Source of material (C 4 H 14 N 2 ) 3 [RhCl 6 ] 2 ×2H 2 Ow as obtained according to the previously reported method [1,2]. The solution of N,N'-dimethylethylenediamine (0.12 ml,1.11 mmol) in 3mlofconcentrated hydrochloric acid was carefully added to the test tube containing 0.10 ml solution of RhCl 3 ×3H 2 O(0.15 mmol RhCl 3 )in6mol/l hydrochloric acid covered by an 1mllayer of concentrated hydrochloricacid. Theobtained triple-phase system was left at room temperature forming single crystals.
Experimental detailsAll Hatoms were located in subsequent difference Fourier maps. Theridingmodel was applied to the Hatomsbonded to Cand N atoms,whereas thepositions of thewater Hatoms were refined restrainingt he O-Ha nd H×××Hd istances to 0.83 and 1.35 Å, respectively [10].The isotropicdisplacementparametersofHatomswere constrained to 1.2 and 1.5 times that of the equivalent isotropicdisplacementparametersoftheir parent N/C-methylene andO/C-methylatoms,respectively.
DiscussionCrystal engineering of inorganic-organic hybrid materials is relevant to several important applications including e.g. gas storage, chemical separation and catalysis [3,4]. Halogenidorhodates(III) with organic cations constitute asubgroup of the large family of inorganic-organic hybrids. The properties of those mixed materials relate to both the inorganic rigid structural skeleton that is usually given by the arrangement of isolated [RhX 6 ] 3-octahedra, and to them ore flexible organic substructure. Also, in most cases, along with the mononuclear inorganic anions water molecules and/or aquahydrogen cations are present in the inorganic segments of those solids [5,6].T he asymmetric unit of the title hexachloridorhodate(III)consists of two half isolated inorganic [RhCl 6 ] 3-octahedra,o ne andah alf of thef lexible organic (C 4 H 14 N 2 ) 2+ cations, and one water molecule. The components of the solid are joined by N/C/O-H×××Cl hydrogen bonds. The shortest is an O-H×××Cl bond with the O×××Cl distance of 3.217(2) Å.The most characteristic structural feature of thesolid is the presence of twoi ndependent octahedraw iths ignificantly differente nvironments. The arrangement of chlorido ligands around the central Rh III atomsslightly deviates from the ideal octahedral geometry. The lengths of crystallographically independent Rh-Cl bonds vary from 2.3379(5) to 2.3480(5) Åa nd from 2.3422 (5) octahedron is surrounded by six N8N8 I cations ( I -x,1-y,1-z;all located at inversion centres) and four water molecules, whereas Z. Kristallogr.