Biocatalytic oligomerization-induced self-assembly of crystalline cellulose oligomers into nanoribbon networks assisted by organic solvents

• Yuuki Hata,
• Yuka Fukaya,
• Toshiki Sawada,
• Masahito Nishiura and
• Takeshi Serizawa

Beilstein J. Nanotechnol. 2019, 10, 1778–1788, doi:10.3762/bjnano.10.173

• structure of the products was analyzed by 1H NMR spectroscopy and MALDI–TOF mass spectrometry. The NMR spectra of the representative products showed proton signals for cellulose oligomers (Figure 5). In addition, the mass spectra further revealed the successful synthesis of cellulose oligomers (Figure 6

• dispersions was dried at 105 °C for 24 h, followed by weighing. For 1H NMR spectroscopy, ATR-FTIR absorption spectroscopy, and XRD measurements, as much as possible of the supernatant after the final centrifugation was removed by pipette, followed by adding water to the products. The resultant product aqueous

• dispersions with residual organic solvents were lyophilized and then stored at 4 °C until use. Characterization of the products For NMR spectroscopy, the lyophilized products were dissolved in 4% NaOD/D2O to obtain product solutions (≥2% (w/v)). 1H NMR spectra were recorded on an AVANCE III HD500 spectrometer

Chiral nanostructures self-assembled from nitrocinnamic amide amphiphiles: substituent and solvent effects

• Hejin Jiang,
• Huahua Fan,
• Yuqian Jiang,
• Li Zhang and
• Minghua Liu

Beilstein J. Nanotechnol. 2019, 10, 1608–1617, doi:10.3762/bjnano.10.156

• four times in EtOH/THF to obtain the target compounds: 2NCLG (0.71 g, 56% yield), 3NCLG (0.94 g, 74% yield) and 4NCLG (0.90 g, 71% yield) (Scheme 1). 2NCLG: 1H NMR (500 MHz, DMSO-d6, 100 °C, TMS) δ 0.83–0.94 (t, 6H), 1.20–1.50 (m, 60H), 1.36–1.50 (m, 4H), 1.80–1.90 (m, 1H), 1.93–2.00 (m, 1H), 2.10–2.20

• (m, 2H), 3.12–3.17 (m, 4H), 4.33–4.44 (q, 1H), 6.73–6.82 (d, 1H), 7.35–7.43 (s, 1H), 7.53–7.66 (m, 2H), 7.68–7.81 (m, 3H), 7.96–8.07 (m, 2H); MALDI–TOF–MS m/z: [M]+ calcd. for C50H88N4O5, 825.26; found, [M + Li]+ 833.5, [M + Na]+ 847.5. 3NCLG: 1H NMR (500 MHz, DMSO-d6, 100 °C, TMS) δ 0.83–0.93 (t, 6H

• C50H88N4O5, 825.26 [M]+; found, [M + Li]+ 833.5, [M + Na]+ 847.5. 4NCLG: 1H NMR (500 MHz, DMSO-d6, 100 °C, TMS) δ 0.80–0.93 (t, 6H), 1.16–1.50 (m, 60H), 1.36–1.52 (m, 4H), 1.81–1.93 (m, 1H), 1.93–2.04 (m, 1H), 2.09–2.29 (m, 2H), 3.03–3.16 (m, 4H), 4.33–4.43 (q, 1H), 6.88–6.98 (d, 1H), 7.33–7.45 (s, 1H), 7.48

Scavenging of reactive oxygen species by phenolic compound-modified maghemite nanoparticles

• Małgorzata Świętek,
• Yi-Chin Lu,
• Rafał Konefał,
• Liliana P. Ferreira,
• M. Margarida Cruz,
• Yunn-Hwa Ma and
• Daniel Horák

Beilstein J. Nanotechnol. 2019, 10, 1073–1088, doi:10.3762/bjnano.10.108

• phenolic compounds Physicochemical characterization The effect of the AA/H2O2 redox system and the phenolic compounds on the molecular structure of chitosan was investigated using ATR-FTIR and 1H NMR spectroscopy. The ATR-FTIR spectra of CS and of chitosans modified with phenolic compounds differed from

• stretching, respectively. In the ATR-FTIR spectra of chitosans modified with phenolic compounds, the peak at 1728 cm−1 was slightly shifted to 1734 cm−1, indicating binding of phenolic compounds to the carbonyl groups of CS. Similar to ATR-FTIR spectra, the 1H NMR spectra of CS and chitosans modified with

• formed, the AA/H2O2 redox system is convenient for chitosan degradation [19][20]. Hydroxyl radicals attack the polysaccharide, forming macroradicals, which are then prone to covalently bind phenolic compounds. According to the ATR-FTIR and 1H NMR spectroscopy results, the structural similarity between CS

Structural and optical properties of penicillamine-protected gold nanocluster fractions separated by sequential size-selective fractionation

• Xiupei Yang,
• Zhengli Yang,
• Fenglin Tang,
• Jing Xu,
• Maoxue Zhang and
• Martin M. F. Choi

Beilstein J. Nanotechnol. 2019, 10, 955–966, doi:10.3762/bjnano.10.96

• accelerating voltage of 200 kV. Proton nuclear magnetic resonance (1H NMR) spectra were performed on a Bruker AC 400 NMR spectrometer (Rheinstetten, Karlsruhe, Germany) in concentrated D2O solutions. At the same time, the fractions were investigated by a matrix-assisted laser desorption ionization time-of

• fractions, indicating that these AuNCs are of polycrystalline structure. 1H NMR spectroscopy The spectra of D2O solutions of free ligand, crude and fractions obtained from SSSP are presented in Figure 5. The proton peaks are in the range of chemical shifts (δ) 1.4–4.8 ppm and the strong peak at 4.79 ppm is

• 1.44 and 1.53 ppm, respectively, are chemically different in the 1H NMR spectrum due to the chirality effect [22] of the adjacent carbon (C* in the right panel of Figure 5). Peak splitting is also observed due to chiral induction in the 1H NMR spectrum of the crude product (spectrum 2) and size

Removal of toxic heavy metals from river water samples using a porous silica surface modified with a new β-ketoenolic host

• Said Tighadouini,
• Smaail Radi,
• Abderrahman Elidrissi,
• Khadija Haboubi,
• Maryse Bacquet,
• Stéphanie Degoutin,
• Mustapha Zaghrioui and
• Yann Garcia

Beilstein J. Nanotechnol. 2019, 10, 262–273, doi:10.3762/bjnano.10.25

• organic layer, extracted with CH2Cl2, was dried and concentrated in vacuo. The resulting residue was chromatographed using silica and dichloromethane as eluent. Final product characteristic: yellow powder; yield: 30%; mp 102 °C; Rf: 0.6 (CH2Cl2/MeOH 9:1)/silica. 1H NMR (DMSO-d6) 3.48 (s, 0.1H, keto, CH2

pH-mediated control over the mesostructure of ordered mesoporous materials templated by polyion complex micelles

• Emilie Molina,
• Mélody Mathonnat,
• Jason Richard,
• Patrick Lacroix-Desmazes,
• Martin In,
• Philippe Dieudonné,
• Thomas Cacciaguerra,
• Corine Gérardin and
• Nathalie Marcotte

Beilstein J. Nanotechnol. 2019, 10, 144–156, doi:10.3762/bjnano.10.14

• DD was calculated from the integration of the amide (δ = 101 ppm) and amine (10 ppm) peaks using the following formula: Note that a similar DD was obtained from liquid 1H NMR data recorded on a Bruker 400 MHz spectrometer using the method reported by Trombotto et al. [30]. The quantity of lactate

• /lactic acid present in the sample was calculated from the liquid 1H NMR spectrum recorded in D2O. The amount of water was deduced from elemental analysis. The molar composition of the repetitive unit constituting the oligochitosan was then: H-(C6H11O4N)0.83(C8H13O5N)0.17-OH, 1.31(C3H6O3), 0.09(H2O

A novel polyhedral oligomeric silsesquioxane-modified layered double hydroxide: preparation, characterization and properties

• Xianwei Zhang,
• Zhongzhu Ma,
• Hong Fan,
• Carla Bittencourt,
• Jintao Wan and
• Philippe Dubois

Beilstein J. Nanotechnol. 2018, 9, 3053–3068, doi:10.3762/bjnano.9.284

• ]. Thereafter, the acylation reaction of OCPS with succinic anhydride was carried out to afford OCPS. The 1H NMR, 13C NMR and 29Si NMR spectra of OAPS and OCPS presented in Figure 2 and the MALDI-TOF-MS spectra, XRD patterns and FTIR spectra of OAPS and OCPS in Figure 3a–c reveal the well-defined structures

• . The SEM images of OCPS in Figure 3d show that OCPS has a micrometer-sized strip geometry. The details are as follows: (1) for OAPS: 1H NMR (DMSO-d6) δ 8.27 (s, NH3, 24H), 2.78 (s, CH2N, 16H), 1.73 (s, SiCH2CH2, 16H), 0.69 (m, SiCH2, 16H); 1H NMR (D2O) δ 2.96 (m, CH2N, 16H), 1.73 (m, SiCH2CH2, 16H

• +) 3200–2800 cm−1, δas(–NH3+) 1606 cm−1, υ(Si–O–Si) 1175–1060 cm−1, υ(Si–C) 800 cm−1; XRD: 2θ 6.72°, 7.32°, 11.00°, 18.55°, 20.34°, 22.03°, 23.01°, 25.57°. (2) for OCPS: 1H NMR (DMSO-d6) δ 11.95 (s, br, COOH, 8H), 7.83 (t, J = 4.9 Hz, NHC=O, 8H), 3.00 (d, J = 5.3 Hz, CH2N, 16H), 2.41 (t, J = 6.6 Hz

Cytotoxicity of doxorubicin-conjugated poly[N-(2-hydroxypropyl)methacrylamide]-modified γ-Fe₂O₃ nanoparticles towards human tumor cells

• Zdeněk Plichta,
• Yulia Kozak,
• Rostyslav Panchuk,
• Viktoria Sokolova,
• Matthias Epple,
• Lesya Kobylinska,
• Pavla Jendelová and
• Daniel Horák

Beilstein J. Nanotechnol. 2018, 9, 2533–2545, doi:10.3762/bjnano.9.236

• diluted in ethyl acetate (50 mL). Residual compounds and ethyl acetate were removed by filtration and vacuum-evaporation, respectively, and MMAA was distilled (100 °C/13 Pa); yield 55%. 1H NMR (CDCl3) δ 1.96 (s, 3H), 3.09 (s, 3H), 3.77 (s, 3H), 4.14 (s, 2H), 5.03 (dd, H), 5.24 (dd, H) (Figure 1a

• /mL) to obtain γ-Fe2O3@PHPMA. Second, P(HPMA-MMAA)-Dox (0.1–13.0 µg) was dissolved in aqueous γ-Fe2O3@PHPMA colloid (2–260 µg; 50 mg γ-Fe2O3/mL) to get γ-Fe2O3@P(HPMA-MMAA)-Dox before use in the cell experiments. Characterization methods 1H NMR (in CDCl3) and FTIR spectra of MMAA were recorded on a

• methyl ester of sarcosine was methacryloylated. Structure and purity of MMAA was confirmed by 1H NMR (Figure 1a), gas chromatography (Figure 1b), and FTIR spectroscopy (Figure 1c). The FTIR spectrum exhibited characteristic peaks at 1745 and 1620 cm−1 ascribed to strong C=O stretching vibrations of ester

Nanoconjugates of a calixresorcinarene derivative with methoxy poly(ethylene glycol) fragments for drug encapsulation

• Alina M. Ermakova,
• Julia E. Morozova,
• Yana V. Shalaeva,
• Victor V. Syakaev,
• Aidar T. Gubaidullin,
• Alexandra D. Voloshina,
• Vladimir V. Zobov,
• Irek R. Nizameev,
• Olga B. Bazanova,
• Igor S. Antipin and
• Alexander I. Konovalov

Beilstein J. Nanotechnol. 2018, 9, 2057–2070, doi:10.3762/bjnano.9.195

• and Discussion Synthesis and characterization of tetraundecylcalix[4]resorcinarene–mPEG conjugate To obtain the amphiphilic calixresorcinarene, tetraundecylcalix[4]resorcinarene 1 was functionalized with tosylated mPEG-550 (2) (Scheme 1). The obtained macrocycle 3 was characterized by 1H NMR, 13С NMR

• and FTIR. Its molecular weight was measured by static light scattering (SLS) and MALDI-TOF. In the 1H NMR spectrum of 3 signals of ethyleneoxy and methoxy groups at 3.65 and 3.37 ppm, respectively, are observed; signals of bridged methylidene groups and aromatic groups are very broad (Figure 1b). Also

• , the strong band of stretching vibrations of the C–O–C groups of PEG at 1110 cm−1 appears, confirming the conjugation of macrocycle and PEG (Figure 1d). In the 1H NMR spectrum of 3, the ratios between the integral intensities of terminal methoxy groups (at 3.37 ppm) and methyl and (CH2)9 groups (at

Nanocomposites comprised of homogeneously dispersed magnetic iron-oxide nanoparticles and poly(methyl methacrylate)

• Sašo Gyergyek,
• David Pahovnik,
• Ema Žagar,
• Alenka Mertelj,
• Rok Kostanjšek,
• Miloš Beković,
• Marko Jagodič,
• Heinrich Hofmann and
• Darko Makovec

Beilstein J. Nanotechnol. 2018, 9, 1613–1622, doi:10.3762/bjnano.9.153

• characterized by transmission electron microscopy (TEM). 1H NMR spectra were recorded in CDCl3 on a 300 MHz Agilent Technologies DD2 NMR spectrometer in the pulse Fourier transform mode with both a relaxation delay and an acquisition time of 5 s. Tetramethylsilane (TMS, δ = 0) was used as an internal chemical

• NMR and FTIR spectra, respectively (Supporting Information File 1, Figures S1 and S2). The shift of the peak for the methine group, denoted with D, from 3.62 ppm in the 1H NMR spectrum of the original ricinoleic acid to 4.88 ppm in the 1H NMR spectrum of RA-MMA, and a pronounced increase in intensity

• of the left-hand side of the vibration band of the carbonyl group confirm the formation of the methacrylic ester of RA (Supporting Information File 1, Figures S3, S4 and S5). The disappearance of the peak representing the MMA double bond in the 1H NMR spectrum of the RA-PMMA reveals the successful

Closed polymer containers based on phenylboronic esters of resorcinarenes

• Tatiana Yu. Sergeeva,
• Rezeda K. Mukhitova,
• Irek R. Nizameev,
• Marsil K. Kadirov,
• Polina D. Klypina,
• Albina Y. Ziganshina and
• Alexander I. Konovalov

Beilstein J. Nanotechnol. 2018, 9, 1594–1601, doi:10.3762/bjnano.9.151

• C–C and C–H bonds at 1191, 1048 and 533 cm−1 are present in the IR spectrum of p(SRA-B) (see Supporting Information File 1, Figure S3). In the 13C and 1H NMR spectra of p(SRA-B), the signals of SRA, BA ester and polystyrene are present (see Supporting Information File 1, Figure S4 and Figure S5

• ). The integrals of proton signals in the 1H NMR spectrum at 1.0–4.5 ppm indicate that p(SRA-B) contains one polystyrene unit per one SRA fragment, i.e., the polystyrene fraction is about 11 wt % of p(SRA-B). According to differential scanning calorimetry (DSC) data, p(SRA-B) is thermally more stable

• and washed with ethanol (3.15 g, 96%). 1H NMR (600 MHz, D2O) δ 7.21 (s, 4H), 4.50 (t, 4H), 4.29 (s, 8H), 3.65 (t, 8H), 2.21 (d, 2H), 1.57 (m, 2H); 13C NMR (600 MHz, D2O) δ 152, 125, 122, 108, 62, 48, 34, 30, 29; IR (cm−1) 3390, 2939, 2871, 1608, 1473, 1213, 1150, 1041, 979, 900, 800, 778, 760, 664

Enzymatically promoted release of organic molecules linked to magnetic nanoparticles

• Chiara Lambruschini,
• Silvia Villa,
• Luca Banfi,
• Fabio Canepa,
• Fabio Morana,
• Annalisa Relini,
• Paola Riani,
• Renata Riva and
• Fulvio Silvetti

Beilstein J. Nanotechnol. 2018, 9, 986–999, doi:10.3762/bjnano.9.92

• 1.0, CHCl3); 1H NMR (300 MHz, DMSO-d6, 25 °C) δ 8.15 (d, 3JH,H = 8.3 Hz, 1H, NH Leu), 8.10 (d, 3JH,H = 7.3 Hz, 1H, NH Lys), 7.26 (d, 3JH,H = 8.3 Hz, 1H, NH Alloc), 6.75 (t, 3JH,H = 5.6 Hz, 1H, NH Boc), 6.00–5.77 (m, 1H, CH2=CHCH2O), 5.28 (dd, 3JH,H = 17.3 Hz, 2JH,H = 1.8 Hz, 1H, CHH=CHCH2O), 5.16 (dd

• chromatography on silica gel eluting with 5% MeOH in DCM + 1% AcOH to give 5 (847 mg, white foam, 67%, AcOH removed as azeotrope with heptane). Rf 0.25 (DCM/MeOH 95:5 + 1% AcOH; HBr followed by ninhydrin). [α]D20 −8.61 (c 1.0, CHCl3); 1H NMR (300 MHz, DMSO-d6, 25 °C) δ 12.46 (brs, 1H, COOH), 8.14 (d, 3JH,H = 8.3

• concentrated and purified by flash column chromatography on silica gel eluting with 5% MeOH in DCM to give 6 (272 mg, off-white solid, 55% from 5). mp 200–201 °C; Rf 0.59 (DCM/MeOH 9:1; UV and HBr followed by ninhydrin). [α]D24 −10.2 (c 1.0, MeOH); 1H NMR (300 MHz, DMSO-d6, 25 °C) δ 8.52 (t, 3JH,H = 5.6 Hz, 1H

Synthesis and characterization of two new TiO₂-containing benzothiazole-based imine composites for organic device applications

• Anna Różycka,
• Agnieszka Iwan,
• Krzysztof Artur Bogdanowicz,
• Michal Filapek,
• Natalia Górska,
• Damian Pociecha,
• Marek Malinowski,
• Patryk Fryń,
• Agnieszka Hreniak,
• Jakub Rysz,
• Paweł Dąbczyński and
• Monika Marzec

Beilstein J. Nanotechnol. 2018, 9, 721–739, doi:10.3762/bjnano.9.67

• unreacted compounds. Finally, the imine was dried at 60 °C under vacuum for 24 h to give the SP1 (70%). 1H NMR (400 MHz, CDCl3), δ [ppm]: 8.78 (s, 2H, –HC=N–), 8.16–8.06 (m, 6H), 7,96 (m, 2H), 7.84 (dd, 4H), 7.58–7.46 (m, 2H), 7.33 (m, 2H), 4.40–4.30 (m, 4H), 3.53–3.38 (m, 8H), 1.91–1.50 (m,12H). Synthesis

• . Then the compound was dried at 60 °C for 12 h to give the SP2 (75%). 1H NMR (400 MHz, CDCl3), δ [ppm]: 8.82 (s, 1H, –HC=N–), 8.16 (dd, 1H), 7,95 (dd, 1H), 7.60 (m, 1H), 7.57–7.43 (m, 3H), 7.30 (d, 2H), 2.63 (t, 2H), 1.62 (m, 2H), 1.35–1.18 (m,18H), 0.87 (t, 3H). Preparation of imine:TiO2 mixture To

• TiO2 (anatase form), SP1:TiO2 and SP2:TiO2 mixtures were obtained using the same spectrometer and spectral parameters. All spectra were recorded using OPUS 7.0 software and plotted with Origin 2017 Pro. The samples were characterized with 1H NMR, using deuterated chloroform (CDCl3) as a solvent with a

Electron interactions with the heteronuclear carbonyl precursor H₂FeRu₃(CO)₁₃ and comparison with HFeCo₃(CO)₁₂: from fundamental gas phase and surface science studies to focused electron beam induced deposition

• Ragesh Kumar T P,
• Paul Weirich,
• Lukas Hrachowina,
• Marc Hanefeld,
• Ragnar Bjornsson,
• Helgi Rafn Hrodmarsson,
• Sven Barth,
• D. Howard Fairbrother,
• Michael Huth and
• Oddur Ingólfsson

Beilstein J. Nanotechnol. 2018, 9, 555–579, doi:10.3762/bjnano.9.53

Design of polar self-assembling lactic acid derivatives possessing submicrometre helical pitch

• Alexej Bubnov,
• Cyril Vacek,
• Michał Czerwiński,
• Terezia Vojtylová,
• Wiktor Piecek and
• Věra Hamplová

Beilstein J. Nanotechnol. 2018, 9, 333–341, doi:10.3762/bjnano.9.33

• recrystallized from methanol. The molecular structure was checked for all synthesised compounds by 1H NMR spectra recorded on a Varian VNMRS 300 instrument, where deuteriochloroform (CDCl3) served as a solvent. The signal of the solvent was used as an internal standard. The purity of the final compounds was

• chloroform solution (c = 0.10) using a polarimeter from Optical Activity Ltd., Ramsey, UK. The optical rotation was found as follows for KL 3/4: +16.0; KL 3/5: +15.0; KL 4/4: +18.9; KL 4/5: +13.5; KL 4/6: +14.1. 1H NMR for KL 3/4 (CDCl3, 300 MHz) 8.29 (d, 2H, ortho to -COOAr), 8.18 (d, 2H, ortho to

• -COOC*), 8.07 (d, 2H, ortho to -CO-), 7.76 (m, 4H, ortho to -Ar), 7.34 (d, 2H, ortho to -OCO), 5.34 (q, 1H, C*H), 4.16 (m, 2H, COOCH2), 3.00 (t, 2H, CH2CO), 1.64 (d, 3H, CH3C*), 1.3–1.7 (m, 6H, CH2), 0.87 (m, 6H, CH3). 1H NMR for KL 3/5 (CDCl3, 300 MHz) 8.29 (d, 2H, ortho to -COOAr), 8.19 (d, 2H, ortho

Dielectric properties of a bisimidazolium salt with dodecyl sulfate anion doped with carbon nanotubes

• Doina Manaila Maximean,
• Viorel Cîrcu and
• Constantin Paul Ganea

Beilstein J. Nanotechnol. 2018, 9, 164–174, doi:10.3762/bjnano.9.19

• characterized by 1H NMR, 13C NMR and IR spectroscopy. Its liquid crystalline properties were analyzed by polarizing optical microscopy (POM), differential scanning calorimetry (DSC) and powder X-ray diffraction (XRD) studies. The dielectric spectra of the ILC doped with different concentrations of carbon

• belonging to the two imidazolium rings are shifted upfield in the 1H NMR spectrum of [bisC8ImC10][C12H25OSO3]2 compared to their position in the 1H NMR of the bromide salt 2. The most significant change was observed for the signal assigned to the proton adjacent to the two nitrogen atoms (Scheme 1). For the

• , 10.75; N, 5.43; found: C, 65.59; H, 11.03; N, 5.27; 1H NMR (500 MHz, CDCl3) δ 9.58 (s, 2H), 7.78 (s, 2H), 7.24 (s, 2H), 4.32–4.20 (m, 8H), 4.01 (t, 4H), 1.94-1.84 (t, 8H), 1.64 (t, 4H), 1.42–1.22 (m, 68H), 0.86 (t, 12H); 13C NMR (125 MHz, CDCl3) δ 136.9, 123.3, 121.6, 67.8, 49.9, 49.4, 31.9; 29.7, 29.6

The rational design of a Au(I) precursor for focused electron beam induced deposition

• Ali Marashdeh,
• Thiadrik Tiesma,
• Niels J. C. van Velzen,
• Sjoerd Harder,
• Remco W. A. Havenith,
• Jeff T. M. De Hosson and
• Willem F. van Dorp

Beilstein J. Nanotechnol. 2017, 8, 2753–2765, doi:10.3762/bjnano.8.274

• described in [12]. The products were analyzed by C and H elemental analysis and showed satisfactory values. MeAu(PMe3), anal. calcd for C4H12PAu: C, 16.68; H, 4.20; found: C, 17.15; H, 4.26. Samples were also analyzed by 1H and 31P NMR spectroscopy. MeAu(PMe3): 1H NMR (400 MHz, C6D6, 25 °C) δ 1.20 (d, 3JHP

Synthesis of [{AgO₂CCH₂OMe(PPh₃)}_n] and theoretical study of its use in focused electron beam induced deposition

• Jelena Tamuliene,
• Julian Noll,
• Peter Frenzel,
• Tobias Rüffer,
• Alexander Jakob,
• Bernhard Walfort and
• Heinrich Lang

Beilstein J. Nanotechnol. 2017, 8, 2615–2624, doi:10.3762/bjnano.8.262

• (1H NMR, CDCl3 δ = 7.26; 13C{1H} NMR, CDCl3 δ = 77.16 ppm) or by external standards (31P{1H} NMR relative to 85% H3PO4 0.0 ppm and P(OMe)3 139.0 ppm). The FTIR spectra were recorded using a Thermo Nicolet IR 200 instrument. Vapor pressure experiments were performed with a Mettler Toledo TGA/DSC1 1100

• : C, 54.69; H, 4.47%; mp 145 °C; IR (KBr, cm−1) υ: 3056 (w), 2977 (w), 1594 (m), 1585 (m), 1575 (CO2,asym, s), 1569 (s), 1479 (m), 1436 (m), 1402 (CO2,sym, m), 1319 (m), 1189 (m), 1104 (s), 1026 (w), 997 (w), 934 (m), 907 (w), 754 (m), 745 (m), 706 (m), 694 (s); 1H NMR (CDCl3) δ 3.44 (s, 3H, CH3

• ), 4.05 (s, 2H, CH2), 7.40–7.50 (m, 15H, C6H5); 13C{1H} NMR (CDCl3) δ 59.0 (CH3), 71.9 (CH2), 129.4 (d, 3JP,C = 11 Hz, mC/C6H5), 130.0 (d, 1JP,C = 40 Hz, iC/C6H5), 131.5 (d, 4JP,C = 2.0 Hz, pC/C6H5), 134.1 (d, 2JPC = 16 Hz, oC/C6H5); 31P{1H} NMR (CDCl3) δ 16.0 (s, AgP(C6H5)3); HRMS (ESI–TOF) m/z: calcd

Imidazolium-based ionic liquids used as additives in the nanolubrication of silicon surfaces

• Patrícia M. Amorim,
• Ana M. Ferraria,
• Rogério Colaço,
• Luís C. Branco and
• Benilde Saramago

Beilstein J. Nanotechnol. 2017, 8, 1961–1971, doi:10.3762/bjnano.8.197

• °C for 5 h. In the end of the reaction the solvent was evaporated and the crude was washed with diethyl ether (5 × 5 mL under vigorous stirring) and then dried in vacuum at 85 °C for 3 days. The pure product was obtained as a viscous brown liquid (31 g, 87%). 1H NMR (DMSO-d6, 400 MHz) δ 3.90 (s, 3H

• days. The pure product was obtained as a brown viscous liquid (8.4g, 78%). 1H NMR (DMSO-d6, 400 MHz) δ 3.87 (s, 3H), 4.84 (d, J = 4.00 Hz, 2H), 5.33 (m, 2H), 6.04 (m, 1H), 7.70 (d, J = 4.00 Hz, 2H), 9.09 ppm (s, 1H); 19F NMR (DMSO-d6, 282 MHz) δ −77.99, −77.62 ppm; FTIR (KBr) : 518.86, 575.30, 642.20

• × 5 mL under vigorous stirring) and then dried in vacuum at 85 °C for 3 days. The pure product was obtained as a viscous brown liquid (5.2 g, 99%). 1H NMR (DMSO-d6, 400 MHz) δ 1.10 (t, J = 12.00 Hz, 3H), 1.44 (t, J = 12.00 Hz, 3H), 3.79 (t, J = 12.00 Hz, 2H), 4.24 (m, 2H), 5.39 (m, 1H), 5.95 (m, 1H

Carbon nano-onions as fluorescent on/off modulated nanoprobes for diagnostics

• Stefania Lettieri,
• Marta d’Amora,
• Adalberto Camisasca,
• Alberto Diaspro and
• Silvia Giordani

Beilstein J. Nanotechnol. 2017, 8, 1878–1888, doi:10.3762/bjnano.8.188

• solution and a white precipitate formed. The precipitate was filtered and washed with fresh chloroform until the total removal of impurities was reached (4.5 g, 8%). 1H NMR (400 MHz, DMSO-d6) δ 2.49 (s, 6H), 6.52 (s, 2H), 10.28 (s, 1H), 10.32 (s, 1H). See Supporting Information File 1, Figure S1. Compound

• a red powder (850 mg, 49%). 1H NMR (400 MHz, chloroform-d) δ 1.43 (s, 6H), 2.08 (s, 6H), 2.56 (s, 6H), 4.78 (s, 1H), 5.97 (s, 2H), 6.63 (s, 2H). See Supporting Information File 1, Figure S2. BODIPY 3 was synthesized by dissolving 220 mg of 2 (0.6 mmol) and 4-(N,N-dimethylamino)benzaldehyde (1.34 g

• plug using acetone before purification by chromatography (SiO2, EtOAc/hexane 2:8, increasing amount of EtOAc). The pure fractions were distilled, and the pure compound was precipitated from DCM in hexane to obtain a black powder (145 mg, 40%). 1H NMR (400 MHz, chloroform-d) δ 1.50 (s, 6H), 2.14 (s, 6H

Self-assembly of chiral fluorescent nanoparticles based on water-soluble L-tryptophan derivatives of p-tert-butylthiacalix[4]arene

• Pavel L. Padnya,
• Irina A. Khripunova,
• Olga A. Mostovaya,
• Timur A. Mukhametzyanov,
• Vladimir G. Evtugyn,
• Vyacheslav V. Vorobev,
• Yuri N. Osin and
• Ivan I. Stoikov

Beilstein J. Nanotechnol. 2017, 8, 1825–1835, doi:10.3762/bjnano.8.184

• ). The melting points were determined using a Boetius Block apparatus. The purity of the compounds was monitored by melting points, boiling points, 1H NMR and thin layer chromatography (TLC) on 200 μm UV 254 silica gel plate using UV light. All experiments (NMR, UV–vis, CD spectroscopy and DLS) were

• dried under reduced pressure over phosphorus pentoxide. L-tryptophan ethyl ester hydrochloride 2: 1H NMR (400 MHz, 298 K, DMSO-d6) δ 1.08 (t, 3JHH = 7.1 Hz, 3H, CH3CH2O–), 3.22–3.30 (m, 2H, CHCH2Trp), 4.07 (q, 3JHH = 7.1 Hz, 2H, CH3CH2O–), 4.19 (m, 1H, NНCHСО), 6.99–7.53 (m, 5H, ArHTrp), 8.55 (s, 1Н

• neutral pH. Then glacial acetic acid was added to pH 6.5. The organic phase was separated, dried over anhydrous magnesium sulfate, after which the benzene was removed under reduced pressure. N-bromoacetyl-L-tryptophan ethyl ester 3: 1H NMR (400 MHz, 298 K, DMSO-d6) δ 1.08 (t, 3JHH = 7.1 Hz, 3H, CH3CH2O

Luminescent supramolecular hydrogels from a tripeptide and nitrogen-doped carbon nanodots

• Maria C. Cringoli,
• Slavko Kralj,
• Marina Kurbasic,
• Massimo Urban and
• Silvia Marchesan

Beilstein J. Nanotechnol. 2017, 8, 1553–1562, doi:10.3762/bjnano.8.157

• Fmoc solid phase peptide synthesis and purified by RP-HPLC, as previously described [25]. The peptide identity and purity was verified by ESI–MS, 1H NMR and 13C NMR. The as-produced NCNDs were synthesized and purified following a reported procedure [6]. Sample preparation Tripeptide hydrogels were

A biofunctionalizable ink platform composed of catechol-modified chitosan and reduced graphene oxide/platinum nanocomposite

• Peter Sobolewski,
• Agata Goszczyńska,
• Małgorzata Aleksandrzak,
• Karolina Urbaś,
• Joanna Derkowska,
• Agnieszka Bartoszewska,
• Jacek Podolski,
• Ewa Mijowska and
• Mirosława El Fray

Beilstein J. Nanotechnol. 2017, 8, 1508–1514, doi:10.3762/bjnano.8.151

• Supporting Information File 1). The obtained 1H NMR spectrum (see Figure S3, Supporting Information File 1) confirms the reaction product and we calculate the DoC as 13%. Despite being on the high end of our desired range, the obtained catechol-modified chitosan (CHI-HCA) readily dissolved in water, up to 3

• ) and lyophilized. The degree of conjugation (DoC, defined as the mol % of chitosan repeating units carrying a catechol group) was calculated from 1H NMR data (see Supporting Information File 1 for details). Preparation of ink and printing The ink was prepared by admixing the rGO–Pt dispersion with a 2

Deposition of exchange-coupled dinickel complexes on gold substrates utilizing ambidentate mercapto-carboxylato ligands

• Martin Börner,
• Laura Blömer,
• Marcus Kischel,
• Peter Richter,
• Georgeta Salvan,
• Dietrich R. T. Zahn,
• Pablo F. Siles,
• Maria E. N. Fuentes,
• Carlos C. B. Bufon,
• Daniel Grimm,
• Oliver G. Schmidt,
• Daniel Breite,
• Bernd Abel and
• Berthold Kersting

Beilstein J. Nanotechnol. 2017, 8, 1375–1387, doi:10.3762/bjnano.8.139

• from an ethanol/water (1:1) solvent system to give 4-methylphenylboronic acid as colorless needles (2.94 g, 21.63 mmol, 37%). 1H NMR (400 MHz, CDCl3) δ 2.42 (s, 3H, CH3), 7.29 (d, 3J = 7.5 Hz, 2H, ArH), 8.13 (d, 3J = 7.5 Hz, 2H, ArH). This material was used without further purification in the next step

• (2.07 g, 12.47 mmol, 35%). 1H NMR (300 MHz, acetone-d6) δ 7.96–8.03 (m, 4H, ArH). This material was used without further purification in the next step. Synthesis of H2L6, step 3,4'-(methylthio)-[1,1'-biphenyl]-4-carboxylic acid 4-Boronobenzoic acid (3.00 g, 18.08 mmol), 4-bromothioanisole (4.41 g, 21.70

• gave 4'-(methylthio)-[1,1'-biphenyl]-4-carboxylic acid as a white solid (1.15 g, 4.71 mmol, 26% based on 4-boronobenzoic acid). 1H NMR (300 MHz, DMSO-d6) δ 2.53 (s, 3H, CH3), 7.38 (d, 3J = 9 Hz, 2H, ArH), 7.71 (d, 3J = 9 Hz, 2H, ArH), 7.71 (d, 3J = 9 Hz, 2H, ArH). This material was used without further

Synthesis, spectroscopic characterization and thermogravimetric analysis of two series of substituted (metallo)tetraphenylporphyrins

• Rasha K. Al-Shewiki,
• Carola Mende,
• Roy Buschbeck,
• Pablo F. Siles,
• Oliver G. Schmidt,
• Tobias Rüffer and
• Heinrich Lang

Beilstein J. Nanotechnol. 2017, 8, 1191–1204, doi:10.3762/bjnano.8.121

• mixtures (ratio 1:1, v/v) as eluent, showing that they were formed in high purity. Furthermore, 1H NMR studies allowed us to monitor the progress of the metalation reactions of 2 and 3, even for the paramagnetic metalloporphyrins 2b,d and 3b,d. For example, the complete metalations of the free-base

• porphyrins 2 and 3 are indicated by the disappearance of their N–H 1H NMR resonances. Electrospray ionization mass spectrometry High-resolution mass spectrometry (HRMS) studies enable one to verify the successful formation of 2/3 and of 2a–d/3a–d. The ESIMS measurements in positive-ionization mode were

• reference signal CDCl3: 1H NMR, δ = 7.26; and 13C{1H} NMR, δ = 77.16. FTIR spectra were recorded in the range of 400–4000 cm−1 with a Perkin-Elmer 1000 FTIR spectrometer as KBr pellets and in the range of 650–4000 cm−1 with a Thermo Scientific Smart iTR, Nicolet iS10. (The two absorptions at ca. 2360 cm−1