COMMAND FILE FOR SHELXL-97 APPLICATION AFTER THE RIETVELD REFINEMENT
TITL Cimetidine P21/n
CELL 1.52904 10.700 18.820 6.825 90. 111.285 90.
ZERR 4 .001 .001 .001  0  0.001  0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC S N C H
UNIT 4 24 40 64
L.S. 10
ACTA
WGHT    0.100000
FVAR       0.20089
S1      1   0.98225   0.41503   0.19332    11.00000     0.06166
C6      3   0.14177   0.39598   0.15023    11.00000     0.07330
N4      2   0.45158   0.37269   0.55990    11.00000     0.06746
N1      2   0.13296   0.23003   0.73484    11.00000     0.01762
N5      2   0.60019   0.40636   0.39380    11.00000     0.02201
N3      2   0.36284   0.44256   0.25554    11.00000     0.03143
C8      3   0.46544   0.40529   0.38373    11.00000     0.08578
C3      3   0.03672   0.28399   0.66286    11.00000     0.07166
C1      3   0.23339   0.25847   0.68097    11.00000     0.04662
N2      2   0.20613   0.31654   0.57497    11.00000     0.02112
C5      3   0.00746   0.40654   0.48431    11.00000     0.04670
C7      3   0.23358   0.46350   0.26609    11.00000     0.03099
C4      3   0.90373   0.28652   0.71387    11.00000     0.04716
C2      3   0.09607   0.33236   0.57021    11.00000     0.05999
N6      2   0.66480   0.49081   0.15447    11.00000     0.01508
C10     3   0.62061   0.45236   0.25369    11.00000     0.00413
C9      3   0.55481   0.39157   0.71394    11.00000     0.04022
HKLF 3
RESULTS

+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
+  SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION  +
+  Copyright(C) George M. Sheldrick 1993-7            Release 97-1  +
+  cim1                         started at 09:47:37 on 25-Jun-1997  +
+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++

TITL Cimetidine P21/n
CELL 1.52904 10.700 18.820 6.825 90. 111.285 90.
ZERR 4 .001 .001 .001  0  0.001  0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC S N C H
UNIT 4 24 40 64

V =     1280.63     F(000) =     536.0     Mu =   2.16 mm-1      Cell Wt =     1009.39    Rho =  1.309

L.S. 10
ACTA
WGHT    0.100000
FVAR       0.20089
S1      1   0.98225   0.41503   0.19332    11.00000     0.06166
C6      3   0.14177   0.39598   0.15023    11.00000     0.07330
N4      2   0.45158   0.37269   0.55990    11.00000     0.06746
N1      2   0.13296   0.23003   0.73484    11.00000     0.01762
N5      2   0.60019   0.40636   0.39380    11.00000     0.02201
N3      2   0.36284   0.44256   0.25554    11.00000     0.03143
C8      3   0.46544   0.40529   0.38373    11.00000     0.08578
C3      3   0.03672   0.28399   0.66286    11.00000     0.07166
C1      3   0.23339   0.25847   0.68097    11.00000     0.04662
N2      2   0.20613   0.31654   0.57497    11.00000     0.02112
C5      3   0.00746   0.40654   0.48431    11.00000     0.04670
C7      3   0.23358   0.46350   0.26609    11.00000     0.03099
C4      3   0.90373   0.28652   0.71387    11.00000     0.04716
C2      3   0.09607   0.33236   0.57021    11.00000     0.05999
N6      2   0.66480   0.49081   0.15447    11.00000     0.01508
C10     3   0.62061   0.45236   0.25369    11.00000     0.00413
C9      3   0.55481   0.39157   0.71394    11.00000     0.04022
HKLF 3


Covalent radii and connectivity table for  Cimetidine P21/n                                                           

S    1.030
N    0.700
C    0.770
H    0.320

S1 - C6_$2 C5_$2
C6 - C7 S1_$1
N4 - C9 C8
N1 - C1 C3
N5 - C10 C8
N3 - C8 C7
C8 - N3 N4 N5
C3 - C2 N1 C4_$1
C1 - N2 N1 C2
N2 - C2 C1
C5 - C2 S1_$1
C7 - N3 C6
C4 - C3_$2
C2 - N2 C3 C5 C1
N6 - C10
C10 - N6 N5
C9 - N4


Operators for generating equivalent atoms:

$1   x-1, y, z
$2   x+1, y, z


    924  Reflections read, of which     0  rejected

  0 =< h =<  9,      0 =< k =< 16,     -6 =< l =<  5,   Max. 2-theta =   84.94

      0  Systematic absence violations

      0  Inconsistent equivalents

    924  Unique reflections, of which      0  suppressed

R(int) = 0.0000     R(sigma) = 0.0950      Friedel opposites merged

Maximum memory for data reduction =  1208 /    9253



  ** Cell contents from UNIT instruction and atom list do not agree **


Unit-cell contents from UNIT instruction and atom list resp.

S         4.00      4.00
N        24.00     24.00
C        40.00     40.00
H        64.00      0.00


Least-squares cycle   1      Maximum vector length =  511      Memory required =   1379 /   96066

wR2 =  0.9272 before cycle   1 for    924 data and    69 /    69 parameters

GooF = S =     9.651;     Restrained GooF =      9.651  for      0 restraints

Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 +   0.00 * P ]   where  P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3


    N      value        esd    shift/esd  parameter

    1     0.36237     0.02650     6.093    OSF
    8     0.07711     0.01805    -4.051     z  C6
   17     0.09755     0.01902     4.202    U11 N1
   21     0.13123     0.02261     4.830    U11 N5
   22     0.38894     0.00738     3.538     x  N3
   25     0.11712     0.02243     3.820    U11 N3
   37     0.14221     0.02598     3.679    U11 C1
   41     0.12475     0.02211     4.686    U11 N2
   49     0.14922     0.02668     4.431    U11 C7
   50     0.87114     0.00895    -3.640     x  C4
   55     0.35000     0.00541     3.260     y  C2
   61     0.13760     0.02111     5.805    U11 N6
   65     0.11381     0.02144     5.115    U11 C10
   69     0.25039     0.02593     8.106    U11 C9

Mean shift/esd =   1.826    Maximum =   8.106 for  U11 C9       

Max. shift = 0.469 A for C6      Max. dU = 0.210 for C9           



Least-squares cycle  10      Maximum vector length =  511      Memory required =   1379 /   96066

wR2 =  0.2128 before cycle  10 for    924 data and    69 /    69 parameters

GooF = S =     1.205;     Restrained GooF =      1.205  for      0 restraints

Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 +   0.00 * P ]   where  P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3


    N      value        esd    shift/esd  parameter

    1     0.50420     0.00376     0.037    OSF

Mean shift/esd =   0.188    Maximum =  -0.606 for   z  C6       

Max. shift = 0.002 A for C6      Max. dU = 0.000 for C4           


Largest correlation matrix elements

    0.838 U11 S1 / OSF                      0.720 U11 C7 / U11 S1                   0.701 U11 C5 / U11 S1
    0.808 U11 N1 / U11 S1                   0.719 U11 N2 / U11 S1                   0.700 U11 C4 / U11 N5
    0.787 U11 C4 / U11 S1                   0.717 U11 C9 / U11 S1                   0.698 U11 C10 / U11 S1
    0.759 U11 C2 / U11 S1                   0.717 U11 C2 / U11 N1                   0.695 U11 C4 / U11 C6
    0.750 U11 C3 / U11 S1                   0.713 U11 C6 / U11 S1                   0.691 U11 C2 / OSF 
    0.743 U11 N4 / U11 S1                   0.711 U11 C1 / U11 S1                   0.690 U11 C4 / U11 N4
    0.727 U11 N3 / U11 S1                   0.710 U11 N6 / U11 S1                   0.683 U11 C2 / U11 N4
    0.725 U11 N1 / OSF                      0.707 U11 C4 / OSF                      0.682 U11 C3 / U11 N1



 Cimetidine P21/n                                                           

ATOM           x         y         z          sof         U11       U22       U33       U23       U13       U12        Ueq

S1          0.98468   0.41389   0.19880     1.00000     0.04633
  0.00223   0.00010   0.00005   0.00019     0.00000     0.00096

C6          0.14412   0.39432   0.14410     1.00000     0.03522
  0.00698   0.00034   0.00020   0.00054     0.00000     0.00120

N4          0.45193   0.37313   0.55985     1.00000     0.04469
  0.00585   0.00028   0.00014   0.00046     0.00000     0.00113

N1          0.12804   0.23565   0.72779     1.00000     0.03509
  0.00569   0.00029   0.00013   0.00039     0.00000     0.00112

N5          0.59391   0.40922   0.39058     1.00000     0.05532
  0.00665   0.00036   0.00012   0.00052     0.00000     0.00132

N3          0.36866   0.44607   0.24637     1.00000     0.05525
  0.00686   0.00037   0.00016   0.00050     0.00000     0.00128

C8          0.46100   0.40386   0.40125     1.00000     0.03615
  0.00712   0.00035   0.00014   0.00060     0.00000     0.00133

C3          0.02816   0.28808   0.66757     1.00000     0.02883
  0.00691   0.00033   0.00017   0.00054     0.00000     0.00119

C1          0.23103   0.25175   0.67590     1.00000     0.05184
  0.00724   0.00034   0.00021   0.00056     0.00000     0.00131

N2          0.21052   0.31729   0.56755     1.00000     0.04183
  0.00543   0.00026   0.00012   0.00042     0.00000     0.00121

C5          0.02485   0.41153   0.49316     1.00000     0.02554
  0.00626   0.00032   0.00015   0.00051     0.00000     0.00129

C7          0.23588   0.46336   0.27745     1.00000     0.02866
  0.00718   0.00032   0.00021   0.00048     0.00000     0.00118

C4          0.89656   0.28138   0.70832     1.00000     0.01420
  0.00602   0.00028   0.00014   0.00049     0.00000     0.00112

C2          0.08661   0.33688   0.57698     1.00000     0.01462
  0.00555   0.00024   0.00014   0.00041     0.00000     0.00116

N6          0.66679   0.48744   0.15076     1.00000     0.05794
  0.00627   0.00030   0.00016   0.00057     0.00000     0.00127

C10         0.62397   0.44966   0.25845     1.00000     0.02596
  0.00779   0.00037   0.00016   0.00058     0.00000     0.00125

C9          0.56400   0.34167   0.72801     1.00000     0.03313
  0.00637   0.00029   0.00020   0.00046     0.00000     0.00124



Final Structure Factor Calculation for  Cimetidine P21/n                                                           

Total number of l.s. parameters =    69     Maximum vector length =  511      Memory required =   1310 /   22995

wR2 =  0.2092 before cycle  11 for    924 data and     0 /    69 parameters

GooF = S =     1.182;     Restrained GooF =      1.182  for      0 restraints

Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 +   0.00 * P ]   where  P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3

R1 =  0.0753 for    849 Fo > 4sig(Fo)  and  0.0789 for all    924 data
wR2 =  0.2092,  GooF = S =   1.182,  Restrained GooF =    1.182  for all data

Occupancy sum of asymmetric unit =   17.00 for non-hydrogen and    0.00 for hydrogen atoms



Analysis of variance for reflections employed in refinement      K = Mean[Fo^2] / Mean[Fc^2]  for group


Fc/Fc(max)       0.000    0.012    0.025    0.040    0.056    0.070    0.093    0.117    0.156    0.211    1.000

Number in group        94.      94.      89.      94.      92.      92.      92.      96.      89.      92.

           GooF      1.517    1.346    1.071    0.945    0.993    1.216    1.219    1.153    1.151    1.062

            K        2.115    1.331    1.169    1.209    1.131    1.083    1.112    1.120    1.017    1.016


Resolution(A)    1.13     1.17     1.22     1.28     1.34     1.43     1.54     1.68     1.94     2.45     inf

Number in group        95.      91.      94.      90.      94.      92.      91.      94.      91.      92.

           GooF      0.985    1.075    0.989    0.985    0.887    1.139    1.324    1.222    1.382    1.621

            K        1.161    1.179    1.062    0.970    1.027    1.083    1.000    1.016    1.083    1.018

            R1       0.107    0.102    0.082    0.078    0.084    0.092    0.083    0.075    0.076    0.054


Recommended weighting scheme:  WGHT      0.1073      0.0920
Note that in most cases convergence will be faster if fixed weights (e.g. the
default WGHT 0.1) are retained until the refinement is virtually complete, and
only then should the above recommended values be used.





Bond lengths and angles

S1 -        Distance       Angles
C6_$2     1.9100 (0.0034) 
C5_$2     1.8963 (0.0036)  109.12 (0.14)
              S1 -          C6_$2        

C6 -        Distance       Angles
C7        1.6828 (0.0054) 
S1_$1     1.9100 (0.0034)   97.62 (0.20)
              C6 -          C7           

N4 -        Distance       Angles
C9        1.4513 (0.0036) 
C8        1.2617 (0.0044)  124.51 (0.30)
              N4 -          C9           

N1 -        Distance       Angles
C1        1.3096 (0.0036) 
C3        1.4022 (0.0039)  112.61 (0.25)
              N1 -          C1           

N5 -        Distance       Angles
C10       1.3063 (0.0040) 
C8        1.4537 (0.0041)  124.44 (0.30)
              N5 -          C10          

N3 -        Distance       Angles
C8        1.4023 (0.0047) 
C7        1.5453 (0.0049)  116.56 (0.26)
              N3 -          C8           

C8 -        Distance       Angles
N3        1.4023 (0.0047) 
N4        1.2617 (0.0044)  130.83 (0.32)
N5        1.4537 (0.0041)  110.93 (0.24) 117.14 (0.31)
              C8 -          N3            N4           

C3 -        Distance       Angles
C2        1.3775 (0.0041) 
N1        1.4022 (0.0039)  100.30 (0.20)
C4_$1     1.5363 (0.0042)  136.99 (0.25) 122.71 (0.24)
              C3 -          C2            N1           

C1 -        Distance       Angles
N2        1.4137 (0.0043) 
N1        1.3096 (0.0036)  110.94 (0.28)
C2        2.1570 (0.0043)   39.71 (0.15)  71.28 (0.19)
              C1 -          N2            N1           

N2 -        Distance       Angles
C2        1.3999 (0.0033) 
C1        1.4137 (0.0043)  100.10 (0.23)
              N2 -          C2           

C5 -        Distance       Angles
C2        1.5695 (0.0040) 
S1_$1     1.8963 (0.0036)  108.10 (0.19)
              C5 -          C2           

C7 -        Distance       Angles
N3        1.5453 (0.0049) 
C6        1.6828 (0.0054)   98.52 (0.26)
              C7 -          N3           

C4 -        Distance       Angles
C3_$2     1.5363 (0.0042) 
              C4 -         

C2 -        Distance       Angles
N2        1.3999 (0.0033) 
C3        1.3775 (0.0041)  115.91 (0.24)
C5        1.5695 (0.0040)  119.96 (0.21) 124.10 (0.21)
C1        2.1570 (0.0043)   40.18 (0.15)  75.81 (0.19) 159.71 (0.19)
              C2 -          N2            C3            C5           

N6 -        Distance       Angles
C10       1.2249 (0.0040) 
              N6 -         

C10 -       Distance       Angles
N6        1.2249 (0.0040) 
N5        1.3063 (0.0040)  172.72 (0.42)
              C10 -         N6           

C9 -        Distance       Angles
N4        1.4513 (0.0036) 
              C9 -         


FMAP and GRID set by program

FMAP   2   3   9
GRID    -4.167  -2  -2     4.167   2   2

R1 =  0.0789 for    924 unique reflections after merging for Fourier


Electron density synthesis with coefficients Fo-Fc

Highest peak    0.33  at  0.9824  0.4192  0.1996  [  0.10 A from S1 ]
Deepest hole   -0.26  at  0.0932  0.9013  0.0959  [  0.59 A from C8 ]

Mean =    0.00,   Rms deviation from mean =    0.07 e/A^3,   Highest memory used =  1556 / 12978


Fourier peaks appended to .res file

             x       y       z       sof     U      Peak   Distances to nearest atoms (including symmetry equivalents)

Q1    1   0.2560  0.4634  0.4553   1.00000  0.05    0.29   1.15 C7  2.20 N3  2.41 C6  2.51 C10
Q2    1   0.9202  0.3055  0.7833   1.00000  0.05    0.26   0.66 C4  1.65 C3  2.71 C2  2.73 N1
Q3    1   0.6063  0.3841  0.8373   1.00000  0.05    0.25   1.07 C9  2.02 N4  2.79 N6  2.84 C8
Q4    1  -0.1067  0.4246  0.4678   1.00000  0.05    0.24   1.38 C5  2.38 S1  2.54 C2  2.75 C10
Q5    1   0.8774  0.2480  0.5984   1.00000  0.05    0.23   0.94 C4  1.69 C3  2.51 N1  2.74 C1
Q6    1   0.1070  0.2047  0.6554   1.00000  0.05    0.23   0.74 N1  1.56 C1  1.80 C3  2.54 C2
Q7    1   0.8997  0.2208  0.6690   1.00000  0.05    0.23   1.17 C4  1.87 C3  2.34 N1  2.77 C8
Q8    1   0.1206  0.3712 -0.0458   1.00000  0.05    0.23   1.30 C6  2.42 C3  2.55 C2  2.70 S1
Q9    1   0.8360  0.3398  0.6694   1.00000  0.05    0.21   1.25 C4  2.28 C3  2.91 N5  2.97 C2
Q10   1   0.8054  0.1961  0.7363   1.00000  0.05    0.21   1.92 C4  2.34 C6  2.49 C8  2.55 N4
Q11   1   0.1763  0.4986  0.0811   1.00000  0.05    0.20   1.42 C7  2.06 C6  2.19 N3  2.63 S1
Q12   1   0.5734  0.3104  0.6272   1.00000  0.05    0.20   0.94 C9  1.69 N4  2.36 C8  2.52 N5
Q13   1   0.5362  0.2890  0.8192   1.00000  0.05    0.20   1.26 C9  2.30 N4  2.64 N1  2.68 C1
Q14   1   0.3090  0.3207  0.9584   1.00000  0.05    0.19   2.22 C1  2.49 N2  2.51 C4  2.56 N1
Q15   1   0.0243  0.2960  0.4534   1.00000  0.05    0.19   1.16 C2  1.45 C3  1.90 N2  2.13 N1
Q16   1   0.6817  0.4060  0.6353   1.00000  0.05    0.19   1.59 N5  2.01 C9  2.32 C8  2.40 N4
Q17   1   0.3525  0.1792  0.7121   1.00000  0.05    0.18   1.84 C1  2.27 S1  2.66 N1  2.72 C5
Q18   1   1.0267  0.2630  1.0398   1.00000  0.05    0.18   2.21 C4  2.31 C9  2.59 C3  2.70 N4
Q19   1   0.1512  0.3589  0.2245   1.00000  0.05    0.18   0.85 C6  2.01 S1  2.14 C7  2.33 N2
Q20   1   0.0372  0.3979  0.4168   1.00000  0.05    0.18   0.64 C5  1.42 S1  1.54 C2  2.33 N2

Shortest distances between peaks (including symmetry equivalents)

     5   7  0.68      2   9  1.15      7  10  1.33     12  18  1.52     12  13  1.55      2   5  1.60      7  14  1.61
     5  14  1.62      5  10  1.72      2   7  1.75      8  19  1.77      4  20  1.77     13  15  1.87      3  16  1.88
     2  18  1.88      5   9  1.89     10  19  1.92      3  13  1.93      3  12  1.93     10  14  1.94     15  20  1.95
     9  16  2.01     15  17  2.03     13  18  2.11     12  16  2.13      6  13  2.14      6  15  2.18     19  20  2.22
     8  14  2.22      6   7  2.27     18  19  2.32      5  15  2.32      4   9  2.33      7   9  2.34      2  10  2.36
     2   8  2.38      8  18  2.43     17  20  2.44      1  11  2.47      5   6  2.48      1  19  2.52      7  18  2.53
     8  10  2.54      8  11  2.54      4  17  2.55      6  17  2.56      1  20  2.57     11  16  2.67      1  16  2.68
    15  19  2.69      7  15  2.71      3   6  2.74     13  17  2.76     17  18  2.76      9  12  2.77      9  10  2.78
     1   4  2.81     10  18  2.81      4  15  2.82     11  19  2.85      2  15  2.86      5  18  2.87     10  18  2.89
     5  17  2.90     15  18  2.90      4  16  2.90     13  14  2.97     14  19  2.98      9  18  2.98


Time profile in seconds
-----------------------

     0.33: Read and process instructions
     0.00: Fit rigid groups
     0.00: Interpret restraints etc.
     0.00: Generate connectivity array
     0.05: Analyse DFIX/DANG restraints
     0.00: Analyse SAME/SADI restraints
     0.00: Generate CHIV restraints
     0.00: Check if bonds in residues restrained
     0.00: Generate DELU restraints
     0.00: Generate SIMU restraints
     0.00: Generate ISOR restraints
     0.00: Generate NCSY restraints
     0.00: Analyse other restraints etc.
     0.44: Read intensity data, sort/merge etc.
     0.00: Set up constraints
     0.00: OSF, H-atoms from difference map
     0.30: Set up l.s. refinement
     0.06: Generate idealized H-atoms
     5.45: Structure factors and derivatives
     2.63: Sum l.s. matrices
     0.00: Generate and apply antibumping restraints
     0.05: Apply other restraints
     0.48: Solve l.s. equations
     0.00: Generate HTAB table
     0.20: Other dependent quantities, CIF, tables
     0.83: Analysis of variance
     0.33: Merge reflections for Fourier and .fcf
     0.17: Fourier summations
     0.33: Peaksearch
     0.05: Analyse peaklist

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+  cim1          finished at 09:47:48   Total elapsed time:      11.8 secs  +
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