Einen Schmelzaufschlu\ zur Bestimmung von Platin, Palladium, Rhodium und Iridium

Ohne Zusammenfassung     

Trennung des Kupfers, Nickels, Eisens und Bleis von Platin, Palladium, Rhodium und Iridium

Ohne Zusammenfassung     

Zur papierchromatographischen Trennung der Edelmetalle Gold, Rhodium, Ruthenium, Palladium, Osmium, Iridium und Platin

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Nitrosodicyanmethanid-Komplexe von Palladium(II) und Platin(II)

Crystal and Molecular Structure of 1,8-Dihydroxy-3,6-dithiaoctan-bis-mercury(II) Chloride The crystal structure of 1,8-dihydroxy-3,6-dithiaoctane-bis-mercury(II) chloride has been determined by X-ray crystal structure analysis. The compound crystallizes monoclinic, space group C2/c with a = 15.311(2), b = 5.870(2), c = 17.479(2) Å, β = 102.76° and 4 formula units per unit cell. The structure was solved by heavy atom technique and refined to a final R value of R = 0.050. Mercury is digonally coordinated by an S and a Cl ligator. In consequence of weak interactions to an oxygen atom of the ligand as well as to three further Cl ions the coordination number is increased to six and a strongly distorted octahedron is formed. The crystal structure is built up from polymeric complex molecules.     

Mit der Frage der Wiedergewinnbarkeit von Mikromengen an Rhodium, Iridium, Palladium und Platin aus Erzen und Konzentraten

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Neutrale und kationische Ruthenium(II)-Komplexe mit trifunktionellen Phosphanliganden

Neutral and Cationic Ruthenium(II) Complexes with Trifunctional Phosphane Ligands Compounds of the type [RuCl₂(RPX₂)₂] 4 – 7 (R = iPr, tBu; X = CH₂CH₂OMe, CH₂CO₂Me) were prepared by reacting RPX₂ with either RuCl₃ · 3H₂O or [RuCl₂(PPh₃)₃], respectively. In 4 – 7 the trifunctional phosphanes coordinate as bidentate ligands to the metal center through the phosphorus atom and the oxygen atom of a methoxy or carbonyl group. The lability of the Ru–O bond allows substitution reactions with CO, tert-butylisonitrile and phenylacetylene. The Ru–Cl bonds in 5 (R = tBu; X = CH₂CH₂OMe) can be cleaved upon treatment with one or two equiv of AgPF₆ yielding mono- or dicationic derivatives. In these complexes the ligands are coordinated to the metal center through the phosphorus and both of the oxygen donor atoms. The reaction of the phosphinoesterenolate compound 17 with Ph₂C=C=O leads to the insertion of two molecules of the ketene into the C–H bond of one of the five-membered metal-enolate rings to yield the “expanded” chelate complex 18 , the structure of which was determined by X-ray crystallography.     

Die papierchromatographische Trennung von Gold(III), Platin(IV), Palladium(n) und Ruthenium(III)

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Metallorganische Verbindungen mit N-substituierten 3-Hydroxy-2-methyl-4-pyridon-Liganden: quadratisch-planare Rhodium(I)-, Iridium(I)- und Palladium(II)-Komplexe

Organometallic Compounds with N -substituted 3-Hydroxy-2-methyl-4-pyridone Ligands: square planar Rhodium(I), Iridium(I), and Palladium(II) Complexes Reactions of [(OC)₂MCl]₂ (M = Rh, Ir) or [(cod)RhCl]₂ with the anions of N-Aryl or N-Alkyl substituted 3-hydroxy-2-methyl-4-pyridones (O–O′) yield complexes of the general formula [L₂M(O–O′)]. Compounds of this type are also available from reactions of [(OC)₂Rh(acac)] with the corresponding neutral ligands. Substitution of one carbonyl-ligand of the N-phenyl complex [(OC)₂Rh(C₁₂H₁₀NO₂)] ( 2 ) with cyclooctene affords [(OC)(C₈H₁₄)Rh(C₁₂H₁₀NO₂)] ( 8 ). The palladium complexes [(R₃P)Pd(O–O′)Cl] (R = Et, Bu), [(C₆H₄CH₂NMe₂) · Pd(O–O′)] and [(Et₃P)₂Pd(O–O′)]BF₄ ( 9 – 12 ) were synthesized from [(R₃P)PdCl₂]₂, [(C₆H₄CH₂NMe₂)PdCl]₂ or [(Et₃P)PdCl₂]. The structures of the N-methyl compounds [(OC)₂Rh(C₇H₈NO₂)] ( 1 ) and [(Ph₃P)Pd(C₇H₈NO₂)Cl] ( 9 ) were determined by single crystal X-ray diffraction.     

Die Trennung des Rhodiums von Platin, Palladium und Iridium durch Ionenaustausch

Ohne Zusammenfassung1 Vgl. Berg, E. W., und W. L. Senn: analyt. Chemistry 27, 1255 (1955); vgl. diese Z. 150, 380 (1956); Cluett, M. L., S. S. Berman und W. A. E. McBryde: Analyst 80, 204 (1955); vgl. diese Z. 150, 380 (1956).     

Silber, Gold, Platin, Rhodium und Palladium

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Palladium(II)‐ und Platin(II)‐Komplexe mit dem Antimalariamittel Mefloquin als Liganden

Metal Complexes of Biologically Important Ligands. CXXVI. Palladium(II) and Platinum(II) Complexes with the Antimalarial Drug Mefloquine as Ligand The coordination sites of the antimalarial drug mefloquine (L) were studied. Reactions of the chloro bridged complexes (allyl)Pd(μ‐Cl)₂Pd(allyl) and (R₃P)(Cl)M(μ‐Cl)₂M(Cl)(PR₃) (M = Pd, Pt) with racemic mefloquine give the compounds (allyl)(Cl)Pd(L) ( 1 ), Cl₂(Et₃P)Pt(L) ( 2 ) and Cl₂(Et₃P)Pd(L) ( 3 ) with coordination of the piperidine N atom of mefloquine. In the presence of NaOMe the N,O‐chelate complexes Cl(Et₃P)Pt(L–H⁺) ( 4 ) and Cl(R₃P)Pd(L–H⁺) ( 5 , 6 , R = Et, nBu) were obtained. Protection of the piperidine N atom of mefloquine by protonation allows the synthesis of the complexes Cl₂(Et₃P)Pt(L + H⁺) ( 7 ) in which mefloquine is coordinated via the quinoline N atom. The structures of 2 , 3 and 4 were determined by X‐ray diffraction analysis. In the crystal of 4 pairs of enantiomers are found which are linked by two hydrogen bridges between the amine group and the chloro ligand.     

Nachweis und Bestimmung von Rhodium neben Platin, Palladium und Gold mit Hilfe der oscillographischen Polarographie

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Die spektrographische Beurteilung der Abtrennung des Platins von Palladium, Rhodium und Iridium

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Kohlenwasserstoffverbrückte Metallkomplexe. XLIX Koordinationschemie von bis(ferrocenyl)substituierten 1,3‐Diketonaten mit Ruthenium,Rhodium, Iridium und Palladium

Hydrocarbon‐bridged Metal Complexes. XLIX. Coordination Chemistry of Bis(ferrocenyl) substituted 1,3 Diketonates with Ruthenium, Rhodium, Iridium, and Palladium The reactions of the enolates of diferrocenoylmethane and of spacer bridged bis‐, tris‐ and tetrakis(ferrocenoyl)‐1,3‐diketones with chlorobridged compounds [(R₃P)PdCl₂]₂, [(η³‐C₃H₅)PdCl]₂, [(p‐cymene)RuCl₂]₂, [Cp*MCl₂]₂ (M = Rh, Ir) give a series of mono‐, bis‐, tris‐ and tetrakis(chelate) complexes 2 – 18 . The structures of (Ph₃P)(Cl)Pd[OC(Fe)CHC(Fc)O] ( 3 ) and (Tol₃P)(Cl) · Pd[OC(Fc)CHC(O)–C(O)CHC(Fc)O]Pd(Cl)(PTol₃) ( 11 ) were determined by X‐ray diffraction. The methine H atom of diferrocenoylmethane and of 3 was substituted by bromine using N‐bromosuccinimide. The electrophilic glycine equivalent α‐bromo‐N‐boc‐glycine ester was added to the methine C‐atom (C3) of diferrocenoylmethane and the product was used as O,O′ chelate ligand.     

Zum Einfluß der Ringgröße auf die Struktur von Metallchelaten. IV. Palladium(II)- und Platin(II)-Komplexe pyridylsubstituierter Dialkylsulfide und -amine

The Influence of Ring Size on the Structure of Metal Chelates with Tridentate Ligands. IV. Palladium(II) and Platinum(II) Complexes of Pyridyl Substituted Dialkyl Sulfides and Amines [β-(Pyridyl-2)-ethyl]-[(pyridyl-2)-methyl]-amine(2,3-py₂tri) forms planar palladium(II) complexes [Pd(2,3-py₂tri)X]X (X = Cl, Br) occupying trans-positions as a tridentate ligand. An analogous behaviour is observed with bis[β-(pyridyl-2)-ethyl]-sulfide(3,3-py₂Stri) in the chelate compounds [Me^II(3,3-py₂Stri)X]X (Me^II = Pd, Pt; X = Cl, Br, J, SCN). On the other hand the rigid ligand bis[(pyridyl-2)-methyl]-sulfide(2,2-py₂Stri) is only bidentate in the complexes Me^II(2,2-py₂Stri)X₂ (Me^II = Pd, Pt; X = Cl, Br, J, SCN), one pyridine group does not interact with the central atom. The reasons are the angular relations within the thioether group of 2,2-py₂Stri which allow a tridentate coordination in a facial conformation (octahedral and trigonal-bipyramidal nickel(II) and copper(II) complexes), but not in a meridional one (planar palladium(II) and platinum(II) complexes). In Pt(2,2-py₂Stri)(SCN)(NCS) one thiocyanato ligand is linked by sulfur, the other one by nitrogen.