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The materials were further investigated by single\u2010crystal XRD and a DFT analysis of their preferential \u201copen and closed\u201d geometries. Conversion of said compounds to their dihydride analogues was undertaken, followed by their application as monomers for polystannane polymer synthesis. The properties of two asymmetrical polystannanes prepared by transition\u2010metal\u2010catalyzed dehydropolymerization of dihydrido(aryl)alkylstannanes (<jats:bold>6<\/jats:bold> and <jats:bold>9<\/jats:bold>) were investigated. The first product was the structurally simple, modest molecular weight, semi\u2010crystalline light\u2010 and moisture\u2010stable polystannane <jats:bold>10<\/jats:bold> with NMR (<jats:sup>119<\/jats:sup>Sn) evidence of prominent Sn\u2190O hypercoordination along the polymer backbone. The second was the lower molecular weight, tosylated four\u2010coordinate polystannane <jats:bold>11<\/jats:bold> with no evidence of hypercoordination. Differential scanning calorimetry (DSC) of polymer <jats:bold>10<\/jats:bold> revealed a reversible semi\u2010crystalline nature, whereas an amorphous character was detected for polymer <jats:bold>11<\/jats:bold>. Polystannane <jats:bold>10<\/jats:bold> was also found to be exceptionally stable to both moisture and light (&gt;6\u2005months) and a promising candidate for the design of readily modified (i.e., tunable) polystannane materials.<\/jats:p>","DOI":"10.1002\/chem.201804145","type":"journal-article","created":{"date-parts":[[2018,9,28]],"date-time":"2018-09-28T18:41:54Z","timestamp":1538160114000},"page":"18762-18771","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":13,"title":["Synthesis and Characterization of Readily Modified Poly(aryl)(alkoxy)stannanes by use of Hypercoordinated Sn Monomers"],"prefix":"10.1002","volume":"24","author":[{"given":"Jeffrey","family":"Pau","sequence":"first","affiliation":[{"name":"Advanced Materials Laboratory, Department of Chemistry and Biology Ryerson University  350 Victoria Street Toronto ON M5B 2K3 Canada"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Gloria M.","family":"D'Amaral","sequence":"additional","affiliation":[{"name":"Advanced Materials Laboratory, Department of Chemistry and Biology Ryerson University  350 Victoria Street Toronto ON M5B 2K3 Canada"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6012-0379","authenticated-orcid":false,"given":"Alan J.","family":"Lough","sequence":"additional","affiliation":[{"name":"X-Ray Laboratory, Department of Chemistry University of Toronto  Toronto ON M5H 3H6 Canada"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"R. 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