Synthesis and Characterization of [NH3（CH2）2NH2（CH2）2NH3]BiCl6

1 INTRODUCTION During the past decade, a series of organic-inor- ganic hybrid compounds based on metal halide units have been prepared and studied[1]. The combination of organic and inorganic components at the mole- cular level affords us the opportunity to design new hybrid materials and modulate the properties of components[2]. As a result, some interesting proper- ties, such as non-linear optical[3], interesting magne- tic[4], efficient luminescence[2], ideal thermal and mechanical sta…     

双核有机锡(Ⅳ)配合物[Ph_3Sn(CH_3OH)O_2CC_6H_4CO_2(CH_3OH)-SnPh_3]·2CH_3OH和[Ph_3SnS_2CN(CH_2CH_2)_2NCS_2SnPh_3]·2CH_3OH的合成、表征和晶体结构

利用三苯基氯化锡和对苯二甲酸二钠、哌嗪荒酸二钠在甲醇中反应 ,合成了双核有机锡 (Ⅳ )配合物 [Ph3 Sn (CH3 OH)O2 CC6H4 CO2 (CH3 OH)SnPh3 ]·2CH3 OH (1)和 [Ph3 SnS2 CN(CH2 CH2 ) 2 NCS2 SnPh3 ]·2CH3 OH (2 ) .通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征 .用X射线单晶衍射测定了这两个化合物的晶体结构 .化合物 1为单斜晶系 ,空间群P2 1/n ,a =1.5 199(5 )nm ,b =0 .90 0 0 (3)nm ,c =1.82 0 6 (6 )nm ,β =113.970 (5 )° ,Z =2 ,V =2 .2 75 5(13)nm3 ,Dc=1.413g/cm3 ,μ =1.146mm-1,F(0 0 0 ) =980 ,R1=0 .0 35 3,wR2 =0 .0 6 0 6 .化合物 2为单斜晶系 ,空间群P2 1/c,a =1.5 0 6 6 (5 )nm ,b =1.0 875 (4 )nm ,c =1.35 42 (5 )nm ,β =91.6 14(5 )°,Z =2 ,V =2 .2 178(14)nm3 ,Dc=1.498g/cm3 ,μ =1.35 1mm-1,F(0 0 0 ) =10 0 8,R1=0 .0 40 1,wR2 =0 .1148.在 1和 2的晶体中 ,锡原子呈五配位畸变三角双锥构型 .配合物 1由未配位的甲醇分子通过氢键作用形成二维网状结构     

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].     

[In2(HPO3)4]·(NH3CH2CH2NH3)的水热合成与晶体结构

用乙二胺作模板剂在水热条件下合成出一个新的三维开放骨架结构的亚磷酸铟[In2(HPO3)4]·(NH3CH2CH2NH3)(1), 并对其晶体结构进行了测定和表征.     

A novel chain-like molybdenum phosphate: hydrothermal synthesis,crystal structure and characterization of [NH3(CH2CH2)2NH3]3[NH3(CH2CH2)2NH2]-Na5[Mo6O12(OH)3(PO4)(HPO4)3]2·4H2O

A novel organic/inorganic hybrid molybdenum phosphate, [NH₃(CH₂CH₂)₂NH₃]₃[NH₃(CH₂CH₂)₂NH₂]Na₅-[Mo₆O₁₂(OH)₃(PO₄)(HPO₄)₃]₂·4H₂O (1), involving molybdenum presented in V oxidation, has been hydrothermally prepared and characterized by elemental analysis, i.r., u.v.–vis., x.p.s., t.g. and single crystal X-ray diffraction. The structure of the title compound (1) may be considered to consist of two [Mo₆O₁₂(OH)₃(PO₄)(HPO₄)₃] units bonded together with NaO₆ octahedra, forming dimers. Further, these dimers connect with each other through four Na⁺ cations as bridges, giving rise to novel one-dimensional chain-like skeleton. Piperazines exist among inorganic chains acting as charge balancing cations.     

Diorganogalliumfluoride. Die Kristallstruktur des Mischkristalls [B(CH2Ph)3]0,92[Ga(CH2Ph)3]0,08 · NCMe

Diorganogallium Fluorides. The Crystal Structure of the Mixed Crystal [B(CH₂Ph)₃]_0.92[Ga(CH₂Ph)₃]_0.08 · NCMe The reaction of GaR₃ with BF₃ · OEt₂ in diethylether leads to the diorganogallium fluorides R₂GaF [R = i-Pr ( 1 ), CH₂Ph ( 2 ), Mes ( 3 )]. Compound 1 is also available by the reaction of i-Pr₂GaBr ( 6 ) with KF at ?20°C in acetonitrile. The by-product B(CH₂Ph)₃, formed together with 2 during the first reaction, crystallizes with ca. 8% Ga(CH₂Ph)₃ in acetonitrile as [B(CH₂Ph)₃]_0.92[Ga(CH₂Ph)₃]_0.08 · NCMe ( 4 ) in the space group P2₁/n with a = 1050.32(7) pm, b = 1159.5(2) pm, c = 1591.6(1) pm and β = 96.931(6)°.     

Stannylierungsexperimente mit NH-funktionellen Aminoiminophosphoranen. Synthese und Struktur der tricyclischen Stannaphosphazene [Me2Sn(tBu2PN)NH]2 und [nBu2Sn(Ph2PN)2NH]2

Stannylation Experiments with NH-functional Aminoiminophosphoranes. Synthesis and Structure of the Tricyclic Stannaphosphazenes [Me₂Sn(^tBu₂PN)NH]₂ and [ⁿBu₂Sn(Ph₂PN)₂NH]₂ Aminoiminophosphoranes ^tBu₂P(NH)NH₂ ( 1 ) and (H₂NPPh₂)N(Ph₂PNH) ( 2 ) react with diaminostannanes R₂Sn(NEt₂)₂ by cyclocondensation to give cyclostannaphosphazenes [Me₂Sn(^tBu₂PN)NH]₂ ( 3 ) and [R₂Sn(Ph₂PN)₂NH]₂ ( 4 a , b ) ( a : R = Me, b : R = ⁿBu). With 2 and Me₃SnNEt₂ the ring compound Me₂Sn(Ph₂PN)₂NSnMe₃ ( 5 ) besides Me₄Sn is formed by per-N-stannylation and Sn-methyl group transfer. The crystal structures of 3 and 4 b were determined by X-ray structure analysis. 3 forms a planar heterotricyclus containing three four-membered rings with two pentacoordinated tin atoms (space group P 1 (No. 2); Z = 1). 4 b consists of a tricyclic molecule with two puckered six-membered rings and one planar four membered tin-nitrogen ring with two pentacoordinated tin atoms (space group P 1 (No. 2); Z = 1).     

Synthesis and Structure of a One‐Dimensional Aluminum Phosphate, [NH3(CH2)2NH2(CH2)3NH3]3+ [Al(PO4)2]3—

A one‐dimensional aluminum phosphate, [NH₃(CH₂)₂NH₂(CH₂)₃NH₃]³⁺ [Al(PO₄)₂]^3—, has been synthesized hydrothermally in the presence of N‐(2‐Aminoethyl‐)1, 3‐diaminopropane (AEDAP) and its structure determined by single crystal X‐ray diffraction. Crystal data: space group = Pbca (no. 61), a = 16.850(2), b = 8.832(1), c = 17.688(4)Å, V = 2632.4(2)ų, Z = 8, R₁ = 0.0389 [5663 observed reflections with I > 2σ(I)]. The structure consists of anionic [Al(PO₄)₂]^3— chains built up from AlO₄ and PO₄ tetrahedra, in which all the AlO₄ vertices are shared and each PO₄ tetrahedron possesses two terminal P=O linkages. The cations, which balances the negative charge of the chains, are located in between the chains and interact with the oxygen atoms through strong N—H···O hydrogen bonds. Additional characterization of the compound by powder XRD and MAS‐NMR has also been performed and described.     

[CH3NH3][NH3(CH2)6NH3]H3[P2Mo2W16O62]·H2O的水热合成与表征

首次合成了[CH3NH3][NH3(CH2)6NH3]H3[P2Mo2W16O62]·H2O,通过元素分析、红外光谱和X射线单晶衍射对合成产物进行了表征,并用TGA-DSC研究了化合物的热稳定性.晶体属单斜晶系,P21/m空间群,a=1.2596(3)nm,b=1.8715(4)nm,c=1.9816(4)nm,α=γ=90°,β=90.16(3)°,V=4.671(2)nm3,Z=2,Mr=4358.66,Dc=3.100g·cm-3,μ=19.978mm-1,F(000)=3792,R=0.0835,Rw=0.2026.结果表明,在晶体结构内形成了0.7364nm×0.8354nm的微孔.     

Solvothermal Synthesis and Crystal Structure of [H2N（CH2）2NH3]{Co[H2N（CH2）2NH2]3}[SbSe4]

1 INTRODUCTION The chalcogenidometallates with open frame- works have attracted considerable interest as pos- sible zeolite-like materials, of which highly interes- ting properties could be expected. Over the last de- cades a large number of thioanti…     

H3N(CH2)7NH3]8(CH3NH3)2Sn(IV)Sn(II)12I46- a mixed-valent hybrid compound with a uniquely templated defect-perovskite structure

The incorporation of H(3)N(CH(2))(7)NH(3) with CH(3)NH(3)SnI(3) resulted in the formation of a mixed-valent and semiconducting (Eg = 0.84 eV) organic-based perovskite, [H(3)N(CH(2))(7)NH(3)](8)(CH(3)NH(3))(2)Sn(iv)Sn(ii)(12)I(46), with a unique 3D defect-perovskite structure with ordered vacancies at the Sn and I sites.     

Synthesis,characterization and some reactions of trans-[Co(NH3)4(CH3NH2)Br]2+ and trans-[Co(NH3)4(CH3NH2)(NO3)]2+ complexes

The preparation of trans-[Co(NH₃)₄(CH₃NH₂)Br]²⁺ and trans-[Co(NH₃)₄(CH₃NH₂)-(NO₃)]²⁺ complexes is described. The UV-VIS spectra of the complexes indicate a decrease of the ligand field compared to the parent pentaammines. Infrared spectra match with the pattern of the corresponding pentaammines. The catalyzed (by Hg²⁺) aquation of the trans-bromomethylamine complex go under retention of the stereochemical configuration. The base hydrolysis (studied at 25°C) products show trans to cis rearrangement for both complexes. ¹H NMR spectroscopy is used for identification of the stereochemical configuration of the compounds.     

Synthesis, Structure Characterization and Biological Activity of Layered Vanadium Oxides [ NH3 （ CH2 ）2 NH （ CH2 ）2 NH3 ] [ V6 O14 ]

Introduction Over the past decades, polyoxometalates(POMs)have been attracting extensive interestowing to the widerange of their topological properties and potential appli-cations in catalysis, photochemistry, electrochromism,and magnetism[1,2]. Meanwhile, owing to the potentialapplication of polyoxometalaes as anticancer and antivi-ral drugs, their complexes have attracted increasing in-terest of both inorganic chemists and biochemists[3]. Itis well known that polyoxometalates are excellent …     

五配位阴离子型有机锡化合物的合成及[C5H5NH][Ph2Sn(μ2-SCH2COO)Cl]和[CH3PhNH2][Ph2Sn(μ2-SCH2COO)Cl]晶体结构

近年来，由于离子型有机锡化合物的分子结构的多样性、较好的生物活性以及在有机合成上的应用，而引起广泛注意，前文报道了Ph3SnCl与HSCH2COOH在有机胺存在下发生Sn-Ph键断裂，生成二苯基锡的离子型有机锡化合物，本文用Ph2SnCl2与HSCH2COOH在有机胺存在下，采用同样的反应条件Sn-Ph键不再断裂，得到与前文结构相类似的化合物，反应方程式如下：