Crystals of suitable sizes were mounted on a Bruker SMART APEX II X-ray diffractometer for data collection and structure determination. X-ray diffraction data were collected using Mo Kα radiation (λ = 0.71073 Å). The program SAINT (Bruker, 2016 ▸ ) was used for data integration and reduction. Direct methods followed by Fourier transformation by employing full-matrix least-squares calculations were carried out to solve the structure by using SHELXTL and SHELXL97 (Sheldrick, 1997 ▸ ) in the case of EX; the APEX3 Suite combined with SHELXL2014/7 and SHELXL2016/6 (Sheldrick, 2015 ▸ ) was used in the case of the co-crystal. Intermolecular interactions were calculated using PLATON (Spek, 2009 ▸ ). The program ORTEP3 (Farrugia, 1997 ▸ ) was utilized to generate a structural representation. Mercury 2.0 was used to create molecular graphics of the interactions (Macrae et al., 2008 ▸ ). Crystallographic data, experimental details and structure-refinement parameters are summarized in Table 1 ▸ .
Smart apex 2 x ray diffractometer
Manufactured by Bruker
Sourced in United States
The SMART APEX II X-ray diffractometer is a versatile and advanced instrument designed for single-crystal X-ray diffraction analysis. It is capable of collecting high-quality diffraction data from small to large single-crystal samples, enabling the determination of crystal structures.
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5 protocols using smart apex 2 x ray diffractometer
1
X-Ray Structural Analysis of Crystals
2
Characterization of Ag3PO4 Microparticles
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The crystalline phases of the Ag3PO4 microparticles were determined through X-ray diffraction (XRD) using a SMART APEX II X-ray diffractometer (Bruker AXS, Billerica, MA, USA) with Cu Kα radiation (λ = 0.15418 nm). The morphologies of the Ag3PO4 microparticles were observed through a HITACHI S-4800 scanning electron microscope (SEM) (Hitachi high technologies corporation, Tokyo, Japan) operating at 15 kV. UV–visible diffuse reflectance spectra (UV-Vis-DRS) of the Ag3PO4 microparticles were collected from an Evolution 2000 UV–Vis spectrometer (Thermo Fisher Scientific Inc., Madison, WI, USA) with BaSO4 employed as the reference. The Brunauer–Emmett–Teller (BET) specific surface area of the Ag3PO4 microparticles was characterized using a PMI C-BET 201A system (Porous Materials Inc., Ithaca, NY, USA).
3
Single Crystal X-Ray Diffraction Analysis
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A single crystal of the compound (2g) with dimensions of 0.30 ×
0.25 × 0.20 mm was chosen for X-ray diffraction studies. The
data were collected on a Bruker SMART APEX II X-ray
diffractometer with graphite monochromated MoKα radiation,
operating at 50 kV and 30 mA. Raw data was processed and
reduced by using APEX2 and SAINT [24 ]. The structure was
solved by direct methods using SHELXS-97 [25 (link)]. All nonhydrogen
atoms were revealed in the first Fourier map itself.
Full-matrix least squares refinement was carried out using
SHELXL-97 [25 (link)]. Anisotropic refinement of non-hydrogen
atoms was started at this stage. Subsequent refinements were
carried out with anisotropic thermal parameters for nonhydrogen
atoms and isotropic temperature factors for the
hydrogen atoms which were placed at chemically acceptable
positions. CCDC- 990917 contains the supplementary
crystallographic data of molecule 2g [26 ]. The X-ray structure of
this compound (2g) was used for the docking studies.
0.25 × 0.20 mm was chosen for X-ray diffraction studies. The
data were collected on a Bruker SMART APEX II X-ray
diffractometer with graphite monochromated MoKα radiation,
operating at 50 kV and 30 mA. Raw data was processed and
reduced by using APEX2 and SAINT [24 ]. The structure was
solved by direct methods using SHELXS-97 [25 (link)]. All nonhydrogen
atoms were revealed in the first Fourier map itself.
Full-matrix least squares refinement was carried out using
SHELXL-97 [25 (link)]. Anisotropic refinement of non-hydrogen
atoms was started at this stage. Subsequent refinements were
carried out with anisotropic thermal parameters for nonhydrogen
atoms and isotropic temperature factors for the
hydrogen atoms which were placed at chemically acceptable
positions. CCDC- 990917 contains the supplementary
crystallographic data of molecule 2g [26 ]. The X-ray structure of
this compound (2g) was used for the docking studies.
4
Analytical Techniques for Compound Characterization
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Analytical thin-layer
chromatography
(TLC) was performed on Kieselgel 60 F254 glass plates precoated with
a 0.2 mm thickness of silica gel. The TLC plates were visualized by
UV (254 nm), potassium permanganate, or ceric ammonium molybdate stain.
Flash chromatography was carried out with Kieselgel 60 (230–400
mesh) silica gel. Melting points: Barnstead/Electrothermal 9300, measurements
were performed in open glass capillaries. IR spectra: Bruker α-P.
NMR spectra: Bruker AV 300 MHz (1H NMR: 300 MHz, 13C NMR: 75 MHz), AV 400 MHz (1H NMR: 400 MHz, 13C NMR: 100 MHz), AV 500 MHz (1H NMR: 500 MHz, 13C NMR: 125 MHz), and AV2 500 MHz (19F NMR: 470 MHz), the
spectra were recorded in CDCl3, MeOD, and DMSO-d6 using tetramethylsilane (TMS) as the internal
standard and are reported in ppm. 1H NMR data are reported
as follows: (s = singlet, d = doublet, t = triplet, q = quartet, dd
= doublet of doublet, m = multiplet; coupling constant(s) J are given in Hz; integration, proton assignment). High-resolution
mass spectra (HRMS): JEOL JMS-700. X-ray crystallography: Bruker SMART
APEX II X-ray diffractometer. UV–VIS spectra: SCINCO S-4100
diffuse reflectance-ultraviolet/visible (DR-UV/VIS) spectrophotometer.
All solvents were purified using a column filter solvent purification
system before use unless otherwise indicated. Reagents were purchased
and used without further purification.
chromatography
(TLC) was performed on Kieselgel 60 F254 glass plates precoated with
a 0.2 mm thickness of silica gel. The TLC plates were visualized by
UV (254 nm), potassium permanganate, or ceric ammonium molybdate stain.
Flash chromatography was carried out with Kieselgel 60 (230–400
mesh) silica gel. Melting points: Barnstead/Electrothermal 9300, measurements
were performed in open glass capillaries. IR spectra: Bruker α-P.
NMR spectra: Bruker AV 300 MHz (1H NMR: 300 MHz, 13C NMR: 75 MHz), AV 400 MHz (1H NMR: 400 MHz, 13C NMR: 100 MHz), AV 500 MHz (1H NMR: 500 MHz, 13C NMR: 125 MHz), and AV2 500 MHz (19F NMR: 470 MHz), the
spectra were recorded in CDCl3, MeOD, and DMSO-d6 using tetramethylsilane (TMS) as the internal
standard and are reported in ppm. 1H NMR data are reported
as follows: (s = singlet, d = doublet, t = triplet, q = quartet, dd
= doublet of doublet, m = multiplet; coupling constant(s) J are given in Hz; integration, proton assignment). High-resolution
mass spectra (HRMS): JEOL JMS-700. X-ray crystallography: Bruker SMART
APEX II X-ray diffractometer. UV–VIS spectra: SCINCO S-4100
diffuse reflectance-ultraviolet/visible (DR-UV/VIS) spectrophotometer.
All solvents were purified using a column filter solvent purification
system before use unless otherwise indicated. Reagents were purchased
and used without further purification.
5
Ethyl Isocyanoacetate Compound Synthesis
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All reagents were purchased from commercial
sources without purification unless mentioned otherwise. Ethyl isocyanoacetate
was distilled under reduced pressure prior to use. N,N-Dimethylformamide, 1,4-dioxane, was obtained
from Extra-Dry Grade. All reactions were monitored by liquid chromatography–mass
spectrometry (LC-MS). The NMR spectrum was recorded on Bruker spectrometers
(400, 500, or 600 MHz for 1H, 100, 125, or 150 MHz for 13C, respectively). Chemical shifts are reported in δ
parts per million (ppm), and the signals are described as br (broad),
s (singlet), d (doublet), t (triplet), q (quartet), and m (multiple).
Coupling constants (J values) are given in hertz
(Hz). High-resolution mass spectroscopy (HRMS) was performed by a
Q-TOF mass spectrometer with ESI resources. Single-crystal X-ray diffraction
data were recorded on a Bruker SMART APEX II X-ray diffractometer.
Microwave-assisted reactions were performed on a CEM Explorer 48 MW
reactor.
sources without purification unless mentioned otherwise. Ethyl isocyanoacetate
was distilled under reduced pressure prior to use. N,N-Dimethylformamide, 1,4-dioxane, was obtained
from Extra-Dry Grade. All reactions were monitored by liquid chromatography–mass
spectrometry (LC-MS). The NMR spectrum was recorded on Bruker spectrometers
(400, 500, or 600 MHz for 1H, 100, 125, or 150 MHz for 13C, respectively). Chemical shifts are reported in δ
parts per million (ppm), and the signals are described as br (broad),
s (singlet), d (doublet), t (triplet), q (quartet), and m (multiple).
Coupling constants (J values) are given in hertz
(Hz). High-resolution mass spectroscopy (HRMS) was performed by a
Q-TOF mass spectrometer with ESI resources. Single-crystal X-ray diffraction
data were recorded on a Bruker SMART APEX II X-ray diffractometer.
Microwave-assisted reactions were performed on a CEM Explorer 48 MW
reactor.
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