1. Status and developments in BL13-XALOC at Alba

2. Why XALOC
Difractòmetre
Orienta la mostra
Robot
Posiciona la mostra
Detector
Flux congelador a -173º C
Microscopi
XALOC-BL13 beamline determines the 3D structure of macromolecules (proteins, ADN/ARN) using X-ray crystallography
0,1 mm
Detector
Cabina Experimental de Xaloc-BL13

3. 3D image at atomic resolution of a protein+DNA
3. Solve a
X-ray diffraction pattern
of protein crystal at the pixel detector
Protein crystal
3D image at atomic resolution of a protein+DNA

4. High demand User Operation Cycle 1 (2012+) Cycle 2 (2013) 97 BT days
34 Udays (29 proposals)
Users can not manage LN2, safety training is not yet on-line, improve User office portal (introduce coworkers), user accounts
~50 proposals

5. Beamline status Beamline status : Operative (but not completed yet)
Very positive comments from all (!) users
Typical beam size at sample is 5010 um FWHM (HV) as seen on a 20-um fluorescence screen
Unfocused and defocused modes were tested although not currently used.
Very reliable beam optics (alignment done daily in 10’)
Beam at sample drifts (typically downwards 1 um/hour)
Beam recovered easily after a shutdown.
Beam aligned using EH positioning tables Optics (mirror pitches) could also be used.
Measured beam flux is >2·1012 ph/s/250mA
5010 mm
(FWHM, HV)
Flux (ph/s/250mA)
E (keV) #3 #5 #7 #9
#11
#13
Underlying: diagnostics are very important

6. Vertical Focusing Mirror Horizontal Focusing Mirror
Beamline description
Beamline concept : In-vacuum Undulator IVU Channel-cut Si(111) monochromator + KB focusing mirrors
Beamline status : Operative
Vertical Focusing Mirror
Mono- chromator
Horizontal Focusing Mirror
Diffractometer
Detector
Distance from source (m)
20.100
Sample changer
22.800
24.785
Dv = 3.47
29.375
Dh = 5.4
Experimental
Hutch

7. Horizontal Focusing Mirror Vertical Focusing Mirror
XALOC Layout m
Detector
Diffractometer m
Dh = 5.4
Photon shutter
Horizontal Focusing Mirror m
Dv = 3.47
Vertical Focusing Mirror m
Sample changer
Monochromator
Attenuator
Other optical elements
Fluorescence screens
Diode XBPMs
Slits
FE trigger unit

8. Optics
Channel cut Si(111), 6 mm gap, by CINEL (crystals by Crystal Scientific)
5-22 keV, with 1 mm excursion (Pt-K →Se-K: 30 mm; complete Se-MAD: 11 mm)
2nd xtal pitch (stepper motor)
2nd xtal pitch
V feedback (piezo)
Bremsstrahlung block
I0 diode
beam
channel cut crystal
cryogenic pipes
accelerometer
Resolution Bragg
Repeatability Bragg
1.10 ± 0.08 mrad
(0.064 mdeg)
2 mrad monodirectional
4 mrad bidirectional
Measured at 1 full step
In range 5-23 deg
Measures limited by thermal drift

9. Horizontal Focusing Mirror
Optics: mirrors
2 mirrors, in a Kirkpatrick-Baez configuration
Manufactured by IRELEC, surfaces made by InSync
Elliptically bent using 2 motors, equipped with strain gauges
Equipped with accelerometers to monitor pitch vibrations
Fully installed
VFM
HFM
Optical length
300 mm
600 mm
Stripes
Si, Rh, Ir Z
Roll
Pitch/Z
Range
10 mm
15 mrad
Tbd
Resolution
0.08 mm
1 mrad -
Repeatability
4 mm
1 mm
tbd
Vertical Focusing Mirror
Horizontal Focusing Mirror

10. Lysozyme data set at Rsym (inner shell)<5%
High quality data: Lysozyme
Test lysozyme crystal at 100K.
Excellent overall statistics: Rsym = 3.8 % (90 deg)
Also at the lowest resolution shell (2.76A): Rsym= 2 %.
Resolution 1.26 Å.
Molecular replacement rendered excellent ED maps.
lysozyme (a=b=79 Å c=37 Å; P43212)
sample-det distance=200 mm
l= Å, exp time =1 s, Dw = 1°
Atomic resolution data:
T98D-SH3 domain of c-Src Tyr kinase
P3121 , a = b =31.5 Å, c = Å
First data set collected at 12.6 keV and at 0.93 Å resolution:
0.5 deg oscillation, 90 deg, 1.3 sec exp time
Rsym = 3.8 % (90 deg)
Second data set collected at 15 keV and at 0.96 Å resolution: deg oscillation, 205 deg, 2.6 sec exp time
Rsym= 3.9 % P
Crystals from A. Cámara, UA, Almería

11. Solve a structure using MAD at Se-K edge
SAD data collection: meganuclease I-Dmol D. Mobilis
First ab initio solved structure, by Se K-edge SAD
Protein-DNA complex (PDB 2VS8)
Se-Met SAD 360˚, 2.4 Å resolution, 1 sec exp time
P21, a = 106.6, b = 70.3, c = 107.1, b = 119.9
Protein
DNA
Fluorescence scan widget
Crystals from G. Montoya, CNIO, Madrid

12. Solve a structure with a unit cell par. a>400 Å
Human Rhinovirus 2
Monoclinic cell
a = 470 Å, b= 376 Å, c = 465 Å
= 90˚, = 99˚, = 90˚
Diffraction to 4 Å.
Crystal-detector distance 750 cm
(max. distance 1350 cm)
Crystals from N. Verdaguer, IBMB, Barcelona

13. Detectors at the Experimental Hutch
Fluorescence Si-drift detector
Diamond X-ray position monitors
Pixel main detector
PIN Diodes
and YAG fluorescence screens

14. Detector Pilatus 6M (Dectris) Photon counting pixel detector
Preliminary tests on integration into BL successfully passed
Currently ending manufacturing phase
Estimated delivery in May 2011
Data transfer and storage system to be defined
ALBA turn = 893 ns
124 ns
Area
431 x 448 mm2
Pixel size
172 mm
Point spread
1 pixel
Max. framing rate
12 Hz
Dynamic Range
20 bits (106 ct)
Usable count rate
2x106 cts/s
Energy trimming
Yes, recommended E0/2
Gain
3, Fast, standard, high

15. ? ? Detector. What else? 320 um Silicon: needed thicker
Smaller pixel size
Tiling is tolerable, but gaps should be reduced
2.3 ms dead time: can be smaller?
Area, area
Triggers, triggers, triggers
ALBA turn = 893 ns
124 ns ?
Area
431 x 448 mm2
Pixel size
172 mm
Point spread
1 pixel
Max. framing rate
12 Hz
Dynamic Range
20 bits (106 ct)
Usable count rate
2x106 cts/s
Energy trimming
Yes, recommended E0/2
Gain
3, Fast, standard, high ?

16. Other projects Transmissive PIN diode Collaboration with CNM Pinhole
10x10mm2
transmissive (10 um thick)
Pinhole
Heavy Z material, 80 um thick
Hole 3-20 um diameter
High precision tools
Sharp tips <1um
Slit blades
Fluorescence dot
Mounted in a sample holder
1 um diameter
Used to position beam and spindle

17. The XALOC Team Engineering Computing Experiments
Carles Colldelram Mech Engineer
Alex Enrique Mech Technician
Fabien Rey Alignment
Marcos Quispe Cryogenics
Computing
Guifré Cuní Controls Engineer
Oscar Matilla Electronic Engineer
Julio Lidón
Xavi Fariña Elec technician
Experiments
Jordi Juanhuix
Jordi Benach
Fernando Gil
J.C. Martínez metrology
Josep Nicolás mirrors, metrology
Igors Sics diagnostics
First data set
April 2012
First Official Users 18 July 2012
Thank you for your attention