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)°.

Tin(IV) porphyrin functionalization of electrochemically active fluoride-doped tin-oxide (FTO) via Huisgen [3+2] click chemistry

2011 ◽  
Vol 15 (01) ◽  
pp. 75-82 ◽  
Author(s):  
Shiva Prasad ◽  
Mohan Bhadbhade ◽  
Pall Thordarson
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Click Chemistry ◽  
Tin Oxide ◽  
Photoelectron Spectroscopy ◽  
High Resolution Mass Spectrometry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Electrochemically Active ◽  
Resolution Mass

A novel tetra-alkyne terminated tin(IV) porphyrin 3 was synthesized in good yields and characterized using NMR spectroscopy, high resolution mass spectrometry and X-ray crystallography, the latter revealing interactions with hexane molecules that stabilize the crystal structure of the tin(IV) porphyrin 3. It was then linked to a conductive fluorine-doped tin oxide (FTO) surfaces using Huisgen [3+2] click chemistry. The attachment of the tin(IV) porphyrin to the FTO surface 6 was characterized by X-ray photoelectron spectroscopy (XPS), indicating the presence of the 1,2,3-triazole unit. Electrochemical measurements of the tin(IV) porphyrin modified FTO surface 7 show that it is still electrochemically active with oxidation (Epa) and reduction peaks (Epc) for the ferricyanide redox couple observed at Epc and Epa of -0.144 and +0.568 V vs. Ag | AgCl respectively, representing a modest shift of ca . +/- 0.1–0.15 V, compared to unmodified FTO.

Synthesis and crystal structure of (Ag,Pd)22Se6

2013 ◽  
Vol 28 (1) ◽  
pp. 13-17 ◽  
Author(s):  
F. Laufek ◽  
A. Vymazalová ◽  
D.A. Chareev ◽  
A.V. Kristavchuk ◽  
J. Drahokoupil ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Glass Tube ◽  
Structure Type ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
Silica Glass Tube

The (Ag,Pd)22Se6 phase was synthesized from individual elements by silica glass tube technique and structurally characterized from powder X-ray diffraction data. The (Ag,Pd)22Se6 phase crystallizes in Fm$\overline3$m symmetry, unit-cell parameters: a = 12.3169(2) Å, V = 1862.55(5) Å3, Z = 4, and Dc = 10.01 g/cm3. The crystal structure of the (Ag,Pd)22Se6 phase represents a stuffed 3a.3a.3a superstructure of the Pd structure (fcc), where only 4 from 108 available octahedral holes are occupied. Its crystal structure is related to the Cr23C6 structure type.

scholarly journals Synthesis and crystal structure of the quaternary semiconductor Cu2NiGeS4, a new stannite-type compound

2019 ◽  
Vol 65 (4 Jul-Aug) ◽  
pp. 355 ◽  
Author(s):  
G. E. Delgado ◽  
And V. Sagredo
Keyword(s):  
Crystal Structure ◽  
Rietveld Refinement ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Quaternary Compound ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters

The crystal structure of the quaternary compound Cu2NiGeS4, belonging to the system I2-II-IV-VI4, was characterized by Rietveld refinement using X-ray powder diffraction data. This material crystallize with a stannite structure in the tetragonal space group I2m (Nº 121), Z = 2, unit cell parameters a = 5.3384(1) Å, c = 10.5732(3) Å, V = 301.32(3) Å3, acknowledged as a normal valence adamantane-structure.

scholarly journals Synthesis and crystal structure of 1-ethyl-3-(phenyl)-1,2,3-triazolium percholorate

2003 ◽  
Vol 1 (4) ◽  
pp. 477-490
Author(s):  
Beeranahally Doreswamy ◽  
Madegowda Mahendra ◽  
Sridhar Anandalwar ◽  
Javaregowda Prasad ◽  
Kempegowda Mantelingu ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Structural Type ◽  
Monoclinic Space Group ◽  
Intermolecular Hydrogen Bonds ◽  
Nitrenium Ions ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography

AbstractThe isolation of stable carbenes of the Arduengo (1a) and Wanzlick (2a) type has prompted us to look for stable nitrenium ions of the related structural type 1-ethyl-3-(phenyl)-1,2,3-triazolium perchlorate (6+). The title compound C10H14Cl N3O4 was isolated and structure was investigated by X-ray crystallography. It crystallizes in the monoclinic space group P21/c with cell parameters a=6.697(4) Å, b=9.724(9) Å, c=19.844(2) Å and Z=4. The final residual factor is R1=0.0471 for 1545 reflections with I>2σ(I). The structure exhibits intermolecular hydrogen bonds.

scholarly journals Synthesis and spectroscopic properties of geminal-bis(tertbutylamino) phosphazenes obtained by the reaction of spiro and ansa phenoxyphosphazenes with the tert-butylamine and the crystal structure of 2,2-[2,2’-metheylenebis(4-chlorophenoxy)]-4,4-bis(tert-butylamino)-6,6-dichlorocyclo- 2λ5,4λ5,6λ5-triphosphazatriene

2011 ◽  
Vol 76 (6) ◽  
pp. 831-840
Author(s):  
Diğdem Erdener ◽  
Mustafa Yildiz ◽  
Hüseyin Ünver ◽  
Ocak İskeleli ◽  
Nuri Durlu
Keyword(s):  
Crystal Structure ◽  
31P Nmr ◽  
Spectroscopic Properties ◽  
Monoclinic Space Group ◽  
Spectroscopic Techniques ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Tert Butylamine

The condensation reactions of partly substituted spiro and ansa phenoxycyclotriphosphazenes, N3P3[2,2'-methylenebis(4-chlorophenoxide)]Cl4 (1 and 2) with tert-butylamine produce disubstituted geminal-bis(tert-butylamino)phenoxyphosphazene derivatives (3 and 4). The structures of these compounds were characterized by elemental analysis, and IR, 1H-, 13C-, 31P-NMR and mass spectroscopic techniques. Compound 3 was also examined by X-ray crystallography and found to be crystallized in the monoclinic space group P21/n with the unit cell parameters: a = 10.842(4), b = 9.375(5), c = 29.104(11) ?, ? = 99.25(3)?, V = 2920(2) ?3, Dx = 1.404 g cm-3.

Protein interactions of dirhodium tetraacetate: a structural study

2020 ◽  
Vol 49 (8) ◽  
pp. 2412-2416 ◽  
Author(s):  
Giarita Ferraro ◽  
Alessandro Pratesi ◽  
Luigi Messori ◽  
Antonello Merlino
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Protein Interactions ◽  
High Resolution Mass Spectrometry ◽  
Rnase A ◽  
Pancreatic Ribonuclease ◽  
X Ray ◽  
X Ray Crystallography ◽  
Model Protein ◽  
Resolution Mass

The interactions between the cytotoxic paddlewheel dirhodium complex [Rh2(μ-O2CCH3)4] and the model protein bovine pancreatic ribonuclease (RNase A) were investigated by high-resolution mass spectrometry and X-ray crystallography.

Synthesis and crystal structure of a homoleptic diruthenium complex containing tetra-2-pyridyl-1,4-pyrazine (tppz)

2017 ◽  
Vol 72 (10) ◽  
pp. 759-762 ◽  
Author(s):  
Marion Graf ◽  
Peter Mayer ◽  
Hans-Christian Böttcher
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Title Complex ◽  
Dinuclear Complex ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diruthenium Complex

AbstractTreatment of hydrated ruthenium(III) chloride with tetra-2-pyridyl-1,4-pyrazine (tppz) in refluxing ethoxyethanol afforded the homoleptic dinuclear complex [(tppz)Ru(μ-tppz)Ru(tppz)]4+ (1) besides small amounts of the species [Ru(tppz)2]2+. The title complex 1 was obtained as purple crystals and characterized as its hexafluoridophosphate salt by NMR spectroscopy, mass spectrometry and microanalyses. The molecular structure of 1(PF6)4 has been established by X-ray crystallography.

scholarly journals Synthesis and crystal structure of a mixed alkaline-earth powellite, Ca0.84Sr0.16MoO4

2020 ◽  
Vol 76 (2) ◽  
pp. 121-124
Author(s):  
Ryan M. Kissinger ◽  
Saehwa Chong ◽  
Brian J. Riley ◽  
Jarrod V. Crum
Keyword(s):  
Crystal Structure ◽  
Alkaline Earth ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
Xrd Pattern ◽  
X Ray ◽  
Cell Parameters ◽  
Good Agreement

A mixed alkaline-earth powellite, Ca0.84Sr0.16MoO4 (calcium strontium molybdate), was synthesized by a flux method and its crystal structure was solved using single-crystal X-ray diffraction (SC-XRD) data. The compound crystallized in the I41/a space group as with a typical CaMoO4 powellite, but with larger unit-cell parameters and unit-cell volume as a result of the partial incorporation of larger Sr cations into the Ca sites within the crystal. The unit cell and volume were well fitted with the trendline calculated from literature values, and the powder X-ray diffraction (P-XRD) pattern of the ground crystal is in good agreement with the calculated pattern from the solved structure.

scholarly journals Dehydration synthesis and crystal structure of terbium oxychloride, TbOCl

2020 ◽  
Vol 76 (5) ◽  
pp. 621-624
Author(s):  
Saehwa Chong ◽  
Brian J. Riley ◽  
Zayne J. Nelson
Keyword(s):  
Crystal Structure ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Good Agreement

Terbium oxychloride, TbOCl, was synthesized via the simple heat-treatment of TbCl3·6H2O and its structure was determined by refinement against X-ray powder diffraction data. TbOCl crystallizes with the matlockite (PbFCl) structure in the tetragonal space group P4/nmm and is composed of alternating (001) layers of (TbO) n and n Cl−. The unit-cell parameters, unit-cell volume, and density were compared to the literature data of other isostructural rare-earth oxychlorides in the same space group and showed good agreement when compared to the calculated trendlines.

Synthesis and Crystal Structure of Schiff Bases Based on AMTTO (AMTTO = 4-Amino-6-methyl-3-thio-3,4-dihydro-1,2,4-triazin- 5(2H)-one)

2006 ◽  
Vol 61 (11) ◽  
pp. 1421-1425 ◽  
Author(s):  
Maasoomeh Tabatabaee ◽  
Mitra Ghassemzadeh ◽  
Behnaz Zarabi ◽  
Bernhard Neumüllerc
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Microwave Irradiation ◽  
Schiff Bases ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

Reaction of 4-amino-6-methyl-3-thio-3,4-dihydro-1,2,4-triazin-5(2H)-one (1) with 2-methoxybenzaldehyde, 4-methoxybenzaldehyde, 2-pyridinecarbaldehyde, and 2,4-dichlorobenzaldehyde under classical heating and microwave irradiation in a solventfree system led to the corresponding imines (Schiff bases) 2-5. All synthesized compounds have been characterized by IR and NMR spectroscopy, mass spectrometry and by X-ray diffraction studies.

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