Summary report for Directory: diska/04src0343

Report generated Apr 28, 2004; 08:45:57

Unit cell

25884 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) 12.0135 +/- 0.0002

b (Angstrom) 13.9841 +/- 0.0003

c (Angstrom) 17.1398 +/- 0.0003

alpha (°) 93.9597 +/- 0.0010

beta (°) 105.5361 +/- 0.0009

gamma (°) 90.9923 +/- 0.0008

Volume (A**3) 2765.70 +/- 0.09
Mosaicity (°) 0.3730 +/- 0.0010

Symmetry used in scalepack	p1
a (Angstrom)	12.0135 +/- 0.0002
b (Angstrom)	13.9841 +/- 0.0003
c (Angstrom)	17.1398 +/- 0.0003
alpha (°)	93.9597 +/- 0.0010
beta (°)	105.5361 +/- 0.0009
gamma (°)	90.9923 +/- 0.0008
Volume (A**3)	2765.70 +/- 0.09
Mosaicity (°)	0.3730 +/- 0.0010

Data collection

Summary

Total number of images collected	476
Total exposure time	15.7 hours
Data collection exposure time	15.6 hours
Data collection wall-clock time	16.4 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	45.00 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°	120 seconds	Yes
data collection	s02f	35	`70.0`° omega	2.000°	120 seconds	Yes
data collection	s03f	35	`70.0`° omega	2.000°	120 seconds	Yes
data collection	s04f	35	`70.0`° omega	2.000°	120 seconds	Yes
data collection	s05f	68	`136.0`° omega	2.000°	120 seconds	Yes
data collection	s06f	68	`136.0`° omega	2.000°	120 seconds	Yes
data collection	s07f	46	`92.0`° omega	2.000°	120 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`12`
Zero sigma or profile test	`2`
Overload or incomplete profile	`1080`
Sigma cutoff	`5`
High resolution limit	`109`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`42658`
Number of 'partial' reflections	`14785`
Total number of integrated reflections	`55856`
Total number of unique reflections	`12649`
Data completeness	`99.9%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`73.2`
Average Sigma(I)	`2.3`
Overall R-merge (linear)	`0.053`

Sadabs result in sad.abs

Parameter refinement on 43122 reflections reduced R(int) from 0.0876 to 0.0310

Before rejection, 55091 reflections total and 12712 unique

After rejection, 54606 reflections total and 12708 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.9  0.0329   0.864 - 0.950   0.978 - 1.041   1.209   21300   17772
    2  -18.3  0.0338   0.936 - 0.997   0.977 - 1.023   1.229    4000    3265
    3  -18.3  0.0349   1.253 - 1.342   0.976 - 1.034   1.232    3982    3219
    4  -18.3  0.0349   0.937 - 1.000   0.976 - 1.007   1.248    4015    3240
    5  -18.3  0.0335   0.917 - 1.013   0.979 - 1.027   1.182    7991    6553
    6  -18.3  0.0347   0.851 - 0.924   0.977 - 1.034   1.213    7996    6640
    7  -18.3  0.0350   1.110 - 1.188   0.976 - 1.035   1.239    5322    4358

Ratio of minimum to maximum apparent transmission: 0.937682

Metadata

Supervisor Service

Operator Peter Horton

User Craig Matthews

Local Code LJD378Mn

Formula C72 H66 N36 O32 Cl8 Mn4

Crystal Colour Orange

Crystal Habit Block

Crystal Size 0.2 x 0.14 x 0.08 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Solvents Methanol Water

Supervisor	Service
Operator	Peter Horton
User	Craig Matthews
Local Code	LJD378Mn
Formula	C72 H66 N36 O32 Cl8 Mn4
Crystal Colour	Orange
Crystal Habit	Block
Crystal Size	0.2 x 0.14 x 0.08 (mm3)
Temperature	120(K)
Generator	50 (kV) 85 (mA)
Solvents	Methanol Water

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          ' & \w scans'
_diffrn_detector_area_resol_mean   9.091

_computing_data_collection
'COLLECT (Hooft, 1998)'
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1999)'
#Although determined using DirAx, the cell is refined in the HKL package during data reduction
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 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/