Summary report for Directory: diska/2005src1386r

Report generated Nov 14, 2005; 16:03:41

Unit cell

6786 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) 9.4034 +/- 0.0014

b (Angstrom) 17.583 +/- 0.003

c (Angstrom) 27.594 +/- 0.004

alpha (°) 90.000

beta (°) 92.106 +/- 0.008

gamma (°) 90.000

Volume (A**3) 4559.3 +/- 1.2
Mosaicity (°) 2.774 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	9.4034 +/- 0.0014
b (Angstrom)	17.583 +/- 0.003
c (Angstrom)	27.594 +/- 0.004
alpha (°)	90.000
beta (°)	92.106 +/- 0.008
gamma (°)	90.000
Volume (A**3)	4559.3 +/- 1.2
Mosaicity (°)	2.774 +/- 0.002

Data collection

Summary

Total number of images collected	1409
Total exposure time	18.8 hours
Data collection exposure time	18.8 hours
Data collection wall-clock time	20.6 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	70.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	452	`361.6`° phi	0.800°	48 seconds	Yes
data collection	s02f	321	`256.8`° phi	0.800°	48 seconds	Yes
data collection	s03f	79	`63.2`° omega	0.800°	48 seconds	Yes
data collection	s04f	91	`72.8`° omega	0.800°	48 seconds	Yes
data collection	s05f	66	`52.8`° omega	0.800°	48 seconds	Yes
data collection	s06f	86	`68.8`° omega	0.800°	48 seconds	Yes
data collection	s07f	67	`53.6`° omega	0.800°	48 seconds	Yes
data collection	s08f	120	`96.0`° omega	0.800°	48 seconds	Yes
data collection	s09f	119	`95.2`° omega	0.800°	48 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`3907`
Zero sigma or profile test	`206`
Overload or incomplete profile	`9974`
Sigma cutoff	`912`
Low resolution limit	`84`
High resolution limit	`102`

Final Data Set

Scale factor range	4.33-14.69
Number of 'full' reflections	`0`
Number of 'partial' reflections	`45213`
Total number of integrated reflections	`30400`
Total number of unique reflections	`9064`
Data completeness	`80.5%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`205.4`
Average Sigma(I)	`13.6`
Overall R-merge (linear)	`0.089`

Sadabs Results

Parameter refinement on 40831 reflections reduced R(int) from 0.2470 to 0.0970

Before rejection, 58791 reflections total and 10749 unique

After rejection, 52994 reflections total and 10715 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -20.4  0.0843   1.131 - 1.944   0.814 - 1.597   1.569   15136   12332
    2   29.9  0.1073   0.571 - 0.835   0.782 - 1.450   1.635   14281    9797
    3  -29.3  0.1233   0.709 - 0.974   0.843 - 1.448   1.704    2948    2012
    4   29.3  0.1110   0.376 - 0.513   0.781 - 2.462   1.723    2320    1548
    5  -29.3  0.3121   0.508 - 0.699   0.938 - 1.568   2.105    1955     644
    6   29.3  0.1375   0.350 - 0.758   0.860 - 2.541   1.776    2228    1537
    7  -29.3  0.1242   0.403 - 0.532   0.930 - 1.397   1.645    3257    2136
    8  -29.3  0.1850   0.470 - 0.855   0.914 - 2.322   1.725    5760    3071
    9  -29.3  0.1161   0.771 - 1.341   0.871 - 2.510   1.658    5109    3528

Sadabs Results

Parameter refinement on 29979 reflections reduced R(int) from 0.1801 to 0.1190

Before rejection, 48123 reflections total and 8674 unique

After rejection, 44751 reflections total and 8671 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   20.4  0.1041   0.546 - 1.033   0.887 - 2.455   1.499   11185    8555
    2  -29.9  0.1245   0.612 - 0.910   0.886 - 1.501   1.506   10756    6676
    3   29.3  0.1339   0.564 - 0.783   0.887 - 1.880   1.598    2515    1645
    4  -29.3  0.1386   0.580 - 1.040   0.868 - 1.619   1.510    3415    1831
    5   29.3  0.1775   0.643 - 0.933   0.905 - 1.538   1.541    2444    1340
    6  -29.3  0.1679   0.854 - 1.183   0.868 - 1.466   1.619    3157    1757
    7   29.3  0.1365   0.505 - 0.686   0.919 - 1.583   1.521    2454    1462
    8   29.3  0.2057   0.752 - 1.377   0.868 - 2.789   1.587    4483    2168
    9   29.3  0.1362   0.546 - 0.787   0.905 - 1.573   1.497    4342    2551

Ratio of minimum to maximum apparent transmission: 0.307220

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. I. R. Butler

Local Code IAN4

Formula C46 H27 P3 Br2 Fe1 Ni1

Crystal Colour Dark Red

Crystal Habit Slab

Crystal Size 0.26 x 0.24 x 0.1 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. I. R. Butler
Local Code	IAN4
Formula	C46 H27 P3 Br2 Fe1 Ni1
Crystal Colour	Dark Red
Crystal Habit	Slab
Crystal Size	0.26 x 0.24 x 0.1 (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/