Summary report for Directory: diska/2005src0633

Report generated May 13, 2005; 08:20:07

Unit cell

9630 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) 8.5597 +/- 0.0003

b (Angstrom) 15.8654 +/- 0.0005

c (Angstrom) 16.0164 +/- 0.0004

alpha (°) 99.7427 +/- 0.0018

beta (°) 96.411 +/- 0.002

gamma (°) 91.1695 +/- 0.0014

Volume (A**3) 2128.59 +/- 0.11
Mosaicity (°) 0.593 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	8.5597 +/- 0.0003
b (Angstrom)	15.8654 +/- 0.0005
c (Angstrom)	16.0164 +/- 0.0004
alpha (°)	99.7427 +/- 0.0018
beta (°)	96.411 +/- 0.002
gamma (°)	91.1695 +/- 0.0014
Volume (A**3)	2128.59 +/- 0.11
Mosaicity (°)	0.593 +/- 0.002

Data collection

Summary

Total number of images collected	337
Total exposure time	16.5 hours
Data collection exposure time	16.5 hours
Data collection wall-clock time	17.6 hours

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°	180 seconds	Yes
data collection	s02f	17	`34.0`° omega	2.000°	180 seconds	Yes
data collection	s03f	55	`110.0`° omega	2.000°	180 seconds	Yes
data collection	s04f	23	`46.0`° omega	2.000°	180 seconds	Yes
data collection	s05f	53	`106.0`° omega	2.000°	180 seconds	Yes
Phi/Chi	i01f - i08f	8			30 seconds

Scalepack Scaling

Deleted observations

Rejected	`555`
Zero sigma or profile test	`2`
Overload or incomplete profile	`1268`
Sigma cutoff	`33`
High resolution limit	`22`

Final Data Set

Scale factor range	9.48-10.23
Number of 'full' reflections	`29779`
Number of 'partial' reflections	`21713`
Total number of integrated reflections	`49411`
Total number of unique reflections	`9782`
Data completeness	`99.6%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`19.7`
Average Sigma(I)	`1.2`
Overall R-merge (linear)	`0.068`

Sadabs Results

Parameter refinement on 27664 reflections reduced R(int) from 0.0932 to 0.0430

Before rejection, 49295 reflections total and 9798 unique

After rejection, 48359 reflections total and 9791 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0678   0.787 - 0.941   0.961 - 1.173   1.213   27082   16922
    2   -6.8  0.0658   1.301 - 1.421   0.991 - 1.114   1.163    2232    1407
    3   -6.8  0.0614   1.196 - 1.305   0.969 - 1.115   1.168    8088    5264
    4   -6.8  0.0619   1.234 - 1.329   0.965 - 1.149   1.166    3155    2048
    5   -6.8  0.0644   0.777 - 0.891   0.963 - 1.156   1.179    7802    4997

Ratio of minimum to maximum apparent transmission: 0.819872

Metadata

Group Service

Operator Simon Coles

Sample Owner Lancaster

Local Code AM521(b)

Formula C30H29B2F15LiO4P

Crystal Colour Colourless

Crystal Habit Plate

Crystal Size 0.12 x 0.12 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Lancaster
Local Code	AM521(b)
Formula	C30H29B2F15LiO4P
Crystal Colour	Colourless
Crystal Habit	Plate
Crystal Size	0.12 x 0.12 x 0.04 (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/