Crystal structures of synthetic and natural stepanovite and zhemchuzhnikovite were determined by single-crystal XRD. Diffraction measurements were made on Bruker D8 APEX2 and Bruker APEX DUO x-ray diffractometers, using graphite-monochromated MoKα radiation (λ = 0.71073 Å). Data were collected in ω scan mode (2θ ≤ 54°). Structures were solved by direct methods in SHELXS and refined using SHELXL (35 ) on F2 using all data. Hydrogen atoms were located using the electron difference map when permitted by data quality. Calculations were performed and images were prepared using WinGX program suite (36 ). Structures have been deposited to the CSD, with deposition codes 1408093 to 1408095 for synthetic samples and 1431678 and 1431679 for natural samples.
Apex duo
Manufactured by Bruker
Sourced in Germany
The APEX DUO is a high-performance mass spectrometer designed for advanced analytical applications. It offers a dual-source configuration, allowing for both electrospray ionization (ESI) and atmospheric-pressure chemical ionization (APCI) capabilities within a single instrument. The APEX DUO provides accurate mass measurements and high-resolution data to support a wide range of research and analytical needs.
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Lab products found in correlation
Gf254, by Qingdao Haiyang Chemical (3 mentions)
D8 venture, by Bruker (2 mentions)
Apex2, by Bruker (2 mentions)
Av 500, by Bruker (1 mentions)
Sephadex lh 20, by Cytiva (1 mentions)
P 1020 polarimeter, by Jasco (1 mentions)
Chirascan spectrometer, by Applied Photophysics (1 mentions)
Uv 2401a spectrophotometer, by Shimadzu (1 mentions)
Cobra cooling device, by Oxford Cryosystems (1 mentions)
Apex3, by Bruker (1 mentions)
Saint program, by Siemens (1 mentions)
G6230 tof ms spectrometer, by Agilent Technologies (1 mentions)
Cary 5000 uv vis nir spectrometer, by Agilent Technologies (1 mentions)
Apex 2 ccd detector, by Bruker (1 mentions)
J 710 spectrometer, by Jasco (1 mentions)
S 4700 electron microscope, by Hitachi (1 mentions)
Bx41 microscope, by Olympus (1 mentions)
Jsm 7401f fe sem, by JEOL (1 mentions)
Q200 differential scanning calorimeter, by TA Instruments (1 mentions)
Am 400 spectrometer, by Bruker (1 mentions)
31 protocols using apex duo
1
Structural Determination of Stepanovite and Zhemchuzhnikovite by XRD
2
Comprehensive Characterization of ZnO Nanostructures
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Scanning
electron microscopy (SEM) was performed with a HITACHI, SU8010 FESEM
instrument with an energy-dispersive X-ray spectroscopy analysis system
operated at 50 kV. X-ray diffraction (XRD) patterns were obtained
using Bruker APEX DUO. XRD patterns were taken using Cu Kα as
the radiation source with a 1° divergence slit, 0.2° receiving
slit, and carbon monochromators at 1° min–1 (2θ range 20°–70°). Time-of-flight secondary
ion mass spectrometry (TOF-SIMS, Munich, Germany) is used to characterize
the surface composition of the ZnO NRs on the FTO substrate. The primary
ion source was a pulsed 69Ga+ source (pulsing
current 2.5 pA and a pulse width of 30 ns) operated at 15 keV with
a post-acceleration of 10 kV. The analysis area of 100 nm × 100
nm, data acquisition time of 30 s, and charge compensation by applying
low-energy electrons (∼30 eV) from a pulsed flood gun were
used for the measurements. The mass resolution measured on the ZnO+/– signal was m/Δm = 4000 in the positive and negative detection modes. Calibration
of the mass spectra in the positive detection was based on the peaks
such as H+ (1.007 m/z), B+ (11.0082 m/z), 64Zn+ (63.922 m/z), 66Zn+ (65.919 m/z), and in the negative detection mode on C– (12.0004 m/z), O– (15.995 m/z), CO2– (44.003 m/z), HCO2– (45.0118 m/z), 64ZnO– (79.922 m/z), and 64ZnO– (81.9189 m/z).
electron microscopy (SEM) was performed with a HITACHI, SU8010 FESEM
instrument with an energy-dispersive X-ray spectroscopy analysis system
operated at 50 kV. X-ray diffraction (XRD) patterns were obtained
using Bruker APEX DUO. XRD patterns were taken using Cu Kα as
the radiation source with a 1° divergence slit, 0.2° receiving
slit, and carbon monochromators at 1° min–1 (2θ range 20°–70°). Time-of-flight secondary
ion mass spectrometry (TOF-SIMS, Munich, Germany) is used to characterize
the surface composition of the ZnO NRs on the FTO substrate. The primary
ion source was a pulsed 69Ga+ source (pulsing
current 2.5 pA and a pulse width of 30 ns) operated at 15 keV with
a post-acceleration of 10 kV. The analysis area of 100 nm × 100
nm, data acquisition time of 30 s, and charge compensation by applying
low-energy electrons (∼30 eV) from a pulsed flood gun were
used for the measurements. The mass resolution measured on the ZnO+/– signal was m/Δm = 4000 in the positive and negative detection modes. Calibration
of the mass spectra in the positive detection was based on the peaks
such as H+ (1.007 m/z), B+ (11.0082 m/z), 64Zn+ (63.922 m/z), 66Zn+ (65.919 m/z), and in the negative detection mode on C– (12.0004 m/z), O– (15.995 m/z), CO2– (44.003 m/z), HCO2– (45.0118 m/z), 64ZnO– (79.922 m/z), and 64ZnO– (81.9189 m/z).
3
Spectroscopic Characterization of Compounds
4
Single-Crystal X-Ray Analysis of Co(μ-tph)(2,2′-bipy)
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The crystal data and collection details pertaining to single-crystal X-ray analysis of Co(μ-tph)(2,2′-bipy) (2) are given in Table S1.† The XRD data of complex 2 were collected using a Bruker APEX DUO diffractometer equipped with a Cobra cooling device (Oxford Cryosystems) with graphite-monochromated Mo Kα radiation (λ = 0.71073 Å) and a charge-coupled device as the area detector. Data collection, integration, scaling, and absorption correction were performed with Bruker Apex 3 software. Data reduction was performed using SAINT2 and XPREP. All of the data were corrected for Lorentzian, polarization, and absorption effects using the SADABS4 program. Structure determination and refinement using the OLEX2 interface was performed using the full matrix least-squares method based on F2 against all reflections, as implemented in SHELXL2014/7.6. The hydrogen atoms bonded to carbon atoms were fixed using the HFIX command in SHELX-TL.
5
Crystal Structure Analysis of R-Block
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Single crystal data of R-Block were collected on a Bruker APEX DUO (for R-Block) diffractometer using graphite-monochromated Mo Kα radiation, λ = 0.71073 Å. The data were integrated using the Siemens SAINT program [65 ]. Adsorption corrections were applied. The structure was solved by direct methods and refined on F2 by full-matrix least-squares using SHELXTL [66 ]. All non-hydrogen atoms were refined anisotropically. All hydrogen atoms bound to carbon were refined isotropically in riding mode. For R-Block , hydrogen atoms of water molecules were detected via experimental electron density and then refined isotropically with a reasonable restriction of O-H bond distances and H-O-H angles. The residual electron densities were of no chemical significance. The crystallographic data are shown in Supplementary Table S1 , and the selected bond lengths and angles are shown in Supplementary Table S2 . Deposition Number 2086976 contains the supplementary crystallographic data. These data can be obtained free of charge from the Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif (accessed on 3 June 2021).
6
Structural Analysis of Teuvincenone F
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Crystals of Teuvincenone F were obtained in MeOH. Crystallographic data were collected at 100 K on a Bruker APEX DUO diffractometer equipped with an APEX II CCD using Cu Kα radiation. Cell refinement and data reduction were performed with Bruker SAINT. The structures were solved by direct methods using SHELXS-97 (Sheldrick and Schneider, 1997 (link)). Refinements were performed with SHELXL-97 using full-matrix least-squares, with anisotropic displacement parameters for all the non-hydrogen atoms. The non-hydrogen atoms were refined anisotropically, and hydrogen atoms were fixed at calculated positions. Molecular graphics were computed with PLATON (Spek, 2015 (link)). Crystallographic data for the structure reported have been deposited at the Cambridge Crystallographic Data Center as supplementary publications no. CCDC 1547843 for Teuvincenone F. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB 1EZ, U.K. [fax: int. +44(0) (1223) 336 033); e-mail: deposit@ccdc.cam.ac.uk ].
7
L-Threonine X-ray Diffraction Protocol
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The X-ray diffraction data of L-threonine were collected on a Bruker APEX DUO diffractometer equipped with microfocus MoKα radiation (λ = 0.71073 Å) and a Photon II detector. The APEX 3 program50 was used for determination of the unit cell parameters and data collection. The Bruker SAINT51 software package was used to integrate diffraction frames, and the diffraction data were corrected for absorption effects using the numerical method (SADABS)52 (link). The structure determination and refinement, using the OLEX2 interface53 (link), were performed by using the full matrix least-squares method based on F2 against all reflections with SHELXL-2014/754 (link). All hydrogen atoms bonded to carbon atoms were fixed using the HFIX command in SHELX-TL. Hydrogens on non-carbon atoms were located from the difference Fourier map. The final CIF was verified by using PLATON55 (link) and did not show any missing symmetry. The geometrical calculations were performed by using PLATON55 (link) and PARST56 (link). The graphics containing the structures were generated using Mercury 3.757 (link), X-Seed58 (link), and POV-Ray59 . Additional details of the data collection and structural refinement parameters are provided in Supplementary Table 1 .
8
Crystallization of β-CD-MetAMC Complex
9
Crystallographic Analysis of 1·Guest Complex
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Crystallographic data for 1·guest was collected on Bruker Apex duo equipment with Ga radiation (λ = 1.34139 Å) at 173 K. The data integration and empirical absorption correction were carried out using SAINT program. Using Olex2 and SHELXTL, the structure was solved by direct method and refined matrix least-squares on F2 with anisotropic displacement. Non-hydrogen atoms were refined anisotropically, hydrogen atoms were constrained to ideal geometries. The SQUEEZE routine in the program PLATON was used to exclude the contribution from highly disordered solvent molecules that cannot be modeled even with restraints and the SQUEEZE results are appended to the CIF file.17 (link) Details of the data collection and crystallographic information are summarized in Table S1.†
10
Spectroscopic and Structural Characterization
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Optical rotations, IR, and UV spectra were recorded on a JASCO P-1020 polarimeter (Tokyo, Japan), Hercules Bio-Rad FTS-135 series spectrometer (CA, USA), and Shimadzu UV-2401 PC ultraviolet–visible spectrophotometer (Tokyo, Japan), respectively. Electrospray ionization mass spectra (ESI-MS) and high-resolution electrospray ionization mass spectra (HR-ESI-MS) were carried out on an Agilent G6230 TOF MS spectrometer. 1D- and 2D-NMR spectra were recorded on a Bruker DRX-500, 600 or 800 spectrometer (Karlsruhe, Germany). The X-ray diffraction instrument (Bruker APEX DUO, Karlsruhe, Germany) was used for characterizing the structures of the crystal. Macroporous resin D101 and silica gel (200–300 mesh) were used for column chromatography (CC), and TLC analysis with silica gel GF254 plates were visualized by heating after spraying with 10% H2SO4/EtOH. All CC and TLC materials were purchased from Qingdao Haiyang Chemical Co. Ltd., China. Reverse-phase semipreparative HPLC (Capcell Pak MGII C18 column, 5 μm, 250 mm × 10 mm, Tokyo, Japan) was performed on a Hanbon series (Jiangsu Hanbon Science & Technology Co., China) at 25 °C with a flowing rate of 3.0 mL/min.
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