Summary report for Directory: home/diska/04src0896r

Report generated Nov 02, 2004; 13:11:24

Unit cell

8435 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) 12.7393 +/- 0.0009

b (Angstrom) 26.485 +/- 0.002

c (Angstrom) 16.3749 +/- 0.0013

alpha (°) 90.000

beta (°) 95.732 +/- 0.004

gamma (°) 90.000

Volume (A**3) 5497.2 +/- 0.7
Mosaicity (°) 2.253 +/- 0.003

Symmetry used in scalepack	p2
a (Angstrom)	12.7393 +/- 0.0009
b (Angstrom)	26.485 +/- 0.002
c (Angstrom)	16.3749 +/- 0.0013
alpha (°)	90.000
beta (°)	95.732 +/- 0.004
gamma (°)	90.000
Volume (A**3)	5497.2 +/- 0.7
Mosaicity (°)	2.253 +/- 0.003

Data collection

Summary

Total number of images collected	275
Total exposure time	135.6 minutes
Data collection exposure time	134.5 minutes
Data collection wall-clock time	157.3 minutes

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	147	`294.0`° phi	2.000°	30 seconds	Yes
data collection	s02f	53	`106.0`° omega	2.000°	30 seconds	Yes
data collection	s03f	67	`134.0`° omega	2.000°	30 seconds	Yes
Phi/Chi	i01f - i08f	8			8 seconds

Scalepack Scaling

Deleted observations

Rejected	`369`
Zero sigma or profile test	`79`
Overload or incomplete profile	`2518`
Sigma cutoff	`110`
High resolution limit	`732`

Final Data Set

Scale factor range	7.02-10.78
Number of 'full' reflections	`0`
Number of 'partial' reflections	`45413`
Total number of integrated reflections	`32293`
Total number of unique reflections	`11647`
Data completeness	`90.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`43.3`
Average Sigma(I)	`4.3`
Overall R-merge (linear)	`0.074`

Sadabs Results

Parameter refinement on 27482 reflections reduced R(int) from 0.1692 to 0.0703

Before rejection, 50436 reflections total and 12989 unique

After rejection, 48147 reflections total and 12961 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.9  0.0960   0.741 - 0.965   0.843 - 1.564   1.459   30357   17909
    2   18.3  0.0776   0.744 - 0.859   0.924 - 1.260   1.418    7288    4731
    3  -18.3  0.1003   0.669 - 1.172   0.924 - 3.972   1.547   10502    5746

Ratio of minimum to maximum apparent transmission: 0.212314

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. R. B. Bedford

Local Code MB 247B

Formula C52 H47 O3 P4 F6 Pd Sb

Crystal Colour Yellow

Crystal Habit Cut Block

Crystal Size 0.17 x 0.08 x 0.06 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. R. B. Bedford
Local Code	MB 247B
Formula	C52 H47 O3 P4 F6 Pd Sb
Crystal Colour	Yellow
Crystal Habit	Cut Block
Crystal Size	0.17 x 0.08 x 0.06 (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/