Summary report for Directory: home/diska/2007src1055

Report generated Aug 03, 2007; 16:34:30

Unit cell

12338 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) 5.37320 +/- 0.00010

b (Angstrom) 13.4962 +/- 0.0004

c (Angstrom) 15.8088 +/- 0.0005

alpha (°) 95.3885 +/- 0.0013

beta (°) 98.4984 +/- 0.0017

gamma (°) 101.2010 +/- 0.0018

Volume (A**3) 1103.32 +/- 0.05
Mosaicity (°) 0.442 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	5.37320 +/- 0.00010
b (Angstrom)	13.4962 +/- 0.0004
c (Angstrom)	15.8088 +/- 0.0005
alpha (°)	95.3885 +/- 0.0013
beta (°)	98.4984 +/- 0.0017
gamma (°)	101.2010 +/- 0.0018
Volume (A**3)	1103.32 +/- 0.05
Mosaicity (°)	0.442 +/- 0.002

Data collection

Summary

Total number of images collected	327
Total exposure time	44.9 minutes
Data collection exposure time	44.2 minutes
Data collection wall-clock time	68.3 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	181	`362.0`° phi	2.000°	8 seconds	Yes
data collection	s02f	13	`26.0`° omega	2.000°	8 seconds	Yes
data collection	s03f	52	`104.0`° omega	2.000°	8 seconds	Yes
data collection	s04f	24	`48.0`° omega	2.000°	8 seconds	Yes
data collection	s05f	49	`98.0`° omega	2.000°	8 seconds	Yes
Phi/Chi	i01f - i08f	8			5 seconds

Scalepack Scaling

Deleted observations

Rejected	`2`
Zero sigma or profile test	`1`
Overload or incomplete profile	`592`
Sigma cutoff	`198`
High resolution limit	`78`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`15000`
Number of 'partial' reflections	`7121`
Total number of integrated reflections	`21197`
Total number of unique reflections	`5008`
Data completeness	`99.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`40.6`
Average Sigma(I)	`1.3`
Overall R-merge (linear)	`0.216`

Sadabs Results

Parameter refinement on 15813 reflections reduced R(int) from 0.1450 to 0.0586

Before rejection, 21050 reflections total and 5052 unique

After rejection, 18538 reflections total and 5028 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0651   0.830 - 1.248   0.983 - 1.130   2.149   10628    7755
    2   11.1  0.0571   0.510 - 0.610   0.995 - 1.050   2.057     657     509
    3   11.1  0.0482   0.519 - 0.959   0.984 - 1.040   1.949    3052    2474
    4   11.1  0.0528   0.839 - 0.984   0.997 - 1.062   2.062    1350    1039
    5   11.1  0.0543   0.511 - 0.994   0.998 - 1.118   2.055    2851    2138

Ratio of minimum to maximum apparent transmission: 0.870535

Metadata

Group Service

Operator Louise Male

Sample Owner Dr John Spencer

Local Code Sami cyclohexanone

Formula C14 H15 N1 O1

Crystal Colour Pale Brown

Crystal Habit Needle

Crystal Size 0.85 x 0.08 x 0.06 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Louise Male
Sample Owner	Dr John Spencer
Local Code	Sami cyclohexanone
Formula	C14 H15 N1 O1
Crystal Colour	Pale Brown
Crystal Habit	Needle
Crystal Size	0.85 x 0.08 x 0.06 (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/