NMR experiments were performed with a Bruker Avance II 300 (magnetic field of 7.05 T) spectrometer in a 4-mm triple resonance sample head (also from Bruker) at a rotation speed of 10 kHz. The 29Si MAS NMR measurements were performed using a single-pulse quantitative experiment with a 90° pulse length of 3.5 μs, a recycle delay of 60 s, and no proton decoupling during acquisition. The spectra are indirectly referenced with N(SiMe3)3/σ(iso) = 2.4 ppm, with respect to tetramethylsilanes [σ(iso) = 0.0 ppm].
Avance 2 300
Manufactured by Bruker
Sourced in United States
The Avance II 300 is a high-performance nuclear magnetic resonance (NMR) spectrometer produced by Bruker. It is designed to provide advanced capabilities for analyzing and characterizing chemical compounds and materials. The Avance II 300 operates at a magnetic field strength of 7.0 Tesla, enabling high-resolution NMR experiments.
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Lab products found in correlation
Esquire 3000 plus, by Bruker (3 mentions)
500 ms lc ion trap mass spectrometer, by Agilent Technologies (2 mentions)
Fts 3000 mx, by Bio-Rad (2 mentions)
Avance 3 400, by Bruker (2 mentions)
Avance 400 spectrometer, by Bruker (2 mentions)
Avance 400, by Bruker (2 mentions)
Vertex 70, by Bruker (2 mentions)
Ni no3 2 6h2o, by Merck Group (1 mentions)
Co no3 2 6h2o, by Merck Group (1 mentions)
Lambda 35, by PerkinElmer (1 mentions)
Nicolet ir200, by Thermo Fisher Scientific (1 mentions)
Avance 3 600, by Bruker (1 mentions)
Microtof 2 spectrometer, by Bruker (1 mentions)
Polygram sil g uv254, by Macherey-Nagel (1 mentions)
Avance 3 800, by Bruker (1 mentions)
Zq 2000 mass spectrometer, by Waters Corporation (1 mentions)
C18 column, by Waters Corporation (1 mentions)
Hct116, by Keygen Biotech (1 mentions)
Hct 8, by Keygen Biotech (1 mentions)
Sw620, by Keygen Biotech (1 mentions)
29 protocols using avance 2 300
1
Quantitative 29Si MAS NMR Experiments
2
Synthesis and Characterization of Pyrazole-Derived Metal Complexes
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5-methyl 3-pyrazole carbohydrazide was prepared according to a literature process [34] (link). 3-(hydroxyimino) butan-2-one, Co(NO3)2.6H2O and Ni(NO3)2.6H2O were purchased from Aldrich and used as received. Infrared spectra (4000–400 cm−1) were recorded on a Nicolet Impact 400D or a BIO-RAD FTS 3000 MX spectrophotometer instrument in KBr pellets; wave numbers are in cm−1; abbreviations: vs, very strong; s, strong; ms, medium strong; m, medium; br, broad. UV-Vis spectra were recorded in 10−4 M MeOH solutions of the complexes with a Perkin Elmer instrument (Lambda 35). 1H NMR spectra were recorded at ambient temperature on a Bruker Avance II 300 (Ultra Shield Magnet) spectrometer operating at 300.130 MHz. The chemical shifts (δ) are reported in ppm using tetramethyl silane as the internal reference. Electrospray mass spectra (ESI-MS) were run with an ion-trap instrument (Varian 500-MS LC Ion Trap Mass Spectrometer) equipped with an electrospray ion source. For electrospray ionization, the drying gas and flow rate were optimized according to the particular sample with 35 p.s.i. nebulizer pressure. Scanning was performed from m/z 50 to 1000 in CH3OH solution. The compounds were studied in both positive and negative modes (capillary voltage = 80–105 V). Other abbreviations used (NMR): s: singlet, T1: type-I binding mode as HL−, T2: type-II binding mode as L2−.
3
Synthesis and Characterization of Coordination Compounds
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Compounds 1 [29 (link)], 2 [22 (link)], 6 [23 (link)], 7 [24 (link)], 12 [21 (link)], 23 [30 (link)], and 1,4,8,11-tetraazatriciclo[9.3.1.14,8]hexadecane [23 (link)] were prepared according to published procedures. All other reagents were commercial grade and used without further purification. NMR spectra were recorded in a Bruker AVANCE II 300 or 400 MHz spectrometer, at 296 K unless stated otherwise, referenced internally to residual proton-solvent (1H) or solvent (13C) resonances, and reported relative to tetramethyl silane (0 ppm). 19F NMR was referenced to external CF3COOH (−76.55 ppm). 1H-13C{1H} HSQC and 1H-1H COSY NMR experiments were performed in order to perform all the assignments. Elemental analyses were obtained from Laboratório de Análises do IST.
4
Synthesis of Heterocyclic Compounds
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7,16-Bis[2-(3-bromopropoxy)benzoyl]-5,14-dihydrodibenzo[b,i][1,4,8,11]tetraazacyclotetradecine, 7,16-Bis[2-hydroxybenzoyl]-5,14-dihydrodibenzo[b,i][1,4,8,11]tetraazacyclotetradecine and 9-(6-bromopentyl)adenine were prepared by the procedure described earlier [13 (link)–15 (link)]. All reagents were purchased from commercial sources (Sigma-Aldrich) and were used as received. Solvents were dried by using standard methods and were freshly distilled before use.
1H and 13C NMR were run on Bruker AVANCE II 300 and Bruker AVANCE III 600 spectrometers. Chemical shifts (δ) are expressed in parts per million and J values in hertz. Signal multiplicities are denoted as s (singlet), d (doublet), t (triplet), q (quartet), and m (multiplet). The IR-ATR spectra were recorded with a Thermo Fisher Scientific Nicolet IR200. ESI mass spectra were taken on a Bruker Daltonics microTOF-II spectrometer.
1H and 13C NMR were run on Bruker AVANCE II 300 and Bruker AVANCE III 600 spectrometers. Chemical shifts (δ) are expressed in parts per million and J values in hertz. Signal multiplicities are denoted as s (singlet), d (doublet), t (triplet), q (quartet), and m (multiplet). The IR-ATR spectra were recorded with a Thermo Fisher Scientific Nicolet IR200. ESI mass spectra were taken on a Bruker Daltonics microTOF-II spectrometer.
5
Organic Synthesis Procedures and Characterization
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Chemicals were purchased from Sigma Aldrich (Taufkirchen, Germany), TCI (Eschborn, Germany) or from abcr GmbH (Germany) and used without further purification. The solvents were purified by distillation and dried according to usual standard laboratory methods. Reactions with air- and moisture-sensitive compounds were carried out in vacuum-heated flasks under a nitrogen atmosphere. Solutions at 0 °C were obtained with the aid of an ice-water bath. Thin-layer chromatography (TLC) was carried out on silica gel-coated films Polygram® SIL G/UV254 (Macherey-Nagel, layer thickness 0.2 mm). In addition to UV detection (254 nm), common staining reagents such as molybdophosphoric acid or potassium permanganate were used as staining solutions. Flash column chromatography was carried out on silica gel 60 Å (grain size 35–70 μm) from Fisher Scientific. The NMR spectra were recorded with Avance II 300 (300 MHz for 1H, 75 MHz for 13C) and Avance III 400 (400 MHz for 1H, 100 MHz for 13C) spectrometers from Bruker at room temperature. Tetramethylsilane served as the internal standard. The chemical shifts are given in ppm relative to the standard. The coupling constants J are given in Hertz (Hz). Full synthetic details of the synthesized compounds are given in the Supporting Information.
6
Comprehensive Chemical Analysis of Anticancer Compounds
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All commercially available chemicals were from Sigma Chemical Co. and purified when necessary. The purity of all compounds was identified with TLC (Qingdao silica gel F254, 0.25 mm layer thickness) or HPLC (Waters, C18 column, 4.6×150 mm). Bruker Avance II-300 or Bruker Avance III-800 spectrometer was used to record the 1H NMR (300 or 800 MHz) and 13C NMR (75or 200 MHz) spectra, while DMSO-d6 was the solvent and tetramethylsilane was the internal standard. ZQ 2000 mass spectrometer (Waters, US) or Fourier transform ion cyclotron resonance (FT-ICR, 9.4T solariX, Bruker, US) with dual ion source of ESI/matrix-assisted laser desorption ionization ESI/MS was used for mass analyses.
HCT-116, LS174T, SW620, SGC7901, Eca109, MKN28, HCT-8, and S180 cells were purchased from key GENBioTECH (Nanjing China). Male ICR mice (22 ± 2 g) were purchased commercially from Laboratory Animal Center of Capital Medical University. In vitro and in vivo assays were examined by the Ethics Committee of Capital Medical University. The committee approved that the assays can use the mentioned cells and mice can be used for the assays, and assured that the welfare of mice met the requirements of Animal Welfare Act and NIH Guide for Care and Use of Laboratory Animals.
Biological data were statistically analyzed with ANOVA, and the P-value less than 0.05 was considered statistically significant.
HCT-116, LS174T, SW620, SGC7901, Eca109, MKN28, HCT-8, and S180 cells were purchased from key GENBioTECH (Nanjing China). Male ICR mice (22 ± 2 g) were purchased commercially from Laboratory Animal Center of Capital Medical University. In vitro and in vivo assays were examined by the Ethics Committee of Capital Medical University. The committee approved that the assays can use the mentioned cells and mice can be used for the assays, and assured that the welfare of mice met the requirements of Animal Welfare Act and NIH Guide for Care and Use of Laboratory Animals.
Biological data were statistically analyzed with ANOVA, and the P-value less than 0.05 was considered statistically significant.
7
Spectroscopic Characterization of Compounds
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Mass spectra were recorded on a Bruker Esquire 3000 Plus, with the electrospray (ESI) technique. UV−Vis spectra were recorded with 1 cm quartz cells on an Evolution 600 spectrophotometer (Thermo Electron Scientific Instrument LCC, Madison, WI, USA). 1H, 13C{1H} and 19F NMR (CFCl3 used as standard), including 2D experiments, were recorded at room temperature on a Bruker Avance 400 spectrometer (Bruker, Billerica, MA, USA) (1H, 400 MHz, 13C, 100.6 MHz, 19F, 376.5 MHz) or on a Bruker Avance II 300 ((Bruker, Billerica, MA, USA) (1H, 300 MHz; 13C, 75.5 MHz; 19F, 282.3 MHz) with chemical shifts (δ, ppm) reported relative to the solvent peaks of the deuterated solvent [50 (link)].
8
Quantifying Tissue Mechanics via μMRI
9
Spectroscopic Characterization of Chemical Compounds
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Mass spectra were recorded on a BRUKER ESQUIRE 3000 PLUS, with the electrospray (ESI) technique. The attenuated total reflection (ATR–FTIR) spectra of solid samples were recorded on a PerkinElmer FT‐IR spectrometer equipped with a universal ATR sampling accessory. 1H and 13C{1H} APT NMR, including 2 D experiments, were recorded at room temperature on a BRUKER AVANCE 400 spectrometer (1H, 400 MHz; 13C, 100.6 MHz; 19F, 376.5 MHz) or on a BRUKER AVANCE II 300 spectrometer (1H, 300 MHz; 13C, 75.5 MHz; 19F, 282.3 MHz), with chemical shifts (ppm) reported relative to the solvent peaks of the deuterated solvent.17
10
Synthesis of Phosphine-Stabilized Silylenes
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All manipulations were performed under inert atmosphere of argon by using Schlenk or high‐pressure NMR tube techniques. Dry, oxygen‐free solvents were employed. 1H, 11B, 19F, 13C, 29Si and 31P NMR spectra were recorded on Bruker Avance II 300 MHz, Avance III HD 400 MHz and Avance I and II 500 MHz spectrometers. 1H, 29Si and 13C NMR chemical shifts are reported in ppm relative to SiMe4 as internal standard. 31P NMR chemical shifts are expressed in ppm relative to 85 % H3PO4. 11B chemical shifts are relative to BF3⋅OEt2 and 19F chemical shifts are relative to CFCl3 as external reference. The following abbreviations and their combinations are used: br, broad; s, singlet; d, doublet; t, triplet; q, quartet, m, multiplet. 1H and 13C resonance signals were attributed by means of 2D COSY, HSQC and HMBC experiments. GC‐MS analyses were performed on a MS Perkin Elmer Clarus MS560 and GC PerkinElmer Clarus 500. The phosphine‐stabilized silylenes 1‐Cl [34] and 1‐H [12a] were synthesized as previously reported.
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