The title compound, CHN ·Cl, is as an amidinium salt that was isolated as unexpected product from the reaction between aceto-nitrile, chloro-form and pyrrolidine under refluxing conditions. The packing features two N-H⋯Cl hydrogen bonds to generate centrosymmetric tetra-mers (two cations and two anions) and van der Waals inter-actions.
View Article and Find Full Text PDFActa Crystallogr E Crystallogr Commun
June 2015
Yellow crystals of the title compound 3-amino-4-nitro-benzyl acetate, C9H10N2O4, were isolated from the reaction of acetic anhydride with (5-amino-2-nitro-phen-yl)methanol, prepared from reduction of commerically available 5-amino-2-nitro-benzoic acid with borane-THF. The mol-ecule is essentially planar (r.m.
View Article and Find Full Text PDFActa Crystallogr C Struct Chem
April 2015
The cationic pseudo-square-planar complex tetrakis(1-methyl-2,3-dihydro-1H-imidazole-2-thione-κS)gold(III) trichloride sesquihydrate, [Au(C4H6N2S)4]Cl3·1.5H2O, was isolated as dark-red crystals from the reaction of chloroauric acid trihydrate (HAuCl4·3H2O) with four equivalents of methimazole in methanol. The Au(III) atoms reside at the corners of the unit cell on an inversion center and are bound by the S atoms of four methimazole ligands in a planar arrangement, with S-Au-S bond angles of approximately 90°.
View Article and Find Full Text PDFPreviously, hydridotris(pyrazolyl)borate (Tp) Ru(II) alkyl and aryl complexes of the type TpRu(L)(NCMe)R (R = methyl or aryl; L = charge-neutral two-electron donating ligand) were demonstrated to activate aromatic C-H bonds. To determine the impact of replacing the anionic Tp ligand with charge-neutral poly(pyrazolyl)alkane ligands, [(C(pz)4)Ru(P(OCH2)3CEt)(NCMe)Me][BAr'4] (pz = pyrazolyl, BAr'4 = tetrakis[3,5-bis(trifluoromethyl)phenyl]borate) was prepared. Heating a C6D6 solution of [(C(pz)4)Ru(P(OCH2)3CEt)(NCMe)Me][BAr'4] with 1 equiv of NCMe resulted in C-H activation of the 5-position of a pyrazolyl ring to yield [(κ(3)-(N,C(5),N)C(pz)4)Ru(P(OCH2)3CEt)(NCMe)2][BAr'4] and CH4.
View Article and Find Full Text PDFTreatment of RuCl(2)(PPh(3))(3) with sodium 2,2,2-tris(pyrazolyl)ethoxide [NaOCH(2)C(pz)(3); pz = pyrazolyl] affords the asymmetric heteroscorpionate complex cis-(Ep(OX))RuCl(PPh(3))(2) (1), (Ep(OX) = κ(3)-N,N,O-OCH(2)C(pz)(3)), which can be converted to Ru(II) compounds (2-6), (Ep(OX))RuCl(L)(L') [(2) L = PPh(3), L' = P(OCH(2))(3)CEt; (3) L = L' = P(OCH(2))(3)CEt; (5) L, L' = PPh(3), CO; (6) L = L' = CO]. Compounds 1 and 3 react with CHCl(3) at 60 and 100 °C, respectively, to yield cationic tris(pyrazolyl)methane Ru(II) complexes, [(κ(3)-N,N,N-Mp)RuCl(L)(2)]Cl [Mp = HC(pz)(3); (7) L = PPh(3); (8) L = P(OCH(2))(3)CEt]. The complexes have been characterized by (1)H, (13)C, and (31)P{(1)H} NMR spectroscopy, elemental analysis, high resolution mass spectrometry, and cyclic voltammetry.
View Article and Find Full Text PDFThe reaction of N-heterocyclic carbene, L:, with BeCl(2) quantitatively yields L:BeCl(2)1 (L: = :C{N(2,6-Pr(i)(2)C(6)H(3))CH}(2)). The carbene-stabilized beryllium borohydride monomer L:Be(BH(4))(2)2 is prepared by the reaction of 1 with LiBH(4). Compound 3, prepared by the reaction of 2 with Na(2)[Fe(CO)(4)]·dioxane, represents an unusual "dual reduction" of the imidazole ring (i.
View Article and Find Full Text PDFPotassium graphite reduction of L:Ga(Mes)Cl(2) [L: = :C{(i-Pr)NC(Me)}(2), Mes = 2,4,6-Me(3)C(6)H(2)] (1) in hexane yields the organogallium dimer L:(Mes)(Cl)Ga-Ga(Cl)(Mes):L (2), while potassium reduction of 1 in toluene affords the neutral aromatic Ga(6) octahedron L:Ga[Ga(4)Mes(4)]Ga:L (3).
View Article and Find Full Text PDFReaction of RLi with lead(II) bromide affords the diaryl lead(II) compounds PbR2 (R1 = 2,4,6-triphenylphenyl, 1; R2 = 2,6-bis(1'-naphthyl)phenyl, 2), which have monomeric, carbene-like structures with bent two-coordinate Pb(II) centers.
View Article and Find Full Text PDFPotassium reduction of RZn(mu-I)2Li(OEt2)2 (R = [{(2,6-Pri2C6H3)N(Me)C}2CH]) affords the second compound with a Zn-Zn bond, RZn-ZnR. The air- and moisture-sensitive title compound was characterized by 1H NMR, elemental analyses, and single-crystal X-ray diffraction. The Zn-Zn bond was determined to be 2.
View Article and Find Full Text PDFThe zirconocene-complexed dibismuthene, Cp2Zr(BiR)2 (Cp = C5H5; R = C6H3-2,6-Mes2), was prepared by the reaction of sodium metal with Cp2ZrCl2 and RBiCl2. The air- and moisture-sensitive dark reddish/brown compound is the first organometallic compound containing Bi-Zr bonds and the only example of a ZrBi2 ring. Moreover, our computations on associated model systems offer insight into the nature of the interaction of the heaviest dipnictene with a metallocene center.
View Article and Find Full Text PDFReaction of lead(II) chloride with biphenylmagnesium bromide yields Bp(3)Pb-PbBp(3) and [(THF)(3)Mg(mu-Cl)(3)Mg(THF)(3)][Pb(PbBp(3))(3)](Bp = biphenyl), which, upon single crystal X-ray crystallographic analysis, reveals an interesting variation of Pb-Pb bond distances.
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