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1.
Martin Haehnel Dr. Sven Hansen Jacqueline B. Priebe Dr. Anke Spannenberg Dr. Perdita Arndt Prof. Dr. Angelika Brückner Prof. Dr. Uwe Rosenthal 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(23):7568-7574
A study of the coordination chemistry of different bis(diphenylphosphino)methanide ligands [Ph2PC(X)PPh2] (X=H, SiMe3) with Group 4 metallocenes is presented. The paramagnetic complexes [Cp2Ti{κ2‐P,P‐Ph2PC(X)PPh2}] (X=H ( 3 a ), X=SiMe3 ( 3 b )) have been prepared by the reactions of [(Cp2TiCl)2] with [Li{C(X)PPh2}2(thf)3]. Complex 3 b could also be synthesized by reaction of the known titanocene alkyne complex [Cp2Ti(η2‐Me3SiC2SiMe3)] with Ph2PC(H)(SiMe3)PPh2 ( 2 b ). The heterometallacyclic complex [Cp2Zr(H){κ2‐P,P‐Ph2PC(H)PPh2}] ( 4 aH ) has been prepared by reaction of the Schwartz reagent with [Li{C(H)PPh2}2(thf)3]. Reactions of [Cp2HfCl2] with [Li{C(X)PPh2}2(thf)3] gave the highly strained corresponding metallacycles [Cp2M(Cl){κ2‐P,P‐Ph2PC(X)PPh2}] ( 5 aCl and 5 bCl ) in very good yields. Complexes 3 a , 4 aH , and 5 aCl have been characterized by X‐ray crystallography. Complex 3 a has also been characterized by EPR spectroscopy. The structure and bonding of the complexes has been investigated by DFT analysis. Reactions of complexes 4 aH , 5 aCl , and 5 bCl did not give the corresponding more unsaturated heterometallacyclobuta‐2,3‐dienes. 相似文献
2.
Reactions of copper(I) halides (Cl, Br, I) with 1‐methyl‐1, 3‐imidazoline‐2‐thione (mimzSH) in 1 : 2 molar ratio yielded sulfur‐bridged dinuclear [Cu2X2(μ‐S‐mimzSH)2(η1‐S‐mimzSH)2] (X = I, 1 , Br, 2 ; Cl, 3 ) complexes. Copper(I) iodide with 1,3‐imidazoline‐2‐thione (imzSH2) and Ph3P in 1 : 1 : 1 molar ratio has also formed a sulfur‐bridged dinuclear [Cu2I2(μ‐S‐imzSH2)2(PPh3)2] ( 4 ) complex. The central Cu(μ‐S)2Cu cores form parallelograms with unequal Cu–S bond distances {2.324(2), 2.454(3) Å} ( 1 ); {2.3118(6), 2.5098(6) Å} ( 2 ); {2.3075(4), 2.5218(4) Å} ( 3 ); {2.3711(8), 2.4473(8) Å} ( 4 ). The Cu···Cu separations, 2.759–2.877Å in complexes 1 – 3 are much shorter than 3.3446Å in complex 4 . The weak intermolecular interactions {H2CH···S# ( 2 ); CH···Cl# ( 3 ); NH···I# ( 4 )} between dimeric units in complexes 2 – 4 lead to the formation of linear 1D polymers. 相似文献
3.
Soufiane S. Nadif Dr. Matthew E. O'Reilly Dr. Ion Ghiviriga Dr. Khalil A. Abboud Prof. Adam S. Veige 《Angewandte Chemie (International ed. in English)》2015,54(50):15138-15142
A chemically non‐innocent pyrrole‐based trianionic (ONO)3? pincer ligand within [(pyr‐ONO)TiCl(thf)2] ( 2 ) can access the dianionic [(3H‐pyr‐ONO)TiCl2(thf)] ( 1‐THF ) and monoanionic [(3H,4H‐pyr‐ONO)TiCl2(OEt2)][B{3,5‐(CF3)2C6H3}4] ( 3‐Et2O ) states through remote protonation of the pyrrole γ‐C π‐bonds. The homoleptic [(3H‐pyr‐ONO)2Zr] ( 4 ) was synthesized and characterized by X‐ray diffraction and NMR spectroscopy in solution. The protonation of 4 by [H(OEt2)2][B{C6H3(CF3)2}4] yields [(3H,4H‐pyr‐ONO)(3H‐pyr‐ONO)Zr][B{3,5‐(CF3)2C6H3}4] ( 5 ), thus demonstrating the storage of three protons. 相似文献
4.
Damir A. Safin Dr. Piotr Mlynarz F. Ekkehardt Hahn Prof. Dr. Maria G. Babashkina Felix D. Sokolov Nail G. Zabirov Joanna Galezowska Henryk Kozlowski 《无机化学与普通化学杂志》2007,633(9):1472-1479
Structure and magnetic properties of N‐diisopropoxyphosphorylthiobenzamide PhC(S)‐N(H)‐P(O)(OiPr)2 ( HLI ) and N‐diisopropoxyphosphoryl‐N′‐phenylthiocarbamide PhN(H)‐C(S)‐N(H)‐P(O)(OiPr)2 ( HLII ) complexes with the CoII cation of formulas [Co{PhC(S)‐N‐P(O)(OiPr)2}2] ( 1 ), [Co{PhN(H)‐C(S)‐N‐P(O)(OiPr)2}2] ( 2 ), [Co{PhC(S)‐N(H)‐P(O)(OiPr)2}2{PhC(S)‐N‐P(O)(OiPr)2}2] ( 1a ) and [Co{PhC(S)‐N‐P(O)(OiPr)2}2}(2,2′‐bipy)] ( 3 ), [Co{PhC(S)‐N‐P(O)(OiPr)2}2(1,10‐phen)] ( 4 ), [Co{PhN(H)‐C(S)‐N‐P(O)(OiPr)2}2(2,2′‐bipy)] ( 5 ), [Co{PhN(H)‐C(S)‐N‐P(O)(OiPr)2}2(1,10‐phen)] ( 6 ) were investigated. Paramagnetic shifts in the 1H NMR spectrum were observed for high‐spin CoII complexes with HLI,II , incorporating the S‐C‐N‐P‐O chelate moiety and two aromatic chelate ligands. Investigation of the thermal dependence of the magnetic susceptibility has shown that the extended materials 1‐2 and 6 show ferromagnetic exchange between distorted tetrahedral ( 1 , 2 ) or octahedral ( 1a , 6 ) metal atoms whereas 3 and 5 show antiferromagnetic properties. Compound 4 behaves as a spin‐canted ferromagnet, an antiferromagnetic ordering taking place below a critical temperature, Tc = 115 K. Complexes 1 and 1a were investigated by single crystal X‐ray diffraction. The cobalt(II) atom in complex 1 resides a distorted tetrahedral O2S2 environment formed by the C=S sulfur atoms and the P=O oxygen atoms of two deprotonated ligands. Complex 1a has a tetragonal‐bipyramidal structure, Co(Oax)2(Oeq)2(Seq)2, and two neutral ligand molecules are coordinated in the axial positions through the oxygen atoms of the P=O groups. The base of the bipyramid is formed by two anionic ligands in the typical 1,5‐O,S coordination mode. The ligands are in a trans configuration. 相似文献
5.
Daniel Werner Prof. Dr. Glen B. Deacon Prof. Dr. Peter C. Junk Prof. Dr. Reiner Anwander 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(15):4426-4438
Four new cerium(III) formamidinate complexes comprising [Ce(p‐TolForm)3], [Ce(DFForm)3(thf)2], [Ce(DFForm)3], and [Ce(EtForm)3] were synthesized by protonolysis reactions using [Ce{N(SiMe3)2}3] and formamidines of varying functionality, namely N,N′‐bis(4‐methylphenyl)formamidine (p‐TolFormH), N,N′‐bis(2,6‐difluorophenyl)formamidine (DFFormH), and the sterically more demanding N,N′‐bis(2,6‐diethylphenyl)formamidine (EtFormH). The bimetallic cerium lithium complex [LiCe(DFForm)4] was synthesized by treating a mixture of [Ce{N(SiHMe2)2}3(thf)2] and [Li{N(SiHMe2)2}] with four equivalents of DFFormH in toluene. Oxidation of the trivalent cerium(III) formamidinate complexes by trityl chloride (Ph3CCl) caused dramatic color changes, although the cerium(IV) species appeared transient and reformed cerium(III) complexes and N′‐trityl‐N,N′‐diarylformamidines shortly after oxidation. The first structurally characterized homoleptic cerium(IV) formamidinate complex [Ce(p‐TolForm)4] was obtained through a protonolysis reaction between [Ce{N(SiHMe2)2}4] and four equivalents of p‐TolFormH. [Ce{N(SiHMe2)2}4] was also treated with DFFormH and EtFormH, but the resulting cerium(IV) complexes decomposed before isolation was possible. The new cerium(IV) silylamide complex [Ce{N(SiMe3)2}3(bda)0.5]2 (bda=1,4‐benzenediolato) was synthesized by treatment of [Ce{N(SiMe3)2}3] with half an equivalent of 1,4‐benzoquinone, and showed remarkable resistance towards protonolysis or reduction. 相似文献
6.
The preparation, characterisation and X-ray structures of the three Ni(II) salts [Ni{ArP(OH)S2}2(thf)2] (1) (Ar = 4-anisyl), [Ni{PhP(OH)Se2}2(thf)2] (2) and [Ni{P(OH)2S2}2(thf)4] (3) are reported. 相似文献
7.
Reactions of the oxorhenium(V) complexes [ReOX3(PPh3)2] (X = Cl, Br) with the N‐heterocyclic carbene (NHC) 1,3,4‐triphenyl‐1,2,4‐triazol‐5‐ylidene (LPh) under mild conditions and in the presence of MeOH or water give [ReOX2(Y)(PPh3)(LPh)] complexes (X = Cl, Br; Y = OMe, OH). Attempted reactions of the carbene precursor 5‐methoxy‐1,3,4‐triphenyl‐4,5‐dihydro‐1H‐1,2,4‐triazole ( 1 ) with [ReOCl3(PPh3)2] or [NBu4][ReOCl4] in boiling xylene resulted in protonation of the intermediately formed carbene and decomposition products such as [HLPh][ReOCl4(OPPh3)], [HLPh][ReOCl4(OH2)] or [HLPh][ReO4] were isolated. The neutral [ReOX2(Y)(PPh3)(HLPh)] complexes are purple, airstable solids. The bulky NHC ligands coordinate monodentate and in cis‐position to PPh3. The relatively long Re–C bond lengths of approximate 2.1Å indicate metal‐carbon single bonds. 相似文献
8.
A reaction of the potassium salts of RC(S)NHP(S)(OiPr)2 (R = PhNH, HL I; Ph, HL II) with a mixture of AgNO3 and Ph2P(CH2)1 − 3PPh2 or Ph2P(C5H4FeC5H4)PPh2 in aqueous EtOH/CH2Cl2 leads to [Ag2(Ph2PCH2PPh2)2LINO3] ( 1 ), [Ag{Ph2P (CH2)2PPh2}LI,II] ( 2, 6 ), [Ag{Ph2P(CH2)3PPh2}LI,II] ( 3, 7 ), [Ag{Ph2P(C5H4FeC5H4)PPh2}LI,II] ( 4, 8 ), and [Ag2(Ph2PCH2PPh2)LII2] ( 5 ) complexes. The structures of these compounds were investigated by 1H and 31P{1H} NMR spectroscopy and elemental analyses. It was established that the binuclear complexes 1 and 5 are luminescent in the solid state at ambient conditions. © 2010 Wiley Periodicals, Inc. Heteroatom Chem 21:386–391, 2010; View this article online at wileyonlinelibrary.com . DOI 10.1002/hc.20627 相似文献
9.
Oliver J. Cooper Dr. David P. Mills Dr. Jonathan McMaster Dr. Floriana Tuna Prof. Eric. J. L. McInnes Dr. William Lewis Prof. Alexander J. Blake Dr. Stephen T. Liddle 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(22):7071-7083
Treatment of [K(BIPMMesH)] (BIPMMes={C(PPh2NMes)2}2?; Mes=C6H2‐2,4,6‐Me3) with [UCl4(thf)3] (1 equiv) afforded [U(BIPMMesH)(Cl)3(thf)] ( 1 ), which generated [U(BIPMMes)(Cl)2(thf)2] ( 2 ), following treatment with benzyl potassium. Attempts to oxidise 2 resulted in intractable mixtures, ligand scrambling to give [U(BIPMMes)2] or the formation of [U(BIPMMesH)(O)2(Cl)(thf)] ( 3 ). The complex [U(BIPMDipp)(μ‐Cl)4(Li)2(OEt2)(tmeda)] ( 4 ) (BIPMDipp={C(PPh2NDipp)2}2?; Dipp=C6H3‐2,6‐iPr2; tmeda=N,N,N′,N′‐tetramethylethylenediamine) was prepared from [Li2(BIPMDipp)(tmeda)] and [UCl4(thf)3] and, following reflux in toluene, could be isolated as [U(BIPMDipp)(Cl)2(thf)2] ( 5 ). Treatment of 4 with iodine (0.5 equiv) afforded [U(BIPMDipp)(Cl)2(μ‐Cl)2(Li)(thf)2] ( 6 ). Complex 6 resists oxidation, and treating 4 or 5 with N‐oxides gives [{U(BIPMDippH)(O)2‐ (μ‐Cl)2Li(tmeda)] ( 7 ) and [{U(BIPMDippH)(O)2(μ‐Cl)}2] ( 8 ). Treatment of 4 with tBuOLi (3 equiv) and I2 (1 equiv) gives [U(BIPMDipp)(OtBu)3(I)] ( 9 ), which represents an exceptionally rare example of a crystallographically authenticated uranium(VI)–carbon σ bond. Although 9 appears sterically saturated, it decomposes over time to give [U(BIPMDipp)(OtBu)3]. Complex 4 reacts with PhCOtBu and Ph2CO to form [U(BIPMDipp)(μ‐Cl)4(Li)2(tmeda)(OCPhtBu)] ( 10 ) and [U(BIPMDipp)(Cl)(μ‐Cl)2(Li)(tmeda)(OCPh2)] ( 11 ). In contrast, complex 5 does not react with PhCOtBu and Ph2CO, which we attribute to steric blocking. However, complexes 5 and 6 react with PhCHO to afford (DippNPPh2)2C?C(H)Ph ( 12 ). Complex 9 does not react with PhCOtBu, Ph2CO or PhCHO; this is attributed to steric blocking. Theoretical calculations have enabled a qualitative bracketing of the extent of covalency in early‐metal carbenes as a function of metal, oxidation state and the number of phosphanyl substituents, revealing modest covalent contributions to U?C double bonds. 相似文献
10.
Dr. Hajime Kameo Tatsuya Kawamoto Prof. Shigeyoshi Sakaki Prof. Didier Bourissou Prof. Hiroshi Nakazawa 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(7):2370-2375
Si?F bond cleavage of fluoro‐silanes was achieved by transition‐metal complexes under mild and neutral conditions. The Iridium‐hydride complex [Ir(H)(CO)(PPh3)3] was found to readily break the Si?F bond of the diphosphine‐ difluorosilane {(o‐Ph2P)C6H4}2Si(F)2 to afford a silyl complex [{[o‐(iPh2P)C6H4]2(F)Si}Ir(CO)(PPh3)] and HF. Density functional theory calculations disclose a reaction mechanism in which a hypervalent silicon species with a dative Ir→Si interaction plays a crucial role. The Ir→Si interaction changes the character of the H on the Ir from hydridic to protic, and makes the F on Si more anionic, leading to the formation of Hδ+???Fδ? interaction. Then the Si?F and Ir?H bonds are readily broken to afford the silyl complex and HF through σ‐bond metathesis. Furthermore, the analogous rhodium complex [Rh(H)(CO)(PPh3)3] was found to promote the cleavage of the Si?F bond of the triphosphine‐monofluorosilane {(o‐Ph2P)C6H4}3Si(F) even at ambient temperature. 相似文献
11.
Tobias Niebel Daniel G. MacDonald Chhatra B. Khadka John F. Corrigan Prof. Dr. 《无机化学与普通化学杂志》2010,636(6):1095-1099
The trans‐bis(trimethylsilyl)chalcogenolate palladium complexes, trans‐[Pd(ESiMe3)2(PnBu3)2] [E = S ( 1 ) and Se ( 2 )] were synthesized in good yields and high purity by reacting trans‐[PdCl2(PBu3)2] with LiESiMe3 (E = S, Se), respectively. These complexes were characterized by 1H, 13C{1H}, 31P{1H} (and 77Se{1H}) NMR spectroscopy and single‐crystal X‐ray analysis. The reaction of 2 with propionyl chloride led to the formation of trans‐[Pd(SeC(O)CH2CH3)2(PnBu3)2] ( 3 ), a trans‐bis(selenocarboxylato) palladium complex and thus established a new method for the formation of this type of complex. Complex 3 was characterized by 1H, 13C{1H}, 31P{1H} and 77Se{1H} NMR spectroscopy and a single‐crystal X‐ray structure analysis. 相似文献
12.
Reaction of RuCl2(PPh3)3 with N‐Phenyl‐pyridine‐2‐carbaldehyde thiosemicarbazone (C5H4N–C2(H)=N3‐N2H–C1(=S)N1HC6H5, Hpytsc‐NPh) in presence of Et3N base led to loss of ‐N2H‐proton and yielded the complex [Ru(pytsc‐NPh)2(Ph3P)2] ( 1 ). Similar reactions of precursor RuCl2[(p‐tolyl)3P]3 with a series of thiosemicarbazone ligands, viz. pyridine‐2‐carbaldehyde thiosemicarbazone (Hpytsc), salicylaldehyde thiosemicarbazone (H2stsc), and benzaldehyde thiosemicarbazone (Hbtsc), have yielded the complexes, [Ru(pytsc)2{(p‐tolyl)3P}2] ( 2 ), [Ru(Hstsc)2{(p‐tolyl)3P}]2 ( 3 ), and [Ru(btsc)2{(p‐tolyl)3P}2] ( 4 ), respectively. The reactions of precursor Ru2Cl4(dppb)3 {dppb = Ph2P–(CH2)4–PPh2} with H2stsc, Hbtsc, furan‐2‐carbaldehyde thiosemicarbazone (Hftsc) and thiophene‐2‐carbaldehyde thiosemicarbazone (Httsc) have formed complexes of the composition, [Ru(Hstsc)2(dppb)] ( 5 ), [Ru(btsc)2(dppb)] ( 6 ), [Ru(ftsc)2(dppb)] ( 7 ), and [Ru(ttsc)2(dppb)] ( 8 ). The complexes have been characterized by analytical data, IR, NMR (1H, 31P) spectroscopy and X‐ray crystallography ( 1 and 5 ). The proton NMR confirmed loss of –N2H– proton in all the compounds, and 31P NMR spectra reveal the presence of equivalent phosphorus atoms in the complexes. In all the compounds, thiosemicarbazone ligands coordinate to the RuII atom via hydrazinic nitrogen (N2) and sulfur atoms. The arrangement around each metal atom is distorted octahedral with cis:cis:trans P, P:N, N:S, S dispositions of donor atoms. 相似文献
13.
Maryam Shafaei‐Fallah Weifeng Shi Dieter Fenske Alexander Rothenberger 《无机化学与普通化学杂志》2006,632(6):1091-1096
Syntheses and Structures of Transition Metal Complexes with Dithiophosphinato and Trithiophosphinato Ligands The reactions of MnCl2 with Ph2P(S)(SSiMe3) produced [Mn(S2PPh2)2(thf)2] ( 1 ) and [Mn(S2PPh2)2(dme)] ( 2 ) (DME = 1,2‐Dimethoxyethane). The compounds [Co6(S3PPh)2(μ4‐S)2(μ3‐S)2(PPh3)4] ( 3 ), [Co2(S3PPh)2(PPh3)2] ( 4 ), [Ni(S2PPh)(PPhEt2)2] ( 5 ), [Ni(S3PPh)(PPhEt2)2] ( 6 ) and [Cu4(S3PPh)2(dppp)2] ( 8 ) [dppp = 1,3‐Bis(diphenylphosphanyl)propane] were obtained from reactions of first‐row transition metal halides with PhP(S)(SSiMe3)2 in the presence of tertiary phosphines. In a reaction of PhP(S)(SSiMe3)2 with PhPEt2 PhPEt2PS2Ph ( 7 ) was isolated. All compounds were characterized by X‐ray crystallography. 相似文献
14.
D. C. Menezes F. T. Vieira G. M. de Lima J. L. Wardell M.E. Corts M. P. Ferreira M. A. Soares A. Vilas Boas 《应用有机金属化学》2008,22(4):221-226
The in vitro antifungal activity of the dithiocarbamate organotin complexes [Sn{S2CN(CH2)4}2Cl2] ( 1 ), [Sn{S2CN(CH2)4}2Ph2] ( 2 ), [Sn{S2CN(CH2)4}Ph3] ( 3 ), [Sn{S2CN(CH2)4}2n‐Bu2] ( 4 ), [Sn{S2CN(CH2)4}Cy3] {Cy = cyclohexyl} ( 5 ), [Sn{S2CN(C2H5)2}2Cl2] ( 6 ), [Sn{S2CN(C2H5)2}2Ph2] ( 7 ), [Sn{S2CN(C2H5)2}Ph3] ( 8 ), [Sn{S2CN(C2H5)2}3Ph] ( 9 ) and [Sn{S2CN(C2H5)2}Cy3] ( 10 ) has been screened against Candida albicans (ATCC 18804), Candida tropicalis (ATCC 750) and resistant Candida albicans collected from HIV‐positive Brazilian patients with oral candidiasis. All compounds exhibited antifungal activities and complexes 3 and 8 displayed the best results. We have investigated the effect of compounds 1–10 on the cellular activity of the yeast cultures. Changes in mitochondrial function have not been detected. However, all drugs reduced ergosterol biosynthesis. Preliminary studies on DNA integrity indicated that the compounds do not cause gross damage to yeast DNA. The data suggest that these compounds share some mechanisms of action on cell membranes similar to that of polyene but not with azole drugs, normally used in Candida infections. Copyright © 2008 John Wiley & Sons, Ltd. 相似文献
15.
Robert J. Brown Donna S. Amenta John W. Gilje Glenn P. A. Yap 《Acta Crystallographica. Section C, Structural Chemistry》2013,69(10):1104-1107
The aminophosphane ligand 1‐amino‐2‐(diphenylphosphanyl)ethane [Ph2P(CH2)2NH2] reacts with dichloridotris(triphenylphosphane)ruthenium(II), [RuCl2(PPh3)3], to form chloridobis[2‐(diphenylphosphanyl)ethanamine‐κ2P,N](triphenylphosphane‐κP)ruthenium(II) chloride toluene monosolvate, [RuCl(C18H15P)(C14H16NP)2]Cl·C7H8 or [RuCl(PPh3){Ph2P(CH2)2NH2}2]Cl·C7H8. The asymmetric unit of the monoclinic unit cell contains two molecules of the RuII cation, two chloride anions and two toluene molecules. The RuII cation is octahedrally coordinated by two chelating Ph2P(CH2)2NH2 ligands, a triphenylphosphane (PPh3) ligand and a chloride ligand. The three P atoms are meridionally coordinated, with the Ph2P– groups from the ligands being trans. The two –NH2 groups are cis, as are the chloride and PPh3 ligands. This chiral stereochemistry of the [RuCl(PPh3){Ph2P(CH2)2NH2}2]+ cation is unique in ruthenium–aminophosphane chemistry. 相似文献
16.
Rare examples of amido‐iodo complexes of selected divalent lanthanides can be synthesized by using deprotonated Ap*H {Ap*H = 2,6‐diisopropylphenyl)‐[6‐(2,4,6‐triisopropylphenyl)‐pyridin‐2‐yl]‐amine} as a stabilizing ligand. Reaction of [Ap*K]n with [LnI2(thf)n] (Ln = Eu, Yb, n = 4,5) in THF leads to [Ln(Ap*)I(thf)2]2 (Ln = Eu, Yb). An attempted reduction of these divalent heteroleptic complexes with KC8 to synthesize complexes containing an unsupported Ln–Ln bond resulted in the formation of [Ln(Ap*)2(thf)2]. These lanthanide complexes were characterized by X‐ray structure analysis. 相似文献
17.
Investigations of the Synthesis of [CpxSb{M(CO)5}2] (Cpx = Cp, Cp*; M = Cr, W) The reaction of CpSbCl2 with [Na2{Cr2(CO)10}] leads to the chlorostibinidene complex [ClSb{Cr(CO)5}2(thf)] ( 1 ), whereas the reaction of CpSbCl2 with [Na2{W2(CO)10}] results in the formation of the complexes [ClSb{W(CO)5}3] ( 2 ), [Na(thf)][Cl2Sb{W(CO)5}2] ( 3 ), [ClSb{W(CO)5}2(thf)] ( 4 ) and [Sb2{W(CO)5}3] ( 5 ). The stibinidene complex [CpSb{Cr(CO)5}2] ( 6 ) is obtained by the reaction of [ClSb{Cr(CO)5}2] with NaCp, while its Cp* analogue [Cp*Sb{Cr(CO)5}2] ( 7 ) is formed via the metathesis of Cp*SbCl2 with [Na2{Cr2(CO)10}]. The products 2 , 3 , 4 and 7 are additionally characterised by X‐ray structure analyses. 相似文献
18.
Magnetic Coupling between Metal Spins through the 7,7,8,8‐Tetracyanoquinodimethane (TCNQ) Dianion
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Dr. Mohamed R. Saber Dr. Andrey V. Prosvirin Assoc. Prof. Brendan F. Abrahams Dr. Robert W. Elliott Prof. Richard Robson Prof. Kim R. Dunbar 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(25):7593-7597
A family of magnetic metal–organic frameworks, (Ph3PMe)2[M2(TCNQ)3] {M=Fe2+, Co2+, Ni2+ and Zn2+} have been prepared and structurally characterized. The honeycomb‐like “layers” consist of MII ions doubly bridged with dinitrilomethane moieties of two 7,7,8,8‐tetracyanoquinodimethane (TCNQ) dianions which are further connected through phenyl rings to form a 3D dianionic framework [M2TCNQ3]2? with Ph3PMe+ cations filling cavities that run along the c axis. Studies of the magnetic coupling through the TCNQ dianion in these structures revealed that it can promote long‐range magnetic ordering despite the long coupling pathway. 相似文献
19.
《Polyhedron》1987,6(6):1503-1507
The pentacoordinate rhodium nitrosyl complexes [RhBr2(NO)L2 [L = P(OPh)2Ph, P(OMe)Ph2 or P(OPri)Ph2] have been synthesized and the structures of [RhBr2(NO){P(OMe)Ph2}2] and [RhBr2(NO){P(OPri)Ph2}2] have been determined X-ray crystallographically. Both of these latter compounds are tetragonal pyramidal with the nitrosyl group apical. The methoxydiphenylphosphine ligands in [RhBr2(NO){P(OMe)Ph2}2] are cis-disposed whereas the larger cis-propoxydiphenylphosphine ligands in [RhBr2(NO){P(OPri)Ph2}2] are mutually trans. The nitrosyl group in trans-[RhBr2(NO){P(OPri)Ph2}2] eclipses an Rh-P axis but in cis-[RhBr2(NO){P(OMe)Ph2}2] it is staggered with respect to the P-Rh-P linkage. The isomeric behaviour of nitrosyl complexes of type [RhX2(NO)L2] (X = halogen, L = phosphorus donor ligand) is rationalized in terms of the size of the ligand L. 相似文献
20.
Nermin Biricik Zhaofu Fei Rosario Scopelliti PaulJ. Dyson 《Helvetica chimica acta》2003,86(10):3281-3287
The polydentate phosphinoamines 1,3‐{(Ph2P)2N}2C6H4 and 2,6‐{(Ph2P)2N}2C5H3N have been prepared in a single step from the reaction of the amines 1,3‐(NH2)2C6H4 or 2,6‐(NH2)2C5H3N with Ph2PCl in presence of Et3N (1 : 4 : 4 molar ratio) in CH2Cl2. Reaction of 1,3‐{(Ph2P)2N}2C6H4 or 2,6‐{(Ph2P)2N}2C5H3N with elemental sulfur or selenium in CH2Cl2 affords the corresponding tetrasulfide or tetraselenide, respectively, in good yield. The complexes [1,3‐{Mo(CO)4(Ph2P)2N}2(C6H4)] and [2,6‐{Mo(CO)4(Ph2P)2N}2(C5H3N)] were prepared from the reaction of these phosphinoamines with [Mo(CO)4(nbd)] (nbd=norbornadiene) in toluene, and the structure of the latter complex has been determined by single‐crystal X‐ray diffraction analysis. 相似文献