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1.
Formation and Structure of [Al_(13)(μ_3-OH)_6(μ_2-OH)_6(μ_2-OH)_(12)(H_2O)_(24)]Cl_(15)·13H_2O 总被引:1,自引:0,他引:1
1 INTRODUCTION At present, the polyaluminium compounds are mainly studied by single-crystal X-ray diffraction method to obtain the components, structures and exis- tence forms of aluminium in hydrolysis system, and then hydrolysis courses and mechanisms of each hydrolytic polyaluminium cation could be further dis- closed[1~5]. Generally, the single crystals suitable for X-ray diffraction are obtained from the crystallization of polyaluminium cations into sulfates or selenates. Following … 相似文献
2.
V. V. Tatarchuk A. P. Sergievskaya N. V. Kuratieva I. V. Korol’kov L. A. Sheludyakova S. A. Gromilov 《Journal of Structural Chemistry》2014,55(1):142-146
The crystals of the [Pd3(μ-OH)(μ-CH3COO)5] complex are obtained and characterized using powder and single crystal X-ray diffraction and IR spectroscopy. The crystal structure (a = 15.6942(6) Å, b = 11.7190(3) Å, c = 9.7871(3) Å, V = 1800.05(10) Å3, space group Pna21, Z = 4) is formed from neutral trinuclear cyclic molecules of [Pd3(μ-OH)(μ-CH3COO)5], in which the OH? group, together with five CH3COO? anions, is a bridge ligand. 相似文献
3.
A novel Mg6 cluster molecule with the formula of Mg6(
3-OH)2(
3-Br)2(-Br)8(THF)8 (1) has been isolated in 38% yield from a reaction of the Grignard reagent, 2-naphthyl-Mg-Br with BBr3 in THF. The structure of 1, determined by a single-crystal X-ray diffraction analysis, contains two Mg3 triangles linked together by two bridging bromide ligands. Within each Mg3 triangle, one hydroxide and one bromide ligand function as triply bridging ligands capping both sides of the Mg3 triangle. The coordination geometry around each Mg(II) ion is approximately octahedral. NMR studies revealed that compound 1 is highly fluxional in solution. 相似文献
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5.
A series of novel chiral complexes with ,1and ,2 coordination of organic ligands were prepared by reactions of Os3(CO)11(MeCN) and (-H)Os3(CO)10(-OH) withL--serine ethyl ester and ethanolamine. The diastereomeric cluster complexes with serine ligands were separated by crystallization or chromatography. The structures of the compounds obtained were confirmed by1H NMR and IR spectroscopy, mass-spectrometry, elemental analysis, and X-ray diffraction analysis.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 525–530, March, 1994. 相似文献
6.
Henkelis JJ Jones LF de Miranda MP Kilner CA Halcrow MA 《Inorganic chemistry》2010,49(23):11127-11132
The reaction of CuX(2) (X(-) ≠ F(-)) salts with 1 equiv of 3-pyridyl-5-tert-butylpyrazole (HL) in basic methanol yields blue solids, from which disk complexes of the type [Cu(7)(μ(3)-OH)(4)(μ-OR)(2)(μ-L)(6)](2+) and/or the cubane [Cu(4)(μ(3)-OH)(4)(HL)(4)](4+) can be isolated by recrystallization under the appropriate conditions. Two of the disk complexes have been prepared in crystalline form: [Cu(7)(μ(3)-OH)(4)(μ-OCH(2)CF(3))(2)(μ-L)(6)][BF(4)](2) (2) and [Cu(7)(μ(3)-OH)(4)(μ-OCH(3))(2)(μ-L)(6)]Cl(2)·xCH(2)Cl(2) (3·xCH(2)Cl(2)). The molecular structures of both compounds as solvated crystals can be described as [Cu?Cu(6)(μ-OH)(4)(μ-OR)(2)(μ-L)(6)](2+) (R = CH(2)CF(3) or CH(3)) adducts. The [Cu(6)(μ-OH)(4)(μ-OR)(2)(μ-L)(6)] ring is constructed of six square-pyramidal Cu ions, linked by 1,2-pyrazolido bridges from the L(-) ligands and by basal, apical-bridging hydroxy or alkoxy groups, while the central Cu ion is bound to the four metallamacrocyclic hydroxy donors in a near-regular square-planar geometry. The L(-) ligands project above and below the metal ion core, forming two bowl-shaped cavities that are fully (R = CH(2)CF(3)) or partially (R = CH(3)) occupied by the alkoxy R substituents. Variable-temperature magnetic susceptibility measurements on 2 demonstrated antiferromagnetic interactions between the Cu ions, yielding a spin-frustrated S = (1)/(2) magnetic ground state that is fully populated below around 15 K. Electrospray ionization mass spectrometry, UV/vis/near-IR, and electron paramagnetic resonance measurements imply that the heptacopper(II) disk motif is robust in organic solvents. 相似文献
7.
Jinling Li Ziwei Gao Li Han Lingxiang Gao Caiyun Zhang Wayne Tikkanen 《Journal of organometallic chemistry》2009,694(21):3444-3451
A new and facile method is presented for the synthesis of zirconocene carboxylate compounds, in which zirconocene dichloride (Cp2ZrCl2) is dissolved in 1 M aqueous HCl solution and the requisite ligand is dissolved in an organic solvent. Five such compounds [Cp2ZrCl(μ2-O′,O′′C-C6H5)] (1), [Cp2ZrCl(μ2-O′,O′′C-C6H3Cl2)] (2), [Cp2Zr(μ2-O′,O′′C-C6H3(OH)Cl)2] (3), [Cp2Zr(μ2-O′,O′′C-C6H3(OH)(NO2))2] (4), and [Cp2Zr(μ2-O′,O′′C-C6H(OH)Cl3)2] (5) have been obtained by this method. The effect of pH on the stability of Cp2ZrCl2 in 1 M HCl solution has been investigated by UV/vis spectrophotometry and 1H NMR spectrometry. The results showed that the aqueous Cp2ZrCl2 solutions became less stable with increasing pH, liberating cyclopentadiene. Accordingly, at higher pH (~7), two trinuclear zirconium monocyclopentadienyl compounds, [(CpZr)3(μ2-O′,O′′C-C6H3Cl2)3(μ3-OH)(μ2-OH)3](Cl2C6H3COO)2 (6) and [(CpZr)3(μ2-O′,O′′C-C6H4Cl)3(μ3-OH)(μ2-OH)3]Cl2·CH2Cl2 (7), were obtained. All compounds 1–7 have been characterized by FT-IR, 1H NMR spectra and elemental analysis. In all of the compounds, the aromatic acid acts as a bidentate ligand in coordinating to the zirconium; both chelating and bridging modes are observed. X-ray crystallographic studies on 1, 6, and 7 have revealed that the geometries at zirconium are distorted octahedral in 6 and 7, and distorted trigonal-bipyramidal in 1. 相似文献
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9.
Rui Yao WANG Zhe Ming WANG Song GAO Tian Zhu JIN Zhi Da CHEN Chun Hua YAN Guang Xian XU 《中国化学快报》1998,(12)
Inthepastfewyears,nearly50kindsofrareearthcomplexeswithaminoacidswerestructurallycharacterizedl.AllofthesecomplexesweresynthesizedunderpHI--4.Astheaminoacidligandsinthesecomplexesareintheirinnersaltformsandtheandnogroupsareprotonned,theycoordinatewithrareearthionsonlybyusingtheircarboxylgroups.Wehavenoticedthatthedeprotonizationoftheprotonnedaminogroupsisnecessarybeforethenitrogenatomsoftheaminogroupscancoordinatewiththemetalions.BycarefullyadjustingthePHvalueofasolutiontoabout5,wecrystalliz… 相似文献
10.
Jason K. Vohs L. Ellen Downs Jessica Stasalovich Michael Barfield Gregory H. Robinson 《Journal of Cluster Science》2002,13(4):601-608
The synthesis and molecular structures of tris(pentamethylphenyl)aluminum, (C6Me5)3Al, (I), and the magnesium cluster [Mg6(
3-OH)2(
3-Br)2(
2-Br)8(OEt2)8] (II), are reported. Both compounds were isolated from the same system. The aluminum atom in (I) resides in an almost idealized trigonal planar environment. The dihedral angles of the pentamethylphenyl rings relative to the AlC3plane in (I) are 67.2, 62.4, and 61.2°. The neutral magnesium cluster, (II), is interesting in that contains six magnesium atoms each of which resides in octahedral environments. 相似文献
11.
Ram A. Lal Arvind Kumar Ibanphylla Syiemlieh 《Journal of Coordination Chemistry》2017,70(15):2722-2735
A copper(II)–nickel(II)-based catalyst system has been synthesized and characterized by elemental analysis, molar conductance, mass spectra, magnetic moment, EPR, UV-Vis, IR spectroscopy, and cyclic voltammetry. The structure of the complex was established by X-ray crystallography. The complex is an efficient catalyst, which oxidizes primary and secondary alcohols to the corresponding aldehydes and ketones at 70 °C employing 15% H2O2 as the oxidant in the absence of a base and co-catalyst. 相似文献
12.
The trinuclear osmium carbonyl cluster, [Os3(CO)10(MeCN)2], is allowed to react with 1 equiv. of [IrCp1Cl2]2 (Cp1 = pentamethylcyclopentadiene) in refluxing dichloromethane to give two new osmium–iridium mixed-metal clusters, [Os3Ir2(Cp1)2(μ-OH)(μ-CO)2(CO)8Cl] (1) and [Os3IrCp1(μ-OH)(CO)10Cl] (2), in moderate yields. In the presence of a pyridyl ligand, [C5H3N(NH2)Br], however, the products isolated are different. Two osmium–iridium clusters with different coordination modes of the pyridyl ligand are afforded, [Os3IrCp1(μ-H)(μ-Cl)(η3,μ3-C5H2N(NH2)Br)(CO)9] (3) and [Os3IrCp1(μ-Cl)2 (η2,μ3-C5H3N(NH)Br)(CO)7] (4). All of the new compounds are characterized by conventional spectroscopic methods, and their structures are determined by single-crystal X-ray diffraction analysis. 相似文献
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14.
S. E. Nefedov E. V. Kushan M. A. Yakovleva D. G. Chikhichin G. L. Kamalov 《Russian Journal of Inorganic Chemistry》2012,57(3):358-366
A room-temperature reaction of cupric acetate dihydrate with 3,5-bis(trifluoromethyl)pyrazole ((CF3)2pzH) in chloroform in the presence of triethylamine gave a complex of the formula [Cu2(??-(CF3)2pz)2(??-OH2)(OC(Me)OHNEt3)(OH2)(HCCl3)(OOCMe)(??-OOCMe)]2 (2). Heating of this complex at 180°C in dibenzyl ether (DBE) in air yielded the tetranuclear pyrazolate-benzoate cluster Cu4(??4-OH)(??-(CF3)2pz)4(??-OOCPh)2(??-OH)2(OH2)(Et3NH)[O(CH2Ph)2]2. It was suggested that such complexes can be intermediates in the liquid-phase oxidation of DBE with atmospheric oxygen in the presence of copper complexes containing pyrazolate bridges. 相似文献
15.
Mien Wei Lum 《Journal of organometallic chemistry》2003,687(1):203-208
Reaction of the cluster Os3(μ-H)(μ-OH)(CO)10 (1) with 1-naphthol afforded the isomeric clusters 2a and 3a with the formulae Os3(μ-H)2(μ3-1-OC10H6)(CO)9. A similar reaction with 2-naphthol, however, gave Os3(μ-H)(μ-2-OC10H7)(CO)10, 4b, and the analogue of 2a. These clusters have been structurally characterised to confirm the mode of anchoring of the naphthols. 相似文献
16.
T. N. Fedotova G. G. Aleksandrov G. N. Kuznetsova 《Russian Journal of Inorganic Chemistry》2006,51(4):549-556
The diamines PtbipyCl2, and PtenCl2 and their aqua and hydroxy derivatives react with acetonitrile to give the Pt(II) acetamidates [Pt(2,2′-bipy)(NHCOCH3)2] · 4.125 H2O (I) and [enPt(μ-NHCOCH3(μ-OH)Pten](NO3)2 · H2O (II), which are characterized by X-ray diffraction. The crystals of I are triclinic, a = 7.137(10) Å, b = 12.655(3) Å, c = 21.914(6) Å, α = 81.82(2)°, β = 82.12(2)°, γ = 77.72(2)°, V = 1908.6(7) Å3, space group P $\overline 1 $ , Z = 4, R = 0.033 for 3700 reflections. Complex I is a mononuclear acetamidate with terminal (NHCOCH3)? ligands. The crystals of II are monoclinic, a = 11.413(2) Å, b = 10.981(2) Å, c = 14.385(3) Å, β = 105.90(3)°, V = 1733.8(6) Å3, space group P21/n, R = 0.028 for 2797 reflections. Complex II is a dimer with bridging (NHCOCH3)? and (OH)? groups. The Pt-Pt distance is 3.1667(7) Å. 相似文献
17.
Di-μ-hydroxo bridge-cleavage reactions between [Co(nta)(μ-OH)]2 2− and different monodentate ligands
The cleavage of the di--hydroxo bridges of [Co(nta)(-OH)]2
2– by dimethylaminopyridine (dmap) and pyridine (py) has been investigated. [Co(nta)(-OH)]2
2– equilibrates rapidly in aqueous basic solutions with a mono--hydroxo bridged CoIII species [pK
OH = 3.26(2)] and both these species react with the incoming ligand to form different ion associated species which react in the subsequent rate-determining steps (k
1 and k
2) to form presumably a ligand-substituted, mono-bridged species, [(nta)(OH)Co--OH-Co(nta)(L)]2–. Values for k
2, the preferred mono--hydroxo bridged substitution pathway for these reactions, vary between 6.8(2) × 10–4 s–1 (py) and 8.5(4) × 10–2 s–1 (dmap). 相似文献
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19.
Through reductive reaction between PhL1 and μ-S2 Fe (CO/6,tollowed by nucleophilicsubstitution of the intermediate (μ-PhS} (μ-LIS} Fe2 (CO)6 toward RX,nine Fe-S clus-ter complexes of (μ-PhS)(μ-RS)Fe2(CO)6 series have been synthesized.The influence of RX structures on the activities in nucleophilic substitution has been examined and possible steroisomers and isomer ratios of the complexes determined.In addition,the regular variations of isomer's CH3-S and CH2-S which are caused by the anisotropic effects of C-O and orientations of unshared electron pairs on sulfurs,have also been preliminarily discussed. 相似文献
20.
A binuclear tin complex [Sn_2Cl_6(μ-OH)_2(DMF)_2]·4DMF has been synthesized through direct reaction of SnCl_4·5H_2O with DMF. Its molecular and crystal structure has been determined by single X-ray diffraction technique. The crystal is triclinic with space group P1. The unit cell parameters are a=0.9153(2), b=1.0722(3), c=1.2192(3) nm, α=63.07(2), β=93.26(2), γ=65.75 (2), V=0.92821(36) nm, D_c=1.649 g·cm~(-3), Z=1, The tin atom in the complex takes six-coordinated distorted octahedral configuration with sp~3 d~2 hybrid. The two tin atoms are connected through hydroxyl bridge to form a plane at the molecular center. The four noncoordinated DMF molecules distribute symmetrically around the dimer. The whole complex has an inversion center which coincides with the gravity center of the parallelogram. 相似文献