Synthesis and EPR Spectral Studies of Mono- and Binuclear Cobalt(II) and Nickel(II) Complexes with New 20‐Membered Dithiatetraazamacrocyclic [N4S2] Ligand
摘要:
A new ligand, 6,10,16,20-tetraketo-8,18-dithia-1,5,11,15-tetraazacycloeicosane [N4S2] (L), and its complexes with cobalt(II) and nickel(H), have been synthesized and characterized by elemental analyses, molar conductance, magnetic susceptibility measurements, EPR and electronic spectral studies. The complexes were found to have the general composition [ML]X-2 and [M2LX2]X-2 for mono and binuclear complexes (M = Co, Ni; X = Cl, NO3, and SCN; and L = macrocyclic ligand). The mononuclear complexes of Co(H) and Ni(II) were found to have six-coordinated octahedral geometry. However, the binuclear complexes of Co(H) and Ni(H) are square-planar.
Synthesis and characterization of the pentadentate macrobicyclic ligand, 14-thia-1,4,8,11-tetraazabicyclo[9.5.3]nonadecane (L1) and its nickel(II) complexes. X-ray crystal structure of [Ni(L1)(ClO<sub>4</sub>)](ClO<sub>4</sub>)·2[Ni(L1)(OH<sub>2</sub>)](ClO<sub>4</sub>)<sub>2</sub>·6H<sub>2</sub>O
作者:Kevin R Coulter、Alexander McAuley、Steven Rettig
DOI:10.1139/v00-207
日期:2001.5.1
been determined. The ligand adopts a trans-III configuration. The Ni(II) ion is pseudooctahedral with Ni-S = 2.3896(10) A in [Ni(L1)(ClO4)]+ and 2.4193(10) A, 2.4225(10) A, in the two [Ni(L1)(H2O)]2+ cations. Both nickel(II) and nickel(III) complexes are six-coordinate in solution. Oxidation of the [Ni(L1)(OH2)]2+ complex with K2S2O8 in aqueous solution yielded an ESR active Ni(III) species and the
五齿大环,14-thia-1,4,8,11-四氮杂双环[9.5.3]十九烷(L1),已通过1-thia-4,8-二氮杂环十二烷([10]aneN2S)的高稀释环化合成(2) 使用 N,N'-双(α-氯乙酰胺) 丙烷 (3) 并随后还原二氧代中间体。[Ni(L1)(ClO4)](ClO4)·2[Ni(L1)(OH2)](ClO4)2·6H2O配合物的结构(单斜晶系,P21/c,a = 13.9261(4) A, b = 30.279(2) A, c = 17.1248(3) A, β = 94.5065(3)°) 在 R = 0.039 (Rw = 0.034) 时,911 个参数使用 18 266 次反射,I > 3σI 已确定。配体采用反式 III 构型。Ni(II) 离子是假八面体,[Ni(L1)(ClO4)]+ 中的 Ni-S = 2.3896(10) A,两个 [Ni(L1)]+
Isolation and characterization of an unusually stable formamidinium-containing macrotricyclic complex of lithium ion formed during the synthesis of 14-thia-1,4,8,11-tetraaza-bicyclo[9,5,3]nonadecane
作者:Tosha M Barclay、Alexander McAuley、S Subramanian
DOI:10.1139/v07-066
日期:2007.7.1
la cavite du produit 4 trop petite pour l'inclusion d'ions demetauxdetransition. La reaction du cation complexe [Li(4)] 2+ avec le PdCl 2 conduit a la formation dusel trimetallique [Li(4)-PdCl2-[Li(4)](C1O 4 ) 4 dans lequel deux ions [Li(4)] 2+ sont reunis par un pont de coordination du PdCl 2 avec les groupes thioethers donneurs lateraux. Une etude de la structure cristalline de ce sel trimetallique
: Utilisant le 1,3-bis(chloroacetamido)propane (5) comme intermediaire common, on a implementation une synthese efficace des syntheses par etape du l-thia-4,8-diazacyclodecane, du [10]aneN 2 S (8) et du macrobicyle pentadentate 17-thia-1,4,8,11-tetraazabicyclo[9.5.3]nonadecane (11)。Au cours de l'etude de lacondensation du produit 5 avec le produit 8, en utilisant le Li 2 CO 3 comme base, le cation
PALLADIUM ION ADSORBENT AND METHOD FOR SEPARATING AND RECOVERING PALLADIUM USING SAME
申请人:Tosoh Corporation
公开号:EP2468397A1
公开(公告)日:2012-06-27
To provide a solid-liquid palladium ion adsorbent which has both extraction performance and selectivity of a liquid-liquid palladium extracting agent in a conventional solvent extraction method and which does not require use of an organic solvent, and methods for selectively separating and recovering palladium, using it.
Palladium is selectively separated and recovered by using a palladium ion adsorbent comprising an amide-containing cyclic sulfide compound represented by the following formula (1) or (2), or a palladium ion adsorbent having the amide-containing cyclic sulfide compound represented by the following formula (1) or (2) fixed on a carrier:
wherein R is each independently a hydrogen atom, a methyl group, an ethyl group, a C3-30 linear or branched chain hydrocarbon group, a C3-10 alicyclic hydrocarbon group or a C6-14 aromatic hydrocarbon group, m is an integer of 1 or 2, n is each independently an integer of from 1 to 12, and L is each independently a methylene group, an ethylene group, a C3-8 alkylene group or a C6-14 arylene group;
wherein R is each independently a hydrogen atom, a methyl group, an ethyl group, a C3-30 linear or branched chain hydrocarbon group, a C3-10 alicyclic hydrocarbon group or a C6-14 aromatic hydrocarbon group, n is each independently an integer of from 1 to 4, and L is each independently a methylene group, an ethylene group, a C3-8 alkylene group or a C6-14 arylene group.
Synthesis and EPR Spectral Studies of Mono- and Binuclear Cobalt(II) and Nickel(II) Complexes with New 20‐Membered Dithiatetraazamacrocyclic [N<sub>4</sub>S<sub>2</sub>] Ligand
作者:Sulekh Chandra、Nidhi Gupta、Lokesh Kumar Gupta
DOI:10.1081/sim-120037516
日期:2004.5
A new ligand, 6,10,16,20-tetraketo-8,18-dithia-1,5,11,15-tetraazacycloeicosane [N4S2] (L), and its complexes with cobalt(II) and nickel(H), have been synthesized and characterized by elemental analyses, molar conductance, magnetic susceptibility measurements, EPR and electronic spectral studies. The complexes were found to have the general composition [ML]X-2 and [M2LX2]X-2 for mono and binuclear complexes (M = Co, Ni; X = Cl, NO3, and SCN; and L = macrocyclic ligand). The mononuclear complexes of Co(H) and Ni(II) were found to have six-coordinated octahedral geometry. However, the binuclear complexes of Co(H) and Ni(H) are square-planar.
Template synthesis and characterization of host (nanopores of zeolite Y)/guest (Co(II)-tetraoxodithiatetraaza macrocyclic complexes) nanocomposite materials
作者:Masoud Salavati-Niasari
DOI:10.1016/j.poly.2008.07.008
日期:2008.10
A series of Co(II) tetraoxodithiatetraaza macrocyclic complexes ([18]aneN(4)S(2), [20]aneN(4)S(2), Bzo(2)[18]aneN(4)S(2) and Bzo(2)[20]aneN(4)S(2)) have been encapsulated in the nanopores of zeolite Y by template condensation reaction. Co(II) complexes with tetraoxodithiatetraaza macrocyclic ligand were entrapped in the nanopores of zeolite Y by a two-steps process in the liquid phase: (i) ion-exchange of [bis(diamine)cobalt(II)] (diamine = 1,2-diaminoethane, 1,3-diaminopropane, 1,2-diaminobenzene, 1,3-diaminobenzene); [Co(N-N)(2)](2+)-NaY: in the nano-cavity of the zeolite, and (ii) in situ template condensation of the cobalt(II) precursor complex with thiodiglycolic acid. The mode of bonding and overall geometry of the complexes and new host/guest nanocomposite materials ([Co([18]aneN(4)S(2))](2+)-NaY, [Co([20]a-neN(4)S(2))](2+)-NaY, [Co(Bzo(2)[18]aneN(4)S(2))](2+)-NaY, [Co(Bzo(2)[20]aneN(4)S(2))(2+)-NaY) has been inferred through FT-IR, DRS and UV-Vis spectroscopic techniques, BET technique, molar conductance and magnetic moment data, XRD and elemental analysis, as well as nitrogen adsorption. The average number of encapsulated Co complexes per nano-cavity was determined to be 0.33 for the Co complexes-NaY. An octahedral geometry around the cobalt(II) ion is suggested for the complexes and new host/guest nanocomposite materials. (C) 2008 Elsevier Ltd. All rights reserved.