Summary report for Directory: diska/2005src1110

Report generated Oct 20, 2005; 15:52:53

Unit cell

8850 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) 10.0682 +/- 0.0011

b (Angstrom) 15.0129 +/- 0.0018

c (Angstrom) 17.284 +/- 0.002

alpha (°) 67.130 +/- 0.006

beta (°) 78.309 +/- 0.007

gamma (°) 77.734 +/- 0.006

Volume (A**3) 2331.2 +/- 0.5
Mosaicity (°) 2.505 +/- 0.004

Symmetry used in scalepack	p1
a (Angstrom)	10.0682 +/- 0.0011
b (Angstrom)	15.0129 +/- 0.0018
c (Angstrom)	17.284 +/- 0.002
alpha (°)	67.130 +/- 0.006
beta (°)	78.309 +/- 0.007
gamma (°)	77.734 +/- 0.006
Volume (A**3)	2331.2 +/- 0.5
Mosaicity (°)	2.505 +/- 0.004

Data collection

Summary

Total number of images collected	346
Total exposure time	15.3 hours
Data collection exposure time	15.0 hours
Data collection wall-clock time	15.6 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	35.00 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°	160 seconds	Yes
data collection	s02f	17	`34.0`° omega	2.000°	160 seconds	Yes
data collection	s03f	16	`32.0`° omega	2.000°	160 seconds	Yes
data collection	s04f	16	`32.0`° omega	2.000°	160 seconds	Yes
data collection	s05f	59	`118.0`° omega	2.000°	160 seconds	Yes
data collection	s06f	27	`54.0`° omega	2.000°	160 seconds	Yes
data collection	s07f	22	`44.0`° omega	2.000°	160 seconds	Yes
Phi/Chi	i01f - i08f	8			100 seconds

Scalepack Scaling

Deleted observations

Rejected	`651`
Zero sigma or profile test	`1177`
Overload or incomplete profile	`3214`
Sigma cutoff	`808`
Low resolution limit	`3`
High resolution limit	`1700`

Final Data Set

Scale factor range	1.47-10.45
Number of 'full' reflections	`0`
Number of 'partial' reflections	`44081`
Total number of integrated reflections	`37130`
Total number of unique reflections	`10038`
Data completeness	`95.6%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`27.1`
Average Sigma(I)	`5.5`
Overall R-merge (linear)	`0.230`

Sadabs Results

Parameter refinement on 14369 reflections reduced R(int) from 0.2070 to 0.0874

Before rejection, 41235 reflections total and 10691 unique

After rejection, 39657 reflections total and 10683 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.1488   0.817 - 1.511   0.901 - 1.328   1.315   22809   11290
    2   -9.8  0.5816   0.837 - 0.962   0.919 - 1.314   1.595    1721     359
    3  -11.2  0.7376   1.278 - 1.628   0.970 - 1.239   1.561    1044     151
    4  -11.2  0.7345   0.980 - 1.218   0.950 - 1.127   1.566    1006     123
    5  -11.2  0.2632   0.486 - 1.111   0.919 - 1.253   1.441    7368    2583
    6  -11.2  0.2523   0.953 - 1.139   0.948 - 1.355   1.464    3180    1033
    7  -11.2  0.2248   0.285 - 0.361   0.952 - 1.131   1.427    2529    1081

Sadabs Results

Parameter refinement on 14650 reflections reduced R(int) from 0.2003 to 0.1101

Before rejection, 44189 reflections total and 10644 unique

After rejection, 42586 reflections total and 10640 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -11.8  0.1737   0.501 - 0.924   0.891 - 1.362   1.325   22428   10349
    2    9.8  0.5993   2.102 - 2.476   0.974 - 1.141   1.550    2150     431
    3   11.2  0.8501   2.528 - 3.339   0.911 - 1.469   1.580    2005     281
    4   11.2  1.0499   4.208 - 5.252   0.891 - 1.267   1.562    2022     274
    5   11.2  0.3378   0.693 - 1.640   0.930 - 1.520   1.467    7743    2451
    6   11.2  0.2959   1.178 - 1.383   0.987 - 1.311   1.439    3497    1098
    7   11.2  0.2443   0.693 - 0.962   0.891 - 1.374   1.452    2741    1082

Ratio of minimum to maximum apparent transmission: 0.665167

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. S. S. Turner

Local Code PM002

Formula C42 H24 N6 S10 Fe1 Zn1

Crystal Colour Dark Red

Crystal Habit Plate

Crystal Size 0.1 x 0.05 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. S. S. Turner
Local Code	PM002
Formula	C42 H24 N6 S10 Fe1 Zn1
Crystal Colour	Dark Red
Crystal Habit	Plate
Crystal Size	0.1 x 0.05 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/