Summary report for Directory: diska/04src0560

Report generated Jul 19, 2004; 15:16:57

Unit cell

5953 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) 8.5267 +/- 0.0003

b (Angstrom) 9.6619 +/- 0.0003

c (Angstrom) 21.9357 +/- 0.0009

alpha (°) 86.769 +/- 0.002

beta (°) 85.9878 +/- 0.0014

gamma (°) 84.710 +/- 0.002

Volume (A**3) 1792.78 +/- 0.11
Mosaicity (°) 0.632 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	8.5267 +/- 0.0003
b (Angstrom)	9.6619 +/- 0.0003
c (Angstrom)	21.9357 +/- 0.0009
alpha (°)	86.769 +/- 0.002
beta (°)	85.9878 +/- 0.0014
gamma (°)	84.710 +/- 0.002
Volume (A**3)	1792.78 +/- 0.11
Mosaicity (°)	0.632 +/- 0.002

Data collection

Summary

Total number of images collected	270
Total exposure time	45.2 minutes
Data collection exposure time	44.6 minutes
Data collection wall-clock time	69.5 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	40.00 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°	10 seconds	Yes
data collection	s02f	18	`36.0`° omega	2.000°	10 seconds	Yes
data collection	s03f	31	`62.0`° omega	2.000°	10 seconds	Yes
data collection	s04f	32	`64.0`° omega	2.000°	10 seconds	Yes
Phi/Chi	i01f - i08f	8			4 seconds

Scalepack Scaling

Deleted observations

Rejected	`908`
Zero sigma or profile test	`2`
Overload or incomplete profile	`912`
Sigma cutoff	`3`
High resolution limit	`42`

Final Data Set

Scale factor range	9.01-10.80
Number of 'full' reflections	`12422`
Number of 'partial' reflections	`8876`
Total number of integrated reflections	`18852`
Total number of unique reflections	`7327`
Data completeness	`89.3%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`104.9`
Average Sigma(I)	`4.0`
Overall R-merge (linear)	`0.041`

Sadabs Results

Parameter refinement on 18168 reflections reduced R(int) from 0.0919 to 0.0484

Before rejection, 20976 reflections total and 7686 unique

After rejection, 19857 reflections total and 7627 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.6  0.0462   0.909 - 1.139   0.956 - 1.144   1.460   14345   13367
    2  -13.2  0.0530   0.753 - 0.813   0.956 - 1.050   1.621    1176    1092
    3  -15.0  0.0476   0.895 - 0.969   0.956 - 1.080   1.657    2100    1989
    4  -15.0  0.0481   0.709 - 0.765   0.974 - 1.154   1.622    2236    2032

Ratio of minimum to maximum apparent transmission: 0.828604

Metadata

Group Service

Operator Simon Coles

Sample Owner Pelter

Local Code AP/RTP 24

Formula C40H54B2Sn

Crystal Colour Colourless

Crystal Habit Slab

Crystal Size 0.6 x 0.32 x 0.2 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Pelter
Local Code	AP/RTP 24
Formula	C40H54B2Sn
Crystal Colour	Colourless
Crystal Habit	Slab
Crystal Size	0.6 x 0.32 x 0.2 (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. 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/