Summary report for Directory: home/diska/07skc0027

Report generated May 09, 2007; 09:30:54

Unit cell

1011 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p222

a (Angstrom) 3.9532 +/- 0.0005

b (Angstrom) 11.497 +/- 0.002

c (Angstrom) 18.703 +/- 0.003

alpha (°) 90.000

beta (°) 90.000

gamma (°) 90.000

Volume (A**3) 850.0 +/- 0.2
Mosaicity (°) 1.959 +/- 0.007

Symmetry used in scalepack	p222
a (Angstrom)	3.9532 +/- 0.0005
b (Angstrom)	11.497 +/- 0.002
c (Angstrom)	18.703 +/- 0.003
alpha (°)	90.000
beta (°)	90.000
gamma (°)	90.000
Volume (A**3)	850.0 +/- 0.2
Mosaicity (°)	1.959 +/- 0.007

Data collection

Summary

Total number of images collected	164
Total exposure time	127.7 minutes
Data collection exposure time	124.3 minutes
Data collection wall-clock time	137.1 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	33.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	72	`136.8`° phi	1.900°	47 seconds	Yes
data collection	s02f	34	`64.6`° omega	1.900°	47 seconds	Yes
data collection	s03f	50	`95.0`° omega	1.900°	47 seconds	Yes
Phi/Chi	i01f - i08f	8			25 seconds

Scalepack Scaling

Deleted observations

Rejected	`103`
Overload or incomplete profile	`304`
Sigma cutoff	`264`
High resolution limit	`50`

Final Data Set

Scale factor range	10.00-12.73
Number of 'full' reflections	`0`
Number of 'partial' reflections	`6644`
Total number of integrated reflections	`4908`
Total number of unique reflections	`1139`
Data completeness	`94.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`47.9`
Average Sigma(I)	`2.7`
Overall R-merge (linear)	`0.095`

Sadabs Results

Parameter refinement on 4323 reflections reduced R(int) from 0.1359 to 0.0616

Before rejection, 6617 reflections total and 1209 unique

After rejection, 5732 reflections total and 1204 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   13.5  0.0824   0.760 - 1.142   0.907 - 1.308   2.064    2693    1761
    2   12.9  0.0748   0.770 - 0.936   0.876 - 1.298   2.093    1223     699
    3   12.9  0.0772   0.771 - 0.883   0.912 - 1.315   2.124    1816    1108

Ratio of minimum to maximum apparent transmission: 0.666268

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code 2Meimdz MalA WU

Formula C7H10O4N2

Crystal Colour Colourless

Crystal Habit Lath

Crystal Size 0.19 x 0.04 x 0.01 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Sam Callear
Sample Owner
Local Code	2Meimdz MalA WU
Formula	C7H10O4N2
Crystal Colour	Colourless
Crystal Habit	Lath
Crystal Size	0.19 x 0.04 x 0.01 (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 2007/2 (Sheldrick, G.M., 2007)'

_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    '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/