Summary report for Directory: diska/04src0544

Report generated Jul 09, 2004; 08:26:02

Unit cell

5568 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) 13.7375 +/- 0.0003

b (Angstrom) 12.3538 +/- 0.0003

c (Angstrom) 13.8158 +/- 0.0003

alpha (°) 90.000

beta (°) 90.2174 +/- 0.0012

gamma (°) 90.000

Volume (A**3) 2344.67 +/- 0.09
Mosaicity (°) 0.4120 +/- 0.0010

Symmetry used in scalepack	p2
a (Angstrom)	13.7375 +/- 0.0003
b (Angstrom)	12.3538 +/- 0.0003
c (Angstrom)	13.8158 +/- 0.0003
alpha (°)	90.000
beta (°)	90.2174 +/- 0.0012
gamma (°)	90.000
Volume (A**3)	2344.67 +/- 0.09
Mosaicity (°)	0.4120 +/- 0.0010

Data collection

Summary

Total number of images collected	338
Total exposure time	13.9 hours
Data collection exposure time	13.8 hours
Data collection wall-clock time	14.6 hours

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	181	`271.5`° phi	1.500°	150 seconds	Yes
data collection	s02f	22	`33.0`° omega	1.500°	150 seconds	Yes
data collection	s03f	80	`120.0`° omega	1.500°	150 seconds	Yes
data collection	s04f	47	`70.5`° omega	1.500°	150 seconds	Yes
Phi/Chi	i01f - i08f	8			40 seconds

Scalepack Scaling

Deleted observations

Rejected	`131`
Zero sigma or profile test	`9`
Overload or incomplete profile	`938`
Sigma cutoff	`16`
High resolution limit	`45`

Final Data Set

Scale factor range	10.00-10.85
Number of 'full' reflections	`21570`
Number of 'partial' reflections	`13393`
Total number of integrated reflections	`33938`
Total number of unique reflections	`5598`
Data completeness	`100.0%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`32.4`
Average Sigma(I)	`1.2`
Overall R-merge (linear)	`0.046`

Sadabs Results

Parameter refinement on 21989 reflections reduced R(int) from 0.0790 to 0.0352

Before rejection, 33564 reflections total and 5615 unique

After rejection, 33204 reflections total and 5611 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0454   0.834 - 0.959   0.973 - 1.124   1.150   18460   13371
    2  -11.2  0.0451   1.087 - 1.153   0.984 - 1.158   1.178    2022    1396
    3  -11.2  0.0449   1.105 - 1.249   0.970 - 1.147   1.166    8069    5810
    4  -11.2  0.0477   0.847 - 0.894   0.970 - 1.140   1.143    4653    3271

Ratio of minimum to maximum apparent transmission: 0.838178

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. C. D. Gabbutt

Local Code NAR2-59

Formula C29 H25 N1 O5 S1

Crystal Colour Yellow

Crystal Habit Shard

Crystal Size 0.16 x 0.14 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. C. D. Gabbutt
Local Code	NAR2-59
Formula	C29 H25 N1 O5 S1
Crystal Colour	Yellow
Crystal Habit	Shard
Crystal Size	0.16 x 0.14 x 0.04 (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    'graphite'
_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. SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10

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/