Synthesis and Crystal Structure of [Copper(1,10-phenanthroline)_2(pyridine)]perchlorates

1 INTRODUCTIONThe molecular structures of five-coordinated copper (II) complexes show an extensive variability ranging from trigonal bipyramidal to square pyramidal stereochemistry, with most complexes displaying a structure which is intermediate between these two extremes[1,2]. Most crystal structures of 1,10-phenanthroline with copper (II) complexes are known, [Cu (phen)2X]Y, where X = Cl, Br, I, CN, NCS, H2O or thiourea and Y = perchlorate, nitrate, tetrafluoroborate, chloride o…     

具有非正规自旋态的氮氧自由基桥联双镍配合物的合成,…

合成了４种氮氧自由基桥联的五氟丙酸镍双核配合物［Ｎｉ（ｐｒｐｒ）２］２ＮＩＴＲ．ｎＨ２Ｏ对该配合物进行了元素分析和热重－热分析，测定了红外光谱、紫外－可见光谱、电子顺磁共振和摩尔导，讨论了配合物的结构，测量了［Ｎｉ（ｐｆｐｒ）２］ＺＮＩＴｐｈＣｌ．４Ｈ２Ｏ和［Ｎｉ（ｐｆｐｒ）２］ＺＮＩＴＰｈＯＭｅ．４Ｈ２Ｏ的变温磁化率（４－３００Ｋ），表明配合物具有非正规自旋态的Ｎｉ（Ⅱ）－Ｃｕ（Ⅱ）三核体系的地     

Synthesis and properties of the copper(Ⅱ) complexes with stable radical

Four novel copper(Ⅱ) complexes have been synthesized,namely Cu(hfac)2NITPhNO2 (1),Cu(hfac)2NITPhCH3 (2),Cu(pfpr)2NITPhNO2,(3) and Cu(Pfpr)2NITPhCH3 (4),where hfac= hexafluoro-acetylacetonate,pfpr=pentafluoropropionate,NITR.=2-R-4,4,5,5-tetraniethyl-4,5-dihydro-1H-imidazolyl-1-oxyl-3-oxide.(R=4-nitrophenyl,4-methylphenyl).These complexes were rharicter-ized by elemental analyses,IR,electronic spectra and molar conductance.The temperature-dependent magnetic susceptibility of complexes 1 and 3 have been studied in the 4 300 K range,giving I he exchange integral J=10.56 cm-1 for complex 1 and J =-30.9 cm-1 for complex 3.     

4-(4-N,N-二甲胺基)苯基-7,7-二甲基-5-氧代-3,4,5,6,7,8-六氢香豆素酮的合成和晶体结构

标题化合物C19H23NO3由4-N,N-二甲胺基苯甲醛、5,5-二甲基-1,3-环己二酮、麦氏酸在乙二醇中于80℃反应2.5小时而得。结构通过单晶X-射线衍射法确定,其晶体属单斜晶系, C19H23NO3,空间群P21, a = 9.364(2), b = 5.974(1), c = 15.731(3)?, b = 102.87(3)°, V = 857.9(3)?3, Z = 2, Dc = 1.213Mg/m3, μ(MoKa) = 0.082mm-1, F(000)=336。晶体结构用直接法解出,经用全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R=0.0521, wR=0.1392。在分子结构中,存在3个平面, C(10)~C(15)构成平面1,C(5)-C6)-C(8)-C(9)-O(2)构成平面2,C(1)-C(2)- C(4)-C(5)-C(9)构成平面3,平面1与平面2的最小二乘面的两面角为88.77°,平面1与平面3的最小二乘面的两面角为86.58°,平面2与平面3的最小二乘面的两面角为1.86°.     

Synthesis and Structure of the Manganese Complex with 2-Aminopyridine N-oxide

1 INTRODUCTIONMany complexes of 2-aminopyridine N-oxide (apo) have been characterized by infrared spectra, X-ray powder diffraction spectra, and by magnetic measurements and electronic spectra to liquid nitrogen temperature, but very few are on their crystal X-ray studies[1~3]. We have been studying complexes of pyridine N-oxide ligands containing a donor substitutes at the 2-position, in an attempt to broaden the range of N-oxide ligands complexes[4,5]. As continuing work of research on…     

Synthesis,Crystal Structures,Hirshfeld Surfaces,Thermo Characteristics and Solubility of Co-crystal of Buprofezin with Hydrofluoric Acid

A new kind of co-crystal of buprofezin(C(16)H(24)FN3OS) with hydrofluoric acid has been prepared through evaporation technique. It crystallizes in the triclinic space group P1, with a = 9.9733(8), b = 10.3460(9), c = 10.5739(12) ?, a = 68.655(9), b = 73.291(9), g = 66.738(8)o, V = 920.34(17) ?~3, Mr = 325.44, Dc = 1.174 g/cm^3, Z = 2, F(000) = 348, m = 0.190 mm^-1, the final GOOF = 1.042, R = 0.0485 and wR = 0.1167. Single-crystal X-ray diffraction, XRPD, DSC, TGA, Hirshfeld surface analysis, Raman spectroscopy and FT-IR were used to characterize the co-crystal. It has a twodimensional plane structure, and the intermolecular interactions of co-crystal are mainly H–F×××H, H–O×××H and H–O×××H. Thermology study further confirmed that co-crystal has stronger thermal stability and higher melting point than buprofezin, and it has stronger water solubility. The results show that this co-crystal is valuable for the study of residual activity and application effects of buprofezin.     

一个含铜(Ⅱ)四氮大环阳离子和锰(Ⅱ)一维链阴离子化合物{[Cu(trans[14]diene)SCN]2Mn(SCN)4(4,4''''-bipy)·4H2O}n的合成和结构

报道了一维化合物{[Cu(trans[14]diene)SCN]2Mn(SCN)4(4,4'-bipy)·4H2O}n(trans[14]diene为5,7,7,12,14,14-六甲基-1,4,8,11-四氮杂十四环-4,11-二烯,4,4'-bipy为4,4'-联吡啶)的合成、表征和结构分析.该晶体属三斜晶系,具有P1-空间群.α＝0.95920(10)nm,b＝1.06800(10)nm,c＝1.7316(2)nm,α＝84.400(10)°,β＝74.850(10)°,γ＝69.650(10)°,V＝1.6053(3)nm3,Z＝1,Dc＝1.365g/cm3,F(000)＝691,最终R[I＞2σ(I)]＝0.0474,R(全部)＝0.0625,GOF(F2)＝1.222.该化合物含[Mn(SCN)4(4,4'-bipy)n]2-链和两个[Cu(trans[14]diene)SCN]+阳离子.     

双自由基桥联双铜(Ⅱ)配合物的合成、结构、磁性和分子力学研究

合成和表征了双自由基桥联的双核铜配合物［Ｃｕ（ｈｆａｃ）_２］_２　ＰｈＢＮＭ,其中ｈｆａｃ为 六氟乙酰丙酮负离子,ＰｈＢＮＭ为２,５－二甲基－１,４－二（４,４,５,５－四甲基－３－氧化咪唑啉１－氧 基自由基）苯．配合物的晶体为单斜晶系, Ｃ２／ｃ空间群, ａ＝１．９０１２（４） ｎｍ, ｂ＝１．３７１８（３） ｎｍ, ｃ＝２．１６２ ０（４） ｎｍ,β＝９７．５５（３）°, Ｚ＝４． Ｘ射线衍射结果表明该配合物存在两种构象,其 比例为 ７：３．用分子力学 ＭＭＸ计算了这两种构象的能量分别为 Ｅ_１＝７４０ ｋＪ／ｍｏｌ,Ｅ２＝７７１ ｋＪ／ｍｏｌ．运用不同的自旋多重度作参数,通过ＣＮＤＯ／Ｋ对配合物中磁偶合体系的轨道能 量进行计算,当体系中成单电子为反铁磁偶合时,轨道能量较低,这与磁性测量及其理 论拟合结果一致。     

Synthesis, structure, magnetic properties and molecular mechanics study on the dinuclear copper (II) with biradical

Dinuclear copper complex with biradicals [Cu(hfac)2]2PhBNM(PhBNM = 2,5-bimethyl-1,4-bis(4,4,5,5-tetramethyllimidazoline-1-oxyl-3-oxide)phenyl,hfac=hexafluoroacetylacetonate) has been synthesized and characterized. It crystallized in the monoclinic system, with space group C2/c, a=1.9012(4), b=1.3718(3), c=2.1620(4) nm, β=97.55(3)°, Z=4. The X-ray structure analysis shows that the molecular structure consists of two kinds of conformations. The ratio of them is 7:3. The energy of two conformations, calculated with molecular mechanics, are different, E1=740 kJ/mol, and E2=771 kJ · mol-1. The CNDO/k results on the complex indicate that the orbital energy of low spin state is lower than that of high spin state, which correspond with the results of magnetic measurement.     

Synthesis and Crystal Structure of Dinuclear Zinc（II） Complex with 3—Me—N—oxopyridine—2—thiol

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｔｕｄｉｅｓｏｆｔｈｅｃｏｏｒｄｉｎａｔｉｏｎｃｈｅｍｉｓｔｒｙｏｆｚｉｎｃ(ＩＩ)ｈａｖｅａｒｏｕｓｅｄｍｏｒｅａｎｄｍｏｒｅｉｎｔｅｒｅｓｔｉｎｌａｓｔｄｅｃａｄｅｉｎｖｉｅｗｏｆｔｈｅｉｒｂｉｏｌｏｇｉｃａｌｍｏｄｅｌｉｎｇａｐｐｌｉｃａ ｔｉｏｎｓ[1 ,2 ] ａｎｄｓｏｌｉｄ ｓｔａｔｅｍａｔｅｒｉａｌｓ[3 ,4] .ＷｅｈａｖｅｂｅｅｎｉｎｔｅｒｅｓｔｅｄｉｎｔｈｅｓｔｕｄｙｏｆｔｒａｎｓｉｔｉｏｎｍｅｔａｌｃｏｍｐｌｅｘｅｓｏｆＮ ｏｘｏｐｙｒｉｄｉｎｅ 2 ｔｈｉｏｌ(…