尼龙1010骤冷退火样品的晶体结构

尼龙1010的晶体结构属三斜晶系.作者最近导出了X射线衍射法(WAXD)测定尼龙1010结晶度的公式,进而考查了等温结晶时结晶温度T_C对结晶度X_C、晶粒尺寸L_(100)和氢键面相对衍射强度R的影响.发现X_C和L_(100)均随T_C升高而增大,达196℃后又减小;而R与T_C的关系则相反,呈线性降低.结晶速率快有利于分子链在垂直于氢键面的(100)晶面生长,但R值却降低了.本文利用WAXD考查了尼龙1010不同骤冷退火条件样品的晶体结构.     

3,3,6,6-四甲基-9-邻氯苯基-1,8-二氧代-3,4,5,6,7,9-六氧化氧杂蒽的合成和晶体结构

标题化合物C23H25对O3Cl是由邻氯苯甲醛与5，5-二甲基1，3-环己二酮在N，N-二甲基甲酸腹中反应而得。结构通过单晶X-射线衍射法确定，其晶体属于单科晶系，空间群=1632。晶体结构用直接法解出，使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=0．054，Rw一0．063。在晶体结构中，吡喃环与苯环之间的两面角为92．43°。     

二(三甲硅基环戊二烯基)二氯合锆的合成和晶体结构

在 THF中 ,通过三甲硅基环戊二烯基锂与四氯化锆反应合成了标题化合物 ,经元素分析 ,IR和 1 H NMR谱表征了其结构 ,并用 X-射线衍射测定了晶体结构 ,该晶体属于三斜晶系 ,空间群为 P1 ,晶体学参数 :a=0 .6787(6) ,b=1 .2 92 4 (2 ) ,c=1 .30 34(2 ) nm,α=67.83(1 ) ,β=82 .50 (3) ,γ=75.64 (3)°,V=1 .0 2 5nm3 ,Z=2 ,Dx=1 .41 5 g· cm-3 ,μ=8.989cm-1 ,F (0 0 0 ) =448,R=0 .0 32。质谱研究表明 ,化合物在质谱过程中发生二聚 C*p2 ZrClZr C*P2Cl(C*P=C5H4Si Me3 )。     

Interaction of 4-Isopropoxalyl-1,5-diphenyl-2,3-dihydro-2,3-pyrroledione with Thiosemicarbazide: Synthesis and Crystal and Molecular Structure of (3aS*)(4R*)(6aR*)-4,6a-dihydroxy-4-isopropoxycarbonyl-1-thiocarbamoyl-3,5-diphenyl-1,3a,4,5,6,6a-hexahydropyrrolo[3,4-d]pyrazol-6-one

4-Isopropoxalyl-1,5-diphenyl-2,3-dihydro-2,3-pyrroledione reacts with thiosemicarbazide to form (3aS*)(4R*)(6aR*)-4,6a-dihydroxy-4-isopropoxycarbonyl-1-thiocarbamoyl-3,5-diphenyl-1,3a,4,5,6,6a-hexahydropyrrolo[3,4-d]pyrazol-6-one. The molecular and crystal structure of the latter was studied by single crystal X-ray diffraction.     

Synthesis and crystal structure of a new one-dimensional system with end-to-end single dicyanamide bridges between nickel(II) centres

The complex [Ni(tn)₂{N(CN)₂}]ClO₄ (tn=trimethylenediamine) has been synthesized and the structure has been determined. The complex forms a one-dimensional chain structure via the bidentate bridging ligand dicyanamide. A two-dimensional networks is formed via interchain hydrogen bond interactions.     

A Two-dimensional Lanthanide Coordination Framework with a New Amide-type Tripodal Ligand, 2,2′,2＂-Nitrilotris{[（2′- benzylaminoformyl）phenoxy]ethyl}amine

The La(III) complex with a new amide‐type tripodal ligand,2,2′.2″‐nitrilotris{[(2′‐benzylaminofomyl)‐phenoxylethyl)amine (L), was synthesized and characterized by X‐ray crystallographic analysis. Crystal data: C₄₈H_55.50LaN₇O_18.75, M_r=1169.40, monoclinic. space group, P2₁/n, a= 1.0644(3) nm. b=2.3889(5) nm, c= 2.1917(5) nm, β=90.65°, V=5.573(2) nm³, Z=1, D_c=1.394 g°cm^?3, R₁=0.0487, wR [1>2s?(I)]=0.1266. The results reveal that each La(III) ion binds to 9 oxygen atoms, three of which belong to carbonyl groups from three tripodal ligands and six to three bidentate nitrate groups and a two‐dimensional sheet of 4.8² networks is assembled by metal‐ligand coordination interaction. L, a heptadentate compound, merely acts as a tridentate bridging spacer due to its steric hindrance and links the La(III) ions as three‐connected nodes.     

界面作用对HDPE/POEg/CaCO_3三元复合材料韧性的影响

通过界面改性,制备了以CaCO3为核,马来酸酐接枝乙烯-辛烯共聚物弹性体(POEg)为壳的高密度聚乙烯(HDPEg)/弹性体(POE)/CaCO3的三元复合材料.由于“核-壳”结构的形成,弹性体和CaCO3表现出协同的增韧作用.同未经表面处理的CaCO3复合材料相比,在相同的CaCO3含量的情况下,表面处理的CaCO3由于与弹性体形成更强的界面粘结,使得三元复合材料的“脆-韧”转变发生在较低的弹性体含量.     

Synthesis and Structure of Ag_3PSe_4

The title compound Ag3PSe4 was synthesized by the reaction of Ag powder,P2Se5 and Se in a molar ratio of 1:1:1 at 500℃ and structurally characterized by X-ray crystallography.The crystal belongs to orthorhombic,space group Pmn21 with cell parameters:a=7.689(4),b=6.660(3),c=6.379(4)A,V=326.7(3)A^3,Z=2,Dc=6.816g/cm^3,Mr=670.42,F(000)=584,μ=31.302mm^-1,R=0.0606,wR=0.1289 and S=1.012,The 3-D structure can be regarded as constructed from the stacking of puckered Ag-P-Se honeycomb-like sheets along the c direction,in which the Ag,P and Se atoms are bonded to each other to form a chair-like six-membered ring,and the rings then build the sheets by sharing edges.     

Crystal and Molecular Structures of Two Derivatives of 1, 3a, 5-Trisubstituted-3a ,4,5,11-Tetrahydro-1,2,4-Oxadiazolino[5,4-d] [1, 5]Benzothiazepine

The structures of two derivatives of the title compound [C24H22N2OS, Mr = 386. 5 for (1); C25H22N2O3S, Mr = 430. 5 for (2)] were determined by using X-ray single-crystal strcuture analysis method. The final discrepancies are R = 0. 071 and 0. 077, respectively, for the reflections measured on a four-circle diffractometer. The space group for compound (1) is P bca with a=1. 6639(4), b=2.0286(3), c= 1.1742(1) nm, V = 3. 964(1) nm3, F(000) = 1632 e, Z=8; and (2) belongs to P21/n space group, and the cell dimensions are a=1. 1115(4), b=0. 8932(7), c=2. 186(3) nm, β=97. 52 (1)°? V=2.151(4) nm3, F(000) = 904 e, Z=4.The molecular backbones are very similar, each is a tricyclic system. The central seven-membered ring is in a twisted-boat conformation, and is cis-fused to 1,2,4-oxa-diazolino ring, while the latter moiety is in an envelope form. There are conjugated but non-coplanar effects in each structure. All bond lengths and angles in the molecules are normally acceptable. The crystal structure on the whol     

铁基超细粒子催化剂结构与还原行为的Mssbauer谱研究

铁基超细粒子催化剂具有优良的F-T反应性能。本工作利用原位Mssbauer谱辅以XRD技术研究了含有钾助剂的F-T合成铁基超细粒子催化剂的结构与还原行为,考察了催化剂组成和第二金属组分(Mn,Zn,Mg)的影响。“纯”铁超细粒子催化剂在氢气中很容易经Fe_3O_4还原为零价铁。第二金属组分的引入,一方面阻碍了催化剂的还原,另一方面稳定了Fe~(2+)的存在而使其成为还原的主要中间相,这有利于反应条件下形成类尖晶石结构的活性相。对于Fe-Mn催化剂,上述效应随锰含量的增加而更趋显著。铁基超细粒子催化剂在氢气中的还原能力依“纯”Fe>Fe-Zn>Fe-Mn>Fe-Mg的顺序递减,这在一定程度上反映了铁与第二金属组分之间相互作用的强弱。