Summary report for Directory: home/diska/04src1119

Report generated Dec 03, 2004; 09:20:51

Unit cell

28252 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) 20.4953 +/- 0.0003

b (Angstrom) 25.3649 +/- 0.0004

c (Angstrom) 25.2079 +/- 0.0004

alpha (°) 90.000

beta (°) 111.5484 +/- 0.0006

gamma (°) 90.000

Volume (A**3) 12188.7 +/- 0.3
Mosaicity (°) 0.8530 +/- 0.0010

Symmetry used in scalepack	p2
a (Angstrom)	20.4953 +/- 0.0003
b (Angstrom)	25.3649 +/- 0.0004
c (Angstrom)	25.2079 +/- 0.0004
alpha (°)	90.000
beta (°)	111.5484 +/- 0.0006
gamma (°)	90.000
Volume (A**3)	12188.7 +/- 0.3
Mosaicity (°)	0.8530 +/- 0.0010

Data collection

Summary

Total number of images collected	989
Total exposure time	12.4 hours
Data collection exposure time	12.3 hours
Data collection wall-clock time	13.7 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	50.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	201	`150.8`° omega	0.750°	45 seconds	Yes
data collection	s02f	195	`146.2`° omega	0.750°	45 seconds	Yes
data collection	s03f	192	`144.0`° omega	0.750°	45 seconds	Yes
data collection	s04f	196	`147.0`° omega	0.750°	45 seconds	Yes
data collection	s05f	197	`147.8`° omega	0.750°	45 seconds	Yes
Phi/Chi	i01f - i08f	8			30 seconds

Scalepack Scaling

Deleted observations

Rejected	`2358`
Zero sigma or profile test	`127`
Overload or incomplete profile	`11524`
Sigma cutoff	`475`
Low resolution limit	`3`
High resolution limit	`1760`

Final Data Set

Scale factor range	3.77-10.28
Number of 'full' reflections	`0`
Number of 'partial' reflections	`180870`
Total number of integrated reflections	`172079`
Total number of unique reflections	`28390`
Data completeness	`99.9%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`84.8`
Average Sigma(I)	`3.6`
Overall R-merge (linear)	`0.081`

Sadabs Results

Parameter refinement on 105798 reflections reduced R(int) from 0.1893 to 0.0569

Before rejection, 174695 reflections total and 28680 unique

After rejection, 170588 reflections total and 28664 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -21.2  0.0708   0.864 - 1.072   0.968 - 1.113   1.413   34967   22950
    2  -20.8  0.0690   0.800 - 1.094   0.951 - 1.083   1.410   33667   22088
    3  -21.1  0.0913   0.590 - 1.432   0.968 - 1.201   1.480   33605   19770
    4  -21.1  0.0811   0.691 - 1.529   0.951 - 1.098   1.460   34198   21517
    5  -21.1  0.0820   0.989 - 1.206   0.969 - 1.195   1.474   34151   21100

Ratio of minimum to maximum apparent transmission: 0.791904

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. C. J. Matthews

Local Code LJD465Mn3

Formula C72 H64 N36 O32 Cl8 Mn4

Crystal Colour Orange

Crystal Habit Block

Crystal Size 0.18 x 0.15 x 0.08 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. C. J. Matthews
Local Code	LJD465Mn3
Formula	C72 H64 N36 O32 Cl8 Mn4
Crystal Colour	Orange
Crystal Habit	Block
Crystal Size	0.18 x 0.15 x 0.08 (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/