Summary report for Directory: diska/2010src0796

Report generated Aug 24, 2010; 13:07:36

Unit cell

13752 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) 4.1302 +/- 0.0002

b (Angstrom) 12.9513 +/- 0.0009

c (Angstrom) 13.0829 +/- 0.0009

alpha (°) 62.708 +/- 0.003

beta (°) 86.496 +/- 0.004

gamma (°) 86.546 +/- 0.004

Volume (A**3) 620.35 +/- 0.07
Mosaicity (°) 0.957 +/- 0.004

Symmetry used in scalepack	p1
a (Angstrom)	4.1302 +/- 0.0002
b (Angstrom)	12.9513 +/- 0.0009
c (Angstrom)	13.0829 +/- 0.0009
alpha (°)	62.708 +/- 0.003
beta (°)	86.496 +/- 0.004
gamma (°)	86.546 +/- 0.004
Volume (A**3)	620.35 +/- 0.07
Mosaicity (°)	0.957 +/- 0.004

Data collection

Summary

Total number of images collected	324
Total exposure time	109.7 minutes
Data collection exposure time	107.0 minutes
Data collection wall-clock time	124.7 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	31.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	176	`352.0`° phi	2.000°	20 seconds	Yes
data collection	s02f	24	`48.0`° omega	2.000°	20 seconds	Yes
data collection	s03f	13	`26.0`° omega	2.000°	20 seconds	Yes
data collection	s04f	51	`102.0`° omega	2.000°	20 seconds	Yes
data collection	s05f	52	`104.0`° omega	2.000°	20 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`1`
Zero sigma or profile test	`3`
Overload or incomplete profile	`378`
Sigma cutoff	`280`
High resolution limit	`2`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`4559`
Number of 'partial' reflections	`7938`
Total number of integrated reflections	`11489`
Total number of unique reflections	`2878`
Data completeness	`98.5%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`40.5`
Average Sigma(I)	`1.7`
Overall R-merge (linear)	`0.135`

Sadabs Results

Parameter refinement on 7507 reflections reduced R(int) from 0.0900 to 0.0507

Before rejection, 11715 reflections total and 2885 unique

After rejection, 10310 reflections total and 2863 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0615   0.765 - 1.045   0.971 - 1.206   2.107    5823    3609
    2   11.1  0.0613   0.801 - 0.865   0.977 - 1.138   2.036     723     476
    3   11.1  0.0540   0.781 - 0.948   0.971 - 1.049   2.076     357     227
    4   11.1  0.0589   0.496 - 0.674   0.977 - 1.118   2.085    1686    1108
    5   11.1  0.0563   0.922 - 1.307   0.971 - 1.085   2.099    1721    1069

Ratio of minimum to maximum apparent transmission: 0.805120

Metadata

Group Service

Operator Graham Tizzard

Sample Owner Dr J Spencer

Local Code GRE.Js5

Formula C16H13N1O2

Crystal Colour Yellow

Crystal Habit Plate

Crystal Size 0.16 x 0.1 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Graham Tizzard
Sample Owner	Dr J Spencer
Local Code	GRE.Js5
Formula	C16H13N1O2
Crystal Colour	Yellow
Crystal Habit	Plate
Crystal Size	0.16 x 0.1 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/