fIAPP and hf-IAPP/Nle3-VF were made by aging IAPP (1024 µM) or a mixture of IAPP (1024 µM) and Nle3-VF (2048 µM) in ddH2O for 3 days. A droplet of each solution was placed between glass rods supported by plasticine balls and allowed to dry (humidified atmosphere, 2–4 days, RT). X-ray diffraction data were collected at the facility Single-Crystal X-Ray Diffractometry of the TUM Catalysis Research Center (CRC) using a Bruker D8 Venture diffractometer equipped with a CPAD detector (Bruker Photon II), an IMS micro source with CuKα radiation (λ = 1.54178 Å) and a Helios optic using the APEX3 software package (Version 2019–1.0, Bruker AXS Inc., Madison, Wisconsin, USA, 2019).
Apex3
Manufactured by Bruker
Sourced in United States
The APEX3 is a high-performance nuclear magnetic resonance (NMR) spectrometer produced by Bruker. It is designed to provide precise and reliable data for chemical analysis and structural characterization of materials. The APEX3 offers advanced capabilities for a wide range of NMR applications.
Automatically generated - may contain errors
Lab products found in correlation
D8 venture, by Bruker (10 mentions)
D8 quest, by Bruker (7 mentions)
D8 quest eco, by Bruker (4 mentions)
D8 quest diffractometer, by Bruker (3 mentions)
Shelxtl suite, by Bruker (2 mentions)
Smart apex 2 ccd diffractometer, by Bruker (2 mentions)
Sadabs, by Bruker (2 mentions)
Synergy ds diffractometer, by Rigaku (2 mentions)
Shelxtl, by Bruker (2 mentions)
Apex 2 diffractometer, by Bruker (2 mentions)
Infinity cell, by Bruker (2 mentions)
7.0 tesla superconducting magnet, by Bruker (2 mentions)
Photon100 cmos detector, by Bruker (2 mentions)
Miniflex 600, by Rigaku (2 mentions)
Xcalibur 2, by Rigaku (2 mentions)
Crysalis program package, by Rigaku (2 mentions)
Micromount, by MiTeGen (1 mentions)
Photon 100 cmos detector, by Oxford Cryosystems (1 mentions)
Cryostream 800 plus, by Oxford Cryosystems (1 mentions)
Shelxtl software package, by Bruker (1 mentions)
61 protocols using apex3
1
Structural Analysis of Amyloid Fibrils
2
Single Crystal X-Ray Diffraction Analysis
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A colourless plate-like crystal of 8 with dimensions of 0.11 × 0.19 × 0.22 mm, selected under the polarising microscope (Leica M165Z), was mounted on a MicroMount (MiTeGen, USA) consisting of a thin polymer tip with a wicking aperture. The X-ray diffraction measurements were carried out on a Bruker kappa-II CCD diffractometer at 150 K using IµS Incoatec Microfocus Source with Mo Kα radiation (λ = 0.710723 Å). The single crystal, mounted on the goniometer using a cryo-loop for intensity measurements, was coated with immersion oil type NVH and then quickly transferred to the cold nitrogen stream generated by an Oxford Cryostream 700 series. Symmetry-related absorption corrections using the program SADABS [33 ] were applied, and the data were corrected for Lorentz and polarisation effects using Bruker APEX3 software [33 ]. The structure was solved by program SHELXT [34 (link)] (with intrinsic phasing), and the full-matrix least-square refinements were carried out using SHELXL-2014 [35 (link)] through Olex2 [36 (link)] suite of software. The non-hydrogen atoms were refined anisotropically. Molecular graphics were generated using Mercury [37 (link)]. Key crystallographic data and refinement details are presented in Table 1 .
3
X-ray Crystallographic Data Collection and Analysis
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X-ray crystal structure data was collected in each case from a multi-faceted crystal of suitable size and quality selected from a representative sample of crystals of the same habit using an optical microscope. The crystals were mounted on MiTiGen loops and data collection carried out in a cold stream of nitrogen (150 K; Bruker D8 QUEST ECO; Mo Kα radiation). All diffractometer manipulations were carried out using Bruker APEX3 software.41 (link) Structure solution and refinement was carried out using XS, XT and XL software, embedded within Olex2.42 (link) For each structure, the absence of additional symmetry was confirmed using ADDSYM incorporated in the PLATON program.43 (link)
4
Single Crystal Structure of Compound 3
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Single crystals of 3 were grown by slow vapor diffusion of hexanes into ethyl acetate solutions of 3 . Intensity data were collected on a Bruker D8 Venture kappa diffractometer equipped with a Photon II detector. An Iμs microfocus source provided the Mo Kα radiation (λ = 0.71073 A) that was monochromated with multilayer mirrors. The collection, cell refinement, and integration of intensity data were carried out with the APEX3 software (Bruker, 2018 ). A multi-scan absorption correction was performed with SADABS (Krause et al., 2015 (link)). The initial structure solution was solved with the intrinsic phasing methods SHELXT (Sheldrick, 2015b (link)) and refined with the full-matrix least-squares SHELXL (Sheldrick, 2015a (link)) program. The 1 3 5 and -2 5 4 reflections were omitted from the final refinement due to being partially obscured by the beam stop in some orientations.
Crystal data for 3: C12H12N2O2S, Mr = 248.30, crystal size 0.374 × 0.363 × 0.254 mm3, monoclinic, space group P21/n, a = 7.9829(5), b = 14.2529(8), c = 20.6830(11) Å, α = 90°, β = 91.442(2)°, γ = 90°, V = 2352.6(2) Å3, Z = 8, ρcalcd = 1.402 mg m−3, T = 100 (2) K, R1[F2 > 2σ(F2)] = 0.0288, and wR2 = 0.0790.
Crystal data for 3: C12H12N2O2S, Mr = 248.30, crystal size 0.374 × 0.363 × 0.254 mm3, monoclinic, space group P21/n, a = 7.9829(5), b = 14.2529(8), c = 20.6830(11) Å, α = 90°, β = 91.442(2)°, γ = 90°, V = 2352.6(2) Å3, Z = 8, ρcalcd = 1.402 mg m−3, T = 100 (2) K, R1[F2 > 2σ(F2)] = 0.0288, and wR2 = 0.0790.
5
Single Crystal X-Ray Diffraction Analysis
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Suitable single crystals of 1,10-phenatroline-1-N-oxide derivatives were mounted on the Mitegen loops with oil. Data sets were collected at 100 K or room temperature on a Bruker D8 Venture (SC-XRD) diffractometer (Bruker Daltonik, Bremen, Germany) system using INCOATEC IμS 3.0 dual (Mo, Cu) sealed tube microsources (Mo-Kα irradiation (λ = 0.71073 Å) was applied for all measurements). and Photon II Charge-integrating Pixel Array detector. Bruker APEX3 software was applied to collect and made the absorption correction using the MULTI-SCAN method and integration of the data sets [45 ]. The structures were solved by the direct method using SHELXT [46 (link)] and refined on F2 data using full matrix least-squares by SHELXL [47 (link)], were managed with OLEX2 [48 (link)] and WinGX software suites [49 (link)]. All non-hydrogen atoms were refined anisotropically. All hydrogens were included in the model at geometrically calculated positions and refined using the riding model. OH (water) hydrogens were located on the difference electron density map.
The optimized structures of the compounds were analyzed using PLATON [50 (link)]; publication materials were prepared with the Mercury CSD-4.3.0 [51 (link)] and OLEX2 software.
The crystallographic data for all compounds were deposited in the Cambridge Crystallographic Data Centre (CCDC) with the No. CCDC 2075043, 2075044, 2075045, 2075046.
The optimized structures of the compounds were analyzed using PLATON [50 (link)]; publication materials were prepared with the Mercury CSD-4.3.0 [51 (link)] and OLEX2 software.
The crystallographic data for all compounds were deposited in the Cambridge Crystallographic Data Centre (CCDC) with the No. CCDC 2075043, 2075044, 2075045, 2075046.
6
X-ray Diffraction Structural Characterization
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The selected crystal was mounted on MiTeGen® loops in Paratone oil on a Bruker D8 diffractometer equipped with a PHOTON100 CMOS detector and Oxford Cryosystems Cryostream 800 plus, on beamline 11.3.1 of the Advanced Light Source at LBNL. A sphere of data were collected at 100 K using Bruker APEX3 software27 in shutterless mode with ω rotations at fixed φ values at λ = 0.7749 Å, from a channel cut silicon [111] monochromator. The intensity data were integrated and corrections applied with SAINT v8.34a,28 absorption and other corrections were made using TWINABS 2012/1.29 (link) Dispersion corrections appropriate for this wavelength were calculated using the Brennan method in XDIP with in WinGX.30 (link) The structures were solved with a dual space method with SHELXT 2014/4 and refined using SHELXL 2014/7.31 (link) Once the refinement had converged, SQUEEZE was used to mask the electron density in the pores.32 (link)
7
Single-Crystal X-Ray Structural Analysis
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X-ray data was collected from multi-faceted crystals of suitable size and quality selected from a representative sample of crystals of the same habit using an optical microscope. Each crystal was mounted on a MiTiGen loop and data collection carried out in a cold stream of nitrogen (150 K; Bruker D8 QUEST ECO; Mo Kα radiation). All diffractometer manipulations were carried out using Bruker APEX3 software. 42 Structure solution and refinement was carried out using XS, XT and XL software, embedded within OLEX2. 43 For each structure, the absence of additional symmetry was confirmed using ADDSYM incorporated in the PLATON program. 44
8
X-ray Structural Characterization of Halogenated Compounds
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X-ray crystal structure data was using collected from multi-faceted crystals of suitable size and quality selected from a representative sample of crystals of the same habit using an optical microscope. In each case, crystals were mounted on MiTiGen loops with data collection carried out in a cold stream of nitrogen (150 K; Bruker D8 QUEST ECO ). All diffractometer manipulations were carried out using Bruker APEX3 software. 49 Structure solution and refinement was carried out using XS, XT and XL software, embedded within the Bruker SHELXTL suite. 50 For each structure, the absence of additional symmetry was confirmed using ADDSYM incorporated in the PLATON program. Crystal structure data for 3-Br: X-ray quality crystals were grown following diffusion of diethylether vapor into CH2Cl2 at room temperature. Crystal structure parameters: Crystal structure data for 3-I: X-ray quality crystals were grown following diffusion of diethylether vapor into CH2Cl2 at room temperature. Crystal structure parameters:
9
X-ray Crystallographic Structure Determination
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X-ray crystal structure data was using collected from a multi-faceted crystals of suitable size and quality selected from a representative sample of crystals of the same habit using an optical microscope. The crystal was mounted on MiTiGen loops with data collection carried out in a cold stream of nitrogen (150 K; Bruker D8 QUEST ECO; Mo K α radiation). All diffractometer manipulations were carried out using Bruker APEX3 software. 58 Structure solution and refinement was carried out using XS and XL software, embedded within the Bruker SHELXTL suite. 59 The absence of additional symmetry was confirmed using ADDSYM incorporated in the PLATON program. 60
10
Separation and X-ray Structural Analysis of Chiral Compound S37
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The racemate S37 had been separated into its enantiomers S37a (eluted first) and S37b (eluted second) by chiral high-performance liquid chromatography, as described previously (Marcinkowski et al., 2019) .
Crystals could be obtained from a super-saturated solution of S37a in 1,4-dioxane. Diffraction data were collected on a Bruker-AXS D8 Venture instrument equipped with an Incoatec Microfocus Source using Cu Ka radiation and a Photon detector. The APEX3 software (Bruker AXS Inc., 2016) was used for data collection and reduction. The structure was solved and refined using SHELXT (Sheldrick, 2015b) and SHELXL (Sheldrick, 2015a) , respectively. The absolute configuration of 37a was unequivocally determined by an X-ray crystal structure analysis by anomalous dispersion with a Flack parameter of 0.037(4). ORTEP for Windows (Farrugia, 1997) was used to create the drawing of the structure.
Crystals could be obtained from a super-saturated solution of S37a in 1,4-dioxane. Diffraction data were collected on a Bruker-AXS D8 Venture instrument equipped with an Incoatec Microfocus Source using Cu Ka radiation and a Photon detector. The APEX3 software (Bruker AXS Inc., 2016) was used for data collection and reduction. The structure was solved and refined using SHELXT (Sheldrick, 2015b) and SHELXL (Sheldrick, 2015a) , respectively. The absolute configuration of 37a was unequivocally determined by an X-ray crystal structure analysis by anomalous dispersion with a Flack parameter of 0.037(4). ORTEP for Windows (Farrugia, 1997) was used to create the drawing of the structure.
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