Synthesis and Properties of Dinuclear Cu( Ⅱ ) Complexes Derived from Oxamidobis(propionato)cuprate( Ⅱ )

Three dinuclear complexes were synthesized and designated as Cu(obp)CuL where obp =oxamidobis(propionato), L=2,2' -bipyridyl(bpy) (1), 1 , 10-phenathroline(phen)(2) and 5-nitro-1, 10-phenathroline(NO2-phen)(3). The complexes were characterized by elemental analyses, in fared and electronic spectra, magnetic susceptibilities and ESR spectra, indicating antiferromagnetic spin exchange interactions between metal ions.     

Synthesis and Properties of u-Oxamido Heterobinuclear Cu(Ⅱ)-Co(Ⅱ) Complexes

Three heterobinuclear complexes were synthesized, namely [Cu (oxpn) Co (L)2] (ClO4)2·xH2O(L= 2,2'-bipyridyl(bpy), 1,10-phenanthroline(phen) , and 5-nitro-1, 10-phenanthroline (NO2-phen)), where oxpn represents N, N'-bis(3-aminopropyl) oxam-ido. Based on 1R, elemental analysis, conductivity measurement and electronic spectra, these complexes were characterized by an extended oxamido-bridged structure with Cu(Ⅱ) in a planar environment and Co(Ⅱ) in a octahedral environment. The symmetry of the cation is very close to C2v.The complexes were also characterized with variable temperature (4~300K) magnetic susceptibility, and the data were fit for the susceptibility equation derived from spin Hamilton, H= -2JS1.S2-DSx12 by least square strategy. The exchange integral, J, was found to be -22.36 cm-1 (for bpy);-15.45 cm-1 (for phen); -19. 10cm-1(for NO2-phen), indicating that there is a weak antiferromagnetic spin-exchange interaction between the metal ions.     

Synthesis and Magnetism of μ-IsophthalatoOxovanadium(Ⅱ) Binuclear Complexes

INTRoDUCTIONThestudyoflong-rangemagneticinteractiotisofbinuclearcom-plexeswithextendedbridgedstructureareofcurrentinterestinrecentyears.Inviewoftheeffectivebridgingfunctionofisophthalatedianion(abbreviatedasIPHTA),thispa-perdealswiththesguthesis,characterizationandrnagnetismoftwonewp-IPHTAoxo-vanadium(ll)binuclearcomplexes.Synthesisof[(Vo),(IPHTA)(phen),]SO4(1)Asolutionofpiperidiniumisophthalate'(134.4mg,O.4mmol)andphen(l44.2mg,o.8mmol)inmethanol(1omL)wasaddedslow1ytoamethanolsolut…     

Synthesis and Structures of Dinuclear Aluminum Complexes Based on Bis(β-diketiminate) Ligands

A series of ten dinuclear aluminum alkyl complexes based on rigid, semirigid, and flexible bis(β-diketiminate) ligands (NacNac) has been obtained from the reaction of trimethylaluminum and the corresponding bis(β-diketimine)s. All compounds were fully characterized using NMR and IR spectroscopy and elemental analysis. The molecular structures of five compounds have been investigated by means of single-crystal X-ray diffraction analysis.     

Synthesis, Structure and Magnetic Properties of Novel Carboxylato-bridged Pentanuclear Copper(Ⅱ)-Lanthanoid(Ⅲ) Complexes

ＩｎｔｒｏｄｕｃｔｉｏｎＰｏｌｙｎｕｃｌｅａｒｍｉｘｅｄ－ｍｅｔａｌｃｏｍｐｌｅｘｅｓｃｏｎｔａｉｎｉｎｇｂｏｔｈｔｒａｎｓｉｔｉｏｎａｎｄｌａｎｔｈａｎｏｉｄｍｅｔａｌｉｏｎｓａｒｅｏｆｓｐｅｃｉａｌｃｕｒｅｎｔｉｎｔｅｒｅｓｔｉｎｒｅｌａｔｉｏｎ...     

Design,Synthesis and Biological Evaluation of Novelα-Acyloxycarboxamide-Based Derivatives as c-Met Inhibitors

Dysregulated HGF/c-Met signalling has been associated with many human cancers,poor clinical outcomes,and even resistance acqui-sition to some approved targeted ...     

Synthesis,Crystal Structure and Catalytic Activity Palladium (Ⅱ) Complexes Containing Bulky Azole Ligands

Bulky azole ligands in combination with PdCl_2 provide three new palladium(II) complexes. All these complexes, as pre-catalysts, have high catalytic efficiency for the Suzuki-Miyaura cross-coupling reactions of sterically hindered aryl chlorides and good to high yields are obtained with low catalysts loadings(0.1 mol%) under mild conditions in air.     

Synthesis and Crystal Structures of the α and β Forms of Bis(salicylaldoxime)copper(Ⅱ) Complexes

Modified α and β bis(salicylaldoxime)copper(Ⅱ) have been obtained by recrystallization from ethyl acetate(CCDC Nos. 212157 & 212158). The X-ray analysis reveals that the two modificated forms have the same structure with different geometric parameters. The α form crystallizes in the P2(1)/c space group and the β form in the P1 space group. Both the crystal structures consist of centrosymmetric monomeric molecules of Cu(OC6H4CNOH)2. The IR spectra are in agreement with the structural data.     

Synthesis and Characterization of Aryl Acylguanidines and Their Copper(Ⅱ) Complexes

A series of eight N-mono-substituted aryl acylguanidines L~(1～8) were synthesized from the reactions of their parent acylthioureas and respective primary amines, including five R~1C(O)N=C(NHR~2)_2 with balanced arms(denoted as R~1–R~2–R~2: Ph–Ar'–Ar', L~1(1); Ph–Ar'–Ar', L~2(2); 1-Naph–Ar'–Ar', L~3(3); 1-Naph–Ar'–Ar', L~4(4); 2-Naph–Ar'–Ar', L`5(5); Ar' = 2,6-Me_2C_6H_3, Ar' = 2,6-iPr_2C_6H_3) and three R~1C(O)N=C(NHR~2)NHR~3 with unbalanced arms(denoted as R~1–R~2–R~3: Ph–Ar'–Ph, L~6(6); Ph–Ar' –Ph, L~7(7); Ph–Ar' –Ar', L~8(8)). Treatment of L~(1～5)(1～5) with copper acetate in a molar ratio of 2:1 in dichloromethane led to the formation of homoleptic Cu(Ⅱ) complexes trans-L_2~(n')Cu(9～13), in which the Cu(Ⅱ) center was stabilized by deprotonated ligands Ln'(n = 1～5) in the O,N-bidentate mode. When similar reactions of L~6(Ph–Ar'–Ph)(6) and L~7(Ph–Ar'–Ph)(7) that contain unbalanced arms were investigated, the Cu(Ⅱ) products trans-L_2~(6')Cu(14) and trans-L_2~(7')Cu(15) were formed by deprotonating the bulky amine groups in Ln(-NHAr' for L~6 and-NHAr' for L~7) rather than the-NHPh group. In sharp contrast, trans-L_2~(8')Cu(16) was obtained from two-arm unbalanced L~8(Ph–Ar'–Ar')(8) not by deprotonating the more bulky-NHAr' group but the relatively less bulky-NHAr' group. In a further exploration, the reaction of 1:1 mixed ligands Ln and Lm with copper acetate was found to give only homoleptic Cu(Ⅱ) complex L_2~(n')Cu instead of the heteroleptic one L~(n')CuL~(m'). The in vitro antibacterial activity of L~n was evaluated against S. aureus, E. coli and C. albicans by determining the minimum inhibitory concentrations(MICs) using Kirby-Bauer test.     

Synthesis and Biological Evaluation of Pyranone Analogues of Territrem B

As a highly selective and potent acetylcholinesterase(AChE)inhibitor,territrem B wasisolated by Ling et al.from a strain of Aspergillus terreus in19791,2.Zhao et alreported mimic preparation of territrem B analogues from triterpenoids and found thatthe enone moiety and aromatic ring played important roles in their syntheticcompounds3,4.To further detect essential pharmacophors for AChE inhibitors,wesimplified the A/B ring system of territrem B and synthesized a number of pyranonepharmacop…     

Syntheses,Characterization and Crystal Structures of Dithiocarbamate-based Mononuclear Palladium(Ⅱ) Complexes

By employing the dithiocarbamate salt(K(PPDC), where PPDC = 4?-pyridyl-1-piperazine-4-dithiocarbamate) as the functional ligand and di-palladium complexes [(N^N)_2Pd_2(NO_3ˉ)_2](NO3ˉ)2(N^N = 2,2?-bipyridine, bpy; 4,4?-dimethylbipyridine, dmbpy) as corner, two novel single metal complexes with Pd(II) centers have been obtained. These organic-metal complexes were characterized by NMR, ESI-MS, elemental analysis, Uv-vis spectra and single-crystal X-ray diffraction analysis. Compound 1·(PF6)2([(bpy)Pd(PPDC)]·(PF6)2) crystallizes in triclinic, space group P1, a = 8.3968(5), b = 11.5565(7), c = 18.2234(11) ?, α = 97.505(1), β = 91.424(1), γ = 106.146(1)o, C22H24N6S2P2F12 Pd, Mr = 832.93, V = 1680.58(18) ?~3, Z = 2, Dc = 1.646 Mg/m3, μ(MoK α) = 0.863 mm-1, F(000) = 828, the final R = 0.0455 and wR = 0.1390 for 6981 observed reflections with I 2σ(I). Similarly, compound 2·(PF6)2([(dmbpy)Pd(PPDC)]·(PF6)2) also crystallizes in triclinic, space group P1, a = 13.9467(3), b = 14.8390(2), c = 17.0632(3) ?, α = 81.8680(10), β = 87.051(2), γ = 83.4590(10)o, C_(22)H_(25)N_5S_2P_2F_(12)Pd, M_r = 819.93, V = 3470.81(11) ?~3, Z = 4, D_c = 1.569 Mg/m~3, μ(CuK α) = 7.115 mm~(-1), F(000) = 1632, the final R = 0.0606 and w R = 0.1637 for 12835 observed reflections with I 2σ(I). Crystallography reveals that each metal center coordinates with two N atoms from bpy and two S atoms from PPDC in the square coordination mode. In the crystal structure of complex 1, a weak Pd···Pd interaction can be observed. Interestingly, it was also found that the mononuclear moieties of complex 2 could be packed into a 3-D porous framework via multiple intermolecular C–F···H hydrogen-boding interactions which extended in the a, b, and c axes with PF_6ˉ anions frozen inside.     

Synthesis and Magnetic Studies of Oxamido-Bridged Cu(Ⅱ)-Fe(Ⅱ) Heterobinuclear Complexes

~The~andmagneti~Of~~areatoPicthahasndchinndinndnd.bondinthewiin-wtofbinudearCU(n)-Fe(u)-,chewedwiththe~alleq-nettrioftwnew~-,[CU(oxa)Fe(L)21sa(Lbo1,1o-~(Phen)nd5-nithe1'1o-~(NQ-Phen)),whereOxaisN,N'-bis(2-amhathy).edfor.-Synboor(1)ToCh(oxae)2(94.2mp'o.4ed)theindri(5nd)wasbo-lyadtalaedboofso.Wio(111.2mp,o.4nuno)inmeto(1ond)ndaboofPhen(144-2mp,o.8mrnO)inrne~(1OrnL)underN2atrmpe.theedfor2hthegreddebm~thuSfo~wereforoff,washededtimeswithrne~anddiethyletheranddriedoverP2QUnderededpe.ha:C,…     

Synthesis and Crystal Structure of Cobalt(Ⅱ) and Copper(Ⅱ) Complexes Involving L-Aamino Alcohols

Two novel L-amino alcohol coordination cobalt and copper complexes I and Ⅱ were obtained separately from the direct reaction of L-plenylglycinol with Co(Ⅱ) acetate tetrahydrate in anhydrous ethanol and L-leucinol with Cu(Ⅱ) chloride dihydrate in anhydrous methanol. The structures of I and Ⅱ were determined by single-crystal X-ray diffraction and further characterized by elemental analysis and IR. For I: [Co3(C51H66N3O16)]2(OAc), monoclinic, space group P21, a = 15.022(3), b = 14.242(3), c = 28.922(6) , β = 98.944(4)o, V = 6112(2) 3, Z = 4, Dc = 1.339 g/cm3, the final R = 0.0860 for 21906 observed reflections with I 2(I). For Ⅱ: Cu2[C24H58N4O7Cl]Cl, orthorhombic, space group P212121, a = 6.1861(13), b = 20.838(4), c = 28.274(6) , V = 3644.6(13) 3, Z = 4, Dc = 1.310 g/cm3, the final R = 0.0642 for 11106 observed reflections with I 2(I). The complexes were then used to catalyze the Henry reaction and catalytic activity determined by 1H NMR.     

A Novel Dinuclear Copper(Ⅱ) Complex: Synthesis,Crystal Structure,Properties and Hirshfeld Surface Analysis

A novel copper complex [Cu_2(L)(DMF)_2](1, H_4L =(1 Z,N?Z)-3,5-dibromo-N?-((3,5-dibromo-2-hydroxyphenyl)(hydroxy)methylene)-2-hydroxybenzohydrazonic acid which was synthesized by in-situ oxidation reaction derived from H_2hdb(H_2hdb = 6,6?-((1 E,1?E)-hydrazine-1,2-diylidenebis(methanylylidene)) bis(2,4-dibromophenol)) has been synthesized and characterized by IR, elemental analysis(CHN), TG and single-crystal X-ray diffraction. The single crystal belongs to monoclinic system, space group P21/c with a = 13.538(1), b = 3.912(1), c = 23.778(1) ?, β = 105.232(5)o, Mr = 857.08, V = 1214.9(1) ?~3, Z = 2, Dc = 2.343 g/cm~3, F(000) = 824, μ = 8.375 mm~(–1), R = 0.0566, and w R = 0.1610. Compound 1 displays weak anti-ferromagnetic interactions through a η~1:η~1:η~1:η~1:η~1:η~1:μ_2-L~(4-) bridging mode. Hirshfeld surface analysis revealed that complex 1 was supported mainly by Br···H and H···H intermolecular interactions.     

Synthesis and Characterization of Two Novel High Valent Dinuclear Complexes with a Triphenolate Ligand Bearing Functional Groups

Two novel high valent complexes [M2(III, III)L(p--OAc)2].PF6 (M=Mn, Fe; 9) were prepared, where L was the tri-anion of 2,6-bis{[(2-hydroxy-3-(morpholin-4-yl methyl)-5-tertbutyl benzyl)(pyridyl-2-methyl)amino]methyl}-4-methyl phenol which contained additional phenolic, tert-butyl and morpholin-4-yl methyl groups compared to its parent [Mn2(Ⅱ, Ⅱ)(bpmp)(μ-OAc)2]-ClO4 (10). These improvements decreased the difference between the new model and (Mn)4 cluster (OEC in nature).     

Synthesis and Biological Evaluation of Novel Isonucleosides with 1,2,4‐Triazole‐3‐Carboxamide

Novel 1,2,4‐triazole isonucleosides (1 and 2) were efficiently synthesized starting from D‐ribose and D‐xylose, respectively. The key steps were condensation of cyclic sulfate 8 with methyl‐1,2,4‐triazole‐3‐carboxylate and nucleophilic displacement of the tosylate 15 with methyl‐1,2,4‐triazole‐3‐carboxylate, respectively.     

Synthesis and Structure of a Dinuclear Copper(Ⅱ)-ditetrazolate Involving in situ Ligand Synthesis

The hydrothermal reaction of 1,2-dicyanobenzene with NaN3 in the presence of CuCl2, 2,2′-bipyridine and H2O affords a novel dinuclear copper(II)-ditetrazolate, [Cu(bpy)- (pdtz)]2 (Hpdtz = 5,5′-1,2-phenylene-ditetrazole, bpy = 2,2′-bipyridine). The pdtz ligand is generated in situ through Sharpless 2+3 cycloaddition reaction. Its crystal structure was deter- mined by single-crystal X-ray diffraction method. The crystal crystallizes in the monoclinic system, space group P21/n with a = 8.2096(16), b = 18.580(4), c = 11.838(2) , β = 103.12(3)o, V = 1758.5(6) 3, Z = 2, Mr = 863.83, Dc = 1.631 g/cm3, F(000) = 876 and μ = 1.272 mm-1. In this novel dinuclear structure, the pdtz ligand adopts a peculiar μ2-η1,η2 coordination mode.