    REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
                          P R O M E T H E U S  HAS BEEN CALLED FOR  S T R U C T U R E R E F I N E M E N T

                                         REFINEMENTS OF  STRUCTURES  WITH  NOT  MORE  THAN
                                         SIXTY ATOMS PER ASYMMETRIC UNIT AND NOT MORE THAN
                                         TWENTY  DIFFERENT  SCATTERING   CURVES   CAN   BE
                                         PERFORMED.  THERMAL  MOTIONS UP TO SIXTH ORDER IN
                                         FOUR DIFFERENT STRUCTURE FACTOR EQUATIONS  CAN BE
                                         INVESTIGATED.            EXTINCTION CORRECTION OF
                                         ZACHARIASEN  REVISED BY HAMILTON AND COPPENS   AS
                                         WELL AS THE EXTINCTION CORRECTION OF BECKER   AND
                                         COPPENS ARE INCLUDED.     GENERAL CONSTRAINTS FOR
                                         'SHAPE REFINEMENT' ETC.  AND  SPECIAL  PARAMETERS
                                               FOR 'RIGID BODY' MOTIONS ARE AVAILABLE.    
                                         INFORMATION  ABOUT THIS  PROGRAM   IS   AVAILABLE
                                          FROM   W.F. KUHS    UNI KARLRUHE      TEL. 3317 





                                            LABEL  OF THE UNIT MAIN  =  LABELofRUN#1





                                   SUBSTANCE=               TEMPERATURE=               SPECIAL=
 
 
 
 
 
 
 
 
    REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE REFINE
1STARTING TIME
 -------------


 PROGRAM START   29-Aug-94  11:48:45


 TITLE OF THE CYCLE
 ------------------

 Example-file for REFI                                                   

0CONTROL-PARAMETER
 -----------------

 P 3 0 2   0 0 0 0 0   1 1 1 1 1 1 1 6   0.000     1.000     2.000     0   0 0 0      0

0LATTICE PARAMETERS
 ------------------

0REAL CELL                  4.51100   4.51100   7.34900  ( A )       90.00000  90.00000 120.00000    (DEGREES)
0VOLUME OF REAL CELL      129.5104                      (A**3)
0RECIPROCAL CELL            0.25597   0.25597   0.13607  (1/A)       90.00000  90.00000  60.00000    (DEGREES)
 
0SYMMETRY OF CELL
 ----------------

 CENTRIC   CELL OF TYPE   P

 
          X         Y         Z           1. CARD
         -Y         X -Y      Z           2. CARD
          Y -X     -X         Z           3. CARD
         -Y        -X         Z           4. CARD
          X         X -Y      Z           5. CARD
          Y -X      Y         Z           6. CARD
         -X        -Y    1/2  Z           7. CARD
          Y         Y -X 1/2  Z           8. CARD
          X -Y      X    1/2  Z           9. CARD
          Y         X    1/2  Z          10. CARD
         -X         Y -X 1/2  Z          11. CARD
          X -Y     -Y    1/2  Z          12. CARD

0SCATTERING CURVES
 -----------------



 LABEL       A(1)       B(1)       A(2)       B(2)       A(3)       B(3)       A(4)       B(4)       C          DFR      DFI

 O          0.000000   0.000000   0.000000   0.000000   0.000000   0.000000   0.000000   0.000000   0.580000

 LABEL       A(1)       B(1)       A(2)       B(2)       A(3)       B(3)       A(4)       B(4)       C          DFR      DFI

 D          0.000000   0.000000   0.000000   0.000000   0.000000   0.000000   0.000000   0.000000   0.667400

 LABEL       A(1)       B(1)       A(2)       B(2)       A(3)       B(3)       A(4)       B(4)       C          DFR      DFI

 H          0.000000   0.000000   0.000000   0.000000   0.000000   0.000000   0.000000   0.000000  -0.374100

0SCALING
 -------
0SCALE FACTORS    100.0000

0MODEL OF EXTINCTION
 -------------------

0CORRECTION BY BECKER & COPPENS.


0PARAMETERS OF EXTINCTION
 ------------------------
 
0 NO EXTINCTION CORRECTION                                                   

0ATOMPARAMETER 
 -------------

0ATOM LABEL     X       Y       Z       TEMPERATURE FACTOR DATA(BETAS)

      O 1       0.3333  0.6667  0.0621  0.05853  0.05853  0.01812  0.02926  0.00000  0.00000
      D 1       0.3333  0.6667  0.1983  0.06688  0.06688  0.01634  0.03344  0.00000  0.00000
      D 2       0.4539  0.9079  0.0171  0.06472  0.05705  0.01938  0.02853  0.00085  0.00170
0ATOM LABEL   TF  SCAT.  SITE   OCCUP  OCCA          (TF = ORDER OF TEMP.-FACTOR)

      O 1      4  1  0  0.167   1.000   0.000
      D 1      4  2  3  0.167   0.500   0.485
      D 2      4  2  3  0.500   0.500   0.485

0PARAMETER SELECTION INFORMATION
 -------------------------------
 
 SCALE FACTORS          1
 ATOMPARAMETER          O 1     0 001 101000  1010010000  101010010000000
                        D 1     1 001 101000  0000010000  100000010000000
                        D 2     0 101 111010  1010011000  101000010000000

0ORIENTATION MATRIX FOR 4-CIRCLE DIFFRACTOMETER IN BUSING & LEVY GEOMETRY
 ------------------------------------------------------------------------


   -0.160460   0.073140  -0.048780
   -0.056710  -0.161240  -0.104680
   -0.191210  -0.184920   0.071980
0INVERSE UB-MATRIX

   -4.009104   0.486293  -2.009711
    3.120152  -2.703139  -1.816666
   -2.634095  -5.652689   3.886987
0DETERMINANT OF UB-MATRIX

   0.007723




0DEPENDENT PARAMETER INFORMATION
 -------------------------------

 
   1  6  1  5     1.000    1  8  1  5     0.500    1 12  1 11    -1.000    1 14  1 11     0.500    1 15  1 11    -0.500
   1 18  1 16     1.000    1 20  1 16     0.500    1 22  1 21     1.000    1 24  1 21     0.500    1 26  1 21     0.500
   1 29  1 21     0.500    1 27  1 25     0.500    1 30  1 25    -0.500    1 33  1 25    -1.000    1 31  1 28     0.500
   1 34  1 28     1.000    3  1  2  1     1.000    2  6  2  5     1.000    2  8  2  5     0.500    2 12  2 11    -1.000
   2 14  2 11     0.500    2 15  2 11    -0.500    2 18  2 16     1.000    2 20  2 16     0.500    2 22  2 21     1.000
   2 24  2 21     0.500    2 26  2 21     0.500    2 29  2 21     0.500    2 27  2 25     0.500    2 30  2 25    -0.500
   2 33  2 25    -1.000    2 31  2 28     0.500    2 34  2 28     1.000    3  3  3  2     2.000    3  8  3  6     0.500
   3 10  3  9     2.000    3 14  3 11     0.667    3 14  3 12     0.167    3 15  3 12     0.500    3 19  3 17     2.000
   3 20  3 18     2.000    3 26  3 22     0.167    3 29  3 22     0.500    3 26  3 24     0.667    3 27  3 25     0.667
   3 35  3 32     2.000    3 27  3 33     0.167    3 30  3 33     0.500    3 31  3 34     0.500

0CORE ALLOCATION
 ---------------

 DIMENSION OF ARRAY 'A' (COMMON LSMAT ) =     594               CURRENT MAXIMUM IS  10500


0PARAMETERS OF  HKL-CARDS   
 ------------------------

0FORMAT FOR STRUCTURE FACTOR INPUT    (A4, 9X,3I3, 3X, I3, 3X,F9.0, 9X,F5.0)                                  

0INTENSITY ON CARD.
0STANDARD DEVIATIONS OF F*F ON CARD.   THESE ARE ALTERED BY AN IGNORANCE FACTOR.
                                       SIGMA WILL BE COMPUTED  BY  SQRT(SIGMA**2 + (I(OBS)* 0.020 )**2)
                                       SIGMA(F) = SIGMA(F*F)/(2*F)          IF F*F  GREATER  SIGMA(F*F)
                                       SIGMA(F) = SQUAREROOT(SIGMA(F*F))/2  IF F*F LESS THAN SIGMA(F*F)
                                       FORMULAS  FROM  REES  ACTA CRYSTALLOGRAPHICA  A32, P.483 (1976).

0REJECT-PARAMETER
 ----------------
0REFLECTIONS WITH I/SIGMA(I) (OR F/SIGMA(F)) .LT.    2.00  ARE REJECTED.

0MEASURING CONDITIONS
 --------------------
0REFLECTIONS ARE  MEASURED  WITH   NEUTRON  RADIATION.
0WAVE LENGTH (ANGSTROMS)     0.701950


0ABSORPTION WEIGHTED AVERAGED PATH LENGTH
 ----------------------------------------

 AVERAGED PATHLENGTH OF THE BEAM 300.00 MICROMETER.




0USED STRUCTURE FACTOR EQUATION WAS       NO. 2
 ----------------------------------



 **************************************************************************************************
 *                                                                                                *
 *  --                                                                                            *
 *  |                   K         KL    I-                      KLM                      KLMN -I  *
 *  /   F *EXP(I*2PI*H X  - H H *B   )* I 1-I*4/3*PI**3*H H H *C   + 2/3*PI**4*H H H H *D      I  *  
 *  --   J            K J    K L  J     I-               K L M  J               K L M N  J    -I  *
 *  J                                                                                             *
 **************************************************************************************************   PDF = GRAM-CHARLIER-SERIES


1Example-file for REFI                                                        RESULTS OF STRUCTURE FACTOR CALCULATIONS
                                                                              STRUCTURE FACTOR EQUATION NO.   2
0++++  R-VALUES BEFORE THE FIRST REFINEMENT  ++++
0ALL REFLECTIONS              NUMERATOR    DENOMINATOR    NUMBER      R(INT) 
 
          WEIGHTED R              26.44         711.60       304      0.037

          UNWEIGHTED R             4.70          86.93       304      0.054

              RANGES OF F(OBS)
                                  22.73         658.09       260      0.035
                                  10.38         212.07        27      0.049
                                   4.87         122.44         9      0.040
                                   3.03          57.72         2      0.053
                                   2.62          57.72         2      0.045
                                   2.60          57.72         2      0.045
                                   0.00           0.00         0      0.000
                                   5.30          57.72         2      0.092

              RANGES OF (SIN(THETA)/LAMBDA)**2
                                   8.67         173.16        18      0.050
                                  10.61         212.07        27      0.050
                                  10.48         223.54        30      0.047
                                   9.71         244.88        36      0.040
                                   8.06         261.33        41      0.031
                                   7.95         264.50        42      0.030
                                   8.57         264.50        42      0.032
                                  10.29         336.55        68      0.031

 UNREJECTED REFLECTIONS
 
          WEIGHTED R              23.81         711.25       194      0.033

          UNWEIGHTED R             2.79          82.91       194      0.034

              RANGES OF F(OBS)
                                  19.60         625.41       150      0.031
                                  10.38         265.34        27      0.039
                                   4.87         153.19         9      0.032
                                   3.03          72.22         2      0.042
                                   2.62          72.22         2      0.036
                                   2.60          72.22         2      0.036
                                   0.00           0.00         0      0.000
                                   5.30          72.22         2      0.073

              RANGES OF (SIN(THETA)/LAMBDA)**2
                                   8.51         210.54        17      0.040
                                  10.34         260.38        26      0.040
                                  10.48         279.69        30      0.037
                                   9.65         297.75        34      0.032
                                   7.53         274.99        29      0.027
                                   6.78         260.38        26      0.026
                                   6.41         210.54        17      0.030
                                   6.37         197.77        15      0.032


 SUM FCALC                             83.36
 WEIGHTED    "GOODNESS OF FIT"          1.86
1Example-file for REFI                                                                     CYCLE NO.   0


 
 ESTIMATED STD. DEV. FOR OBS. OF UNIT WEIGHT             1.13                              STRUCTUREFACTOR EQUATION NO.   2
                                                                                           REFINEMENT ON     FOBS

 
0 NO EXTINCTION CORRECTION                                                   
0                            PARAMETER                   OLD          CHANGE         NEW         ERROR         SHIFT/ERROR NP.DAMP.
 




                           SCALE FACTOR  1          100.0000         3.0684     103.0684        1.28120            2.39    1      

 
0  ATOM  1    O 1          EQUIPOINT FRACTION =  0.167
 
                           OCCUPANCY SPECIES  1         1.00000                     1.00000
 
                           X                          0.3333300                   0.3333300
                           Y                          0.6666700                   0.6666700
                           Z                          0.0621100     -0.0000693    0.0620407     0.0003708         -0.19    2      
 
                           U11                        4.5251999      0.0278434    4.5530434     0.1235921          0.23    3      
                           U22                        4.5251999                   4.5530434     0.1235921
                           U33                        4.9590006      0.0661141    5.0251145     0.1868726          0.35    4      
                           U12                        2.2625999                   2.2765217     0.0617960
                           U13                        0.0000000                   0.0000000
                           U23                        0.0000000                   0.0000000
 
                           C(111)                     0.4200E-02     0.3552E-03   0.4555E-02    0.1873E-02         0.19    5      
                           C(222)                    -0.4200E-02                 -0.4555E-02    0.1873E-02
                           C(333)                    -0.1600E-02     0.3416E-04  -0.1566E-02    0.9922E-03         0.03    6      
                           C(112)                     0.2100E-02                  0.2278E-02    0.9365E-03
                           C(122)                    -0.2100E-02                 -0.2278E-02    0.9365E-03
                           C(113)                     0.1700E-02    -0.3413E-03   0.1359E-02    0.9831E-03        -0.35    7      
                           C(133)                     0.0000E+00                  0.0000E+00
                           C(223)                     0.1700E-02                  0.1359E-02    0.9831E-03
                           C(233)                     0.0000E+00                  0.0000E+00
                           C(123)                     0.8500E-03                  0.6794E-03    0.4915E-03
 
                           D(1111)                   0.014000000    0.000283721  0.014283722   0.006756287         0.04    8      
                           D(2222)                    0.1400E-01                  0.1428E-01    0.6756E-02
                           D(3333)                   0.003100000    0.000135154  0.003235154   0.001155322         0.12    9      
                           D(1112)                    0.7000E-02                  0.7142E-02    0.3378E-02
                           D(1113)                   0.001000000    0.000526851  0.001526851   0.000930784         0.57   10      
                           D(1122)                    0.7000E-02                  0.7142E-02    0.3378E-02
                           D(1123)                    0.5000E-03                  0.7634E-03    0.4654E-03
                           D(1133)                   0.001900000    0.000453000  0.002353000   0.000823954         0.55   11      
                           D(1222)                    0.7000E-02                  0.7142E-02    0.3378E-02
                           D(1223)                   -0.5000E-03                 -0.7634E-03    0.4654E-03
                           D(1233)                    0.9500E-03                  0.1176E-02    0.4120E-03
                           D(1333)                    0.0000E+00                  0.0000E+00
                           D(2223)                   -0.1000E-02                 -0.1527E-02    0.9308E-03
                           D(2233)                    0.1900E-02                  0.2353E-02    0.8240E-03
                           D(2333)                    0.0000E+00                  0.0000E+00
0  ATOM  2    D 1          EQUIPOINT FRACTION =  0.167
 
                           OCCUPANCY SPECIES  2         0.48500        0.00108      0.48608       0.00339          0.32   12      
                           OCCUPANCY SPECIES  3         0.01500                     0.01392
                           TOTAL OCCUPANCY (FIXED) =    0.50000
 
                           X                          0.3333300                   0.3333300
                           Y                          0.6666700                   0.6666700
                           Z                          0.1983300     -0.0002008    0.1981292     0.0003981         -0.50   13      
 
                           U11                        5.1711001      0.0700591    5.2411594     0.1335584          0.52   14      
                           U22                        5.1711001                   5.2411594     0.1335584
                           U33                        4.4710999     -0.0267141    4.4443860     0.1031170         -0.26   15      
                           U12                        2.5855501                   2.6205797     0.0667792
                           U13                        0.0000000                   0.0000000
                           U23                        0.0000000                   0.0000000
 
                           C(111)                     0.0000E+00                  0.0000E+00
                           C(222)                     0.0000E+00                  0.0000E+00
                           C(333)                     0.0000E+00                  0.0000E+00
                           C(112)                     0.0000E+00                  0.0000E+00
                           C(122)                     0.0000E+00                  0.0000E+00
                           C(113)                     0.0000E+00    -0.7837E-03  -0.7837E-03    0.1702E-02        -0.46   16      
                           C(133)                     0.0000E+00                  0.0000E+00
                           C(223)                     0.0000E+00                 -0.7837E-03    0.1702E-02
                           C(233)                     0.0000E+00                  0.0000E+00
                           C(123)                     0.0000E+00                 -0.3919E-03    0.8512E-03
 
                           D(1111)                   0.000000000    0.006037908  0.006037908   0.008811858         0.69   17      
                           D(2222)                    0.0000E+00                  0.6038E-02    0.8812E-02
                           D(3333)                    0.0000E+00                  0.0000E+00
                           D(1112)                    0.0000E+00                  0.3019E-02    0.4406E-02
                           D(1113)                    0.0000E+00                  0.0000E+00
                           D(1122)                    0.0000E+00                  0.3019E-02    0.4406E-02
                           D(1123)                    0.0000E+00                  0.0000E+00
                           D(1133)                   0.000000000   -0.001235415 -0.001235415   0.001167483        -1.06   18      
                           D(1222)                    0.0000E+00                  0.3019E-02    0.4406E-02
                           D(1223)                    0.0000E+00                  0.0000E+00
                           D(1233)                    0.0000E+00                 -0.6177E-03    0.5837E-03
                           D(1333)                    0.0000E+00                  0.0000E+00
                           D(2223)                    0.0000E+00                  0.0000E+00
                           D(2233)                    0.0000E+00                 -0.1235E-02    0.1167E-02
                           D(2333)                    0.0000E+00                  0.0000E+00
0  ATOM  3    D 2          EQUIPOINT FRACTION =  0.500
 
                           OCCUPANCY SPECIES  2         0.48500                     0.48608     0.0033902
                           OCCUPANCY SPECIES  3         0.01500                     0.01392
                           TOTAL OCCUPANCY (FIXED) =    0.50000
 
                           X                          0.4539500     -0.0001810    0.4537690     0.0001660         -1.09   19      
                           Y                          0.9079000                   0.9075380     0.0003320
                           Z                          0.0170600      0.0002454    0.0173054     0.0002416          1.02   20      
 
                           U11                        5.0042000      0.0998691    5.1040688     0.0973740          1.03   21      
                           U22                        4.4109001     -0.0019629    4.4089375     0.0482563         -0.04   22      
                           U33                        5.3013005      0.2349055    5.5362058     0.1186342          1.98   23      
                           U12                        2.2054501                   2.2044687     0.0241281
                           U13                        0.1237000      0.0073604    0.1310605     0.0184110          0.40   24      
                           U23                        0.2474000                   0.2621209     0.0368219
 
                           C(111)                     0.0000E+00    -0.2574E-02  -0.2574E-02    0.2389E-02        -1.08   25      
                           C(222)                     0.0000E+00                  0.0000E+00
                           C(333)                     0.0000E+00     0.3777E-03   0.3777E-03    0.6237E-03         0.61   26      
                           C(112)                     0.0000E+00                 -0.1716E-02
                           C(122)                     0.0000E+00                  0.0000E+00
                           C(113)                     0.0000E+00     0.5463E-03   0.5463E-03    0.1007E-02         0.54   27      
                           C(133)                     0.0000E+00    -0.5155E-03  -0.5155E-03    0.3876E-03        -1.33   28      
                           C(223)                     0.0000E+00                  0.0000E+00
                           C(233)                     0.0000E+00                 -0.1031E-02    0.7752E-03
                           C(123)                     0.0000E+00                  0.0000E+00
 
                           D(1111)                   0.000000000    0.005103470  0.005103470   0.005058693         1.01   29      
                           D(2222)                    0.0000E+00                  0.0000E+00
                           D(3333)                   0.000000000    0.001575196  0.001575196   0.000713807         2.21   30      
                           D(1112)                    0.0000E+00                  0.0000E+00
                           D(1113)                    0.0000E+00                  0.0000E+00
                           D(1122)                    0.0000E+00                  0.0000E+00
                           D(1123)                    0.0000E+00                  0.0000E+00
                           D(1133)                   0.000000000    0.000449125  0.000449125   0.000693914         0.65   31      
                           D(1222)                    0.0000E+00                  0.0000E+00
                           D(1223)                    0.0000E+00                  0.0000E+00
                           D(1233)                    0.0000E+00                  0.0000E+00
                           D(1333)                    0.0000E+00                  0.0000E+00
                           D(2223)                    0.0000E+00                  0.0000E+00
                           D(2233)                    0.0000E+00                  0.0000E+00
                           D(2333)                    0.0000E+00                  0.0000E+00



                         MAXIMUM SHIFT/ERROR =       2.39

                         AVERAGE SHIFT/ERROR =       0.70

0REMARK
 ------

 UIJ ARE MULTIPLIED BY 10**2. 

0REMARK
 ------

 THERMAL PARAMETERS OF THIRD, FOURTH, FIFTH AND SIXTH ORDER ARE MULTIPLIED BY 10**3, 10**4, 10**5 AND 10**6 RESPECTIVELY.
1Example-file for REFI                                                   
0CORRELATION COEFICIENTS WITH LARGEST MAGNITUDES

  PARAMETERS   VALUE     PARAMETERS   VALUE     PARAMETERS   VALUE     PARAMETERS   VALUE   

     4     9   0.9498       3     8   0.9462      14    17   0.8876      23    30   0.8793

     2     6   0.8689      21    29   0.8470       1     3   0.8130      20    26   0.7769

     1    12  -0.7249       1     4   0.7094      13    16   0.6896       3    12  -0.6775

     1     8   0.6755       2     7   0.6690       4    11   0.6570       1    11   0.6240

     8    12  -0.5953       4    12  -0.5943       3    11   0.5904       1     9   0.5693
1RESULTS IN SHORTENED FORM
 -------------------------

 DETAILED RESULTS OF THE FOLLOWING CYCLES ARE WRITTEN TO  UNIT  NO.    15

0NUMBER OF CYCLE   R(W) <UNREJ. REFLEC.>     R  <UNREJ. REFLEC.>     GOODNESS OF FIT     MAX.SHIFT/ERROR


       1                 0.03347                   0.03366                1.8646                2.3949
       2                 0.02026                   0.01960                1.1288                0.2254
       3                 0.02024                   0.01958                1.1276                0.0023
1TITLE OF THE CYCLE
 ------------------

 CYCLE 6                                                                 

0CONTROL-PARAMETER
 -----------------

 P 3 0 0   0 0 0 0 0   0 0 0 0 0 0 0 0   0.000     0.000     0.000     0   0 0 0      0

0CORE ALLOCATION
 ---------------

 DIMENSION OF ARRAY 'A' (COMMON LSMAT ) =     594               CURRENT MAXIMUM IS  10500

1CYCLE 6                                                                      RESULTS OF STRUCTURE FACTOR CALCULATIONS
                                                                              STRUCTURE FACTOR EQUATION NO.   2
0++++ NUMBER OF CYCLE =          4   ++++   
0ALL REFLECTIONS              NUMERATOR    DENOMINATOR    NUMBER      R(INT) 
 
          WEIGHTED R              18.48         711.60       304      0.026

          UNWEIGHTED R             3.44          84.33       304      0.041

              RANGES OF F(OBS)                                                        LOWER -         UPPER -      LIMIT 
                                  17.49         653.01       256      0.027           0.010           0.535
                                   4.24         234.45        33      0.018           0.535           1.060
                                   2.54         115.44         8      0.022           1.060           1.585
                                   0.69          70.69         3      0.010           1.585           2.110
                                   0.00           0.00         0      0.000           2.110           2.635
                                   1.36          70.69         3      0.019           2.635           3.160
                                   0.00           0.00         0      0.000           3.160           3.685
                                   2.97          40.81         1      0.073           3.685           4.210

              RANGES OF  SIN(THETA)/LAMBDA    
                                   4.77         191.43        22      0.025           0.128           0.404
                                   4.10         212.07        27      0.019           0.404           0.556
                                   4.93         234.45        33      0.021           0.556           0.675
                                   5.79         244.88        36      0.024           0.675           0.776
                                   7.16         270.72        44      0.026           0.776           0.866
                                   8.46         273.78        45      0.031           0.866           0.946
                                   7.86         273.78        45      0.029           0.946           1.021
                                   7.70         294.31        52      0.026           1.021           1.090

 UNREJECTED REFLECTIONS
 
          WEIGHTED R              14.40         711.25       194      0.020

          UNWEIGHTED R             1.57          80.43       194      0.020

              RANGES OF F(OBS)                                                        LOWER -         UPPER -      LIMIT 
                                  13.10         617.02       146      0.021           0.010           0.535
                                   4.24         293.34        33      0.014           0.535           1.060
                                   2.54         144.43         8      0.018           1.060           1.585
                                   0.69          88.45         3      0.008           1.585           2.110
                                   0.00           0.00         0      0.000           2.110           2.635
                                   1.36          88.45         3      0.015           2.635           3.160
                                   0.00           0.00         0      0.000           3.160           3.685
                                   2.97          51.06         1      0.058           3.685           4.210

              RANGES OF  SIN(THETA)/LAMBDA    
                                   4.51         234.01        21      0.019           0.128           0.404
                                   3.44         260.38        26      0.013           0.404           0.556
                                   4.93         293.34        33      0.017           0.556           0.675
                                   5.67         293.34        33      0.019           0.675           0.776
                                   6.47         288.86        32      0.022           0.776           0.866
                                   7.26         270.21        28      0.027           0.866           0.946
                                   4.63         210.54        17      0.022           0.946           1.021
                                   1.66         102.13         4      0.016           1.021           1.090


 SUM FCALC                             83.00
 WEIGHTED    "GOODNESS OF FIT"          1.13
1CYCLE 6                                                                                   CYCLE NO.   4


 
 ESTIMATED STD. DEV. FOR OBS. OF UNIT WEIGHT             1.13                              STRUCTUREFACTOR EQUATION NO.   2
                                                                                           REFINEMENT ON     FOBS

 
0 NO EXTINCTION CORRECTION                                                   
0                            PARAMETER                   OLD          CHANGE         NEW         ERROR         SHIFT/ERROR NP.DAMP.
 




                           SCALE FACTOR  1          103.0813         0.0000     103.0813        0.77276            0.00    1      

 
0  ATOM  1    O 1          EQUIPOINT FRACTION =  0.167
 
                           OCCUPANCY SPECIES  1         1.00000                     1.00000
 
                           X                          0.3333300                   0.3333300
                           Y                          0.6666700                   0.6666700
                           Z                          0.0620377      0.0000000    0.0620378     0.0002222          0.00    2      
 
                           U11                        4.5524879     -0.0000003    4.5524879     0.0747570          0.00    3      
                           U22                        4.5524879                   4.5524879     0.0747570
                           U33                        5.0259485     -0.0000009    5.0259476     0.1150820          0.00    4      
                           U12                        2.2762439                   2.2762439     0.0373785
                           U13                        0.0000000                   0.0000000
                           U23                        0.0000000                   0.0000000
 
                           C(111)                     0.4534E-02    -0.8441E-07   0.4534E-02    0.1114E-02         0.00    5      
                           C(222)                    -0.4534E-02                 -0.4534E-02    0.1114E-02
                           C(333)                    -0.1575E-02     0.3426E-07  -0.1574E-02    0.6040E-03         0.00    6      
                           C(112)                     0.2267E-02                  0.2267E-02    0.5568E-03
                           C(122)                    -0.2267E-02                 -0.2267E-02    0.5568E-03
                           C(113)                     0.1349E-02     0.2521E-07   0.1349E-02    0.5897E-03         0.00    7      
                           C(133)                     0.0000E+00                  0.0000E+00
                           C(223)                     0.1349E-02                  0.1349E-02    0.5897E-03
                           C(233)                     0.0000E+00                  0.0000E+00
                           C(123)                     0.6744E-03                  0.6744E-03    0.2949E-03
 
                           D(1111)                   0.014265490   -0.000000084  0.014265406   0.004096580         0.00    8      
                           D(2222)                    0.1427E-01                  0.1427E-01    0.4097E-02
                           D(3333)                   0.003254977   -0.000000001  0.003254976   0.000722540         0.00    9      
                           D(1112)                    0.7133E-02                  0.7133E-02    0.2048E-02
                           D(1113)                   0.001527900   -0.000000007  0.001527893   0.000555923         0.00   10      
                           D(1122)                    0.7133E-02                  0.7133E-02    0.2048E-02
                           D(1123)                    0.7640E-03                  0.7639E-03    0.2780E-03
                           D(1133)                   0.002349758   -0.000000002  0.002349756   0.000508559         0.00   11      
                           D(1222)                    0.7133E-02                  0.7133E-02    0.2048E-02
                           D(1223)                   -0.7640E-03                 -0.7639E-03    0.2780E-03
                           D(1233)                    0.1175E-02                  0.1175E-02    0.2543E-03
                           D(1333)                    0.0000E+00                  0.0000E+00
                           D(2223)                   -0.1528E-02                 -0.1528E-02    0.5559E-03
                           D(2233)                    0.2350E-02                  0.2350E-02    0.5086E-03
                           D(2333)                    0.0000E+00                  0.0000E+00
0  ATOM  2    D 1          EQUIPOINT FRACTION =  0.167
 
                           OCCUPANCY SPECIES  2         0.48607        0.00000      0.48607       0.00204          0.00   12      
                           OCCUPANCY SPECIES  3         0.01393                     0.01393
                           TOTAL OCCUPANCY (FIXED) =    0.50000
 
                           X                          0.3333300                   0.3333300
                           Y                          0.6666700                   0.6666700
                           Z                          0.1981311      0.0000000    0.1981311     0.0002374          0.00   13      
 
                           U11                        5.2394176     -0.0000033    5.2394142     0.0814792          0.00   14      
                           U22                        5.2394176                   5.2394142     0.0814792
                           U33                        4.4449992     -0.0000023    4.4449964     0.0604402          0.00   15      
                           U12                        2.6197088                   2.6197071     0.0407396
                           U13                        0.0000000                   0.0000000
                           U23                        0.0000000                   0.0000000
 
                           C(111)                     0.0000E+00                  0.0000E+00
                           C(222)                     0.0000E+00                  0.0000E+00
                           C(333)                     0.0000E+00                  0.0000E+00
                           C(112)                     0.0000E+00                  0.0000E+00
                           C(122)                     0.0000E+00                  0.0000E+00
                           C(113)                    -0.7753E-03     0.1854E-07  -0.7753E-03    0.1010E-02         0.00   16      
                           C(133)                     0.0000E+00                  0.0000E+00
                           C(223)                    -0.7753E-03                 -0.7753E-03    0.1010E-02
                           C(233)                     0.0000E+00                  0.0000E+00
                           C(123)                    -0.3877E-03                 -0.3877E-03    0.5049E-03
 
                           D(1111)                   0.005934633    0.000000005  0.005934638   0.005522407         0.00   17      
                           D(2222)                    0.5935E-02                  0.5935E-02    0.5522E-02
                           D(3333)                    0.0000E+00                  0.0000E+00
                           D(1112)                    0.2967E-02                  0.2967E-02    0.2761E-02
                           D(1113)                    0.0000E+00                  0.0000E+00
                           D(1122)                    0.2967E-02                  0.2967E-02    0.2761E-02
                           D(1123)                    0.0000E+00                  0.0000E+00
                           D(1133)                  -0.001211036   -0.000000047 -0.001211083   0.000665997         0.00   18      
                           D(1222)                    0.2967E-02                  0.2967E-02    0.2761E-02
                           D(1223)                    0.0000E+00                  0.0000E+00
                           D(1233)                   -0.6055E-03                 -0.6055E-03    0.3330E-03
                           D(1333)                    0.0000E+00                  0.0000E+00
                           D(2223)                    0.0000E+00                  0.0000E+00
                           D(2233)                   -0.1211E-02                 -0.1211E-02    0.6660E-03
                           D(2333)                    0.0000E+00                  0.0000E+00
0  ATOM  3    D 2          EQUIPOINT FRACTION =  0.500
 
                           OCCUPANCY SPECIES  2         0.48607                     0.48607     0.0020445
                           OCCUPANCY SPECIES  3         0.01393                     0.01393
                           TOTAL OCCUPANCY (FIXED) =    0.50000
 
                           X                          0.4537697      0.0000000    0.4537697     0.0000999          0.00   19      
                           Y                          0.9075394                   0.9075394     0.0001998
                           Z                          0.0173168      0.0000000    0.0173168     0.0001492          0.00   20      
 
                           U11                        5.1042280     -0.0000023    5.1042256     0.0610748          0.00   21      
                           U22                        4.4083257     -0.0000006    4.4083247     0.0285559          0.00   22      
                           U33                        5.5433731     -0.0000049    5.5433683     0.0775435          0.00   23      
                           U12                        2.2041628                   2.2041624     0.0142780
                           U13                        0.1305893     -0.0000002    0.1305891     0.0108339          0.00   24      
                           U23                        0.2611786                   0.2611781     0.0216677
 
                           C(111)                    -0.2653E-02    -0.5636E-08  -0.2653E-02    0.1467E-02         0.00   25      
                           C(222)                     0.0000E+00                  0.0000E+00
                           C(333)                     0.4411E-03    -0.4777E-08   0.4411E-03    0.4105E-03         0.00   26      
                           C(112)                    -0.1768E-02                 -0.1768E-02
                           C(122)                     0.0000E+00                  0.0000E+00
                           C(113)                     0.5935E-03    -0.1665E-07   0.5935E-03    0.6264E-03         0.00   27      
                           C(133)                    -0.5216E-03     0.2046E-07  -0.5216E-03    0.2405E-03         0.00   28      
                           C(223)                     0.0000E+00                  0.0000E+00
                           C(233)                    -0.1043E-02                 -0.1043E-02    0.4810E-03
                           C(123)                     0.0000E+00                  0.0000E+00
 
                           D(1111)                   0.005266139   -0.000000089  0.005266050   0.003331403         0.00   29      
                           D(2222)                    0.0000E+00                  0.0000E+00
                           D(3333)                   0.001690432   -0.000000026  0.001690405   0.000511597         0.00   30      
                           D(1112)                    0.0000E+00                  0.0000E+00
                           D(1113)                    0.0000E+00                  0.0000E+00
                           D(1122)                    0.0000E+00                  0.0000E+00
                           D(1123)                    0.0000E+00                  0.0000E+00
                           D(1133)                   0.000469891   -0.000000004  0.000469887   0.000449049         0.00   31      
                           D(1222)                    0.0000E+00                  0.0000E+00
                           D(1223)                    0.0000E+00                  0.0000E+00
                           D(1233)                    0.0000E+00                  0.0000E+00
                           D(1333)                    0.0000E+00                  0.0000E+00
                           D(2223)                    0.0000E+00                  0.0000E+00
                           D(2233)                    0.0000E+00                  0.0000E+00
                           D(2333)                    0.0000E+00                  0.0000E+00



                         MAXIMUM SHIFT/ERROR =       0.00

                         AVERAGE SHIFT/ERROR =       0.00

0REMARK
 ------

 UIJ ARE MULTIPLIED BY 10**2. 

0REMARK
 ------

 THERMAL PARAMETERS OF THIRD, FOURTH, FIFTH AND SIXTH ORDER ARE MULTIPLIED BY 10**3, 10**4, 10**5 AND 10**6 RESPECTIVELY.
1CYCLE 6                                                                 
0CORRELATION COEFICIENTS WITH LARGEST MAGNITUDES

  PARAMETERS   VALUE     PARAMETERS   VALUE     PARAMETERS   VALUE     PARAMETERS   VALUE   

     4     9   0.9531       3     8   0.9482      23    30   0.9044      14    17   0.8970

     2     6   0.8715      21    29   0.8645       1     3   0.8158      20    26   0.7992

     1    12  -0.7239       1     4   0.7174       1     8   0.6814      13    16   0.6792

     3    12  -0.6765       2     7   0.6699       4    11   0.6699       1    11   0.6462

     3    11   0.6107       4    12  -0.5994       8    12  -0.5971       1     9   0.5819
1TITLE OF THE CYCLE
 ------------------

 CYCLE 6A                                                                

0CONTROL-PARAMETER
 -----------------

 P 2 1 0   5 0 0 0 0   0 0 0 0 0 0 0 0   0.000     0.000     0.000     0   0 0 0      0
1CYCLE 6A                                                                     STRUCTURE FACTORS          PAGE  1
0       H    K    L      F(OBS)     F(CALC)     A(CALC)     B(CALC)     DELTA F   DELT/WEIGHT   EXT. FACTOR      SINT/LAM


        6    2    1       0.098        0.068      -0.068       0.000       0.030        3.6470 *      1.0000        0.9254       
        6    1    4       0.050        0.007       0.007       0.000       0.043        3.5746 *      1.0000        0.8823       
        4    2    6       0.055        0.015      -0.015       0.000       0.040        3.5856 *      1.0000        0.7908       
1CYCLE 6A                                                                     RESULTS OF STRUCTURE FACTOR CALCULATIONS
                                                                              STRUCTURE FACTOR EQUATION NO.   2
0++++ NUMBER OF CYCLE =          5   ++++   
0ALL REFLECTIONS              NUMERATOR    DENOMINATOR    NUMBER      R(INT) 
 
          WEIGHTED R              18.48         711.60       304      0.026

          UNWEIGHTED R             3.44          84.33       304      0.041

              RANGES OF F(OBS)                                                        LOWER -         UPPER -      LIMIT 
                                  17.49         653.01       256      0.027           0.010           0.535
                                   4.24         234.45        33      0.018           0.535           1.060
                                   2.54         115.44         8      0.022           1.060           1.585
                                   0.69          70.69         3      0.010           1.585           2.110
                                   0.00           0.00         0      0.000           2.110           2.635
                                   1.36          70.69         3      0.019           2.635           3.160
                                   0.00           0.00         0      0.000           3.160           3.685
                                   2.97          40.81         1      0.073           3.685           4.210

              RANGES OF  SIN(THETA)/LAMBDA    
                                   4.77         191.43        22      0.025           0.128           0.404
                                   4.10         212.07        27      0.019           0.404           0.556
                                   4.93         234.45        33      0.021           0.556           0.675
                                   5.79         244.88        36      0.024           0.675           0.776
                                   7.16         270.72        44      0.026           0.776           0.866
                                   8.46         273.78        45      0.031           0.866           0.946
                                   7.86         273.78        45      0.029           0.946           1.021
                                   7.70         294.31        52      0.026           1.021           1.090

 UNREJECTED REFLECTIONS
 
          WEIGHTED R              14.40         711.25       194      0.020

          UNWEIGHTED R             1.57          80.43       194      0.020

              RANGES OF F(OBS)                                                        LOWER -         UPPER -      LIMIT 
                                  13.10         617.02       146      0.021           0.010           0.535
                                   4.24         293.34        33      0.014           0.535           1.060
                                   2.54         144.43         8      0.018           1.060           1.585
                                   0.69          88.45         3      0.008           1.585           2.110
                                   0.00           0.00         0      0.000           2.110           2.635
                                   1.36          88.45         3      0.015           2.635           3.160
                                   0.00           0.00         0      0.000           3.160           3.685
                                   2.97          51.06         1      0.058           3.685           4.210

              RANGES OF  SIN(THETA)/LAMBDA    
                                   4.51         234.01        21      0.019           0.128           0.404
                                   3.44         260.38        26      0.013           0.404           0.556
                                   4.93         293.34        33      0.017           0.556           0.675
                                   5.67         293.34        33      0.019           0.675           0.776
                                   6.47         288.86        32      0.022           0.776           0.866
                                   7.26         270.21        28      0.027           0.866           0.946
                                   4.63         210.54        17      0.022           0.946           1.021
                                   1.66         102.13         4      0.016           1.021           1.090


 SUM FCALC                             83.00
 WEIGHTED    "GOODNESS OF FIT"          1.13










  **************************************
  *                                    *
  * PARAMETERS WRITTEN OUT TO UNIT  10 *
  *                                    *
  **************************************


0PROGRAM FINISHED    29-Aug-94  11:48:48
