Synthesis, characterization, thermal properties of silicon(iv) compounds containing guanidinato ligands and their potential as CVD precursors

RSC Advances ◽  
2015 ◽  
Vol 5 (88) ◽  
pp. 71637-71643 ◽  
Author(s):  
Liyong Du ◽  
Wenxiang Chu ◽  
Hongyan Miao ◽  
Chongying Xu ◽  
Yuqiang Ding

The title compounds of the type (Me3Si)2N–C(N′R)(–N′′RSiMe3) (with R = iPr or Cy) as potential CVD precursors have been synthesized and characterized by X-ray diffraction, 1H NMR, 13C NMR, 29Si NMR and elemental analysis where necessary.

2005 ◽  
Vol 60 (10) ◽  
pp. 1049-1053 ◽  
Author(s):  
Zeanab Talaei ◽  
Ali Morsali ◽  
Ali R. Mahjoub

Two new ZnII(phen)2 complexes with trichloroacetate and acetate anions, [Zn(phen)2(CCl3COO)- (H2O)](ClO4) and [Zn(phen)2(CH3COO)](ClO4), have been synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR spectroscopy. The single crystal X-ray data of these compounds show the Zn atoms to have six-coordinate geometry. From IR spectra and X-ray crystallography it is established that the coordination of the COO− group is different for trichloroacetate and acetate. The former acts as a monodentate whereas the latter acts as a bidentate ligand.


2021 ◽  
Author(s):  
Adedibu Clement Tella ◽  
Samson Owalude ◽  
Vincent Adimula ◽  
Adetola Oladipo ◽  
Victoria Olayemi ◽  
...  

Abstract The coordination polymer [Cu2(TDPH)4(QNX)].DMF, (QNX = Quinoxaline; TDPH = 3,3-thiodipropionic acid), has been prepared by reaction of copper acetate, TDPH, and quinoxaline. The compound was characterized by elemental analysis, FTIR spectroscopy, and single-crystal X-ray diffraction. The crystal is monoclinic with a P21/n space group and dimensions of a = 12.889(3) Å, b = 14.983(4) Å, c = 14.091(3) Å, α = 90 °, β = 90.200(11) °, γ = 90 °, V = 2721.18 (2) Å3, Z = 4. The ligands are hexagonally coordinated to the Cu(II) centre in the form of Cu2O4N with one nitrogen atom from the quinoxaline ligand, and four oxygen atoms from four TDPH molecules in a monodentate fashion. The Cu-Cu bond length was 2.642(1) and 2.629(1) Å for the Cu1----Cu1 and Cu2----Cu2 bonds. The QNX ligand bridged the two copper atoms. The catalytic reduction of 4-nitrophenol to 4-aminophenol using NaBH4 in the presence of [Cu2(TDPH)4(QNX)].DMF, as catalyst was completed within 11 minutes. The 4-aminophenol product was confirmed using 1H NMR spectroscopy.


RSC Advances ◽  
2019 ◽  
Vol 9 (36) ◽  
pp. 20505-20512 ◽  
Author(s):  
Mixia Hu ◽  
YaLi Yan ◽  
Baohua Zhu ◽  
Fei Chang ◽  
Shiyong Yu ◽  
...  

Five Mn(i) photo-activated carbon monoxide-releasing molecules were synthesized by reactions of MnBr(CO)5 with L1–L4, and characterized via single crystal X-ray diffraction, 1H-NMR, 13C-NMR, IR, UV-vis and fluorescence spectroscopy.


2015 ◽  
Vol 1120-1121 ◽  
pp. 877-881
Author(s):  
Chao Jun He ◽  
Yu Min Yang ◽  
Kong Yang Wu

The biotransformation of 18β-glycyrrhetinic acid by Colletotrichum lini AS3.4486 was investigated. The conversion reaction was carried out for 72h, and the sole product was isolated by column chromatography and elucidated as 7β,15α-dihydroxy-18β-glycyrrhetinic acid by HR-ESI-MS, 1H-NMR , 13C-NMR and single–crystal X-ray diffraction. The crystal of the conversion product belongs to orthorhombic, space group P212121 with 11.828(1), 13.213(2), 19.606(2) Å , V = 3064.0 Å3, Z = 4. This study povides a new method for the synthesis of 7β,15α-dihydroxy-18β-glycyrrhetinic acid.


2007 ◽  
Vol 62 (3) ◽  
pp. 475-482 ◽  
Author(s):  
Karsten Schubert ◽  
Helmar Görls ◽  
Wolfgang Weigand

Starting from 4-bromoacetophenone 1, the 4-bromo-β -hydroxydithiocinnamic acid 2 and the 4-bromo-β -hydroxydithiocinnamic acid hexyl ester 3 were prepared using carbon disulfide and potassium-tert-butylate as a base. Acting as a ligand, the acid gives 1,1-ethenedithiolato complexes with (Ph3P)2Pt(II) (4a), (Et3P)2Pt(II) (4b), dppePt(II) (4c), (Ph3P)2Pd(II) (4d), dppePd(II) (4e), and dppeNi(II) (4f). In contrast to the acid, the deprotonated ester 3 forms a monoanionic bidentate ligand. [O,S] Complexes of Pt(II) (5a), Pd(II) (5b) and Ni(II) (5c) were obtained. All complexes have been fully characterised using 1H NMR, 13C NMR and 31P NMR spectroscopy, mass spectrometry, infrared spectroscopy and elemental analyses. The molecular structures of the complexes 4b and 5a - 5c were determined by X-ray diffraction analyses.


2014 ◽  
Vol 2014 ◽  
pp. 1-16 ◽  
Author(s):  
Mohamed A. Riswan Ahamed ◽  
Raja S. Azarudeen ◽  
N. Mujafar Kani

Terpolymer of 2-amino-6-nitro-benzothiazole-ethylenediamine-formaldehyde (BEF) has been synthesized and characterized by elemental analysis and various spectral techniques like FTIR, UV-Visible, and1H and13C-NMR. The terpolymer metal complexes were prepared with Cu2+, Ni2+, and Zn2+metal ions using BEF terpolymer as a ligand. The complexes have been characterized by elemental analysis and IR, UV-Visible, ESR,1H-NMR, and13C-NMR spectral studies. Gel permeation chromatography was used to determine the molecular weight of the ligand. The surface features and crystalline behavior of the ligand and its complexes were analyzed by scanning electron microscope and X-ray diffraction methods. Thermogravimetric analysis was used to analyze the thermal stability of the ligand and its metal complexes. Kinetic parameters such as activation energy(Ea)and order of reaction (n) and thermodynamic parameters, namely,ΔS,ΔF,S*, andZ, were calculated using Freeman-Carroll (FC), Sharp-Wentworth (SW), and Phadnis-Deshpande (PD) methods. Thermal degradation model of the terpolymer and its metal complexes was also proposed using PD method. Biological activities of the ligand and its complexes were tested againstShigella sonnei,Escherichia coli,Klebsiellaspecies,Staphylococcus aureus,Bacillus subtilis, andSalmonella typhimuriumbacteria andAspergillus flavus,Aspergillus niger,Penicilliumspecies,Candida albicans,Cryptococcus neoformans,Mucor speciesfungi.


2020 ◽  
Author(s):  
Sergey Zubkevich ◽  
Vladislav Tuskaev ◽  
Svetlana Gagieva ◽  
Alexander Pavlov ◽  
Viktor N. Khrustalev ◽  
...  

<div>Nickel(II) complexes with pyrazole-based ligands are widely employed in catalysis of ethylene</div><div>oligomerization and subsequent Friedel-Crafts alkylation of toluene. We have prepared ten new</div><div>nickel(II) dibromide complexes with various substituted bis(azolyl)methanes. They have been</div><div>characterized using <sup>1</sup>H NMR, IR, MALDI-TOF and elemental analysis. The structures of three</div><div>complexes have been unambiguously established using X-ray diffraction. It was found that these</div><div>complexes in the presence of Et<sub>2</sub>AlCl or Et<sub>3</sub>Al<sub>2</sub>Cl<sub>3</sub> are active both in ethylene oligomerization and</div><div>Friedel-Crafts alkylation processes (activity up to 3720 kgoligomer·mol[Ni]<sup>−1</sup>·h<sup>−1</sup>). The use of Et<sub>3</sub>Al<sub>2</sub>Cl<sub>3</sub></div><div>results in the higher share of alkylated products (up to 60%). Moreover, catalytic systems activated with</div><div>Et<sub>3</sub>Al<sub>2</sub>Cl<sub>3</sub> produced small amounts of odd carbon number olefins (up to 0.8%). The Friedel-Crafts</div><div>alkylation was used as a trap for previously undetected short-chain odd carbon number olefins (C<sub>3</sub> and</div><div>C<sub>5</sub>).</div>


2003 ◽  
Vol 58 (5) ◽  
pp. 389-394 ◽  
Author(s):  
Alexander A. Trifonov ◽  
Mikhail N. Bochkarev ◽  
Herbert Schumann ◽  
Sebastian Dechert

Racemic trans-2-(9(H)-fluoren-9-yl)cyclohexanol, C13H9-cyclo-C6H10-OH (1), reacts with two equivalents of potassium naphthalenide in THF to give the dipotassium salt [C13H8-cyclo-C6H10-O]- K2(THF) (2). Recrystallization of 2 from pyridine affords the solvent free salt [C13H8-cyclo-C6H10- O]K2 (3). The reactions of LaI3(THF)4 with one equivalent of 2 or of YbI2(THF)2 with equimolar amounts of 2 produce the alkoxolanthanum diiodide (C13H9-cyclo-C6H10-O)LaI2(DME)2 (4) and the ytterbium dialkoxide (C13H9-cyclo-C6H10-O)2Yb(THF)0.5(5), respectively. [(Me3Si)2N]3Y reacts with three equivalents of 1 with elimination of hexamethyldisilazane and formation of the yttrium trialkoxide (C13H9-cyclo-C6H10-O)3Y (6). The compounds 2 to 5 were characterized by elemental analyses, 1H NMR, 13C NMR and IR spectra. The molecular structure of 4 was determined by single crystal X-ray diffraction.


2007 ◽  
Vol 62 (4) ◽  
pp. 605-609 ◽  
Author(s):  
Li Tao ◽  
Yang Bingqin ◽  
Gao Bo

Two novel ester ferrocenophanes have been prepared by esterification of 1,1′-ferrocenedi(carbonyl chloride) with glycol and 1,4-butanediol, respectively. Both of them have been characterized by IR, elemental analysis, MALDI-TOF MS and 1H NMR spectroscopic methods, and their structures have been elucidated by X-ray diffraction. The intermolecular associations based on C-H···O hydrogen bonds have also been discussed. These molecules are assembled into chains, and the chains are further assembled into a 3D structure through several hydrogen bonds.


1979 ◽  
Vol 57 (12) ◽  
pp. 1456-1461 ◽  
Author(s):  
Gregorio G. Trigo ◽  
Carmen Avendaño ◽  
Emilia Santos ◽  
John T. Edward ◽  
Sin Cheong Wong

The tropane-3-spiro-5′-hydantoin (α isomer) obtained from tropinone by the Bucherer–Bergs reaction has been shown by 13C nmr and X-ray diffraction studies to have the 4′-carbonyl group in the equatorial position; the β isomer, obtained via the Strecker reaction, has this group axial. The results of these two reactions on cis-bicyclo[3.3.0]octan-3-one and on cis-3,4-dimethylcyclopentanone show, on the basis of the 1H nmr, 13C nmr, and X-ray diffraction studies of the products, a stereochemical course related to the preferred conformation of the cyclopentane rings.


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