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