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 10.015
PD2 1 10.0000 10.0000 10.0000 10.500000 10.015
CR1 2 0.3434 0.2496 0.8156 11.0000 10.015
CR2 2 0.6566 0.2504 0.6844 11.0000 10.015
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
[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 .0150
.0000 .0000 .0000 .0000 .0000
0PD2 .0000 .0000 .0000 .5000 .0150
.0000 .0000 .0000 .0000 .0000
0CR1 .3874 .2116 .8305 1.0000 .0150
.0085 .0059 .0051 .0000 .0000
0CR2 .6997 .2445 .7061 1.0000 .0150
.0086 .0063 .0053 .0000 .0000
RESIDUALS BEFORE CYCLE 5 FOR [Pd(NH3)4]Cr2O7 P21/c
R = .3555 RW = .3555 RG = .3613 RM = .3613
1 DIFFERENCE MAP 1 FOR [Pd(NH3)4]Cr2O7 P21/c
MAXIMUM = 230.41, MINIMUM = -186.12
MULTIPLIED BY 75.2228 (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 1 .69
3 CR1 .3874 .2116 -.1695 1.0000 1 1.37
4 CR2 .6997 .2445 .7061 1.0000 0 .00
5 Q 1 230. .2870 .0355 .0477 1.0000 1 .69
6 Q 2 222. .6653 .1337 .6208 1.0000 0 .00
7 Q 3 209. .3459 .0788 -.1812 1.0000 1 .00
8 Q 4 205. .0112 -.0002 .1347 1.0000 1 1.28
9 Q 5 205. -.0112 .0002 .8653 ** .000 FROM 8
10 Q 6 205. .0112 -.0002 .1347 ** .000 FROM 8
11 Q 7 205. .9888 .0002 .8653 ** .000 FROM 8
12 Q 8 194. .7071 .2432 .3395 1.0000 0 .00
13 Q 9 193. .3684 .2410 -.2673 1.0000 1 1.28
14 Q 10 191. .9673 .0889 .5827 1.0000 0 .00
15 Q 11 185. -.0044 .1691 .0115 1.0000 0 .00
16 Q 12 185. .9956 .1691 .0115 ** .000 FROM 15
17 Q 13 181. .2851 .0404 .5390 1.0000 0 .00
18 Q 14 175. .9562 .2314 .4571 1.0000 0 .00
BONDS (INCLUDING SYMMETRY RELATED ATOMS)
2- 5 2.19 2- 5 2.19 4- 6 1.61 3- 7 1.57 5- 7 2.91 2- 8 1.58 5- 8 2.65
2- 8 1.58 5- 8 2.75 3- 13 1.18 7- 13 2.17 1- 14 1.49 1- 14 1.49 15- 18 1.32
5
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 89 81 3 -1 5 1 13 -46 3 2 4 2 105 119 3 -3 1 4 32 11 5 -7 2 6 22 95 8
2 0 0 80 110 3 1 5 1 39 3 4 5 4 2 69 103 10 0 1 4 23 1 3 -3 2 6 60 59 4
3 0 0 455 235 5 2 5 1 57 -35 2 2 5 2 71 43 3 2 1 4 58 -94 6 0 3 6 43 50 5
1 1 0 31 28 3 1 6 1 83 -62 2 3 5 2 87 20 4 -5 2 4 126 155 6 1 5 6 53 6 4
2 1 0 64 29 2 2 7 1 77 28 6 -1 6 2 124 134 5 -3 2 4 91 110 4 4 5 6 26 -5 8
3 1 0 58 -96 4 3 9 1 3 33 2 0 6 2 195 172 5 -2 2 4 162 258 4 -2 1 7 87 10 5
0 2 0 26 9 5 -5 0 2 161 143 6 1 6 2 51 70 3 -1 2 4 96 38 3 -2 2 7 87 -5 4
1 2 0 272 251 2 -3 0 2 69 47 2 -1 7 2 46 -54 7 0 2 4 106 140 3 -1 2 7 46 -14 7
2 2 0 211 206 3 -2 0 2 343 300 3 -7 1 3 29 2 8 1 2 4 89 216 3 -1 3 7 32 29 2
3 3 0 54 76 4 -1 0 2 145 139 3 -2 1 3 37 -4 4 -1 3 4 40 27 1 -6 4 7 18 -3 4
0 4 0 333 266 4 0 0 2 20 53 4 -1 1 3 45 13 1 1 3 4 65 -55 4 -3 5 7 66 -19 10
1 4 0 109 94 3 1 0 2 307 305 2 0 1 3 39 -17 1 3 3 4 56 -19 3 -1 6 7 12 -26 10
1 5 0 12 46 4 3 0 2 126 96 6 1 1 3 5 14 0 -3 4 4 112 126 6 -3 0 8 42 11 8
-2 1 1 23 17 2 -3 1 2 174 -64 2 -3 2 3 16 -27 7 -1 4 4 171 206 4 0 0 8 82 45 8
-1 1 1 6 -17 6 0 1 2 20 26 1 -2 2 3 66 38 4 0 4 4 161 141 4 2 0 8 104 91 19
0 1 1 0 10 0 1 1 2 89 -75 2 -3 3 3 34 13 2 2 4 4 122 147 6 -2 3 8 74 20 5
1 1 1 11 2 3 2 1 2 27 39 2 -2 3 3 13 11 2 3 8 4 30 119 8 1 3 8 59 39 9
-3 2 1 39 30 2 3 1 2 58 58 2 0 3 3 40 42 2 0 1 5 18 7 4 0 7 8 60 -23 17
-2 2 1 27 -17 3 -3 2 2 202 223 4 -1 4 3 31 38 3 -2 2 5 50 -23 3 -5 1 9 10 -7 10
-1 2 1 17 -14 1 -2 2 2 2 29 1 0 4 3 42 9 3 1 2 5 56 3 4 -1 1 9 37 8 8
0 2 1 44 41 2 -1 2 2 176 193 2 1 4 3 36 -44 7 2 2 5 55 12 4 -2 3 9 10 4 3
1 2 1 88 -40 1 0 2 2 321 273 2 -2 5 3 47 -13 2 -2 3 5 38 24 2 -2 4 9 27 -31 6
2 2 1 57 18 2 -1 3 2 9 -17 1 -2 6 3 73 61 6 -2 4 5 55 37 6 0 1 10 68 -46 10
-2 3 1 19 -42 1 1 3 2 68 63 3 -2 9 3 29 -9 7 0 6 5 51 -37 4 -1 2 10 83 78 9
-1 3 1 10 40 3 -5 4 2 135 131 6 -1 0 4 318 272 4 -5 8 5 62 30 22 -3 4 10 78 121 16
0 3 1 36 -23 1 -2 4 2 130 229 4 1 0 4 71 57 5 -7 0 6 88 54 19 0 4 10 60 99 14
2 3 1 32 31 1 -1 4 2 154 122 3 2 0 4 187 189 5 0 1 6 68 -52 3 -3 5 10 5 -2 2
-2 5 1 38 50 4 0 4 2 46 64 3
1
1 [Pd(NH3)4]Cr2O7 P21/c
DEVIATIONS GREATER THAN 2 SIGMA
H K L FO FC D/SIGMA
3 0 0 454.93 236.45 5.41
-3 1 2 174.50 64.55 2.72
-2 4 2 129.89 230.76 2.50
-2 2 4 161.79 259.45 2.42
1 2 4 88.71 217.28 3.18
3 8 4 30.49 120.75 2.23
-2 2 7 86.75 4.90 2.03
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 4320 5574 2776 3716 3223 2691 2697 2648 3935
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 2080 2392 3038 7445 4936 2458 2877 4046 2858 4095
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 1986 2607 2684 2242 3221 2871 3306 5511 4496 7231
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 2727 3184 3843 6098 2087 2434 1519 4920 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 5887 3323 4530 2024 3583 3585 1623 3536 6761 2594 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 6703 2451 3653 2190 4933 2967 3685 4804 3413 1497 2875 0 0 0 0