Summary report for Directory: diska/2009src0216r

Report generated Mar 02, 2009; 18:05:44

Unit cell

16828 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) 6.2066 +/- 0.0003

b (Angstrom) 17.1960 +/- 0.0008

c (Angstrom) 15.1712 +/- 0.0006

alpha (°) 90.000

beta (°) 90.442 +/- 0.003

gamma (°) 90.000

Volume (A**3) 1619.15 +/- 0.13
Mosaicity (°) 0.626 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	6.2066 +/- 0.0003
b (Angstrom)	17.1960 +/- 0.0008
c (Angstrom)	15.1712 +/- 0.0006
alpha (°)	90.000
beta (°)	90.442 +/- 0.003
gamma (°)	90.000
Volume (A**3)	1619.15 +/- 0.13
Mosaicity (°)	0.626 +/- 0.002

Data collection

Summary

Total number of images collected	251
Total exposure time	149.1 minutes
Data collection exposure time	147.1 minutes
Data collection wall-clock time	160.1 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	32.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	123	`246.0`° phi	2.000°	36 seconds	Yes
data collection	s02f	13	`26.0`° omega	2.000°	36 seconds	Yes
data collection	s03f	25	`50.0`° omega	2.000°	36 seconds	Yes
data collection	s04f	31	`62.0`° omega	2.000°	36 seconds	Yes
data collection	s05f	51	`102.0`° omega	2.000°	36 seconds	Yes
Phi/Chi	i01f - i08f	8			15 seconds

Scalepack Scaling

Deleted observations

Rejected	`5`
Zero sigma or profile test	`7`
Overload or incomplete profile	`500`
Sigma cutoff	`446`
High resolution limit	`72`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`13323`
Number of 'partial' reflections	`10606`
Total number of integrated reflections	`22406`
Total number of unique reflections	`3822`
Data completeness	`99.9%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`13.1`
Average Sigma(I)	`0.9`
Overall R-merge (linear)	`0.206`

Sadabs Results

Parameter refinement on 13981 reflections reduced R(int) from 0.1354 to 0.0937

Before rejection, 22341 reflections total and 3847 unique

After rejection, 18947 reflections total and 3828 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   12.6  0.1294   0.724 - 0.900   0.967 - 1.222   2.045    9819    5620
    2   12.0  0.1308   0.583 - 0.608   0.967 - 1.098   2.049     899     520
    3   12.0  0.1197   0.750 - 0.849   1.014 - 1.159   2.049    1899    1128
    4   12.0  0.1195   0.732 - 0.886   0.987 - 1.152   1.990    2373    1450
    5   12.0  0.1183   0.756 - 0.943   1.014 - 1.215   1.962    3957    2374

Ratio of minimum to maximum apparent transmission: 0.791249

Metadata

Group Service

Operator Sam Callear

Sample Owner Dr J Spencer

Local Code RRPSAN02

Formula C14H21ClN3PPdS

Crystal Colour Colourless

Crystal Habit Plate

Crystal Size 0.09 x 0.07 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	RRPSAN02
Formula	C14H21ClN3PPdS
Crystal Colour	Colourless
Crystal Habit	Plate
Crystal Size	0.09 x 0.07 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/