Summary report for Directory: diska/04src0562

Report generated Jul 20, 2004; 09:01:23

Unit cell

3410 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) 8.3045 +/- 0.0007

b (Angstrom) 7.9058 +/- 0.0004

c (Angstrom) 24.205 +/- 0.002

alpha (°) 90.000

beta (°) 92.368 +/- 0.003

gamma (°) 90.000

Volume (A**3) 1587.8 +/- 0.2
Mosaicity (°) 0.398 +/- 0.003

Symmetry used in scalepack	p2
a (Angstrom)	8.3045 +/- 0.0007
b (Angstrom)	7.9058 +/- 0.0004
c (Angstrom)	24.205 +/- 0.002
alpha (°)	90.000
beta (°)	92.368 +/- 0.003
gamma (°)	90.000
Volume (A**3)	1587.8 +/- 0.2
Mosaicity (°)	0.398 +/- 0.003

Data collection

Summary

Total number of images collected	170
Total exposure time	14.6 hours
Data collection exposure time	14.4 hours
Data collection wall-clock time	14.7 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	93	`186.0`° phi	2.000°	320 seconds	Yes
data collection	s02f	19	`38.0`° omega	2.000°	320 seconds	Yes
data collection	s03f	50	`100.0`° omega	2.000°	320 seconds	Yes
Phi/Chi	i01f - i08f	8			100 seconds

Scalepack Scaling

Deleted observations

Rejected	`118`
Zero sigma or profile test	`120`
Overload or incomplete profile	`546`
Sigma cutoff	`28`
High resolution limit	`32`

Final Data Set

Scale factor range	9.07-10.04
Number of 'full' reflections	`13870`
Number of 'partial' reflections	`5709`
Total number of integrated reflections	`18884`
Total number of unique reflections	`3694`
Data completeness	`95.0%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`6.0`
Average Sigma(I)	`1.0`
Overall R-merge (linear)	`0.200`

Sadabs Results

Parameter refinement on 5401 reflections reduced R(int) from 0.0839 to 0.0615

Before rejection, 18385 reflections total and 3701 unique

After rejection, 17886 reflections total and 3695 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    2.4  0.2164   0.977 - 1.086   0.941 - 1.100   1.212   10365    4005
    2   -1.8  0.2126   0.441 - 0.478   0.933 - 1.100   1.259    1970     723
    3   -1.8  0.2096   0.946 - 1.073   0.948 - 1.048   1.183    5551    2110

Ratio of minimum to maximum apparent transmission: 0.847886

Metadata

Group Service

Operator Simon Coles

Sample Owner Pelter

Local Code AP / RTP 26

Formula C38 H48 B2 Sn

Crystal Colour Colourless

Crystal Habit Plate

Crystal Size 0.08 x 0.06 x 0.01 (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 26
Formula	C38 H48 B2 Sn
Crystal Colour	Colourless
Crystal Habit	Plate
Crystal Size	0.08 x 0.06 x 0.01 (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/