Preparation and Characterization of the First Organosulfonium Azides

2009 ◽  
Vol 64 (4) ◽  
pp. 467-469 ◽  
Author(s):  
Thomas M. Klapötke ◽  
Matthias Scherr ◽  
Burkhard Krumm
Keyword(s):  
Molecular Structure ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
Silver Azide ◽  
X Ray

The first triorganosulfonium azides [Me3S]N3 and [Ph3S]N3 were prepared by reaction of the corresponding sulfonium bromides/iodides with silver azide and characterized by spectroscopic methods. The molecular structure of [Ph3S]N3 as well as that of the precursor, [Ph3S]Br, have been determined by X-ray diffraction.

Synthesis and Electrochemistry of Aluminum Porphycenes: Crystal and Molecular Structure of Methyl-σ-Bonded Aluminum Etioporphycene

1997 ◽  
Vol 01 (02) ◽  
pp. 109-119 ◽  
Author(s):  
ROGER GUILARD ◽  
VIRGINIE PICHON-PESME ◽  
HASSANE LACHEKAR ◽  
CLAUDE LECOMTE ◽  
ALLY M. AUKAULOO ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Structural Data ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Axial Ligands ◽  
Uv Visible

The synthesis and characterization of three monomeric aluminum porphycenes with anionic or σ-bonded axial ligands is reported. The investigated compounds are represented as ( EtioPc ) Al ( CH 3) and ( EtioPc ) AlX where EtioPc represents the dianion of etioporphycene and X = Cl − or OH −. Each synthesized complex was characterized by mass spectrometry. 1 H NMR, IR and UV-visible spectroscopies as well as by electrochemistry. Comparisons are made between the properties of complexes in the aluminum etioporphycene series and related chloro- or methyl σ-bonded Al ( III ) porphyrins containing octaethylporphyrin ( OEP ) or tetraphenylporphyrin ( TPP ) macrocycles. Comparisons are also made between the currently investigated compounds and a previously reported Al ( III ) μ-oxo dimer, [( EtioPc ) Al ]2 O . In addition, the crystal and molecular structure of ( EtioPc ) Al ( CH 3) was determined by X-ray diffraction. The molecular structure of this methyl-σ-bonded aluminum etioporphycene provides the first structural data for an aluminum porphycene compound. The aluminum(III) atom in ( EtioPc ) Al ( CH 3) is pentacoordinated and is located 0.54 Å from the plane of the four N -nitrogens.

scholarly journals Synthesis and Characterization of New Diiron and Diruthenium μ-Aminocarbyne Complexes Containing Terminal S-, P- and C-Ligands

2007 ◽  
Vol 62 (3) ◽  
pp. 427-438 ◽  
Author(s):  
Vincenzo G. Albano ◽  
Luigi Busetto ◽  
Fabio Marchetti ◽  
Magda Monari ◽  
Stefano Zacchini ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Coordination Mode ◽  
Bond Cleavage ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dithiocarbamate Ligand ◽  
High Yields

The diiron aminocarbyne complexes [Fe2{μ-CN(Me)(R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (R = Xy1, 1a; R = Me, 1b; R = CH2Ph, 1c; Xy1 = 2,6-Me2C6H3) undergo replacement of the coordinated nitrile by halides, diethyldithiocarbamate, and dicyanomethanide to give [Fe2{μ-CN(Me) (R)}(μ-CO)(CO)(X)(Cp)2] complexes (R = Me, X = Br, 4a; R = Me, X = I, 4b; R = CH2Ph, X = Cl, 4c; R = CH2Ph, X = Br, 4d; R = CH2Ph, X = I, 4e; R = Xy1, X = SC(S)NEt2, 5a; R = Me, X = SC(S)NEt2, 5b; R = Xy1, X = CH(CN)2, 7), in good yields. The molecular structure of 5a shows an unusual η1 coordination mode of the dithiocarbamate ligand. Similarly, treatment of [M2{μ-CN(Me) (R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (M = Fe, R = Xy1, 1a; M = Fe, R = Me, 1b; M = Ru, R = Xy1, 2a; M = Ru, R = Me, 2b) with a series of phosphanes generates the cationic complexes [M2{μ- CN(Me)(R)}(μ-CO)(CO)(P)(Cp)2][SO3CF3] (M = Fe, R = Xy1, P = PPh2H, 6a; M = Fe, R = Xy1, P = PPh3, 6b; M = Fe, R = Xy1, P = PMe3, 6c; M = Fe, R = Me, P = PMe2Ph, 6d; M = Fe, R = Me, P = PPh3, 6e; M = Fe, R = Me, P = PMePh2, 6f; M = Ru, R = Xy1, P = PPh2H, 6g; M = Ru, R = Me, P = PPh2H, 6h), in high yields. The molecular structure of 6a has been elucidated by an X-ray diffraction study. The reactions of [Fe2{μ-CN(Me)(Xyl)}(μ-CO)(CO)(NCR′)(Cp)2][SO3CF3] [R′ = Me, 1a; R′ = tBu, 3] with PhLi and PPh2Li yield [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(Ph)(Cp)2] (8) and [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(PPh2)(Cp)2] (9), respectively. The molecular structure of 8 has been ascertained by X-ray diffraction. Conversely, the reaction of 1a with MeLi generates the aminoalkylidene compound [Fe2{C(Me)N(Me)(Xy1)}(μ-CO)2(CO)(Cp)2] (10).Finally, the acetone complex [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(OCMe2)(Cp)2][SO3CF3] (12) reacts with lithium acetylides to give complexes [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(C≡CR)(Cp)2] (R = p-C6H4Me, 11a; R = Ph, 11b; R = SiMe3, 11c), in high yields. Filtration through alumina of a solution of 11a in CH2Cl2 results in hydration of the acetylide group and C-Si bond cleavage, affording [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO){C(O)Me}(Cp)2] (12).

Synthesis and Structures of Cycloalkanetellurium(IV) Fluorides and Azides

2006 ◽  
Vol 61 (5) ◽  
pp. 528-534 ◽  
Author(s):  
Thomas M. Klapötke ◽  
Burkhard Krumm ◽  
Peter Mayer ◽  
Matthias Scherr
Keyword(s):  
Molecular Structure ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
X Ray

Telluracycloalkanes were fluorinated with XeF2 and the resulting tellurium(IV) fluorides were reacted with (CH3)3SiN3 to obtain the corresponding tellurium(IV) azides. The products, (CH2)5TeF2, (CH2)4TeF2, (CH2)5Te(N3)2 and (CH2)4Te(N3)2, were characterized by spectroscopic methods. The molecular structure of (CH2)4TeF2 as well as the structure of an oxygen bridged species, [(CH2)5TeN3]2O, have been determined by X-ray diffraction.

Synthese und Molekülstruktur des [α-(Dichlormethylsilyl)ethyl]- dichlorboran-dimethylsulfid / Synthesis and Molecular Structure of [α-(Dichloromethylsilyl)ethyl]- dichloroborane-dimethylsulfide

1999 ◽  
Vol 54 (5) ◽  
pp. 624-626 ◽  
Author(s):  
Lutz Ruwisch ◽  
Ralf Riedel ◽  
Uwe Klingebiel ◽  
Mathias Noltemeyer
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Markovnikov Rule

[α-(Dichloromethylsilyl)ethyl]-dichloroborane-dimethylsulfide has been synthesized by the reaction of dichloromethylvinylsilane with dichloroborane-dimethylsulfide and its molecular structure determined by single crystal X-ray diffraction and by spectroscopic methods. Following the Markovnikov rule, a chiral methine group is formed as a bridge between silicon and boron.

scholarly journals Synthesis and characterization of novel coumarin-based terpyridine ligands and their Zn(II) complexes

2020 ◽  
Vol 44 (11-12) ◽  
pp. 721-726
Author(s):  
Xiaolong Wang ◽  
Xian Yue ◽  
Long Deng
Keyword(s):  
Solvothermal Method ◽  
Emission Spectra ◽  
Synthesis And Characterization ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Terpyridine Ligands ◽  
Distorted Trigonal Bipyramidal

Two novel mononuclear Zn(II) complexes, [ZnL1Cl2] (1) (L1=( E)-3-(4-(2,2′:6′,2″-tripyridyl)-4′-styryl)-7-diethylaminocoumarin) and [ZnL2Cl2] (2) (L2=3-(4-(2,2′:6′,2″-tripyridyl)-4′-phenylimine)-7-diethylaminocoumarin), were obtained by the solvothermal method from ZnCl2 and coumarin-based terpyridine ligands. The complexes were characterized by spectroscopic methods and single-crystal X-ray diffraction. The Zn2+ in the complexes is coordinated by three nitrogen atoms of the terpyridine ligand and two chloride anions, forming a distorted trigonal bipyramidal environment. Moreover, the UV–Vis absorption and emission spectra of the ligands and complexes in diluted dichloromethane solutions were measured.

scholarly journals Synthesis and Characterization of Ammonium Acesulfamate

2014 ◽  
Vol 69 (6) ◽  
pp. 737-741 ◽  
Author(s):  
Gustavo A. Echeverría ◽  
Oscar E. Piro ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Molecular Structure ◽  
Ammonium Carbonate ◽  
Crystal And Molecular Structure ◽  
13C Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
1H And 13C Nmr ◽  
X Ray

Ammonium acesulfamate, (NH4)C4H4NO4S, was prepared by the reaction of acesulfamic acid and ammonium carbonate in aqueous solution, and characterized by elemental analysis and 1H and 13C NMR spectroscopy. Its crystal and molecular structure was determined by single-crystal X-ray diffraction methods. The substance crystallizes in the orthorhombic space group Pnma with Z = 4 molecules per unit cell. The NH4+ ion generates medium to strong hydrogen bonds with the carbonylic oxygen, the iminic nitrogen and the sulfonyl oxygen atoms of the acesulfamate anion. The FTIR spectrum of the compound was also recorded and is briefly discussed.

scholarly journals Characterization of cellulose nanocrystalline isolated from banana peduncles using acid hydrolysis

2021 ◽  
Vol 922 (1) ◽  
pp. 012072
Author(s):  
Ratna ◽  
S Aprilia ◽  
N Arahman ◽  
A A Munawar
Keyword(s):  
Molecular Structure ◽  
Acid Hydrolysis ◽  
Acid Concentration ◽  
Sulfuric Acid Concentration ◽  
Sulfamic Acid ◽  
Nanocrystalline Powder ◽  
Cellulose Content ◽  
X Ray Diffraction ◽  
X Ray

Abstract The study aimed to characterize cellulose nanocrystalline (NCCs) from banana peduncles using acid hydrolysis. The NCCs isolation process was done by hydrolysis using H2SO4 with concentrations of 1M, 2M, and 3M at a microwave power of 100 Watts within 1 hour of hydrolysis. The product of NCCs was characterized in term of yield, chemical composition (by FTIR), and its crystallinity. The result showed that the highest yield of 88.33% was obtained in acid hydrolysis at the concentration of 1M H2SO4. The results of the FTIR test showed that non-cellulose content had been removed and demonstrated that the molecular structure of cellulose does not change even when treated at different acid concentrations. X-Ray Diffraction analysis showed that crystallinity decreased by increasing the sulfamic acid concentration. The thermogravimetric analysis confirmed the heat resistance analysis and showed that the NCCs is gradually decomposed at a temperature range of 268.3–415.25 ¼C. The colour of cellulose nanocrystalline powder darkens as the sulfuric acid concentration increases.

scholarly journals Hydrosilyation of CO2 using a silatrane hydride: structural characterization of a silyl formate compound

2021 ◽  
Vol 99 (2) ◽  
pp. 259-267
Author(s):  
Serge Ruccolo ◽  
Erika Amemiya ◽  
Daniel G. Shlian ◽  
Gerard Parkin
Keyword(s):  
Molecular Structure ◽  
Density Functional Theory ◽  
Oxygen Atom ◽  
Structural Characterization ◽  
Density Functional ◽  
Density Functional Theory Calculations ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray

The silatrane hydride compound, [N(CH2CH2O)3]SiH, reacts with CO2 in the presence of the [tris(2-pyridylthio)methyl]zinc hydride complex, [Tptm]ZnH, to afford the silyl formate and methoxide derivatives, [N(CH2CH2O)3]SiO2CH and [N(CH2CH2O)3]SiOCH3. The molecular structure of [N(CH2CH2O)3]SiO2CH has been determined by X-ray diffraction, thereby demonstrating that the formate ligand adopts a distal conformation in which the uncoordinated oxygen atom resides with a trans-like disposition relative to silicon. Density functional theory calculations indicate that the atrane motif of [N(CH2CH2O)3]SiO2CH is flexible, such that the energy of the molecule changes relatively little as the Si···N distance varies over the range 2.0–3.0 Å.

Synthesis and molecular structure of [Rh(η5-C5H5)(coe)(PtBu2H)] (coe=cis-cyclooctene)

2019 ◽  
Vol 74 (5) ◽  
pp. 455-457 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Peter Mayer ◽  
Daniel Beck
Keyword(s):  
Molecular Structure ◽  
Nmr Spectroscopy ◽  
Single Crystals ◽  
Structural Characterization ◽  
Title Compound ◽  
Good Yield ◽  
X Ray Diffraction ◽  
X Ray

AbstractThe synthesis and structural characterization of the new olefinic complex [Rh(η5-C5H5)(coe)(PtBu2H)] (2, coe = cis-cyclooctene) is reported. The title compound was easily prepared in good yield by a thermolytic approach using [Rh(η5-C5H5)(coe)2] (1) and the secondary phosphane in toluene under reflux conditions. The compound 2 has been characterized by NMR spectroscopy and microanalysis. Single crystals of 2 were grown from n-hexane and the molecular structure has been established by X-ray diffraction.

scholarly journals [Re(CO)3Cl(C5H4ClP)2] and [Re(CO)2Cl(C5H4ClP)3]: synthesis and characterization of two novel rhenium(i) phosphinine complexes

RSC Advances ◽  
2016 ◽  
Vol 6 (17) ◽  
pp. 14134-14139 ◽  
Author(s):  
Manuela Hollering ◽  
Richard O. Reithmeier ◽  
Simon Meister ◽  
Eberhardt Herdtweck ◽  
Fritz E. Kühn ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

Two novel rhenium(i) phosphinine complexes [Re(CO)3Cl(η1-C5H4ClP)2] (1) and [Re(CO)2Cl(η1-C5H4ClP)3] (2) were synthesized and the molecular structure of both was determined by single crystal X-ray diffraction.

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