Summary report for Directory: home/diska/2005sjc0007

Report generated Apr 03, 2005; 12:57:38

Unit cell

1662 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p222

a (Angstrom) 8.8265 +/- 0.0002

b (Angstrom) 10.6191 +/- 0.0003

c (Angstrom) 13.4494 +/- 0.0004

alpha (°) 90.000

beta (°) 90.000

gamma (°) 90.000

Volume (A**3) 1260.61 +/- 0.06
Mosaicity (°) 0.563 +/- 0.002

Symmetry used in scalepack	p222
a (Angstrom)	8.8265 +/- 0.0002
b (Angstrom)	10.6191 +/- 0.0003
c (Angstrom)	13.4494 +/- 0.0004
alpha (°)	90.000
beta (°)	90.000
gamma (°)	90.000
Volume (A**3)	1260.61 +/- 0.06
Mosaicity (°)	0.563 +/- 0.002

Data collection

Summary

Total number of images collected	198
Total exposure time	39.4 minutes
Data collection exposure time	38.7 minutes
Data collection wall-clock time	54.5 minutes

Experimental Conditions

Wavelength	0.71073 A
Cryostat setting	274.00K
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	93	`186.0`° phi	2.000°	12 seconds	Yes
data collection	s02f	23	`46.0`° omega	2.000°	12 seconds	Yes
data collection	s03f	23	`46.0`° omega	2.000°	12 seconds	Yes
data collection	s04f	51	`102.0`° omega	2.000°	12 seconds	Yes
Phi/Chi	i01f - i08f	8			5 seconds

Scalepack Scaling

Deleted observations

Rejected	`117`
Overload or incomplete profile	`790`
Sigma cutoff	`8`
High resolution limit	`5`

Final Data Set

Scale factor range	9.48-14.00
Number of 'full' reflections	`10662`
Number of 'partial' reflections	`7430`
Total number of integrated reflections	`17278`
Total number of unique reflections	`1675`
Data completeness	`99.6%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`209.1`
Average Sigma(I)	`3.5`
Overall R-merge (linear)	`0.044`

Sadabs Results

Parameter refinement on 14108 reflections reduced R(int) from 0.1738 to 0.0421

Before rejection, 16747 reflections total and 1683 unique

After rejection, 16478 reflections total and 1682 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0378   0.957 - 1.098   0.939 - 1.132   1.449    8087    6934
    2   -6.8  0.0582   0.676 - 0.813   0.973 - 1.250   1.419    1909    1598
    3   -6.8  0.0583   0.724 - 0.885   0.914 - 1.205   1.400    1904    1569
    4    3.8  0.0383   0.685 - 1.096   0.914 - 1.250   1.397    4578    3993

Ratio of minimum to maximum apparent transmission: 0.730644

Metadata

Group Personal

Operator Simon Coles

Sample Owner SJC

Local Code 2005sjc0007

Formula C5H10Cl4N4P3

Crystal Colour Colourless

Crystal Habit Rod

Crystal Size 0.45 x 0.12 x 0.1 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Personal
Operator	Simon Coles
Sample Owner	SJC
Local Code	2005sjc0007
Formula	C5H10Cl4N4P3
Crystal Colour	Colourless
Crystal Habit	Rod
Crystal Size	0.45 x 0.12 x 0.1 (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/