CAJ | 학술논문

目的确定标题化合物(C18H23NO3,Mr=301.37) 的新晶型.方法制备化合物晶体,并用单晶X-射线对其晶型结构进行确定.结果新晶型属于单斜晶系,空间群为P21/n,晶胞参数为a=0.687 288(16) nm,b=1.026 47(2) nm,c=2.143 46(5) nm,β=94.579(2)°,V=1.507 34(6) nm3,Z=4,Dx=1.340 mg/m3,λ(Cu Kα)=0.154 184 nm,F(000)=653.6,μ(Cu Kα)=0.74 mm-1,R=0.082,wR=0.219.测定中衍射仪共收集到2 707个独立反射,其中的2 396个符合条件I>2σ(I).五元内酰胺环与C1~C4平面间的二面角为66.3°.晶体中的各分子通过C-H…O键相互连接,同时还存在分子内氢键C(10)-H(10A)…O(3)和C(13)-H(13A)…O(3).分子内氢键和分子键范德华力的存在是该结构稳定的原因.结论标题化合物存在多晶型.
목적 학정표제화합물(C18H23NO3,Mr=301.37) 적신정형.방법 제비화합물정체,병용단정X-사선대기정형결구진행학정.결과신정형속우단사정계,공간군위P21/n,정포삼수위a=0.687 288(16) nm,b=1.026 47(2) nm,c=2.143 46(5) nm,β=94.579(2)°,V=1.507 34(6) nm3,Z=4,Dx=1.340 mg/m3,λ(Cu Kα)=0.154 184 nm,F(000)=653.6,μ(Cu Kα)=0.74 mm-1,R=0.082,wR=0.219.측정중연사의공수집도2 707개독립반사,기중적2 396개부합조건I>2σ(I).오원내선알배여C1~C4평면간적이면각위66.3°.정체중적각분자통과C-H…O건상호련접,동시환존재분자내경건C(10)-H(10A)…O(3)화C(13)-H(13A)…O(3).분자내경건화분자건범덕화력적존재시해결구은정적원인.결론 표제화합물존재다정형.
Objective To determine a new crystal form of the title compound(C18H23NO3,Mr=301.37).Methods To prepare the crystals and determine the rystal structure by single-crystal X-ray diffraction.Results The crystal belonged to monoclinic,space group P21/n,with a=0.687 288(16) nm, b=1.026 47(2) nm,c=2.143 46(5) nm,β=94.579(2)°,V=1.507 34(6) nm3,Z=4,Dx=1.340 mg/m3,λ(Cu Kα)=0.154 184 nm,F(000)=653.6,μ(Cu Kα)=0.74 mm-1,R=0.082 and wR=0.219. A total of 2 707 independent reflections were collected,of which 2 396 with I>2σ(I)were observed. The dihedral angle between five-membered lactam ring and the C1-C4 plane was 66.3°. The individual molecules in the crystal structure were linked via C-H…O interactions leading to the formation of a supra-molecule. To our interest,intramolecular C(10)-H(10A)…O(3) and C(13)-H(13A)…O(3) hydrogen bonds were found in each molecule. Intramolecular hydrogen bonds and intermolecular van der Waals force contributed to the stability of the structure.Conclusion The title compound had polymorphic crystal structure.