Synthesis and Crystal Structures of Antimony(III) Complexes With a Bis(amino)silane Ligand

Bis(amino)silane bearing bulky substituents on nitrogen, LH₂ [L = Me₂Si(NDipp)₂, Dipp = 2, 6‐diisopropylphenyl] was reacted with nBuLi (ratio 1:1 and 1:2) in toluene. The Me₂Si(LiNDipp)₂ was treated with SbCl₃ in a 1:1 ratio to yield the four‐membered SiN₂Sb ring compound of composition [η²(N,N)‐Me₂Si(NDipp)₂SbCl] ( 1 ). The mono lithiated bis(amino)silane was used to synthesize the monodentate heterotetraatomic complex [(η¹‐Me₂SiNDipp)NHDippSbCl₂] ( 2 ) by the reaction with SbCl₃. The complexes were characterized by ¹H and ¹³C NMR, elemental analysis, IR, and single‐crystal X‐ray structural analysis.     

Synthesis and Crystal Structure of Bis（tetra－hydrofurfurylcyclopentadienyl）ytterbium Chloride

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＢｉｓ（ｔｅｔｒａ－ｈｙｄｒｏｆｕｒｆｕｒｙｌｃｙｃｌｏｐｅｎｔａｄｉｅｎｙｌ）ｙｔｔｅｒｂｉｕｍＣｈｌｏｒｉｄｅＺＨＵＡＮＧＸｉｕ－ｌｉ;ＺＨＡＮＧＳｕｏ－ｂｏ;ＨＵＮｉｎｇ－ｈａｉａｎｄ...     

Synthesis,Characterization, Crystal Structure,and hybrid DFT Computation of Antimony(III) Chloride Diazide,SbCl(N3)2

SbCl(N₃)₂ was synthesized by the reaction of two equivalents of sodium azide with SbCl₃ in CH₂Cl₂. The structure of the compound was determined by X‐ray structure determination. SbCl(N₃)₂ crystallizes in the monoclinic space group C2/c with a = 11.694(4), b = 7.751(4) and c = 12.241(5) Å, β = 100.45(1)°, with 8 formula units per unit cell. The SbCl(N₃)₂ molecules show interactions to form chains. The frequencies obtained by Raman and infrared spectroscopy were assigned to the normal modes of the SbCl(N₃)₂ molecules in comparison with computational results.     

Synthesis and Physicochemical Characteristics of New Tetrachloroferrates(III) with Dimethylammonium Cation: X‐ray Crystal Structure of Bis(dimethylammonium) Chloride Tetrachloroferrate(III)

Two new tetrachloroferrates(III) have been synthesized of molecular formulas [(CH₃)₂NH₂][FeCl₄] and [(CH₃)₂NH₂]₂FeCl₅. The differences in their physicochemical properties have been highlighted using thermal analysis (TG‐MS) and differential scanning calorimetry (DSC). The crystal and molecular structure of [(CH₃)₂NH]₂FeCl₅ was determined. The iron(III) cation is four coordinated by chloride ions, and it adopts a slightly distorted tetrahedral coordination with three angles smaller and three larger than the tetrahedral one. In the structure four intermolecular N‐H···Cl hydrogen bonds link the [(CH₃)₂NH₂]⁺ cations to dimers via a Cl^? bridge.     

1-甲基-2-咪唑醛肟锰(III)配合物的合成、晶体结构及电化学性质研究

采用溶剂扩散法获得了锰(III)的两个单核配合物 [Mn(Miao)2(H2O)2]ClO4(1)和[Mn(Miao)2(DMF)2]ClO4(2)（HMiao = 1-甲基-2-咪唑醛肟,DMF = N,N-二甲基甲酰胺）的晶体。X-射线衍射单晶结构表明：两种配合物均属三斜晶系,空间群Pī,锰与配位原子形成稳定的八面体结构。采用Gaussian03W程序计算了HMiao配体的电荷密度,理论计算与实际配位形式完全吻合。通过循环伏安法测定了两种锰配合物在DMF 溶液中的电化学性质。     

Synthesis and Crystal Structure of Bis(N,N''''- cyclohexyl-N''''''''-bis(trimethylsilyl)samarium Chloride

1INTRODUCTIONTheguanidinateanions,[(RN)2C(NR2?]-,canbeeasilymodifiedinbothelectronicdensityandstericbulkinessbyadjustingthesubstituents(RorR?onnitrogenatoms.Inthiscase,theyhavealrea-dybeenattractedmuchattentioninthecoordinationandorganometallicchemistry…     

对称吡啶双酰胺及其稀土配合物的合成、表征与荧光性质的研究

以元素分析、红外光谱、差热及核磁进行表征了配体及其五种稀土（La^3＋,Eu^3＋,Tb^3＋,Gd^3＋,Yb^3＋）配合物,确定了其组成,研究了部分配合物的固态荧光.同时以低温磷光光谱确定了配体的三重态能级为22989 cm^-1,研究了配体与稀土离子的能级匹配情况,详细讨论了配合物的发光性能.结果发现,铽配合物能发出很强的特有荧光,而铕配合物所发荧光很弱,说明配体L与Tb^3＋ 的^5D4匹配.对于Tb^3＋而言,当2000 cm^-1〈ΔE（T-^5D4）〈3000 cm^-1时,稀土铽离子发出强的荧光;对于Eu^3＋ 而言,ΔE（T-^5D1）超过3000 cm^-1时,则几乎不发荧光.     

Synthesis and Structure of Oxygen-Containing Antimony Complexes (Ar2SbO)4(O2)2

Russian Journal of General Chemistry - Triarylantimony Ar3Sb (Ar = 4-FC6H4, 3-MeC6H4) is oxidized by hydrogen peroxide to form tetranuclear complexes [(4-FC6H4)2SbO]4(O2)2 and...     

Synthesis and Structure of Co(III) Complexes with 2-Pyridinecarboxylic Acid

The Co(III) complexes with pyridinecarboxylic acid, Na[Co(Pc)₂(NO₂)₂] (I) and NH₄[Co(Pc)₂(NO₂)₂] (II), where Pc is the 2-pyridinecarboxylate anion, have been synthesized and studied by X-ray diffraction. In the crystal, the complex anions are combined through the Na⁺ and NH ₄ ⁺ cations. In II, the anion and the cation are combined by hydrogen bonds.     

Synthesis of Bis(tricarbonylcyclopentadienylmolybdenum)bismuth(III) Chloride and Its Reaction with Metals

Polynuclear organometallic compounds [CpMo(CO)₃]₂BiCl and [CpMo(CO)₃]BiCl₂ were prepared by reaction of bismuth with tricarbonylcyclopentadienylmolybdenum chloride in dimethyl sulfoxide (DMSO). [CpMo(CO)₃]₂BiCl is reduced with magnesium or indium in tetrahydrofuran to give bismuth, [CpMo(CO)₃]₃Bi, and magnesium or indium chloride. In the presence of DMSO, the reaction of [CpMo(CO)₃]₂BiCl with magnesium or indium yields bismuth and the organomolybdenum derivative of magnesium or lithium, respectively.     

含硫、氮配位的二正丁基锡二（二苯基卡巴腙）合成及晶体结构研究

以乙醇钠作碱，用二正丁基二氯化锡或三正丁基氯化锡与二苯基硫代卡巴腙反 应，合成了二正丁基锡二(二苯基硫代卡巴腙)[(n-Bu)_2Sn(sN_4C_13H_11)_2]．通 过元素分析、红外光谱、紫外光谱和核磁共振氢谱对其结构进行了表征．用X射线 单晶衍射测定了该化合物的晶体结构。化合物为单斜晶系，空间群P2_1／c，α=2 ．0215(7)nm，b=1．3103(5)nm，c=2．8171 (10)nm，β=95．412(7)°，Z=8， V=7．428(5)nm~3，Dc=1．330g／cm~3，μ=0．834 mm~-l， F(OOO)=3056， R_l=0．0575， wR_2=0.0959．化合物中，中心锡原子为六配位畸变八面体构型     

双(2,4-二甲基戊二烯基)氯化钆的合成及晶体结构

合成双(2,4-二甲基戊二烯基)氯化钆{[2,4-(CH₃)₂C₅H₅]₂GD_cl}₂,并测定了晶体结构.晶体为单斜晶系,P2₁/n空间群.晶胞参数a=0.89141(18)nm,b=1.4486(3)nm,c=1.15925(15)nm,β=92.996(18)°,V=1.4949(4)nm³,Z=3.     

Synthesis and Crystal Structure of Tetrabonzoato Bis （2－Aminothiazol） Dicopper（Ⅱ）

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＴｅｔｒａｂｏｎｚｏａｔｏＢｉｓ（２－Ａｍｉｎｏｔｈｉａｚｏｌ）Ｄｉｃｏｐｐｅｒ（Ⅱ）ＷａｎｇＤｏｎｇ－Ｍｅｉ；ＨｏｕＹｉ－Ｍｉｎ；ＹａｎｇＲｕｉＮａ；ＨｕＸｉａｏ－Ｙｕａｎ；ＸｕｏＢａｏ－...     

三(邻甲基苄基)氯化锡和二(对甲基苄基)二氯化锡的合成和晶体结构

将邻甲基氯苄和对甲基氯苄在适当的溶剂中与锡粉反应，合成了三(邻甲基苄基)氯化锡1和二(对甲基苄基)二氯化锡2，用X射线衍射方法测定了化合物的晶体结构。化合物(1)的晶体属三方晶系，空间群为R3，晶体学参数：a=1.329 36(8) nm，b=1.329 36(8) nm，c=2.147 0(3) nm，α=β=90°，γ=120°，V=3.285 8(5) nm³，Z=6，D_c=1.424 g·cm^-3，μ(Mo Kα)=12.93 cm^-1，F(000)=1 428，R₁=0.037 1，wR=0.110 2。化合物2的晶体属单斜晶系，空间群为C2/c，晶体学参数：a=2.850 4(3) nm，b=0.491 23(5) nm，c=1.215 32(12) nm，β=112.517(2)°，V=1.571 9(3) nm³，Z=4，D_c=1.690 g·cm^-3，μ(Mo Kα)=19.49 cm^-1，F(000)=792，R₁=0.038 0，wR₂=0.109 4；中心锡原子为畸变四面体配位构型。     

Synthesis,Structure, and Luminescent Properties of Antimony(III) Complexes with N,N"-Diphenylguanidine

Complexes of antimony(III) halides with N,N"-diphenylguanidine were synthesized for the first time and studied using X-ray diffraction analysis and luminescence spectroscopy. The mechanism of sensitization of Sb³⁺luminescence involving the low-lying state of the charge transfer was proposed.     

Crystal Structure of Bis｛1-(2-methoxyethyl)indenyl｝dysprosium Chloride

1　INTRODUCTION　　Organolanthanidecomplexeshavebeenextensivelystudied.However,thestud-iesofindenylrareearthcomplexeswererelativelylimited[1].Althoughaseriesoftri-indenyltetrahydrofuranatolanthanide((C9H7)3Ln·THF)havebeensynthesizedandstudiedbyTsutsuiandGyslingabout30yearsago[2],onlyafewcrystalstruc-turesofindenyllanthanidecomplexeshavebeenreported[1].Moreover,mostofthereportedindenyllanthanidecomplexesweresynthesisedbymetatheticalreactionsofanhydrouslanthanidetrichlorideswithindenyls…     

二(四氢糠基茚)稀土氯化物的合成及晶体结构

将四氢糠基茚锂分别与无水三氯化钇和无水三氯化钆以摩尔比2;1反应,除去不溶物和溶剂后,将产物在甲苯/THF中冷冻得到晶体(C₄H₇OCH₂C₉H₆)₂LnCl[Ln=Y(1);Ln=Gd(2)].这两种配合物都是单分子无溶剂化合物,在空气中稳定.配合物1和2的晶体结构都属于正交晶系,P2₁2₁2₁空间群,晶胞参数分别为a=1.04252(9)nm,b=1.47455(12)nm,c=1.49799(13)nm,Z=4,Dc=1.508g/cm³;a=1.03701(10)nm,b=1.47233(12)nm,c=1.51354(14)nm,Z=4,Dc=1.699g/cm³.它们的结构相似,但空间构象不同.稀土中心离子分别与两个茚中的五元环和两个氧原子及氯原子成键,形成九配位结构.     

Antimony(III) Complexes with Quaternary Ammonium Bases: Synthesis, Spectral, and Luminescent Properties

Complexes of antimony(III) halides with quaternary ammonium bases of different composition were synthesized and characterized by elemental and X-ray diffraction analyses and IR and luminescence spectroscopy. For complexes [R"₃R"N]SbHal₄ (Hal = Cl^–, Br^–, R" = R" = CH₃, C₂H₅, C₄H₉), the maximum of the emission band and fluorescence intensity was found to depend on the nature of the halide ion and the alkyl radical length.     

两个由双咪唑基配体构筑的锰、镉配合物的合成及晶体结构

通过水热法合成了2个金属-有机配位聚合物[Mn（dipha）（1,3-bix）]_n·nH₂O（1）和[Cd₂（NIPH）₂（bimb）_2.5（H₂O）]_n·3nH₂O（2）（H₂dipha=2,2’-联苯二甲酸,1,3-bix=1,3-双（咪唑基-1-甲基）-苯,H₂NIPH=5-硝基间苯二甲酸,bimb=1,4-双（咪唑基-1-甲基）-丁烷）。并对其进行了元素分析、红外光谱、热重和X-射线单晶衍射测定。这2个配合物通过氢键和π-π相互作用形成了超分子网状结构。此外还研究了配合物2的荧光性质。