Dibenzoyl peroxide undergoes oxidative addition on metallic copper powder with 2,2′-bipyridine(or imidazole)in a mixed solvent(methanol and tetrahydrofuran),and affords the Cu(Ⅱ)complexes-[Cu(Ce(C_6H_5COO)_2(2,2'...Dibenzoyl peroxide undergoes oxidative addition on metallic copper powder with 2,2′-bipyridine(or imidazole)in a mixed solvent(methanol and tetrahydrofuran),and affords the Cu(Ⅱ)complexes-[Cu(Ce(C_6H_5COO)_2(2,2'-bipy)]H_2O(1) and[Cu(C_6H_5COO)_2(C_3H_4N_2)_2](2).The structure was solved by direct methods and Fourier synthesis.C_(24)H_(20)N_2O_5Cu (1),Mr=479.78,space group P2(1)/c,a=6.986(7), b=18.833(I),c=17.021(3),α=γ=90°,Z=4,V=2218.1~3,Dc=1.443g/cm\+3,R=0.055 Rw=0.062.Complex(2),C_(20)H_(18)N_4O_4Cu(2),Mr=441.74,space group P2(1)/n,a=8.699(4), b=9.840(6),c=12.399(5),α=γ=90°,β=100.8°,Z=4,V=1010.9~3,Dc=1.654g/cm\+3,R=0.055, Rw=0.062.展开更多
At room temperature, dibenzoyl peroxide and pyridine N-oxide reacted with metallic copper powder in a mixed solvent(dichloromethane, trichloromethane and tetrahydrofuran), resulting in a binuclear copper(Ⅱ) complex. ...At room temperature, dibenzoyl peroxide and pyridine N-oxide reacted with metallic copper powder in a mixed solvent(dichloromethane, trichloromethane and tetrahydrofuran), resulting in a binuclear copper(Ⅱ) complex. [Cu (C_5H_5NO)-(C_6H_5COO)_2]_2. The structure of the complex was characterized by elemental analyses.IR spectra and X-ray single crystal analysis. The crystal is triclinic, space group P1,with cell parameters . a= 9. 262(4) ,b= 10. 697(2) , c=10. 881 (3 )A , a=59. 60( 2 ),β= 74. 83 ( 3 ) .Y = 72. 80 ( 2 )°. V= 880. 0 A ̄3 . D_c = 1 . 5 20 g/cm ̄3 . Z = 1 . μ= 1 2. 7 cm-1, R=0. 044 ,R_w=0. 048 for 3477 reflections with I>3σ(I), M_r=805. 78. Each copper(Ⅱ) atom is coordinated by four bridging bidentate benzoate ligands and one pyridine M-oxide.展开更多
At room temperature, the reaction of dibenzoyl peroxide with metallic copper powder in the presence of pyridine affords the copper(Ⅱ) complex [Cu(C 5H 5N) 2(H 2O)\|(C 6H 5COO) 2]. Crystal is monoclinic, M r =483.002,...At room temperature, the reaction of dibenzoyl peroxide with metallic copper powder in the presence of pyridine affords the copper(Ⅱ) complex [Cu(C 5H 5N) 2(H 2O)\|(C 6H 5COO) 2]. Crystal is monoclinic, M r =483.002, space group Cc with parameters: a=6\^078(4), b=15.879(4), c=23.091(3), β=97.61(2)°, V=2209.1(2) 3, Z=4, D c =1\^464g/cm 3, μ =10.279 cm -1 , F(000)=996, R=0\^031, R w =0.036, 1595 reflections with I≥3σ(I ) were considered to be observed. Each copper(Ⅱ) ion is coordinated by two monodentate benzoate ligands, two pyridines and one water molecule. The complex is also characterized by its IR, XPS and thermal properties.展开更多
Reaction of Cu with dibenzovi peroxide, 2-aminothiazol gave a binuclear complex [Cu_2 (C_6H_5COO)_4(C_3H_4N_2S)_2]. Crystal of the title compound is monoclinic system space group P2_1/n , M_r = 807. 84 with cell param...Reaction of Cu with dibenzovi peroxide, 2-aminothiazol gave a binuclear complex [Cu_2 (C_6H_5COO)_4(C_3H_4N_2S)_2]. Crystal of the title compound is monoclinic system space group P2_1/n , M_r = 807. 84 with cell parameters a= 10. 685 ( 1 ), b=19. 028(6), c=17. 046(9) , β=96. 49(33) ̄°, Z=4, V=3443. 4, D_c=1. 565 g/cm ̄-3, μ= 14. 078 cm ̄-1, F(000)= 824. The final refinement with 3429 observed reflections is converged with R= 0. 046 and R_w=0. 053. X-ray crystal structure analysis revealed that each copper ion is coordinated by four bridging birfentate benzoate ligandsand one Zaminothiazol to form a binuclear molecule. In the crvstal, there are intramolecular hydrogen bonds N (1)- H ( 1 )-O(4) and N (3)- H (3)-O(1) with NO distance of 3. 005, N-H-O angle of 131. 9°.展开更多
Dibenzoyl peroxide undergoes oxidative addition with metallic copper powder and 2, 2’-bipyridine in a mixed solvent (methanol and tetrahydrofuran ) to afford copper(Ⅱ) complex [Cu(2, 2’-bipy) (C<sub>6&...Dibenzoyl peroxide undergoes oxidative addition with metallic copper powder and 2, 2’-bipyridine in a mixed solvent (methanol and tetrahydrofuran ) to afford copper(Ⅱ) complex [Cu(2, 2’-bipy) (C<sub>6</sub>H<sub>5</sub>COO)<sub>2</sub>]· H<sub>2</sub>O. The structure of the cornplex was solved by direct methods and refined by block-diagonal and full-ma-trix least-squares method to a final R of 0. 055 for 2654 independent reflections of I 】3σ(I). Crystals are monoclinic,space group P2<sub>1</sub>/c , Mr= 479. 78 with cell parameters a= 6. 986(7) , b= 18. 833(1), c= 17. 021(3), β=97. 96(1)°, Z=4, Dc=1. 437g. cm ̄(-3), V= 2218. 1. Each copper ion is coordinated by the oxygen atoms of two benzoato groups and the nitrogen atoms of 2. 2’-bipyridine in a planar square geometry.展开更多
At room temperature, dibenzoyl peroxide undergoes oxidative addition reaction with metallic copper powder and pyridine N-oxide (triphenylphosphine oxide or 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin) which affords t...At room temperature, dibenzoyl peroxide undergoes oxidative addition reaction with metallic copper powder and pyridine N-oxide (triphenylphosphine oxide or 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin) which affords the last products as binuclear copper(II) complexes, [Cu(C5H5NO)-(C6H5COO)2]2(1), [Cu(OPPh3)(C6H5COO)2]2(2) and [Cu(C6H5COO)(C26H2oN2)](3, C26H2oN2 is 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin). The structure of the complexes were characterized by elemental analyses, IR spectra, TG-DTA and magnetic property. Crystals(1) are triclinic, space group P1,a=0.92617(36),b=1.06973(17), c=1.08813(29) nm, a=59.60(2)°, β=74.83(3)°,γ=72.80(2)°, V=0.880 nm3, Dc=1.520 g/cm3, Z=1, R=0.044, Rw=0.048, Mr=805.78, 3477 reflections with I > 3σ(I). Each copper(Ⅱ) ion is coordinated by two bridging bidentate benzoate ligands and one pyridine N-oxide or triphenylphosphine oxide to form dimeric binuclear molecules. The structure of the compound(1) shows a clear centre of symmetry.展开更多
At room temperature, dibenzoyl peroxide undergoes oxidative addition reaction with metallic copper powder and 4 dimethylamine pyridine which affords the last products as binuclear copper?complex (1), [Cu(C6H5COO)2(C7H...At room temperature, dibenzoyl peroxide undergoes oxidative addition reaction with metallic copper powder and 4 dimethylamine pyridine which affords the last products as binuclear copper?complex (1), [Cu(C6H5COO)2(C7H10N2)]2. This complex is further characterized by spectroscopic methods. The structure of complex (1) has been determined by a single crystal X ray analysis. Crystallographic data are as follows: monoclinic, space group P21/n, a=10.446(2)?, b=11.140(5)?, c=17.179(3)?, β=95.92(3)°, V=1988.4(7)?3, Z=4, F(000)=884, μ=11.27cm-1, D(calcd.)=1.429g·cm-3, R=0.0399, Rw=0.1202. Each copper?ion is coordinated by two bridging bidentate benzoate and 4 dimethylamine pyridine to form dimeric molecule. CCDC: 188744.展开更多
文摘Dibenzoyl peroxide undergoes oxidative addition on metallic copper powder with 2,2′-bipyridine(or imidazole)in a mixed solvent(methanol and tetrahydrofuran),and affords the Cu(Ⅱ)complexes-[Cu(Ce(C_6H_5COO)_2(2,2'-bipy)]H_2O(1) and[Cu(C_6H_5COO)_2(C_3H_4N_2)_2](2).The structure was solved by direct methods and Fourier synthesis.C_(24)H_(20)N_2O_5Cu (1),Mr=479.78,space group P2(1)/c,a=6.986(7), b=18.833(I),c=17.021(3),α=γ=90°,Z=4,V=2218.1~3,Dc=1.443g/cm\+3,R=0.055 Rw=0.062.Complex(2),C_(20)H_(18)N_4O_4Cu(2),Mr=441.74,space group P2(1)/n,a=8.699(4), b=9.840(6),c=12.399(5),α=γ=90°,β=100.8°,Z=4,V=1010.9~3,Dc=1.654g/cm\+3,R=0.055, Rw=0.062.
文摘At room temperature, dibenzoyl peroxide and pyridine N-oxide reacted with metallic copper powder in a mixed solvent(dichloromethane, trichloromethane and tetrahydrofuran), resulting in a binuclear copper(Ⅱ) complex. [Cu (C_5H_5NO)-(C_6H_5COO)_2]_2. The structure of the complex was characterized by elemental analyses.IR spectra and X-ray single crystal analysis. The crystal is triclinic, space group P1,with cell parameters . a= 9. 262(4) ,b= 10. 697(2) , c=10. 881 (3 )A , a=59. 60( 2 ),β= 74. 83 ( 3 ) .Y = 72. 80 ( 2 )°. V= 880. 0 A ̄3 . D_c = 1 . 5 20 g/cm ̄3 . Z = 1 . μ= 1 2. 7 cm-1, R=0. 044 ,R_w=0. 048 for 3477 reflections with I>3σ(I), M_r=805. 78. Each copper(Ⅱ) atom is coordinated by four bridging bidentate benzoate ligands and one pyridine M-oxide.
文摘At room temperature, the reaction of dibenzoyl peroxide with metallic copper powder in the presence of pyridine affords the copper(Ⅱ) complex [Cu(C 5H 5N) 2(H 2O)\|(C 6H 5COO) 2]. Crystal is monoclinic, M r =483.002, space group Cc with parameters: a=6\^078(4), b=15.879(4), c=23.091(3), β=97.61(2)°, V=2209.1(2) 3, Z=4, D c =1\^464g/cm 3, μ =10.279 cm -1 , F(000)=996, R=0\^031, R w =0.036, 1595 reflections with I≥3σ(I ) were considered to be observed. Each copper(Ⅱ) ion is coordinated by two monodentate benzoate ligands, two pyridines and one water molecule. The complex is also characterized by its IR, XPS and thermal properties.
文摘Reaction of Cu with dibenzovi peroxide, 2-aminothiazol gave a binuclear complex [Cu_2 (C_6H_5COO)_4(C_3H_4N_2S)_2]. Crystal of the title compound is monoclinic system space group P2_1/n , M_r = 807. 84 with cell parameters a= 10. 685 ( 1 ), b=19. 028(6), c=17. 046(9) , β=96. 49(33) ̄°, Z=4, V=3443. 4, D_c=1. 565 g/cm ̄-3, μ= 14. 078 cm ̄-1, F(000)= 824. The final refinement with 3429 observed reflections is converged with R= 0. 046 and R_w=0. 053. X-ray crystal structure analysis revealed that each copper ion is coordinated by four bridging birfentate benzoate ligandsand one Zaminothiazol to form a binuclear molecule. In the crvstal, there are intramolecular hydrogen bonds N (1)- H ( 1 )-O(4) and N (3)- H (3)-O(1) with NO distance of 3. 005, N-H-O angle of 131. 9°.
文摘Dibenzoyl peroxide undergoes oxidative addition with metallic copper powder and 2, 2’-bipyridine in a mixed solvent (methanol and tetrahydrofuran ) to afford copper(Ⅱ) complex [Cu(2, 2’-bipy) (C<sub>6</sub>H<sub>5</sub>COO)<sub>2</sub>]· H<sub>2</sub>O. The structure of the cornplex was solved by direct methods and refined by block-diagonal and full-ma-trix least-squares method to a final R of 0. 055 for 2654 independent reflections of I 】3σ(I). Crystals are monoclinic,space group P2<sub>1</sub>/c , Mr= 479. 78 with cell parameters a= 6. 986(7) , b= 18. 833(1), c= 17. 021(3), β=97. 96(1)°, Z=4, Dc=1. 437g. cm ̄(-3), V= 2218. 1. Each copper ion is coordinated by the oxygen atoms of two benzoato groups and the nitrogen atoms of 2. 2’-bipyridine in a planar square geometry.
基金Project supported by the National Natural Science Foundation of China and Nanjing Coordination Key Lab Foundation of China.
文摘At room temperature, dibenzoyl peroxide undergoes oxidative addition reaction with metallic copper powder and pyridine N-oxide (triphenylphosphine oxide or 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin) which affords the last products as binuclear copper(II) complexes, [Cu(C5H5NO)-(C6H5COO)2]2(1), [Cu(OPPh3)(C6H5COO)2]2(2) and [Cu(C6H5COO)(C26H2oN2)](3, C26H2oN2 is 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin). The structure of the complexes were characterized by elemental analyses, IR spectra, TG-DTA and magnetic property. Crystals(1) are triclinic, space group P1,a=0.92617(36),b=1.06973(17), c=1.08813(29) nm, a=59.60(2)°, β=74.83(3)°,γ=72.80(2)°, V=0.880 nm3, Dc=1.520 g/cm3, Z=1, R=0.044, Rw=0.048, Mr=805.78, 3477 reflections with I > 3σ(I). Each copper(Ⅱ) ion is coordinated by two bridging bidentate benzoate ligands and one pyridine N-oxide or triphenylphosphine oxide to form dimeric binuclear molecules. The structure of the compound(1) shows a clear centre of symmetry.
文摘At room temperature, dibenzoyl peroxide undergoes oxidative addition reaction with metallic copper powder and 4 dimethylamine pyridine which affords the last products as binuclear copper?complex (1), [Cu(C6H5COO)2(C7H10N2)]2. This complex is further characterized by spectroscopic methods. The structure of complex (1) has been determined by a single crystal X ray analysis. Crystallographic data are as follows: monoclinic, space group P21/n, a=10.446(2)?, b=11.140(5)?, c=17.179(3)?, β=95.92(3)°, V=1988.4(7)?3, Z=4, F(000)=884, μ=11.27cm-1, D(calcd.)=1.429g·cm-3, R=0.0399, Rw=0.1202. Each copper?ion is coordinated by two bridging bidentate benzoate and 4 dimethylamine pyridine to form dimeric molecule. CCDC: 188744.