Summary report for Directory: home/diska/2007sot0277

Report generated Feb 22, 2007; 10:48:07

Unit cell

3504 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) 11.0537 +/- 0.0003

b (Angstrom) 11.9883 +/- 0.0004

c (Angstrom) 11.2576 +/- 0.0004

alpha (°) 90.000

beta (°) 96.476 +/- 0.002

gamma (°) 90.000

Volume (A**3) 1482.28 +/- 0.08
Mosaicity (°) 0.537 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	11.0537 +/- 0.0003
b (Angstrom)	11.9883 +/- 0.0004
c (Angstrom)	11.2576 +/- 0.0004
alpha (°)	90.000
beta (°)	96.476 +/- 0.002
gamma (°)	90.000
Volume (A**3)	1482.28 +/- 0.08
Mosaicity (°)	0.537 +/- 0.002

Data collection

Summary

Total number of images collected	232
Total exposure time	77.2 minutes
Data collection exposure time	75.9 minutes
Data collection wall-clock time	85.7 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	51	`102.0`° omega	2.000°	20 seconds	Yes
data collection	s02f	50	`100.0`° omega	2.000°	20 seconds	Yes
data collection	s03f	25	`50.0`° omega	2.000°	20 seconds	Yes
data collection	s04f	51	`102.0`° omega	2.000°	20 seconds	Yes
data collection	s05f	47	`94.0`° omega	2.000°	20 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`565`
Zero sigma or profile test	`2`
Overload or incomplete profile	`814`
Sigma cutoff	`509`
High resolution limit	`37`

Final Data Set

Scale factor range	8.98-13.28
Number of 'full' reflections	`13377`
Number of 'partial' reflections	`8777`
Total number of integrated reflections	`20568`
Total number of unique reflections	`3562`
Data completeness	`99.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`43.9`
Average Sigma(I)	`1.1`
Overall R-merge (linear)	`0.065`

Sadabs Results

Parameter refinement on 10298 reflections reduced R(int) from 0.0952 to 0.0449

Before rejection, 20984 reflections total and 3586 unique

After rejection, 18233 reflections total and 3573 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    3.7  0.0596   0.934 - 1.235   0.986 - 1.097   2.082    4299    1968
    2   10.2  0.0471   0.700 - 0.950   0.964 - 1.033   2.044    4074    1993
    3   10.2  0.0572   0.561 - 0.719   0.976 - 1.055   2.076    1912     883
    4    7.3  0.0552   0.888 - 1.239   0.950 - 1.050   2.019    4270    1992
    5   10.2  0.0484   0.804 - 0.976   1.002 - 1.083   2.021    3678    1758

Ratio of minimum to maximum apparent transmission: 0.866271

Metadata

Group Departmental

Operator Mark Light

Supervisor Phil Gale

Sample Owner Gareth Bates

Local Code

Formula C12 H12 N2 O2

Crystal Colour Colourless

Crystal Habit Block

Crystal Size 0.2 x 0.2 x 0.1 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Departmental
Operator	Mark Light
Supervisor	Phil Gale
Sample Owner	Gareth Bates
Local Code
Formula	C12 H12 N2 O2
Crystal Colour	Colourless
Crystal Habit	Block
Crystal Size	0.2 x 0.2 x 0.1 (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/