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Data for Time-resolved powder X-ray diffraction of the solvothermal crys-tallization of cobalt gallate spinel photocatalyst reveals transient layered double hydroxides Daniel Sean Cook (22102370) Yue Wu (1262184) Karla Lienau (1334529) Rene More (2044663) Reza J. Kashtiban (1423762) Oxana Magdysyuk (5082287) Greta R. Patzke (1396339) Richard I. Walton (1328463) Cobalt Gallates Gallium Hydroxides Migrated from ePrints High energy X-ray diffraction is used to follow in situ the crystallization of a cobalt gallate from metallic gallium under solvothermal conditions in an aminoalcohol, revealing the formation and decay of transient metastable layered double hydroxides. Photocatalytic studies show the spinel product has activity as a water oxidation catalyst for oxygen evolution.<br><br>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. 2017-06-13T00:00:00Z Dataset Dataset 10.82444/warw.33740161.v1 https://figshare.com/articles/dataset/Data_for_Time-resolved_powder_X-ray_diffraction_of_the_solvothermal_crys-tallization_of_cobalt_gallate_spinel_photocatalyst_reveals_transient_layered_double_hydroxides/33740161 CC BY 4.0