Summary report for Directory: diska/04src0437

Report generated Jun 04, 2004; 08:41:39

Unit cell

9833 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) 15.6008 +/- 0.0002

b (Angstrom) 12.4267 +/- 0.0002

c (Angstrom) 23.0629 +/- 0.0003

alpha (°) 90.000

beta (°) 109.1068 +/- 0.0007

gamma (°) 90.000

Volume (A**3) 4224.81 +/- 0.10
Mosaicity (°) 0.4310 +/- 0.0010

Symmetry used in scalepack	p2
a (Angstrom)	15.6008 +/- 0.0002
b (Angstrom)	12.4267 +/- 0.0002
c (Angstrom)	23.0629 +/- 0.0003
alpha (°)	90.000
beta (°)	109.1068 +/- 0.0007
gamma (°)	90.000
Volume (A**3)	4224.81 +/- 0.10
Mosaicity (°)	0.4310 +/- 0.0010

Data collection

Summary

Total number of images collected	432
Total exposure time	14.2 hours
Data collection exposure time	14.2 hours
Data collection wall-clock time	14.8 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	40.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	282	`282.0`° phi	1.000°	120 seconds	Yes
data collection	s02f	63	`63.0`° omega	1.000°	120 seconds	Yes
data collection	s03f	79	`79.0`° omega	1.000°	120 seconds	Yes
Phi/Chi	i01f - i08f	8			30 seconds

Scalepack Scaling

Deleted observations

Rejected	`216`
Zero sigma or profile test	`9`
Overload or incomplete profile	`1282`
Sigma cutoff	`18`
High resolution limit	`43`

Final Data Set

Scale factor range	9.83-10.79
Number of 'full' reflections	`19624`
Number of 'partial' reflections	`25821`
Total number of integrated reflections	`42574`
Total number of unique reflections	`10083`
Data completeness	`99.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`86.9`
Average Sigma(I)	`2.8`
Overall R-merge (linear)	`0.033`

Sadabs Results

Parameter refinement on 35442 reflections reduced R(int) from 0.0497 to 0.0301

Before rejection, 44308 reflections total and 10119 unique

After rejection, 43879 reflections total and 10114 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.6  0.0318   1.039 - 1.168   0.942 - 1.082   1.157   29279   24817
    2  -15.0  0.0325   1.019 - 1.085   0.982 - 1.112   1.124    6416    5297
    3   15.0  0.0319   0.607 - 0.657   0.961 - 1.053   1.185    8184    6848

Ratio of minimum to maximum apparent transmission: 0.846865

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. Ian Butler

Local Code 6-163

Formula C30 H52 Cl2 Fe1 P2 Pd2

Crystal Colour Orange

Crystal Habit Sheet

Crystal Size 0.24 x 0.18 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. Ian Butler
Local Code	6-163
Formula	C30 H52 Cl2 Fe1 P2 Pd2
Crystal Colour	Orange
Crystal Habit	Sheet
Crystal Size	0.24 x 0.18 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    'graphite'
_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. SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10

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/