Synthesen und Kristallstrukturen von [(t-Bu4Sb4)Fe(CO)4], [(t-Bu4Sb4)Mo(CO)5] und [(t-Bu3Sb4)Mo(η5-C5Me5)(CO)3]

Syntheses and Crystal Structures of [( t -Bu₄Sb₄)Fe(CO)₄], [( t -Bu₄Sb₄)Mo(CO)₅], and [( t -Bu₃Sb₄)Mo(η⁵-C₅Me₅)(CO)₃] t-Bu₄Sb₄ reacts with Fe₂(CO)₉ to form [(t-Bu₄Sb₄)Fe(CO)₄] ( 1 ). [(t-Bu₄Sb₄)Mo(CO)₅] ( 2 ) is formed from (thf)Mo(CO)₅ and t-Bu₄Sb₄. [(t-Bu₃Sb₄)Mo(η⁵-C₅Me₅)(CO)₃] ( 3 ) is a product of the reaction of t-Bu₄Sb₄ with [(η⁵-C₅Me₅)Mo(CO)₃]₂. The crystal structures of 1–3 are reported.     

Tetracarbonylchrom-Komplexe mit Me2SbESbMe2 (E = O,S) und MeSb(SSbMe2)2 als Liganden

Tetracarbonyl Chromium Complexes with Me₂SbESbMe₂ (E = O, S) and MeSb(SSbMe₂)₂ as Ligands Me₂SbOSbMe₂ reacts with nbdCr(CO)₄ (nbd = norbornadiene) to form cyclo-[Me₂SbOSbMe₂Cr(CO)₄]₂ ( 1 ). The reaction of Me₂SbSSbMe₂ with nbdCr(CO)₄ gives cis-[(Me₂SbSSbMe₂)₂Cr(CO)₄] ( 2 ), a complex stable only in solution. With excess nbdCr(CO)₄ also cyclo[Me₂SbSSbMe₂Cr(CO)₄]₂ ( 3 ) and cyclo[MeSb(SSbMe₂)₂Cr(CO)₄] ( 4 ) form in low yield. The crystal structures of 1 , 3 and 4 · nbdCr(CO)₄ are reported. The novel ligand MeSb(SSbMe₂)₂ is formed by elimination of Me₃Sb from Me₂SbSSbMe₂.     

基于两个取代四甲基环戊二烯基配体的金属羰基化合物的合成及晶体结构

配体[C₅Me₄HR][R=4-BrPh(1),(MeC₅H₃N)CH₂(2)]分别与Mo(CO)₆,Ru₃(CO)₁₂和Fe(CO)₅在二甲苯中加热回流,得到了6个双核配合物trans-[η⁵-C₅Me₄R]₂Mo₂(CO)₆(3,4),trans-[(η⁵-C₅Me₄R)Ru(CO)(μ-CO)]₂(5,6)和trans-[η⁵-(C₅Me₄R)Fe(CO)(μ-CO)]₂(7,8,).通过元素分析、红外光谱、核磁共振氢谱对配合物的结构进行了表征,并用X-射线单晶衍射法测定了配合物3,5,6和8的结构.     

基于两个取代四甲基环戊二烯基配体的金属羰基化合物的合成及晶体结构(英文)

配体[C5Me4HR][R=4-Br Ph(1),(Me C5H3N)CH2(2)]分别与Mo(CO)6,Ru3(CO)12和Fe(CO)5在二甲苯中加热回流,得到了6个双核配合物trans-[η5-C5Me4R]2Mo2(CO)6(3,4),trans-[(η5-C5Me4R)Ru(CO)(μ-CO)]2(5,6)和trans-[η5-(C5Me4R)Fe(CO)(μ-CO)]2(7,8)。通过元素分析、红外光谱、核磁共振氢谱对配合物的结构进行了表征,并用X-射线单晶衍射法测定了配合物3,5,6和8的结构。     

Reaktionen von R4Sb2 (R = Me,Et) mit (Me3SiCH2)3M (M = Ga,In) und Kristallstrukturen von [(Me3SiCH2)2InSbMe2]3 und [(Me3SiCH2)2GaOSbEt2]2

Reactions of R₄Sb₂ (R = Me, Et) with (Me₃SiCH₂)₃M (M = Ga, In) and Crystal Structures of [(Me₃SiCH₂)₂InSbMe₂]₃ and [(Me₃SiCH₂)₂GaOSbEt₂]₂ The reaction of (Me₃SiCH₂)₃In with Me₂SbSbMe₂ gives [(Me₃SiCH₂)₂InSbMe₂]₃ ( 1 ) and Me₃SiCH₂SbMe₂. [(Me₃SiCH₂)₂GaOSbEt₂]₂ ( 2 ) is formed by the reaction of (Me₃SiCH₂)₃Ga with Et₂SbSbEt₂ and oxygen. The syntheses and the crystal structures of 1 and 2 are reported.     

[μ‐(Me3SiCH2Sb)5–Sb1,Sb3–{W(CO)5}2] und [{(Me3Si)2CHSb}3Fe(CO)4] – zwei cyclische Komplexe mit Antimon‐Liganden

Syntheses and Crystal Structures of [μ‐(Me₃SiCH₂Sb)₅–Sb¹,Sb³–{W(CO)₅}₂] and [{(Me₃Si)₂CHSb}₃Fe(CO)₄] – Two Cyclic Complexes with Antimony Ligands cyclo‐(Me₃SiCH₂Sb)₅ reacts with [(THF)W(CO)₅] (THF = tetrahydrofuran) to form cyclo‐[μ‐(Me₃SiCH₂Sb)₅–Sb¹,Sb³–{W(CO)₅}₂] ( 1 ). The heterocycle cyclo‐ [{(Me₃Si)₂CHSb}₃Fe(CO)₄] ( 2 ) is formed by an insertion reaction of cyclo‐[(Me₃Si)₂CHSb]₃ and [Fe₂(CO)₉]. The crystal structures of 1 and 2 are reported.     

Structure of d-Metal Complexes with Methylimino-Acetic Acid N-oxide

The complexes of Co(II), Zn(II), and Mn(II) with methylimino-acetic acid N-oxide were investigated by single crystal X-ray diffraction. The nitrone ligand is shown to bind to the metal atom via the carboxyl and nitrone oxygens. All the compounds are isostructural.     

Highly Ordered LB Films of Amphiphilic Complexes With 8-Hydroxyquinoline

Organicelectrolndnescent(EL)deviceshaverecentlyreceivedmuchattentionbecausetheycanpotentiallyproduceemissionsofallcolorsandbecauseoftheirpossibleapplicationaslarge-arealight-easttingdisplays'-'.Variousorganicmaterialswereusedastheemittinglayers.The8-hydroxyquinolinecomplexes,suchasAlq,'-',Znq2,Beq2,andMgq,'(qis8-hydroxyquinoline)wereespeciallyusedaseasttingelementsowingtotheirhighexternalquantumefficiency,luminousefficiency,brightnessandlowerdrivingvoltage.SincetheLangmuir-Blodgett(LB)film…     

Synthesis,characterizations and crystal structures of new antimony (III) complexes with dithiocarbamate ligands

Eight new antimony (III) complexes containing dithiocarbamate ligands (R₂NCS₂)₂SbBr [R₂NCS₂ = OC₄H₈NCS₂ (1), C₂H₅NC₄H₈NCS₂ (2), Me₂NCS₂ (3), C₄H₈NCS₂ (4)] and (R₂NCS₂)₃Sb[R₂NCS₂ = C₅H₁₀NCS₂ (5), Bz₂NCS₂ (6), Et₂NCS₂ (7), (HOCH₂CH₂)₂NCS₂ (8)] have been synthesized by the reactions of antimony (III) halides with dithiocarbamate ligands in 1:2 or 1:3 stoichiometries. All the complexes have been characterized by elemental analysis, melting point as well as spectral [IR and NMR (¹H and ¹³C)] studies. The crystal structures of complexes 1, 5 and 8 have been determined by X-ray single crystal diffraction, and their electrochemical character has also been studied.     

Charge Transfer Complexes of 1,3,6-Trinitro-9,10-phenanthrenequinone with Polycyclic Aromatic Compounds

Understanding the interactions of organic donor and acceptor molecules in binary associates is crucial for design and control of their functions. Herein, we carried out a theoretical study on the properties of charge transfer complexes of 1,3,6-trinitro-9,10-phenanthrenequinone (PQ) with 23 aromatic π-electron donors. Density functional theory (DFT) was employed to obtain geometries, frontier orbital energy levels and amounts of charge transfer in the ground and first excited states. For the most effective donors, namely, dibenzotetrathiafulvalene, pentacene, tetrathiafulvalene, 5,10-dimethylphenazine, and tetramethyl-p-phenylenediamine, the amount of charge transfer in the ground state was shown to be 0.134−0.240 e⁻. Further, a novel charge transfer complex of PQ with anthracene was isolated in crystalline form and its molecular and crystal structure elucidated by single-crystal synchrotron X-ray diffraction.     

芳基取代茚基钌羰基化合物的合成及晶体结构

配体C₉H₇R(R=Ph(1),4-tolyl(2),4-chlorophenyl(3),4-methoxyphenyl(1),2-thienyl(5))分别与Ru₃(CO)₁₂在甲苯或二甲苯中加热回流,得到了5个双核配合物[(η⁵-C₉H₆R)Ru(CO)]₂(μ-CO)₂(R=Ph(6),4-tolyl(7),4-chlorophenyl(8),4-methoxyphenyl(9),2-thienyl(10))。通过元素分析、红外光谱、核磁共振氢谱对配合物的结构进行了表征,并用X-射线单晶衍射法测定了配合物6,7和10的结构。     

取代四甲基环戊二烯基钌羰基化合物的合成及结构

将配体[C5Me4HR](R=cyclopentyl,cyclohexyl,nPr)分别与Ru3(CO)12在二甲苯中加热回流,合成了3个新的双核配合物[(η5-C5Me4R)Ru(CO)(μ-CO)]2(R=cyclopentyl(1),cyclohexyl(2),nPr(3))。利用红外光谱、元素分析、核磁共振氢谱对它们的结构进行了表征,用X-射线单晶衍射法测定了1和2的结构。     

烃基取代茚基钌羰基化合物的合成及晶体结构(英文)

配体C9H7R(R=CH2CH2CH3(1),CH(CH3)2(2),C5H9(3),CH2C6H5(4),CH2CH=CH2(5))分别与Ru3(CO)12在二甲苯或庚烷中加热回流,得到了6个双核配合物[(η5-C9H6R)Ru(CO)(μ-CO)]2(R=CH2CH2CH3(6),CH(CH3)2(7),C5H9(8),CH2C6H5(9),CH2CH=CH2(10))和[(η5-C9H6)(H3CH2C)CHCH(CH2CH3)(η5-C9H6)][Ru(CO)(μ-CO)]2(11)。通过元素分析、红外光谱、核磁共振氢谱对配合物的结构进行了表征,并用X-射线单晶衍射法测定了配合物6,9,10和11的结构。     

烃基取代茚基钌羰基化合物的合成及晶体结构

配体C₉H₇R(R=CH₂CH₂CH₃ (1),CH₂(CH₃)₂ (2),C₅H₉ (3),CH₂C₆H₅ (4),CH₂CH=CH₂ (5))分别与Ru₃(CO)12在二甲苯或庚烷中加热回流,得到了6个双核配合物[(η⁵-C₉H₆R)Ru(CO)(μ-CO)]₂(R=CH₂CH₂CH₃ (6),CH₂(CH₃)₂ (7),C₅H₈ (8),CH₂C₆H₅ (9),CH₂CH=CH₂ (10))和[(η⁵-C₉H₆)(H₃CH₂C)CHCH(CH₂CH₃)(η⁵-C₉H₆)] [Ru(CO)(μ-CO)]₂ (11).通过元素分析、红外光谱、核磁共振氢谱对配合物的结构进行了表征,并用X-射线单晶衍射法测定了配合物6,9,10和11的结构.     

取代四甲基环戊二烯基钌羰基化合物的合成及结构

将配体[C₅Me₄HR](R=cyclopentyl,cyclohexyl,ⁿPr)分别与Ru₃(CO)₁₂在二甲苯中加热回流,合成了3个新的双核配合物[(η⁵-C₅Me₄R)Ru(CO)(μ-CO)]₂(R=cyclopentyl(1),cyclohexyl(2),ⁿPr(3))。利用红外光谱、元素分析、核磁共振氢谱对它们的结构进行了表征,用X-射线单晶衍射法测定了1和2的结构。     

Synthesis and Structural Characterization of a Ruthenium Complex： trans-RuCle（COD）Py2

A new ruthenium complex trans-RuCl2（COD）Py2 has been synthesized and characterized by elemental analysis, IR, IH NMR and single-crystal X-ray diffraction. Crystal data： trans- RuCl2（COD）Py2, Mr = 438.35, monoclinic, space group P21/c, a = 8.9116（9）, b = 14.6175（15）, c = 13.7582（14）A, β = 101.994（1）°, V= 1753.1（3）A^3, Z= 4, Dc= 1.661 g/cm^3, F（000）= 888,μ = 1.199 mm^-1, R = 0.0376 and wR = 0.0789 for 2492 observed reflections with I 〉 2σ（I）.     

Direct Synthesis of Hetero Bimetallic Complexes

The concept of direct synthesis (the use of metals or their oxides as the starting materials for obtaining coordination compounds) has been further developed as anion-deficient and ligand-deficient methods for synthesis of heterometallic complexes. We have used the example of coordination compounds with amino alcohols and ethelenediamines to demonstrate the advantages of the proposed approach for obtaining polynuclear, mixed-anion, and mixed-valence heterometallic complexes. We present the most interesting crystal structures of the Cu–M (Co, Zn, Cd, Pb) hetero bimetallic complexes. It is shown that direct synthesis of hetero trimetallic complexes can be a further possible development of the new concept.     

芳基取代茚基钌羰基化合物的合成及晶体结构

配体C₉H₇R(R=Ph (1),4-tolyl (2),4-chlorophenyl (3),4-methoxyphenyl (4),2-thienyl (5))分别与Ru₃(CO)₁₂在甲苯或二甲苯中加热回流,得到了5个双核配合物[(η⁵-C₉H₆R)Ru(CO)]₂(μ-CO)₂(R=Ph (6),4-tolyl (7),4-chlorophenyl (8),4-methoxyphenyl (9),2-thienyl (10))。通过元素分析、红外光谱、核磁共振氢谱对配合物的结构进行了表征,并用X-射线单晶衍射法测定了配合物6,7和10的结构。     

Synthesis and Structural Characterization of a Ruthenium Complex:trans-RuCl_2(COD)Py_2

A new ruthenium complex trans-RuCl2(COD)Py2 has been synthesized and charac- terized by elemental analysis, IR, 1H NMR and single-crystal X-ray diffraction. Crystal data: trans- RuCl2(COD)Py2, Mr = 438.35, monoclinic, space group P21/c, a = 8.9116(9), b = 14.6175(15), c = 13.7582(14) , β = 101.994(1)°, V = 1753.1(3) 3, Z = 4, Dc = 1.661 g/cm3 , F(000) = 888, μ = 1.199 mm-1, R = 0.0376 and wR = 0.0789 for 2492 observed reflections with I > 2σ(I).     

用X—射线光电子能谱对钇的配位化合物价态的研究

二价的配合物3p能级分裂间距大于三价Y的化合物,二价Y的4s多重分裂也是鉴别Y的价态指纹。