

2021 ◽  
Vol 12 (2) ◽  
pp. 216-221
Author(s):  
Joana Hipolito ◽  
Luis Alves ◽  
Ana Martins
Keyword(s):  
Solid State ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Tetrahedral Geometry ◽  
Triclinic Space Group ◽  
Space Group ◽  
High Yields

New Ti(IV), Zr(IV) and Al(III) salen-based complexes of formulae [(L)TiCl2], 2, [(L)ZrCl2], 3, and [(L){Al(CH2CH(CH3)2)2}2], 4, where L = meso-(R,S)-diphenylethylene-salen, were synthesized in high yields. [(L){Al(CH2CH(CH3)2)2}2] is a bimetallic complex that results from the reaction of H2L with either 1 or 2 equivalent of Al(CH2CH(CH3)2)3. The solid-state molecular structures of compounds 2 and 4·(C7H8) were obtained by single-crystal X-ray diffraction. Crystal data for C44H54Cl2N2O2Ti, (2a): monoclinic, space group C2/c (no. 15), a = 27.384(1) Å, b = 12.1436(8) Å, c = 28.773(2) Å, β = 112.644(2)°, V = 8830.6(9) Å3, Z = 8, μ(MoKα) = 0.350 mm-1, Dcalc = 1.146 g/cm3, 26647 reflections measured (5.204° ≤ 2Θ ≤ 50.7°), 8072 unique (Rint = 0.0967, Rsigma = 0.1241) which were used in all calculations. The final R1 was 0.0640 (I > 2σ(I)) and wR2 was 0.1907 (all data). Crystal data for C62H72Cl2N2O2Ti (2b): monoclinic, space group P21/c (no. 14), a = 19.606(1) Å, b = 12.793(1) Å, c = 23.189(2) Å, β = 105.710(4)°, V = 5599.0(7) Å3, Z = 4, μ(MoKα) = 0.291 mm-1, Dcalc = 1.182 g/cm3, 37593 reflections measured (3.65° ≤ 2Θ ≤ 50.928°), 10304 unique (Rint = 0.0866, Rsigma = 0.1032) which were used in all calculations. The final R1 was 0.0593 (I > 2σ(I)) and wR2 was 0.1501 (all data). Crystal data for C67H97Al2N2O2 (4·(C7H8)): triclinic, space group P-1 (no. 2), a = 10.0619(9) Å, b = 16.612(2) Å, c = 21.308(2) Å, α = 67.193(5)°, β = 78.157(6)°, γ = 77.576(5)°, V = 3176.8(6) Å3, Z = 2, μ(MoKα) = 0.088 mm-1, Dcalc = 1.063 g/cm3, 42107 reflections measured (5.382° ≤ 2Θ ≤ 51.624°), 12111 unique (Rint = 0.0624, Rsigma = 0.0706) which were used in all calculations. The final R1 was 0.0568 (I > 2σ(I)) and wR2 was 0.1611 (all data). The solid-state molecular structure of [(L){Al(CH2CH(CH3)2)2}2] reveals that both metal centres display a slightly distorted tetrahedral geometry bridged by the salen ligand. Both [(L)TiCl2] and [(L)ZrCl2] complexes display octahedral geometry with trans-chlorido ligands.

Characterization of some mesogenic alkyl 1-thioglycosides

2002 ◽  
Vol 80 (8) ◽  
pp. 1162-1165 ◽  
Author(s):  
B Henrissat ◽  
G K Hamer ◽  
M G Taylor ◽  
R H Marchessault
Keyword(s):  
Phase Transition ◽  
Liquid Crystal ◽  
Solid State ◽  
Solid State Nmr ◽  
Liquid Crystalline ◽  
Liquid Crystal Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Liquid Crystalline Phases

A series of dodecyl 1-thio-β-D-glycosides has been synthesized and characterized (DSC, NMR, CP MAS, X-ray diffraction) as possible new marking materials with liquid-crystalline properties. These compounds undergo solid to liquid crystal phase transitions at various temperatures, which depend on the nature of the carbohydrate part of the structure. Their liquid-crystalline phases show extreme shear thinning behaviour.Key words: liquid crystal, powder X-ray diffraction, phase transition, thioglycoside, solid-state NMR, marking material

scholarly journals Characterization of a brazilian smectite by solid state NMR and X-ray diffraction techniques

1997 ◽  
Vol 8 (6) ◽  
pp. 581-586 ◽  
Author(s):  
Alcides Wagner Serpa Guarino ◽  
Rosane A. S. San Gil ◽  
Helena Polivanov ◽  
Sonia M.C. Menezes
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals Making and Characterization of Limnpo4 Using Solid State Reaction Method for Lithium Ion Battery Cathodes

2019 ◽  
pp. 583-588
Author(s):  
Adelyna Oktavia ◽  
Kurnia Sembiring ◽  
Slamet Priyono
Keyword(s):  
Solid State ◽  
Lithium Ion Battery ◽  
Lithium Ion ◽  
Solid State Reaction Method ◽  
Raw Material ◽  
X Ray Diffraction ◽  
Solid State Method ◽  
X Ray ◽  
General Investigation

Hospho-material of olivine, LiMnPO4 identified as promising for cathode material generation next Lithium-ion battery and has been successfully synthesized by solid-state method with Li2Co3, 2MnO2, 2NH4H2PO4 as raw material. The influence of initial concentration of precursors at kalsinasi temperatures (400-800 ° C) flows with nitrogen. The purity and composition phase verified by x-ray diffraction analysis (XRD), scanning electron microscopy (SEM), spectroscopy, energy Dispersive x-ray Analysis (EDS), Raman spectra. General investigation shows that there is a correlation between the concentration of precursors, the temperature and the temperature of sintering kalsinasi that can be exploited to design lithium-ion next generation.

Imidazole-containing Bispidine Ligands: Synthesis, Structure and Cu(II) Complexation

2011 ◽  
Vol 66 (7) ◽  
pp. 721-728 ◽  
Author(s):  
Martin Walther ◽  
Madlen Matterna ◽  
Stefanie Juran ◽  
Silke Fähnemann ◽  
Holger Stephan ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Enol Form ◽  
Trans Configuration ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Impact ◽  
Configurational Isomerism

The preparation and characterization of tris-pyridyl bispidine (3,7-diazabicyclo[3.3.1]nonane) derivatives with benzimidazole and imidazole donor groups at the N-3 position of the bispidine skeleton and their copper(II) complexes are reported. The impact of the hetaryl substituents on the configurational isomerism of piperidones and their corresponding bispidones has been studied by NMR spectroscopy, revealing the exclusive appearance in the enol form for the piperidones in solution and the trans-configuration regarding the two pyridyl substituents, as well as the sole formation of the unsymmetric exo-endo isomers for the corresponding bispidones. Thus, the bispidones are preorganized ligands for building pentacoordinated complexes, confirmed by the preparation and characterization of the corresponding Cu(II) complexes. Of the di-pyridyl piperidones with benzimidazole and imidazole substituents, and of the Cu(II) complex of the benzimidazole-containing bispidone, crystals have become available for the analysis by X-ray diffraction, showing that the piperidones form the enol tautomers also in the solid state.

Synthesis and Characterization of 3Y-TZP by Gel Solid-State Method

2011 ◽  
Vol 412 ◽  
pp. 61-64
Author(s):  
Xiao Bo Wu ◽  
Da Zhi Sun ◽  
Dan Yu Jiang ◽  
Hai Fang Xu ◽  
De Xin Huang ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Solid State ◽  
Sintering Behavior ◽  
X Ray Diffraction ◽  
Solid State Method ◽  
X Ray ◽  
Powder Particles ◽  
State Method ◽  
Average Size

3Y-TZP powder has been successfully synthesized by gel solid-state method. The structural phases of powder particles were analyzed by X-ray diffraction and the morphology was analyzed by scanning electron microscopy. The average size of grains was 230 nm. The sintering behavior, mechanical properties and microstructure of 3Y-TZP ceramics sintered by this powder were investigated. The experiment results showed that the mechanical properties of ceramics were excellent.

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 SOLID STATE CHARACTERIZATION OF A NOVEL PHYSICAL INTERACTION (PARACETAMOL-CHLORPHENIRAMINE MALEATE)

2018 ◽  
Vol 10 (1) ◽  
pp. 21
Author(s):  
Iyan Sopyan ◽  
Intan Mutiara Sari ◽  
Insan Sunan K.
Keyword(s):  
Solid State ◽  
Pure Substance ◽  
Physical Interaction ◽  
X Ray Diffraction ◽  
Chlorpheniramine Maleate ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Ingredients ◽  
Ft Ir

Objective: Interactions of active pharmaceutical ingredients (API) as well as pharmaceutical excipients don’t occur in a pharmaceutical dosage form. Base on structures of paracetamol (PCT) and chlorphenamine maleate (CTM), its combination is possible to give a physical interaction in the solid state. This study was conducted to investigate the physical interaction of PCT and CTM in the solid state.Methods: Characterization used the polarization microscope, solubility test, powder x-ray diffraction (PXRD) to observe peak shifting in 2Ɵ angle, and fourier transform infrared spectroscopy (FT-IR) to examine wavenumber shifting.Results: Results of solubility exhibited an increased solubility percentage with increasing concentration. Polarization microscope analysis presented a combination of crystal morphology after the two substances were mixed in an equimolar ratio. The result of melting point determination of each pure substance was 172 °C for PCT, 132 °C for CTM, and 170 °C for the mixture of the two substances in various ratios. Diffractogram showed the shifting at angle 2Ɵ: 20.715, 19.355-23.500 and 21.840, 26.455-20.330 for concentration ratio of PCT: CTM in (132:0.5) and (330:1) respectively and any change in the functional group was observed from infrared spectrum.Conclusion: All evaluation of PCT and CTM in the solid state has exhibited the interaction in solid condition.

Synthesis, Structure and Characterization of a Novel Two-Dimensional Supramolecular Mn(II) Coordination Polymer Constructed from a 1,10-Phenanthroline Derivative and a Flexible Dicarboxylate

2010 ◽  
Vol 65 (9) ◽  
pp. 1173-1176 ◽  
Author(s):  
Zhi-Guo Kong ◽  
Xiao-Yuan Ma ◽  
Zhan-Lin Xu
Keyword(s):  
Ir Spectroscopy ◽  
Glutaric Acid ◽  
Title Complex ◽  
Two Dimensional ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
1D Chains

The title complex, [Mn2(glu)(L)2(HL)2]・0.5H2O (H2glu = glutaric acid, HL = 2-(2-chloro-6-fluorophenyl)-1Himidazo[ 4,5-f][1,10]phenanthroline) has been synthesized using a hydrothermal method and characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. Crystal data: C162H88Cl8F8Mn4N32O9, triclinic, space group P1¯, a = 14.932(5), b = 16.414(5), c = 17.891(5) Å , α = 115.851(5), β = 91.288(5), γ = 112.894(5)◦, V = 3536.4(19) Å3, Z = 1. Compound 1 exhibits 1D chains which are further stacked by C-H...π interactions to give two-dimensional supramolecular layers.

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