X-ray single-crystal diffraction data were collected on a Rigaku Oxford Diffraction SuperNova diffractometer equipped with Atlas CCD detector and micro-focus Cu-Kα radiation (λ = 1.54184Å) for BTI and molecule T3 . For molecules T1 and T2 , crystal data were collected on a BRUKER KappaCCD diffractometer, equipped with a graphite monochromator utilizing MoKα radiation (λ = 0.71073Å). The structures were solved by direct methods and refined on F2 by full matrix least-squares techniques using SHELX programs (G. M. Sheldrick 2014–2016, SHELXT 2014/5 and SHELXL 2016/4). All non-H atoms were refined anisotropically and multiscan empirical absorption was corrected using CrysAlisPro program (CrysAlisPro, Agilent Technologies, V1.171.40.45, 2019) for BTI and molecule T3 and using SADABS program (Sheldrick, Bruker, 2008) for molecules T1 and T2 . The H atoms were included in the calculation without refinement. CCDC 2083265 (BTI ), 2116980 (T1 ), 2116981 (T2 ) and 2116982 (T3 ) contains the supplementary crystallographic data for this paper.
Kappa ccd diffractometer
Manufactured by Bruker
Sourced in United States
The Kappa CCD diffractometer is a single-crystal X-ray diffraction instrument manufactured by Bruker. It is used for the determination of crystal structures and the analysis of chemical compositions. The core function of the Kappa CCD diffractometer is to collect high-quality X-ray diffraction data from single-crystal samples.
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Lab products found in correlation
Crysalis pro, by Agilent Technologies (1 mentions)
Oxford diffraction supernova diffractometer, by Rigaku (1 mentions)
Smart apex 2 diffractometer, by Bruker (1 mentions)
X ray diffractometer, by Rigaku (1 mentions)
Quanta 250 feg, by Thermo Fisher Scientific (1 mentions)
Inova 500, by Bruker (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Drx 400, by Bruker (1 mentions)
Apexii detector, by Bruker (1 mentions)
Melting point apparatus, by Thermo Fisher Scientific (1 mentions)
Avance 2 spectrometer, by Bruker (1 mentions)
13 protocols using kappa ccd diffractometer
1
Single-crystal X-ray Diffraction Analysis
2
X-Ray Crystallography of Organic Compounds
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Example 5
X-Ray Crystallography. X-ray diffraction data were collected on either a Nonius kappaCCD diffractometer (MoK□ X-rays: 1,9-DMeiPrPT) or a Bruker-Nonius X8 Proteum diffractometer (CuK□ X-rays: 1,9-DMeEPT, 1,9-DMePhPT). Raw data were integrated using the Denzo-SMN package23 (kappaCCD) or by APEX2 (X8 Proteum).24 Scaling and merging for all datasets were performed using SADAB S.25 All structures were solved using SHELXT26 and refined with SHELXL-2014/7.27 Hydrogen atoms were included using the riding-model approximation. Non-hydrogen atoms were refined with anisotropic displacement parameters. Atomic scattering factors were taken from the International Tables for Crystallography, vol. C.28 Reference is made to
3
Structural Analysis of HDMPA Polymorphs
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The crystal structures of form II HDMPA were determined by single-crystal X-ray diffraction at both 90 K (low temperature, LT) and 296 K (room temperature, RT).
Data collection was carried out at 90 K on a Nonius kappaCCD diffractometer with MoKα radiation (λ = 0.71073 Å),33 and at 296 K on a Bruker SMART APEX II diffractometer.
Cell refinement and data reduction were done using SCALEPACK and DENZO-SMN for the low temperature structure,34 and SADABS and Bruker SMART for the room temperature structure. Structure solution and refinement were carried out using the SHELXS and SHELXL2016 programs, respectively.35,36 (link)Powder X-ray diffraction (PXRD) data for each sample were collected on a Rigaku X-ray diffractometer with CuKα radiation (40 kV, 40 mA, λ = 1.5406 Å) between 5.0–50.0° (2θ) at ambient temperatures. The finely ground sample was placed on a quartz plate in an aluminum holder.
Data collection was carried out at 90 K on a Nonius kappaCCD diffractometer with MoKα radiation (λ = 0.71073 Å),33 and at 296 K on a Bruker SMART APEX II diffractometer.
Cell refinement and data reduction were done using SCALEPACK and DENZO-SMN for the low temperature structure,34 and SADABS and Bruker SMART for the room temperature structure. Structure solution and refinement were carried out using the SHELXS and SHELXL2016 programs, respectively.35,36 (link)Powder X-ray diffraction (PXRD) data for each sample were collected on a Rigaku X-ray diffractometer with CuKα radiation (40 kV, 40 mA, λ = 1.5406 Å) between 5.0–50.0° (2θ) at ambient temperatures. The finely ground sample was placed on a quartz plate in an aluminum holder.
4
Single-Crystal Structure Determination of Abexinostat Tosylate
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Example 4
A saturated solution of abexinostat tosylate in 2,2,2-trifluoroethanol is prepared by stirring a suspension for 24 hours at ambient temperature, followed by filtration. 1 mL of the resulting solution is then poured into a 1.8-mL HPLC vial, to which 0.25 mL of water is added. The solution is maintained at ambient temperature for 75 minutes. After centrifuging and then drying, the solid is isolated for analysis. From among the crystals obtained a crystal of sufficient quality is taken for single-crystal X-ray diffraction analysis. The crystalline structure of the above single crystal was determined using a Bruker Kappa CCD diffractometer equipped with an FR590 generator having a molybdenum anticathode (λMoKα1=0.7093 Å) with an angular range from 2° to 27.5° in terms of θ. The following parameters were established:
-
- crystal unit cell: triclinic
- unit cell parameters: a=10.467 Å, b=14.631 Å, c=20.159 Å, α=73.971°, β=79.040°, γ=72.683°
- space group: P−1
- number of molecules in the unit cell: 4
- volume of the unit cell: Vunit cell=2813.0 Å3
- density: d=1.345 g/cm3.
5
Structural Analysis of AS Adsorbent Materials
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The crystal structure of the various AS material (AS, AS400, AS600 and AS800) adsorbent materials was investigated by single-crystal X-ray diffraction, XRD investigation was accomplished on a Bruker-Nonius Kappa CCD diffractometer with CuKα radiation source (λ = 1.5406 Å). This measurement was carried out using a diffractometer that worked at 45 kV with a step scan time of 18.87 s. The XRD explored under step–scan mode and the registered intensities of the diffracted X-rays were detected every 0.026° over 2 range of 20–45°. Moreover, the morphologies of the arranged sludge samples were investigated and imaged by field-emission scanning electron microscope with typical magnifications of ×8000 and ×60,000. (SEM) (FE-SEM, Quanta FEG 250, FEI Company, Hillsboro, OR, USA).
6
Characterization of Organic Compounds
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Solvents, inorganic salts and organic reagents were purchased from commercial resources and used without further purification unless otherwise noted. All of the compounds for which analytical and spectroscopic data are quoted were homogeneous by TLC. TLC analyses were performed using silica gel plates (E. Merck silica gel 60 F-254) and components were visualized by the following methods: ultraviolet light absorbance, iodine adsorbed on silica gel, and ninhydrin spray. Melting points were measured with a Kofler apparatus and are uncorrected. Column chromatography was carried out on silica gel (E. Merck, 70–230 mesh). THF was dried over Na in presence of benzophenone under an Ar atmosphere. All the compounds were characterized by 1H and 13C NMR spectroscopy. NMR spectra were recorded using Varian Inova 500 and Bruker DRX-400 spectrometers: chemical shifts are in ppm and J coupling constants in Hz. High-resolution ES mass spectra were obtained with a Micromass Q-TOF UltimaTM API. Optical rotations were measured with a Jasco 1010 polarimeter (k = 589 nm). One suitable crystal was mounted at room temperature on a Bruker–Nonius Kappa-CCD diffractometer.
7
Single-Crystal X-Ray Diffraction Analysis of UPJS-17
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The single‐crystal X‐ray diffraction data set was measured on a Nonius Kappa CCD diffractometer equipped with a Bruker APEX II detector. For UPJS‐17 Cu/Kα (λ=1.54178 Å) at 288(2) K radiation was used. Data reduction was carried out by the diffractometer software. The phase problem was solved by direct methods and refined with full‐matrix least‐squares on F2 using the Shelx‐18 program suite.
[29] Hydrogen atoms were refined isotropically and all other atoms anisotropically. Hydrogen atoms residing on aromatic carbon atoms were included in an ideal position with the C−H bond fixed to 0.95 Å and Uiso(H) assigned to 1.2 Ueq of the adjacent carbon atom. The contribution of guest molecules located in the pores was substracted by the SQUEEZE procedure in Platon.
[18] (link) The structure figures were drawn using DIAMOND software.
[30] Crystal data forUPJS‐17 is summarized in Table S1 in the Supporting Information.
Deposition Number2167706 (for UPJS‐17 ) contains the supplementary crystallographic data for this paper. These data are provided free of charge by the joint Cambridge Crystallographic Data Centre and Fachinformationszentrum Karlsruhe Access Structures service .
[29] Hydrogen atoms were refined isotropically and all other atoms anisotropically. Hydrogen atoms residing on aromatic carbon atoms were included in an ideal position with the C−H bond fixed to 0.95 Å and Uiso(H) assigned to 1.2 Ueq of the adjacent carbon atom. The contribution of guest molecules located in the pores was substracted by the SQUEEZE procedure in Platon.
[18] (link) The structure figures were drawn using DIAMOND software.
[30] Crystal data for
Deposition Number
8
NMR Characterization of Antimicrobial Compounds
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Nuclear magnetic resonance (NMR) experiments were carried out with a 400 MHz Bruker Avance II Spectrometer (Ryerson University) using deuterated chloroform (CDCl3) unless otherwise noted. 1H and 13C spectra were referenced to the residual CHCl3 (7.26 and 77.0 ppm, respectively) solvent signals, while 19F resonance was referenced against the internal standard CFCl3. 29Si NMR was referenced against the internal standard tetramethylsilane (TMS). Peak assignments in the 1H NMR spectra are given in δ (ppm) and were made with the assistance of 2D COSY spectra, while assignments in the 13C NMR spectra (proton-decoupled) were made with the assistance of 2D HSQC spectra. High resolution mass spectrometry (HRMS) was carried out using electrospray ionization time of flight (ESI-ToF). Melting points were measured in open air using a Fisher Scientific melting point apparatus. A Bruker-Nonius Kappa-CCD diffractometer was used to obtain the X-ray information of the crystal structures of two precursor materials 5 (CCDC 1842645 ) and 9 (CCDC 1842536 ) and two active antimicrobials 6a (CCDC 1842528 ), and 10 (CCDC 1842659 ) have been deposited with the Cambridge Crystallographic Data Centre.
9
Single Crystal X-Ray Diffraction Analysis
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Suitable single crystals were picked up in each of powdered samples. The studied crystals were often of poor quality because of their lamellar feature (see below). The data collections were carried out at ambient temperature on a Bruker-Nonius Kappa CCD diffractometer using graphite monochromatic MoKα. Data integration was processed with the set of programs from Nonius using the Eval CCD formalism. The crystal shape and size optimization for absorption were performed with the X-Shape program while refinements were carried out with the JANA2006 program.
10
Structural Analysis of Organometallic Compounds
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