Summary report for Directory: diska/04src0339

Report generated Apr 27, 2004; 09:15:10

Unit cell

26481 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) 14.6319 +/- 0.0002

b (Angstrom) 12.0514 +/- 0.0002

c (Angstrom) 14.9097 +/- 0.0002

alpha (°) 90.000

beta (°) 111.3965 +/- 0.0007

gamma (°) 90.000

Volume (A**3) 2447.90 +/- 0.06
Mosaicity (°) 0.3670 +/- 0.0010

Symmetry used in scalepack	p2
a (Angstrom)	14.6319 +/- 0.0002
b (Angstrom)	12.0514 +/- 0.0002
c (Angstrom)	14.9097 +/- 0.0002
alpha (°)	90.000
beta (°)	111.3965 +/- 0.0007
gamma (°)	90.000
Volume (A**3)	2447.90 +/- 0.06
Mosaicity (°)	0.3670 +/- 0.0010

Data collection

Summary

Total number of images collected	579
Total exposure time	8.0 hours
Data collection exposure time	8.0 hours
Data collection wall-clock time	8.9 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	45.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	290	`290.0`° phi	1.000°	50 seconds	Yes
data collection	s02f	144	`144.0`° omega	1.000°	50 seconds	Yes
data collection	s03f	137	`137.0`° omega	1.000°	50 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`7`
Zero sigma or profile test	`5`
Overload or incomplete profile	`746`
Sigma cutoff	`1`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`16297`
Number of 'partial' reflections	`14612`
Total number of integrated reflections	`29037`
Total number of unique reflections	`5875`
Data completeness	`99.4%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`121.8`
Average Sigma(I)	`3.2`
Overall R-merge (linear)	`0.120`

Sadabs result in sad.abs

Parameter refinement on 25073 reflections reduced R(int) from 0.1093 to 0.0295

Before rejection, 30183 reflections total and 5878 unique

After rejection, 29686 reflections total and 5869 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.9  0.0305   0.913 - 1.276   0.906 - 1.264   1.147   15163   13233
    2  -18.3  0.0310   0.899 - 1.307   0.915 - 1.310   1.151    7323    6324
    3  -18.3  0.0306   0.696 - 1.045   0.915 - 1.275   1.088    7200    6327

Ratio of minimum to maximum apparent transmission: 0.691275

Metadata

Supervisor Service

Operator Peter Horton

User Duncan Bruce

Local Code C3F7 Pt 1,1

Formula C24 H22 N1 O4 F7 Pt1

Crystal Colour Orange

Crystal Habit Slab

Crystal Size 0.13 x 0.09 x 0.03 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Solvents

Supervisor	Service
Operator	Peter Horton
User	Duncan Bruce
Local Code	C3F7 Pt 1,1
Formula	C24 H22 N1 O4 F7 Pt1
Crystal Colour	Orange
Crystal Habit	Slab
Crystal Size	0.13 x 0.09 x 0.03 (mm3)
Temperature	120(K)
Generator	50 (kV) 85 (mA)
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          '\p & \w scans'
_diffrn_detector_area_resol_mean   9.091

_computing_data_collection
'COLLECT (Hooft, 1999)'
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1999)'
#Although determined using DirAx, the cell is refined in the HKL package during data reduction
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1999)'

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., 1999.

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. SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10

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/