Two new manganese(Ⅱ ) trinuclear complexes and two new nickel (Ⅱ) trinuclear compIexes, namely, [Mn3 (BZT ) (Phen )6] (ClO4 )3 (complex 1 ), [Mn (BZT)· (Nphen )6] (ClO4 )3 (complex 2), [Ni3 (BZT) (Phen)6] (ClO4...Two new manganese(Ⅱ ) trinuclear complexes and two new nickel (Ⅱ) trinuclear compIexes, namely, [Mn3 (BZT ) (Phen )6] (ClO4 )3 (complex 1 ), [Mn (BZT)· (Nphen )6] (ClO4 )3 (complex 2), [Ni3 (BZT) (Phen)6] (ClO4 )3· 5H2O (complex3) and [Ni3 (BZT ) (Nphen )6] (ClO4 )3 (complex 4 ) (BZT = 1, 3, 5-benzenetricarboxylato, Phen = 1, 10-phenthroline, Nphen = 5-nitro-1, 10-phenanthroline )have been synthesized. The complexes were characterized using elemental analysis,IR and electronic reflection spectra. These complexes are proposed to have extended 1, 3, 5-benzenetricarboxylato-bridged structure and to consist of three manganese (Ⅱ) or three nickel(Ⅱ). The X-band ESR spectra of the complex 1 and complex 2were recorded at room temperature. The variable-temperature magnetic susceptibilities of complex 1 and complex 3 were measured over 4. 2-300 K. According to experimental results of the variable-temperature magnetic susceptibility, the magnetic interaction between the paramagnetic centers is too weak to be detected using the usual magnetic susceptibility technique.展开更多
The treatment of bis(2-hydroxybenzyl)-amine(HL) with NaOH and Co(Ⅱ)(NO) 2 gives isostructural one-dimensional coordination polymers [(NaOC2H5)CoL2]n(1). The cobalt ions have an octahedral geometry and are coordinate...The treatment of bis(2-hydroxybenzyl)-amine(HL) with NaOH and Co(Ⅱ)(NO) 2 gives isostructural one-dimensional coordination polymers [(NaOC2H5)CoL2]n(1). The cobalt ions have an octahedral geometry and are coordinated by two crystallographically independent ligands which are further linked by μ -O\-\{phenol\} bridged Co and Na atoms to give a one-dimentional structure.展开更多
A new complex { [Cu（NIT4py）2（ip）]·6H2O }, （NIT4py=2-（4＂-pyridinyl）-4,4,5,5-tetra methylimidazoline-1-oxyl-3-oxide and ip = isophthalate dianion） has been synthesized and structurally characterized by X-r...A new complex { [Cu（NIT4py）2（ip）]·6H2O }, （NIT4py=2-（4＂-pyridinyl）-4,4,5,5-tetra methylimidazoline-1-oxyl-3-oxide and ip = isophthalate dianion） has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in orthorhombic, space group Cmcm with a = 25.161（3）, b =10.045（1）, c = 15.450（2） A°, C32H48N6O14CU, Mr = 804.30, V= 3904.8（8） ,A°^3, Z = 4, De = 1.368 g/cm^3, μ（MoKa） = 0.630 mm^-1, F（000） = 1692, the final R = 0.0326 and wR = 0.0787 for 1843 independent reflections with Rint = 0.0372. Each Cu（Ⅱ） ion is four-coordinated by two carboxylate oxygen atoms and two pyridyl-N atoms from NIT4py radicals to furnish a rhombus geometry. The central Cu（Ⅱ） ion is located at an inversion center and a crystallographic two-fold axis. Each isophthalate dianion binds two Cu（Ⅱ） ions in bis-monodentate mode, leading to a 1-D chain, a＇ these 1-D chains are further linked into a 2-D network via hydrogen-bonding interactions.展开更多
A new one-dimensional （1-D） Zn（Ⅱ） nitronyl nitroxide complex bridged by pyridine-2,4-dicarboxylate anion, [Zn（NIT4Py）（2,4-PDA）（H2O）2], （NIT4Py = 2-（4′-pyridyl）-4,4,5,5- tetramethylimidazoline-1-oxyl-3-o...A new one-dimensional （1-D） Zn（Ⅱ） nitronyl nitroxide complex bridged by pyridine-2,4-dicarboxylate anion, [Zn（NIT4Py）（2,4-PDA）（H2O）2], （NIT4Py = 2-（4′-pyridyl）-4,4,5,5- tetramethylimidazoline-1-oxyl-3-oxide and 2,4-PDA = pyridine-2,4-dicarboxylate anion）, has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a = 16.834（2）, b = 7.4376（10）, c = 18.295（3） A, β = 102.848（2）°, V = 2233.2（5） A^3, C19H23N4O3Zn, Mr = 500.78, Dc = 1.489 g/cm^3,μ（MoKa） = 1.152 mm^-1, F（000） = 1036, Z = 4, the final R = 0.0390 and wR = 0.0915 for 3234 observed reflections. In the complex, each zinc（Ⅱ） ion is six-coordinated by one nitrogen atom of the radical ligand （NIT4Py）, one nitrogen atom and two oxygen atoms of two 2,4-PDA anions and two oxygen atoms of two water molecules. Each 2,4-PDA anion bridges two Zn（Ⅱ） ions via a tridentate mode into a 1-D chain, and these 1-D chains are further linked into a 2-D network via hydrogen-bonding interactions.展开更多
A new Zn（Ⅱ） nitronyl nitroxide complex [Zn（NIT4Py）（PDA）（HzO）3] （NIT4Py = 2-（4＇-pyridyl）-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, H2PDA = pyridine-2,5-dicarboxylic acid） has been synthesized and str...A new Zn（Ⅱ） nitronyl nitroxide complex [Zn（NIT4Py）（PDA）（HzO）3] （NIT4Py = 2-（4＇-pyridyl）-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, H2PDA = pyridine-2,5-dicarboxylic acid） has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in monoclinic, space group P2 1/c with a = 16.881（8）, b = 7.356（4）, c = 18.857（9） A°,β = 108.616（6）°, V = 2219.1 （19）A°^3 ,C 19H25N4O9Zn, Mr = 518.80, Dc = 1.553 g/cm^3, μ（MoKa） = 1.165 mm^-1, F（000） = 1076, Z = 4, the final R = 0.0269 and wR = 0.0715 for 3193 observed reflections with I 〉 2σ（I）. The complex exists as discrete mononuclear molecules and the zinc（Ⅱ） ion is six-coordinated with one radical ligand （NIT4Py）, one bidentate pyridine-2,5-dicarboxylate anion and three water molecules. A three-dimensional network structure is formed through the intermolecular interactions.展开更多
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
CuLaSm(C4O4 )4(H2O)16]·2H2O was obtained as a single crystal from a mixture of squaric acid, lanthanum chloride, samarium chloride, and copper chloride in water. The complex crystallized in the monoclinic system,...CuLaSm(C4O4 )4(H2O)16]·2H2O was obtained as a single crystal from a mixture of squaric acid, lanthanum chloride, samarium chloride, and copper chloride in water. The complex crystallized in the monoclinic system, space group P2_1,with a=6. 728(1) . b=32. 117(9),c=8. 150(1) A ,β=111. 60(1),Z=2, M_r=1125. 24, V= 1637(1 ) A3, Dc= 2. 28g/cm3, μ(MoKα) = 38. 36 cm-1, F(000)= 1104, R= 0. 040 for 2823 independent observed reflections. The coordinated environments of the lanthanides are a 4-capped square antiprism and a 4,4, 4-tricapped trigonal prism, and that of the copper is a distorted octahedron. The complex is the first example that contains copper and two kinds of different lanthanides when the squarate is employed as the ligand.展开更多
The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-dien...The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-diene and mnt2- = cis-1, 2-dicyano-1,2-ethylenedithiolato. Its crystal structure has been determined by X-raycrystallography analysis with 4827 independent reflections (Fo>4σ(F0). The bimetallic complex salt [Ni (trans [14] diene )] [Ni (mnt )2] (C24 H32N8Ni2S4, Mr = 678. 24 )crystallizes in the triclinic system with space group P1, a = 9. 2911 (9), b= 11. 7075(12), c=15. 799(2) A, α=68. 384(7), β=79. 324(7), γ=67. 581(6)°, V=1474. 9(3) A3, Dc=1. 527 Mg/m3, Z=2, λ=0. 71073 A, μ=1. 589mm-1, F(000) =704,R=0. 0367. The structure consists of slightly distorted Square planar units [Ni(trans[14]diene)]2+ and [Ni(mnt)2]2-.展开更多
文摘Two new manganese(Ⅱ ) trinuclear complexes and two new nickel (Ⅱ) trinuclear compIexes, namely, [Mn3 (BZT ) (Phen )6] (ClO4 )3 (complex 1 ), [Mn (BZT)· (Nphen )6] (ClO4 )3 (complex 2), [Ni3 (BZT) (Phen)6] (ClO4 )3· 5H2O (complex3) and [Ni3 (BZT ) (Nphen )6] (ClO4 )3 (complex 4 ) (BZT = 1, 3, 5-benzenetricarboxylato, Phen = 1, 10-phenthroline, Nphen = 5-nitro-1, 10-phenanthroline )have been synthesized. The complexes were characterized using elemental analysis,IR and electronic reflection spectra. These complexes are proposed to have extended 1, 3, 5-benzenetricarboxylato-bridged structure and to consist of three manganese (Ⅱ) or three nickel(Ⅱ). The X-band ESR spectra of the complex 1 and complex 2were recorded at room temperature. The variable-temperature magnetic susceptibilities of complex 1 and complex 3 were measured over 4. 2-300 K. According to experimental results of the variable-temperature magnetic susceptibility, the magnetic interaction between the paramagnetic centers is too weak to be detected using the usual magnetic susceptibility technique.
基金Supported by the NationalNaturalScience Foundation of China( No.2 0 1710 2 6 ) and Tianjin Natural Science Founda-tion( No.0 136 0 5 811)
文摘The treatment of bis(2-hydroxybenzyl)-amine(HL) with NaOH and Co(Ⅱ)(NO) 2 gives isostructural one-dimensional coordination polymers [(NaOC2H5)CoL2]n(1). The cobalt ions have an octahedral geometry and are coordinated by two crystallographically independent ligands which are further linked by μ -O\-\{phenol\} bridged Co and Na atoms to give a one-dimentional structure.
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 complex { [Cu（NIT4py）2（ip）]·6H2O }, （NIT4py=2-（4＂-pyridinyl）-4,4,5,5-tetra methylimidazoline-1-oxyl-3-oxide and ip = isophthalate dianion） has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in orthorhombic, space group Cmcm with a = 25.161（3）, b =10.045（1）, c = 15.450（2） A°, C32H48N6O14CU, Mr = 804.30, V= 3904.8（8） ,A°^3, Z = 4, De = 1.368 g/cm^3, μ（MoKa） = 0.630 mm^-1, F（000） = 1692, the final R = 0.0326 and wR = 0.0787 for 1843 independent reflections with Rint = 0.0372. Each Cu（Ⅱ） ion is four-coordinated by two carboxylate oxygen atoms and two pyridyl-N atoms from NIT4py radicals to furnish a rhombus geometry. The central Cu（Ⅱ） ion is located at an inversion center and a crystallographic two-fold axis. Each isophthalate dianion binds two Cu（Ⅱ） ions in bis-monodentate mode, leading to a 1-D chain, a＇ these 1-D chains are further linked into a 2-D network via hydrogen-bonding interactions.
基金This work was supported by the National Natural Science Foundation of China (No. 20331010 and 20571045)
文摘A new one-dimensional （1-D） Zn（Ⅱ） nitronyl nitroxide complex bridged by pyridine-2,4-dicarboxylate anion, [Zn（NIT4Py）（2,4-PDA）（H2O）2], （NIT4Py = 2-（4′-pyridyl）-4,4,5,5- tetramethylimidazoline-1-oxyl-3-oxide and 2,4-PDA = pyridine-2,4-dicarboxylate anion）, has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a = 16.834（2）, b = 7.4376（10）, c = 18.295（3） A, β = 102.848（2）°, V = 2233.2（5） A^3, C19H23N4O3Zn, Mr = 500.78, Dc = 1.489 g/cm^3,μ（MoKa） = 1.152 mm^-1, F（000） = 1036, Z = 4, the final R = 0.0390 and wR = 0.0915 for 3234 observed reflections. In the complex, each zinc（Ⅱ） ion is six-coordinated by one nitrogen atom of the radical ligand （NIT4Py）, one nitrogen atom and two oxygen atoms of two 2,4-PDA anions and two oxygen atoms of two water molecules. Each 2,4-PDA anion bridges two Zn（Ⅱ） ions via a tridentate mode into a 1-D chain, and these 1-D chains are further linked into a 2-D network via hydrogen-bonding interactions.
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 Zn（Ⅱ） nitronyl nitroxide complex [Zn（NIT4Py）（PDA）（HzO）3] （NIT4Py = 2-（4＇-pyridyl）-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, H2PDA = pyridine-2,5-dicarboxylic acid） has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in monoclinic, space group P2 1/c with a = 16.881（8）, b = 7.356（4）, c = 18.857（9） A°,β = 108.616（6）°, V = 2219.1 （19）A°^3 ,C 19H25N4O9Zn, Mr = 518.80, Dc = 1.553 g/cm^3, μ（MoKa） = 1.165 mm^-1, F（000） = 1076, Z = 4, the final R = 0.0269 and wR = 0.0715 for 3193 observed reflections with I 〉 2σ（I）. The complex exists as discrete mononuclear molecules and the zinc（Ⅱ） ion is six-coordinated with one radical ligand （NIT4Py）, one bidentate pyridine-2,5-dicarboxylate anion and three water molecules. A three-dimensional network structure is formed through the intermolecular interactions.
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.
文摘CuLaSm(C4O4 )4(H2O)16]·2H2O was obtained as a single crystal from a mixture of squaric acid, lanthanum chloride, samarium chloride, and copper chloride in water. The complex crystallized in the monoclinic system, space group P2_1,with a=6. 728(1) . b=32. 117(9),c=8. 150(1) A ,β=111. 60(1),Z=2, M_r=1125. 24, V= 1637(1 ) A3, Dc= 2. 28g/cm3, μ(MoKα) = 38. 36 cm-1, F(000)= 1104, R= 0. 040 for 2823 independent observed reflections. The coordinated environments of the lanthanides are a 4-capped square antiprism and a 4,4, 4-tricapped trigonal prism, and that of the copper is a distorted octahedron. The complex is the first example that contains copper and two kinds of different lanthanides when the squarate is employed as the ligand.
文摘The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-diene and mnt2- = cis-1, 2-dicyano-1,2-ethylenedithiolato. Its crystal structure has been determined by X-raycrystallography analysis with 4827 independent reflections (Fo>4σ(F0). The bimetallic complex salt [Ni (trans [14] diene )] [Ni (mnt )2] (C24 H32N8Ni2S4, Mr = 678. 24 )crystallizes in the triclinic system with space group P1, a = 9. 2911 (9), b= 11. 7075(12), c=15. 799(2) A, α=68. 384(7), β=79. 324(7), γ=67. 581(6)°, V=1474. 9(3) A3, Dc=1. 527 Mg/m3, Z=2, λ=0. 71073 A, μ=1. 589mm-1, F(000) =704,R=0. 0367. The structure consists of slightly distorted Square planar units [Ni(trans[14]diene)]2+ and [Ni(mnt)2]2-.
