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Coordination Chemistry of P‐rich Phosphanes and Silylphosphanes. XVII [1] [Co(g5‐Me5C5)(g3‐tBu2PPCH–CH3)] from [Co(g5‐Me5C5)(g2‐C2H4)2] and tBu2P–P=P(Me)tBu2 [Co(η5‐Me5C5)(η3‐tBu2PPCH–CH3)] 1 is formed in the reaction of [Co(η5‐Me5C5)(η2‐C2H4)2] 2 with tBu2P–P 4 (generated from tBu2P–P=P(Me)tBu2 3 ) by elimination of one C2H4 ligand and coupling of the phosphinophosphinidene with the second one. The structure of 1 is proven by 31P, 13C, 1H NMR spectra and the X‐ray structure analysis. Within the ligand tBu2P1P2C1H–CH3 in 1 , the angle P1–P2–C1 amounts to 90°. The Co, P1, P2, C1 atoms in 1 look like a „butterfly”︁. The reaction of 2 with a mixture of tBu2P–P=P(Me)tBu2 3 and tBu–C?P 5 yields [Co(η5‐Me5C5){η4‐(tBuCP)2}] 6 and 1 . While 6 is spontaneously formed, 1 appears only after complete consumption of 5 . 相似文献
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Ingo Krossing Ulli Englert Eberhard Matern Jolanta Olkowska‐Oetzel Jerzy Pikies Gerhard Fritz 《无机化学与普通化学杂志》2002,628(2):446-452
tBu2P‐P=P(Me)tBu2 reacts with [Fe2(CO)9] to give [μ‐(1, 2, 3:4‐η‐tBu2P1‐P2‐P3‐P4tBu2){Fe(CO)3}{Fe(CO)4}] ( 1 ) and [trans‐(tBu2MeP)2Fe(CO)3]( 2 ). With [(η2‐C8H14)2Fe(CO)3] in addition to [μ‐(1, 2, 3:4‐η‐tBu2P1‐P2‐P3‐P4tBu2){Fe(CO)2PMetBu2}‐{Fe(CO)4}] ( 10 ) and 2 also [(μ‐PtBu2){μ‐P‐Fe(CO)3‐PMetBu2}‐{Fe(CO)3}2(Fe‐Fe)]( 9 ) is formed. 1 crystallizes in the monoclinic space group P21/c with a = 875.0(2), b = 1073.2(2), c = 3162.6(6) pm and β = 94.64(3)?. 2 crystallizes in the monoclinic space group P21/c with a = 1643.4(7), b = 1240.29(6), c = 2667.0(5) pm and β = 97.42(2)?. 9 crystallizes in the monoclinic space group P21/n with a = 1407.5(5), b = 1649.7(5), c = 1557.9(16) pm and β = 112.87(2)?. 相似文献
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Helmut Goesmann Eberhard Matern Jolanta Olkowska‐Oetzel Jerzy Pikies Gerhard Fritz 《无机化学与普通化学杂志》2001,627(6):1181-1184
Coordination Chemistry of P‐rich Phosphanes and Silylphosphanes. XXIII. Reactions of tBu2P–P=P(Me)tBu2 with (Et3P)2NiCl2 and [{η2‐C2H4}Ni(PEt3)2] tBu2P–P=P(Me)tBu2 ( 1 ) forms with (Et3P)2NiCl2 ( 2 ) and Na(Nph) the [μ‐(1,3 : 2,3‐η‐tBu2P4tBu2){Ni(PEt3)Cl}2] ( 3 ) as main product. Using Na/Hg instead as reducing agent the Ni0 compounds [{η2‐tBu2P–P}Ni(PEt3)2] ( 4 ), [{η2‐tBu2P–P=P–PtBu2}Ni(PEt3)2] ( 5 ) and [(Et3P)Ni(μ‐PtBu2)]2 ( 6 ) with four‐membered Ni2P2 ring result. [{η2‐C2H4}Ni(PEt3)2] yields with 1 also 4 . The compounds were characterized by 1H and 31P{1H} NMR investigations and 3 also by a single crystal X‐ray analysis. It crystallizes triclinic in the space group P 1 with a = 1129.4(2), b = 1256.8(3), c = 1569.5(3) pm, α = 72.44(3)°, β = 70.52(3)° and γ = 74.20(3)°. 相似文献
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Coordination Chemistry of P‐rich Phosphanes and Silylphosphanes XXI The Influence of the PR3 Ligands on Formation and Properties of the Phosphinophosphinidene Complexes [{η2‐tBu2P–P}Pt(PR3)2] and [{η2‐tBu2P1–P2}Pt(P3R3)(P4R′3)] (R3P)2PtCl2 and C2H4 yield the compounds [{η2‐C2H4}Pt(PR3)2] (PR3 = PMe3, PEt3, PPhEt2, PPh2Et, PPh2Me, PPh2iPr, PPh2tBu and P(p‐Tol)3); which react with tBu2P–P=PMetBu2 to give the phosphinophosphinidene complexes [{η2‐tBu2P–P}Pt(PMe3)2], [{η2‐tBu2P–P}Pt(PEt3)2], [{η2‐tBu2P–P}Pt(PPhEt2)2], [{η2‐tBu2P–P}Pt(PPh2Et)2], [{η2‐tBu2P–P}Pt(PPh2Me)2], [{η2‐tBu2P–P}Pt(PPh2iPr], [{η2‐tBu2P–P}Pt(PPh2tBu)2] and [{η2‐tBu2P–P}Pt(P(p‐Tol)3)2]. [{η2‐tBu2P–P}Pt(PPh3)2] reacts with PMe3 and PEt3 as well as with tBu2PMe, PiPr3 and P(c‐Hex)3 by substituting one PPh3 ligand to give [{η2‐tBu2P1–P2}Pt(P3Me3)(P4Ph3)], [{η2‐tBu2P1–P2}Pt(P3Ph3)(P4Me3)], [{η2‐tBu2P1–P2}Pt(P3Et3)(P4Ph3)], [{η2‐tBu2P1–P2}Pt(P3MetBu2)(P4Ph3)], [{η2‐tBu2P1–P2}Pt(P3iPr3)(P4Ph3)] and [{η2‐tBu2P1–P2}Pt(P3(c‐Hex)3)(P4Ph3)]. With tBu2PMe, [{η2‐tBu2P–P}Pt(P(p‐Tol)3)2] forms [{η2‐tBu2P1–P2}Pt(P3MetBu2)(P4(p‐Tol)3)]. The NMR data of the compounds are given and discussed with respect to the influence of the PR3 ligands. 相似文献
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Majid M. Heravi Naser Montazeri Mohammad Rahimizadeh Mehdi Bakavoli Mitra Ghassemzadeh 《Journal of heterocyclic chemistry》2005,42(5):1021-1025
In an attempt to discover bicyclic compounds containing the 1,2,4‐triazine moiety, 1,2,4‐triazolo[1,5‐d]‐1,2,4‐triazine‐5‐thiones from one pot reaction of arylnitriles with 4‐amino‐1,2,4‐triazine‐3‐thione‐5‐one in the presence of potassium tert‐butoxide were synthesized. 相似文献
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Phosphinophosphiniden-Phosphorane tBu2P?P = P(R)tBu2 aus Li(THF)2[η2-(tBu2P)2P] und Alkylhalogeniden
The Phosphinophosphinidene-phosphoranes tBu2P? P = P(R)tBu2 from Li(THF)2[η2-(tBu2P)2P] and Alkyl Halides We report the formation of tBu2P? P = P(R)tBu2 a and (tBu2)2PR b (with R = Me, Et, nPr, iPr, nBu, PhCH2, H2C = CH? CH2 and CF3) reactions of Li(THF)2[η2-(tBu2P)2P] 2 with MeCl, MeI, EtCl, EtBr, nPrCl, nPrBr, iPrCl, nBuBr, PhCH2Cl, H2C = CH? CH2Cl or CF3Br. In THF solutions the ylidic compounds a predominate, whereas in pentane the corresponding triphosphanes b are preferrably formed. With ClCH2? CH = CH2 only b is produced; CF3Br however yields both tBu2P? P = P(Br)tBu2 and tBu2P? P = P(CF3)tBu2, but no b . The ratio of a:b is influenced by the reaction temperature, too. The compounds tBu2P? P = P(Et)tBu2 4a and (tBu2P)2PEt 4 b , e. g., are produced in a ratio of 4:3 at ?70°C in THF, and 1:1 at 20°C; whereas 1:1 is obtained at ?70°C in pentane, and 1:2 at 20°C. Neither tBuCl nor H2C = CHCl react with 2 . The compounds a decompose thermally or under UV irradiation forming tBu2PR and the cyclophosphanes (tBu2P)nPn. 相似文献
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Il Kim Jia‐Min Zhou Hoeil Chung 《Journal of polymer science. Part A, Polymer chemistry》2000,38(9):1687-1697
Polymerizations of higher α‐olefins, 1‐pentene, 1‐hexene, 1‐octene, and 1‐decene were carried out at 30 °C in toluene by using highly isospecific rac‐Me2Si(1‐C5H2‐2‐CH3‐4‐t Bu)2Zr(NMe2)2 (rac‐1) compound in the presence of Al(iBu)3/[CPh3][B(C6F5)4] as a cocatalyst formulation. Both the bulkiness of monomer and the lateral size of polymer influenced the activity of polymerization. The larger lateral of polymer chain opens the π‐ligand of active site wide and favors the insertion of monomer, while the large size of monomer inserts itself into polymer chain more difficultly due to the steric hindrance. Highly isotactic poly(α‐olefin)s of high molecular weight (MW) were produced. The MW decreased from polypropylene to poly(1‐hexene), and then increased from poly(1‐hexene) to poly(1‐decene). The isotacticity (as [mm] triad) of the polymer decreased with the increased lateral size in the order: poly(1‐pentene) > poly(1‐hexene) > poly(1‐octene) > poly(1‐decene). The similar dependence of the lateral size on the melting point of polymer was recorded by differential scanning calorimetry (DSC). 1H NMR analysis showed that vinylidene group resulting from β‐H elimination and saturated methyl groups resulting from chain transfer to cocatalyst are the main end groups of polymer chain. The vinylidene and internal double bonds are also identified by Raman spectroscopy. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 1687–1697, 2000 相似文献
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Prof. Dr. Thomas M. Klapötke Franz A. Martin Norbert T. Mayr Jörg Stierstorfer 《无机化学与普通化学杂志》2010,636(15):2555-2564
3,5‐Diamino‐1,2,4‐triazole ( 1 , guanozol) was protonated with diluted hydrochloric acid, nitric acid, as well as perchloric acid forming 3,5‐diamino‐1,2,4‐triazolium chloride hemihydrate ( 2 ), 3,5‐diamino‐1,2,4‐triazolium nitrate ( 3 ) and 3,5‐diamino‐1,2,4‐triazolium perchlorate ( 4 ), respectively. In a second step 4 reacted with potassium dinitramide forming 3,5‐diamino‐1,2,4‐triazolium dinitramide ( 5 ) and low soluble potassium perchlorate. Compounds 2 – 5 were characterized by low temperature single X‐ray diffraction, IR and Raman as well as multinuclear NMR spectroscopy, mass spectrometry and differential scanning calorimetry. The heats of formation of 1 – 5 were calculated by the CBS‐4M method to be 81.1 ( 1 ), 124.7 ( 2 ), –76.1 ( 3 ), –25.2 ( 4 ) and 138.7 ( 5 ) kJ·mol–1. With these values as well as the X‐ray densities several detonation parameters were calculated using both computer codes EXPLO5.03 and EXPLO5.04. In addition, the sensitivities of 1 – 5 were determined by the BAM drophammer and friction tester as well as a small scale electrical discharge device. 相似文献
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Svitlana V. Shishkina Irina S. Konovalova Svitlana S. Kovalenko Lyudmila L. Nikolaeva Natalya D. Bunyatyan Sergiy M. Kovalenko 《Acta Crystallographica. Section C, Structural Chemistry》2021,77(1):20-28
The dipharmacophore compound 3‐cyclopropyl‐5‐(3‐methyl‐[1,2,4]triazolo[4,3‐a]pyridin‐7‐yl)‐1,2,4‐oxadiazole, C12H11N5O, was studied on the assumption of its potential biological activity. Two polymorphic forms differ in both their molecular and crystal structures. The monoclinic polymorphic form was crystallized from more volatile solvents and contains a conformer with a higher relative energy. The basic molecule forms an abundance of interactions with relatively close energies. The orthorhombic polymorph was crystallized very slowly from isoamyl alcohol and contains a conformer with a much lower energy. The basic molecule forms two strong interactions and a large number of weak interactions. Stacking interactions of the `head‐to‐head' type in the monoclinic structure and of the `head‐to‐tail' type in the orthorhombic structure proved to be the strongest and form stacked columns in the two polymorphs. The main structural motif of the monoclinic structure is a double column where two stacked columns interact through weak C—H…N hydrogen bonds and dispersive interactions. In the orthorhombic structure, a single stacked column is the main structural motif. Periodic calculations confirmed that the orthorhombic structure obtained by slow evaporation has a lower lattice energy (0.97 kcal mol?1) compared to the monoclinic structure. 相似文献
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《Journal of heterocyclic chemistry》2017,54(4):2258-2265
The present study emphasizes on the dealklylation of 3‐aryl‐5‐alkyl‐2‐oxo‐Δ4‐1,3,4‐oxadiazoles when reacted with formamide resulting in the formation of 2‐aryl‐2H‐1,2,4‐triazol‐3(4H )‐ones as major product. Subsequent reactions of 2‐aryl‐2H‐1,2,4‐triazol‐3(4H )‐one gave triazolo[3,4‐b ][1,3,4]thiadiazoles and triazolo[3,4‐b ][1,3,4]thiadiazines derivatives incorporated with 1,2,4‐triazol‐3‐one. 相似文献
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Antonio Guirado Jos A. Sandoval Enrique Alarcn María Vera Delia Bautista Jesús Glvez 《Journal of heterocyclic chemistry》2019,56(6):1873-1878
The first synthetic approach to hitherto unknown 3‐aryl‐5‐dichloromethyl‐Δ2‐1,2,4‐oxadiazolines, of synthetic and biological interest, has been developed involving high‐yield reactions between N‐(2,2‐dichlorovinyl)benzimidoyl chlorides and hydroxylamine. The molecular structure of one member of this new family of compounds—5‐dichloromethyl‐3‐(4‐fluorophenyl)‐1,2,4‐oxadiazoline—has been determined by X‐ray crystallography. Density functional theory calculations supporting the proposed reaction pathway for the formation of these products have been carried out. 相似文献
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