Data for cell confirmation by FULLPROF, step 2
Na/COO 0 5 1 15 2 0 1 1 0 0 1 0 0 0 0 0 0 0 0 1 0 1 0 0 0 1 1 0 1 0 0 2 0 0 1.540560 1.544390 0.5000 90.0000 9.0000 0.7995 0.0000 80.00 0.0000 20 0.01 0.40 0.40 0.40 0.20 10.00 0.02 130.00 0.000 0.000 10.40 2746.58 11.40 2372.05 12.98 1955.90 14.56 1706.21 15.56 1622.98 18.14 1464.84 20.14 1364.97 21.12 1332.06 28.08 1404.55 35.04 1794.20 40.60 1893.88 48.14 1830.45 59.48 1540.48 67.82 1231.80 116.68 1065.34 1.00 10.00 130.00 170.00 11 !Number of refined parameters -0.0760 11.00 0.0000 0.00 0.0000 0.00 0.000000 0.00 0 Na/COO 0 0 0 1.0 0.0 0.0 2 0 0 0 0 0.00 0 5 0 P 2/M <-- Space group symbol 0.10000E-01 0.4000 0.0000 0.0000 0.0000 0.0000 0 Scale ETA Bov Strain 0.00000 21.00 0.00 0.00 0.00 0.00 0.03500 0.02000 0.02500 0.0000 0.0000 0.0000 0.0000 0 U V W X Y Siz12 51.00 41.00 31.00 0.00 0.00 0.00 0.00 10.422929 5.255810 3.482510 90.000000 93.089134 90.000000 Cell params 81.00000 91.00000 101.00000 0.00000 111.00000 0.00000 1.00000 0.00000 0.04000 0.05000 0.00000 0.00000 O1 O2 A-symtry Params 0.00 0.00 61.00 71.00 0.00 0.00
Results
******************************************************* *** PROGRAM FULLPROF (Version 3.1d - Jul96-LLB JRC) *** ******************************************************* Rietveld, Profile Matching & Integrated Intensity Refinement of X-ray and/or Neutron Data Date: 02/10/97 Time: 14:04:41.07 => PCR file code: naoxa0 => DAT file code: naoxa0 => Title: Na/COO ==> CONDITIONS OF THIS RUN: => Global Refinement of X-ray powder diffraction data Bragg-Brentano or Debye-Scherrer geometry => The 5th default profile function was selected => Data supplied in free format => Wavelengths: 1.54056 1.54439 => Base of peaks: 2.0*HW* 9.00 => Cos(Monochromator angle)= 0.7995 => Absorption correction (muR-eff): 0.0000 ==> Angular range, step and number of points: 2Thmin: 10.0000 2Thmax: 130.0000 Step: 0.0200 No. of points: 6001 => Pattern Matching (fixed scale) for phase: 1 => Scor: 3.5305 ==> RESULTS OF REFINEMENT: => No. of fitted parameters: 11 ------------------------------------------------------------------------------ => Phase No. 1 Na/COO P 2/M ------------------------------------------------------------------------------ => No. of reflections: 729 ==> PROFILE PARAMETERS: => Cell parameters : 10.42180 0.00018 5.25704 0.00008 3.48356 0.00007 90.00000 0.00000 93.09650 0.00098 90.00000 0.00000 => Overall scale factor : 0.010000000 0.000000000 => ETA(p-V) or M(P-VII) : 0.33686 0.00293 => Overall Tem. factor : 0.00000 0.00000 => Halfwidth parameters : 0.01735 0.00255 0.02924 0.00272 0.02184 0.00064 => Preferred orientation: 1.00000 0.00000 0.00000 0.00000 => Asymmetry parameters : 0.07615 0.00509 0.06018 0.00088 0.00000 0.00000 0.00000 0.00000 => X and Y parameters : 0.00000 0.00000 0.00000 0.00000 => Strain parameters : 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 => Size parameters : 0.00000 0.00000 0.00000 0.00000 ==> GLOBAL PARAMETERS: => Zero-point: -0.0857 0.0013 => Cos( theta)-shift parameter : 0.0000 0.0000 => Sin(2theta)-shift parameter : 0.0000 0.0000 ==> RELIABILITY FACTORS FOR POINTS WITH BRAGG CONTRIBUTIONS: => N-P+C: 5621 => Rp: 4.47 Rwp: 6.08 Rexp: 1.50 Chi2: 16.4 L.S. refinement => Conventional Rietveld R-factors ==> => Rp: 6.42 Rwp: 8.01 Rexp: 1.98 Chi2: 16.4 => Deviance: 0.962E+05 Dev* : 17.11 => DW-Stat.: 0.2156 DW-exp: 1.9212 => N-sigma of the GoF: 817.616 => Phase: 1 => Bragg R-factor: 2.16 Vol: 190.578 Fract(%): 0.00 => Rf-factor= 1.32 ATZ: 0.000 Brindley: 1.0000
The 120 first reflexions extracted
by using the Le Bail method in P2/m
=> Phase no.: 1 Phase name Na/COO No. Code H K L Mult Hw ETA/M 2theta Icalc Iobs Sigma 1 1 0 1 0 2 0.163 0.337 16.851 319.4 324.0 18.818 2 1 2 0 0 2 0.163 0.337 17.026 5235.8 5301.1 80.195 3 1 1 1 0 4 0.165 0.337 18.897 1321.0 1337.4 53.610 4 1 2 1 0 4 0.170 0.337 24.044 1203.2 1218.4 55.425 5 1 0 0 1 2 0.172 0.337 25.587 2361.0 2397.6 55.576 6 1 3 0 0 2 0.172 0.337 25.660 739.1 741.2 17.054 7 1 1 0 -1 2 0.173 0.337 26.554 10.2 10.3 7.957 8 1 1 0 1 2 0.174 0.337 27.448 101.8 104.7 36.059 9 1 2 0 -1 2 0.176 0.337 30.097 3775.4 3822.0 73.479 10 1 0 1 1 4 0.177 0.337 30.797 5289.7 5336.1 55.819 11 1 3 1 0 4 0.177 0.337 30.858 7290.6 7408.4 66.859 12 1 1 1 -1 4 0.178 0.337 31.617 31745.0 32297.1 168.697 13 1 2 0 1 2 0.178 0.337 31.678 13102.0 13111.5 64.635 14 1 1 1 1 4 0.179 0.337 32.383 3078.2 3115.9 57.151 15 1 0 2 0 2 0.180 0.337 34.081 1670.2 1692.5 42.406 16 1 4 0 0 2 0.181 0.337 34.444 16173.3 16385.8 136.835 17 1 2 1 -1 4 0.181 0.337 34.690 3367.6 3394.3 49.009 18 1 1 2 0 4 0.182 0.337 35.186 1.0 0.9 0.154 19 1 3 0 -1 2 0.182 0.337 35.518 0.1 0.1 0.035 20 1 2 1 1 4 0.183 0.337 36.091 2791.8 2828.8 67.808 21 1 3 0 1 2 0.184 0.337 37.563 23.4 23.7 6.555 22 1 2 2 0 4 0.185 0.337 38.333 1622.9 1654.0 38.132 23 1 4 1 0 4 0.185 0.337 38.580 15111.6 15290.4 139.761 24 1 3 1 -1 4 0.186 0.337 39.556 291.3 294.7 25.029 25 1 3 1 1 4 0.188 0.337 41.431 7477.6 7577.6 109.054 26 1 4 0 -1 2 0.189 0.337 42.203 2889.7 2926.1 67.180 27 1 0 2 1 4 0.190 0.337 43.099 22.8 22.2 4.622 28 1 3 2 0 4 0.190 0.337 43.145 73.9 75.8 13.609 29 1 5 0 0 2 0.191 0.337 43.443 9.9 9.9 2.766 30 1 1 2 -1 4 0.191 0.337 43.717 406.9 412.0 29.341 31 1 1 2 1 4 0.192 0.337 44.301 6586.9 6678.1 97.348 32 1 4 0 1 2 0.192 0.337 44.566 2838.7 2862.8 52.377 33 1 4 1 -1 4 0.193 0.337 45.746 407.2 412.9 28.823 34 1 2 2 -1 4 0.194 0.337 46.098 2766.4 2800.6 65.638 35 1 5 1 0 4 0.195 0.337 46.912 36.5 37.0 4.054 36 1 2 2 1 4 0.195 0.337 47.214 5412.4 5482.8 96.430 37 1 4 1 1 4 0.196 0.337 47.971 75.1 75.9 16.602 38 1 4 2 0 4 0.198 0.337 49.237 1425.3 1443.5 56.431 39 1 5 0 -1 2 0.198 0.337 49.782 43.7 44.2 4.114 40 1 3 2 -1 4 0.199 0.337 50.045 4863.4 4926.0 92.462 41 1 3 2 1 4 0.201 0.337 51.616 3159.8 3200.8 77.835 42 1 0 3 0 2 0.201 0.337 52.153 21.9 22.7 3.620 43 1 5 0 1 2 0.202 0.337 52.390 130.8 133.1 8.557 44 1 0 0 2 2 0.202 0.337 52.576 2371.9 2411.6 58.482 45 1 6 0 0 2 0.202 0.337 52.733 893.7 897.3 18.587 46 1 1 0 -2 2 0.202 0.337 52.855 688.2 682.4 13.122 47 1 5 1 -1 4 0.202 0.337 52.932 1485.8 1507.1 28.059 48 1 1 3 0 4 0.202 0.337 52.944 1572.9 1601.2 29.990 49 1 1 0 2 2 0.203 0.337 53.866 75.6 76.3 15.387 50 1 2 0 -2 2 0.204 0.337 54.687 2079.2 2107.5 62.211 51 1 2 3 0 4 0.205 0.337 55.269 5636.3 5735.7 82.034 52 1 4 2 -1 4 0.205 0.337 55.318 2575.5 2579.5 33.512 53 1 5 1 1 4 0.205 0.337 55.435 1038.5 1045.8 15.374 54 1 0 1 2 4 0.206 0.337 55.613 651.7 666.2 15.018 55 1 6 1 0 4 0.206 0.337 55.765 1901.8 1926.5 44.402 56 1 1 1 -2 4 0.206 0.337 55.882 388.1 381.7 10.593 57 1 5 2 0 4 0.207 0.337 56.337 88.2 91.0 9.725 58 1 2 0 2 2 0.207 0.337 56.652 1966.3 1995.8 59.094 59 1 1 1 2 4 0.207 0.337 56.857 591.2 591.2 20.545 60 1 4 2 1 4 0.208 0.337 57.269 183.8 186.3 21.832 No. Code H K L Mult Hw ETA/M 2theta Icalc Iobs Sigma 61 1 2 1 -2 4 0.208 0.337 57.649 204.0 206.7 25.261 62 1 3 0 -2 2 0.209 0.337 57.971 91.5 91.5 10.137 63 1 6 0 -1 2 0.209 0.337 58.082 278.4 282.9 24.977 64 1 0 3 1 4 0.210 0.337 58.970 856.5 860.3 31.792 65 1 3 3 0 4 0.210 0.337 59.007 1101.6 1123.6 36.778 66 1 1 3 -1 4 0.211 0.337 59.465 372.5 378.8 25.314 67 1 2 1 2 4 0.211 0.337 59.550 213.3 213.4 13.928 68 1 1 3 1 4 0.211 0.337 59.935 11.2 11.6 5.454 69 1 3 0 2 2 0.213 0.337 60.801 106.9 107.7 6.749 70 1 3 1 -2 4 0.213 0.337 60.830 221.0 222.2 11.461 71 1 6 0 1 2 0.213 0.337 60.908 662.9 672.8 24.334 72 1 6 1 -1 4 0.213 0.337 60.937 848.6 861.9 29.556 73 1 2 3 -1 4 0.213 0.337 61.397 404.3 408.8 30.443 74 1 5 2 -1 4 0.214 0.337 61.709 490.1 495.6 32.118 75 1 2 3 1 4 0.215 0.337 62.318 63.7 66.0 13.756 76 1 7 0 0 2 0.215 0.337 62.414 34.9 34.0 4.667 77 1 4 0 -2 2 0.215 0.337 62.566 427.4 433.0 33.381 78 1 3 1 2 4 0.216 0.337 63.582 545.4 555.7 35.464 79 1 6 1 1 4 0.217 0.337 63.687 336.1 336.9 17.007 80 1 5 2 1 4 0.217 0.337 63.990 590.2 601.7 24.015 81 1 4 3 0 4 0.217 0.337 64.009 447.8 452.2 17.758 82 1 0 2 2 4 0.217 0.337 64.154 221.3 217.5 8.294 83 1 6 2 0 4 0.218 0.337 64.292 641.7 657.5 25.982 84 1 1 2 -2 4 0.218 0.337 64.400 211.8 209.4 9.777 85 1 3 3 -1 4 0.218 0.337 64.692 392.9 397.8 26.451 86 1 7 1 0 4 0.219 0.337 65.156 1091.9 1110.4 41.379 87 1 1 2 2 4 0.219 0.337 65.297 608.7 612.5 18.300 88 1 4 1 -2 4 0.219 0.337 65.305 624.7 630.9 18.921 89 1 3 3 1 4 0.220 0.337 66.031 748.8 758.9 27.230 90 1 2 2 -2 4 0.220 0.337 66.028 792.0 803.5 29.114 91 1 4 0 2 2 0.220 0.337 66.168 656.1 662.6 22.603 92 1 7 0 -1 2 0.222 0.337 67.058 18.2 18.3 13.110 93 1 2 2 2 4 0.223 0.337 67.792 26.7 27.0 22.538 94 1 5 0 -2 2 0.223 0.337 68.334 19.8 20.0 21.368 95 1 4 1 2 4 0.224 0.337 68.831 82.0 83.4 26.044 96 1 3 2 -2 4 0.224 0.337 68.986 15.4 15.3 3.585 97 1 6 2 -1 4 0.225 0.337 69.087 19.6 19.2 3.633 98 1 4 3 -1 4 0.225 0.337 69.248 245.1 248.7 29.987 99 1 7 1 -1 4 0.226 0.337 69.704 264.3 267.3 32.685 100 1 7 0 1 2 0.226 0.337 70.109 3.8 3.8 3.272 101 1 5 3 0 4 0.226 0.337 70.146 4.5 4.7 4.657 102 1 5 1 -2 4 0.228 0.337 70.958 83.7 85.0 19.524 103 1 4 3 1 4 0.228 0.337 70.974 73.0 73.7 15.978 104 1 3 2 2 4 0.229 0.337 71.573 104.3 105.3 16.209 105 1 6 2 1 4 0.229 0.337 71.672 221.0 225.5 23.011 106 1 0 4 0 2 0.229 0.337 71.761 70.8 70.1 7.225 107 1 1 4 0 4 0.230 0.337 72.421 816.9 827.2 53.085 108 1 8 0 0 2 0.230 0.337 72.619 1.6 1.4 0.133 109 1 5 0 2 2 0.230 0.337 72.641 0.7 0.6 0.064 110 1 7 1 1 4 0.230 0.337 72.705 0.1 0.0 0.008 111 1 7 2 0 4 0.231 0.337 73.062 9.1 9.3 3.835 112 1 4 2 -2 4 0.231 0.337 73.204 108.8 110.1 27.141 113 1 2 4 0 4 0.233 0.337 74.386 420.3 425.5 47.039 114 1 5 3 -1 4 0.234 0.337 74.974 75.2 77.7 12.146 115 1 8 1 0 4 0.234 0.337 75.180 317.6 322.0 19.100 116 1 6 0 -2 2 0.234 0.337 75.182 310.3 314.3 18.562 117 1 5 1 2 4 0.234 0.337 75.201 257.9 259.2 14.981 118 1 4 2 2 4 0.237 0.337 76.567 208.7 212.1 30.664 119 1 8 0 -1 2 0.237 0.337 76.763 241.7 244.0 22.912 120 1 5 3 1 4 0.238 0.337 77.065 97.2 98.0 8.602