Summary report for Directory: diska/2009src0671

Report generated Jul 10, 2009; 14:32:50

Unit cell

9591 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack c2

a (Angstrom) 18.9488 +/- 0.0006

b (Angstrom) 5.60240 +/- 0.00010

c (Angstrom) 20.7934 +/- 0.0006

alpha (°) 90.000

beta (°) 90.3551 +/- 0.0016

gamma (°) 90.000

Volume (A**3) 2207.36 +/- 0.10
Mosaicity (°) 0.450 +/- 0.002

Symmetry used in scalepack	c2
a (Angstrom)	18.9488 +/- 0.0006
b (Angstrom)	5.60240 +/- 0.00010
c (Angstrom)	20.7934 +/- 0.0006
alpha (°)	90.000
beta (°)	90.3551 +/- 0.0016
gamma (°)	90.000
Volume (A**3)	2207.36 +/- 0.10
Mosaicity (°)	0.450 +/- 0.002

Data collection

Summary

Total number of images collected	258
Total exposure time	136.0 minutes
Data collection exposure time	134.7 minutes
Data collection wall-clock time	150.6 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	33.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	123	`196.8`° phi	1.600°	32 seconds	Yes
data collection	s02f	67	`107.2`° omega	1.600°	32 seconds	Yes
data collection	s03f	60	`96.0`° omega	1.600°	32 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test	`3`
Overload or incomplete profile	`314`
Sigma cutoff	`91`
Low resolution limit	`8`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`7821`
Number of 'partial' reflections	`5062`
Total number of integrated reflections	`12385`
Total number of unique reflections	`2791`
Data completeness	`99.1%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`53.1`
Average Sigma(I)	`1.8`
Overall R-merge (linear)	`0.144`

Sadabs Results

Parameter refinement on 10284 reflections reduced R(int) from 0.0982 to 0.0604

Before rejection, 12322 reflections total and 2794 unique

After rejection, 10903 reflections total and 2776 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   13.5  0.0665   0.811 - 1.057   0.980 - 1.155   2.147    5290    4279
    2   12.9  0.0567   0.719 - 0.987   0.973 - 1.107   2.089    2983    2514
    3   12.9  0.0516   0.714 - 1.068   0.968 - 1.144   2.041    2630    2239

Ratio of minimum to maximum apparent transmission: 0.838230

Metadata

Group Service

Operator Graham Tizzard

Sample Owner Dr AK Croft

Local Code AGSBn

Formula C21H26O9S

Crystal Colour Colourless

Crystal Habit Rod

Crystal Size 0.02 x 0.02 x 0.15 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Graham Tizzard
Sample Owner	Dr AK Croft
Local Code	AGSBn
Formula	C21H26O9S
Crystal Colour	Colourless
Crystal Habit	Rod
Crystal Size	0.02 x 0.02 x 0.15 (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/