Summary report for Directory: diska/2009src0113

Report generated Feb 11, 2009; 12:22:55

Unit cell

25207 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) 15.8650 +/- 0.0012

b (Angstrom) 5.6205 +/- 0.0004

c (Angstrom) 16.4742 +/- 0.0012

alpha (°) 90.000

beta (°) 106.779 +/- 0.004

gamma (°) 90.000

Volume (A**3) 1406.45 +/- 0.18
Mosaicity (°) 1.197 +/- 0.004

Symmetry used in scalepack	p2
a (Angstrom)	15.8650 +/- 0.0012
b (Angstrom)	5.6205 +/- 0.0004
c (Angstrom)	16.4742 +/- 0.0012
alpha (°)	90.000
beta (°)	106.779 +/- 0.004
gamma (°)	90.000
Volume (A**3)	1406.45 +/- 0.18
Mosaicity (°)	1.197 +/- 0.004

Data collection

Summary

Total number of images collected	227
Total exposure time	114.0 minutes
Data collection exposure time	110.7 minutes
Data collection wall-clock time	120.5 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	51	`102.0`° omega	2.000°	30 seconds	Yes
data collection	s02f	48	`96.0`° omega	2.000°	30 seconds	Yes
data collection	s03f	47	`94.0`° omega	2.000°	30 seconds	Yes
data collection	s04f	44	`88.0`° omega	2.000°	30 seconds	Yes
data collection	s05f	29	`58.0`° omega	2.000°	30 seconds	Yes
Phi/Chi	i01f - i08f	8			25 seconds

Scalepack Scaling

Deleted observations

Rejected	`3`
Zero sigma or profile test	`8`
Overload or incomplete profile	`872`
Sigma cutoff	`632`
High resolution limit	`93`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`5030`
Number of 'partial' reflections	`16180`
Total number of integrated reflections	`18568`
Total number of unique reflections	`3516`
Data completeness	`99.4%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`12.3`
Average Sigma(I)	`1.0`
Overall R-merge (linear)	`0.257`

Sadabs Results

Parameter refinement on 9735 reflections reduced R(int) from 0.1641 to 0.0828

Before rejection, 19193 reflections total and 3567 unique

After rejection, 16409 reflections total and 3556 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    3.2  0.1233   0.591 - 1.143   0.974 - 1.552   1.981    3864    1908
    2   10.2  0.1334   0.635 - 1.031   0.975 - 1.187   2.017    3595    1651
    3   10.2  0.1344   0.750 - 1.094   0.974 - 1.347   2.056    3552    1681
    4    6.5  0.1324   0.684 - 0.987   1.003 - 1.355   2.062    3406    1516
    5   10.2  0.1619   0.646 - 0.819   0.989 - 1.379   2.046    1992     853

Ratio of minimum to maximum apparent transmission: 0.627880

Metadata

Group Service

Operator Sam Callear

Sample Owner Dr J Spencer

Local Code HP153(C)AMINO

Formula C16H17FN4O

Crystal Colour Colourless

Crystal Habit Lath

Crystal Size 0.43 x 0.05 x 0.01 (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	HP153(C)AMINO
Formula	C16H17FN4O
Crystal Colour	Colourless
Crystal Habit	Lath
Crystal Size	0.43 x 0.05 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 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/