=============================================================================== PLATON/ASYM-(Version 230517)-[Mode=2] FCF-File Validation for:gore001 =============================================================================== For Documentation: http://http://www.platonsoft.nl/FCF-VALIDATION.pdf Section 1 =============================================================================== General Data =============================================================================== Crystal Data From: gore001.cif Fo/Fc Data From: gore001.fcf FCF-TYPE=LIST4 Space Group : P21 Wavelength (Ang) : 1.54178 Unit Cell (CIF) : 5.3119 18.1819 6.2695 90.000 98.887 90.000 SHELX WGHT Pars. : 0.0813 0.6412 Extinction Par. : 0.0360 Section 2 =============================================================================== Reflections with abs((I(obs) - I(calc)) / SigW(I)) > 3.0 [I(calc) from FCF] =============================================================================== Nr H K L Theta I(obs) I(calc) Sigma(I) Ratio SigW(I) RatioW ------------------------------------------------------------------------------- 1 1 -8 0 21.69 895.07 1304.48 53.52 -7.65 112.39 -3.64 2 1 2 0 9.77 4857.38 3552.79 206.29 6.32 387.58 3.37 3 6 7 0 68.43 38.50 83.69 2.61 -17.31 9.05 -4.99 4 0 22 0 68.87 24.24 48.37 2.50 -9.65 6.55 -3.69 5 2 0 1 19.65 22.64 41.69 0.75 -25.40 5.61 -3.40 6 6 1 1 65.49 29.26 61.37 2.17 -14.80 7.36 -4.36 7 -6 9 1 71.95 31.15 55.59 2.61 -9.36 7.22 -3.39 8 5 13 1 70.35 31.57 63.82 2.78 -11.60 7.77 -4.15 9 4 17 1 71.84 20.99 42.00 1.86 -11.30 5.83 -3.60 10 -1 22 1 71.71 39.80 67.67 3.29 -8.47 8.41 -3.31 11 -5 -14 2 71.30 43.23 90.24 3.23 -14.55 9.75 -4.82 12 4 15 2 67.77 25.99 47.09 2.30 -9.17 6.45 -3.27 13 -4 -16 3 69.47 57.57 111.17 3.88 -13.81 11.51 -4.66 14 -5 -13 3 71.36 11.86 37.91 1.15 -22.65 5.07 -5.14 15 -5 -12 3 67.45 33.43 81.25 2.61 -18.32 8.77 -5.45 16 2 18 3 66.58 26.46 61.60 2.30 -15.28 7.33 -4.79 17 -2 19 3 66.48 32.25 84.47 2.27 -23.00 8.83 -5.92 18 -1 19 3 62.94 62.81 116.40 5.23 -10.25 12.44 -4.31 19 0 20 3 67.90 31.38 64.28 2.20 -14.95 7.60 -4.33 20 -3 -16 4 65.99 59.62 107.92 4.11 -11.75 11.47 -4.21 21 -4 -14 4 67.62 18.83 66.84 1.69 -28.41 7.25 -6.62 22 -5 -10 4 67.54 60.74 113.15 4.29 -12.22 11.84 -4.43 23 3 12 4 61.25 20.99 39.36 2.09 -8.79 5.74 -3.20 24 3 14 4 68.20 22.75 48.74 2.03 -12.80 6.36 -4.09 25 -3 16 4 65.99 76.66 119.61 5.03 -8.54 12.89 -3.33 26 2 16 4 66.38 12.08 28.73 1.42 -11.73 4.52 -3.68 27 0 17 4 61.16 98.57 151.47 6.74 -7.85 15.80 -3.35 28 1 17 4 64.27 15.86 30.92 1.65 -9.13 4.87 -3.09 29 -2 18 4 68.98 33.22 83.67 2.27 -22.22 8.81 -5.73 30 -1 18 4 65.59 29.64 50.06 2.37 -8.62 6.76 -3.02 31 -1 -17 5 71.57 15.98 33.19 1.38 -12.47 4.95 -3.48 32 -3 -14 5 67.13 55.19 86.37 3.87 -8.06 10.09 -3.09 33 -4 -12 5 69.59 42.68 81.62 3.09 -12.60 9.20 -4.23 34 -4 -11 5 66.19 7.18 22.20 0.98 -15.33 3.73 -4.02 35 4 -5 5 70.66 31.74 61.57 1.68 -17.76 7.32 -4.08 36 -5 -4 5 64.46 55.68 112.39 4.01 -14.14 11.57 -4.90 37 4 -4 5 69.22 9.95 21.30 0.94 -12.07 3.76 -3.02 38 -5 -3 5 63.55 19.02 48.67 1.82 -16.29 6.17 -4.80 39 -5 -2 5 62.91 22.95 55.32 2.06 -15.71 6.78 -4.78 40 -5 7 5 69.17 23.08 42.98 1.69 -11.78 5.91 -3.37 41 -4 12 5 69.59 32.47 70.33 2.34 -16.18 8.03 -4.71 42 2 13 5 65.94 31.64 66.06 1.66 -20.73 7.58 -4.54 43 1 14 5 62.68 15.35 29.89 1.69 -8.60 4.80 -3.03 44 2 14 5 69.94 39.37 65.84 2.95 -8.97 8.17 -3.24 45 0 15 5 62.84 29.87 66.32 2.57 -14.18 7.79 -4.68 46 1 16 5 71.30 6.51 17.05 0.88 -11.98 3.27 -3.23 47 2 -9 6 67.80 30.28 56.35 2.30 -11.33 7.13 -3.66 48 -4 -8 6 69.94 37.16 90.96 2.68 -20.07 9.45 -5.69 49 2 -8 6 65.40 17.75 33.65 1.59 -10.00 5.10 -3.12 50 3 -4 6 69.93 15.72 42.75 1.18 -22.91 5.53 -4.89 51 -4 8 6 69.94 35.27 95.16 2.55 -23.49 9.60 -6.24 52 2 9 6 67.80 25.44 55.08 1.79 -16.56 6.76 -4.38 53 1 12 6 69.03 20.71 42.36 1.79 -12.09 5.82 -3.72 54 -1 13 6 67.14 13.84 32.97 1.42 -13.47 4.87 -3.93 55 -1 14 6 71.34 71.83 120.26 4.88 -9.92 12.74 -3.80 56 0 8 7 69.21 32.56 69.98 2.24 -16.71 7.98 -4.69 -------- -------- Average = -13.69 -4.03 Note: SigW(I) is the SHELXL optimized weight For I(calc) < 2 Sigma(I): = 1.27 and = 0.43 Section 3 =============================================================================== Missing Reflections (Asym. Refl. Unit) below sin(th)/lambda = 0.5 =============================================================================== Nr H K L sin(th)/lambda Theta I(calc) I(calc)/I(max) ------------------------------------------------------------------------------- 1 0 2 0 0.055 4.86* 1442.54 0.39253 2 -1 2 1 0.127 11.33 1181.93 0.32162 3 -2 9 2 0.338 31.39 486.37 0.13235 4 -1 11 2 0.349 32.57 726.81 0.19778 5 -3 0 3 0.345 32.12 321.91 0.08760 6 -4 2 3 0.422 40.63 893.37 0.24310 7 -2 3 4 0.358 33.53 805.09 0.21908 8 0 5 4 0.351 32.76 637.68 0.17352 ** Note: I(max) is the maximum I(obs) encountered in the fcf-file ** Starred Reflections have a Theta below Theta(Min) = 7.15 From CIF: Theta(Min) = 7.15 Section 4: =============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) =============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing ------------------------------------------------------------------------------- 50.43 0.500 0.988 652 644 8 57.99 0.550 0.991 860 852 8 67.68 0.600 0.991 1128 1118 10 ------------------------------------------------------------ ACTA Min. Res. --- 72.02 0.617 0.989 1220 1206 14 Note: The Reported Completeness refers to the Actual H,K,L Index Range Section 5 =============================================================================== R-Value Statistics as a Function of Resolution (in Resolution Shell) =============================================================================== Theta sin(Th)/L # R1 wR2 S Rs av(I/SigW) av(I) av(SigW) ------------------------------------------------------------------------------- 27.72 0.302 236 0.051 0.127 1.128 0.051 8.70 575.26 58.83 35.88 0.380 251 0.036 0.086 0.741 0.040 8.41 180.36 19.75 42.14 0.435 285 0.033 0.086 0.708 0.040 7.90 146.31 16.09 47.60 0.479 244 0.042 0.104 0.836 0.039 7.71 129.61 14.15 52.70 0.516 290 0.050 0.122 0.917 0.041 7.23 85.76 10.14 57.71 0.548 273 0.053 0.128 0.886 0.048 6.53 70.13 8.87 62.86 0.577 259 0.069 0.168 1.055 0.057 5.95 50.15 7.19 68.50 0.603 258 0.113 0.310 1.763 0.069 5.26 48.90 7.63 72.02 0.617 114 0.162 0.436 2.219 0.072 4.74 34.99 6.36 R(sig) = sum(sig(I)) / sum(I) = 0.0471 ------------------------------------------------------------------------------- From FCF: R1 = 0.0545( 2204), wR2 = 0.1524( 2210), S = 1.177 From CIF: R1 = 0.0545( 2204), wR2 = 0.1524( 2210), S = 1.177, Npar = 145 No (SHELXL) Optimized Weights: wR2 = 0.1556 , S = 3.88 Section 6 =============================================================================== Summary of Reflection Data in FCF - Note: Friedel Pairs Averaged =============================================================================== Total # of Reflections in FCF. 2210 (Hmax = 6, Kmax = 22, Lmax = 7) Obs Number above Rep. Theta(Max) . 1 Actual Theta(Max) (Deg.) ... 72.022 (Hmax = 6, Kmax = 22, Lmax = 7) Exp Reported Theta(Max) (Deg.) ... 72.022 (Hmax = 6, Kmax = 22, Lmax = 7) Rep Actual Theta(Min) (Deg.) ... 7.149 Reported Theta(Min) (Deg.) ... 7.149 Unique (Expected) ............ 1219 Unique (in FCF) .............. 1206 Observed [I .gt. 2 Sig(I)] ... 1204 Less-Thans ................... 2 Negative Intensities ......... 0 Negative Intensities < - 2 SIG 0 Missing (Total) .............. 14 Missing Below Th(Min) ........ 1 Missing Th(Min) to STh/L=0.600 9 Missing STh/L=0.600 to Th(Max) 4 Missing Very Strong Refl. .... 0 Beamstop Effected Reflections 0 Space Group Extinctions ...... 11 Intensity Distribution [Decay of I/Sigma(I) versus sin(theta)/lambda] =============================================================================== sh st/l Ang # 0.25 1.0 2.0 Percent Distr. for I .gt. 2.0 * sig(I) =============================================================================== 1 0.301 1.661 234 100.0 100.0 100.0 **************************************** 2 0.379 1.318 251 100.0 100.0 99.6 **************************************** 3 0.434 1.152 283 100.0 100.0 100.0 **************************************** 4 0.478 1.046 240 100.0 100.0 100.0 **************************************** 5 0.515 0.971 290 100.0 100.0 99.7 **************************************** 6 0.547 0.914 268 100.0 99.3 98.5 ***************************************. 7 0.576 0.868 260 100.0 100.0 100.0 **************************************** 8 0.602 0.830 255 100.0 100.0 100.0 **************************************** 9 0.626 0.798 129 100.0 100.0 100.0 **************************************** I I I Percent Observed: 0 50 100 Maximum Percentage of Reflections with I .gt. 2*s(I) in any Resolution Shell100 Section 7 =============================================================================== Analysis of Variance (F(obs) and F(calc) from FCF) =============================================================================== :: Hmax = 6, Kmax = 22, Lmax = 7 :: Sigma Includes SHELXL WGHT Par. 0.0813 0.6412 :: K = Mean[Fo^2]/Mean[Fc^2] for Group - (Fo^2, Fc^2 from FCF) Fc/Fc(max) 0.000 0.053 0.076 0.098 0.115 0.135 0.157 0.184 0.225 0.296 1.000 Number in Group 222 221 221 221 221 221 221 221 221 220 GooF 0.862 1.059 1.190 1.269 1.502 1.384 1.387 0.914 0.913 1.096 K 1.142 1.021 1.012 1.019 1.009 1.026 1.020 1.025 1.010 1.015 Resolution(A) 0.81 0.84 0.88 0.92 0.96 1.02 1.09 1.20 1.36 1.69 6.19 Number in Group 222 221 221 221 221 221 220 222 221 220 GooF 2.235 1.431 1.036 0.921 0.972 0.871 0.801 0.717 0.790 1.181 K 0.841 0.994 1.056 1.079 1.091 1.064 1.040 1.014 0.962 1.017 Resolution Dependence for Fc/Fc(max) .LT. 0.076 Resolution(A) 0.81 0.84 0.88 0.92 0.96 1.02 1.09 1.20 1.36 1.69 6.19 Number in Group 71 73 59 52 52 39 36 33 16 12 GooF 1.216 1.022 0.865 0.859 0.978 0.680 0.886 0.767 0.849 0.769 K 0.850 1.016 1.044 1.085 1.176 1.120 1.161 1.042 1.026 1.059 Abs(H) 0 1 2 3 4 5 6 Number 241 496 460 407 317 209 80 PerObs Fo2 100 99 99 99 98 100 99 PerObs Fc2 100 99 98 99 99 100 96 Abs(K) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 Number 76 148 141 141 140 140 140 134 133 119 115 113 109 100 PerObs Fo2 99 100 100 100 99 100 99 99 100 99 99 100 98 99 PerObs Fc2 93 100 100 99 99 100 99 99 100 99 100 100 98 99 Abs(L) 0 1 2 3 4 5 6 7 Number 216 425 394 366 317 254 171 67 PerObs Fo2 99 98 99 99 100 99 100 99 PerObs Fc2 100 97 99 99 100 98 98 100 I------------I-----------I------------I-----------I------------I-----------I------------I-----------I 3.500=Max- - I Normal Probability Plot (S.C.Abrahams and E.T.Keve (1971). Acta Cryst. A27, 157-165.) x I I x I I Sample Size = 2210 NPP for (Fobs**2 - Fcalc**2) / Sigma(Fobs**2) I I CC = 0.9476 xxxxx I 2.235 - Est. Intercept = 0.0778 Sigma Includes SHELXL WGHT Par. 0.0813 0.6412 xxxxx - I Est. Slope = 1.0772 xxxxxx I I xxxxx I I xxxxx I I xxxxxx I 0.969 - xxxxxx - I xxxxxx I I xxxxx I I xxxxxx I I xxxxx I -0.296 - xxxx - I xxxxx I I xxx I I xxxx I I xxx I -1.562=Mid- xx - I xxx I I xx I I xx I I xx I -2.827 - xx - I x I I xx I I xx I I x I -4.093 - xx - I xxx I I xx I I xxx I I xx I -5.358 - x - I xx I I x I I x I I I -6.624=Min- x Vertical: Experimental Data, Horizontal: Theoretical Data - I------------I-----------I------------I-----------I------------I-----------I------------I-----------I -3.420 -1.710 0.000 1.710 3.420 Section 8 =============================================================================== Check for Unaccounted Twinning with the TwinRotMat Algorithm - N(selec) = 50 =============================================================================== Note: This Analysis is Based on Fc calculated from Coordinates in the CIF. =============================================================================== No Applicable Twin Law(s) Detected from Fo/Fc Analysis-or Already Accounted for Section 8 =============================================================================== Check for Unaccounted Twinning with the TwinRotMat Algorithm - N(selec) = 50 =============================================================================== Note: This Analysis is Based on Fc Taken from Fo/Fc File =============================================================================== No Applicable Twin Law(s) Detected from Fo/Fc Analysis-or Already Accounted for Section 9 =============================================================================== Bijvoet Pair Analysis - F(calc) from CIF =============================================================================== Excluded Outliers with Observed Bijvoet Difference > 288.36, or FCKD=0.0 =============================================================================== Nr H1 K1 L1 FOK1 H2 K2 L2 FOK2 FOKD FCKD SIGD =============================================================================== 1 -1 -3 1 2646.24 -1 3 1 2298.96 347.28 65.72 181.21 Flack Parameter Value (CIF) 0.01( 2) Number of Bijvoet Pairs ... 1004[Expected 1141] Number of Centro Reflns ... 76 Friedel Pair Coverage ..... 88% Res.Scat................... 0.0268 Friedif ................... 419 DLC DLO |I+-I-| DEL DEL SIG --- --- ------- H1 K1 L1 I1(obs) H2 K2 L2 I2(obs) OBS CALC DEL SIG DLC I+ + I- =============================================================================== -2 -1 1 6.6 -2 1 1 17.5 -10.8 -10.2 0.55 18.63 1.06 0.53226 -3 -3 1 51.2 -3 3 1 31.6 19.6 20.8 1.60 13.01 0.94 0.26863 0 -4 1 5.4 0 4 1 2.2 3.1 4.0 0.34 11.82 0.78 0.70064 -1 -5 1 8.1 -1 5 1 3.0 5.1 5.2 0.44 11.81 0.98 0.51105 1 -1 3 9.7 1 1 3 3.8 5.9 6.0 0.51 11.72 0.98 0.34679 -3 -1 3 19.4 -3 1 3 10.9 8.5 9.8 0.87 11.22 0.86 0.27548 -2-13 3 12.4 -2 13 3 5.1 7.3 7.0 0.76 9.26 1.03 0.41476 0 -5 2 67.3 0 5 2 57.1 10.2 22.4 2.52 8.91 0.45 0.16880 -4 -3 1 19.6 -4 3 1 32.1 -12.5 -9.8 1.14 8.62 1.27 0.18755 -1-13 2 30.1 -1 13 2 52.7 -22.5 -15.6 1.87 8.34 1.45 0.19539 3 -8 3 4.6 3 8 3 8.7 -4.1 -4.9 0.60 8.30 0.84 0.36127 2-10 1 49.5 2 10 1 86.6 -37.1 -25.2 3.07 8.20 1.48 0.19440 0-13 3 26.6 0 13 3 44.2 -17.6 -16.7 2.08 8.03 1.05 0.21566 -1 -5 5 10.4 -1 5 5 15.7 -5.4 -5.5 0.74 7.44 0.97 0.26745 -4 -2 4 47.0 -4 2 4 72.0 -25.0 -20.8 2.88 7.23 1.20 0.17622 1-16 0 8.8 1 16 0 20.5 -11.7 -8.1 1.15 7.04 1.44 0.30393 -3-13 3 4.3 -3 13 3 10.2 -5.9 -5.1 0.73 7.02 1.15 0.29755 -2 -7 4 13.4 -2 7 4 22.0 -8.5 -6.3 0.92 6.83 1.36 0.23553 -3 -2 2 13.0 -3 2 2 17.6 -4.7 -4.7 0.72 6.60 0.99 0.12414 -1 -4 6 17.8 -1 4 6 24.7 -6.9 -7.6 1.15 6.59 0.92 0.18525 -5 -6 4 7.8 -5 6 4 14.1 -6.3 -5.7 0.87 6.52 1.11 0.32948 3 -2 3 9.8 3 2 3 2.9 6.9 5.6 0.86 6.52 1.23 0.46028 4 -2 3 12.4 4 2 3 21.5 -9.1 -8.3 1.29 6.43 1.10 0.27313 5 -7 1 7.0 5 7 1 4.2 2.9 4.0 0.63 6.37 0.72 0.41101 -1 -2 4 6.1 -1 2 4 8.9 -2.8 -3.2 0.51 6.36 0.88 0.24100 2-11 0 27.5 2 11 0 20.6 6.9 8.1 1.29 6.29 0.85 0.19039 -1 -7 1 101.6 -1 7 1 87.3 14.2 25.1 4.06 6.20 0.57 0.12959 3 -6 2 70.1 3 6 2 57.1 12.9 16.5 2.74 6.03 0.78 0.13213 1 -3 5 33.1 1 3 5 49.3 -16.2 -16.6 2.78 5.97 0.98 0.20269 -2 -4 6 41.5 -2 4 6 57.8 -16.3 -14.0 2.40 5.86 1.16 0.17319 -2 -2 6 8.3 -2 2 6 13.3 -5.0 -4.5 0.78 5.77 1.11 0.22474 -4-11 2 27.9 -4 11 2 17.7 10.2 10.8 1.89 5.69 0.94 0.20388 -4 -8 2 9.3 -4 8 2 17.3 -8.0 -5.4 0.96 5.65 1.46 0.25662 2-12 0 28.9 2 12 0 45.4 -16.4 -12.4 2.27 5.48 1.32 0.18417 2 -7 3 4.1 2 7 3 6.7 -2.6 -3.2 0.59 5.41 0.81 0.34208 -1-13 4 79.6 -1 13 4 69.7 9.9 20.3 3.79 5.36 0.49 0.14360 -2 -5 4 114.2 -2 5 4 98.8 15.4 23.2 4.42 5.25 0.66 0.11094 -1-10 1 90.3 -1 10 1 132.5 -42.2 -22.7 4.33 5.24 1.86 0.09392 6 -1 0 7.1 6 1 0 1.7 5.4 2.9 0.55 5.24 1.85 0.50224 1-18 0 42.9 1 18 0 33.5 9.4 12.0 2.30 5.21 0.78 0.16212 3 -7 4 13.2 3 7 4 9.2 4.0 3.9 0.75 5.20 1.03 0.17314 1 -1 4 62.8 1 1 4 82.6 -19.9 -18.8 3.67 5.11 1.06 0.13115 4 -9 1 6.9 4 9 1 13.3 -6.4 -5.1 0.99 5.10 1.25 0.29912 2-10 4 24.5 2 10 4 18.6 5.9 7.2 1.42 5.06 0.82 0.16555 -4-12 3 9.7 -4 12 3 24.8 -15.1 -8.7 1.75 5.00 1.73 0.25486 5 -3 0 30.6 5 3 0 23.3 7.2 7.5 1.51 4.98 0.96 0.16277 3-13 0 45.5 3 13 0 74.1 -28.6 -16.8 3.52 4.78 1.70 0.14971 2 -2 2 122.4 2 2 2 173.8 -51.3 -41.1 8.62 4.77 1.25 0.14927 2 -5 4 105.2 2 5 4 85.6 19.5 20.8 4.40 4.73 0.94 0.11352 1 -6 3 47.0 1 6 3 63.3 -16.3 -13.3 2.83 4.70 1.22 0.12613 Hooft y Parameter Value . -0.017(10) Section 9 =============================================================================== Bijvoet Pair Analysis - F(calc) from CIF =============================================================================== Excluded Outliers with Observed Bijvoet Difference > 288.36, or FCKD=0.0 =============================================================================== Nr H1 K1 L1 FOK1 H2 K2 L2 FOK2 FOKD FCKD SIGD =============================================================================== 1 -1 -3 1 2646.24 -1 3 1 2298.96 347.28 65.72 181.21 Flack Parameter Value (CIF) 0.01( 2) Number of Bijvoet Pairs ... 1004[Expected 1141] Number of Centro Reflns ... 76 Friedel Pair Coverage ..... 88% Res.Scat................... 0.0268 Friedif ................... 419 DLC DLO |I+-I-| DEL DEL SIG --- --- ------- H1 K1 L1 I1(obs) H2 K2 L2 I2(obs) OBS CALC DEL SIG DLC I+ + I- =============================================================================== -2 -1 1 6.6 -2 1 1 17.5 -10.8 -10.2 0.55 18.63 1.06 0.53226 -3 -3 1 51.2 -3 3 1 31.6 19.6 20.8 1.60 13.01 0.94 0.26863 0 -4 1 5.4 0 4 1 2.2 3.1 4.0 0.34 11.82 0.78 0.70064 -1 -5 1 8.1 -1 5 1 3.0 5.1 5.2 0.44 11.81 0.98 0.51105 1 -1 3 9.7 1 1 3 3.8 5.9 6.0 0.51 11.72 0.98 0.34679 -3 -1 3 19.4 -3 1 3 10.9 8.5 9.8 0.87 11.22 0.86 0.27548 -2-13 3 12.4 -2 13 3 5.1 7.3 7.0 0.76 9.26 1.03 0.41476 0 -5 2 67.3 0 5 2 57.1 10.2 22.4 2.52 8.91 0.45 0.16880 -4 -3 1 19.6 -4 3 1 32.1 -12.5 -9.8 1.14 8.62 1.27 0.18755 -1-13 2 30.1 -1 13 2 52.7 -22.5 -15.6 1.87 8.34 1.45 0.19539 3 -8 3 4.6 3 8 3 8.7 -4.1 -4.9 0.60 8.30 0.84 0.36127 2-10 1 49.5 2 10 1 86.6 -37.1 -25.2 3.07 8.20 1.48 0.19440 0-13 3 26.6 0 13 3 44.2 -17.6 -16.7 2.08 8.03 1.05 0.21566 -1 -5 5 10.4 -1 5 5 15.7 -5.4 -5.5 0.74 7.44 0.97 0.26745 -4 -2 4 47.0 -4 2 4 72.0 -25.0 -20.8 2.88 7.23 1.20 0.17622 1-16 0 8.8 1 16 0 20.5 -11.7 -8.1 1.15 7.04 1.44 0.30393 -3-13 3 4.3 -3 13 3 10.2 -5.9 -5.1 0.73 7.02 1.15 0.29755 -2 -7 4 13.4 -2 7 4 22.0 -8.5 -6.3 0.92 6.83 1.36 0.23553 -3 -2 2 13.0 -3 2 2 17.6 -4.7 -4.7 0.72 6.60 0.99 0.12414 -1 -4 6 17.8 -1 4 6 24.7 -6.9 -7.6 1.15 6.59 0.92 0.18525 -5 -6 4 7.8 -5 6 4 14.1 -6.3 -5.7 0.87 6.52 1.11 0.32948 3 -2 3 9.8 3 2 3 2.9 6.9 5.6 0.86 6.52 1.23 0.46028 4 -2 3 12.4 4 2 3 21.5 -9.1 -8.3 1.29 6.43 1.10 0.27313 5 -7 1 7.0 5 7 1 4.2 2.9 4.0 0.63 6.37 0.72 0.41101 -1 -2 4 6.1 -1 2 4 8.9 -2.8 -3.2 0.51 6.36 0.88 0.24100 2-11 0 27.5 2 11 0 20.6 6.9 8.1 1.29 6.29 0.85 0.19039 -1 -7 1 101.6 -1 7 1 87.3 14.2 25.1 4.06 6.20 0.57 0.12959 3 -6 2 70.1 3 6 2 57.1 12.9 16.5 2.74 6.03 0.78 0.13213 1 -3 5 33.1 1 3 5 49.3 -16.2 -16.6 2.78 5.97 0.98 0.20269 -2 -4 6 41.5 -2 4 6 57.8 -16.3 -14.0 2.40 5.86 1.16 0.17319 -2 -2 6 8.3 -2 2 6 13.3 -5.0 -4.5 0.78 5.77 1.11 0.22474 -4-11 2 27.9 -4 11 2 17.7 10.2 10.8 1.89 5.69 0.94 0.20388 -4 -8 2 9.3 -4 8 2 17.3 -8.0 -5.4 0.96 5.65 1.46 0.25662 2-12 0 28.9 2 12 0 45.4 -16.4 -12.4 2.27 5.48 1.32 0.18417 2 -7 3 4.1 2 7 3 6.7 -2.6 -3.2 0.59 5.41 0.81 0.34208 -1-13 4 79.6 -1 13 4 69.7 9.9 20.3 3.79 5.36 0.49 0.14360 -2 -5 4 114.2 -2 5 4 98.8 15.4 23.2 4.42 5.25 0.66 0.11094 -1-10 1 90.3 -1 10 1 132.5 -42.2 -22.7 4.33 5.24 1.86 0.09392 6 -1 0 7.1 6 1 0 1.7 5.4 2.9 0.55 5.24 1.85 0.50224 1-18 0 42.9 1 18 0 33.5 9.4 12.0 2.30 5.21 0.78 0.16212 3 -7 4 13.2 3 7 4 9.2 4.0 3.9 0.75 5.20 1.03 0.17314 1 -1 4 62.8 1 1 4 82.6 -19.9 -18.8 3.67 5.11 1.06 0.13115 4 -9 1 6.9 4 9 1 13.3 -6.4 -5.1 0.99 5.10 1.25 0.29912 2-10 4 24.5 2 10 4 18.6 5.9 7.2 1.42 5.06 0.82 0.16555 -4-12 3 9.7 -4 12 3 24.8 -15.1 -8.7 1.75 5.00 1.73 0.25486 5 -3 0 30.6 5 3 0 23.3 7.2 7.5 1.51 4.98 0.96 0.16277 3-13 0 45.5 3 13 0 74.1 -28.6 -16.8 3.52 4.78 1.70 0.14971 2 -2 2 122.4 2 2 2 173.8 -51.3 -41.1 8.62 4.77 1.25 0.14927 2 -5 4 105.2 2 5 4 85.6 19.5 20.8 4.40 4.73 0.94 0.11352 1 -6 3 47.0 1 6 3 63.3 -16.3 -13.3 2.83 4.70 1.22 0.12613 Hooft y Parameter Value . -0.015(18) I------------I-----------I------------I-----------I------------I-----------I------------I-----------I 7.180=Max- x - I Student-t Probability Plot (S.C.Abrahams and E.T.Keve (1971). Acta Cryst. A27, 157-1x5.)x I I x xx I I Sample Size = 994 PP for (delta(G * Fcalc**2) - delta(Fobs**2))/Sigma I I CC = 0.9660 Sigma = sqrt(sigma(Fobs1**2) + sigma(Fobs2**2))x I 5.021 - Est. Intercept = 0.7409 xxxxxx - I Est. Slope = 1.8575 G = 1.0299 - nu = 5.77 I xxx I I xxxx I I xxx I 2.862 - xxxx - I xxxx I I xxx I I xxx I I xxx I 0.702 - xxxx - I xxx I I xxx I I xx I I xxx I -1.457=Mid- xx - I xx I I xx I I xx I I xx I -3.616 - xx - I xx I I xx I I x I I xx I -5.775 - xx - I xx I I x I I xx I I x I -7.935 - x - I xxx I I x xx I I x x I I x I -10.094=Min- x Vertical: Experimental Data, Horizontal: Theoretical Data - I------------I-----------I------------I-----------I------------I-----------I------------I-----------I -6.121 -3.061 0.000 3.061 6.121 Section 10: ================================================================================ Analysis of Difference Map Grid Point Density - (MIN = -0.35, MAX = 0.46 eA-3) ================================================================================ Frequency Plot Sqrt(Frequency) - Average = 0.000, Sigma = 0.091 eA-3 =============================================================================== Note: F(obs) from FCF and F(calc) from CIF model -0.40 0 -0.35 6 ** -0.30 24 *** -0.25 106 ******* -0.20 516 **************** -0.15 1746 ***************************** -0.10 4082 ******************************************** -0.05 6644 ******************************************************** 0.00 7522 ************************************************************ 0.05 5964 ***************************************************** 0.10 3436 ***************************************** 0.15 1616 **************************** 0.20 654 ****************** 0.25 276 *********** 0.30 106 ******* 0.35 46 ***** 0.40 22 *** 0.45 2 * 0.50 0 0.55 0 =============================================================================== Unique Density Maxima in Difference Map (CutOff level = 0.10 eA-3) =============================================================================== # x y z (e/A^3) Shortest Contacts within 3.2 Ang. (Excl. H) =============================================================================== 1 0.203 0.141 0.875 0.46 C3 1.08; C2 1.16; C1 1.24; S1 1.30; 2 0.866 0.155 0.954 0.42 S1 1.23; C3 2.22; C1 2.29; C4 2.44; 3 0.957 0.205 0.714 0.42 C1 1.26; S1 1.43; O1 1.57; C8 2.66; 4 0.109 0.143 0.809 0.39 C1 0.81; S1 1.23; C2 1.37; C3 1.56; 5 0.633 0.922 0.616 0.34 O2 1.31; C7 1.33; C6 1.48; C9 1.54; 6 0.378 0.982 0.398 0.34 O2 1.32; C6 1.44; N1 2.12; O3 2.18; 7 0.942 0.643 0.913 0.34 S1 1.29; C3 1.35; C4 1.77; C5 2.29; 8 0.179 0.233 0.815 0.33 S1 1.31; C1 1.65; O1 2.32; C2 2.57; 9 0.049 0.733 0.934 0.33 S1 1.31; C3 2.82; O1 2.92; C9 2.95; 10 0.108 0.732 0.033 0.32 S1 1.19; C1 2.66; C8 2.80; C3 2.95; 11 0.507 0.437 0.628 0.32 O2 1.21; C7 1.38; C10 1.50; C6 1.85; 12 0.703 0.829 0.272 0.30 C10 1.31; C7 1.68; C8 1.89; C9 2.43; 13 0.881 0.701 0.227 0.28 C1 1.00; S1 1.13; O1 1.80; C2 2.12; 14 0.698 0.517 0.532 0.27 C6 1.34; N1 1.41; O2 1.76; O3 2.23; 15 0.446 0.344 0.441 0.27 C7 0.78; C9 1.13; C8 1.48; O2 1.71; 16 0.268 0.187 0.088 0.26 S1 1.36; C3 1.49; C5 1.64; C2 2.55; 17 0.359 0.070 0.566 0.26 N1 1.22; C2 1.51; C6 1.62; O3 2.08; 18 0.559 0.938 0.677 0.26 C6 1.06; O2 1.20; O3 1.56; C7 1.81; 19 0.330 0.910 0.340 0.25 O2 1.21; C7 1.57; C8 1.86; C10 2.11; 20 0.477 0.392 0.385 0.25 O2 1.01; C7 1.08; C9 1.47; C6 1.78; 21 0.689 0.863 0.421 0.25 C7 0.74; C10 1.10; C9 1.53; C8 1.83; 22 0.810 0.595 0.410 0.25 C2 1.26; C1 1.34; N1 1.44; O1 1.67; 23 0.754 1.006 0.225 0.24 C10 1.97; C4 2.25; C5 2.61; O3 2.71; 24 0.509 0.921 0.762 0.24 O2 1.50; C6 1.51; C9 2.05; O3 2.12; 25 0.644 0.957 0.737 0.24 C6 1.20; O3 1.20; O2 1.80; C9 2.18; Density Maxima within 1.2 Angstrom from Atoms (CutOff level = 0.10 eA-3) =============================================================================== Atom # e/A^3 Ang # e/A^3 Ang # e/A^3 Ang # e/A^3 Ang =============================================================================== S1 13 0.28 1.13: 10 0.32 1.19: O2 20 0.25 1.01: 18 0.26 1.20: C1 4 0.39 0.81: 13 0.28 1.00: C2 1 0.46 1.16: C3 1 0.46 1.08: C6 18 0.26 1.06: C7 21 0.25 0.74: 15 0.27 0.78: 20 0.25 1.08: C9 15 0.27 1.13: C10 21 0.25 1.10: H10B 12 0.30 0.85: =============================================================================== Unique Density Minima in Difference Map (CutOff level = -0.10 eA-3) =============================================================================== # x y z (e/A^3) Shortest Contacts within 3.2 Ang. (Excl. H) =============================================================================== 1 0.245 0.548 0.375 -0.35 O3 0.76; C6 1.82; N1 2.65; C1 2.70; 2 0.950 0.439 0.059 -0.34 C4 2.19; N1 2.66; O3 2.75; C9 2.78; 3 0.144 0.971 0.906 -0.33 C4 1.87; N1 1.92; C2 2.63; C3 2.65; 4 0.049 0.422 0.937 -0.30 C10 2.08; C4 2.40; C9 2.94; O3 3.19; 5 0.635 0.219 0.496 -0.29 C8 1.86; O1 2.26; C5 2.60; C1 2.88; 6 0.138 0.176 0.872 -0.28 S1 0.69; C1 1.22; C3 1.60; C2 1.81; 7 0.054 0.577 0.648 -0.27 O1 1.96; C4 1.97; C1 2.57; C5 2.67; 8 0.107 0.223 0.878 -0.26 S1 0.75; C1 1.73; C3 2.35; O1 2.53; 9 0.700 0.260 0.653 -0.26 C8 1.02; C7 2.51; O1 2.67; S1 2.69; 10 0.055 0.452 0.616 -0.25 C10 1.59; O2 2.46; O3 2.50; C7 2.59; 11 0.399 0.641 0.711 -0.25 C5 0.87; C3 2.36; O1 2.50; 12 0.832 0.951 0.968 -0.25 O3 2.31; C4 2.33; C10 2.39; C9 2.71; 13 1.011 0.439 0.772 -0.25 C10 1.73; C4 2.24; O2 2.64; C7 3.12; 14 0.393 0.123 0.749 -0.24 C2 0.70; C1 1.59; N1 1.89; C3 1.96; 15 0.983 0.935 0.501 -0.24 C10 1.91; O2 2.16; O3 2.34; C9 2.37; 16 0.846 0.437 0.972 -0.24 C4 2.09; N1 2.84; C10 3.14; C3 3.18; 17 0.909 0.456 0.898 -0.24 C4 1.65; C10 2.68; O2 2.96; C3 2.98; 18 0.378 0.668 0.524 -0.24 C5 2.01; O1 2.13; C1 2.74; C8 2.75; 19 0.527 0.046 0.369 -0.23 C5 1.88; O3 1.94; C6 1.95; O2 2.55; 20 0.936 0.813 0.066 -0.22 S1 2.21; C10 2.54; C9 2.64; C8 2.86; 21 0.454 0.097 0.230 -0.22 C5 0.66; C3 1.56; C4 2.13; C2 2.80; 22 0.698 0.044 0.701 -0.22 O3 0.69; C6 1.56; N1 2.24; C2 2.42; 23 0.486 0.704 0.431 -0.22 C8 2.01; C1 2.52; O1 2.63; C2 2.66; 24 0.593 0.735 0.912 -0.21 C5 2.07; S1 2.11; C3 2.44; C9 2.75; 25 0.661 0.167 0.628 -0.21 O1 2.21; C1 2.38; C2 2.56; C8 2.61; Density Minima within 1.2 Angstrom from Atoms (CutOff level = -0.10 eA-3) =============================================================================== Atom # e/A^3 Ang # e/A^3 Ang # e/A^3 Ang # e/A^3 Ang =============================================================================== S1 6 -0.28 0.69: 8 -0.26 0.75: O3 22 -0.22 0.69: 1 -0.35 0.76: C2 14 -0.24 0.70: C5 21 -0.22 0.66: 11 -0.25 0.87: C8 9 -0.26 1.02: H2 14 -0.24 0.48: H4A 7 -0.27 1.02: H4B 17 -0.24 1.03: H5A 11 -0.25 1.11: H5B 21 -0.22 0.82: 11 -0.25 1.16: H5C 11 -0.25 0.94: 21 -0.22 1.02: H8A 9 -0.26 1.03: H8B 9 -0.26 1.07: H10C 10 -0.25 0.65: 15 -0.24 1.14: #=============================================================================== # R= 0.0545( 2204), wR2= 0.1525( 2210), S = 1.178 (From CIF+FCF data) # R= 0.0545( 2204), wR2= 0.1524( 2210), S = 1.177 (From FCF data only) # R= 0.0545( 2204), wR2= 0.1524( 2210), S = 1.177, Npar= 145, Flack 0.01(2) # Number Bijvoet Pairs = 1004 ( 88%), 991 Selected for: Parsons 0.024(6) # P2(tr) 1.000, P3(tr) 1.000, P3(tw) 0.000, Student-T Nu = 6, Hooft-0.015(18) #===============================================================================