Summary report for Directory: diska/2009src0345r

Report generated Apr 07, 2009; 12:55:25

Unit cell

55702 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) 23.3867 +/- 0.0014

b (Angstrom) 6.8700 +/- 0.0003

c (Angstrom) 24.3510 +/- 0.0015

alpha (°) 90.000

beta (°) 89.943 +/- 0.003

gamma (°) 90.000

Volume (A**3) 3912.4 +/- 0.4
Mosaicity (°) 1.288 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	23.3867 +/- 0.0014
b (Angstrom)	6.8700 +/- 0.0003
c (Angstrom)	24.3510 +/- 0.0015
alpha (°)	90.000
beta (°)	89.943 +/- 0.003
gamma (°)	90.000
Volume (A**3)	3912.4 +/- 0.4
Mosaicity (°)	1.288 +/- 0.002

Data collection

Summary

Total number of images collected	361
Total exposure time	95.0 minutes
Data collection exposure time	93.7 minutes
Data collection wall-clock time	110.7 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	40.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	196	`254.8`° phi	1.300°	15 seconds	Yes
data collection	s02f	65	`84.5`° omega	1.300°	15 seconds	Yes
data collection	s03f	92	`119.6`° omega	1.300°	15 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`4`
Zero sigma or profile test	`57`
Overload or incomplete profile	`1664`
Sigma cutoff	`858`
High resolution limit	`229`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`27`
Number of 'partial' reflections	`30478`
Total number of integrated reflections	`17423`
Total number of unique reflections	`7199`
Data completeness	`74.6%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`37.7`
Average Sigma(I)	`2.5`
Overall R-merge (linear)	`0.101`

Sadabs Results

Parameter refinement on 19912 reflections reduced R(int) from 0.3194 to 0.0744

Before rejection, 30995 reflections total and 9330 unique

After rejection, 25679 reflections total and 9169 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.8  0.0747   0.670 - 1.037   0.922 - 1.298   2.056   14254    9306
    2   18.3  0.0751   0.638 - 0.780   0.916 - 1.185   2.065    5271    3176
    3   18.3  0.0691   0.660 - 0.817   0.965 - 1.365   2.039    6154    4212

Ratio of minimum to maximum apparent transmission: 0.671606

Metadata

Group Service

Operator Sam Callear

Sample Owner Prof P.Taylor

Local Code SM 114bis

Formula C15H17ClN4O6Si

Crystal Colour Colourless

Crystal Habit Block

Crystal Size 0.17 x 0.12 x 0.05 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Sam Callear
Sample Owner	Prof P.Taylor
Local Code	SM 114bis
Formula	C15H17ClN4O6Si
Crystal Colour	Colourless
Crystal Habit	Block
Crystal Size	0.17 x 0.12 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 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/