The crystal and molecular structure of a valinomycin analogue cyclo[(D-Val-L-Lac-L-Ala-D-Hyi)2(D-Val-L-Lac-L-Val-D-Hyi)]. H2O(C50H82N6 O18.H2O)

The crystal and molecular structure of the valinomycin analogue, cyclo[(D-Val-L-Lac-L-Ala-D-Hyi)2(D-Val-L-Lac-L-Val-D-Hyi)] has been solved by x-ray direct methods using the "Shake and Bake" procedure. The crystals, grown from a mixture of octane/CH2Cl2, belong to space group P2(1) (Z = 4) with cell parameters a = 10.29, b = 32.08, c = 18.73 A, beta = 97.05 degrees, and contain two molecules per asymmetric unit. After anisotropic refinement the standard reliability factor was Rl = 0.058. The conformations of both independent molecules is similar to that observed for isoleucinomycin, cyclo[-(D-Ile-L-Lac-L-Ile-D-Hyi)3] [V. Z. Pletnev et al. (1980) Biopolymers, Vol. 19, pp. 1517-1534]. The structure has an asymmetric conformation stabilized by six intramolecular H bonds, five bonds being of the 4-->1 type and one bond being of the 5-->1 type. One water molecule is caged in the internal cavity of each cyclodepsipeptide. This conformation could represent an intermediate state between free and complexed forms of valinomycin.     

Hydrothermal synthesis and crystal structure study of two novel 3-D mellitates {Nd2[C6(COO)6](H2O)6} and {Ho2[C6(COO)6](H2O)6}

Two novel 3-D coordination compounds, Nd2[C6(COO)6](H2O)6(1)and Ho2[C6(COO)6](H2O)6(2), were hydrothermally synthe-sized from mellitic acid and neodymium perchlorate (or holmium perchlorate) in the alkaline aqueous solution and characterized with ele-mental analysis, TG, IR spectrum, and single crystal X-ray diffraction. The two compounds were isostructural and crystallized in the ortho-rhombic system, space group Pnnm, with a=1.3531 (4) nm, b=0.6687 (2) nm, c=1.0224(3) nm, V=0.92523(5) nm3, Z=4, D=2.630 g/cm3, F(000)=696.0, Goof=1.052. Final R indices [I 2Σ(I)]: R1=0.0195, wR2=0.0382 for 1; a=1.3411(2) nm, b=0.6586(1) nm, c=1.0116(2) nm, V=0.8935(3) nm3, Z=4, D=2.877 g/cm3, F(000)=724.0, Goof=1.061. Final R indices [I 2Σ(I)]: R1=0.0200, wR2=0.0479 for 2. In the two compounds 1 and 2, the mellitic acid ligand, in which all the carboxylate groups were deprotonated, had only one kind of coordination mode to bridge metal ions to form four-connected three-dimensional diamondiod networks.     

Phase Equilibrium of Ternary Systems LaX 3 C 18 H 16 N 3O 2Cl H 2O

Ａｎｔｉｐｙｒｉｎｅａｎｄｓｏｍｅｏｆｉｔｓｄｅｒｉｖａｔｉｖｅｓｃａｎｂｅｕｓｅｄｉｎｓｙｎｅｒｇｉｓｔｉｃｅｘｔｒａｃｔｉｏｎｏｆｔｈｅｒａｒｅｅａｒｔｈｉｏｎｓ．Ｓｏｍｅｏｆｔｈｅｉｒｒａｒｅｅａｒｔｈｃｏｍｐｌｅｘｅｓｓｈｏｗｔｈｅｌｕｍｉｎ...     

Synthesis and Crystal Structure of Europium Associate (C 34 H 54 N 2O 10 )[Eu(NO 3) 5]

Ｌａｒｉａｔｅｔｈｅｒｓａｒｅｒｅｃｏｇｎｉｚｅｄａｓｐｏｔｅｎｔｉａｌｃａｔｉｏｎｂｉｎｄｅｒｓ．Ｔｈｅｙｏｆｅｒｓｅｌｅｃｔｉｏｎａｎｄａｍｏｄｉｆｉｃａｔｉｏｎｆｏｒｔｈｅｃａｔｉｏｎｂｉｎｄｉｎｇａｂｉｌｉｔｙｏｆｔｈｅｐａｒｅｎｔｃｒ...     

La(C7H5O3)2·(C9H6NO)的合成及热化学研究

研究由七水氯化镧与水杨酸、8-羟基喹啉反应合成镧与水杨酸、8-羟基喹啉多元混合配合物,并对该配合物进行表征.测定该合成反应的标准摩尔反应焓以及配合物的标准摩尔生成焓.通过红外光谱、元素分析、摩尔电导率、差热热重分析以及化学分析等方法来确定配合物的组成.应用溶解量热法分别测定了七水氯化镧、水杨酸、8-羟基喹啉和配合物在298.15 K、混合量热溶剂(VDMFVEtOHVHClO4=110.5)中的标准摩尔溶解焓.通过设计热化学循环,根据盖斯定律计算了合成反应的标准摩尔反应焓以及配合物的标准摩尔生成焓.该配合物的分子式是La(C7H5O3)2·(C9H6NO).各物质的溶解焓分别为△sH(I○)mLaCl3·7H2O(s),298.15 K]=-96.45±0.18 kJ·mol-1,△sH(I○)m[2 C7H6O3(s),298.15 K]=14.99±0.17 kJ·ml-1,△SH(I○)m[C9H7NO(s),298.15 K]=-3.86±0.06kJ·mdl-1及△S(I○)m[La(C7H5O3)2·(C9H6NO)(s),298.15K]=-117.78±0.11kJ·mol-1.反应LaCl3·7H2O(s)+2C7H6O3(s)+C9H7NO(s)=La(C7H5O3)2·(C9H6NO)(s)+3HCl(g)+7H2O(1)的标准摩尔反应焓为91.57±0.33 kJ·mol-1.La(C7H5O3)2·(C9H7NO)(s)的标准摩尔生成焓为△sH(I○)m[La(C7H5O3)2·(C9H6NO)(s),298.15 K]=-2076.5±3.9 kJ·mol-1.     

Y(C_(16)H_(16)N_2O_2)(NO_3)_3(CH_3SOCH_3)的合成和晶体结构

合成了硝酸钇（Ⅲ）与双希夫碱Ｎ，Ｎ′－二亚水杨基乙二胺、二甲基亚砜的配合物〔Ｙ（Ｃ６Ｈ４ＯＨＣＨＮＣ２Ｈ４ＮＣＨＣ６Ｈ４ＯＨ）（ＮＯ３）３（ＣＨ３ＳＯＣＨ３）〕。ｘ—射线单晶结构分析表明该晶体属单斜晶系、空间群为Ｐ２１／ｎ，ａ＝０．９６３１（２）ｎｍ，ｂ＝１．６４１４（５）ｎｍ，ｃ＝１．６２０９（３）ｎｍ，β＝１０２．９８（２）°，Ｚ＝４，Ｄｘ＝１．６５３Ｍｇ·ｍ－３。Ｙ（Ⅲ）配位数为９，配位几何为畸变的单帽四方反棱柱，所有的配位原子均为氧原子，分别来自三个硝酸根，一个二甲基亚砜和二个双希夫碱，中心离子被双希夫碱桥联，组成一维无限长链。     

新型间硝基苯甲酸稀土配位聚合物[Nd2(C7H4O4N)7(H2O)4]n的水热合成和晶体结构

采用水热方法合成出一种新型的间硝基苯甲酸稀土配位聚合物[Nd2(C7H4O4N)7H2O]n,并通过元素分析、红外光谱、X射线单晶结构分析对该配位聚合物进行了表征.标题配位聚合物的晶体属于三斜晶系,P1空间群,晶胞参数a=0.9848(2)nn,b=1.131 4(2)nm,c=1.366 3(3)nm,α=69.22(3).,β=82.48(3).,γ=82.21(3).,V=1.4045(5)nm3,Dc=1.806g/cm3,Z=1.结构分析表明:标题化合物是由稀土金属Nd(Ⅲ)和间硝基苯甲酸组成的配位聚合物,此聚合物通过Ln-O-C-O-Ln形成无限一维链状结构,进一步又通过分子间氢键连接形成复杂的三维氢键网络结构.     

Crystalline and molecular structure of the K+-complex of meso-valinomycin, cyclo(-(D-Val-L-Hyi-L-Val-D-Hyi)3-).KAuCl4

Crystal structure of the complex of meso-valinomycin with KAuCl4 (C60H102N6O18KAuCl4) was determined using direct X-ray diffraction analysis. The conformational state of the complex is similar to that determined earlier for free meso-valinomycin. Characteristic of it is the centrosymmetric bracelet shape stabilized by six intramolecular NH...OC hydrogen bonds of 4 --> 1 type. The K+ ion is located in an inner negatively charged octahedral cavity formed by six carbonyl oxygen atoms of ester groups. The observed differences in conformational angles of the complex and free are caused by readjustment of the geometry of the ion-binding cavity to the size of the ion bound during complexation.     

Synthesis and Crystal Structure of a 4f-3d Complex [La(DMF)_6(H_2O)_3][Cr(CN)_6]·2H_2O

Ｒｅｃｅｎｔｌｙ ,ｔｈｅｒｅｈａｓｂｅｅｎｃｏｎｓｉｄｅｒａｂｌｅｉｎ ｔｅｒｅｓｔｉｎｌａｎｔｈａｎｉｄｅ(Ⅲ )ｈｅｘａｃｙａｎｏｆｅｒｒａｔｅｓａｎｄｔｈｅａｎａｌｏｇｏｕｓｃｏｂａｌｔ(Ⅲ )ａｓｗｅｌｌａｓｃｈｒｏｍｉｕｍ(Ⅲ )ｃｏｍｐｌｅｘｅｓｂｅｃａｕｓｅｏｆｔｈｅｉｒｐｏｔｅｎｔｉａｌａｓｃａｔａｌｙｔｉｃ ,ｓｅｍｉｃｏｎｄｕｃｔｉｖｅ ,ａｎｄｍａｇｎｅｔｉｃｍａｔｅ ｒｉａｌｓ[1～ 4] .Ｆｏｒｅｘａｍｐｌｅ ,ｍａｇｎｅｔｉｃｓｔｕｄｉｅｓｏｎａｓｅｒｉｅｓｏｆｔｈｒｅｅ ｄｉｍｅｎｓｉｏ…     

新型电荷转移配合物(C9H8N)10(NH4)3[Y(SiMo11O39)2]·20H2O的合成与表征

由三元杂多化合物 (NH4) 1 3 [Y(Si Mo1 1 O3 9) 2 ]· 36 H2 O与喹啉反应合成了电荷转移化合物 (C9H8N) 1 0(NH4) 3 [Y(Si Mo1 1 O3 9) 2 ]· 2 0 H2 O。采用元素分析、X射线粉末衍射、红外光谱、固体漫反射电子光谱进行了表征。结果表明 :喹啉通过 N原子结合质子形成阳离子与稀土杂多阴离子成盐 ,固体化合物中阴离子和阳离子之间存在较强的相互作用 ;化合物在光激发下发生分子内电荷转移 ,导致有机 C9H8N 大阳离子的氧化和稀土杂多阴离子的还原 ,标题化合物颜色由黄转变为深蓝色     

[Nd(PW11O39)(H2O)3](H2bpy)2·4H2O的水热合成及晶体结构

采用水热法合成稀土无机有机杂化化合物[Nd(PW11O39)(H2O)3 ](H2bpy)2·4H2O.采用NdCl3·6H2O,(NH4)3PW12O40·3H2O, 4,4'-联吡啶(bpy),和去离子水(摩尔比为4∶1∶4∶3900, pH=6)在130℃下进行水热反应3天,得到标题化合物的紫红色块状晶体,并进行了红外光谱分析,元素分析.用单晶X射线衍射法测得晶体结构,属三斜晶系,空间群为P-1,晶胞参数为a=1.18824(9) nm,b =1.35707(10)nm,c=1.77691(13)nm,α=71.551(2)°,β=82.478(2)°,γ=80.568(2)°.该晶体由无机的共价链∞1[Nd(PW11O39)(H2O)3]4- 和有机的二质子化的4,4'-联吡啶(H2bpy)2 及结晶水分子堆积而成的, 是一个新的稀土磷钨酸盐无机有机杂化化合物.     

一维链状镍配合物[Ni(C14H10N2O2)(Mf)]n的合成和晶体结构

合成了含水杨醛缩苯甲酰腙的一维链状镍配合物[Ni(C14H10N2O2)(Mf)]n(Mf=C4H9NO,即吗啡啉),通过元素分析,红外、电子光谱和X-射线单晶衍射进行了表征.晶体属单斜晶系,空间群为P21/c,a=0.9708(4)nm,b=1.4783(7)nm,c=1.2275(4)nm,β=95.728(14)°,V=1.7528(12)nm3,Z=4,Mr=384.07,Dc=1.455 g·cm-3,μ=1.129mm-1,F(000)=800,R=0.0759,wR=0.2155.中心镍离子与水杨醛缩苯甲酰腙配体提供的2个氧原子与1个氮原子以及1个配位吗啡啉的氮原子配位,形成了N2O2的平面四边形的配位构型.晶体内每个配合物分子通过分子间氢键与相邻另一个配合物分子缔合成一个沿c轴方向的一维链状结构,N…N氢键键长为0.3239(10)nm,N-H…N氢键键角为173.56 °.