BSI wiki

Training on 2015.03.30

FR-X generator: 45 kV, 66 mA, 70 μ cross-section, 180 μ beam, 1.7 miliradians divergence

Pilatus 300K detector: 3 chips, shorter exposure time, no readout (no shutter closing), almost never overloaded (>1.5 millions), water circulation at room temperature, dry air

>thread

command on camserver gives the temperature and humidity level Green light at the back of the detector to check before use.

Cryostream should be at 100 K

Close 3 glass doors, push the green light on the left

Run HKL_3000_P300KChi (the other HKL_3000 version is for data integration only)

Collect/Connect to initialize (also open an instrument server window in the background)

0.25° oscillation by default As a “rule of thumb” set the detector distance (in mm) to half the longest unit cell parameter (in Å) ¹⁾

Align/Zero goniostat resets all positions (parameters in /hkl_dc.ini)

2θ always swings away (clockwise)

Set the directory /data/user/project1_crystal1

dtdisplay

• middle click > zoom area
• middle click > reset zoom
• control + left click > move around
• measure /Measure Left 1x, 2x, 3x or 4x (to average)

Never collect at 2θ = 0, use at least 2θ = 2 to offset the center horizontally and avoid thus avoid missing data due to the gaps between detectors

Index

• Refine in triclinic (P1)
• Fit Basic
• Fit All
• Mosaicity (by default it cannot estimate well the mosaicity²⁾, so you need to select)
• To process up to the corner, you need to index up to the corner!

Strategy

• HKL_3000 strategy only works for single axis
• Rigaku_Strategy is specially made for FR-X on the 4 axis
• Choose I want to make changes
• Completeness 99% (to reduce collect time)
• Redundancy 3.0 (4.0 by default)
• Distance (the distance from the first image is set)
• Suggested distance is not useful
• Edit preferences is possible

You can swing the slider on Time window to adjust/reduce the number of collected frames Don't forget to adjust the Mosaicity value! If anomalous data is required, adjust the redundancy accordingly

For some pins, Chi 60° may be too high and should be restricted to 50°

Close the window and choose Setup DC to transfer the informations to HKL data collection window Exposure time is not imported from the strategy and should adjusted manually