The title compound C35H30Br2O3 (C32H24Br2O2·CH3COCH3) has been synthesized by the dimerization of 2-(4'-bromobenzal)-1-indenone induced by low-valent titanium reagent, and characterized by elemental analysis...The title compound C35H30Br2O3 (C32H24Br2O2·CH3COCH3) has been synthesized by the dimerization of 2-(4'-bromobenzal)-1-indenone induced by low-valent titanium reagent, and characterized by elemental analysis, IR,^1H NMR and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^- with a = 10.273(7), b = 11.036(7), c = 13.944(9) ,A°, a = 73.972(9), β =76.577(10),γ= 88.871(10)°, V = 1476.3(17)A°^3, Mr = 658.41, Z = 2, Dr = 1.481 g/cm^3, μ(MoKa) = 2.780 mm^-1, F(000) = 668, the final R = 0.0452 and wR = 0.0975. X-ray analysis reveals that the two cyclopentane rings spiro-fused each other adopt envelope conformations, while the other cyclopentane ring (C(1)--C(2)-C(7)-C(9)) is coplanar. In addition, there is a classical intermolecular hydrogen bond O(1)-H(1)...O(2) connecting the adjacent molecules into dimers.展开更多
The present paper describes the preparation of new organic reagent 2-[2-(6-chloro benzothiazolyl) azo]-resorcinol (6-CIBTAR = LH2) and used for the spectrophotometric determination of traces microgram amount of ni...The present paper describes the preparation of new organic reagent 2-[2-(6-chloro benzothiazolyl) azo]-resorcinol (6-CIBTAR = LH2) and used for the spectrophotometric determination of traces microgram amount of nickel (II) and copper (II) was found to form Ni(II)-CIBTAR at pH 7.5 giving a green coloured complex with maximum absorption at wavelength 636 nm and copper (II) was found to from Cu(II)-CIBTAR at pH 6.5 giving green bluish coloured complex with maximum absorption at wavelength 648 nm. The molar absorptivity (~) of the complexes are 0.3695 ~ 104 L.moll-cml and 0.3933 ~ 154 L'mol'l.cm1 for Ni(II) and Cu(II) respectively. Calibration curves for the determination of nickel(II) and copper (II) conformed to beers law over the concentration rang of (1-20) μg.mL-1. The DL (detection limit), RSD (relative standard deviations), RE (relative errors) and recovery for Ni(II) and Cu(II) complexes were found to be D.L = 0.45, 0.61; R.S.D% = 1.81, 2.04; Erei% = 1.3, 0.86 and Re% = 98.7, 99.14 respectively. The analytical data show the metal to reagent ratio (mole ratio method; M:L) in Ni(II) and Cu(II) complexes are 1:2.展开更多
The rare earth (RE=La, Y, Gd) salicylates were synthesized by the rheological phase reaction method. The complexes were characterized by elemental analysis, infrared spectra (IR), X-ray powder diffraction (XRD) and th...The rare earth (RE=La, Y, Gd) salicylates were synthesized by the rheological phase reaction method. The complexes were characterized by elemental analysis, infrared spectra (IR), X-ray powder diffraction (XRD) and thermal gravity analysis (TG). They can be represented by general formula RE(HSal)3 (RE=La, Y, Gd; HSal= C6H4(OH)COO). The crystals of them are monoclinic and have layered structure. The mechanism of thermal decomposition of rare earth salicylates was studied by using TG, DTA, IR and gas chromatography-mass spectrometry (GC-MS). The thermal decomposition of the rare earth salicylates in nitrogen gas proceeded in three stages: firstly, they were decomposed to form RE2(Sal)3(Sal=C6H4OCOO) and salicylic acid; then, RE2(Sal)3 were decomposed further to form RE2O(CO3)2 and some organic compounds; finally, RE2O(CO3)2 were decomposed to form rare earth metal oxides (RE2O3) and carbon dioxide. The organic compounds obtained from the second step of the reaction are mainly dibenzofuran, xanthenone, 6H-benzo[c]chromen-6-one, 6-phenyl-6H-benzo[c]chromene, and 1,3-diphenyl-1, 3-dihydro-2-benzofuran.展开更多
基金This work was supported by the Natural Science Foundation of Jiangsu Education Department (No. 03KJB 150136)
文摘The title compound C35H30Br2O3 (C32H24Br2O2·CH3COCH3) has been synthesized by the dimerization of 2-(4'-bromobenzal)-1-indenone induced by low-valent titanium reagent, and characterized by elemental analysis, IR,^1H NMR and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^- with a = 10.273(7), b = 11.036(7), c = 13.944(9) ,A°, a = 73.972(9), β =76.577(10),γ= 88.871(10)°, V = 1476.3(17)A°^3, Mr = 658.41, Z = 2, Dr = 1.481 g/cm^3, μ(MoKa) = 2.780 mm^-1, F(000) = 668, the final R = 0.0452 and wR = 0.0975. X-ray analysis reveals that the two cyclopentane rings spiro-fused each other adopt envelope conformations, while the other cyclopentane ring (C(1)--C(2)-C(7)-C(9)) is coplanar. In addition, there is a classical intermolecular hydrogen bond O(1)-H(1)...O(2) connecting the adjacent molecules into dimers.
文摘The present paper describes the preparation of new organic reagent 2-[2-(6-chloro benzothiazolyl) azo]-resorcinol (6-CIBTAR = LH2) and used for the spectrophotometric determination of traces microgram amount of nickel (II) and copper (II) was found to form Ni(II)-CIBTAR at pH 7.5 giving a green coloured complex with maximum absorption at wavelength 636 nm and copper (II) was found to from Cu(II)-CIBTAR at pH 6.5 giving green bluish coloured complex with maximum absorption at wavelength 648 nm. The molar absorptivity (~) of the complexes are 0.3695 ~ 104 L.moll-cml and 0.3933 ~ 154 L'mol'l.cm1 for Ni(II) and Cu(II) respectively. Calibration curves for the determination of nickel(II) and copper (II) conformed to beers law over the concentration rang of (1-20) μg.mL-1. The DL (detection limit), RSD (relative standard deviations), RE (relative errors) and recovery for Ni(II) and Cu(II) complexes were found to be D.L = 0.45, 0.61; R.S.D% = 1.81, 2.04; Erei% = 1.3, 0.86 and Re% = 98.7, 99.14 respectively. The analytical data show the metal to reagent ratio (mole ratio method; M:L) in Ni(II) and Cu(II) complexes are 1:2.
基金Project supported by the Natural Science Foundation of Hubei Education Committee (No. 2003A010) and Introducing Able Person Foundation of Zhejiang Normal University.
文摘The rare earth (RE=La, Y, Gd) salicylates were synthesized by the rheological phase reaction method. The complexes were characterized by elemental analysis, infrared spectra (IR), X-ray powder diffraction (XRD) and thermal gravity analysis (TG). They can be represented by general formula RE(HSal)3 (RE=La, Y, Gd; HSal= C6H4(OH)COO). The crystals of them are monoclinic and have layered structure. The mechanism of thermal decomposition of rare earth salicylates was studied by using TG, DTA, IR and gas chromatography-mass spectrometry (GC-MS). The thermal decomposition of the rare earth salicylates in nitrogen gas proceeded in three stages: firstly, they were decomposed to form RE2(Sal)3(Sal=C6H4OCOO) and salicylic acid; then, RE2(Sal)3 were decomposed further to form RE2O(CO3)2 and some organic compounds; finally, RE2O(CO3)2 were decomposed to form rare earth metal oxides (RE2O3) and carbon dioxide. The organic compounds obtained from the second step of the reaction are mainly dibenzofuran, xanthenone, 6H-benzo[c]chromen-6-one, 6-phenyl-6H-benzo[c]chromene, and 1,3-diphenyl-1, 3-dihydro-2-benzofuran.