Summary report for Directory: home/diska/2005slh0428

Report generated May 08, 2005; 20:12:29

Unit cell

3111 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack c2

a (Angstrom) 10.2942 +/- 0.0004

b (Angstrom) 29.7386 +/- 0.0014

c (Angstrom) 9.2931 +/- 0.0004

alpha (°) 90.000

beta (°) 90.374 +/- 0.003

gamma (°) 90.000

Volume (A**3) 2844.9 +/- 0.2
Mosaicity (°) 1.582 +/- 0.002

Symmetry used in scalepack	c2
a (Angstrom)	10.2942 +/- 0.0004
b (Angstrom)	29.7386 +/- 0.0014
c (Angstrom)	9.2931 +/- 0.0004
alpha (°)	90.000
beta (°)	90.374 +/- 0.003
gamma (°)	90.000
Volume (A**3)	2844.9 +/- 0.2
Mosaicity (°)	1.582 +/- 0.002

Data collection

Summary

Total number of images collected	364
Total exposure time	61.9 minutes
Data collection exposure time	60.6 minutes
Data collection wall-clock time	91.2 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	302	`302.0`° phi	1.000°	10 seconds	Yes
data collection	s02f	54	`54.0`° omega	1.000°	10 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`273`
Zero sigma or profile test	`7`
Overload or incomplete profile	`816`
Sigma cutoff	`14`

Final Data Set

Scale factor range	10.00-13.59
Number of 'full' reflections	`0`
Number of 'partial' reflections	`14572`
Total number of integrated reflections	`13437`
Total number of unique reflections	`3308`
Data completeness	`99.1%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`238.8`
Average Sigma(I)	`6.1`
Overall R-merge (linear)	`0.038`

Sadabs Results

Parameter refinement on 13212 reflections reduced R(int) from 0.0750 to 0.0372

Before rejection, 14636 reflections total and 3333 unique

After rejection, 14429 reflections total and 3332 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0369   0.751 - 1.060   0.914 - 1.365   1.507   12235   11232
    2  -11.2  0.0417   0.913 - 1.033   0.951 - 1.258   1.675    2194    1996

Ratio of minimum to maximum apparent transmission: 0.669645

Metadata

Group Mike Hursthouse

Operator Susanne Huth

Sample Owner

Local Code CAG 153

Formula C46 H54 N4 O4 P2 S4 Ni1 Pt1

Crystal Colour Green

Crystal Habit Slab

Crystal Size 0.2 x 0.1 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Susanne Huth
Sample Owner
Local Code	CAG 153
Formula	C46 H54 N4 O4 P2 S4 Ni1 Pt1
Crystal Colour	Green
Crystal Habit	Slab
Crystal Size	0.2 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    '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/