The XRD pattern was measured used a Bruker D8 QUEST. The SEM images were recorded on a SU8000 Schottky field emission scanning electron microscope (SFE-SEM) equipped with a Rontec EDX system. The UV-Vis absorbance spectra were recorded on a Lambda 35 UV-Vis spectrophotometer. X-ray photoelectron spectra (XPS) were recorded on a Thermo Scientific ESCALAB 250 instrument (150 W, spot size of 500 μm and Al Kα radiation at 1486.6 eV) to obtain the surface elements. Photoluminescence (PL) spectroscopy measurement was performed on a Cary Eclipse spectrophotometer.
D8 quest
Manufactured by Bruker
Sourced in United States, Germany
The D8 Quest is a versatile X-ray diffractometer designed for a wide range of applications. It features a high-performance, air-cooled X-ray source and a state-of-the-art 2D detector, providing efficient data collection and analysis.
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Lab products found in correlation
Apex3, by Bruker (7 mentions)
Escalab 250xi, by Thermo Fisher Scientific (4 mentions)
Escalab 250, by Thermo Fisher Scientific (3 mentions)
Apex3 suite, by Bruker (2 mentions)
Shelxt, by Bruker (2 mentions)
Photon 100, by Bruker (2 mentions)
Shelxtl, by Bruker (2 mentions)
Apexiv suite2022, by Bruker (2 mentions)
Shelxtl software package, by Bruker (2 mentions)
Apex2, by Bruker (2 mentions)
Low temperature device, by Oxford Cryosystems (2 mentions)
Q exactive, by Thermo Fisher Scientific (2 mentions)
Eclipse spectrophotometer, by Agilent Technologies (1 mentions)
Tecnai g2 f30, by Thermo Fisher Scientific (1 mentions)
Alpha 300r, by WITec (1 mentions)
Dimension fastscan, by Bruker (1 mentions)
E4980a precision lcr meter, by Agilent Technologies (1 mentions)
Lambda 950, by PerkinElmer (1 mentions)
Smartlab 9 kw, by Rigaku (1 mentions)
Kappa apex 2, by Bruker (1 mentions)
98 protocols using d8 quest
1
Multi-Technique Material Characterization
2
Comprehensive Material Characterization
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The surface morphologies and thicknesses were studied by an AFM (Dimension Fast Scan, Bruker), the microstructure and the composition were confirmed through a TEM (Tecnai G2 F30, FEI), EDX, XRD (D8QUEST, Bruker), and XPS (ESCALab250 Xi, Thermo Fisher Scientific), and Raman and PL spectra were carried out on a confocal Raman/PL system (Alpha 300R, WITec).
3
X-ray Diffraction Analysis of Crystallographic Complexes
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The X-ray diffraction data were collected on a Bruker Smart Apex I (1 , 8 ), Oxford Xcalibur Eos (3 –5 , 12 ) and Bruker D8 Quest (10 , 13 ) diffractometers (Mo-Kα radiation, ω-scan technique, λ = 0.71073 Å). The intensity data were integrated by SAINT (1 , 8 , 10 , 13 ) [84 ] and CrysAlisPro (3 –5 , 12 ) [85 ] programs. SADABS program (1 , 8 , 10 , 13 ) [86 (link)] and SCALE3 ABSPACK algorithm (3 -5 , 12 ) [85 ] were used to perform absorption corrections. All structures were solved by dual method [87 (link)] and refined on using SHELXTL package [88 (link)]. All non-hydrogen atoms were refined anisotropically. The hydrogen atoms were placed in calculated positions and were refined in the riding model (Uiso(H) = 1.5 Ueq(C) for CH3-groups and Uiso(H) = 1.2 Ueq(C) for other groups). The main crystallographic data and structure refinement details for all complexes are presented in Table S1 . CCDC 2174897 (1 ), 2174898 (3 ), 2174899 (4 ∙n-hexane), 2174900 (5 ; low resolution-IAM), 2174901 (5 ; high resolution-IAM), 2174902 (5 ; high resolution multipole refinement), 2174903 (8 ∙toluene), 2174904 (10∙ 3.5toluene), 2174905 (12∙ 0.25toluene), and 2174906 (13 ∙6toluene) contain the supplementary crystallographic data. These data can also be obtained free of charge at ccdc.cam.ac.uk/structures/ (accessed on 19 September 2022) from the Cambridge Crystallographic Data Centre.
4
Characterization of FAPbI3 Single Crystals
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Powder XRD measurements were performed using a Rigaku (SmartLab-9 kW) x-ray diffractometer equipped with a Cu tube operated at 40 kV and 20 mA. Single-crystal XRD was measured on a Bruker (D8 Quest) x-ray diffractometer. The UV-Vis-NIR absorbance of the FAPbI3 SCs was studied using a spectrophotometer (PerkinElmer, Lambda 950) equipped with an integrating sphere. Photoluminescence spectra were collected using a PicoQuant FT-300 and MT-100 spectrometer, and a 510-nm laser was used as the pulsed excitation source. Capacitance of the SCs at different frequencies was measured in the dark by an impedance analyzer (Agilent-E4980A Precision LCR Meter). The conductivity of the SCs at different temperature was measured using a high-precision source meter (Keysight B2902A). X-ray photoelectron spectroscopy spectra were acquired with a photoelectron spectrometer (Thermo Fisher Scientific, Escalab-250Xi). All the photographs of the FAPbI3 SCs were taken using a digital camera.
5
Nuclear Magnetic Resonance and X-ray Diffraction Analysis
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1H and 13C Nuclear Magnetic Resonance (NMR) spectra were recorded using a 400 MHz Bruker (Billerica, MA, USA) instrument or using a 500 MHz JEOL system (Peabody, MA, USA) equipped with a Royal HFX probe in the deuterated solvents described in each experimental procedure. The chemical shifts (δ) are described in parts per million (ppm) downfield from an internal standard of tetramethylsilane (TMS). Melting points (°C) were obtained on an SMP30 melting point apparatus and are uncorrected. High-Resolution Mass Spectrometry (HRMS) was recorded using the analytical service within the Centre of Marine Sciences (CCMAR, Algarve, Portugal) and was conducted on a Thermo Scientific High Resolution Mass Spectrometer (HRMS) (Waltham, MA, USA), model Orbitrap Elite, capable of MSn, n up to 10. X-ray diffraction data were collected on Bruker Kappa Apex II and D8 Quest diffractometers (Billerica, MA, USA) using graphite monochromated MoKα (λ = 0.71073 Å) radiation (see Section 3.4 for more details).
Safety. Organic peroxides are potentially hazardous compounds (inflammable and explosive) and must be handled carefully: (1) a safety shield should be used for all reactions involving H2O2; (2) direct exposure to strong heat or light, mechanical shock, oxidizable organic materials, or transition-metal ions should be avoided.
Safety. Organic peroxides are potentially hazardous compounds (inflammable and explosive) and must be handled carefully: (1) a safety shield should be used for all reactions involving H2O2; (2) direct exposure to strong heat or light, mechanical shock, oxidizable organic materials, or transition-metal ions should be avoided.
6
Single-Crystal XRD Analysis of Compound 1
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A suitable single crystal with dimensions of 0.20 × 0.21 × 0.22 mm3 of compound 1 was carefully selected under an optical microscope for single crystal XRD analysis. Single-crystal structure determination by X-ray diffraction was performed on a Bruker D8 Quest diffractometer with graphite-monochromated Mo-Kα (λ = 0.71073 Å) radiation at a temperature of 296 K. Data processing was accomplished with the saint-processing program. The structure was solved by a direct method using the SHELXTL-2014 crystallographic software package.41,42 The zinc and sulphur atoms were first located, whereas the carbon, nitrogen and oxygen atoms were found in the different Fourier maps. All the hydrogen atoms were placed geometrically and refined in a riding model. All of the non-hydrogen atoms were refined anisotropically.
The detailed crystallographic data and selected bond lengths as well as the bond angles for compound 1 are listed inTable 1 and S1.† CCDC-1892957 contains the supplementary crystallographic data for this paper.
The detailed crystallographic data and selected bond lengths as well as the bond angles for compound 1 are listed in
7
Glycine-Sulfamic Acid Cocrystal Structure
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The crystal structure
of the glycine–sulfamic acid 2:1 ionic cocrystal was determined
at −100 °C on a Bruker D8 Quest fixed-χ single-crystal
diffractometer equipped with a sealed-tube X-ray source that delivers
Mo Kα (λ = 0.71073 Å), a TRIUMPH monochromator, a
PHOTON 100 detector, and a nitrogen-flow Oxford Cryosystem attachment.
Unit cell determination, data reduction, and absorption correction
(multiscan method) were conducted using the Bruker APEX3 suite.31 Using Olex2,32 (link) the
structure was solved with the ShelXT structure solution program33 (link) using intrinsic phasing and refined with the
ShelXL refinement package34 (link) using least-squares
minimization.
of the glycine–sulfamic acid 2:1 ionic cocrystal was determined
at −100 °C on a Bruker D8 Quest fixed-χ single-crystal
diffractometer equipped with a sealed-tube X-ray source that delivers
Mo Kα (λ = 0.71073 Å), a TRIUMPH monochromator, a
PHOTON 100 detector, and a nitrogen-flow Oxford Cryosystem attachment.
Unit cell determination, data reduction, and absorption correction
(multiscan method) were conducted using the Bruker APEX3 suite.31 Using Olex2,32 (link) the
structure was solved with the ShelXT structure solution program33 (link) using intrinsic phasing and refined with the
ShelXL refinement package34 (link) using least-squares
minimization.
8
Comprehensive Analytical Characterization
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Optical rotations were measured with a Jasco P-1020 polarimeter. UV spectra were obtained using a Shimadzu UV-2401A spectrophotometer. A Tenor 27 spectrophotometer was used for IR spectra as KBr pellets. 1D and 2D NMR spectra were recorded on Bruker spectrometer with TMS as internal standard. HRESIMS was performed on a triple quadrupole mass spectrometer. Semi-preparative HPLC was performed on an Agilent 1100 liquid chromatograph with a Waters X-Bridge Prep Shield RP18 (10 × 150 mm) column. Column chromatography (CC) was performed using silica gel (100–200 mesh and 300–400 mesh, Qingdao Marine Chemical, Inc., Qingdao, People's Republic of China) and Sephadex LH-20 (40–70 μm, Amersham Pharmacia Biotech AB, Uppsala, Sweden). Microplate reader (BioTek ELx800) was used in antibacterial assay. X-ray diffraction was carried out on BRUKER D8 QUEST.
9
Single Crystal X-Ray Diffraction Analysis
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Single crystal X-ray diffraction (SXRD) measurements were collected on a Bruker D8 Quest diffractometer with sealed tube (MoKa radiation) and Triumph monochromator (λ = 0.71073 Å). The software package Saint was used for the intensity integration39 . Absorption correction was performed with SADABS40 .The structures were solved with direct methods using SHELXT41 (link). Least-squares refinement was performed with SHELXL-201442 (link) against of all reflections. Non-hydrogen atoms were refined freely with anisotropic displacement parameters. Hydrogen atoms were placed on calculated positions or located in difference Fourier maps. All calculated hydrogen atoms were refined with a riding model. For high temperature SXRD, the crystal was sealed in a capillary and an Oxford Cryostream 700 plus was used to heat the crystal to the desired temperature.
10
Crystalline Structure Characterization of Synthesized Nanoparticles
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The crystalline structure characterization
of the synthesized NPs was carried out on a Bruker D8 QUEST single
crystal diffractometer recorded using Cu Kαλ = 1.5418
Å radiation at room temperature (300 K). Frames were collected
via ω/φ scans and then processed to obtain diffractograms
of intensity vs 2θ between 30 and 90°. The HighScore
Plus software was used for raw data treatment, and a database associated
with the software was implemented for the search-match phase identification
analyses.
of the synthesized NPs was carried out on a Bruker D8 QUEST single
crystal diffractometer recorded using Cu Kαλ = 1.5418
Å radiation at room temperature (300 K). Frames were collected
via ω/φ scans and then processed to obtain diffractograms
of intensity vs 2θ between 30 and 90°. The HighScore
Plus software was used for raw data treatment, and a database associated
with the software was implemented for the search-match phase identification
analyses.
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