The crystallographic data were measured on a Bruker SMART APEX II CCD single crystal diffractometer with MoKα radiation (1 –7 , 9 , 10 , and 12 –14 ) and an XtaLAB Synergy, Dualflex, HyPix diffractometer from Rigaku with CuKα radiation (11 ). The data were refined by SHELXL,[28] and all non‐proton coordinate values and anisotropic temperature factors were refined by the full‐matrix least‐squares method. All proton positions in the structure were determined by theoretical calculation
Smart apexii ccd
Manufactured by Bruker
Sourced in Germany
The SMART APEXII CCD is a high-performance X-ray detector developed by Bruker for crystallographic applications. It features a charge-coupled device (CCD) technology that allows for efficient and accurate data collection during X-ray diffraction experiments. The SMART APEXII CCD provides reliable and precise measurements, making it a valuable tool for researchers and scientists in the field of structural analysis.
Automatically generated - may contain errors
Lab products found in correlation
Dualflex, by Rigaku (1 mentions)
Hypix, by Rigaku (1 mentions)
Titan cubed themis g2 300, by Thermo Fisher Scientific (1 mentions)
Tecnai t20, by Thermo Fisher Scientific (1 mentions)
Phi 5000c esca system, by PerkinElmer (1 mentions)
A300 esr spectrometer, by Bruker (1 mentions)
Nmr 600, by Bruker (1 mentions)
Ics 2000, by Thermo Fisher Scientific (1 mentions)
Jem 2100f, by JEOL (1 mentions)
Shelxl 2014, by Bruker (1 mentions)
13 protocols using smart apexii ccd
1
Structural Analysis of Crystalline Compounds
2
Single-Crystal X-Ray Diffraction of H2NPV
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
The single-crystal
X-ray diffraction data of H2NPV was recorded at 100(2)
K temperature on a diffractometer, Bruker SMART APEX-II CCD, by the
use of graphite monochromated Mo Kα radiation (λ = 0.71073
Å). The structure-solving procedures were completed with the
help of the Bruker Apex-III suite. The integration of data was done
by the SAINT42 program and, simultaneously,
the absorption corrections were performed with SADABS.42 The anisotropic thermal parameters for all non-hydrogen
atoms with full matrix least-squares refinements were calculated on F2 using SHELXL-2014.43 (link)Figure S1 shows the ORTEP view of the
ligand. The refined and solving crystallographic parameters are listed
inTable S1 .
X-ray diffraction data of H2NPV was recorded at 100(2)
K temperature on a diffractometer, Bruker SMART APEX-II CCD, by the
use of graphite monochromated Mo Kα radiation (λ = 0.71073
Å). The structure-solving procedures were completed with the
help of the Bruker Apex-III suite. The integration of data was done
by the SAINT42 program and, simultaneously,
the absorption corrections were performed with SADABS.42 The anisotropic thermal parameters for all non-hydrogen
atoms with full matrix least-squares refinements were calculated on F2 using SHELXL-2014.43 (link)
ligand. The refined and solving crystallographic parameters are listed
in
3
Multi-technique Characterization of Novel Materials
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
The XRD data were characterized by Bruker SMART APEX (II)-CCD (Germany). X-ray photoelectron spectroscopy was recorded on a Perkin Elmer PHI 5000 C ESCA system (Perkin Elmer, USA). The high-resolution transmission electron microscopy images and the EDX spectroscopy spectra were recorded by a JEM 2100 F (JEOL, Japan) and a Tecnai T20 (FEI, USA) transmission electron microscope. The HAADF-STEM, EELS, and the EDX mapping experiments were performed using Titan Cubed Themis G2 300 (FEI) microscope equipped with Super-X detectors at 200 kV. N2-TPD measurements were performed on a Micrometrics Autochem II 2920 system. Electron-spin resonance signals were recorded on a Bruker ESR A300 spectrometer at room temperature. XANES and EXAFS data were collected on beamline 14 W at the Shanghai Synchrotron Radiation Facility (SSRF). The UV–Vis absorption spectrum was recorded by an ultraviolet-visible spectrometer (U-3900H, Hitachi, Japan). 1H-NMR (nuclear magnetic resonance) measurements were performed on a Bruker NMR600. IC analysis was performed on an ICS-2000 (Thermo Fisher Scientific) equipped with an isocratic pump.
4
Single Crystal X-ray Diffraction of Complexes
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Single crystals of 1–3 and 5–7 complexes were grown from their saturated
solutions in hexane and toluene at −30 °C. In a typical
procedure, a specimen of suitable size and quality was obtained from
the solution, coated with Paratone oil, and mounted on a glass capillary.
Reflection data were collected using a Bruker SMART Apex II-CCD area
detector diffractometer with graphite-monochromated Mo Kα radiation
(λ = 0.71073 Å). The hemisphere of the reflection data
was collected as ω-scan frames with 0.3° per frame and
an exposure time of 10 s per frame. Cell parameters were determined
and refined using the SMART program.15 Data
reduction was performed using SAINT software.16 The data were corrected for Lorentz and polarization effects, and
an empirical absorption correction was applied using the SADABS program.17 The structures of the prepared compounds were
solved by direct methods, and all non-hydrogen atoms were subjected
to anisotropic refinement by the full-matrix least-squares method
on F2 using the SHELXTL/PC package.18 Hydrogen atoms were placed at their geometrically
calculated positions and refined based on the corresponding carbon
atoms with isotropic thermal parameters. CCDC 2052996–2053001
for complexes1–3 and 5–7 contains
the supplementary crystallographic data for this article.
solutions in hexane and toluene at −30 °C. In a typical
procedure, a specimen of suitable size and quality was obtained from
the solution, coated with Paratone oil, and mounted on a glass capillary.
Reflection data were collected using a Bruker SMART Apex II-CCD area
detector diffractometer with graphite-monochromated Mo Kα radiation
(λ = 0.71073 Å). The hemisphere of the reflection data
was collected as ω-scan frames with 0.3° per frame and
an exposure time of 10 s per frame. Cell parameters were determined
and refined using the SMART program.15 Data
reduction was performed using SAINT software.16 The data were corrected for Lorentz and polarization effects, and
an empirical absorption correction was applied using the SADABS program.17 The structures of the prepared compounds were
solved by direct methods, and all non-hydrogen atoms were subjected
to anisotropic refinement by the full-matrix least-squares method
on F2 using the SHELXTL/PC package.18 Hydrogen atoms were placed at their geometrically
calculated positions and refined based on the corresponding carbon
atoms with isotropic thermal parameters. CCDC 2052996–2053001
for complexes
the supplementary crystallographic data for this article.
5
Single Crystal X-Ray Diffraction Analysis
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Intensity data sets were collected at room temperature, on a BRUKER SMART APEXII CCD [24 ] area-detector diffractometer equipped with graphite monochromated Mo Kα radiation (λ = 0.71073 Å). The data were reduced by using the program SAINT [24 ] and empirical absorption corrections were done by using the SADABS [24 ]. The structures were solved by direct methods using SHELXS-97 [25 (link)] and refined anisotropically by full-matrix least-squares method using SHELXL-97 [25 (link)] within the WINGX suite of software, based on F2 with all reflections. All carbon hydrogens were positioned geometrically and refined by a riding model with Uiso 1.2 times that of attached atoms. All non H atoms were refined anisotropically. The molecular structures were drawn using the ORTEP-III [26 (link)] and POV-ray [27 ]. Crystal data and the selected parameters are summarized in (Tables 1 and 2 ) respectively. The crystals remained stable throughout the data collection. The CIF files of complexes 1 and 2 ate provided as Additional files 1 and 2 respectively.
6
Single-Crystal X-ray Analysis of Compound 1′
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
A single crystal of 1′ was mounted on a glass
capillary. Data of X-ray diffraction were
collected by a Bruker Smart APEX II CCD single-crystal diffractometer
using Mo Kα radiation (λ = 0.71073 Å) to 2θmax of 50.0° at 293 K. The crystallographic calculation
was performed by a direct method using SHELXL 2014.33 All non-hydrogen atoms and hydrogen atoms were refined
anisotropically and isotropically, respectively. The occupy factor
of solvent water O(7) and O(8) is 0.5, and the hydrogen atoms of the
solvent are not found. Atomic coordinates, thermal parameters, and
intramolecular bond lengths and angles are given in theSupporting Information (CIF file format).
capillary. Data of X-ray diffraction were
collected by a Bruker Smart APEX II CCD single-crystal diffractometer
using Mo Kα radiation (λ = 0.71073 Å) to 2θmax of 50.0° at 293 K. The crystallographic calculation
was performed by a direct method using SHELXL 2014.33 All non-hydrogen atoms and hydrogen atoms were refined
anisotropically and isotropically, respectively. The occupy factor
of solvent water O(7) and O(8) is 0.5, and the hydrogen atoms of the
solvent are not found. Atomic coordinates, thermal parameters, and
intramolecular bond lengths and angles are given in the
7
Single Crystal X-ray Diffraction Protocol
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
The X-ray diffraction data for the single crystal of 6 were collected on a Bruker Smart Apex II CCD diffractometer (ω-scan mode) using graphite monochromated MoKα (0.71073 Å) radiation at 150 K. The structure was solved by the direct methods using SHELXT–2014/5 [39 (link)] and refined by the full-matrix least-squares on F2 using SHELXL–2017/1 [40 (link)]. Calculations were mainly performed using WinGX–2014.1 suite of programs [41 (link)]. Non-hydrogen atoms were refined anisotropically. The hydrogen atoms were inserted at the calculated positions and refined as riding atoms.
The crystal data, data collection and structure refinement details for 6 are summarized inTable S1 of the Supplementary Material . The crystallographic data for the investigated crystal 6 have been deposited in the Cambridge Crystallographic Data Centre as supplementary publication CCDC number 1876720. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif , by emailing data_request@ccdc.cam.ac.uk , or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336033.
The crystal data, data collection and structure refinement details for 6 are summarized in
8
Structural Analysis of Crystalline Compounds
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
X-ray diffraction experiments of the studied compounds were done on a diffractometer (Bruker SMART APEXII CCD) using CuKα radiation. Diffraction data were processed with SAINT ver. 8.34A, SADABS ver. 2014/4 (structure 1c with TWINABS ver. 2008/4) and XPREP ver. 2014/2. The structures were solved with the ShelXT (Version 2018/2) [15 (link)] and refined with ShelXL 2018/3 [16 (link)]. For visualization, ShelXle [17 (link)] and Olex2 [18 (link)] programs were used. Structure 1c was refined as a three-component twin with the following contributions: 0.88, 0.11, and 0.01. All H atoms (except those in NH and NH2 groups) were geometrically optimized. All studied crystals were obtained by slow evaporation of solvent. The solvent used is a mixture of methanol and DMF (1:1). Programs publCIF [19 (link)] and Mercury [20 (link)] were used to prepare the manuscript. CCDC 2189843, 2189844, 2189856 contain the supplementary crystallographic data for this paper. The data were provided free of charge by the Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/structures (accessed on 13 July 2022).
9
Single Crystal X-Ray Structural Analysis
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Appropriate individual crystals of complex 1 and complex 2 were selected and mounted onto thin glass fibers. We collected the data at 296(2) K in a Bruker Smart ApexII CCD instrument (Bruker Corp., Karlsruhe, Germany) fitted with graphite monochromatic Mo-Ko radiation (λ = 0.71073 Å). The absorption effects were semi-empirically calibrated. Olex2 [33 (link)] was employed to solve the structures and refined with SHELXL-97 crystallographic software [34 (link)]. Non-hydrogen atoms were anisotropically refined. Hydrogen atoms bound to carbons were placed in geometrical idealized positions, followed by refinement with a riding model. All other hydrogens were localized in the final difference Fourier map. The full-matrix least-squares refinement final cycle was based on the observed reflections along with variable parameters. Crystallographic as well as structural refinement data for complex 1 and complex 2 are listed in Table 1 . Selected bond lengths (Å) as well as angles (°) are listed in Table S1 . CCDC 2013056 and CCDC 2013057 for complex 1 and complex 2 harbor supplementary crystallographic data were provided freely by the Cambridge Crystallographic Data Centre (Cambridge, UK).
10
Single Crystal X-ray Structural Analysis
Check if the same lab product or an alternative is used in the 5 most similar protocols
+ Expand
Suitable single crystals of 1 and 2 were selected for collection of intensity data on a Bruker SMART APEX II CCD diffractometer using a ϕ-ω scan mode at 291 K for compound 1 and 296(2) K for compound 2 [monochromate Mo Kα radiation (λ = 0.71073 Å)]. SADABS was applied for multi-scan absorption corrections of all intensity data. The structures were solved by direct methods, and SHELXTL software was used to refine F2 by full-matrix least squares procedures (Sheldrick, 2008 (link)). All hydrogen atoms were fixed in calculated positions and refined isotropically. The crystallographic data of compounds 1 and 2 are listed in Table 1 . The selected bond lengths and angles are shown in Table 2 . The hydrogen bond parameters are listed in Supplementary Table S1 .
About PubCompare
Our mission is to provide scientists with the largest repository of trustworthy protocols and intelligent analytical tools, thereby offering them extensive information to design robust protocols aimed at minimizing the risk of failures.
We believe that the most crucial aspect is to grant scientists access to a wide range of reliable sources and new useful tools that surpass human capabilities.
However, we trust in allowing scientists to determine how to construct their own protocols based on this information, as they are the experts in their field.
Ready to get started?
Sign up for free.
Registration takes 20 seconds.
Available from any computer
No download required
Revolutionizing how scientists
search and build protocols!