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+ +
+ SHELXS-86 - CRYSTAL STRUCTURE SOLUTION - MSDOS VERSION +
+ +
+ PDCR8 STARTED AT 18: 0 ON 17-FEB-1997 +
+ +
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TITL [Pd(NH3)4]Cr2O7 P21/c
CELL 1.5418 7.7692 11.5738 11.8505 90.0 105.468 90.0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC PD 19.3319 0.698655 15.5017 7.98929 5.29537 25.2052 =
0.605844 76.8986 5.26593 0.1215 3.9337 0. 0.7 106.4
SFAC CR 10.6406 6.1038 7.3537 0.392 3.324 20.2626 1.4922 =
98.7399 1.1832 -0.1635 2.4439 0. 0.3 51.996
SFAC O N H
UNIT 4 8 28 16 48
V = 1026.99 AT VOL = 18.3 F(000) = 760.0 MU = 1.06 MM-1
MAX SINGLE PATTERSON VECTOR = 134.7 CELL WT = 1562.04 RHO = 2.526
PATT
HKLF 3
** WARNING - IT WOULD BE BETTER TO INPUT F-SQUARED THAN F SO
** THAT ZERO AND NEGATIVE INTENSITIES ARE TREATED CORRECTLY
137 REFLECTIONS READ, OF WHICH 0 REJECTED
MAXIMUM H, K, L AND 2-THETA = 7. 9. 10. 98.07
137 UNIQUE REFLECTIONS, OF WHICH 119 OBSERVED
R(INT) = 0.0000 R(SIGMA) = 0.0594 FRIEDEL OPPOSITES MERGED
NUMBER OF UNIQUE DATA AS A FUNCTION OF RESOLUTION IN ANGSTROMS
RESOLUTION INF 5.00 3.50 2.50 2.00 1.70 1.50 1.40 1.30 1.20 1.10 1.00
N(OBSERVED) 8. 14. 21. 29. 15. 12. 5. 4. 4. 3. 4.
N(MEASURED) 10. 14. 23. 31. 15. 12. 5. 4. 6. 7. 10.
N(THEORY) 10. 15. 45. 61. 88. 98. 74. 91. 140. 185. 266.
TWO-THETA 0.0 17.7 25.4 35.9 45.3 53.9 61.9 66.8 72.7 79.9 89.0 100.9
OBSERVED E .GT. 1.000 1.100 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900
NUMBER 49 35 28 23 19 15 10 8 8 6
CENTRIC ACENTRIC 0KL H0L HK0 REST
MEAN ABS(E*E-1) 0.968 0.736 0.521 0.498 0.911 0.645
HIGHEST MEMORY FOR DATA REDUCTION = 350 + 715 + 685
0.0 MINUTES CPU TIME
SUMMARY OF PARAMETERS FOR [Pd(NH3)4]Cr2O7 P21/c
ESEL EMIN 1.000 EMAX 5.000 DELU 0.005 RENORM 0.700 AXIS 0
OMIT S 4.00 2THETA(MAX) 180.0
PATT M -2 THRESH 25.0 RMIN 1.60 MAXVECS 288
FMAP CODE 6
PLAN NPEAKS 200 DEL1 0.500 DEL2 1.500
TIME T 999999.
FMAP AND GRID SET BY PROGRAM
FMAP 6 -1 13
GRID -5.000 -2 -1 5.000 2 1
SUPER-SHARP PATTERSON FOR [Pd(NH3)4]Cr2O7 P21/c
MAXIMUM = 999.10, MINIMUM = -208.73 HIGHEST MEMORY USED = 10156 + 1569 + 1569
0.0 MINUTES CPU TIME
X Y Z WEIGHT PEAK VECTOR
1 0.0000 0.0000 0.0000 4. 999. 0.00
2 0.0000 0.0000 0.5000 4. 376. 5.93
3 0.3169 0.2538 0.2924 1. 339. 4.71
4 0.0000 0.5000 0.5000 4. 310. 8.28
5 0.0434 0.5000 0.0501 2. 280. 5.82
6 0.3434 0.2527 0.7854 1. 259. 5.08
7 0.3321 0.0000 0.5217 2. 227. 6.83
8 0.0617 0.2676 0.2391 1. 203. 4.14
9 0.2093 0.5000 0.0384 2. 199. 6.00
10 0.4215 0.5000 0.5388 2. 197. 9.15
11 0.3903 0.0000 0.9998 2. 188. 3.03
12 0.0000 0.2806 0.5000 2. 178. 6.76
13 0.3883 0.0000 0.5944 2. 177. 6.32
14 0.3415 0.1286 0.3796 1. 170. 4.81
15 0.3069 0.2980 0.2029 1. 168. 4.51
16 0.2970 0.0840 0.3580 1. 167. 4.36
17 0.1075 0.0000 0.7396 2. 161. 3.41
18 0.3216 0.0558 0.8129 1. 160. 3.81
19 0.2965 0.0882 0.9184 1. 159. 2.91
20 0.0297 0.5000 0.2272 2. 158. 6.36
21 0.1391 0.5000 0.9691 2. 145. 5.92
22 0.3058 0.5000 0.8888 2. 143. 6.52
23 0.3422 0.5000 0.7752 2. 138. 7.17
24 0.2300 0.0000 0.8094 2. 136. 3.23
25 0.0290 0.3974 0.8635 1. 135. 4.90
26 0.3433 0.4323 0.2663 1. 133. 6.13
27 0.3404 0.2044 0.5833 1. 124. 6.63
28 0.3572 0.4025 0.4370 1. 121. 6.97
29 0.0373 0.4330 0.7494 1. 118. 5.87
30 0.3152 0.0000 0.1006 2. 118. 2.42
31 0.3503 0.0629 0.0780 1. 118. 2.73
32 0.3612 0.4399 0.8731 1. 116. 6.19
33 0.3425 0.0000 0.3946 2. 113. 4.72
34 0.0945 0.0655 0.1937 1. 107. 2.34
35 0.2966 0.4230 0.1417 1. 107. 5.48
36 0.3489 0.3601 0.9331 1. 106. 5.15
37 0.3502 0.3775 0.7447 1. 106. 6.33
38 0.3436 0.0256 0.0981 1. 102. 2.63
39 0.3982 0.0816 0.6833 1. 102. 5.54
40 0.0138 0.3319 0.3590 1. 101. 5.71
41 0.3929 0.2819 0.1042 1. 101. 4.41
42 0.3137 0.1328 0.5027 1. 99. 7.12
43 0.4004 0.1364 0.2645 1. 97. 4.10
44 0.0469 0.1236 0.0887 1. 90. 1.76
45 0.9916 0.0676 0.2977 1. 90. 3.63
46 0.2624 0.3079 0.5818 1. 88. 6.84
47 0.2482 0.0000 0.6144 2. 85. 5.41
48 0.4055 0.5000 0.0309 2. 84. 6.55
49 0.3079 0.4574 0.6362 1. 83. 7.60
50 0.9899 0.1721 0.0639 1. 82. 2.14
51 0.3399 0.5000 0.3383 2. 79. 7.13
52 0.3088 0.3554 0.5634 1. 79. 7.49
53 0.3392 0.1918 0.0247 1. 79. 3.40
54 0.0640 0.3202 0.9557 1. 76. 3.79
55 0.4130 0.5000 0.4203 2. 76. 7.75
56 0.0540 0.2657 0.6588 1. 75. 5.19
57 0.3874 0.2409 0.0236 1. 66. 4.06
58 0.2599 0.4442 0.7453 1. 65. 6.55
59 0.3627 0.1393 0.1340 1. 63. 3.27
60 0.3958 0.5000 0.6360 2. 61. 8.28
61 0.3498 0.3208 0.6349 1. 60. 6.79
62 0.0585 0.3762 0.4575 1. 59. 6.87
63 0.0469 0.1055 0.6771 1. 59. 4.12
64 0.2995 0.0000 0.6901 2. 51. 4.84
65 0.0917 0.3840 0.9396 1. 43. 4.59
66 0.1821 0.3003 0.8645 1. 39. 4.23
67 0.3967 0.1865 0.5022 1. 39. 7.66
68 0.4824 0.0000 0.2684 2. 38. 4.22
69 0.0500 0.4260 0.3564 1. 35. 6.44
70 0.1603 0.0000 0.3403 2. 25. 3.89
LOCATION OF HEAVY ATOMS FROM PATTERSON
696 E-VALUES GREATER THAN 1.000 SELECTED FOR RE
TRIAL ATOMS FOR OPTIMISED RE = 0.345 R(PAT) = 0.337
AT.NO. X Y Z S.O.F. SELFMF SUPMF MINIMUM DISTANCES (SELF FIRST)
46.* 0.000 0.000 0.000 0.5000 309.9 999.0 7.77
24.* 0.000 0.000 0.500 0.5000 309.9 43.0 7.77 5.79
TRIAL ATOMS FOR OPTIMISED RE = 0.385 R(PAT) = 0.461
AT.NO. X Y Z S.O.F. SELFMF SUPMF MINIMUM DISTANCES (SELF FIRST)
46.* 0.000 0.000 0.250 1.0000 43.0 999.0 5.79
24.* 0.683 0.746 0.958 1.0000 26.1 130.8 5.93 4.65
TRIAL ATOMS FOR OPTIMISED RE = 0.284 R(PAT) = 0.375
AT.NO. X Y Z S.O.F. SELFMF SUPMF MINIMUM DISTANCES (SELF FIRST)
46.* 0.171 0.000 0.197 1.0000 66.0 999.0 4.72
24.* 0.488 0.254 0.490 1.0000 96.1 93.0 5.71 4.71
TRIAL ATOMS FOR OPTIMISED RE = 0.420 R(PAT) = 0.419
AT.NO. X Y Z S.O.F. SELFMF SUPMF MINIMUM DISTANCES (SELF FIRST)
46.* 0.203 0.250 0.015 1.0000 84.0 999.0 5.93
24.* 0.203 0.750 0.515 1.0000 84.0 40.1 5.93 3.07
POSSIBLE HEAVY ATOM POSITIONS FOR [Pd(NH3)4]Cr2O7 P21/c
X Y Z 1/MULT R(PAT) RE(HA) SELFMF
0.000 0.000 0.000 0.5000 0.337 0.345 309.9
0.171 0.000 0.197 1.0000 0.375 0.284 66.0
0.203 0.250 0.015 1.0000 0.419 0.420 84.0
0.000 0.000 0.250 1.0000 0.461 0.385 43.0
0.194 0.120 0.012 1.0000 0.553 0.402 66.1
0.211 0.250 0.269 1.0000 0.632 0.319 65.8
0.022 0.250 0.025 1.0000 0.665 0.284 47.6
0.158 0.127 0.146 1.0000 0.628 0.383 51.9
0.153 0.250 0.444 1.0000 0.731 0.191 9.0
0.195 0.000 0.500 1.0000 0.655 0.355 46.4
0.161 0.028 0.406 1.0000 0.730 0.312 33.7
0.000 0.250 0.250 1.0000 0.751 0.317 43.0
0.198 0.093 0.251 1.0000 0.756 0.351 31.5
0.170 0.250 0.169 1.0000 0.806 0.272 16.1
0.181 0.220 0.437 1.0000 0.797 0.338 22.9
** IT WILL NOW BE ASSUMED THAT THE FIRST ATOM IN THE ABOVE LIST IS A CORRECT
HEAVY ATOM. IF THIS IS NOT TRUE, THE REST OF THE OUTPUT WILL BE WORTHLESS.
IN SUCH A CASE, RERUN THE JOB WITH A DIFFERENT ATOM FROM THE ABOVE LIST
INSERTED BETWEEN THE PATT AND HKLF INSTRUCTIONS
0.1 MINUTES CPU TIME
TENTATIVE HEAVY ATOM ASSIGNMENT FOR [Pd(NH3)4]Cr2O7 P21/c
NAME SFAC X Y Z S.O.F. SELFMF SUPMF
PD1 1 0.000 0.000 0.000 0.5000 309.9 999.0
CR1 2 0.000 0.000 0.500 0.5000 309.9 43.0
ATOM PEAK X Y Z SOF HEIGHT DISTANCES AND ANGLES
PD1 0. 0.0000 0.0000 0.0000 0.500 1.29 0 17 1.526
3 17 1.526 180.0
CR1 0. 0.0000 0.0000 -0.5000 0.500 1.67 0 3 0.688
0 6 1.178 105.5
1 3 0.688 180.0 74.5
2 6 1.178 74.5 180.0 105.5
1 269. 0.3059 -0.2183 -0.1891 1.000 1.05 0 2 1.864
0 10 1.267 104.2
0 12 1.721 162.2 92.1
2 259. 0.3354 -0.3687 -0.1309 1.000 1.82 0 1 1.864
0 19 1.884 132.5
3 256. 0.0145 -0.0263 -0.4462 1.000 1.72 0 CR1 0.688
0 6 1.514 48.6
0 18 1.894 116.1 75.5
1 3 1.376 0.0 48.6 116.1
2 6 1.195 71.8 120.3 145.4 71.8
5 200. 0.1034 0.0131 -0.2453 1.000 0.77 0 7 1.881
0 12 1.882 96.9
0 17 1.708 53.9 101.1
6 179. 0.1418 0.0075 -0.5176 1.000 0.79 0 CR1 1.178
0 3 1.514 26.0
1 3 1.195 33.7 59.7
7 178. -0.0454 -0.1036 -0.2134 1.000 2.41 0 5 1.881
0 13 1.292 74.2
0 17 1.635 57.6 119.1
10 169. 0.2771 -0.2306 -0.2988 1.000 1.39 0 1 1.267
0 18 1.678 132.6
12 164. 0.3187 -0.0704 -0.1996 1.000 0.00 0 1 1.721
0 5 1.882 117.9
13 155. -0.1056 -0.0812 -0.3237 1.000 2.71 0 7 1.292
17 142. 0.0296 0.0023 -0.1222 1.000 1.19 0 PD1 1.526
0 5 1.708 168.9
0 7 1.635 119.8 68.4
18 140. 0.1934 -0.1419 -0.4121 1.000 1.39 0 3 1.894
0 10 1.678 135.1
19 139. 0.4154 -0.4285 0.0220 1.000 1.63 0 2 1.884
ATOM CODE X Y Z HEIGHT SYMMETRY TRANSFORMATION
3 1 -0.0145 0.0263 -0.5538 1.63 0.0000-X 0.0000-Y -1.0000-Z
6 2 -0.1418 -0.0075 -0.4824 2.56 0.0000-X 0.0000-Y -1.0000-Z
17 3 -0.0296 -0.0023 0.1222 1.39 0.0000-X 0.0000-Y 0.0000-Z
MOLECULE 2 SCALE 1.000 INCHES = 2.540 CM PER ANGSTROM
ATOM PEAK X Y Z SOF HEIGHT DISTANCES AND ANGLES
4 205. 0.4053 0.2247 0.3159 1.000 0.00 0 9 1.839
8 178. 0.2897 0.4340 0.4313 1.000 1.62 0 9 1.853
0 15 1.683 106.1
9 175. 0.4332 0.3813 0.3398 1.000 0.50 0 4 1.839
0 8 1.853 110.5
0 16 1.703 95.9 126.9
15 144. 0.4271 0.5004 0.5470 1.000 0.90 0 8 1.683
1 15 1.788 81.9
16 143. 0.4156 0.4157 0.1974 1.000 0.90 0 9 1.703
ATOM CODE X Y Z HEIGHT SYMMETRY TRANSFORMATION
15 1 0.5729 0.4996 0.4530 0.00 1.0000-X 1.0000-Y 1.0000-Z
MOLECULE 3
ATOM PEAK X Y Z SOF HEIGHT DISTANCES AND ANGLES
11 166. 0.0782 0.2264 0.7570 1.000
MOLECULE 4
ATOM PEAK X Y Z SOF HEIGHT DISTANCES AND ANGLES
14 153. 0.3227 0.1720 0.1212 1.000
0.0 MINUTES CPU TIME
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+ FINISHED AT 18: 0 ON 17-FEB-1997 +
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