The complex(C24H24NO)2Cu·CH3CN（HL=S-（1-Benzy1-pyrrolidin-2-yl）-diphenyl-methanol）was （synthesized） by the electrochemical oxidation of Cu metal anodes in acetonitrile solution.The final product was （characterized） by elementary analysis,IR,and SEM and the structure was determined by single-crystal X-ray diffraction.The crystal belongs to trigonal,space group P3121 with a=9.8201（15）,b=9.82501（15）,c=36.516（6）?,α=β=90°,γ=120°,V=3049.6（8）?3,Z=3,ρcalc.=1.290g/cm3,F（000）=1251.In the complex two hydroxy oxygen atoms and two pyrrolidin nitrogen atoms from the ligand coordinate to copper（II）ion,forming a distorted square plane.
A Fe（Ⅲ） compex with OPPh3,[Fe（OPPh3）4Cl2][FeCl4],has been synthesized and characterized by elemental analysis and IRspectrum.The crystal structure of the title complex has been determined by simgle crystal X-ray diffraction techmiques.The crystal belongs to monoclinic,space group P21/c.The cell parameters are :a=13.9323（13）,b=27.5290（2）,c=18.2095（17）,β= 104.460（2）o,V=6762.9（11）3,Z=4,DC=1.412 g/cm3,μ=0.809 mm-1,F（000）=2952,R1=0.0796 and ωR2=0.1752for 10419 observed reflections（I>2σ（I）） out of 12343 unique data.In the cations[Fe（OPPh3）4Cl2]+,the Fe（Ⅲ） center adopts a slight distoned octahedral geometry comprised oftwo OPPh3 oxygen atoms and two Cl-ions at the equatorial positions,and two OPPh3 oxygenatoms at the axial positions.In the anions[FeCl4]-,The Fe（Ⅲ） ion has a sIightly distortedtetrahedI.al coordination geometry and is bonded to four Cl-ions.
A new compound（ClO4）2（H2O）0.5（azpy）was synthesized.Its structure was determined by single X-ray diffraction.The crystal belongs to triclinic system,space group P1.The crystallographic data:a=11.813（2）,b=12.574（2）,c=14.580（3）*!,a=84.048（6）,β=77.878（15）,γ=67.902（12）°,V=1961.1（7）*!3,Z=2,F（000）=926,Mr=904.57,Dc=1.532Mg/m3,μ=0.542mm-1,R1=0.0770,and wR2=0.1373.In the ctystal Mn（Ⅱ）ion is coordinated with six nitrogen from three phen ligands to form a distorted octahedron geometry.
