摘要
标题化合物C1 7H1 9NO2 是由苯甲醛、5,5 二甲基 1 ,3 环己二酮、丙二酸亚异丙酯及醋酸铵在微波辐照下干反应而得。结构通过单晶X 射线衍射法确定 ,其晶体属于单斜晶系 ,空间群P2 1 /a ,a =7.52 4 (2 ) ,b =2 2 .483(3) ,c =9.2 73(2 ) ,β =1 1 3 0 4 (2 )°,V =1 44 3.7(5) 3,Mr=2 69.34,Dc=1 .2 39g/cm3,Z =4,μ(MoKα) =0 81cm- 1 ,F(0 0 0 ) =576,在 6 <2θ <51 0°范围内收集 2 994个独立衍射点 ,其中可观测衍射点 2 0 91个 [I >2 .50σ(I) ]。晶体结构用直接法解出 ,经用全矩阵最小二乘法对原子参数进行修正 ,最后的偏离因子为R =0 .0 4 4 ,Rw=0 .0 58。在晶体结构中 ,O(3) -C(9) -C(4) -C(5) -N(1 )构成一个平面 ,该平面与苯环的二面角为 84.2
The title coumound (C 23 H 25 O 3Cl) has been synthesized by reaction of p chlorobenzaldehyde and 5,5 dimethyl 1,3 cyclohexanedionein ethyldiole and its structure was determined by single crystal X ray diffraction. The crystal is monoclinic, space group, P2 1/n, a=6.048(1), b=19\^543(3), c=17.420(3), β=97.29(1)°, V=2042.2(6) 3, M r=384.90, D c =1.252g/cm 3, Z=4, μ (Mo Kα )=2\^06cm -1 , F (000)=816. The structure was solved by direct methods ,and refined by full matrix least square method to a final R=0.039, R w =0.047. X ray analysis reveals that the dihedral angle plane 1(C(8)-C(9)-C(19)) and plane 2 is 16.24°, between plane 1 and plane 3 (C(7)-C(8)-C(9)) is 177\^37°, between plane 1 and plane 4 (C(1)-(5)-C(6)) is 161.12°, between plane 2 and plane 4 is 81\^98°, between plane 3 and plane 4 is 79\^15°.
