Raw data for "X-ray studies bridge the molecular and macro length scales during the emergence of CoO assemblies"

<strong>Raw data for „X-ray studies bridge the molecular and macro length scales during the emergence of CoO assemblies“</strong> <strong>TEM and SEM</strong> SEM image of CoO assemblies after 90 min TEM images of CoO assemblies after 5, 10, 15, 20, 40, 60 and 90 min HR-TEM images of CoO assemblies after 90 min ED patterns of CoO assemblies after 10, 15 and 20 min <strong>HERFD-XANES</strong> In situ spectra for the CoO synthesis at 160°C were recorded at beamline ID26 at the European Synchrotron Radiation Facility (ESRF), Grenoble, France. Using a Si (111) double crystal monochromator, the incident energy was varied from 7.70 to 7.78 keV. The emitted fluorescence was measured with an emission spectrometer in Rowland geometry with five Si (531) analyzer crystals aligned at the Bragg angle of 77°. HERFD-XANES spectra were recorded in continuous scan mode every 80 s with average energy steps of 0.05 eV. The data set consists of one file containing a sequential set of energy scans, representing the pre- and main edge regions of the HERFD-XANES spectra. Important column identifiers: incident energy: “arr_hdh_ene” incident intensity: “I02” fluorescence intensity: “apd” <strong>X-ray total scattering</strong> Data was taken at beamline P21.1 of PETRA III at Deutsches Elektronen-Synchrotron (DESY), Hamburg, Germany. Diffraction patterns were recorded every 10 s at an X-ray energy of 102.92 keV (λ = 0.121 Å) with an XRD1621 detector (Perkin Elmer Inc., USA) with a pixel size of 200 × 200 μm² and a sample-to-detector distance of 0.411 m. The dataset consist of in situ data set of CoO nanoassembly synthesis at 160°C in situ data set of CoO nanoassembly synthesis at 140°C ex situ samples prepared at 160 °C at different times commercial reference compounds in powder and 0.1 M BnOH solution data format: 2D scattering patterns in .tif format The total scattering data is split into individual archives for the above subsets. <strong>SAXS and PXRD</strong> <strong>data set “laboratory_SAXS_data”:</strong> Data were recorded with the laboratory molybdenum anode microfocus X-ray setup at LMU, Munich. SAXS data are multiple successive 20 min exposures. Transmission data are 10 s exposures with the beamstop removed. data format: .tif detector images recorded with a Dectris Pilatus 300K.<br> <em>X-ray wavelength:</em> 0.71075 Angstrom<br> Calibrant for sample-to-detector distance, beam center and detector tilt: Silver behenate (AgBeh) <strong>data set “synchrotron_SAXS_data”:</strong> Data were recorded at beamline P03 at PETRA III, DESY, Hamburg. Data are recorded separately at a long and a short sample-to-detector distance. At the long distance, the exposure time is 5x0.1s. At the short distance, the exposure time is 1x0.5s. data format: .cbf detector images recorded with a Dectris Pilatus 1M.<br> X-ray wavelength: 0.961 Angstrom<br> Calibrant for sample-to-detector distance, beam center and detector tilt: Silver behenate (AgBeh) <strong>data set “laboratory_PXRD_data”:</strong> Data were recorded with the laboratory molybdenum anode microfocus X-ray setup at LMU, Munich. The overlap for stitching is 10 px in both horizontal and vertical direction. The recording sequence is<br> 01 02 07<br> 03 04 08<br> 05 06 09<br> 10 11 12<br> 13 14 15<br> with 3 images at each position, to take the median. The exposure time per image is 1200 s. For LaB6 the sequence is<br> 01 02<br> 03 04<br> 05 06<br> 07 08<br> 09 10<br> with 5 images at each position, to take the median. The exposure time per image is 300 s. data format: .tif detector images recorded with a Dectris Pilatus 100K.<br> X-ray wavelength: 0.71 Angstrom<br> Calibrant for sample-to-detector distance, beam center and detector tilt: Lanthanum hexaboride NIST SRM 660c (LaB6)《X射线研究揭示CoO组装体形成过程中分子与宏观尺度的桥梁效应》原始数据 <strong>透射电子显微镜（TEM）与扫描电子显微镜（SEM）</strong> 反应90分钟后的CoO组装体SEM图像；反应5、10、15、20、40、60及90分钟后的CoO组装体TEM图像；反应90分钟后的CoO组装体高分辨透射电子显微镜（HR-TEM）图像；反应10、15及20分钟后的CoO组装体电子衍射（ED）图谱 <strong>高能量分辨荧光检测X射线吸收近边结构光谱（HERFD-XANES）</strong> 于法国格勒诺布尔欧洲同步辐射装置（ESRF）的ID26光束线采集了160°C下CoO合成过程的原位光谱。采用Si(111)双晶单色仪，入射能量扫描范围为7.70至7.78 keV。发射荧光通过罗兰圆几何结构的发射光谱仪进行检测，该系统搭载5块对准77°布拉格角的Si(531)分析晶体。HERFD-XANES光谱以连续扫描模式采集，每80秒记录一组，能量步长平均值为0.05 eV。本数据集包含一个文件，其中包含一系列连续的能量扫描数据，涵盖HERFD-XANES光谱的预边和主边区域。关键列标识符如下：入射能量："arr_hdh_ene"；入射强度："I02"；荧光强度："apd" <strong>X射线全散射</strong> 实验数据采集于德国汉堡德国电子同步加速器（DESY）的PETRA III装置P21.1光束线。X射线能量设定为102.92 keV（波长λ=0.121 Å），采用XRD1621探测器（Perkin Elmer Inc.，美国），探测器像素尺寸为200×200 μm²，样品-探测器距离为0.411 m，每10秒记录一组衍射图谱。本数据集包含以下内容：160°C下CoO纳米组装体合成的原位数据集、140°C下CoO纳米组装体合成的原位数据集、160°C下不同反应时间制备的非原位样品、粉末态及0.1 M苄醇（BnOH）溶液态的商用参比化合物。数据格式为.tif格式的二维散射图案。全散射数据按上述子集拆分为独立归档文件。 <strong>小角X射线散射（SAXS）与粉末X射线衍射（PXRD）</strong> <strong>"实验室SAXS数据集（laboratory_SAXS_data）"：</strong> 数据采集于德国慕尼黑路德维希-马克西米利安大学（LMU）的实验室钼阳极微聚焦X射线装置。SAXS数据为多组连续20分钟曝光的结果；透射数据为移除光阑后的10秒曝光数据。数据格式为.tif格式，由Dectris Pilatus 300K探测器采集。<br> <em>X射线波长：</em>0.71075 埃<br> 用于校准样品-探测器距离、光束中心及探测器倾斜度的标准物质：山嵛酸银（AgBeh） <strong>"同步辐射SAXS数据集（synchrotron_SAXS_data）"：</strong> 数据采集于德国汉堡DESY的PETRA III装置P03光束线。分别在长、短两种样品-探测器距离下采集数据：长距离模式下，曝光时间为5×0.1秒；短距离模式下，曝光时间为1×0.5秒。数据格式为.cbf格式，由Dectris Pilatus 1M探测器采集。<br> X射线波长：0.961 埃<br> 校准标准物质：山嵛酸银（AgBeh） <strong>"实验室PXRD数据集（laboratory_PXRD_data）"：</strong> 数据采集于LMU慕尼黑的实验室钼阳极微聚焦X射线装置。图像拼接时水平与垂直方向的重叠区域均为10像素。采集序列如下：<br> 01 02 07<br> 03 04 08<br> 05 06 09<br> 10 11 12<br> 13 14 15<br> 每个位置采集3张图像以取中位数，单张图像曝光时间为1200秒。六硼化镧（LaB6）标准样品的采集序列为：<br> 01 02<br> 03 04<br> 05 06<br> 07 08<br> 09 10<br> 每个位置采集5张图像以取中位数，单张图像曝光时间为300秒。数据格式为.tif格式，由Dectris Pilatus 100K探测器采集。<br> X射线波长：0.71 埃<br> 校准标准物质：六硼化镧NIST SRM 660c（LaB6）