Summary report for Directory: diska/2010src0401

Report generated May 21, 2010; 14:16:37

Unit cell

35554 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) 7.3738 +/- 0.0004

b (Angstrom) 24.541 +/- 0.002

c (Angstrom) 21.2954 +/- 0.0016

alpha (°) 90.000

beta (°) 97.475 +/- 0.004

gamma (°) 90.000

Volume (A**3) 3820.8 +/- 0.5
Mosaicity (°) 1.198 +/- 0.003

Symmetry used in scalepack	p2
a (Angstrom)	7.3738 +/- 0.0004
b (Angstrom)	24.541 +/- 0.002
c (Angstrom)	21.2954 +/- 0.0016
alpha (°)	90.000
beta (°)	97.475 +/- 0.004
gamma (°)	90.000
Volume (A**3)	3820.8 +/- 0.5
Mosaicity (°)	1.198 +/- 0.003

Data collection

Summary

Total number of images collected	235
Total exposure time	268.8 minutes
Data collection exposure time	266.0 minutes
Data collection wall-clock time	286.8 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	39.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	126	`252.0`° phi	2.000°	70 seconds	Yes
data collection	s02f	13	`26.0`° omega	2.000°	70 seconds	Yes
data collection	s03f	31	`62.0`° omega	2.000°	70 seconds	Yes
data collection	s04f	57	`114.0`° omega	2.000°	70 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`7`
Zero sigma or profile test	`28`
Overload or incomplete profile	`1012`
Sigma cutoff	`1310`
Low resolution limit	`11`
High resolution limit	`137`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`9092`
Number of 'partial' reflections	`24803`
Total number of integrated reflections	`23739`
Total number of unique reflections	`7822`
Data completeness	`87.2%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`18.5`
Average Sigma(I)	`2.3`
Overall R-merge (linear)	`0.209`

Sadabs Results

Parameter refinement on 15881 reflections reduced R(int) from 0.1358 to 0.0778

Before rejection, 32228 reflections total and 8691 unique

After rejection, 27069 reflections total and 8534 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.2  0.1352   0.834 - 1.096   0.960 - 1.154   2.124   15978    7654
    2   17.6  0.1056   0.414 - 0.456   0.956 - 1.190   2.166     853     484
    3   17.6  0.1068   0.417 - 0.512   0.952 - 1.113   2.085    3314    1663
    4   17.6  0.1282   0.954 - 1.544   0.956 - 1.341   2.068    6924    3278

Ratio of minimum to maximum apparent transmission: 0.710015

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr J Spencer

Local Code JA61

Formula C18 H16 N2 O3 S Fe

Crystal Colour Orange

Crystal Habit Needle

Crystal Size 0.26 x 0.02 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr J Spencer
Local Code	JA61
Formula	C18 H16 N2 O3 S Fe
Crystal Colour	Orange
Crystal Habit	Needle
Crystal Size	0.26 x 0.02 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/