The title compound Fe(CH4N2S)2Cl22(C11H6N2O) (Mr = 643.35) has been prepared and its crystal structure was determined by X-ray diffraction method with the following data: triclinic, space group P1, a = 7.3742(10), b =...The title compound Fe(CH4N2S)2Cl22(C11H6N2O) (Mr = 643.35) has been prepared and its crystal structure was determined by X-ray diffraction method with the following data: triclinic, space group P1, a = 7.3742(10), b = 13.0427(12), c = 15.215(2) , a = 88.969(12), b = 78.004(12), g = 79.689(11)o, V = 1408.1(3) 3, Z = 2, Dx = 1.517 g/cm3, m = 0.912 mm-1 and F(000) = 656. The final R = 0.030 and wR = 0.078 for 4070 observed reflections (I > 2s(I)), and R = 0.064 and wR = 0.091 for 5516 independent ones. The crystal consists of tetrahedral Fe(II) complex and hydrogen bonded 4,5-diazafluoren-9-one (dafone). The carbonyl bridge in dafone distorts the bipyridine moiety and results in the longer N…N separation of 3.071(3) and 3.061(3) ? There exists an extensive intermolecular hydrogen bond network in the crystal, and p-p stacking is observed between the neighboring dafone rings.展开更多
The polymorphic isomer [Cu(dafone)2(H2O)2](Hphth)2 1 (dafone = 4,5- diazafluoren-9-one, phth = 1,2-benzenedicarboxyl) has been synthesized and the structure was determined by single-crystal X-ray diffraction. Crystal ...The polymorphic isomer [Cu(dafone)2(H2O)2](Hphth)2 1 (dafone = 4,5- diazafluoren-9-one, phth = 1,2-benzenedicarboxyl) has been synthesized and the structure was determined by single-crystal X-ray diffraction. Crystal data: C38H26CuN4O12, monoclinic, space group P21/a with a = 11.5863(18), b = 25.512(4), c = 11.878(2) ?, β = 111.696(3)o, V = 3262.1(9) ?3, Mr = 794.17, Z = 4, Dc = 1.617 g/cm3, F(000) = 1628, μ = 0.748 mm-1, R = 0.0603 and wR = 0.1132 for 6878 observed reflections with I > 2σ(I). 1 consists of one [Cu(dafone)2(H2O)2]2+ cation and two monoprotonated 1,2-benzenedicarboxyl (Hphth) anions and forms a two-dimensional hydrogen bond network via intermolecular hydrogen bond interactions between the coordinated water molecules and carboxylato-oxygen atoms from monoprotonated benzenedicarboxyl anions.展开更多
Two new sterol have been isolated from the South China Sea marine organism. Compound 1 was isolated from the sponge Polymastia sobustia and compound 2 was obtained from the soft coral Sinularia inexplicata. Their stru...Two new sterol have been isolated from the South China Sea marine organism. Compound 1 was isolated from the sponge Polymastia sobustia and compound 2 was obtained from the soft coral Sinularia inexplicata. Their structures were established as 3 beta-hydroxy-stigmast-5en-7-one and 24-methylene cholestan -3 beta, 6 beta, 9 alpha, 19-tetrol by variety of spectral analysis such as IR, EIMS, 1DNMR, H-1-H-1 COSY, HMQC, HMBC, NOESY.展开更多
基金This work was supported by the National Natural Science Foundation of China (29973036)
文摘The title compound Fe(CH4N2S)2Cl22(C11H6N2O) (Mr = 643.35) has been prepared and its crystal structure was determined by X-ray diffraction method with the following data: triclinic, space group P1, a = 7.3742(10), b = 13.0427(12), c = 15.215(2) , a = 88.969(12), b = 78.004(12), g = 79.689(11)o, V = 1408.1(3) 3, Z = 2, Dx = 1.517 g/cm3, m = 0.912 mm-1 and F(000) = 656. The final R = 0.030 and wR = 0.078 for 4070 observed reflections (I > 2s(I)), and R = 0.064 and wR = 0.091 for 5516 independent ones. The crystal consists of tetrahedral Fe(II) complex and hydrogen bonded 4,5-diazafluoren-9-one (dafone). The carbonyl bridge in dafone distorts the bipyridine moiety and results in the longer N…N separation of 3.071(3) and 3.061(3) ? There exists an extensive intermolecular hydrogen bond network in the crystal, and p-p stacking is observed between the neighboring dafone rings.
基金This work was supported by the Natural Science Foundation of University of Jiangsu Province (No. 03KJB150118) and the Funds of Key Laboratory of Organic Synthesis of Jiangsu Province.
文摘The polymorphic isomer [Cu(dafone)2(H2O)2](Hphth)2 1 (dafone = 4,5- diazafluoren-9-one, phth = 1,2-benzenedicarboxyl) has been synthesized and the structure was determined by single-crystal X-ray diffraction. Crystal data: C38H26CuN4O12, monoclinic, space group P21/a with a = 11.5863(18), b = 25.512(4), c = 11.878(2) ?, β = 111.696(3)o, V = 3262.1(9) ?3, Mr = 794.17, Z = 4, Dc = 1.617 g/cm3, F(000) = 1628, μ = 0.748 mm-1, R = 0.0603 and wR = 0.1132 for 6878 observed reflections with I > 2σ(I). 1 consists of one [Cu(dafone)2(H2O)2]2+ cation and two monoprotonated 1,2-benzenedicarboxyl (Hphth) anions and forms a two-dimensional hydrogen bond network via intermolecular hydrogen bond interactions between the coordinated water molecules and carboxylato-oxygen atoms from monoprotonated benzenedicarboxyl anions.
文摘Two new sterol have been isolated from the South China Sea marine organism. Compound 1 was isolated from the sponge Polymastia sobustia and compound 2 was obtained from the soft coral Sinularia inexplicata. Their structures were established as 3 beta-hydroxy-stigmast-5en-7-one and 24-methylene cholestan -3 beta, 6 beta, 9 alpha, 19-tetrol by variety of spectral analysis such as IR, EIMS, 1DNMR, H-1-H-1 COSY, HMQC, HMBC, NOESY.
