Summary report for Directory: home/diska/06skc0002

Report generated Jan 28, 2006; 16:29:20

Unit cell

7364 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) 8.7148 +/- 0.0003

b (Angstrom) 11.4826 +/- 0.0003

c (Angstrom) 16.9691 +/- 0.0005

alpha (°) 81.721 +/- 0.002

beta (°) 81.8140 +/- 0.0018

gamma (°) 77.9870 +/- 0.0017

Volume (A**3) 1632.45 +/- 0.09
Mosaicity (°) 0.592 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	8.7148 +/- 0.0003
b (Angstrom)	11.4826 +/- 0.0003
c (Angstrom)	16.9691 +/- 0.0005
alpha (°)	81.721 +/- 0.002
beta (°)	81.8140 +/- 0.0018
gamma (°)	77.9870 +/- 0.0017
Volume (A**3)	1632.45 +/- 0.09
Mosaicity (°)	0.592 +/- 0.002

Data collection

Summary

Total number of images collected	332
Total exposure time	110.5 minutes
Data collection exposure time	109.2 minutes
Data collection wall-clock time	135.1 minutes

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°	20 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	20 seconds	Yes
data collection	s03f	16	`32.0`° omega	2.000°	20 seconds	Yes
data collection	s04f	55	`110.0`° omega	2.000°	20 seconds	Yes
data collection	s05f	56	`112.0`° omega	2.000°	20 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`165`
Zero sigma or profile test	`1`
Overload or incomplete profile	`978`
Sigma cutoff	`24`
High resolution limit	`66`

Final Data Set

Scale factor range	9.75-15.77
Number of 'full' reflections	`20950`
Number of 'partial' reflections	`15422`
Total number of integrated reflections	`35180`
Total number of unique reflections	`7466`
Data completeness	`99.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`27.9`
Average Sigma(I)	`1.3`
Overall R-merge (linear)	`0.072`

Sadabs Results

Parameter refinement on 19643 reflections reduced R(int) from 0.1167 to 0.0527

Before rejection, 34560 reflections total and 7505 unique

After rejection, 34105 reflections total and 7504 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0709   1.086 - 1.544   0.947 - 1.183   1.323   19197   11551
    2   -8.7  0.0648   0.580 - 0.650   0.947 - 1.134   1.300    1506     955
    3   -8.7  0.0634   0.586 - 0.618   0.971 - 1.143   1.325    1527     978
    4   -8.7  0.0635   0.602 - 0.674   0.957 - 1.194   1.278    5897    3755
    5   -8.7  0.0591   0.610 - 0.703   0.947 - 1.149   1.265    5978    3858

Ratio of minimum to maximum apparent transmission: 0.792986

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code wp5 a6

Formula

Crystal Colour Colourless

Crystal Habit Fragment

Crystal Size 0.1 x 0.1 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	wp5 a6
Formula
Crystal Colour	Colourless
Crystal Habit	Fragment
Crystal Size	0.1 x 0.1 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    '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/