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Synthesis and Crystal Structure Determination of Lead(II) Oxide Halide Alcoholates with Different Connectivity of Pb4O4 Heterocubane‐like Subunits The reaction of red lead(II) oxide (Litharge) and lead(II) halide (Cl? and Br?) with diethylene glycole at a temperature of 180 °C leads to the isotypic compounds [Pb6(C4H8O3)O2Cl6] (1) and [Pb6(C4H8O3)O2Br6] (2) . In a similar synthesis with PbI2 as educt at temperature of 160 °C the two modifications β‐[Pb6(C4H8O3)O2I6] (3) and α‐[Pb6(C4H8O3)O2I6] (4) were found, whereas at a reaction temperature of 180 °C [Pb9(C2H4O2)(C4H8O3)O3I8] (5) was surprisingly obtained as product. The X‐ray diffraction data show that at a temperature of 180 °C a splitting of the ether took place. The cited compounds show cubane like subunits built by lead and oxygen atoms. These fragments are connected by alkoholate molecules. In 5 additionally an I6 octahedra centered by lead is observed. 相似文献
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Ulrike Riese Naim Faza Werner Massa Klaus Harms Thees Breyhan Paul Knochel Jürgen Ensling Vadim Ksenofontov Philipp Gütlich Kurt Dehnicke 《无机化学与普通化学杂志》1999,625(9):1494-1499
The phosphoraneiminato complexes [MnBr(NPEt3)]4 ( 1 ) and [M4Br5{NP(NMe2)3}3] with M = Mn ( 2 ) and M = Co ( 3 ) are prepared by melting reactions from the anhydrous metal dibromides with the silylated phosphaneimines Me3SiNPR3 (R = Et, NMe2) in the presence of potassium fluoride. All complexes are characterized by crystal structure analyses. 1 forms an only slightly distorted Mn4N4 heterocubane skeleton with an approximate Td symmetry and short Mn…Mn distances of average 295.7 pm. In the structures of 2 and 3 one μ3-NPEt3 ligand of 1 is replaced by one bromine atom with μ3-function. This leads to the novel heterocubane type M4N3Br with approximate C3 symmetry. The deformation of the cubic skeleton leads to metal-metal distances of different lengths, i. e. 292.7 and 323.6 pm in 2 and 274.4 and 306.2 pm in 3 . Temperature dependent magnetic susceptibility measurements between 300 and 5 K on 1 have shown that strong antiferromagnetic coupling exists between the Mn(II) ions with S = 5/2, with a large negative Weiss constant of Θ = –694 K. 相似文献
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[{Cp(CO)3Mo}4In4(PSiMe3)4], an Organometallic In4P4-Heterocubane [{Cp(CO)3Mo}InCl2] reacts with P(SiMe3)3 in THF as solvent to form [{Cp(CO)3Mo}4In4(PSiMe3)4] 1. 1 crystallizes in the space group P1 . The lattice constants (at 208 K) are: a = 1 770.1(6), b = 1 490.3(6), c = 1 317.5(6) pm, α = 76.59(4),β = 88.54(3), γ = 88.98(3)°. According to the crystal structure analysis, 1 contains a slightly distorted In4P4-core with an alternating arrangement of In and P atoms. The In atoms are coordinated roughly tetrahedrally by three PSiMe3 groups (In–P: 256.9(3)–262.3(3) pm) and a {Cp(CO)3Mo} substituent (In? Mo: 278.0(2)–279.5(3) pm). 相似文献
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On the Chemistry of Gallium. 13. Synthesis and Structure of Tetrakis[(2,2,6,6-tetramethylpiperidino)gallium Sulfide] – A New Route to Gallium Sulfur Heterocubanes The reaction of bis(2,2,6,6-tetramethylpiperidino)chloro gallane with potassium thiocyanate does not yield in a simple substitution product of the halide, but affords under elimination of the cyanamide tmp-CN the heterocubane (tmpGaS)4. This amino substituted GaS cubane, prepared in a unique manner, was characterized by means of NMR spectroscopy and X ray crystal structure analysis. 相似文献
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R*OCH2CH2CH2SO2Ph (R*OH = MenOH, (–)‐menthol, ( 3a ); BorOH, (1S)‐(–)‐borneol, ( 3b )) were found to react with n‐BuLi in n‐pentane/n‐hexane and toluene/n‐hexane under deprotonation yielding LiCH(CH2CH2OR*)SO2Ph (R* = Men, ( 4a ); Bor, ( 4b )) which reacted with n‐Bu3SnCl forming the requisite tri(n‐butyl)tin compounds n‐Bu3SnCH(CH2CH2OR*)SO2Ph (R* = Men, ( 5a ); Bor, ( 5b )) as diastereomeric mixtures. The identities of 5a and 5b were unambiguously proved by 1H, 13C and 119Sn NMR spectroscopic measurements. Solutions of 4a afforded crystals of [{LiCH(CH2CH2OMen)SO2Ph}4] ( 4a′ ) for which the structure was determined by single‐crystal X‐ray crystallography. Complex 4a′ crystallized in a tetrameric structure without any additional solvent molecules. There were found direct Li–C bonds (Li1–C1/Li2–C20 2.231(9)/2.236(9) Å). The tetrahedral donor set of Li is completed by three oxygen atoms. One oxygen atom comes from the OMen substituent via intramolecular coordination and two oxygen atoms come from SO2 groups of neighboured LiCH(CH2CH2OMen)SO2Ph moieties. Thus, a heterocubane structure with a Li4S4 core is built up. 相似文献
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Mark Niemeyer 《无机化学与普通化学杂志》2004,630(2):252-256
An Unusual Ambivalent Tin(II)‐oxo Cluster The reaction of the copper aryl CuDmp (Dmp = 2, 6‐Mes2C6H3; Mes = 2, 4, 6‐Me3C6H2) with the stannanediyl Sn{1, 2‐(tBuCH2N)2C6H4} followed by hydrolysis affords in the presence of lithium‐tert‐butoxide the tin(II)‐oxo cluster {(Et2O)(LiOtBu)(SnO)(CuDmp)}2 ( 5 ) in small yield. The solid state structure of the colorless compound shows a central Li2Sn2O2(OtBu)2 fragment with heterocubane structure. In addition, the Li‐acceptor and O(Sn)‐donor atoms are used for the coordination of one molecule diethylether and copper aryl CuDmp, respectively. 相似文献
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By reaction of MIICl2·x H2O (M = Fe (x = 4), Co, Ni (x = 6)) and LiOH·H2O in diethylene glycol (DEG) rod‐like crystals of the composition MII4Cl4(OCH2CH2OCH2CH2OH)4 are formed. According to X‐ray diffraction data obtained by both, single crystals and powders, the CoII and NiII compounds crystallize monoclinic with C2/c (CoII4Cl4(OCH2CH2OCH2CH2OH)4 ( 1 ): a = 2084.1(4), b = 919.0(2), c = 1754.0(4) pm, β = 124.3(1)°, Z = 4; NiII4Cl4(OCH2CH2OCH2CH2OH)4 ( 2 ): a = 2055.2(4), b = 932.1(2), c = 1727.4(4) pm, β = 125.2(1)°, Z = 4), whereas FeII4Cl4(OCH2CH2OCH2CH2OH)4 ( 3 ) crystallizes tetragonal with (a = 1251.4(2), c = 915.3(2) pm, Z = 2). All compounds exhibit analogous molecular structures which are built of a heterocubane‐type core consisting of four metal ions and four deprotonated oxygen atoms of four coordinated diethylene glycol molecules. Neutrality of charge is realized by additional coordination of four chloride anions. In addition to the structural characterization, the thermal and magnetical properties of the title compounds are investigated in detail. 相似文献