Synthesis and Spectroscopic Properties of Alkylquinoline‐8‐ol Extractants and their Cu(II)‐, Zn(II)‐ and Cd(II)‐Complexes
A series of deprotonizable chelating agents HL being characteristic of 2‐, 5‐ and 7‐alkyl substituted 8‐hydroxyquinolines or 5‐ and 7‐alkyl substituted 8‐hydroxyquinaldines of different alkyl chain length, H1–H5, and their Cu(II)‐, Zn(II)‐ und Cd(II)‐complexes, M(1)2–M(5)2, have been synthesized. Influences of the alkyl groups, including substituent effects on the spectroscopic properties (MS, IR, UV‐VIS, 1H und 13C NMR) of the free ligands and its complexes are studied.
New ether-phosphines of the type Ph2P~D (2d, 2g-1, 2n-p) with different electronic and steric properties which are provided with open-chained or cyclic ether moieties are obtained by reaction of LiPPh2 with the corresponding chloromethyl substituted ethers ClCH2~D (1d, 1g-1, 1n-p) in THF. The ligands 2d, 2g-1, and 2n-p are characterized by selected IR and NMR data which function as probes for complexation to transition metals.
Synthesis, Crystal Structure, and Fluxional Behavior of cis-Cl,Ru(CO)(P -O)(P"O) with cis-Positioned (Ether-Phosphane) Ligands * Reaction of the ether-phosphane ligands 2a-c with C12Ru-(PPh3)3 (1) results in the formation of the bis(che1ate) complexes trans-C12Ru(PnO), (3a-c) (P-0 = q'-P-coordinated; PnO = q2-0,Fcoordinated). With CO both Ru -0 bonds are cleaved to give aII-trans-Cl,Ru(CO),(P -O), (4a-c). The mono(che1a-te) complexes 5a-c are obtained from stoichiometric amounts of 3a-c and 4a-c. Upon heating the kinetically controlled products 5 a -c are transformed into the thermodynamically more stable isomers cis-Cl,Ru(CO)(P -O)(PnO) (6a-c). Both 5 a -c and 6 a -c show fluxional behavior. The higher coalescence temperatures and estimated AG* values of 6 a -c (75, 67, and ?O"C, respectively) compared to 5 a -c (55, 0, and -l O T , respectively) indicate different exchange mechanisms for 5 and 6. According to an X-ray structure analysis, 6b crystallizes in the monoclinic space group P2,/c with Z = 4. The action of CO on 6 a -c affords the cis,cis,trans complexes ?a-c.
Aufgrund des hemilabilen Charakters von
Resultate und DiskussionDie Bis(chelat)ruthenium ( Beim Erhitzen der Verbindungen 5a-c in Chloroform oder durch langsames Kristallisieren aus CH2C12/n-Hexan-
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