CANADIAN MACROMOLECULAR CRYSTALLOGRAPHY FACILITY

CMCF-ID

Canadian Macromolecular Crystallography Facility - Insertion Device

  Normal Operations

The scientific goal of the CMCF-ID (08ID) beamline is to operate a protein crystallography beamline suitable for studying small crystals and crystals with large unit cells. Significant upgrades to the beamline were commissioned in May 2022, increasing the overall flux, enabling micro-focus beam sizes down to 5 µm, and significantly improving sample throughput.

The overall design of the beamline consists of white beam slits (WBS), an indirectly cryo-cooled double crystal multilayer monochromator (DCMM) supporting operation in monochromatic DCM mode or a high-flux "pink-beam" DMM mode, and vertical, horizontal, and micro-focusing mirrors. The innovative endstation utilizes an Arinax MD2-S microdiffractometer, Eiger X 9M X-ray detector, and ISARA sample automounter for rapid data collection both on-site and remotely. Beamline controls are based on EPICS and complemented with MxDC, a user-friendly interface developed in-house.

The source of X-rays on CMCF-ID is a small-gap undulator insertion device. As its name suggests, the undulator produces a periodic magnetic field that causes the path of the orbiting electrons to undulate, resulting in an emitted X-ray beam of higher spectral brilliance than could be produced by the simpler path taken by the electrons through a bending magnet.

The beamline is equipped with a Bruker XFlash 410 Spectrometer to perform X-ray Fluorescence spectroscopy and metal identification. The much higher flux of the CMCF-ID beamline makes it ideal for the collection of native datasets while still allowing for MAD/SAD data collection. Users are also encouraged to consider the use of CMCF-BM beamline for experimental phasing to reduce the risk of radiation damage.

Note: Data collection using the high-flux DMM mode poses a significant risk of sample destruction prior to full dataset collection, and is currently not recommended for most experiments. Users wishing to use DMM mode should reach out to your local contact well ahead of their planned beamtime.

Schematic

Layout
Component Distance from Source
WBS (White Beam Slits) 40.3 m (Horizontal Slits) 41.5 m (Vertical Slits)
DCMM (Double Crystal Multilayer Monochromator) 42.4 m
VFM (Vertically Focusing Mirror) 46.5 m
HFM (Horizontally Focusing Mirror) 48.4 m
μVFM (Vertically micro Focusing Mirror) 50.4 M
Sample 50.9 m

Beamline Specifications

Source
Typical Ring Current 220 mA (top-up mode)
Insertion Device 20 mm asymmetric hybrid small-gap in-vacuum undulator (SGU)
Insertion Device (SGU) Details
Operational Gap Range 5 mm - 15 mm
Number of Poles 190
Total Length of Magnet Assemblies 3821 mm
Permanent Magnet Blocks NdFeB Dysprosium
Minimum Remanance 1.19T
Minimum Intrinsic Coercivity at 20°C 39.0 kOe
Poles Vanadium Permendur
Total Power 11.4 kW (at 500 mA ring current)
SGU Properties at Minimum Gap
Peak Flux Density 1.066 T
Effective Flux Density 0.981 T
Effective k 1.83
Higher Order Contributions 8.4%
Photon Energy, n = 1 1.49 keV
Maximum Magnetic Load 9.5 kN
Beam
Spectral Range (keV) DCM mode: 5.0-20.0 keV
High flux DMM mode: 7.2-10.4 keV
Flux on Sample @ 200 mA (ph/s) DCM mode: 8.2 × 10^12 at 12 keV
High flux DMM mode: 1.2 x 10 ^14 at 9.72 keV
Flux density @ 200 mA (ph/s/mm^2) DCM mode: 1.8 x 10^16
DMM mode: 2.6 x 10^17
Energy Bandwidth (ΔE/E) DCM mode: 1.5 x 10^-4
DMM mode: 1 x 10^-2
Focal Size (FWHM) @ 12 keV (H x V) 53.6 µm x 8.6 µm
Aperture sizes (µm) 5, 10, 20, 30, 50
Beam Divergence at Sample (H x V) @ 12 keV 1.82 mrad x 0.34 mrad

Beamline Hardware

Optics
Monochromator Axilon double crystal/multi-layer monochromator (DCMM) Comprising a pair of indirectly cryo-cooled SI(111) crystals (DCM mode) arranged in series with a pair of Mo/B4C-coated Si(111) multilayers (DMM mode) with 300 bilayers.
Mirrors Vertical Mirror: Si(001) with 2 stripes (Si, Rh/Ir). r.m.s. slope error 0.37 µrad
Horizontal Mirror: Rh/Ir coated Si(001). r.m.s. slope error 0.78 µrad
Vertical micro Focusing Mirror: Rh/Ir coated Si(001). r.m.s. slope error 0.15 µrad
All mirrors are flat and shaped using elliptical benders (FMB Oxford).
Horizontal Demagnification (1/Mx) 6.8
Vertical Demagnification (1/My) 12.0
Endstation
Additional Instrumentation Bruker XFlash 410 fluorescence detector, HC1 humidity control device
Pin Length 18 mm Hampton Cryopin
Cryo Capability Oxford Instruments Cryojet, 90-300K
Automounter ISARA (single gripper) supporting Uni-Pucks, 464 pin capacity, approx 20 s duty-cycle
Goniometer
Goniometer Arinax MD2-S microdiffractometer and SmartMagnet sample holder
Maximum Rotation Speed (deg/s) 500
Sphere of Confusion 1 µm radius @ 100 deg/s
Visualization System
Type Arinax B-Zoom On-Axis Visualization (OAV)
Orientation Along beam axis
Zoom range 2.5x-30x
Maximum Field of View 2.4 x 1.9 mm
Minimum Field of View 0.38 x 0.24 mm
Detector
Current Detector Eiger X 9M
Crystal-Detector Distance 115 mm - 1000 mm
Readout Time Continuous readout, 3.0 µs dead time, duty cycle >99%
X-ray Sensitive Surface (W x H) 245.2 x 233.2 mm (57,180.64 mm²) Si-diode array, 450 µm thickness
Head Dimensions (W x H x D) 34.0 x 37.0 x 50.0 cm
2Θ Range 20° - not currently in use
Resolution 3,110 x 3,269, 75 x 75 µm pixel size
Detector History May 2017 - May 2020: Pilatus3 S 6M
April 2010 - February 2017: Rayonix MX300 CCD
Before April 2010: Rayonix MX225 CCD

Techniques

Single crystal X-ray diffraction including:

  • Routine data collection
  • MAD, SAD, S-SAD experiments
  • XRF on crystals