Summary report for Directory: diska/04src1116

Report generated Dec 01, 2004; 08:51:33

Unit cell

8784 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p1

a (Angstrom) 9.2375 +/- 0.0003

b (Angstrom) 12.7526 +/- 0.0007

c (Angstrom) 18.1555 +/- 0.0009

alpha (°) 88.621 +/- 0.002

beta (°) 80.921 +/- 0.003

gamma (°) 86.131 +/- 0.003

Volume (A**3) 2106.95 +/- 0.17
Mosaicity (°) 1.129 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	9.2375 +/- 0.0003
b (Angstrom)	12.7526 +/- 0.0007
c (Angstrom)	18.1555 +/- 0.0009
alpha (°)	88.621 +/- 0.002
beta (°)	80.921 +/- 0.003
gamma (°)	86.131 +/- 0.003
Volume (A**3)	2106.95 +/- 0.17
Mosaicity (°)	1.129 +/- 0.002

Data collection

Summary

Total number of images collected	349
Total exposure time	14.4 hours
Data collection exposure time	14.2 hours
Data collection wall-clock time	14.8 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	`362.0`° phi	2.000°	150 seconds	Yes
data collection	s02f	17	`34.0`° omega	2.000°	150 seconds	Yes
data collection	s03f	27	`54.0`° omega	2.000°	150 seconds	Yes
data collection	s04f	58	`116.0`° omega	2.000°	150 seconds	Yes
data collection	s05f	58	`116.0`° omega	2.000°	150 seconds	Yes
Phi/Chi	i01f - i08f	8			60 seconds

Scalepack Scaling

Deleted observations

Rejected	`193`
Zero sigma or profile test	`9`
Overload or incomplete profile	`1744`
Sigma cutoff	`58`
High resolution limit	`55`

Final Data Set

Scale factor range	9.03-10.65
Number of 'full' reflections	`12174`
Number of 'partial' reflections	`30979`
Total number of integrated reflections	`39681`
Total number of unique reflections	`9406`
Data completeness	`97.1%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`19.6`
Average Sigma(I)	`1.6`
Overall R-merge (linear)	`0.077`

Sadabs Results

Parameter refinement on 22374 reflections reduced R(int) from 0.0764 to 0.0492

Before rejection, 40403 reflections total and 9634 unique

After rejection, 39692 reflections total and 9626 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0736   0.870 - 1.077   0.952 - 1.179   1.317   21543   13213
    2  -11.2  0.0756   0.815 - 0.885   0.987 - 1.188   1.335    1728    1097
    3  -11.2  0.0876   0.932 - 1.019   0.980 - 1.204   1.377    2968    1685
    4  -11.2  0.0769   0.748 - 0.875   0.952 - 1.268   1.285    6697    4105
    5  -11.2  0.0800   0.829 - 0.949   0.967 - 1.215   1.282    6756    4128

Ratio of minimum to maximum apparent transmission: 0.750711

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. C. J. Matthews

Local Code LJD459Mn

Formula C72 H66 N36 O32 Cl8 Mn4

Crystal Colour Orange

Crystal Habit Slab

Crystal Size 0.24 x 0.1 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. J. Matthews
Local Code	LJD459Mn
Formula	C72 H66 N36 O32 Cl8 Mn4
Crystal Colour	Orange
Crystal Habit	Slab
Crystal Size	0.24 x 0.1 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. (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/