Metallkomplexe mit biologisch wichtigen Liganden, CXLVI [1]. Bis(allyl)-N,O-α-Aminocarboxylat-Rhodium-Komplexe / Metal Complexes of Biologically Important Ligands, CXLVI [1]. Bis(allyl)-N,O-α-Aminocarboxylate-Rhodium Complexes

2002 ◽  
Vol 57 (7) ◽  
pp. 810-818 ◽  
Author(s):  
Walter Ponikwar ◽  
Peter Mayer ◽  
Wolfgang Beck

The reactions of [(η3-C3H5)2Rh-μ-Cl]2 with the anions of α-amino acids (glycine, L-alanine, L-valine, L-isoleucine, L-proline, L-phenylalanine, L-phenylglycine, L-thyrosine) afford the N,O-chelates (η3-C3H5)2Rh(α-amino carboxylate). For complex (η3-C3H5)2Rh(glycinate) dynamic behaviour in solution could be observed by 1H NMR. The structure of (η3-C3H5)2Rh(L-prolinate) was determined by X-ray diffraction.

1981 ◽  
Vol 46 (10) ◽  
pp. 2345-2353 ◽  
Author(s):  
Karel Baše ◽  
Bohumil Štíbr ◽  
Jiří Dolanský ◽  
Josef Duben

The 6-N(CH3)3-6-CB9H11 carbaborane reacts with sodium in liquid ammonia with the formation of 6-CB9H12- which was used as a starting compound for preparing the 4-CB8H14, 9-L-6-CB9H13 (L = (CH3)2S, CH3CN and P(C6H5)3), 1-(η5-C5H5)-1,2-FeCB9H10-, and 2,3-(η5-C5H5)2-2,31-Co2CB9H10- carboranes. The 4-CB8H14 compound was dehydrogenated at 623 K to give 4-(7)-CB8H12 carborane. Base degradation of 6-N(CH3)3-6-CB9H11 in methanol resulted in the formation of 3,4-μ-N(CH3)3CH-B5H10. The structure of all compounds was proposed on the basis of their 11B and 1H NMR spectra and X-ray diffraction was used in the case of the transition metal complexes.


1995 ◽  
Vol 73 (7) ◽  
pp. 1164-1174 ◽  
Author(s):  
Doris Freiesleben ◽  
Kurt Polborn ◽  
Christian Robl ◽  
Karlheinz Sünkel ◽  
Wolfgang Beck

Schiff bases from ferrocene aldehyde and α-amino acidates react with PdCl2 or Na2PdCl4 to give N,O-chelate complexes (2a–e, 3). The related N-ferrocenylmethylen-α-amino acid esters give, with Pd(OAc)2, cyclopalladated acetate-bridged complexes (4a,b). N,O-chelate complexes (5–7) are obtained from Na2PdCl4 with N-ferrocenylmethyl prolinate and-alaninate as well as with N,N-dibenzyl glycinate. The ethyl ester of N,N-dibenzylglycine and Pd(OAc)2 form the cyclopalladated acetate-bridged complex 8, while the ester of N-monobenzylglycine and Na2PdCl4 affords trans-PdCl2(L)2 with a monodentate N-coordinated ligand. The structures of 2a, 4a, 5, 7, and 9 were determined by X-ray diffraction. Keywords: ferrocene, amino acids, palladium(II) complexes, crystal structures.


2019 ◽  
Vol 48 (17) ◽  
pp. 5614-5620
Author(s):  
Joshua Greenough ◽  
Zheng Zhou ◽  
Zheng Wei ◽  
Marina A. Petrukhina

Two new organometallic cyclooctatetraenyl complexes of the type [M2(COT)3(THF)2] (M = Y and La) have been prepared, using optimized synthetic procedures, and fully characterized by X-ray diffraction analysis, IR and 1H NMR spectroscopies.


1998 ◽  
Vol 53 (12) ◽  
pp. 1501-1505 ◽  
Author(s):  
Markus Prem ◽  
Kurt Polbom ◽  
Wolfgang Beck

Abstract The reaction of cis-(Ph3P)2PtCl2 with BOC-N-glycine and FMOC-N-alanine gives the carboxylate coordinated complexes cis-(Ph3P)2 Pt(Cl)(O2CCH2NHBOC) (1) and cis- (Ph3 P)2Pt(Cl)(O2CC(H)(Me)NHFMOC (2). Chloride and proton abstraction from 1 affords the N,O-chelate complex (Ph3P)2Pt(O2CCH2NBOC) (3). From the chloro-bridged compounds [Cp*MCl2]2 (M = Rh, Ir), [(p-cymene)RuCl2]2 and BOC-N-L-MetGlyOH (L) the compounds Cp*M(Cl)2L (4, 5) and (p-cymene)Ru(Cl)2L (6 ) with the mono-dentate dipeptide are obtained which in the presence of NaOMe form O,N,S-bis(chelate) complexes 7 - 9 . The X-ray diffraction analysis of the iridium O,N,S chelate complex 8 shows a five membered and a seven membered chelate ring.


1990 ◽  
Vol 68 (11) ◽  
pp. 1923-1931 ◽  
Author(s):  
Michael D. Clerk ◽  
Michael J. Zaworotko ◽  
Bozena Borecka ◽  
T. Stanley Cameron ◽  
Donald L. Hooper ◽  
...  

Carbanion sources (organolithium and Grignard reagents) react with [(mesitylene)2Fe]2+ and [(mesitylene)(Ch)Fe]+ cations (Ch = cyclohexadienyl) to afford neutral Ch2Fe and ChCh′Fe ("pseudoferrocene") complexes, respectively. Addition of R− (R− = methyl, phenyl, benzyl, and t-butyl) occurs stereospecifically via exo addition at an unsubstituted carbon atom of the arene ring. The synthesis and characterization of these complexes is detailed and the structure of bis(η5-exo-6-phenyl-1,3,5-trimethylcyclohexadienyl)iron(II), 3b, has been determined by single crystal X-ray diffraction analysis. 3b crystallizes in the triclinic space group [Formula: see text], with a = 11.947(2), b = 12.784(1), c = 8.865(2), α = 108.59(1)°, β = 108.19(1)°, γ = 84.91(1)°, and Dcalcd 1.227 g cm−3 for Z = 2. Least-squares refinement gave a conventional R value of 0.0452 for 2080 independent observed reflections. The structure reveals that the complex adopts a gauche-eclipsed conformation. The variable temperature (vt) 1H NMR spectra of pseudoferrocenes are interpreted in terms of restricted ring rotation around the ligand—metal—ligand axis. Keywords: arene, cyclohexadienyl, pseudoferrocene, variable temperature NMR, X-ray diffraction.


1994 ◽  
Vol 49 (9) ◽  
pp. 1193-1202 ◽  
Author(s):  
Yuanlin Zhou ◽  
Barbara Wagner ◽  
Kurt Polborn ◽  
Karlheinz Sünkel ◽  
Wolfgang Beck

A series of complexes with anions of N-[1,2:3,4-di-O-isopropylidene-6-deoxy-α-D-galactopvranos-6-yl]-α-aminoacids has been obtained and characterized by spectroscopic data: 1-4 (R' = 6-deoxy-galactopyranosyl), (η5-C5Me5)(Cl) 5, 6 (M = Rh, Ir), (η5-C5Me5)M(CH3SCH2CH2CH(CO2)NHR') 7,8 (M = Rh, Ir), M(NHR 'CHRCO2)2 9-16 (M = Cu, Pd), (η2-C2H4)(Cl)Pt(NHR'CHRCO2) 17-20, Cl2M(CH3SCH2CH2CH(CO2R)NHR) 21-24 (M = Pd, Pt), Cl2M(NHR'CHRCO2Me)2 25-31 (M = Pd, Pt). The structures of 3 (R = CH2CH2SMe), 4 (R = CH2Ph), 7 (M = Ir) and 21 (M = Pd, R = H) have been determined by X-ray diffraction


1999 ◽  
Vol 23 (3) ◽  
pp. 178-179
Author(s):  
Wendy I. Cross ◽  
Kevin R. Flower ◽  
Robin G. Pritchard

The acetic acid esters of 1-(4-methylphenylazo)naphthalen-2-ol 1 and 2-(4-methylphenylazo)-4-methylphenol 3 are prepared and characterised by single crystal X-ray diffraction studies and 13C{1H}NMR spectroscopy; the position of the C(2)13C resonance for the ester is used to predict the position of resonant frequency of the equivalent carbon in the parent alcohols and hence, calculate the position of the azo-hydrazone equilibrium in these compounds.


e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Shahram Mehdipour-Ataei ◽  
Leila Akbarian-Feizi

AbstractA diamine monomer containing ester, amide and ether functional groups was prepared and its polymerization reaction with different diisocyanates to give main chain poly(ester amide ether urea)s was investigated. The monomer was synthesized via reaction of terephthaloyl chloride with 4-hydroxybenzoic acid and subsequent reaction of the resulted diacid with 1,8-diamino-3,6-dioxaoctane. The polymers were characterized by FT-IR and 1H-NMR spectroscopic method and elemental analysis. The resulting polymers exhibited excellent solubility in polar solvents. Crystallinity of the resulted polymers was evaluated by wide-angle X-ray diffraction (WXRD) method, and they exhibited semi-crystalline patterns. The glass transition temperatures (Tg) of the polymers determined by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) were in the range of 88-112 °C. The temperatures for 10% weight loss (T10) from their thermogravimetric analysis (TGA) curves were found to be in the range of 297-312 °C in air. Also the prepared polyureas showed liquid crystalline character.


2014 ◽  
Vol 70 (a1) ◽  
pp. C534-C534
Author(s):  
Nasreddine Ghouari ◽  
Nourreedine Benali-Cherif

The theme of this work is part of the study of intermolecular interactions that hold the crystal structures of hybrid compounds based sulphuric acid, nitric acid, Melamine, Diethylamine, L-(+) - glutamic acid, DL-2-amino butyric acid. The aim of this work is to enlarge our laboratory researches [1-3] and methods in synthesis of new hybrid compounds consisting in organic cation(s) and mineral anion(s). We have obtained single crystals of a few samples after several trials and we plan to synthesize and characterize these crystals by X-ray diffraction, FTIR and Raman. The crystals structures allow us to study the 3D network hydrogen bonding, electron density and collect several other informations useful in FTIR and Raman studies of these hybrid compounds.


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