Summary report for Directory: diska/06skc0040

Report generated Sep 01, 2006; 09:58:45

Unit cell

1224 reflections with 1.00°<theta<27.48° (resolution between 20.40A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p1

a (Angstrom) 5.749 +/- 0.003

b (Angstrom) 6.541 +/- 0.003

c (Angstrom) 9.904 +/- 0.005

alpha (°) 80.39 +/- 0.02

beta (°) 78.71 +/- 0.02

gamma (°) 71.72 +/- 0.03

Volume (A**3) 344.6 +/- 0.3
Mosaicity (°) 3.557 +/- 0.013

Symmetry used in scalepack	p1
a (Angstrom)	5.749 +/- 0.003
b (Angstrom)	6.541 +/- 0.003
c (Angstrom)	9.904 +/- 0.005
alpha (°)	80.39 +/- 0.02
beta (°)	78.71 +/- 0.02
gamma (°)	71.72 +/- 0.03
Volume (A**3)	344.6 +/- 0.3
Mosaicity (°)	3.557 +/- 0.013

Data collection

Summary

Total number of images collected	672
Total exposure time	9.3 hours
Data collection exposure time	9.2 hours
Data collection wall-clock time	10.6 hours

Experimental Conditions

Wavelength	0.71073 A

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Detector distance	Used in scaling
cell determination	i01f	10	`10.0`° phi	1.000°	30 seconds	45.00 mm	No
data collection	t01f	358	`358.0`° phi	1.000°	50 seconds	31.00 mm	Yes
data collection	t02f	34	`34.0`° omega	1.000°	50 seconds	31.00 mm	Yes
data collection	t03f	111	`111.0`° omega	1.000°	50 seconds	31.00 mm	Yes
data collection	t04f	48	`48.0`° omega	1.000°	50 seconds	31.00 mm	Yes
data collection	t05f	111	`111.0`° omega	1.000°	50 seconds	31.00 mm	Yes

Scalepack Scaling

Deleted observations

Rejected	`122`
Zero sigma or profile test	`1744`
Overload or incomplete profile	`556`
Sigma cutoff	`925`
High resolution limit	`65`

Final Data Set

Scale factor range	9.04-10.12
Number of 'full' reflections	`0`
Number of 'partial' reflections	`7622`
Total number of integrated reflections	`5705`
Total number of unique reflections	`1398`
Data completeness	`85.1%`
Resolution range	20.40-0.77 A
Theta range	1.00°-27.48°
Average Intensity	`19.4`
Average Sigma(I)	`3.3`
Overall R-merge (linear)	`0.110`

Sadabs Results

Parameter refinement on 2174 reflections reduced R(int) from 0.0972 to 0.0601

Before rejection, 6531 reflections total and 1455 unique

After rejection, 6445 reflections total and 1454 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.1481   1.131 - 1.744   0.902 - 1.499   1.146    3600    1441
    2   -7.8  0.1601   0.125 - 0.142   0.905 - 1.324   1.061     278     111
    3   -7.8  0.1429   1.226 - 1.569   0.940 - 1.482   1.134    1016     395
    4   -7.8  0.1481   0.345 - 0.387   0.905 - 1.505   1.175     434     161
    5   -7.8  0.1369   1.013 - 1.306   0.904 - 1.301   1.141    1117     452

Ratio of minimum to maximum apparent transmission: 0.599478

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code wp8 c10

Formula C7H13O5N1

Crystal Colour Colourless

Crystal Habit Block

Crystal Size 0.16 x 0.11 x 0.07 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Sam Callear
Sample Owner
Local Code	wp8 c10
Formula	C7H13O5N1
Crystal Colour	Colourless
Crystal Habit	Block
Crystal Size	0.16 x 0.11 x 0.07 (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/