Summary report for Directory: home/diska/2005slh0421

Report generated May 08, 2005; 17:08:53

Unit cell

5860 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) 9.2600 +/- 0.0003

b (Angstrom) 10.4422 +/- 0.0003

c (Angstrom) 15.0672 +/- 0.0004

alpha (°) 79.2581 +/- 0.0015

beta (°) 84.6705 +/- 0.0017

gamma (°) 65.4151 +/- 0.0015

Volume (A**3) 1301.44 +/- 0.07
Mosaicity (°) 0.551 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	9.2600 +/- 0.0003
b (Angstrom)	10.4422 +/- 0.0003
c (Angstrom)	15.0672 +/- 0.0004
alpha (°)	79.2581 +/- 0.0015
beta (°)	84.6705 +/- 0.0017
gamma (°)	65.4151 +/- 0.0015
Volume (A**3)	1301.44 +/- 0.07
Mosaicity (°)	0.551 +/- 0.002

Data collection

Summary

Total number of images collected	296
Total exposure time	195.7 minutes
Data collection exposure time	193.0 minutes
Data collection wall-clock time	218.9 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	181	`362.0`° phi	2.000°	40 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	40 seconds	Yes
data collection	s03f	16	`32.0`° omega	2.000°	40 seconds	Yes
data collection	s04f	22	`44.0`° omega	2.000°	40 seconds	Yes
data collection	s05f	53	`106.0`° omega	2.000°	40 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`140`
Overload or incomplete profile	`734`
Sigma cutoff	`10`

Final Data Set

Scale factor range	9.89-18.67
Number of 'full' reflections	`16926`
Number of 'partial' reflections	`11135`
Total number of integrated reflections	`27063`
Total number of unique reflections	`5970`
Data completeness	`99.0%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`39.5`
Average Sigma(I)	`1.6`
Overall R-merge (linear)	`0.061`

Sadabs Results

Parameter refinement on 19332 reflections reduced R(int) from 0.1112 to 0.0514

Before rejection, 26574 reflections total and 5959 unique

After rejection, 26223 reflections total and 5958 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0602   1.034 - 1.670   0.953 - 1.150   1.358   16666   12637
    2   -6.8  0.0661   0.487 - 0.544   0.953 - 1.085   1.381    1332     982
    3   -6.8  0.0547   1.010 - 1.117   0.965 - 1.093   1.340    1334    1059
    4   -6.8  0.0690   0.483 - 0.607   0.953 - 1.094   1.387    1925    1427
    5   -6.8  0.0507   0.519 - 0.604   0.953 - 1.111   1.243    4966    3975

Ratio of minimum to maximum apparent transmission: 0.828724

Metadata

Group Mike Hursthouse

Operator Susanne Huth

Sample Owner

Local Code CAG 149

Formula C34 H32 N6 O4 P2 S4 Ni1

Crystal Colour Red

Crystal Habit Lath

Crystal Size 0.12 x 0.04 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Susanne Huth
Sample Owner
Local Code	CAG 149
Formula	C34 H32 N6 O4 P2 S4 Ni1
Crystal Colour	Red
Crystal Habit	Lath
Crystal Size	0.12 x 0.04 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 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/