1
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
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
SFAC O N H
UNIT 4 8 28 16 48
V = 1026.99 F(000) = 759.95 MU = 10.04
MERG 2
L.S. 4
FVAR 1.
PD1 1 10.0000 10.0000 10.5000 10.500000 0.015
PD2 1 10.0000 10.0000 10.0000 10.500000 0.015
BOND 1
FMAP 2
PLAN 10
GRID -4 -1 -2 4 1 2
LIST 1 1
HKLF 3
137 REFLEXIONS READ, OF WHICH 0 REJECTED
END
1SORT-MERGE FOR [Pd(NH3)4]Cr2O7 P21/c
INCONSISTENCIES
H K L ESD/F SIGMA/F N
137 UNIQUE REFLEXIONS, R = .0000
OVERALL SCALE 1.50290 ESTIMATED U = .076
SIN(THETA)/LAMBDA .00 .07 .14 .21 .28 .35 .42 .49 .56 .63 .70 .77 .84 .91 .98
R.M.S.(E) .210 .923 .995 .997 .999 1.011 1.051 1.000 .000 .000 .000 .000 .000 .000 .000
MEAN ABS(E*E-1) .922 1.153 1.305 1.108 .793 .733 .860 .962 .000 .000 .000 .000 .000 .000 .000
EFFECTIVE N .2 9.6 25.3 37.3 27.2 15.2 13.1 9.1 .0 .0 .0 .0 .0 .0 .0
RESIDUALS BEFORE CYCLE 1 FOR [Pd(NH3)4]Cr2O7 P21/c
R = .6588 RW = .6588 RG = .6338 RM = .6196
[Pd(NH3)4]Cr2O7 P21/c
ATOM X/A Y/B Z/C K U11 U22 U33 U23 U13 U12
0PD1 .0000 .0000 .5000 .5000 .0835
.0000 .0000 .0000 .0000 .0413
0PD2 .0000 .0000 .0000 .5000 .0001
.0000 .0000 .0000 .0000 .0191
RESIDUALS BEFORE CYCLE 5 FOR [Pd(NH3)4]Cr2O7 P21/c
R = .6180 RW = .6180 RG = .6058 RM = .6058
RESIDUALS BEFORE CYCLE 5 FOR [Pd(NH3)4]Cr2O7 P21/c
1 DIFFERENCE MAP 1 FOR [Pd(NH3)4]Cr2O7 P21/c
MAXIMUM = 510.79, MINIMUM = -199.43
MULTIPLIED BY 101.0084 (SCAN 2)
ATOM HEIGHT X/A Y/B Z/C S.O.F. MOLECULE ELEVATION
1 PD1 .0000 .0000 .5000 .5000 0 .00
2 PD2 .0000 .0000 .0000 .5000 0 .00
3 Q 1 511. 1.3434 .2496 .8156 1.0000 1 1.40
4 Q 2 511. .3434 .2496 .8156 ** .000 FROM 3
5 Q 3 511. .6566 .2504 .6844 1.0000 1 .00
6 Q 4 511. .6566 .2496 .1844 ** .000 FROM 5
7 Q 5 204. .2907 .0000 .5571 1.0000 0 .00
8 Q 6 204. .7093 .0000 .4429 ** .000 FROM 7
9 Q 7 198. .9192 .2418 .7568 1.0000 1 .76
10 Q 8 198. 1.0808 .2582 .7432 1.0000 1 .65
11 Q 9 174. 1.3252 .0716 .8025 1.0000 1 .70
12 Q 10 174. .6748 .4284 .6975 1.0000 1 .70
13 Q 11 155. .4925 .2513 .7469 1.0000 1 .70
BONDS (INCLUDING SYMMETRY RELATED ATOMS)
1- 7 2.18 1- 7 2.18 5- 9 1.99 3- 10 1.99 9- 10 1.32 3- 11 2.07 11- 12 1.66
5- 12 2.07 3- 13 1.58 5- 13 1.64
1 OBSERVED AND CALCULATED STRUCTURE FACTORS FOR [Pd(NH3)4]Cr2O7 P21/c PAGE 1
H K L FO FC S H K L FO FC S H K L FO FC S H K L FO FC S H K L FO FC S
1 0 0 79 177 2 -1 5 1 11 21 3 2 4 2 93 115 3 -3 1 4 29 0 4 -7 2 6 20 59 8
2 0 0 71 157 3 1 5 1 35 21 4 5 4 2 61 72 9 0 1 4 20 0 3 -3 2 6 53 99 4
3 0 0 404 132 4 2 5 1 51 25 2 2 5 2 63 0 3 2 1 4 52 0 5 0 3 6 38 0 5
1 1 0 27 0 3 1 6 1 74 0 2 3 5 2 77 0 3 -5 2 4 112 86 6 1 5 6 47 0 4
2 1 0 57 0 2 2 7 1 69 31 5 -1 6 2 110 106 4 -3 2 4 81 116 4 4 5 6 23 0 7
3 1 0 51 0 4 3 9 1 2 37 2 0 6 2 173 106 4 -2 2 4 144 129 3 -2 1 7 77 29 4
0 2 0 23 172 4 -5 0 2 143 92 5 1 6 2 45 102 3 -1 2 4 85 136 3 -2 2 7 77 0 3
1 2 0 241 165 2 -3 0 2 61 134 2 -1 7 2 41 0 6 0 2 4 94 134 2 -1 2 7 41 0 6
2 2 0 187 147 3 -2 0 2 305 155 3 -7 1 3 25 37 7 1 2 4 79 125 3 -1 3 7 28 30 2
3 3 0 48 0 3 -1 0 2 129 169 2 -2 1 3 33 13 3 -1 3 4 35 0 1 -6 4 7 16 0 4
0 4 0 296 142 4 0 0 2 18 171 4 -1 1 3 40 10 1 1 3 4 58 0 4 -3 5 7 58 34 8
1 4 0 97 138 3 1 0 2 272 160 2 0 1 3 34 10 0 3 3 4 50 0 3 -1 6 7 11 0 9
1 5 0 11 0 4 3 0 2 112 118 5 1 1 3 4 13 0 -3 4 4 99 102 5 -3 0 8 38 83 7
-2 1 1 20 9 1 -3 1 2 155 0 2 -3 2 3 14 0 6 -1 4 4 151 117 4 0 0 8 73 84 7
-1 1 1 5 4 5 0 1 2 17 0 1 -2 2 3 59 0 3 0 4 4 143 116 4 2 0 8 92 72 16
0 1 1 0 2 0 1 1 2 79 0 2 -3 3 3 30 23 2 2 4 4 108 98 5 -2 3 8 65 0 5
1 1 1 10 5 2 2 1 2 24 0 2 -2 3 3 12 18 2 3 8 4 27 63 7 1 3 8 52 0 8
-3 2 1 35 0 2 3 1 2 52 0 1 0 3 3 36 15 1 0 1 5 16 20 3 0 7 8 53 0 15
-2 2 1 24 0 3 -3 2 2 179 127 3 -1 4 3 27 0 2 -2 2 5 44 0 3 -5 1 9 9 37 9
-1 2 1 15 0 1 -2 2 2 2 146 1 0 4 3 37 0 3 1 2 5 50 0 3 -1 1 9 33 34 7
0 2 1 39 0 2 -1 2 2 156 158 2 1 4 3 32 0 6 2 2 5 48 0 4 -2 3 9 9 35 2
1 2 1 78 0 1 0 2 2 285 160 2 -2 5 3 42 25 2 -2 3 5 33 24 2 -2 4 9 24 0 6
2 2 1 50 0 2 -1 3 2 8 0 1 -2 6 3 65 0 6 -2 4 5 49 0 6 0 1 10 60 0 9
-2 3 1 16 15 1 1 3 2 60 0 3 -2 9 3 26 36 7 0 6 5 45 0 4 -1 2 10 73 67 8
-1 3 1 9 11 3 -5 4 2 120 81 6 -1 0 4 283 143 4 -5 8 5 55 0 20 -3 4 10 69 62 14
0 3 1 32 10 1 -2 4 2 115 124 3 1 0 4 63 131 4 -7 0 6 78 60 17 0 4 10 53 61 13
2 3 1 28 17 1 -1 4 2 137 133 3 2 0 4 166 115 4 0 1 6 60 0 3 -3 5 10 5 0 2
-2 5 1 34 23 3 0 4 2 41 135 3
1
1 [Pd(NH3)4]Cr2O7 P21/c
DEVIATIONS GREATER THAN 2 SIGMA
H K L FO FC D/SIGMA
3 0 0 403.90 132.88 4.58
0 2 0 22.92 172.26 2.52
0 4 0 296.09 143.08 2.58
-2 0 2 304.71 155.47 2.52
0 0 2 18.00 171.94 2.60
-3 1 2 154.92 .00 2.62
-2 2 2 2.20 146.53 2.44
0 2 2 285.16 160.93 2.10
-1 0 4 282.77 144.14 2.34
1ANALYSIS OF VARIANCE FOR [Pd(NH3)4]Cr2O7 P21/c
GGG UGG GUG UUG GGU UGU GUU UUU ALL
N 20 31 12 18 13 11 18 14 137
V 8845 7181 4787 5914 4739 4490 2092 1717 5858
SIN THETA 0.00 - .20 - .25 - .29 - .33 - .37 - .41 - .47 - .55 - .67 - .76
N 16 12 13 14 14 14 15 12 13 14
V 7899 6024 7683 9495 2904 3803 4898 4705 3207 3360
SQRT(F/FMAX) 0.00 - .17 - .24 - .29 - .32 - .36 - .39 - .43 - .49 - .60 - 1.00
N 14 13 18 13 16 13 10 14 12 14
V 4150 6184 2095 4233 4732 5203 5616 5788 2503 12192
ABS(H) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 REST
N 24 42 37 23 1 6 1 3 0 0 0 0 0 0 0
V 7050 5015 5224 7597 2282 3804 1596 2605 0 0 0 0 0 0 0
ABS(K) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 REST
N 17 26 29 19 20 12 7 3 2 2 0 0 0 0 0
V 10516 4687 6190 3515 4729 3493 5271 4422 4673 2596 0 0 0 0 0
ABS(L) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 REST
N 13 21 30 16 20 8 7 7 6 4 5 0 0 0 0
V 10894 3234 7637 2961 4963 4241 4118 3943 4575 2291 2747 0 0 0 0