Synthesis and Crystal Structure of Sm Cu7.73In3.27: a New 3D Framework Based on [Cu5In4M4]（M=Cu/In） Cluster

A new intermetallic compound, SmC u7.73In3.27, has been synthesized by solid-state reaction of the corresponding pure elements at high temperature, and structurally characterized by single-crystal X-ray diffraction study. SmC u7.73In3.27 crystallizes in tetragonal space group P4/mbm with a = 8.6213(4), c = 10.2538(9), V = 762.13(8) A3, Z = 4, Mr = 1018.90, Dc = 8.880 g/cm3, μ =38.244 mm-1, F(000) = 1789, and the final R = 0.0374 and w R = 0.0836 for 514 observed reflections with I 2σ(I). The structure of SmC u7.69In3.31 belongs to a new structure type and features a three-dimensional(3D) [Cu5In2M4](M = Cu/In) framework composed of [Cu5In4M4] clusters interconnected via sharing In atoms as well as Cu–In and In–In bonds. The Sm atoms are located in the one-dimensional(1D) tunnels along the c-axis. The structural relationship of the title compound with other similar Sm-Cu-In phases was also studied. Band structure calculations based on Density Functional Theory(DFT) method indicate that SmC u7.69In3.31 is metallic.     

Synthesis,Crystal Structure and Band Structure of Tb3Co4Sn（13）

A new intermetallic compound,Tb3Co4Sn13,has been synthesized by solid-state reaction of the corresponding pure elements in a welded tantalum tube at high temperature.Its crystal structure was established by single-crystal X-ray diffraction.Tb3Co4Sn13 crystallizes in cubic,space group Pm3n(No.223) with a = 9.5072(2) ,V = 859.33(3) 3,Z = 2,Mr = 2255.45,Dc = 8.717 g/cm3,μ = 34.369 mm-1,F(000) = 1906,and the final R = 0.0140 and wR = 0.0312 for 199 observed reflections with I > 2σ(I).The structure of Tb3Co4Sn13 belongs to the Yb3Rh4Sn13 type.It is isostructural with RE3Co4Sn13(RE = La,Ce),featuring a 3D [Co4Sn12] framework based on [CoSn6] trigonal prisms.The [CoSn6] trigonal prisms are interconnected via corner-sharing and Sn-Sn bonds to form a 3D [Co4Sn12] framework.The other Sn and Tb atoms are located in the spacers of the 3D framework.Band structure calculations indicate that Tb3Co4Sn13 is metallic.     

两个含2-巯基吡啶-1-氧Au(Ⅰ)配合物的合成、晶体结构与荧光性能

采用溶液法合成了2个含2-巯基吡啶-1-氧(mpo)的Au(Ⅰ)配合物:(ph3P)Au(mpo)(1)和[Au(mpo)2][Na(H2O)4].H2O(2)。通过X-射线单晶衍射与元素分析等方法确定了其晶体结构。配合物1属单斜晶系,空间群为P21/c,而配合物2属正交晶系,空间群为Pnma。配合物1的结构为零维的(ph3P)Au(mpo),而配合物2的结构是Au(mpo)2单元与一维Na(H2O)4带以及游离水分子通过氢键连结而成的三维结构。荧光测试表明,化合物2在300 nm紫外光激发下可以发射较强的蓝光(423.5 nm)。     

Synthesis, Crystal Structure and Chemical Bonding of a New Binary Lu-Sn Phase: Lu11Sn10

A new tetragonal phase of Lu11Sn10 is obtained from high temperature reaction of the pure elements in a welded tantalum tube. Its crystal structure was established by single-crystal X-ray diffraction. Lu11Sn10 crystallizes in the tetragonal space group I4/mmm (No.139) with a=11.2953(18), c=16.424(4), V=2095.5(7)3 , Z=4, Mr=3111.57, Dc=9.863 g/cm3 , μ=62.897 mm-1, F(000)=5124, and the final R=0.0348 and wR=0.0894 for 706 observed reflections with I>2σ(I). The structure of Lu11Sn10 may be derived from the Ho11Ge10 structural type. It is isostructural with Dy11Sn10 , featuring a three-dimensional (3D) framework composed of [Sn4] squares and [Sn2] dimers interlinked via Sn-Sn bonds with two types of one-dimensional (1D) tunnels along the c-axis, which are occupied by isolated Sn atoms, [Sn2] dimers and all the Lu atoms. Band structure calculation based on density functional theory method indicates that Lu11Sn10 is metallic.     

极性金属间化合物MgIn2的合成、晶体结构及能带特征

在惰性气氛氩气保护下,通过高温固相反应合成得到了一个二元极性金属间化合物MgIn2。经X-射线单晶衍射与元素分析等方法确定了其晶体结构。MgIn2属立方体系,空间群为Fd3m(No.227),晶体学参数a=0.956 13(16)nm,V=0.874 1(3)nm3,Z=8,R1=0.035 3,wR2=0.082 8。MgIn2属于CaAl2结构类型,其结构特征为[In4]四面体通过共用顶点In原子链接而成的三维框架结构,Mg原子填充在三维框架的空隙中。能带结构计算表明MgIn2属于金属性的化合物。     

Synthesis and Structure of a New Coordination Polymer Based on Indium and 1,4-Benzenedicarboxylate

A new coordination polymer {[In(bdc)(OH)]·4H2O}n(H2bdc=1,4-benzenedi-carboxylic acid) has been synthesized through hydrothermal conditions,and was characterized by X-ray single-crystal diffraction and other measurements.The complex crystallizes in the orthorhombic system,space group Imma with a=18.3621(13),b=7.1932(5),c=11.8278(8),V=1562.24(19)3,Z=4.Dc=1.565g/cm3,Mr=368.00,F(000)=728,μ(MoKα)=1.542 mm-1,S=1.019,R=0.0468 and wR=0.1326 for 884 observed reflections(2σ(Ⅰ)).The title compound represents a 3-D framework containing four kinds of tunnels in different shapes and sizes.     

Two-dimensional Supramolecular Structure of a Mercury（Ⅱ） Iodide Complex with Organosulfide

A mercury（Ⅱ） iodide complex with organosulfide [Hg（pymt）（pymtH）I] 1 （pymt = the anion of pyrimidine-2-thiolate） has been synthesized by slow evaporation of the solution at room temperature and structurally characterized by single-crystal X-ray diffraction. Basic ideas and data collected are given. X-ray diffraction analysis reveals that complex 1 is mononuclear. Crystallographic data： C8H7HgIN4S2, Mr = 550.79, monoclinic system, space group P21/c, a = 11.218（4）, b = 9.551（3）, c = 15.877（4） A^°, β = 129.697（15）°, V = 1308.9（7） A^°^3, Z = 4, Mr = 550.79, Dc = 2.795 g/cm^3, F（000） = 995, μ（MoKa） = 14.415 mm^-1, 2（MoKa） = 0.71073 A^°, T= 293（2） K, 2θmax = 54.9°, GOOF= 1.053, the final R = 0.0310 and wR = 0.0742 for 2547 observed reflections with I 〉 2σ（I） （refinement on F^2）. Complex 1 is connected through hydrogen bonds to give a one-dimensional supramolecular chain structure. Furthermore, π-π interactions are also found between the pyrimidine rings with the center-to-center distances of 3.439（4） and 3.603（4） A^°, so complex 1 expands the chains into a two-dimensional network.     

Synthesis and Crystal Structure of a 2-D Hydrogen-bonded Supramolecular Network {[Cu_4(OH)_4(2,2'-bpy)_4(bqdc)]·2ClO_4}_n

The title compound {[Cu4(OH)4(2,2'-bpy)4(bqdc)]·2ClO4}n 1 (bqdc = 2,2'-biquino- line-4,4'-dicarboxylic acid) has been synthesized by hydrothermal method. Its crystal structure is of triclinic, space group P1 with a = 7.6561(5), b = 12.4652(8), c = 15.7501(10) , α = 80.0480(10), β = 87.7900(10), γ = 74.0800(1)o, V = 1423.65(16) 3, Z = 2, C30H23ClN5O8Cu2, Mr = 744.06, Dc = 1.736 g/cm3, μ = 1.651 mm─1, F(000) = 754, the final R = 0.0421 and wR = 0.1163 for 4973 observed reflections with I > 2σ(I). In 1, tetra-copper chair-like clusters of [Cu4(OH)4(2,2'-bpy)4]4+ are connected by bqdc ligands to form one-dimensional chains, which are further connected by hydrogen bonds to generate a two-dimensional supramolecular network .     

两个含2-巯基吡啶-1-氧Au(Ⅰ)配合物的合成、晶体结构与荧光性能

采用溶液法合成了2个含2-巯基吡啶-1-氧(mpo)的Au(Ⅰ)配合物:(ph₃P)Au(mpo) (1)和[Au(mpo)₂][Na(H₂O)₄]·H₂O (2)。通过X-射线单晶衍射与元素分析等方法确定了其晶体结构。配合物1属单斜晶系, 空间群为P2₁/c, 而配合物2属正交晶系, 空间群为Pnma。配合物1的结构为零维的(ph₃P)Au(mpo), 而配合物2的结构是Au(mpo)₂单元与一维Na(H₂O)₄带以及游离水分子通过氢键连结而成的三维结构。荧光测试表明, 化合物2在300 nm紫外光激发下可以发射较强的蓝光(423.5 nm)。     

极性金属间化合物LuSn2的合成、晶体结构及能带特征

在惰性气氛氩气保护下,通过高温固相反应合成得到了一个新的二元极性金属间化合物LuSn2。经X-射线单晶衍射与元素分析等方法确定了其晶体结构。LuSn2属正交晶系,空间群为Cmcm,晶体学参数a=0.435 11(10)nm,b=1.601 6(4)nm,c=0.427 80(8)nm,V=0.298 12(11)nm3,Z=4,R1=0.017 0,wR2=0.032 4。LuSn2属于ZrSi2结构类型,其结构中包含有一维"之"字型Sn链与二维四方格子状Sn层,Lu原子排列在Sn链与Sn层的空隙中。能带结构计算表明LuSn2呈金属导电性。