Summary report for Directory: diska/2009src0656

Report generated Jul 07, 2009; 07:37:46

Unit cell

107917 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) 13.1678 +/- 0.0012

b (Angstrom) 10.7827 +/- 0.0012

c (Angstrom) 16.8284 +/- 0.0018

alpha (°) 90.000

beta (°) 90.022 +/- 0.006

gamma (°) 90.000

Volume (A**3) 2389.4 +/- 0.4
Mosaicity (°) 2.886 +/- 0.003

Symmetry used in scalepack	p2
a (Angstrom)	13.1678 +/- 0.0012
b (Angstrom)	10.7827 +/- 0.0012
c (Angstrom)	16.8284 +/- 0.0018
alpha (°)	90.000
beta (°)	90.022 +/- 0.006
gamma (°)	90.000
Volume (A**3)	2389.4 +/- 0.4
Mosaicity (°)	2.886 +/- 0.003

Data collection

Summary

Total number of images collected	477
Total exposure time	10.6 hours
Data collection exposure time	10.5 hours
Data collection wall-clock time	10.8 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	36.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	247	`247.0`° phi	1.000°	80 seconds	Yes
data collection	s02f	56	`56.0`° omega	1.000°	80 seconds	Yes
data collection	s03f	26	`26.0`° omega	1.000°	80 seconds	Yes
data collection	s04f	93	`93.0`° omega	1.000°	80 seconds	Yes
data collection	s05f	47	`47.0`° omega	1.000°	80 seconds	Yes
Phi/Chi	i01f - i08f	8			50 seconds

Scalepack Scaling

Deleted observations

Rejected	`3`
Zero sigma or profile test	`7`
Overload or incomplete profile	`1218`
Sigma cutoff	`1794`
High resolution limit	`360`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`0`
Number of 'partial' reflections	`21964`
Total number of integrated reflections	`13738`
Total number of unique reflections	`4756`
Data completeness	`83.3%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`195.4`
Average Sigma(I)	`8.2`
Overall R-merge (linear)	`0.145`

Sadabs Results

Parameter refinement on 16919 reflections reduced R(int) from 0.1266 to 0.0657

Before rejection, 26543 reflections total and 5779 unique

After rejection, 22407 reflections total and 5738 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.9  0.0585   0.751 - 1.007   0.786 - 1.286   2.025   11846    7713
    2   15.6  0.1368   0.797 - 1.138   0.995 - 1.295   2.489    2611    1237
    3   15.4  0.0622   0.653 - 0.740   0.988 - 1.166   2.088    1094     720
    4   15.4  0.0667   0.721 - 1.074   0.906 - 1.460   2.062    4648    3078
    5   15.4  0.0843   0.747 - 0.913   0.995 - 1.255   2.195    2208    1287

Ratio of minimum to maximum apparent transmission: 0.538150

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr NC Fletcher

Local Code CTMN0163B

Formula C20 H24 N3 Cl Ru B F4

Crystal Colour Yellow

Crystal Habit Shard

Crystal Size 0.16 x 0.04 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr NC Fletcher
Local Code	CTMN0163B
Formula	C20 H24 N3 Cl Ru B F4
Crystal Colour	Yellow
Crystal Habit	Shard
Crystal Size	0.16 x 0.04 x 0.02 (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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/