Summary report for Directory: diska/2005src1009

Report generated Aug 05, 2005; 16:18:21

Unit cell

2845 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) 5.9961 +/- 0.0002

b (Angstrom) 10.4376 +/- 0.0005

c (Angstrom) 11.9311 +/- 0.0006

alpha (°) 109.211 +/- 0.002

beta (°) 91.493 +/- 0.003

gamma (°) 106.257 +/- 0.002

Volume (A**3) 671.16 +/- 0.05
Mosaicity (°) 0.417 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	5.9961 +/- 0.0002
b (Angstrom)	10.4376 +/- 0.0005
c (Angstrom)	11.9311 +/- 0.0006
alpha (°)	109.211 +/- 0.002
beta (°)	91.493 +/- 0.003
gamma (°)	106.257 +/- 0.002
Volume (A**3)	671.16 +/- 0.05
Mosaicity (°)	0.417 +/- 0.002

Data collection

Summary

Total number of images collected	246
Total exposure time	81.2 minutes
Data collection exposure time	80.2 minutes
Data collection wall-clock time	100.2 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	30.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	91	`182.0`° phi	2.000°	20 seconds	Yes
data collection	s02f	22	`44.0`° omega	2.000°	20 seconds	Yes
data collection	s03f	23	`46.0`° omega	2.000°	20 seconds	Yes
data collection	s04f	54	`108.0`° omega	2.000°	20 seconds	Yes
data collection	s05f	48	`96.0`° omega	2.000°	20 seconds	Yes
Phi/Chi	i01f - i08f	8			7 seconds

Scalepack Scaling

Deleted observations

Rejected	`21`
Zero sigma or profile test	`2`
Overload or incomplete profile	`270`
Sigma cutoff	`7`
High resolution limit	`6`

Final Data Set

Scale factor range	8.38-10.00
Number of 'full' reflections	`8289`
Number of 'partial' reflections	`3598`
Total number of integrated reflections	`11556`
Total number of unique reflections	`3071`
Data completeness	`99.2%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`45.9`
Average Sigma(I)	`1.9`
Overall R-merge (linear)	`0.041`

Sadabs Results

Parameter refinement on 7269 reflections reduced R(int) from 0.0662 to 0.0292

Before rejection, 11195 reflections total and 3070 unique

After rejection, 11129 reflections total and 3068 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0352   1.100 - 1.281   0.940 - 1.242   1.226    4380    3049
    2   -6.8  0.0373   0.892 - 1.016   0.962 - 1.224   1.201     966     694
    3   -6.8  0.0362   0.359 - 0.386   0.940 - 1.191   1.182    1004     748
    4   -6.8  0.0386   1.283 - 1.559   0.940 - 1.224   1.189    2524    1807
    5   -6.8  0.0356   0.880 - 0.957   0.940 - 1.216   1.177    2255    1584

Ratio of minimum to maximum apparent transmission: 0.756809

Metadata

Group Service

Operator Simon Coles

Sample Owner Skabara

Local Code Dendralene1

Formula C28H18Br2N2O4S2

Crystal Colour Orange

Crystal Habit Rod

Crystal Size 0.28 x 0.1 x 0.07 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Skabara
Local Code	Dendralene1
Formula	C28H18Br2N2O4S2
Crystal Colour	Orange
Crystal Habit	Rod
Crystal Size	0.28 x 0.1 x 0.07 (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/