Synthesis, Crystal Structure and Thermal Stability of Complex Na_3[Na_5(dhns)_2]·(phen)_4·2H_2O with Bihydroxynaphthalenedisulfonate

2,7-二羟基萘-3,6-二磺酸二钠盐(nA2H2dHnS)与邻菲罗啉在乙醇/水溶液中自组装得到一新的配合物nA3[nA5(dHnS)2]·(PHEn)4·2H2O(1),并用CHn元素分析、Ir、TgA和X-射线单晶衍射分析进行了表征。晶体属正交晶系,PnA21空间群,A=2.829 85(12)nM,b=1.038 99(14)nM,C=2.259 23(13)nM,V=6.642 6(10)nM3,z=4,dC=1.573 g.CM-3,r1=0.050 6,Wr2=0.124 0,S=1.05。A new complex,Na3[Na5(dhns)2]·(phen)4·2H2O,was obtained from the self-assembly of disodium 2,7dihydroxy-naphthalene-3,6-disulfonate(Na2H2dhns) and 1,10-phenanthroline(Phen) in a water-ethanol solution.The compound was characterized by elemental analysis,IR,TGA,and X-ray diffraction single crystal structure analyses.The compound crystallizes in the orthorhombic system,space group Pna21,a=2.829 85(12) nm,b=1.038 99(14) nm,c=2.259 23(13) nm,V=6.642 6(10) nm3,Z=4,Dc=1.573 g·cm-3,R1=0.050 6,wR2=0.124 0,S=1.05.CCDC: 881794.福建省教育厅科技基金(No.JA08212); 福建省科技厅科技项目(No.2008F5053)资助项

VPO催化剂前驱体的溶液法合成和结构研究

VPO polymer β NH 4(VO 2)(HPO 4) was synthesized from the mixture of NH 4VO 3 and NH 4H 2PO 4 in aqueous acidic solution. This hydrogenphosphate vanadate crystallizes in the orthorhombic space group Pbca with a=0.680 60(8) nm, b=0.925 70(5) nm, c=1.773 70(2) nm, V=1.117 5(3) nm 3, Z=8, D c=1.743 g·cm -3 , μ=88.54 cm -1 and R=0.051. The structure is built up from VO 5 square pyramid linked by trans vertices through the bridged oxygen atom to form an one dimensional isolated chain of {VO 2HPO 4} n- nunning along the a axis

Synthesis and Crystal Structure of Porous Zinc(Ⅱ) Coordination Polymer{[Zn(L)_2(H_2O)_2]·H_2O}_n Constructed by Isonicotinoylhydrazone Ligand

以邻甲酰基苯磺酸钠和异烟肼为原料在乙醇/水溶液中制备了一种酰腙类SCHIff碱配体(nAl),采用常规溶液挥发法合成了由该配体构筑的zn((Ⅱ)配位聚合物{[zn(l)2(H2O)2]·4H2O}n。利用元素分析、Ir、TgA和X-射线单晶衍射分析对配合物进行了表征。配合物晶体属三斜晶系,P1空间群,晶胞参数A=0.786 98(4)nM,b=0.869 26(5)nM,C=1.180 44(7)nM,α=103.353(5)°,β=100.965(4)°,γ=93.123(4)°,z=1,V=0.767 24(7)nM3,dC=1.697 g·CM-3。每个zn(Ⅱ)离子被2个配体l-阴离子双重桥联形成二核环状结构单元,并通过共用锌离子形成一维链配位聚合物,链与链之间通过氢键扩展为具有一维开放孔道的三维超分子网络结构。An acylhydrazone-type Schiff base ligand(NaL) was synthesized by reaction of sodium 2-formylbenzene sulfonate with isoniazide in a mixture of ethanol and water.A Zn(Ⅱ) coordination polymer {[Zn(L)2(H2O)2]·4H2O}n have been synthesized by employing the solution preparation method at room temperature and characterized by elemental analysis,IR,TGA and X-ray diffraction structural analysis.Crystal data:triclinic system,space group P1,a=0.786 98(4) nm,b=0.869 26(5) nm,c=1.180 44(7) nm,α=103.353(5)°,β=100.965(4)°,γ=93.123(4)°,Z=1,V =0.767 24(7) nm3,Dc=1.697 g·cm-3.Each Zn (Ⅱ) ion is bridged by two L-ligands in the monodentatemonodentate mode to form a ring-like dimer units,and a one-dimensional chain is built by sharing a Zn (Ⅱ) ion between the units.The adjacent chains are linked into a 3D supramolecular network structure via hydrogen bonds and π-π interactions with a 1D open channel that are occupied by solvent molecules.CCDC:934292.泉州师范学院学科建设资金; 国家级大学生创新创业训练计划项目(No.201310399018)资

Synthesis and Crystal Structure of a Novel Self-assembled1,4-dimethyl Cucurbituril Silver(I) Complex

Crystals of a new 1,4-dimethyl cucurbituril(TMeQ6) with Silver(I) ion were synthesized, and the structure was determined by X-ray diffraction technique. There are two kinds of TMeQ6 A and B which formed molecular encapsulates with two silver ion lids in the self-assembled entities. One dimensional supramolecular tubes are formed from the encapsulates A, and two dimensional molecular sieves are formed from the encapsulates B, the tubes and the sieves stack together alternately in the self-assembled entities. CCDC: 271401.国家自然科学基金资助项目(No.20362003);; 科技部国际科技合作重点项目计划(No.2003DF000030);; 贵州省省长资金项目;; 贵州省国际科技合作重点项目计划(No.2005400101

A Molecular Bowl with Barium Ion As Bottom

A molecular bowl with barium ion covering one portal of decamethylcucurbit[5]uril as a‘metal-ion- bottom’has been synthesized. The structure of the molecular bowl has been confirmed by the single crystal X-ray diffraction determination. It belongs to orthorhombic with space group of Pna21. The crystal unit cell parameters are: a=3.2108(6) nm, b=1.4742(3) nm, c=1.1516(2) nm, and V=5.4509(18) nm3, Dc=1.677 Mg·m-3, Z=4, F(000)= 2832, R=0.0551, wR=0.1568. CCDC: 290552.国家自然科学基金资助项目(No.20362003);; 科技部国际科技合作重点项目计划(No.2003DF000030);; 贵州省省长资金项目;; 贵州省国际科技合作重点项目计划(No.2005400101)

Study of the Interaction of Disubstituted Cucurbit[6]uril with 2-(Aminomethyl)pyridine

分别用核磁共振、紫外可见吸收和X射线单晶衍射方法研究对称四甲基六元瓜环与2-氨基甲基吡啶的相互作用及其结构特征.1HNMR谱图和紫外可见吸收光谱图清晰表明,2-氨基甲基吡啶与对称四甲基六元瓜环有明显的相互作用,客体2-氨基甲基吡啶的吡啶环部分进入了瓜环空腔,1HNMR谱图相关质子峰的积分强度以及客体吸光度随主体瓜环浓度变化明确表示它们之间形成了1∶1的包结配合物,此包结比并不随瓜环的浓度增加而改变.X射线单晶衍射法对包结配合物晶体的测定进一步证实了核磁共振、紫外可见吸收方法所得结论.Interaction and structure of a host-guest inclusion complex of symmetrical tetramethyl substi- tuted cucurbit[6]uril (TMeQ[6]) with 2-(aminomethyl)pyridine (amp) have been studied by using 1H NMR technique, UV-visible spectrophotometry and single crystal X-ray diffraction determination. The experimen- tal results from 1H NMR and UV-visible spectra revealed that the amp as a guest enters into the cavity of TMeQ[6] to form a host-guest inclusion complex of TMeQ[6] and amp with a constant ratio of 1∶1. The single crystal X-ray diffraction determination further confirmed the conclusions.国家自然科学基金(Nos.200261002,20362003);; 科技部国际科技合作重点计划(No.2003DF000030);; 贵州省省长资金;; 贵州省教育厅自然科学研究资助项目

Investigation of Structures of the Self-assembled Pseudorotaxane of Cucurbiturils with Some Alkyldiamines

以1H核磁共振技术和X射线单晶衍射分析方法考察了 3种瓜环与长链二胺 ( 1,7 庚二胺与 1,8 辛二胺 )相互作用的结构特征 .1HNMR分析表明瓜环 (Q[6]和Q[7] )与有机二胺 ( 1,7 庚二胺与 1,8 辛二胺 )有较强的相互作用 ,形成自组装类轮烷结构 ;Q[8]与 1,7 庚二胺与 1,8 辛二胺之间相互作用力相对较弱 ;晶体结构测定结果表明 ,六元瓜环与辛二胺自组装形成的类轮烷实体中 ,辛二胺是以直链状穿过六元瓜环的空腔 ,两配位氨基留在瓜环两端口之外 .The structures of self-assembled pseudorotaxane of cucurbit[n]urils(n=6～8) with some alkyldiamines have been investigated by 1H NMR technique and single crystal X-ray diffraction method. The results reveal that the interaction between cucurbit[6]uril or cucurbit[7]uril and 1,7-diaminoheptane or 1,8-diaminooctane is stronger than that between cucurbit[8]uril and 1,7-diaminoheptane or 1,8-diaminooctane, and the pseudorotaxanes of cucurbit[n]urils with the alkyldiamines were observed. Particularly, in the pseudorotaxane of cucurbit[6]uril with 1,8-diaminooctane, the amino groups of 1,8-diaminooctane are left outside the ports of cucurbit[6]uril.国家自然科学基金(No.200261002);; 贵州省重点基金(No.20023004);; 贵州省国际合作(No.200211003)资助项目

对称四取代六元瓜环的合成及其2,2-联吡啶主客体化合物

利用二甲基取代甘脲的二醚与甘脲二聚体成功合成了新型取代六元瓜环——对称四甲基六元瓜环. 该瓜环的结构已被晶体结构鉴定、核磁共振谱以及质谱方法所证实, 分子中所含两个二甲基取代甘脲处于对位. 1H NMR表明该瓜环容易与吡啶衍生物形成主客体配合物

铟硼磷酸盐结构中的交叠生长规律研究

Several indium borophosphates have been reported recently, including KIn[BP2O8(OH)](I) and NaIn[BP2O8(OH)](H). The latter two compounds were synthesized under mild hydrothermal conditions, and have the same molar ratio (M-I:In:B:P:O:H) in molecular formula but with different structure types. Compound I crystallizes in the triclinic system with space group P (1) over bar (No.2), a=0.52638(4) nm, b=0.84791(5) nm, c=0.81469(9) nm, alpha=91.1741(7)degrees, beta=93.061(7)degrees, gamma=79.823(5)degrees, V=0.3573 nm(3), Z=2; while compound II possesses a monoclinic structure with space group P2(1)/n (No.14) with a=0.5177(1) nm, b=1.6815(3) nm, c=0.7684(2) nm, beta=94.10(3)degrees, V=0.6672(2) nm(3), Z=4. Eight- membered-ring and six-membered-ring are formed by alternating borate, phosphate tetrahedra and In-coordination octahedron sharing corners via common oxygen atoms in compound I and H respectively. The polyhedra in the structure are oriented along certain direction to form alternating layered fragments. These two structure types can be considered as intergrowth structures, which consist of the same layered fragments growing in different orientations. Other structure intergrowth possibilities are also expected in similar systems

A molecular bowl with barium ion as bottom

A molecular bowl with barium ion covering one portal of decamethylcucurbit[5]uril as a 'metal-ion-bottom' has been synthesized. The structure of the molecular bowl has been confirmed by the single crystal X-ray diffraction determination. It belongs to orthorhombic with space group of Pna2(1). The crystal unit cell parameters are: a=3.2108(6) nm, b=1.4742(3) nm, c=1.151 6(2) run, and V=5.4509(18) nm(3), D-c=1.677 Mg(.)m(3), Z=4, F(000)= 2832, R=0.0551, wR=0.1568