Synthesis and Crystal Structure of N-Phenylbis（ferrocenecarboxyl）imide

The ferrocenyl compound,N-phenylbis(ferrocenecarboxyl)imide (C28H23NO2Fe2,Mr=517.17),was synthesized and structurally characterized by means of X-ray single-crystal dif-fraction. It crystallizes in monoclinic,space group C2/c with a=21.374(14),b=10.430(7),c= 10.741(7) ,β=114.184(8)°,V=2184(2) 3,Z=4,Dc=1.573 g/cm3,F(000)=1064,μ(MoKα)= 1.355 mm–1,T=291(2) K,the final R=0.0548 and wR=0.1437 for 1524 observed reflections with I > 2σ(I). In this compound,the nitrogen atom links two ferrocenyl groups and one phenyl group forming a novel imido derivative.     

Hydrothermal Synthesis and Crystal Structure of a Highly Reduced Mixed Molybdenum-vanadium Polyoxometalate with Phosphorus-centered [Ni(phen)3]2H2·[PmoⅤ4MoⅥ4VⅣ6M2M44]5-·4H2O(M=0.78MoⅤ+0.22VⅣ)

Polyoxometalates(POMs0) containing Keggin moieties exhibit a wide variety of compositions and have considerable structrral versatility as well as important magnetic, optical,and catalytic proper-ties[1-6].     

Synthesis and axial ligation behaviour of sterically hindered Zn(II)-porphyrin liquid crystals

A new class of low melting liquid crystalline octaalkyloxyporphyrins have been synthesised. Their Zn(II)-complexes display an interesting ligation behaviour towards amines (of varying shapes and sizes), ascribed to the steric hindrance or hydrophobic pockets on both the faces of the porphryin as evidenced from the crystal structure of Zn(II)-octabutyloxyporphyrin.     

表面能与晶体生长/溶解动力学研究的新动向

界面现象使物质在结晶过程中出现了临界现象.但最近的研究指出在物质溶解过程中,在表面能量的控制下也存在着临界现象以及尺寸效应.实验发现,当晶体自身小到一 定的程度时(通常在纳米尺度上并和临界蚀坑的大小相近),在溶解过程中其速度会自发降 低,反应被抑制乃至停止.尽管在热力学上表面能的因素可以赋予小颗粒晶体较大的溶解度 ,但表面能却也能通过对临界条件的控制而使这些微粒在动力学上不被溶解.这个发现不仅 解决了纳米颗粒在水溶液中稳定性的问题,而且还从动力学的角度解释了生物矿物选择纳米 尺度作为其基本构成单元的原因.由于表面能和晶体生长/溶解的动力学有着密切的关系, 我们可以通过对表面能的调节来修改它们的动力学速度和晶体的形貌.反过来,也可以用动力学的方法来测定表面能及表面吸附/脱附常数等.相对于常规的界面研究手段,通过生 长和溶解动力学途径所得的数据有着很好的可靠性及重复性.我们认为,晶体生长和溶解的 动力学和表面能的研究相结合,不仅为界面研究提供了新的思路和方法,而且也会推动晶体生长和材料科学的发展.     

Bildung und Kristallstruktur eines dimeren sauerstoffverbrückten Titanaminobisphenoxides

Formation and Crystal Structure of an Oxygen Bridged Titanium Amino Bisphenoxide Di‐(μ‐oxo)‐titan‐bis[aminobisphenoxide] ( 3 ) was obtained by reaction of (i‐Prop)₂TiL* ( 2 ) {L* = O‐4, 6‐(t‐Bu)₂C₆H₂‐2‐CH₂‐[1, 4‐N₂C₅H₁₀]‐2'‐CH₂‐4', 6'‐(t‐Bu)₂C₆H₂O] with water in a molar ratio 1:1 in diethylether. Both i‐Propyl moieties are substituted yielding the dimeric oxygen bridged amino bisphenoxide complex. The six coordinate Ti atoms are a result of Ti—N and Ti—O interactions of the corresponding atoms of the amino bisphenoxide ligand and the bridging O atoms. The central planar Ti₂O₂ ring may be considered as the general structural feature of the title compound: Space group P1¯, Z = 1, lattice dimensions at —60°C: a = 11.6899(4), b = 11.7873(4), c = 12.6462(4) Å, α = 98.070(1), β = 99.660(1), γ = 95.343(1)°, R₁ = 0.0469, wR₂ = 0.1049, GooF = 0.939.     

A New Family of Binary Layered Compounds of Platinum with Alkali Metals (A = K,Rb, Cs)

By reacting platinum with alkali metals (A = K, Rb, Cs) a new family of binary alkali metal platinides has been synthesized and characterized by chemical analysis, X‐ray powder diffraction, thermal analysis (DTA and DSC), and magnetic measurements. All three compounds exhibit similar XRD‐patterns with strong reflections that can be indexed on the basis of a rhombohedral crystal system (K_xPt: a = 2.6462(1), c = 17.123(1); Rb_xPt: a = 2.6415(1) Å, c = 17.871(1) Å; Cs_xPt: a = 2.6505(1) Å, c = 18.536(1) Å; x < ½. The a lattice constant is independent on the alkali metal used and of value close to the Pt–Pt distance in NaPt₂ (2.645Å). The c parameter increases monotonically with the growing atomic radius of the alkali metal. The average structure of the alloys consists of cubic close packed layers of platinum atoms with layers of disordered alkali metals in between. For all compounds besides the strong reflections small satellites are observed which cannot be indexed together with the rhombohedral peaks in any rational 3‐dimensional lattice. However, these satellites can be indexed as incommensurate modulations within the ab plane (found propagation vectors k = (0.1011, 0.2506, 0) for Cs_xPt, and k = (0.0168, 0.2785, 0) for Rb_xPt).     

混合价聚十五钒酸盐[V_(15)O_(36)Cl](NH_4)_3Na_7·30H_2O的合成与晶体结构

以XRD法确定制得的标题晶体属空间群D_(3A)~3,a=13.111,c=11.130。结构由帕特逊-极小函数法结合差值法解出,经精修得一致性因子R_w=0.0344。晶胞中坐落在6m2特殊位置上的是包合1个Cl~-的聚十五钒酸根[V_(15)O_(36)Cl]~(10-),配合键价法确认这是四价钒占主导地位的一类特种混合价同多酸根。     

Synthesis and Crystal Structure of 3-Benzoyl-7,7-dimethyl-4-phenyl-2-phenylamino-4,6,7,8-tetrahydro-chromen-5-one

The title compound (C30H27NO3) was synthesized via a one-pot procedure starting from β-benzoylthioacetanilide, benzaldehyde and 5,5-dimethyl-1,3-cyclohexanedione, and its struc- ture was determined by single-crystal X-ray diffraction analysis. The crystal belongs to triclinic system, space group P, with a = 6.325(2), b = 11.243(3), c = 17.553(4) , α = 87.306(4), β = 80.822(4), γ = 77.798(4)°, V = 1204.2(5) 3, Z = 2, Mr = 449.53, Dc = 1.240 g/cm3, μ = 0.080 mm-1, F(000) = 476, the final R = 0.0459 and wR = 0.0970 for 2301 observed reflections with I > 2σ(I).     

晶种诱导Nonasil(HMI)的合成

以不同分子筛(Nonasil, MCM-22或MCM-49)为晶种, 在水热条件下以六亚甲基亚胺(HMI)为模板剂, 对纯硅沸石Nonasil(HMI)的合成进行了研究. 并且对各种合成参数, 包括晶种类型、硅源、晶化温度和Na+浓度等对Nonasil(HMI)合成的影响进行了探讨. 发现在适量的Na+存在条件下, 晶种的引入大大缩短了晶化时间; 不同类型的晶种对晶化速度有不同程度的提高. 特别是用异类晶种(如MCM-22或MCM-49)能够合成高结晶度的Nonasil(HMI).