Synthesis and Crystal Structure of Diethyl-2,6-dimethyl-3,5-diyl-(1-(2-chlorobenzoyl)-1H- pyrazole-3-diethyl-carboxylate)-pyridine

The reaction of hydrazine hydrate with a new α,γ-diketone ester 3, derived from the reaction of 2,6-dimethyl-3,5-diacetyl-pyridine 2 with diethyl oxalate in the presence of sodium ethoxide, afforded the pyrazole derivative 4. Treatment of 4 with 2-chlorobenzoyl chloride gave diethyl 2,6-dimethyl-3,5-diyl-（1-2（chlorobenzoyl）-1H-pyrazole-3-diethyl-carboxylate） pyridine 5. Fine crystal of 5 suitable for XRD analysis was obtained form recrystalization in ethyl acetate. The crystal belongs to the triclinic system, space group P1^-, with a = 1.0342（11）, b = 1.2211（12）, c = 1.5013（15） nm, α = 82.5190（10）,β = 85.7960（10）,γ = 85.3150（10）°, V= 1.8697（3） nm^3, Dc= 1.173 g/cm^3, μ = 0.219 mm^-1, F（000） = 684, Z = 2, the final R = 0.0720 and wR = 0.2211.

The First Example of a Supramolecular Structure Containing [2-(1H-Pyrazol-3-yl)-pyridine] Complex and both α-and β-Octamolybdates

The title compound, [Ni（C8N3H7）3]4[Mo8O26]2·6H2O 1, has been synthesized from the reaction of 2-（1H-pyrazol-3-yl）-pyridine （L） with （NH4）2MoO4·2H2O and NiCl2·6H2O. Elemental analysis, IR, UV spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure of the compound. Crystal data： C96H96Mo16N36Ni4O58, Mr = 4451.97, monoclinic system, space group P21/n, a = 20.846（5）, b = 14.825（5）, c = 23.122（5） A ,β= 91.594（5）°, V = 7143（3）A^3, Z = 2, F（000） = 4344, Dc = 2.070 g/cm^3,μ = 1.968 mm^-1, R = 0.0452 and wR = 0.1056 for 17102 independent reflections （Rint = 0.0442） and 11074 observed reflections （I 〉 2σ（I））. Structural analysis indicates that two kinds of octamolybdates （[α-Mo8026]^4- and [β-Mo8026]^4-） co-exist in the compound. This is the first example of a supramolecular structure containing L complex as well as both α- and β-octamolybdate clusters.

A New Zn(Ⅱ) Coordination Polymer Constructed from 4-(1H-pyrazol-3-yl)pyridine as Fluorescent Sensor for Fe^(3+)

A new Zn(Ⅱ) coordination polymer, [Zn(4-PP)(1,4-BDC)?(H_2O)]_n(1, 4-PP = 4-(1 H-pyrazol-3-yl)pyridine, 1,4-H_2BDC = 1,4-benzenedicarboxylic acid), has been synthesized and structurally characterized by single-crystal X-ray diffraction as well as elemental analysis, IR spectra, XRPD and TG. Structural analysis reveals that Zn(Ⅱ) ions are bridged by COO-from 1,4-BDC^(2-)to form a binuclear structure as the second building units(SBUs). Zn_2 clusters can be clarified as 4-connected nodes, so the framework of 1 can be considered as a 2 D(44?62)-sql sheet. Fluorescence measurements show that 1 has highly selective and sensitive detection of Fe^(3+) in water medium.

基于4-(1H-吡唑-3-基)-吡啶构筑的新型Zn(Ⅱ)配位聚合物的合成、晶体结构和性质研究

采用水热法,合成了一个Zn(II)配位聚合物[Zn3(4-PP)4(OH)2(SO4)2(H2O)2]n(1,4-PP=4-(1H-pyrazol-3-yl)pyridine),并用元素分析、红外光谱和X-射线单晶衍射对其进行了表征,测定了其热重性质和荧光性质。该配位聚合物1属于单斜晶系,P21/c群,其晶胞参数为:a=12.303(3)nm,b=6.0083(12)nm,c=25.308(5)nm,β=101.40(3)°,F(000)=1056,Dc=1.882 g/cm3,V=1833.8(6)nm3,Mr=1038.94,Z=2,μ(Mo Kα)=2.140 mm-1,R1=0.0672,wR2=0.1300。在该配位聚合物1中,金属锌(II)与SO2-4以及OH-形成纯无机的二维层状结构,而4-PP配体仅作为端基配体;二维结构进一步通过氢键的作用形成三维超分子结构。(CCDC:1007042)

新型混配配合物双(3,5-二甲基吡唑)和2,6-吡啶二甲酸合锌的合成及其晶体结构

合成了新型混配配合物双(3,5-二甲基吡唑)和2,6-吡啶二甲酸合锌(1),其结构经1H NMR,IR和元素分析表征。X-射线单晶衍射分析结果表明,1属单斜晶系,空间群C2/c,晶胞参数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=1.588g.cm-3,μ=1.424 mm-1,F(000)=872,差值电子密度最高和最低峰为293 e.nm-3和-279 e.nm-3。