Data as prepared for the SHELX76 refinement with partial data : 242 hkl
TITL Na2C2O4 P21/a partial data delta 2-theta = 0.04
CELL 1.5418 10.4222 5.2573 3.4832 90.0 93.099 90.0
LATT 1
SYMM 0.5-X,0.5+Y,-Z
SFAC NA 4.7626 3.285 3.1736 8.8422 1.2674 0.3136 1.1128 =
129.424 0.676 0.1353 0.1239 0 1.2
SFAC C O
UNIT 4 4 8
MERG 2
L.S. 4
FVAR 1.
NA 1 0.3571 0.0546 0.8101 11.000000 0.05
C 2 0.0760 0.0565 0.6242 11.000000 0.05
O1 3 0.1487 -0.1356 0.6612 11.000000 0.05
O2 3 0.4316 -0.2415 1.2448 11.000000 0.05
BOND 1
FMAP 2
PLAN 10
GRID -2 -2 -2 2 2 2
LIST 1 1
HKLF 3
END
Results
242 REFLEXIONS READ, OF WHICH 0 REJECTED
END
SORT-MERGE FOR Na2C2O4 P21/a partial data delta 2-t
INCONSISTENCIES
H K L ESD/F SIGMA/F N
242 UNIQUE REFLEXIONS, R = .0000
OVERALL SCALE .22593 ESTIMATED U = .077
SIN(THETA)/LAMBDA .00 .07 .14 .21 .28 .35 .42 .49 .56 .63 .70 .77 .84 .91 .98
R.M.S.(E) .000 .216 .785 .930 .971 .954 1.027 1.000 1.000 1.000 .000 .000 .000 .000 .000
MEAN ABS(E*E-1) .000 .945 .829 .835 .794 .693 .783 .744 .750 .632 .000 .000 .000 .000 .000
EFFECTIVE N .0 1.2 6.9 15.6 22.1 30.9 43.5 54.0 59.7 8.0 .0 .0 .0 .0 .0
RESIDUALS BEFORE CYCLE 1 FOR Na2C2O4 P21/a partial data delta 2-t
R = .5042 RW = .5042 RG = .4821 RM = .3456
RESIDUALS BEFORE CYCLE 2 FOR Na2C2O4 P21/a partial data delta 2-t
R = .3319 RW = .3319 RG = .3557 RM = .3182
RESIDUALS BEFORE CYCLE 3 FOR Na2C2O4 P21/a partial data delta 2-t
R = .2445 RW = .2445 RG = .2868 RM = .2864
RESIDUALS BEFORE CYCLE 4 FOR Na2C2O4 P21/a partial data delta 2-t
R = .2444 RW = .2444 RG = .2838 RM = .2838
RESIDUALS BEFORE CYCLE 4 FOR Na2C2O4 P21/a partial data delta 2-t
UNIT WEIGHTS
CYCLE 4
ESD SHIFT/ESD
1 OVERALL SCALE 1.29188 .04299 -.016
2 NA X/A .35391 .00101 .049
3 NA Y/B .05500 .00221 -.340
4 NA Z/C .80301 .00316 -.007
5 NA U11 .02715 .00340 .100
6 C X/A .06602 .00264 .121
7 C Y/B .04125 .00580 .214
8 C Z/C .64319 .00819 .093
9 C U11 .02739 .00704 -.004
10 O1 X/A .15013 .00152 -.002
11 O1 Y/B -.12715 .00344 .057
12 O1 Z/C .65019 .00478 .024
13 O1 U11 .01571 .00457 -.189
14 O2 X/A .42982 .00180 -.021
15 O2 Y/B -.23030 .00388 -.004
16 O2 Z/C 1.25765 .00529 .029
17 O2 U11 .02444 .00504 -.023
CORRELATION MATRIX ELEMENTS GREATER THAN 0.5
1. 5. .5382
Na2C2O4 P21/a partial data delta 2-t
ATOM X/A Y/B Z/C K U11 U22 U33 U23 U13 U12
0NA .3539 .0550 .8030 1.0000 .0271
.0010 .0022 .0032 .0000 .0034
0C .0660 .0412 .6432 1.0000 .0274
.0026 .0058 .0082 .0000 .0070
0O1 .1501 -.1272 .6502 1.0000 .0157
.0015 .0034 .0048 .0000 .0046
0O2 .4298 -.2303 1.2576 1.0000 .0244
.0018 .0039 .0053 .0000 .0050
RESIDUALS BEFORE CYCLE 5 FOR Na2C2O4 P21/a partial data delta 2-t
R = .2459 RW = .2459 RG = .2835 RM = .2835
RESIDUALS BEFORE CYCLE 5 FOR Na2C2O4 P21/a partial data delta 2-t
UNIT WEIGHTS
Na2C2O4 P21/a partial data delta 2-t
NA X/A = .3539 Y/B = .0550 Z/C = .8030
O1 ---NA 2.364 ( .019 ) 1, .0000, .0000, .0000
O2 ---NA 2.291 ( .022 ) 1, .0000, .0000, .0000
O2 -NA -O1 99.4 ( .8 )
NA X/A = .6461 Y/B = .9450 Z/C = .1970
NA ---NA 3.323 ( .021 ) -1, 1.0000, .0000, 2.0000
O2 ...NA 2.455 -1, 1.0000, .0000, 2.0000
NA X/A = .1461 Y/B = .5550 Z/C = .1970
O1 ...NA 2.298 2, .0000, -1.0000, 1.0000
NA X/A = .8539 Y/B = .4450 Z/C = .8030
C X/A = .0660 Y/B = .0412 Z/C = .6432
O1 ---C 1.245 ( .034 ) 1, .0000, .0000, .0000
C X/A = .9340 Y/B = .9588 Z/C = .3568
C ---C 1.711 ( .054 ) -1, .0000, .0000, 1.0000
C X/A = .4340 Y/B = .5412 Z/C = .3568
O2 ...C 1.250 2, .0000, -1.0000, 2.0000
C X/A = .5660 Y/B = .4588 Z/C = .6432
O1 X/A = .1501 Y/B = .8728 Z/C = .6502
NA ---O1 2.364 ( .019 ) 1, .0000, .0000, .0000
C ---O1 1.245 ( .034 ) 1, .0000, .0000, .0000
C -O1 -NA 109.8 ( 1.7 )
O1 X/A = .8499 Y/B = .1272 Z/C = .3498
O1 X/A = .3499 Y/B = .3728 Z/C = .3498
NA ...O1 2.298 2, .0000, .0000, 1.0000
O2 ...O1 2.276 2, .0000, -1.0000, 2.0000
O1 X/A = .6501 Y/B = .6272 Z/C = .6502
O2 X/A = .4298 Y/B = .7697 Z/C = .2576
NA ---O2 2.291 ( .022 ) 1, .0000, .0000, .0000
O2 X/A = .5702 Y/B = .2303 Z/C = .7424
NA ...O2 2.455 -1, 1.0000, .0000, 2.0000
O2 X/A = .0702 Y/B = .2697 Z/C = .7424
C ...O2 1.250 2, .0000, .0000, 2.0000
O1 ...O2 2.276 2, .0000, .0000, 2.0000
O2 X/A = .9298 Y/B = .7303 Z/C = .2576
1 DIFFERENCE MAP 1 FOR Na2C2O4 P21/a partial data delta 2-t
MAXIMUM = 170.06, MINIMUM = -164.16
MULTIPLIED BY 90.1616 (SCAN 2)
ATOM HEIGHT X/A Y/B Z/C S.O.F. MOLECULE ELEVATION
1 NA .3539 .0550 .8030 1.0000 1 1.65
2 C .0660 .0412 .6432 1.0000 1 2.11
3 O1 .1501 -.1272 .6502 1.0000 1 1.94
4 O2 .4298 -.2303 1.2576 1.0000 1 3.05
5 Q 1 170. .3628 .1931 .4545 1.0000 1 .38
6 Q 2 151. .0031 .3043 .9010 1.0000 1 3.05
7 Q 3 151. .5031 .1957 .9010 ** .000 FROM 6
8 Q 4 143. .4338 .3764 1.0251 1.0000 1 1.94
9 Q 5 137. .3742 -.0067 .3194 1.0000 1 .00
10 Q 6 137. .3742 -.0067 .3193 ** .000 FROM 9
11 Q 7 125. .1304 .2476 .5751 1.0000 1 1.56
12 Q 8 124. .0637 .0909 .8441 1.0000 1 2.76
13 Q 9 123. .0212 .1328 1.0075 1.0000 1 3.43
14 Q 10 123. .0212 .1328 1.0075 ** .000 FROM 13
15 Q 11 122. .3420 .3433 1.1575 1.0000 1 2.71
16 Q 12 122. .2775 .1366 .3120 1.0000 1 .23
17 Q 13 114. .2824 -.0814 .4099 1.0000 1 .66
BONDS (INCLUDING SYMMETRY RELATED ATOMS)
2- 2 1.71 1- 3 2.36 2- 3 1.25 1- 3 2.30 1- 4 2.29 2- 4 1.25 1- 5 1.42
3- 5 1.02 2- 6 1.79 1- 6 2.20 4- 6 .93 1- 6 1.74 1- 8 2.02 2- 8 1.44
3- 8 1.47 6- 8 1.28 1- 9 1.74 4- 9 1.33 5- 9 1.16 2- 11 1.30 9- 11 1.34
1- 11 2.10 4- 11 .89 2- 12 .75 3- 12 1.63 6- 12 1.31 11- 12 1.45 4- 12 1.01
8- 12 1.22 8- 12 1.53 2- 13 1.46 6- 13 .99 12- 13 .77 2- 13 1.81 12- 13 1.58
13- 13 1.46 4- 13 1.30 8- 13 1.43 8- 13 .92 1- 15 1.96 5- 15 1.31 8- 15 1.10
1- 15 2.34 2- 15 1.55 3- 15 .69 12- 15 1.63 1- 16 1.90 5- 16 1.04 15- 16 1.40
3- 16 1.46 9- 16 1.26 9- 17 1.10 11- 17 1.28 1- 17 1.68 3- 17 1.67 5- 17 1.67
16- 17 1.20
1MOLECULE 1 FOR Na2C2O4 P21/a partial data delta 2-t
MATRIX .4825 .8448 .2312 -.8300 .5253 -.1873 -.2797 -.1015 .9547 SCALE = 1.000 INCHES PER ANGSTROM
3
2
17 12
13
9
4 6
16 11
1
5
15
8
1 OBSERVED AND CALCULATED STRUCTURE FACTORS FOR Na2C2O4 P21/a partial data delta 2-t 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
2 0 0 15 13 0 -6 0 1 14 -15 1 -4 3 1 10 -8 1 2 1 2 7 -5 0 -2 5 2 1 -1 0
4 0 0 52 -51 0 -4 0 1 27 -29 0 -3 3 1 12 -12 0 3 1 2 14 -15 0 -1 5 2 2 0 0
6 0 0 19 10 0 -2 0 1 22 -20 0 -2 3 1 11 -9 0 4 1 2 6 5 1 0 5 2 7 -3 1
8 0 0 0 -3 0 0 0 1 16 -15 0 -1 3 1 10 -7 0 7 1 2 6 6 1 1 5 2 4 4 2
10 0 0 25 -23 1 2 0 1 39 9 0 1 3 1 2 3 0 8 1 2 1 -2 0 2 5 2 7 -3 2
12 0 0 6 5 1 4 0 1 29 31 0 2 3 1 5 -4 1 9 1 2 4 2 0 3 5 2 4 1 1
1 1 0 6 4 0 8 0 1 6 -5 1 5 3 1 7 5 0 10 1 2 9 -9 1 -8 0 3 9 -12 2
2 1 0 7 6 0 10 0 1 9 -8 1 6 3 1 10 9 0 -7 2 2 6 4 1 -4 0 3 13 12 1
3 1 0 22 17 0 -8 1 1 6 -5 0 7 3 1 6 3 1 -6 2 2 15 -14 1 -2 0 3 6 -1 1
4 1 0 40 -36 0 -7 1 1 10 -11 1 9 3 1 2 -1 1 -5 2 2 7 8 0 0 0 3 5 2 1
5 1 0 3 0 0 -4 1 1 8 -8 0 10 3 1 4 -3 1 -4 2 2 7 7 1 4 0 3 3 -7 0
6 1 0 21 -19 0 -3 1 1 6 -6 0 -9 4 1 8 2 1 -3 2 2 2 -5 0 6 0 3 8 -10 1
7 1 0 19 -15 0 -2 1 1 17 20 0 -8 4 1 9 10 2 -1 2 2 6 -4 0 -8 1 3 2 1 0
9 1 0 8 -2 0 -1 1 1 49 -57 0 -7 4 1 15 -13 1 0 2 2 6 -2 0 -6 1 3 3 4 0
10 1 0 6 8 1 0 1 1 19 23 0 -5 4 1 10 -8 1 2 2 2 3 -3 1 -5 1 3 10 -9 1
11 1 0 4 3 0 1 1 1 15 17 0 -4 4 1 12 -18 0 3 2 2 6 -4 0 -3 1 3 13 -14 1
12 1 0 5 -2 1 2 1 1 16 13 0 -2 4 1 4 -1 1 4 2 2 10 6 1 2 1 3 7 -3 0
0 2 0 17 15 0 3 1 1 31 33 0 -1 4 1 1 1 0 6 2 2 8 -9 1 3 1 3 7 -12 0
1 2 0 0 1 0 4 1 1 4 3 0 1 4 1 7 -4 0 8 2 2 13 -10 1 4 1 3 4 1 0
2 2 0 13 -11 0 5 1 1 16 -21 0 2 4 1 14 -6 0 9 2 2 2 2 1 5 1 3 3 3 0
3 2 0 4 -2 0 6 1 1 9 -10 0 3 4 1 21 15 1 -9 3 2 6 -7 1 6 1 3 5 0 0
4 2 0 16 -14 0 7 1 1 0 -1 0 4 4 1 12 9 1 -8 3 2 11 10 1 -7 2 3 1 -3 0
5 2 0 5 -1 0 8 1 1 16 -10 0 8 4 1 4 -5 1 -7 3 2 10 7 1 -6 2 3 4 -6 0
6 2 0 16 16 0 9 1 1 13 17 0 -4 5 1 11 -11 1 -6 3 2 8 6 1 -5 2 3 7 11 0
7 2 0 2 1 0 11 1 1 6 -5 1 -1 5 1 5 7 0 -5 3 2 8 13 1 -4 2 3 1 1 0
10 2 0 6 -7 0 -10 2 1 8 -3 1 1 5 1 5 -4 1 -3 3 2 9 -8 1 -3 2 3 12 -4 1
11 2 0 3 -1 1 -9 2 1 11 12 1 2 5 1 10 9 1 -2 3 2 13 11 1 2 2 3 9 14 1
2 3 0 37 34 0 -8 2 1 15 10 1 3 5 1 10 -7 1 -1 3 2 8 -6 0 3 2 3 7 2 1
5 3 0 2 -3 1 -7 2 1 10 -15 0 4 5 1 11 -12 1 0 3 2 13 12 0 5 2 3 12 -13 1
6 3 0 15 -12 0 -6 2 1 2 -2 0 5 5 1 2 3 0 1 3 2 9 9 1 6 2 3 4 -5 1
7 3 0 14 -19 0 -5 2 1 12 -12 0 6 5 1 3 1 0 2 3 2 21 -23 0 -6 3 3 10 -8 1
9 3 0 7 1 0 -4 2 1 23 -6 0 -10 0 2 8 8 2 3 3 2 7 -8 0 -5 3 3 6 -5 1
10 3 0 2 -1 1 -3 2 1 30 29 0 -8 0 2 13 14 1 4 3 2 12 -10 1 -4 3 3 2 4 1
0 4 0 6 4 0 -2 2 1 21 22 0 -4 0 2 17 14 1 6 3 2 12 13 1 -3 3 3 1 4 0
1 4 0 18 -18 1 -1 2 1 8 -7 0 -2 0 2 31 30 0 7 3 2 7 8 1 -2 3 3 9 9 1
2 4 0 13 10 1 0 2 1 1 2 0 0 0 2 34 -40 0 -7 4 2 2 -3 0 1 3 3 5 -1 0
4 4 0 6 3 1 1 2 1 31 -31 0 2 0 2 32 -37 0 -6 4 2 7 9 1 2 3 3 3 2 0
5 4 0 7 7 1 2 2 1 30 -31 0 4 0 2 20 23 0 -5 4 2 11 7 1 3 3 3 2 -1 1
6 4 0 13 -11 0 3 2 1 25 24 0 6 0 2 10 6 0 -4 4 2 6 6 1 4 3 3 3 2 1
7 4 0 5 -2 0 4 2 1 7 -4 0 10 0 2 8 11 1 -3 4 2 7 -1 0 5 3 3 3 1 0
9 4 0 6 -4 1 6 2 1 10 12 0 -10 1 2 1 0 0 -2 4 2 8 -8 1 -3 4 3 5 -3 0
1 5 0 12 -4 0 7 2 1 19 -18 1 -7 1 2 16 10 0 -1 4 2 14 -17 0 -2 4 3 6 6 1
2 5 0 7 -2 1 8 2 1 5 -2 0 -6 1 2 4 1 0 1 4 2 4 1 0 1 4 3 6 5 1
4 5 0 15 -10 1 9 2 1 0 0 0 -3 1 2 10 -7 0 2 4 2 7 -1 1 -2 0 4 6 -10 1
6 5 0 8 -7 1 10 2 1 2 0 1 -2 1 2 7 -8 0 3 4 2 13 11 1 2 0 4 7 13 1
7 5 0 3 -1 0 -9 3 1 5 2 0 -1 1 2 9 9 0 4 4 2 5 -5 0 -2 1 4 5 7 1
0 6 0 6 -6 1 -8 3 1 6 6 0 0 1 2 13 11 0 6 4 2 2 1 1 -1 1 4 2 -3 0
-12 0 1 10 2 1 -6 3 1 6 8 0 1 1 2 11 8 0 -3 5 2 3 0 0 1 1 4 6 -8 1
-8 0 1 14 14 1 -5 3 1 6 -2 0
1
1 Na2C2O4 P21/a partial data delta 2-t
DEVIATIONS GREATER THAN 2 SIGMA
H K L FO FC D/SIGMA
6 0 0 19.25 9.98 2.43
1 5 0 12.37 4.14 2.16
-12 0 1 9.54 1.71 2.06
2 0 1 39.03 8.59 7.99
-1 1 1 48.79 56.85 2.12
-4 2 1 22.54 6.06 4.33
2 4 1 13.66 5.79 2.06
-3 2 3 11.64 3.57 2.12
1ANALYSIS OF VARIANCE FOR Na2C2O4 P21/a partial data delta 2-t
GGG UGG GUG UUG GGU UGU GUU UUU ALL
N 40 21 30 32 38 22 29 30 242
V 314 252 252 342 644 318 229 273 367
SIN THETA 0.00 - .38 - .49 - .59 - .65 - .71 - .76 - .80 - .85 - .88 - .91
N 25 23 26 27 22 25 21 27 23 23
V 668 479 217 285 378 382 276 238 180 302
SQRT(F/FMAX) 0.00 - .20 - .27 - .33 - .35 - .38 - .43 - .47 - .52 - .61 - 1.00
N 24 24 28 23 24 26 21 25 23 24
V 149 188 258 211 375 285 254 373 380 783
ABS(H) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 REST
N 12 27 37 26 30 19 27 18 16 12 12 3 3 0 0
V 324 294 591 332 394 270 274 294 243 335 220 129 482 0 0
ABS(K) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 REST
N 33 55 52 46 35 20 1 0 0 0 0 0 0 0 0
V 640 297 345 231 319 324 3 0 0 0 0 0 0 0 0
ABS(L) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 REST
N 47 82 71 37 5 0 0 0 0 0 0 0 0 0 0
V 334 476 267 290 354 0 0 0 0 0 0 0 0 0 0