Encaging palladium(0) in layered double hydroxide: A sustainable catalyst for solvent-free and ligand-free Heck reaction in a ball mill

• Wei Shi,
• Jingbo Yu,
• Zhijiang Jiang,
• Qiaoling Shao and
• Weike Su

Beilstein J. Org. Chem. 2017, 13, 1661–1668, doi:10.3762/bjoc.13.160

• °, 33°, 38°, 60°, indexing to (003), (006), (009), (015), (110) reflections, which indicates the highly neat degree and well-crystallinity structure of LDH materials without phase impurities apparent. Moreover, the MgAl-LDHs presents an interlayer distance of 0.82 nm from the basal spacing of d003

Mechanochemical synthesis of graphene oxide-supported transition metal catalysts for the oxidation of isoeugenol to vanillin

• Ana Franco,
• Sudipta De,
• Alina M. Balu,
• Araceli Garcia and
• Rafael Luque

Beilstein J. Org. Chem. 2017, 13, 1439–1445, doi:10.3762/bjoc.13.141

• mesoporous nature of the RGO can be easily observed from SEM images (Figure 2a and b), whereas metal-supported RGO materials show a smooth surface with decreased crystallinity. TEM images of RGO materials with different thickness show a sheet like morphology with different transparencies (Figure 3). Dark

Glycoscience@Synchrotron: Synchrotron radiation applied to structural glycoscience

• Serge Pérez and
• Daniele de Sanctis

Beilstein J. Org. Chem. 2017, 13, 1145–1167, doi:10.3762/bjoc.13.114

Molecular-level architectural design using benzothiadiazole-based polymers for photovoltaic applications

• Vinila N. Viswanathan,
• Arun D. Rao,
• Upendra K. Pandey,
• Arul Varman Kesavan and
• Praveen C. Ramamurthy

Beilstein J. Org. Chem. 2017, 13, 863–873, doi:10.3762/bjoc.13.87

• dissociation will decrease, and hence, the overall device efficiency too. Moreover, for efficient OPV systems, a moderately high charge carrier mobility is required, which is attainable by increasing the crystallinity of polymers with firmly packed polymer chains. However, an increase in polymer crystallinity

• will simultaneously decrease their processability in solution. This will result in the reduced formation of the desired bicontinuous morphology with the acceptor [16]. Hence, when designing new molecules for OPV applications, a subtle balance between lowering the band gap, crystallinity, and solubility

Fluorescent carbon dots from mono- and polysaccharides: synthesis, properties and applications

• Stephen Hill and
• M. Carmen Galan

Beilstein J. Org. Chem. 2017, 13, 675–693, doi:10.3762/bjoc.13.67

• ). In the absence of KH2PO4, irregular black carbon aggregates were obtained. Raman and TEM analysis showed both types of FCDs had graphitic crystallinity. This example highlights that an inorganic-based dehydrating agent could be used instead of a traditional diamine SPA to induce CD dehydration and

• crystallinity with blue-green emission. Most reported CD syntheses, regardless of the type of starting material or synthetic method, tend to produce CDs with blue-green fluorescence emission. Jana et al. reported a carbohydrate-based preparation to access yellow and red emissive CDs, demonstrating that fine

• reaction without either strong heating, N-doping or surface passivation occurring. Also remarkably, the CDs produced by this method were found by HRTEM to have graphite crystallinity. This feature is interesting as, until now, it was thought that this type of crystallinity in a bottom-up constructed

Sulfamide chemistry applied to the functionalization of self-assembled monolayers on gold surfaces

• Loïc Pantaine,
• Vincent Humblot,
• Vincent Coeffard and
• Anne Vallée

Beilstein J. Org. Chem. 2017, 13, 648–658, doi:10.3762/bjoc.13.64

• substrates were annealed in a butane flame to ensure a good crystallinity of the topmost layers and rinsed in a bath of absolute ethanol during 15 min before adsorption. All SAM preparations hve been performed on cleaned gold samples checked by polarisation modulation reflection absorption infrared

Dynamics and interactions of ibuprofen in cyclodextrin nanosponges by solid-state NMR spectroscopy

• Monica Ferro,
• Franca Castiglione,
• Nadia Pastori,
• Carlo Punta,
• Lucio Melone,
• Walter Panzeri,
• Barbara Rossi,
• Francesco Trotta and
• Andrea Mele

Beilstein J. Org. Chem. 2017, 13, 182–194, doi:10.3762/bjoc.13.21

• the reflexes of IbuNa, shown in upper traces of the figure (Figure 10f). As a final remark, the PXRD patterns show that ibuprofen entrapped into the nanosponge network still retains crystallinity, thus confirming that the formation of the polymer-drug association is a mild process. Conclusion The

Extrusion – back to the future: Using an established technique to reform automated chemical synthesis

• Deborah E. Crawford

Beilstein J. Org. Chem. 2017, 13, 65–75, doi:10.3762/bjoc.13.9

• well as the reaction between triphenylphosphine and nickel thiocyanate, both in the presence of stoichiometric amounts of MeOH (Figure 6) [2]. High-quality products were obtained, as determined by 1H NMR spectroscopy, PXRD analysis (which gave sharp diffraction patterns, indicating high crystallinity

Supramolecular frameworks based on [60]fullerene hexakisadducts

• Andreas Kraft,
• Johannes Stangl,
• Ana-Maria Krause,
• Klaus Müller-Buschbaum and
• Florian Beuerle

Beilstein J. Org. Chem. 2017, 13, 1–9, doi:10.3762/bjoc.13.1

• stabilities and metal-free synthesis, but in most cases, have the disadvantages of poor crystallinity and limited processability or solution-phase characterization. In contrast, the formation of robust porous structures by means of supramolecular interactions between rigid organic molecules might be a

Effects of solvent additive on “s-shaped” curves in solution-processed small molecule solar cells

• John A. Love,
• Shu-Hua Chou,
• Ye Huang,
• Guilllermo C. Bazan and
• Thuc-Quyen Nguyen

Beilstein J. Org. Chem. 2016, 12, 2543–2555, doi:10.3762/bjoc.12.249

• kinetics of phase separation. In this class of small molecule systems, this is often attributed to asserting control over the crystallization and phase-separation processes within the blend; DIO helps induce crystallinity of the donor material [40][41][42][54][55][56]. Grazing incidence wide-angle X-ray

• stacking in P3HT (i.e., (100) planes). In the film cast with DIO, this peak is more prominent suggesting a greater degree of crystallinity. There is also a peak at 0.74 Å−1, which corresponds to the second order reflection. There is even a small peak at 1.11 Å−1, which likely corresponds to a third-order

• -on” orientation adopted by p-SIDT(FBTTh2)2 [40], demonstrating how sensitive molecular self-assembly can be to relatively small molecular design choices. However, consistent with previous reports of related molecules, DIO does seem to improve crystallinity. Atomic force microscopy (AFM) topography

Separation and identification of indene–C₇₀ bisadduct isomers

• Bolong Zhang,
• Jegadesan Subbiah,
• David J. Jones and
• Wallace W. H. Wong

Beilstein J. Org. Chem. 2016, 12, 903–911, doi:10.3762/bjoc.12.88

• the numerous possible isomers in IC70BA, our group took interest in examining the possibility of isolating single isomers from the mixture. It was anticipated that material containing a single isomer would have higher crystallinity compared to the mixture and this would have significant effects on

• was used with P3HT in solar cell devices that showed higher performance compared to devices containing the isomer mixture. Analysis of the materials and devices indicated that the single isomer had better charge transport properties probably as a result of higher crystallinity of the material. It is

• with apparent decrease in Jsc with increasing fraction purity and crystallinity. The crystallinity of a given fraction can be considered as dependent on the symmetry of the assigned isomer configuration. That is, the degree of symmetry varies in the order C1 < C2 < Cs, which resulted in the order of

Polydisperse methyl β-cyclodextrin–epichlorohydrin polymers: variable contact time ¹³C CP-MAS solid-state NMR characterization

• Isabelle Mallard,
• Davy Baudelet,
• Franca Castiglione,
• Monica Ferro,
• Walter Panzeri,
• Enzio Ragg and
• Andrea Mele

Beilstein J. Org. Chem. 2015, 11, 2785–2794, doi:10.3762/bjoc.11.299

• X-ray powder diffraction (XRPD) profiles of CRYSMEB and polymer D1. The upper trace clearly displays the typical halos of the amorphous material. This finding was indeed unexpected, as the starting material was supposed to show non-negligible crystallinity. Similar patterns are observed for D1, as

• occurred when the amount of the guest molecule toluene is varied. The line width of the spectral bands in the 13C CP-MAS NMR spectra can be qualitatively associated with the crystallinity of the samples: the more crystalline the sample is the sharper are the peaks. However, in the present case the XRPD

Physical properties and biological activities of hesperetin and naringenin in complex with methylated β-cyclodextrin

• Waratchada Sangpheak,
• Jintawee Kicuntod,
• Roswitha Schuster,
• Thanyada Rungrotmongkol,
• Peter Wolschann,
• Nawee Kungwan,
• Helmut Viernstein,
• Monika Mueller and
• Piamsook Pongsawasdi

Beilstein J. Org. Chem. 2015, 11, 2763–2773, doi:10.3762/bjoc.11.297

• , as well as a decrease in the crystallinity of guest molecules, brought about by complexation with CDs [53]. Cytokine levels in response to treatment with inclusion complexes of flavanones To investigate the anti-inflammatory effect of the inclusion complexes compared to free compounds, we used LPS

Synthesis of racemic and chiral BEDT-TTF derivatives possessing hydroxy groups and their achiral and chiral charge transfer complexes

• Sara J. Krivickas,
• Chiho Hashimoto,
• Junya Yoshida,
• Akira Ueda,
• Kazuyuki Takahashi,
• John D. Wallis and
• Hatsumi Mori

Beilstein J. Org. Chem. 2015, 11, 1561–1569, doi:10.3762/bjoc.11.172

• , anions, and included H2O solvent, which improve the crystallinity and facilitate the extraction of physical properties. Both salts are semiconductors with relatively low resistivities at room temperature and activation energies of 1.2 ohm cm with Ea = 86 meV for θ21-[(S,S)-2]3[(R,R)-2]3(ClO4)2 and 0.6

• ][17], ethylenedioxy [18], and pyrazino [19]), due to the difficulty of chiral-crystal growth. In order to improve the crystallinity, the inclusion of hydroxy groups in the BEDT-TTF molecule has been postulated to produce hydrogen bonding interactions between electron-donor molecules, electron-acceptor

• , presumably helping the crystallinity of the complex based upon chiral molecules. The crystal structure of the chiral salt α’-[(R, R)-2]2ClO4(H2O) is shown in Figure 3. The crystallographically independent molecules are two (R,R)-2 donors, one ClO4− anion, and one H2O molecule as an included solvent. There

Carboxylated dithiafulvenes and tetrathiafulvalene vinylogues: synthesis, electronic properties, and complexation with zinc ions

• Yunfei Wang and
• Yuming Zhao

Beilstein J. Org. Chem. 2015, 11, 957–965, doi:10.3762/bjoc.11.107

• Figure 4 confirm that coordinate polymer 8 possesses crystallinity in the solid state. Actually, the diffraction patterns were found to bear resemblance to those of zincite ZnO. Such crystalline features hence point to a possibility of the coordination polymer to take some kind of framework-like

• tuning the side groups of the TTFV ligand to produce Zn complexes with better crystallinity. Finally, the Zn-TTFV coordination polymer exhibited significant microporosity and surface area. Overall, our current studies have cast a light on the fundamental redox and solid-state properties of the class of

Chemoselective O-acylation of hydroxyamino acids and amino alcohols under acidic reaction conditions: History, scope and applications

• Tor E. Kristensen

Beilstein J. Org. Chem. 2015, 11, 446–468, doi:10.3762/bjoc.11.51

• acids can also impart a reduced tendency for crystallinity in the resulting amino acid derivatives, prohibiting, or at least, severely restricting the use of convenient recrystallization for purification on a multigram-scale. In the case of hydroxy-α-amino acids, any side-chain acylation will, often for

• , making the crystalline hydrochlorides unavailable from MeSO3H medium, thereby complicating the isolation and purification process due to the poor crystallinity of methanesulfonate salts, which in fact, quite frequently are ionic liquids. On the positive side, MeSO3H is biodegradable. In addition to the

Inclusion of trans-resveratrol in methylated cyclodextrins: synthesis and solid-state structures

• Lee Trollope,
• Dyanne L. Cruickshank,
• Terence Noonan,
• Susan A. Bourne,
• Milena Sorrenti,
• Laura Catenacci and
• Mino R. Caira

Beilstein J. Org. Chem. 2014, 10, 3136–3151, doi:10.3762/bjoc.10.331

• , prepared by either the suspension method or using microwave irradiation, yielded highly amorphous products, evident from their PXRD traces [9]; in this case, the absence of characteristic peaks for RSV and the reduction in the degree of crystallinity of the product were considered as indirect proof of

• phase (e.g., a hydrate of the guest compound) might be generated during attempted complexation. Loss of crystallinity of CD inclusion compounds also results when they dehydrate, rendering their PXRD traces less informative. There is, hitherto, a distinct lack of information on the structural nature of

Release of β-galactosidase from poloxamine/α-cyclodextrin hydrogels

• César A. Estévez,
• José Ramón Isasi,
• Eneko Larrañeta and
• Itziar Vélaz

Beilstein J. Org. Chem. 2014, 10, 3127–3135, doi:10.3762/bjoc.10.330

• causing increased contact with the medium. Thus, the lactase activity data in acidic media for the commercial tablets could not be collected. The type of drug, its polymorphism, crystallinity, particle size and other factors can influence the release kinetics. A water-soluble drug incorporated into a

Modification of physical properties of poly(L-lactic acid) by addition of methyl-β-cyclodextrin

• Toshiyuki Suzuki,
• Ayaka Ei,
• Yoshihisa Takada,
• Hiroki Uehara,
• Takeshi Yamanobe and
• Keiko Takahashi

Beilstein J. Org. Chem. 2014, 10, 2997–3006, doi:10.3762/bjoc.10.318

• plastics. In this study, the effect of methylcyclodextrin (MeCD) addition on the structure and physical properties, especially the drawing behavior, of PLLA was investigated. Through thermal analysis, it was found that MeCD addition lowers the crystallinity and enhances the mobility of PLLA. The sample

• melting point (Tm), and improvement in structural distribution with temperature. DSC-Raman measurements simultaneously supplied information about crystallinity and thermal properties. Thus, it was concluded that MeCD had high affinity for PLLA, and the addition of MeCD increased the amorphous component of

• PLLA and enhanced the drawability. Keywords: crystallinity; DSC; methyl-β-cyclodextrin; poly(L-lactic acid); Raman spectroscopy; Introduction Poly(L-lactic acid) (PLLA) has attracted attention because it is a biodegradable polymer derived from carbon-neutral resources. However, its melting point (Tm

Solution processable diketopyrrolopyrrole (DPP) cored small molecules with BODIPY end groups as novel donors for organic solar cells

• Diego Cortizo-Lacalle,
• Calvyn T. Howells,
• Upendra K. Pandey,
• Joseph Cameron,
• Neil J. Findlay,
• Anto Regis Inigo,
• Tell Tuttle,
• Peter J. Skabara and
• Ifor D. W. Samuel

Beilstein J. Org. Chem. 2014, 10, 2683–2695, doi:10.3762/bjoc.10.283

• over conjugated polymers, such as (i) synthetic reproducibility, (ii) higher structural versatility, (iii) ease of purification by recrystallisation and/or chromatography and therefore monodispersity, (iv) higher degrees of crystallinity and (vi) the possibility of vacuum deposition or solution

Scalable synthesis of 5,11-diethynylated indeno[1,2-b]fluorene-6,12-diones and exploration of their solid state packing

• Bradley D. Rose,
• Peter J. Santa Maria,
• Aaron G. Fix,
• Chris L. Vonnegut,
• Lev N. Zakharov,
• Sean R. Parkin and
• Michael M. Haley

Beilstein J. Org. Chem. 2014, 10, 2122–2130, doi:10.3762/bjoc.10.219

• silyl groups. The high crystallinity of the majority of the compounds examined permitted facile growth of large single crystals, of approximately several millimeters, from hexanes solution. Single crystals for 8g and 8j were grown from chlorobenzene due to the low solubility and crystallinity of these

Supercritical carbon dioxide: a solvent like no other

• Jocelyn Peach and
• Julian Eastoe

Beilstein J. Org. Chem. 2014, 10, 1878–1895, doi:10.3762/bjoc.10.196

• groups that have thermodynamically favourable interactions with CO2; (d) low crystallinity; this can be decreased by increased branching structures on side chains and finally (e) a low glass transition temperature (Tg) [92]. There are also several factors that have been identified as having a negative

One-pot stereoselective synthesis of α,β-differentiated diamino esters via the sequence of aminochlorination, aziridination and intermolecular S_N2 reaction

• Yiwen Xiong,
• Ping Qian,
• Chenhui Cao,
• Haibo Mei,
• Jianlin Han,
• Guigen Li and
• Yi Pan

Beilstein J. Org. Chem. 2014, 10, 1802–1807, doi:10.3762/bjoc.10.189

• of product 5o had a good crystallinity and were suitable for single crystal X-ray analysis (Figure 1). Crystallographic analysis has revealed that the anti-vicinal diamino ester was obtained. As a result, the stereochemistry of the other products was assigned (anti-isomer) based on the similarity of

The influence of intraannular templates on the liquid crystallinity of shape-persistent macrocycles

• Joscha Vollmeyer,
• Ute Baumeister and
• Sigurd Höger

Beilstein J. Org. Chem. 2014, 10, 910–920, doi:10.3762/bjoc.10.89

• crystallinity in 2. From the DSC and POM investigations in combination with the chemical structure of the compounds the following observations can be summarized: Although 1d has an empty lumen it has a similar melting point (62 °C) as 1a (63 °C), whose cavity crosses an alkyl bridge. Prolonging the intraannular

The difluoromethylene (CF₂) group in aliphatic chains: Synthesis and conformational preference of palmitic acids and nonadecane containing CF₂ groups

• Yi Wang,
• Ricardo Callejo,
• Alexandra M. Z. Slawin and
• David O’Hagan

Beilstein J. Org. Chem. 2014, 10, 18–25, doi:10.3762/bjoc.10.4

• significantly higher melting point and good crystallinity of 6c can be attributed to the relative orientation of the two CF2 groups. They are pointing perfectly anti-parallel to each other such that their dipoles cancel out in the extended anti-zig-zag chain conformation. We are currently exploring if this is a