Summary report for Directory: diska/2005src0806b

Report generated Jun 27, 2005; 15:46:26

Unit cell

11708 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) 13.1663 +/- 0.0002

b (Angstrom) 13.5696 +/- 0.0002

c (Angstrom) 15.5439 +/- 0.0002

alpha (°) 102.4235 +/- 0.0007

beta (°) 104.1498 +/- 0.0009

gamma (°) 92.9015 +/- 0.0009

Volume (A**3) 2614.12 +/- 0.07
Mosaicity (°) 0.4750 +/- 0.0010

Symmetry used in scalepack	p1
a (Angstrom)	13.1663 +/- 0.0002
b (Angstrom)	13.5696 +/- 0.0002
c (Angstrom)	15.5439 +/- 0.0002
alpha (°)	102.4235 +/- 0.0007
beta (°)	104.1498 +/- 0.0009
gamma (°)	92.9015 +/- 0.0009
Volume (A**3)	2614.12 +/- 0.07
Mosaicity (°)	0.4750 +/- 0.0010

Data collection

Summary

Total number of images collected	332
Total exposure time	88.6 minutes
Data collection exposure time	87.5 minutes
Data collection wall-clock time	114.5 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	31.00 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°	16 seconds	Yes
data collection	s02f	17	`34.0`° omega	2.000°	16 seconds	Yes
data collection	s03f	17	`34.0`° omega	2.000°	16 seconds	Yes
data collection	s04f	56	`112.0`° omega	2.000°	16 seconds	Yes
data collection	s05f	53	`106.0`° omega	2.000°	16 seconds	Yes
Phi/Chi	i01f - i08f	8			8 seconds

Scalepack Scaling

Deleted observations

Rejected	`290`
Zero sigma or profile test	`6`
Overload or incomplete profile	`1752`
Sigma cutoff	`22`
High resolution limit	`9`

Final Data Set

Scale factor range	8.99-10.76
Number of 'full' reflections	`39209`
Number of 'partial' reflections	`20798`
Total number of integrated reflections	`57849`
Total number of unique reflections	`11971`
Data completeness	`99.9%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`84.6`
Average Sigma(I)	`2.4`
Overall R-merge (linear)	`0.032`

Sadabs Results

Parameter refinement on 47359 reflections reduced R(int) from 0.0502 to 0.0304

Before rejection, 57105 reflections total and 11977 unique

After rejection, 56593 reflections total and 11969 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0329   1.067 - 1.206   0.967 - 1.087   1.369   32360   27411
    2   -7.8  0.0311   0.641 - 0.685   0.993 - 1.038   1.289    2650    2284
    3   -7.8  0.0295   0.982 - 1.028   0.969 - 1.073   1.305    2674    2296
    4   -7.8  0.0310   0.796 - 0.904   0.967 - 1.062   1.297    9745    8440
    5   -7.8  0.0307   0.714 - 0.803   0.975 - 1.045   1.246    9164    7962

Ratio of minimum to maximum apparent transmission: 0.889861

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. R. B. Bedford

Local Code MB428 (large)

Formula C57 H54 O3 P3 Cl1 Ru1

Crystal Colour Colourless

Crystal Habit Cut Block

Crystal Size 0.48 x 0.32 x 0.24 (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	MB428 (large)
Formula	C57 H54 O3 P3 Cl1 Ru1
Crystal Colour	Colourless
Crystal Habit	Cut Block
Crystal Size	0.48 x 0.32 x 0.24 (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/