Summary report for Directory: diska/05src0094

Report generated Jan 25, 2005; 10:28:04

Unit cell

5303 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) 10.9644 +/- 0.0003

b (Angstrom) 11.0473 +/- 0.0004

c (Angstrom) 11.1885 +/- 0.0003

alpha (°) 109.0970 +/- 0.0013

beta (°) 100.3638 +/- 0.0018

gamma (°) 96.1842 +/- 0.0017

Volume (A**3) 1239.36 +/- 0.07
Mosaicity (°) 0.447 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	10.9644 +/- 0.0003
b (Angstrom)	11.0473 +/- 0.0004
c (Angstrom)	11.1885 +/- 0.0003
alpha (°)	109.0970 +/- 0.0013
beta (°)	100.3638 +/- 0.0018
gamma (°)	96.1842 +/- 0.0017
Volume (A**3)	1239.36 +/- 0.07
Mosaicity (°)	0.447 +/- 0.002

Data collection

Summary

Total number of images collected	276
Total exposure time	64.8 minutes
Data collection exposure time	63.5 minutes
Data collection wall-clock time	88.2 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	181	`362.0`° phi	2.000°	14 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	14 seconds	Yes
data collection	s03f	16	`32.0`° omega	2.000°	14 seconds	Yes
data collection	s04f	27	`54.0`° omega	2.000°	14 seconds	Yes
data collection	s05f	28	`56.0`° omega	2.000°	14 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`105`
Zero sigma or profile test	`1`
Overload or incomplete profile	`572`
Sigma cutoff	`2`
High resolution limit	`1`

Final Data Set

Scale factor range	9.78-10.54
Number of 'full' reflections	`13496`
Number of 'partial' reflections	`6553`
Total number of integrated reflections	`18960`
Total number of unique reflections	`5654`
Data completeness	`99.0%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`74.5`
Average Sigma(I)	`2.6`
Overall R-merge (linear)	`0.032`

Sadabs Results

Parameter refinement on 15096 reflections reduced R(int) from 0.0733 to 0.0296

Before rejection, 18965 reflections total and 5660 unique

After rejection, 18789 reflections total and 5656 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0313   1.008 - 1.113   0.947 - 1.125   1.274   13061   10999
    2  -11.2  0.0274   0.795 - 0.835   0.947 - 1.059   1.258    1001     853
    3  -11.2  0.0291   0.628 - 0.656   0.971 - 1.106   1.140    1008     848
    4  -11.2  0.0329   0.877 - 0.919   0.947 - 1.047   1.292    1812    1523
    5  -11.2  0.0304   0.771 - 0.818   0.987 - 1.069   1.236    1907    1581

Ratio of minimum to maximum apparent transmission: 0.841105

Metadata

Group Service

Operator Mark Light

Sample Owner Robin Bedford

Local Code rmf264.3

Formula C26 H22 N2 Cl1 Fe1

Crystal Colour Dark Red

Crystal Habit Block

Crystal Size 0.4 x 0.25 x 0.2 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Mark Light
Sample Owner	Robin Bedford
Local Code	rmf264.3
Formula	C26 H22 N2 Cl1 Fe1
Crystal Colour	Dark Red
Crystal Habit	Block
Crystal Size	0.4 x 0.25 x 0.2 (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/