Three new complexes of N salicylidenamino acid with Zn? have been synthesized. The compositions and structures of the obtained complexes have been characterized by elemental analyses, molar conductance, infrared spect...Three new complexes of N salicylidenamino acid with Zn? have been synthesized. The compositions and structures of the obtained complexes have been characterized by elemental analyses, molar conductance, infrared spectra, TG DTA and X ray powder diffraction. The three complexes have the compositions of Zn(sal β ala)·H2O(1),Zn(sal γ aba)·H2O(2),Zn(sal DL met)·1.5H2O(3)(sal=salicylidene,β ala=β alanine,γ aba=γ aminobutyric acid,DL met=DL methionine) and the molecular formula of ZnC10H11O4N, ZnC11H13O4N, ZnC12H16O4.5NS respectively. Infrared spectra of the complexes indicate that water has been coordinated. The thermal decomposition processes of the complexes show that the first weight losses are in good agreement with the water contents, and the compositions of the final residues are zinc oxide. The results of indexes to the X ray powder diffraction data indicate that the crystal structure of the three complexes belong to triclinic system. The lattice parameters are:a=1.9522nm,b=1.3904nm,c=2.0235nm,α=97.33°,β=98.66°,γ=99.05° for 1;a=1.3944nm,b=2.0880nm,c=2.4455nm,α=92.99°,β=95.48°,γ=96.18° for 2;a=2.1892nm,b=1.9171nm,c=1.4546nm,α=94.76°,β=95.09°,γ=94.12° for 3 respectively.展开更多
The crystal structures of normethisterone, gestonoronacetat, and griseofulvin were directly determined from the X-ray powder diffraction (XRPD) using the direct space approach by means of material studio (MS), the Rie...The crystal structures of normethisterone, gestonoronacetat, and griseofulvin were directly determined from the X-ray powder diffraction (XRPD) using the direct space approach by means of material studio (MS), the Rietveld refinement (RR), based on MS and generalized structural analysis system (GSAS) programs, was examined to practice and expand the Rietveld (whole-profile) technique in the pharmaceutical field. The RR converges to Rwp =8.85%, 10.56%, and 5.92% for normethisterone (6.88%), gestonoronacetat (9.58%), and griseofulvin (5.24%), respectively. The crystallographic data obtained from the powder diffraction data were compared with the single-crystal X-ray diffraction (SXRD) data. The results showed that the maximum relative errors of lengths a, b, and c and volume were respectively 0.18%, 0.18%, 0.22%, and 0.39% between SXRD and XRPD. Thus, MS and GSAS programs were useful to powder diffractionists in determining the crystal structure of organic polycyclic molecules.展开更多
文摘Three new complexes of N salicylidenamino acid with Zn? have been synthesized. The compositions and structures of the obtained complexes have been characterized by elemental analyses, molar conductance, infrared spectra, TG DTA and X ray powder diffraction. The three complexes have the compositions of Zn(sal β ala)·H2O(1),Zn(sal γ aba)·H2O(2),Zn(sal DL met)·1.5H2O(3)(sal=salicylidene,β ala=β alanine,γ aba=γ aminobutyric acid,DL met=DL methionine) and the molecular formula of ZnC10H11O4N, ZnC11H13O4N, ZnC12H16O4.5NS respectively. Infrared spectra of the complexes indicate that water has been coordinated. The thermal decomposition processes of the complexes show that the first weight losses are in good agreement with the water contents, and the compositions of the final residues are zinc oxide. The results of indexes to the X ray powder diffraction data indicate that the crystal structure of the three complexes belong to triclinic system. The lattice parameters are:a=1.9522nm,b=1.3904nm,c=2.0235nm,α=97.33°,β=98.66°,γ=99.05° for 1;a=1.3944nm,b=2.0880nm,c=2.4455nm,α=92.99°,β=95.48°,γ=96.18° for 2;a=2.1892nm,b=1.9171nm,c=1.4546nm,α=94.76°,β=95.09°,γ=94.12° for 3 respectively.
文摘The crystal structures of normethisterone, gestonoronacetat, and griseofulvin were directly determined from the X-ray powder diffraction (XRPD) using the direct space approach by means of material studio (MS), the Rietveld refinement (RR), based on MS and generalized structural analysis system (GSAS) programs, was examined to practice and expand the Rietveld (whole-profile) technique in the pharmaceutical field. The RR converges to Rwp =8.85%, 10.56%, and 5.92% for normethisterone (6.88%), gestonoronacetat (9.58%), and griseofulvin (5.24%), respectively. The crystallographic data obtained from the powder diffraction data were compared with the single-crystal X-ray diffraction (SXRD) data. The results showed that the maximum relative errors of lengths a, b, and c and volume were respectively 0.18%, 0.18%, 0.22%, and 0.39% between SXRD and XRPD. Thus, MS and GSAS programs were useful to powder diffractionists in determining the crystal structure of organic polycyclic molecules.
