A new Nd（Ⅲ） nitronyl nitroxide complex [Nd（NIT2Py）2（NO3）3] （NIT2Py = 2-（2＇-pyridyl）-4,4,5,5-tetramethylimidazoline-l-oxyl-3-oxide） has been synthesized and structurally characterized by X-ray diffraction. ...A new Nd（Ⅲ） nitronyl nitroxide complex [Nd（NIT2Py）2（NO3）3] （NIT2Py = 2-（2＇-pyridyl）-4,4,5,5-tetramethylimidazoline-l-oxyl-3-oxide） has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.396（4）, b =11.134（4）, c = 23.360（7） A°, β = 98.178（6）°, V= 3191.2（18） A°^3, C24H32N9NdO13, Mr = 798.83, Dc =1.663 g/cm^3, μ（MoKa） = 1.704 mm^-1, F（000） = 1612, Z = 4, the final R = 0.0425 and wR = 0.0957 for 6532 independentreflections with Rint = 0.0642 and 4552 observed reflections （I 〉 2σ（I））. The complex exists as discrete mononuclear molecules and the neodymium（Ⅲ） ion is ten-coordinated with three bidentate nitrate anions and two radical ligands （NIT2Py） via bidentate chelating mode.The optical properties of the complex are discussed.展开更多
A new bimetallic cyano-bridged complex, [NdFe(CN)6(DMF)4(H2O)3]H2O (DMF = N,N-dimethylformamide) 1, has been obtained by the reaction of hexacyanoferrate potassium with neodymium (Ⅲ) chloride in H2O/EtOH/DMF (volume ...A new bimetallic cyano-bridged complex, [NdFe(CN)6(DMF)4(H2O)3]H2O (DMF = N,N-dimethylformamide) 1, has been obtained by the reaction of hexacyanoferrate potassium with neodymium (Ⅲ) chloride in H2O/EtOH/DMF (volume ratio: 2:2:1), and its structure was determined by means of single-crystal X-ray diffraction. The compound crystallizes in space group P21/n of monoclinic system with cell parameters: a = 17.646(1), b = 8.9011(3), c = 19.945(1) ? b = 95.835(2)? V = 3116.6(3) ?, Z = 4, Dc = 1.536 g/cm3, Mr = 720.66, F(000) = 1456, m = 2.166 mm-1, R = 0.0386, wR = 0.1120 and S = 1.061. The central Nd (Ⅲ) ion is coordinated by seven oxygen atoms of four DMF molecules and three water molecules and one nitrogen atom of the bridging cyanide in a slightly distorted square-antiprism arrangement, and the Fe (Ⅲ) ion is in an almost octahedral environment coordinated to six cyano-ligands, of which one cyanide ligand bridges the Nd (Ⅲ) ion to form a bimetallic complex. Molecules of complexes in the crystal lattice are held together by hydrogen bonding, forming a three-dimensional framework.展开更多
Crystal structure of tetra(1,10-Phenanthroline)neodymium (Ⅲ) tetra(4-aminobenzoate)-hydrate, [Nd(p-ABA)4·2Phen]H+3O·2Phen (p-ABA:p-aminobenzoate,Phen:1,10-phenanthroline) has been determined by X-ray diffra...Crystal structure of tetra(1,10-Phenanthroline)neodymium (Ⅲ) tetra(4-aminobenzoate)-hydrate, [Nd(p-ABA)4·2Phen]H+3O·2Phen (p-ABA:p-aminobenzoate,Phen:1,10-phenanthroline) has been determined by X-ray diffraction.The complex crystallizes in monoclinic, space group C2/c.The cell dimensions are a=1.9067 (5) nm,b=1.9192 (3) nm,c=2.0190 (4) nm,β=117.25 (2) °.V=6.568 (3) nm3, Mr= 1428.63,Z=4 and Dx= 1.45 g·cm-3.The coordination number of Nd atom is 10, and the coordinated polyhedron around the Nd atom is distorted trigonal prism.展开更多
C6H5COCHCOCF3)3[(C6H5)3PO]2Eu,Mr=1354.01,triclinic P1,a=11.244(3),b=12.252(3),c=23.784(1),α=79.66(2),β=76.38(3),γ=71.44(3)°,V=2999.33,Z=2,Dc=1.499g/cm3,μ(MoKα)=11.79 cm-1,final R=0.066(Rw=0.069) for 7899 obs...C6H5COCHCOCF3)3[(C6H5)3PO]2Eu,Mr=1354.01,triclinic P1,a=11.244(3),b=12.252(3),c=23.784(1),α=79.66(2),β=76.38(3),γ=71.44(3)°,V=2999.33,Z=2,Dc=1.499g/cm3,μ(MoKα)=11.79 cm-1,final R=0.066(Rw=0.069) for 7899 observed reflections with I】3σ(Ⅰ),The europium ion(Ⅲ) is coordinated by eight oxygen atoms,of which six from C6H5COCHCOCF3 and the other two from (C6H5)3PO,to form a dodecahedral configuration with the average distance of Eu-O(C6H5COCHCOCF3) of 2.410 and that of Eu-O[(C6H5)3PO] of 2.385.The coordination of Eu(Ⅲ) with the ligands was characterized by IR and Raman spectroscopy.The molecular rigidity,which effects luminescence of the complexes,was discussed by fluorescence spectroscopy of the Eu(Ⅲ) complexes.展开更多
A terbium(Ⅲ) complex [Tb2(NO3)(DMPA)5(phen) 2] (HDMPA=homoveratric acid, C12H12O4; phen=1,10- phenanthroline), was synthesized and characterized by elemental analysis, IR and TG-DTG. Its crystal structure was determi...A terbium(Ⅲ) complex [Tb2(NO3)(DMPA)5(phen) 2] (HDMPA=homoveratric acid, C12H12O4; phen=1,10- phenanthroline), was synthesized and characterized by elemental analysis, IR and TG-DTG. Its crystal structure was determined by single crystal X-ray diffraction method. The complex, C74H71N5O23Tb2, crystallizes in the monoclinic system, space group P21/n. The emission spectrum of complex, there are four main peaks, 489, 545, 584 and 622 nm, respectively, corresponding to 5D4→7F6, 5D4→7F5, 5D4→7F4 and 5D4→7F3 transitions of Tb(Ⅲ). The intensity of 5D4→7F5 is much stronger than others.展开更多
基金This work was supported by the National Natural Science Foundation of China (No. 20331010) and Natural Science Foundation of Tianjin (No. 033602011)
文摘A new Nd（Ⅲ） nitronyl nitroxide complex [Nd（NIT2Py）2（NO3）3] （NIT2Py = 2-（2＇-pyridyl）-4,4,5,5-tetramethylimidazoline-l-oxyl-3-oxide） has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.396（4）, b =11.134（4）, c = 23.360（7） A°, β = 98.178（6）°, V= 3191.2（18） A°^3, C24H32N9NdO13, Mr = 798.83, Dc =1.663 g/cm^3, μ（MoKa） = 1.704 mm^-1, F（000） = 1612, Z = 4, the final R = 0.0425 and wR = 0.0957 for 6532 independentreflections with Rint = 0.0642 and 4552 observed reflections （I 〉 2σ（I））. The complex exists as discrete mononuclear molecules and the neodymium（Ⅲ） ion is ten-coordinated with three bidentate nitrate anions and two radical ligands （NIT2Py） via bidentate chelating mode.The optical properties of the complex are discussed.
基金This work was supported by the National Natural Science Foundation of China (No. 20001007 20131020) Natural Science Foundation of the Chinese Academy of Sciences (KJCX2-H3) and Fujian province (2000F006)
文摘A new bimetallic cyano-bridged complex, [NdFe(CN)6(DMF)4(H2O)3]H2O (DMF = N,N-dimethylformamide) 1, has been obtained by the reaction of hexacyanoferrate potassium with neodymium (Ⅲ) chloride in H2O/EtOH/DMF (volume ratio: 2:2:1), and its structure was determined by means of single-crystal X-ray diffraction. The compound crystallizes in space group P21/n of monoclinic system with cell parameters: a = 17.646(1), b = 8.9011(3), c = 19.945(1) ? b = 95.835(2)? V = 3116.6(3) ?, Z = 4, Dc = 1.536 g/cm3, Mr = 720.66, F(000) = 1456, m = 2.166 mm-1, R = 0.0386, wR = 0.1120 and S = 1.061. The central Nd (Ⅲ) ion is coordinated by seven oxygen atoms of four DMF molecules and three water molecules and one nitrogen atom of the bridging cyanide in a slightly distorted square-antiprism arrangement, and the Fe (Ⅲ) ion is in an almost octahedral environment coordinated to six cyano-ligands, of which one cyanide ligand bridges the Nd (Ⅲ) ion to form a bimetallic complex. Molecules of complexes in the crystal lattice are held together by hydrogen bonding, forming a three-dimensional framework.
文摘Crystal structure of tetra(1,10-Phenanthroline)neodymium (Ⅲ) tetra(4-aminobenzoate)-hydrate, [Nd(p-ABA)4·2Phen]H+3O·2Phen (p-ABA:p-aminobenzoate,Phen:1,10-phenanthroline) has been determined by X-ray diffraction.The complex crystallizes in monoclinic, space group C2/c.The cell dimensions are a=1.9067 (5) nm,b=1.9192 (3) nm,c=2.0190 (4) nm,β=117.25 (2) °.V=6.568 (3) nm3, Mr= 1428.63,Z=4 and Dx= 1.45 g·cm-3.The coordination number of Nd atom is 10, and the coordinated polyhedron around the Nd atom is distorted trigonal prism.
文摘C6H5COCHCOCF3)3[(C6H5)3PO]2Eu,Mr=1354.01,triclinic P1,a=11.244(3),b=12.252(3),c=23.784(1),α=79.66(2),β=76.38(3),γ=71.44(3)°,V=2999.33,Z=2,Dc=1.499g/cm3,μ(MoKα)=11.79 cm-1,final R=0.066(Rw=0.069) for 7899 observed reflections with I】3σ(Ⅰ),The europium ion(Ⅲ) is coordinated by eight oxygen atoms,of which six from C6H5COCHCOCF3 and the other two from (C6H5)3PO,to form a dodecahedral configuration with the average distance of Eu-O(C6H5COCHCOCF3) of 2.410 and that of Eu-O[(C6H5)3PO] of 2.385.The coordination of Eu(Ⅲ) with the ligands was characterized by IR and Raman spectroscopy.The molecular rigidity,which effects luminescence of the complexes,was discussed by fluorescence spectroscopy of the Eu(Ⅲ) complexes.
文摘A terbium(Ⅲ) complex [Tb2(NO3)(DMPA)5(phen) 2] (HDMPA=homoveratric acid, C12H12O4; phen=1,10- phenanthroline), was synthesized and characterized by elemental analysis, IR and TG-DTG. Its crystal structure was determined by single crystal X-ray diffraction method. The complex, C74H71N5O23Tb2, crystallizes in the monoclinic system, space group P21/n. The emission spectrum of complex, there are four main peaks, 489, 545, 584 and 622 nm, respectively, corresponding to 5D4→7F6, 5D4→7F5, 5D4→7F4 and 5D4→7F3 transitions of Tb(Ⅲ). The intensity of 5D4→7F5 is much stronger than others.
