Summary report for Directory: home/diska/2007src0079

Report generated Feb 09, 2007; 12:47:55

Unit cell

3349 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) 15.7998 +/- 0.0007

b (Angstrom) 5.17620 +/- 0.00010

c (Angstrom) 16.9784 +/- 0.0006

alpha (°) 90.000

beta (°) 99.7232 +/- 0.0017

gamma (°) 90.000

Volume (A**3) 1368.60 +/- 0.08
Mosaicity (°) 0.507 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	15.7998 +/- 0.0007
b (Angstrom)	5.17620 +/- 0.00010
c (Angstrom)	16.9784 +/- 0.0006
alpha (°)	90.000
beta (°)	99.7232 +/- 0.0017
gamma (°)	90.000
Volume (A**3)	1368.60 +/- 0.08
Mosaicity (°)	0.507 +/- 0.002

Data collection

Summary

Total number of images collected	240
Total exposure time	103.1 minutes
Data collection exposure time	101.8 minutes
Data collection wall-clock time	121.4 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	35.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	109	`218.0`° phi	2.000°	26 seconds	Yes
data collection	s02f	27	`54.0`° omega	2.000°	26 seconds	Yes
data collection	s03f	51	`102.0`° omega	2.000°	26 seconds	Yes
data collection	s04f	45	`90.0`° omega	2.000°	26 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`403`
Overload or incomplete profile	`488`
Sigma cutoff	`175`
High resolution limit	`62`

Final Data Set

Scale factor range	8.82-15.67
Number of 'full' reflections	`10799`
Number of 'partial' reflections	`6145`
Total number of integrated reflections	`16124`
Total number of unique reflections	`3475`
Data completeness	`99.7%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`55.7`
Average Sigma(I)	`1.6`
Overall R-merge (linear)	`0.063`

Sadabs Results

Parameter refinement on 12451 reflections reduced R(int) from 0.1094 to 0.0531

Before rejection, 16402 reflections total and 3504 unique

After rejection, 14519 reflections total and 3494 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0570   0.729 - 0.957   0.963 - 1.083   2.108    6895    5069
    2   14.6  0.0619   0.870 - 0.965   0.976 - 1.056   2.069    1631    1252
    3   14.6  0.0471   0.773 - 0.987   0.990 - 1.075   2.031    3172    2412
    4   14.6  0.0469   0.712 - 1.284   0.963 - 1.070   1.982    2821    2217

Ratio of minimum to maximum apparent transmission: 0.889747

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. E. McDonald

Local Code JEHD-1-133

Formula C13 H13 N1 O5 S1

Crystal Colour Colourless

Crystal Habit Needle

Crystal Size 0.41 x 0.06 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. E. McDonald
Local Code	JEHD-1-133
Formula	C13 H13 N1 O5 S1
Crystal Colour	Colourless
Crystal Habit	Needle
Crystal Size	0.41 x 0.06 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 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    '10cm confocal mirrors'
_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/