Two title compounds, 4,4?diformyl-diphenoxyethane (compound 1, C16H14O4) and 4,4?4创-triformyl-triphenoxytriethylamine (compound 2, C27H27NO6), were synthesized by condensation of 4-hydroxybenzaldehyde with 1,2-dichlo...Two title compounds, 4,4?diformyl-diphenoxyethane (compound 1, C16H14O4) and 4,4?4创-triformyl-triphenoxytriethylamine (compound 2, C27H27NO6), were synthesized by condensation of 4-hydroxybenzaldehyde with 1,2-dichloroethane and tris(2-chloroethyl)amine, respectively in dimethyl formamide in the presence of anhydrous potassium carbonate. The crystal data are: monoclinic, P21/c, a = 7.571(2), b = 12.608(3), c = 7.357(2) ? b = 105.823(6)? V = 675.7(2) 3, Mr = 270.3, Z = 2, Dc = 1.328 g/cm3, F(000) = 284, m(MoKa) = 0.096 mm-1, R = 0.0537 and wR = 0.2189 for compound 1; and monoclinic, P21/n, a = 11.7162(6), b = 9.0042(6), c = 22.908(2) ? b = 99.505(1)? V = 2383.5(3) ?, Mr = 461.50, Z = 4, Dc = 1.286 g/cm3, F(000)= 976, m(MoKa) = 0.091 mm-1, R = 0.0464 and wR = 0.1462 for compound 2. The molecule of compound 1 (dialdehyde) is located at the crystallographic inversion center nearby the midpoint of C(8)C(8A) single bond. The three chains in the molecule of compound 2 (trialdehyde) are of non-crystallographic pseudo-C3 symmetry, and each of them is quite planar.展开更多
C_(86)H_(72)Cl_(20)Ni_6S_(12) , Mr = 2551. 62, monoclinic, space group C2/c, crystal data: a = 30. 322(5), b=14. 168(3), c=26. 453(4) A ,β=101. 00(4)°, V = 11155. 6 A3, Z=4, Dx=1. 519 g/cm3, λ(MoKα) = 0. 71069...C_(86)H_(72)Cl_(20)Ni_6S_(12) , Mr = 2551. 62, monoclinic, space group C2/c, crystal data: a = 30. 322(5), b=14. 168(3), c=26. 453(4) A ,β=101. 00(4)°, V = 11155. 6 A3, Z=4, Dx=1. 519 g/cm3, λ(MoKα) = 0. 71069 A ,μ=17. 370 cm-1, F(000) = 5152, T = 293 K, final R = 0. 078, Rw = 0. 086 for 5610 (I>3σ(I)) reflections. The crystal is composed of discrete [Ni (SCH2C6H4Cl-p)2]6 and CCl4 solvent molecules. The coordination geometries of the Ni atoms are perfect planes sharing S...S edges. The six NiS4 squares are linked with each other forming a hexagonal prism. The p-ClC6H4CH2S- side chains in the molecule are arranged in the axial and equatorial positions alternately with respect to the pseudo-hexagonal axis of the molecule.展开更多
基金The authors thank the financial support of the Natural Science Foundation of Fujian Province (No. E0110010)
文摘Two title compounds, 4,4?diformyl-diphenoxyethane (compound 1, C16H14O4) and 4,4?4创-triformyl-triphenoxytriethylamine (compound 2, C27H27NO6), were synthesized by condensation of 4-hydroxybenzaldehyde with 1,2-dichloroethane and tris(2-chloroethyl)amine, respectively in dimethyl formamide in the presence of anhydrous potassium carbonate. The crystal data are: monoclinic, P21/c, a = 7.571(2), b = 12.608(3), c = 7.357(2) ? b = 105.823(6)? V = 675.7(2) 3, Mr = 270.3, Z = 2, Dc = 1.328 g/cm3, F(000) = 284, m(MoKa) = 0.096 mm-1, R = 0.0537 and wR = 0.2189 for compound 1; and monoclinic, P21/n, a = 11.7162(6), b = 9.0042(6), c = 22.908(2) ? b = 99.505(1)? V = 2383.5(3) ?, Mr = 461.50, Z = 4, Dc = 1.286 g/cm3, F(000)= 976, m(MoKa) = 0.091 mm-1, R = 0.0464 and wR = 0.1462 for compound 2. The molecule of compound 1 (dialdehyde) is located at the crystallographic inversion center nearby the midpoint of C(8)C(8A) single bond. The three chains in the molecule of compound 2 (trialdehyde) are of non-crystallographic pseudo-C3 symmetry, and each of them is quite planar.
文摘C_(86)H_(72)Cl_(20)Ni_6S_(12) , Mr = 2551. 62, monoclinic, space group C2/c, crystal data: a = 30. 322(5), b=14. 168(3), c=26. 453(4) A ,β=101. 00(4)°, V = 11155. 6 A3, Z=4, Dx=1. 519 g/cm3, λ(MoKα) = 0. 71069 A ,μ=17. 370 cm-1, F(000) = 5152, T = 293 K, final R = 0. 078, Rw = 0. 086 for 5610 (I>3σ(I)) reflections. The crystal is composed of discrete [Ni (SCH2C6H4Cl-p)2]6 and CCl4 solvent molecules. The coordination geometries of the Ni atoms are perfect planes sharing S...S edges. The six NiS4 squares are linked with each other forming a hexagonal prism. The p-ClC6H4CH2S- side chains in the molecule are arranged in the axial and equatorial positions alternately with respect to the pseudo-hexagonal axis of the molecule.
