The crystal structure of the title compound, diethyl 5-acetoxy-3-（4-chlorophenyl）-4,5- dihydroisoxazol-5-yl-5-phosphonate （C15H19CINO6P, Mr = 375.73）, has been synthesized by the treatment of nitrile oxides and l-...The crystal structure of the title compound, diethyl 5-acetoxy-3-（4-chlorophenyl）-4,5- dihydroisoxazol-5-yl-5-phosphonate （C15H19CINO6P, Mr = 375.73）, has been synthesized by the treatment of nitrile oxides and l-acetyloxy-vinylphosphonate under very mild conditions in good yields, and determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group C2/c with a = 16.914（10）, b = 10.567（7）, c = 21.927（13） A, β = 110.249（11）°, V = 3677（4） A^3, Z = 8, Dc = 1.358 g/cm^3, F（000） = 1568,/l（MoKa） = 0.324 mm^-1）, S = 1.011, the final R = 0.0661 and wR = 0.1556. The X-ray analytic results showed that the dihedral angle between the phenyl group and the isoxazoline ring is 10.7°.展开更多
Two novel transition metal phosphonate compounds, [Co（H2BDPP）（phen）]n 1 （BDPP = p-O3PCH2（C6H4）CH2PO3, phen = 1,10-phenanthroline） and [Pb3（BCP）2]n 2 （BCP = OOC（C6H4）CH2PO3）, have been synthesized and str...Two novel transition metal phosphonate compounds, [Co（H2BDPP）（phen）]n 1 （BDPP = p-O3PCH2（C6H4）CH2PO3, phen = 1,10-phenanthroline） and [Pb3（BCP）2]n 2 （BCP = OOC（C6H4）CH2PO3）, have been synthesized and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in the monoclinic system, space group C2/c with a = 21.169（4）, b = 12.001（2）, c = 7.6211（15）A, β = 98.03（3）°, V= 1917.2（6）A^3, C20H18N2O6P2Co, Mr = 505.22, Z = 8, De= 1.737 g/cm^3, p = 1.107 mm^-1, F（000） = 1020, the final R= 0.0450 and wR = 0.1306 for 2072 observed reflections （I 〉 2σ（I）. Compound 2 crystallizes in the monoclinic system, space group C2/c with a = 4.7167（9）, b = 18.753（2）, c = 22.781（3）A, β = 91.07（3）°, V= 2014.7（14）A^, C8H6O5PPb1.5, Mr = 523.88, Z = 8, Dc = 3.454 g/cm^3, p = 25.222 mm^-1, F（000） = 1856, the final R = 0.0441 and wR = 0.1906 for 2259 observed reflections （I 〉 2σ（I）. In compound 1, the 1D chain running along the c axis is bridged by four ligands （trans- HO3PCH2C6H4CH2PO3H） in four different directions to extend the structure into a three- dimensional network. In compound 2, the Pb（II） displays 4- and 5-coordination modes. There is a one-dimensional P-O-Pb band along the a axis formed by PO3 groups and Pb（II） cations. These bands are joined by μ2-O of -COO to yield two-dimensional inorganic P-O-Pb layers which are pillared by the OOCC6HaCH2PO3 ligands to form a three-dimensional network. Moreover, compound 2 displays a strong emission band attributed to the ligand-centered （LC） transition.展开更多
When N-cyanoimido-(O,O-diethyl)phosphonyl/S-methyl thiocarbonate (1) was treated with o-phenylenediamine in the presence of Et3N in ethanol, diethyl benzimidazole-2-yl phosphonate (2) was obtained and hydrolyzed durin...When N-cyanoimido-(O,O-diethyl)phosphonyl/S-methyl thiocarbonate (1) was treated with o-phenylenediamine in the presence of Et3N in ethanol, diethyl benzimidazole-2-yl phosphonate (2) was obtained and hydrolyzed during the recrystallization in MeOH/H2O, generating ethyl benzimidazole-2-yl phosphonate (3). The crystal structure of compound 3 was determined by X-ray diffraction method. The crystals belong to monoclinic, space group C2/c, a = 1.78406(18), b = 0. 83725(9), c= 1.67401(18) nm, β= 118.997(2)°, V = 2. 1870(4) nm3Z = 8, Dc = 1.374 g/cm3, F(000) = 944. The final R and wR are 0.0499 and 0.1436, respectively. The mechanism of the above reaction is also discussed.展开更多
文摘The crystal structure of the title compound, diethyl 5-acetoxy-3-（4-chlorophenyl）-4,5- dihydroisoxazol-5-yl-5-phosphonate （C15H19CINO6P, Mr = 375.73）, has been synthesized by the treatment of nitrile oxides and l-acetyloxy-vinylphosphonate under very mild conditions in good yields, and determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group C2/c with a = 16.914（10）, b = 10.567（7）, c = 21.927（13） A, β = 110.249（11）°, V = 3677（4） A^3, Z = 8, Dc = 1.358 g/cm^3, F（000） = 1568,/l（MoKa） = 0.324 mm^-1）, S = 1.011, the final R = 0.0661 and wR = 0.1556. The X-ray analytic results showed that the dihedral angle between the phenyl group and the isoxazoline ring is 10.7°.
基金supported by the State Key Laboratory of Structural Chemistry, National Natural Science Foundation of China (20873021)the Young Talent Programmed of Fujian Province (No. 2006F3072)
文摘Two novel transition metal phosphonate compounds, [Co（H2BDPP）（phen）]n 1 （BDPP = p-O3PCH2（C6H4）CH2PO3, phen = 1,10-phenanthroline） and [Pb3（BCP）2]n 2 （BCP = OOC（C6H4）CH2PO3）, have been synthesized and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in the monoclinic system, space group C2/c with a = 21.169（4）, b = 12.001（2）, c = 7.6211（15）A, β = 98.03（3）°, V= 1917.2（6）A^3, C20H18N2O6P2Co, Mr = 505.22, Z = 8, De= 1.737 g/cm^3, p = 1.107 mm^-1, F（000） = 1020, the final R= 0.0450 and wR = 0.1306 for 2072 observed reflections （I 〉 2σ（I）. Compound 2 crystallizes in the monoclinic system, space group C2/c with a = 4.7167（9）, b = 18.753（2）, c = 22.781（3）A, β = 91.07（3）°, V= 2014.7（14）A^, C8H6O5PPb1.5, Mr = 523.88, Z = 8, Dc = 3.454 g/cm^3, p = 25.222 mm^-1, F（000） = 1856, the final R = 0.0441 and wR = 0.1906 for 2259 observed reflections （I 〉 2σ（I）. In compound 1, the 1D chain running along the c axis is bridged by four ligands （trans- HO3PCH2C6H4CH2PO3H） in four different directions to extend the structure into a three- dimensional network. In compound 2, the Pb（II） displays 4- and 5-coordination modes. There is a one-dimensional P-O-Pb band along the a axis formed by PO3 groups and Pb（II） cations. These bands are joined by μ2-O of -COO to yield two-dimensional inorganic P-O-Pb layers which are pillared by the OOCC6HaCH2PO3 ligands to form a three-dimensional network. Moreover, compound 2 displays a strong emission band attributed to the ligand-centered （LC） transition.
基金Project (No. 29772020) supported by the National Natural Science Foundation of China
文摘When N-cyanoimido-(O,O-diethyl)phosphonyl/S-methyl thiocarbonate (1) was treated with o-phenylenediamine in the presence of Et3N in ethanol, diethyl benzimidazole-2-yl phosphonate (2) was obtained and hydrolyzed during the recrystallization in MeOH/H2O, generating ethyl benzimidazole-2-yl phosphonate (3). The crystal structure of compound 3 was determined by X-ray diffraction method. The crystals belong to monoclinic, space group C2/c, a = 1.78406(18), b = 0. 83725(9), c= 1.67401(18) nm, β= 118.997(2)°, V = 2. 1870(4) nm3Z = 8, Dc = 1.374 g/cm3, F(000) = 944. The final R and wR are 0.0499 and 0.1436, respectively. The mechanism of the above reaction is also discussed.
