Data for "Synthesis of zirconium(IV) and hafnium(IV) isopropoxide, sec-butoxide and tert-butoxide"

Data of the figures in the publication "Synthesis of zirconium(IV) and hafnium(IV) isopropoxide, sec-butoxide and tert-butoxide".

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Table of contents:

Figure 1. The synthesis of zirconium(iv) and hafnium(iv) isopropoxide isopropanol complex. (A) General reaction scheme of both the method making use of ammonia stock solution in isopropanol, and gaseous ammonia, (B) ¹H NMR, and (C) ¹³C NMR of zirconium(iv) and hafnium(iv) isopropoxide isopropanol complex in C₆D₆.

Figure 2. Exchange reaction of zirconium isopropoxide isopropanol complex with the more Lewis base TOPO. (A) General reaction scheme, (B) ¹H NMR of the as-synthesized zirconium(iv) isopropoxide isopropanol complex where the ratio between the three resonances (6.5, 4.5 and 1.5 ppm) equals to 1 : 5 : 30 (= 4 isopropoxides and 1 isopropanol), (C) to which an excess of TOPO is added where the ratio between the three resonances (4.5, 4.0 and 3.0 ppm) equals to 4 : 1 : 1 (confirms the correct stoichiometry of 4 isopropoxides and 1 isopropanol), and (D) ³¹P NMR of the mixture in C₆D₆.

Figure 3. The synthesis of zirconium(iv) and hafnium(iv) diethylamido complex. (A) General reaction scheme, (B) ¹H NMR, and (C) ¹³C NMR of zirconium(iv) and hafnium(iv) diethylamido complex in C₆D₆.

Figure 4. The synthesis of zirconium(iv) and hafnium(iv) tert-butoxide complex. (A) General reaction scheme, (B) ¹H NMR, and (C) ¹³C NMR of zirconium(iv) and hafnium(iv) tert-butoxide complex in C₆D₆.

Figure 5. The synthesis of zirconium(iv) sec-butoxide. (A) General reaction scheme, (B) ¹H NMR, and (C) ¹³C NMR of zirconium(iv) sec-butoxide in C₆D₆.

Figure 6. Interaction of zirconium sec-butoxide with TOPO. (A) ¹H NMR of the as-synthesized zirconium(iv) sec-butoxide to which TOPO is added, and (B) ³¹P NMR of the mixture in C₆D₆.

Figure S1. Schematic diagram of the reversible glass frit and pictures of the air- and moisture-free Schlenk filtration.

Figure S2. Powder XRD of (left) the synthesized Zr(OiPr)4.iPrOH and the calculated powder diffraction pattern from the CSD reference JETWOU, and (right) the synthesized Hf(OiPr)4.iPrOH and the calculated powder diffraction pattern from the CSD reference NAYDAS.