The Crystal Structure of N-Benzoyl-N''-(2-hydroxyethyl)-thiourea

Thiourea compounds are excellent agents of bioactive substance. A number of biological activities are associated with substituted thiourea derivatives. A survey of literature reveals that some work has been reported on benzoylthiourea, which has found plenty of applications as a facile and simple ligand in determination of trances of the transition metal and as an available starting material in preparation of a wide variety of metal complexes. In recent years,N-benzoyl-N'-(2-hydroxyethyl)-thiourea has attracted considerable attention as selective reagents for the liquid-liquid extraction and preconcentration of platinum group metals and its antifungle activity.As a part of our works in studying coordination behaviours of N-benzoyl-N'-(2-hydroxyethyl)-thiourea and its bioactivity, in view of these observations and in continuation of our previous works on it, the present work was reported on the crystal structure of N-benzoyl-N'-( 2-hydroxyethyl)-thiourea.The crystals structure in the monoclinic system and space group of P21/c of N-benzoyl-N'-(2-hydroxyethyl)- thiourea (C10H12N2O2S) was determined from single-crystal X-ray diffraction analysis, a = 17.083 (3) A, b = 4.5490 (10) A, c = 14.279 (3)A, a = 90.00°, a = 102.44(3)°, a = 90.00 °, Ⅴ = 1083.6 (4)A3, Z = 4, Dc = 1.375 Mg/m3, i (Mo Ka)= 0.280 mm-1, F(000) =472. The final R and u R are 0.0399 and 0.0881 for 783 observed reflections [Ⅰ＞26(Ⅰ)].Fig. 1 shows the molecular crystal structure of N-benzoyl-N'-(2-hydroxyethyl)thiourea indicating that the carbonyl and thiocarbonyl moieties are pointing in approximate opposite directions. The six atoms in the ring structure hydrogen bonded are almost in one plane. The N(2)-H proton pendant arm extends to the carbonyl oxygen atom, forms hydrogen bond between them.The existence of hydrogen bond in benzoyl-thiourea molecular six-membered ring structure has significant implications on coordination properties, suggest the possibility of intramolecular hydrogen bond controlled coordination behaviors of these potentially bidentate ligands. In the coordination compound reported by Bourne et al.,cis-bis(N-benzoyl-N'-propylthiourea)dichloroplatinum(Ⅱ), the two ligand molecules bind to Pt(Ⅱ)via the sulfur atoms only, the carbonyl oxygen atom being locked into hydrogen bond similar to that in the free ligands.     

武定恐龙化石的显微拉曼光谱研究

本文首次利用激光显微拉曼光谱、原子光谱和偏光显微镜等方法 ,对云南武定的恐龙化石进行了分析研究。实验发现 ,恐龙化石表面和截面的拉曼光谱 ,均为典型的方解石 (CaCO3 )晶体的拉曼谱 ,并未发现有其他成分的拉曼谱。原子发射光谱的分析结果表明 ,恐龙化石中的主要元素有Ca(>10 % ) ,其次是Si(5 0 % )和P(4 0 % ) ,还有Fe(1 0 % )等 ,但未发现铱、钍等稀有元素。由恐龙化石截面在偏光显微镜下的图像可以知道 ,恐龙化石表面层的成分主要是方解石晶体 ;内部的主要成分为方解石 (CaCO3 )晶体 ,此外还有纤维状一水二氧化硅 (分子式SiO2 ·nH2 O ,属非晶态 )等成分。激光拉曼光谱能快速无损地准确检测出恐龙化石的主要成分是方解石 (CaCO3 ) ,拉曼光谱对恐龙化石的分析结果与原子光谱、偏光显微镜的分析结果是一致的     

Potential of zero total charge of platinum single crystals: A local approach to stepped surfaces vicinal to Pt(111)

The electrochemical behavior of platinum single-crystal electrodes is revisited, with special emphasis on the determination of the potential of zero charge. We show that the measure of the charge displaced during CO adsorption allows the determination of the potential of zero total charge (PZTC). The estimation of the potential of zero free charge (PZFC) is discussed, with different degrees of approximation. The application of this methodology to the study of the PZTC of platinum stepped surfaces vicinal to Pt(111) reveals a marked decrease of the PZTC due to the introduction of surface steps. This effect is interpreted as the result of the existence of markedly smaller surface potentials localized on step sites. The importance of considering local aspects of the interface is emphasized with the use of N₂O reduction as a sensitive probe to the local structure of the surface. It is proposed that the different local maxima observed in the absolute value of the reduction current correspond to the local values of PZTC. It is shown that there is, in general, good agreement between the overall PZTC, obtained from the CO displacement, and that calculated from the local values inferred from the N₂O reduction. Further insight is obtained with the application of the laser-induced temperature jump method. This technique is useful to calculate the potential of maximum entropy of the double-layer formation. The resulting value of this potential for Pt(111) is discussed in the light of the PZFC value obtained from different approaches. For stepped surfaces vicinal to Pt(111), two local maxima in the entropy of the double layer are observed that are close to the local PZTC values estimated from the N₂O reduction. This result suggests the existence of cooperative effects in the organization of the water dipoles close to the electrode surface. Published in Russian in Elektrokhimiya, 2006, Vol. 42, No. 11, pp. 1275–1292. Based on the report delivered at the 8th International Frumkin Symposium “Kinetics of the Electrode Processes,” October 18–22, 2005, Moscow. The text was submitted by the authors in English.     

Habit modification of calcium carbonate in the presence of malic acid

The ability of malic acid to control calcium carbonate morphology has been investigated by aging calcium chloride solution in the presence of urea in a 90 °C bath. Malic acid favors the formation of calcite. A transition from single block to aggregate with special morphology occurs upon increasing malic acid concentration. The morphological development of CaCO₃ crystal obviously depends on the starting pH. CaCO₃ crystal grows from spindle seed to dumbbell in the pH regime from 7 to 11; while it evolves from spindle seed, through peanut, to sphere at pH=11.5. Both dumbbell and sphere consist of rods that are elongated along c-axis and capped with three smooth, well-defined rhombic {1 0 4} faces. A tentative growth mechanism is proposed based on the fractal model suggested by R. Kniep and S. Busch [Angew. Chem. Int. Ed. Engl. 35 (1996) 2624].     

Rakanmakilactones A-F, new cytotoxic sulfur-containing norditerpene dilactones from leaves of Podocarpus macrophyllus var. maki

Six new S-containing norditerpene dilactones, rakanmakilactones A-F (5-10), were isolated from the leaves of Podocarpus macrophyllus D. Don var. maki Endl., along with four known norditerpene dilactones (1-4). Their structures, stereochemistry and absolute configurations were determined by spectroscopic studies (HRMS, IR, ¹H, ¹³C and 2D NMR), and single-crystal X-ray analyses. Rakanmakilactones were found to have a cytotoxic effect against P388 murine leukemia cells.     

Catalytic Active Site for NO Decomposition Elucidated by Surface Science and Real Catalyst

Comprehensive studies combining surface science and real catalyst were performed to get further insight into catalytic active site and reaction mechanism for NO decomposition over supported palladium and cobalt oxide-based catalysts. On palladium single-crystal model catalysts, adsorption, dissociation and desorption behavior of NO was found to be closely related to the surface structures, the stepped surface palladium being active for dissociation of NO. In accordance with this result, the activity of powder Pd/Al₂O₃ catalysts for NO decomposition was directly related to the number of step sites exposed on the surface, suggesting that the step sites act as the catalytic active site for NO decomposition on Pd/Al₂O₃. NO decomposition over cobalt oxide was found to be significantly promoted by addition of alkali metals. Surface science study and catalyst characterization led to the same conclusion that the interface between the alkali metal and Co₃O₄ serves as the catalytic active site. From the results of in situ Fourier transform infrared (FT-IR) spectroscopy and isotopic transient kinetic analysis, a reaction mechanism was proposed in which the reaction is initiated by NO adsorption onto alkali metals to form NO₂⁻ species and then NO₂⁻ species react with the adsorbed NO species to form N₂ over the interface between the alkali metal and Co₃O₄.     

The Crystal Structure of Sr2TiSi2O8

Sr₂TiSi₂O₈ single crystals were grown by Czochralski pulling and from a high-temperature solution. X-ray diffractometry revealed the modulated crystal structure of Sr₂TiSi₂O₈ to belong to the 5D superspace group P4bm (−α, α, 1/2; α, α, 1/2) with α=0.3. Atomic positions, anisotropic displacement factors and positional modulation parameters for Sr₂TiSi₂O₈ are determined and discussed. The positional modulation is further investigated by electron diffraction and high-resolution transmission electron microscopy. In the latter experiments, the 2D modulation appears to be superimposed by some 1D modulation waves. This effect is discussed in terms of growth conditions.     

Ferrocene Compounds. XXXI. Structure of 3-Ferrocenylpropanoic Acid

The title compound was prepared by modified procedure and characterized by means of IR, [¹H] and [¹³C] NMR spectroscopy. The structure was also determined by a single-crystal X-ray diffraction (XRD). 3-Ferrocenylpropanoic acid crystallizes as orange prisms in the triclinic space group P with a = 7.645(1) Å, b = 7.953(1) Å, c = 9.961(1) Å, = 81.67(1), = 68.43(1), = 83.76(1), V = 556.3(1) ų, Z = 2, R = 0.0435. In the ferrocene skeleton, Fe-C distances are in the range 2.033(2)–2.052(2) Å and C C distances in the range 1.412(5)–1.431(3) Å. The angle defined by ring centers and Fe atom is 177.7(1). The cyclopentadienyl rings are twisted from the eclipsed conformation by 8.3(2) (average value). In the structure was observed strong intermolecular hydrogen bond of 2.670(3) Å forming cyclic dimers of the R₂ ² (8) type.     

P(St-co-MAA)乳液体系对CaCO3结晶的调控

大量研究表明, 有机/无机界面上的相互作用[1]是控制无机结晶的晶型、形貌、粒径等特征的决定因素. 本文利用乳液聚合方法合成了在诱导无机矿化后依然保持较为刚性界面的、能与无机离子作用的微球, 并在乳液中进行碳酸钙结晶实验, 用XRD, FTIR和SEM等手段对结晶进行了表征.