Summary report for Directory: diska/2008src1017

Report generated Oct 03, 2008; 18:00:25

Unit cell

48165 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p1

a (Angstrom) 10.6069 +/- 0.0012

b (Angstrom) 10.7107 +/- 0.0013

c (Angstrom) 10.7782 +/- 0.0015

alpha (°) 83.058 +/- 0.007

beta (°) 64.192 +/- 0.006

gamma (°) 88.751 +/- 0.009

Volume (A**3) 1093.6 +/- 0.2
Mosaicity (°) 2.564 +/- 0.006

Symmetry used in scalepack	p1
a (Angstrom)	10.6069 +/- 0.0012
b (Angstrom)	10.7107 +/- 0.0013
c (Angstrom)	10.7782 +/- 0.0015
alpha (°)	83.058 +/- 0.007
beta (°)	64.192 +/- 0.006
gamma (°)	88.751 +/- 0.009
Volume (A**3)	1093.6 +/- 0.2
Mosaicity (°)	2.564 +/- 0.006

Data collection

Summary

Total number of images collected	330
Total exposure time	131.9 minutes
Data collection exposure time	130.5 minutes
Data collection wall-clock time	148.1 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	32.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	181	`362.0`° phi	2.000°	24 seconds	Yes
data collection	s02f	13	`26.0`° omega	2.000°	24 seconds	Yes
data collection	s03f	25	`50.0`° omega	2.000°	24 seconds	Yes
data collection	s04f	53	`106.0`° omega	2.000°	24 seconds	Yes
data collection	s05f	50	`100.0`° omega	2.000°	24 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`4`
Zero sigma or profile test	`306`
Overload or incomplete profile	`1016`
Sigma cutoff	`1118`
High resolution limit	`381`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`0`
Number of 'partial' reflections	`20315`
Total number of integrated reflections	`15920`
Total number of unique reflections	`4799`
Data completeness	`97.1%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`17.1`
Average Sigma(I)	`1.8`
Overall R-merge (linear)	`0.413`

Sadabs Results

Parameter refinement on 10413 reflections reduced R(int) from 0.3055 to 0.1000

Before rejection, 19367 reflections total and 5008 unique

After rejection, 15729 reflections total and 4937 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   12.6  0.1054   0.507 - 1.296   0.911 - 1.423   1.914    9322    5604
    2   12.0  0.1767   0.381 - 0.447   0.913 - 1.228   2.257     506     236
    3   12.0  0.3632   0.361 - 0.545   1.007 - 1.332   2.322     967     243
    4   12.0  0.3386   0.692 - 1.305   0.911 - 1.493   2.346    2478     733
    5   12.0  0.1292   0.478 - 0.693   0.947 - 1.374   2.047    2456    1323

Ratio of minimum to maximum apparent transmission: 0.609985

Metadata

Group Service

Operator Richard Stephenson

Sample Owner Prof P.G Taylor

Local Code SM 51L

Formula C10H22N2O2Si2

Crystal Colour Colourless

Crystal Habit Fragment

Crystal Size 0.14 x 0.08 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Richard Stephenson
Sample Owner	Prof P.G Taylor
Local Code	SM 51L
Formula	C10H22N2O2Si2
Crystal Colour	Colourless
Crystal Habit	Fragment
Crystal Size	0.14 x 0.08 x 0.02 (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/