Summary report for Directory: diska/2005slh1128

Report generated Sep 29, 2005; 13:00:28

Unit cell

7252 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) 9.8837 +/- 0.0002

b (Angstrom) 11.8446 +/- 0.0003

c (Angstrom) 14.5108 +/- 0.0003

alpha (°) 104.0099 +/- 0.0011

beta (°) 95.5232 +/- 0.0014

gamma (°) 98.0781 +/- 0.0012

Volume (A**3) 1616.80 +/- 0.06
Mosaicity (°) 0.6260 +/- 0.0010

Symmetry used in scalepack	p1
a (Angstrom)	9.8837 +/- 0.0002
b (Angstrom)	11.8446 +/- 0.0003
c (Angstrom)	14.5108 +/- 0.0003
alpha (°)	104.0099 +/- 0.0011
beta (°)	95.5232 +/- 0.0014
gamma (°)	98.0781 +/- 0.0012
Volume (A**3)	1616.80 +/- 0.06
Mosaicity (°)	0.6260 +/- 0.0010

Data collection

Summary

Total number of images collected	301
Total exposure time	100.1 minutes
Data collection exposure time	98.7 minutes
Data collection wall-clock time	123.5 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	30.00 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°	20 seconds	Yes
data collection	s02f	17	`34.0`° omega	2.000°	20 seconds	Yes
data collection	s03f	17	`34.0`° omega	2.000°	20 seconds	Yes
data collection	s04f	55	`110.0`° omega	2.000°	20 seconds	Yes
data collection	s05f	23	`46.0`° omega	2.000°	20 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`199`
Zero sigma or profile test	`3`
Overload or incomplete profile	`1226`
Sigma cutoff	`35`
High resolution limit	`116`

Final Data Set

Scale factor range	9.19-10.10
Number of 'full' reflections	`19606`
Number of 'partial' reflections	`15359`
Total number of integrated reflections	`33412`
Total number of unique reflections	`7364`
Data completeness	`99.9%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`209.0`
Average Sigma(I)	`4.8`
Overall R-merge (linear)	`0.045`

Sadabs Results

Parameter refinement on 27916 reflections reduced R(int) from 0.0708 to 0.0439

Before rejection, 32976 reflections total and 7413 unique

After rejection, 32586 reflections total and 7410 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0425   0.947 - 1.066   0.941 - 1.183   1.359   20565   17977
    2   -6.8  0.0473   0.753 - 0.813   0.941 - 1.048   1.373    1710    1510
    3   -6.8  0.0414   0.691 - 0.720   0.964 - 1.086   1.371    1714    1470
    4   -6.8  0.0460   0.900 - 0.980   0.943 - 1.086   1.361    6178    5315
    5   -6.8  0.0499   0.756 - 0.814   0.941 - 1.093   1.406    2419    2065

Ratio of minimum to maximum apparent transmission: 0.795380

Metadata

Group Personal

Operator Mike Hursthouse

Sample Owner SLH/CAG

Local Code CAG161

Formula C28H32N2O4P2S4Cd1

Crystal Colour Colourless

Crystal Habit Block

Crystal Size 0.3 x 0.2 x 0.2 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Personal
Operator	Mike Hursthouse
Sample Owner	SLH/CAG
Local Code	CAG161
Formula	C28H32N2O4P2S4Cd1
Crystal Colour	Colourless
Crystal Habit	Block
Crystal Size	0.3 x 0.2 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/