Reaction mixtures at elevated temperatures were heated in an oil bath unless otherwise noted. All chemicals were used as received. Petroleum ether (PE) refers to the fraction boiling in the 60–90 °C range. Melting points were measured on a RY-I apparatus and uncorrected. NMR spectra were recorded on a Bruker AV 400 spectrometer at 400 MHz (1H NMR), 101 MHz (13C NMR). Chemical shifts were reported in ppm relative to internal TMS for 1H NMR data, deuterated solvent for 13C NMR data, respectively. Data are presented in the following space: chemical shift, multiplicity, coupling constant in hertz (Hz), and signal area integration in natural numbers. High-resolution mass spectra (HRMS) were obtained on Bruker maXis impact instrument with ESI ion source and TOF mass analyzer.
Maxis impact instrument
Manufactured by Bruker
The Maxis Impact instrument is a high-performance mass spectrometer designed for accurate, high-resolution mass analysis. It features an advanced ion optics system and high-speed data acquisition capabilities to deliver precise and reliable results.
Automatically generated - may contain errors
Lab products found in correlation
Av 400 spectrometer, by Bruker (1 mentions)
Tof mass analyzer, by Bruker (1 mentions)
Fluoromax 4 instrument, by Horiba (1 mentions)
Thermogravimetric analyzer, by PerkinElmer (1 mentions)
Cary 660 ftir spectrometer, by Agilent Technologies (1 mentions)
Advance 400 mhz, by Bruker (1 mentions)
Advance 600 mhz, by Bruker (1 mentions)
Ultimate 3 000 hplc instrument, by Thermo Fisher Scientific (1 mentions)
Dataanalysis 4, by Bruker (1 mentions)
Dpx 300 mhz nmr spectrometer, by Bruker (1 mentions)
Alpha platinum atr, by Bruker (1 mentions)
Spectrum one ft ir spectrometer, by Bruker (1 mentions)
Av spectrometers, by Bruker (1 mentions)
7 protocols using maxis impact instrument
1
Organic Compound Characterization Protocol
2
Comprehensive Physical Characterization of Samples
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1H and 13C NMR
spectra were measured on a 400 MHz NMR spectrometer. The ESI-MS spectra
were recorded on a Bruker maXis Impact instrument, using electrospray
ionization (ESI) in a positive ion mode method. The steady-state fluorescence
spectra were measured on a Horiba Scientific Instrument/Fluoromax-4
instrument. The absorption spectra were measured on Shimadzu UV-NIR-3600.
Elemental analyses were carried out on a Thermofinnigan FLASH EA 1112
series CHNS instrument. The SEM, AFM, and TEM images of the samples
were measured on JSM-7600F working at 5 kV, Nano Surf Flex AFM, and
JEOL TEM 2100F instruments, respectively. All of the solvents used
were of HPLC grade and were dried by following standard procedures
immediately before use.
spectra were measured on a 400 MHz NMR spectrometer. The ESI-MS spectra
were recorded on a Bruker maXis Impact instrument, using electrospray
ionization (ESI) in a positive ion mode method. The steady-state fluorescence
spectra were measured on a Horiba Scientific Instrument/Fluoromax-4
instrument. The absorption spectra were measured on Shimadzu UV-NIR-3600.
Elemental analyses were carried out on a Thermofinnigan FLASH EA 1112
series CHNS instrument. The SEM, AFM, and TEM images of the samples
were measured on JSM-7600F working at 5 kV, Nano Surf Flex AFM, and
JEOL TEM 2100F instruments, respectively. All of the solvents used
were of HPLC grade and were dried by following standard procedures
immediately before use.
3
Characterization of Novel Organic Compounds
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All chemicals
were purchased from Sigma-Aldrich. 1H and 13C NMR spectra were recorded on a JEOL JNM ECX-500 FT-NMR spectrometer
using CDCl3 and DMSO-d6 as
solvents. Fourier-transform infrared spectroscopy spectra were recorded
on an Agilent Cary-660 FT-IR spectrometer with a Diamond ATR accessory.
HR-MS spectra were recorded on the Bruker Maxis Impact instrument.
TGA measurements were performed on a PerkinElmer thermogravimetric
analyzer (model: Pyris 1 TGA) at a heating rate of 10 °C min–1 under an N2 atmosphere.
were purchased from Sigma-Aldrich. 1H and 13C NMR spectra were recorded on a JEOL JNM ECX-500 FT-NMR spectrometer
using CDCl3 and DMSO-d6 as
solvents. Fourier-transform infrared spectroscopy spectra were recorded
on an Agilent Cary-660 FT-IR spectrometer with a Diamond ATR accessory.
HR-MS spectra were recorded on the Bruker Maxis Impact instrument.
TGA measurements were performed on a PerkinElmer thermogravimetric
analyzer (model: Pyris 1 TGA) at a heating rate of 10 °C min–1 under an N2 atmosphere.
4
Characterization of Organic Compounds
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Chemicals and solvents
were supplied by Fisher Chemicals, Sigma-Aldrich, Lancaster Chemicals
Ltd., and Tokyo chemicals industry, used as received. Deuterated solvents
were obtained from Goss Scientific Instruments Ltd. and Cambridge
Isotope Laboratories Inc. All commercial starting materials were used
as supplied, without further purification. Off-line NMR data were
recorded on a Bruker Advance 600 MHz or a Bruker Advance 400 MHz instrument,
in deuterated solvent, at T = 298 K, using TMS as
the scale reference. Chemical shifts are reported using the δ-scale,
referenced to the residual solvent protons in the deuterated solvent
for 1H and 13C NMR (i.e., 1H, δ
(CDCl3) = 7.26; 13C, δ (CDCl3) = 77.16). All chemical shifts are given in ppm, and all coupling
constants (J) are given in Hz (J) as absolute values. Characterization of spin multiplicities: s
= singlet, d = doublet, t = triplet, q = quartet, m = multiplet, dd
= double doublet, dt = double triplet, dq = double quartet, and ddt
= double doublet of triplets. Chromatographic separation of the reaction
mixture was achieved with a reverse phase column by Agilent (Poroshell
120 HPH C18, 3.0 × 100 mm, 2.7 μm) on a Thermo Fisher UltiMate
3000 HPLC instrument. The MS apparatus was a Bruker MaXis Impact instrument,
acquisition range at 50–2000 m/z.
were supplied by Fisher Chemicals, Sigma-Aldrich, Lancaster Chemicals
Ltd., and Tokyo chemicals industry, used as received. Deuterated solvents
were obtained from Goss Scientific Instruments Ltd. and Cambridge
Isotope Laboratories Inc. All commercial starting materials were used
as supplied, without further purification. Off-line NMR data were
recorded on a Bruker Advance 600 MHz or a Bruker Advance 400 MHz instrument,
in deuterated solvent, at T = 298 K, using TMS as
the scale reference. Chemical shifts are reported using the δ-scale,
referenced to the residual solvent protons in the deuterated solvent
for 1H and 13C NMR (i.e., 1H, δ
(CDCl3) = 7.26; 13C, δ (CDCl3) = 77.16). All chemical shifts are given in ppm, and all coupling
constants (J) are given in Hz (J) as absolute values. Characterization of spin multiplicities: s
= singlet, d = doublet, t = triplet, q = quartet, m = multiplet, dd
= double doublet, dt = double triplet, dq = double quartet, and ddt
= double doublet of triplets. Chromatographic separation of the reaction
mixture was achieved with a reverse phase column by Agilent (Poroshell
120 HPH C18, 3.0 × 100 mm, 2.7 μm) on a Thermo Fisher UltiMate
3000 HPLC instrument. The MS apparatus was a Bruker MaXis Impact instrument,
acquisition range at 50–2000 m/z.
5
Quantification of FKGK18 in Murine Serum
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Submandibular vein blood from mice was obtained between 0 and 72 h following FKGK18 administration. To 100 μL of serum sample, 1 mL of chloroform and 50 μL of 1 mol/L aqueous hydrochloric acid were added and the mixture vortexed for 30 s, centrifuged for 5 min, and the organic layer transferred to a clean tube. The remaining aqueous layer was re-extracted with 1 mL of chloroform by the same procedure. The two organic layers were combined, dried, reconstituted in methanol, and analyzed for FKGK18 by high-resolution mass spectrometry, recorded with a quadrupole time-of-flight Bruker maXis impact instrument using negative ion mode electrospray ionization protocol. Data acquisition was carried out with Bruker Daltonics DataAnalysis 4.1.
6
Characterization of Sorption Properties
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General procedures Chemicals were obtained from commercial sources and used as received. NMR spectra were recorded on a Bruker DPX 300 MHz NMR spectrometer. ESI-MS were measured on a Bruker Maxis Impact instrument in positive ion mode. Infra-red spectra were recorded as solid phase samples on a Bruker ALPHA Platinum ATR. Elemental analyses were performed by the service at University of Leeds or the London Metropolitan University. Gas and vapour sorption studies were performed on samples from the same batch of compounds 1 and 3. Samples were washed with acetone, dried under vacuum and then underwent further drying under vacuum at 100 °C overnight immediately prior to measurements. Ethanol sorption was measured at 298 K using a MicrotracBEL Belsorp-Max gas/vapor adsorption measurement instrument. Other gases were measured using a Micromeritics instrument at temperatures indicated.
7
Synthesis and Characterization of Organometallic Complexes
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All manipulations were performed under an atmosphere of argon, using Schlenk and glove box techniques unless otherwise 22 were synthesised using literature protocols. All other solvents and reagents are commercial products and were used as received. NMR spectra were recorded on Bruker AV spectrometers at 298 K unless otherwise stated. 1 H NMR spectra recorded in 1,2-C 6 H 4 F 2 were referenced using the highest intensity peak of the highest (δ 6.865) frequency fluoroarene multiplet. 13 C{ 1 H} NMR spectra recorded in 1,2-C 6 H 4 F 2 were referenced using an internal sealed capillary of C 6 D 6 . Chemical shifts are quoted in ppm and coupling constants in Hz. IR spectra were recorded on a PerkinElmer Spectrum One FT-IR spectrometer at 293 K. ESI-MS analyses were recorded on Bruker Maxis Impact instrument. Microanalyses were performed by Stephen Boyer at London Metropolitan University.
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