粉末X射线衍射法监测发光有机分子结构转化的综合实验教学

潘梅, 王中豪

Comprehensive Laboratory Teaching of Monitoring Structure Transformation of Photoluminescent Organic Molecular by Powder X-ray Diffraction

Mei Pan, Zhonghao Wang

表1 晶体B、C1、C、G和F的晶体学和结构精修数据

晶胞参数 晶体B 晶体C1 晶体C 晶体G 晶体F Empirical formula C34H30F3N3O7 C35H31F3N4O7 C30H21F3N2O6 C35H32F3N3O7 C29H17F3N2O5 CCDC number 1470803 1470804 1470805 1470806 1470807 Color colorless colorless colorless colorless pale yellow Temperature/K 150 150 150 150 150 Wavelength/Å Mo Kα, Mo Kα, Mo Kα, Mo Kα, Cu Kα, 0.71073 0.71073 0.71073 0.71073 1.5418 Crystal system Triclinic Triclinic Triclinic Triclinic Monoclinic Space group P${\rm{\bar 1}}$ P${\rm{\bar 1}}$ P${\rm{\bar 1}}$ P${\rm{\bar 1}}$ P21/n Unit cell dimensions a = 10.4101(6) Å a = 10.3694(3) Å a = 9.4844(5) Å a = 9.1127(3) Å a = 14.8457(2) Å b = 12.6325(6) Å b = 12.9551(5) Å b = 11.9760(6) Å b = 12.7452(7) Å b = 20.0452(3) Å c = 13.2754(6) Å c = 13.3347(5) Å c = 12.6807(6) Å c = 14.6534(9) Å c = 16.2309(2)Å α = 91.976(4)° α = 87.150(3)° α = 70.466(4)° α = 89.060(5)° α = 90° β = 92.533(4)° β = 86.739(3)° β = 70.427(4)° β = 89.138(4)° β = 104.788(10)° γ = 113.252(5)° γ = 66.714(3)° γ = 75.767(4)° γ = 69.885(4)° γ = 90° Volume/Å3 1599.86 1642.03 1264.39 1597.79 4670.09 Z 2 2 2 2 8 Dcalc/(g∙cm−3) 1.349 1.368 1.477 1.379 1.509 μ/mm−1 0.105 0.911 0.118 0.108 0.118 F(000) 676.0 704.0 580.0 692.0 2176.0 GOF 1.071 1.039 1.001 0.999 1.035 R1 (all) 0.0739 (4631) 0.0383 (5491) 0.0492 (3682) 0.0545 (3223) 0.0476 (6299) wR2 [I > 2∙(I)] 0.1921 (6825) 0.1099 (6494) 0.1212 (5395) 0.1473 (4291) 0.1483 (7819)