scholarly journals Synthesis, Crystal Structure and Interaction with Bovine Serum Albumin (BSA) of Two α-Aminophosphonic Acids Derivatives

2019 ◽  
pp. 1-7
Author(s):  
Wei Huang ◽  
Wen-Ling Wang
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Binding Constants ◽  
Ionization Mass ◽  
Monoclinic System ◽  
X Ray ◽  
X Ray Crystallography ◽  
Aminophosphonic Acids ◽  
Amino Phosphonate ◽  
Ft Ir

Two α-amino-phosphonate derivatives (1 & 2) were synthesized and their compositions and structures were characterized by Elemental Analysis (EA), FT-IR Spectrascopy (FT-IR), Electrospray Ionization Mass Spectrometry (ESI-MS), Nuclear Magnetic Resonance (NMR, 1H, 13C and 31P) and X-ray crystallography. Compound 1 & 2 were crystallized in monoclinic system with the space group P2(1)/n and P2(1)/c, respectively. The interaction effects of two α-aminophosphonate derivatives (1 & 2) with BSA were investigated and the binding constants were 1.07 × 104 M-1, 1.68 × 104 M-1, respectively. Besides, the values of n were indicated that 1:1 complex was formed between BSA and 1&2.

scholarly journals Syntheses and Reactivity of New Zwitterionic Imidazolium Trihydridoborate and Triphenylborate Species

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3184
Author(s):  
Maura Pellei ◽  
Riccardo Vallesi ◽  
Luca Bagnarelli ◽  
H. V. Rasika Dias ◽  
Carlo Santini
Keyword(s):  
Mass Spectrometry ◽  
Ionization Mass ◽  
Alkyl Aryl ◽  
X Ray ◽  
X Ray Crystallography ◽  
Microwave Assisted ◽  
Ft Ir ◽  
11B Nmr ◽  
New Compounds ◽  
Ft Ir Spectroscopy

In this study, four new N-(alkyl/aryl)imidazolium-borates were prepared, and their deprotonation reactions were investigated. Addition of BH3•THF to N-benzylimidazoles and N-mesitylimidazoles leads to imidazolium-trihydridoborate adducts. Ammonium tetraphenylborate reacts with benzyl- or mesityl-imidazoles with the loss of one of the phenyl groups yielding the corresponding imidazolium-triphenylborates. Their authenticity was confirmed by CHN analysis, 1H-NMR, 13C-NMR, 11B-NMR, FT-IR spectroscopy, and electrospray ionization mass spectrometry (ESI-MS). 3-Benzyl-imidazolium-1-yl)trihydridoborate, (HImBn)BH3, and (3-mesityl-imidazolium-1-yl)trihydridoborate, (HImMes)BH3, were also characterized by X-ray crystallography. The reactivity of these new compounds as carbene precursors in an effort to obtain borate-NHC complexes was investigated and a new carbene-borate adduct (which dimerizes) was obtained via a microwave-assisted procedure.

scholarly journals Reaction with Proteins of a Five-Coordinate Platinum(II) Compound

2019 ◽  
Vol 20 (3) ◽  
pp. 520 ◽  
Author(s):  
Giarita Ferraro ◽  
Tiziano Marzo ◽  
Maria Cucciolito ◽  
Francesco Ruffo ◽  
Luigi Messori ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Platinum Complexes ◽  
Rnase A ◽  
Side Chain ◽  
Planar Geometry ◽  
Ionization Mass ◽  
X Ray ◽  
X Ray Crystallography ◽  
Egg White Lysozyme ◽  
Square Planar

Stable five-coordinate Pt(II) complexes have been highlighted as a promising and original platform for the development of new cytotoxic drugs. Their interaction with proteins has been scarcely studied. Here, the reactivity of the five-coordinate Pt(II) compound [Pt(I)(Me) (dmphen)(olefin)] (Me = methyl, dmphen = 2,9-dimethyl-1,10-phenanthroline, olefin = dimethylfumarate) with the model proteins hen egg white lysozyme (HEWL) and bovine pancreatic ribonuclease (RNase A) has been investigated by X-ray crystallography and electrospray ionization mass spectrometry. The X-ray structures of the adducts of RNase A and HEWL with [Pt(I)(Me)(dmphen)(olefin)] are not of very high quality, but overall data indicate that, upon reaction with RNase A, the compound coordinates the side chain of His105 upon releasing the iodide ligand, but retains the pentacoordination. On the contrary, upon reaction with HEWL, the trigonal bi-pyramidal Pt geometry is lost, the iodide and the olefin ligands are released, and the metal center coordinates the side chain of His15 probably adopting a nearly square-planar geometry. This work underlines the importance of the combined use of crystallographic and mass spectrometry techniques to characterize, in detail, the protein–metallodrug recognition process. Our findings also suggest that five-coordinate Pt(II) complexes can act either retaining their uncommon structure or functioning as prodrugs, i.e., releasing square-planar platinum complexes as bioactive species.

scholarly journals Synthesis and Crystal Structure of Unexpected (1S,4R,5R,6S)-4-Cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonan-6-yl Acetate

2017 ◽  
Vol 70 (12) ◽  
pp. 1269
Author(s):  
Steven Gareth Williams ◽  
Mohan Bhadbhade ◽  
Roger Bishop ◽  
Alison Thavary Ung
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
High Resolution Mass Spectrometry ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Ir And Nmr Spectroscopy ◽  
Resolution Mass

The reaction of (–)-β-pinene with KCN under a mild bridged Ritter reaction gave (1S,5R,6S)-2,2,6-trimethyl-3-aza-bicyclo[3.3.1]non-3-en-6-yl acetate that subsequently reacted to provide an unexpected (1S,4R,5R,6S)-4-cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonane-6-yl acetate. The structure of the compound was determined by high-resolution mass spectrometry, and IR and NMR spectroscopy and confirmed by single crystal X-ray crystallography. The compound crystallises in the monoclinic P21 space group, with unit cell parameters a 8.6120 (17), b 7.4570 (15), c 11.189 (2) Å, and β 110.16 (3)°.

Synthesis, Crystal Structure, Spectroscopic and Thermal Properties of a Novel Mixed Ligand Copper(II) Complex with 5,5-Dimethylhydantoin and Benzylamine

2006 ◽  
Vol 61 (2) ◽  
pp. 133-138 ◽  
Author(s):  
Murat Taş ◽  
Serkan Soylu ◽  
Hümeyra Batı
Keyword(s):  
Crystal Structure ◽  
Thermal Analyses ◽  
Crystal Data ◽  
Monoclinic System ◽  
Magnetic Susceptibility Data ◽  
X Ray ◽  
Susceptibility Data ◽  
Ft Ir ◽  
Complex Features ◽  
Water Ligands

AbstractThe crystal structure of the newly synthesized complex, trans-aqua-bis(benzylamino)-bis(5,5-dimethylhydantoinato) copper(II) was determined by X-Ray single crystal data. The thermal analyses, FT-IR and magnetic susceptibility data are also presented. The complex crystallizes in the monoclinic system, space group C2. The complex features a distorted square pyramidal [CuN4O] coordination with 5,5-dimethylhydantoinato, benzylamine and water ligands. The 5,5-dimethylhydantoinato anion is bonded to the copper(II) ion via its deprotonated N atom in the 3-position.

Combined analysis of 1,3-benzodioxoles by crystalline sponge X-ray crystallography and laser desorption ionization mass spectrometry

The Analyst ◽  
2018 ◽  
Vol 143 (6) ◽  
pp. 1475-1481 ◽  
Author(s):  
Yukako Hayashi ◽  
Kazuaki Ohara ◽  
Rika Taki ◽  
Tomomi Saeki ◽  
Kentaro Yamaguchi
Keyword(s):  
Mass Spectrometry ◽  
Laser Desorption ◽  
Promising Method ◽  
Ionization Mass Spectrometry ◽  
Ionization Mass ◽  
Laser Desorption Ionization ◽  
Combined Analysis ◽  
X Ray ◽  
X Ray Crystallography ◽  
Desorption Ionization

The combination of X-ray analysis and laser desorption ionization by using crystalline sponge will be a promising method to determine guest structures.

Synthesis, crystal structure, aggregation-induced emission (AIE) and electroluminescence properties of a novel emitting material based on pyrrolo[3,2-b]pyrrole

2020 ◽  
Vol 8 (40) ◽  
pp. 14208-14218
Author(s):  
Hongbo Wang ◽  
Jinnan Huo ◽  
Hongbo Tong ◽  
Xuehong Wei ◽  
Ying Zhang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Donor Group ◽  
Aggregation Induced Emission ◽  
X Ray ◽  
X Ray Crystallography

A novel electroluminescent material based on pyrrolo[3,2-b]pyrrole as skeleton and donor group and dimesitylborons as accept groups has been synthesized and characterized by elemental analysis, mass spectrometry, NMR spectroscopy and X-ray crystallography.

scholarly journals Crystal structure of an oxalate-bridged tetranuclear 8-hydroxyquinoline Zn(II) cluster: [Zn4Q6(Ox)]0.5n

2011 ◽  
Vol 76 (4) ◽  
pp. 529-537 ◽  
Author(s):  
Jiajun Wang ◽  
Qiang Wang ◽  
Yanjun Sun ◽  
Yuemei Wang ◽  
Guosheng Zhao ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
Chain Structure ◽  
Stacking Interactions ◽  
Monoclinic System ◽  
X Ray ◽  
X Ray Crystallography ◽  
Polymeric Chains

The chain structure of a tetranuclear zinc(II) cluster [Zn4Q6(Ox)]0.5n ([Zn4 (C9H6NO)6(C2O4)]0.5n) (1) (Q = 8- hydroxyquinoline anion, Ox = oxalate dianion) was determined by X-ray crystallography and characterized by elemental analysis, IR spectroscopy and thermal analysis. It crystallizes in the monoclinic system, space group P21/n (No. 14), with the lattice parameters a = 13.2222(15) ?, b = 11.0566(12) ?, c = 16.2224(18) ?, ? = 92.1770(10)?, V = 2369.9(5) ?3, Z = 4, Mr = 607.23 g mol-1, Dc = 1.702 g cm-3. The tetranuclear zinc(II) clusters form 1D polymeric chains parallel to the b-axis. The ?-? stacking interactions involving aryl rings support the formation of the 1D polymeric structure. The neighboring polymeric chains are connected by C-H???? interactions.

scholarly journals Weak protein–cationic co-ion interactions addressed by X-ray crystallography and mass spectrometry

2014 ◽  
Vol 70 (8) ◽  
pp. 2217-2231 ◽  
Author(s):  
Philippe Bénas ◽  
Nicolas Auzeil ◽  
Laurent Legrand ◽  
Franck Brachet ◽  
Anne Regazzetti ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Protein Solubility ◽  
Ionization Mass ◽  
X Ray ◽  
Esi Ms ◽  
X Ray Crystallography ◽  
Egg White Lysozyme ◽  
Ion Interactions ◽  
Carboxylic Groups ◽  
Hen Egg White

The adsorption of Rb+, Cs+, Mn2+, Co2+and Yb3+onto the positively charged hen egg-white lysozyme (HEWL) has been investigated by solving 13 X-ray structures of HEWL crystallized with their chlorides and by applying electrospray ionization mass spectrometry (ESI-MS) first to dissolved protein crystals and then to the protein in buffered salt solutions. The number of bound cations follows the order Cs+< Mn2+≃ Co2+< Yb3+at 293 K. HEWL binds less Rb+(qtot= 0.7) than Cs+(qtot= 3.9) at 100 K. Crystal flash-cooling drastically increases the binding of Cs+, but poorly affects that of Yb3+, suggesting different interactions. The addition of glycerol increases the number of bound Yb3+cations, but only slightly increases that of Rb+. HEWL titrations with the same chlorides, followed by ESI-MS analysis, show that only about 10% of HEWL binds Cs+and about 40% binds 1–2 Yb3+cations, while the highest binding reaches 60–70% for protein binding 1–3 Mn2+or Co2+cations. The binding sites identified by X-ray crystallography show that the monovalent Rb+and Cs+preferentially bind to carbonyl groups, whereas the multivalent Mn2+, Co2+and Yb3+interact with carboxylic groups. This work elucidates the basis of the effect of the Hofmeister cation series on protein solubility.

scholarly journals Oxido- and Dioxido-Vanadium(V) Complexes Supported on Carbon Materials: Reusable Catalysts for the Oxidation of Cyclohexane

Nanomaterials ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 1456
Author(s):  
Manas Sutradhar ◽  
Marta A. Andrade ◽  
Sónia A. C. Carabineiro ◽  
Luísa M. D. R. S. Martins ◽  
Maria de Fátima C. Guedes da Silva ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Carbon Materials ◽  
Ionization Mass ◽  
X Ray Diffraction ◽  
Functionalized Carbon Nanotubes ◽  
X Ray ◽  
Tert Butylhydroperoxide ◽  
Ft Ir ◽  
First Time ◽  
Catalytic Performances

Oxidovanadium(V) and dioxidovanadium(V) compounds, [VO(OEt)L] (1) and [Et3NH][VO2L] (2), were synthesized using an aroylhydrazone Schiff base (5-bromo-2-hydroxybenzylidene)-2-hydroxybenzohydrazide (H2L). They were characterized by elemental analysis, Fourier-transform infrared spectroscopy (FT-IR), (1H and 51V) nuclear magnetic resonance (NMR), electrospray ionization mass spectrometry (ESI-MS) and single crystal X-ray diffraction analyses. Both complexes were immobilized on functionalized carbon nanotubes and activated carbon. The catalytic performances of 1 and 2, homogenous and anchored on the supports, were evaluated for the first time towards the MW-assisted peroxidative oxidation (with tert-butylhydroperoxide, TBHP) of cyclohexane under heterogeneous conditions. The immobilization of 1 and 2 on functionalized carbon materials improved the efficiency of catalytic oxidation and allowed the catalyst recyclability with a well-preserved catalytic activity.

scholarly journals X-ray crystal structure analysis of 5-bromospiro[indoline-3,7'-pyrano[3,2-C:5,6-C']dichromene]-2,6',8'-trione

2021 ◽  
Vol 12 (2) ◽  
pp. 187-191
Author(s):  
Varun Sharma ◽  
Bubun Banerjee ◽  
Gurpreet Kaur ◽  
Vivek Kumar Gupta
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Crystal Structure Analysis ◽  
One Pot ◽  
X Ray ◽  
X Ray Crystallography ◽  
Naturally Occurring ◽  
Three Component Reaction ◽  
Ft Ir ◽  
Solvent Molecules

An analog of spirooxindole[pyrano-bis-2H-l-benzopyran] derivatives namely 5-bromospiro [indoline-3,7'-pyrano[3,2-c:5,6-c']dichromene]-2,6',8'-trione was synthesized via one-pot pseudo three-component reaction of one equivalent of 5-bromoisatin and two equivalents of 4-hydroxycoumarin using mandelic acid as a naturally occurring organo catalyst in aqueous ethanol under reflux conditions. The synthesized compound was characterized by FT-IR, 1H NMR, 13C NMR, and HRMS data. Crystal structure was determined by using single X-ray crystallography technique. It was found that the crystals are triclinic with space group P-1, C108H60Br4N4O29S2: a = 11.8333(6) Å, b = 12.8151(6) Å, c = 17.1798(8) Å, α = 77.317(4)°, β = 74.147(4)°, γ = 66.493(5)°, V = 2280.0(2) Å3, Z = 1, T = 149.99(10) K, μ(MoKα) = 1.902 mm-1, Dcalc = 1.647 g/cm3, 11545 reflections measured (3.836° ≤ 2Θ ≤ 50.998°), 8310 unique (Rint = 0.0488, Rsigma = 0.0875) which were used in all calculations. The final R1 was 0.0622 (I > 2σ(I)) and wR2 was 0.1994 (all data). The crystal structure was solved by direct methods and refined by full-matrix least-squares procedure to a final R-value of 0.0622 for 6264 observed reflections. The crystal structure was stabilized by an elaborate system of N-H···O, O-H···O, C-H···π, and π···π interactions involving solvent molecules to form supramolecular structure.

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