The title compound (C28H27NO5S3, Mr= 553. 69) was prepared bythe reaction of a-thiobenzoylthioformmorholine with diethyl acetylene dicarboxylate.The crystal is monoclinic, space group P21/n with a= 9. 160(3), b= 17. 7...The title compound (C28H27NO5S3, Mr= 553. 69) was prepared bythe reaction of a-thiobenzoylthioformmorholine with diethyl acetylene dicarboxylate.The crystal is monoclinic, space group P21/n with a= 9. 160(3), b= 17. 726(3), c=16. 602(3) A ; β= 100. 375(13)°; V=2651. 4(10) A3, Z=4, Dc= 1. 387 g/cm3, μ(MoKa) =0. 319 mm-1, F(000) =1160, R=0. 0428, wR(F2) =0. 0910 for 2438 observed reflections (I】2(I)). X-ray analysis reveals that interatomic distances for C(5)-C(6), C(13)-C(14) and C(21)-C(22) are 1. 331(4), 1. 351(4), 1. 344(4)A respectively, which show that they are normal C=C double bonds. All S-C bondlengths are similar to typical S-C single bonds (1. 75 - 1. 78 A ). The five-membered ring A (C(5) -C(6) -S(2)-C(13) -S(1) ) (Fig. 1) and six-membered ringB (C(14) -C(15) -C(20) -C(21)-C(22)-S(3) ) (Fig. 1) adopt the flat twist conformation. Furthermore, the morpholine ring adopts chair conformtion.展开更多
The mixed-ligand complexes of molybdenum(VI) with dithiolphenols (DP) {2,6-dithiol-4-methylphenol (DTMP), 2,6-dithiol-4-ethylphenol (DTEP) and 2,6-dithiol-4-tert-butylphenol (DTBP)} in the presence of hydrophobic amin...The mixed-ligand complexes of molybdenum(VI) with dithiolphenols (DP) {2,6-dithiol-4-methylphenol (DTMP), 2,6-dithiol-4-ethylphenol (DTEP) and 2,6-dithiol-4-tert-butylphenol (DTBP)} in the presence of hydrophobic amines have been investigated by spectrophotometric method. The condition of complexing and extraction, physical-chemical and analytical characteristics of this complex have been found. As hydrophobic amine 2(N, N-dimethylaminomethyl)-4-methylrphenol (АP1) and 2(N, N-dimethylaminomethyl)-4-xlor-phenol (AP2), 2 (N, N-dimethylamino-methyl)-4-brom-phenol (AP3) were used. It has been found that mixed-ligand complex was formed in weakly acidic medium (pH 4.1 - 5.9). The maximum analytical signal when complexing Mo(V) is observed at 516 - 534 nm. The calculated molar absorption (εmax) belongs to the range (4.16 - 5.35) × 104. The Beer’s law was applicable in the range of 0.3 - 22 μg/ml. The extraction photometric methods of the molybdenum determination were processed. The influence of diverse ions on determination of molybdenum has been studied. The proposed method was applied successfully to determine amount of molybdenum in steel and in soil.展开更多
We report an electrochemically assisted mechanically controllable break junction （EC-MCBJ） approach to investigating single molecule conductance. Electrode pairs connected with a gold nanobridge were fabricated by e...We report an electrochemically assisted mechanically controllable break junction （EC-MCBJ） approach to investigating single molecule conductance. Electrode pairs connected with a gold nanobridge were fabricated by electrochemical deposition and then mounted on a homebuilt MCBJ platform. A large number of Au- molecule-Au junctions were produced sequentially by repeated breaking and reconnecting of the gold nanobridge. In order to measure their single molecule conductance, statistical conductance histograms were generated for benzene-l,4-dithiol （BDT） and 4,4＇-bipyridine （BPY）. The values extracted from these histograms were found to be in the same range as values previously reported in the literature. Our method is distinct from the ones used to acquire these previously reported literature values, however, in that it is faster, simpler, more cost-effective, and changing the electrode material is more convenient.展开更多
文摘The title compound (C28H27NO5S3, Mr= 553. 69) was prepared bythe reaction of a-thiobenzoylthioformmorholine with diethyl acetylene dicarboxylate.The crystal is monoclinic, space group P21/n with a= 9. 160(3), b= 17. 726(3), c=16. 602(3) A ; β= 100. 375(13)°; V=2651. 4(10) A3, Z=4, Dc= 1. 387 g/cm3, μ(MoKa) =0. 319 mm-1, F(000) =1160, R=0. 0428, wR(F2) =0. 0910 for 2438 observed reflections (I】2(I)). X-ray analysis reveals that interatomic distances for C(5)-C(6), C(13)-C(14) and C(21)-C(22) are 1. 331(4), 1. 351(4), 1. 344(4)A respectively, which show that they are normal C=C double bonds. All S-C bondlengths are similar to typical S-C single bonds (1. 75 - 1. 78 A ). The five-membered ring A (C(5) -C(6) -S(2)-C(13) -S(1) ) (Fig. 1) and six-membered ringB (C(14) -C(15) -C(20) -C(21)-C(22)-S(3) ) (Fig. 1) adopt the flat twist conformation. Furthermore, the morpholine ring adopts chair conformtion.
文摘The mixed-ligand complexes of molybdenum(VI) with dithiolphenols (DP) {2,6-dithiol-4-methylphenol (DTMP), 2,6-dithiol-4-ethylphenol (DTEP) and 2,6-dithiol-4-tert-butylphenol (DTBP)} in the presence of hydrophobic amines have been investigated by spectrophotometric method. The condition of complexing and extraction, physical-chemical and analytical characteristics of this complex have been found. As hydrophobic amine 2(N, N-dimethylaminomethyl)-4-methylrphenol (АP1) and 2(N, N-dimethylaminomethyl)-4-xlor-phenol (AP2), 2 (N, N-dimethylamino-methyl)-4-brom-phenol (AP3) were used. It has been found that mixed-ligand complex was formed in weakly acidic medium (pH 4.1 - 5.9). The maximum analytical signal when complexing Mo(V) is observed at 516 - 534 nm. The calculated molar absorption (εmax) belongs to the range (4.16 - 5.35) × 104. The Beer’s law was applicable in the range of 0.3 - 22 μg/ml. The extraction photometric methods of the molybdenum determination were processed. The influence of diverse ions on determination of molybdenum has been studied. The proposed method was applied successfully to determine amount of molybdenum in steel and in soil.
文摘We report an electrochemically assisted mechanically controllable break junction （EC-MCBJ） approach to investigating single molecule conductance. Electrode pairs connected with a gold nanobridge were fabricated by electrochemical deposition and then mounted on a homebuilt MCBJ platform. A large number of Au- molecule-Au junctions were produced sequentially by repeated breaking and reconnecting of the gold nanobridge. In order to measure their single molecule conductance, statistical conductance histograms were generated for benzene-l,4-dithiol （BDT） and 4,4＇-bipyridine （BPY）. The values extracted from these histograms were found to be in the same range as values previously reported in the literature. Our method is distinct from the ones used to acquire these previously reported literature values, however, in that it is faster, simpler, more cost-effective, and changing the electrode material is more convenient.
