新马兜铃内酯的晶体结构

从绵毛马兜铃的根茎中分离出一种新的倍半萜内酯, 它的分子式由高分辨质谱数据确定为C~1~5H~2~0O~2, 它的结构用单晶X射线衍射法测定, 晶体属三斜晶系, 空间群为P1, a=0.6275(3)nm, b=0.8057(4)nm, c=1.3622(6)nm; α=88.78(4)°,β=91.44(4)°, γ=105.20(4)°; Z=2.3107。     

电子探针定量分析的标准样品——几种多元氧化物单晶

在很高的温度和适宜的生长条件下,分别采用熔盐籽晶法和高温引上法生长了高质量的YAP、NAB、KTP、LN、BBO、SBN等多元氧化物单晶,它们具有优良的物理化学性能,严格的化学比,固定的组成与结构以及较好的化学均匀性和电子束轰击下的稳定性。广泛地用于激光和非线性光学领域。我们选用这些晶体为原材料研制电子探针定量分析的标准样品。经过测量和标定,这些单晶标样符合中华人民共和国国家标准GB 4930-85(电子探针显微分析标准样品通用技术条件)的规定。含有稀土元素的标样如NAB和YAP能发出绿色荧光,是电子显微术中理想的阴极发光材料。     

THE FORMATION AND CRYSTAL STRUCTURE OF DIHYDRONITIDINE AND DISCUSSION OF ANTICANCER MECHANISM OF NITIDINE CATION

The paper reports the formation and crystal structure of dihydronitidine, expounds thereasons and conditions of easily formed oxynitidine, and discusses anticancer mechanism ofnitidine (cation). The crystallographic parameters of dihydronitidine are: space group P2_(1/n),a= 12.54(1), b = 9. 148(5), c = 14.748(8)A, β= 92. 12(6)°,Z =4. 4108 independent reflec-tions were collected within the range of 3°≤2θ≤54°, of which 2137 intensity data with I≥3σ(I) were used in the structural determination. The crystal structure has been refined byfull matrix least-square method to a final R of 0.050.     

ICP—AES法测定硼酸铝钇钕（NYAB）激光晶体中的Nd

应用ICP-AES法分析自倍频激光晶体(NYAB)样品中的Nd,在石墨坩埚中于500℃用NaOH熔融分解样品,方法的回收率为96%～105%,测定的相对标准偏差为1.42%,方法简便,可给出满意的分析结果。     

几种双核簇合物的EPR谱

本文报导了四个双铜,四个双钼簇合物的EPR谱。这些谱可分成两类:一种类似于单核化合物的EPR谱,谱参数与单核谱相近,但谱强度较单核谱弱,文中称之为“碎片型”;另一类的谱参数与双核偶合的体系相同,谱的强度与双核偶合程度有关、反映双核偶合成簇的性质,称之为“簇型”。两类谱受温度和溶剂的影响分别呈现正常与反常的顺磁性。本文对它们与簇合物结构-性质间的关系作了初步探讨。     

Synthesis of Cyanobenzaldehydes （m—,o—,p—）by Molecular oxygen Oxidation Methods

Cyanobenzaldehydes (m-,o-,p-) were synthesized by oxidation of corresponding tolunitriles with molecular oxygen,catalyzed by cobalt acetate and sodium bromide.     

Synthesis and Characterization of a Novel Biomaterial： Maleic Anhydride-modified Poly（dl-lactic acid）

A novel modified poly(dl-lactic acid) (PDLLA) was obtained by covalently grafting of maleic anhydride onto the backbone of PDLLA, attempting to improve PDLLA‘s hydrophilicity and cell affinity and to provide reactive groups for further chemical modification. FTIR, ^13 C NMR and DSC were used to characterize the maleic anhydride-modified PDLLA.     

An open chain product in the reaction of benzil with thiocarbohydrazide

An open chain compound was obtained by reaction of benzil with thiocarbohy-drazide in acidic condition. Its derivative, namely, benzil bis-(5-isopropylidene-3-thiocarbohydrazone) has been structurally characterized by X-ray single crystal diffraction method. Crystallographic data: C22H26N8S2, Mr=466.62, monoclinic, space group C2/c, a=12.215(3), b=11.473(2), c=17.032 (3)A, B=98.96(2)0, V=2357.7(9)A3, Z=4, Dc=1.32 g/cm3, F(000)=1040, u(Mo Ka)=2.43 cm-1. Final R=0.050, Rw=0.061 for 1103 unique and observed reflections with I> 3o(I). The effect of the structures on the formation of the open-chain intermediates during the cyclization of (2:2) Schiff base macrocyclic compound has been discussed and a possible mechanism for the ring closure has been suggested.     

QSAR Studies on the COX-2 Inhibition by 3,4-Diarylcycloxazolones Based on MEDV Descriptor

Selective inhibition of cyclooxygenase-2 (COX-2) might avoid the side effects of current available nonsteroidal antiinflammatory drugs while retaining their therapeutic efficacy. A novel variable selection and modeling method based on prediction is developed to construct the quantitative structure-activity relationships (QSAR) between the molecular electronegativity distance vector (MEDV) based on 13 atomic types and the biological activities of a set of selective cyclooxygenase-2 inhibitory molecules, 3,4-diarylcycloxazolones (DAA) plus indomethacin,naproxen, and celecoxib. Using multiple linear regression, a 5-variable linear model is developed with the calibrated correlation coefficient of 0.9271 and root mean square error of 0.17 in modeling stage and the validated correlation coefficient of 0.9030 and root mean square error of 0.20 in leave-one-out validation step, respectively. To further test the predictive ability of the model, 20 DAA compounds are picked up to construct a training set which is used to build a QSAR model and then the model is employed to predict the biological activities of the balance compounds. The predicted correlation coefficient and root mean square error are 0.9332 and 0.19, respectively.     

STUDIES ON cis-trans-ISOMERIZATION AND REACTION KINETICS OF A μ, η~2-VINYL LIGAND IN A TRIOSMIUM CLUSTER

The dihydride cluster H_2O_(s_3)(CO)_(10) reacts with ethyne to give a cis-adduct [O_(s_3)H(μ,η~2-CH=CH_2)(CO)_(10)]. The high deuterated cluster D_2O_(s_3)(CO)_(10), the reaction of D_2O_(s_3)(CO)_(10)with ethyne C_2H_2 to form the vinyl product cluster [O_(s_3)D(μ, η~2-CH=CHD)(CO)_(10)], and thereaction of H_2O_(s_3)(CO)_(10) with the deuterated ethyne C_2D_2 to form [O_(s_3)H(μ,η~2-CD=CDH)(CO)_(10)] have been reported primarily in this paper. The two cis-adducts undergo cis-trans-isomerization of μ,η~2-vinyl ligands under a small amount of the nucleophile pyridine. Usingthe combination of deuteration and dynamic ~1H,~2H NMR spectra, we report the experimen-tal evidence determined by the dynamic ~1H, ~2H NMR spectra, mechanism, and kinetic dataof the isomerization.