Summary report for Directory: home/diska/2005slh0424

Report generated Jul 29, 2005; 09:51:58

Unit cell

4266 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) 25.0172 +/- 0.0010

b (Angstrom) 8.8336 +/- 0.0002

c (Angstrom) 16.5575 +/- 0.0006

alpha (°) 90.000

beta (°) 97.2625 +/- 0.0016

gamma (°) 90.000

Volume (A**3) 3629.7 +/- 0.2
Mosaicity (°) 0.858 +/- 0.002

Symmetry used in scalepack	c2
a (Angstrom)	25.0172 +/- 0.0010
b (Angstrom)	8.8336 +/- 0.0002
c (Angstrom)	16.5575 +/- 0.0006
alpha (°)	90.000
beta (°)	97.2625 +/- 0.0016
gamma (°)	90.000
Volume (A**3)	3629.7 +/- 0.2
Mosaicity (°)	0.858 +/- 0.002

Data collection

Summary

Total number of images collected	183
Total exposure time	89.5 minutes
Data collection exposure time	88.1 minutes
Data collection wall-clock time	102.0 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	30.80 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	125	`250.0`° phi	2.000°	30 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	30 seconds	Yes
data collection	s03f	34	`68.0`° omega	2.000°	30 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`152`
Zero sigma or profile test	`3`
Overload or incomplete profile	`786`
Sigma cutoff	`11`
High resolution limit	`1`

Final Data Set

Scale factor range	7.00-11.51
Number of 'full' reflections	`9683`
Number of 'partial' reflections	`13312`
Total number of integrated reflections	`22011`
Total number of unique reflections	`4441`
Data completeness	`99.3%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`129.1`
Average Sigma(I)	`3.7`
Overall R-merge (linear)	`0.049`

Sadabs Results

Parameter refinement on 16838 reflections reduced R(int) from 0.0809 to 0.0429

Before rejection, 21556 reflections total and 4456 unique

After rejection, 21294 reflections total and 4455 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.2  0.0433   1.024 - 1.251   0.942 - 1.184   1.407   15383   12458
    2   -7.6  0.0425   0.567 - 0.627   0.942 - 1.133   1.394    1776    1483
    3   -7.6  0.0582   0.611 - 0.793   0.942 - 1.272   1.455    4135    3208

Ratio of minimum to maximum apparent transmission: 0.740814

Metadata

Group Personal

Operator Mike Hursthouse

Sample Owner S L Huth

Local Code 150c

Formula C34H32N6O4P2S4Ni1I2

Crystal Colour Orange

Crystal Habit Lath

Crystal Size 0.2 x 0.06 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Personal
Operator	Mike Hursthouse
Sample Owner	S L Huth
Local Code	150c
Formula	C34H32N6O4P2S4Ni1I2
Crystal Colour	Orange
Crystal Habit	Lath
Crystal Size	0.2 x 0.06 x 0.02 (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/