EPSRC
National Crystallography Service |
Data Collection Summary kccd1
(dellboy) |
Summary report for Directory: diska/2007src0256
Report generated Feb 23, 2007; 15:12:31
Unit cell
56688 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement
Symmetry used in scalepack | p1 |
a (Angstrom) | 9.5626 +/- 0.0004 |
b (Angstrom) | 10.5996 +/- 0.0006 |
c (Angstrom) | 19.5666 +/- 0.0011 |
alpha (°) | 91.038 +/- 0.003 |
beta (°) | 90.726 +/- 0.003 |
gamma (°) | 90.039 +/- 0.004 |
Volume (A**3) | 1982.78 +/- 0.18 |
---|
Mosaicity (°) | 1.772 +/- 0.003 |
Data collection
Summary
Total number of images collected | 356 |
Total exposure time | 71.5 minutes |
Data collection exposure time | 70.8 minutes |
Data collection wall-clock time | 99.9 minutes |
Experimental Conditions
Wavelength | 0.71073 A |
Crystal to detector distance | 35.00 mm |
Scans
Type | Name | # images | Total Rotation | Per frame Rotation | Exposure per frame | Used in scaling |
data collection | s01f | 181 | 362.0° phi | 2.000° | 12 seconds | Yes |
data collection | s02f | 17 | 34.0° omega | 2.000° | 12 seconds | Yes |
data collection | s03f | 26 | 52.0° omega | 2.000° | 12 seconds | Yes |
data collection | s04f | 28 | 56.0° omega | 2.000° | 12 seconds | Yes |
data collection | s05f | 36 | 72.0° omega | 2.000° | 12 seconds | Yes |
data collection | s06f | 60 | 120.0° omega | 2.000° | 12 seconds | Yes |
Phi/Chi | i01f - i08f | 8 | | | 5 seconds |
Scalepack Scaling
Deleted observations
Rejected | 595 |
Zero sigma or profile test | 7 |
Overload or incomplete profile | 1568 |
Sigma cutoff | 122 |
High resolution limit | 61 |
Final Data Set
Scale factor range | 9.72-12.95 |
Number of 'full' reflections | 1180 |
Number of 'partial' reflections | 32160 |
Total number of integrated reflections | 21620 |
Total number of unique reflections | 6936 |
Data completeness | 75.6% |
Resolution range | 7.00-0.77 A |
Theta range | 2.91°-27.48° |
Average Intensity | 107.8 |
Average Sigma(I) | 4.5 |
Overall R-merge (linear) | 0.050 |
Sadabs Results
Parameter refinement on 23146 reflections reduced R(int) from 0.1138 to 0.0612
Before rejection, 33733 reflections total and 8691 unique
After rejection, 32022 reflections total and 8655 unique
Runs
Run 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I)
1 11.8 0.0594 0.830 - 1.027 0.926 - 1.342 1.365 17419 12615
2 11.2 0.0765 0.631 - 0.734 0.973 - 1.220 1.444 1320 1004
3 9.5 0.0795 0.819 - 0.945 0.958 - 1.213 1.471 2202 1653
4 11.2 0.0680 0.578 - 0.741 0.927 - 1.048 1.502 2386 1682
5 11.2 0.0547 0.850 - 1.120 0.927 - 1.176 1.417 3092 2418
6 11.2 0.0605 0.771 - 0.961 0.951 - 1.130 1.475 5603 4170
Ratio of minimum to maximum apparent transmission: 0.690349
Metadata
Group | Service |
Operator | Simon Coles |
Sample Owner | Davies |
Local Code | 306-721-2 |
Formula | C18H24N5O2P3 |
Crystal Colour | Colourless |
Crystal Habit | Slab |
Crystal Size | 0.4 x 0.2 x 0.2 (mm3) |
Temperature | 120(K) |
Generator | 50 (kV) 85 (mA) |
Primary Solvent | |
Other Solvents | |
File Explanations
SampleCode.zip
SampleCode.hkl
- data corrected using SADABS
SampleCode_merge_none.hkl
- equivalents and friedels kept separate (See "Final Data
Set" table in this report)
SampleCode.p4p
- skeleton p4p file for use with XPREP
SampleCode.htm
- this summary file
Southampton CIF entry fields
_exptl_absorpt_process_details 'SADABS V2.10
(Sheldrick, G.M.,
2003)'
_diffrn_ambient_temperature
120(2)
_diffrn_radiation_wavelength
0.71073
_diffrn_radiation_type
MoK\a
_diffrn_radiation_source
'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD
camera on \k-goniostat'
_diffrn_measurement_method
'\f & \w scans'
_diffrn_detector_area_resol_mean 9.091
_computing_data_collection
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W.,
1998)'
Software References
Unit Cell Determination using DirAx:
Duisenberg AJM. Indexing in Single-Crystal Diffractometry with an
Obstinate List of Reflections. Journal
of Applied Crystallography 1992; 25: 92-96.
Duisenberg AJM, Hooft RWW, Schreurs AMM, Kroon J. Accurate cells from
area-detector images. Journal of
Applied Crystallography 2000; 33:
893-898.
Diffractometer control and strategy
calculation using COLLECT:
Hooft RWW.
COLLECT data collection software, Nonius B.V., 1998.
Standard
Data Reduction using HKL(Denzo
& Scalepack):
Otwinowski Z, Minor W.
Processing of X-ray diffraction data collected in oscillation mode. Macromolecular Crystallography, Pt
A. 1997; 276: 307-326.
Absorption Correction
Sheldrick, G. M. (2003). SADABS. Version 2.10. Bruker AXS Inc., Madison,
Wisconsin, USA.
Non-Standard Data Reduction using
EvalCCD:
Duisenberg AJM, Kroon-Batenburg LMJ, Schreurs AMM. An intensity
evaluation method: EVAL-14. Journal
of Applied Crystallography 2003; 36: 220-229.
For more information visit the service web site at: http://www.soton.ac.uk/~xservice/