XtaLAB Synergy-S

Pensando en su éxito, hemos producido el difractómetro XtaLAB Synergy-S para la difracción de rayos X de monocristal. Con una combinación de componentes de punta y un software inspirado en el usuario; vinculados por medio de una arquitectura altamente paralelizada, el XtaLAB Synergy-S produce datos rápidos y precisos de una manera inteligente.

El sistema se basa en nuestra nueva serie de fuentes de microfoco PhotonJet-S. Esta tercera generación de fuentes ha sido diseñada para maximizar los fotones de rayos X en la muestra mediante el uso de una combinación de nuevas ópticas, nuevos tubos más duraderos, y un sistema de alineación mejorada. Los PhotonJets están disponibles en longitudes de onda Cu, Mo o Ag, ya sea en una configuración de fuente única o doble.

El nuevo goniómetro kappa ha sido completamente rediseñado para incorporar una mayor velocidad de motor y un brazo telescópico único de dos thetas para proporcionar una flexibilidad total en su experimento de difracción. El goniómetro es compatible con la más amplia variedad de detectores para satisfacer sus necesidades. CCD o HPC? Usted elije.

Beneficios:

Mejora significativa en la calidad y la velocidad de la recolección de datos sobre los anteriores sistemas de microfoco de tubo sellado.
Una distancia del detección más larga o más corta significa que se puede analizar una variedad más amplia de muestras con una precisión excepcional.
Mínimo tiempo de inactividad con tubo de rayos X de larga duración, compatible con diagnósticos y solución de problemas en línea.

$A fast and agile single crystal X-ray diffractometer for small molecule 3D structure analysis$

Features

Fuente de alto flujo y aumento de la velocidad del goniómetro para permitir experimentos más ágiles y rápidos.
Telescópico único de brazo dos thetas para llegar a distancias largas y cortas de cristal a detector.
Diseño de goniómetro kappa mejorado con posicionamiento simétrico 2θ.
Nueva fuente de alto flujo con tubos de rayos X de más larga duración.
Mecanismo de alineamiento óptico de rayos X mejorado para un fácil mantenimiento.
La más amplia variedad de detectores disponibles: HPC o CCD
Caja de diseño inspirado en el usuario para un mejor flujo de trabajo
Nueva iluminación de la caja y del cristal controlada electrónicamente.

This video shows the XtaLAB Synergy-S single crystal X-ray diffractometer in action. Watch the fast diffractometer race the Rigaku office coffee machine to obtain a the X-ray crystal structure; this system is fast!

If you are unable to view this video, click here to download it (392 MB).

HyPix-6000HE: Hybrid photon counting X-ray detector

PILATUS3 R 200K: Low maintenance, direct photon counting X-ray detector

PILATUS3 R 300K: Direct photon counting X-ray detector with larger active area

XtaLAB Synergy accessories

	Description
Oxford Cryo 800	El Oxford Cryostream Cooler: La serie Cryostream 800 es el sistema de baja temperatura a base de nitrógeno líquido más resistente, eficiente y fácil de usar disponible hoy en día. Las características específicas incluyen un sistema de flujo laminar superior, es decir, prácticamente cero riesgo de formación de hielo, extremadamente silencioso y un sistema de inicio rápido que resulta en un tiempo de enfriamiento de 100K de sólo 20 minutos

CrysAlis^Pro v40

Now with full 64 bit compatibility!

Rigaku Oxford Diffraction single crystal X-ray diffractometers come complete with CrysAlis^Pro, our user-inspired data collection and data processing software for small molecule and protein crystallography. Designed around an easy-to-use graphical user interface, CrysAlis^Pro can be operated under fully automatic, semi-automatic or manual control.

The latest release, CrysAlis^Pro v.40, is now fully 64 bit compatible and ready for the future. As modern diffractometers increase in performance and speed, your experiments generate bigger and bigger images and datasets. Additionally, supporting large detectors with very high pixel counts, such as those more commonly found at synchrotrons, requires large amounts of memory. Moving to 64 bit gives applications access to more memory, enabling the handling of these very large image sizes and data sets.

Expanded support for older Rigaku instrumentation and third party hardware is also in this release.

See below for other new software features that have recently been introduced.

How to get CrysAlis^Pro

The software is freely available for users of Rigaku Oxford Diffraction single crystal X-ray instruments and can be downloaded from our forum. Please register at http://www.rigakuxrayforum.com. Any queries related to the software may be answered on the forum.

CrysAlis^Pro: Seamless from start to finish

CrysAlis^Pro combines automated crystal screening, the fastest and most accurate strategy software available, concurrent data reduction and automatic small molecule structure solution. Visual feedback is provided for each step with clear, color-coded guidance so that both novices and experts can collect high-quality data in the shortest time possible.

CrysAlis^Pro is built on a command line interface and the GUI retains full manual control options for those that want them. It is your choice how to analyse your data.

CrysAlis^Pro processes data using sophisticated algorithms to provide the highest quality data. As technology or approaches change, our software team incorporates these to further advance data analysis and processing.

Processing of challenging and non-standard data collections

CrysAlisPro Ewald3D

CrysAlis^Pro contains a comprehensive and highly effective range of tools for tackling a wide range of samples from easy to challenging, and non-standard crystal samples. For example, EwaldExplorer and Ewald 3D (NEW!) easily identify effects, problems or artifacts in difficult or problematic datasets.

Ewald3D allows visualization of measured reciprocal space in 3-dimensions and in an undistorted way. Identifying diffuse scatter, modulation, subtle twinning, or incorrect instrument models is quick and easy with this brand new feature.

Supporting a range of crystallographic setups and applications

In addition to standard data collection routines, CrysAlis^Pro contains tools for working with non-standard experimental setups and sample types, including:

High pressure data collections
Variable temperature and multi-wavelength experiments
Powder experiments (data collection and processing)
Automatic screening or full data collections of several in situ protein crystals
Highly absorbing samples
Up to 8-fold twinned samples
Charge density measurements
Absolute structure determination

Software Compatibility

Exporting frames or data from CrysAlis^Pro into suitable alternative formats such as mosFLM, XDS, Denzo (HKL 2000) or another Esperanto format is easily achieved. Use CrysAlis^Pro’s data collection strategy to achieve the best data coverage in the quickest possible time and then automatically output into HKLF format for small molecule datasets or into the MTZ format for protein datasets.

CrysAlis^Pro is used by numerous research groups to process their synchrotron data. Our software is capable of importing data from several different detector types; known or unknown.

AutoChem

AutoChem is the ultimate productivity tool for small molecule chemists, offering fast, fully automatic structure solution and refinement during data collection. Developed in collaboration with OlexSys Ltd (Durham University, UK), AutoChem works in conjunction with Olex2 where more advanced structure solution and refinement functionality exists. AutoChem is seamlessly integrated within CrysAlis^Pro, and forms an integral part of our ‘What is this?’ feature.

The ‘What is this?’ feature gives you structures in seconds and ensures you are not wasting time collecting full datasets on known samples or starting materials. It is an alternative pre-experiment option, which is used to plan your full data collections.

日本語

Dr John Bacsa, Emory University

bacsa I underestimated the impact a new system would have on the workflow and our ability to analyse multiple samples. It has allowed us to remain competitive, and to be able to provide the necessary service support for research groups in the department.

Read more about Dr John Bacsa, Emory University

Dr. Henrik Friis, Natural History Museum at the University of Oslo

Friis Dr. Henrik Friis is Associate Professor in Mineralogy in the Natural History Museum, University of Oslo. Prior to the installation of the new XtaLAB Synergy-S system in early 2018, Dr. Friis had no direct access to a single-crystal X-ray diffractometer system: yet he depends upon single-crystal diffraction techniques extensively to advance his work in relation to a wide range of recently-discovered minerals and new materials research. With a large number of collaborators, worldwide, Henrik was in a position to collect some single-crystal data in the laboratories of his research partners and at a number of central research facilities. There were several reasons for purchasing the XtaLAB Synergy-S system, as discussed, below.

Read more about Dr. Henrik Friis, Natural History Museum at the University of Oslo

Dr. Samantha N. MacMillan, Cornell University

macmillan My decision was ultimately cemented by doing a demo of the instrument and I would recommend that anyone considering making a purchase do one, either in person or virtually. I absolutely would recommend my new system – the combination of speed, quality and design has transformed the way that we are doing research in the facility.

Read more about Dr. Samantha N. MacMillan, Cornell University

Prof. Christine McKenzie, University of Southern Denmark

mckenzie The “What-Is-This (WIT)” function means that students’ crystals can be checked more or less immediately. There is no longer the sense that we can’t waste our time and valuable machine time on crystals of well-known compounds.

Read more about Prof. Christine McKenzie, University of Southern Denmark

Papers published using the XtaLAB Synergy-S

Lipowska M, Klenc J, Taylor A T, Marzilli L G. “fac-99m Tc/Re-tricarbonyl complexes with tridendate aminocarboxyphosphonate ligands: suitability of the phosphonate group in chelate ligand design of new imaging agents.” Inorg. Chim. Acta (2018) just accepted 10 Nov https://www.sciencedirect.com/science/article/pii/S0020169318314464
Gradstein F M, Waskowska A, Kopaevich L, Watkins D K, Friis H, Pérez Panera J. “Berriasian planktonic foraminifera and calcareous nannofossils from Crimea Mountains, with reference to microfossil evolution.” Swiss Journal of Palaeontology (2018), just accepted 22 Oct https://link.springer.com/article/10.1007%2Fs13358-018-0175-8
Alexandropoulos D I, Alaimo A A, Sun D, Stamatatos T C. “A New {Dy5} Single-Molecule Magnetic Bearing the Schiff Base Ligand N-Naphthalidene-2-amino-5-chlorophenol.” Magnetochemistry (2018) 4(4):48 https://doi.org/10.3390/magnetochemistry4040048
Getmanenko Y A, Mullins C S, Nesterov V N, Lake S, Risko C, Johnston-Halperin E. “Magnetic ordering in a vanadium-organic coordination polymer using a pyrrolo[2,3-d:5,4-d’]bis(thiazole)-based ligand.” RSC Adv. (2018) 8:36223-36232 https://pubs.rsc.org/en/content/articlehtml/2018/ra/c8ra05697h
Worrell A, Sun D, Mayans J, Lampropoulous C, Escuer A, Stamatatos T C. “Oximato-Based Ligands in 3d/4f-Metal Cluster Chemistry: A Family of {Cu3Ln} Complexes with a “Propeller”-like Topology and Single-Molecule Magnetic Behavior.” Inorg. Chem. (2018), just accepted 17 Oct https://pubs.acs.org/doi/ipdf/10.1021/acs.inorgchem.8b02495
VanGelder L E, Petel B E, Nachtigall O, Martinez G, Brennessel W W, Matson E M. “Organic Functionalization of Polyoxovanadate-alkoxide Clusters: Improving the Solubility of Multimetallic Charge Carriers for Nonaqueous Redox Flow Batteries.” ChemSusChem (2018), just accepted 15 Oct https://onlinelibrary.wiley.com/doi/pdf/10.1002/cssc.201802029
Tan Y S, Chun, H Z, Jotani M M, Tiekink E R T. “Steric control of supramolecular association in structures of Zn(S2COR)2 with N,N’-bis(pyridine-4ylmethyl)oxalamide.” Z. Kristallogr. Cryst. Mater. (2018), published 8 Oct https://doi.org/10.1515/zkri-2018-2120
Pejić J, Vušak D, Szalontai G, Prugovečki B, Mrvoš-Sermek D, Matković-Čalogović D, Sabolović J. “Disorder at the Chiral Cα Center and Room Temperature Solid-State cis-trans Isomerization; Synthesis and Structural Characterization of Copper(II) Complexes with D-allo, L-Isoleucine.” Crys. Growth Des. (2018) 18(9):5138-5154 https://pubs.acs.org/doi/abs/10.1021/acs.cgd.8b00589
Meyer R L, Brennessel W W, Matson E M. “Synthesis of a gallium-functionalised polyoxovanadate-alkoxide cluster: Toward a general route for a heterometal installation.” Polyhedron (2018), 156: 303-311 https://www.sciencedirect.com/science/article/pii/S027753871830576X?via%...
Ravat P, Šolomek T, Häussinger D, Blacque O, Juríček M. “Dimethylcethrene: A Chiroptical Diradicaloid Photswitch.” J. Am.. Chem Soc. (2018) 140: 10839 – 10847 https://pubs.acs.org/doi/pdf/10.1021/jacs.8b05465
Shapiro J A, Morrison K R, Chodisetty S S, Musaev D G, Wuest W M. “Biologically Inspired Total Synthesis of Ulbactin F, an Iron-Binding Natural Product.” Org. Lett. (2018), 20(18): 5922-5926 https://pubs.acs.org/doi/abs/10.1021/acs.orglett.8b02599
Zhao C, Schwartz T, Stöger B, White F J, Chen J, Ma D, Fröhlich J, Kautny P. “Controlling excimer formation in indolo[3,2,1-jk]carbazole/9H-carbazole based host materials for RGB PhOLEDs” J. Mat. Chem. C. (2018), 6: 9914-9924 https://pubs.rsc.org/en/content/articlepdf/2018/tc/c8tc03537g
Movassaghi S, Leung E, Hanif M, Lee B Y T, Holtkamp H U, Tu J K Y, Söhnel T, Jamieson S M F, Hartinger C G. “A Bioactive L-Phenylalanine-Derived Arene in Miltitargeted Organoruthenium Compounds: Impact on the Antiproliferative Activity and Mode of Action” Inorg. Chem (2018) 57(14) 8521-8529 https://pubs.acs.org/doi/abs/10.1021/acs.inorgchem.8b01187
Su Y, Su H-F, Wang Z, Li Y, Schein S, Zhao Q, Wang X, Tung C-H, Sun D. “Three Silver Nests Capped by Thiolate/Phenylphosphonate.” Chemistry:A European Journal (2018), 24(56): 15096-15103 https://onlinelibrary.wiley.com/doi/abs/10.1002/chem.201803203
Wu Y, Halat D M, Wei F, Binford T, Seymour I D, Gaultois M W, Shaker S, Wang J, Grey C P, Cheetham A K. “Mixed X-site formate-hypophosphite hybrid perovskites.” Chemistry: A European Journal (2018), 24(44): 11309-11313 https://onlinelibrary.wiley.com/doi/abs/10.1002/chem.201803061
Morgan M T, Yang B, Harankhedkar S, Nabatilan A, Bourassa D, McCallum A M, Sun F, Wu R, Forest C R, Fahrni C J. “Stabilization of aliphatic phosphines by auxillary phosphine sulfides offers zeptomolar affinity and unprecedented selectivity for probing biological Cu(II).” Angew. Chem (2018) 130(31): 9859-9863 https://onlinelibrary.wiley.com/doi/abs/10.1002/ange.201804072
Scholl K, Dillashaw J, Timpy E, Lam Y, DeRatt L, Benton T R, Powell J P, Houk K N Morgan J M. “Quinine-Promoted, Enantioselective Boron-Tethered Diels-Alder Reaction by Anomeric Control of Transition-State Conformation.” J. Org Chem. (2018) 83: 5756-5765 https://pubs.acs.org/doi/abs/10.1021/acs.joc.8b00938
Akondi S M, Gangireddy P, Pickel T C, Liebeskind L S. “Aerobic, Diselenide-Catalyzed Redox Dehydration: Amides and Peptides.” Org. Lett. (2018) 20: 538-541 https://pubs.acs.org/doi/10.1021/acs.orglett.7b03620
Cundari T R, Jacobs B P, MacMillan S N, Wolczanski P T. “Dispersion forces play a role in (Me2IPr)Fe(=NAd)R2 (Ad = adamantly; R=neoPe, 1-nor) insertions and Fe-R bond dissociation enthalpies (BDEs)” Dalton Transactions (2018) 47: 6025-6030 http://pubs.rsc.org/en/Content/ArticleLanding/2018/DT/C7DT04145D#!divAbs...
Vaccarello D N, O’Connor K S, Iacono P, Rose J M, Cherian A E, Coates G W. “Synthesis of Semicrystalline Plyolefin Materials: Precision Methyl Branching via Stereoretentive Chain Walking.” J. Am. Chem. Soc. (2018) 140(20): 6208-6211 https://pubs.acs.org/doi/10.1021/jacs.8b02963
Molčanov K, Mou Z, Kertesz M, Kojić-Prodić B, Stalke D, Demeshko S, Šantić A, Stilinović. “Two-electron / multicenter – pancake bonding in π-stacked trimers in a salt of tetrachloroquinone anion.” Chemistry: A European Journal, (2018) 24(33): 8292-8297 https://onlinelibrary.wiley.com/doi/pdf/10.1002/chem.201800672
Milić J, Zalibera M, Talaat D, Nomrowski J, Trapp N, Ruhlmann L, Boudon C, Wenger O S, Savitsky A, Lubitz W, Diederich F. “Photoredox-Switchable Resorcin[4]arene Cavitands: Radical Control of Molecular Gripping Machinery via Hydrogen Bonding.” Chemistry: A European Journal, (2017) 24(6): 1431-1440 https://onlinelibrary.wiley.com/doi/abs/10.1002/chem.201704788
Haberland S, Finke A D, Kerisit N, Katan C, Trolez Y, Gawel P, Leito I, Lõkov M, Järviste R, Kaupmees K, Trapp N, Ruhlmann L, Boudon C, Himmel D, Diederich F. “Enhancement of Push-Pull Properties of Pentafulvene and Pentafulvene Derivatives by Protonation at Carbon.” Eur J. Org. Chem., (2018) 6:739-749 https://onlinelibrary.wiley.com/doi/abs/10.1002/ejoc.201800039
Hao W, Harenberg J H, Wu X, MacMilan S N, Lin S. “Diastereo- and Entatioselective Formal [3 + 2] Cycloaddition of Cyclopropyl Ketones and Alkenes via Ti-Catalyzed radical Redox Relay” J. Am. Chem. Soc. (2018) 140(10): 3514-3517 https://pubs.acs.org/doi/10.1021/jacs.7b13710
Ye K-Y, Pombar G, Fu N, Sauer G S, Keresztes I, Lin S. “Anodically Coupled Electrolysis for the Heterodifunctionalization of Alkenes.” J. Am. Chem. Soc. (2018) 140(7): 2438-2441 https://pubs.acs.org/doi/10.1021/jacs.7b13387
Junker A K, Hill L R, Thompson A L, Faulkner S, Sørensen T J. “Shining light on the antenna chromophore in lanthanide based dyes.” Dalton Trans., (2018) 47: 4794-4803 http://dx.doi.org/10.1039/C7DT04788F
Nievergelt P P, Babor M, Čejka J, Spingler B. “A high-throughput screening method for the nano-crystallization of salts of organic cations.” Chem. Sci., (2018) 9: 3716-3722 http://pubs.rsc.org/en/content/articlepdf/2018/sc/c8sc00783g. An additional news article is available at https://phys.org/news/2018-03-method-medication.html
Sarkar K, Dastidar P. “Supramolecular hydrogel derived from a C3-symmetric boronic acid derivative for stimuli-responsive release of insulin and doxorubicin.” Langmuir (2018) 34(2): 685-692. http://pubs.acs.org/doi/abs/10.1021/acs.langmuir.7b03326)
Urgiles J, Nathan S R, MacMillan S N, Wilson J J. “Dinuclear nitrido-bridged ruthenium complexes bearing diimine ligands.” Dalton Trans. (2017) 46: 14256-14263. http://pubs.rsc.org/en/content/articlelanding/2017/dt/c7dt03085a#!divAbs...
Hao W, Wu X, Sun J Z, Siu J C, MacMillan S, Lin S. “Radical Redox-Relay Catalysis: Formal [3+2] Cycloaddition of N-Acylaziridines and Alkenes.” J. Am. Chem. Soc. (2017) 139 (35): 12141-12144. http://pubs.acs.org/doi/abs/10.1021/jacs.7b06723
Phukkaphan N, Cruickshank D L, Murray K S, Phonsri W, Harding P, Harding D. J. “Hysteretic spin crossover driven by anion conformational change.” Chem. Comm. (2017) 53: 9801-9804. http://pubs.rsc.org/en/content/articlelanding/2017/cc/c7cc05998a#!divAbs...
Riwar L-J, Trapp N, Kuhn B, Diederich F. “Substituent Effects in Parallel-Displaced π–π Stacking Interactions: Distance Matters.” Angew. Chem. Int. Ed. (2017) 56 (37): 11252-11257. http://onlinelibrary.wiley.com/wol1/doi/10.1002/anie.201703744/full
Diederich F, Trapp N, Wörle M. “Small Molecule Crystallography in the Laboratory of Organic Chemistry at ETH Zürich.” Israel Journal of Chemistry (2017) 57 (1-2): 39-54. http://onlinelibrary.wiley.com/doi/10.1002/ijch.201600030/full
Gropp C, Husch T, Trapp N, Reiher M, Diederich F. “Dispersion and Halogen-Bonding Interactions: Binding of the Axial Conformers of Monohalo- and (±)-trans-1,2-Dihalocyclohexanes in Enantiopure Alleno-Acetylenic Cages.” J. Am. Chem. Soc. (2017) 139 (35): 12190-12200 http://pubs.acs.org/doi/pdf/10.1021/jacs.7b05461

ELement ANalyzer

Elemental analysis attachment for single crystals

The ELement ANalyzer is a state-of-the-art attachment that allows us to obtain qualitative information on elements in a single crystal at the same time as X-ray diffraction data collection for a single crystal structural analysis. By measuring the X-ray fluorescence spectrum emitted during X-ray diffraction experiments with the ELement ANalyzer, it becomes possible to perform elemental analysis on a single grain of crystal. The ELement ANalyzer can be used for confirmation the presence of central metal(s) in a mononuclear or polynuclear complex or solvent in a crystal for small molecule X-ray crystallography. There is a broad range of possible applications of the ELement ANalyzer in scientific fields.
ELAL Figure 1

Determine the presence and type of central metal in a metal complex

ELAL Figure 2

Confirmation of counter ion exchange

ELAL Figure 3

Evaluation of heavy atom derivative

ELAL Figure 4

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Detector		HyPix-6000HE
Active area		77.5 mm x 80.0 mm
Dynamic quantum efficiency (Cu-Kα)		> 98%
Dynamic range		31-bits
Counting rate per pixel		1 x 10⁶ X-ray photons/sec
Readout speed		0 ms in ZeroDeadTime mode
Maximum frame rate		100 Hz
Point-spread function		1 pixel
Cooling		Air-cooled
Humidity control		Not required
Pixel size		100 μm x 100 μm

Detector		PILATUS3 R 200K
Active area		83.8 mm x 70.0 mm
Sensor		Reverse-biased silicon diode array
Dynamic quantum efficiency (Cu-Kα; Mo-Kα)		> 98%; > 76%
Dynamic range		20-bits
Counting rate per pixel		2 x 10⁶ X-ray photons/sec
Readout speed		7 msec
Maximum frame rate		20 Hz
Point-spread function		1 pixel
Cooling		Air-cooled
Humidity control		Nitrogen or dry air flow
Pixel size		172 μm x 172 μm

Detector		PILATUS3 R 300K
Active area		83.8 mm x 106.5 mm
Sensor		Reverse-biased silicon diode array
Dynamic quantum efficiency (Cu-Kα; Mo-Kα)		> 98%; > 76%
Dynamic range		20-bits
Counting rate per pixel		1 x 10⁷ X-ray photons/sec
Readout speed		7 msec
Maximum frame rate		20 Hz
Point-spread function		1 pixel
Cooling		Water-cooled
Humidity control		Nitrogen or dry air flow
Pixel size		172 μm x 172 μm

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Difractómetro de rayos X con microfoco único o dual para todas sus necesidades de cristalografía

Un sistema rápido y ágil para el análisis en 3D de pequeña molécula/H2>