Co_3(CO)_7(μ_3-S)(μ,η~2-SCNR_2)的合成和晶体结构

Co2 (CO) 8 与 4个二硫代双 (烷基硫代甲酰胺 )类前配体 [R2 NC(S) S]2 反应 ,得 4个含烷基硫代甲酰胺基的三核钴羰基硫簇合物 .通过元素分析、IR、 1H NMR和 MS等方法表征了它们的结构 ,用 X射线衍射法测定了其中一个簇合物 Co3 (CO) 7(μ3 - S) [μ,η2 - SCN(i- Pr) 2 ]( )的晶体结构 .晶体属单斜晶系 ,P2 1/n空间群 ,晶胞参数 a=1.1452 (2 ) nm,b=1.50 2 8(3) nm,c=1.2 144 (2 ) nm,α=90°,β =92 .15(3)°,γ =90°,V =2 .0 885(7) nm3 ,Z=4 ,F (0 0 0 ) =10 96 ,Dc=1.74 7mg· m-3 ,GOF(F2 ) =0 .835,μ=2 .588nm-1.最终因子 R[I>2 σ(I) ]=0 . 0 4 0 7,Rw=0 .0 6 2 4

Hydrophobic pocket modification and humanized catalytic antibodies with glutathione peroxidase activity (I) - Preparation and characterization of haptenes and conjugates

The thiol group of glutathione (GSH) was protected by 2,4-dinitrochlorobenzene (DNCB), the product S-substituted dinitrophenyl GSH(GSH-S-DNP) was alcoholized to obtain haptenes 4 and 5 respectively. As haptenes, the two GSH derivatives were characterized by means of H-1 NMR, MALDI-TOF-MS and IR, followed by individually coupling with bovine serum albumin (BSA) via glutaraldehyde. BSB-Hp4 and BSA-Hp5 were purified by Sephadex G-25 gel filtration chromatography. For each conjugate, the average haptene-BSA ratio was 12 : 1. The electrophoresis analysis showed that the average molecular weight of each conjugate was 76 500. The CD spectrum indicated that the conjugates had more a-helix content than BSA did.

Synthesis, structure and properties of alpha-Keggin-type of K6H3[ZnW11O40Al]center dot 9.5H(2)O

A new heteropolycomplex, K6H3[ZnW11O40Al] . 9.5H(2)O was prepared and characterized by means of elemental analysis, IR, UV spectroscopy, Al-27 NMR, electrochemistry and X-ray crystallography. The crystal of K6H3[ZnW11O40Al] . 9.5H(2)O is cubic, space group Fm-3m, with lattice constants a=b=c=2. 144 8(2) nm, V = 9.866(2) nm(3), Mo radiation, R = 0.057 8 for 497 independent data with [I>2 delta(I)]. The anion is of alpha-type Keggin structure with C-s symmetry.

4－（2－氨基噻唑）－间苯二酚为柱前衍化剂液相色谱／电化学检测Fe、Co、Ni

４－（２－氨基噻唑）－间苯二酚为柱前衍化剂液相色谱／电化学检测Ｆｅ、Ｃｏ、Ｎｉ格日勒，李惠梅，李南强，汪尔康（中国科学院长春应用化学研究所电分析化学开放实验室，北京大学化学系，长春，１３００２２）关键词液相色谱，Ｆｅ，Ｃｏ，Ｎｉ，４－（２－氨基噻唑）...

THE CLEAVAGE REACTION OF THE MO-MO TRIPLE BOND - THE CRYSTAL-STRUCTURES OF MOLYBDENUM COMPLEXES [CPMO(CO)(2)(C(5)H(4)NS)], [CPMO(CO)(2)(C(9)H(6)NS)]O=PPH(3) AND [CPMO(CO)(2)(S(2)CNME(2)]

The reactions of [Cp2Mo2(CO)4] (1) with 2,2'-dipyridyl disulphide (C5H4NS-)2, 8,8'-diquinolyl disulphide (C9H6NS-)2 and tetramethyl thiuram disulphide (Me2NC(S)S-)2 in toluene solution resulted in the cleavage of the Mo-Mo triple bond to yield molybdenum complexes [CpMo(CO)2(C5H4NS)] (2), [CpMo(CO)2(C9H6NS)] (3) and [CpMo(CO)2(S2CNMe2)] (4), respectively. The molecular structures of 2, 3 . O=PPh3 and 4 were determined by X-ray diffraction studies. Crystals of 2 are monoclinic, space group P2(1)/n, with Z = 4, in a unit cell of dimensions a = 6.448(1), b = 12.616(2), c = 14.772(2) angstrom, beta = 92.85(1)-degrees. The structure was refined to R = 0.028 and R(w) = 0.039 for 1357 observed reflections. Crystals of 3 . O=PPh3 are triclinic, space group P1BAR, with Z = 2, in a unit cell of dimensions a = 11.351(3), b = 13.409(3), c = 9.895(2) angstrom, alpha = 94.59(2), beta = 90.35(2), gamma = 78.07(2)-degrees. The structure was refined to R = 0.033 and R(w) = 0.037 for 3260 observed reflections. Crystals of 4 are monoclinic, space group P2(1)/a and Z = 4 with a = 12.468(5), b = 7.637(2), c = 13.135(4) angstrom, beta = 96.62(3). The structure was refined to R = 0.032 and R(w) = 0.042 for 1698 observed reflections. Each of complexes 2-4 contains a cyclopentadienyl ligand, a cis pair of carbonyls and a chelate ligand (S,N donor or S,S donor). All the compounds have distorted square-pyramid structures.

STRUCTURE OF AN ERBIUM COORDINATION COMPOUND WITH L-PROLINE, ([ER(PRO)2(H2O)5]CL3)(N)

catena-Poly[{pentaaqua(L-proline-O)-erbium-mu-(L-proline-O:O')} trichloride], {[Er(C5H9-NO2)2(H2O)5]Cl3}n, M(r) = 594.0, monoclinic, P2(1), a = 8.294 (1), b = 10.981 (3), c = 11.934 (3) angstrom, beta = 107.04 (2)degrees, V = 1039.2 (4) angstrom3, Z = 2, D(x) = 1.90 g cm-3, lambda(Mo Kalpha) = 0.71069 angstrom, mu = 45.2 cm-1, F(000) = 586, T = 298 K, R = 0.0244 for 1711 unique reflections [I > 3 sigma(I(o))]. The crystal consists of one-dimensional chains of infinite length in which one L-proline ligand bridges two neighboring Er ions, the other L-proline ligand being monodentate.

Total synthesis of bis-(2,3-dibromo-4,5-dihydroxyphenyl)-methane as potent PTP1B inhibitor

Protein tyrosine phosphatase 1B (PTP1B) plays an important role as a negative regulator and has been proved to be an effective target for the treatment of type 2 diabetes mellitus. Bis-(2,3-dibromo-4,5-dihydroxyphenyl)-methane 7 was first reported as a natural bromophenol with significant inhibition against PTP1B which was isolated from red algae Rhodomela confervoides. Intrigued by its astonishing activity (IC50 = 2.4 mu mol/L), compound 7 was synthesized with the overall yield of 24% and evaluated for its PTP1B inhibitory activity compared with natural compound. (C) 2008 Li Jun Han. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.