Source of materialAsolution of bis(2-hydroxyethyl)selenide (0.17 g, 1.00 mmol) in CH 2 Cl 2 (10 ml) was added to as tirred mixture of [CN(iPr) C 2 Me 2 N(iPr)] (0.36 g, 2.00 mmol) and MoO 2 Cl 2 (0.20 g, 1.00 mmol) in CH 2Cl2 (10 ml) at 0°C. The mixture of the reaction was allowed to come to room temperature and stirred overnight. The resulting suspension was filtered. The filtrate was concentrated to ca. 10 ml in vacuo and diethyl ether (5 ml) was added. The solution was stored overnight at room temperature to yield yellow crystals suitable for X-ray diffraction analysis. Crystals were collected on afilter, washed once with diethyl ether (5 ml) and dried in vacuo. Elemental analysis -found: C, 22.84 %; H, 3.72 %; N, 4.62 %; calculated for C 22H42Mo6N4O19:C,21.27 %; H, 3.41 %; N, 4.51 %.
Experimental detailsHydrogen atoms bound to carbon atoms were positioned geometrically and refined using ariding model, with d(C-H) =0.95 Å (CH), 0.98 Å (CH 3 )and U iso (H) =1.2 U eq (CH) or 1.5 U eq (CH 3 ).
DiscussionThe hexamolybdate cluster [Mo 6O19] 2-features six terminal oxygen atoms aligned along the unit cell axes, which could make it serve as an octahedrally-directing template. So the hexamolybdate has been extensively studied and employed as build-