Summary report for Directory: home/diska/2007src0927

Report generated Jul 20, 2007; 14:49:56

Unit cell

57249 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p2

a (Angstrom) 9.68270 +/- 0.00010

b (Angstrom) 22.3776 +/- 0.0002

c (Angstrom) 16.0124 +/- 0.0002

alpha (°) 90.000

beta (°) 91.8463 +/- 0.0006

gamma (°) 90.000

Volume (A**3) 3467.69 +/- 0.06
Mosaicity (°) 0.5550 +/- 0.0010

Symmetry used in scalepack	p2
a (Angstrom)	9.68270 +/- 0.00010
b (Angstrom)	22.3776 +/- 0.0002
c (Angstrom)	16.0124 +/- 0.0002
alpha (°)	90.000
beta (°)	91.8463 +/- 0.0006
gamma (°)	90.000
Volume (A**3)	3467.69 +/- 0.06
Mosaicity (°)	0.5550 +/- 0.0010

Data collection

Summary

Total number of images collected	442
Total exposure time	61.3 minutes
Data collection exposure time	60.2 minutes
Data collection wall-clock time	78.2 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	35.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	214	`214.0`° phi	1.000°	8 seconds	Yes
data collection	s02f	111	`111.0`° omega	1.000°	8 seconds	Yes
data collection	s03f	109	`109.0`° omega	1.000°	8 seconds	Yes
Phi/Chi	i01f - i08f	8			8 seconds

Scalepack Scaling

Deleted observations

Rejected	`7`
Zero sigma or profile test	`8`
Overload or incomplete profile	`1592`
Sigma cutoff	`116`
High resolution limit	`6`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`11239`
Number of 'partial' reflections	`27992`
Total number of integrated reflections	`36460`
Total number of unique reflections	`8161`
Data completeness	`99.9%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`284.7`
Average Sigma(I)	`5.5`
Overall R-merge (linear)	`0.116`

Sadabs Results

Parameter refinement on 36118 reflections reduced R(int) from 0.1330 to 0.0386

Before rejection, 37662 reflections total and 8168 unique

After rejection, 35250 reflections total and 8160 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0374   0.858 - 1.057   0.967 - 1.081   2.735   17975   17109
    2   14.6  0.0344   0.795 - 1.432   0.968 - 1.045   2.585    7911    7545
    3   14.6  0.0324   0.627 - 1.012   0.967 - 1.061   2.548    9364    8971

Ratio of minimum to maximum apparent transmission: 0.894089

Metadata

Group Service

Operator Simon Coles

Sample Owner Davies

Local Code 307-475-A

Formula C10H15Cl3N5OP3

Crystal Colour Colourless

Crystal Habit Prism

Crystal Size 0.2 x 0.06 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Davies
Local Code	307-475-A
Formula	C10H15Cl3N5OP3
Crystal Colour	Colourless
Crystal Habit	Prism
Crystal Size	0.2 x 0.06 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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/