What the Chemical Instrumentation enter Can Do For You X ...fassciencecores.yale.edu/sites/default/files/12-9-09.pdf2009/12/09 · Cueva de los Cristales – Mexico National Geographic

What the Chemical Instrumentation Center Can Do For You

X-ray Diffraction and Other Available Services

Christopher Incarvito

Yale FASCoffee with the CoresDecember 9, 2009

Chemical Instrumentation Center

Resource– Shared instrumentation– Open access– Collaborative environment

Training– Necessary skills for operation– Encourage responsibility

Expertise– Disseminate fundamentals– Design and support challenging experiments

Evolution– Meet the demands of current and future research– Implement new techniques and instrumentation

CIC


CIC

Chemical Instrumentation Center– NMR Spectroscopy– X-ray Diffraction– Mass Spectroscopy– Optical Spectroscopy


CIC

Chemical Instrumentation Center– NMR Spectroscopy– X-ray Diffraction– Mass Spectroscopy– Optical Spectroscopy

Biophysical Instrumentation Center– NMR Spectroscopy– X-ray Diffraction– Mass Spectroscopy– Optical Spectroscopy

Instrumentation

Mass Spectrometry– Applied Biosystems Voyager-

DE Pro MALDI-TOF MS– Waters Alliance HPLC/ ESI-

MSAgilent 5973 GC-MS– HP 5971A GC-MS

Optical Spectroscopy– Thermo FT-IR-Raman– Cary 3E UV-VIS– PE-341 Polarimeter– Varian SpectrAA-200 Atomic

Absorption– ASI ReactIR 1000

X-ray Crystallography– Rigaku R-Axis-Spider Single

Crystal Diffractometer– Rigaku SCXMini Single

Crystal Diffractometer– Bruker D8 Focus Powder

Diffractometer

CIC

NMR Spectroscopy– Varian Inova 800 MHz– Varian Inova 600 MHz– Varian Unity Plus 600 MHz– Varian Inova 500 MHz

widebore– Varian Inova 500 MHz – Bruker Avance 500 MHz – Bruker DRX 500 MHz – Bruker DPX 400 MHz – Bruker DPX 400 MHz– GE Omega 300 MHz– GE QE-Plus 300 MHz – Bruker AC 250 MHz

EPR– Bruker Elexsys E-500– Varian E-9

BIC Resources– BC Analytical Ultracentrifuge– Horiba Spectrofluorimeter– Waters LCT MS– Rigaku 007HF rotating anode XRD– Spectrophysics CD spec– Biacore

High-Performance Computing

Crystallization Automation

etc.

Personnel - CIC

Christopher Incarvito, Ph.D.– Director– [email protected]

Eric Paulson, Ph.D.– Manager, NMR Resources– [email protected]

Xiaoling Wu, Ph.D.– NMR Spectroscopist– [email protected]

Jefferson Chin– Instrument Support– [email protected]

Jack Brenner– Research Support– [email protected]

CIC

Personnel - CIC






CIC

Personnel - CIC






CIC

Personnel - CIC






CIC

Personnel - CIC






CIC

Personnel - BIC

Wuyi Meng, Ph.D.– X-ray Crystallographer– [email protected]

David Keller– Instrument Support– [email protected]

CIC

Personnel - BIC

Wuyi Meng, Ph.D.– X-ray Crystallographer– [email protected]

David Keller– Instrument Support– [email protected]

CIC

Personnel

CIC


CIC

CRB 100NMR

– 400 MHz (x2)– 500 MHz (x2)

MS– GC-MS– LC-MS– MALDI-ToF MS

Optical– FT-IR– FT-Raman– UV-VIS– Polarimeter

Biophysical– ITC– DSC

CIC


Facilities – 1 of 5

SCL 123XRD

– Bruker D8-Focus pXRD– Rigaku SCXMini single crystal XRD– Rigaku R-Axis Spider XRD– Rigaku 007HF rotating anode XRD– Optical Microscopes

CIC



SCL 135/148NMR

– 300 MHz (x2)– 500 MHz WB– 600 MHz– 800 MHz

Electronics Shop

Future Home of BIC– ITC– DSC– AUC– TD-Fluoresence– Biacore– ToF-MS

CIC



Bass PitNMR

– 500 MHz– 600 MHz

CIC



CIC



CIC


Web Support

Eric Paulson

CIC


Web Support

Next Generation

All InstrumentationManuals/ProtocolsIntegrated Wiki

Chemical Instrumentation Center Primary Users

ChemistryMB&BMCDBPhysicsGeologyPharmacologyEtc.

CIC

Chemical Instrumentation Center Collaborations

Industry

AchillionATMI

Beta PharmaBioRelix

Cara TherapeuticsCarestream HealthcareCyalume Technologies

EMD SeronoForma Therapeutics

HenkelHeritage Technologies

NeurogenRaindance Technolgies

Rib-X

CIC

Academia

Albertus Magnus UCentenary College

Fairfield UInstitute for Neurodegenerative Disorders

NIHOhio State

SCSUSyracuse U

Trinity CollegeU of Connecticut

UCSDUIUC

Wesleyan U


ResourceTrainingExpertiseEvolution

CIC

X-ray Diffraction

CIC

X-Rray Diffraction

nλ=2dsinθ

CIC

X-Rray Diffraction

CIC

X-Rray Diffraction

www.mitegen.com

CIC

X-Rray Diffraction

CIC

X-Rray Diffraction

Bruker D8-Focus Powder XRDRigaku SCXMini Single Crystal XRDRigaku R-Axis SPIDER Multipurpose XRDRigaku 007-HF Rotating Anode XRD

CIC

XRD Bruker D8-Focus

Powders– Polycrystalline– Amorphous

Thin FilmsMineralsParticle Size AnalysisQualitativeQuantitative

CIC

XRD Bruker D8-Focus

Sealed Tube Cu Target– 1.5418 Å

NaI Scintillation Detector

Variable Slits– Optimizing Resolution

Versatile and Upgradeable

CIC

XRD Bruker D8-Focus

CIC

XRD Rigaku SCXMini

Small Molecule Single Crystal– Organic– Inorganic– Organometallic

Routine analysisAbsolute Configuration

– (> Na)User friendly

CIC

XRD Rigaku SCXMini

Sealed Tube Mo Target– 0.7107 Å

Multilayer Optics– 300 – 800 micron beam

CCD Detector

-50 °C N2 Stream

CIC

XRD Rigaku SCXMini

Max Resolution ~ 0.65 ÅRapid Data Collection

> 100 data setsPublication data > 25 structures

CIC

XRD Rigaku SCXMini

Training available

Bystander-friendly

CIC

XRD Rigaku R-Axis SPIDER

Small Molecule Single Crystal– Organic– Inorganic– Organometallic

Mini-proteinsPowders (Phase-ID)FilmsIrregular samplesTwinned CrystalsIncommensurate StructuresAbsolute Configuration

– (> Oxygen)

CIC


Sealed Tube Cu Target– 1.5418 Å


Curved Image Plate Detector

-180 °C N2 Stream– Not shown

CIC


Cu Source– 1.5418 Å– Max resolution 0.83 Å

Mo Source– 0.7107 Å

– Max resolution 0.4 Å !!!

CIC

Chandrima Chatterjee– Vaccaro Lab

Liquid at RT!!!

Hexafluoroacetylacetone

CIC


Chandrima Chatterjee

CIC



CIC



CIC



CIC



CIC



CIC


SiGe Analysis

CIC


CIC


CIC


Versatile– Multiwavelength– Open design– Etc.

CIC

XRD Rigaku 007 HF

CIC

XRD Rigaku 007 HF

CIC

XRD Rigaku 007 HF

CIC

XRD Rigaku 007 HF

CIC

XRD Rigaku 007 HF

Rotating Anode Cu Source– 1.5418 Å


CCD Detector– Rigaku Saturn 944+

-180 °C N2 Stream

CIC

XRD Rigaku 007 HF

CIC

XRD Rigaku 007 HF

Rotating Anode Cu Source– 1.5418 Å


IP Detector– Mar 345 DTB

-180 °C N2 Stream– Not shown

XRD Rigaku 007 HF

CIC

Real data

CIC

XRD Rigaku 007 HF

Protein Samples– Screening– Full data collection

CIC

XRD Rigaku 007 HF

Protein Samples– Screening– Full data collection

MB&B 760 – Principles of Macromolecular Crystallography– Yorgo Modis– Yong Xiong– Wuyi Meng

Difficult Small Molecule Samples?

CIC

XRD Rigaku 007 HF

Cueva de los Cristales – MexicoNational Geographic

CIC

XRD Rigaku 007HF - CCD

Held in a film of oilCrystal dimensions

0.005 x 0.020 x 0.050 mm

Organic Sample – CHNO only

Dr. Lee Daniels

Rigaku Americas Corporation

CIC

XRD Rigaku 007 HF

Saturn 944+ CCD2 ° oscillations45 sec/°0.84 Å resolutionPublication quality

CIC

X-Rray Diffraction

Yale-Rigaku Symposium on X-ray Diffractionwww.yalerigakusymposium.org

Acknowledgements

Department of ChemistryCIC StaffOffice of the ProvostLisa D’Angelo

Next Coffee with the CoresAndy Sherman, HPC Resource

CIC

X-Rray Diffraction

10201020SynchotronNSLSII

10141014SynchotronNSLS

1091010AllCCD, IPCu007HF

Small molecule, mini-proteinIrregular

IPMoCu (1.5418 Å)

R-Axis Rapid

SM Single Crystal

CCDMo (0.71073 Å)

SCXMini

Brilliance(photons/sec/mm2/mR2

Flux(photons/sec/mm2)

SampleDetector Source(target, λ)

Documents

What the Chemical Instrumentation enter Can Do For You X ...fassciencecores.yale.edu/sites/default/files/12-9-09.pdf2009/12/09 · Cueva de los Cristales – Mexico National Geographic