Summary report for Directory: diska/2005src1566

Report generated Jan 12, 2006; 17:14:26

Unit cell

10126 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack r3

a (Angstrom) 24.588 +/- 0.003

b (Angstrom) 24.588 +/- 0.003

c (Angstrom) 48.256 +/- 0.006

alpha (°) 90.000

beta (°) 90.000

gamma (°) 120.000

Volume (A**3) 25266. +/- 5.
Mosaicity (°) 2.678 +/- 0.002

Symmetry used in scalepack	r3
a (Angstrom)	24.588 +/- 0.003
b (Angstrom)	24.588 +/- 0.003
c (Angstrom)	48.256 +/- 0.006
alpha (°)	90.000
beta (°)	90.000
gamma (°)	120.000
Volume (A**3)	25266. +/- 5.
Mosaicity (°)	2.678 +/- 0.002

Data collection

Summary

Total number of images collected	565
Total exposure time	14.0 hours
Data collection exposure time	14.0 hours
Data collection wall-clock time	14.7 hours

Experimental Conditions

Wavelength	0.71073 A
Cryostat setting	120.00K
Crystal to detector distance	60.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	228	`228.0`° phi	1.000°	90 seconds	Yes
data collection	s02f	165	`165.0`° omega	1.000°	90 seconds	Yes
data collection	s03f	164	`164.0`° omega	1.000°	90 seconds	Yes
Phi/Chi	i01f - i08f	8			40 seconds

Scalepack Scaling

Deleted observations

Rejected	`552`
Zero sigma or profile test	`48`
Overload or incomplete profile	`3740`
Sigma cutoff	`344`
High resolution limit	`4252`

Final Data Set

Scale factor range	7.67-14.04
Number of 'full' reflections	`0`
Number of 'partial' reflections	`56700`
Total number of integrated reflections	`45294`
Total number of unique reflections	`11917`
Data completeness	`94.9%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`77.9`
Average Sigma(I)	`5.6`
Overall R-merge (linear)	`0.070`

Eval Integration

Number of reflections	`80439`
Unique reflections	`13018`
Weak reflections	`33229`
Negative intensities	`577`
Rejected observations	`3`
R-sym	`0.221`
R-meas	`0.238`

Sadabs Results

Parameter refinement on 37833 reflections reduced R(int) from 0.0628 to 0.0430

Before rejection, 75960 reflections total and 35087 unique

After rejection, 74398 reflections total and 35041 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   26.3  0.0616   1.179 - 1.552   0.879 - 1.254   1.386   29519   18978
    2  -25.7  0.0626   0.700 - 0.844   0.918 - 1.471   1.404   22241   13818
    3   25.7  0.0866   0.714 - 0.934   0.876 - 1.847   1.520   22638   12686

Sadabs Results

Parameter refinement on 36147 reflections reduced R(int) from 0.3086 to 0.0938

Before rejection, 77172 reflections total and 29995 unique

After rejection, 65714 reflections total and 29179 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -26.3  0.1128   0.624 - 0.986   0.825 - 1.521   1.451   26019   14048
    2   25.7  0.1167   0.680 - 0.888   0.780 - 1.577   1.476   19624   10420
    3  -25.7  0.1483   0.894 - 1.220   0.805 - 1.590   1.604   20071    8880

Ratio of minimum to maximum apparent transmission: 0.474102

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. S. Aldridge

Local Code NDC92

Formula C92 H100 O4 B1 Cl1 F24 Fe2 Ga2

Crystal Colour Light Pink

Crystal Habit Block

Crystal Size 0.14 x 0.1 x 0.06 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. S. Aldridge
Local Code	NDC92
Formula	C92 H100 O4 B1 Cl1 F24 Fe2 Ga2
Crystal Colour	Light Pink
Crystal Habit	Block
Crystal Size	0.14 x 0.1 x 0.06 (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/