A new one-dimensional [CuC16H18N4O4S]n(1) was synthesized by the self-assembly of a ligand 2,5-thiophenediformates, 3,5-dimethylpyrazole and copper(II), and characterized by elemental analysis, IR and single-crystal X-ray diffraction. 1 crystallizes in monoclinic, space group C2/c with unit cell parameters, a=18.6156(4), b=5.96110(10), c= 18.1598(4)Å, =115.467(2)°, Z=4, V=1819.37(7)Å3, Mr = 425.94, Dc = 1.555g/cm3, μ=1.345mm-1, and F(000)= 876. The final R and wR are 0.0328 and 0.0816 for 7611 observed reflections with I>2σ(I). 1 shows an infinite 1-D polymeric chain structure based on the repeated basic units Cu(II)(3,5-dimethylpyrazole)2(2,5-thiophene diformate). The Cu(II)center acts as the joint of the unit, and is coordinated in a slightly distorted octahedral geometry comprised of four O atoms from two different 2,5-thiophenediformate ligands and two N atoms of two trans 3,5-dimethylpyrazole ligands.
A Cu(II) complex of tetra(3,5-diphenyl pyrazole) [Cu(C(15)H(12)N(2))(2)Cl(2)](2) (1) was syn-thesized, and its structure was determined by single-crystal X-ray diffraction and further characterized by elemental analysis, NMR and IR. 1 belongs to the monoclinic system, space group P2(1)/c with a = 13.3780(5), b = 15.1392(6), c = 15.5923(6) angstrom, beta = 124.522(2)degrees, Z = 2 and V = 2601.86(17) angstrom(3). In 1, each Cu(2+) ion is coordinated with two N atoms from two tetra(3,5-diphenyl pyrazole) ligands and three Cl(-) anions to give a distorted square-pyramidal geometry, which is further linked through edge-sharing bridging by Cl(-) anions to form a centrosymmetric dinuclear structure.
A novel mixed-ligand Zn(Ⅱ) complex(1) with 2,6-pyridinediformicacids and bis(3,5-dimethyl pyrazole) was synthesized.The structure was characterized by 1H NMR,IR,elemental analysis and X-ray single crystal diffraction.1 belongs to monoclinic,a space group C2/c with a=13.976(5),b=9.541(3),c=14.238(7),α=90.000°,β=111.386(3)°,γ=90.000°,Z=4,V=1 767.8(12) 3,Dc=1.588 g·cm-3,μ=1.424 mm-1,F(000)=872.The summit value and minimum of difference of electron density were 293 e·nm-3 and-279 e·nm-3,respectively.
Co(Ⅱ) complex of dichlorides and bi(3,5-dimethyl pyrazole) was synthesized,its crystal and molecular structure was determined by X-ray singlecrystal diffraction method.A crystal of the said compound was monoclinic with a space group C 2/c,a = 14.992(7),b = 8.206(3),c = 24.179(11),α=90.00°,β= 95.35(3) °,γ=90.00°,Z=8,V= 2962(2)3,Dc= 1.445 g·cm3,μ= 1.504mm-1,F(000)= 1320.The summit value and minimum of difference of electron density were 636 and-883e·nm-3 respectively.
3,5-Diphenyl pyrazole was synthesized with its crystal and molecular structure determined by X-ray singlecrystal diffraction method.A crystal of the said compound was monoclinic with a space group C2/c,a=16.942(2),b=17.153(2),c=17.658(2),α=90°,β= 109.600(2)°,γ=90°,Z=16,V= 4834.4(12)3,Dc=1.555g/cm3,μ=0.073mm-1,F(000)=868.The summit value and minimum of difference of electron density were 147and-307e.nm-3 respectively.
Co(II) Complex of 2,6-pyridinediformates was synthesized.Its crystal and molecular structure was determined by X-ray single crystal diffraction method.A crystal of the said compound was monoclinic with a space group P 21/c,a=13.8584(11),b=10.0806(8),c=13.6858(10),α=90.00°,β=115.843(5)°,γ=90.00°,Z=4,V=1720.7(2)3,Dc=1.719g/cm3,μ=1.064mm-1,F(000)=908.The summit value and minimum of difference of electron density were 711 and-756e.nm-3 respectively.
Four pyrazoles and their new heterocyclic acylamide derivatives, which are 3,5- di- methylpyrazole, 5-methyl-3-phenylpyrazole, 3,5-diphenylpyrazole, 3-ethoxycarbonyl-5-phenyl- pyrazole, 2,5-bis(3,5-dimethylpyrazolyl-1-carbonyl)thiophene(L1), 2,5-bis(5-methyl-3-phenyl- pyrazolyl-1-carbonyl)thiophene(L2), 2,5-bis(3,5-diphenylpyrazolyl-1-carbonyl)thiophene(L3) and 2,5-bis(3-ethoxycarbonyl-5-phenyl-1-carbonyl)thiophene(L4) were synthesized, and their relevant structures were characterized by elemental analysis, MS, IR, 1 HNMR and 13CNMR spectra. Copyright CJI.
Novel Schiff base of disalicyl imine of open chain crown ether was synthesized by the condensation of the intermediate,2,2′-bi 1,2-bioxyethyl benzaldehyde and o-amino-p-methyl-phenol.The favorable conditions of preparing the intermediate were found,i.e.pH of reacting solution was 8,the reacting time was about 13 h,the reacting temperature was 70~80 °C and the mole ratio of salicylaldehyde to 1,2-dichroloethane was 2.5 to 1.The intermediate yield was 48.0%.The conditions of synthesizing the Schiff base were that the pH of reacting solution was 8,the reacting time was about 12 h,the reacting temperature was 80 °C and that the mole ratio of o-amino-p-methyl-phenol to the intermediate was 2.4 to 1.The yield was 78.5%.The novel Schiff base was characterized by elemental,UV,IR,()~1H NMR and()~(13)C NMR analyses.
Four novel 2,5-bis(3,5-disubstituded-pyrazolyl-1-carbonyl)thiophenes were synthesized by the reaction of 3,5-disubstituded-pyrazole(2a~2d) with 2,5-bis(chloroformyl)thiophene. 2 was prepared from β-diketone and hydrazine hydrate by cyclization. The structures were characterized by 1H NMR,13C NMR,IR,MS and elemental analysis.