Mercuration of acetone in the acetone-mercury(II) perchlorate-2-(2′-pyridyl)quinoxaline(L) system (original) (raw)
Related papers
Polyhedron, 2009
Several mercury(II) complexes of 2-quinaldic acid (quinH; IUPAC name: quinoline-2-carboxylic acid) were synthesized and characterized. [Hg(quin) 2 (OH 2 )] (1) was obtained as the reaction product of mercury(II) chloride and 2-quinaldic acid in an aqueous media, while a mixture of 1, [(quinH 2 )(HgCl 3 )]Á 2quinHÁH 2 O (2), and [Hg(quin) 2 (EtOH)]ÁH 2 O (3) was obtained from a 96% ethanol solution. Pure [HgCl(quin)(quinH)] (4) was obtained as the first reaction product when the reaction was performed in absolute alcohol. After isolation of 4 from the filtrate the mixture of 1-3 was again obtained. The Xray single-crystal structure analysis reveals that the ligand, 2-quinaldic acid is coordinated to the Hg 2+ ion as a N,O-chelating quinaldate ion in structures 1, 3 and 4. In the structure of 2 polymeric ½HgCl 3 n nÀ anions are formed with a very deformed trigonal-bipyramidal 3 + 2 mercury coordination sphere while the ligand, 2-quinaldic acid exists in the zwitterionic form as quinH, and as a cation, quinH 2 þ . The coordination polyhedron in 1 and 4 can be described as 2 + 3 and 4 + 1 deformed trigonal-bipyramidal and square-pyramidal geometry with the water molecule and chlorine atom at the fifth site in 1 and 4, respectively. The coordination sphere in 3 is square-pyramidal with the ethanol molecule at the vertex, however through additional HgÁÁÁO contacts centrosymmetric dimers are formed resulting in a 5 + 1 effective octahedral mercury coordination.
Inorganica Chimica Acta, 2005
An X-ray crystal structure has shown that the previously reported bis(p-hydroxytetrafluorophenyl)mercury crystallises as a monohydrate [Hg(C 6 F 4 OH-p) 2 (OH 2)] exhibiting rare coordination of water to a diorganomercurial. The stereochemistry of the three-coordinate mercury is T-shaped with the water coordinated perpendicular to the near linear C-Hg-C unit. The molecules are linked in chains by hydrogen bonding between the hydroxy groups, and the chains into layers by hydrogen bonding between the water oxygen and an OH group. Thermogravimetric analysis shows two water molecules are eliminated together, both the coordinated water and one formed through condensation of the linked-OH groups. In [Hg(p-MeOC 6 H 4)(O 2 CC 6 F 4 OMe-p)], molecules with a near linear strongly bonded C-Hg-O arrangement are observed. These are linked into a linear polymer through Hg-O (carboxylate) bridges giving alternate four-membered and eight-membered rings giving mercury overall square planar stereochemistry.
Journal of Molecular Structure, 2004
Solution studies and X-ray crystallography were used to investigate the complexation of Hg(II) by the proton transfer compound (pyda•H 2) (pydc) (pyda ¼ 2,6-pyridinediamine and pydc•H 2 ¼ 2,6-pyridinedicarboxilic acid), LH 2. The protonation constants of the building blocks of the LH 2 adduct, the equilibrium constants for the reaction of pydc•H 2 with pyda and the stoichiometry and stability of the Hg(II) complex with LH 2 on aqueous solution were accomplished by potentiometric pH titration. The solution studies strongly support a self-association between (pydc) 22 and (pyda•H 2) 2þ. The most aboundant ternary complex of mercury(II) formed in aqueous solution is Hg(pydc) 2 (pyda) 2 which existed at pH. 9.0 by an extent of 86.5%, while a (pyda•H) 2 [Hg(pydc)] 2 complex species exists in about 35% in a pH range of 3.5-4.5. The complexation reactions of LH 2 with HgCl 2 lead to the formation of a crystalline anionic {(pyda•H) 2 [Hg(pydc)Cl] 2 •2H 2 O} n complex. The Hg(II) complex shows 1 H and 13 C NMR resonances of cationic counter ion (pyda•H) þ and signals corresponding to the coordinated ligands (pydc) 22. This complex crystallizes in the triclinic space group P 1 with a ¼ 7:078ð2Þ Å , b ¼ 10:152ð3Þ Å , c ¼ 10:784ð3Þ Å , a ¼ 96:107ð6Þ8; b ¼ 99:163ð7Þ8; g ¼ 101:792ð6Þ8 and Z ¼ 1: Coordination number around each Hg(II) atom is six, with distorted octahedral geometry. The binuclear units of the polymeric complex are linked into infinite network via additional Hg-O bonds.
Synthesis and spectroscopic characteristic of mercury(II) complexes with 2-(2'-pyridyl)quinoline
Acta Chimica Slovenica, 2003
Various complexes Hg(PQ)X 2 (PQ = 2-(2'-pyridyl)quinoline, X = Cl - , Br - , I - , N 3 -, NO 2 -, NO 3 -, and SCN - ) have been synthesized by direct reaction of HgX 2 (X = Cl - , Br - , and I - ) with PQ or by the reaction of HgCl 2 with either NaN 3 , NaNO 2 , NaNO 3 , or NaSCN followed by the addition of 2-(2'-pyridyl)quinoline solution to the reaction mixture. The new complexes have been characterized by elemental analysis, conductivity measurements, electronic absorption, IR, 1 H, and 1 3 C NMR.
Acta Crystallographica Section E Crystallographic Communications, 2015
In the mononuclear title complex, [HgCl2(C22H17N3)], synthesized from the quinoline-derived Schiff baseN1-phenyl-N4-[(quinolin-2-yl)methylidene]benzene-1,4-diamine (PQMBD) and HgCl2, the coordination sphere around the Hg2+atom is distorted tetrahedral, comprising two Cl atoms [Hg—Cl = 2.3487 (14) and 2.4490 (15) Å] and two N atom donors from the PQMBD ligand,viz. the quinolyl and the imine N atom [Hg—N = 2.270 (4) and 2.346 (4) Å, respectively]. The dihedral angle between the two benzene rings attached to the amino group is 43.7 (3)°. In the crystal, N—H...Cl and C—H...Cl hydrogen bonds, as well as π–π stacking interactions between one phenyl ring and the pyridine ring of the quinoline moiety of an adjacent molecule [centroid-to-centroid separation = 3.617 (4) Å] are observed, resulting in a three-dimensional network.
Polyhedron, 2004
Syntheses and structural studies for the two complexes dichloro-{2-[(E)-2-(4-methylphenyl)-1-diazenyl]pyridine}Hg(II) (1) and dichloro-{2-[(E)-2-(3-methylphenyl)-1-diazenyl]pyridine}Hg(II) (2) are reported. The solid-state structures of the complexes were determined by X-ray diffraction methods and in addition, the complexes were characterized in solution using 1 H, 13 C and 199 Hg NMR spectroscopy. The X-ray structures reveal that the complexes adopt surprisingly different structures. Complex 2 has an extended polymeric structure with 2-[(E)-2-(3-methylphenyl)-1-diazenyl]pyridine behaving as a monodentate ligand via the pyridyl nitrogen, and all the chlorine atoms serving to bridge mercury atoms, whereas complex 1 has a dimeric structure with 2-[(E)-2-(4methylphenyl)-1-diazenyl]pyridine behaving as a bidentate ligand via the pyridyl nitrogen and one of the azo nitrogens, with a terminal chlorine on each Hg and a l,l 0-dichloro bridge between the mercury atoms. But the coordination geometry around the mercury atom is similar in both complexes, each showing a distorted trigonal bipyramidal arrangement of the donor atoms. These complexes were characterized in solution by 1 H, 13 C, 199 Hg NMR spectroscopy.
1999
Bis[N-(propionyl-2-thiolato)glycine]mercury(II), Hg[SCH(CH3)CO-NHCH2COOH](2), was obtained by the reaction of an aqueous solution of N-(2-mercaptopropionyl)glycine and mercury(II) acetate. From the 4-methylpyridine (gamma-picoline) solution it crystallizes as a 1:2 solvate, Hg[SCH(CH3)CONHCH2COOH](2) . 2C(6)H(7)N, in the triclinic system, space group P (1) over bar with a = 4.810(5) Angstrom, b = 9.711(4) Angstrom, c = 15.615(8) Angstrom, alpha = 105.76(4)degrees, beta = 103.44(4)degrees, gamma = 94.01(4)degrees, Z = 1, R = 0.027. Two N-(propionyl-2-thiolato)glycine molecules are bonded centrosymmetrically to mercury over sulfur atoms as mercaptide at a distance of 2.341(2) Angstrom. Hg(mpgH)(2) molecules are connected by centrosymmetrically related hydrogen bonds N1-H ... O3 of 2.922(5) Angstrom into chains along [100]. Each molecule also forms two hydrogen bonds O1-H ... N2 of 2.612(6) Angstrom with two gamma-picoline molecules. The structure of complexes and binding to sulfur wer...
Polyhedron, 2007
Novel mercury(II) compounds of 3-hydroxypicolinic acid (HpicOH; IUPAC name: 3-hydroxy-2-pyridinecarboxylic acid) were synthesized and characterized. HgCl(picOH) (1) and HgBr 2 (HpicOH) (2) were obtained as reaction products from the reaction of the corresponding mercury(II) halide with HpicOH, irrespective of the molar ratio of the reactants. From the reaction of HpicOH and mercury(II) acetate, Hg(picOH) 2 (3) was obtained, while mercury(II) nitrate monohydrate gave the 1/1 solvate with water Hg(picO-H) 2 AE H 2 O (3a). Infrared, 1 H and 13 C NMR spectroscopic data were analyzed for complexes 1, 2 and 3. X-ray crystal structure analysis of 1 and 2 revealed their polymeric nature and different coordination modes of HpicOH. In 1 the deprotonated picolinic acid is N,Ochelating and bridging, while in 2 HpicOH is a O-monodentate weakly bound ligand. Compound 1 consists of HgCl(picOH) moieties with two linear covalent bonds, Hg-N 2.143(4) and Hg-Cl 2.298(1) Å , and four additional HgÁ Á ÁO contacts (2.460(3)-2.904(3) Å ) in which both oxygen atoms from the carboxylic group are bridging and involved in coordination to three neighboring mercury atoms, thus forming infinite layers. The coordination of mercury is 2 + 4. 2 consists of {HgBr 2 (HpicOH)} moieties, which are linked into chains by means of mercury to bromine secondary long range interactions. The coordination sphere of mercury can be described as irregular 2 + 3 formed by two covalently bonded bromine atoms (Hg-Br 2.277(1) and 2.366(1) Å ), two bridging bromine atoms (HgÁ Á ÁBr 3.309(1) and 3.247(1) Å ) and by the HpicOH ligand attached to mercury in the zwitterionic form via the carboxylic oxygen atom (HgÁ Á ÁO 2.602(7) Å ).