Metallkomplexe mit biologisch wichtigen Liganden, LXXIII [1] Komplexe von Palladium(II), Platin(II), Rhodium(III) und Iridium(III) mit N-6-Deoxy-galactopyranosyl-α-Aminosäuren / Metal Complexes with Biologically Im portant Ligands, LXXIII [1] Organometallic Compounds of Palladium(II), Platinum (II), Rhodium (III) and Iridium (III) with N-6-Deoxy-galactopyranosyl-α-amino Acids

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

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.


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.


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.


1994 ◽  
Vol 49 (11) ◽  
pp. 1569-1579 ◽  
Author(s):  
Elfriede Schuhmann ◽  
Christian Robl ◽  
Wolfgang Beck

N.O-Chelate complexes of R,S-2-(3-thienyl)glycinate (L) have been obtained: ML2 (M = Ni, Cu), (n-Bu3P)(Cl)M(L) (M = Pd. Pt), (η3-C3H5)Pd(L), C6H4CH,CHNMe2Pd(L), (η6-p-cymene)(Cl)Ru(L), (η5-C5Me5)(Cl)M(L) (M = Rh, Ir) and (η5-C5H5)(OC)2Mo(L). The methyl ester of R,S-2-(3-thienvl)glycine (L') forms the complexes trans-CT2PdL′2, cis- Cl2Pt(L')2, (η-Bu3P)(Cl2)M(L') (M = Pd, Pt) and (η5-C5Me5)(Cl)2M(L') (M = Rh, Ir) in which the ligand L' is coordinated through the amino group. The structures of (η3-C3H5)Pd(L) and of (η5-C5Me5)(Cl2)Ir(L') have been determined by X-ray diffraction. N- Benzoyl-2-(3-thienylglycine methyl ester reacts with Cr(CO)6 to yield a tricarbonyl complex with an η6-coordinated phenyl group. N-Benzoyl-R,S-2-(3-thienyl)glycinate (L") and (η5- C5H5)2TiCl2 give the diastereoisomers [(η5-C5H5)2Ti(R-L")(R-L")2/(η5-C5H5)2Ti(S-L") (S-L")] and (η5-C5H5)2Ti(R-L")(S-L") with Ti-O-bonds.


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.


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.


1974 ◽  
Vol 15 (3) ◽  
pp. 424-429 ◽  
Author(s):  
N. G. Bokii ◽  
Yu. T. Struchkov ◽  
D. N. Kravtsov ◽  
E. M. Rokhlina

RSC Advances ◽  
2016 ◽  
Vol 6 (36) ◽  
pp. 30277-30284 ◽  
Author(s):  
Zhi-Wen Liu ◽  
Xiao-Jun Huang ◽  
Han-Lin Xiao ◽  
Guo Liu ◽  
Jian Zhang ◽  
...  

The structures and absolute configurations of seven new iboga-type alkaloids 1–7 were determined by spectroscopic data, Mosher's method, single crystal X-ray diffraction and ECD analyses.


2014 ◽  
Vol 10 ◽  
pp. 2677-2682 ◽  
Author(s):  
Zhi Kai Guo ◽  
Rong Wang ◽  
Wei Huang ◽  
Xiao Nian Li ◽  
Rong Jiang ◽  
...  

An unusual C18 norditerpenoid, aspergiloid I (1), was isolated from the culture broth of Aspergillus sp. YXf3, an endophytic fungus derived from Ginkgo biloba. Its structure was unambiguously established by analysis of HRMS–ESI and spectroscopic data, and the absolute configuration was determined by low-temperature (100 K) single crystal X-ray diffraction with Cu Kα radiation. This compound is structurally characterized by a new carbon skeleton with an unprecedented 6/5/6 tricyclic ring system bearing an α,β-unsaturated spirolactone moiety in ring B, and represents a new subclass of norditerpenoid, the skeleton of which is named aspergilane. The hypothetical biosynthetic pathway for 1 was also proposed. The cytotoxic, antimicrobial, anti-oxidant and enzyme inhibitory activities of 1 were evaluated.


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