共查询到20条相似文献,搜索用时 15 毫秒
1.
Chen J Lu SF Huang ZX Yu RM Wu QJ 《Chemistry (Weinheim an der Bergstrasse, Germany)》2001,7(9):2002-2006
Reaction of [Mo3Y(mu-S)3(dtp)4(H2O)] (Y = O, S; dtp = S2P(OC2H5)2(-)) with HgI2 gave the novel compound [[Mo3S7(dtp)3]4 x I][(HgI3)3] x 4H2O (1), which contains a [[Mo3S7(dtp)3]4 x I] tetramer and (HgI3)-. Compound 1 has been characterized by IR, Raman, UV/Vis, and NMR spectroscopy and single-crystal X-ray diffraction analysis. It is shown that this formation process can be referred to as a new cluster reaction. The structure and spectroscopic data of the tetramer is also compared with that of the related discrete cluster [Mo3S7(dtp)3 x I]. Crystal data: space group F23, a = 26.786(3) A, V = 19218.7(4) A3, Z = 4, R = 0.059. 相似文献
2.
Dietrich HM Grove H Törnroos KW Anwander R 《Journal of the American Chemical Society》2006,128(5):1458-1459
Complete donor-induced alkylaluminate cleavage of halfmetallocene complex Cp*Y(AlMe4)2, that is, treatment of Cp*Y(AlMe4)2 with 2 equiv of diethyl ether, produces [Cp*Y(mu2-Me)2]3 in high yield (95%). In contrast, the equimolar reaction of Cp*Y(AlMe4)2 with diethyl ether reproducibly formed complex [Cp*4Y4(mu2-CH3)2{(CH3)Al(mu2-CH3)2}4(mu4-CH)2] in low yield (10-30%) via a multiple C-H bond activation. The synthesis of the heterooctametallic yttrium-aluminum-methine cluster was also accomplished in moderate yield (47%) by the equimolar reaction of discrete Cp*Y(AlMe4)2 and [Cp*Y(mu2-Me)2]3 in the absence of any donor solvent and "free" AlMe3. This gives strong evidence that preformed heterometal-bridged Y-CH3-Al moieties are prone to multiple hydrogen abstraction in the presence of a highly basic reagent such as [Cp*Y(mu2-Me)2]3. The monocylopentadienyl complexes [Cp*Y(mu2-Me)2]3 and [Cp*4Y4(mu2-CH3)2{(CH3)Al(mu2-CH3)2}4(mu4-CH)2] were structurally characterized. 相似文献
3.
YU Rong-Min LU Shao-Fang HUANG Xiao-Ying HUANG Jian-QuanState Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou Fujian China 《中国化学》1997,15(2):114-122
The trimetallic cluster W2CuAgS4(TDT)2(PPh3)2-CH2Cl2 (TDT= [S2(C6H3)CH3]2-) (2) has been prepared from the reaction of the well-defined molecule building block [W2S4(TDT)2]2-(1) with AgNO3,CuBr and PPh3.The structure contains a [W2CuAgS4]4+ distorted cubane-like core.Two types of metal-metal bonds exist in the core.One is W-W bond of which length is 0.2871(1) nm,the other is W-M' (M'=Cu or Ag) bonds,whose mean distance is 0.2980 nm.The details of synthesis,structure,IR,UV-Vis and 31P NMR spectra are reported.The crystallographic data are:space group F21/n,with 0=1.6987(4),6=1.7763(6),c=1.8918(5) nm,β=98.54(2)°,V=5.645(3) nm3,Z=4,and final R=0.043 for 6437 observed reflections. 相似文献
4.
Negishi Y Kurashige W Kamimura U 《Langmuir : the ACS journal of surfaces and colloids》2011,27(20):12289-12292
We report the isolation and structural characterization of an octaneselenolate-protected Au(25) cluster ([Au(25)(SeC(8)H(17))(18)](-)). Isolated [Au(25)(SeC(8)H(17))(18)](-) was characterized by various analytical techniques. The results strongly suggest that [Au(25)(SeC(8)H(17))(18)](-) possesses a similar geometric structure to the well-studied thiolate (RS)-protected Au(25) cluster ([Au(25)(SR)(18)](-)) and that the charge transfer between the metal atoms and ligands in [Au(25)(SeC(8)H(17))(18)](-) is lower than that in [Au(25)(SR)(18)](-). To the best of our knowledge, this is the first report of the isolation of a selenolate-protected gold cluster. [Au(25)(SeC(8)H(17))(18)](-) is an ideal compound for determining how changing the ligand from thiolate to selenolate affects the fundamental properties of a cluster. 相似文献
5.
《Journal of Coordination Chemistry》2012,65(15):2669-2678
Three reduced molybdenum(V) phosphates, Na2[H2DaHex]4.5[H3O]{Mn[Mo6O12(OH)3(HPO4)2(PO4)2]2}·2H2O (1), [H2DaHex]4[Zn(H2O)]2{Zn[Mo6O12(OH)3(HPO4)2(PO4)2]2}·6H2O (2), and [H2DaHex]3.5[Cd(H2O)2]1.5[Cd(H2O)]{Cd[Mo6O12(OH)3(HPO4)2(PO4)2]2}·3.5H2O (3) (DaHex?=?1,6-diaminylhexane), were hydrothermally synthesized by using the same organic template (DaHex) and characterized by elemental analysis, IR, TGA, powder XRD, and single-crystal X-ray diffraction. Crystallographic analysis reveals that the compounds contain M[P4Mo6]2 (M?=?Mn for 1, Zn for 2, Cd for 3) polyanions, which are further connected by various metal ions to form different topological structures. In 1, the cluster anion Mn[P4Mo6]2 is discrete. For 2 and 3, M[P4Mo6]2 (Zn for 2, Cd for 3) clusters are linked by transition metal ions to form different infinite chains. Then, all the 1-D chains are further packed into 3-D supramolecular structures via hydrogen-bonding interactions. The formations of 1, 2, and 3 demonstrate that not only organic templates, but transition metal ions also play very important roles in the M-P4Mo6 system. 相似文献
6.
Hebden TJ Denney MC Pons V Piccoli PM Koetzle TF Schultz AJ Kaminsky W Goldberg KI Heinekey DM 《Journal of the American Chemical Society》2008,130(32):10812-10820
Reaction of NaBH4 with (tBuPOCOP)IrHCl affords the previously reported complex (tBuPOCOP)IrH2(BH3) (1) (tBuPOCOP = kappa(3)-C6H3-1,3-[OP(tBu)2]2). The structure of 1 determined from neutron diffraction data contains a B-H sigma-bond to iridium with an elongated B-H bond distance of 1.45(5) A. Compound 1 crystallizes in the space group P1 (Z = 2) with a = 8.262 (5) A, b = 12.264 (5) A, c = 13.394 (4) A, and V = 1256.2 (1) A(3) (30 K). Complex 1 can also be prepared by reaction of BH3 x THF with (tBuPOCOP)IrH2. Reaction of (tBuPOCOP)IrH2 with pinacol borane gave initially complex 2, which is assigned a structure analogous to that of 1 based on spectroscopic measurements. Complex 2 evolves H2 at room temperature leading to the borane complex 3, which is formed cleanly when 2 is subjected to dynamic vacuum. The structure of 3 has been determined by X-ray diffraction and consists of the (tBuPOCOP)Ir core with a sigma-bound pinacol borane ligand in an approximately square planar complex. Compound 3 crystallizes in the space group C2/c (Z = 4) with a = 41.2238 (2) A, b = 11.1233 (2) A, c = 14.6122 (3) A, and V = 6700.21 (19) A(3) (130 K). Reaction of (tBuPOCOP)IrH2 with 9-borobicyclononane (9-BBN) affords complex 4. Complex 4 displays (1)H NMR resonances analogous to 1 and exists in equilibrium with (tBuPOCOP)IrH2 in THF solutions. 相似文献
7.
WJ Gee JG Maclellan CM Forsyth B Moubaraki KS Murray PC Andrews PC Junk 《Inorganic chemistry》2012,51(16):8661-8663
Sequestration of peroxide derived from molecular oxygen has resulted in the templated synthesis of a terbium picolinate cluster, isolated as a 2D sodiated network in the solid state. This first example of an air-stable rare-earth peroxide cluster represents key evidence for a peroxide-containing intermediate in rare-earth-cluster-catalyzed oxidation reactions. Luminescent and magnetic properties have also been investigated. 相似文献
8.
L. Bourget P. Hubert Mutin A. Vioux J. M. Frances 《Journal of polymer science. Part A, Polymer chemistry》1998,36(13):2415-2425
Low-viscosity, methoxylated polysiloxane resins incorporating Me2SiO2/2 (D) and SiO4/2 (Q) units were prepared using nonhydrolytic condensation between Si—Cl and Si—OMe groups with the formation of MeCl, catalyzed by a Lewis acid. With the commonly used catalysts, condensation between two Si—OMe groups, with formation of Me2O, also took place to a large extent, hindering the control of the degree of condensation of the resins. Several catalysts were tested by monitoring the formation of MeCl and Me2O using sealed NMR tubes and 1H-NMR spectroscopy. The best compromise between reactivity and selectivity was obtained with ZrCl4. Resins with various compositions were prepared in the absence of solvent by condensation between Me2SiCl2 and Si(OMe)4 at 130°C, catalyzed by 1 mol % ZrCl4. They were characterized using viscosimetry, gas chromatography coupled with mass-spectrometry (GC-MS), and quantitative 29Si-NMR spectroscopy. The resins consisted of a complicated mixture of oligomers, linear or branched (n > 1) and cyclic (n > 3), with a high degree of D/Q bonding. The distribution of Si—OMe and Si—OSi bonds and the bonding between D and Q units were found to be nearly random. This was ascribed to the occurrence of Si—OSi/Si—OMe and Si—OSi/Si—OSi redistribution reactions that reached equilibrium during the synthesis. © 1998 John Wiley & Sons, Inc. J. Polym. Sci. A Polym. Chem. 36: 2415–2425, 1998 相似文献
9.
Mixed guanidinato/alkylimido/azido tungsten(VI) complexes: synthesis and structural characterization
A series of structurally characterized new examples of pentacoordinated heteroleptic tungsten(VI)-guanidinates complexes are described. Starting out from [WCl(2)(Nt-Bu)(2)py(2)] (1) (py = pyridine) and the guanidinato transfer reagents (TMEDA)Li[(Ni-Pr)(2)CNi-Pr(2)] (2a) (TMEDA = N,N,N',N'-tetramethylethylendiamine) and [Li(NC(NMe(2))(2))](x) (2b), the title compounds [WCl(Nt-Bu)(2)[(Ni-Pr)(2)CNi-Pr(2)]] (3) and [W(Nt-Bu)(2)Cl{NC(NMe(2))(2)]](2) (6) were selectively formed by the elimination of one mole equivalent of lithium chloride. The isopropyl-substituted guanidinato ligand [(Ni-Pr)(2)CNi-Pr(2)} of monomeric 3 is N(1),N(3)-bonded to the tungsten center. The introduction of the sterically less-demanding tetramethyl guanidinato ligand [NC(NMe(2))(2)] expectedly leads to dimeric 6 exhibiting a planar W(2)N(2) ring with the guanidinato group bridging the two tungsten centers via the deprotonated imino N-atom. The remaining chloro ligand of 3 is labile and can be substituted by sterically less-crowded groups such as dimethylamido or azido that yield the presumably monomeric compounds 4 and 5, respectively. A similar treatment of 6 with sodium azide yields the dimeric azido derivative 7. Reacting [WCl(2)(Nt-Bu)(2)py(2)] directly with an excess of sodium azide leads to the dimeric bis-azide species [[W(Nt-Bu)(2)(N(3))(mu(2)-N(3))py](2)]. The new compounds were fully characterized by single-crystal X-ray diffractometry (except 2, 4, and 5), NMR, IR, and mass-spectroscopy as well as elemental analysis. Compound 5, [W(N(3))(Nt-Bu)(2)[(Ni-Pr)(2)CNi-Pr(2)]], can be sublimed at 80 degrees C, 1 Pa. 相似文献
10.
Ying-Hua Sun Ji-Qing Xu Ling Ye Xiao-Bing Cui Yong Li Hai-Hui Yu Guang-Hua Li Guang-Di Yang Yan Chen 《Journal of Molecular Structure》2005,740(1-3):193-201
Two new interesting polyoxometalate derivatives 1 and 2 constructed of modified metal–oxo cluster ions carrying positive and negative changes, respectively, was hydrothermally prepared and structurally characterized by IR, ESR, XPS, elemental analysis and X-ray crystallography. The result of structure determination shows that compound 1 and 2 are isostructural and both contain polyoxocation and polyoxoanion, and both cation and anion are built on mixed Mo–V tetra-capped pseudo-Keggin units with P centre, [Mo8V8O40(PO4)]n−, bonded to four or two [Ni(2,2′-bipy)2H2O]2+ complexes, respectively, via terminal oxygen of the capping V atoms. Magnetism measurement indicates that there exists antiferromagnetic interaction in complex 1 and 2. 相似文献
11.
12.
The synthesis of cyclic thiolactones, 2,5,8-trithiacyclododecane-1,9-dione (4), 2,5,8,14,17,20-hexathiacyclotetracosane-1,9,13,21-tetraone (5), 2,5,8-trithiacyclotetradecane-1,9-dione (6) and 2,5,8,16,19,22-hexathiacyclooctacosane-1,9,15,23-tetraone (7) was achieved by tin-template reaction of 2,2-dibutyl-2-stanna-1,3,6-trithiacyclooctane (1) with corresponding diacyl chlorides. The structures of 12-, 14-, 24- and 28-membered ring systems of 4, 6, 5, and 7, respectively, were investigated by X-ray structure analysis. These investigations revealed that, in the solid-state, thiolactones 4 and 7 form tubular assemblies. However, the crystal structure of 5 forms layered packing dominated by CH?O hydrogen bonds whereas 6 forms three-dimensional network via CH?O hydrogen bonds and van der Waals interactions. 相似文献
13.
Filipe A. Almeida Paz 《Journal of solid state chemistry》2004,177(10):3423-3432
A three-dimensional diamondoid cadmium-organic framework, formulated as [Cd(NDC)(H2O)] (I) (where NDC2−=2,6-naphtalenedicarboxylate), has been hydrothermally synthesized and structurally characterized using single-crystal X-ray diffraction. The hydrothermal synthesis of I has been optimized by modifying the composition of the reactive mixture and the temperature programme, so that a highly crystalline and pure homogeneous phase could be obtained. A novel layered structure, formulated as [Cd2(NDC)(OH)2], was isolated when the molar ratio of triethylamine exceeds ca. 0.7. Both products have been characterized using powder X-ray diffraction, IR and Raman spectroscopies, and elemental and thermal analyses. 相似文献
14.
The reaction of (NBu(4))(2)[Pt(C triple bond CPh)(4)] with Cd(ClO(4))(2).6H(2)O in a 1:1 molar ratio yields a white solid [PtCd(C triple bond CPh)(4)](n) 1 (75% yield) together with yellow crystals of a very unusual decanuclear platinum-cadmium cluster [Pt(4)Cd(6)(C triple bond CPh)(4)(mu-C triple bond CPh)(12)(mu(3)-OH)(4)] 2 in low yield. Slow diffusion of acetonic solutions of the starting materials under aerobic conditions only produces crystals of 2 which have been shown by an X-ray analysis to be composed of a big hexanuclear cation [Cd(6)(mu(3)-OH)(4)](8+) and four [Pt(C triple bond CPh)(4)](2-) anions, held together by Pt.Cd and pi.Cd acetylide interactions. On the other hand, treatment of the insoluble product 1 with 1 equiv of NBu(4)X yields tetranuclear mixed-metal soluble complexes (NBu(4))(2)[[Pt(mu-C triple bond CPh)(4)](2)(CdX)(2)] (X = Cl A, Br 3, CN 4), which contain two platinate fragments connected by two CdX units through Pt.Cd and mainly Cd.C(alpha) interactions. All complexes are strongly emissive in the solid state at room temperature. 相似文献
15.
Protasiewyck GM Nunes FS 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2006,65(3-4):549-552
Herein we describe the synthesis and spectroscopic (infrared and UV-vis) analysis of [Cu(II)(dohpn)(L)](n+) (dohpn=imineoximic tetraazamacrocyclic ligand 2,3,9,10-tetramethyl-1,4,8,11-tetraazaundecane-1,3,8,10-tetraen-11-ol-1-olate) and L=SCN(-), I(-), Cl(-) (n=0) and 4-aminopyridine (ampy), 4,4'-bipyridine (bipy), imidazole (im), 2-aminopyrazine (ampz) and water (n=1+). The following order of the Jahn-Teller stabilization energy (cm(-1)) was observed: I(-)(6452)相似文献
16.
The reaction of Ru3(CO)12 with 3,3 dimethylthietane (DMT) at 68°C yielded the new tetraruthenium cluster complex Ru4(CO)12(-SCH2CMe2CH2)2,1 in 23% yield. Compound1 was characterized crystallographically and was shown to consist of a puckered square of four ruthenium atoms with two DMT ligands bridging opposite sides of the cluster via the sulfur atoms. Compound1 reacts with CO (98°C/1 atm) to yield the new tetraruthenium complex Ru4(CO)13 (-SCH2CMe2CH2),2 in 69% yield. Compound2 consists of a butterfly tetrahedral cluster of four ruthenium atoms with a DMT ligand bridging the wing-tip metal atoms. Addition of DMT to2 regenerates1 in 67% yield. Crystal data—1: space group =
,a=17.490(2) Å,b=18.899(3) Å,c=9.781(1) Å, =93.06(1)°, =91.06(1)°, =105.239(9)°,Z=4, 5799 reflections,R=0.026; for2: space group = P21/n,a=15.430(3) Å,b=18.285(4) Å,c=9.850(2) Å, =90.05(2)°,Z=4, 2111 reflections,R=0.036. 相似文献
17.
G. L. Zhang L. Ran X. Q. Luo R. G. Hu J. Zeng 《Russian Journal of Coordination Chemistry》2013,39(11):792-797
A new bimetallic cluster complex with the formular {[Cu(Phen)2]2V4O12} · MeOH · 5H2O has been synthesized and structurally characterized by elemental analyses, IR spectrum, and single crystal X-ray diffraction. The heterobimetallic cluster complex is composed of a discrete V4O 12 4? cluster covalently attached to two [Cu(Phen)2] 2 2+ fragments. The nonclassical hydrogen bonds and π-π stacking contribute to the formation of the three-dimensional supramolecular structure. Microdilution broth method indicated that the complex showed significant activity against B. subtilis, S. aureus, and E. coli. 相似文献
18.
The reaction of Pt2Os4(CO)18 (1) with H2 in refluxing octane (125°C) yielded the new compound Pt5Os6(CO)25 (2), 58%. Compound 2 was characterized by IR, elemental and single crystal X-ray diffraction analyses. Compound 2 contains 11 metal atoms. five platinum, and six osmium. The cluster can be viewed as two fused trigonal bipyramidal clusters that share one platinum vertex. These two clusters are also joined by three metal-metal bonds, and Os(CO)4 groups bridge two of these three metal-metal bonds. Crystal data for 2·CH2Cl2: space group itP1¯ma=12.250(1) Å,b=17.476(4) Å,c=11.89(2) Å,=109.87(1)°,=112.66(1)°,=83.05(2)°,Z=2, 2986 reflections,R=0.033. 相似文献
19.
20.
Antonio Aronne Elisa Marenna Valeria Califano Esther Fanelli Pasquale Pernice Marco Trifuoggi Alessandro Vergara 《Journal of Sol-Gel Science and Technology》2007,43(2):193-204
(Nb2O5)
x
·(SiO2)1−x
gels of four different compositions with x = 0.025 (2.5Nb), 0.050 (5Nb), 0,10 (10Nb) and 0.20 (20Nb) were synthesized at room temperature from niobium penta-chloride
and tetra-ethoxysilane and their structural evolution with the temperature was examined by X-ray diffraction, thermogravimetry/differential
thermal analysis, Raman and IR spectroscopy (Fourier transform). The synthesis procedure tuned in this work allowed to obtain
for each studied composition transparent chemical gels in which the niobium dispersion resulted to be strongly dependent on
the Nb2O5 loading: it was on the atomic scale for the 2.5Nb and 5Nb gel samples whereas the gel structure of the 10Nb and 20Nb appears
formed by phase separated niobia-silica nanodomains. All dried gels keep their amorphous nature up to 873 K, while at higher
temperatures crystallization of T- and H-Nb2O5 polymorphs were observed according to the Nb2O5 loading: at low loading T-Nb2O5 was the main crystallising phase, whereas at higher one the H-Nb2O5 prevails. Particularly, T-Nb2O5 was the sole crystallising phase in the whole explored temperature range for the 2.5Nb, keeping its nanosize up to 1273 K
for all samples except for the 20Nb. 相似文献