Summary report for Directory: diska/2009src0462

Report generated Apr 27, 2009; 17:01:10

Unit cell

13380 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) 4.95560 +/- 0.00010

b (Angstrom) 15.8959 +/- 0.0004

c (Angstrom) 15.8659 +/- 0.0004

alpha (°) 90.000

beta (°) 92.2566 +/- 0.0016

gamma (°) 90.000

Volume (A**3) 1248.85 +/- 0.05
Mosaicity (°) 0.445 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	4.95560 +/- 0.00010
b (Angstrom)	15.8959 +/- 0.0004
c (Angstrom)	15.8659 +/- 0.0004
alpha (°)	90.000
beta (°)	92.2566 +/- 0.0016
gamma (°)	90.000
Volume (A**3)	1248.85 +/- 0.05
Mosaicity (°)	0.445 +/- 0.002

Data collection

Summary

Total number of images collected	299
Total exposure time	31.2 minutes
Data collection exposure time	30.7 minutes
Data collection wall-clock time	43.5 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	55	`82.5`° omega	1.500°	6 seconds	Yes
data collection	s02f	68	`102.0`° omega	1.500°	6 seconds	Yes
data collection	s03f	64	`96.0`° omega	1.500°	6 seconds	Yes
data collection	s04f	40	`60.0`° omega	1.500°	6 seconds	Yes
data collection	s05f	64	`96.0`° omega	1.500°	6 seconds	Yes
Phi/Chi	i01f - i08f	8			4 seconds

Scalepack Scaling

Deleted observations

Rejected	`4`
Zero sigma or profile test	`11`
Overload or incomplete profile	`572`
Sigma cutoff	`163`
High resolution limit	`28`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`10629`
Number of 'partial' reflections	`7868`
Total number of integrated reflections	`17657`
Total number of unique reflections	`2977`
Data completeness	`99.9%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`35.9`
Average Sigma(I)	`1.0`
Overall R-merge (linear)	`0.164`

Sadabs Results

Parameter refinement on 12608 reflections reduced R(int) from 0.1444 to 0.0573

Before rejection, 17375 reflections total and 2986 unique

After rejection, 15096 reflections total and 2980 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   -3.6  0.0589   1.786 - 2.532   0.965 - 1.104   2.009    2887    2102
    2   10.2  0.0513   2.363 - 3.238   0.879 - 1.046   1.995    3543    2488
    3   10.2  0.0590   0.728 - 1.096   0.973 - 1.135   2.023    3314    2350
    4   10.2  0.0746   0.334 - 0.399   0.972 - 1.115   2.141    2024    1312
    5   10.2  0.0630   0.302 - 0.671   0.999 - 1.085   1.997    3328    2341

Ratio of minimum to maximum apparent transmission: 0.774481

Metadata

Group Service

Operator Sam Callear

Sample Owner Dr J Spencer

Local Code HP166

Formula C15H11N3O2

Crystal Colour Colourless

Crystal Habit Needle

Crystal Size 0.67 x 0.07 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Sam Callear
Sample Owner	Dr J Spencer
Local Code	HP166
Formula	C15H11N3O2
Crystal Colour	Colourless
Crystal Habit	Needle
Crystal Size	0.67 x 0.07 x 0.04 (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/