摘要
本文研究了Cu(PMBP)_2和HPMBP的单晶体结构,晶体学参数为:(1)HPMBP,C_(17)H_(14)0_2N_2,M=278.31,单斜晶系,空间群P2_1/a,a=11.406(5),b=9.087(1),c=13.467(3)(?),β=90.76(3)°,V=1395.7(?)~3,Z=4,D_c=1.324g cm^(-3),μ=0.95cm^(-1).(2)Cu(PMBP)_2,C_(34)H_(26)O_4N_4Cu,M=618.16,单斜晶系,空间群P_2_1/c,a=6.809(3),b=23.722(8),c=9.102(3)(?),β=108.94(4)°,V=1390.7(?)~3,Z=2,D_c=1.476g cm^(-3) μ=8.67cm^(-1).结果表明,HPMBP具有烯醇式结构,其中两个给体氧原子处于有利于形成六元螯合环的几何位置;在配合物Cu(PMBP)_2中,Cu原子为对称中心,两个配体中的四个氧原子形成以Cu为中心的近似平面正方形的配位结构,Cu-O距离分别为1.906和1.896(?).
The single crystals of HPMBP suitable for X-ray analysis were obtained from its ethanol solution, and Cu(PMBP)2 from trichloromethane / tetrahydrofuran solution. The three ditnentional data were collected with Enraf-Nonius CAD4 diffractometer, using MoKx radiation. The crystallographic parameters are as follows: (1) HPMBP, monoclinic, space group P2,/a, a= 11.406(5), b = 9.087(1), c=13.467(3)A, β = 90.76(3)°,V=1395.7A3, Z = 4; (2) Cu(PMBP)2, monoclinic, space group P21/c, a = 6.809(3), b = 23.722(8), c = 9.102(3)A, β= 108.94(4)° , V=1390.7A3, Z=2. The final discrepancy factors for HPMBP are R = 0.056, Rω = 0.059, and R = 0.071, Rω = 0.070 for Cu(PMBP)2.
The structure of HPMBP shows that the two phenyl groups are all twisted to the pyrazol ring in the molecule, and the two O atoms located with each other in geometrically favourable position for chelating reaction. In Cu(PMBP)2 molecule, Cu atom is located at the symmetry center, and coordinated by four O atoms with a squareplanar configuration. The distance Cu(l)-O(l 1) is 1..906, Cu(l)-O(12) 1.896A. The coplanarity of the atoms in the ligands within the complex is much better than those in the free ligand.
出处
《无机化学学报》
SCIE
CAS
CSCD
北大核心
1991年第2期129-132,共4页
Chinese Journal of Inorganic Chemistry
关键词
铜
配合物
HPMBP
晶体结构
l-phenyl-3-methyl-4-benzoyl-pyrazolone-5, copper, crystal, structure
