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A. Sánchez - One of the best experts on this subject based on the ideXlab platform.
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Synthesis and NMR spectroscopy of dichlorobis (acetophenonethiosemicarbazone) mercury (II) formed from Phenylmercury.(II) chloride and acetophenonethiosemicarbazone: the first example of symmetrisation in organomercury (II)-thiosemicarbazone chemistr
Inorganica Chimica Acta, 1998Co-Authors: Tarlok S. Lobana, Josés. Casas, A. Sánchez, María S. García-tasendeAbstract:Abstract The reaction of Phenylmercury.II) chloride with acetophenonethiosemicarbazone (Hatsc) in ethanol in 1:1 mole ratio undergoes symmetrisation forming the products, HgCl2(Hatse)2 and Ph2Hg instead of the anticipated compound PhHgCl(Hatse). The analytical data, some physical properties, IR and NMR (1H, 11C, 199Hg) spectroscopy all support the formation of HgCl2(Hatse)2, 199Hg NMR of the solid obtained from the filtrate of the reaction provides evidence for Ph2Hg. This reaction represents the first example of a symmetrisation phenomenon observed in organomercury (II)-thiosemicarbazone chemistry.
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Synthesis, structure and spectral properties of [(HgPh)2TbSMe]; a dinuclear 2-S-methylthiobarbiturate of Phenylmercury.II) exhibiting linkage isomerism
Journal of Organometallic Chemistry, 1996Co-Authors: Rosa Carballo, Josés. Casas, María S. García-tasende, A. SánchezAbstract:Abstract The reaction of 2-S-methylthiobarbituric acid (H2TbSMe) with Phenylmercury.II) acetate in ethanol afforded the title complex, which crystallizes in the space group P21/c (No. 14). The asymmetric unit consists of two independent [(HgPh)2TbSMe] molecules: in molecule 1, the two organometallic moieties are bound primarily to the nitrogen atoms of the ligand ring (N(1) and N(3)); in molecule 2, one Phenylmercury.II) is N(1)-bound but the other is bound to the exocyclic oxygen contiguous to N(3). Hence molecules 1 and 2 are linkage isomers. Several weak intra- and intermolecular interactions are also observed. In DMSO solution, 1H, 13C and 199Hg NMR measurements suggest fast exchange of Phenylmercury.II) between N- and O-coordination, with prevalence of the former.
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Phenylmercury.II) dithiophosphates. Crystal structure of (O,O′-diethyldithiophosphate) Phenylmercury.II)
Journal of Crystallographic and Spectroscopic Research, 1992Co-Authors: E. M. Vázquez-lópez, A. Sánchez, A. Castiñeiras, J. S. Casas, J. SordoAbstract:The Phenylmercury. II ) derivatives PhHgS_2P(OR)_2 (R=C_2H_5, C_6H_11 and C_6H_5) have been synthesized. (O,O′-diethyldithiophosphate) Phenylmercury.II), C_10H_15HgO_2PS_2, crystallizes in the monoclinic space group P 2_1/ c (n° 14) with a =7.330(5), b =18.085(2), c =11.552(4)Å, β =105.96(5)°, V =1472.3(6)Å^3, Z =4, D =2.088 g.cm^−3. The mercury atom is coordinated to the phenyl carbon atom and to a ligand sulphur atom in an almost linear arrangement (C-Hg-S angle, 176.0(2)°. The ligand is almost monodentate, its second sulphur atom only being involved in a weak secondary intermolecular bond. IR and Raman studies of the other two compounds suggest the same coordination scheme. Positive ion FAB and^13C,^31P and^199Hg NMR spectra are also discussed.
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Phenylmercury.II) dithiophosphates. Crystal structure of (O,O'-diethyldithiophosphate) Phenylmercury.II)
Journal of Crystallographic and Spectroscopic Research, 1992Co-Authors: E. M. Vázquez-lópez, Josés. Casas, A. Sánchez, A. Castiñeiras, J. SordoAbstract:The Phenylmercury.II) derivatives PhHgS2P(OR)2 (R=C2H5, C6H11 and C6H5) have been synthesized. (O,O′-diethyldithiophosphate) Phenylmercury.II), C10H15HgO2PS2, crystallizes in the monoclinic space groupP21/c (n° 14) witha=7.330(5),b=18.085(2),c=11.552(4)A,β=105.96(5)°,V=1472.3(6)A3,Z=4,D=2.088 g.cm−3. The mercury atom is coordinated to the phenyl carbon atom and to a ligand sulphur atom in an almost linear arrangement (C-Hg-S angle, 176.0(2)°. The ligand is almost monodentate, its second sulphur atom only being involved in a weak secondary intermolecular bond.IR and Raman studies of the other two compounds suggest the same coordination scheme. Positive ion FAB and13C,31P and199Hg NMR spectra are also discussed.
Josés. Casas - One of the best experts on this subject based on the ideXlab platform.
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Synthesis and NMR spectroscopy of dichlorobis (acetophenonethiosemicarbazone) mercury (II) formed from Phenylmercury.(II) chloride and acetophenonethiosemicarbazone: the first example of symmetrisation in organomercury (II)-thiosemicarbazone chemistr
Inorganica Chimica Acta, 1998Co-Authors: Tarlok S. Lobana, Josés. Casas, A. Sánchez, María S. García-tasendeAbstract:Abstract The reaction of Phenylmercury.II) chloride with acetophenonethiosemicarbazone (Hatsc) in ethanol in 1:1 mole ratio undergoes symmetrisation forming the products, HgCl2(Hatse)2 and Ph2Hg instead of the anticipated compound PhHgCl(Hatse). The analytical data, some physical properties, IR and NMR (1H, 11C, 199Hg) spectroscopy all support the formation of HgCl2(Hatse)2, 199Hg NMR of the solid obtained from the filtrate of the reaction provides evidence for Ph2Hg. This reaction represents the first example of a symmetrisation phenomenon observed in organomercury (II)-thiosemicarbazone chemistry.
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symmetrisation isomerism and structural studies on novel Phenylmercury.ii thiosemicarbazonates correlation of the energy barrier to rotation of the amino group with the bonding parameters of the thioamide group
Journal of The Chemical Society-dalton Transactions, 1997Co-Authors: Tarlok S. Lobana, Josés. Casas, A. Castiñeiras, Agustin Sanchez, Maria S Garciatasende, Ezequiel M VazquezlopezAbstract:The reactions of Phenylmercury.II) acetate with a series of alkyl, aryl and heterocyclic thiosemicarbazones in ethanol formed novel Phenylmercury.II) derivatives of stoichiometry [HgPhL] [HL = RN3N2HC1(S)N1H2 = cyclopentanone 1, cyclohexanone 2, benzaldehyde 3, 2-hydroxybenzaldehyde 4, 4-methoxybenzaldehyde 5, pyrrole-2-carbaldehyde 6, thiophene-2-carbaldehyde 7 or furan-2-carbaldehyde 8 thiosemicarbazone], characterised with the help of analytical data, physical properties, IR, far-IR, multinuclear NMR (1H, 13C, 199Hg) spectroscopy and X-ray crystallography of complexes 1, 5 and 6. The 1H and 13C NMR data suggest that the N2H group is deprotonated during reaction with Phenylmercury.II) acetate and co-ordination occurs via the N3,S atoms in a chelating mode. The 199Hg NMR data suggest symmetrisation phenomenon for complexes 3 and 5, 2[HgPhL] ⇌ HgPh2 + [HgL], which is supported also by 1H and 13C NMR data. The δ(Hg) values reveal that shielding of Hg with the change of organic group in the thiosemicarbazones decreases in the order: 2-hydroxybenzene ⋙ furan > benzene > 4-methoxybenzene thiophene ≈ cyclohexanone ≈ cyclopentanone > pyrrole and the Lewis basicity of the thiosemicarbazones varies in the opposite order. The 1H and 13C NMR data reveal that 7 and 8 show isomerism. There are two strong [Hg–C 2.063(7) 1, 2.069(10) 5, 2.049(11) 6; Hg–S 2.382(2) 1, 2.357(3) 5, 2.377(3) A 6] and one weak bond [Hg–N3 2.489(6) 1, 2.611(7) 5, 2.492(9) A 6], with CPh–Hg–S bond angles of 162.9(2), 174.2(3), 165.8(3)° respectively. The weak intermolecular interactions via Hg · · · N2 [3.001(6) A] in 1 and via Hg · · · S in 5 [3.518(3) A] and 6 [3.528(3) A] form centrosymmetric dimers and Hg formally acquires four-co-ordination with two strong (Hg–C, Hg–S), one weak (Hg · · · N3) and one secondary (Hg · · · N2 or S) bonds. The preferred dimer formation via N2 nitrogen in 1, rather than via sulfur atoms (5 and 6) despite Hg · · · S affinity represents an unusual bonding mode. From the low-temperature 1H NMR studies of some selected complexes, the energy barrier (ΔGTc*, Tc is coalescence temperature) to rotation of the amino group about the C1–N1 bond was calculated and correlated with bonding parameters of the thioamide group in the solid state.
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Synthesis, structure and spectral properties of [(HgPh)2TbSMe]; a dinuclear 2-S-methylthiobarbiturate of Phenylmercury.II) exhibiting linkage isomerism
Journal of Organometallic Chemistry, 1996Co-Authors: Rosa Carballo, Josés. Casas, María S. García-tasende, A. SánchezAbstract:Abstract The reaction of 2-S-methylthiobarbituric acid (H2TbSMe) with Phenylmercury.II) acetate in ethanol afforded the title complex, which crystallizes in the space group P21/c (No. 14). The asymmetric unit consists of two independent [(HgPh)2TbSMe] molecules: in molecule 1, the two organometallic moieties are bound primarily to the nitrogen atoms of the ligand ring (N(1) and N(3)); in molecule 2, one Phenylmercury.II) is N(1)-bound but the other is bound to the exocyclic oxygen contiguous to N(3). Hence molecules 1 and 2 are linkage isomers. Several weak intra- and intermolecular interactions are also observed. In DMSO solution, 1H, 13C and 199Hg NMR measurements suggest fast exchange of Phenylmercury.II) between N- and O-coordination, with prevalence of the former.
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Phenylmercury.II) dithiophosphates. Crystal structure of (O,O'-diethyldithiophosphate) Phenylmercury.II)
Journal of Crystallographic and Spectroscopic Research, 1992Co-Authors: E. M. Vázquez-lópez, Josés. Casas, A. Sánchez, A. Castiñeiras, J. SordoAbstract:The Phenylmercury.II) derivatives PhHgS2P(OR)2 (R=C2H5, C6H11 and C6H5) have been synthesized. (O,O′-diethyldithiophosphate) Phenylmercury.II), C10H15HgO2PS2, crystallizes in the monoclinic space groupP21/c (n° 14) witha=7.330(5),b=18.085(2),c=11.552(4)A,β=105.96(5)°,V=1472.3(6)A3,Z=4,D=2.088 g.cm−3. The mercury atom is coordinated to the phenyl carbon atom and to a ligand sulphur atom in an almost linear arrangement (C-Hg-S angle, 176.0(2)°. The ligand is almost monodentate, its second sulphur atom only being involved in a weak secondary intermolecular bond.IR and Raman studies of the other two compounds suggest the same coordination scheme. Positive ion FAB and13C,31P and199Hg NMR spectra are also discussed.
María S. García-tasende - One of the best experts on this subject based on the ideXlab platform.
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Synthesis and NMR spectroscopy of dichlorobis (acetophenonethiosemicarbazone) mercury (II) formed from Phenylmercury.(II) chloride and acetophenonethiosemicarbazone: the first example of symmetrisation in organomercury (II)-thiosemicarbazone chemistr
Inorganica Chimica Acta, 1998Co-Authors: Tarlok S. Lobana, Josés. Casas, A. Sánchez, María S. García-tasendeAbstract:Abstract The reaction of Phenylmercury.II) chloride with acetophenonethiosemicarbazone (Hatsc) in ethanol in 1:1 mole ratio undergoes symmetrisation forming the products, HgCl2(Hatse)2 and Ph2Hg instead of the anticipated compound PhHgCl(Hatse). The analytical data, some physical properties, IR and NMR (1H, 11C, 199Hg) spectroscopy all support the formation of HgCl2(Hatse)2, 199Hg NMR of the solid obtained from the filtrate of the reaction provides evidence for Ph2Hg. This reaction represents the first example of a symmetrisation phenomenon observed in organomercury (II)-thiosemicarbazone chemistry.
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Synthesis, structure and spectral properties of [(HgPh)2TbSMe]; a dinuclear 2-S-methylthiobarbiturate of Phenylmercury.II) exhibiting linkage isomerism
Journal of Organometallic Chemistry, 1996Co-Authors: Rosa Carballo, Josés. Casas, María S. García-tasende, A. SánchezAbstract:Abstract The reaction of 2-S-methylthiobarbituric acid (H2TbSMe) with Phenylmercury.II) acetate in ethanol afforded the title complex, which crystallizes in the space group P21/c (No. 14). The asymmetric unit consists of two independent [(HgPh)2TbSMe] molecules: in molecule 1, the two organometallic moieties are bound primarily to the nitrogen atoms of the ligand ring (N(1) and N(3)); in molecule 2, one Phenylmercury.II) is N(1)-bound but the other is bound to the exocyclic oxygen contiguous to N(3). Hence molecules 1 and 2 are linkage isomers. Several weak intra- and intermolecular interactions are also observed. In DMSO solution, 1H, 13C and 199Hg NMR measurements suggest fast exchange of Phenylmercury.II) between N- and O-coordination, with prevalence of the former.
J. Sordo - One of the best experts on this subject based on the ideXlab platform.
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Phenylmercury.II) dithiophosphates. Crystal structure of (O,O′-diethyldithiophosphate) Phenylmercury.II)
Journal of Crystallographic and Spectroscopic Research, 1992Co-Authors: E. M. Vázquez-lópez, A. Sánchez, A. Castiñeiras, J. S. Casas, J. SordoAbstract:The Phenylmercury. II ) derivatives PhHgS_2P(OR)_2 (R=C_2H_5, C_6H_11 and C_6H_5) have been synthesized. (O,O′-diethyldithiophosphate) Phenylmercury.II), C_10H_15HgO_2PS_2, crystallizes in the monoclinic space group P 2_1/ c (n° 14) with a =7.330(5), b =18.085(2), c =11.552(4)Å, β =105.96(5)°, V =1472.3(6)Å^3, Z =4, D =2.088 g.cm^−3. The mercury atom is coordinated to the phenyl carbon atom and to a ligand sulphur atom in an almost linear arrangement (C-Hg-S angle, 176.0(2)°. The ligand is almost monodentate, its second sulphur atom only being involved in a weak secondary intermolecular bond. IR and Raman studies of the other two compounds suggest the same coordination scheme. Positive ion FAB and^13C,^31P and^199Hg NMR spectra are also discussed.
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Phenylmercury.II) dithiophosphates. Crystal structure of (O,O'-diethyldithiophosphate) Phenylmercury.II)
Journal of Crystallographic and Spectroscopic Research, 1992Co-Authors: E. M. Vázquez-lópez, Josés. Casas, A. Sánchez, A. Castiñeiras, J. SordoAbstract:The Phenylmercury.II) derivatives PhHgS2P(OR)2 (R=C2H5, C6H11 and C6H5) have been synthesized. (O,O′-diethyldithiophosphate) Phenylmercury.II), C10H15HgO2PS2, crystallizes in the monoclinic space groupP21/c (n° 14) witha=7.330(5),b=18.085(2),c=11.552(4)A,β=105.96(5)°,V=1472.3(6)A3,Z=4,D=2.088 g.cm−3. The mercury atom is coordinated to the phenyl carbon atom and to a ligand sulphur atom in an almost linear arrangement (C-Hg-S angle, 176.0(2)°. The ligand is almost monodentate, its second sulphur atom only being involved in a weak secondary intermolecular bond.IR and Raman studies of the other two compounds suggest the same coordination scheme. Positive ion FAB and13C,31P and199Hg NMR spectra are also discussed.
Kamalendu Dey - One of the best experts on this subject based on the ideXlab platform.
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Two-dimensional supramolecular assembly of Phenylmercury.II) and cadmium(II) complexes with a tridentate thiohydrazone NNS donor ligand: Synthesis, coordination behavior and crystal structure
Polyhedron, 2007Co-Authors: Susobhan Biswas, Saikat Sarkar, Ian M. Steele, Sougata Sarkar, Golam Mostafa, Bijali Bikash Bhaumik, Kamalendu DeyAbstract:Abstract The reaction of Phenylmercury.II) acetate and cadmium(II) acetate with a refluxed solution of diacetylmonoxime and morpholine N-thiohydrazide formed a novel Phenylmercury.II) complex, [PhHg(Hdammthiol)] (1) and a cadmium(II) complex, [Cd(Hdammthiol)2] (2), respectively (where H2dammthiol is the thiol form of diacetylmonoximemorpholine N-thiohydrazone (Hdammth) formed by the condensation of diacetylmonoxime and morpholine N-thiohydrazide in the presence of Phenylmercury.II) and cadmium(II) ions). The complexes were characterised by elemental analyses and spectral data (electronic, infrared and 1H NMR) and also by X-ray crystal structure analysis. The X-ray crystallography shows that the Phenylmercury.II) complex attained a tricoordinated distorted T-shaped structure, while the cadmium(II) complex attained a trapezoidal bipyramidal geometry. The Phenylmercury.II) complex forms a two-dimensional sheet via C–H⋯O and O–H⋯N hydrogen bonding and also forms a two-dimensional supramolecular dimer, having C–H⋯π synthons. Intermolecular C–H⋯O and O–H⋯O hydrogen bonding of the cadmium(II) complex forms a two-dimensional supramolecular sheet along the bc plane and posses an impressively short intermolecular C(sp3)⋯O(sp3) contact.