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1.
Reactions of (IPr)Cu(X) (X = Cl or trifluoromethanesulfonate, IPr = 1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene) complexes with the strong acids HOTf or HCl result in protonation of the C2 carbon of the IPr ligand to form imidazolium cations. Coordination of the imidazolium to the resulting CuI system depends upon the identity of the two counterions (chloride or triflate). The copper complexes [(IPrH)Cu(OTf)(μ-OTf)]2 and [IPrH][CuCl2] as well as the imidazolium salt [IPrH][OTf] have been characterized by NMR spectroscopy and single crystal X-ray diffraction studies. 相似文献
2.
Cameron Jones David P. Mills Richard P. Rose Andreas Stasch William D. Woodul 《Journal of organometallic chemistry》2010,695(22):2410-2417
Reactions of the anionic gallium(I) heterocycle salt, [K(tmeda)][Ga(DAB)] (DAB = {N(Dip)C(H)}2; Dip = C6H3Pri2-2,6), with a series of groups 6-9 and 11 metal halide complexes have given rise to the metal gallyl complexes, [CpCr(IMes){Ga(DAB)}] (IMes = :C{(Mes)NC(H)}2; Mes = mesityl), [M(tmeda){Ga(DAB)}2] (M = Mn, Fe or Co) and [Cu(dppe){Ga(DAB)}] (dppe = 1,2-bis(diphenylphosphino)ethane). The majority of the complexes have been crystallographically characterized. The reactivity of the previously reported copper(I) gallyl complex, [(IPr)Cu{Ga(DAB)}] (IPr = :C{(Dip)NC(H)}2), towards a variety of unsaturated substrates has been explored. Three crystallographically characterized complexes have arisen from this phase of the study, viz. [(IPr)CuCCPh], [(IPr)Cu{Ga(DAB)}(CNBut)] and [(IPr)Cu{κ1-OC(O)C(CNHDip)(NHDip)}]. The results of these investigations show that the reactivity of [(IPr)Cu{Ga(DAB)}] is significantly different to that of related copper boryl complexes. 相似文献
3.
Matja? Kristl Brina Dojer Amalija Golobi? Miha Drofenik 《Journal of fluorine chemistry》2010,131(9):907-914
The first layered hydroxylammonium fluorometalates, (NH3OH)2CuF4 and (NH3OH)2CoF4, were prepared by the reaction of solid NH3OHF and the aqueous solution of copper or cobalt in HF. Both compounds crystallize in monoclinic, P21/c, unit cell with parameters: a = 7.9617(2) Å, b = 5.9527(2) Å, c = 5.8060(2) Å, β = 95.226(2)° for (NH3OH)2CuF4 and a = 8.1764(3) Å, b = 5.8571(2) Å, c = 5.6662(2) Å, β = 94.675(3)° for (NH3OH)2CoF4, respectively. Magnetic susceptibility was measured between 2 K and 300 K giving the effective Bohr magneton number of 2.1 for Cu and 5.2 BM for Co. At low temperatures both complexes undergo a transition to magnetically ordered phase. The thermal decomposition of both compounds was studied by TG, DSC and X-ray powder diffraction. The thermal decomposition of (NH3OH)2CuF4 is a complex process, yielding NH4CuF3 as an intermediate product and impure Cu2O as the final residue, while (NH3OH)2CoF4 decomposes in two steps, obtaining CoF2 after the first step and CoO as the final product. 相似文献
4.
A series of new palladacycloalkanes of formula cis-[PdL2(CH2)n] (9. n = 6, L = PPh3; 10. n = 6, L2 = dppe; 11. n = 8, L = PPh3; 12. n = 8, L2 = dppe) have been prepared by two routes. In the first route, the precursor bis(1-alkenyl) complexes cis-[PdL2((CH2)nCHCH2)2] (1. n = 2, L = PPh3, 2. n = 2, L2 = dppe, 3. n = 3, L = PPh3, 4. n = 3, L2 = dppe) were allowed to react with Grubb’s 2nd generation catalyst to give the palladacycloalkenes, cis-[PdL2(CH2)nCHCH(CH2)n] (5. n = 2, L = PPh3, 6. n = 2, L2 = dppe, 7. n = 3, L = PPh3, 8. n = 3, L2 = dppe), which were then hydrogenated to the palladacycloalkanes, 9-12. In the second route, the di-Grignard reagents BrMg(CH2)nMgBr (n = 6, 8) were reacted with the palladium complex [PdCl2(COD)] followed by immediate ligand displacement to form the respective palladacycloalkanes 10 and 12. The complexes obtained were characterized by a range of spectroscopic and analytical techniques. Thermal decomposition studies were carried out on the palladacycloalkanes 9-12 and the main organic products shown to be 1-alkenes and 2-alkenes. 相似文献
5.
The reaction between uranyl nitrate hexahydrate and phenolic ligand precursor [(N,N-bis(2-hydroxy-3,5-dimethylbenzyl)-4-amino-1-butanol) · HCl], H3L1 · HCl, leads to a uranyl complex [UO2(H2L1)2] (1a) and [UO2(H2L1)2] · 2CH3CN (1b). The ligand [(N,N-bis(2-hydroxy-5-tert-butyl-3-methylbenzyl)-4-amino-1-butanol)H3L2 · HCl], H3L2 · HCl, yields a uranyl complex with a formula [UO2(H2L2)2] · CH3CN (2). The ligand [(N,N-bis(2-hydroxy-3,5-dimethylbenzyl)-5-amino-1-pentanol) · HCl], H3L3 · HCl, produces a uranyl complex with a formula [UO2(H2L3)2] · 2CH3CN (3) and the ligand [(N,N-bis(2-hydroxy-5-tert-butyl-3-methylbenzyl)-5-amino-1-pentanol) · HCl], H3L4 · HCl, leads to a uranyl complex with a formula [UO2(H2L4)2] · 2CH3CN (4). The ligand [(N,N-bis(2-hydroxy-5-tert-butyl-3-methylbenzyl)-6-amino-1-hexanol) · HCl], H3L5 · HCl, leads to a uranyl complex with a formula [UO2(H2L5)2] · 4toluene (5). The complexes 1–5 are obtained using a molar ratio of 1:2 (U to L) in the presence of a base (triethylamine). The molecular structures of 1a, 1b, 3, 4 and 5 were verified by X-ray crystallography. All complexes are neutral zwitterions and have similar centrosymmetric, mononuclear, distorted octahedral uranyl structures with the four coordinating phenoxo ligands in an equatorial plane. In uranyl ion extraction studies from water to dichloromethane with ligands H3L1 · HCl–H3L5 · HCl, ligands H3L1 · HCl, H3L4 · HCl and H3L5 · HCl are the most effective ones. 相似文献
6.
A new pentacoordinated ferrous compound [TPAFeCl]+ (TPA = tris(2-pyridylmethyl)amine) was synthesized from the reaction between H3TPA(ClO4)3 and Fe(PnPr3)2Cl2 in MeCN. The unique trigonal bipyramidal [TPAFeCl]+ complex was characterized as a S = 2 high spin complex based on the crystallographic structure, magnetic susceptibility, 1H NMR spectrum and semi-empirical ZINDO/S calculations. Crystal of [TPAFeCl]2(FeCl4)(MeCN)2 was monoclinic with a = 12.019(2) Å, b = 27.550(5) Å, c = 14.138(2) Å, β = 94.168(3)°, V = 4668.9(13) Å3, space group C/c, and the unit cell contained a racemic mixture of Δ and Λ isomers with ferrous tetrachloride anion. 相似文献
7.
8.
Melita Tramšek 《Journal of fluorine chemistry》2005,126(7):1088-1094
New compounds of the type M2(H2F3)(HF2)2(AF6) with M = Ca, A = As and M = Sr, A = As, P) were isolated. Ca2(H2F3)(HF2)2(AsF6) was prepared from Ca(AsF6)2 with repeated additions of neutral anhydrous hydrogen fluoride (aHF). It crystallizes in a space group P4322 with a = 714.67(10) pm, c = 1754.8(3) pm, V = 0.8963(2) nm3 and Z = 4. Sr2(H2F3)(HF2)2(AsF6) was prepared at room temperature by dissolving SrF2 in aHF acidified with AsF5 in mole ratio SrF2:AsF5 = 2:1. It crystallizes in a space group P4322 with a = 746.00(12) pm, c = 1805.1(5) pm, V = 1.0046(4) nm3 and Z = 4. Sr2(H2F3)(HF2)2(PF6) was prepared from Sr(XeF2)n(PF6)2 in neutral aHF. It crystallizes in a space group P4122 with a = 737.0(3) pm, c = 1793.7(14) pm, V = 0.9744(9) nm3 and Z = 4. The compounds M2(H2F3)(HF2)2(AF6) gradually lose HF at room temperature in a dynamic vacuum or during being powdered for recording IR spectra or X-ray powder ray diffraction patterns. All compounds are isotypical with coordination of nine fluorine atoms around a metal center forming a distorted Archimedian antiprism with one face capped. This is the first example of the compounds in which H2F3− and HF2− anions simultaneously bridge metal centers forming close packed three-dimensional network of polymeric compounds with low solubility in aHF. The HF2− anions are asymmetric with usual F?F distances of 227.3-228.5 pm. Vibrational frequency (ν1) of HF2− is close to that in NaHF2. The anion H2F3− exhibits unusually small F?F?F angle of 95.1°-97.6° most probably as a consequence of close packed structure. 相似文献
9.
Pavel Kopel Jiří Kameníček Václav Petříček Aleš Kurečka Božena Kalinska Jerzy Mrozinski 《Polyhedron》2007
Nickel and copper complexes containing 1,3,5-benzenetricarboxylic acid, with a combination of selected N-donor ligands and Schiff bases, of the composition Ni3(bimz)6(btc)2 · 12H2O (1), Ni3(btz)9(btc)2 · 12H2O (2), Ni2(L1)(btc) · 7H2O (3), Ni3(L2)2(Hbtc) · 9H2O (4), Ni2(L3)(btc) · 4H2O (5), Cu2(L4)(btc) · 7H2O (6), [Cu3(pmdien)3(btc)](ClO4)3 · 6H2O (7) and [Cu3(mdpta)3(btc)](ClO4)3 · 4H2O (8); H3btc = 1,3,5-benzenetricarboxylic acid, bimz = benzimidazole, btz = 1,2,3-benztriazole, L1 = 2-[(phenylimino)methyl]phenol, L2 = N,N′-bis-(salicylidene)propylenediamine, L3 = 2-{[(2-nitrophenyl)methylene]amino}phenol, L4 = 2-[(4-methoxy-phenylimino)methyl]phenol, pmdien = N,N,N′,N″,N″-pentamethyldiethylenetriamine, mdpta = N,N-bis-(3-aminopropyl)methylamine, have been synthesized. The complexes have been studied by elemental analysis, IR, UV–Vis spectroscopies, magnetochemical and conductivity measurements and selected compounds also by thermal analysis. The crystal and molecular structure of complex 8 was solved. The complex is trinuclear with btc3−-bridge. The coordination polyhedron around each copper atom can be described as a distorted square with a CuON3 chromophore formed by one oxygen atom of carboxylate and three nitrogen atoms of mdpta. The magnetic properties of 8 have been studied in the 1.8–300 K temperature range revealing a very weak antiferromagnetic exchange interaction with J = −0.56 cm−1 for g = 2.13(9). The antimicrobial activities against selected strains of bacteria were evaluated. It was found that only complex 5 is able to inhibit the growth of Staphylococcus strains. 相似文献
10.
Gerry Rother Ronald Stief Ursula Bentrup Werner Massa 《Journal of fluorine chemistry》2011,132(10):740-746
Using biprotonated dabco (1,4-diazabicyclo[2.2.2]octane) or pipz (piperazine) as counter cations, mixed-ligand fluoromanganates(III) with dimeric anions could be prepared from hydrofluoric acid solutions. The crystal structures were determined by X-ray diffraction on single crystals: dabcoH2[Mn2F8(H2O)2]·2H2O (1), space group P21, Z = 2, a = 6.944(1), b = 14.689(3), c = 7.307(1) Å, β = 93.75(3)°, R1 = 0.0240; pipzH2[Mn2F8(H2O)2]·2H2O (2), space group , Z = 2, a = 6.977(1), b = 8.760(2), c = 12.584(3) Å, α = 83.79(3), β = 74.25(3), γ = 71.20(3)°, R1 = 0.0451; (dabcoH2)2[Mn2F8(H2PO4)2] (3), space group P21/n, Z = 4, a = 9.3447(4), b = 12.5208(4), c = 9.7591(6) Å, β = 94.392(8)°, R1 = 0.0280. All three compounds show dimeric anions formed by [MnF5O] octahedra (O from oxo ligands) sharing a common edge, with strongly asymmetric double fluorine bridges. In contrast to analogous dimeric anions of Al or Fe(III), the oxo ligands (H2O (1,2) or phosphate (3)) are in equatorial trans-positions within the bridging plane. The strong pseudo-Jahn-Teller effect of octahedral Mn(III) complexes is documented in a huge elongation of an octahedral axis, namely that including the long bridging Mn-F bond and the Mn-O bond. In spite of different charge of the anion in the fluoride phosphate, the octahedral geometry is almost the same as in the aqua-fluoro compounds. The strong distortion is reflected also in the ligand field spectra. 相似文献
11.
Fluorophilic ethers having the structure RC(CF3)2O(CH2)3CnF2n + 1 are obtained in high yields, when F-tert-butyl alcohol (R = CF3), F-acetone hydrate (R = O(CH2)3CnF2n + 1), F-pinacol (R = C(CF3)2O(CH2)3CnF2n + 1) are reacted with 3-perfluoroalkyl-1-propanols (CnF2n + 1(CH2)3OH, n = 4, 6, 8, 10) in a Mitsunobu reaction (Ph3P/DIAD [i-PrO2CN = NCO2Pr-i]/ether). The parent lipophilic ethers with the structure of (CF3)3CO(CH2)3CnH2n + 1 were prepared analogously using the corresponding fatty alcohols and F-tert-butyl alcohol. To achieve ideal separations, products were transferred to orthogonal phases relative to the other reaction components using fluorous extraction, fluorous solid-organic liquid filtration, or steam-distillation. Selected physical properties including melting and boiling point, together with fluorous partition coefficients of these ethers were determined and the figures obtained were qualitatively analyzed using relevant thermodynamic theories. Some of these ethers are liquids with rather low freezing points and are miscible with fluorocarbon solvents. 相似文献
12.
Qi-Ying Lv Shu-Zhong Zhan Jian-Ge Wang An Ding 《Journal of organometallic chemistry》2008,693(7):1155-1158
In the presence of CoCl2 · 6H2O, the reaction of TCNE (tetracyanoethylene) with CH3OH forms a dicyanomethylacetate molecule, which has been obtained as one solvent molecule in one new compound {[Co(bpy)2CN2][(NC)2C-CO2CH3]} · 2H2O (1). It was characterized by IR spectra, UV-Vis spectra, and cyclic voltammogram. Its structure was determined by X-ray crystallography: 1 crystallizes in P2(1)/n with a = 13.3368(17), b = 12.5299(16), c = 16.074(2) Å, α = 90, β = 94.6320(10), γ = 90°, and Z = 2. 相似文献
13.
Christopher P. Morley Christopher A. Webster 《Journal of organometallic chemistry》2006,691(20):4244-4249
Room temperature reaction of [Pd2(dba)3]/PR3 or [Pt(C2H4)(PR3)2] (dba = dibenzylideneacetone; R = Et, Bu) with the diselenides (R′Se)2 (R′ = Ph, Fc) yielded the oxidative addition products trans-[M(SeR′)2(PR3)2] (M = Pd, Pt). These have been characterised by multinuclear NMR and UV-Vis spectroscopy, mass spectrometry, and, in the cases of trans-[Pt(SePh)2(PR3)2] (R = Et, Bu) and trans-[Pt(SeFc)2(PBu3)2], also by X-ray crystallography. 相似文献
14.
Dénes Szabó 《Journal of fluorine chemistry》2006,127(11):1496-1504
(Nonafluoro-tert-butyloxy)ethyl tosylate 4 was prepared in 65% yield from nonafluoro-tert-butanol 1 using commercially available reagents. Further reaction of 4 with HNR1R2 (R1 = R2 = H, CH3; R1 = H, R2 = CH3, (CH2)3C8F17, CH2CH2OC(CF3)3) affords the appropriate (CF3)3COCH2CH2NR1R2 amines in 20-69% yields. Improved overall yields of [(CF3)3COCH2CH2]3−nNRn to 1 were obtained by the reaction of (CF3)3CONa 2 and (XCH2CH2)3−nNRn (X = Cl, n = 0, 1, 2, R = CH3; X = CH3SO2O, n = 1, R = CH3SO2) nitrogen mustards and a similar reactive β-substituted ethyl amine. The title amines are mobile colorless liquids and volatile with steam. The bulky fluorous ponytail (CF3)3CO(CH2)2 displays high acidic stability and increases fluorous character almost as much as the classical straight-chain C8F17(CH2)3 ponytail. 相似文献
15.
Jennifer Houghton Adrian C. Whitwood Sónia A. Carabineiro Maria M. Marques 《Journal of organometallic chemistry》2008,693(4):717-724
Reaction between 3-((1R,2R)-2-{[1-(3,5-di-tert-butyl-2-hydroxy-phenyl)-meth-(E)-ylidene]-amino}-cyclohexyl)-1-isopropyl-4-phenyl-3H-imidazol-1-ium bromide (1a) or the derivative 3-((1R,2R)-2-{[1-(2-hydroxy-5-nitro-phenyl)-meth-(E)-ylidene]-amino}-cyclohexyl)-1-isopropyl-4-phenyl-3H-imidazol-1-ium bromide (1b) and metal halides MClx.yTHF (M = Zr, x = 4, y = 2; M = V, x = y = 3; M = Cr, x = y = 3), in THF, at −78 °C gives the metal complexes of general formula [MClx(κ2-N,O-OC6H2R1R2C(H)N-C6H10-Im)2][Br]2 (where M = Zr, x = 2, R1 = R2 = tBu, 2; M = Zr, x = 2, R1 = H, R2 = NO2, 3; M = V, x = 1, R1 = R2 = tBu, 4; M = Cr, x = 1, R1 = R2 = tBu, 5; M = Fe, x = 0, R1 = R2 = tBu, 6; Im = 1-isopropyl-4-phenyl-3H-imidazol-1-ium-3-yl). 1H and 13C NMR spectroscopy of 2 and 3 indicate κ2-N,O-ligand coordination via the phenoxy-imine moiety with pendant imidazolium salt that is corroborated by a single crystal structure of 6. Compounds 2, 3, 4 and 5 were tested as precatalysts for ethylene polymerisation in the presence of methylaluminoxane (MAO) cocatalyst, showing low activity. Selected polymer samples were characterised by GPC showing multimodal molecular weight distributions. 相似文献
16.
A template 2:2:4 condensation of 2,6-diformyl-4-methyl-phenol, triethylenetetramine and zinc acetate gave rise to the crystallisation of [{Zn4(H4L1)(OAc)4}{Zn(OAc)3(H2O)}(OAc)] · 7H2O (1 · 7H2O), being H6L1 a macrocyclic diphenolate Schiff base ligand. Changing some operation conditions, other template reactions yielded dinuclear complexes of the type Zn2(Ln)(OAc) · xH2O, where H3Ln (n = 2, 3) are podant triphenolate Schiff base ligands derived from a 3:1 condensation of the corresponding 2,6-diformyl-4-alkyl-phenol (alkyl = Me or But, respectively) and triethylenetetramine. After recrystallisation, these two latter complexes could be X-ray characterised as Zn2(L2)(OAc) · 1.25H2O · 0.5MeCN (2 · 1.25H2O · 0.5MeCN), and Zn2(L3)(OAc) (3). Furthermore, after addition of a 3:1 molar ratio of 2-amino-4-methyl-phenol to 3, this underwent imidazolidine hydrolysis and a double imine condensation, yielding Zn2(L4)(OAc)(HOAc) · 2H2O (4 · 2H2O), where H3L4 is an acyclic pentadentate Schiff base derived from the 1:2 condensation of 2,6-diformyl-4-tert-butyl-phenol and 2-amino-4-methyl-phenol. 相似文献
17.
Luigi Busetto 《Journal of organometallic chemistry》2008,693(1):57-67
The bridging aminocarbyne complexes [Fe2{μ-CN(Me)(R)}(μ-CO)(CO)2(Cp)2][SO3CF3] (R = Me, 1a; Xyl, 1b; 4-C6H4OMe, 1c; Xyl = 2,6-Me2C6 H3) react with acrylonitrile or methyl acrylate, in the presence of Me3NO and NaH, to give the corresponding μ-allylidene complexes [Fe2{μ-η1:η3- Cα(N(Me)(R))Cβ(H)Cγ(H)(R′)}(μ-CO)(CO)(Cp)2] (R = Me, R′ = CN, 3a; R = Xyl, R′ = CN, 3b; R = 4-C6H4OMe, R′ = CN, 3c; R = Me, R′ = CO2Me, 3d; R = 4-C6H4OMe, R′ = CO2Me, 3e). Likewise, 1a reacts with styrene or diethyl maleate, under the same reaction conditions, affording the complexes [Fe2{μ-η1:η3-Cα(NMe2)Cβ(R′)Cγ(H)(R″)}(μ-CO)(CO)(Cp)2] (R′ = H, R″ = C6H5, 3f; R′ = R″ = CO2Et, 3g). The corresponding reactions of [Ru2{μ-CN(Me)(CH2Ph)}(μ-CO)(CO)2(Cp)2][SO3CF3] (1d) with acrylonitrile or methyl acrylate afford the complexes [Ru2{μ-η1:η3-Cα(N(Me)(CH2Ph))Cβ(H)Cγ(H)(R′)}(μ-CO)(CO)(Cp)2] (R′ = CN, 3h; CO2Me, 3i), respectively.The coupling reaction of olefin with the carbyne carbon is regio- and stereospecific, leading to the formation of only one isomer. C-C bond formation occurs selectively between the less substituted alkene carbon and the aminocarbyne, and the Cβ-H, Cγ-H hydrogen atoms are mutually trans.The reactions with acrylonitrile, leading to 3a-c and 3h involve, as intermediate species, the nitrile complexes [M2{μ-CN(Me)(R)}(μ-CO)(CO)(NC-CHCH2)(Cp)2][SO3CF3] (M = Fe, R = Me, 4a; M = Fe, R = Xyl, 4b; M = Fe, R = 4-C6H4OMe, 4c; M = Ru, R = CH2C6H5, 4d).Compounds 3a, 3d and 3f undergo methylation (by CH3SO3CF3) and protonation (by HSO3CF3) at the nitrogen atom, leading to the formation of the cationic complexes [Fe2{μ-η1:η3-Cα(N(Me)3)Cβ(H)Cγ(H)(R)}(μ-CO)(CO)(Cp)2][SO3CF3] (R = CN, 5a; R = CO2Me, 5b; R = C6H5, 5c) and [Fe2{μ-η1:η3-Cα(N(H)(Me)2)Cβ(H)Cγ(H)(R)}(μ-CO)(CO)(Cp)2][SO3CF3] (R = CN, 6a; R = CO2Me, 6b; R = C6H5, 6c), respectively.Complex 3a, adds the fragment [Fe(CO)2(THF)(Cp)]+, through the nitrile functionality of the bridging ligand, leading to the formation of the complex [Fe2{μ-η1:η3-Cα(NMe2)Cβ(H)Cγ(H)(CNFe(CO)2Cp)}(μ-CO)(CO)(Cp)2][SO3CF3] (9).In an analogous reaction, 3a and [Fe2{μ-CN(Me)(R)}(μ-CO)(CO)2(Cp)2][SO3CF3], in the presence of Me3NO, are assembled to give the tetrameric species [Fe2{μ-η1:η3-Cα(NMe2)Cβ(H)Cγ(H)(CN[Fe2{μ- CN(Me)(R)}(μ-CO)(CO)(Cp)2])}(μ-CO)(CO)(Cp)2][SO3CF3] (R = Me, 10a; R = Xyl, 10b; R = 4-C6H4OMe, 10c).The molecular structures of 3a and 3b have been determined by X-ray diffraction studies. 相似文献
18.
Reaction of potassium hypersilylchalcogenolates (Me3Si)3SiEK (E = S, Se, Te) with organochlorosilanes R4 − xSiClx (R = Me, Ph; x = 1-4) and methylchlorodisilanes (Si2Me5Cl, 1,2-Si2Me4Cl2) yields organosilicon hypersilylchalcogenolates [(Me3Si)3SiE]xSiR4 − x (x = 1-4) and [(Me3Si)3SiE]xSi2Me6 − x (x = 1, 2). A partial substitution product, [(Me3Si)3SiSe]2SiPhCl (2) has been obtained by reaction of PhSiCl3 with 1.5 equivalents (Me3Si)3SiSeK. Besides characterization by 1H, 13C, 29Si, 77Se and 125Te NMR spectroscopy the compounds [(Me3Si)3SiTe]2SiPh2 (1), [(Me3Si)3SiSe]2SiPhCl (2) and [(Me3Si)3SiSe]2Si2Me4(3) have also been analyzed by crystal structure analyses.Starting from (Me3Si)5Si2K treatment with sulfur gave the highly branched potassium heptasilanylthiolate (Me3Si)5Si2SK. Reactions with methylchlorosilanes Me4 − xSiClx (x = 1, 2, 3) yielded organosilicon heptasilanylthiolates [(Me3Si)3Si-(Me3Si)2Si-S]xSiMe3 − x. 相似文献
19.
To explore the anion receptor potential of [Co(phen)2(CO)3]+ for the pentafluorobenzoate ion, [Co(phen)2(CO)3](Pfbz)·6H2O (where phen = 1,10-phenanthroline and Pfbz = pentafluorobenzoate) was synthesized by reacting appropriate salts in aqueous medium. A detailed packing analysis has been undertaken to delineate the role of second sphere C-H?F interactions amid other heteroatom interactions. The complex salt has been characterized by elemental analyses, spectroscopic studies (IR, UV/Vis, multinuclear NMR) and solubility product measurement. The complex salt crystallizes in the monoclinic crystal system with space group P21/n having the cell dimensions a = 13.377(3) Å, b = 17.204(3) Å, c = 15.408(3) Å, β = 108.11(3)°, V = 3370.1(12) Å3 and Z = 4. Single crystal X-ray structure determination revealed ionic structure consisting of complex cation, [Co(phen)2(CO)3]+, Pfbz anion and six lattice water molecules. In the crystal lattice, discrete ions [Co(phen)2CO3]+ are forming rectangular voids in which the Pfbz anions are entrapped. Crystal lattice is stabilized by electrostatic forces of attraction and hydrogen bonding interactions, i.e. O-H?O, C-H?O, and C-H?F, involving second sphere coordination besides π?π interactions. 相似文献
20.
Two quinoxaline derivatives pqCH3 and pqCl (where pq stands for 2-(2′-pyridyl)quinoxaline) were prepared by condensation of 2-acetyl pyridyl with 2-amino-4-methylphenylamine or 2-amino-4-chlorophenylamine, correspondingly and were studied spectroscopically and electrochemically, in correlation with the originally reported pq. Their novel corresponded complexes namely, fac-[Re(CO)3Cl(L)] (where L = pqCH32 and pqCl 3) were synthesized, characterized, studied and compared to Re(CO)3Clpq, 1. Complex 2 crystallizes in space group C2/c with a = 20.4476(17) Å, b = 15.4521(13) Å, c = 15.2887(13) Å, β = 126.1210(11)°, Z = 8 and V = 3902.0(6) Å3. The substitution of -H by -CH3 or -Cl at 6-position of pq has a minor electronic effect on the pyridyl ring of the ligands, but seems to influence the quinoxaline moiety enough to alter the spectroscopical and electrochemical features. 相似文献