C 32 H 32 Mn 2 N 8 O 12 ,orthorhombic, Pccn (no. 56), a =13.028(2) Å, b =19.081(3) Å, c =7.
Source of materialMn(CH 3 COO) 2 · 4H 2 O(0.123 g, 0.5 mmol) and 4,4'-bipyridine (0.96 g, 0.5 mmol) were refluxed in anhydrous methanol (10 ml) for 50 min, then, cyanoacetic acid (0.88 g, 1mmol) was added. The pH value was adjusted to 3with 0.5 MCH 3 COOH solution. The mixture was further stirred for 2h,then filtered. The resulting clear solution was diffused with diethyl ether vapor at room temperature for two weeks. Dark green crystals were obtained, collected by filtration and dried in air (yield, 0.156 g, 37 %). Elemental analysis -found: C, 46.48 %; H, 34.59 %; N, 13.46.%; calculated for C32H32N8O12Mn2:C ,4 6.27 %; H, 34.88.%; N, 13.49 %. IR data are available in the CIF.
Experimental detailsThe positions of the water hydrogen atoms were found from Fourier difference synthesis and refined isotropically. The remaining hydrogen atoms were generated theoretically, and included as fixed contributions without futher refinement.