High-performance liquid chromatography (HPLC) was measured on a Waters 2487 (600E) equipment with a column of Poroshell 120 (EC-C18, 2.7 μm, 4.6 × 150 mm), using acetonitrile/water mixture (ratio = 9:1, v/v) with a flow rate of 1.0 mL/min. Nuclear magnetic resonance (NMR) spectra were carried out on a Bruker AVIII 400 MHz NMR spectrometer equipped with a Dual Probe, using deuterated chloroform (CDCl3) as the solvent. High-resolution mass spectra (HRMS) were measured on a GCT premier CAB048 mass spectrometer manipulated in a GC-TOF module with chemical ionization (CI). Ultraviolet-visible (UV-Vis) spectra were collected on a Varian Cary 50 Conc UV-Visible Spectrophotometer with Peltier. Photoluminescence (PL) spectra and their lifetimes at room temperature and 77 K were recorded on an Edinburgh FLS980 Spectrometer. Absolute quantum yield (QY) was collected on a Hamamatsu Quantum Yield Spectrometer C11347 Quantaurus. Single-crystal X-ray diffraction (XRD) was carried out on a Rigaku Oxford Diffraction (SuperNova) with Atlas diffractometer (Cu Kα (λ = 1.54184 Å)). The single-crystal structures were solved with Olex2 software. Dynamic light scattering (DLS) measurements for the diameter of aggregates were measured on a Malvern Zetasizer Nano ZS equipment at room temperature. All digital photos of crystals and amorphous compounds were recorded on a Canon EOS 60D camera.
Oxford diffraction
Manufactured by Rigaku
The Oxford Diffraction is a laboratory equipment product designed for X-ray diffraction analysis. It provides the core function of collecting and analyzing diffraction data from crystalline materials to determine their atomic and molecular structures.
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Lab products found in correlation
Eos 60d camera, by Canon (2 mentions)
Aviii 400 mhz nmr spectrometer, by Bruker (2 mentions)
Quantum yield spectrometer c11347 quantaurus, by Hamamatsu Photonics (2 mentions)
Fls980 spectrometer, by Edinburgh Instruments (2 mentions)
Zetasizer nano z, by Malvern Panalytical (1 mentions)
Cary 50 uv visible spectrophotometer, by Agilent Technologies (1 mentions)
Fluorolog 3 spectrofluorometer, by Horiba (1 mentions)
Zetasizer nano zs equipment, by Malvern Panalytical (1 mentions)
Crysalis pro, by Agilent Technologies (1 mentions)
Xtalab synergy, by Rigaku (1 mentions)
6 protocols using oxford diffraction
1
Comprehensive Characterization of Organic Compounds
2
Single-crystal XRD structural analysis
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Single-crystal XRD for an HB CT crystal was carried out on a Rigaku Oxford Diffraction CCD single-crystal diffractometer furnished with a graphite monochromator and Mo Kα radiation (0.71073 Å) at 293 K. Unit cell measurement, data collection, integration, scaling, and absorption corrections were executed using Rigaku Oxford Diffraction. Multiscan absorption corrections were carried out using SADABS-2014. The crystal structure was solved by direct methods with SHELXS-97 and refined using the full matrix least squares process using the SHELXL-2014 stream in the OLEX2 Software. Aromatic and H(N) hydrogen positions were derived from geometrical considerations, methyl and H(O) ones from difference maps. All H-atoms were then refined at idealized positions riding on the parent atoms with isotropic displacement parameters Uiso(H) = 1.2U ∼ eq ∼ (C/N) or 1.5U ∼ eq ∼ (–CH ∼ 3∼ and –OH hydrogens). All methyl and OH hydrogen atoms were allowed to rotate but not to tip (AFIX 43, 137, 147). The packing figure of the crystal was produced using Mercury 3.8 software.
3
Comprehensive Characterization of Organic Compounds
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NMR measurements of 1H and 13C were conducted on a Bruker AVIII 400 MHz NMR spectrometer equipped with a Dual Probe. High-resolution mass spectra (HRMS) were performed on a CT Premier CAB048 mass spectrometer using a positive ESI-TOF module. Ultraviolet-visible (UV-Vis) spectra were recorded on a Varian Cary 50 UV-Visible Spectrophotometer. Photoluminescence (PL) spectra were carried out on Fluorolog®-3 (HORIBA) spectrofluorometer. Absolute quantum yields (QY) were collected using an integrating sphere on a Hamamatsu Quantum Yield Spectrometer C11347 Quantaurus. Fluorescence lifetime was recorded on an Edinburgh FLS980 Spectrometer. Dynamic light scattering (DLS) of the diameters of aggregates was measured on Malvern Zetasizer Nano ZS equipment at room temperature. Single-crystal structures of four compounds were confirmed through single-crystal X-ray diffraction on a Rigaku Oxford Diffraction (SuperNova) with Atlas diffractometer (Cu Kα (λ = 1.54184 Å) and solved using Olex2 software. All digital photographs of the solution, mixture, and crystalline powder were recorded using a Canon EOS 60D camera.
4
Single-Crystal X-Ray Diffraction Protocols
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Single-crystal X-ray diffraction
data were collected using a Nonius KappaCCD diffractometer (2 and 5a ) or an Oxford Diffraction (Rigaku Oxford
Diffraction) SuperNova diffractometer (1 , 3b , 3c , 4 , 5b ) fitted with an
Oxford Cryosystems Cryostream 600 Series/700 Plus open-flow nitrogen
cooling device.123 (link) Data for3a were collected at Diamond Light Source (beamline I19)124 (link) fitted with an Oxford Cryosystems HeliX open-flow
helium cryostat.125 (link) DENZO/SCALEPACK,126 (link) CrysAlisPro,127 or
CrystalClear were used for data collection and reduction as appropriate.
The structures were solved ab initio using SIR92128 (link) or SUPERFLIP.129 (link) All structures were refined with full-matrix least-squares on F2 using CRYSTALS.130 (link),131 (link) Hydrogen atoms were, in some cases, visible in the difference Fourier
map and treated in the usual manner.132 (link) In the remaining cases, and particularly for disordered assemblies,
hydrogen atoms were added geometrically. Full structural data are
included in theSI , including CIF files, and have been submitted to the CCDC
as numbers 1444134–1444141. These data can also be obtained
free of charge from The Cambridge Crystallographic Data Centre viahttp://www.ccdc.cam.ac.uk/data_request/cif .
data were collected using a Nonius KappaCCD diffractometer (
Diffraction) SuperNova diffractometer (
Oxford Cryosystems Cryostream 600 Series/700 Plus open-flow nitrogen
cooling device.123 (link) Data for
helium cryostat.125 (link) DENZO/SCALEPACK,126 (link) CrysAlisPro,127 or
CrystalClear were used for data collection and reduction as appropriate.
The structures were solved ab initio using SIR92128 (link) or SUPERFLIP.129 (link) All structures were refined with full-matrix least-squares on F2 using CRYSTALS.130 (link),131 (link) Hydrogen atoms were, in some cases, visible in the difference Fourier
map and treated in the usual manner.132 (link) In the remaining cases, and particularly for disordered assemblies,
hydrogen atoms were added geometrically. Full structural data are
included in the
as numbers 1444134–1444141. These data can also be obtained
free of charge from The Cambridge Crystallographic Data Centre via
5
Structural Analysis of BEA Salts
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Data for BEA salts 11 , 15 , and 16 were collected on a Rigaku Oxford Diffraction «Rigaku «XtaLAB Synergy» diffractometer using monochromated CuKα radiation. Experimental details are shown in Table 2 . Structures were solved by direct methods and refined by full-matrix least-squares methods with the SHELXL program [46 (link)] as incorporated into the OLEX2 program package [47 (link)]. The carbon- and nitrogen-bound H atoms were placed in calculated positions and were included in the refinement in the riding model approximation with Uiso(H) set to 1.2Ueq(C) and C–H 0.95 Å for the CH groups, with Uiso(H) set to 1.2Ueq(C) and C–H 0.99 Å for the CH2 groups and with Uiso(H) set to 1.2Ueq(N) and N–H 0.91 Å for the NH2 groups. The oxygen-bound H atoms were located in the difference Fourier map. Empirical absorption correction was applied in the CrysAlisPro program complex (CrysAlisPro, Agilent Technologies, Yarnton, UK. Version 1.171.36.32). Supplementary crystallographic data have been deposited at Cambridge Crystallographic Data Centre (2,236,100 for 11 , 2,236,099 for 15 and 2,236,098 for 16 ) and can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif (accessed on 13 January 2023).
6
Synthesis and Crystal Structure of Compound 1
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Compound 1 was acquired as colorless crystals from CH3OH using the vapor diffusion method. The single crystal X-ray diffraction data was obtained on a Rigaku Oxford Diffraction with Cu-Kα radiation (λ = 1.54178 A). The structures were solved by direct methods using the SHELXS-97 program (University of Göttingen, Göttingen, Germany) and refined using full-matrix least-squares difference Fourier techniques using Olex2 software (Durham University, Durham, UK). Crystallographic data for 1 have been deposited with the Cambridge Crystallographic Data Centre. Copies of the data can be obtained, free of charge, on application to the Director, CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: 44-(0)1223-336033, or e-mail: [email protected] ).
Crystal data of (1 ): C18H18N2O3, Mr = 310.34, triclinic, a = 5.9198(6) Å, b = 11.5313(9) Å, c = 11.6390(8) Å, α = 66.749(7), β = 88.243(7), γ = 79.762(7), V = 717.68(10) Å3, space group P−1, Z = 2, Dcalcd = 1.436 mg/m3, μ = 0.805 mm−1, and F(000) = 328.0. Crystal dimensions: 0.08 × 0.05 × 0.02 mm3. Independent reflections: 2838 (Rint = 0.0448). The final R1 values were 0.0474, ωR2 = 0.1324 (I > 2σ(I)). The goodness of fit on F2 was 1.031. CCDC number: 1820872.
Crystal data of (
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