ChemInform Abstract: PREPARATION AND CHARACTERIZATION OF ADDUCTS OF BISMUTH PENTAFLUORIDE AND ANTIMONY PENTAFLUORIDE AND VIBRATIONAL SPECTROSCOPY, X-RAY POWDER DIFFRACTION, AND SINGLE-CRYSTAL X-RAY CRYSTALLOGRAPHY

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

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The Synthesis and Characterization of a Novel One-Dimensional Bismuth (III) Coordination Polymer as a Precursor for the Production of Bismuth (III) Oxide Nanorods

Crystals ◽

10.3390/cryst12010113 ◽

2022 ◽

Vol 12 (1) ◽

pp. 113

Author(s):

Younes Hanifehpour ◽

Babak Mirtamizdoust ◽

Jaber Dadashi ◽

Ruiyao Wang ◽

Mahboube Rezaei ◽

...

Keyword(s):

Single Crystal ◽

Coordination Compound ◽

Organic Ligand ◽

One Dimensional ◽

X Ray ◽

X Ray Crystallography ◽

Oxide Nanorods ◽

Pure Phase ◽

3D Framework

A novel Bi (III) coordination compound, [Bi(HQ)(Cl)4]n ((Q = pyridine-4-carbaldehyde thiosemicarbazone), was prepared in this research using a sonochemical technique. SEM, infrared spectroscopy (IR), XRD, and single-crystal X-ray analysis were utilized to analyze the Bi(III) coordination compound. The structure determined using single-crystal X-ray crystallography indicates that the coordination compound is a 1D polymer in solid state and that the coordination number of bismuth (III) ions is six, (BiSCl5), with one S donor from the organic ligand and five Cl donors from anions. It is equipped with a hemidirectional coordination sphere. It is interesting that the ligand has been protonated in the course of the reaction with a Cl- ion balancing the charge. This compound’s supramolecular properties are directed and regulated by weak directional intermolecular interactions. Through π–π stacking interactions, the chains interact with one another, forming a 3D framework. Thermolysis of the compound at 170 °C with oleic acid resulted in the formation of pure phase nanosized Bi (III) oxide. SEM technique was used to examine the morphology and size of the bismuth (III) oxide product produced.

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Powder diffraction study of arsenic-substituted nasicon structures MeZr2As(3−x)PxO12 (Me=Na+, K+)

Powder Diffraction ◽

10.1017/s0885715600010150 ◽

1998 ◽

Vol 13 (4) ◽

pp. 227-231 ◽

Cited By ~ 6

Author(s):

D. Mazza ◽

M. Lucco-Borlera ◽

S. Ronchetti

Keyword(s):

Single Crystal ◽

Diffraction Study ◽

Key Words ◽

Powder Diffraction ◽

Mixed Oxides ◽

Structural Data ◽

Nasicon Structure ◽

Ionic Conductors ◽

X Ray

Three new mixed oxides having the nasicon structure and containing arsenic(V) as tetrahedral ion were prepared and X-ray analyzed. The stoichiometry of the three phases can be expressed by the comprehensive notation MeZr2As(3−x)PxO12 where Me stands for Na+ or K+, x equals to 0 and 1.5 when Me=Na, while x equals to 1.5 when Me=K. For two other compositions of the above series, the powder patterns were calculated on the basis of the structural data from single crystal determinations, thus permitting us to complete the characterization of the solids, with nasicon framework, deriving from MeZr2P3O12 (Me=Na+, K+) by partial (50%) or complete (100%) substitution of As for P.Key words: nasicon, ionic conductors, phosphates, arsenates

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X-ray crystallography, mass spectrometry and single crystal microspectrophotometry: A multidisciplinary characterization of catechol 1,2 dioxygenase

Biochimica et Biophysica Acta (BBA) - Proteins and Proteomics ◽

10.1016/j.bbapap.2010.09.008 ◽

2011 ◽

Vol 1814 (6) ◽

pp. 817-823 ◽

Cited By ~ 16

Author(s):

Chiara Micalella ◽

Sara Martignon ◽

Stefano Bruno ◽

Barbara Pioselli ◽

Raffaella Caglio ◽

...

Keyword(s):

Mass Spectrometry ◽

Single Crystal ◽

X Ray ◽

X Ray Crystallography ◽

Catechol 1,2 Dioxygenase

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STRUCTURAL CHARACTERIZATION OF 2-AMINO-2-OXOACETIC ACID BY X-RAY POWDER DIFFRACTION AND QUANTUM CHEMISTRY

Periódico Tchê Química ◽

10.52571/ptq.v16.n33.2019.531_periodico33_pgs_516_523.pdf ◽

2019 ◽

Vol 16 (33) ◽

pp. 516-523

Author(s):

G. E. DELGADO ◽

L. M. BELANDRIA ◽

M. GUILLEN ◽

A.. J. MORA ◽

L. E. SEIJAS

Keyword(s):

Hydrogen Bonds ◽

Single Crystal ◽

Structural Study ◽

Powder Diffraction ◽

Structural Characterization ◽

Structure Determination ◽

Spectroscopic Techniques ◽

X Ray Diffraction ◽

X Ray

2-amino-2-oxoacetic acid, carbamoyl formic acid, or oxamic acid is an active pharmaceutical ingredient (API) of great importance mainly because is an inhibitor of lactic dehydrogenase (LDH). It acts as an inhibitor to the metabolic pathways of the tumor cells and exhibited significant anticancer activity against nasopharyngeal carcinoma (NPC) cells in vitro and can be considered as a potential drug for the treatment of type 2 diabetes. Also, this compound could be used as a building block in the design of supramolecular architectures based on hydrogen bonds through the complimentary hydrogen-bond functionalities of the carbonyl and amide functional groups present. Single-crystal X-ray diffraction is the most powerful technique for crystal structure determination of small molecules. However, for several materials, including oxamic acid, it could be complicated to grow single crystals of suitable size and quality that make them appropriated to structure analysis. For this reason, the structural study was conducted with powder X-ray diffraction which is a process significantly more challenging than structure determination from single-crystal data. Oxamic acid has been characterized by FT-IR and NMR spectroscopic techniques, thermal TGA-DSC analysis, semi-empirical PM7 calculations, and X-ray powder diffraction. The title compound crystallizes in the monoclinic system with space group Cc, Z=4, and unit cell parameters a= 9.4994(4) Å, b= 5.4380(2) Å, c= 6.8636(3) Å, b= 107.149(2)°, V= 338.79(2) Å3. The molecule has a trans conformation. The molecular structure and crystal packing are stabilized mainly by intra- and intermolecular O--H···O and N--H···O hydrogen bonds. The structural characterization of this type of API compound is important to understand its mechanisms of action due to its considerable biological effects. In particular, for oxamic acid, this structural study would allow subsequent examination of its medicinal properties as an antitumor and antidiabetic agent.

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Bleaching the Record: After 200 Years, Single Crystal X-Ray Crystallography Reveals the Structure and Hydrogen-Bonding Properties of Hypochlorite and Hypobromite Ions in the Solid State

10.26434/chemrxiv.14706612 ◽

2021 ◽

Author(s):

Filip Topic ◽

Joseph Marrett ◽

Tristan Borchers ◽

Hatem M. Titi ◽

Christopher J. Barrett ◽

...

Keyword(s):

Solid State ◽

Single Crystal ◽

Gas Phase ◽

X Ray ◽

X Ray Crystallography ◽

Single Crystal Structures ◽

Hypohalous Acids ◽

Bonding Properties ◽

Insight Into

<div>We report the first single crystal structures of hypochlorite and hypobromite salts, including hydrated sodium hypochlorite - a ubiquitous bleaching and disinfection agent in use for almost 200 years. The structures represent the first characterization of fundamentally important hypochlorite and hypobromite anions in the solid state, by X-ray crystallography and are supported by Raman spectroscopy on individual crystals. The structural analysis provides insight into supramolecular chemistry of the hypohalite ions in the hydrated environment of the NaOCl<sup>.</sup>5H<sub>2</sub>O and NaOBr<sup>.</sup>5H<sub>2</sub>O solid salts, and reveals measured Cl-O and Br-O bond lengths of 1.69 A and 1.82 A, respectively, which are significantly longer than those for corresponding higher-valence oxoanions, and in agreement with the values spectroscopically determined for hypohalous acids and corresponding oxides in the gas phase.<br></div>

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The Synthesis and Structural Characterization of a Two-Dimensional Coordination Polymer [Co(H2O)(phen)(μ4-bta)1/2]n (H4bta = Benzenetetracarboxylic Acid)

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc20010870 ◽

2001 ◽

Vol 66 (6) ◽

pp. 870-876 ◽

Cited By ~ 8

Author(s):

De-Qing Chu ◽

Ji-Qing Xu ◽

Ao-Qing Tang

Keyword(s):

Coordination Polymer ◽

Single Crystal ◽

Structural Characterization ◽

Two Dimensional ◽

Polymeric Structure ◽

X Ray ◽

X Ray Crystallography

Complex [Co(H2O)(phen)(μ4-bta)1/2]n was hydrothermally synthesized from sodium benzene-1,2,4,5-tetracarboxylate, 1,10-phenanthroline and CoCl2·6H2O, and structurally characterized by single-crystal X-ray crystallography, showing that it possesses a novel two-dimensional polymeric structure.

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