A new mono-nuclear CuII complex [Cu（DPP）（DP）Br]（ClO4）H2O （DPP = 2-（3,5- dimethyl-1H-pyrazol-1-yl）-1,10-phenanthroline, DP = 3,5-dimethyl-1H-pyrazole） has been syn- thesized with 2-（3,5-dimethyl-1H-pyrazol-1...A new mono-nuclear CuII complex [Cu（DPP）（DP）Br]（ClO4）H2O （DPP = 2-（3,5- dimethyl-1H-pyrazol-1-yl）-1,10-phenanthroline, DP = 3,5-dimethyl-1H-pyrazole） has been syn- thesized with 2-（3,5-dimethyl-1H-pyrazol-1-yl）-1,10-phenanthroline and 3,5-dimethyl-1H-pyrazole as ligands, and its crystal structure was determined by X-ray crystallography. The crystal is of monoclinic system, space group P21/c with a = 13.765（2）, b = 17.044（3）, c = 10.9044（16）, β= 97.112（2）°, V = 2538.5（6）3, Z = 4, C22H24BrClCuN6O5, Mr = 631.37, Dc = 1.652 g/cm3, F（000） = 1276 and μ= 2.585 mm-1. In the crystal, DPP functions as a tridentate ligand and CuII ions assume a distorted square pyramidal geometry with Br atom lying on the apex, and at the same time, there is π-π stacking between adjacent complexes, which deals with two 1,10-phenanthroline plane rings. In addition to the π-π stacking, there are C-H···Br non-classic hydrogen bonds between adjacent complexes. The theoretical calculations reveal that the π-π stacking and C-H···Br non-classic hydrogen bond result in a weak anti-ferromagnetic interaction with 2J = -5.34 cm-1 and a weak ferromagnetic 2J = 5.92 cm-1, respectively. The magnetic coupling sign from the π-π stacking could be explained with McConnell I spin-polarization mechanism.展开更多
The mononuclear radical anionic complex [1-N-methyl-1,10-phenanthrolium][Ni（dmit）2]（dmit = 1,3-dithiole-2-thione-4,5-dithiolate） with a new countercation has been prepared and its crystal structure was determined ...The mononuclear radical anionic complex [1-N-methyl-1,10-phenanthrolium][Ni（dmit）2]（dmit = 1,3-dithiole-2-thione-4,5-dithiolate） with a new countercation has been prepared and its crystal structure was determined by X-ray crystallography at 298 and 80 K. In the mononuclear radical anionic complex, the nickel ion assumes a slightly distorted square-planar geometry. There are two and three kinds of intermolecular interactions between adjacent mononuclear radical anionic complexes in the crystal at 298 and 80 K, respectively（i.e., Models A and B at 298 K; and Models C, D and E at 80 K）. The variable-temperature magnetic moments indicate a strong antiferromagnetic interaction between the adjacent mononuclear radical anionic complexes, and the theoretical calculations reveal that the stronger antiferromagnetic coupling strength at lower temperature should be contributed to the larger overlap integrals between the short contact atoms. This study is the first to reveal the mechanism of stronger magnetic coupling strength at lower temperature for a mononuclear radical anionic nickel complex with dmit as the ligand.展开更多
Three new nickel(Ⅱ) binuclear complexes, namely,[Ni_2(CTPHA)(Phen)_4](ClO_4)2·4H_2O (complex 1 ), [Ni_2(CTPHA) (Nphen)_4](ClO_4)_2·2H_2O(complex 2 ) and [Ni2 (CTPHA)(Bpy)4] (ClO4)2 (complex 3 ). (CTPHA = 2-...Three new nickel(Ⅱ) binuclear complexes, namely,[Ni_2(CTPHA)(Phen)_4](ClO_4)2·4H_2O (complex 1 ), [Ni_2(CTPHA) (Nphen)_4](ClO_4)_2·2H_2O(complex 2 ) and [Ni2 (CTPHA)(Bpy)4] (ClO4)2 (complex 3 ). (CTPHA = 2-chloroterephthalate . Phen=1, 10-phenanthroline, Nphen=5-nitro-1, 10-phenanthroline, Bpy=2, 2-bipyridyl), have been synthesized and characterized by elemental analysis, IR, molar conductance and electronic spectra. These complexes are proposed tohave extended Z-chloroterephthalato-bridged structure and to consist of two nickel(Ⅱ). The variable-temperature magnetic susceptibilities of complex 1 were measuredover 4. 2～300 K and the data were fitted by least-squares to a susceptibility equationderived from the Hamiltonian operator, giving the exchange integral ZJ=1. 6 cm-1, which indicate a very weak antiferromagnetic interaction between nickelf (Ⅱ) ions.展开更多
A three-dimensional coordination polymer [Mn2（μ1.3-N3）4（μ-PP）2]n （PP = 3-（pyrazin-2-yloxy）-pyridine） has been synthesized with 3-（pyrazin-2-yloxy）-pyridine and azide anion as mixed bridge ligand, and its c...A three-dimensional coordination polymer [Mn2（μ1.3-N3）4（μ-PP）2]n （PP = 3-（pyrazin-2-yloxy）-pyridine） has been synthesized with 3-（pyrazin-2-yloxy）-pyridine and azide anion as mixed bridge ligand, and its crystal structure was determined by X-ray crystallography. The crystal data： triclinic system, space group P1, with a = 6.794（4）, b = 9.885（6）, c = 9.947（6） A, α = 64.170（6）, β= 84.190（8）, γ= 85.319（8）°, V = 597.7（6）A^3, Z = 1, C18H14Mn2N18O2, Mr = 624.35, Dc = 1.735 g/cm^3, F（000） = 314 and μ = 1.117 mm^-1. In the crystal, the azide anion acts as a bridge ligand and makes adjacent Mn（Ⅱ） ions connect into a two-dimensional sheet on the ab plane, then 3-（pyrazin-2-yloxy）-pyridine serves as a bidentate bridge ligand to connect neighboring sheets along展开更多
A new mono-nuclear Mn（Ⅱ） complex [Mn（MPT）2（NCS）（HOCH3）]ClO4（MPT = 2-methoxyl-1,10-phenanthroline） has been synthesized with 2-methoxyl-1,10-phenanthroline and thiocyanate anion as ligands,and its crystal st...A new mono-nuclear Mn（Ⅱ） complex [Mn（MPT）2（NCS）（HOCH3）]ClO4（MPT = 2-methoxyl-1,10-phenanthroline） has been synthesized with 2-methoxyl-1,10-phenanthroline and thiocyanate anion as ligands,and its crystal structure was determined by X-ray crystallography.The crystal data：monoclinic system,space group P21/c with a = 12.8849（17）,b = 15.684（2）,c = 14.2703（19） ,β = 92.126（2）°,V = 2881.9（7） 3,Z = 4,C28H24ClMnN5O7S,Mr = 664.97,Dc = 1.533 g/cm3,F（000） = 1364 and μ = 0.679 mm-1.In the crystal,MPT functions as a bidentate ligand and Mn（Ⅱ） ion assumes a distorted octahedral geometry.In the crystal there are two types of π-π stacking interactions among the adjacent complexes,which involves 1,10-phenanthroline rings.The theoretical calculations reveal that the two types of π-π stacking resulted in a weak anti-ferromagnetic coupling with 2J =-14.68 cm-1 and a weak ferromagnetic coupling with 2J = 0.70 cm-1,respectively.The theoretical calculations also reveal that there are both spin polarization and spin delocalization in the two π-π stacking systems,and the magnetic coupling signs are unable to explain with McConnell I spin-polarization mechanism.展开更多
The three-dimensional coordination polymer {[Cd(cda)2]2CH3OH}n has been syn- thesized by Na(cda) (cda = carbamyldicyanomethanide anion) and hydrated cadmium perchlorate in methanol solution. The crystal belongs to mon...The three-dimensional coordination polymer {[Cd(cda)2]2CH3OH}n has been syn- thesized by Na(cda) (cda = carbamyldicyanomethanide anion) and hydrated cadmium perchlorate in methanol solution. The crystal belongs to monoclinic, space group C2/c with a = 15.686(3), b = 8.1650(18), c = 13.119(3) ? b = 119.334(2), V = 1464.8(6) 3, Z = 4, C10H12CdN6O4, Mr = 392.66, Dc = 1.780 g/cm3, F(000) = 776 and m = 1.516 mm-1. The structure was refined to R = 0.0248 and wR = 0.0628 for 1176 observed reflections (I > 2s(I)). The Cd(II) ion is coordinated by two amide- oxygen and four nitrile-nitrogen atoms from six different cda bridging ligands, forming a three- dimensional structure.展开更多
The organic salt, (H2Bpy)(cda)2, was synthesized by the reaction of sodium car- bamyldicyanomethanide, 4,4-bipyridyl and manganese(II) perchlorate in water solution. The crystal belongs to monoclinic, space group C2/c...The organic salt, (H2Bpy)(cda)2, was synthesized by the reaction of sodium car- bamyldicyanomethanide, 4,4-bipyridyl and manganese(II) perchlorate in water solution. The crystal belongs to monoclinic, space group C2/c with a = 20.333(7), b = 6.177(2), c = 15.566(5) ? b = 116.860(5), V = 1744(1) ?, Z = 4, C18H14N8O2 (Mr = 374.37), Dc = 1.426 g/cm3, F(000) = 776, m = 0.100 mm-1 and l = 0.71073 ? The structure was refined to R = 0.0560 and wR = 0.1072 for 590 observed reflections (I > 2s(I)). Two nitrogen atoms of the 4,4?bipyridyl molecule bonded to two hydrogen ions, resulting this neutral molecule into a divalent cation. Through the interaction of colorless H2bpy cation and colorless cda anion the red neutral organic salt was formed.展开更多
A two-dimensional coordination polymer [Zn2(DTB)(DMF)4(H2O)2]n has been synthesized by 1,4-dinitro-2,3,5,6-tetracarboxylatebenzenic acid and hydrate zinc perchlorate in the solutions of DMF and H2O. The crystal belo...A two-dimensional coordination polymer [Zn2(DTB)(DMF)4(H2O)2]n has been synthesized by 1,4-dinitro-2,3,5,6-tetracarboxylatebenzenic acid and hydrate zinc perchlorate in the solutions of DMF and H2O. The crystal belongs to the triclinic system, space group P1 with a = 8.887(6), b = 9.225(6), c = 9.828(7) ?, α = 85.249(11), β = 74.863(11), γ = 86.510(13)°, V = 774.4(9), Z = 1, C22H32N6O18Zn2, Mr = 799.28, Dc = 1.714 g/cm3, F(000) = 410 and μ = 1.639 mm-1. The structure was refined to R = 0.0539 and wR = 0.1161 for 1584 observed reflections (I > 2σ(I)). In the complex there exist two kinds of coordination environments for the zinc(II) ions and a two-dimensional sheet is formed via the coordination of carboxylates and zinc(II) ions.展开更多
Two two-dimensional coordination polymers, [Cd（μ1,3-SCN-）2（μ1,6-L）]n 1 and [Co（μ1,3-SCN-）2（μ1,6-L）]n 2, have been synthesized with 2,3-dimethylpyrazine-1,4-dioxide （L） and thiocyanate as mixed bridging l...Two two-dimensional coordination polymers, [Cd（μ1,3-SCN-）2（μ1,6-L）]n 1 and [Co（μ1,3-SCN-）2（μ1,6-L）]n 2, have been synthesized with 2,3-dimethylpyrazine-1,4-dioxide （L） and thiocyanate as mixed bridging ligands, and their crystal structures were determined by X-ray crystallography. Both crystals belong to monoclinic system, space group C2/c. The other crystal parameters are as follows： for complex 1： α = 9.732（3）, b =14.658（5）, c = 8.811（3） A, β = 102.935（4）°, Z = 4, V= 1225.1（7） A^3, C8H8CdN4O2S2, Mr = 368.71, Dc = 1.999 g/cm^3, F（000） = 720 and μ= 2.117 mm^-1; for complex 2： α = 9.528（7）, b = 14.563（11）, c = 8.415（6） A, β= 102.195（9）°, V= 1141.3（14） A^3, Z = 4, C8H8CoN4O2S2, Mr = 315.23, Dc = 1.835 g/cm^3, F（000） = 636 and μ = 1.863 mm^-1. The two complexes show similar two-dimensional sheet structures. Along the c axis one-dimensional chains are constructed by the coordination of Cd（Ⅱ） （or Co（Ⅱ）） ions with μ1,6-L bridging ligand, and the μ1,3-SCN- bridging ligands make the chains connect to each other, resulting in the formation of a two-dimensional sheet on the ac plane.展开更多
Mononuclear complex [Co(cdm)2(H2O)4]?H2O was synthesized by sodium carbamyldicyanomethanide (Nacda) and cobalt perchlorate. The crystal belongs to monoclinic system, space group P21/n with a = 9.366(3), b = 7.392(3), ...Mononuclear complex [Co(cdm)2(H2O)4]?H2O was synthesized by sodium carbamyldicyanomethanide (Nacda) and cobalt perchlorate. The crystal belongs to monoclinic system, space group P21/n with a = 9.366(3), b = 7.392(3), c = 12.039(4)? = 108.335(4)? V = 791.2(5)?, Z = 2, Mr (C8H16CoN6O8) = 383.2, Dc = 1.608 g/cm3, F(000) = 394, = 1.135 mm-1, = 0.71073 ? The structure was refined to R = 0.0240 and wR = 0.0632 for 1267 observed reflections (I > 2(I)). The cobalt(II) atom in the complex is coordinated by two nitrile-nitrogen atoms and four oxygen atoms of H2O, which forms a slightly distorted coordination octahedron around the cobalt(II) ion. The mononuclear complexes are connected by hydrogen bondings and in the crystal there exists a cavity where the uncoordinated H2O molecules are trapped.展开更多
A one-dimensional chain complex {Na[ZnL(H2O)2]}n was synthesized by sodium 2,2-dihydroxyl-malonate (Na2L?) and hydrate zinc perchlorate. The crystal belongs to the mono- clinic system, space group P21/n with a = 5.936...A one-dimensional chain complex {Na[ZnL(H2O)2]}n was synthesized by sodium 2,2-dihydroxyl-malonate (Na2L?) and hydrate zinc perchlorate. The crystal belongs to the mono- clinic system, space group P21/n with a = 5.936(2), b = 7.203(3), c = 19.356(8) ? b = 95.264(6), V = 824.2(6) 3, Z = 4, C3H5NaO8Zn, Mr = 257.43, Dc = 2.075 g/cm3, F(000) = 512 and m = 3.045 mm-1. The structure was refined to R = 0.0381 and wR = 0.0766 for 1188 observed reflections (I > 2s(I)). In the complex the zinc(II) atom is coordinated to six oxygen atoms from two H2O mole- cules, two carboxylate groups, one ionized hydroxyl group and one hydroxyl group. By the coordi- nation of zinc(II) ions and bridging ligand 2-hydroxyl-2-hydroxylate-malonate trivalent anion the one-dimensional chain is constructed.展开更多
基金supported by the National Natural Science Foundation of China (No. 20971080)the Natural Science Foundation of Shandong Province (No. ZR2009BM026 and ZR2009BL002)
文摘A new mono-nuclear CuII complex [Cu（DPP）（DP）Br]（ClO4）H2O （DPP = 2-（3,5- dimethyl-1H-pyrazol-1-yl）-1,10-phenanthroline, DP = 3,5-dimethyl-1H-pyrazole） has been syn- thesized with 2-（3,5-dimethyl-1H-pyrazol-1-yl）-1,10-phenanthroline and 3,5-dimethyl-1H-pyrazole as ligands, and its crystal structure was determined by X-ray crystallography. The crystal is of monoclinic system, space group P21/c with a = 13.765（2）, b = 17.044（3）, c = 10.9044（16）, β= 97.112（2）°, V = 2538.5（6）3, Z = 4, C22H24BrClCuN6O5, Mr = 631.37, Dc = 1.652 g/cm3, F（000） = 1276 and μ= 2.585 mm-1. In the crystal, DPP functions as a tridentate ligand and CuII ions assume a distorted square pyramidal geometry with Br atom lying on the apex, and at the same time, there is π-π stacking between adjacent complexes, which deals with two 1,10-phenanthroline plane rings. In addition to the π-π stacking, there are C-H···Br non-classic hydrogen bonds between adjacent complexes. The theoretical calculations reveal that the π-π stacking and C-H···Br non-classic hydrogen bond result in a weak anti-ferromagnetic interaction with 2J = -5.34 cm-1 and a weak ferromagnetic 2J = 5.92 cm-1, respectively. The magnetic coupling sign from the π-π stacking could be explained with McConnell I spin-polarization mechanism.
基金supported by the National Natural Science Foundation of China(No.20971080)the Natural Science Foundation of Shandong Province(No.ZR2013BM009)
文摘The mononuclear radical anionic complex [1-N-methyl-1,10-phenanthrolium][Ni（dmit）2]（dmit = 1,3-dithiole-2-thione-4,5-dithiolate） with a new countercation has been prepared and its crystal structure was determined by X-ray crystallography at 298 and 80 K. In the mononuclear radical anionic complex, the nickel ion assumes a slightly distorted square-planar geometry. There are two and three kinds of intermolecular interactions between adjacent mononuclear radical anionic complexes in the crystal at 298 and 80 K, respectively（i.e., Models A and B at 298 K; and Models C, D and E at 80 K）. The variable-temperature magnetic moments indicate a strong antiferromagnetic interaction between the adjacent mononuclear radical anionic complexes, and the theoretical calculations reveal that the stronger antiferromagnetic coupling strength at lower temperature should be contributed to the larger overlap integrals between the short contact atoms. This study is the first to reveal the mechanism of stronger magnetic coupling strength at lower temperature for a mononuclear radical anionic nickel complex with dmit as the ligand.
文摘Three new nickel(Ⅱ) binuclear complexes, namely,[Ni_2(CTPHA)(Phen)_4](ClO_4)2·4H_2O (complex 1 ), [Ni_2(CTPHA) (Nphen)_4](ClO_4)_2·2H_2O(complex 2 ) and [Ni2 (CTPHA)(Bpy)4] (ClO4)2 (complex 3 ). (CTPHA = 2-chloroterephthalate . Phen=1, 10-phenanthroline, Nphen=5-nitro-1, 10-phenanthroline, Bpy=2, 2-bipyridyl), have been synthesized and characterized by elemental analysis, IR, molar conductance and electronic spectra. These complexes are proposed tohave extended Z-chloroterephthalato-bridged structure and to consist of two nickel(Ⅱ). The variable-temperature magnetic susceptibilities of complex 1 were measuredover 4. 2～300 K and the data were fitted by least-squares to a susceptibility equationderived from the Hamiltonian operator, giving the exchange integral ZJ=1. 6 cm-1, which indicate a very weak antiferromagnetic interaction between nickelf (Ⅱ) ions.
基金Supported by the National Natural Science Foundation of China (No. 20271043)Natural Science Foundation of Shandong Province (Y2007B26)
文摘A three-dimensional coordination polymer [Mn2（μ1.3-N3）4（μ-PP）2]n （PP = 3-（pyrazin-2-yloxy）-pyridine） has been synthesized with 3-（pyrazin-2-yloxy）-pyridine and azide anion as mixed bridge ligand, and its crystal structure was determined by X-ray crystallography. The crystal data： triclinic system, space group P1, with a = 6.794（4）, b = 9.885（6）, c = 9.947（6） A, α = 64.170（6）, β= 84.190（8）, γ= 85.319（8）°, V = 597.7（6）A^3, Z = 1, C18H14Mn2N18O2, Mr = 624.35, Dc = 1.735 g/cm^3, F（000） = 314 and μ = 1.117 mm^-1. In the crystal, the azide anion acts as a bridge ligand and makes adjacent Mn（Ⅱ） ions connect into a two-dimensional sheet on the ab plane, then 3-（pyrazin-2-yloxy）-pyridine serves as a bidentate bridge ligand to connect neighboring sheets along
基金supported by the National Natural Science Foundation of China (No. 20971080)the Natural Science Foundation of Shandong Province (No. ZR2009BM026)
文摘A new mono-nuclear Mn（Ⅱ） complex [Mn（MPT）2（NCS）（HOCH3）]ClO4（MPT = 2-methoxyl-1,10-phenanthroline） has been synthesized with 2-methoxyl-1,10-phenanthroline and thiocyanate anion as ligands,and its crystal structure was determined by X-ray crystallography.The crystal data：monoclinic system,space group P21/c with a = 12.8849（17）,b = 15.684（2）,c = 14.2703（19） ,β = 92.126（2）°,V = 2881.9（7） 3,Z = 4,C28H24ClMnN5O7S,Mr = 664.97,Dc = 1.533 g/cm3,F（000） = 1364 and μ = 0.679 mm-1.In the crystal,MPT functions as a bidentate ligand and Mn（Ⅱ） ion assumes a distorted octahedral geometry.In the crystal there are two types of π-π stacking interactions among the adjacent complexes,which involves 1,10-phenanthroline rings.The theoretical calculations reveal that the two types of π-π stacking resulted in a weak anti-ferromagnetic coupling with 2J =-14.68 cm-1 and a weak ferromagnetic coupling with 2J = 0.70 cm-1,respectively.The theoretical calculations also reveal that there are both spin polarization and spin delocalization in the two π-π stacking systems,and the magnetic coupling signs are unable to explain with McConnell I spin-polarization mechanism.
基金This work was supported by the National Natural Science Foundation of China (No. 20271043) and Natural Science Foundation of Shandong Province (No. Y2002B10)
文摘The three-dimensional coordination polymer {[Cd(cda)2]2CH3OH}n has been syn- thesized by Na(cda) (cda = carbamyldicyanomethanide anion) and hydrated cadmium perchlorate in methanol solution. The crystal belongs to monoclinic, space group C2/c with a = 15.686(3), b = 8.1650(18), c = 13.119(3) ? b = 119.334(2), V = 1464.8(6) 3, Z = 4, C10H12CdN6O4, Mr = 392.66, Dc = 1.780 g/cm3, F(000) = 776 and m = 1.516 mm-1. The structure was refined to R = 0.0248 and wR = 0.0628 for 1176 observed reflections (I > 2s(I)). The Cd(II) ion is coordinated by two amide- oxygen and four nitrile-nitrogen atoms from six different cda bridging ligands, forming a three- dimensional structure.
基金This work was supported by the National Natural Science Foundation of China (20271043) and the Natural Science Foundation of Shandong province(y2002B10)
文摘The organic salt, (H2Bpy)(cda)2, was synthesized by the reaction of sodium car- bamyldicyanomethanide, 4,4-bipyridyl and manganese(II) perchlorate in water solution. The crystal belongs to monoclinic, space group C2/c with a = 20.333(7), b = 6.177(2), c = 15.566(5) ? b = 116.860(5), V = 1744(1) ?, Z = 4, C18H14N8O2 (Mr = 374.37), Dc = 1.426 g/cm3, F(000) = 776, m = 0.100 mm-1 and l = 0.71073 ? The structure was refined to R = 0.0560 and wR = 0.1072 for 590 observed reflections (I > 2s(I)). Two nitrogen atoms of the 4,4?bipyridyl molecule bonded to two hydrogen ions, resulting this neutral molecule into a divalent cation. Through the interaction of colorless H2bpy cation and colorless cda anion the red neutral organic salt was formed.
基金This work was supported by the National Natural Science Foundation of China (No. 20271043) and Natural Science Foundation of Shandong Province (No. Y2002B10)
文摘A two-dimensional coordination polymer [Zn2(DTB)(DMF)4(H2O)2]n has been synthesized by 1,4-dinitro-2,3,5,6-tetracarboxylatebenzenic acid and hydrate zinc perchlorate in the solutions of DMF and H2O. The crystal belongs to the triclinic system, space group P1 with a = 8.887(6), b = 9.225(6), c = 9.828(7) ?, α = 85.249(11), β = 74.863(11), γ = 86.510(13)°, V = 774.4(9), Z = 1, C22H32N6O18Zn2, Mr = 799.28, Dc = 1.714 g/cm3, F(000) = 410 and μ = 1.639 mm-1. The structure was refined to R = 0.0539 and wR = 0.1161 for 1584 observed reflections (I > 2σ(I)). In the complex there exist two kinds of coordination environments for the zinc(II) ions and a two-dimensional sheet is formed via the coordination of carboxylates and zinc(II) ions.
基金This work was supported by the National Natural Science Foundation of China (No. 20271043) and the Natural Science Foundation of Shandong Province (Y2005B25)
文摘Two two-dimensional coordination polymers, [Cd（μ1,3-SCN-）2（μ1,6-L）]n 1 and [Co（μ1,3-SCN-）2（μ1,6-L）]n 2, have been synthesized with 2,3-dimethylpyrazine-1,4-dioxide （L） and thiocyanate as mixed bridging ligands, and their crystal structures were determined by X-ray crystallography. Both crystals belong to monoclinic system, space group C2/c. The other crystal parameters are as follows： for complex 1： α = 9.732（3）, b =14.658（5）, c = 8.811（3） A, β = 102.935（4）°, Z = 4, V= 1225.1（7） A^3, C8H8CdN4O2S2, Mr = 368.71, Dc = 1.999 g/cm^3, F（000） = 720 and μ= 2.117 mm^-1; for complex 2： α = 9.528（7）, b = 14.563（11）, c = 8.415（6） A, β= 102.195（9）°, V= 1141.3（14） A^3, Z = 4, C8H8CoN4O2S2, Mr = 315.23, Dc = 1.835 g/cm^3, F（000） = 636 and μ = 1.863 mm^-1. The two complexes show similar two-dimensional sheet structures. Along the c axis one-dimensional chains are constructed by the coordination of Cd（Ⅱ） （or Co（Ⅱ）） ions with μ1,6-L bridging ligand, and the μ1,3-SCN- bridging ligands make the chains connect to each other, resulting in the formation of a two-dimensional sheet on the ac plane.
基金This work was supported as key project by the Natural Scientific Foundation of Shandong Province
文摘Mononuclear complex [Co(cdm)2(H2O)4]?H2O was synthesized by sodium carbamyldicyanomethanide (Nacda) and cobalt perchlorate. The crystal belongs to monoclinic system, space group P21/n with a = 9.366(3), b = 7.392(3), c = 12.039(4)? = 108.335(4)? V = 791.2(5)?, Z = 2, Mr (C8H16CoN6O8) = 383.2, Dc = 1.608 g/cm3, F(000) = 394, = 1.135 mm-1, = 0.71073 ? The structure was refined to R = 0.0240 and wR = 0.0632 for 1267 observed reflections (I > 2(I)). The cobalt(II) atom in the complex is coordinated by two nitrile-nitrogen atoms and four oxygen atoms of H2O, which forms a slightly distorted coordination octahedron around the cobalt(II) ion. The mononuclear complexes are connected by hydrogen bondings and in the crystal there exists a cavity where the uncoordinated H2O molecules are trapped.
基金This work was supported by the National Natural Science Foundation of China (No. 20271043) and Natural Science Foundation of Shandong Province (No. Y2002B10)
文摘A one-dimensional chain complex {Na[ZnL(H2O)2]}n was synthesized by sodium 2,2-dihydroxyl-malonate (Na2L?) and hydrate zinc perchlorate. The crystal belongs to the mono- clinic system, space group P21/n with a = 5.936(2), b = 7.203(3), c = 19.356(8) ? b = 95.264(6), V = 824.2(6) 3, Z = 4, C3H5NaO8Zn, Mr = 257.43, Dc = 2.075 g/cm3, F(000) = 512 and m = 3.045 mm-1. The structure was refined to R = 0.0381 and wR = 0.0766 for 1188 observed reflections (I > 2s(I)). In the complex the zinc(II) atom is coordinated to six oxygen atoms from two H2O mole- cules, two carboxylate groups, one ionized hydroxyl group and one hydroxyl group. By the coordi- nation of zinc(II) ions and bridging ligand 2-hydroxyl-2-hydroxylate-malonate trivalent anion the one-dimensional chain is constructed.
