A novel 1,2-diaminocyclohexane(1,2-DACH) decorated manganese thiostannate,namely MnSnS_3(1,2-DACH)(1),has been solvothermally synthesized by the reaction of Mn(CH_3COO)_2·4H_2O,Sn and S in the stoichiomet...A novel 1,2-diaminocyclohexane(1,2-DACH) decorated manganese thiostannate,namely MnSnS_3(1,2-DACH)(1),has been solvothermally synthesized by the reaction of Mn(CH_3COO)_2·4H_2O,Sn and S in the stoichiometric ratio in 1,2-DACH,which acted as an efficient structure-directing agent(SDA) and reactive solvent in the formation of the title compound. Single-crystal X-ray diffraction studies revealed that the title compound crystallizes in the monoclinic space group P2_1/c with a = 12.2458(7),b = 13.8588(7),c = 7.2292(4) ?,β = 99.460(6)°,V = 1210.20(12) ?~3,Z = 4,Dc = 2.108 g·cm^(-3),F(000) = 748,μ = 3.584 mm^(-1),R = 0.0348 and wR = 0.0823(I 〉 2σ(I)). The structure features a neutral two-dimensional(2D) network constructed by the unsaturated [Mn(1,2-DACH)] complexes interconnecting [SnS_3]_n^(2n-) chains via sharing S. Thermal stability and optical property of compound 1 were characterized.展开更多
A novel manganese(H) coordination polymer [Mn(pdc)]n (pdc = pyridine-2,4- dicarboxylate) has been synthesized under hydrothermal conditions. The crystal is of monoclinic, space group P211n with a = 6.506(4), b...A novel manganese(H) coordination polymer [Mn(pdc)]n (pdc = pyridine-2,4- dicarboxylate) has been synthesized under hydrothermal conditions. The crystal is of monoclinic, space group P211n with a = 6.506(4), b = 9.392(6), c = 11.217(7) A, β = 105.650(12)°, V= 660.0(7)A3, Z = 4, Mr = 220.04, Dc = 2.215 g/cm3,μ = 1.971 mm-1, F(000) = 436, Rint = 0.0345, R = 0.0360 and wR = 0.0778 for 1259 observed reflections with I 〉 2σ(I). In the structure, the Mn(Ⅱ) atom is coordinated in a distorted octahedral arrangement by one pyridine N and five carboxylate O atoms from five pdc ligands, each of which coordinates to five Mn atoms to propagate a three-dimensional layered framework.展开更多
A new thiostannate,[tmdpH2]Sn3S7 1(tmdp = 4,4'-trimethylenedipiperidine),has been synthesized under solvothermal conditions and characterized by elemental analysis,IR spectroscopy,and single-crystal X-ray diffracti...A new thiostannate,[tmdpH2]Sn3S7 1(tmdp = 4,4'-trimethylenedipiperidine),has been synthesized under solvothermal conditions and characterized by elemental analysis,IR spectroscopy,and single-crystal X-ray diffraction analysis.In 1,the Sn3S4 secondary incomplete cubane-like building units are bridged by μ2-S atoms to form Sn12S12 rings which are then joined parallelly to the [001] plane,giving the final 2D(Sn3S7^2-)n layer of(6,3) network.The layers are stacked along the c axis so that 24-membered ring channels are generated,in which the organic cations are accommodated.The compound crystallizes in monoclinic,space group C2/c,with a=23.052(3),b=13.4039(12),c=18.412(2)A,β=120.112(4)°,V=4921.3(9)A^3,C13H28N2S7Sn3,Mr=792.86,Z=8,Dc=2.140 g/cm^3,F(000)=3056,μ=3.619 mm^-1,the final R=0.0488 and wR=0.1125 for 4607 observed reflections with I〉2σ(I).展开更多
The novel complex [K(18-C-6)]_2 [Cd(mnt)_2] [18-C-6 = 18-crown-6, mnt =1,2-dicyanoethene-1,2-dithiolate, C_2S_2-(CN)_2^(2-)] was synthesized and characterized by elementalanalysis, IR spectrum and X-ray diffraction an...The novel complex [K(18-C-6)]_2 [Cd(mnt)_2] [18-C-6 = 18-crown-6, mnt =1,2-dicyanoethene-1,2-dithiolate, C_2S_2-(CN)_2^(2-)] was synthesized and characterized by elementalanalysis, IR spectrum and X-ray diffraction analysis. The complex displays two-dimensional networkstructure of [K(18-C-6)] complex segments and [Cd(mnt)_2] complex segment bridged by S-K-S, S-K-Nand N-K-N interactions between adjacent [K(18-C-6)] and [Cd(mnt)_2] units.展开更多
In an attempt to synthesize supra-molecular complex of copper(II) with mixed ligands in a solution reaction of Cu(ClO 4) 2·6H 2O with 4,5-diazafluorene-9-one (dafo) and o-phthalic acid, the bright blue col...In an attempt to synthesize supra-molecular complex of copper(II) with mixed ligands in a solution reaction of Cu(ClO 4) 2·6H 2O with 4,5-diazafluorene-9-one (dafo) and o-phthalic acid, the bright blue column-like crystal [Cu(dafo) 2(H 2O) 2]-(ClO 4) 2 was obtained. Its structure was determined by single-crystal X-ray diffraction study. The crystal belongs to monoclinic system, space group P2(1)/n with cell dimensions: a=0.7947(3) nm, b=1.2021(5) nm, c=1.3190(5) nm, α=90.000(5)°, β=90.000(5)°, γ= 90.000(5)°, V=1.2600(9) nm 3, Z=2, F(000)=670, M r=662.83, D c=1.747 g/cm 3, μ (Mo Kα)=1.154 mm -1, R 1=0.0455, wR 2=0.1041. The analysis of the crystal structure indicates that the complex has a two-dimensional network structure which is formed by hydrogen bonds.展开更多
The copper(Ⅱ) complex [Cu_3(nta)_2(azpy)_2(H_2O)_2]·6H_2O (nta =nitrilotriacetate, azpy = 4,4′-azobispyridine) has been synthesized and characterized. The X-rayanalysis reveals that there are two kinds of copp...The copper(Ⅱ) complex [Cu_3(nta)_2(azpy)_2(H_2O)_2]·6H_2O (nta =nitrilotriacetate, azpy = 4,4′-azobispyridine) has been synthesized and characterized. The X-rayanalysis reveals that there are two kinds of copper(Ⅱ) coordination environments. Cu(1) has adistorted square plane symmetry and Cu(2) has a distorted octahedral symmetry. Cu(1) is linked toCu(2) through nta and bound to Cu(1C) by azpy, and Cu(2) is linked to Cu(2A) through azpy, whichextends to two-dimensional network with large rhombus 1.2 nm x 1.7 nm.展开更多
Two novel one- and two-dimensional network structure bismuth(III) complexes with N,N-di(2-hydroxylethyl)- aminodithiocarboxylate, {Bi[S2CN(C2H4OH)2]2[1,10-Phen]2(NO3)}3H2O (1) and {Bi[S2CN(C2H4OH)2]3}2 (2) were synthe...Two novel one- and two-dimensional network structure bismuth(III) complexes with N,N-di(2-hydroxylethyl)- aminodithiocarboxylate, {Bi[S2CN(C2H4OH)2]2[1,10-Phen]2(NO3)}3H2O (1) and {Bi[S2CN(C2H4OH)2]3}2 (2) were synthesized. Their crystal and molecular structures were determined by X-ray single crystal diffraction analysis. The crystal 1 belongs to monoclinic system with space group C2/c, a=1.6431(7) nm, b=2.4323(10) nm, c=1.2646(5) nm, =126.237(5)o, Z=4, V=4.076(3) nm3, Dc=1.757 Mg/m3, =4.598 mm-1, F(000)=2156, R=0.0211, wR=0.0369. The structure shows a distorted square antiprism configuration with eight-coordination for the central Bi atom. The one-dimensional chain structure was formed by H-bonding interaction between hydroxyl group of N,N-di(2-hydroxylethyl)aminodithiocarboxylate ligands and crystal water. The crystal 2 belongs to monoclinic system with space group P2(1)/c, a=1.1149(4) nm, b=2.1274(8) nm, c=2.2107(8) nm, =98.325(8), Z=4, V=5.188(3) nm3, Dc=1.920 Mg/m3, =7.315 mm-1, F(000)=2944, R=0.0565, wR=0.0772. The structure shows a distorted square antiprism configuration with eight-coordination for the central Bi atoms. The two-dimensional network structure was formed by H-bonding interaction between adjacent molecules.展开更多
基金Financial support from the NNSFC(No.21373223)Chunmiao project of Haixi Institute of Chinese Academy of Sciences(CMZX-2014-001)
文摘A novel 1,2-diaminocyclohexane(1,2-DACH) decorated manganese thiostannate,namely MnSnS_3(1,2-DACH)(1),has been solvothermally synthesized by the reaction of Mn(CH_3COO)_2·4H_2O,Sn and S in the stoichiometric ratio in 1,2-DACH,which acted as an efficient structure-directing agent(SDA) and reactive solvent in the formation of the title compound. Single-crystal X-ray diffraction studies revealed that the title compound crystallizes in the monoclinic space group P2_1/c with a = 12.2458(7),b = 13.8588(7),c = 7.2292(4) ?,β = 99.460(6)°,V = 1210.20(12) ?~3,Z = 4,Dc = 2.108 g·cm^(-3),F(000) = 748,μ = 3.584 mm^(-1),R = 0.0348 and wR = 0.0823(I 〉 2σ(I)). The structure features a neutral two-dimensional(2D) network constructed by the unsaturated [Mn(1,2-DACH)] complexes interconnecting [SnS_3]_n^(2n-) chains via sharing S. Thermal stability and optical property of compound 1 were characterized.
基金This project was supported by the NNSFC (No. 20471061)the Science & Technology Innovation Foundation for the Young Scholar of Fujian Province (No. 2005J059)
文摘A novel manganese(H) coordination polymer [Mn(pdc)]n (pdc = pyridine-2,4- dicarboxylate) has been synthesized under hydrothermal conditions. The crystal is of monoclinic, space group P211n with a = 6.506(4), b = 9.392(6), c = 11.217(7) A, β = 105.650(12)°, V= 660.0(7)A3, Z = 4, Mr = 220.04, Dc = 2.215 g/cm3,μ = 1.971 mm-1, F(000) = 436, Rint = 0.0345, R = 0.0360 and wR = 0.0778 for 1259 observed reflections with I 〉 2σ(I). In the structure, the Mn(Ⅱ) atom is coordinated in a distorted octahedral arrangement by one pyridine N and five carboxylate O atoms from five pdc ligands, each of which coordinates to five Mn atoms to propagate a three-dimensional layered framework.
基金supported by the 973 Program (2007CB815301 and 2006CB932904)the National Natural Science Foundation of China (20333070, 20673118, 20871114)+1 种基金the Science Foundation of CAS (KJCX2-YW-M05)Fujian Province (2006L2005, 2006J0014, 2006F3132)
文摘A new thiostannate,[tmdpH2]Sn3S7 1(tmdp = 4,4'-trimethylenedipiperidine),has been synthesized under solvothermal conditions and characterized by elemental analysis,IR spectroscopy,and single-crystal X-ray diffraction analysis.In 1,the Sn3S4 secondary incomplete cubane-like building units are bridged by μ2-S atoms to form Sn12S12 rings which are then joined parallelly to the [001] plane,giving the final 2D(Sn3S7^2-)n layer of(6,3) network.The layers are stacked along the c axis so that 24-membered ring channels are generated,in which the organic cations are accommodated.The compound crystallizes in monoclinic,space group C2/c,with a=23.052(3),b=13.4039(12),c=18.412(2)A,β=120.112(4)°,V=4921.3(9)A^3,C13H28N2S7Sn3,Mr=792.86,Z=8,Dc=2.140 g/cm^3,F(000)=3056,μ=3.619 mm^-1,the final R=0.0488 and wR=0.1125 for 4607 observed reflections with I〉2σ(I).
文摘The novel complex [K(18-C-6)]_2 [Cd(mnt)_2] [18-C-6 = 18-crown-6, mnt =1,2-dicyanoethene-1,2-dithiolate, C_2S_2-(CN)_2^(2-)] was synthesized and characterized by elementalanalysis, IR spectrum and X-ray diffraction analysis. The complex displays two-dimensional networkstructure of [K(18-C-6)] complex segments and [Cd(mnt)_2] complex segment bridged by S-K-S, S-K-Nand N-K-N interactions between adjacent [K(18-C-6)] and [Cd(mnt)_2] units.
文摘In an attempt to synthesize supra-molecular complex of copper(II) with mixed ligands in a solution reaction of Cu(ClO 4) 2·6H 2O with 4,5-diazafluorene-9-one (dafo) and o-phthalic acid, the bright blue column-like crystal [Cu(dafo) 2(H 2O) 2]-(ClO 4) 2 was obtained. Its structure was determined by single-crystal X-ray diffraction study. The crystal belongs to monoclinic system, space group P2(1)/n with cell dimensions: a=0.7947(3) nm, b=1.2021(5) nm, c=1.3190(5) nm, α=90.000(5)°, β=90.000(5)°, γ= 90.000(5)°, V=1.2600(9) nm 3, Z=2, F(000)=670, M r=662.83, D c=1.747 g/cm 3, μ (Mo Kα)=1.154 mm -1, R 1=0.0455, wR 2=0.1041. The analysis of the crystal structure indicates that the complex has a two-dimensional network structure which is formed by hydrogen bonds.
文摘The copper(Ⅱ) complex [Cu_3(nta)_2(azpy)_2(H_2O)_2]·6H_2O (nta =nitrilotriacetate, azpy = 4,4′-azobispyridine) has been synthesized and characterized. The X-rayanalysis reveals that there are two kinds of copper(Ⅱ) coordination environments. Cu(1) has adistorted square plane symmetry and Cu(2) has a distorted octahedral symmetry. Cu(1) is linked toCu(2) through nta and bound to Cu(1C) by azpy, and Cu(2) is linked to Cu(2A) through azpy, whichextends to two-dimensional network with large rhombus 1.2 nm x 1.7 nm.
基金Project supported by the National Natural Science Foundation of China (No. 20271025) and the Natural Science Foundation of Shandong Province (No. L2003B01).
文摘Two novel one- and two-dimensional network structure bismuth(III) complexes with N,N-di(2-hydroxylethyl)- aminodithiocarboxylate, {Bi[S2CN(C2H4OH)2]2[1,10-Phen]2(NO3)}3H2O (1) and {Bi[S2CN(C2H4OH)2]3}2 (2) were synthesized. Their crystal and molecular structures were determined by X-ray single crystal diffraction analysis. The crystal 1 belongs to monoclinic system with space group C2/c, a=1.6431(7) nm, b=2.4323(10) nm, c=1.2646(5) nm, =126.237(5)o, Z=4, V=4.076(3) nm3, Dc=1.757 Mg/m3, =4.598 mm-1, F(000)=2156, R=0.0211, wR=0.0369. The structure shows a distorted square antiprism configuration with eight-coordination for the central Bi atom. The one-dimensional chain structure was formed by H-bonding interaction between hydroxyl group of N,N-di(2-hydroxylethyl)aminodithiocarboxylate ligands and crystal water. The crystal 2 belongs to monoclinic system with space group P2(1)/c, a=1.1149(4) nm, b=2.1274(8) nm, c=2.2107(8) nm, =98.325(8), Z=4, V=5.188(3) nm3, Dc=1.920 Mg/m3, =7.315 mm-1, F(000)=2944, R=0.0565, wR=0.0772. The structure shows a distorted square antiprism configuration with eight-coordination for the central Bi atoms. The two-dimensional network structure was formed by H-bonding interaction between adjacent molecules.