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Spontaneous self\u2010assembly (SSA) is a primary approach that proceeds by broad screening, typically with simple, flexible ligands and available metal salts. The \u201cdirect synthesis\u201d is a class of SSA, but prescribes the use of zero\u2010valent metal(s) as a starting material, typically oxidized by air oxygen, which results in a deficiency of anions in the reaction mixture and forces deprotonation of the protic ligand(s) with the formation of unexpected products. The \u201cdirect synthesis\u201d approach has been successfully applied to the preparation of heterometallic complexes, which has allowed the isolation of numerous complexes, many with uncommon structures. In this review we summarize our experience in the field of the \u201cdirect synthesis\u201d of polynuclear heterometallic complexes, covering preparative and structural aspects as well as applications of the compounds obtained.<\/jats:p>","DOI":"10.1002\/ejic.201402266","type":"journal-article","created":{"date-parts":[[2014,7,18]],"date-time":"2014-07-18T03:57:51Z","timestamp":1405655871000},"page":"4496-4517","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":40,"title":["Polynuclear Heterometallic Complexes from Metal Powders: The \u201cDirect Synthesis\u201d Approach"],"prefix":"10.1002","volume":"2014","author":[{"given":"Dmytro S.","family":"Nesterov","sequence":"first","affiliation":[]},{"given":"Oksana V.","family":"Nesterova","sequence":"additional","affiliation":[]},{"given":"Vladimir N.","family":"Kokozay","sequence":"additional","affiliation":[]},{"given":"Armando J. 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