Title:     Mo complex of xcrown-ether-substituted triphenyl phosphiine
  
Cell:      10.4784  10.7633  17.0684 105.859  99.743 100.532  
Cell ESDs: 0.0032   0.0034   0.0053   0.004   0.004   0.004  

Formula:  C37 H34 N1 O9 P1 Mo1

Comments:  

You are offered a choice of two space groups. Choose the default (P1).
Run XS. In XSHELL look carefully to decide if two of the peaks assigned
as Mo atoms should be relabelled as P atoms. 

Amidst the spurious peaks the molecule should still be easily visible. 
Delete the spurious peaks. The rest of the Q peaks
can be labelled as C atoms for the first round of refinement.

In REFINE, select the option CGLS -- an alternative quicker
refinement method.

When the model is complete, look carefully at the two molecules.
Are they possibly related by a symmetry operation? What might the symmetry
operation be? 

At this stage you may want to re-solve the structure by Patterson means. 

********************************************
**Re-solving the structure by Patterson method:
Return to XPREP, travel through XPREP as before, but this time select 
space group P-1. In option F (write SHELXTL files) give a new name (KAF_P-1),
and select option Y to write out a new *.hkl file.

Open a new project, name KAF_P-1, and then edit the *.ins file, deleting TREF 
and adding  PATT 5 2.0 0.80 100 12 8. Run XS. Look carefully at the output on the
screen to see which solution has the highest correlation coefficient. 
Edit the *.res file and eliminate 
all other solutions, retaining only the best. You might note that the best solution 
involves a vector with "Length 2.54 A" (that is the expected Mo-P bond length.)  

Now go into XSHELL and select REFINE. In the box marked Plan, change 20 to 50 
(you are missing nearly 50 atoms from your current model). 

After refinement retuurn to XSHELL. If the diagram looks horribly compressed, 
select ATOMS and TRIM. A good proportion of the molecule should be visible.

******************************
***Alternatively, you could have fix up the original model by Changing to a 
higher symmetry space group:

You want to delete one of the molecules and move the other one into the 
correct position in the unit cell. Averaging the coordinates of the two Mo atoms 
(average = (x,y,z).
Then adding to the *.INS file a 
         MOVE -x -y -z 1 
then delete one of the molecules and finally change th space group
        LATT -1  -->>  LATT 1.
Then REFINE. SEE GBJ FOR ASSISTANCE IF THE WHEELS FALL OFF THE TRAIN!!!
**************************************** 
 
  
SFAC C  H  N  O  P  Mo 
UNIT 74 68 2 18 2 2 
L.S. 4
BOND  
FMAP 2
PLAN 20
FVAR  1.000000
MOLE 1
Mo1    6   0.463600  0.481800  1.004700 11.000000  0.050000
Mo2    6  -0.390800 -0.286400  0.560100 11.000000  0.050000
P3a    5   0.296600  0.515800  0.897900 11.000000  0.050000
P4     5   1.149100  1.281800  1.340400 11.000000  0.050000
C1     1  -0.568700 -0.261900  0.449600 11.000000  0.050000
C2     1  -0.700200 -0.819100  0.223200 11.000000  0.050000
C3     1  -0.203500 -0.298500  0.677200 11.000000  0.050000
C4     1   0.776200  1.019900  1.344600 11.000000  0.050000
C5     1  -0.306800 -0.434800  0.486000 11.000000  0.050000
C6     1   0.533000  0.343900  0.935200 11.000000  0.050000
C7     1   0.380600  0.634900  1.080800 11.000000  0.050000
C8     1   0.931300  1.197100  1.141600 11.000000  0.050000
C9     1   0.720400  1.058100  1.193000 11.000000  0.050000
C10    1  -0.644800 -0.857200  0.374900 11.000000  0.050000
C11    1   0.956500  1.315000  1.433500 11.000000  0.050000
C12    1  -0.454600 -0.145800  0.632500 11.000000  0.050000
C13    1  -0.882300 -1.113200  0.135000 11.000000  0.050000
C14    1  -0.162100 -0.188500  0.776700 11.000000  0.050000
C15    1  -0.263500 -0.134500  0.547100 11.000000  0.050000
C16    1   0.573600  0.262900  0.893000 11.000000  0.050000
C17    1  -0.056700 -0.362700  0.554600 11.000000  0.050000
C18    1  -0.059400 -0.297600  0.635800 11.000000  0.050000
C19    1   0.133900  0.498700  0.932300 11.000000  0.050000
C20    1   0.609800  0.620500  0.989100 11.000000  0.050000
C21    1   0.339800  0.333500  1.022800 11.000000  0.050000
C23    1   0.134800  0.561700  1.015600 11.000000  0.050000
C24    1  -0.501900 -0.065900  0.672900 11.000000  0.050000
C25    1  -0.535100 -0.425700  0.573800 11.000000  0.050000
C26    1   0.603500  0.492000  1.108400 11.000000  0.050000
C27    1  -0.856600 -1.003000  0.418700 11.000000  0.050000
C28    1   0.320000  0.675500  0.880800 11.000000  0.050000
C29    1   0.685800  0.499500  1.159900 11.000000  0.050000
C30    1  -0.578000 -0.750300  0.362100 11.000000  0.050000
C31    1  -0.935300 -1.216900  0.265200 11.000000  0.050000
C32    1   0.059900 -0.358500  0.525900 11.000000  0.050000
C33    1  -0.943200 -1.053000  0.196200 11.000000  0.050000
C34    1  -0.614900 -0.306200  0.402700 11.000000  0.050000
C35    1   0.181200 -0.219200  0.663300 11.000000  0.050000
C36    1  -0.250800 -0.479300  0.683400 11.000000  0.050000
C37    1   0.017700  0.560200  1.042200 11.000000  0.050000
C38    1   0.641700  0.942600  1.199700 11.000000  0.050000
C39    1  -0.398600 -0.539500  0.416000 11.000000  0.050000
C40    1  -0.103300  0.419800  0.904100 11.000000  0.050000
C41    1   0.475600  0.741600  1.152000 11.000000  0.050000
C42    1  -0.124600 -0.226900  0.851500 11.000000  0.050000
C43    1  -0.178800 -0.451700  0.482000 11.000000  0.050000
C44    1  -0.467500 -0.645800  0.433600 11.000000  0.050000
C45    1   1.004400  1.410400  1.294900 11.000000  0.050000
C46    1   0.242400  0.388000  0.785700 11.000000  0.050000
C47    1   0.257000  0.651200  1.086000 11.000000  0.050000
C48    1  -0.104700  0.481100  0.988000 11.000000  0.050000
C49    1   0.182300 -0.279700  0.577900 11.000000  0.050000
C50    1  -0.597900 -0.732800  0.287100 11.000000  0.050000
C51    1   0.673900  0.935000  1.281900 11.000000  0.050000
C52    1   0.008600  0.422800  0.875800 11.000000  0.050000
C53    1   0.205100  0.429700  0.715900 11.000000  0.050000
C54    1   1.019500  1.245100  1.366300 11.000000  0.050000
C55    1   0.552500  0.856300  1.137700 11.000000  0.050000
C56    1   0.711200  0.693300  0.989300 11.000000  0.050000
C57    1   0.055100 -0.233700  0.685800 11.000000  0.050000
C58    1  -0.629800 -0.493300  0.580100 11.000000  0.050000
C59    1   0.267300  0.241700  1.025200 11.000000  0.050000
C60    1  -0.632900 -0.876100  0.451500 11.000000  0.050000
C61    1  -0.164100 -0.562100  0.667600 11.000000  0.050000
C62    1   0.487500  0.717300  1.227400 11.000000  0.050000
C63    1   0.871300  1.222100  1.456900 11.000000  0.050000
C64    1   0.746500  1.135600  1.389500 11.000000  0.050000
C65    1  -0.421100 -0.530400  0.334500 11.000000  0.050000
C66    1   0.242600  0.765700  0.900900 11.000000  0.050000
C67    1  -0.331100 -0.736800  0.693500 11.000000  0.050000
C68    1  -0.189800 -0.041400  0.544400 11.000000  0.050000
C69    1   0.444900  0.721700  0.856200 11.000000  0.050000
C70    1   0.400000  0.929300  0.870800 11.000000  0.050000
C71    1   0.709300  1.075400  1.111600 11.000000  0.050000
C73    1  -1.025800 -1.153300  0.228500 11.000000  0.050000
C74    1   0.591000  0.822700  1.294200 11.000000  0.050000
C75    1  -0.366100 -0.513700  0.709500 11.000000  0.050000
C76    1   1.021900  1.443900  1.220400 11.000000  0.050000
C77    1  -0.081200 -0.137000  0.928600 11.000000  0.050000
C78    1  -0.662400 -0.929900  0.180700 11.000000  0.050000
C79    1   0.479900  0.834000  0.852500 11.000000  0.050000
C80    1   0.283100  0.898200  0.897900 11.000000  0.050000
C81    1  -0.512200 -0.629100  0.268900 11.000000  0.050000
C82    1   0.806900  1.210800  1.127400 11.000000  0.050000
C83    1   0.154400  0.203600  0.624800 11.000000  0.050000
C84    1   0.156500  0.337900  0.638100 11.000000  0.050000
C85    1  -0.718500 -1.009800  0.447500 11.000000  0.050000
C86    1  -0.794000 -1.020500  0.110600 11.000000  0.050000
C87    1  -0.207000 -0.695800  0.669700 11.000000  0.050000
C88    1  -0.407100 -0.645600  0.714200 11.000000  0.050000
C90    1   1.037300  1.313800  1.157500 11.000000  0.050000
C91    1   0.229700  0.252700  0.780100 11.000000  0.050000
C92    1  -0.946700 -1.102500  0.416300 11.000000  0.050000
C93    1  -0.158800 -0.058200  0.788900 11.000000  0.050000
C95    1  -0.074700 -0.000500  0.935200 11.000000  0.050000
C96    1  -0.955300 -1.228800  0.344500 11.000000  0.050000
C98    1  -0.116200  0.034100  0.865800 11.000000  0.050000
C101   1   0.191600  0.164900  0.697700 11.000000  0.050000
C124   1   1.186700  1.439500  1.322900 11.000000  0.050000
HKLF 4                                                                           
END  
