Summary report for Directory: diska/04skc0002

Report generated Jul 17, 2004; 09:47:01

Unit cell

2032 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) 7.5646 +/- 0.0009

b (Angstrom) 8.3535 +/- 0.0011

c (Angstrom) 9.2005 +/- 0.0007

alpha (°) 66.417 +/- 0.007

beta (°) 71.945 +/- 0.007

gamma (°) 73.035 +/- 0.006

Volume (A**3) 497.11 +/- 0.10
Mosaicity (°) 0.719 +/- 0.005

Symmetry used in scalepack	p1
a (Angstrom)	7.5646 +/- 0.0009
b (Angstrom)	8.3535 +/- 0.0011
c (Angstrom)	9.2005 +/- 0.0007
alpha (°)	66.417 +/- 0.007
beta (°)	71.945 +/- 0.007
gamma (°)	73.035 +/- 0.006
Volume (A**3)	497.11 +/- 0.10
Mosaicity (°)	0.719 +/- 0.005

Data collection

Summary

Total number of images collected	220
Total exposure time	7.2 hours
Data collection exposure time	7.1 hours
Data collection wall-clock time	7.4 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	179	`358.0`° phi	2.000°	120 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	120 seconds	Yes
data collection	s03f	17	`34.0`° omega	2.000°	120 seconds	Yes
Phi/Chi	i01f - i08f	8			50 seconds

Scalepack Scaling

Deleted observations

Rejected	`35`
Zero sigma or profile test	`1`
Overload or incomplete profile	`170`
Sigma cutoff	`7`
High resolution limit	`9`

Final Data Set

Scale factor range	9.59-10.48
Number of 'full' reflections	`3862`
Number of 'partial' reflections	`3880`
Total number of integrated reflections	`7320`
Total number of unique reflections	`2237`
Data completeness	`98.2%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`13.2`
Average Sigma(I)	`1.3`
Overall R-merge (linear)	`0.082`

Sadabs Results

Parameter refinement on 3791 reflections reduced R(int) from 0.0614 to 0.0470

Before rejection, 7405 reflections total and 2247 unique

After rejection, 7295 reflections total and 2244 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0817   1.068 - 1.275   0.900 - 1.175   1.203    6292    3817
    2   -6.8  0.0736   0.692 - 0.795   0.927 - 1.095   1.159     487     312
    3   -6.8  0.0878   0.234 - 0.250   0.920 - 1.111   1.145     516     301

Ratio of minimum to maximum apparent transmission: 0.765810

Metadata

Group Mike Hursthouse

Operator Suzanna Ward

Sample Owner

Local Code TLT374D E9

Formula C8H12O6N2

Crystal Colour Colourless

Crystal Habit Lath

Crystal Size 0.15 x 0.08 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Suzanna Ward
Sample Owner
Local Code	TLT374D E9
Formula	C8H12O6N2
Crystal Colour	Colourless
Crystal Habit	Lath
Crystal Size	0.15 x 0.08 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/