A Novel Two-dimensional Homochiral Zinc（II） Complex Constructed Based on In Situ Ligand Formation

A novel zinc(Ⅱ) complex, Zn(IBT) 2 (1, HIBT=5-(4-((1H-imidazol-1-yl)methyl)phenyl)-2H-tetrazole) has been synthesized with Zn(NO3)2·6H2O, 4-(imidazol-1-ylmethyl)benzonnitrile (IBN) and NaN 3 by the hydrothermal method, and characterized by elemental analysis, IR and single-crystal X-ray diffraction. Crystallographic data for 1:C22H18N12Zn, Mr=515.85, orthorhombic, Pbcn, a=16.0567(15), b=9.5316(9), c=14.6107(14) , V=2236.1(4)  3 , Z=4, D c=1.532 g/cm3 , μ=1.138 mm-1 , F(000)=1056, R=0.0350 and wR=0.0888 for 1438 observed reflections (I > 2σ(I)) and the goodness-of-fit S=1.002 on F2 . The crystal structural analysis revealed that complex 1 exhibits a rare two-dimensional homochiral wave-like layer structure. In addition, the photoluminescence of complex 1 was studied in the solid state at room temperature together with its theoretical analysis.     

Syntheses and crystal structures of two new coordination polymers constructed from 2‐bromo‐1,4‐benzenedicarboxylate

To explore the possibility of obtaining the metal‐organic frameworks (MOFs) bearing the 2‐bromo‐1,4‐benzenedicarboxylate ligand, one new Mn(II) and one Co(II) coordination polymers, [Mn(HL)₂(bipy)₂·2H₂O]·bipy ( 1 ) and [Co(L)(bpe)] ( 2 ) (bipy=4,4′‐bipyridine; bpe=1,2‐bis(4‐pyridyl)ethene) were synthesized and characterized by elemental analysis and X‐ray diffraction analysis. Compounds 1 exhibits one‐dimensional coordination chains, which are further connected to form two dimensional supramolecular networks through hydrogen bonding interactions. Compound 2 presents a two‐fold interpenetrating two‐dimensional layer structure. The 2‐bromo‐1,4‐benzenedicarboxylate anion exhibits different coordination modes in the two complexes. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

含硫磷桥基的两核铁羰基簇合物的合成和晶体结构

Fe3(CO)12与杂环二硫代次膦酸盐SP(C6H4OR)(S)N(C6H5)NC(Me)(R=Me,Et)反应,得到两个新的含硫磷桥基的双核铁羰基簇合物Fe2(CO)6[μ-η2-SC(Me)NN(C6H5)P(C6H4OMe)](Ⅰ)和Fe2(CO)6[μ-η2-SC(Me)NN(C6H5)P(C6H4OEt)](Ⅱ),以及簇合物Fe3(CO)9(μ3-S)2(已知).对它们进行了元素分析,IR,1HNMR和MS等谱学表征,并用X-ray衍射技术测定了(Ⅰ)的晶体结构.该晶体属单斜晶系,P2(1)/n空间群,晶胞参数a=11.192(2)A,b=14.272(3)A,c=16.281(3)A,β=108.22(3).,V=2470.2(8)A3,Z=4.两核簇合物中含有两个桥基Fe-S-Fe和Fe-P-Fe,而且-C(7)-N(2)-N(1)-链连结在S、P原子间,形成了两个六员螯环Fe(1)SCNNP和Fe(2)PNNCS,增强了簇合物的稳定性.     

A New Dinuclear Copper (II) Complex of a Bis‐macrocyclic Ligand: Synthesis,Characterization, Crystal Structure and Magnetic Properties

A new dinuclear Cu(II) complex, [Cu₂L(N₃)₂](ClO₄)₁.₅ (OH)_4.5 · 2H₂O 0.5C₂H₅OH (1), of a bis‐macrocyclic ligand, 2,6‐bis(l,4,7,10‐tetraazacyclododecan‐10‐ylmethyl)‐methoxybenzene (L), has been synthesized, characterized and structurally determined by X‐ray diffraction analysis. Complex 1 crystallizes in orthorhombic crystal system, Pca2(l) space group with a = 1.5371(3), b = 1.6641(3), c = 3.0950(6) nm, V = 7.917(3) nm³, F_w = 904.62, Z=8, D_c= 1.529 g/cm³ and final R = 0.0568, wR = 0.1406 for 10410 observed reflections with I≥2σ (I). Both Cu(II) centers in the structure are coordinated by four nitrogen atoms of 1,4,7, 10‐tetraazacyclododecane (cyclen) and a nitrogen donor of the axial azide anion. Each Cu(II) center is in a square‐pyramidal coordination environment, and the intra‐and nearest inter‐molecular Cu? Cu nonbonding distances are 0.9855 and 0.7298 nm, respectively. Variable temperature magnetic susceptibility measurements in the range of 4.2–300 K indicate mat there exists weak intra‐ and inter‐molecular antiferromagnetic coupling between the Cu(II) centers with 27= ?4.2 cm^?1 and Θ = ?0.47 K.     

Enantiomeric resolution of some imidazole antifungal agents on chiralpak WH chiral stationary phase using HPLC

Summary The enantiomeric resolution of (±)-econazole, (±)-miconazole and (±)-sulconazole was achieved on a Chiralpak WH column. The mobile phase used was hexane-2-propanol-diethylamine (400:99:1,v/v/v). The flow rates of the mobile phase used were 0.50 and 1.00 mL min⁻¹. The values of α of the resolved enantiomers of econazole, miconazole and sulconazole were in the range of 1.68 to 1.23 while the values of Rs varied from 2.42 to 1.10. The resolution of these antifungal agents on Chiralpak WH column is governed by ligand exchange mechanism. Hydrophobic interactions also play an important role for the enantiomeric resoltuion of antifungal agents on the reported CSP.     

大环多胺配体BDBPH的设计合成及其晶体结构

用Pb(SN)₂作模板,2,6-二甲酰基对甲苯酚与二亚乙基三胺通过[2+2]缩合反应,经NaBH₄还原、脱Pb²⁺、酸化等操作,得晶体BDBPH·6HBr·4H₂O.晶体属单斜晶系,P2_1/c空间群,晶体学参数:a=1.4441(5)nm,b=1.1482(4)nm,c=1.2090(6)nm,α=90°,β=96.92°,γ=90°,V=1.9900nm³大环分子采取椅式构型,6个Br-和4个H₂O分子对称分布于大环两侧.该大环配体结构新颖,可用于多种金属配合物的研究,对进一步了解金属酶活性中心的结构及其催化作用机理具有重要价值.     

Synthesis and Structure of Dimolybdenum(I) Carbonyl Compound with Thiolate and Carboxylate Mixed-tri-bridging Ligands [Bu_4N][Mo_2(CO)_6(SC_6H_4Cl-p)_2(CF_3COO)]

1 INTRODUCTION Molybdenum(I) compounds, in particular Mo(I)-SR compounds, are rare amongst numerous Mo compounds. So far, only the following compounds [Mo2(CO)8-n(SR)2(CH_3CN)n] (R = C6H5, CH_2CO2Et, n = 0, 2)[1～5] have been reported in the literature. Recently, we make an effort to develop investigations on Mo(I) compounds on the basis of preparing new Mo(I) compounds by introducing different functional ligands into Mo2(SR)2(CO)8, then determining their structures and measur…     

Hydrocarbyl Ligand Transformation on the Tungsten–Triosmium Cluster Framework

A comprehensive review of the hydrocarbon derivative chemistry of WOs₃ mixed-metal cluster compounds including synthesis, reactivity, ligand transformation, and solution dynamics is presented.     

Crystal Structure of Bis｛1-(2-methoxyethyl)indenyl｝dysprosium Chloride

1　INTRODUCTION　　Organolanthanidecomplexeshavebeenextensivelystudied.However,thestud-iesofindenylrareearthcomplexeswererelativelylimited[1].Althoughaseriesoftri-indenyltetrahydrofuranatolanthanide((C9H7)3Ln·THF)havebeensynthesizedandstudiedbyTsutsuiandGyslingabout30yearsago[2],onlyafewcrystalstruc-turesofindenyllanthanidecomplexeshavebeenreported[1].Moreover,mostofthereportedindenyllanthanidecomplexesweresynthesisedbymetatheticalreactionsofanhydrouslanthanidetrichlorideswithindenyls…     

Photoreduction of Europium (III) in Sol-Gel Derived Inorganic-Organic Hybrid Materials

Eu²⁺-doped inorganic-organic hybrid materials, which are potentially suitable for a tunable laser in the near ultra violet and blue region, were prepared through the photoreduction of Eu³⁺ ions in the materials under the irradiation of the fourth harmonic wave light (266 nm) of the Nd:YAG laser. The hybrid materials doped with Eu³⁺ ions were prepared from Si(OCH₃)₄, CH₃Si(OCH₃)₃, EuCl₃ and chloropropyltrimethoxysilane (CPTM). After the prehydrolized silica sol was added to the Eu³⁺-containing solution, Eu³⁺-doped transparent inorganic-organic hybrid material was obtained by drying at 50°C. The emission peak around 450–475 nm due to the charge transfer transition (5d-4f) of Eu²⁺ ions increased with the laser irradiation time. Eu³⁺ ions were effectively photoreduced to Eu²⁺ ions in pore-free materials prepared at high CPTM to Eu³⁺ ratios. Eu²⁺ ions were generated by the photodecomposition of the bond between Eu³⁺ and Cl (Cl^– or Cl(CH₂)₃ in CPTM).