Summary report for Directory: diska/2005src1659

Report generated Jan 06, 2006; 15:10:41

Unit cell

3620 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) 7.0311 +/- 0.0006

b (Angstrom) 19.821 +/- 0.002

c (Angstrom) 19.828 +/- 0.002

alpha (°) 88.008 +/- 0.004

beta (°) 79.780 +/- 0.006

gamma (°) 79.781 +/- 0.005

Volume (A**3) 2676.3 +/- 0.5
Mosaicity (°) 1.256 +/- 0.004

Symmetry used in scalepack	p1
a (Angstrom)	7.0311 +/- 0.0006
b (Angstrom)	19.821 +/- 0.002
c (Angstrom)	19.828 +/- 0.002
alpha (°)	88.008 +/- 0.004
beta (°)	79.780 +/- 0.006
gamma (°)	79.781 +/- 0.005
Volume (A**3)	2676.3 +/- 0.5
Mosaicity (°)	1.256 +/- 0.004

Data collection

Summary

Total number of images collected	151
Total exposure time	49.6 minutes
Data collection exposure time	48.2 minutes
Data collection wall-clock time	60.1 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	76	`152.0`° phi	2.000°	20 seconds	Yes
data collection	s02f	67	`134.0`° omega	2.000°	20 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`104`
Zero sigma or profile test	`5`
Overload or incomplete profile	`662`
Sigma cutoff	`13`
High resolution limit	`12`

Final Data Set

Scale factor range	10.00-16.05
Number of 'full' reflections	`3894`
Number of 'partial' reflections	`12407`
Total number of integrated reflections	`13171`
Total number of unique reflections	`8531`
Data completeness	`68.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`91.7`
Average Sigma(I)	`4.8`
Overall R-merge (linear)	`0.040`

Sadabs Results

Parameter refinement on 8089 reflections reduced R(int) from 0.1491 to 0.0380

Before rejection, 15426 reflections total and 9597 unique

After rejection, 15089 reflections total and 9565 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.9  0.0410   0.783 - 0.935   0.895 - 1.289   1.521    7789    6118
    2  -18.3  0.0441   0.775 - 1.323   0.860 - 1.067   1.492    7300    5650

Ratio of minimum to maximum apparent transmission: 0.666984

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. M. A. Beckett

Local Code MAB/CP/02 BANGOR

Formula C24 H28 B3 P1

Crystal Colour Colourless

Crystal Habit Rod

Crystal Size 0.42 x 0.1 x 0.08 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. M. A. Beckett
Local Code	MAB/CP/02 BANGOR
Formula	C24 H28 B3 P1
Crystal Colour	Colourless
Crystal Habit	Rod
Crystal Size	0.42 x 0.1 x 0.08 (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/