The largest database of trusted experimental protocols

Smart apex ccd

Manufactured by Bruker
Sourced in United States

The Smart Apex CCD is a laboratory equipment product from Bruker. It is a charge-coupled device (CCD) detector designed for use in x-ray crystallography applications. The Smart Apex CCD provides high-resolution image capture and data collection capabilities for the analysis of crystal structures.

Automatically generated - may contain errors

20 protocols using smart apex ccd

1

Single Crystal X-ray Diffraction Analysis

Check if the same lab product or an alternative is used in the 5 most similar protocols
The target compounds were dissolved in chloroform and slowly evaporated for 5–10 days to obtain crystals of appropriate size. A Bruker Smart Apex CCD single crystal diffractometer and a graphite monochromator with monochromatized Mo rays (λ = 0.071073 nm) were used to collect single crystal diffraction data within a certain θ range by φ-ω scanning mode. The diffraction intensity data were corrected by empirical absorption and LP. The crystal structures were solved by direct methods. All non-hydrogen coordinates and their anisotropic thermal parameters were modified by the full matrix least square method. All calculations were completed with the Shelx-97 program [36 ]. Crystallographic data and refinement details for 3a3j are given in Tables S1–S3. CCDC: 2102942, 3a. CCDC: 2102943, 3b. CCDC: 2102944, 3c. CCDC: 2102945, 3e. CCDC: 2102946, 3f. CCDC: 2102947, 3g. CCDC: 2102948, 3h. CCDC: 2102949, 3i. CCDC: 2102950, 3j. These data can be obtained free of charge from the Cambridge Crystallographic Data Centre www.ccdc.cam.ac.uk/data_request/cif (accessed on 13 August 2021).
+ Open protocol
+ Expand
2

Structural Determination of Ruthenium Complexes

Check if the same lab product or an alternative is used in the 5 most similar protocols
Data of CR–BPY1 and CR–BPY2 were collected on a Bruker Smart APEX CCD diffractometer with graphite-monochromated Mo-Kα (λ = 0.71073 Å) using the SMART and SAINT programs.34 Their structures were determined and the heavy atoms were found by direct methods using the SHELXTL-97 program package.35 Crystallographic data for them are summarized in Table 3. Except some partly occupied solvent water molecules, the other non-hydrogen atoms were refined anisotropically. Hydrogen atoms within the ligand backbones were fixed geometrically at their positions and allowed to ride on the parent atoms. In both of the two structures, the ruthenium atoms were disordered in the equivalent positions of tungsten atoms. For CR–BPY2, several bond distances constraints were used to help the refinement on the BPY moiety, and thermal parameters on adjacent oxygen atoms of the polyoxometalate anion were restrained to be similar.
+ Open protocol
+ Expand
3

Single-Crystal X-Ray Structural Analysis

Check if the same lab product or an alternative is used in the 5 most similar protocols
The single-crystal X-ray experiment was carried out on a Bruker SMART APEX-CCD-based diffractometer using graphite-mono-chromated Mo Kα radiation (λ = 0.71073 Å) using ω and φ scan mode. The data integration and reduction were processed with SAINT software. An empirical absorption corrections were implemented using SADABS program31 . Data processing was accomplished with the SAINT processing program. The structure was determined by the direct methods using the SHELXS program of the SHELXTL-9732 package and refined with SHELXL-9733 . The positions of the hydrogen atoms were refined isotropically for whole framework. All non-hydrogen atoms were refined anisotropic displacement parameters. Additionally, other details of crystal data, data collection parameters and refinement statistics for 1 and 2 are summarized in Table S1. Selected bond lengths and bond angles, and the hydrogen bonds of two compounds are listed in Tables S2–S5, respectively.
+ Open protocol
+ Expand
4

Characterization of Co/CeO2/C/IL Nanocomposite

Check if the same lab product or an alternative is used in the 5 most similar protocols
Using the UV–Vis spectrophotometer model Shimadzu UV-1800, Germany absorption spectra were recorded. By using Fourier transform infrared spectroscopy (FTIR, MX 300, Mohrsville, PA, USA), the functional groups were studied over wavenumber range of 4000–500 cm−1. Furthermore, FTIR also detects C=C groups of carbon and vibrations of CeO2, which are related to bulk material rather than to functional groups. The surface morphology and size of the nanocomposite were examined by using a scanning electron microscope (SEM, JSM-IT 100 Jeol, Tokyo, Japan), and by using EDX (equipped with the SEM) the elemental analysis was performed. The accelerated voltage of 20 kV was applied to take images at different magnifications. The crystal structure of the Co/CeO2/C/IL was studied by using powder X-ray diffraction (XRD) and a Bruker Smart Apex CCD (Billerica, MA, USA) over the 2θ range of 20–80°. The Raman spectrum at room temperature was recorded by using the portable Raman instrument attached to a microscope (i-Raman B&W TEK Inc, Plainsboro, NJ, USA, 20× objectives).
+ Open protocol
+ Expand
5

Detailed Spectroscopic Characterization of Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
All the chemicals and reagents were purchased from a commercial source and used as received without further purification. 1H and 13C NMR spectra were measured on a Bruker AV 500 (500 MHz) spectrometer in CD2Cl2 with tetramethylsilane (TMS, δ = 0). High-resolution mass spectra (HRMS) were recorded on a GCT premier CAB048 mass spectrometer operating in MALDI-TOF mode. Single-crystal X-ray diffraction intensity data were collected on a Bruker–Nonices Smart Apex CCD diffractometer with graphite monochromated MoKα radiation. Processing of the intensity data was carried out using the SAINT and SADABS routines, and the structure and refinement were conducted using the SHELTL suite of X-ray programs (version 6.10). UV–vis absorption spectrum was measured on a Shimadzu UV-2600 spectrophotometer. PL spectra were recorded on a Horiba Fluoromax-4 spectrofluorometer. Solution fluorescence quantum yields were measured using a Hamamatsu absolute PL quantum yield spectrometer C11347 Quantaurus_QY. High-performance liquid chromatography spectra were measured using Waters alliance e2695 separation module.
+ Open protocol
+ Expand
6

Single-crystal X-ray Diffraction Measurements

Check if the same lab product or an alternative is used in the 5 most similar protocols
Single-crystal X-ray diffraction measurements were carried out on a Bruker SMART APEX CCD based on a diffractometer operating at room temperature. Intensities were collected with graphite monochromatized Mo Kα radiation (λ = 0.71073 Å), operating at 50 kV and 30 mA, and using the ω/2θ scan mode. Data reduction was made with the Bruker SAINT package.55 Absorption corrections were performed using the SADABS program.56 The structures were solved by direct methods and refined based on F2, via full-matrix least-squares, using SHELXL-97 with anisotropic displacement parameters for all non-hydrogen atoms in both structures. Hydrogen atoms bonded to carbon atoms were placed in calculated positions and refined in riding mode, with C–H = 0.93 Å (methane) or 0.96 Å (methyl), and Uiso(H) = 1.2Ueq (Cmethane) or Uiso(H) = 1.5Ueq (Cmethyl). The H2O hydrogen atoms were located in the difference Fourier maps and refined with an O–H distance restraint [0.85(1) Å] and Uiso(H) = 1.5 Ueq(O). All computations were carried out using the SHELXTL-97 program package.57 (link) CCDC 1823177 contains the supplementary crystallographic data for this paper.
+ Open protocol
+ Expand
7

Analytical Methods for Purification and Characterization

Check if the same lab product or an alternative is used in the 5 most similar protocols
Unless otherwise indicated all reagents used in the present work were obtained from Aldrich Chemical Co and were used without further purification. Reagent grade organic solvents were obtained from SDS and high purity de-ionized water was obtained by passing distilled water through a nano-pure Milli-Q water purification system.
Instrumentation and measurements. Quest Finnigan, using acetonitrile as a mobile phase.
X-ray structure determination.
Measurements of the crystals were performed on a Bruker Smart Apex CCD diffractometer using graphite-monochromated Mo Kα radiation (λ = 0.71073Å) from an X-Ray tube. Data collection, Smart V.
+ Open protocol
+ Expand
8

Growth and Structural Analysis of TBA Glycolate Hydrates

Check if the same lab product or an alternative is used in the 5 most similar protocols
Single
crystals of the TBA glycolate hydrates were formed from the aqueous
solution with x = 0.0293 at T =
278.2 K. The subcooling temperature was 2.7 K, which enables to grow
thick crystals. After a sufficient number of suitably sized crystals
grew, the crystals were separated from the residual aqueous solution.
The crystals were preserved in a freezer at 260 K. In the followed
processes, the crystals were kept under this temperature to avoid
melting. A crystal was chosen and mounted on a single-crystal X-ray
diffractometer (Smart APEX CCD, Bruker AXS). The measurement temperature
of the X-ray diffraction (XRD) was 123 K. The X-ray source was Mo
Kα (wave length: 0.7107 Å). The structure was solved and
refined by Shelx.36 (link) A summary of the present
crystal structure analysis is provided in the Supporting Information.
+ Open protocol
+ Expand
9

Synthesis and Characterization of Ba2NaOsO6 Single Crystals

Check if the same lab product or an alternative is used in the 5 most similar protocols
High-quality single crystal of Ba2NaOsO6 with a truncated octahedral morphology were grown from a molten hydroxide flux, as described elsewhere12 (link)17 . Crystal quality was checked by X-ray diffraction, using a Bruker Smart Apex CCD (charge-coupled device) diffractometer, which indicated that the room temperature structure belongs to the Fm m space group12 (link). NMR measurements were performed for a single crystal with a volume of ∼1 mm3. The quality of the sample was confirmed by the sharpness of 23Na NMR spectra both in the high-temperature PM state and low-temperature quadrupolar split spectra.
The sample was both zero-field and field-cooled. We did not detect any influence of the samples cooling history on the NMR spectra. Nevertheless for consistency, all results presented in the paper were obtain in field-cooled conditions. The sample was mounted to one of the crystal faces and rotated with respect to the applied field about an axis using a single axis goniometer. The rotation angle, for applied fields below 9 T, was inferred from the signal of two perpendicularly positioned Hall sensors. In addition, to ensure that data was taken with no external pressure applied, the mounted sample was placed in a solenoid coil with cross sectional area significantly larger than that of the sample. In this way, no pressure is exerted on the sample as coil contracts on cooling.
+ Open protocol
+ Expand
10

Structural Analysis of Compound 1

Check if the same lab product or an alternative is used in the 5 most similar protocols
Single-crystal X-ray structural analysis of 1 in α/α′ coexisting state was performed at 298 K on a Bruker Smart APEX CCD (charge-coupled device) area diffractometer (Bruker AXS K.K.) with a nitrogen-flow temperature controller using graphite-monochromated Mo radiation (λ=0.71073 Å). Empirical absorption corrections were applied using the SADABS programme. The structure was solved by direct methods (SHELXS-97) and refined by full-matrix least-squares calculations on F2 (SHELXL-97) using the SHELX TL programme package. Non-hydrogen atoms were refined anisotropically; hydrogen atoms were fixed at calculated positions by riding model approximation.
+ Open protocol
+ Expand

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

Sign up now

Revolutionizing how scientists
search and build protocols!