Summary report for Directory: diska/2007src0260

Report generated Feb 27, 2007; 15:41:17

Unit cell

23272 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p4

a (Angstrom) 9.4250 +/- 0.0002

b (Angstrom) 9.4250 +/- 0.0002

c (Angstrom) 42.3796 +/- 0.0010

alpha (°) 90.000

beta (°) 90.000

gamma (°) 90.000

Volume (A**3) 3764.61 +/- 0.14
Mosaicity (°) 0.4130 +/- 0.0010

Symmetry used in scalepack	p4
a (Angstrom)	9.4250 +/- 0.0002
b (Angstrom)	9.4250 +/- 0.0002
c (Angstrom)	42.3796 +/- 0.0010
alpha (°)	90.000
beta (°)	90.000
gamma (°)	90.000
Volume (A**3)	3764.61 +/- 0.14
Mosaicity (°)	0.4130 +/- 0.0010

Data collection

Summary

Total number of images collected	544
Total exposure time	182.0 minutes
Data collection exposure time	180.6 minutes
Data collection wall-clock time	228.9 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	50.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	137	`137.0`° omega	1.000°	20 seconds	Yes
data collection	s02f	148	`148.0`° omega	1.000°	20 seconds	Yes
data collection	s03f	109	`109.0`° omega	1.000°	20 seconds	Yes
data collection	s04f	142	`142.0`° omega	1.000°	20 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`2985`
Zero sigma or profile test	`1651`
Overload or incomplete profile	`1212`
Sigma cutoff	`972`
Low resolution limit	`2`
High resolution limit	`121`

Final Data Set

Scale factor range	0.22-11.35
Number of 'full' reflections	`13880`
Number of 'partial' reflections	`15976`
Total number of integrated reflections	`23702`
Total number of unique reflections	`4235`
Data completeness	`92.0%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`28.0`
Average Sigma(I)	`2.1`
Overall R-merge (linear)	`0.172`

Sadabs Results

Parameter refinement on 20808 reflections reduced R(int) from 0.3473 to 0.0891

Before rejection, 32496 reflections total and 4467 unique

After rejection, 28882 reflections total and 4444 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    6.4  0.0873   1.460 - 1.852   0.897 - 1.149   1.381    7117    5872
    2   21.1  0.1956   1.300 - 2.027   0.925 - 1.261   1.423    4813    2494
    3   21.1  0.1065   0.441 - 0.552   0.925 - 1.395   1.223    7011    5080
    4   21.1  0.0920   0.478 - 0.557   0.952 - 2.197   1.294    9941    6988

Ratio of minimum to maximum apparent transmission: 0.408390

Metadata

Group Service

Operator Simon Coles

Sample Owner Davies

Local Code 306-720

Formula C15H17Cl2N4OP3

Crystal Colour Colourless

Crystal Habit Prism

Crystal Size 0.16 x 0.12 x 0.12 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Davies
Local Code	306-720
Formula	C15H17Cl2N4OP3
Crystal Colour	Colourless
Crystal Habit	Prism
Crystal Size	0.16 x 0.12 x 0.12 (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/