Crystal structure of diaqua-(5-sulfosalicylato)-(μ2-hydroxyl)dicopper(II) hemihydrate, Cu2(H2O)2(C7H3O6S)(OH) · 0.5H2O

Abstract

C14H18Cu4O19S2, triclinic, P1 (no. 2), a = 7.403(7) A, b = 8.726(7) A, c = 9.586(1) A, + = 107.58(3)°, * = 96.66(4)°, ( = 102.51(1)°, V = 565.3 A, Z = 1, Rgt(F) = 0.036, wRref(F) = 0.091, T = 173 K. Source of material A mixture of CuCl2.·.2H2O (0.5 mmol) and 5-sulfosalicylic acid (H3L, 0.5mmol) in 12mL distilled water was heated at 450K in a Teflon-lined stainless steel autoclave for seven days. The reaction system was then slowly cooled to room temperature. Green crystals of the title compound suitable for single crystal X-ray diffraction analysis were collected by filtration, washed several times with distilled water and dried in air at ambient temperature (yield 38 % based on Cu). Experimental details All H atoms were positioned geometrically with d(C—H) = 0.93.A and Uiso(H) = 1.2 Ueq(carrier). The H atoms of the water molecules and hydroxy group were not located. The disordered sulfonate O atoms (O1, O1’, O3 and O3’) were refined using O atoms split over two sites, with a total occupancy of 1. The O3W was refined with the occupancy of 0.5 because of its large temperature factors. Discussion The carboxylate groups have a strong ability to bond various metal ions and afford abundant coordination modes, thus rigid carboxylate ligands have been widely used for the design and synthesis of a variety of structures [1]. Introduction of a sulfonate group into rigid carboxylate ligands may result in the formation of unexpected frameworks as the sulfonic group has a different shape and properties in terms of its coordination ability compared to the carboxylate group [2]. Cu1 atom is five-coordinated by five oxygen atoms from two different L ligands, one OH anion and one water molecule (O1W) in distorted square-pyramidal environment. The Cu2 atom is four-coordinated by four oxygen atoms from one L ligand, the sameOH anion and onewatermolecule (O2W) in a strongly distorted tetrahedral coordination. The L trianions link neighboring Cu(II) atoms to form an one-dimensional chain. Z. Kristallogr. NCS 225 (2010) 309-310 / DOI 10.1524/ncrs.2010.0134 309 © by Oldenbourg Wissenschaftsverlag, Munchen Crystal: green block, size 0.21 × 0.28 × 0.33 mm Wavelength: Mo K+ radiation (0.71073 A) .: 39.93 cm−1 Diffractometer, scan mode: Bruker APEX, #/' 2,max: 52.18° N(hkl)measured, N(hkl)unique: 3158, 2211 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 1851 N(param)refined: 181 Programs: SHELXS-97 [3], SHELXL-97 [4], SHELXTL-PLUS [5] Table 1. Data collection and handling. H(2) 2i 0.3435 −0.1879 0.0613 0.024 H(3) 2i 0.1569 −0.3595 −0.1646 0.025 H(5) 2i −0.2928 −0.2235 −0.0283 0.020 Table 2. Atomic coordinates and displacement parameters (in A). Atom Site x y z Uiso