The title complex Cu[C5H3N(CCH3=N-C6H5)2]2(PF6)2 has been synthesized by r eaction of Schiff base C5H3N(CCH3=N-C6H5)2 and cupric sulfate in toluene solut ion. The crystal structure was determined by X-ray diffraction ...The title complex Cu[C5H3N(CCH3=N-C6H5)2]2(PF6)2 has been synthesized by r eaction of Schiff base C5H3N(CCH3=N-C6H5)2 and cupric sulfate in toluene solut ion. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 1041.85. The crystal structure belongs to triclinic system with spacegroup and cell parameters: a=12.6470(10) , b=14. 123(2) , c=15.613(2);á=66.150(10)a=79.470(10)?=78.290(10)穖-3 and F(000)=1064. The final R:R1=0.0668, wR 2=0.1927; R(all data): R1=0.1133, wR2=0.2357. The Cu was coordinated by six nitrogen, at the same time the Cu formed a distorted octahedron, besides the angles and pl anes of this compound were discussed . The result of kinetics of the thermal dec omposition indicated that the first step of it is 2 series chemical reactions, t he function of machanism is f(a)=(1-a)2, and the activation energy is 144.64E/ kJ. CCDC: 180872.展开更多
The title compound (C10H12N2O7, Mr = 272.22) crystallizes in triclinic, space group P1 with a = 5.532(2), b = 9.760(4), c = 11.731(5) ?, α = 68.107(7), β = 89.179(7), γ = 77.830(7)o, V = 573.1(4) ?3, Z = 2, Dc = 1....The title compound (C10H12N2O7, Mr = 272.22) crystallizes in triclinic, space group P1 with a = 5.532(2), b = 9.760(4), c = 11.731(5) ?, α = 68.107(7), β = 89.179(7), γ = 77.830(7)o, V = 573.1(4) ?3, Z = 2, Dc = 1.578 g/cm3, F(000) = 284 and μ(MoKa) = 0.136 mm-1. The final R = 0.0400 and wR = 0.0951 for 1468 observed reflections with I > 2σ(I). The title compound is a 1:1 adduct of sarcosine and 5-nitrosalicylic acid. The nitrogen atom of sarcosine is protonated, and the proton is from the carboxyl group of sarcosine and 5-nitrosalicylic acid with the probability of 50 percent for each. The 5-nitrosalicylic acid and sarcosine molecule of the title adduct are ABAB arranged along the c axis. There exist a lot of hydrogen bonds in the structure, linking sarcosine and 5-nitrosalicylic acid to form a three-dimensional network.展开更多
The thermal behavior of the complex Pr[(C5H8NS2)3(C12H8N2)] in a dry nitrogen flow was examined by TG-DTG analysis. The TG-DTG investigations indicated that Pr[(C5H8NS2)3-(C12H8N2)] was decomposed into Pr2S3 and depos...The thermal behavior of the complex Pr[(C5H8NS2)3(C12H8N2)] in a dry nitrogen flow was examined by TG-DTG analysis. The TG-DTG investigations indicated that Pr[(C5H8NS2)3-(C12H8N2)] was decomposed into Pr2S3 and deposited carbon in one step where Pr2S3 predominated in the final products. The results of non-isothermal kinetic calculations showed that the decomposition stage was the random nucleation and subsequent growth mechanism (n =nential constant In[A/s] was 7.8697. The empirical kinetics model equation was proposed as f(α) =3/2(1-α)[-ln(1-α)]1/3. The X-ray powder diffraction patterns of the thermal decomposition products at 800℃ under N2 atmosphere show that the product can be indexed to the cubic Pr2S3 phase. The transmission electron microscopy (TEM) of the final product reveals the particle appearance of a diameter within 40 nm. The experimental results show that the praseodymium sulfide nanocrystal can be prepared from thermal decomposition of Pr[(C5H8NS2)3(C12H8N2)].展开更多
文摘The title complex Cu[C5H3N(CCH3=N-C6H5)2]2(PF6)2 has been synthesized by r eaction of Schiff base C5H3N(CCH3=N-C6H5)2 and cupric sulfate in toluene solut ion. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 1041.85. The crystal structure belongs to triclinic system with spacegroup and cell parameters: a=12.6470(10) , b=14. 123(2) , c=15.613(2);á=66.150(10)a=79.470(10)?=78.290(10)穖-3 and F(000)=1064. The final R:R1=0.0668, wR 2=0.1927; R(all data): R1=0.1133, wR2=0.2357. The Cu was coordinated by six nitrogen, at the same time the Cu formed a distorted octahedron, besides the angles and pl anes of this compound were discussed . The result of kinetics of the thermal dec omposition indicated that the first step of it is 2 series chemical reactions, t he function of machanism is f(a)=(1-a)2, and the activation energy is 144.64E/ kJ. CCDC: 180872.
文摘The title compound (C10H12N2O7, Mr = 272.22) crystallizes in triclinic, space group P1 with a = 5.532(2), b = 9.760(4), c = 11.731(5) ?, α = 68.107(7), β = 89.179(7), γ = 77.830(7)o, V = 573.1(4) ?3, Z = 2, Dc = 1.578 g/cm3, F(000) = 284 and μ(MoKa) = 0.136 mm-1. The final R = 0.0400 and wR = 0.0951 for 1468 observed reflections with I > 2σ(I). The title compound is a 1:1 adduct of sarcosine and 5-nitrosalicylic acid. The nitrogen atom of sarcosine is protonated, and the proton is from the carboxyl group of sarcosine and 5-nitrosalicylic acid with the probability of 50 percent for each. The 5-nitrosalicylic acid and sarcosine molecule of the title adduct are ABAB arranged along the c axis. There exist a lot of hydrogen bonds in the structure, linking sarcosine and 5-nitrosalicylic acid to form a three-dimensional network.
基金supported by the National Natural Science Foundation of China(Grant No.20171036)Education Committee of Shannxi Province(No.01JK229)
文摘The thermal behavior of the complex Pr[(C5H8NS2)3(C12H8N2)] in a dry nitrogen flow was examined by TG-DTG analysis. The TG-DTG investigations indicated that Pr[(C5H8NS2)3-(C12H8N2)] was decomposed into Pr2S3 and deposited carbon in one step where Pr2S3 predominated in the final products. The results of non-isothermal kinetic calculations showed that the decomposition stage was the random nucleation and subsequent growth mechanism (n =nential constant In[A/s] was 7.8697. The empirical kinetics model equation was proposed as f(α) =3/2(1-α)[-ln(1-α)]1/3. The X-ray powder diffraction patterns of the thermal decomposition products at 800℃ under N2 atmosphere show that the product can be indexed to the cubic Pr2S3 phase. The transmission electron microscopy (TEM) of the final product reveals the particle appearance of a diameter within 40 nm. The experimental results show that the praseodymium sulfide nanocrystal can be prepared from thermal decomposition of Pr[(C5H8NS2)3(C12H8N2)].
