Clathrates with mixed guests

Investigation of the selectivities of two diol organic hosts for pairs of small organic guests gave interesting results which could be correlated with the crystal structures of the inclusion compounds containing mixtures of the two guests; these structures were compared with those of the single guest inclusion compounds.     

一种六核笼状锂配合物的制备、结构及合成机理研究

由[PhN(SiMe₂(OMe))Li]₂与哌啶腈通过加成反应合成了1种新型六核笼状锂配合物3,该配合物晶体结构已经确定,并用¹H NMR和X-单晶衍射对配合物3进行结构表征,其晶体呈笼状结构且属于单斜晶系：P2₁/n,a=1.248 83(19) nm,b=1.402 7(2) nm,c=1.853 4(3) nm;β=95.894(2)°;V=3 229.5(8) nm³,Z=2,R₁=0.047 7,GOF=0.946。     

新型一维麻花状超分子配合物的合成与结构

具有特殊结构及性能的超分子化合物由于其结构上的新颖性及潜在的应用价值而成为人们关注的热点 .以一个苯环为间隔基两端含两个吡啶基团的配体 L1与 Pd( ) ,Pt( )形成 2 -索烃 [1 ] ,与Cd( NO3) 2 则形成具有一维平面结构的聚合物 [2 ] .以联苯为间隔基的配体 L2在 4 ,4′-二联吡啶共同作用下与 Pd( )形成 2 -索烃 [3] .同样以一个苯环为间隔基两端含两个咪唑基团的配体 L3与 Zn( NO3) 2 ,Ag NO3反应得到新型多聚轮烷配合物 [4,5 ] .研究结果表明 ,配体或配位金属离子等的微小差别即导致形成结构不同的超分子化合物 .但这些超分子…     

Synthesis and Crystal Structure of a Cadmium Complex with Isonicotinate

The cadmium(II) complex, [Cd(iso) 2 (H 2 O) 4 ] (where iso is the anion of isonicotinic acid), has been synthesized and characterized by element analysis, thermal analysis and IR spectroscopy. An X-ray crystal structure reveals that the cadmium ion is trans -octahedral with two pyridyl nitrogens and two aqua oxygens in equational positions and two aqua oxygens in axial positions. The complex forms a three-dimensional network through intermolecular hydrogen bonds.     

Gossypol clathrates: Structure and thermal behavior of gossypol solvates with two picoline isomers

Gossypol forms stable solvates with 4- and 2-picolines at room temperature. The solvates are investigated by single crystal X-ray diffraction and thermal analysis. Solvate crystals of gossypol with 4-picoline (1) have the 1:3 composition (gossypol:4-picoline) and crystallize in the P2₁/c space group. This substance is isostructural to a trisolvate of gossypol with pyridine. Solvate crystals of gossypol with 2-picoline (2) have the 1:4 composition (gossypol:2-picoline) and crystallize in the P-1 space group. The unit cell parameters for the investigated structures are as follows: 1 monoclinic crystals, C₃₀H₃₀O₈·3C₆H₇N, a = 10.7530(1) ?, b = 20.7834(3) ?, c = 19.1166(2) ?, β = 95.537(1)°, V = 4252.32(9) ?³, M = 797.92, Z = 4, d _x = 1.246 g/cm³, and R = 0.0489 for 4102 reflections; 2 triclinic crystals, C₃₀H₃₀O₈·4C₆H₇N, a = 11.467(1) ? b = 14.962(2) ?, c = 15.570(3) ?, α = 75.62(1)°, β = 69.83(1)°, γ = 79.58(1)°, V = 2414.6(7) ?³, M = 891.04, Z = 2, d _x = 1.226 g/cm³, and R = 0.0528 for 3779 reflections. The results of the single crystal XRD and thermal analysis confirm that gossypol with 4-picoline forms a trisolvat, and a tetrasolvate with 2-picoline. The transition from 4-picoline to 2-picoline proves to change the type of the host-guest association from one-dimensional to zero-dimensional, i.e., to lead to a new crystal structure. Desolvation of compound 2 begins at a lower temperature than that for compound 1, which is explained by their different crystal structures. Keywords: gossypol, 4-picoline, 2-picoline, clathrate formation, crystal structure.     

Synthesis and Structure of a Titanocene-ferrocenyl Complex

A titanocene-ferrocenyl complex, （5-ferrocenyl-2-hydroxybenzenecarboxylato- O,O′）-bis（methylcyclopentadienyl）titanium（IV） 4, and an unexpected ionic complex, [C7H8NO3]- [（C5H5）Fe（C5H4）SO3]·H2O3 were synthesized and characterized by IR, ^1H NMR and elemental analysis. Compound 3 is of triclinic, space group P1 with a = 5.954（2）, b = 13.208（5）, c = 13.252（5） A, α = 60.993（7）,β = 84.342（8）,γ = 86.933（8）°, Z = 2, V = 906.8（6）A^3, Dc = 1.601 g/cm^3, μ（MoKα） = 0.987 mm^-1, F（000） = 452, the final R = 0.0647 and wR = 0.1333 for 2311 observed reflections （I 〉 2σ（I））. Compound 4 belongs to the monoclinic system, space group P2 1/c with α = 14.3310（9）, b = 12.5065（8）, c = 12.9406（10） A, β = 95.101（4）°, Z = 4, V = 2310.2（3） A^3, Dc = 1.513 g/cm^3, μ（MoKα） = 1.004 mm^-1, F（000） = 1088, the final R = 0.0461 and wR = 0.1048 for 2112 observed reflections （1 〉 2σ（I））.     

Syntheses and Crystal Structures of Three-Dimensional Cyanocadmate Clathrates with Imidazole

The crystal structures of two clathrates with imidazole (=imH), [Cd₃(CN)₆(imH)₂]·C₆H₁₂, I, and [Cd₃(CN)₆(imH)₂]·C₆H₅Cl, II, have been analyzed by single-crystal X-ray diffraction methods. Clathrate I crystallizes in the monoclinic system, space group P2₁/n with a=13.416(2), b=14.140(2), c=14.151(1)Å, β=105.08(9)°, V=2592.1(5)&Aringsup3;, Z=4, R ₁=0.0360, wR ₂=0.0850 for 5931 independent reflections; II: monoclinic P2₁/n, a=12.369(2), b=14.313(2), c=14.416(4)Å, β=106.04(2)°, V=2452.7(9)&Aringsup3;, Z=4, R ₁=0.0398, wR ₂=0.1105 for 5642 independent reflections. The three-dimensional host structures of clathrates I and II are isostructural with each other. The host framework is built through cyanide bridges among two kinds of Cd ions, tetrahedral and octahedral, in a ratio of 2 : 1. The tetrahedral Cd(1) centre is linked to three octahedral Cd(3) atoms and one tetrahedral Cd(2) atom; the tetrahedral Cd(2) centre is ligated by one unidentate imidazole ligand and linked to one tetrahedral Cd(1) atom and two octahedral Cd(3) atoms; the octahedral Cd(3) centre is ligated by one unidentate imidazole ligand and linked to three tetrahedral Cd(1) atoms and two tetrahedral Cd(2) atoms. The novel host structure provides two types of channels, a large, elongated, rectangular channel and a small rectangular channel. The larger channel is occupied by imidazole ligands coordinated to tetrahedral Cd(2) and octahedral Cd(3). The smaller channel accommodates the guest molecules cyclohexane and chlorobenzene.     

一维链状锰配合物的合成、结构及磁性研究

合成了邻硝基苯磺酰化丙氨酸配体2-NBS-AlaH (1)(2-NBS-AlaH=邻硝基苯磺酰化丙氨酸)及其锰的配合物[Mn(4，4′-bipy)(H₂O)₄]₂[(4，4′-bipy)₂(H₂O)₃(2-NBS-Ala)₄] (2)。通过X-射线单晶衍射测定了其结构：配体通过氢键形成了一维链状结构；配合物2中，4，4′-bipy把锰离子连成了一维链状结构。磁性研究表明，配合物由于分子间的自旋耦合呈现出弱的铁磁性。     

Gossypol clathrates: Structure and thermal behavior of the gossypol acridine complex

The natural compound gossypol forms a stable clathrate with acridine. The composition of the clathrate is C₃₀H₃₀O₈·0.5C₁₃H₉N. The unit cell is monoclinic, C2/c space group, a = 11.3213(3) ?, b = 30.5957(13) ?, c = 17.0824(4) ?, γ = 94.153(2)°, V = 5901.5(3) ?³, M = 1153.24, Z = 8, d _x = 1.369 g/cm³, and R = 0.0413 for 4726 reflections. The structure of the clathrate allows one to refer this compound to the ethyl acetate isomorphic host-guest group of gossypol complexes.     

Synthesis and Crystal Structure of a Complex of Melamine with Benzoic Acid

A new complex of melamine（MA） with benzoic acid（HBA） was prepared, affording [（HMA＋）（BA-）]-2H2O. Each HBA molecule is deprotonated and one triazine nitrogen atom of MA is protonated. The adjacent HMA＋ cations are related via an inverse center to form ribbons with a pair of N--H…N hydrogen bonds. COO- groups of BA- anions are hydrogen bonded to alternate sides of the （HMA＋）∞ ribbons to generate indention ID tapes, which are extended into a 3D structure via N--H…O- and N--H…OW hydrogen bonds and π-π stacking interactions. Predominant patterns of the hydrogen bond present in the complex are anion/water and amino/water tape structures. The hydrogen-bonding patterns consist of alternate 6, 10-membered rings sharing two edges. Infrared（IR） spectroscopy conforms that proton transfer has taken place in the complex.     

Crystal Structure of Nickel- and Cobalt-Diazidotetrapyridinemetal(II)-2(Pyridine) Clathrates

[MPy₄(N₃)₂]2Py (M = Ni, Co) are clathrates where two of six pyridine species are included in the crystal structure of the host complex without chemical bonding. The clathrates are isostructural, orthorhombic, space group Pnna (52), Z = 4. For the Ni compound a = 14.958(5), b = 11.909(5), c = 17.517(7) Ú, V = 3120(2) Ú₃, µ = 12.25 cm-¹, final R = 0.057.The Cocompound is of very similar structure (a = 14.980(3), b =11.980(2), c = 17.350(5) Ú, V = 3114(1) Ú³, µ = 46.50 cm-¹. The metal cation in the host molecule is surrounded by six donor nitrogens of two terminal azido-groups in trans-positions and four pyridine ligands. The complex molecule lies on a twofold axis parallel to a.     

Crystal Structure and Properties of a Terbium Benzoate Complex with 1,10-Phenanthroline

1 INTRODUCTION The photoactive lanthanide organic complexessuch as europium and terbium chelating with ?-dike-tones, macrocyclic ligands and a number of polya-mino carboxylates, are of both fundamental and tech-nological interest due to their intense…