Summary report for Directory: home/diska/2005src1099

Report generated Sep 07, 2005; 08:00:20

Unit cell

7845 reflections with 2.91°<theta<27.10° (resolution between 7.00A and 0.78A) were used for unit cell refinement

Symmetry used
in scalepack p1

a (Angstrom) 9.9069 +/- 0.0003

b (Angstrom) 12.5182 +/- 0.0004

c (Angstrom) 15.4400 +/- 0.0004

alpha (°) 102.1218 +/- 0.0017

beta (°) 94.7642 +/- 0.0015

gamma (°) 101.8131 +/- 0.0013

Volume (A**3) 1816.51 +/- 0.09
Mosaicity (°) 0.8630 +/- 0.0010

Symmetry used in scalepack	p1
a (Angstrom)	9.9069 +/- 0.0003
b (Angstrom)	12.5182 +/- 0.0004
c (Angstrom)	15.4400 +/- 0.0004
alpha (°)	102.1218 +/- 0.0017
beta (°)	94.7642 +/- 0.0015
gamma (°)	101.8131 +/- 0.0013
Volume (A**3)	1816.51 +/- 0.09
Mosaicity (°)	0.8630 +/- 0.0010

Data collection

Summary

Total number of images collected	591
Total exposure time	12.2 hours
Data collection exposure time	12.2 hours
Data collection wall-clock time	13.1 hours

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	363	`363.0`° phi	1.000°	75 seconds	Yes
data collection	s02f	33	`33.0`° omega	1.000°	75 seconds	Yes
data collection	s03f	34	`34.0`° omega	1.000°	75 seconds	Yes
data collection	s04f	108	`108.0`° omega	1.000°	75 seconds	Yes
data collection	s05f	45	`45.0`° omega	1.000°	75 seconds	Yes
Phi/Chi	i01f - i08f	8			15 seconds

Scalepack Scaling

Deleted observations

Rejected	`240`
Zero sigma or profile test	`2`
Overload or incomplete profile	`1580`
Sigma cutoff	`55`
High resolution limit	`77`

Final Data Set

Scale factor range	4.91-12.54
Number of 'full' reflections	`1857`
Number of 'partial' reflections	`37511`
Total number of integrated reflections	`37411`
Total number of unique reflections	`7999`
Data completeness	`99.6%`
Resolution range	7.00-0.78 A
Theta range	2.91°-27.10°
Average Intensity	`37.1`
Average Sigma(I)	`2.0`
Overall R-merge (linear)	`0.098`

Sadabs Results

Parameter refinement on 24171 reflections reduced R(int) from 0.1157 to 0.0625

Before rejection, 37501 reflections total and 8035 unique

After rejection, 36890 reflections total and 8033 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    6.4  0.0795   0.784 - 1.178   0.935 - 1.243   1.385   22999   16196
    2   -5.8  0.0851   0.743 - 0.850   0.946 - 1.102   1.353    2046    1381
    3   -5.8  0.0694   0.753 - 0.823   0.996 - 1.109   1.303    2040    1459
    4   -5.8  0.0815   0.805 - 1.018   0.930 - 1.149   1.352    7012    4961
    5   -5.8  0.1756   0.726 - 0.951   0.953 - 1.169   1.607    2793    1379

Ratio of minimum to maximum apparent transmission: 0.748466

Metadata

Group Service

Operator Simon Coles

Sample Owner Butler

Local Code ADS30

Formula C34H38N2BrPPdFe

Crystal Colour Orange

Crystal Habit Plate

Crystal Size 0.08 x 0.03 x 0.01 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Simon Coles
Sample Owner	Butler
Local Code	ADS30
Formula	C34H38N2BrPPdFe
Crystal Colour	Orange
Crystal Habit	Plate
Crystal Size	0.08 x 0.03 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 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/