A new supramolecular assembly obtained by reaction between thiosaccharin and hexamethylenediamine

The crystal structure of hexamethylenediammonium bis(thiosaccharinate) dihydrate, [H3N-(CH2)6-NH3](tsac) 2 · 2 H2O (tsac = C7H4NO 2S2, the anion of thiosaccharin), was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/a with Z = 4. The thiosaccharinate moiety is planar and shows small but significant modifications in the bonding of the thioamide functional group as compared with the protonated neutral molecule. The ionic crystal is further stabilized by an extensive H-bonding network, which links the anions and cations into an infinite three-dimensional supramolecular assembly. The FTIR spectrum of the compound is briefly discussed in comparison with those of the neutral constituent molecules.Centro de Química InorgánicaInstituto de Física La Plat

Synthesis, structural and spectroscopic characterization of thallium(I) acesulfamate

The new acesulfamate salt, TlC4H4NO4S, was prepared by reaction of acesulfamic acid and thallium(I) carbonate in aqueous solution. Its crystal and molecular structure was determined by single crystal X-ray diffraction methods. The substance crystallizes in the monoclinic space group P21/a, with unit cell parameters a = 7.5844(4) Å, b = 9.7268(5) Å, c = 10.8105(5) Å, β = 105.174(6)°, and Z=4 molecules per unit cell, and is isostructural with the corresponding sodium, potassium, rubidium and cesium salts. The FTIR and Raman spectra of the compound are also recorded and briefly discussed.Fil: Baran, Enrique José. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Química Inorgánica "Dr. Pedro J. Aymonino". Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Centro de Química Inorgánica "Dr. Pedro J. Aymonino"; ArgentinaFil: Parajón Costa, Beatriz Susana. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Química Inorgánica "Dr. Pedro J. Aymonino". Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Centro de Química Inorgánica "Dr. Pedro J. Aymonino"; ArgentinaFil: Echeverría, Gustavo Alberto. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Física La Plata. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Física La Plata; ArgentinaFil: Piro, Oscar Enrique. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Física La Plata. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Física La Plata; Argentin

A new supramolecular assembly obtained by reaction between thiosaccharin and hexamethylenediamine

The crystal structure of hexamethylenediammonium bis(thiosaccharinate) dihydrate, [H3N-(CH2)6-NH3](tsac) 2 · 2 H2O (tsac = C7H4NO 2S2, the anion of thiosaccharin), was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/a with Z = 4. The thiosaccharinate moiety is planar and shows small but significant modifications in the bonding of the thioamide functional group as compared with the protonated neutral molecule. The ionic crystal is further stabilized by an extensive H-bonding network, which links the anions and cations into an infinite three-dimensional supramolecular assembly. The FTIR spectrum of the compound is briefly discussed in comparison with those of the neutral constituent molecules.Centro de Química InorgánicaInstituto de Física La Plat

Spontaneous Enantiomorphism in Poly-phased Alkaline Salts of tris(oxalato)ferrate(III): Crystal Structure of Cubic NaRb5[Fe(C2O4)3]2

We show here that the phenomenon of spontaneous resolution of enantiomers occurs during the crystallization of the sodium and rubidium double salts of the transition metal complex tris(oxalato)ferrate(III), namely sodium penta-rubidium bis[tris(oxalate) ferrate (III)], NaRb5[Fe(C2O4)3]2. One enantiomer of the salt crystallizes in the cubic space group P4332 with Z = 4 and a Flack absolute structure parameter x = -0.01(1) and its chiral counterpart in the space group P4132 with x = -0.00(1). All metal ions are at crystallographic special positions: the Fe(III) ion is on a threefold axis, coordinated by three oxalate dianions in a propeller-like conformation. One of the two independent Rb(I) ions is on a twofold axis in an eightfold coordination with neighboring oxalate oxygen atoms, and the other one on a threefold axis in a sixfold RbO6 coordination. The sodium ion is at a site of D3 point group symmetry in a trigonal-antiprismatic NaO6 coordination.Fil: Piro, Oscar Enrique. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Física La Plata. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Física La Plata; ArgentinaFil: Echeverría, Gustavo Alberto. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Física La Plata. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Física La Plata; ArgentinaFil: Baran, Enrique José. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Química Inorgánica "Dr. Pedro J. Aymonino". Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Centro de Química Inorgánica "Dr. Pedro J. Aymonino"; Argentin

Synthesis, structure and magnetic properties of tetrakis-μ-carboxylato-bis(dodecylnicotinato)dicopper(II) complexes; crystal and molecular structure of the decyl carboxylate derivative

Dodecylnicotinate bis-adducts of binuclear copper carboxylates, of the general formula Cu2(O2CCn-1H2n-1)4(C 5H4NCOOC12H25)2, were synthesized for n = 10, 12, 14, 16, 18 and 20, and their crystal structure, thermal behavior and magnetic properties studied. The molecular structure of the decyl derivative has been determined from single-crystal X-ray diffraction data. The dimer is centrosymmetric with the CuII ions in a square-pyramidal coordination with four O-alkyl O atoms [average d(Cu - O) 1.960 (6) Å] in the basal plane and the nicotine N atom at apical positions [d(Cu - N) 2.183 (3) Å]. The copper ions, 2.615 (1) Å apart, are bridged by four O-alkyl carboxylate groups. Both the n = 20 and n = 18 homologues exhibit lamellar phases, which can be related to the supramolecular arrangement found in the n = 10 derivative. The magnetic behavior of the decyl and octadecyl dimers was studied in the 2-300 K temperature range. They exhibit a strong intramolecular antiferromagnetic interaction (Cu-Cu superexchange coupling constant J = -347 cm-1 for the decyl derivative), which can be attributed to a large overlap of the metal 3d orbitals and the oxygen lone pair orbitals of the linking carboxylate groups.Fil: Rusjan, Marcia. Universidad Nacional de General Sarmiento; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Ciudad Universitaria. Instituto de Química, Física de los Materiales, Medioambiente y Energía. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales. Instituto de Química, Física de los Materiales, Medioambiente y Energía; ArgentinaFil: Chaia, Zulema. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Ciudad Universitaria. Instituto de Química, Física de los Materiales, Medioambiente y Energía. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales. Instituto de Química, Física de los Materiales, Medioambiente y Energía; ArgentinaFil: Piro, Oscar Enrique. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Física La Plata. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Física La Plata; ArgentinaFil: Guillon, Daniel. Universite Paul Verlaine-Metz. Institut de Physique, Chimie et Materiaux; FranciaFil: Cukiernik, Fabio Daniel. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Ciudad Universitaria. Instituto de Química, Física de los Materiales, Medioambiente y Energía. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales. Instituto de Química, Física de los Materiales, Medioambiente y Energía; Argentina. Universidad Nacional de General Sarmiento; Argentin

Two new supramolecular assemblies obtained by reaction between saccharin and long-chain diamines

The crystal structures of heptamethylenediammonium bis(saccharinate) monohydrate, [H3N-(CH2)7-NH3J(sac) 2-H2O(1) and octamethylenediammonium bis(saccharinate) hemihydrate, [H3N-(CH2)8-NH3J(sac) 2-0.5H2O(2), were determined by single-crystal X-ray diffraction methods. Compound 1 crystallizes in the triclinic space group PI with 2 molecules per unit cell, and 2 in the mono-clinic space group P2 1/a with Z = 4. The saccharinate moiety is planar in both compounds presenting bonding characteristics comparable to those found in other saccharinate salts. The ionic crystals are fürther stabilized by an extensive H-bonding network, which links the anions and cations into an infinite three-dimensional supramolecular assembly. The FTIR spectra of the adducts are briefly discussed in comparison with those of the constituent molecules.Facultad de Ciencias ExactasCentro de Química Inorgánic

A New Supramolecular Assembly Obtained by Reaction Between Thiosaccharin and Pyridine

The crystal structure of pyridinium thiosaccharinate thiosaccharin, [HNC5H5]+ [(tsac)(Htsac)]− (Htsac = C7H5NO2S2, the thiosaccharin molecule), was determined by single-crystal X-ray diffraction. Both, the thiosaccharinate anion, the corresponding neutral molecule and the pyridinium cation are nearly planar and arranged in the solid state in an almost parallel fashion, hence giving rise to a layered supramolecular structure. The anion shows small but significant modifications in the bonding of the thioamide group as compared with the neutral molecule. The crystal is further stabilized by an extensive H-bonding network. The FTIR spectrum of the compound is briefly commented.Publicado on line en 2014.Centro de Química Inorgánic

A new supramolecular assembly obtained by reaction between thiosaccharin and hexamethylenediamine

The crystal structure of hexamethylenediammonium bis(thiosaccharinate) dihydrate, [H3N-(CH2)6-NH3](tsac) 2 · 2 H2O (tsac = C7H4NO 2S2, the anion of thiosaccharin), was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/a with Z = 4. The thiosaccharinate moiety is planar and shows small but significant modifications in the bonding of the thioamide functional group as compared with the protonated neutral molecule. The ionic crystal is further stabilized by an extensive H-bonding network, which links the anions and cations into an infinite three-dimensional supramolecular assembly. The FTIR spectrum of the compound is briefly discussed in comparison with those of the neutral constituent molecules.Centro de Química InorgánicaInstituto de Física La Plat

Two new supramolecular assemblies obtained by reaction between saccharin and long-chain diamines

The crystal structures of heptamethylenediammonium bis(saccharinate) monohydrate, [H3N-(CH2)7-NH3J(sac) 2-H2O(1) and octamethylenediammonium bis(saccharinate) hemihydrate, [H3N-(CH2)8-NH3J(sac) 2-0.5H2O(2), were determined by single-crystal X-ray diffraction methods. Compound 1 crystallizes in the triclinic space group PI with 2 molecules per unit cell, and 2 in the mono-clinic space group P2 1/a with Z = 4. The saccharinate moiety is planar in both compounds presenting bonding characteristics comparable to those found in other saccharinate salts. The ionic crystals are fürther stabilized by an extensive H-bonding network, which links the anions and cations into an infinite three-dimensional supramolecular assembly. The FTIR spectra of the adducts are briefly discussed in comparison with those of the constituent molecules.Facultad de Ciencias ExactasCentro de Química Inorgánic

The effect of chalcogen substitution on the structure and spectroscopy of 4,7-dimethyl-2: H -chromen-2-one/thione analogues

4,7-Dimethyl-2H-chromen-2-one (1) and its novel sulfur analogue 4,7-dimethyl-2H-chromen-2-thione (2) were synthesized and fully characterized by spectroscopic methods and mass spectrometry. The crystal structure of compound 2 has been determined by X-ray diffraction methods, and it crystallizes in the monoclinic I2/m space group. The molecular skeleton lies in the crystallographic mirror plane, in agreement with the expected theoretical planarity enforced by extended π-bonding. The crystal packing of both compounds is characterized by the R22(8) motif formed by intermolecular C–H⋯X[double bond, length as m-dash]C (X = O and S) hydrogen-bonding interactions involving the 1-benzopyran-2-one/thione moiety, as also identified by Hirshfeld surface analysis. The vibrational properties have been studied by infrared and Raman spectroscopy complemented by quantum chemical calculations and normal coordinate analysis of the potential energy distribution. The UV-Vis spectrum is interpreted in terms of TD-DFT quantum chemical calculations, showing a clear red-shift in the HOMO–LUMO electronic transition when the chromen-2-one ring is converted into chromen-2-thione.Fil: Delgado Espinosa, Zuly Yuliana. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Química Inorgánica "Dr. Pedro J. Aymonino". Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Centro de Química Inorgánica "Dr. Pedro J. Aymonino"; ArgentinaFil: Saeed, Aamer. Quaid-I-Azam University; PakistánFil: Mahmood, Shamsul. Quaid-I-Azam University; PakistánFil: Echeverría, Gustavo Alberto. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Física La Plata. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Física La Plata; ArgentinaFil: Piro, Oscar Enrique. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Física La Plata. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Física La Plata; ArgentinaFil: Erben, Mauricio Federico. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Química Inorgánica "Dr. Pedro J. Aymonino". Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Centro de Química Inorgánica "Dr. Pedro J. Aymonino"; Argentin