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按文献[1]合成Ce(NO_3)_3·C_(12)H_(24)O_6和Pr(NO_3)_3·C_(12)H_(24)O_6(C_(12)H_(24)O_6为18-冠-6)配合物。将配合物溶于CH_3NO_2里,室温下置于有邻苯二甲酸二辛酯干燥器内析出单晶体。在NicoletR_3M/E四园衍射仪上收集晶体X-射线衍射数据。MoK_α辐射,石墨单色器。采用θ/2θ方式扫描,于3°<2θ<45°处收集独立衍射点。对强度数据进行LP因子校正和经验吸收校正。采用Patterson函数分析得到稀土金属原子坐标,后经Fourier合成获得全部非氢原子位置,经对角块矩阵最小二乘法修正。用理论加氢得到全部氢原子坐标。最后对非氢原子进行异性修正,对氢原子进行同性修正,同时经加权修正收敛。
Ce (NO_3) _3 · C_ (12) H_ (24) O_6 and Pr (NO_3) _3 · C_ (12) H_ (24) O_6 (C_ (12) H_ (24) O_6 were synthesized by literature [1] Crown -6) complex. The complex was dissolved in CH_3NO_2, placed in a dioctyl phthalate desiccator precipitated single crystals at room temperature. Crystallographic X-ray diffraction data were collected on a Nicolet R_3M / E quadruple diffractometer. MoK_α radiation, graphite monochromator. Scanning in the θ / 2θ mode, independent diffraction spots were collected at 3 ° <2θ <45 °. LP factor correction and empirical absorption correction of intensity data. The atomic coordinates of rare earth metals were obtained by Patterson function analysis, and all the non-hydrogen atoms were obtained by Fourier synthesis. The positions of all non-hydrogen atoms were corrected by the least square method of diagonal block matrix. Hydrogenation with theoretical hydrogen to get all the coordinates. Finally, heterosexual modification of non-hydrogen atoms, homomorphic modification of hydrogen atoms, while the weighted correction convergence.