Summary report for Directory: diska/04skc0010

Report generated Dec 04, 2004; 10:26:00

Unit cell

2550 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) 7.2887 +/- 0.0004

b (Angstrom) 7.3630 +/- 0.0006

c (Angstrom) 11.6466 +/- 0.0010

alpha (°) 106.348 +/- 0.004

beta (°) 101.098 +/- 0.004

gamma (°) 93.796 +/- 0.004

Volume (A**3) 583.72 +/- 0.08
Mosaicity (°) 0.463 +/- 0.003

Symmetry used in scalepack	p1
a (Angstrom)	7.2887 +/- 0.0004
b (Angstrom)	7.3630 +/- 0.0006
c (Angstrom)	11.6466 +/- 0.0010
alpha (°)	106.348 +/- 0.004
beta (°)	101.098 +/- 0.004
gamma (°)	93.796 +/- 0.004
Volume (A**3)	583.72 +/- 0.08
Mosaicity (°)	0.463 +/- 0.003

Data collection

Summary

Total number of images collected	303
Total exposure time	15.8 hours
Data collection exposure time	15.6 hours
Data collection wall-clock time	16.2 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°	190 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	190 seconds	Yes
data collection	s03f	16	`32.0`° omega	2.000°	190 seconds	Yes
data collection	s04f	57	`114.0`° omega	2.000°	190 seconds	Yes
data collection	s05f	25	`50.0`° omega	2.000°	190 seconds	Yes
Phi/Chi	i01f - i08f	8			100 seconds

Scalepack Scaling

Deleted observations

Rejected	`55`
Zero sigma or profile test	`89`
Overload or incomplete profile	`246`
Sigma cutoff	`24`
High resolution limit	`26`

Final Data Set

Scale factor range	9.14-10.01
Number of 'full' reflections	`7686`
Number of 'partial' reflections	`3951`
Total number of integrated reflections	`11190`
Total number of unique reflections	`2652`
Data completeness	`99.1%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`9.3`
Average Sigma(I)	`1.0`
Overall R-merge (linear)	`0.102`

Sadabs Results

Parameter refinement on 5122 reflections reduced R(int) from 0.0661 to 0.0513

Before rejection, 11023 reflections total and 2666 unique

After rejection, 10813 reflections total and 2663 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0950   0.832 - 0.992   0.883 - 1.097   1.202    6803    3753
    2   -8.7  0.1033   0.773 - 0.808   0.960 - 1.074   1.244     520     275
    3   -8.7  0.1034   0.910 - 0.990   0.963 - 1.089   1.165     527     303
    4   -8.7  0.1005   0.909 - 1.041   0.880 - 1.065   1.160    2108    1166
    5   -8.7  0.1012   0.854 - 0.937   0.906 - 1.098   1.211     855     444

Ratio of minimum to maximum apparent transmission: 0.801835

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code TLT374A AB34

Formula C8H15O6N

Crystal Colour Colourless

Crystal Habit Plate

Crystal Size 0.01 x 0.09 x 0.08 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Sam Callear
Sample Owner
Local Code	TLT374A AB34
Formula	C8H15O6N
Crystal Colour	Colourless
Crystal Habit	Plate
Crystal Size	0.01 x 0.09 x 0.08 (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/