胍基稀土配合物[(CH2)5NC(NiPr)2]3Yb的合成及晶体结构

胍基可以通过改变氮上的取代基来调控配合物的空间及电荷效应,它们作为辅助配体用于稀土金属配合物的合成得到了人们的广泛关注。本文通过胍基锂盐和无水YbCl3以3：1的摩尔比进行复分解反应,合成了均配型稀土化合物[(CH2)5NC(N^iPr)2]3Yb,测得它为正交品系,     

新型三齿含膦配体的Ni(Ⅱ)配合物的合成和晶体结构

A new tridentate Ni(Ⅱ) complex {Ni(H₂O)₃[Ph₂(o-Ph-N-C₇H₇N)]PO}Cl₂ was synthesized by the reaction of a new ligand Ph₂(o-Ph-N-C₇H₇N)]PO with NiCl₂ in CH₃CH₂OH. The complex was characterized by X-ray single crystal diffraction. The crystal structure of the complex belongs to monoclinic space group P2₂/n, a=1.259 28(9) nm, b=1.201 24(8) nm, c=2.039 03(14) nm, V=3.016 8(4) nm^-3, Z=4, and R₂=0.047 1, wR₂=0.120 5. And a molecular CH₂Cl₂ is filled in the crystal structure. CCDC: 241832.     

Crystallographic report: Crystal and molecular structure of Ph3GeO2CC4H3O

The germanium atom in the title compound is in a distorted tetrahedral geometry defined by an oxygen donor, derived from an effectively monodentate carboxylate ligand, and three ipso‐carbon atoms from the phenyl substituents. Copyright © 2005 John Wiley & Sons, Ltd.     

Crystallographic report: Dimeric tetraphenyl‐1‐hydroxo‐3‐trifluoromethanesulfonatodistannoxane, [Ph2(HO)SnOSn(O3SCF3)Ph2]2

The molecular structure of the title compound, obtained by an adventitious phenyl group cleavage of Ph₃SnOSnPh₃ with triflic acid, reveals discrete centrosymmetric units of [Ph₂(HO)SnOSn(O₃SCF₃)Ph₂]₂ that are loosely associated via hydrogen bonding. Copyright © 2004 John Wiley & Sons, Ltd.     

羟化三苯基锡和(双三苄基锡)氧化物的合成及晶体结构研究

在乙醇钠存在下三苯基氯化锡或三苄基氯化锡水解得羟化三苯基锡 (1)或 (双三苄基锡 )氧化物 (2 )。其结构经元素分析、IR和1HNMR表征 ,X 射线单晶衍射测定了其晶体结构。 1为正交晶系 ,空间群P2 1/n,a =0 .830 0 0 (19)nm ,b =1.0 36 5 (2 )nm ,c =1.80 2 6 (4 )nm ,β =95 .4 72 (7)°,Z =4 ,V =1.5 5 0 7(6 )nm3 ,Dc=1.5 72g·cm -3 ,μ=1.6 4 0mm -1,F(0 0 0 ) =72 8,R1=0 .0 30 9,WR2 =0 .0 70 6 ,中心锡原子为五配位的三角双锥构型 ,且通过配位氧原子连成无限链状。 2为正交菱面体晶系 ,空间群R3 ,a =b =c =0 .96 36 (3)nm ,α =β =γ =84 .0 85 (3)° ,Z =1,V =0 .8812 (4 )nm3 ,Dc=1.5 0 8g·cm -3 ,μ =1.4 4 8mm -1,F(0 0 0 ) =4 0 2 ,R1=0 .0 36 0 ,WR2 =0 .0 5 4 2 ,由两个中心锡原子组成一个结构单元的四配位线性聚合体。     

Crystallographic report: 6‐Mercaptopurinate complex of tribenzyltin(IV), (PhCH2)3Sn(C5H3N4S)Sn(PhCH2)3OMe

The title complex displays a binuclear structure in which the geometries of tin atoms are different: one is cis‐trigonal bipyramidal (with a C₃NS donor set) and the other is trans‐trigonal bipyramidal (C₃NO). Copyright © 2004 John Wiley & Sons, Ltd.     

Syntheses and Crystal Structures of Homleptic Lanthanide Complexes [C_6H_5COCHC(CH_3)N-(p-ClC_6H_4)]_3Ln(THF)_n (Ln =Yb,Y,Nd)

Three homoleptic lanthanide complexes, [C6H5COCHC(CH3)N(p-ClC6H4)]3Ln(THF)n(n = 0, Ln = Yb(1); n = 0, Ln = Y(2); n = 1, Ln = Nd(3)), were synthesized by amine elimination reaction of Ln[N(SiMe3)2]3 with 1-phenyl-3-N-(p-chlorophenylimino)-1-butanone. These complexes crystallize in triclinic, space group P1 with a = 9.805(3), b = 14.831(6), c = 16.075(6) A, α = 111.996(9), β = 91.570(7), γ = 93.744(6)°, V = 2159.4(13) A3, Z = 2, D3 c = 1.515 g/cm, F(000) = 986, μ(MoKα) = 2.396 mm-1, R = 0.0360 and wR = 0.0850 for 9548 observed reflections with I 2σ(I) for complex 1; a = 9.861(5), b = 14.852(9), c = 16.111(9) A, α = 112.362(13), β = 91.949(11), γ = 93.678(14)°, V = 2173(2) A3, Z = 2, Dc = 1.377 g/cm3, F(000) = 924, μ(MoKα) = 1.570 mm-1, R = 0.0735 and wR = 0.1389 for 8015 observed reflections with I 2σ(I) for complex 2; and a = 9.308(3), b = 15.357(3), c = 17.419(4) A, α = 66.493(13), β = 88.61(2), γ = 86.664(19)°, V = 2279.4(9) A3, Z = 2, Dc = 1.499 g/cm3, F(000) = 1046, μ(MoKα) = 1.364 mm-1, R = 0.0843 and wR = 0.2280 for 8433 observed reflections with I 2σ(I) for complex 3. Each central metal in complexes 1 and 2 is six-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands to give a distorted octahedral geometry, while the central metal in 3 is seven-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands and one oxygen atom from the solvated THF molecule to complete a distorted monocapped trigonal prism.     

Crystallographic report: Diiodo[tris(2‐pyridyl)amine]mercury(II), [(C5H4N)3N]HgI2

In mononuclear HgI₂[(C₅H₄N)₃N], mercury is tetrahedrally coordinated by two nitrogen atoms of a tris(2‐pyridyl)amine ligand and two iodides. The coordination moieties are connected by weak intermolecular Hg(II)···I interactions to give a one‐dimensional structure. Copyright © 2003 John Wiley & Sons, Ltd.     

[C5H4C(CH3)2CH2CH=CH2]Sm(OH)Cl·2MgCl2·4THF的晶体结构分析

用Ｘ－射线晶体结构衍射法测定了［Ｃ５Ｈ４Ｃ（ＣＨ３）２ＣＨ２ＣＨ＝ＣＨ２］Ｓｍ（ＯＨ）Ｃｌ·２ＭｇＣｌ２·４ＴＨＦ的晶体结构。它属三斜晶系,空间群为Ｐ＾－１,ａ＝１０．７７３（２）,ｂ＝１２．８３６（３）,ｃ＝１５．４７８（３）Ａ,ａ＝１１１．４６（３）,β＝１０７．７１（３）,γ＝９２．５４（３）°,Ｖ＝１８６８（１）Ａ＾３,Ｍｒ＝８２７．９１,Ｄｘ＝１．４７２ｇ／ｃｍ＾３,μ＝２．０００６ｍｍ     

1-甲基-1-丙基-3-丁烯基环戊二烯基钆配合物的合成和晶体 结构分析

用X-射线晶体结构衍射法测定了[C~5H~4C(CH~3)(C~3H~7)CH~2CH=CH~2]Gd(OH)Cl.2MgCl~2.4THF的晶体结构。它属三斜晶系,空间群为P1,a=1.2757(3),b=1.3571(3),c=1.3725(3)nm,α=69.22(3),β=84.91(3),γ=63.48(3)ⅲ,V=1.929(1)nm^3,Mr=862.75,Dx=1.423g/cm^3,μ=2.0832mm^-^1,F(000)=848,Z=2,R=0.096,ωR=0.113(I≥3σ(I))。分子中Gd原子的配位数为8,形成一个严重扭曲的八面体结构;两个Mg原子的配位情况相似,它们的配位数都是6,构成两个扭曲的八面体。这三个八面体通过三个共用平面联接。     

Synthesis and Crystal Structure of [Cu（bbtz）（HCOO）2（H2O）2]n

1 INTRODUCTION Crystal engineering principles have been employ- yed in recent years to produce a variety of coordi- nation networks[1], which are of great current interest not only for their potential properties as functional solid materials[2] in host-guest chemistry, ion ex- change and catalysis, but also for their often com- plicated intriguing architectures and topologies. Ra- tional control the construction of polymeric net- works remains a great challenge in crystal engineer- ing. Mu…     

Crystallographic report: Tetraphenylphosphonium nitratobis (chlorodiphenylstannate)methane, [Ph4P]+[(Ph2ClSn)2CH2 ·NO3]−

The nitrate anion coordinates to the Sn? CH₂? Sn unit of the title phosphonium stannate, [Ph₄P]⁺ [(Ph₂ClSn)₂CH₂ ·NO₃]^?, to give a six‐membered ring having the penta‐coordinated tin atoms in a trigonal bipyramidal geometry. Copyright © 2003 John Wiley & Sons, Ltd.     

Crystallographic report: The crystal structure of 2‐benzo[b]thienylgermatrane

The germanium atom is penta‐coordinated and adopts trigonal bipyramidal geometry. The 2‐benzo[b]thienyl group and the nitrogen atom each occupy an apical position with the transannular N → Ge bond distance being 2.180(4) Å. Copyright © 2003 John Wiley & Sons, Ltd.     

Crystallographic report: Polymeric [diaqua bis(3‐pyridylacrylato)zinc(II)]

The Zn center in [bis(3‐pyridylacrylato)diaquazinc(II)]_n is in a slightly distorted octahedral geometry within a cis‐N₂O₄ donor set. Each tridentate 3‐pyridylacrylate ligand links two Zn centers, resulting in the formation of a linear chain. Copyright © 2005 John Wiley & Sons, Ltd.     

金属碲化物[Ga(en)~3]In~3Te~7晶体结构和性质的研究

以有机溶剂热生长技术(solvothermaltechnique),即在180℃乙二胺(en)溶液中,以GaCl~3,InCl~3,Rb~2Te和Te在密闭容器中反应7d,制备出新的硫族化合物[Ga(en)~3]In~3Te~7。其阴离子基团为Zintlanion:~∞^2[In~3Te~7]^3^-,阳离子基团为Ga与乙二胺(en)的配合物:[Ga(en)~3]^3^+。以单晶X射线衍射技术解得该晶体结构属单钭晶系,空间群为P2~1/c,(no.14),{Ga(en)~3]In~3Te~7的晶胞数据：a=1.0460(2)nm,b=1.6981(3)nm,c=1.4994(6)nm,α=90°,β=95.46(2)°,γ=90°,V=2.651(1)nm^3,Z=4。热分析结果表明,该化合物的热分解分三步进行。光学性质测试表明它们是半导体材料,禁带宽度为1.65eV。     

Crystallographic report: [Bis(3‐pyridylacrylato)cadmium(II)]n

In [bis(3‐pyridylacrylato)cadmium(II)]_n, the local coordination geometry around the cadmium center is based on an octahedron. The carboxylate acts as a tridentate ligand by bridging two cadmium atoms and binds a third cadmium atom via the pyridyl group with the result that a two‐dimensional layered network is formed. Copyright © 2005 John Wiley & Sons, Ltd.     

Crystallographic report: Bis(tetraphenylphosphonium) bis(dichloro‐nitratophenylstannate)methane, [Ph4P+]2 [(PhCl2(NO3)Sn)2CH2]2−

Each tin atom of the title compound is five‐coordinate, defined by 2C, 2Cl and 1O atoms, and shows a distorted square pyramidal configuration stabilized by intramolecular Sn· · ·O or Sn· · ·Cl interactions. Both nitrate anions coordinate the tin atoms in a monodentate mode. Copyright © 2003 John Wiley & Sons, Ltd.     

Crystallographic report: A two‐dimensional zinc phosphate framework: [H3N(CH2)3NH3]0.5[Zn2(PO4)(HPO4)]

The two‐dimensional zinc phosphate [H₃N(CH₂)₃NH₃]_0.5[Zn₂(PO₄)(HPO₄)], has been synthesized hydrothermally using 1,3‐diaminopropane as the template. Its structure contains an inorganic framework with three‐, four‐, or six‐membered rings, built from PO₄, PO₃(OH) and ZnO₄ tetrahedral moieties sharing vertexes. The protonated 1,3‐diaminopropane molecules interact with the framework through hydrogen bonds. Copyright © 2004 John Wiley & Sons, Ltd.     

酰胺型三足体铜配合物[CuL][CuCl2(NO3)2]的合成及晶体结构

The title complex， [CuL][CuCl₂(NO₃)₂] [L=N，N，N′，N′，N″，N″-Hexaisopropyl-2， 2′， 2″-Nitrilotris(2，1-ethoxy)triacetamide]， has been synthesized by using an amide-type tripodal ligand with Cu(NO₃)₂ and then characterized by X-ray single crystal structure analysis. It belongs to monoclinic，space group P2₁/c with a=1.522 7(2) nm，b=1.277 8(2) nm， c=2.184 5(4) nm， β=93.680(10)°， V=4.241 6(12) nm³， Z=4， D_c=1.401 Mg·m^-3， μ=1.189 mm^-1， F(000)=1 880， and final R₁=0.050 9， wR₂=0.125 3. The results show a Cu(Ⅱ) ion was encapsulated by the three chains of the cup-like heptadentate ligand and four-coordinated by the central nitrogen atom and three oxygen atoms from the ligand. CCDC: 648900.     

Tetraammin-Lithium-Kationen zur Stabilisierung phenylsubstituierter Zintl-Anionen: Die Verbindung [Li(NH3)4]2[Sn2Ph4]

Tetraammine Lithium Cations Stabilizing Phenylsubstituted Zintl-Anions: The Compound [Li(NH₃)₄]₂[Sn₂Ph₄] Ruby-red, brittle single crystals of [Li(NH₃)₄]₂[Sn₂Ph₄] were synthesized by the reaction of diphenyltin dichloride and metallic lithium in liquid ammonia at ?35°C. The structure was determined from X-ray singlecrystal diffractometer data: Space group, P1 , Z = 1, a = 9.462(2) Å, b = 9.727(2) Å, c = 11.232(2) Å, α = 66.22(3)°, β = 85.78(3)°, γ = 61.83(3)°, R₁ (F ? 4σF) = 5.13%, wR₂ (F₀² ? 4σF) = 10.5%, N(F ? 4σF) = 779, N(Var.) = 163. The compound contains to Sb₂Ph₄ isosteric centres [Sn₂Ph₄]^2? as anions which are connected to rods by lithium cations in distorted tetrahedral coordination by ammonia. These rods are arranged parallel to one another in the b,c-plane, but stacked along [100].