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Журнал структурной химии  / №5 2015

CRYSTAL STRUCTURES AND CHARACTERIZATION OF TWO RARE-EARTH-GLUTARATE COORDINATION NETWORKS: ONE-DIMENSIONAL [Nd(C5H6O4)(H2O)4]*Cl AND THREE-DIMENSIONAL [Pr(C5H6O4)(C5H7O4)(H2O)]*H2O (330,00 руб.)

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Первый авторHussain
АвторыKhan I.U., Harrison W.T.A., Tahir M.N.
Страниц8
ID359832
АннотацияThe synthesis, crystal structures, and characterization (IR, TGA/DSC) of [Nd(C5H6O4)? ?(H2O)4]?Cl (1) and Pr(C5H6O4)(C5H7O4)(H2O)]?H2O (2) are described. Compound 1 is a onedimensional coordination polymer containing double chains incorporating pairs of edgesharing NdO9 polyhedra linked by glutarate dianions. A network of O—HѱO and O—HѱCl hydrogen bonds helps to consolidate the structure. Compound 2 is a three-dimensional coordination polymer incorporating chains of edge-sharing PrO10 polyhedra. Its glutarate ion adopts an extended conformation, whereas its hydrogen glutarate ion takes on a twisted conformation. O—HѱO hydrogen bonds are seen in the crystal structure, which features small channels occupied by water molecules. Crystal data: 1, C5H14ClNdO8, Mr = 381.85, monoclinic, P21/c (No. 14), a = 8.9763(6) Å, b = 15.9277(11) Å, c = 8.8690(6) Å, E = 112.090(2)q, V = 1174.94(14) Å3, Z = 4, R(F) = 0.016, wR(F 2) = 0.037. 2, C10H17O10Pr, Mr = 438.15, orthorhombic, Pbca (No. 61), a = 16.3030(7) Å, b = 8.6714(4) Å, c = 19.3899(8) Å, V = 2741.1(2) Å3, Z = 8, R(F) = 0.020, wR(F 2) = 0.050.
УДК548.73:547.13:546.65
CRYSTAL STRUCTURES AND CHARACTERIZATION OF TWO RARE-EARTH-GLUTARATE COORDINATION NETWORKS: ONE-DIMENSIONAL [Nd(C5H6O4)(H2O)4]*Cl AND THREE-DIMENSIONAL [Pr(C5H6O4)(C5H7O4)(H2O)]*H2O / S. Hussain [и др.] // Журнал структурной химии .— 2015 .— №5 .— С. 129-136 .— URL: https://rucont.ru/efd/359832 (дата обращения: 23.04.2024)

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Compound 1 is a onedimensional coordination polymer containing double chains incorporating pairs of edgesharing NdO9 polyhedra linked by glutarate dianions. <...> A network of O—H    O and O—H Cl hydrogen bonds helps to consolidate the structure. <...> Its glutarate ion adopts an extended conformation, whereas its hydrogen glutarate ion takes on a twisted conformation. <...> INTRODUCTION Glutaric acid HO2C(CH2)3CO2H (H2glut or C5H8O4) has applications in polymer chemistry [ 1 ] and can form liquid crystals [ 2 ]. <...> In its doubly-deprotonated form (glu2–), it is a versatile bridging ligand with a flexible backbone and many coordination polymers have been reported in combination with both transition metal and rare-earth cations [ 3—8]. <...> Five drops of a 1 N NaOH solution was added to raise the pH of the glutaric acid solution. <...> The mixture was filtered and kept at room temperature for crystallization. <...> After 10 days, pink blocks of 1 were recovered in 43 % yield by filtration and rinsing with ethanol. <...> Eight drops of a 1 N NaOH solution was added to raise the pH of the glutaric acid solution. <...> The solutions were mixed and stirred for 1 h at room temperature. <...> The mixture was filtered and kept at room temperature for crystallization. <...> After 10 days, light green needles of 2 were recovered by vacuum filtration and rinsing with ethanol (yield = 48 %). <...> The IR spectra of 1 and 2 were recorded on a Perkin—Elmer FTIR 180 spectrophotometer using KBr pellets over the frequency range 4000—400 cm–1. <...> The water H atoms were located in difference maps and refined as riding atoms in their as-found relative positions. <...> The carboxylic acid H atom in 2 was located in a different map and its position freely was refined. <...> These assignments are consistent with the different bonding modes of the glutarate ion in the crystal structure of 1 (vide infra). <...> The C=O stretch in free glutaric acid occurs at 1699 cm–1. <...> A strong, very broad band centered around 3350 cm–1 in 1 corresponds to the O—H vibrations of hydrogen bonded water molecules and a cluster of weak, overlapped bands around 645 cm <...>