新型手性二茂铁腙类环钯化合物的合成及其晶体结构

手性二茂铁腙类环钯化合物[(+)-(S)-2-(甲氧基甲基吡咯烷-1-基)-1-乙酰基二茂铁亚胺]在甲醇中与Pd(OAc)2和AcONa·3H2O经不对称环钯化反应合成了两个新型的双-醋酸桥环钯衍生物[syn-(+)-(Rp,S,S,Rp)-3和syn-(+)-(Sp,S,S,Sp)-3];syn-(+)-(Rp,S,S,Rp)-3或syn-(+)-(Sp,S,S,Sp)-3在甲醇中与NaNO2反应合成了两个新型的双亚硝酸桥平面手性环钯化合物[syn-(+)-(Rp,S,S,Rp)-4和syn-(+)-(Sp,S,S,Sp)-4],其结构经1H NMR,元素分析和X-单晶衍射表征。     

新型一维链状化合物N-(m-二茂铁苯基)甲酰胺的合成及晶体结构(英)

N-(m-ferrocenylphenyl)-formamide has been synthesized by the reaction of m-ferrocenyl-aniline with DMF, and characterized by elements analysis, IR, ¹H NMR, and X-ray structure determination. The crystallized was in the monoclinic, P2₁/c space group, with a=0.140 94(3) nm, b=0.102 87(2) nm, c=0.100 26(2) nm, β=104.85(3)° and final R indices [I>2σ(I)] R₁=0.072 7, wR₂=0.184 5. An infinite one-dimensional chain is formed by intermolecular hydrogen bonding N-H…O. Cyclic voltammetry was studied comparing with the parent compound (m-ferrocenylaniline). CCDC: 243511.     

N-二茂铁甲基乙酰胺的合成及其晶体结构

标题化合物(C13H15FeNO)由二茂铁甲酰肟与乙酸乙酯经一锅煮方法制得,其结构通过元素分析,1HNMR,13CNMR,IR和单晶X-射线衍射法确定,化合物具有一维无限链状结构。其晶体属正交晶系,Pbca空间群,M r:257.11,a=9.6101(19),b=9.2313(18),c=25.869(5),v=2295.0(8)3,z=8,D c=1.488Mg.m-3,u=0.71073,F(000)=1072,最终偏离因子为R=0.0517,wR=0.0877。     

对—乙酰苯基二茂铁的晶体结构

单取代二茂铁化合物,尤其是单取代芳基二茂铁化合物,当芳基为带有各种不同取代基苯时,中心铁原子的氧化还原电势会产生相应的变化,茂环上屹化学位移也明显地与Hammett常数相关。在对-乙酰苯基二茂铁的电化学研究中已经证明,它的氧化势     

缬氨醇衍生的手性二茂铁亚胺环钯化合物的合成及晶体结构

含氮配位基团的二茂铁衍生物的环钯化合物在有机合成、催化等领或有着重要的应用,尽管目前已经合成了从多的二茂铁环钯化合物,但其中绝大部分为外消旋体。二茂铁是引入平面手性的理想骨架,通过经典的拆分方法或利用光学纯的二茂铁配体进行不对称环钯化反应可得到具有平面手性的二茂铁环钯化合物,研究发现,利用平面手性的二茂铁环钯化合物与金属汞嘲、锡等的金属转移反应可方便地制备平面构型保持的手性环汞、环锡化合物;还可将它们用于外消旋氨基酸的手性拆分及催化不对称Claisen重排反应（ee值最高可达95％）。     

三脚架结构的多二茂铁基化合物的晶体结构和电化学性质

合成了含有多二茂铁基团的化合物,测定了化合物的晶体结构.化合物为三斜晶系,P-1空间群,晶胞参数a=0.917 44(18)nm,b=1.240 7(3)nm,c=1.504 3(3)nm,α=106.53(3)°,β=101.82(3)°,γ=106.80(3),°对氮原子而言,形成了三角架结构.     

某些有机锡二茂铁和有机胂二茂铁衍生物的合成、表征及晶体结构

N,N-二甲基氨甲基二茂铁的单锂化物与三苄基氯化锡反应,得到1-二甲氨甲基-2-三苄基锡二茂铁(Ⅰ);与二苄基二氯化锡反应,得到二苄基二[2-(二甲氨甲基)二茂铁基]锡(Ⅱ).1-二甲氨甲基-2-(二苯胂基)二茂铁经单锂化后,再与二苯基氯化胂反应,生成1-二甲氨甲基-2,5-二(二苯胂基)二茂铁(Ⅲ);在四甲基乙二胺存在下,1-二甲氨甲基-2-(二苯胂基)二茂铁经双锂化后,再与二苯基氯化胂反应,得到1-二甲氨甲基-2,5,1'-三(二苯胂基)二茂铁(Ⅵ).化合物-经元素分析和¹HNMR表征,还用X射线衍射测定了化合物的晶体结构.化合物晶体为三斜晶系,空间群P1,a=1.0548(2)nm,b=1.3622(3)nm,c=1.5846(3)nm,α=95.87(3)°,β=96.54(3)°,γ=107.67(3)°,Z=2.     

3-二茂铁基二氢吡唑衍生物的合成及晶体结构

以乙酰基二茂铁为原料合成了6种二茂铁取代的4,5-二氢吡唑化合物,用IR、MS、1H NMR测试技术对其结构进行了表征,并采用X射线衍射方法测定了化合物2b的晶体和分子结构。C30H26Fe2N2O(化合物2b)属于三斜晶系,空间群P1,晶胞参数：a=0.9275(4) nm,b=1.1327(5) nm,c=1.1912(5) nm,α=88.67(2)°,β=79.925(18)°,γ=70.345(18)°,V=1.1595(9) nm3,Z=2,F(000)=560,Dc=1.553 g/cm3,μ=1.279 mm-1,R1=0.0351,wR2=0.0934。     

E-苯甲酰二茂铁亚胺的合成、晶体结构和反应性

由苯甲酰二茂铁和一系列伯胺出发,用4A分子筛作为催化剂合成了6种相应的E-构型亚胺化合物,产率为50%～85%.该方法具有很好的通用性,同时适用于芳胺和脂肪胺,并且对杂原子具有耐受性.与文献中使用Al2O3作为催化剂的方法相比,该方法可使反应时间和催化剂的活化时间均大大缩短.所合成的席夫碱用于探索生物碱(一)-Sparteine促进的对映选择性地合成平面手性二茂铁中的反应性.根据所测定的化合物3d晶体结构数据,分析了这类化合物反应活性低的原因是空间位阻所致.而空间位阻较小的二茂铁醛亚胺用于该反应能够顺利进行.     

二茂铁磺酰基苯并咪唑衍生物的合成、表征及晶体结构

以苯并咪唑为原料，经硝化、二茂铁磺酰化，合成了六种未见报道的二茂铁磺酰基硝基苯并咪唑衍生物，其结构经元素分析、质谱、核磁共振确证。由于苯并咪唑的互变异构，经二茂铁磺酰化后，产生两个异构体，通过X射线衍射，测定了异构体的晶体结构。     

Synthesis and structures of new helical, nanoscale ferrocenylphenyl amides

Two novel ferrocenylphenyl-containing amides have been synthesized by reaction of ferrocenylbencarboxylchloride and 1, 2-di-(o_aminophenoxy)ethane. A single crystal X-ray analysis shows that compound 3 crystallizes in the triclinic system, space group P-1, and compound 4 crystallizes in orthorhombic system, space group Pca2₁. There are intramolecular H-bonds in both the compounds, two H-bonds in compound 3 and one in compound 4. The dihedral angels of Cp-ring and phenyl ring range from 3.8° to 20.8°. Translated from Chemical Research and Application, 2006, 18(2) (in Chinese)     

一维链状银配合物的合成及晶体结构

The complex [Ag(L)]NO₃ (1) [L=1,5-bis(imidazol-1-yl)pentane] was synthesized in ethanol and water, and characterized by elemental analysis and X-ray crystal structural analysis. The result shows that the complex crystallizes in monoclinic, space group P2₁/c with a=0.695 7(4) nm, b=0.988 7(4) nm, c=1.974 8(7) nm, β=91.934(19)°, V=1.357 5(10) nm³, Z=4, D_calc=1.831 g·cm^-3, F(000)=752, μ=1.50 cm^-1, the final R=0.036 6, wR=0.091 0. The coordination environment of Ag(Ⅰ) is nearly linear with two N atoms, and each L ligand links two Ag(Ⅰ) atoms using its two imidazolyl N atoms to generate an infinite one-dimensional (1D) chain structure. The 1D chains are further connected by C-H…O hydrogen bonds to give a three-dimensional structure. CCDC: 609514.     

Hydrides,Amides and Imides Mediated Ammonia Synthesis and Decomposition

Ammonia is feeding nearly half the world population and also holds the promise as a carbon‐free energy carrier. The development of ammonia synthesis and decomposition processes under milder conditions is a grand challenge for more than a century. Increasing effort is devoted to this area in recent years and encouraging progress has been achieved. In this paper, we summarize our recent research using alkali or alkaline earth metal amides, imides and hydrides for ammonia synthesis and decomposition. These materials could serve as either indispensible component of active center in thermal catalytic process or nitrogen carrier for chemical looping ammonia synthesis. The synergy of amide, imide, or hydride with transition metals enables ammonia synthesis or decomposition with unprecedented high efficiency under milder reaction conditions, and thus opens an avenue to advance the chemistry or catalysis of N₂ fixation reaction. The compositional and structural diversity of the amide, imide and hydride materials provides plenty of opportunity and potential for further exploration and optimization.     

One-pot Synthesis and Crystal Structure of （1S,2R,3S,4R,5S）-1-Phenyl-2,4-dibenzoyl-3,5-difurylhexanol

(1S,2R,3S,4R,5S)-1-Phenyl-2,4-dibenzoyl-3,5-difurylhexanol 1 was synthesized by one-pot reaction of hypnone and furfurol in alkali H2O/EtOH solution and structurally defined to contain a chair-formed aliphatic carbocycle, on which the bulky substituents occupy the equatorial positions.     

Hydrothermal Synthesis and Crystal Structure of a New Sandwich—type Molybdenum Phosphate

1 INTRODUCTION The synthesis of porous and open-framework transition metal phosphates has received great in- terest due to their various compositions and topolo- gyies, as well as their useful properties such as con- trollable size- and shape-selectivity, rigid frame- works and chemical/thermal stability[1]. Of these phosphates constructed from oxometal polyhedra and PO4 tetrahedron, the most interesting is the [MoV6P4X31]n－ (X=O, OH) family with the dimen- sionalities ranging from …     

Synthesis and Crystal Structure of (E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl Propionate

(E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl propionate (C22H27O6N, Mr = 401.45) has been synthesized by a condensation reaction of paeonol with tyrosin methyl ester hydrochloride, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 11.91291(15), b = 9.49947(12), c = 19.8727(3) , β = 106.1104(15)°, V = 2160.60(5)3, Z = 4, Dc = 1.234 g/cm3, μ = 0.739 mm-1, F(000) = 856, R = 0.0466 and wR = 0.1461 for 3859 observed reflections with (Ⅰ> 2σ(Ⅰ)). In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking enantiomers, and such units are linked by intermolecular O(5)-H(5)…O(1) and intramolecular N(1)-H(1)…O(1) hydrogen bonds.     

希夫碱N,N′-双水杨醛缩连氮的合成与晶体结构研究

由水杨醛与水合肼反应生成希夫碱N ,N′ 双水杨醛缩连氮 ,并用溶液法生长其单晶。X 射线单晶结构分析表明 ,此晶体属于单斜晶系 ,P2 ( 1) /n空间群 ,晶胞参数为 :a =8.4 97( 4 ) ,b =6 .2 90 ( 3) ,c =11.789( 5 ) ,β=10 7.874 ( 7)° ,V =5 99.6 ( 4 ) 3 ,Z =2 ,Dc =1.331g·cm-3 ,F ( 0 0 0 ) =2 5 2 ,结构偏离因子R =0 .0 4 6 9,wR2 =0 .110 8。晶体中一个分子羟基上的氧原子与另一个分子中 -CH =N -上的氢原子之间形成分子间氢键 (O┄H -C)。     

Synthesis and Crystal Structure of a New Complex （H3IDC）（Prz）0.5（H2O）

The compound （H3IDC）（Prz）0.5（H2O） （H3IDC = imidazole-4,5-dicarboxylate, Prz = piperazine） has been prepared from a hydrothermal approach and was characterized by IR analysis and X-ray diffraction. Its crystal structure consists of discrete 4,5-imidazole-dicarboxylate, H2O and piperazine molecules. The whole structural motif was assembled by three different non-covalent interactions of O-H…O, N-H…O and π-π stacking, which play an important role in packing the molecules. Interestingly, the connections between imidazole-4,5-dicarboxylate molecule and water molecule result in a helical polymeric chain. Crystal data for compound 1： monoclinic system, space group P21/c, a = 6.4600（13）, b = 19.910（4）, c = 6.9123（14） A^°, β = 94.26（3）°, V= 886.6（3） A^°^3, Z= 4, C7H10O5N3, Mr = 216.18.     

Synthesis, Characterization, and X-Ray Diffraction Analysis of Triethylenetetraammonium Tetrathiomolybdate

The reaction of gaseous H₂S with aqueous ammonium heptamolybdate in the presence of triethylenetetramine (trien) gave a red complex. The complex was recrystallized in hot water and characterized by element analysis and UV, visible, IR, and ¹H NMR spectroscopy. PMR has revealed accidental magnetic equivalence, resulting from the proximity of [MoS₄]^2- species in one complex molecule to the open triethylenetetramine ligand of another molecule. (TrienH₂)[MoS₄] crystallizes in the orthorhombic crystal system, space group Pca2₁, a=13.045(2), b=16.461(3), c=13.754(2) , =90, =90, =90°, V=2953.5(9) ³, Z=8, R₁=0.0323, wR₂=0.0730. The structure consists of the tetrahedral tetrathiomolybdate anions, forming an extended 3D framework in solids due to the interactions with triene cations via Mo-S...H-N hydrogen bonds.     

Synthesis, Characterization and Fluorescence of a One-dimensional Cadmium（Ⅱ） Compound Involving Covalent and Hydrogen Bonds

1 INTRODUCTION The rational design and synthesis of new metal- organic coordination polymers have generated con- siderable interest in supramolecular chemistry and material science owing to their intriguing structural diversities and potential applications as functional materials[1～3]. Molecular self-assembly has been pro- ved to be an efficient way to construct various inte- resting coordination polymers[4～6]. The coordina- tion covalent bond, hydrogen bond or other mole- cular interact…