Summary report for Directory: home/diska/2005src1012

Report generated Aug 09, 2005; 16:52:13

Unit cell

4871 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) 11.5255 +/- 0.0006

b (Angstrom) 14.0330 +/- 0.0007

c (Angstrom) 14.1936 +/- 0.0005

alpha (°) 90.000

beta (°) 113.617 +/- 0.003

gamma (°) 90.000

Volume (A**3) 2103.36 +/- 0.17
Mosaicity (°) 0.597 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	11.5255 +/- 0.0006
b (Angstrom)	14.0330 +/- 0.0007
c (Angstrom)	14.1936 +/- 0.0005
alpha (°)	90.000
beta (°)	113.617 +/- 0.003
gamma (°)	90.000
Volume (A**3)	2103.36 +/- 0.17
Mosaicity (°)	0.597 +/- 0.002

Data collection

Summary

Total number of images collected	180
Total exposure time	261.3 minutes
Data collection exposure time	258.6 minutes
Data collection wall-clock time	284.7 minutes

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	133	`266.0`° phi	2.000°	90 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	90 seconds	Yes
data collection	s03f	23	`46.0`° omega	2.000°	90 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`168`
Zero sigma or profile test	`1`
Overload or incomplete profile	`760`
Sigma cutoff	`32`

Final Data Set

Scale factor range	8.85-11.18
Number of 'full' reflections	`15447`
Number of 'partial' reflections	`11488`
Total number of integrated reflections	`26051`
Total number of unique reflections	`5021`
Data completeness	`98.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`30.6`
Average Sigma(I)	`1.9`
Overall R-merge (linear)	`0.107`

Sadabs Results

Parameter refinement on 14607 reflections reduced R(int) from 0.1054 to 0.0734

Before rejection, 25368 reflections total and 5016 unique

After rejection, 24993 reflections total and 5014 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.2  0.1016   0.756 - 1.019   0.893 - 1.272   1.387   19612   12150
    2   -6.6  0.1022   0.775 - 0.901   0.954 - 1.214   1.377    2141    1319
    3   -6.6  0.1057   0.854 - 0.948   0.956 - 1.199   1.349    3240    1991

Ratio of minimum to maximum apparent transmission: 0.702345

Metadata

Group Service

Operator Simon Coles

Sample Owner Lancaster

Local Code DP4-9

Formula C22H18N4TiCl2

Crystal Colour Black

Crystal Habit Blade

Crystal Size 0.34 x 0.04 x 0.01 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Lancaster
Local Code	DP4-9
Formula	C22H18N4TiCl2
Crystal Colour	Black
Crystal Habit	Blade
Crystal Size	0.34 x 0.04 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    '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/