syn Skills Beyond School Synthesis Report By www.oecd.org Published On :: Thu, 13 Nov 2014 15:31:00 GMT Higher level vocational education and training (VET) programmes are facing rapid change and intensifying challenges. What type of training is needed to meet the needs of changing economies? How should the programmes be funded? How should they be linked to academic and university programmes? Full Article
syn TDPC Ministerial 2013 Synopsis By www.oecd.org Published On :: Mon, 14 Apr 2014 17:03:00 GMT The summary document of the TDPC Ministerial held in Marseille on 5-6 December 2013 is now availalble. Full Article
syn Syngenta CEO Erik Fyrwald By www.ft.com Published On :: Sun, 27 Aug 2017 18:06:08 GMT The Swiss agricultural chief is overseeing a merger with state-owned ChemChina Full Article
syn Rare inflammatory syndrome linked to Covid-19 kills 3 kids in New York, says governor Andrew Cuomo - Hindustan Times By news.google.com Published On :: Sun, 10 May 2020 01:54:40 GMT Rare inflammatory syndrome linked to Covid-19 kills 3 kids in New York, says governor Andrew Cuomo Hindustan TimesChildren infected with COVID-19 are developing new symptoms similar to Kawasaki disease WIONCOVID-19: Cases surpass 4 million worldwide, New York children die from related inflammation CGTNNew York looking further into emerging COVID-19 issue affecting children The Daily News Online'Every parent's nightmare': New York is investigating the death of a 5-year-old child from an illness linked t Business Insider IndiaView Full coverage on Google News Full Article
syn Three children in New York die from a rare inflammatory syndrome that may be linked to coronavirus By www.dailymail.co.uk Published On :: Sat, 09 May 2020 22:23:57 GMT Three children in New York have died and 73 more cases have been reported of a rare inflammatory syndrome exhibiting symptoms similar to Kawasaki disease or toxic shock-like syndrome. Full Article
syn The Reservation syndrome By indiatogether.org Published On :: Sun, 10 Jul 2011 00:00:00 +0000 There has been a needless focus on the Right to Education Act's provision of aspirational seats in private schools. Only a small fraction of public schools students can benefit from this, writes E S Ramamurthy. Full Article
syn What is syndicalism? By timesofindia.indiatimes.com Published On :: Sun, 31 Jul 2011 05:57:49 IST Syndicalism is a form of trade unionism and has its origins in France. It aims at the abolition of the capitalist owners and the appropriation - by the workers - of all the methods used in an industry, and the products resulting therefrom. Full Article
syn World Down Syndrome Day: ಮಗು ಡೌನ್ ಸಿಂಡ್ರೋಮ್ನಿಂದ ಹುಟ್ಟಲು ಕಾರಣವೇನು? By kannada.boldsky.com Published On :: Sat, 21 Mar 2020 15:37:43 +0530 ಮಗು ಡೌನ್ ಸಿಂಡ್ರೋಮ್ನಿಂದ(ವಿಶೇಷ ಚೇತನವಾಗಿ) ಹುಟ್ಟಲು ಕಾರಣವೇನೆಂದು ವೈದ್ಯರು ಹೇಳಿದರೂ ಹಾಗೇಕೆ ಹುಟ್ಟುತ್ತಾರೆ ಎಂಬುವುದು ಇನ್ನೂ ತಿಳಿದು ಬಂದಿಲ್ಲ. ಆದ್ದರಿಂದ ಮಗು ಡೌನ್ ಸಿಂಡ್ರೋಮ್ನಿಂದ ಹುಟ್ಟುವ ಸಾಧ್ಯತೆ ಇದೆಯೇ ಎಂದು ಹೇಳಲು ಸಾಧ್ಯವಾಗುವುದಿಲ್ಲ. ಡೌನ್ ಸಿಂಡ್ರೋಮ್ನಿಂದ ಮಕ್ಕಳು ಹುಟ್ಟುವ ಸಮಸ್ಯೆ ವಿಶ್ವದ ಎಲ್ಲಾ ಕಡೆ ಕಂಡು ಬರುತ್ತದೆ. ವಿಶ್ವದಲ್ಲಿ ಹುಟ್ಟುವ ಮಕ್ಕಳಲ್ಲಿ ಶ. 3ರಿಂದ Full Article
syn Synthetic bedding 'can cause asthma' By timesofindia.indiatimes.com Published On :: Tue, 11 Aug 2009 12:53:53 IST A new study has claimed synthetic bedding can aggravate asthma more than feather products as it contains high levels of fungal cells. Full Article
syn Rare syndrome tied to COVID-19 kills three children in New York, Cuomo says By feeds.reuters.com Published On :: Sun, 10 May 2020 11:08:30 +0530 Three children in New York have died from a rare inflammatory syndrome believed to be linked to the novel coronavirus, Governor Andrew Cuomo said on Saturday, a development that may augur a pandemic risk for the very young. Full Article health
syn Rare syndrome tied to COVID-19 kills three children in New York, Cuomo says By feeds.reuters.com Published On :: Sun, 10 May 2020 07:09:57 +0530 Three children in New York have died from a rare inflammatory syndrome believed to be linked to the novel coronavirus, Governor Andrew Cuomo said on Saturday, a development that may augur a pandemic risk for the very young. Full Article topNews
syn Rare syndrome tied to COVID-19 kills three children in New York, Cuomo says By feeds.reuters.com Published On :: Sun, 10 May 2020 07:09:57 +0530 Three children in New York have died from a rare inflammatory syndrome believed to be linked to the novel coronavirus, Governor Andrew Cuomo said on Saturday, a development that may augur a pandemic risk for the very young. Full Article topNews
syn Synopsis of the signal systems based upon the dot and dash and two-arm semaphore codes. By library.mit.edu Published On :: Sun, 30 Mar 2014 06:16:01 EDT Archives, Room Use Only - UG582.S4 S96 1914 Full Article
syn Asynchronous stack traces: why `await` beats `Promise#then()` By mathiasbynens.be Published On :: Mon, 02 Oct 2017 15:29:55 +0200 Compared to using promises directly, not only can async and await make code more readable for developers — they enable some interesting optimizations in JavaScript engines, too! This write-up is about one such optimization involving stack traces for asynchronous code. Full Article
syn Mixing and matching genes of marine and terrestrial origin in the biosynthesis of the mupirocin antibiotics By feeds.rsc.org Published On :: Chem. Sci., 2020, Advance ArticleDOI: 10.1039/C9SC06192D, Edge Article Open Access   This article is licensed under a Creative Commons Attribution 3.0 Unported Licence.Luoyi Wang, Zhongshu Song, Paul R. Race, James Spencer, Thomas J. Simpson, Matthew P. Crump, Christine L. WillisWhere the sea meets the land: the mupirocin biosynthetic gene cluster (BGC) from the terrestrial bacterium Pseudomonas fluorescens was repurposed via a plug-and-play approach with heterologous genes from the marine strain that produces thiomarinol.To cite this article before page numbers are assigned, use the DOI form of citation above.The content of this RSS Feed (c) The Royal Society of Chemistry Full Article
syn Fast identification of mineral inclusions in diamond at GSECARS using synchrotron X-ray microtomography, radiography and diffraction By scripts.iucr.org Published On :: 2019-07-19 Mineral inclusions in natural diamond are widely studied for the insight that they provide into the geochemistry and dynamics of the Earth's interior. A major challenge in achieving thorough yet high rates of analysis of mineral inclusions in diamond derives from the micrometre-scale of most inclusions, often requiring synchrotron radiation sources for diffraction. Centering microinclusions for diffraction with a highly focused synchrotron beam cannot be achieved optically because of the very high index of refraction of diamond. A fast, high-throughput method for identification of micromineral inclusions in diamond has been developed at the GeoSoilEnviro Center for Advanced Radiation Sources (GSECARS), Advanced Photon Source, Argonne National Laboratory, USA. Diamonds and their inclusions are imaged using synchrotron 3D computed X-ray microtomography on beamline 13-BM-D of GSECARS. The location of every inclusion is then pinpointed onto the coordinate system of the six-circle goniometer of the single-crystal diffractometer on beamline 13-BM-C. Because the bending magnet branch 13-BM is divided and delivered into 13-BM-C and 13-BM-D stations simultaneously, numerous diamonds can be examined during coordinated runs. The fast, high-throughput capability of the methodology is demonstrated by collecting 3D diffraction data on 53 diamond inclusions from Juína, Brazil, within a total of about 72 h of beam time. Full Article text
syn An enlightening procedure to explain the extreme power of synchrotron radiation By scripts.iucr.org Published On :: 2019-10-10 A simple approach exploits quantum properties to justify the dependence on γ4 of the total synchrotron emitted power. It also clarifies some apparent puzzles and brings to light the underlying, multiple relativistic phenomena. Full Article text
syn Coherence properties of the high-energy fourth-generation X-ray synchrotron sources By scripts.iucr.org Published On :: 2019-11-01 An analysis of the coherence properties of the fourth-generation high-energy storage rings with emittance values of 10 pm rad is performed. It is presently expected that a storage ring with these low emittance values will reach diffraction limit at hard X-rays. Simulations of coherence properties were performed with the XRT software and an analytical approach for different photon energies from 500 eV to 50 keV. It was demonstrated that a minimum photon emittance (diffraction limit) reached at such storage rings is λ/2π. Using mode decomposition it is shown that, for the parameters of the storage ring considered in this work, the diffraction limit will be reached for soft X-ray energies of 500 eV. About ten modes will contribute to the radiation field at 12 keV photon energy and even more modes give a contribution at higher photon energies. Energy spread effects of the electron beam in a low-emittance storage ring were analysed in detail. Simulations were performed at different relative energy spread values from zero to 2 × 10−3. A decrease of the degree of coherence with an increase of the relative energy spread value was observed. This analysis shows that, to reach the diffraction limit for high photon energies, electron beam emittance should go down to 1 pm rad and below. Full Article text
syn Methods for dynamic synchrotron X-ray respiratory imaging in live animals By scripts.iucr.org Published On :: 2020-01-01 Small-animal physiology studies are typically complicated, but the level of complexity is greatly increased when performing live-animal X-ray imaging studies at synchrotron and compact light sources. This group has extensive experience in these types of studies at the SPring-8 and Australian synchrotrons, as well as the Munich Compact Light Source. These experimental settings produce unique challenges. Experiments are always performed in an isolated radiation enclosure not specifically designed for live-animal imaging. This requires equipment adapted to physiological monitoring and test-substance delivery, as well as shuttering to reduce the radiation dose. Experiment designs must also take into account the fixed location, size and orientation of the X-ray beam. This article describes the techniques developed to overcome the challenges involved in respiratory X-ray imaging of live animals at synchrotrons, now enabling increasingly sophisticated imaging protocols. Full Article text
syn The HARE chip for efficient time-resolved serial synchrotron crystallography By scripts.iucr.org Published On :: 2020-02-27 Serial synchrotron crystallography (SSX) is an emerging technique for static and time-resolved protein structure determination. Using specifically patterned silicon chips for sample delivery, the `hit-and-return' (HARE) protocol allows for efficient time-resolved data collection. The specific pattern of the crystal wells in the HARE chip provides direct access to many discrete time points. HARE chips allow for optical excitation as well as on-chip mixing for reaction initiation, making a large number of protein systems amenable to time-resolved studies. Loading of protein microcrystals onto the HARE chip is streamlined by a novel vacuum loading platform that allows fine-tuning of suction strength while maintaining a humid environment to prevent crystal dehydration. To enable the widespread use of time-resolved serial synchrotron crystallography (TR-SSX), detailed technical descriptions of a set of accessories that facilitate TR-SSX workflows are provided. Full Article text
syn True and magnetic north to synch at Greenwich for first time in 360 years - New Atlas By newatlas.com Published On :: Tue, 03 Sep 2019 02:35:17 GMT True and magnetic north to synch at Greenwich for first time in 360 years New Atlas Full Article
syn Structure of the 4-hydroxy-tetrahydrodipicolinate synthase from the thermoacidophilic methanotroph Methylacidiphilum fumariolicum SolV and the phylogeny of the aminotransferase pathway By scripts.iucr.org Published On :: 2020-04-28 The enzyme 4-hydroxy-tetrahydrodipicolinate synthase (DapA) is involved in the production of lysine and precursor molecules for peptidoglycan synthesis. In a multistep reaction, DapA converts pyruvate and l-aspartate-4-semialdehyde to 4-hydroxy-2,3,4,5-tetrahydrodipicolinic acid. In many organisms, lysine binds allosterically to DapA, causing negative feedback, thus making the enzyme an important regulatory component of the pathway. Here, the 2.1 Å resolution crystal structure of DapA from the thermoacidophilic methanotroph Methylacidiphilum fumariolicum SolV is reported. The enzyme crystallized as a contaminant of a protein preparation from native biomass. Genome analysis reveals that M. fumariolicum SolV utilizes the recently discovered aminotransferase pathway for lysine biosynthesis. Phylogenetic analyses of the genes involved in this pathway shed new light on the distribution of this pathway across the three domains of life. Full Article text
syn The crystal structure of the heme d1 biosynthesis-associated small c-type cytochrome NirC reveals mixed oligomeric states in crystallo By journals.iucr.org Published On :: The crystal structure of the c-type cytochrome NirC from Pseudomonas aeruginosa has been determined and reveals the simultaneous presence of monomers and 3D domain-swapped dimers in the same asymmetric unit. Full Article text
syn Synthesis and crystal structure of [Cs([2.2.2]crypt)]2[Mo(CO)5] By scripts.iucr.org Published On :: 2019-09-12 Reduction of the heteroleptic metal carbonyl complex Mo(CO)3(η5-Cp)H with the metallic salt Cs5Bi4 in the presence of [2.2.2]crypt (= 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane) in liquid ammonia led to single crystals of bis[(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)caesium] pentacarbonylmolybdate, [Cs(C18H36N2O6)]2[Mo(CO)5] or [Cs([2.2.2]crypt)]2[Mo(CO)5]. The twofold negatively charged anionic complex corresponds to the 18 valence electron rule. It consists of an Mo atom coordinated by five carbonyl ligands in a shape intermediate between trigonal–bipyramidal and square-pyramidal. The Mo—C distances range from 1.961 (3) to 2.017 (3) Å, and the C≡O distances from 1.164 (3) to 1.180 (4) Å. Full Article text
syn Some chalcones derived from thiophene-3-carbaldehyde: synthesis and crystal structures By scripts.iucr.org Published On :: 2019-06-04 The synthesis, spectroscopic data and crystal and molecular structures of four 3-(3-phenylprop-1-ene-3-one-1-yl)thiophene derivatives, namely 1-(4-hydroxyphenyl)-3-(thiophen-3-yl)prop-1-en-3-one, C13H10O2S, (1), 1-(4-methoxyphenyl)-3-(thiophen-3-yl)prop-1-en-3-one, C14H12O2S, (2), 1-(4-ethoxyphenyl)-3-(thiophen-3-yl)prop-1-en-3-one, C15H14O2S, (3), and 1-(4-bromophenyl)-3-(thiophen-3-yl)prop-1-en-3-one, C13H9BrOS, (4), are described. The four chalcones have been synthesized by reaction of thiophene-3-carbaldehyde with an acetophenone derivative in an absolute ethanol solution containing potassium hydroxide, and differ in the substituent at the para position of the phenyl ring: –OH for 1, –OCH3 for 2, –OCH2CH3 for 3 and –Br for 4. The thiophene ring in 4 was found to be disordered over two orientations with occupancies 0.702 (4) and 0.298 (4). The configuration about the C=C bond is E. The thiophene and phenyl rings are inclined by 4.73 (12) for 1, 12.36 (11) for 2, 17.44 (11) for 3 and 46.1 (6) and 48.6 (6)° for 4, indicating that the –OH derivative is almost planar and the –Br derivative deviates the most from planarity. However, the substituent has no real influence on the bond distances in the α,β-unsaturated carbonyl moiety. The molecular packing of 1 features chain formation in the a-axis direction by O—H⋯O contacts. In the case of 2 and 3, the packing is characterized by dimer formation through C—H⋯O interactions. In addition, C—H⋯π(thiophene) interactions in 2 and C—H⋯S(thiophene) interactions in 3 contribute to the three-dimensional architecture. The presence of C—H⋯π(thiophene) contacts in the crystal of 4 results in chain formation in the c-axis direction. The Hirshfeld surface analysis shows that for all four derivatives, the highest contribution to surface contacts arises from contacts in which H atoms are involved. Full Article text
syn Synthesis, crystal structure and Hirshfeld surface analysis of 2-chloro-3-[(E)-(2-phenylhydrazinylidene)methyl]quinoline By scripts.iucr.org Published On :: 2019-06-07 A new quinoline-based hydrazone, C16H12ClN3, was synthesized by a condensation reaction of 2-chloro-3-formylquinoline with phenylhydrazine. The quinoline ring system is essentially planar (r.m.s. deviation = 0.012 Å), and forms a dihedral angle of 8.46 (10)° with the phenyl ring. The molecule adopts an E configuration with respect to the central C=N bond. In the crystal, molecules are linked by a C—H⋯π-phenyl interaction, forming zigzag chains propagating along the [10overline{3}] direction. The N—H hydrogen atom does not participate in hydrogen bonding but is directed towards the phenyl ring of an adjacent molecule, so linking the chains via weak N—H⋯π interactions to form of a three-dimensional structure. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions to the crystal packing are from H⋯H (35.5%), C⋯H/H⋯C (33.7%), Cl⋯H/H⋯Cl (12.3%), N⋯H/H⋯N (9.5%) contacts. Full Article text
syn Crystal structure of 3,14-diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.07,12]docosane dinitrate dihydrate from synchrotron X-ray data By scripts.iucr.org Published On :: 2019-05-31 The crystal structure of title salt, C22H46N42+·2NO3−·2H2O, has been determined using synchrotron radiation at 220 K. The structure determination reveals that protonation has occurred at diagonally opposite amine N atoms. The asymmetric unit contains half a centrosymmetric dication, one nitrate anion and one water molecule. The molecular dication, C22H46N42+, together with the nitrate anion and hydrate water molecule are involved in an extensive range of hydrogen bonds. The molecule is stabilized, as is the conformation of the dication, by forming intermolecular N—H⋯O, O—H⋯O, together with intramolecular N—H⋯N hydrogen bonds. Full Article text
syn Crystal structure, synthesis and thermal properties of tetrakis(4-benzoylpyridine-κN)bis(isothiocyanato-κN)iron(II) By scripts.iucr.org Published On :: 2019-05-31 The asymmetric unit of the title compound, [Fe(NCS)2(C12H9NO)4], consists of an FeII ion that is located on a centre of inversion, as well as two 4-benzoylpyridine ligands and one thiocyanate anion in general positions. The FeII ions are coordinated by two N-terminal-bonded thiocyanate anions and four 4-benzoylpyridine ligands into discrete complexes with a slightly distorted octahedral geometry. These complexes are further linked by weak C—H⋯O hydrogen bonds into chains running along the c-axis direction. Upon heating, this complex loses half of the 4-benzoylpyridine ligands and transforms into a compound with the composition Fe(NCS)2(4-benzoylpyridine)2, that might be isotypic to the corresponding MnII compound and for which the structure is unknown. Full Article text
syn Synthesis, characterization, and crystal structure of aquabis(4,4'-dimethoxy-2,2'-bipyridine)[μ-(2R,3R)-tartrato(4−)]dicopper(II) octahydrate By scripts.iucr.org Published On :: 2019-06-11 Typical electroless copper baths (ECBs), which are used to chemically deposit copper on printed circuit boards, consist of an aqueous alkali hydroxide solution, a copper(II) salt, formaldehyde as reducing agent, an l-(+)-tartrate as complexing agent, and a 2,2'-bipyridine derivative as stabilizer. Actual speciation and reactivity are, however, largely unknown. Herein, we report on the synthesis and crystal structure of aqua-1κO-bis(4,4'-dimethoxy-2,2'-bipyridine)-1κ2N,N';2κ2N,N'-[μ-(2R,3R)-2,3-dioxidosuccinato-1κ2O1,O2:2κ2O3,O4]dicopper(II) octahydrate, [Cu2(C12H12N2O2)2(C4H2O6)(H2O)]·8H2O, from an ECB mock-up. The title compound crystallizes in the Sohncke group P21 with one chiral dinuclear complex and eight molecules of hydrate water in the asymmetric unit. The expected retention of the tartrato ligand's absolute configuration was confirmed via determination of the absolute structure. The complex molecules exhibit an ansa-like structure with two planar, nearly parallel bipyridine ligands, each bound to a copper atom that is connected to the other by a bridging tartrato `handle'. The complex and water molecules give rise to a layered supramolecular structure dominated by alternating π stacks and hydrogen bonds. The understanding of structures ex situ is a first step on the way to prolonged stability and improved coating behavior of ECBs. Full Article text
syn Synthesis and crystal structure of calcium hydrogen phosphite, CaHPO3 By scripts.iucr.org Published On :: 2019-06-14 The hydrothermal synthesis and crystal structure of the simple inorganic compound CaHPO3, which crystallizes in the chiral space group P43212, are reported. The structure is built up from distorted CaO7 capped trigonal prisms and HPO3 pseudo pyramids, which share corners and edges to generate a three-dimensional network. Full Article text
syn Syntheses, crystal structures, and comparisons of rare-earth oxyapatites Ca2RE8(SiO4)6O2 (RE = La, Nd, Sm, Eu, or Yb) and NaLa9(SiO4)6O2 By scripts.iucr.org Published On :: 2019-06-21 Six different rare-earth oxyapatites, including Ca2RE8(SiO4)6O2 (RE = La, Nd, Sm, Eu, or Yb) and NaLa9(SiO4)6O2, were synthesized using solution-based processes followed by cold pressing and sintering. The crystal structures of the synthesized oxyapatites were determined from powder X-ray diffraction (P-XRD) and their chemistries verified with electron probe microanalysis (EPMA). All the oxyapatites were isostructural within the hexagonal space group P63/m and showed similar unit-cell parameters. The isolated [SiO4]4− tetrahedra in each crystal are linked by the cations at the 4f and 6h sites occupied by RE3+ and Ca2+ in Ca2RE8(SiO4)6O2 or La3+ and Na+ in NaLa9(SiO4)6O2. The lattice parameters, cell volumes, and densities of the synthesized oxyapatites fit well to the trendlines calculated from literature values. Full Article text
syn Synthesis, detailed geometric analysis and bond-valence method evaluation of the strength of π-arene bonding of two isotypic cationic prehnitene tin(II) complexes: [{1,2,3,4-(CH3)4C6H2}2Sn2Cl2][MCl4]2 (M = Al and Ga) By scripts.iucr.org Published On :: 2019-06-25 From solutions of prehnitene and the ternary halides (SnCl)[MCl4] (M = Al, Ga) in chlorobenzene, the new cationic SnII–π-arene complexes catena-poly[[chloridoaluminate(III)]-tri-μ-chlorido-4':1κ2Cl,1:2κ4Cl-[(η6-1,2,3,4-tetramethylbenzene)tin(II)]-di-μ-chlorido-2:3κ4Cl-[(η6-1,2,3,4-tetramethylbenzene)tin(II)]-di-μ-chlorido-3:4κ4Cl-[chloridoaluminate(III)]-μ-chlorido-4:1'κ2Cl], [Al2Sn2Cl10(C10H14)2]n, (1) and catena-poly[[chloridogallate(III)]-tri-μ-chlorido-4':1κ2Cl,1:2κ4Cl-[(η6-1,2,3,4-tetramethylbenzene)tin(II)]-di-μ-chlorido-2:3κ4Cl-[(η6-1,2,3,4-tetramethylbenzene)tin(II)]-di-μ-chlorido-3:4κ4Cl-[chloridogallate(III)]-μ-chlorido-4:1'κ2Cl], [Ga2Sn2Cl10(C10H14)2]n, (2), were isolated. In these first main-group metal–prehnitene complexes, the distorted η6 arene π-bonding to the tin atoms of the Sn2Cl22+ moieties in the centre of [{1,2,3,4-(CH3)4C6H2}2Sn2Cl2][MCl4]2 repeating units (site symmetry overline{1}) is characterized by: (i) a significant ring slippage of ca 0.4 Å indicated by the dispersion of Sn—C distances [1: 2.881 (2)–3.216 (2) Å; 2: 2.891 (3)–3.214 (3) Å]; (ii) the non-methyl-substituted arene C atoms positioned closest to the SnII central atom; (iii) a pronounced tilt of the plane of the arene ligand against the plane of the central (Sn2Cl2)2+ four-membered ring species [1: 15.59 (11)°, 2: 15.69 (9)°]; (iv) metal–arene bonding of medium strength as illustrated by application of the bond-valence method in an indirect manner, defining the π-arene bonding interaction of the SnII central atoms as s(SnII—arene) = 2 − Σs(SnII—Cl), that gives s(SnII—arene) = 0.37 and 0.38 valence units for the aluminate and the gallate, respectively, indicating that comparatively strong main-group metal–arene bonding is present and in line with the expectation that [AlCl4]− is the slightly weaker coordinating anion as compared to [GaCl4]−. Full Article text
syn Synthesis and crystal structure of a new hybrid organic–inorganic material containing neutral molecules, cations and heptamolybdate anions By scripts.iucr.org Published On :: 2019-06-21 The title compound, hexakis(2-methyl-1H-imidazol-3-ium) heptamolybdate 2-methyl-1H-imidazole disolvate dihydrate, (C4H7N2)6[Mo7O24]·2C4H6N2·2H2O, was prepared from 2-methylimidazole and ammonium heptamolybdate tetrahydrate in acid solution. The [Mo7O24]6− heptamolybdate cluster anion is accompanied by six protonated (C4H7N2)+ 2-methylimidazolium cations, two neutral C4H6N2 2-methylimidazole molecules and two water molecules of crystallization. The cluster consists of seven distorted MoO6 octahedra sharing edges or vertices. In the crystal, the components are linked by N—H⋯N, N—H⋯O, O—H⋯O, N—H⋯(O,O) and O—H⋯(O,O) hydrogen bonds, generating a three-dimensional network. Weak C—H⋯O interactions consolidate the packing. Full Article text
syn Syntheses, crystal structures and Hirshfeld surface analyses of (3aR,4S,7R,7aS)-2-(perfluoropyridin-4-yl)-3a,4,7,7a-tetrahydro-4,7-methanoisoindole-1,3-dione and (3aR,4S,7R,7aS)-2-[(perfluoropyridin-4-yl)oxy]-3a,4,7,7a- By scripts.iucr.org Published On :: 2019-07-12 The syntheses and crystal structures of the title compounds, C14H8F4N2O2 and C14H8F4N2O3, are reported. In each crystal, the packing is driven by C—H⋯F intertactions, along with a variety of C—H⋯O, C—O⋯π, and C—F⋯π contacts. Hirshfeld surface analysis was conducted to aid in the visualization of these various influences on the packing: they showed that the largest contributions to the surface contacts arise from H⋯F/F⋯H interactions, followed by H⋯H and O⋯H/H⋯O. Full Article text
syn (3,5-Dimethyladamantan-1-yl)ammonium methanesulfonate (memantinium mesylate): synthesis, structure and solid-state properties By scripts.iucr.org Published On :: 2019-07-26 The asymmetric unit of the title compound, C12H22N+·CH3O3S−, consists of three (3,5-dimethyladamantan-1-yl)ammonium cations, C12H22N+, and three methanesulfonate anions, CH3O3S−. In the crystal, the cations and anions associate via N—H⋯O hydrogen bonds into layers, parallel to the (001) plane, which include large supramolecular hydrogen-bonded rings. Full Article text
syn Syntheses and crystal structures of a new family of hybrid perovskites: C5H14N2·ABr3·0.5H2O (A = K, Rb, Cs) By scripts.iucr.org Published On :: 2019-07-26 The syntheses and crystal structures of three hybrid perovskites, viz. poly[1-methylpiperizine-1,4-diium [tri-μ-bromido-potassium] hemihydrate], {(C5H14N2)[KBr3]·0.5H2O}n, (I), poly[1-methylpiperizine-1,4-diium [tri-μ-bromido-rubidium] hemihydrate], {(C5H14N2)[RbBr3]·0.5H2O}n, (II), and poly[1-methylpiperizine-1,4-diium [tri-μ-bromido-caesium] hemihydrate], {(C5H14N2)[CsBr3]·0.5H2O}n, (III), are described. These isostructural (space group Amm2) phases contain a three-dimensional, corner-sharing network of distorted ABr6 octahedra (A = K, Rb, Cs) with the same topology as the classical perovskite structure. The doubly protonated C5H14N22+ cations occupy interstices bounded by eight octahedra and the water molecules lie in square sites bounded by four octahedra. N—H⋯Br, N—H⋯(Br,Br), N—H⋯O and O—H⋯Br hydrogen bonds consolidate the structures. Full Article text
syn Syntheses and structures of piperazin-1-ium ABr2 (A = Cs or Rb): hybrid solids containing `curtain wall' layers of face- and edge-sharing ABr6 trigonal prisms By scripts.iucr.org Published On :: 2019-07-26 The isostructural title compounds, poly[piperazin-1-ium [di-μ-bromido-caesium]], {(C4H11N2)[CsBr2]}n, and poly[piperazin-1-ium [di-μ-bromido-rubidium]], {(C4H11N2)[RbBr2]}n, contain singly-protonated piperazin-1-ium cations and unusual ABr6 (A = Cs or Rb) trigonal prisms. The prisms are linked into a distinctive `curtain wall' arrangement propagating in the (010) plane by face and edge sharing. In each case, a network of N—H⋯N, N—H⋯Br and N—H⋯(Br,Br) hydrogen bonds consolidates the structure. Full Article text
syn Synthesis and structure of 2,4,6-tricyclobutyl-1,3,5-trioxane By scripts.iucr.org Published On :: 2019-10-03 The synthesis and structure of 2,4,6,-tricyclobutyl-1,3,5-trioxane, C15H24O3 1, is described. It was formed in 39% yield during the work-up of the Swern oxidation of cyclobutylmethanol and may serve as a stable precursor of the cyclobutane carbaldehyde. The molecule of 1 occupies a special position (3.m) located at the center of its 1,3,5-trioxane ring. The latter is in a chair conformation, with the symmetry-independent O and C atoms deviating by 0.651 (4) Å from the least-squares plane of the other atoms of the trioxane ring. All three cyclobutane substituents, which have a butterfly conformation with an angle between the two planes of 25.7 (3)°, are in the cis conformation relative to the 1,3,5-trioxane ring. Intermolecular C—H⋯O interactions between the 1,3,5-trioxane rings consolidate the crystal structure, forming stacks along the c-axis direction. The crystal studied was refined a as a racemic twin. Full Article text
syn Synthesis and structure of push–pull merocyanines based on barbituric and thiobarbituric acid By scripts.iucr.org Published On :: 2019-08-16 Two compounds, 1,3-diethyl-5-{(2E,4E)-6-[(E)-1,3,3-trimethylindolin-2-ylidene]hexa-2,4-dien-1-ylidene}pyrimidine-2,4,6(1H,3H,5H)-trione or TMI, C25H29N3O3, and 1,3-diethyl-2-sulfanylidene-5-[2-(1,3,3-trimethylindolin-2-ylidene)ethylidene]dihydropyrimidine-4,6(1H,5H)-dione or DTB, C21H25N3O2S, have been crystallized and studied. These compounds contain the same indole derivative donor group and differ in their acceptor groups (in TMI it contains oxygen in the para position, and in DTB sulfur) and the length of the π-bridge. In both materials, molecules are packed in a herringbone manner with differences in the twist and fold angles. In both structures, the molecules are connected by weak C—H⋯O and/or C—H⋯S bonds. Full Article text
syn Synthesis and crystal structure of 1,3-bis(4-hydroxyphenyl)-1H-imidazol-3-ium chloride By scripts.iucr.org Published On :: 2019-08-16 Imidazolium salts are common building blocks for functional materials and in the synthesis of N-heterocyclic carbene (NHC) as σ-donor ligands for stable metal complexes. The title salt, 1,3-bis(4-hydroxyphenyl)-1H-imidazol-3-ium chloride (IOH·Cl), C15H13N2O2+·Cl−, is a new imidazolium salt with a hydroxy functionality. The synthesis of IOH·Cl was achieved in high yield via a two-step procedure involving a diazabutadiene precursor followed by ring closure using trimethylchlorosilane and paraformaldehyde. The structure of IOH·Cl consists of a central planar imidazolium ring (r.m.s. deviation = 0.0015 Å), with out-of-plane phenolic side arms. The dihedral angles between the 4-hydroxyphenyl substituents and the imidazole ring are 55.27 (7) and 48.85 (11)°. In the crystal, O—H⋯Cl hydrogen bonds connect the distal hydroxy groups and Cl− anions in adjacent asymmetric units, one related by inversion (−x + 1, −y + 1, −z + 1) and one by the n-glide (x − {1over 2}, −y + {1over 2}, z − {1over 2}), with donor–acceptor distances of 2.977 (2) and 3.0130 (18) Å, respectively. The phenolic rings are each π–π stacked with their respective inversion-related [(−x + 1, −y + 1, −z + 1) and (−x, −y + 1, −z + 1)] counterparts, with interplanar distances of 3.560 (3) and 3.778 (3) Å. The only other noteworthy intermolecular interaction is an O⋯O (not hydrogen bonded) close contact of 2.999 (3) Å between crystallographically different hydroxy O atoms on translationally adjacent molecules (x + 1, y, x + 1). Full Article text
syn Syntheses and crystal structures of 2-methyl-1,1,2,3,3-pentaphenyl-2-silapropane and 2-methyl-1,1,3,3-tetraphenyl-2-silapropan-2-ol By scripts.iucr.org Published On :: 2019-08-23 The sterically hindered silicon compound 2-methyl-1,1,2,3,3-pentaphenyl-2-silapropane, C33H30Si (I), was prepared via the reaction of two equivalents of diphenylmethyllithium (benzhydryllithium) and dichloromethylphenylsilane. This bisbenzhydryl-substituted silicon compound was then reacted with trifluoromethanesulfonic acid, followed by hydrolysis with water to give the silanol 2-methyl-1,1,3,3-tetraphenyl-2-silapropan-2-ol, C27H26OSi (II). Key geometric features for I are the Si—C bond lengths that range from 1.867 (2) to 1.914 (2) Å and a τ4 descriptor for fourfold coordination around the Si atom of 0.97 (indicating a nearly perfect tetrahedron). Key geometric features for compound II include Si—C bond lengths that range from 1.835 (4) to 1.905 (3) Å, a Si—O bond length of 1.665 (3) Å, and a τ4 descriptor for fourfold coordination around the Si atom of 0.96. In compound II, there is an intramolecular C—H⋯O hydrogen bond present. In the crystal of I, molecules are linked by two pairs of C—H⋯π interactions, forming dimers that are linked into ribbons propagating along the b-axis direction. In the crystal of II, molecules are linked by C—H⋯π and O—H⋯π interactions that result in the formation of ribbons that run along the a-axis direction. Full Article text
syn Crystal structure and Hirshfeld surface analysis of lapachol acetate 80 years after its first synthesis By scripts.iucr.org Published On :: 2019-08-19 Lapachol acetate [systematic name: 3-(3-methylbut-2-enyl)-1,4-dioxonaphthalen-2-yl acetate], C17H16O4, was prepared using a modified high-yield procedure and its crystal structure is reported for the first time 80 years after its first synthesis. The full spectroscopic characterization of the molecule is reported. The molecular conformation shows little difference with other lapachol derivatives and lapachol itself. The packing is directed by intermolecular π–π and C—H⋯O interactions, as described by Hirshfeld surface analysis. The former interactions make the largest contributions to the total packing energy in a ratio of 2:1 with respect to the latter. Full Article text
syn Synthesis, characterization, crystal structure and supramolecularity of ethyl (E)-2-cyano-3-(3-methylthiophen-2-yl)acrylate and a new polymorph of ethyl (E)-2-cyano-3-(thiophen-2-yl)acrylate By scripts.iucr.org Published On :: 2019-08-23 The synthesis, crystal structure and structural motif of two thiophene-based cyanoacrylate derivatives, namely, ethyl (E)-2-cyano-3-(3-methylthiophen-2-yl)acrylate (1), C11H11NO2S, and ethyl (E)-2-cyano-3-(thiophen-2-yl)acrylate (2), C10H9NO2S, are reported. Derivative 1 crystallized with two independent molecules in the asymmetric unit, and derivative 2 represents a new monoclinic (C2/m) polymorph. The molecular conformations of 1 and the two polymorphs of 2 are very similar, as all non-H atoms are planar except for the methyl of the ethyl groups. The intermolecular interactions and crystal packing of 1 and 2 are described and compared with that of the reported monoclinic (C2/m) polymorph of derivative 2 [Castro Agudelo et al. (2017). Acta Cryst. E73, 1287–1289]. Full Article text
syn Synthesis and crystal structure of tert-butyl 1-(2-iodobenzoyl)cyclopent-3-ene-1-carboxylate By scripts.iucr.org Published On :: 2019-08-30 1-(2-Iodobenzoyl)-cyclopent-3-ene-1-carboxylates are novel substrates to construct bicyclo[3.2.1]octanes with antibacterial and antithrombotic activities. In this context, tert-butyl 1-(2-iodobenzoyl)-cyclopent-3-ene-1-carboxylate, C17H19IO3, was synthesized and structurally characterized. The 2-iodobenzoyl group is attached to the tertiary C atom of the cyclopent-3-ene ring. The dihedral angle between the benzene ring and the mean plane of the envelope-type cyclopent-3-ene ring is 26.0 (3)°. In the crystal, pairs of C-H⋯O hydrogen bonds link the molecules to form inversion dimers. Full Article text
syn The synthesis and crystal structure of bis[3,3-diethyl-1-(phenylimino-κN)thiourea-κS]silver hexafluoridophosphate By scripts.iucr.org Published On :: 2019-08-30 The structure of the title complex, [Ag(C11H15N3S)2]PF6, has monoclinic (P21/c) symmetry, and the silver atom has a distorted square-planar geometry. The coordination complex crystallized from mixing silver hexafluoridophosphate with a concentrated tetrahydrofuran solution of N,N-diethylphenylazothioformamide [ATF; systematic name: 3,3-diethyl-1-(phenylimino)thiourea] under ambient conditions. The resultant coordination complex exhibits a 2:1 ligand-to-metal ratio, with the silver(I) atom having a fourfold AgN2S2 coordination sphere, with a single PF6 counter-ion. In the crystal, however, one sulfur atom from an ATF ligand of a neighboring complex coordinates to the silver atom, with a bond distance of 2.9884 (14) Å. This creates a polymeric zigzag chain propagating along the c-axis direction. The chains are linked by C—H⋯F hydrogen bonds, forming slabs parallel to the ac plane. Full Article text
syn Synthesis and redetermination of the crystal structure of salicylaldehyde N(4)-morpholinothiosemicarbazone By scripts.iucr.org Published On :: 2019-08-30 The structure of the title compound (systematic name: N-{[(2-hydroxyphenyl)methylidene]amino}morpholine-4-carbothioamide), C12H15N3O2S, was previously determined (Koo et al., 1977) using multiple-film equi-inclination Weissenberg data, but has been redetermined with higher precision to explore its conformation and the hydrogen-bonding patterns and supramolecular interactions. The molecular structure shows intramolecular O—H⋯N and C—H⋯S interactions. The configuration of the C=N bond is E. The molecule is slightly twisted about the central N—N bond. The best planes through the phenyl ring and the morpholino ring make an angle of 43.44 (17)°. In the crystal, the molecules are connected into chains by N—H⋯O and C—H⋯O hydrogen bonds, which combine to generate sheets lying parallel to (002). The most prominent contribution to the surface contacts are H⋯H contacts (51.6%), as concluded from a Hirshfeld surface analysis. Full Article text
syn Crystal structures, syntheses, and spectroscopic and electrochemical measurements of two push–pull chromophores: 2-[4-(dimethylamino)benzylidene]-1H-indene-1,3(2H)-dione and (E)-2-{3-[4-(dimethylamino)phenyl By scripts.iucr.org Published On :: 2019-10-03 The title pull–push chromophores, 2-[4-(dimethylamino)benzylidene]-1H-indene-1,3(2H)-dione, C18H15NO2 (ID[1]) and (E)-2-{3-[4-(dimethylamino)phenyl]allylidene}-1H-indene-1,3(2H)-dione, C20H17NO2 (ID[2]), have donor–π-bridge–acceptor structures. The molecule with the short π-bridge, ID[1], is almost planar while for the molecule with a longer bridge, ID[2], is less planar. The benzene ring is inclined to the mean plane of the 2,3-dihydro-1H-indene unit by 3.19 (4)° in ID[1] and 13.06 (8)° in ID[2]. The structures of three polymorphs of compound ID[1] have been reported: the α-polymorph [space group P21/c; Magomedova & Zvonkova (1978). Kristallografiya, 23, 281–288], the β-polymorph [space group P21/c; Magomedova & Zvonkova (1980). Kristallografiya, 25 1183–1187] and the γ-polymorph [space group Pna21; Magomedova, Neigauz, Zvonkova & Novakovskaya (1980). Kristallografiya, 25, 400–402]. The molecular packing in ID[1] studied here is centrosymmetric (space group P21/c) and corresponds to the β-polymorph structure. The molecular packing in ID[2] is non-centrosymmetric (space group P21), which suggests potential NLO properties for this crystalline material. In both compounds, there is short intramolecular C—H⋯O contact present, enclosing an S(7) ring motif. In the crystal of ID[1], molecules are linked by C—H⋯O hydrogen bonds and C—H⋯π interactions, forming layers parallel to the bc plane. In the crystal of ID[2], molecules are liked by C—H⋯O hydrogen bonds to form 21 helices propagating along the b-axis direction. The molecules in the helix are linked by offset π–π interactions with, for example, a centroid–centroid distance of 3.9664 (13) Å (= b axis) separating the indene rings, and an offset of 1.869 Å. Spectroscopic and electrochemical measurements show the ability of these compounds to easily transfer electrons through the π-conjugated chain. Full Article text
syn Synthesis, crystal structure and Hirshfeld surface analysis of 4-[3-(4-hydroxyphenyl)-4,5-dihydro-1H-pyrazol-5-yl]-2-methoxyphenol monohydrate By scripts.iucr.org Published On :: 2019-10-03 In the title pyrazoline derivative, C16H16N2O3·H2O, the pyrazoline ring has an envelope conformation with the substituted sp2 C atom on the flap. The pyrazoline ring makes angles of 86.73 (12) and 13.44 (12)° with the trisubstituted and disubstituted benzene rings, respectively. In the crystal structure, the molecules are connected into chains running in the b-axis direction by O—H⋯N hydrogen bonding. Parallel chains interact through N—H⋯O hydrogen bonds and π–π stacking of the trisubstituted phenyl rings. The major contribution to the surface contacts are H⋯H contacts (44.3%) as concluded from a Hirshfeld surface analysis. Full Article text
syn High-pressure synthesis and crystal structure of SrGa4As4 By scripts.iucr.org Published On :: 2019-10-22 Strontium tetragallate(II,III) tetraarsenide, SrGa4As4, was synthesized in a Walker-type multianvil apparatus under high-pressure/high-temperature conditions of 8 GPa and 1573 K. The compound crystallizes in a new structure type (P3221, Z = 3) as a three-dimensional (3D) framework of corner-sharing SrAs8 quadratic antiprisms with strontium situated on a twofold rotation axis (Wyckoff position 3b). This arrangement is surrounded by a 3D framework which can be described as alternately stacked layers of either condensed GaIIIAs4 tetrahedra or honeycomb-like layers built up from distorted ethane-like GaII2As6 units comprising Ga—Ga bonds. Full Article text
syn Crystal structure, synthesis and thermal properties of bis(acetonitrile-κN)bis(4-benzoylpyridine-κN)bis(isothiocyanato-κN)nickel(II) By scripts.iucr.org Published On :: 2019-10-22 In the crystal structure of the title compound, [Ni(NCS)2(CH3CN)2(C12H9NO)2] or Ni(NCS)2(4-benzoylpyridine)2(acetonitrile)2, the NiII ions are octahedrally coordinated by the N atoms of two thiocyanate anions, two 4-benzoylpyridine ligands and two acetonitrile molecules into discrete complexes that are located on centres of inversion. In the crystal, the discrete complexes are linked by centrosymmetric pairs of weak C—H⋯S hydrogen bonds into chains. Thermogravimetric measurements prove that, upon heating, the title complex loses the two acetonitrile ligands and transforms into a new crystalline modification of the chain compound [Ni(NCS)2(4-benzoylpyridine)2], which is different from that of the corresponding CoII, NiII and CdII coordination polymers reported in the literature. IR spectroscopic investigations indicate the presence of bridging thiocyanate anions but the powder pattern cannot be indexed and, therefore, this structure is unknown. Full Article text