scholarly journals SYNTHESIS AND STRUCTURE OF TWO PALLADIUM(II) COMPLEXES BEARING ACETONITRILE AND N-HETEROCYCLIC CARBENE DERIVED FROM IMIDAZOLE

2019 ◽  
Vol 57 (4) ◽  
pp. 468
Author(s):  
Mai Thi Cam Truong ◽  
Chi Thi Thanh Nguyen
Keyword(s):  
Single Crystal ◽  
Diffraction Study ◽  
13C Nmr ◽  
Nmr Spectra ◽  
High Yield ◽  
13C Nmr Spectra ◽  
Trans Position ◽  
X Ray Diffraction ◽  
Imidazolium Chloride ◽  
X Ray

The reaction of [PdCl2(CH3CN)2] (1) with either 1,3-bis(2,4,6-trimethylphenyl)imidazolium chloride (IMes·HCl) or 1,3-bis(2,6-diisoproylphenyl)imidazolium chloride (IPr·HCl) in the present of Ag2O afforded two mixed monocarbene-CH3CN complexes, namely trans-[PdCl2(CH3CN)(IMes] (2) and trans-[PdCl2(CH3CN)(IPr)] (3), with the high yield (85-90%). The structure of 2 and 3 were elucidated by ESI mass, IR, 1H NMR and 13C NMR spectra. For 2, single-crystal X-ray diffraction study was also carried out. The results show that the CH3CN in 2 and 3 coordinates with Pd(II) via the N atom, the deprotonated imidazolium salts are bound up with Pd(II) via the C atom (NCHN) and occupy trans-position in comparison with the CH3CN.

Mercury(II) complexes of new bidentate phosphorus ylides: synthesis, spectra and crystal structures

2014 ◽  
Vol 68 (5) ◽  
Author(s):  
Seyyed Sabounchei ◽  
Mohammad Panahimehr ◽  
Hamid Khavasi ◽  
Fateme Bagherjeri ◽  
Collete Boscovic
Keyword(s):  
Single Crystal ◽  
Nmr Spectra ◽  
Mononuclear Complex ◽  
13C Nmr Spectra ◽  
Phosphonium Salts ◽  
X Ray Diffraction ◽  
Phosphorus Ylides ◽  
X Ray ◽  
Mononuclear Complexes ◽  
Tetrahedral Environment

AbstractThe reaction of dppm (1,1-bis(diphenylphosphino)methane) with 2-bromo-4-phenylacetophenone and benzyl bromoacetate in chloroform produces new phosphonium salts, [Ph2PCH2PPh2CH2C(O) C6H4Ph]Br (I) and [Ph2PCH2PPh2CH2COOCH2Ph]Br (II). By allowing the phosphonium salts to react with the appropriate base, the bidentate phosphorus ylides, Ph2PCH2PPh2=C(H)C(O)C6H4Ph (III) and Ph2PCH2PPh2=C(H)C(O)OCH2Ph (IV), were obtained. The reaction of these ligands with mercury(II) halides in dry methanol led to the formation of the mononuclear complexes {HgX2[(Ph2PCH2PPh2C(H)C(O)C6H4Ph)]} (X = Cl (V); X = Br (VI); X = I (VII)) and {HgX2[(Ph2PCH2PPh2C(H)COOCH2Ph)]} (X = Cl (VIII); X = Br (IX); X = I (X)). The FTIR and 1H, 31P and 13C NMR spectra were studied. The structure of compound III was unequivocally determined by the single-crystal X-ray diffraction technique. Single-crystal X-ray analysis of the {HgBr2[(Ph2PCH2PPh2C(H)C(O)C6H4Me)]} complex (XI) revealed the presence of a mononuclear complex containing the Hg atom in a distorted tetrahedral environment. In all complexes, the ylides referred to above were coordinated through the ylidic carbon and the phosphine atom.

Oligophosphan-Liganden, XIV [1] Bis(distickstoff)molybdän-KomplexeMo(N2)2[PhP(CH2CH2CH2PPh2)2](PR3) / Oligophosphine Ligands, XIV [1] Bis(dinitrogen)molybdenum Complexes Mo(N2)2[PhP(CH2CH2CH2PPh2)2](PR3)

1986 ◽  
Vol 41 (1) ◽  
pp. 70-75 ◽  
Author(s):  
Lutz Dahlenburg ◽  
Bernd Pietsch
Keyword(s):  
Single Crystal ◽  
Diffraction Study ◽  
Nmr Spectra ◽  
Nitrogen Atmosphere ◽  
Octahedral Geometry ◽  
X Ray Diffraction ◽  
Molybdenum Complexes ◽  
X Ray ◽  
Sodium Amalgam ◽  
Dinitrogen Complexes

The reaction of MoCl3(THF)3 with PhP(CH2CH2CH2PPh2)2 in THF/CH2Cl2 gave MoCl3(PhP(CH2CH2CH2PPh2)2) ·CH2CI2 (1). Sodium amalgam reduction of I in the presence of the monotertiary phosphines PMe3-nPhn (n = 0, 1, 2), in THF under nitrogen atmosphere, yielded the bis(dinitrogen) complexesMo(N2)2[PhP(CH2CH2CH2PPh2)2](PMe3) (2),Mo(N2)2[PhP(CH2CH2CH2PPh2)2](PMe2Ph) (3), andMo(N2)2[PhP(CH2CH2CH2PPh2)2I(PMePh2) (4).The homologous PPh3 and i-Pr3P derivatives as well as the attempted tris(dinitrogen) species Mo(N2)2[PhP(CH2CH2CH2PPh2)2] could not be isolated. Compounds 2-4 were assigned trans coordination of the N2 ligands on the basis of their IR, Raman, and 31P NMR spectra. The trans- octahedral geometry of these complexes was also confirmed by a single-crystal X-ray diffraction study performed on 3.

scholarly journals THE INTERACTION BETWEEN [Pt(µ-Cl)(Safrole-1H)]2 AND 1,3-DIISOPROPYLBENZIMIDAZOLIUM BROMIDE IN THE PRESENCE OF Ag2O

2020 ◽  
Vol 58 (6) ◽  
pp. 728
Author(s):  
Nguyen Thi Thanh Chi
Keyword(s):  
Single Crystal ◽  
Nmr Spectra ◽  
Molar Ratio ◽  
Trans Position ◽  
Dimeric Complex ◽  
X Ray Diffraction ◽  
Factors Affecting ◽  
X Ray ◽  
In Trans ◽  
Main Factors

The interaction of the dimeric complex [Pt(µ-Cl)(Saf)]2 (1) (Saf: deprotonated safrole) with the salt iPr2-bimy·HBr in the presence of Ag2O in acetone solvent was studied. The obtained products were mixed complexes of [PtCl(Saf)(iPr2-bimy)] (2) and [PtBr(Saf)(iPr2-bimy)] (3) with different molar ratio (PI, PII, PIII)  depended on the used molar ratio of 1:salt:Ag2O. In the case of this ratio being 1:2:1.1, the mixture PI with 75% for the complex 2 was obtained. When concentration of the salt was increased, the product was PII with the molar ratio of 2 : 3 of 1 : 3. However, when both the salt and Ag2O were increased at the same time, 2 and 3 in PIII had equal molar proportions. The two main factors affecting the 2 : 3 molar ratio are the different solubility of AgCl and AgBr and the different coordinating ability of Cl- and Br- ligands. The structure of 2 and 3 was determined by 1H NMR spectra and single crystal X-ray diffraction. The results reveal that Saf in 2 and 3 coordinates with Pt(II) via C=Colefinic and C5 of benzene ring. Meanwhile, iPr2-bimy coordinates with Pt(II) through CNCN and is in trans-position compared with the C=Colefinic bond.

The Electron Effect of Aromatic Group: Control Conformation of 2-Aromatic Cyclododecanone Derivatives

2020 ◽  
Vol 24 (10) ◽  
pp. 1139-1147
Author(s):  
Yang Mingyan ◽  
Wang Daoquan ◽  
Wang Mingan
Keyword(s):  
1H Nmr ◽  
13C Nmr ◽  
Nmr Spectra ◽  
Coupling Constants ◽  
The Other ◽  
Repulsive Interaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electron Effect ◽  
Group Control

2-Phenylcyclododecanone and 2-cyclohexylcyclododecanone derivatives were synthesized and characterized by 1H NMR, 13C NMR, HR-ESI-MS and X-ray diffraction. Their preferred conformations were analyzed by the coupling constants in the 1H NMR spectra and X-ray diffraction, which showed the skeleton ring of these derivatives containing [3333]-2-one conformation, and the phenyl groups were located at the side-exo position of [3333]-2-one conformation due to the strong π-π repulsive interaction between the π- electron of benzene ring and π-electron of carbonyl group. The cyclohexyl groups were located at the corner-syn or the side-exo position of [3333]-2-one conformation depending on the hindrance of the other substituted groups. The π-π electron effect played a crucial role in efficiently controlling the preferred conformation of 2-aromatic cyclododecanone and the other 2-aromatic macrocyclic derivatives with the similar preferred square and rectangular conformations.

Unusual Rearrangement of Naphthalene in the Synthesis of a Novel B8-B8-Bridged Derivative in the [(1,2-C2B9H11)2-3-Co]- Series. X-Ray Structure and 11B NMR Spectra of [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- (CH3)4N+

1997 ◽  
Vol 62 (5) ◽  
pp. 746-751 ◽  
Author(s):  
Andreas Franken ◽  
Jaromír Plešek ◽  
Christiane Nachtigal
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Nucleophilic Substitution ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Unusual Rearrangement ◽  
Multinuclear Nmr Spectroscopy ◽  
11B Nmr ◽  
Isolated Compound

On treatment of the [(1,2-C2B9H11)2Co]- ion with naphthalene in presence of AlCl3 a remarkably bridged [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- ion is obtained as a single isolated compound. The triatomic -CH2-C9H6- bridge is derived from the rearranged naphthalene nucleus. The mechanism of this reaction is obscure but it does resemble the "Electrophile-Induced Nucleophilic Substitution" reported earlier. The structure of the compound was established by multinuclear NMR spectroscopy and by single crystal X-ray diffraction.

Structural Study of an Unusual Diels-Alder Adduct

1992 ◽  
Vol 45 (12) ◽  
pp. 2089 ◽  
Author(s):  
EL Ghisalberti ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Diffraction Study ◽  
Structural Study ◽  
Spectroscopic Studies ◽  
Diels Alder ◽  
X Ray Diffraction ◽  
X Ray ◽  
Naturally Occurring ◽  
Chemical Evidence ◽  
Alder Adduct

The structure of the compound obtained on heating the naturally occurring clerodane furanoditerpene (1) had been formulated as (2) on the basis of spectroscopic studies. A single-crystal X-ray diffraction study on the dihydro derivative of (2) has confirmed this and provides support for the stereochemistry previously assigned to (1) on the basis of chemical evidence.

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