Summary report for Directory: home/diska/2007src0806

Report generated Jul 02, 2007; 12:04:53

Unit cell

37147 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) 11.9359 +/- 0.0003

b (Angstrom) 17.2845 +/- 0.0005

c (Angstrom) 21.4406 +/- 0.0006

alpha (°) 90.000

beta (°) 92.5812 +/- 0.0017

gamma (°) 90.000

Volume (A**3) 4418.8 +/- 0.2
Mosaicity (°) 0.655 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	11.9359 +/- 0.0003
b (Angstrom)	17.2845 +/- 0.0005
c (Angstrom)	21.4406 +/- 0.0006
alpha (°)	90.000
beta (°)	92.5812 +/- 0.0017
gamma (°)	90.000
Volume (A**3)	4418.8 +/- 0.2
Mosaicity (°)	0.655 +/- 0.002

Data collection

Summary

Total number of images collected	219
Total exposure time	65.8 minutes
Data collection exposure time	64.4 minutes
Data collection wall-clock time	73.9 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	33.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	151	`271.8`° phi	1.800°	18 seconds	Yes
data collection	s02f	60	`108.0`° omega	1.800°	18 seconds	Yes
Phi/Chi	i01f - i08f	8			10 seconds

Scalepack Scaling

Deleted observations

Rejected	`5`
Zero sigma or profile test	`1`
Overload or incomplete profile	`1370`
Sigma cutoff	`1270`
Low resolution limit	`7`
High resolution limit	`10`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`24124`
Number of 'partial' reflections	`23892`
Total number of integrated reflections	`43441`
Total number of unique reflections	`10460`
Data completeness	`99.2%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`27.3`
Average Sigma(I)	`1.7`
Overall R-merge (linear)	`0.200`

Sadabs Results

Parameter refinement on 26414 reflections reduced R(int) from 0.1725 to 0.0665

Before rejection, 46160 reflections total and 10522 unique

After rejection, 39822 reflections total and 10445 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   13.5  0.0931   0.729 - 1.227   0.986 - 1.152   2.093   28357   15810
    2   12.9  0.0944   0.579 - 0.871   0.990 - 1.122   2.044   11465    6257

Ratio of minimum to maximum apparent transmission: 0.855616

Metadata

Group Service

Operator Louise Male

Sample Owner Dr Simon Aldridge

Local Code AEJB 31

Formula C29 H31 Fe1 B1 N1

Crystal Colour Orange

Crystal Habit Plate

Crystal Size 0.09 x 0.05 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Louise Male
Sample Owner	Dr Simon Aldridge
Local Code	AEJB 31
Formula	C29 H31 Fe1 B1 N1
Crystal Colour	Orange
Crystal Habit	Plate
Crystal Size	0.09 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 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/