Summary report for Directory: home/diska/06skc0013

Report generated Mar 18, 2006; 19:23:45

Unit cell

3149 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p2

a (Angstrom) 8.8691 +/- 0.0007

b (Angstrom) 13.2988 +/- 0.0017

c (Angstrom) 12.1250 +/- 0.0014

alpha (°) 90.000

beta (°) 109.500 +/- 0.007

gamma (°) 90.000

Volume (A**3) 1348.1 +/- 0.3
Mosaicity (°) 1.416 +/- 0.005

Symmetry used in scalepack	p2
a (Angstrom)	8.8691 +/- 0.0007
b (Angstrom)	13.2988 +/- 0.0017
c (Angstrom)	12.1250 +/- 0.0014
alpha (°)	90.000
beta (°)	109.500 +/- 0.007
gamma (°)	90.000
Volume (A**3)	1348.1 +/- 0.3
Mosaicity (°)	1.416 +/- 0.005

Data collection

Summary

Total number of images collected	258
Total exposure time	254.9 minutes
Data collection exposure time	250.9 minutes
Data collection wall-clock time	272.3 minutes

Experimental Conditions

Wavelength	0.71073 A
Cryostat setting	120.00K
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	178	`356.0`° phi	2.000°	60 seconds	Yes
data collection	s02f	29	`58.0`° omega	2.000°	60 seconds	Yes
data collection	s03f	27	`54.0`° omega	2.000°	60 seconds	Yes
data collection	s04f	16	`32.0`° omega	2.000°	60 seconds	Yes
Phi/Chi	i01f - i08f	8			30 seconds

Scalepack Scaling

Deleted observations

Rejected	`210`
Zero sigma or profile test	`49`
Overload or incomplete profile	`1070`
Sigma cutoff	`70`
High resolution limit	`31`

Final Data Set

Scale factor range	4.04-10.99
Number of 'full' reflections	`3066`
Number of 'partial' reflections	`17587`
Total number of integrated reflections	`19375`
Total number of unique reflections	`3219`
Data completeness	`99.5%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`13.7`
Average Sigma(I)	`1.6`
Overall R-merge (linear)	`0.180`

Sadabs Results

Parameter refinement on 7541 reflections reduced R(int) from 0.1230 to 0.0757

Before rejection, 18941 reflections total and 3234 unique

After rejection, 18518 reflections total and 3234 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.1514   1.014 - 1.556   0.931 - 1.239   1.384   13486    6214
    2   -4.9  0.1430   0.337 - 0.368   0.931 - 1.215   1.355    2120    1103
    3  -11.2  0.3708   1.267 - 1.697   0.944 - 1.192   1.539    1866     498
    4  -11.2  0.1695   0.292 - 0.324   0.932 - 1.205   1.366    1046     469

Ratio of minimum to maximum apparent transmission: 0.751479

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code wp5 c6

Formula C12H18O4N2

Crystal Colour Colourless

Crystal Habit Shard

Crystal Size 0.1 x 0.07 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	wp5 c6
Formula	C12H18O4N2
Crystal Colour	Colourless
Crystal Habit	Shard
Crystal Size	0.1 x 0.07 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 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    '10cm confocal mirrors'
_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/