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

• detector and in Bragg–Brentano geometry, using Cu Kα radiation (λ = 1.54060 Å) with a Ni filter. The data were collected in open air and with a quartz monocrystal zero background sample holder with 0.2 mm depth. Solid-state CP-MAS 13C NMR spectra were recorded on a Bruker Avance 600 spectrometer, operating

Inclusion complexes of 2-methoxyestradiol with dimethylated and permethylated β-cyclodextrins: models for cyclodextrin–steroid interaction

• Mino R. Caira,
• Susan A. Bourne,
• Halima Samsodien and
• Vincent J. Smith

Beilstein J. Org. Chem. 2015, 11, 2616–2630, doi:10.3762/bjoc.11.281

• (λmax = 198.5 nm) in methanol/water (1:1 v/v) solution. This instrument was also used for solubility and dissolution rate assays (details below). Single crystal X-ray diffraction analysis Intensity data were collected on a Nonius Kappa CCD diffractometer using graphite-monochromated Mo Kα-radiation (λ

Smart molecules for imaging, sensing and health (SMITH)

• Bradley D. Smith

Beilstein J. Org. Chem. 2015, 11, 2540–2548, doi:10.3762/bjoc.11.274

• course. (left) Association of ZnDPA probe with phosphatidylserine head group. (middle) False colored fluorescence image of a living rat bearing two tumors. There is increased accumulation of the cell death probe in the tumor that has been treated by focal beam radiation. (right) Fluorescence image of

Comparison of the catalytic activity for the Suzuki–Miyaura reaction of (η⁵-Cp)Pd(IPr)Cl with (η³-cinnamyl)Pd(IPr)(Cl) and (η³-1-t-Bu-indenyl)Pd(IPr)(Cl)

• Patrick R. Melvin,
• Nilay Hazari,
• Hannah M. C. Lant,
• Ian L. Peczak and
• Hemali P. Shah

Beilstein J. Org. Chem. 2015, 11, 2476–2486, doi:10.3762/bjoc.11.269

• crystallography X-ray diffraction experiments were carried out on a Rigaku MicroMax-007HF diffractometer coupled to a Saturn994+ CCD detector with Cu Kα radiation (λ = 1.54178 Å) at −180 °C. The crystals were mounted on MiTeGen polyimide loops with immersion oil. The data frames were processed using Rigaku

Self-assemblies of γ-CDs with pentablock copolymers PMA-PPO-PEO-PPO-PMA and endcapping via atom transfer radical polymerization of 2-methacryloyloxyethyl phosphorylcholine

• Jing Lin,
• Tao Kong,
• Lin Ye,
• Ai-ying Zhang and
• Zeng-guo Feng

Beilstein J. Org. Chem. 2015, 11, 2267–2277, doi:10.3762/bjoc.11.247

• adamantane standard. Wide angle X-ray diffraction (WXRD) patterns were recorded on a Shimadzu XD-D1 X-ray diffractometer with Ni-filtered Cu Kα (1.54 Å) radiation (20 kV, 40 mA). Powder samples were scanned from 2θ = 4.5–60° at a speed of 5°/min. FTIR spectra were measured using a Shimadzu IR Prestige-21

Ru complexes of Hoveyda–Grubbs type immobilized on lamellar zeolites: activity in olefin metathesis reactions

• Hynek Balcar,
• Naděžda Žilková,
• Martin Kubů,
• Michal Mazur,
• Zdeněk Bastl and
• Jiří Čejka

Beilstein J. Org. Chem. 2015, 11, 2087–2096, doi:10.3762/bjoc.11.225

• samples were degassed on a Micromeritics FlowPrep060 instrument under helium at 110 °C for 6 h. X-ray powder diffraction (XRD) data were obtained on a Bruker AXS D8 Advance diffractometer with a graphite monochromator and a Vantec-1 position sensitive detector using Cu Kα radiation (at 40 kV and 30 mA) in

• Bragg−Brentano geometry. The X-ray photoelectron spectra (XPS) of the samples were measured using a modified ESCA 3 MkII multitechnique spectrometer equipped with a hemispherical electron analyzer operated in a fixed transmission mode. Al Kα radiation (1486.6 eV) was used for electron excitation. The

Investigation of the role of stereoelectronic effects in the conformation of piperidones by NMR spectroscopy and X-ray diffraction

• Cesar Garcias-Morales,
• David Ortegón-Reyna and
• Armando Ariza-Castolo

Beilstein J. Org. Chem. 2015, 11, 1973–1984, doi:10.3762/bjoc.11.213

• on a glass fiber and collected on an Enraf-Nonius CAD-4 diffractometer, a Kappa CCD with an area detector using Mo Kα (λ = 0.71073 Å) radiation at 293 K. Intensity data were collected and processed using CAD4 EXPRESS Software. The structures were solved using WinGX [68] by direct methods with SHELXS

Hexacoordinate Ru-based olefin metathesis catalysts with pH-responsive N-heterocyclic carbene (NHC) and N-donor ligands for ROMP reactions in non-aqueous, aqueous and emulsion conditions

• Shawna L. Balof,
• K. Owen Nix,
• Matthew S. Olliff,
• Sarah E. Roessler,
• Arpita Saha,
• Kevin B. Müller,
• Ulrich Behrens,
• Edward J. Valente and
• Hans-Jörg Schanz

Beilstein J. Org. Chem. 2015, 11, 1960–1972, doi:10.3762/bjoc.11.212

• radiation and the charge-coupled area detector (CCD) detector on an Oxford Diffraction Systems Gemini S diffractometer. The solid contents of latexes were determined using a Mettler Toledo HR73 moisture meter. The droplet diameter was determined using an Autosizer IIC from Malvern Instruments. Materials and

• was truncated to isolate the sample, sealed with epoxy, and mounted on a pin; the pin was placed on a goniometer head. The crystallographic properties and data were collected using Mo Kα radiation and the charge-coupled area detector (CCD) detector on an Oxford Diffraction Systems Gemini S

• diffractometer at 300(1) K. A preliminary set of cell constants was calculated from reflections observed on three sets of 5 frames which were oriented approximately in mutually orthogonal directions of reciprocal space. Data collection was carried out using Mo Kα radiation (graphite monochromator) with 8 runs

Effective ascorbate-free and photolatent click reactions in water using a photoreducible copper(II)-ethylenediamine precatalyst

• Redouane Beniazza,
• Natalia Bayo,
• Florian Molton,
• Carole Duboc,
• Stéphane Massip,
• Nathan McClenaghan,
• Dominique Lastécouères and
• Jean-Marc Vincent

Beilstein J. Org. Chem. 2015, 11, 1950–1959, doi:10.3762/bjoc.11.211

• , has been synthesized and characterized by different techniques including single crystal X-ray diffraction. Highly efficient photoreduction was demonstrated when solutions of 1 in hydrogen atom donating solvents, such as THF or MeOH, were exposed to UVA radiation (350–400 nm) provided by a low pressure

Synthesis and structures of ruthenium–NHC complexes and their catalysis in hydrogen transfer reaction

• Chao Chen,
• Chunxin Lu,
• Qing Zheng,
• Shengliang Ni,
• Min Zhang and
• Wanzhi Chen

Beilstein J. Org. Chem. 2015, 11, 1786–1795, doi:10.3762/bjoc.11.194

• -crystal X-ray diffraction data were collected at 298(2) K on a Siemens Smart-CCD area-detector diffractometer with a MoKα radiation (λ = 0.71073 Å) by using a ω-2θ scan mode. Unit-cell dimensions were obtained with least-squares refinement. Data collection and reduction were performed using the Oxford

Fe(II)/Et₃N-Relay-catalyzed domino reaction of isoxazoles with imidazolium salts in the synthesis of methyl 4-imidazolylpyrrole-2-carboxylates, its ylide and betaine derivatives

• Ekaterina E. Galenko,
• Olesya A. Tomashenko,
• Alexander F. Khlebnikov,
• Mikhail S. Novikov and
• Taras L. Panikorovskii

Beilstein J. Org. Chem. 2015, 11, 1732–1740, doi:10.3762/bjoc.11.189

• performed on Agilent Technologies SuperNova diffractometer at 100 K using monochromated Cu Kα radiation. Thin-layer chromatography (TLC) was conducted on aluminium sheets with 0.2 mm silica gel (fluorescent indicator, Macherey-Nagel). The isoxazoles 7 [37][38] and imidazolium salts 9 [29] were synthesized

Preparative semiconductor photoredox catalysis: An emerging theme in organic synthesis

• David W. Manley and
• John C. Walton

Beilstein J. Org. Chem. 2015, 11, 1570–1582, doi:10.3762/bjoc.11.173

• photoredox catalysts (PRCs), have been exploited that enable visible and UVA radiation to be put to use without directly breaking chemical bonds. Typically, PRCs when photoexcited mediate electron transfer between suitable precursor substrates thus generating radical ions and thereby launching fresh

Deproto-metallation of N-arylated pyrroles and indoles using a mixed lithium–zinc base and regioselectivity-computed CH acidity relationship

• Mohamed Yacine Ameur Messaoud,
• Ghenia Bentabed-Ababsa,
• Madani Hedidi,
• Aïcha Derdour,
• Floris Chevallier,
• Yury S. Halauko,
• Oleg A. Ivashkevich,
• Vadim E. Matulis,
• Laurent Picot,
• Valérie Thiéry,
• Thierry Roisnel,
• Vincent Dorcet and
• Florence Mongin

Beilstein J. Org. Chem. 2015, 11, 1475–1485, doi:10.3762/bjoc.11.160

• were studied with graphite monochromatized MoKα radiation (λ = 0.71073 Å). X-ray diffraction data were collected at T = 150(2) K using an APEXII Bruker-AXS diffractometer. The structure was solved by direct methods using the SIR97 program [56], and then refined with full-matrix least-square methods

Tetrathiafulvalene-based azine ligands for anion and metal cation coordination

• Awatef Ayadi,
• Aziz El Alamy,
• Olivier Alévêque,
• Magali Allain,
• Nabil Zouari,
• Mohammed Bouachrine and
• Abdelkrim El-Ghayoury

Beilstein J. Org. Chem. 2015, 11, 1379–1391, doi:10.3762/bjoc.11.149

• (9:1, v/v). Melting points were measured with a Melting Point Apparatus SMP3. X-ray single-crystal diffraction data for complex 3 were collected at 180 K on an Agilent SuperNova diffractometer equipped with Atlas CCD detector and mirror monochromated micro-focus Cu Kα radiation (λ = 1.54184 Å). For

• ligand L1, crystal data were collected at 293 K on a Bruker KappaCCD diffractometer, equipped with a graphite monochromator utilizing MoKα radiation (λ = 0.71073Å). The two structures were solved by direct methods, expanded and refined on F2 by full matrix least-squares techniques using SHELX97 programs

Regioselective synthesis of chiral dimethyl-bis(ethylenedithio)tetrathiafulvalene sulfones

• Flavia Pop and
• Narcis Avarvari

Beilstein J. Org. Chem. 2015, 11, 1105–1111, doi:10.3762/bjoc.11.124

• performed on a Nonius Kappa CCD diffractometer, using graphite-monochromated Mo Kα radiation (λ = 0.71073 Å). The structures were solved (SHELXS-97) by direct methods and refined (SHELXL-97) by full-matrix least-square procedures on F2 [34]. The non-H atoms were refined with anisotropic displacement

Synthesis of photoresponsive cholesterol-based azobenzene organogels: dependence on different spacer lengths

• Yuchun Ren,
• Bin Wang and
• Xiuqing Zhang

Beilstein J. Org. Chem. 2015, 11, 1089–1095, doi:10.3762/bjoc.11.122

• described elsewhere [28]. General measurements NMR spectra were recorded with a Bruker-400 NMR spectrometer. Powder X-ray diffraction (XRD) measurements were carried out on a Rigaku D/max 2500PC (Japan)-type single-crystal diffractometer using Cu Kα radiation to determine the crystal structure. Infrared

Synthesis and characterization of the cyanobenzene-ethylenedithio-TTF donor

• Sandrina Oliveira,
• Dulce Belo,
• Isabel C. Santos,
• Sandra Rabaça and
• Manuel Almeida

Beilstein J. Org. Chem. 2015, 11, 951–956, doi:10.3762/bjoc.11.106

• mass spectrometer (ESI-QIT/MS). X-ray diffraction studies were performed with a Bruker APEX-II CCD detector diffractometer using graphite monochromated Mo Kα radiation (λ = 0.71073 Å), in the φ and ω scan modes. A semi empirical absorption correction was carried out using SADABS [24]. Data collection

Synthesis of tripodal catecholates and their immobilization on zinc oxide nanoparticles

• Franziska Klitsche,
• Julian Ramcke,
• Julia Migenda,
• Andreas Hensel,
• Tobias Vossmeyer,
• Horst Weller,
• Silvia Gross and
• Wolfgang Maison

Beilstein J. Org. Chem. 2015, 11, 678–686, doi:10.3762/bjoc.11.77

• XRD analysis, the functionalized particles were dispersed in MeOH, dropped on a standard crystal Si support. Then the solvent was evaporated. The samples were analyzed using a Philips X`Pert PRO MPD diffractometer (Cu Kα radiation, variable entrance slit, Bragg–Brentano geometry, secondary

Trifluoromethyl-substituted tetrathiafulvalenes

• Olivier Jeannin,
• Frédéric Barrière and
• Marc Fourmigué

Beilstein J. Org. Chem. 2015, 11, 647–658, doi:10.3762/bjoc.11.73

• radiation (λ = 0.71073 Å). Structures were solved by direct methods (SHELXS-97) and refined (SHELXL-97) [48] by full-matrix least-squares methods, as implemented in the WinGX software package [49]. Absorption corrections were applied. Hydrogen atoms were introduced at calculated positions (riding model

TTFs nonsymmetrically fused with alkylthiophenic moieties

• Rafaela A. L. Silva,
• Bruno J. C. Vieira,
• Marta M. Andrade,
• Isabel C. Santos,
• Sandra Rabaça,
• Dulce Belo and
• Manuel Almeida

Beilstein J. Org. Chem. 2015, 11, 628–637, doi:10.3762/bjoc.11.71

• electrolyte. Crystal structure determination X-ray diffraction studies were performed with a Bruker APEX-II CCD detector diffractometer using graphite-monochromated Mo Kα radiation (λ = 0.71073 Å), in the φ and ω scans mode. A semi empirical absorption correction was carried out using SADABS [25]. Data

Molecular cleft or tweezer compounds derived from trioxabicyclo[3.3.1]nonadiene diisocyanate and diacid dichloride

• Gert Kollenz,
• Ralf Smounig,
• Ferdinand Belaj,
• David Kvaskoff and
• Curt Wentrup

Beilstein J. Org. Chem. 2015, 11, 1–8, doi:10.3762/bjoc.11.1

• 925965 and 925966. X-ray diffraction data for 4 All the measurements were performed using graphite-monochromatized MoKα radiation at 100 K: C36H66N4O5, Mr 634.93, monoclinic, space group P21/c, a = 21.0815(7) Å, b = 20.1551(6) Å, c = 17.9547(6) Å, β = 92.203(2)°, V = 7623.3(4) Å3, Z = 8, dcalc = 1.106 g

• wR2 = 0.1708 (GOF = 1.015) were obtained. The largest peak in a difference Fourier map was 0.400 eÅ−3. X-ray diffraction data for 5 All the measurements were performed using graphite-monochromatized MoKα radiation at 100 K: C26H44N2O7, Mr 496.63, monoclinic, space group C2/c, a = 16.8698(6) Å, b

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

• co-crystallization from different solutions, by co-evaporation using a rotavapor, or by exposure to microwave radiation. Characterization of the products was achieved using DSC and simultaneous thermogravimetric analysis (TGA/DSC), with support from FTIR spectroscopy and PXRD, where necessary. An

• decomposition (curve not shown). It was ascertained that the kneading treatment (KN) and exposure to irradiation with microwave radiation (MW) had no significant effect on RSV. (Further experimental data on this aspect and all other methods employed in this study are provided in Supporting Information File 1

Recent advances in the electrochemical construction of heterocycles

• Robert Francke

Beilstein J. Org. Chem. 2014, 10, 2858–2873, doi:10.3762/bjoc.10.303

• byproduct, higher temperatures lead to preferential formation of the desired cyclization product. In the reported case, the use of ultrasonic radiation leads to significantly better results compared to conventional heating. These results suggest that the effect of ultrasound on the selectivity is

Preparation and evaluation of cyclodextrin polypseudorotaxane with PEGylated liposome as a sustained release drug carrier

• Kayoko Hayashida,
• Taishi Higashi,
• Daichi Kono,
• Keiichi Motoyama,
• Koki Wada and
• Hidetoshi Arima

Beilstein J. Org. Chem. 2014, 10, 2756–2764, doi:10.3762/bjoc.10.292

• diffractometer (Tokyo, Japan) with a Ni filtered Cu Kα radiation, a voltage of 40 kV, a current of 40 mA, a scanning speed of 5°/min, a time constant of 2 s, and a scan range of 2θ = 5–35°. Effects of CDs on the entrapment ratio of DOX into LP or PEG-LP DOX/PEG-LP was prepared with HSPC/cholesterol/PEG-DSPE (47

Aspergiloid I, an unprecedented spirolactone norditerpenoid from the plant-derived endophytic fungus Aspergillus sp. YXf3

• Zhi Kai Guo,
• Rong Wang,
• Wei Huang,
• Xiao Nian Li,
• Rong Jiang,
• Ren Xiang Tan and
• Hui Ming Ge

Beilstein J. Org. Chem. 2014, 10, 2677–2682, doi:10.3762/bjoc.10.282

• derived from Ginkgo biloba. Its structure was unambiguously established by analysis of HRMS–ESI and spectroscopic data, and the absolute configuration was determined by low-temperature (100 K) single crystal X-ray diffraction with Cu Kα radiation. This compound is structurally characterized by a new

• -temperature (100 K) single-crystal X-ray diffraction experiment, which is shown in Figure 3. As compound 1 has a relatively high percentage of oxygen, it shows enough anomalous dispersion of Cu Kα radiation and allows to determinate the absolute stereochemistry with the Hooft parameter 0.17(15) for 992

• solution of 2 mL methanol with two drops of distilled water. The single crystal X-ray diffraction data were collected at 100 K with Cu Kα radiation (λ = 1.54178 Å) on a Bruker APEX DUO CCD diffractometer, equipped with an Oxford Cryostream 700+ cooler. Structures were solved using the program SHELXS-97 [15