10.1021/ic049325x.s002 Scott D. Bunge Scott D. Bunge Timothy J. Boyle Timothy J. Boyle Harry D. Pratt Harry D. Pratt Todd M. Alam Todd M. Alam Mark A. Rodriguez Mark A. Rodriguez Synthesis and Characterization of a Series of Rubidium Alkoxides and Rubidium−Titanium Double Alkoxides American Chemical Society 2004 compound 2 multinuclear NMR spectroscopy n n OAr ligands OCH DMP Compounds 4 OC 6 H 3 tetranuclear structure bipyramidal Ti metal centers terminal ONep ligands Compound 1 Rubidium Alkoxides μ 3 alkoxide 6 CH 3 DIP tetrahedral Ti center terminal py Rb coordination dinculear species 2004-09-20 00:00:00 Journal contribution https://acs.figshare.com/articles/journal_contribution/Synthesis_and_Characterization_of_a_Series_of_Rubidium_Alkoxides_and_Rubidium_Titanium_Double_Alkoxides/3324478 This report investigates the structural aspects of the products isolated from the reactions of a series of titanium alkoxides {[Ti(OR)<sub>4</sub>]<i><sub>n</sub></i> <i>n </i>= 2, OR = OCH<sub>2</sub>C(CH<sub>3</sub>)<sub>3</sub> (ONep) (<b>1</b>); <i>n </i>= 1, OC<sub>6</sub>H<sub>3</sub>(CH<sub>3</sub>)<sub>2</sub>-2,6 (DMP) (<b>2</b>)} with rubidium alkoxides {[Rb(OR)]<sub>∞</sub> where OR = (ONep) (<b>3</b>), (DMP) (<b>4</b>), and OC<sub>6</sub>H<sub>3</sub>(CH(CH<sub>3</sub>)<sub>2</sub>)<sub>2</sub>-2,6 (DIP) (<b>5</b>)}. The resultant double alkoxides were determined by single crystal X-ray diffraction to be [Rb(μ-ONep)<sub>4</sub>(py)Ti(ONep)]<sub>2</sub> (<b>6</b>), [Rb(μ-DMP)Ti(DMP)<sub>4</sub>]<sub>∞</sub> (<b>7</b>), and [Rb(μ-DMP)<sub>2</sub>(μ-ONep)<sub>2</sub>Ti(ONep)]<sub>∞</sub> (<b>8</b>). Compound <b>1</b> is the previously reported dinculear species with trigonal bipyramidal Ti metal centers whereas compound <b>2</b> is a monomer with a tetrahedral Ti center. Suitable X-ray quality crystals of <b>3</b> were not isolated. Compounds <b>4</b> and <b>5</b> demonstrate extended polymeric networks with Rb coordination ranging from two to five utilizing terminal μ- and μ<sub>3</sub>-OR ligands and π-interactions of neighboring OAr ligands. The double alkoxide <b>6</b> revealed a simple tetranuclear structure with μ-ONep acting as the bridge, terminal ONep ligands on the Ti, and one terminal py on the Rb. For <b>7 </b>and <b>8</b>, the π-interaction facilitated the formation of extended polymeric systems. All complexes were further characterized by FT-IR and multinuclear NMR spectroscopy.