Summary report for Directory: home/diska/04src0845

Report generated Oct 06, 2004; 13:06:02

Unit cell

4247 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) 6.7423 +/- 0.0002

b (Angstrom) 11.8006 +/- 0.0004

c (Angstrom) 11.9563 +/- 0.0004

alpha (°) 87.720 +/- 0.002

beta (°) 86.640 +/- 0.002

gamma (°) 81.468 +/- 0.002

Volume (A**3) 938.67 +/- 0.05
Mosaicity (°) 0.716 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	6.7423 +/- 0.0002
b (Angstrom)	11.8006 +/- 0.0004
c (Angstrom)	11.9563 +/- 0.0004
alpha (°)	87.720 +/- 0.002
beta (°)	86.640 +/- 0.002
gamma (°)	81.468 +/- 0.002
Volume (A**3)	938.67 +/- 0.05
Mosaicity (°)	0.716 +/- 0.002

Data collection

Summary

Total number of images collected	354
Total exposure time	177.0 minutes
Data collection exposure time	174.3 minutes
Data collection wall-clock time	203.2 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°	30 seconds	Yes
data collection	s02f	56	`112.0`° omega	2.000°	30 seconds	Yes
data collection	s03f	55	`110.0`° omega	2.000°	30 seconds	Yes
data collection	s04f	54	`108.0`° omega	2.000°	30 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`86`
Overload or incomplete profile	`792`
Sigma cutoff	`26`
High resolution limit	`141`

Final Data Set

Scale factor range	3.96-11.65
Number of 'full' reflections	`11240`
Number of 'partial' reflections	`11124`
Total number of integrated reflections	`21407`
Total number of unique reflections	`4297`
Data completeness	`100.0%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`74.7`
Average Sigma(I)	`3.0`
Overall R-merge (linear)	`0.072`

Sadabs Results

Parameter refinement on 15867 reflections reduced R(int) from 0.2303 to 0.0531

Before rejection, 21424 reflections total and 4354 unique

After rejection, 21131 reflections total and 4354 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0657   0.589 - 2.173   0.922 - 1.204   1.409   10987    8531
    2   -8.7  0.0623   0.843 - 1.180   0.913 - 1.108   1.423    3463    2699
    3   -8.7  0.0604   0.814 - 1.541   0.920 - 1.095   1.391    3373    2568
    4   -8.7  0.0607   0.452 - 0.668   0.913 - 1.215   1.369    3308    2591

Ratio of minimum to maximum apparent transmission: 0.751461

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. I. R. Butler

Local Code Yellow 1

Formula C20 H18 N1 O2 Br1 Si1

Crystal Colour White

Crystal Habit Needle

Crystal Size 0.2 x 0.06 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. I. R. Butler
Local Code	Yellow 1
Formula	C20 H18 N1 O2 Br1 Si1
Crystal Colour	White
Crystal Habit	Needle
Crystal Size	0.2 x 0.06 x 0.02 (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/