Me2sicl2

Cellulose nanocrystals were supplied by Celluforce (Montreal, QC, Canada). Cyclohexane (reagent grade, purity 99%) was supplied by Sigma Aldrich, and trans-β-farnesene (reagent grade, purity > 99%) was provided by amyris (Emeryville, CA, USA). The Cyclohexane was washed with sulfuric acid and then refluxed in two stages, the first with lithium aluminum hydride and the second with metallic sodium. The trans-β-farnesene was washed two times with a 1 M sodium hydroxide solution, then dried over sodium sulfate and finally distilled under reflux and metallic sodium. Diisobutyl aluminum hydride (DIBAH, 1 M in hexane, reagent grade) and dimethyl dichlorosilane (Me₂SiCl₂, purity > 99.5%) were purchased from Sigma Aldrich. The latter was used in solution with purified Cyclohexane at a concentration of 0.22 M. Neodymium versatate (NdV₃-40, 0.54 M in hexane, reagent grade) was provided by Solvay (Brussels, Belgium).

The β-myrcene monomer (purity of ≈89%, acquired from VENTOS, Barcelona, Spain) was distilled under vacuum pressure in the presence of metallic sodium before use. To remove the organic (aromatic) traces in the industrial-grade cyclohexane, it was washed with concentrated sulfuric acid (200 mL of sulfuric acid per 1 L of cyclohexane) and then cleaned with distilled water until neutral pH was obtained. Afterward, the cyclohexane was dried by double distillation with reflux: the first with lithium aluminum hydride and the second with metallic sodium, all in a nitrogen atmosphere. Both the cyclohexane solvent and distilled β-myrcene were stored in a stainless steel container with a nitrogen atmosphere.
The catalyst system comprised NdV₃ as the catalyst (0.54 M solution in hexanes, reagent grade, obtained from Solvay, Jalisco, Mexico), DIBAH as the cocatalyst (molarity 0.95–1.10 mol L, acquired from Sigma Aldrich, Burlington, MA, USA) and Me₂SiCl₂ (purity > 99.50%, acquired from Sigma Aldrich) as the halide donor. Using distilled cyclohexane, a 0.22 M solution of the Me₂SiCl₂ was prepared. Tetrahydrofuran (THF) HPLC grade (purity > 99.90%, acquired from Sigma Aldrich) was used as the eluent and to prepare the GPC samples.