Summary report for Directory: diska/04skc0008

Report generated Sep 02, 2004; 15:44:49

Unit cell

5939 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) 7.8500 +/- 0.0003

b (Angstrom) 9.6846 +/- 0.0004

c (Angstrom) 17.9489 +/- 0.0006

alpha (°) 101.644 +/- 0.003

beta (°) 93.991 +/- 0.003

gamma (°) 92.7917 +/- 0.0018

Volume (A**3) 1330.48 +/- 0.09
Mosaicity (°) 0.878 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	7.8500 +/- 0.0003
b (Angstrom)	9.6846 +/- 0.0004
c (Angstrom)	17.9489 +/- 0.0006
alpha (°)	101.644 +/- 0.003
beta (°)	93.991 +/- 0.003
gamma (°)	92.7917 +/- 0.0018
Volume (A**3)	1330.48 +/- 0.09
Mosaicity (°)	0.878 +/- 0.002

Data collection

Summary

Total number of images collected	343
Total exposure time	227.2 minutes
Data collection exposure time	224.5 minutes
Data collection wall-clock time	256.8 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°	40 seconds	Yes
data collection	s02f	17	`34.0`° omega	2.000°	40 seconds	Yes
data collection	s03f	57	`114.0`° omega	2.000°	40 seconds	Yes
data collection	s04f	25	`50.0`° omega	2.000°	40 seconds	Yes
data collection	s05f	55	`110.0`° omega	2.000°	40 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`123`
Zero sigma or profile test	`6`
Overload or incomplete profile	`792`
Sigma cutoff	`15`
High resolution limit	`3`

Final Data Set

Scale factor range	9.47-10.73
Number of 'full' reflections	`12244`
Number of 'partial' reflections	`17958`
Total number of integrated reflections	`28352`
Total number of unique reflections	`6103`
Data completeness	`98.5%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`28.1`
Average Sigma(I)	`1.5`
Overall R-merge (linear)	`0.062`

Sadabs Results

Parameter refinement on 20403 reflections reduced R(int) from 0.0735 to 0.0522

Before rejection, 28660 reflections total and 6120 unique

After rejection, 28360 reflections total and 6118 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0592   0.852 - 1.067   0.896 - 1.207   1.283   15716   12015
    2   -8.7  0.0613   0.547 - 0.581   0.897 - 1.125   1.307    1245     948
    3   -8.7  0.0712   0.863 - 0.966   0.941 - 1.094   1.230    4796    3586
    4   -8.7  0.0624   0.902 - 0.980   0.968 - 1.107   1.324    1966    1486
    5   -8.7  0.0613   0.871 - 0.991   0.896 - 1.105   1.230    4637    3504

Ratio of minimum to maximum apparent transmission: 0.741865

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code TLT374C EF34

Formula C12H26O6N1Br1

Crystal Colour Colourless

Crystal Habit Block

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	TLT374C EF34
Formula	C12H26O6N1Br1
Crystal Colour	Colourless
Crystal Habit	Block
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    '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/