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New linear heterometallic Co3Li2 and Co4Li2 arrays have been assembled with the use of disiloxanediolate and silsesquioxane ligands. Treatment of anhydrous CoCl2 with in situ‐prepared (Ph2SiOLi)2O afforded (thf)Co[Co{μ‐(Ph2SiO)2O}{(μ‐Cl)2Li(thf)2}]2 (5) as dark blue prisms in 73 % yield, while the analogous reaction of CoCl2 with in situ‐prepared Cy7Si7O9(OLi)3 (Cy = cyclohexyl) gave royal blue [Co...
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