Summary report for Directory: diska/05src0140

Report generated Feb 01, 2005; 13:44:46

Unit cell

7762 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) 11.2483 +/- 0.0006

b (Angstrom) 9.0504 +/- 0.0004

c (Angstrom) 34.6733 +/- 0.0018

alpha (°) 90.000

beta (°) 97.650 +/- 0.002

gamma (°) 90.000

Volume (A**3) 3498.4 +/- 0.3
Mosaicity (°) 0.583 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	11.2483 +/- 0.0006
b (Angstrom)	9.0504 +/- 0.0004
c (Angstrom)	34.6733 +/- 0.0018
alpha (°)	90.000
beta (°)	97.650 +/- 0.002
gamma (°)	90.000
Volume (A**3)	3498.4 +/- 0.3
Mosaicity (°)	0.583 +/- 0.002

Data collection

Summary

Total number of images collected	267
Total exposure time	218.8 minutes
Data collection exposure time	216.7 minutes
Data collection wall-clock time	237.3 minutes

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	38	`76.0`° omega	2.000°	50 seconds	Yes
data collection	s02f	24	`48.0`° omega	2.000°	50 seconds	Yes
data collection	s03f	50	`100.0`° omega	2.000°	50 seconds	Yes
data collection	s04f	74	`148.0`° omega	2.000°	50 seconds	Yes
data collection	s05f	73	`146.0`° omega	2.000°	50 seconds	Yes
Phi/Chi	i01f - i08f	8			15 seconds

Scalepack Scaling

Deleted observations

Rejected	`77`
Zero sigma or profile test	`29`
Overload or incomplete profile	`594`
Sigma cutoff	`19`
Low resolution limit	`1`
High resolution limit	`106`

Final Data Set

Scale factor range	9.55-10.10
Number of 'full' reflections	`19951`
Number of 'partial' reflections	`11835`
Total number of integrated reflections	`30231`
Total number of unique reflections	`8488`
Data completeness	`99.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`17.5`
Average Sigma(I)	`1.5`
Overall R-merge (linear)	`0.062`

Sadabs Results

Parameter refinement on 16838 reflections reduced R(int) from 0.0886 to 0.0421

Before rejection, 30073 reflections total and 8530 unique

After rejection, 29735 reflections total and 8524 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -21.1  0.0462   0.942 - 1.015   0.968 - 1.029   1.314    2801    2007
    2  -21.1  0.0673   0.778 - 0.826   0.981 - 1.026   1.252    2971    1711
    3  -21.1  0.0689   0.917 - 0.990   0.981 - 1.078   1.259    6605    3940
    4  -21.1  0.0591   0.907 - 0.995   0.981 - 1.124   1.274    7967    5065
    5  -21.1  0.0652   0.923 - 1.002   0.964 - 1.108   1.266    9391    5656

Ratio of minimum to maximum apparent transmission: 0.857366

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. R. B. Bedford

Local Code rmfsalentbu

Formula C32 H46 N2 O2 Cl1 Fe1

Crystal Colour Dark Red

Crystal Habit Cut Shard

Crystal Size 0.32 x 0.22 x 0.08 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. R. B. Bedford
Local Code	rmfsalentbu
Formula	C32 H46 N2 O2 Cl1 Fe1
Crystal Colour	Dark Red
Crystal Habit	Cut Shard
Crystal Size	0.32 x 0.22 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    '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/