Crystal structure of diaquabis(1,10-phenanthroline-k2N, N')sodium chloride, [Na(H2O)2(C12H8N2)2]Cl

Abstract

C 24H 20ClN 4 NaO 2 ,monoclinic, P 121 / c 1(no. 14), a =16.352(3) Å, b =15.579(3) Å, c =9.132(2) Å, b =104.54(3)°, V =2251.8 Å 3 , Z =4, R gt (F) =0.056, wRref(F 2 ) =0.161, T =293 K. Source of materialThe title compound was obtainedserendipitously from the reaction of manganic dichloride dihydrate (0.40 g, 2.47 mmol), 1,10-phenanthroline monohydrate (0.13 g, 0.66 mmol), phthalic acid (0.43 g, 2.59 mmol) in water (10 mL), and then the pHwas raised to about 8.5 with 1.0 Msolutionofsodium carbonate. The mixture was stirred for ca. 4h.Subsequently, the resultingsuspension was heated in a2 5m lTeflon-lined stainless steel autoclavea t 453 Kfor 5days. After the autoclave was cooled to room temperature, the solid was filtered off. The resulting yellow filtrate was allowed to stand at room temperature and slow evaporation for two years afforded yellowish block-shapedcrystals. DiscussionSix-coordinatedsodium(I)environments are present in the most of the comparativelyf ew sodium(I)c omplexes, such as in 1,7-bis(2,2¢ -dihydroxybiphen-3-yl)-4,10-dimethyl-1,4,7,10-tetraazacyclododecane)sodium acetonitrile solvate figure, top). The Na-Nbond distances are in the range of 2.460(2) Åto 2.563(2) Å.The Na-O2and Na-O1bond lengths are 2.358(2) Åand 2.401(2) Å,r espectively. The monovalent [Na(H 2 O) 2 (phen) 2 ] + complex cations are interlinked via hydrogen bonds between the Cl -anions and Oatoms of the coordinated water molecules. The chelating phen ligands exhibit nearly perfect co-planarity, each phen ligand is sandwiched by two phen ligands from two neighboring mononuclear complex cations. The mean interplanar distances are 3.469 Åand 3.566 Å,a lternatively, indicating p -p stacking interactions along [010] direction (figure, bottom). Moreover, there are weak hydrogen bonds between Cl -anions and o -phenanthroline H3atoms ( d (C3···Cl1) = 3.706 Å, Ð C3-H3···Cl1 =146.5°). Through the hydrogen bonds and p -p stacking interactions, athree-dimensional supramolecular network is constructed.