一种新奇的d-f异双核配合物[Fe(phen)_3]_2[FeCe(tiron)_3]·6H_2O的水热合成、晶体结构和磁性

硝酸铁,硝酸铈,邻菲咯啉(phen)和钛铁试剂(Tiron)通过水热方法合成了一种d-f异双核配合物[Fe(phen)3]2[FeCe(tiron)3]·6H2O,tiron=C6H2O8S2。X-射线单晶衍射分析表明,晶体属立方晶系,P213空间群,晶胞参数为:a=2.19409(4)nm,V=10.5624(3)nm3,Z=4,F(000)=4648,R1=0.0451,wR2=0.1077,S=1.072。在具有C3对称性的[FeCe(tiron)3]6-单元中,Fe髥与6个酚氧配位形成一个反三棱柱配位多面体,Ce髥则与3个桥联的酚氧μ2-O和3个磺酸基的氧形成另一个与FeO6共用底面的反三棱柱配位多面体CeO6。配阳离子通过phen-phen之间的π-π相互作用和与配阴离子间的静电引力等作用组装成一种三角梅状准主/客体型的超分子。在2~300K温度范围内测试了配合物的变温磁化率,结果表明,Ce髥-Fe髥之间存在典型的反铁磁性相互作用。     

A three-dimensional framework structure constructed from 2-(2-pyridyl-N-oxide) ethylphosphonic acid and Nd(III)

A multistep synthesis for 2-(2-pyridyl-N-oxide) ethylphosphonic acid 6-H2 is described along with its spectroscopic (IR, NMR) data and a single-crystal X-ray diffraction structure analysis. Combination of the ligand with Nd(OH)3 results in the formation of a complex Nd(6-H)3. Single-crystal X-ray diffraction analysis reveals a three-dimensional crystal network generated by hydrogen-bonded chains along the crystallographic c axis. The hydrogen bonds are formed between phosphonic acid anion (6-H)(-1) protons on one chain and pyridyl N-oxide oxygen atoms in neighboring chains. The asymmetric unit contains 1/3[Nd(6-H)3] and there are two unique Nd(III) atoms, each with point symmetry. As a result, each Nd(III) ion is bound to six (6-H)(-1) ligands and the symmetry about the Nd(III) ion is octahedral with each vertex occupied by a phosphonate oxygen atom. The Nd-O bond lengths are essentially identical: Nd(1)-O(3), 2.336 (1) A; Nd(2)-O(4), 2.340 (1) A. The monoanionic ligand (6-H)(-1), therefore, serves to bridge the unique Nd(III) centers.     

Synthesis and Crystal Structure of Tetrabonzoato Bis （2－Aminothiazol） Dicopper（Ⅱ）

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＴｅｔｒａｂｏｎｚｏａｔｏＢｉｓ（２－Ａｍｉｎｏｔｈｉａｚｏｌ）Ｄｉｃｏｐｐｅｒ（Ⅱ）ＷａｎｇＤｏｎｇ－Ｍｅｉ；ＨｏｕＹｉ－Ｍｉｎ；ＹａｎｇＲｕｉＮａ；ＨｕＸｉａｏ－Ｙｕａｎ；ＸｕｏＢａｏ－...     

一维螺旋链状过渡金属-苹果酸配合物的合成、晶体结构及表征

本文用铜、邻菲咯啉、钼酸铵和苹果酸合成了1种新型配合物Cu₂(phen)₂( μ-O)₂Mo(C₄H₃O₅)₂·7H₂O(1,phen=1,10-邻菲咯啉,C₄H₃O₅^3-=苹果酸根阴离子),并对它进行了单晶X射线衍射,红外光谱,元素分析等表征。X射线衍射分析表明配合物为苹果酸和邻菲咯啉桥联形成的三核铜及钼中心的一维螺旋链状结构,并通过氢键自组装成三维超分子化合物。另外,对配合物的固态的固体荧光性能也进行了研究。     

Synthesis,Structure and Electrochemistry of Triruthenium Cluster Complex [Ru_3(μ_3- O)(μ-CH_3CO_2)_6(py)_2(PPh_2py)](PF_6)·CH_2Cl_2

1 INTRODUCTION The transition metal cluster complexes exhi- biting multistep redox processes have attracted more and more attention because of their potential applications in the areas of photonic and electronic devices[1～4]. The oxo-centered carboxyla…     

邻苯二甲酸根桥联镍配位聚合物的合成与晶体结构

合成了邻苯二甲酸根桥联镍配位聚合物{ [ Ni(phth) (phen) (H2O) ]·H2O}n(phth:邻苯二甲酸根二价阴离子;phen: 1, 10-邻菲咯啉),并得到了它的单晶.用X射线单晶衍射法测定了配合物的晶体结构.     

1，3，5－三咪唑基苯－醋酸锌配合物的合成、结构和离子交换性质研究

报道了一个由新型三角架配体1,3,5-三咪唑基苯（L）与Zn(CH_3COO)_2· 2h_2O组装得到的配合物：[Zn(L)_2(H_2O)_2]-(CH_3COO)_2·2H_2O (1)，用X射线 单晶衍射法测定了配合物的晶体结构，该晶体属单斜晶系，空间群P2_1/n，晶胞参 数a = 0.8339(1) nm, b = 1.2209(2) nm, c = 1.7565(3) nm, β = 94.880(3)° ，D_c = 1.383 g/cm~3, μ = 1.505 mm~(-1), F(000) = 1560, R_1 = 0.0429, wR_2 = 0.0713。配合物1具有二维层状结构，醋酸根阴离子位于层与层之间的孔 道中，并且可以被硝酸根离子交换。     

苯并18－冠－6与M2[Pt(SCN)6](M=Na,K)配合物的合成、结构

合成了苯并18－冠－6(B18C6)与M2[Pt(SCN)6](M=Na,K)的配合物：{[Na (B18C6)]6[Pt(SCN)6]}[Pt(SCN)6](SCN)2(1),[K(B18C6)]2[Pt(SCN)6]·4H2O(2). 通过元素分析、红外光谱、单晶X射线衍射进行了表征.1为单斜晶系、空间群R3^-, a=b=1.9933(3)nm,c=2.9760(6)nm,α=β=90°,γ=120°,V=10.240(3)nm^3,Z=3, Dcalcd=1.564g/cm^3,F(000)=4908,R1=0.0535,wR2=0.1030.2为三斜晶纱、空间群 P1^-,a=1.1692(3)nm,b=1.1853(4)nm,c=1.2381(5)nm,α=61.419(5)°,β=80.757 (8)°,γ=89.003(5)°,V=1.4836(9)nm^3,Z=1,Dcalcd=1.476g/cm^3,F(000)=666, R1=0.0696,wR2=0.1346.1由{[Na(B18C6)]6[Pt(SCN)6]}^4+配阳离子、[Pt(SCN)6] ^2-配阴离子和SCN^-阴离子组成。相邻{[Na(B18C6)]6[Pt(SCN)6]}^4+通过Na-O键 形成三维网状结构。[Pt(SCN)6]^2-和SCN^-仅起平衡电荷的作用.2由两个[K (B18C6)]^+配阳离子和一个[Pt(SCN)6]^2-配阴离子组成。相邻[K(B18C6)]2[Pt (SCN)6]离子对通过K－O键形成一维链状结构。     

三核铜(Ⅰ/Ⅱ)配合物[Cu(en)_2]·[Cu(pht)_2]_2的合成、晶体结构及与DNA相互作用的研究

报道了多核铜配合物[Cu(en)_2]·[Cu(pht)_2]_2(Hpht:苯妥英,即5,5-二苯基-2,2-咪唑烷酮;en:乙二胺)的溶剂热合成、晶体结构及其与DNA的相互作用.该晶体属三斜晶系,P_1~-空间群,晶胞参数:a=0.8453(2)nm,b=1.1878(3)nm,c=1.5674(4)nm,a=101.197(3)°,β=97.690(3)°,γ=103.283(3)°,V=1.476(6)nm~3,D_c=1.480 g/cm~3,Z=1,F(000)=679,μ=1.139nm~(-1),R_1=0.0402,wR_2=0.0962[I>2σ(Ⅰ)],GOF=1.035.XPS和X射线单晶衍射数据显示该配合物分子由混价铜组成,包括两个一价铜和一个二价铜,其中每个Cu(Ⅰ)分别与两个苯妥英配体提供的氮原子配位,N-Cu(Ⅰ)-N的夹角为177°,一个Cu(Ⅱ)与六个配位原子配位(CuN_4O_2),形成一个稍变形八面体结构.配合物与DNA相互作用研究表明,该配合物主要是以插入方式与小牛胸腺DNA结合.     

Synthesis, Crystal Structure and Photoluminescent Property of a Novel Disilver Complex with Pyrazinyl Oxime Ligand

<正>A novel binuclear Ag(I) complex [Ag_2(C_6H_6N_3O)_2(C_6H_7N_3O)_2]·2CH_3CN (1) was synthesized by the evaporation reaction of silver nitrate and (E)-1-(pyrazin-2-yl)ethanone oxime (HL). The complex was characterized by elemental analysis, IR spectrum and X-ray single-crystal diffraction analysis. It crystallizes in the monoclinic space group C2/c with a = 22.7089(3), b = 11.5443(7), c = 16.1468(4) , β = 127.7150(10)°, V = 3348.6(2) ~3, D_c = 1.675 g/cm~3, M_r = 844.42, Z = 4, F(000) = 1696.0, μ = 1.226 mm~(-1), the final R =0.0250 and wR = 0.070. The coordination around the silver(I) atom is a distorted trigonal-bipyramidal geometry involving one protonated pyrazinyl oxime ligand (HL), one deprotonated oxime ligand (L~-) and one CH_3CN solvate molecule in the asymmetric unit of complex 1.     

Synthesis and Crystal Structure of［Na（DB18C6）（H_2O）_2］_2Mo_6O_（19）·3DMF·2CH_3OH

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MOLECULAR STRUCTURE OF ORGANOLANTHANIDE COMPLEX [Li(THF)_4]_2[{ (η~5-CH_3C_5H_4)NdCl(μ_2-Cl)NdCl_2(η~5-CH_3C_5H_4)}_2(μ_4-O)]

<正> The crystal structure of the complex [Li(THF)4]2[{(η5-CH3C5H4)Nd-Cl(μ2-Cl)NdCl2(η5-CH3C5H4)}2(μ4-O)] has been determined by X-ray diffraction technique. The crystal is monoclinic of space group C2/c with a = 22. 740(7) ,b= 18. 319 (6),c=18. 330(6) A,β=93. 04(3)°,V = 7624. 93A3,Dc= 1. 55g/cm3,Z = 4,F(000) = 2800,μ=15. 02cm-1. The complex is consisted of two [Li(THF)4]+cations and one [{(η5-CH3C5H4)NdCl(μ2-Cl)NdCl2(η5-CH3C5H4)}2(μ4-O)]2-dianion. The two units [Cη5-CH3C5H4)NdCl(μ2-Cl)NdCl2(η5-CH3C5H4)] in the tetra nnclear-neodymium dianion are connected by a μ4-O bridge with the average Nd -μ4-O 2. 36(1) A ,Nd -C(ring) 2. 76(3)A,Nd-Cl 2. 823(7)A and Nd-μ2-Cl 2. 798(7)A.     

2,5-吡啶二羧酸及碳酸根构筑的三维Sm-Cu配合物的合成及晶体结构研究

<正>近年来,以多羧酸为配体的稀土-过渡金属配位聚合物由于其拓扑结构的多样性和在磁性、催化、化学吸附、光学性质和电子导体等方面的功能特性已经受到研究人员的广泛关注[1-5]。由于稀土元素与过渡元素相比较他们具有各自不同的配位模     

一维链状配位聚合物[Zn(tpa)(tripy)]n·nH2O的合成与结构表征

采用水热法合成了新的一维链状锌的配位聚合物[Zn(tpa)(tripy)]_n·nH₂O(tpa=对苯二甲酸,tripy=4′-(4-甲氧基苯基)-2,2′∶6′,2″-三联吡啶),通过红外光谱和元素分析对该配位聚合物进行了结构表征,用Ｘ射线单晶衍射测定了晶体结构。 结果表明,该配位聚合物属单斜晶系,P21/c空间群,a＝0.855 0(2) nm,b＝2.825 0(6) nm,c＝1.096 0(2) nm,β＝107.14(3)°,V＝2.529 7(9) nm³,Z＝4,D_c＝1.541 g/cm³,M_r＝586.88,F(000)＝1 208。 最终偏离因子R₁＝0.100 6,ωR₂＝0.264 8。 该化合物中Zn原子和2个对苯二甲酸酸根中的2个O原子和1个三联吡啶中的3个N原子配位。 相对于配体,该配位聚合物表现出明显增强的荧光发射性质。     

K_(4.5)Na_4(H_3O)_(3.5)[Ce(SiW_(11)O_(39))_2]·23H_2O的合成和晶体结构

合成了标题化合物K4.5Na4(H_3O)3.5 [Ce(SiW11O39)2]·23H_2O,用单晶X-ray 衍射方法测定了它的结构,该晶体属三斜晶系,空间群P,a=16.531(4) ,b=23.193(4),c=12.764 (2)?,α= 99.740(6),β = 91.90(1), γ = 94.84(1)°,V = 4801(2) ?3,Mr = 6180.91, Z=2,Dc = 4.276 g·cm－3,μ(MoKα)= 27.06 mm－1, F(000)= 5359, R = 0.0781 ,wR = 0.1838,I >2((I) 的可观察衍射点11936个。该分子是由2个α-SiW11O39结构单元通过1个铈离子联结起来,铈离子八配位,形成了1个畸变的十二面体结构,Ce-O键长2.39(2)～2.45(3) ?。在杂多化合物中,硅氧四面体的氧原子存在μ4-Oc和μ3-Oc的2种配位状态。     

Der Einfluss unterschiedlicher Trägheitsmomente auf die Thermodiffusion von H35Cl,D35Cl,H37Cl und D37Cl

The analysis of measurements of the thermal diffusion factor α in the systems H³⁵Cl/H³⁷Cl, D³⁵Cl/D³⁷Cl and H³⁵Cl/D³⁵Cl shows that α may be approximated by the expression α = C_m \frac{{m_1 ? m_2 }}{{m_1 + m_2 }} + C_\theta \frac{{\theta _1 ? \theta _2 }}{{\theta _1 + \theta _2 }}.     

Structure and Magnetic Property of an Oxygenand Carboxamide-bridged One-dimensional Iron（Ⅲ） Complex [Fe2（μ-O）（bpb）2]n

The structure of the title complex [Fe2(μ-O)(bpb)2]n (bpb 2=1,2-bis(pyridine-2carboxamido) benzenate) has been characterized by single-crystal X-ray diffraction analysis.The complex (C36 H24 Fe2N8O5,Mr=760.33) crystallizes in the monoclinic space group P2 1/c with a=8.4615(17),b=33.704(7),c=11.173(2),β=91.12(3)o,V=3185.7(11)3,Z=4,D c=1.585 g/cm 3,μ(MoK)=0.970 mm-1,F(000)=1552,R int=0.0381,the final R=0.0454 and wR=0.1114.The magnetic susceptibilities of the complex have been examined in the temperature range of 2-300 K.The magnetic data were fitted to give the parameters of J d=-77.7(9) and J c=-11.5(6) cm-1.     

Preparation of the hydrocarbon-soluble trifluoro complex LTiF3 with a β-diketiminato ligand

The β-diketiminato fluoride complex (LTiF₃) (1) (L = HC(CMeN(2,6-iPr₂C₆H₃))₂, “NacNac”) has been obtained using two synthetic routes, interaction of TiF₄ and NacNacK·2THF in toluene and interaction of LTiCl₃ and 3 equiv. of Me₃SnF in toluene. The trifluoro complex (LTiF₃) (1) is soluble in the non-polar solvents toluene and hexane and moderately active in polymerization of ethylene; the activity is higher than that of LTiMe₃ and comparable with that of the oxo-bridged complexes LTiCl(μ-O)₂TiClL and LTiMe(μ-O)₂TiMeL·toluene. Compound 1 was characterized by single crystal X-ray structural analysis, elemental analysis, NMR spectroscopy, and mass spectrometry. Complex 1 in the solid state is a centrosymmetric dimer containing two LTiF₂ moieties connected by two bridging fluorines, whereas C₆D₆ and CD₃CN solutions of 1 contain the monomeric complex at room temperature.     

Synthesis and Crystal Structure of a Two-dimensional Cobalt Complex with 5-Tert-butyl Isophthalic Acid

The self-assembly of Co(OAc)·4H2O with H2tbip and bipy (H2tbip = 5-tert-butyl isophthalic acid, bipy = 4,4'-bipyridine) generates one new complex, [Co3(tbip)2(Htbip)2(bipy)]n, which has been characterized by elemental analysis, X-ray diffraction, and IR spectroscopy. Single-crystal X-ray analysis reveals that it crystallizes in the triclinic space group P1 with a = 9.471(6), b = 12.597(8), c = 12.899(8), α = 84.660(7), β = 70.548(7), γ = 81.965(7)o, V = 1435.1(15)3, Mr = 1215.85, Dc = 1.407 g/cm3, Z = 1, F(000) = 629, μ(MoKα) = 0.926 mm-1, the final R = 0.0623 and wR = 0.1724. The complex consists of a tbip bridged trinuclear cobalt() unit and is further linked by 4,4'-bipyridine molecule to form a 2D supramolecular network.     

六核钴羰基簇的P(OC_2H_5)_3取代衍生物的合成、表征与结构

用P(OC_2H_5)_3与母体簇Co_6(μ_6-P)(μ-SCH_2CH_2CH_2S)(μ- PSCH_2CH_2CH_2S)(CO)_(12)进行取代反应得到一个二取代产物Co_6(μ_6-P)(μ- SCH_2CH_2CH_2S)(μ-PSCH_2CH_2CH_2S)(μ-CO)(CO)_9[P(OC_2H_5)_2]_2（I）, 同时还得到了两个一取代产物Co_6(μ_6-P)(μ-SCH_2CH_2CH_2S)(μ- PSCH_2CH_2CH_2S)(CO)_(11)[P(OC_2H_5)_3]（II a和II b,II b是II a的一个同 分异构体,其谱学数据与II a不同）。对合成的三个簇合物进行了元素分析、IR、 ~1H NMR、~(31)P NMR和MS谱学表征,对I做了X射线单晶衍射测定,其晶体属于单 斜晶系,P2_1/n空间群,晶胞参数：a = 1.1170(2) nm,b = 2.3554(5) nm,c = 1.7977(4) nm,β = 99.50(3)°,V = 4.6649(17) nm~3,Z = 4,D_c = 1.763 g/cm~3,F(000) = 2488,μ = 24.64 cm~(-1)。X射线晶体结构分析表明,取代 位置发生在簇合物顶端的两个钴原子上。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,最后的偏离因子为R_1 = 0.0497,wR_2 = 0.1386。