scholarly journals DIBUTYLTIN(IV) ALKYLCYCLOHEXYLDITHIOCARBAMATES: SPECTROSCOPIC CHARACTERIZATION AND CRYSTAL STRUCTURES OF DIBUTYLTIN(IV) N-METHYL AND N-ETHYLCYCLOHEXYLDITHIOCARBAMATE

2017 ◽  
Vol 25 (2) ◽  
pp. 419-426
Author(s):  
Normah Awang ◽  
Ibrahim Baba ◽  
Y. Farina Abd. Aziz ◽  
Bohari M. Yamin

A new series of dibutyltin(IV) alkylcyclohexyldithiocarbamates of the type (C4H9)2Sn[S2CNR(C6H11)]2 (R = CH3, C2H5, i-C3H7) have been successfully synthesized using in-situ method. These compounds were characterized by elemental analysis, infrared and 13C NMR spectroscopy. A single crystal X-ray analysis of dibutyltin(IV) ethylcyclohexyldithiocarbamate, (C4H9)2Sn[S2CN(C2H5)(C6H11)]2 (compound 2) showed that the system of this crystal is triclinic with space group P-1 while dibutyltin(IV) methylcyclohexyldithiocarbamate, (C4H9)2Sn[S2CN(CH3)(C6H11)]2 (compound 1) has monoclinic system and it’s space group is P21/c. In the crystal structure of compound 2, the dithiocarbamate ligands are bidentically chelated to the tin atom with non-equivalent of the Sn-S distances: Sn(1)-S(1) = 2.9255(11) and Sn(1)-S(2) = 2.5419(10); Sn(1)-S(3) = 2.8922(9) and Sn(1)-S(4) = 2.5293(10) Å while in compound 1, the dithiocarbamate ligands were anisobidentically  chelated to the tin atom.       

Synthesis ◽  
2020 ◽  
Vol 53 (02) ◽  
pp. 365-370
Author(s):  
Lucas Pizzuti ◽  
Izamara Casadia ◽  
Thalita O. Daher ◽  
Sidnei Moura ◽  
Davi F. Back ◽  
...  

A convenient domino route for the synthesis of novel 1,3-dihydrofuro[3,4-c]pyridines from pyridoxal and alkyl, aryl or heteroaryl ketones under basic conditions is reported. A series of nine derivatives is obtained in 53–90% yields after stirring reactants for 48 hours at room temperature. Most products are easily isolated by filtration followed by recrystallization from ethanol. All products were fully characterized by FTIR, HRMS, and 1H and 13C NMR spectroscopy. The X-ray crystal structure of a representative example of the 1,3-dihydrofuro[3,4-c]pyridine series is also presented.


2018 ◽  
Vol 28 (2) ◽  
pp. 55
Author(s):  
Mohammedl Mujbe Hasson

A new N, N'-imidazolium salt 1-(2,6-diisopropylphenyl)-3- (4,6-dimorpholino -1,3,5-traizine-2-yl)-1H-imidazol-3-ium chloride) as a precursor of N - heterocyclic carbene ligand was prepared via the reaction of 1 - (2, 6 - diisopropyl phenyl - 1H - imidazole) with 1, 3, 5 - triazine derivative bearing morpholine substituent (2, 6 -dimorpholine - 6- chloro-1, 3, 5-triaziazine). Linear coordi-nated Ag (І) NHC complex was synthesised via deprotonation of the imidazolium salt and reac-tion with Ag2O in darkness at room temperature by in situ method. The complex was synthesised for using as transfer agent to prepare another transition metals complexes by transmetallation method in the future. The imidazolium salt and their silver complex have been characterized by 1 H and 13C NMR spectroscopy as well as mass spectrometry.


2017 ◽  
Vol 72 (6) ◽  
pp. 425-432
Author(s):  
Waly Diallo ◽  
Libasse Diop ◽  
Cheikh Abdoul Khadir Diop ◽  
Laurent Plasseraud ◽  
Hélène Cattey

AbstractTwo new dialkyammonium selenate salts [i-Pr2NH2]2[SeO4] (1) and [n-Bu2NH2][HSeO4] (2) have been isolated and characterized by single-crystal X-ray diffraction. Salt 1 crystallizes in the monoclinic system, space group P21/n with a=8.7190(5), b=8.8500(4), c=22.5953(9) Å, β=94.6290(17)°, V=1737.84(14) Å3 and Z=4. Salt 2 crystallizes in the monoclinic system space group P21/n with a=10.9328(9), b=8.1700(6), c=13.8095(11) Å, β=97.130(3)°, V=1223.94(17) Å3 and Z=4. In both salts, dialkylammonium cations and selenate anions are connected through NH···O and OH···O hydrogen bonds. In the crystal structure, 1 and 2 are organized in layer-like arrangements. Structural characterizations were completed by infrared and 1H, 13C{1H} and 77Se NMR spectroscopy and elemental analysis which corroborate the X-ray elucidations.


2011 ◽  
Vol 76 (7) ◽  
pp. 995-1001 ◽  
Author(s):  
Verica Glodjovic ◽  
Gordana Radic ◽  
Snezana Stanic ◽  
Frank Heinemann ◽  
Srecko Trifunovic

(S,S)-Ethylenediamine-N,N'-di-2-propanoic acid hydrochloride, (S,S)-H2eddp?HCl, was prepared and its crystal structure determined. The compound was characterized by infrared and 1H- and 13C-NMR spectroscopy. It forms P1 in the space group of a triclinic crystal system with a = 5.3902(2) ?, b = 5.8967(2) ?, c = 10.3319(2) ?, ? = 99.625(2)?, ? = 91.645(2)?, ? = 109.995(2)? and Z = 1.


2013 ◽  
Vol 78 (10) ◽  
pp. 1531-1537
Author(s):  
Dejana Dimitrijevic ◽  
Sladjana Novakovic ◽  
Gordana Radic ◽  
Verica Jevtic ◽  
Laura Menéndez-Taboada ◽  
...  

The synthesis of butyl N-(3-chloropropyl)-(2S)-alaninate hydrochloride is reported here. The compound was characterized by elemental analysis, infrared, 1H and 13C NMR spectroscopy. The structure of butyl N-(3-chloropropyl)-(2S)-alaninate hydrochloride was confirmed by single-crystal X-ray analysis.


2004 ◽  
Vol 69 (8-9) ◽  
pp. 651-660 ◽  
Author(s):  
Katarina Andjelkovic ◽  
Gordana Jakovljevic ◽  
Mario Zlatovic ◽  
Zivoslav Tesic ◽  
Dusan Sladic ◽  
...  

Complexes of Zn(II), Pd(II) and Pt(II) with 2?-[1-(2-pyridinyl)ethylidene ]oxamohydrazide (Hapsox) were synthesized and their structures were determined. All the complexes are of a neutral type with two apsox ligands coordinated to Zn(II) and one apsox ligand coordinated to Pd(II) or Pt(II). In each case, the polydentate was coordinated via pyridine and hydrazone nitrogens and ?-oxyazine oxygen, forming an octahedral geometry around Zn(II), and a square planar one around Pd(II) and Pt(II). The structure determination was performed by IR, 1H-NMR and 13C-NMR spectroscopy, and for the Zn(II) complex by X-ray structure analysis.


1990 ◽  
Vol 45 (10) ◽  
pp. 1416-1424 ◽  
Author(s):  
W. Preetz ◽  
P. Hollmann ◽  
G. Thiele ◽  
H. Hillebrecht

The triply bonded octahalogenodiosmate(III) anions [Os2X8]2-, previously known with X = Cl, Br, have now been extended to include the iodide with two staggered OsI4 units. This compound was prepared by treating [Os2Cl8]2- with Nal at room temperature in acetone solution. The structure determination by X-ray diffractometry on single crystals of (PPN)2[Os2I8] · 2 CH2Cl2, reveals crystallization in the monoclinic system, space group P21/c with Z = 4. The Os-Os triple bond is with 2.212(1) Å the longest within the three octahalogenodiosmates(III). The Raman spectra show ν(OsOs) at 285, [Os2Cl8]2-; at 287, [Os2Br8]2- and for the iodo compound at 270.1 cm-1 with up to three overtones. The spectroscopic constants are calculated to be ω1 = 270.9 cm-1; X11 = -0.50 cm-1. The 10 Κ UV-VIS spectra of solid [(n-C4H9)4N]2[Os2X8] exhibit δ-π* transitions with maxima at 723, 690 and 643 nm, superimposed by vibrational fine structures with long progressions of 195, 211 and 183 cm-1 for X = Cl, Br, I, respectively. Oxidation of [Os2X8]2-, X = Cl, Br with the corresponding halogen leads to the cleavage of the Os-Os bond, and the dekahalogenodiosmates(IV), [Os2X10]2-, are formed


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