The zip file contains raw experimental data for paper acs_chemmater_7b01761. The data are arranged in the following directories:

(1) Ex situ XRD. This includes xy (ascii) and raw (Bruker format) powder X-ray patterns of spinels prepared at Diamond light source (Figure 4), LDHs prepared offline (Figure 2a, EXP8, and Figure S9, EXP13) and in a subfolder thermodiffractometry (Figure S7b). 

(2) In Situ Diamond XRD data. This includes the two datasets plotted in Figure 1(a) (55140) and Figure 1(c) (55152).

(3) TGA. This contains the thermogravimetric analysis (TGA-DSC-MS) plotted in Figure S7a of the isolated LDH (EXP8). TGA-DSC is LDH.txt and MS is LDH8.acs.

(4) XANES. This contains Co K-edge XANES data plotted in Figure S8 and Figure S11, with filenames according to the sample identity.