РУсскоязычный Архив Электронных СТатей периодических изданий
Журнал структурной химии/2015/№ 5/

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

The 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.

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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. <...> 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. <...> INTRODUCTION Glutaric acid HO2C(CH2)3CO2H (H2glut or C5H8O4) has applications in polymer chemistry [ 1 ] and can form liquid crystals [ 2 ]. <...> In this paper, as an extension of these studies, we describe the syntheses, characterizations, and single crystal structures of two rare-earth glutarate networks: [Nd(C5H6O4)(H2O)4]Cl (1) and [Pr(C5H6O4)(C5H7O4)(H2O)]H2O (2). <...> Five drops of a 1 N NaOH solution was added to raise the pH of the glutaric acid solution. <...> Eight drops of a 1 N NaOH solution was added to raise the pH of the glutaric acid solution. <...> For both structures, the C-bound H atoms were geometrically placed (C—H = 0.97 Е) and refined as riding atoms. <...> 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. <...> Molecular graphics were generated with ORTEP-3 [ 11 ] and ATOMS [12 ]. <...> These assignments are consistent with the different bonding modes of the glutarate ion in the crystal structure of 1 (vide infra). <...> 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–1 can be tentatively assigned to Nd—O bond vibrations [ 14 ]. <...> The IR spectrum of 1 shows strong, sharp bands at 1640 cm–1, 1528 cm–1, and loss of 18 %, which was completed by 240 C. This is in good agreement with a decomposition scheme that loses the four water molecules from 1 (calc. = 19 %). <...> Compound 1 is <...>
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