The preparation of peroxodisulfated zirconia titania(PSZT) solid super acid has been investigated as function of molar ratio of Ti to Zr, impregnation time, calcination time and temperature in esterification of maleic...The preparation of peroxodisulfated zirconia titania(PSZT) solid super acid has been investigated as function of molar ratio of Ti to Zr, impregnation time, calcination time and temperature in esterification of maleic anhydride with n octanol. The highest yield of dioctyl maleate was 98 2% at the optimum reaction conditions.展开更多
The novel seven coordinate complex [(n Bu)2Sn(C10H8N2O3)(C2H5OH)]2 (C10H8N2O32- is the dinegative ion of 2 oxo propionic acid benzoyl hydrazone) was synthesized by the reaction of (n Bu)2SnO with 2 oxo propionic acid ...The novel seven coordinate complex [(n Bu)2Sn(C10H8N2O3)(C2H5OH)]2 (C10H8N2O32- is the dinegative ion of 2 oxo propionic acid benzoyl hydrazone) was synthesized by the reaction of (n Bu)2SnO with 2 oxo propionic acid benzoyl hydrazone in 1∶ 1 molar ratio in benzene ethanol (V/V, 3/1), and its structure was characterized by X ray single crystal diffraction. The crystal belongs to a tetragonal system with space group I41/a, a=2.4890(2)nm, b=2.4890(2)nm, c=1.5170(3)nm, V=9.398(2)nm3, Z=8, F(000)=3968, Dc=1.366g· cm- 3, and the structure was refined to final R1=0.0530, wR2=0.0971. The structure of the title complex is described as a dimer through weak interactions of Sn… O bonding and hydrogen bond. The tin atoms rendered seven coordination in a distorted pentagonal bipyramid geometry structure, four oxygen atoms [O1, O2, O2# 1 and O4] and one nitrogen atom N2 formed the equatorial plane and C11 Sn1 C15 is the axis. CCDC: 212696.展开更多
We reported the synthesis of [Ni（hmta）][SSP(OC10H7-2)2]2(where hmta is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,and 2-C10H7O-is 2-nathphthyloxy).The complex is characterized by elemental analysis,...We reported the synthesis of [Ni（hmta）][SSP(OC10H7-2)2]2(where hmta is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,and 2-C10H7O-is 2-nathphthyloxy).The complex is characterized by elemental analysis,IR spectra,1HNMR spectra,electronic spectra and TG-DTA thermal analysis,and its crystal structure has been determined.The compound belongs to triclinic system,space group P ī with the following crystallographic parameters:a=7.691（2）,b=10.505（5）,c=17.692（5）,α=105.52（3）°,β=90.09（3）°,γ=103.92（4）°,V=1333.5（8）3,DC=1.377g/cm3,F（000）=582,μ（Mo Kα）=0.631mm-1,Z=1,and final R=0.0752,wR=0.1957 for 2425 observed reflections（I>2σ（I））.The analytical results of crystal structure and spectroscopic properties show that a square planar complex cation [Ni（hmta）]2+ is formed by coordination of four nitrogen atoms of ligand hmta to Ni（Ⅱ）.There isn’t interaction of Ni（Ⅱ） with sulfur atom of (2—C10H7O)2PSS-anion,but there are three N-H…S hydrogen bonds between [Ni（hmta）]2+ complex cation and(2—C10H7O)2PSS-anion in the compound.展开更多
Binuclear Copper (Ⅰ) Complex {Cu [ WS2P(C2H5O)2] (C10H8N2) } 2 was synthesized and characterized by elemental analysis, IR and X-ray diffraction analysis. The crystal belongs to triclinic system, space group P1 with ...Binuclear Copper (Ⅰ) Complex {Cu [ WS2P(C2H5O)2] (C10H8N2) } 2 was synthesized and characterized by elemental analysis, IR and X-ray diffraction analysis. The crystal belongs to triclinic system, space group P1 with Z = l, cell dimentions are a = 1. 0613 (5), b = 1. 0723 (3), c = 0. 9397 (2) um, a = 111. 11 (4), β = 115. 57(6), y = 85. 28(2)", V= 0. 8583(6) "nm3. The structure was refined to R = 0. 039 and Rw = 0. 042 for 2527 reflection with Ⅰ > 36(Ⅰ). The complex exists as a centrosymmetric dimer with a Cu-S-P-S-Cu-S-P-S chair eight-membered ring in which Cu atoms are bridged by di-AS-P-S groups.展开更多
The adductive reaction of Ni[S2P(OCH2CH2Ph)2]2 with pyridine was studied by spectrographic method and the equilibrium constants was found to be β1=(1.12±0.09)×102,β2=(2.40±0.41)×104,R1=0.997,R2=0...The adductive reaction of Ni[S2P(OCH2CH2Ph)2]2 with pyridine was studied by spectrographic method and the equilibrium constants was found to be β1=(1.12±0.09)×102,β2=(2.40±0.41)×104,R1=0.997,R2=0.998.The adduct Ni[S2P(OCH2CH2Ph)2]2·2Py was characterized by elemental analysis,IR spectra,single-crystal X-ray diffraction method.The crystal structure belongs to monoclinic system,space group P 21/c with the following crystallographic parameters:a=9.240(3),b=16.124(8),c=14.148(7),α=90.00°,β=92.07(4)°,γ=90.00°.展开更多
Oxidation process of Co(C 6 H 11 O) 2 PS 2 2 and substitute-reduction reaction of Co C 6 H 11 O) 2 PS 2 3 with pyridine have been studied by spectrophotome tric methods,respectively.The equ ilibrium constant was found...Oxidation process of Co(C 6 H 11 O) 2 PS 2 2 and substitute-reduction reaction of Co C 6 H 11 O) 2 PS 2 3 with pyridine have been studied by spectrophotome tric methods,respectively.The equ ilibrium constant was found to be K=0.63±0.02(mol·dm -3 ) -3 .The crystal structure of Co 6 H 11 O) 2 PS 2 2·2Py has been determined by X-ray diff-raction method.The crystal belongs to triclinic system,space groupP1,with cell parameters:a=6.944(2)?,b=9.277(3)?,c=15.981(6)?,α=91.79(3)°,β=99.55(3)°,γ=94.44(3)°,V=1011.2(6)? 3 ,Z =2,M r =803.94,D c =1.320Mg ·m -3 ,F(000)=425,μ=0.747mm -1 ,final R=0.0700and w R=0.1988for 3626re-flections with I≥2σ(I).The cobalt atom in the title complex has a octahedral geometry with four Co-S bonds and two Co-N bonds.The central atom P is t etrahedrally surrounded by two sulp hur atoms and two oxygen atoms in the dicyclohexyldithiophosphate liga nd.The six carbon atoms of cyclohexyl take the chair conformation.展开更多
文摘The preparation of peroxodisulfated zirconia titania(PSZT) solid super acid has been investigated as function of molar ratio of Ti to Zr, impregnation time, calcination time and temperature in esterification of maleic anhydride with n octanol. The highest yield of dioctyl maleate was 98 2% at the optimum reaction conditions.
文摘The novel seven coordinate complex [(n Bu)2Sn(C10H8N2O3)(C2H5OH)]2 (C10H8N2O32- is the dinegative ion of 2 oxo propionic acid benzoyl hydrazone) was synthesized by the reaction of (n Bu)2SnO with 2 oxo propionic acid benzoyl hydrazone in 1∶ 1 molar ratio in benzene ethanol (V/V, 3/1), and its structure was characterized by X ray single crystal diffraction. The crystal belongs to a tetragonal system with space group I41/a, a=2.4890(2)nm, b=2.4890(2)nm, c=1.5170(3)nm, V=9.398(2)nm3, Z=8, F(000)=3968, Dc=1.366g· cm- 3, and the structure was refined to final R1=0.0530, wR2=0.0971. The structure of the title complex is described as a dimer through weak interactions of Sn… O bonding and hydrogen bond. The tin atoms rendered seven coordination in a distorted pentagonal bipyramid geometry structure, four oxygen atoms [O1, O2, O2# 1 and O4] and one nitrogen atom N2 formed the equatorial plane and C11 Sn1 C15 is the axis. CCDC: 212696.
文摘We reported the synthesis of [Ni（hmta）][SSP(OC10H7-2)2]2(where hmta is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,and 2-C10H7O-is 2-nathphthyloxy).The complex is characterized by elemental analysis,IR spectra,1HNMR spectra,electronic spectra and TG-DTA thermal analysis,and its crystal structure has been determined.The compound belongs to triclinic system,space group P ī with the following crystallographic parameters:a=7.691（2）,b=10.505（5）,c=17.692（5）,α=105.52（3）°,β=90.09（3）°,γ=103.92（4）°,V=1333.5（8）3,DC=1.377g/cm3,F（000）=582,μ（Mo Kα）=0.631mm-1,Z=1,and final R=0.0752,wR=0.1957 for 2425 observed reflections（I>2σ（I））.The analytical results of crystal structure and spectroscopic properties show that a square planar complex cation [Ni（hmta）]2+ is formed by coordination of four nitrogen atoms of ligand hmta to Ni（Ⅱ）.There isn’t interaction of Ni（Ⅱ） with sulfur atom of (2—C10H7O)2PSS-anion,but there are three N-H…S hydrogen bonds between [Ni（hmta）]2+ complex cation and(2—C10H7O)2PSS-anion in the compound.
文摘Binuclear Copper (Ⅰ) Complex {Cu [ WS2P(C2H5O)2] (C10H8N2) } 2 was synthesized and characterized by elemental analysis, IR and X-ray diffraction analysis. The crystal belongs to triclinic system, space group P1 with Z = l, cell dimentions are a = 1. 0613 (5), b = 1. 0723 (3), c = 0. 9397 (2) um, a = 111. 11 (4), β = 115. 57(6), y = 85. 28(2)", V= 0. 8583(6) "nm3. The structure was refined to R = 0. 039 and Rw = 0. 042 for 2527 reflection with Ⅰ > 36(Ⅰ). The complex exists as a centrosymmetric dimer with a Cu-S-P-S-Cu-S-P-S chair eight-membered ring in which Cu atoms are bridged by di-AS-P-S groups.
文摘The adductive reaction of Ni[S2P(OCH2CH2Ph)2]2 with pyridine was studied by spectrographic method and the equilibrium constants was found to be β1=(1.12±0.09)×102,β2=(2.40±0.41)×104,R1=0.997,R2=0.998.The adduct Ni[S2P(OCH2CH2Ph)2]2·2Py was characterized by elemental analysis,IR spectra,single-crystal X-ray diffraction method.The crystal structure belongs to monoclinic system,space group P 21/c with the following crystallographic parameters:a=9.240(3),b=16.124(8),c=14.148(7),α=90.00°,β=92.07(4)°,γ=90.00°.
文摘Oxidation process of Co(C 6 H 11 O) 2 PS 2 2 and substitute-reduction reaction of Co C 6 H 11 O) 2 PS 2 3 with pyridine have been studied by spectrophotome tric methods,respectively.The equ ilibrium constant was found to be K=0.63±0.02(mol·dm -3 ) -3 .The crystal structure of Co 6 H 11 O) 2 PS 2 2·2Py has been determined by X-ray diff-raction method.The crystal belongs to triclinic system,space groupP1,with cell parameters:a=6.944(2)?,b=9.277(3)?,c=15.981(6)?,α=91.79(3)°,β=99.55(3)°,γ=94.44(3)°,V=1011.2(6)? 3 ,Z =2,M r =803.94,D c =1.320Mg ·m -3 ,F(000)=425,μ=0.747mm -1 ,final R=0.0700and w R=0.1988for 3626re-flections with I≥2σ(I).The cobalt atom in the title complex has a octahedral geometry with four Co-S bonds and two Co-N bonds.The central atom P is t etrahedrally surrounded by two sulp hur atoms and two oxygen atoms in the dicyclohexyldithiophosphate liga nd.The six carbon atoms of cyclohexyl take the chair conformation.
