Summary report for Directory: home/diska/2005src0805

Report generated Jun 24, 2005; 13:22:02

Unit cell

3695 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) 22.3373 +/- 0.0006

b (Angstrom) 11.3994 +/- 0.0004

c (Angstrom) 15.5860 +/- 0.0004

alpha (°) 90.000

beta (°) 128.1586 +/- 0.0014

gamma (°) 90.000

Volume (A**3) 3120.60 +/- 0.17
Mosaicity (°) 0.568 +/- 0.002

Symmetry used in scalepack	c2
a (Angstrom)	22.3373 +/- 0.0006
b (Angstrom)	11.3994 +/- 0.0004
c (Angstrom)	15.5860 +/- 0.0004
alpha (°)	90.000
beta (°)	128.1586 +/- 0.0014
gamma (°)	90.000
Volume (A**3)	3120.60 +/- 0.17
Mosaicity (°)	0.568 +/- 0.002

Data collection

Summary

Total number of images collected	250
Total exposure time	82.9 minutes
Data collection exposure time	81.6 minutes
Data collection wall-clock time	102.0 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	131	`262.0`° phi	2.000°	20 seconds	Yes
data collection	s02f	55	`110.0`° omega	2.000°	20 seconds	Yes
data collection	s03f	56	`112.0`° omega	2.000°	20 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`117`
Zero sigma or profile test	`4`
Overload or incomplete profile	`712`
Sigma cutoff	`7`
High resolution limit	`95`

Final Data Set

Scale factor range	9.51-10.33
Number of 'full' reflections	`13813`
Number of 'partial' reflections	`9270`
Total number of integrated reflections	`22465`
Total number of unique reflections	`3741`
Data completeness	`100.0%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`63.4`
Average Sigma(I)	`2.0`
Overall R-merge (linear)	`0.054`

Sadabs Results

Parameter refinement on 16634 reflections reduced R(int) from 0.0668 to 0.0483

Before rejection, 22131 reflections total and 3768 unique

After rejection, 21886 reflections total and 3768 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0535   0.866 - 0.964   0.929 - 1.137   1.405   11700    9074
    2  -11.2  0.0523   0.896 - 1.030   0.928 - 1.112   1.419    5045    3877
    3  -11.2  0.0528   0.824 - 0.967   0.965 - 1.155   1.371    5141    3923

Ratio of minimum to maximum apparent transmission: 0.803397

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. A. G.W. Hodson

Local Code CROIN

Formula C19 H13 N2 O4 Cl1 Mo1

Crystal Colour Red

Crystal Habit Block

Crystal Size 0.12 x 0.07 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. A. G.W. Hodson
Local Code	CROIN
Formula	C19 H13 N2 O4 Cl1 Mo1
Crystal Colour	Red
Crystal Habit	Block
Crystal Size	0.12 x 0.07 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    '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/