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1.
The reactions of RNHSi(Me) 2Cl (1, R= t-Bu; 2, R=2,6-(Me 2CH) 2C 6H 3) with the carborane ligands, nido-1-Na(C 4H 8O)-2,3-(SiMe 3) 2-2,3-C 2B 4H 5 (3) and Li[ closo-1-R′-1,2-C 2B 10H 10] (4), produced two kinds of neutral ligand precursors, nido-5-[Si(Me) 2N(H)R]-2,3-(SiMe 3) 2-2,3-C 2B 4H 5, (5, R= t-Bu) and closo-1-R′-2-[Si(Me) 2N(H)R]-1,2-C 2B 10H 10 (6, R= t-Bu, R′=Ph; 7, R=2,6-(Me 2CH) 2C 6H 3, R′=H), in 85, 92, and 95% yields, respectively. Treatment of closo-2-[Si(Me) 2NH(2,6-(Me 2CH) 2C 6H 3)]-1,2-C 2B 10H 11 (7) with three equivalents of freshly cut sodium metal in the presence of naphthalene produced the corresponding cage-opened sodium salt of the “carbons apart” carborane trianion, [ nido-3-{Si(Me) 2N(2,6-(Me 2CH) 2C 6H 3)}-1,3-C 2B 10H 11] 3− (8) in almost quantitative yield. The reaction of the trianion, 8, with anhydrous MCl 4 (M=Ti and Zr) in 1:1 molar ratio in dry tetrahydrofuran (THF) at −78 °C, resulted in the formation of the corresponding half-sandwich neutral d 0-metallacarborane, closo-1-M[(Cl)(THF) n]-2-[1′-η 1σ-N(2,6-(Me 2CH) 2C 6H 3)(Me) 2Si]-2,4-η 6-C 2B 10H 11 (M=Ti (9), n=0; M=Zr (10), n=1) in 47 and 36% yields, respectively. All compounds were characterized by elemental analysis, 1H-, 11B-, and 13C-NMR spectra and IR spectra. The carborane ligand, 7, was also characterized by single crystal X-ray diffraction. Compound 7 crystallizes in the monoclinic space group P2 1/ c with a=8.2357(19) Å, b=28.686(7) Å, c=9.921(2) Å; β=93.482(4)°; V=2339.5(9) Å 3, and Z=4. The final refinements of 7 converged at R=0.0736; wR=0.1494; GOF=1.372 for observed reflections. 相似文献
2.
Reactions of [(η 6-arene)RuCl 2] 2 (1) (η 6-arene= p-cymene (1a), 1,3,5-Me 3C 6H 3 (1b), 1,2,3-Me 3C 6H 3 (1c) 1,2,3,4-Me 4C 6H 2(1d), 1,2,3,5-Me 4C 6H 2 (1e) and C 6Me 6 (1f)) or [Cp*MCl 2] 2 (M=Rh (2), Ir (3); Cp*=C 5Me 5) with 4-isocyanoazobenzene (RNC) and 4,4′-diisocyanoazobenzene (CN–R–NC) gave mononuclear and dinuclear complexes, [(η 6-arene)Ru(CNC 6H 4N=NC 6H 5)Cl 2] (4a–f), [Cp*M(CNC 6H 4N=NC 6H 5)Cl 2] (5: M=Rh; 6: M=Ir) , [{(η 6-arene)RuCl 2} 2{μ-CNC 6H 4N=NC 6H 4NC}] (8a–f) and [(Cp*MCl 2) 2(μ-CNC 6H 4N=NC 6H 4NC)}] (9: M=Rh; 10: M=Ir) , respectively. It was confirmed by X-ray analyses of 4a and 5 that these complexes have trans-forms for the ---N=N--- moieties. Reaction of [Cp*Rh(dppf)(MeCN)](PF 6) 2 (dppf=1,1′-bis (diphenylphosphino)ferrocene) with 4-isocyanoazobenzene gave [Cp*Rh(dppf)(CNC 6H 4N=NC 6H 5)](PF 6) 2 (7), confirmed by X-ray analysis. Complex 8b reacted with Ag(CF 3SO 3), giving a rectangular tetranuclear complex 11b, [{(η 6-1,3,5-Me 3C 6H 3)Ru(μ-Cl} 4(μ-CNC 6H 4N=NC 6H 4NC) 2](CF 3SO 3) 4 bridged by four Cl atoms and two μ-diisocyanoazobenzene ligands. Photochemical reactions of the ruthenium complexes (4 and 8) led to the decomposition of the complexes, whereas those of 5, 7, 9 and 10 underwent a trans-to- cis isomerization. In the electrochemical reactions the reductive waves about −1.50 V for 4 and −1.44 V for 8 are due to the reduction of azo group, [---N=N---]→[---N=N---] 2−. The irreversible oxidative waves at ca. 0.87 V for the 4 and at ca. 0.85 V for 8 came from the oxidation of Ru(II)→Ru(III). 相似文献
3.
The sterically hindered zinc chalcogenolato complexes [Zn(EAr″) 2] 2 (E = S, Se; Ar″ = 2,4,6-Bu t3C 6H 2) react with 1 equivalent of tert-butylisocyanide in non-coordinating solvents to give Zn(EC 6H 2Bu t3) 2(CNBu t) (1, E = S; 2, E = Se) as thermally stable crystalline adducts; the compounds are thought to be chalcogenolato-bridged dimers. In the presence of excess isocyanide ligand the 1 : 2 adducts Zn(EAr″) 2(CNBu t) 2 (3, E = S; 4, E = Se) are isolated. The compounds represent the first examples of well-characterized isocyanide complexes of zinc. The X-ray structure of 4 showed that it is monomeric with a distorted tetrahedral coordination geometry of the metal centre, which reflects the steric requirements of the chalcogenolato and isocyanide ligands, respectively. 相似文献
4.
Elementary sulfur and selenium combine (in boiling heptane) with [(tBuCp) 2-Zr(C 6H 4R) 2] (Cp = η 5-C 5H 4; R = OCH 3) to give the corresponding dichalcogenophenylenezirconocene. With tellurium, the reaction proceeds only at lower temperature (in boiling hexane), affording the first ditellurophenylenezirconocene. As no metallacycle was obtained with the Cp ligand or when the metal is Hf, complexes of the general type [(RCp) 2MSe 2C 6H 4- o] (M = Ti, Zr, Hf; R = H, t-Bu, (CH 3) 5) have been synthesized by allowing metallocene dichlorides to react with potassium benzenediselenolate, prepared by cleaving [(t-BuCp) 2ZrSe 2C 6H 4- o] with t-BuOK. 相似文献
5.
Reaction of [Cp *TiF 3] (Cp * = (ν 5-C 5Me 5)) with Me 3SiOSO 2- p-C 6H 4CH 3, Me 3SiOPOPh 2 and 1,2-(Me 3SiOCO) 2C 6H 4 yields the dinuclear complexes [{Cp *TiF(μ-F)(μ-OSO 2- p-C 6H 4CH 4)} 2] (1), [{Cp *TiF(μ-F)(μ-OPOPh 2)} 2] (2) and [{Cp *TiF(μ-F)(μ-OCO- o-C 6H 4CO 2SiMe 3)} 2] (3). The molecular structures of 1 and 2 have been determined by single-crystal X-ray analysis. In complexes 1-3, the two titanium atoms are connected by bridging fluorine atoms as well as bridging sulfonate, phosphinate and carboxylate groups respectively. Each titanium atom is also bonded to a terminal fluorine atom. Reaction of [Cp 2*ZrF 2] with 1,2-(Me 3SiOCO) 2C 6H 4 leads to the mononuclear pentacoordinate 18-electron species [Cp 2*ZrF(μ-OCO- o-C 6H 4CO 2SiMe 3)] (4) and its structure was determined by X-ray crystallographic methods. 相似文献
6.
The reaction of the metallocene dichlorides Cp 2MCl 2 (Cp = η 5-C 5H 5; M = Ti, Zr, Hf, Mo, W) and Cp 2′TiCl 2 (Cp′ = η 5-C 5H 4CH 3) with equimolar amounts of dilithium-benzene- o-diselenolate, 1,2-(LiSe) 2C 6H 4, gives the chelate complexes Cp 2M(Se 2C 6H 4) (M = Ti (I), Zr (II), Hf (III), Mo (IV), W (V)) and Cp 2′Ti(Se 2C 6H 4) (VI). CpTiCl 3 reacts with 1,2-(LiSe) 2C 6H 4 to give CpTiCl(Se 2C 6H 4) (VII). The ring inversion activation parameters for I–VI can be determined by means of temperature-dependent 1H NMR spectroscopy in solution. The fragmentation behaviour of I–VII in the mass spectrometer has been investigated by pursuing metastable transitions, using linked-scan techniques. 相似文献
7.
Methods are described for achieving stepwise replacement of all BH terminal hydrogens in CoC 2B 4 clusters with halogen or alkyl groups, leading to complexes such as Cp*Co(2,3-Et 2C 2B 4X 4) (X=Me or I) and Cp*Co(2,3-Et 2C 2B 4IMe 2[O 3SCF 3]). Building on earlier work on B-functionalization of small metallacarboranes via metal-catalyzed cross-coupling, two- and three-dimensional macrocycles containing four to six metal centers have been constructed systematically from monomeric precursor complexes. 相似文献
8.
The mono- and bis-cyclopentadienyl compounds 1-(Cp″)-4-(CH 3)C 6H 4 (1) and 1, 4-(Cp″) 2C 6H 4 (2) (Cp″ = 3,4-dimethylcyclopenta-1,3-diene-1-yl) have been synthesized. The reactions of the lithium salts of 1 and 2 with CpZrCl 3 · dme (dme = dimethoxyethane) and Cp*ZrCl 3(CP* = C 5(CH 3) 5) yielded the mono- and bi-nuclear bridged zirconocenes 1-(Cp″ZrCpCl 2)-4-(CH 3)C 6H 4 (3), 1,4-(Cp″ZrCpCl 2) 2C 6H 4 (4) and 1,4-(Cp″ZrCp*Cl 2) 2C 6H 4 (5). When activated with methylaluminoxane (MAO), the mono- and bi-nuclear zirconocenes 3 and 4 catalyse the polymerization of propene. The influence of the catalyst composition on the polymerization kinetics and molecular weight is discussed. 相似文献
9.
The synthesis of half-sandwich transition metal complexes containing both 1,2-dichalcogenolato-1,2-dicarba-closo-docecaborane (Cab(E,E)) [Cab(E,E)=E(2)C(2)(B(10)H(10)); E = S, Se] and N-heterocyclic carbene (NHC) ligands is described. Addition of mono-NHC ligand to the 16e half-sandwich dichalcogenolato carborane complexes [Cp*Rh(Cab(E,E))], [Cp*Ir(Cab(S,S))], [(p-cymene)Ru(Cab(S,S))] (Cp* = pentamethylcyclopentadienyl) gives corresponding mononuclear 18e dithiolate complexes of the type [LM(Cab(E,E))(NHC)]: [Cp*M(Cab(S,S))(1-ethenyl-3-methylimidazolin-2-ylidene)] (M = Ir (2), Rh (3)), [Cp*Rh(Cab(E,E))(3-methyl-1-picolyimidazolin-2-ylidene)] [E = S (6), Se (7)], [(p-cymene)Ru(Cab(S,S))(NHC)] [NHC = 1-ethenyl-3-methylimidazolin-2-ylidene (4), 3-methyl-1-picolyimidazolin-2-ylidene (8)], whereas bis-NHC give centrosymmetric binuclear complexes [{Cp*M(Cab(S,S))}(2)(1,1'-dimethyl-3,3'-methylene(imidazolin-2-ylidene))] [M = Rh (10), Ir (11)]. The complexes were characterized by IR, NMR spectroscopy and elemental analysis. In addition, X-ray structure analyses were performed on complexes 2-4, 6, 8, 10 and 11. 相似文献
10.
The reaction of CpTiCl 3 with two equivalents of 1,2(LiS) 2C 6H 4 and one equivalent of Ph 4PBr in acetone/pentane affords the new anionic titanium(IV) complex [Ph 4P][CpTi(1,2-S 2C 6H 4) 2], which has been characterized by chemical analysis and by 1H NMR and IR spectroscopy. The structure of the five-coordinated, half-sandwich bis(dithiolato)titanate anion in the tetraphenyl phosphonium salt has been determined by an X-ray diffraction study. The anion has the two five-membered TiS 2C 2 chelate rings folded along the S---S axes by 36 and 23°, with one chelate ligand plane arranged exo, the other endo in relation to to the Cp ligand. 相似文献
11.
An S,S′-thioether—thioester chelating ligand [7,8- μ-SCH 2C(O)S-7,8-C 2B 9H 10] − (L 1), incorporating the unit [—(C) 2B 9H 10] − has been synthesized. Reactions have been conducted with RhCl(PPh 3) 3 and PdCl 2(PPh 3) 2 complexes in ethanol. With Rh, L 1 maintains its original cyclic nature and most probably chelation via thioether—thioester takes place. The carborane negative charge may stabilize this original thioether—thioester complex. The other two Rh positions are occupied by two PPh 3 ancillary ligands forming [Rh(L 1)(PPh 3) 2]. The reaction of L 1 with Pd induces ligand modifications and the cyclic nature of L 1 is lost. A transesterification process leading to a dianionic ligand L 2, [7-S-8-SCH 2C(O)OCH 2CH 3−7,8-C 2B 9H 10] 2− has taken place. In this way L 2 is capable of compensating the dipositive Pd charge. The other two Pd positions are occupied by two PPh 3. This reaction has been extended to methanol and isopropanol solvents. The crystal structure of [Pd(L 2)(PPh 3) 2] has been determined. 相似文献
12.
In order to investigate the influence of organic groups on the types of organoarsenic polymolybdates, the reations of p-aminophenylarsonic acid with sodium molybdate were tested at pH=3-5. Six salts were prepared and characterized. (1) (CN3H8)4 [(p-NH3C6H4As)2Mo6O25] · H2O, (2) (CN3H6)4 [(p-, NH3C6H4As )2Mo6O25 ] · 6H20, (3) Cs4 [(p-NH3C6H4As)2Mo6O25] · 4H2O, (4) C(CH3)4N]4[(p-NH3C6H4As)2Mo6O25] · 5H2O, (5) [(n-C4H9)4N]3Na[(p-NH3C6H4As)2Mo6O25] · 2H2O, (6) Ba2 NH3C6H4As)2Mo6O25] · 10H2O. The IR, UV spectra, and electrochemical behavior are reported and discussed. They should belong to the same type as that for phenyl derivative or the nitrophenyl derivatives. But the ammo groups can accept protons, so that the anion' s charge decreases. Very similar to the tungsten congener (CN3H6)4[(p-NH3C,H4As)2W6O25] · 4H2O, [(RAs)2Mo6O25]4- type of complexes are formed. 相似文献
13.
The reaction of the labelled carborane ligand [3-Et-7,8-Ph 2-7,8- nido-C 2B 9H 8] 2− with a source of {Pt(PMe 2Ph) 2} 2+ affords non-isomerised 1,2-Ph 2-3,3-(PMe 2Ph) 2-6-Et-3,1,2- closo-PtC 2B 9H 8 (1). The analogous reaction between [3-F-7,8-Ph 2-7,8- nido-C 2B 9H 8] 2− and {Pt(PMe 2Ph) 2} 2+ yields 1,8-Ph 2-2,2-(PMe 2Ph) 2-4-F-2,1,8- closo-PtC 2B 9H 8 (3). Compound 1 has a heavily slipped structure ( Δ 0.72 Å), which to some degree obviates the need for C atom isomerisation. However, that it is a kinetic product of the reaction is evident from the fact that it reverts to isomerised 1,8-Ph 2-2,2-(PMe 2Ph) 2-4-Et-2,1,8- closo-PtC 2B 9H 8 (2) slowly at room temperature but more rapidly with gentle warming. The heteroatom and labelled-B atom positions in the isomerised compounds 2 and 3 may be explained most simply by the rotation of a CB 2 face of an intermediate based on the structure of 1. Compounds 1–3 were characterised by a combination of spectroscopic and crystallographic techniques. 相似文献
14.
The new diphenolato complexes [{Mo(NO){HB(dmpz) 3}Cl} 2Q] where dmpz = 3,5-dimethylpyrazolyl and Q = OC 6H 4(C 6H 4O ( n = 1 or 2), OC 6H 4CR=CRC 6H 4O (R = H or Et), and OC 6H 4CH=CHC 6H 4CH=CHC 6H 4O have been prepared and their electrochemical properties (cyclic and differential pulse voltammetry) compared with previously reported analogues where Q = OC 6H 4O, OC 6H 4EC 6H 4O (E = SO 2, CO and S), OC 6H 4 (CO)C 6H 4 C 6H 4(CO)C 6H 4O and 1,5- and 2,7-O 2C 10H 6. The electrochemical interaction between the redox centres in the new complexes is very weak, in contrast to that in the 1,4-benzenediolato and naphthalendiolato species. The EPR spectra of the reduced mixed-valence species [{Mo(NO){HB(dmpz) 3}Cl} 2Q] − where Q = 1,3- and 1,4-OC 6H 4O and OC 6H 4SC 6H 4O shows that they are valence-trapped at room temperature, whereas those of the dianions [{Mo(NO){HB(dmpz) 3}Cl} 2Q] 2− where Q = 1,4-OC 6H 4O, OC 6H 4EC 6H 4O (E = CO or S) and OC 6H 4CH=CHC 6H 4CH=CHC 6H 4O shows that the unpaired spins on each molybdenum centre are strongly correlated ( J, the spin exchange integral A Mo, the metal-hyperfine coupling constant). The electrochemical properties and the comproportionation constants for the reaction [{Mo(NO){HB(dmpz) 3} Cl} 2Q] + [{Mo(NO){HB(dmpz) 3}Cl}O] 2] 2−2[{Mo(NO) {HB(dmpz) 3}Cl} 2Q] − where Q = diphenolato bridge, are compared with related compounds containing benzenediamido and dianilido bridges. 相似文献
15.
LnCl 3 (Ln=Nd, Gd) reacts with C 5H 9C 5H 4Na (or K 2C 8H 8) in THF (C 5H 9C 5H 4 = cyclopentylcyclopentadienyl) in the ratio of 1 : to give (C 5H 9C 5H 4)LnCl 2(THF) n (orC 8H 8)LnCl 2(THF) n], which further reacts with K 2C 8H 8 (or C 5H 9C 5H 4Na) in THF to form the litle complexes. If Ln=Nd the complex (C 8H 8)Nd(C 5H 9C 5H 4)(THF) 2 (a) was obtained: when Ln=Gd the 1 : 1 complex [(C 8H 8)Gd(C %H 9)(THF)][(C 8H 8)Gd(C 5H 9H 4)(THF) 2] (b) was obtained in crystalline form. The crystal structure analysis shows that in (C8H8)Ln(C5H9C5H4)(THF)2 (Ln=Nd or Gd), the Cyclopentylcyclopentadieny (η5), cyclooctatetraenyl (η8) and two oxygen atoms from THF are coordinated to Nd3+ (or Gd3+) with coordination number 10. The centroid of the cyclopentadienyl ring (Cp′) in C5H9C5H4 group, cyclooctatetraenyl centroid (COTL) and two oxygens (THF) form a twisted tetrahedron around Nd3+ (or Gd3+). In (C8H8)Gd(C5H9C5H4)(THF), the cyclopentyl-cyclopentadienyl (η5), cyclooctatetraenyl (η8) and one oxygen atom are coordinated to Gd3+ with the coordination number of 9 and Cp′, COT and oxygen atom form a triangular plane around Gd3+, which is almost in the plane (dev. -0.0144 Å). 相似文献
16.
The aryldiazenido ligands provide the fourth member of the isoelectronic series CO, NO +, RNC, RN 2+ of ligands for transition metal complexes. The first aryldiazenido metal complex was reported in 1964 when p-CH 3OC 6H 4N 2Mo(CO) 2C 5H 5 was prepared by the reaction of NaMo(CO) 3C 5H 5 with p-CH 3OC 6H 4N 2+BF 4−. This review surveys the development of organometallic aryldiazenido chemistry since that time. Such organometallic aryldiazenido derivatives, including RN 2M(CO) 2C 5H 5, RN 2M(CO) 2(Pz 3BH) (M = Cr, Mo, W), [(η 6-Me 6C 6)Cr(CO) 2N 2Ar] +, [(MeC 15H 4)M′(CO) 2N 2Ar] + M′ = Mn, Re), [ trans-PhN 2Fe(CO) 2(PPh 3) 2] +, and PhN 2M′(CO) 2(PPh 3) 2(PPh 3) 2 can be obtained by reactions of arenediazonium salts with suitably chosen transition metal nucleophiles. Analogous methods cannot be used to prepare alkyldiazenido transition metal complexes because of the instability of alkyldiazonium salts. However, the alkyldiazenido derivatives RCH 2N 2M(CO) 2C 5H 5 (R = H or Me 3Si) can be obtained from HM(CO) 3C 5H 5 and the corresponding diazoalkanes. Important aspects of the chemical reactivity of RN 2M(CO) 2Q derivatives (Q = C 5H 5, Pz 3BH) include CO substitution reactions, coordination of the second nitrogen in the RN 2 ligand to give heterobimetallic complexes such as C 5H 5Mo(CO) 2(μ-NNC 6H 4Me)(CO) 2C 5H 5, oxidative addition rections with X 2 X = Cl, Br, I), SnX 4, RSSR, and CINO, and reactions with further RN 2+ to give bis(aryldiazenido) derivatives (RN 2) 2MQL + (L = CO, X −, etc.). Dearylation of an aryldiazenido ligand to a dinitrogen ligand can be effected by reaction of [(MeC 5H 4)M′(CO) 2N 2Ar] + with certain nucleophiles to give (MeC 5H 4)M′(CO) 2N 2. 相似文献
17.
以半夹心结构铑的化合物Cp*Rh(CN^tBu)Cl2(1)(Cp*=η^5-C5Me5)与Fe(C5H4ELi)2.2THF反应,合成出异双核二茂铁化合物Cp*Rh(CN^tBu)(EC5H4)2Fe[E=S(2),Se(3),Te(4)]。通过AgBF4氧化2和3得到二茂铁离子型化合物[Cp*Rh(CN^tBu)(EC5H4)2Fe]BF4[E=S(5),Se(6)]。采用元素分析、红外光谱、^1H和13CNMR谱以及EI-MS表征了所合成的化合物。 相似文献
18.
139La-NMR chemical shifts were measured for several anionic complexes of formulae Li(C 4H 8O 2) 3/2 [La(ν 3-C 3H 5) 4], [Li(C 4H 8O 2) 2][Cp′ nLa(ν 3-C 3]H 5) 4−n] (Cp′ = Cp(ν 5-C 5H 5); n = 1, 2 and Cp′ = Cp * (ν 5-C 5Me5); N = 1) and Li[R nLa(ν 3-C 3H 4) 4− n] (R = N(SiMe 3) 2; n = 1, 2 and R = CCsIMe 3; n = 4), as well as for neutral compounds for formulae La(ν 3-C 3H 5) 3L n (L = (C 4H 8O 2) 1.5, (HMPT) 2, TMED), Cp′ nLa(ν 3-C 3H 5) 3−n (Cp′= Cp(ν 5-Cp 5H 5), Cp *(ν 5-C 5Me 5); n = 1, 2) and La(ν 3-C 3H 2) 2X(THF) 2 X = Cl, Br, I). Typical ranges of the 139La-NMR chemical shifts were found for the different types of complex independent of number and kind of organyl groups directly bonded to lanthanum. Zusammenfassung139La-NMR-Spektroskopie wurde an einer Reihe anionischer Allyllanthanat(III)-Komplexe der Zusammensetzung
]- [La)ν3-C3H5)4, [Li(C4H8)2][Cp′nLa(ν3-C3H5)4−n(Cp′ = Cp(ν5-C5H5); n = 1, 2 und Cp′ = Cp * (ν5-C5Me5); N = 1) und Li[RnLa(ν3-C3H5)4−n (R = B(SiMe3)2; n = 1, 2 und R = CCSiMe3; n = 4 sowie neutraler Allyllanthan(III)-Komplexe der Zusammensetzung La(ν3-C3H5)3Ln (Ln = (C4H8O2)1.5, (HMPT)2, TMED), Cp′n, La(ν3-C3H5)3−n (Cp′ = Cp(ν5-C5H5), Cp * (ν5- Cp5Me5); n = 1, 2) und La(ν3-Cp3H5)2X(THF)2 (X = Cl, Br, I) durchgefürt. In Abhängikeit von der Anzahl und der Art der am Lanthan gebundenen Gruppen wurden für die verschieden Komplextypen charakteristische Resonanzbereiche ermittelt. 相似文献
19.
1,2-二(1-苯基环己基环戊二烯基)四甲基二硅烷与Fe(CO) 5在二甲苯中加热回流生成二铁化合物(Me 2SiSiMe 2)[(1-Ph-c-C 6H 10C 5H 3)Fe(CO)] 2(μ-CO) 2(2).通过柱层析分离到化合物2的顺反异构体2c和2t,并分别进行热重排反应,发现顺式底物2c重排生成反式重排产物[Me 2Si(c-C 6H 10PhC 5H 3)Fe(CO) 2] 2(3t),而反式底物2t重排则生成顺式重排产物3c.这表明重排反应是立体专一性的.通过X射线衍射分析测定了化合物2c和3t的晶体结构. 相似文献
20.
合成双(2,4-二甲基戊二烯基)氯化钆{[2,4-(CH 3) 2C 5H 5] 2GD cl} 2,并测定了晶体结构.晶体为单斜晶系,P2 1/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)nm 3,Z=3. 相似文献
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