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1.
A new polymer azido-bridged copper(II) complex [Cu4(En)2(μ1,1-N3)4(μ1,1,1-N3)2(μ1,3-N3)2]
n
(I) (En = ethylenediamine) has been synthesized and crystallography characterized. Complex I shows one-dimensional coordination polymeric structure based on a tetranuclear cluster unit [Cu4(En)2(μ1,1-N3)4(μ1,1,1-N3)2(μ1,3-N3)2], in which the azido ions display three different bridging modes. 相似文献
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C. Sivasankar 《Journal of organometallic chemistry》2004,689(16):2726-2732
The reaction of [Cu3(dppm)3(μ3-OH)](ClO4)2 (1) with heterocumulenes (XCS; X = NPh, NMe and S) has been studied. The μ3-OH ligand inserts into PhNCS and MeNCS only in the presence of methanol. Insertion products are formed in accord with earlier observations made with copper(I)-aryloxides. On heating, the insertion products convert to a S bridged cluster [Cu4(dppm)4(μ4-S)](ClO4)2 (8), having a tetrameric core. However, in the reaction with CS2, 1 is converted to 8 even at room temperature in the presence of methanol. On the other hand, the dimeric complex [Cu2(dppm)2(CH3CN)4](ClO4)2, reacts with CS2 to give (diphenylphosphinomethyl)-diphenylphosphine sulfide, Ph2P-CH2-P(S)Ph2 (dppmS), which forms the complex [Cu(dppmS)2]ClO4 (9). A single crystal X-ray crystallographic study of 9, the first copper(I) complex of dppmS has been taken up to confirm the mono-oxidation of the dppm ligand and the nuclearity of the complex. Reactions of complex 1 with heterocumulenes and with elemental sulfur, are compared. 相似文献
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Reactions of [(dtc)2Mo2(S)2(μ-S)2] with one or two equivalents of CuBr in CH2Cl2 afforded two new heterobimetallic sulfide clusters, [(dtc)2Mo2(μ3-S)(μ-S)3(CuBr)] (1) and [(dtc)2Mo2(μ3-S)4(CuBr)2] (2). Both compounds were characterized by elemental analysis, IR, UV-vis and X-ray analysis. Compound 1 contains a butterfly-shaped Mo2S4Cu core in which one CuBr unit is coordinated by one bridging S and two terminal S atoms of the [(dtc)2Mo2(S)2(μ-S)2] moiety. In the structure of 2, one [(dtc)2Mo2(S)2(μ-S)2] moiety and two CuBr units are held together by six Cu-μ3-S bonds, forming a cubane-like Mo2S4Cu2 core. 相似文献
6.
P. A. Abramov M. N. Sokolov A. V. Virovets V. P. Fedin 《Journal of Structural Chemistry》2009,50(1):162-165
The crystal structure of [(C5Me4Et)3Rh3(μ3-Se)2](PF6)2 and [(C5Me4Et)2Rh2(μ2-Cl)3]PF6, obtained in the reaction of [(C5Me4Et)Rh(C6H6)](PF6)2 with ZnSe in 4M HCl under hydrothermal conditions, is determined. In agreement with the 18VE rule, the triangular cluster
contains single metal-metal bonds (Rh-Rh 2.864(1) ?), whereas they are absent in the binuclear complex (Rh ...Rh 3,216(1)
?).
Original Russian Text Copyright ? 2009 by P. A. Abramov, M. N. Sokolov, A. V. Virovets, and V. P. Fedin
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 1, pp. 169–172, January–February, 2009. 相似文献
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Bojan Kozlevčar Lea Glažar Gordana Pirc Zvonko Jagličić Amalija Golobič Primož Šegedin 《Polyhedron》2007
Two novel polynuclear complexes with methanoate anions and 3-hydroxypyridine ligands [Cu(μ-HCO2)2(3-pyOH)]n (1) and [Cu2(μ-HCO2)2(μ-3-pyOH)2(3-pyOH)2(HCO2)2]n (2), respectively, were synthesized and characterized. The central copper atom in 1 is surrounded by four methanoates and a 3-pyOH molecule, forming a square-pyramidal CuO3NO chromophore. All the methanoates are bidentate and serve as bridges between the adjacent copper ions via syn-anti and anti–anti coordination. The basal square coordination axes are formed by O(syn), N(3-pyOH) (1.974(2), 2.016(2) Å) and O(anti), O(anti) (1.945(2), 1.960(2) Å), while the third O(anti) (2.247(2) Å) is on the top of the pyramid. A ferromagnetic transition with an exchange constant 2J/kB = 9.2 cm−1 is found for 1 below 20 K. This interaction probably takes place through two syn-anti methanoates extended in a chain through the 2D structure. On the other hand, two monoatomic Cu–O–Cu intra-dinuclear asymmetric (1.986(2), 2.415(2) Å) bridges of two methanoates in [Cu2(HCO2)4(3-pyOH)4] (2) are present. An elongated distorted octahedral coordination sphere around each copper(II) atom is completed by an additional monodentate terminal methanoate (1.975(2) Å), two N-coordinated 3-pyOH (2.005(2), 2.002(2) Å) and the third weakly O-coordinated 3-pyOH (2.732(2) Å). Although a shorter Cu?Cu distance is noticed in 2 than in 1 (4.690(1) Å 1, 3.442(1) Å 2), much weaker ferromagnetism is found in 2. 相似文献
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Van An Du Gregor N. Stipicic Maria Bendova Ulrich Schubert 《Monatshefte für Chemie / Chemical Monthly》2010,10(2):671-675
Abstract
Thermolysis of cis-Fe(CO)4(SiCl3)2 results in the formation of the novel compound Fe2(CO)6(μ2-SiCl2)3, which was characterized by single crystal X-ray diffraction. Density functional theory calculations were carried out to elucidate possible reaction steps leading to the formation of Fe2(CO)6(SiCl2)3, including CO dissociation and chlorine abstraction by a SiCl3 radical generated from homolytic Fe–Si bond cleavage involving a singlet–triplet intersystem crossing. 相似文献11.
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Michael I. Bruce Paul A. Humphrey Allan H. White 《Journal of organometallic chemistry》2004,689(15):2558-2561
The reaction between AuMe(PPh3) and Ru3(μ-H)3(μ3-CBr)(CO)9 (1) affords the novel heptanuclear cluster Au4Ru3(μ3-CMe)(Br)(CO)9(PPh3)3 (2), containing an Au/Ru3/Au trigonal pyramidal cluster face-capped by two Au(PPh3) groups and a CMe ligand, together with Au2Ru3(μ-H)(μ3-CMe)(CO)9(PPh3)2 (3), formed by isolobal replacement of two of the three μ-H atoms in 1 by Au(PPh3) groups. The latter co-crystallises with the analogous μ3-CH complex, as also shown spectroscopically. 相似文献
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Nicola E. Cameron William Henderson Brian K. Nicholson 《Journal of organometallic chemistry》2008,693(25):3711-3714
Reaction of the metalloligand [Pt2(μ-S)2(PPh3)4] with 0.5 mol equivalents of durene-1,4-bis(mercuric acetate) [AcOHgC6Me4HgOAc] in methanol gives the polynuclear complex [{Pt2(μ-S)2(PPh3)4}2(μ-1,4-C6Me4Hg2)]2+, isolated as its and salts. Positive-ion ESI mass spectra indicate that [{Pt2(μ-S)2(PPh3)4}2(μ-1,4-C6Me4Hg2)]2+ undergoes fragmentation by successive loss of PPh3 ligands, while the ESI mass spectrum of the salt showed additional ions [Pt2(μ-S)2(PPh3)4(HgC6Me4HgPh)]+ and [Pt2(μ-S)2(PPh3)4HgPh]+ as a result of phenyl transfer from to Hg. A single-crystal X-ray structure determination on [{Pt2(μ-S)2(PPh3)4}2(μ-1,4-C6Me4Hg2)](BPh4)2 shows that the cation crystallises on a centre of symmetry, with structural features that are comparable to those of the previously characterised complex [Pt2(μ-S)2(PPh3)4HgPh]BPh4. 相似文献
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I. V. Anan’ev M. A. Yakovleva E. V. Perova S. E. Nefedov 《Russian Journal of Inorganic Chemistry》2010,55(7):1057-1063
The product of the thermal reaction between cobalt acetate hydrate and benzoic acid reacts with a triethylamine excess to
form the trinuclear complex Co3(μ-OOCPh)4(μ,η2-OOCPh)2[OC(Ph)OHNEt3]2, and its reaction with 3,5-dimethylpyrazole yields the mononuclear complex Co(Hdmpz)2(OOCPh)2. The compound structures are discussed on the basis of X-ray crystallographic data. 相似文献
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Maxim N. Sokolov Artyom L. Gushchin Dmitrii Yu. Naumov Olga A. Gerasko Vladimir P. Fedin 《Journal of Cluster Science》2005,16(3):309-318
Mechanochemical reaction of cluster coordination polymers
(Q=S, Se) with solid
leads to the cluster core excision with the formation of anionic complexes
. Extraction of the reaction mixture with water followed by crystallization gives crystalline
(main product) and
(1) (minor product). In the case of the Se cluster, the
complex could not be isolated, and the treatment of the aqueous extract with PPh3 gave
(2) in a low yield. Alternatively, it was obtained from
and
in high yield. Both 1 and 2 were characterized by X-ray structure analysis.
Dedicated to Academician I. I. Moiseev on the occasion of his 75th birthday and in recognition of his outstanding contribution
to cluster chemistry. 相似文献
16.
Chao Xu Jing-Jing Zhang Taike Duan Quan Chen Qian-Feng Zhang 《Journal of Cluster Science》2010,21(4):813-823
Abstract
Reaction of the [Me4N]2[Cd(SPh-4-Me)4] with two equivalents of [M(PPh3)2NO3] afforded the neutral linear trinuclear complexes [Cd(μ-SPh-4-Me)4{M(PPh3)2}2] (M = Cu 1, Ag 2) in which two [M(PPh3)2]+ fragments chelate with the opposite edges of a tetrahedral [Cd(SPh-4-Me)4]2− moiety via the sulfur atoms of the Me-4-PhS− species. Treatment of [Sn(SPh)4] with two equivalents of [Ag(PPh3)2NO3] gave the neutral linear trinuclear complex [Sn(μ-SPh)6(AgPPh3)2] (3) that is composed of a central distorted SnS6 octahedron sharing two opposite planes with two slightly distorted AgS3P tetrahedrons. Complexes 2 and 3 are air and optically stable. Their nonlinear optical absorption and refraction were investigated under the same conditions. The nonlinear optical absorption and refraction of complex 2 were determined to be α 2 = 3.11 × 10−11 m/W and n 2 = 4.15 × 10−12 esu, respectively. The nonlinear optical absorption and refraction of complex 3 were determined to be α 2 = 8.36 × 10−11 m/W and n 2 = 1.47 × 10−11 esu, respectively. 相似文献17.
T. Yu. Glazunova A. I. Boltalin S. I. Troyanov 《Russian Journal of Coordination Chemistry》2005,31(4):247-252
Novel anhydrous trinuclear 3-oxo complexes of Cr(III), Cr3(3-O)(CF3COO)6(CH3COOH)2(CF3COO) (I) and of Cr(III,III,II), Cr3(3-O)(CF3COO)6(CH3COOH)2(THF) (II) (where THF is (CH2)4O) are synthesized by anodic dissolution of metallic chromium in solutions of trifluoroacetic acid in acetonitrile and in tetrahydrofuran and their structures are studied by X-ray diffraction analysis. Complex I forms orthorhombic crystals with space group Pna21, a = 9.778(1) , b = 16.042(2) , c = 22.851(4) , Z = 4, R
1 = 0.0332; complex II crystallizes in monoclinic system: space group P21/c, a = 9.866(1) , b = 17.895(2) , c = 21.167(4) , = 100.75(2)°, Z = 4, R = 0.0422. The average Cr-(3-O) distances in compounds I and II are almost equal (1.943(3) and 1.927(3) ). An average length of the Cr-O bond in octahedral surrounding of metal atoms is different in complexes I and II (1.985(4) and 2.003(3) , respectively), which is specified by different oxidation states of the metal atom. The CrCr distances lie in an interval of 3.366(1)–3.337(1) .__________Translated from Koordinatsionnaya Khimiya, Vol. 31, No. 4, 2005, pp. 266–272.Original Russian Text Copyright © 2005 by Glazunova, Boltalin, Troyanov. 相似文献
18.
The compounds [{VO(O2)2(NH3)}2{μ-Cu(NH3)4}] (1) and [Zn(NH3)4][VO(O2)2(NH3)]2 (2) were prepared and characterized by elemental analysis and infrared spectra. The single crystal X-ray study revealed that the structure of 1 consists of trinuclear complex molecules [(NH3)OV(O2)2{μ-Cu(NH3)4}(O2)2VO(NH3)] with a rare heterobimetalic peroxo bridge: copper(II)–peroxo ligand–vanadium(V). The structure of 2 is composed of tetraamminezinc(II) cations and ammineoxodiperoxovanadate(V) anions. In course of thermal decomposition of 1 performed up to 620 °C, the following intermediate products: [Cu(NH3)2(VO3)2], and subsequently a mixture of V2O5 with monoclinic β-Cu2V2O7, were gradually formed. The final product of decomposition is Cu(VO3)2. The thermal decomposition of 2 is a two-step process. In the first stage, [Zn(NH3)3(VO3)2] as supposed intermediate was formed, which transformed at higher temperatures by release of ammonia molecules to the monoclinic modification of Zn(VO3)2. 相似文献
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I. V. Medrish A. V. Virovets E. V. Peresypkina L. B. Serezhkina 《Russian Journal of Inorganic Chemistry》2008,53(7):1034-1039
Single crystals of Cs4[(UO2)2(C2O4)(SO4)2(NCS)2] · 4H2O (I) and (NH4)4[(UO2)2(C2O4)(SO4)2(NCS)2] · 6H2O (II) have been synthesized and studied by X-ray diffraction. The crystals of both compounds are orthorhombic with the space group
Pbam, Z = 2, and unit cell parameters a = 12.0177(3) ?, b = 18.6182(5) ?, c = 6.7573(10) ?, R = 0.0376 (I); a = 11.6539(9) ?, b = 18.3791(13) ?, c = 6.7216(5) ?, R = 0.0179 (II). The main structural units of crystals I and II are [(UO2)2(C2O4)(SO4)2(NCS)2]4− chains belonging to the crystal-chemical group A2K02B22M21 (A = UO22+, K02 = C2O42−, B2 = SO42−, M1 = NCS−) of the uranyl complexes. The uranium-containing chains are joined into a three-dimensional framework due to a system of
electrostatic interactions with the cesium or ammonium ions in the structure of I. In the structure of II, this framework is additionally stabilized by hydrogen bonds involving the outer-sphere water molecules and ammonium ions.
Original Russian Text ? I.V. Medrish, A.V. Virovets, E.V. Peresypkina, L.B. Serezhkina, 2008, published in Zhurnal Neorganicheskoi
Khimii, 2008, Vol. 53, No. 7, pp. 1115–1120. 相似文献
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The mixed-valence manganese(Ⅲ/Ⅳ) complex [Mn2(cyclen)2(μ-O)2](ClO4)3-4H2O (1) (cyclen=1,4,7,10-tetraazacyclododecan) with chemical formula C16H48Cl3Mn2N8O18 has been synthesized and characterized by single crystal X-ray diffraction analysis, elemental analysis, IR and electronic spectra. The results showed that the manganese(Ⅲ/Ⅳ) ions were six-coordinated by four nitrogen atoms from cyclen and two oxygen atoms from the oxygen bridge, forming a distorted octahedron geometry. There were two very strong peaks in the range of 400-700 nm in electronic spectrum, which was similar to Mn catalase and Mn ribonucleotide reductase extracted from organisms.Electrochemical study indicated that the complex underwent a quasi-reversible one-electron reduction and oxidation at E1/2=0.827 V in acetonitrile. 相似文献