Summary report for Directory: diska/04skc0005

Report generated Aug 27, 2004; 09:39:14

Unit cell

4219 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) 7.5009 +/- 0.0002

b (Angstrom) 7.7284 +/- 0.0002

c (Angstrom) 16.3428 +/- 0.0005

alpha (°) 88.2929 +/- 0.0018

beta (°) 86.3862 +/- 0.0014

gamma (°) 89.7975 +/- 0.0016

Volume (A**3) 945.09 +/- 0.05
Mosaicity (°) 0.344 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	7.5009 +/- 0.0002
b (Angstrom)	7.7284 +/- 0.0002
c (Angstrom)	16.3428 +/- 0.0005
alpha (°)	88.2929 +/- 0.0018
beta (°)	86.3862 +/- 0.0014
gamma (°)	89.7975 +/- 0.0016
Volume (A**3)	945.09 +/- 0.05
Mosaicity (°)	0.344 +/- 0.002

Data collection

Summary

Total number of images collected	344
Total exposure time	5.7 hours
Data collection exposure time	5.6 hours
Data collection wall-clock time	6.2 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	32.00 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°	60 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	60 seconds	Yes
data collection	s03f	57	`114.0`° omega	2.000°	60 seconds	Yes
data collection	s04f	25	`50.0`° omega	2.000°	60 seconds	Yes
data collection	s05f	57	`114.0`° omega	2.000°	60 seconds	Yes
Phi/Chi	i01f - i08f	8			25 seconds

Scalepack Scaling

Deleted observations

Rejected	`76`
Overload or incomplete profile	`488`
Sigma cutoff	`11`
High resolution limit	`9`

Final Data Set

Scale factor range	9.93-10.50
Number of 'full' reflections	`16052`
Number of 'partial' reflections	`5406`
Total number of integrated reflections	`20862`
Total number of unique reflections	`4308`
Data completeness	`99.6%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`21.4`
Average Sigma(I)	`1.1`
Overall R-merge (linear)	`0.051`

Sadabs Results

Parameter refinement on 15719 reflections reduced R(int) from 0.0554 to 0.0415

Before rejection, 20587 reflections total and 4317 unique

After rejection, 20420 reflections total and 4315 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0494   0.909 - 1.007   0.960 - 1.120   1.149   11199    9343
    2   -8.7  0.0442   0.633 - 0.672   0.987 - 1.112   1.084     877     733
    3   -8.7  0.0532   0.922 - 0.997   0.960 - 1.104   1.167    3432    2816
    4   -8.7  0.0520   0.905 - 0.959   0.962 - 1.090   1.114    1457    1217
    5   -8.7  0.0505   0.945 - 1.032   0.961 - 1.107   1.117    3455    2873

Ratio of minimum to maximum apparent transmission: 0.857154

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code TLT374B CD910

Formula C9H18O6N2

Crystal Colour Colourless

Crystal Habit Fragment

Crystal Size 0.1 x 0.08 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Sam Callear
Sample Owner
Local Code	TLT374B CD910
Formula	C9H18O6N2
Crystal Colour	Colourless
Crystal Habit	Fragment
Crystal Size	0.1 x 0.08 x 0.04 (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/