Optical rotation values were measured at 25 °C using a JASCO P-2000 polarimeter (Tokyo, Japan) with a 1 cm cell. UV and IR spectra were obtained using a Perkin-Elmer Lambda 35 spectrophotometer (Waltham, MA, USA) and a JASCO FT/IR-4200 spectrometer (Tokyo, Japan), respectively. Circular dichroism (CD) spectra were acquired on an Applied Photophysics Chirascan V100 CD spectrometer (Leatherhead, UK) using a 1 mm CD cell. NMR spectra were collected using Bruker Avance 600 and 850 MHz NMR spectrometers (Billerica, MA, USA) located at the National Center for Inter-University Research Facilities (NCIRF), Seoul National University. Low-resolution electrospray ionization (ESI) data were acquired using an Agilent Technologies 6130 quadrupole mass spectrometer (Santa Clara, CA, USA) coupled with an Agilent Technologies 1200-series HPLC with a reversed-phase C18 column (Phenomenex Luna, 100 × 4.6 mm). High-resolution FAB mass spectrometric data were obtained using a JEOL JMS 700 mass spectrometer (Tokyo, Japan) at the National Center for Inter-University Research Facilities (NCIRF). HPLC isolation was performed on a Gilson 321 (Middleton, WI, USA) equipped with a UV detector Gilson UV-Vis-151 (Middleton, WI, USA). X-ray crystallographics were collected on a Rigaku R-AXIS RAPID diffractometer (Tokyo, Japan) using graphite-monochromated Mo Kα radiation (λ = 0.71075 Å).
R axis rapid diffractometer
Manufactured by Rigaku
Sourced in Japan
The R-AXIS RAPID diffractometer is a compact and versatile X-ray diffraction instrument designed for single-crystal structure determination. It features a high-intensity rotating anode X-ray source and a curved image plate detector, providing rapid and accurate data collection for a wide range of crystallographic applications.
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Lab products found in correlation
Rapid auto, by Rigaku (2 mentions)
6130 quadrupole mass spectrometer, by Agilent Technologies (1 mentions)
Jms 700 mass spectrometer, by JEOL (1 mentions)
Lambda 35 spectrophotometer, by Jasco (1 mentions)
Chirascan v100 cd spectrometer, by Applied Photophysics (1 mentions)
Ft ir 4200 spectrometer, by Jasco (1 mentions)
1200 series hplc, by Phenomenex (1 mentions)
Uv vis 151, by Gilson (1 mentions)
P 2000 polarimeter, by Jasco (1 mentions)
Dibutylphthalate polystyrene xylene (dpx), by Bruker (1 mentions)
Ft ir 6300, by Jasco (1 mentions)
R axis rapid 2 diffractometer, by Rigaku (1 mentions)
Crystalstructure, by Rigaku (1 mentions)
Silica gel 60 rp 18 f254s, by Merck Group (1 mentions)
Accutof lc plus jms t100lp, by JEOL (1 mentions)
67ga gacl3, by Fujifilm (1 mentions)
Ultima 4, by Rigaku (1 mentions)
Smz1500, by Nikon (1 mentions)
17 protocols using r axis rapid diffractometer
1
Analytical Techniques for Structural Characterization
2
Synthetic Protocols for Pyrazole and Formimidamide Derivatives
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Melting points were determined with a Sanyo (Gallenkamp)
instrument.
Infrared spectra were recorded using KBr pellets and a Jasco FT-IR
6300 instrument, and νmax was recorded in cm–1. 1H, and 13C NMR spectra were
evaluated with a Bruker DPX instrument at 600 MHz for 1H NMR and 100 MHz for 13C NMR and DMSO-d6 as a solvent, with TMS as an internal standard. Chemical
shifts are reported in d (parts per million). Mass
spectra were measured using a GCeMS DFS Thermo spectrometer in the
EI (70 eV) mode. The single crystal X-ray diffraction analysis was
made on the Rigaku R-AXIS RAPID diffractometer using filtered Mo Kα
radiation at −123 °C. The structure was solved by direct
methods, and the structure refinement was performed by SHELXL 2017/1.
All nonhydrogen atoms were refined anisotropically. The hydrogen atoms
were placed at calculated positions and refined using a riding model.
All solids were crystallized using the appropriate solvent (15.0 mL)
described in the experimental part, and the solids were heated at
60–65 °C (ethanol or ethanol/water) or at 35–40
°C (acetone) until they dissolved followed by filtering while
hot and then cooling. The 5-amino-1-phenyl-1H-pyrazole-4-carbonitrile8 (15 (link)) and N′,N″-(1,4-phenylene)-bis(N,N-dimethylformimidamide) 2 were prepared following
previously reported procedures.19 (link)
instrument.
Infrared spectra were recorded using KBr pellets and a Jasco FT-IR
6300 instrument, and νmax was recorded in cm–1. 1H, and 13C NMR spectra were
evaluated with a Bruker DPX instrument at 600 MHz for 1H NMR and 100 MHz for 13C NMR and DMSO-d6 as a solvent, with TMS as an internal standard. Chemical
shifts are reported in d (parts per million). Mass
spectra were measured using a GCeMS DFS Thermo spectrometer in the
EI (70 eV) mode. The single crystal X-ray diffraction analysis was
made on the Rigaku R-AXIS RAPID diffractometer using filtered Mo Kα
radiation at −123 °C. The structure was solved by direct
methods, and the structure refinement was performed by SHELXL 2017/1.
All nonhydrogen atoms were refined anisotropically. The hydrogen atoms
were placed at calculated positions and refined using a riding model.
All solids were crystallized using the appropriate solvent (15.0 mL)
described in the experimental part, and the solids were heated at
60–65 °C (ethanol or ethanol/water) or at 35–40
°C (acetone) until they dissolved followed by filtering while
hot and then cooling. The 5-amino-1-phenyl-1H-pyrazole-4-carbonitrile
previously reported procedures.19 (link)
3
Single Crystal X-ray Diffraction Analysis
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The data for 1 , 2 , and 3 were measured on Rigaku R-AXIS RAPID diffractometer using multi-layer mirror monochromated Mo Kα (λ = 0.71073 Å) radiation. The data for 4 were measured on Rigaku R-AXIS RAPID II diffractometer using multi-layer mirror monochromated Cu Kα (λ = 1.54178 Å) radiation. Crystal data and experimental details are listed in Table S1 . The calculations were performed with the Olex2 software package [50 (link)]. All structures were solved using ShelXT [51 (link)] structure solution program using the intrinsic phasing method, and the other atoms were found in subsequent Fourier maps. The structures were refined with ShelXL [52 (link)] using least squares minimization. All non-hydrogen atoms were anisotropically refined, unless otherwise stated. The hydrogen atoms were placed at their idealized positions, and the riding model was assumed, unless otherwise stated. CCDC-1970392 (1 ), 2167309 (2 ), 2167311 (3 ), 2167310 (4 ) contain the supplementary crystallographic data for this paper. 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 22 August 2022.
4
Single-crystal Photochemical Structural Analysis
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Single-crystal diffraction data for compound 1 were collected using an R-AXIS RAPID diffractometer (Rigaku) equipped with monochromatic Cu-Kα and Mo-Kα radiation sources. Measurements were performed at 223 and 293 K. The low temperature measurements were conducted to obtain the crystal structure after light irradiation. At first, measurements were taken before irradiation at 223 K. Following this, the crystal sample was irradiated with UV light for several seconds at 293 K while being rotated, as photochemical reactions are slow at low temperature. After irradiation, the structure was determined again at 223 K to preserve photoproducts in the crystal. The crystal structure at 293 K in the absence of UV light was also determined, to correlate with the bending behaviour observed at room temperature. Crystal structures were solved by using the direct method of SHELXD2013, and refined on F2 by the full-matrix least-squares method, SHELXL.26 (link) Calculations were performed using the software package CrystalStructure (Rigaku).27
5
Single Crystal Diffraction Analysis
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The single crystal diffraction data were collected on an R-AXIS RAPID diffractometer (Rigaku, Japan) at 150 K using the Crystal-Clear software package. The structures were solved by direct methods and expanded using Fourier techniques. The structure refinement was performed using SHELXL-2017/1. All non-hydrogen atoms were refined anisotropically, and hydrogen atoms were placed at calculated positions and refined using the riding model. The crystallographic data for the structure reported in this paper have been deposited at the Cambridge Crystallographic Data Centre as a supplementary publication (CCDC 2000224–2000226 ).
6
Single Crystal X-Ray Diffraction of Compound 3
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A single crystal of 3 was mounted on a glass fiber. All measurements were made using a Rigaku R-Axis Rapid diffractometer and graphite-monochromated Mo-Kα radiation (λ = 0.71075 Å). Data were collected at a temperature of –100 °C to a maximum value of 2θ of 54.8°. An empirical absorption correction was applied, which resulted in transmission factors ranging from 0.653 to 0.977. The structure was solved using SIR2004 (ref. 25 ) and refined using SHELXL-97 with full-matrix least-squares techniques on F2.26 Non-hydrogen atoms were refined anisotropically; hydrogen atoms were refined using the riding model. All calculations were performed using Crystal Structure 4.0 (Crystal Structure Analysis Package, Rigaku, Japan), except for refinement, which was performed using SHELXL-97.26 The image presented herein was generated using ORTEP-32 software.27
7
Single-Crystal Diffraction at 90K
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Single-crystal diffraction measurements at 90 K for crystals of A and B, immersed in a paratone N-oil and mounted on Micro Mounts holder, were conducted using Rigaku R-axis RAPID diffractometer. Collected data were processed by using RAPID AUTO (Rigaku). Crystal structures were solved by a direct method with SIR2011 (ref. 12 (link)) for A and SHELXS97 (ref. 13 (link)) for B using CrystalStructure 4.2 crystallographic software package14 with the exception of refinement, which was performed using SHELXL-2018/3 (ref. 15 ) by a full-matrix least-squares technique. For disordered parts, isotropic refinements were performed. The disordered model was fixed with some restraints and constraints. Molecular graphics were prepared using Mercury 3.8 software.16 (link)
8
Structural Determination of Diclofenac-Proline Cocrystals
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Single-crystal X-ray diffraction data were collected in ω-scan mode using a Rigaku R-AXIS RAPID diffractometer (Tokyo, Japan) with a Mo Kα radiation (λ = 0.71075 Å) rotating anode source. The integrated and scaled data were empirically corrected for absorption effects using ABSCOR. The initial structures were solved using direct methods with SHELXT and refined with SHELXL. All nonhydrogen atoms were refined anisotropically. All hydrogen atoms were found in a difference Fourier map; however, they were placed by geometrical calculations and treated using a riding model during the refinement. Two salt cocrystals of diclofenac sodium–proline–water were found and determined successfully, which then were named NDPT (from condition I) and NDPM (from condition II).
9
Synthetic protocols for DOTA-based radiopharmaceuticals
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1H NMR spectra were recorded on
a JEOL JNM-ECS 400 spectrometer (JEOL, Tokyo, Japan). Mass spectrometry
was performed using an AccuTOF LC-plus (JMS-T100LP, JEOL, Tokyo, Japan).
The analytical methods for reversed-phase HPLC (RP-HPLC) are described
in detail in theSupporting Information . Radiochemical conversions and in vitro stability
were determined by reversed-phase (RP)-TLC (Silica gel 60 RP-18 F254S, Merck, Tokyo, Japan) developed with a mixture of 0.1%
aqueous TFA and MeCN with 0.1% TFA (2:3, v/v). [67Ga]GaCl3 was purchased from FUJIFILM RI Pharma (Tokyo, Japan). p-NO2-Bn-DOTA and DOTA were purchased from Macrocyclics
(Texas, USA) and Tokyo Chemical Industry (Tokyo, Japan), respectively.
DOTA-Bn-TOC and DOTATOC were prepared from the same procedure described
previously.29 (link) The syntheses of DOTAGAMBu, DO3AMBu, and p-NO2-Bn-DO3A are described in theSupporting Information . The other chemicals obtained from the commercial sources were of
reagent grade or higher and were used without further purification.
Data for single crystal X-ray diffraction analyses were collected
on a Rigaku R-AXIS RAPID diffractometer using a graphite monochromator
with Cu Kα radiation (l = 1.54187 Å).
Data collection and reduction were performed using RAPID AUTO. The
crystallography structures were solved by direct methods using SHELXL97
and refined with SHELXL97.
a JEOL JNM-ECS 400 spectrometer (JEOL, Tokyo, Japan). Mass spectrometry
was performed using an AccuTOF LC-plus (JMS-T100LP, JEOL, Tokyo, Japan).
The analytical methods for reversed-phase HPLC (RP-HPLC) are described
in detail in the
were determined by reversed-phase (RP)-TLC (Silica gel 60 RP-18 F254S, Merck, Tokyo, Japan) developed with a mixture of 0.1%
aqueous TFA and MeCN with 0.1% TFA (2:3, v/v). [67Ga]GaCl3 was purchased from FUJIFILM RI Pharma (Tokyo, Japan). p-NO2-Bn-DOTA and DOTA were purchased from Macrocyclics
(Texas, USA) and Tokyo Chemical Industry (Tokyo, Japan), respectively.
DOTA-Bn-TOC and DOTATOC were prepared from the same procedure described
previously.29 (link) The syntheses of DOTAGAMBu, DO3AMBu, and p-NO2-Bn-DO3A are described in the
reagent grade or higher and were used without further purification.
Data for single crystal X-ray diffraction analyses were collected
on a Rigaku R-AXIS RAPID diffractometer using a graphite monochromator
with Cu Kα radiation (l = 1.54187 Å).
Data collection and reduction were performed using RAPID AUTO. The
crystallography structures were solved by direct methods using SHELXL97
and refined with SHELXL97.
10
Single-Crystal X-Ray Structural Analysis
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Single-crystal X-ray
crystallographic analysis was performed using a Rigaku R-AXIS RAPID
diffractometer. The initial structural model was resolved by the intrinsic
phasing method (SHELXT)47 (link) and was refined
by using the least-square method of the squared amplitudes of the
structure factor (SHELXL).48 (link) Non-hydrogen
atoms were refined using an anisotropic temperature factor, and the
hydrogen atoms are fixed to the positions calculated by the riding
model. Olex2 Version 1.3.0 program49 (link) was
used for all analysis.
crystallographic analysis was performed using a Rigaku R-AXIS RAPID
diffractometer. The initial structural model was resolved by the intrinsic
phasing method (SHELXT)47 (link) and was refined
by using the least-square method of the squared amplitudes of the
structure factor (SHELXL).48 (link) Non-hydrogen
atoms were refined using an anisotropic temperature factor, and the
hydrogen atoms are fixed to the positions calculated by the riding
model. Olex2 Version 1.3.0 program49 (link) was
used for all analysis.
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