The reaction of lanthanum(Ⅲ) nitrate and 5-nitroisophthalic acid in isopropanol/H2O under hydrothermal conditions leads to a 3D lanthanum-containing coordination polymer with the general chemical formula {[La6(Nip)9(H2O)4 ]·(H2O)4 }∞(1,Nip=5-nitroisophthalate).The single-crystal X-ray analyses show that this compound crystallizes in the orthorhombic system,space group Ima2 with a=9.7769(12),b=28.239(3),c=21.149(2),V=5839.1(11)3,Z=2,Mr=2859.61,Dc =1.626 g/cm 3,F(000)=2752.14040 reflections are collected,of which 5275 are unique (R int=0.0241).Final GOOF=1.083,R=0.0406 and wR=0.1182,R indices based on 5183 reflections with I〉2σ(I)(refinement on F2),443 parameters,1 restraint.Lp and absorption corrections were applied,=2.242mm-1.Absolute structure parameter x=0.08(3).The crystal structure can be described as the butterfly-liked hexanuclear lanthanum entities {La6O6(CO2)8 } covalently linked to each other by nitroisophthalate ligands into an intricate three-dimensional structure.The fluorescence spectroscopy of compound 1 has been investigated.
A new 1D infinite neutral chain (Ph3SnO2SeOCH2CH3)n (1) based on organotin and selenious acid monoethyl ester has been synthesized successfully and characterized by IR, elemental analysis, and X-ray single-crystal diffraction. In the compound 1, the Sn atom exists in slightly distorted trigonal bipyramidal geometry and the Se center is tri-coordinated with a distorted pyramidal arrangement. It is noted that the synthesis is facile and selenium oxide is directly introduced into synthesis route replacing organoseleninic acid under room temperature.
The salts of para-tungstic and para-molybdic were heterogenized for their effective use as solid catalysts in the transesterification reaction of dimethyl carbonate and phenol by inserting them between the layers of Mg2Al-hydrotalcite. These catalysts were characterized by FT-IR spectra and X-ray powder diffraction. Polyoxometalates (POMs) clusters were intercalated into the interlayer of layered double hydroxide (LDH) via anion exchange with organic acid precursor in Mg2Al-LDH, and the integrity of the clusters [W7O24 ]^6- and [Mo7O24 ]^6- was maintained. The intercalated para-molybdic cluster showed high catalytic activity and reusability in the transesterification under mild reaction conditions. When the reaction was carried out at 180 ℃, with a molar ratio of phenol to DMC of 1 : 1, a reaction time 10 h, and a catalyst amount 1% (wt), the conversion of phenol was 10.0 %, the selectivities of diphenyl carbonate and methyl phenyl carbonate were 10.7 % and 86.1%, respectively.