Summary report for Directory: diska/04src0682

Report generated Aug 18, 2004; 13:48:12

Unit cell

10667 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) 9.9370 +/- 0.0003

b (Angstrom) 13.2341 +/- 0.0005

c (Angstrom) 19.5482 +/- 0.0007

alpha (°) 72.8293 +/- 0.0017

beta (°) 87.894 +/- 0.002

gamma (°) 84.875 +/- 0.002

Volume (A**3) 2446.19 +/- 0.15
Mosaicity (°) 0.659 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	9.9370 +/- 0.0003
b (Angstrom)	13.2341 +/- 0.0005
c (Angstrom)	19.5482 +/- 0.0007
alpha (°)	72.8293 +/- 0.0017
beta (°)	87.894 +/- 0.002
gamma (°)	84.875 +/- 0.002
Volume (A**3)	2446.19 +/- 0.15
Mosaicity (°)	0.659 +/- 0.002

Data collection

Summary

Total number of images collected	319
Total exposure time	209.8 minutes
Data collection exposure time	208.4 minutes
Data collection wall-clock time	239.9 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	33.00 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	16	`32.0`° omega	2.000°	40 seconds	Yes
data collection	s03f	58	`116.0`° omega	2.000°	40 seconds	Yes
data collection	s04f	56	`112.0`° omega	2.000°	40 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`106`
Zero sigma or profile test	`66`
Overload or incomplete profile	`1120`
Sigma cutoff	`94`
High resolution limit	`141`

Final Data Set

Scale factor range	8.15-10.66
Number of 'full' reflections	`26591`
Number of 'partial' reflections	`22730`
Total number of integrated reflections	`47274`
Total number of unique reflections	`11091`
Data completeness	`99.7%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`13.6`
Average Sigma(I)	`1.2`
Overall R-merge (linear)	`0.085`

Sadabs Results

Parameter refinement on 23833 reflections reduced R(int) from 0.0801 to 0.0454

Before rejection, 47186 reflections total and 11189 unique

After rejection, 46651 reflections total and 11185 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   10.1  0.0757   0.852 - 1.144   0.919 - 1.329   1.308   27660   15680
    2   -9.6  0.0830   0.820 - 0.905   0.956 - 1.149   1.315    2073    1063
    3   -9.6  0.0759   0.809 - 1.095   0.921 - 1.151   1.276    8654    4797
    4   -9.6  0.0803   0.810 - 1.126   0.919 - 1.179   1.322    8264    4452

Ratio of minimum to maximum apparent transmission: 0.691448

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. P. J. Murphy

Local Code MD92

Formula C52 H68 O4 Br4

Crystal Colour Colourless

Crystal Habit Plate

Crystal Size 0.38 x 0.29 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. P. J. Murphy
Local Code	MD92
Formula	C52 H68 O4 Br4
Crystal Colour	Colourless
Crystal Habit	Plate
Crystal Size	0.38 x 0.29 x 0.04 (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/