COMMAND FILE FOR THE SHELXL-97 APPLICATION TO THE CIMETIDINE
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
S1 1 0.9845 0.4155 0.1894 11.000000 0.05
X1 2 1.1306 0.4027 0.1580 11.000000 0.05
X2 2 1.4542 0.3760 0.5303 11.000000 0.05
X3 2 1.1253 0.2302 0.7204 11.000000 0.05
X4 2 1.6110 0.4146 0.3926 11.000000 0.05
X5 2 1.3572 0.4440 0.2194 11.000000 0.05
X6 2 1.4604 0.4060 0.4097 11.000000 0.05
X7 3 1.0240 0.2870 0.6435 11.000000 0.05
X8 3 1.2434 0.2524 0.6879 11.000000 0.05
X9 3 1.1971 0.3173 0.5485 11.000000 0.05
X10 3 1.0390 0.4136 0.4908 11.000000 0.05
X11 3 1.2421 0.4605 0.2669 11.000000 0.05
X12 3 0.8994 0.2834 0.6915 11.000000 0.05
X13 3 1.0866 0.3353 0.5644 11.000000 0.05
X14 3 1.6747 0.4927 0.1602 11.000000 0.05
X15 3 1.6247 0.4552 0.2491 11.000000 0.05
X16 3 1.5116 0.3864 0.8810 11.000000 0.05
HKLF 3
END
RESULT
+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
+ SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION +
+ Copyright(C) George M. Sheldrick 1993-7 Release 97-1 +
+ cim started at 17:21:25 on 24-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
S1 1 0.9845 0.4155 0.1894 11.000000 0.05
X1 2 1.1306 0.4027 0.1580 11.000000 0.05
X2 2 1.4542 0.3760 0.5303 11.000000 0.05
X3 2 1.1253 0.2302 0.7204 11.000000 0.05
X4 2 1.6110 0.4146 0.3926 11.000000 0.05
X5 2 1.3572 0.4440 0.2194 11.000000 0.05
X6 2 1.4604 0.4060 0.4097 11.000000 0.05
X7 3 1.0240 0.2870 0.6435 11.000000 0.05
X8 3 1.2434 0.2524 0.6879 11.000000 0.05
X9 3 1.1971 0.3173 0.5485 11.000000 0.05
X10 3 1.0390 0.4136 0.4908 11.000000 0.05
X11 3 1.2421 0.4605 0.2669 11.000000 0.05
X12 3 0.8994 0.2834 0.6915 11.000000 0.05
X13 3 1.0866 0.3353 0.5644 11.000000 0.05
X14 3 1.6747 0.4927 0.1602 11.000000 0.05
X15 3 1.6247 0.4552 0.2491 11.000000 0.05
X16 3 1.5116 0.3864 0.8810 11.000000 0.05
HKLF 3
Covalent radii and connectivity table for Cimetidine P21/n
S 1.030
N 0.700
C 0.770
H 0.320
S1 - X1 X10
X1 - X11 S1
X2 - X6
X3 - X8 X7
X4 - X15 X6
X5 - X11 X6
X6 - X2 X5 X4
X7 - X13 X3 X12
X8 - X3 X9
X9 - X13 X8
X10 - X13 S1
X11 - X5 X1
X12 - X7
X13 - X9 X7 X10
X14 - X15
X15 - X14 X4
X16 - no bonds found
378 Reflections read, of which 0 rejected
0 =< h =< 9, 0 =< k =< 16, -5 =< l =< 5, Max. 2-theta = 84.94
0 Systematic absence violations
0 Inconsistent equivalents
378 Unique reflections, of which 0 suppressed
R(int) = 0.0000 R(sigma) = 0.0700 Friedel opposites merged
Maximum memory for data reduction = 1078 / 4705
** 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 = 1249 / 96066
wR2 = 0.7649 before cycle 1 for 378 data and 69 / 69 parameters
GooF = S = 10.656; Restrained GooF = 10.656 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 0.19941 0.01251 -7.445 OSF
Mean shift/esd = 0.667 Maximum = -7.445 for OSF
Max. shift = 0.151 A for X12 Max. dU =-0.045 for X11
Least-squares cycle 10 Maximum vector length = 511 Memory required = 1249 / 96066
wR2 = 0.4031 before cycle 10 for 378 data and 69 / 69 parameters
GooF = S = 2.686; Restrained GooF = 2.686 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 0.20089 0.00456 0.045 OSF
Mean shift/esd = 0.094 Maximum = 0.367 for z X13
Max. shift = 0.016 A for X13 Max. dU =-0.004 for X16
Largest correlation matrix elements
0.722 U11 S1 / OSF 0.512 U11 X3 / OSF
Cimetidine P21/n
ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq
S1 0.98225 0.41503 0.19332 1.00000 0.06166
0.02034 0.00098 0.00053 0.00147 0.00000 0.00502
X1 1.14177 0.39598 0.15023 1.00000 0.07330
0.05762 0.00273 0.00128 0.00446 0.00000 0.01071
X2 1.45158 0.37269 0.55990 1.00000 0.06746
0.05492 0.00250 0.00156 0.00463 0.00000 0.01045
X3 1.13296 0.23003 0.73484 1.00000 0.01762
0.04104 0.00201 0.00097 0.00309 0.00000 0.00807
X4 1.60019 0.40636 0.39380 1.00000 0.02201
0.04319 0.00208 0.00093 0.00365 0.00000 0.00764
X5 1.36284 0.44256 0.25554 1.00000 0.03143
0.04670 0.00229 0.00120 0.00343 0.00000 0.00813
X6 1.46544 0.40529 0.38373 1.00000 0.08578
0.06496 0.00342 0.00157 0.00526 0.00000 0.01153
X7 1.03672 0.28399 0.66286 1.00000 0.07166
0.07582 0.00380 0.00200 0.00560 0.00000 0.01234
X8 1.23339 0.25847 0.68097 1.00000 0.04662
0.07100 0.00368 0.00175 0.00522 0.00000 0.01018
X9 1.20613 0.31654 0.57497 1.00000 0.02112
0.05293 0.00276 0.00162 0.00400 0.00000 0.00850
X10 1.00746 0.40654 0.48431 1.00000 0.04670
0.06649 0.00345 0.00145 0.00522 0.00000 0.01111
X11 1.23358 0.46350 0.26609 1.00000 0.03099
0.05289 0.00249 0.00147 0.00420 0.00000 0.00979
X12 0.90373 0.28652 0.71387 1.00000 0.04716
0.06733 0.00337 0.00141 0.00554 0.00000 0.00999
X13 1.09607 0.33236 0.57021 1.00000 0.05999
0.07446 0.00384 0.00183 0.00558 0.00000 0.01181
X14 1.66480 0.49081 0.15447 1.00000 0.01508
0.04689 0.00224 0.00122 0.00414 0.00000 0.00823
X15 1.62061 0.45236 0.25369 1.00000 0.00413
0.04903 0.00231 0.00124 0.00378 0.00000 0.00775
X16 1.55481 0.33157 0.73394 1.00000 0.10022
0.08825 0.00441 0.00199 0.00712 0.00000 0.01657
Final Structure Factor Calculation for Cimetidine P21/n
Total number of l.s. parameters = 69 Maximum vector length = 511 Memory required = 1180 / 22995
wR2 = 0.4024 before cycle 11 for 378 data and 0 / 69 parameters
GooF = S = 2.680; Restrained GooF = 2.680 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 = 0.1817 for 350 Fo > 4sig(Fo) and 0.1898 for all 378 data
wR2 = 0.4024, GooF = S = 2.680, Restrained GooF = 2.680 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 0.014 0.028 0.040 0.057 0.072 0.092 0.122 0.180 0.254 1.000
Number in group 40. 40. 35. 38. 37. 37. 38. 39. 36. 38.
GooF 3.010 3.147 2.769 2.656 1.977 3.129 1.988 2.634 2.788 2.370
K 30.324 5.526 2.419 1.835 1.407 1.374 1.181 1.077 1.123 0.933
Resolution(A) 1.13 1.22 1.31 1.40 1.52 1.71 1.90 2.13 2.53 3.21 inf
Number in group 38. 38. 38. 38. 37. 38. 40. 36. 37. 38.
GooF 2.098 2.321 2.055 2.521 2.297 2.647 3.740 2.358 3.305 2.886
K 1.461 1.370 1.202 1.581 1.162 1.117 1.149 0.988 0.985 0.944
R1 0.352 0.322 0.299 0.275 0.216 0.206 0.168 0.124 0.134 0.103
Recommended weighting scheme: WGHT 0.1840 55.8211
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.
Most Disagreeable Reflections (* if suppressed or used for Rfree)
h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A)
-3 6 2 73.30 22.52 4.02 0.028 2.12
4 2 1 104.12 4.43 3.49 0.012 2.03
0 6 1 582.80 183.30 3.08 0.080 2.81
-4 1 1 3025.22 1497.79 3.01 0.228 2.65
-3 0 1 698.59 176.51 2.80 0.078 3.52
-4 2 2 727.83 289.50 2.54 0.100 2.36
-1 2 2 1526.76 3082.98 2.46 0.327 3.20
-1 5 2 96.15 244.60 2.45 0.092 2.53
-1 7 2 118.83 1.19 2.43 0.006 2.11
-6 2 1 1427.30 634.87 2.31 0.148 1.74
1 0 1 1155.78 2227.72 2.30 0.278 4.65
-7 1 2 752.20 119.08 2.29 0.064 1.52
-2 7 3 235.04 586.70 2.18 0.142 1.73
-1 1 3 132.21 45.30 2.16 0.040 2.23
2 7 4 61.85 9.37 2.06 0.018 1.23
-7 2 2 432.90 67.87 2.01 0.048 1.50
2 3 0 154.85 54.97 2.00 0.044 3.90
2 9 3 72.45 2.03 1.99 0.008 1.34
2 11 0 97.13 18.56 1.99 0.025 1.62
0 2 2 82.07 211.59 1.95 0.086 3.01
-1 3 1 2138.28 1356.65 1.94 0.217 4.53
-5 1 1 5245.16 3291.22 1.94 0.337 2.12
2 7 1 58.76 11.29 1.90 0.020 2.10
-3 2 3 151.16 88.49 1.86 0.055 2.13
-4 12 2 339.18 788.44 1.85 0.165 1.32
-5 9 3 774.21 188.99 1.85 0.081 1.37
4 1 1 422.60 211.93 1.81 0.086 2.07
-1 6 5 93.25 22.89 1.81 0.028 1.22
0 9 1 78.50 0.54 1.80 0.004 1.99
-1 16 1 289.79 51.23 1.76 0.042 1.16
0 10 0 398.40 935.23 1.75 0.180 1.88
3 4 2 559.01 236.90 1.74 0.091 1.82
0 4 3 69.10 134.80 1.74 0.068 1.93
-2 1 1 201.24 119.66 1.73 0.064 4.72
-6 2 2 1122.18 632.55 1.72 0.148 1.73
-5 5 4 1082.52 512.32 1.65 0.133 1.43
1 4 3 616.93 993.56 1.63 0.185 1.79
1 7 0 2695.26 1827.31 1.60 0.251 2.60
-7 3 2 112.41 43.47 1.57 0.039 1.48
-6 11 2 33.92 69.78 1.56 0.049 1.23
0 2 1 4609.58 6940.36 1.56 0.490 5.27
-6 9 2 76.75 7.04 1.55 0.016 1.35
-7 10 2 15.86 42.62 1.54 0.038 1.18
-5 12 1 23.31 68.71 1.53 0.049 1.26
-4 6 1 396.42 190.48 1.52 0.081 2.03
-4 3 2 105.14 10.11 1.52 0.019 2.27
0 7 2 132.21 11.36 1.48 0.020 2.05
-3 3 1 2572.65 1787.87 1.48 0.249 3.07
-1 1 2 173.99 91.44 1.48 0.056 3.35
0 5 1 128.80 64.80 1.47 0.047 3.24
Bond lengths and angles
S1 - Distance Angles
X1 1.8689 (0.0269)
X10 1.9114 (0.0338) 110.80 (1.32)
S1 - X1
X1 - Distance Angles
X11 1.6251 (0.0343)
S1 1.8689 (0.0268) 101.47 (1.67)
X1 - X11
X2 - Distance Angles
X6 1.4048 (0.0350)
X2 -
X3 - Distance Angles
X8 1.3650 (0.0332)
X7 1.4021 (0.0359) 99.87 (2.32)
X3 - X8
X4 - Distance Angles
X15 1.3650 (0.0264)
X6 1.4185 (0.0394) 113.17 (2.29)
X4 - X15
X5 - Distance Angles
X11 1.4649 (0.0303)
X6 1.3286 (0.0346) 132.75 (2.48)
X5 - X11
X6 - Distance Angles
X2 1.4048 (0.0350)
X5 1.3286 (0.0345) 118.39 (2.97)
X4 1.4185 (0.0393) 112.70 (2.93) 127.35 (2.91)
X6 - X2 X5
X7 - Distance Angles
X13 1.3868 (0.0385)
X3 1.4021 (0.0359) 103.62 (3.09)
X12 1.5837 (0.0416) 132.63 (3.44) 123.30 (3.17)
X7 - X13 X3
X8 - Distance Angles
X3 1.3650 (0.0331)
X9 1.2843 (0.0317) 116.44 (3.07)
X8 - X3
X9 - Distance Angles
X13 1.2036 (0.0328)
X8 1.2843 (0.0317) 104.22 (3.31)
X9 - X13
X10 - Distance Angles
X13 1.6697 (0.0415)
S1 1.9114 (0.0338) 106.42 (1.98)
X10 - X13
X11 - Distance Angles
X5 1.4649 (0.0303)
X1 1.6251 (0.0343) 100.40 (2.06)
X11 - X5
X12 - Distance Angles
X7 1.5837 (0.0416)
X12 -
X13 - Distance Angles
X9 1.2036 (0.0327)
X7 1.3868 (0.0386) 115.52 (3.67)
X10 1.6697 (0.0415) 129.91 (3.66) 114.41 (3.38)
X13 - X9 X7
X14 - Distance Angles
X15 1.1993 (0.0267)
X14 -
X15 - Distance Angles
X14 1.1993 (0.0267)
X4 1.3650 (0.0264) 167.01 (2.59)
X15 - X14
FMAP and GRID set by program
FMAP 2 3 9
GRID -4.167 -2 -2 4.167 2 2
R1 = 0.1854 for 378 unique reflections after merging for Fourier
Electron density synthesis with coefficients Fo-Fc
Highest peak 0.40 at 0.4393 0.9381 -0.0161 [ 0.80 A from X10 ]
Deepest hole -0.43 at 0.0644 0.3941 0.1535 [ 0.84 A from X1 ]
Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 1426 / 12312
Fourier peaks appended to .res file
x y z sof U Peak Distances to nearest atoms (including symmetry equivalents)
Q1 1 1.0607 0.4381 0.5161 1.00000 0.05 0.40 0.80 X10 2.03 X13 2.10 S1 2.71 X9
Q2 1 1.1591 0.5470 0.1282 1.00000 0.05 0.35 1.86 X11 2.28 S1 2.83 X5 2.86 X1
Q3 1 1.5706 0.3795 0.8178 1.00000 0.05 0.33 1.05 X16 1.76 X2 2.80 X6 3.00 X14
Q4 1 1.2337 0.4810 0.4357 1.00000 0.05 0.31 1.20 X11 2.28 X5 2.44 X1 2.47 X15
Q5 1 1.4210 0.4647 0.1298 1.00000 0.05 0.29 1.30 X5 1.97 X6 2.00 X14 2.00 X15
Q6 1 1.0562 0.3151 0.6770 1.00000 0.05 0.28 0.62 X7 1.02 X13 1.78 X3 1.82 X12
Q7 1 1.4024 0.4634 0.4686 1.00000 0.05 0.28 1.41 X5 1.51 X6 1.83 X2 1.83 X11
Q8 1 1.2420 0.3442 0.5435 1.00000 0.05 0.27 0.72 X9 1.65 X13 1.89 X8 2.27 X2
Q9 1 0.9977 0.4030 0.3046 1.00000 0.05 0.27 0.75 S1 1.19 X10 2.16 X1 2.19 X13
Q10 1 1.1586 0.3643 -0.0453 1.00000 0.05 0.26 1.53 X1 2.46 X7 2.53 X13 2.72 X11
Q11 1 1.6515 0.4528 0.1368 1.00000 0.05 0.25 0.73 X14 0.97 X15 2.20 X4 3.17 X6
Q12 1 1.2619 0.2329 0.5412 1.00000 0.05 0.25 1.20 X8 1.73 X9 2.23 X3 2.64 X13
Q13 1 1.1196 0.2986 0.0946 1.00000 0.05 0.23 1.87 X1 2.77 X7 2.79 X12 2.80 X16
Q14 1 1.0965 0.4391 0.0070 1.00000 0.05 0.23 1.23 X1 1.90 X11 2.11 S1 2.74 X5
Q15 1 1.2158 0.2569 0.3892 1.00000 0.05 0.22 1.72 X9 1.93 X8 2.35 X16 2.52 X13
Q16 1 0.8663 0.2443 0.6056 1.00000 0.05 0.22 1.06 X12 1.88 X7 2.68 X3 2.73 X8
Q17 1 1.3228 0.2191 0.6530 1.00000 0.05 0.22 1.28 X8 2.17 X9 2.30 X3 3.00 S1
Q18 1 0.8947 0.2365 0.7942 1.00000 0.05 0.22 1.11 X12 2.21 X7 2.66 X2 2.72 X3
Q19 1 1.1435 0.2256 0.9696 1.00000 0.05 0.21 1.57 X3 2.27 X7 2.55 X4 2.56 X16
Q20 1 1.4171 0.3157 0.3340 1.00000 0.05 0.20 1.76 X6 1.80 X2 2.08 X12 2.47 X5
Shortest distances between peaks (including symmetry equivalents)
12 17 0.84 18 20 1.02 12 15 1.07 16 18 1.22 1 9 1.51 10 14 1.65 13 19 1.68
10 13 1.70 4 7 1.77 16 20 1.84 15 17 1.89 8 15 1.92 6 10 2.04 13 15 2.05
8 12 2.11 2 14 2.20 15 18 2.24 1 4 2.26 16 19 2.29 5 11 2.30 2 4 2.32
6 16 2.33 19 20 2.39 5 7 2.39 7 7 2.41 3 11 2.45 5 11 2.46 18 19 2.50
6 19 2.52 8 17 2.53 6 8 2.53 2 14 2.56 15 20 2.57 1 6 2.57 1 8 2.58
6 18 2.61 10 19 2.62 12 18 2.63 1 1 2.64 4 8 2.67 9 14 2.70 6 13 2.70
13 14 2.70 13 16 2.73 15 19 2.75 8 9 2.76 4 9 2.77 13 18 2.79 8 20 2.79
13 18 2.84 4 14 2.87 3 7 2.88 18 19 2.88 6 9 2.90 9 17 2.91 10 16 2.92
15 16 2.93 17 18 2.94 3 15 2.95 7 20 2.95 3 5 2.95 3 12 2.95 2 9 2.97
7 8 2.98 12 20 2.98 8 13 2.99 4 11 3.00 9 13 3.00
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
0.00: 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.
0.22: Read intensity data, sort/merge etc.
0.00: Set up constraints
0.05: OSF, H-atoms from difference map
0.05: Set up l.s. refinement
0.00: Generate idealized H-atoms
2.47: Structure factors and derivatives
1.09: Sum l.s. matrices
0.00: Generate and apply antibumping restraints
0.00: Apply other restraints
0.38: Solve l.s. equations
0.00: Generate HTAB table
0.22: Other dependent quantities, CIF, tables
0.77: Analysis of variance
0.17: Merge reflections for Fourier and .fcf
0.27: Fourier summations
0.11: Peaksearch
0.05: Analyse peaklist
+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
+ cim finished at 17:21:31 Total elapsed time: 6.3 secs +
+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++