Summary report for Directory: diska/2006src0701

Report generated Jun 02, 2006; 14:14:41

Unit cell

3562 reflections with 1.00°<theta<27.48° (resolution between 20.40A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p1

a (Angstrom) 8.03340 +/- 0.00010

b (Angstrom) 10.0789 +/- 0.0002

c (Angstrom) 11.1829 +/- 0.0003

alpha (°) 97.4515 +/- 0.0012

beta (°) 111.0052 +/- 0.0012

gamma (°) 103.9928 +/- 0.0013

Volume (A**3) 796.46 +/- 0.03
Mosaicity (°) 0.3770 +/- 0.0010

Symmetry used in scalepack	p1
a (Angstrom)	8.03340 +/- 0.00010
b (Angstrom)	10.0789 +/- 0.0002
c (Angstrom)	11.1829 +/- 0.0003
alpha (°)	97.4515 +/- 0.0012
beta (°)	111.0052 +/- 0.0012
gamma (°)	103.9928 +/- 0.0013
Volume (A**3)	796.46 +/- 0.03
Mosaicity (°)	0.3770 +/- 0.0010

Data collection

Summary

Total number of images collected	303
Total exposure time	79.7 minutes
Data collection exposure time	79.2 minutes
Data collection wall-clock time	108.0 minutes

Experimental Conditions

Wavelength	0.71073 A

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Detector distance	Used in scaling
cell determination	i01f	10	`10.0`° phi	1.000°	3 seconds	45.00 mm	No
data collection	s01f	181	`362.0`° phi	2.000°	16 seconds	30.00 mm	Yes
data collection	s02f	17	`34.0`° omega	2.000°	16 seconds	30.00 mm	Yes
data collection	s03f	23	`46.0`° omega	2.000°	16 seconds	30.00 mm	Yes
data collection	s04f	17	`34.0`° omega	2.000°	16 seconds	30.00 mm	Yes
data collection	s05f	55	`110.0`° omega	2.000°	16 seconds	30.00 mm	Yes

Scalepack Scaling

Deleted observations

Rejected	`121`
Overload or incomplete profile	`550`
Sigma cutoff	`6`

Final Data Set

Scale factor range	9.66-11.17
Number of 'full' reflections	`12446`
Number of 'partial' reflections	`4835`
Total number of integrated reflections	`16570`
Total number of unique reflections	`3659`
Data completeness	`99.5%`
Resolution range	20.40-0.77 A
Theta range	1.00°-27.48°
Average Intensity	`182.9`
Average Sigma(I)	`4.2`
Overall R-merge (linear)	`0.027`

Sadabs Results

Parameter refinement on 13738 reflections reduced R(int) from 0.0618 to 0.0253

Before rejection, 16468 reflections total and 3657 unique

After rejection, 16286 reflections total and 3651 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0250   1.053 - 1.212   0.961 - 1.120   1.283   10291    8847
    2   -6.8  0.0248   0.441 - 0.459   0.961 - 1.073   1.167     853     745
    3   -6.8  0.0287   0.679 - 0.717   0.971 - 1.085   1.195    1204    1056
    4   -6.8  0.0215   0.931 - 0.966   0.971 - 1.036   1.203     872     751
    5   -6.8  0.0255   0.922 - 1.074   0.961 - 1.072   1.195    3066    2667

Ratio of minimum to maximum apparent transmission: 0.857974

Metadata

Group Service

Operator Simon Coles

Sample Owner Davies

Local Code 306-133-A

Formula C3H4BrCl4N4O4P3

Crystal Colour Colourless

Crystal Habit Slab

Crystal Size 0.38 x 0.2 x 0.05 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Davies
Local Code	306-133-A
Formula	C3H4BrCl4N4O4P3
Crystal Colour	Colourless
Crystal Habit	Slab
Crystal Size	0.38 x 0.2 x 0.05 (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/