A new ionic pair complex,1,2′-dinithile-1,2′-dithiolene nickel(II) containing substituted benzylpyridinium [Bz(Me)Py]2[Ni(mnt)2],is prepared and characterized by elemental analyses,IR,UV-VIS and single crystal X-ray...A new ionic pair complex,1,2′-dinithile-1,2′-dithiolene nickel(II) containing substituted benzylpyridinium [Bz(Me)Py]2[Ni(mnt)2],is prepared and characterized by elemental analyses,IR,UV-VIS and single crystal X-ray diffraction.Where [Bz(Me)Py]+ was 1-(1′-phenylethyl)-pyridinium and mnt2-is 1,2′-dinithile-1,2′-dithiolene.The crystal structure was solved by direct method and refined by full-matrix least-squares methods for All the nonhydrogen atoms.The final R1 and wR2 for all data were 0.0450 and 0.1236,respectively.The complex is composed of two [Bz(Me)Py]+ cations and a [Ni(mnt)2]2-anion.The [Ni(mnt)2]2-anions form a stepwise structure by π-π stacking interactions between the CN groups.The cation-anion C-H···N hydrogen bonds and cation-cation C-H···π interactions give further rise to a network structure.展开更多
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 title compound 4, 5-bis ( 2,-dinitrophenylthio )-1, 3-dithiole-2-thione [C3S5(C6H3N2O4)2] crystallizes in the orthogonal system, space group P212121,with a=10. 134(3) , b=20. 488(4), c=9. 656(3)A , V=2005. 1 A3, D...The title compound 4, 5-bis ( 2,-dinitrophenylthio )-1, 3-dithiole-2-thione [C3S5(C6H3N2O4)2] crystallizes in the orthogonal system, space group P212121,with a=10. 134(3) , b=20. 488(4), c=9. 656(3)A , V=2005. 1 A3, D_c=1. 76 g/cm￣3 , Z=4, M.=530. 56, λ=0. 71069 A, F(000)= 1072 , μ=6.1 cm￣(-1), T=296K.Final R= 0. 038, R.= 0. 045 for 1799 reflections with I≥3.5σ(I). In this nonplanar neutral molecule both nitrobenzol rings are approximately perpendicular to the dithiole ring with an asymmetric configuration.展开更多
The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characteriz...The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characterized by X ray diffraction study, IR and UV Vis spectroscopy. Crystallographic data : space group: P2 1/n, a=11.843(2), b=11 079(1), c = 15.404(1) , β=110.33(1)°, V = 1895.1 3, Z=2, D c =1.62 g/cm 3 , μ =17.6 cm -1 , F (000)=956, R=0.052, R w =0.061. In the structure of the title complex, the tto (tto=tetrathioxalato) ligand in bridging form is chelated to two nickel atoms and dmit (dmit=1,3 dithiole 2 thione 4,5 dithiolate) ligands coordinated to nickel atoms.展开更多
文摘A new ionic pair complex,1,2′-dinithile-1,2′-dithiolene nickel(II) containing substituted benzylpyridinium [Bz(Me)Py]2[Ni(mnt)2],is prepared and characterized by elemental analyses,IR,UV-VIS and single crystal X-ray diffraction.Where [Bz(Me)Py]+ was 1-(1′-phenylethyl)-pyridinium and mnt2-is 1,2′-dinithile-1,2′-dithiolene.The crystal structure was solved by direct method and refined by full-matrix least-squares methods for All the nonhydrogen atoms.The final R1 and wR2 for all data were 0.0450 and 0.1236,respectively.The complex is composed of two [Bz(Me)Py]+ cations and a [Ni(mnt)2]2-anion.The [Ni(mnt)2]2-anions form a stepwise structure by π-π stacking interactions between the CN groups.The cation-anion C-H···N hydrogen bonds and cation-cation C-H···π interactions give further rise to a network structure.
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 title compound 4, 5-bis ( 2,-dinitrophenylthio )-1, 3-dithiole-2-thione [C3S5(C6H3N2O4)2] crystallizes in the orthogonal system, space group P212121,with a=10. 134(3) , b=20. 488(4), c=9. 656(3)A , V=2005. 1 A3, D_c=1. 76 g/cm￣3 , Z=4, M.=530. 56, λ=0. 71069 A, F(000)= 1072 , μ=6.1 cm￣(-1), T=296K.Final R= 0. 038, R.= 0. 045 for 1799 reflections with I≥3.5σ(I). In this nonplanar neutral molecule both nitrobenzol rings are approximately perpendicular to the dithiole ring with an asymmetric configuration.
文摘The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characterized by X ray diffraction study, IR and UV Vis spectroscopy. Crystallographic data : space group: P2 1/n, a=11.843(2), b=11 079(1), c = 15.404(1) , β=110.33(1)°, V = 1895.1 3, Z=2, D c =1.62 g/cm 3 , μ =17.6 cm -1 , F (000)=956, R=0.052, R w =0.061. In the structure of the title complex, the tto (tto=tetrathioxalato) ligand in bridging form is chelated to two nickel atoms and dmit (dmit=1,3 dithiole 2 thione 4,5 dithiolate) ligands coordinated to nickel atoms.
