Kappa – from a users Kappa – from a users perspective ?perspective ?

Standard todayStandard today

Most Labs/synchrotrons use single rotation Most Labs/synchrotrons use single rotation axis for data collectionaxis for data collection

WHY IS THIS?WHY IS THIS?

The persistence of a single The persistence of a single rotation axisrotation axis

Historical – rotation method –Arndt Wonacott camera etc Historical – rotation method –Arndt Wonacott camera etc

Cost, ease of implementation, simplicityCost, ease of implementation, simplicity

Implementation of control softwareImplementation of control software

Commercially available products –heavily erred to single Commercially available products –heavily erred to single rotation axis solutionsrotation axis solutions

Multi-axes alternatives have been bulky and not easily Multi-axes alternatives have been bulky and not easily incorporated into a standard PX setupincorporated into a standard PX setup

The persistence of a single The persistence of a single rotation axisrotation axis

Software for utilizing kappa – some say not readily Software for utilizing kappa – some say not readily accessible and easily incorporated? accessible and easily incorporated?

- Or is this just a lack of will and man-power…- Or is this just a lack of will and man-power…- Jim Pflugrath D*Trek – in use at SBC since 1997 - Jim Pflugrath D*Trek – in use at SBC since 1997 - Bruker/Nonius have very successful system ??- Bruker/Nonius have very successful system ??

““||Data collection on the Nonius KappaCCD is performed with the Data collection on the Nonius KappaCCD is performed with the NoniusNonius Collect software Collect software, an intuitive and user friendly , an intuitive and user friendly GUI driven program suite, which provides smooth and directed transitions through the phases of indexing, data collection GUI driven program suite, which provides smooth and directed transitions through the phases of indexing, data collection strategy, face indexing and crystal description etcstrategy, face indexing and crystal description etc .”.”

Commercially available systems from Nonius and HuberCommercially available systems from Nonius and Huber--still somewhat big and precision on the order of 20-30 micron sphere of confusionstill somewhat big and precision on the order of 20-30 micron sphere of confusion

No concerted effort from user community ??No concerted effort from user community ??

Nonius kappaNonius kappa

Huber kappaHuber kappa

Use of KappaUse of Kappa Alignment of crystalAlignment of crystal

-allows for intelligent and most efficient route to collection of a complete data set -allows for intelligent and most efficient route to collection of a complete data set

-allows measurement of Friedel mates at same time important for accurate -allows measurement of Friedel mates at same time important for accurate measurement of very small anom. Differencesmeasurement of very small anom. Differences

- Completion of data from multiple crystals –a real problem today due to radiation - Completion of data from multiple crystals –a real problem today due to radiation damage from high intensity sourcesdamage from high intensity sources

- Collection of diffraction data from around more than one rotation axis - Collection of diffraction data from around more than one rotation axis significantly improves scaling of data (we want to measure symmetry related significantly improves scaling of data (we want to measure symmetry related measurements in as different a way as possible)measurements in as different a way as possible)

-empirical absorption corrections – although less critical at shorter wavelengths-empirical absorption corrections – although less critical at shorter wavelengthshas become critical for longer wavelength experiments that are utilizing the very has become critical for longer wavelength experiments that are utilizing the very small anomalous signal originating for naturally occurring sulphur atoms in small anomalous signal originating for naturally occurring sulphur atoms in

proteinsproteins

Mini-KappaMini-Kappa Design compact kappa which will not Design compact kappa which will not compromise a standard PX sample /Detector compromise a standard PX sample /Detector environmentenvironment High accuracy to match the current state High accuracy to match the current state of the art 3of the art 3rdrd generation synchrotron sources generation synchrotron sources Rosenbaum/Rock at APS produced a mini-Rosenbaum/Rock at APS produced a mini-kappa which met to some extent these needskappa which met to some extent these needs Commercial minikappa from ADSCCommercial minikappa from ADSC

Rosenbaum/RockRosenbaum/RockMini-KappaMini-Kappa

ADSC ADSC Mini-KappaMini-Kappa

EMBL/ESRF Micro-KappaEMBL/ESRF Micro-Kappa

Tested very briefly on BM14 mainly to see Tested very briefly on BM14 mainly to see that design was mechanically sound that design was mechanically sound

Performed a real-life S-SAD experimentPerformed a real-life S-SAD experiment

-360 degrees of data collected at -360 degrees of data collected at = 0 = 0

-360 degrees of data collected at -360 degrees of data collected at = max = max Apologies – structure solved but Apologies – structure solved but

S-SAD resultsS-SAD results USE of 90 degrees of USE of 90 degrees of = 0 and = 0 and offset sufficient to give offset sufficient to give interpretable map (caveat Zn was bound!)interpretable map (caveat Zn was bound!)

Mean weight and estimated mapCC as a function of resolution d inf - 4.41 - 3.47 - 3.03 - 2.74 - 2.54 - 2.39 - 2.27 - 2.17 - 2.08 - 2.01 <wt> 0.509 0.525 0.534 0.494 0.535 0.522 0.492 0.477 0.489 0.491 <mapCC> 0.742 0.761 0.778 0.733 0.776 0.770 0.735 0.729 0.741 0.740 N 3771 3826 3719 3909 3807 3739 3729 3756 4017 3408

Pseudo-free CC = 54.53 %