Summary report for Directory: home/diska/05src0098

Report generated Jan 26, 2005; 16:27:25

Unit cell

6243 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) 7.6771 +/- 0.0002

b (Angstrom) 28.6835 +/- 0.0010

c (Angstrom) 13.7836 +/- 0.0005

alpha (°) 90.000

beta (°) 104.2832 +/- 0.0018

gamma (°) 90.000

Volume (A**3) 2941.41 +/- 0.17
Mosaicity (°) 0.551 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	7.6771 +/- 0.0002
b (Angstrom)	28.6835 +/- 0.0010
c (Angstrom)	13.7836 +/- 0.0005
alpha (°)	90.000
beta (°)	104.2832 +/- 0.0018
gamma (°)	90.000
Volume (A**3)	2941.41 +/- 0.17
Mosaicity (°)	0.551 +/- 0.002

Data collection

Summary

Total number of images collected	286
Total exposure time	142.0 minutes
Data collection exposure time	140.0 minutes
Data collection wall-clock time	162.1 minutes

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	45.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	178	`356.0`° phi	2.000°	30 seconds	Yes
data collection	s02f	16	`32.0`° omega	2.000°	30 seconds	Yes
data collection	s03f	68	`136.0`° omega	2.000°	30 seconds	Yes
data collection	s04f	16	`32.0`° omega	2.000°	30 seconds	Yes
Phi/Chi	i01f - i08f	8			15 seconds

Scalepack Scaling

Deleted observations

Rejected	`167`
Zero sigma or profile test	`6`
Overload or incomplete profile	`1290`
Sigma cutoff	`20`
High resolution limit	`26`

Final Data Set

Scale factor range	6.60-11.07
Number of 'full' reflections	`21168`
Number of 'partial' reflections	`11859`
Total number of integrated reflections	`31048`
Total number of unique reflections	`6776`
Data completeness	`98.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`58.1`
Average Sigma(I)	`2.3`
Overall R-merge (linear)	`0.053`

Sadabs Results

Parameter refinement on 21413 reflections reduced R(int) from 0.1145 to 0.0445

Before rejection, 31515 reflections total and 6816 unique

After rejection, 30912 reflections total and 6808 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.9  0.0526   0.806 - 1.132   0.950 - 1.140   1.417   19369   13983
    2  -18.3  0.0498   0.892 - 1.009   0.959 - 1.206   1.388    1370     984
    3  -18.3  0.0529   0.896 - 1.070   0.949 - 1.327   1.428    8367    5911
    4  -18.3  0.0491   0.905 - 0.982   0.964 - 1.215   1.391    1806    1252

Ratio of minimum to maximum apparent transmission: 0.715365

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. S. J. Lancaster

Local Code OP3-113

Formula C57 H53 N4 O2 Cl5 Ti2

Crystal Colour Red

Crystal Habit Shard

Crystal Size 0.19 x 0.13 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. S. J. Lancaster
Local Code	OP3-113
Formula	C57 H53 N4 O2 Cl5 Ti2
Crystal Colour	Red
Crystal Habit	Shard
Crystal Size	0.19 x 0.13 x 0.04 (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/