Sevim Hamamci

Mono- and binuclear copper(II) complexes of saccharin with 2-pyridinepropanol synthesis, spectral, thermal and structural characterization

Mono- and binuclear copper(II) saccharinate (sac) complexes containing 2-pyridinepropanol (pypr) have been prepared and characterized by elemental analyses, i.r., u.v.–vis., magnetic measurements and single crystal X-ray diffraction. The copper(II) ion in trans-[Cu(pypr)2(sac)2] has −1 site symmetry and is octahedrally coordinated by two bidentate neutral pypr (N, O) and two sac (O) ligands. The binuclear copper(II) complex, [Cu2(μ-pypr)2(sac)2], is built up around a centre of symmetry and contains two strongly distorted square–planar coordinated copper(II) ions bridged by two alkoxo groups of the deprotonated pypr ligand, which also coordinates to the copper(II) ions through its nitrogen. In contrast to the mononuclear complex, the sac ligands in the binuclear complex is N-coordinated. The binuclear complex exhibits diamagnetic behaviour. The i.r. spectra and thermal decompositions of both complexes are described.

Synthesis, Crystal and Molecular Structure of 2‐Pyridylethanolbis(saccharinato)mercury(II)

2-Pyridylethanolbis(saccharinato)mercury(II), [Hg(sac) 2 (pyet)], where sac and pyet are the saccharinate anion and the 2-pyridylethanol molecule, respectively, crystallizes in the triclinic space group P1 (No. 2) with a = 10.4518(6), b = 11.3796(6) (5), c = 19.9945(12) A, a = 102.758(3)° β = 98.146(3)°, γ = 104.751(3)°, Z = 4, V = 2193.0(2) A 3 . The unit cell contains two crystallographically independent [Hg(sac) 2 (pyet)] units in which the mercury(II) ion is tetrahedrally coordinated by two nitrogen atoms of two sac ligands, and one nitrogen and one oxygen atoms of one neutral pyet ligands. The pyet acts as a bidentate N- and O-donor ligand forming a six-membered chelate ring, while sac behaves as a monodentate N-donor ligand. The average bite angle of the pyet ligand is 75.8(5)°. The Hg-N sac bond distances are in the range 2.0874(18) and 2.1931(18) A, whereas the Hg-N pyet and Hg-O pyet bond distances are 2.2452(19)-2.3202(19) and 2.6036(17)-2.5902(16) A, respectively. The crystal exhibits two strong hydrogen bonds between the hydroxyl O atom of pyet and sulfonyl O atoms of sac and the C-H...O type weak hydrogen bonds between H atoms of the aromatic rings of the pyet and the sulfonyl O atoms of the sac ligands. Furthermore, packing of the molecules in the solid-state results in aromatic π-π interactions associated with the aromatic rings of sac-sac and py-py.

An eight-coordinate strontium complex with two tetradentate triethanolamine ligands: synthesis, IR spectra, thermal analysis and crystal structure of bis(triethanolamine)strontium(II) saccharinate

Bis(triethanolamine)strontium(II) saccharinate, [Sr(tea) 2 ](sac) 2 was synthesized and characterized by IR spectroscopy, thermal analysis and X-ray diffraction techniques. The compound crystallizes in orthorhombic system and consists of two sac anions and a complex cation, in which each tea ligand behaves as a tetradentate ligand and their configuration results in an eight-coordinate strontium(II) complex with a bicapped trigonal prism geometry. The anions and cations are linked by the intermolecular hydrogen bonds between the hydroxyl hydrogens of the tea ligands and the amine N, and carbonyl O atoms of the neighbouring sac ions, forming one-dimensional chains running parallel to c. The adjacent chains are held together by van der Waals interactions, creating a three-dimensional network. The FTIR spectra and thermal decomposition of the complex were discussed.

Synthesis, Spectra, Thermal Analysis and Crystal Structure of Trans-Bis(2-Pyridinepropanol)Bis (Saccharinato)Cobalt(II)

The title complex, [Co(pypr)2(sac)2] (pypr = 2-pyridinepropanol and sac = saccharinate), has been prepared and characterized by elemental analysis, electronic and FTIR spectra, magnetic susceptibility measurements, thermal analysis and X-ray diffractometry. The complex crystallizes in triclinic space group PI with a = 8.1836(2), b = 10.0062(2), c = 10.4989(3) Å, α = 90.474(1), β = 107.989(1) and γ = 110.923(1)°. The cobalt(II) ion sits on a center of symmetry and is octahedrally coordinated by two pypr and two sac ligands. Both pypr and sac ligands occupy the trans positions of the coordination octahedron. The two pypr ligands are neutral and act as bidentate N- and O-donor ligands forming two symmetry-related seven-membered chelate rings around the cobalt(II) ion, while both sac ligands are O-coordinated through the carbonyl oxygen atoms. On heating the endothermic removal of two pypr ligands occurs in the first stages of decomposition and at higher temperatures the Co/sac intermediate decomposes to Co3O4 and finally to CoO.

Synthesis and Characterization of Silver(I) Saccharinate Complexes with Pyrazole and Imidazole Ligands: [Ag(sac)(pz)(H2O)]n and [Ag(sac)(im)] · 2H2O

Abstract Two new silver(I) saccharinate (sac) complexes, [Ag(sac)(pz)(H2O)]n (1) and [Ag(sac)(im)]·2H2O (2) (pz = pyrazole and im = imidazole), have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̅, respectively. The sac, pz and im ligands all are N-coordinated. In 1, the [Ag(sac)(pz)] units are bridged by aqua ligands to generate a one-dimensional helical chain, in which the silver(I) ions exhibit a distorted square-planar AgN2O2 coordination geometry. The polymeric chains are connected by N-H· · ·O hydrogen bonds into sheets, which are further linked by aromatic π(pz) · · ·π(sac) stacking interactions into a three-dimensional supramolecular network. Complex 2 consists of individual molecules containing linearly coordinated silver(I) ions with a slightly distorted coordination of AgN2. The molecules interact with each other through hydrogen bonds and π· · ·π interactions to form a three-dimensional supramolecular network.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.