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.