Zerrin Heren

The influence of ethanolamines on the hydration and mechanical properties of portland cement

Abstract The effect of ethanolamines—monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA)—on the hydration, mechanical and surface properties of the white Portland cement pastes (white PC) has been investigated. The cement pastes with and without admixtures were cured at various hydration times ranging from 1 day to 90 days. Hydration development of cement pastes were followed by setting times, flexural and compressive strengths, specific surface area measurements and thermal analysis techniques. The measurements showed that all these admixtures retard the hydration of white Portland cement in order TEA>DEA>MEA.

Synthesis, crystal structures, thermal, and spectroscopic properties of four new metal(II) (M = Co, Ni, Cu, Hg) complexes of 2-benzoylbenzoate with 3-picoline

Four 2-benzoylbenzoate (bba) complexes, [Co(bba)2(H2O)2(3-pic)2] (1), [Ni(bba)2(H2O)2(3-pic)2] (2), [Cu(bba)2(3-pic)2] (3), and [Hg(bba)2(3-pic)2] (4), have been synthesized and characterized by IR spectra, thermal (TG, DTG, and DTA) analysis, and single crystal X-ray diffraction. All the complexes consist of neutral monomeric units with 1 and 2 crystallizing in the orthorhombic (P n a 21), 3 in triclinic (P 1), and 4 in monoclinic (P21/c) crystal systems. The metal(II) ions exhibit distorted octahedral coordination for 1, 2, and 3 and mercury(II) exhibits distorted trigonal prism coordination. In 1 and 2, bba is monodentate, whereas in 3 and 4 bba is bidentate. 3-Picoline (3-pic) is a classical N-monodentate ligand. Bba are coordinated to metal(II) with carboxylates and IR spectra of all complexes display characteristic absorptions of carboxylate {υ(OCO)asym and υ(OCO)sym}. Thermogravimetric (TG) analyses show that 1 and 2 are thermally stable (Tdecomp. > 60°C) and 3 and 4 are thermally stable (Tdecomp .  > 120°C).

Synthesis, thermal and spectroscopic properties, and crystal structures of [Co(bba)2(H2O)(phen)] and [Ni(bba)2(H2O)(butOH)(phen)] (bba = 2-benzoylbenzoate, phen = 1,10-phenanthroline, butOH = butanol)

Aquabis(2-benzoylbenzoato)(1,10-phenanthroline)cobalt(II) and aquabis(2-benzoylbenzoato)(butanol)(1,10-phenanthroline)nickel(II) have been prepared and characterized by elemental analyses, IR and electronic spectroscopy, magnetic measurements, and single-crystal X-ray diffraction. [Co(bba)2(H2O)(phen)] (1) and [Ni(bba)2(H2O)(butOH)(phen)] (2) consist of neutral monomeric units and crystallize in the monoclinic (P2(1)) and triclinic (P 1) crystal systems, respectively. The cobalt(II) and nickel(II) sit on inversion centres and exhibit distorted octahedral coordination. Phen is bidentate chelating. In 1, bba is both monodentate and bidentate, whereas in 2 bba is only monodentate. bba ligands are coordinated to metal(II) with carboxylates and IR spectra of both complexes display characteristic absorptions of carboxylate anions {ν(OCO)asym and ν(OCO)sym} of bba. Thermal analysis shows that mass losses of 1 from 105°C to 456°C correspond to decomposition of phen and bba, while for 2 these occur at 271–529°C.

Synthesis, Characterization, and Crystal Structures of a Novel [Zn3(bba)6(3-pic)2] Complex (bba = 2-Benzoylbenzoat, 3-pic = 3-Picoline)

A novel trinuclear hekzakis(μ6-2-benzoylbenzoato-O,O′)-bis(3-picoline)-tri-zinc(II) complex, [Zn3(bba)6(3-pic)2] has been synthesized and characterized by elemental analysis, Fourier-transform infrared (FT-IR), ultraviolet/visible (UV/Vis), and mass spectroscopy, thermal methods, and single-crystal x-ray diffraction. The three Zn(II) centers are in two different coordination environments. The central Zn(II) is in a distorted octahedral geometry, while the two terminal Zn(II) centers adopt a distorted tetrahedral geometry. The central and the terminal metal centers are connected through tri μ-2-benzoylbenzoato-O,O′ bridges. The crystal packing of the trinuclear complex is stabilized by C–H···π interaction between bba ligands. The characteristics of the carboxylate anions with typical υ(OCO)asym and υ(OCO)sym values are 1594 and 1368 cm−1, respectively.

Analysis of triethanolamine in white cement pastes by voltammetric methods

Triethanolamine (TEA) in cement paste has been analysed by square wave voltammetric technique. The technique is sensitive for the quantitative determination of small amounts of TEA. The percentage of the adsorbed TEA is very dependent upon the original TEA content of the cement sample. The adsorption reached a saturation level after 12 hours of hydration and remained almost invariant at longer times.

trans-Bis(2-benzoyl­benzoato-κO1)bis­(ethanol-κO)bis­(1H-imidazole-κN3)nickel(II)

In the title centrosymmetric mononuclear nickel(II) complex, [Ni(C14H9O3)2(C3H4N2)2(CH3CH2OH)2], the central NiII ion lies on an inversion centre and is octahedrally coordinated. The equatorial plane is formed by two O atoms from two symmetry-related 2-benzoylbenzoate ligands and two N atoms from two symmetry-related imidazole ligands, whereas the axial positions are occupied by two O atoms from two ethanol ligands. Intramolecular O---H...O hydrogen bonds stabilize this arrangement. The molecules are linked into chains running along the b axis by N—H⋯O hydrogen bonds.

Bis­(benzimidazole-κN3)bis(2-benzoyl­benzoato-κO)copper(II)

In the title centrosymmetric mononuclear copper(II) compound, [Cu(C14H9O3)2(C7H6N2)2], the central CuII ion is coordinated by two N atoms from two symmetry-related benzimidazole (bim) ligands and two O atoms from two symmetry-related 2-benzoylbenzoate (2-byba) ligands in a square-planar geometry. The molecules are linked into chains running along the b axis by N—H⋯O hydrogen bonds and the chains are cross-linked by C—H⋯π interactions.

cis-Bis(butyl-amine-κN)bis-[sulfa-diazine(1-)-κN,N']copper(II) penta-hydrate.

In the title compound {systematic name: cis-bis[4-amino-N-(pyrimidin-2-yl)benzenesulfonamidato-κ2 N,N′]bis(butylamine-κN)copper(II) pentahydrate}, [Cu(C10H9N4O2S)2(C4H11N)2]·5H2O or [Cu(sdz)2(ba)2]·5H2O [ba is butylamine and sdz = sulfadiazine(1−)], the copper(II) cation is six-coordinated by four N atoms of two sulfadiazine ligands and two N atoms of butylamine ligands. The copper(II) ion and one of the water molecules lie on twofold rotation axes. One of the butyl groups is disordered over two sites, with occupancies of 0.395 (8) and 0.605 (8). The geometry around the S atom is distorted tetrahedral. The crystal structure involves intermolecular N—H⋯N and N—H⋯O hydrogen bonds. N—H⋯N hydrogen bonds between sdz ligands lead to a sheet structure parallel to the ab plane.

Synthesis, Spectral and Thermal Studies, and Crystal Structure of cis-Bis(imidazole)bis(picolinato)copper(II) Dihydrate [Cu(pic)2(im)2] ·2H2O

Abstract The mixed-ligand picolinato (pic) complex of Cu(II) with imidazole (im), [Cu(pic)2(im)2] ・2H2O, was synthesized and characterized by elemental analysis, magnetic susceptibility, spectral methods (UV/vis and FT-IR), simultaneous TG, DTA techniques, mass spectroscopy, and X-ray diffraction. The complex crystallizes in the monoclinic space group Cc with the following unit cell parameters: a = 16.381(1), b = 9.556(1), c = 5.177(1) Å , β = 119.074(5)°, Z = 4. In the octahedral complex, the picolinato ligands are coordinated to the copper(II) ion as bidentate N,O-donors forming chelate rings. The imidazole ligands are N-coordinated at cis positions. The thermal decomposition pathway of the complex has been studied by the help of thermal analyses data (TG and DTA) and of the mass spectroscopic fragmentation pattern. The volatile products observed in the thermal decomposition process were also observed in the mass spectrometer ionisation process, except for the molecular peak, and it was concluded that the ionisation and thermal decomposition pathways of the complex resemble each other.

trans-Diaquabis(ethyl­enediamine)zinc(II) 2-(sulfanilamido)­pyrimidine monohydrate

# 2005 International Union of Crystallography Printed in Great Britain – all rights reserved In the title compound, [Zn(C4H8N4)(H2O)2](C10H9N4O2S)2 H2O, the Zn II ion is octahedrally surrounded by two water O atoms [Zn—O = 2.68 (2) and 2.49 (2) Å] and the four N atoms of two ethylenediamine molecules. Intermolecular O—H N, N—H O and N—H N hydrogen-bond interactions result in the formation of an intricate three-dimensional network.