THE MOLECULAR AND CRYSTAL STRUCTURE OF [Et4N]2[Fe2S2（NO）4]

<正> The compound [Et_4N]_2[Fe_2S_2(NO)_4] (M_r=556.36) crystallizes in the monoclinic,space group P 2_1/n with a=9. 688(3), b=10. 882(2), c=12. 625(2), β=97. 86(3)°, Z=2, V=1318. 4, D_c=1. 40g/cm~3, ;μ(MoK_a)=12. 8cm~(-1) and F(000)=588. The final R=0. 028 and R_w=0. 029 for 2041 reflections (I≥3σ(I)).The crystals of [Et_4N]_2[Fe_2S_2(NO)_4] consist of discrete cations [Et_4N]~+ and anions     

CRYSTAL STRUCTURE OF 2，4—DINITROPHENYL—t—BUTYL NITRONE（DNPBN）

<正> C11H13 N3 O5·t-Bu- N = CHC6H3(NO2)2,Mr = 267. 27, Monoclinic space group C2/c,a= 18. 546(3),b = 5. 729(1),c= 27. 479(5) A,β= 118. 42(1)°/,F = 2567. 6(9)A3,F(000) = 1120,Z=8,Dx=1. 38g/cm3. The structure of DNPBN is akin to that of PBN reported by us except for shorter N - O and C = N bonds.     

CRYSTAL STRUCTURE OF Fe4S4[SC（CH3）3]4[（C4H9）4N]2

<正> Fe_4S_4[SC(CH_3)_3]_4[(C1H_9)_2,Mr=1193. 23,tetragonal,142d,a = 23. 272(2), c= 13. 080(5) A ,V=7084(3) A3,Z=4,DC=1. 12g·cm-3,UUUU(MoKa) = 10. 8cm-1,F(000) = 2568,R=0. 058 for 1005 observed reflections. The cluster anion contains a cubane-type Fe4S4 core compressed along the 4 axis which is crystallographically imposed. Compared to other salts with different cations ,the core is subject to slight structural distortions in different crystalline environments and crystallographic symmetry of the anion is related to that of the cation.     

CRYSTAL STRUCTURE OF [4,4'-bipy-Cu(acac)_2]

<正> Introduction. Copper (Ⅱ) complexes have plentiful and variable steric structures. It plays an important role in a lot of enzymatic reactions. Especially,the active component of some enzymes has a binuclear copper core with bridging ligands. Besides, lots of one-dimension molecular chains and polymers are studied as model of one-dimension conductors. ~ ~     

CRYSTAL STRUCTURE OF BID[N-t-BUTYLBUTEN-2-YLIDENE] DICHLOROPALLADIUM(II)

<正> The title compound, C15H30N2PdCl2 (Mr=427.73), crystallizes in two kinds of crystal forms I and II.I : monoclinic, P21/c, a = 8.234(1), b = 13.702(3), c = 8.939(2) A, β = 93.90(1)°, V = 1010.55 A3, DC = 1.407g/cm3, R = 0.032 for 2098 observed reflections.II: triclinic, Pl, a=8.179(1), b=8.182(1). c=8.231(2) A, α=91.89(1)°, β=91.90(2)°, α=113.80(1)°, V =503.09A3, DC =1.413 g/cm3, R = 0.036 for 1770 observed reflections.The molecules in both crystals I and II possess the identical configurations but there are two orientations of molecules in the crystal II.     

双环[3.3.0]-3,7-辛二烯-2,6-二酮晶体的分子结构

利用 Enraf-Nonius CAD4四圆单晶衍射仪测定了双环[3.3.0]-3,7-辛二烯-2,6-二酮(2)的单晶结构,晶体属三斜晶系,空间群为 PI,晶胞参数为:a=6.596(2)(?),b=7.414(1)(?),c=7.359(1)(?),α=106.64(1)°,β=100.17(1)°,γ=98.44(1)°,ν=331.9((?)~3),Ζ=2。用直接法得到分子的粗结构。对1013个可观察反射点用全矩阵最小二乘法修正,最后得R=0.060,结构测定的结果证实:两个五员环自成一个平面,两平面间夹角为117.3°。     

SYNTHESIS AND CRYSTAL STRUCTURE OF BaGa_4

<正> BaGa4,tetragonal space group I4/mmm with lattice parameters a=b=4.5650(8), c=10.786(2)A, V=224.77(7)A3,Dc=6.15 gcm-3,and Z=2,λ(MoKα)=0.71069A,μ=335.93cm-1,F(OOO) =360. The final R = 0.045, Rw=0.069.The distribution of valence electrons in crystal Ba6a4 is described and a suggestion that two different types of gallium atoms form covalent bonds by utilizing sp3 and dsp3 hybrid orbitals respectively is proposed.     

INTERACTION OF METAL IONS WITH TWO NEW CALIX[4, 8]ARENE DERIVATIVES

Abstract

Two new calixarene derivatives: 5,11,17,23-tetra-t-butyl-25,26,27,28-tetrakis-(piperidinocarbo-nylmethyoxy)calix[4]arene (L⁴) and 5,11,17,23,29,35,41,47-octa-t-butyl-49,50,51,52,53,54,55, 56-octa-(piperidinocarbonylmethoxy)calix[8]arene (L⁸), which show good binding abilities to metal ions, were synthesized by the reaction of the corresponding calixarene derivatives with piperidine. The ligand L⁴ is capable of separating a tight ion-pair formed by Pb²⁺ and the picrate anion in THF. The interactions of the new ligands (Lⁿ n = 4, 8) with Na⁺, Pb²⁺ and Cd²⁺, in the presence or absence of picrate, were investigated by ¹H NMR and electrospray mass spectrometry. It is found that L⁴ reacts with these metal ions to form a unique complex which can be described as [M^m+L⁴]^m+ while L⁸ forms a variety of complexes depending on whether there are picrate anions in solution. [M^m+L⁸]^m+ is formed in the absence of the picrate, and two complexes, [PbL⁸]·CH₃CN·H₂O and [PbNaL⁸]³⁺, are formed in the presence of the picrate. The higher conformational flexibility and larger macro-ring size of L⁸ account for the fact that it forms a variety of complexes as compared with L⁴.     

PREPARATION AND CRYSTAL STRUCTURE OF TETRAKIS(TETRAHYDROFURAN) MAGNESIUM DICHLORIDE[MgCl_2·4THF]

<正> INTRODUCTION. The magnesim, dichloride is widely used as a supporter of the highly efficient Ziegler-Natta catalyst with ether or ester as a donor. To study the interaction between the supporter and the donor would lead to a better understanding of the mechenisms of stereoregular polymerization. Here we wish to report the preparation and X-ray crystal structure of MgCl_2 4THF, which is the first example of the MgCl_2 complex uncontaining coordinated water or solvent water.     

CALIXE[4] ARENE AS A TEMPLATE FOR CONTROLLING REGIOCHEMISTRY OF PHOTODIMERIZATION OF9-SUBSTITUTED ANTHRACENE

Photodimerization of anthracene and its derivatives has been extensively investigated^[1].In general,irradiation of 9-substituted anthracene in organic solvents results in the dimerization of the aromatic rings at 9,10-positions to yield head-to-tail (h-t) rather than head(h-h)photodimers^[2].     

SYNTHESIS AND COMPARATIVE COMPLEXATION STUDIES OF SCHIFF BASE DERIVATIVES OF p-TERT BUTYLCALIX[4]ARENE COPOLYMERS

Two different Schiff base derivatives of p-tert butylcalix[4]arene 3, 6 in which one of them carrying two oxime groups, while the other has a 1,8-octylenediimino bridge, are synthesized. Treatment of these monomers with triethylene ditosylate provided corresponding copolymers 5, 7. Their complexing properties with selected alkali and transition metals are reported here. It has been concluded that the binding ability of Schiff base-calix arene derivatives in transferring the metal cations is due to the presence of soft π-donor systems in the macrocyclic structure.