+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0053c2c started at 12:50:47 on 23-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0053c2c in C2/c CELL 0.71073 9.1937 13.5734 10.5047 90.000 99.252 90.000 ZERR 4.00 0.0006 0.0006 0.0005 0.000 0.004 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 40 64 16 20 V = 1293.83 F(000) = 576.0 Mu = 0.11 mm-1 Cell Wt = 1089.07 Rho = 1.398 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 -x+1/2, -y+1/2, -z+2 HTAB N21 O1A_$1 EQIV_$2 x, y, z+1 HTAB N21 O1B_$2 EQIV_$3 x, -y+1, z+1/2 HTAB N23 O1B_$3 EQIV_$4 -x, y, -z+3/2 HTAB O1W O1A_$4 EQIV_$5 -X, Y, Z DFIX 0.84 0.02 O1W H1W DANG 1.35 0.02 H1W H1W_$5 FMAP 2 PLAN 10 SIZE 0.02 0.07 0.15 ACTA BOND $H WGHT 0.03610 1.40190 L.S. 4 TEMP -153.00 FVAR 0.46358 MOLE 1 C1 1 0.210875 0.298196 0.518252 11.00000 0.01791 0.01689 = 0.01840 -0.00213 0.00499 -0.00272 O1A 4 0.182111 0.302420 0.630785 11.00000 0.02888 0.01994 = 0.01938 0.00010 0.01028 0.00289 O1B 4 0.184200 0.362886 0.433243 11.00000 0.03491 0.01725 = 0.02095 0.00164 0.00779 0.00360 MOLE 2 C22 1 0.192636 0.418231 1.147605 11.00000 0.02452 0.02022 = 0.02176 -0.00134 0.00735 0.00069 AFIX 43 H22 2 0.120770 0.445395 1.193106 11.00000 -1.20000 AFIX 0 C24 1 0.338221 0.395211 1.001960 11.00000 0.01876 0.02162 = 0.01947 -0.00181 0.00301 -0.00196 C25 1 0.365222 0.323563 1.092589 11.00000 0.02272 0.02377 = 0.02307 -0.00079 0.00606 0.00345 AFIX 43 H25 2 0.435093 0.271822 1.094283 11.00000 -1.20000 AFIX 0 C26 1 0.402300 0.414517 0.883336 11.00000 0.02556 0.03612 = 0.02299 0.00198 0.00678 -0.00233 AFIX 137 H26A 2 0.493368 0.376473 0.886221 11.00000 -1.50000 H26B 2 0.424176 0.484916 0.877950 11.00000 -1.50000 H26C 2 0.331651 0.394904 0.807541 11.00000 -1.50000 AFIX 0 N21 3 0.273243 0.339311 1.181569 11.00000 0.02683 0.02085 = 0.01922 0.00287 0.00577 0.00125 AFIX 43 H21 2 0.268855 0.302723 1.250004 11.00000 -1.20000 AFIX 0 N23 3 0.229030 0.453256 1.038983 11.00000 0.02337 0.01726 = 0.02009 0.00148 0.00519 0.00099 AFIX 43 H23 2 0.189645 0.505394 0.997084 11.00000 -1.20000 AFIX 0 MOLE 3 O1W 4 0.000000 0.423138 0.750000 10.50000 0.03142 0.01904 = 0.04510 0.00000 0.02258 0.00000 H1W 2 -0.069880 0.388782 0.782609 11.00000 0.07801 HKLF 4 Covalent radii and connectivity table for 06skc0053c2c in C2/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C1_$6 O1A - C1 O1B - C1 C22 - N21 N23 C24 - C25 N23 C26 C25 - C24 N21 C26 - C24 N21 - C22 C25 N23 - C22 C24 O1W - no bonds found Operators for generating equivalent atoms: $1 -x+1/2, -y+1/2, -z+2 $2 x, y, z+1 $3 x, -y+1, z+1/2 $4 -x, y, -z+3/2 $5 -x, y, z $6 -x+1/2, -y+1/2, -z+1 15274 Reflections read, of which 387 rejected -11 =< h =< 11, -17 =< k =< 17, -13 =< l =< 13, Max. 2-theta = 54.93 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 8 6 0 2.39 1.90 7 10.47 3 7 9 15.68 5.77 4 68.02 2 Inconsistent equivalents 1488 Unique reflections, of which 0 suppressed R(int) = 0.1136 R(sigma) = 0.0517 Friedel opposites merged Maximum memory for data reduction = 1311 / 17412 Special position constraints for O1W x = 0.0000 z = 0.7500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 1571 / 121481 wR2 = 0.1131 before cycle 1 for 1488 data and 92 / 92 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.9046 0.8400 0.0646 0.0200 DFIX O1W H1W 1.2849 1.3500 -0.0651 0.0200 DANG H1W H1W_$5 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.065 0.065 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.072; Restrained GooF = 1.079 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0361 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46358 0.00139 -0.001 OSF Mean shift/esd = 0.002 Maximum = 0.007 for U12 O1B Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 1571 / 121481 wR2 = 0.1131 before cycle 2 for 1488 data and 92 / 92 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.9046 0.8400 0.0646 0.0200 DFIX O1W H1W 1.2849 1.3500 -0.0651 0.0200 DANG H1W H1W_$5 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.065 0.065 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.072; Restrained GooF = 1.079 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0361 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46358 0.00139 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.003 for U12 O1B Max. shift = 0.000 A for H26C Max. dU = 0.000 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 1571 / 121481 wR2 = 0.1131 before cycle 3 for 1488 data and 92 / 92 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.9046 0.8400 0.0646 0.0200 DFIX O1W H1W 1.2849 1.3500 -0.0651 0.0200 DANG H1W H1W_$5 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.065 0.065 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.072; Restrained GooF = 1.079 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0361 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46358 0.00139 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 1571 / 121481 wR2 = 0.1131 before cycle 4 for 1488 data and 92 / 92 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.9046 0.8400 0.0646 0.0200 DFIX O1W H1W 1.2849 1.3500 -0.0651 0.0200 DANG H1W H1W_$5 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.065 0.065 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.072; Restrained GooF = 1.079 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0361 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46358 0.00139 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C22 Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H22 0.1208 0.4454 1.1931 43 0.950 0.000 C22 N21 N23 H25 0.4351 0.2718 1.0943 43 0.950 0.000 C25 C24 N21 H26A 0.4934 0.3765 0.8862 137 0.980 0.000 C26 C24 H26A H26B 0.4242 0.4849 0.8780 137 0.980 0.000 C26 C24 H26A H26C 0.3316 0.3949 0.8075 137 0.980 0.000 C26 C24 H26A H21 0.2689 0.3027 1.2500 43 0.880 0.000 N21 C22 C25 H23 0.1896 0.5054 0.9971 43 0.880 0.000 N23 C22 C24 06skc0053c2c in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.21087 0.29820 0.51825 1.00000 0.01791 0.01689 0.01839 -0.00213 0.00499 -0.00272 0.01750 0.00301 0.00018 0.00012 0.00016 0.00000 0.00079 0.00084 0.00085 0.00066 0.00066 0.00065 0.00037 O1A 0.18211 0.30242 0.63078 1.00000 0.02888 0.01994 0.01938 0.00010 0.01028 0.00289 0.02203 0.00232 0.00014 0.00009 0.00012 0.00000 0.00066 0.00065 0.00066 0.00049 0.00052 0.00051 0.00031 O1B 0.18420 0.36289 0.43324 1.00000 0.03491 0.01725 0.02095 0.00164 0.00779 0.00360 0.02401 0.00235 0.00014 0.00009 0.00012 0.00000 0.00072 0.00064 0.00065 0.00050 0.00053 0.00054 0.00032 C22 0.19264 0.41823 1.14760 1.00000 0.02452 0.02022 0.02176 -0.00134 0.00735 0.00069 0.02177 0.00330 0.00020 0.00013 0.00017 0.00000 0.00087 0.00091 0.00091 0.00068 0.00072 0.00069 0.00040 H22 0.12077 0.44539 1.19311 1.00000 0.02612 0.00000 0.00000 C24 0.33822 0.39521 1.00196 1.00000 0.01876 0.02162 0.01947 -0.00181 0.00301 -0.00195 0.01996 0.00314 0.00018 0.00013 0.00017 0.00000 0.00080 0.00087 0.00086 0.00069 0.00068 0.00068 0.00038 C25 0.36522 0.32356 1.09259 1.00000 0.02271 0.02377 0.02307 -0.00079 0.00606 0.00345 0.02292 0.00335 0.00019 0.00014 0.00017 0.00000 0.00087 0.00093 0.00093 0.00073 0.00073 0.00073 0.00040 H25 0.43509 0.27182 1.09428 1.00000 0.02751 0.00000 0.00000 C26 0.40230 0.41452 0.88334 1.00000 0.02556 0.03612 0.02299 0.00197 0.00678 -0.00233 0.02791 0.00363 0.00021 0.00015 0.00018 0.00000 0.00093 0.00113 0.00096 0.00078 0.00078 0.00080 0.00044 H26A 0.49337 0.37647 0.88622 1.00000 0.04186 0.00000 0.00000 H26B 0.42418 0.48492 0.87795 1.00000 0.04186 0.00000 0.00000 H26C 0.33165 0.39491 0.80754 1.00000 0.04186 0.00000 0.00000 N21 0.27324 0.33931 1.18157 1.00000 0.02683 0.02085 0.01922 0.00287 0.00577 0.00125 0.02207 0.00277 0.00016 0.00011 0.00014 0.00000 0.00078 0.00078 0.00074 0.00059 0.00061 0.00062 0.00035 H21 0.26885 0.30272 1.25000 1.00000 0.02649 0.00000 0.00000 N23 0.22903 0.45326 1.03898 1.00000 0.02337 0.01726 0.02009 0.00148 0.00519 0.00099 0.02006 0.00269 0.00016 0.00011 0.00014 0.00000 0.00073 0.00073 0.00077 0.00056 0.00061 0.00059 0.00034 H23 0.18964 0.50539 0.99708 1.00000 0.02407 0.00000 0.00000 O1W 0.00000 0.42314 0.75000 0.50000 0.03142 0.01904 0.04510 0.00000 0.02258 0.00000 0.03005 0.00181 0.00000 0.00013 0.00000 0.00000 0.00102 0.00096 0.00124 0.00000 0.00094 0.00000 0.00047 H1W -0.06988 0.38879 0.78260 1.00000 0.07804 0.04430 0.00104 0.00194 0.00252 0.00000 0.00984 Final Structure Factor Calculation for 06skc0053c2c in C2/c Total number of l.s. parameters = 92 Maximum vector length = 511 Memory required = 1479 / 22995 wR2 = 0.1131 before cycle 5 for 1488 data and 0 / 92 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.9046 0.8400 0.0646 0.0200 DFIX O1W H1W 1.2850 1.3500 -0.0650 0.0200 DANG H1W H1W_$5 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.065 0.065 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.072; Restrained GooF = 1.079 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0361 * P )^2 + 1.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0485 for 1187 Fo > 4sig(Fo) and 0.0664 for all 1488 data wR2 = 0.1131, GooF = S = 1.072, Restrained GooF = 1.079 for all data Occupancy sum of asymmetric unit = 9.50 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0219 0.0159 0.0146 C1 0.0318 0.0198 0.0145 O1A 0.0360 0.0196 0.0164 O1B 0.0265 0.0212 0.0176 C22 0.0231 0.0193 0.0175 C24 0.0268 0.0240 0.0180 C25 0.0368 0.0270 0.0199 C26 0.0276 0.0219 0.0167 N21 0.0241 0.0194 0.0166 N23 0.0538 0.0190 0.0173 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.018 0.027 0.039 0.051 0.066 0.086 0.111 0.154 1.000 Number in group 151. 155. 142. 156. 151. 137. 151. 147. 148. 150. GooF 1.214 1.128 1.019 1.048 1.030 0.974 1.095 1.086 0.974 1.114 K 6.043 2.151 1.168 1.073 0.978 0.995 1.018 1.001 1.004 0.979 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.14 1.31 1.66 inf Number in group 150. 152. 148. 148. 147. 148. 149. 148. 148. 150. GooF 0.905 1.072 1.067 0.970 0.991 0.938 1.120 0.970 1.178 1.410 K 1.018 1.074 1.060 1.009 1.018 0.989 0.990 0.997 1.029 0.971 R1 0.180 0.156 0.116 0.090 0.076 0.058 0.051 0.040 0.038 0.035 Recommended weighting scheme: WGHT 0.0361 1.4016 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 0 6 338.08 207.93 4.60 0.069 1.73 3 7 0 124.56 68.95 4.16 0.040 1.63 6 6 3 496.14 339.79 4.15 0.089 1.13 0 12 0 45.61 0.02 3.80 0.001 1.13 6 0 0 1787.25 1326.61 3.63 0.175 1.51 6 0 6 53.29 5.41 3.50 0.011 1.06 2 0 0 34780.39 41954.35 3.15 0.985 4.54 -7 13 4 365.15 224.10 3.08 0.072 0.80 -11 3 4 48.52 95.80 3.07 0.047 0.81 3 1 0 356.21 456.06 3.07 0.103 2.95 0 0 4 978.67 791.59 2.93 0.135 2.59 2 12 6 116.88 55.41 2.89 0.036 0.91 -6 12 6 221.85 137.46 2.83 0.056 0.84 -6 6 8 277.66 357.98 2.75 0.091 0.97 0 2 6 15.99 1.08 2.75 0.005 1.67 -4 6 2 471.66 383.46 2.60 0.094 1.58 3 11 3 37.26 14.14 2.59 0.018 1.07 5 9 2 27.90 8.86 2.59 0.014 1.11 5 3 8 75.72 22.57 2.58 0.023 0.96 -5 1 3 2345.31 2020.66 2.58 0.216 1.71 -9 3 6 118.16 76.14 2.56 0.042 0.92 -1 11 9 17.52 74.93 2.54 0.042 0.85 5 7 9 78.91 20.34 2.53 0.022 0.82 3 3 6 80.08 49.53 2.53 0.034 1.34 -6 12 3 70.03 25.82 2.53 0.024 0.90 -7 1 12 33.77 0.44 2.50 0.003 0.78 -7 11 6 69.57 31.66 2.49 0.027 0.83 -1 5 4 319.12 255.77 2.46 0.077 1.88 -3 1 4 1962.02 1709.24 2.44 0.199 2.12 -1 1 3 2023.69 2299.71 2.44 0.231 3.31 -7 5 4 12.58 0.27 2.42 0.003 1.13 5 3 9 29.85 0.34 2.39 0.003 0.89 -4 12 4 33.11 8.14 2.32 0.014 0.97 -9 7 7 3.39 30.41 2.31 0.027 0.82 -5 3 11 13.06 0.00 2.31 0.000 0.88 -3 1 3 22.82 42.67 2.29 0.031 2.44 5 3 3 1267.56 1100.26 2.28 0.160 1.43 1 1 3 861.61 994.64 2.28 0.152 2.99 1 9 1 80.22 114.26 2.28 0.051 1.47 3 15 1 82.65 42.40 2.27 0.031 0.86 -2 4 6 708.57 608.94 2.26 0.119 1.53 0 8 6 47.74 73.69 2.23 0.041 1.21 -4 4 2 7.83 0.27 2.22 0.002 1.85 -7 7 5 13.71 0.94 2.21 0.005 1.01 -8 4 6 274.12 218.81 2.21 0.071 0.98 5 9 4 74.89 111.44 2.20 0.051 1.02 0 2 0 336.41 270.73 2.18 0.079 6.79 -7 7 1 688.85 802.67 2.18 0.136 1.09 -7 5 9 16.22 2.14 2.18 0.007 0.89 -2 6 3 12.34 1.22 2.18 0.005 1.80 Bond lengths and angles C1 - Distance Angles O1B 1.2483 (0.0021) O1A 1.2535 (0.0020) 126.55 (0.15) C1_$6 1.5701 (0.0033) 117.16 (0.18) 116.29 (0.18) C1 - O1B O1A O1A - Distance Angles C1 1.2535 (0.0020) O1A - O1B - Distance Angles C1 1.2483 (0.0021) O1B - C22 - Distance Angles N21 1.3187 (0.0023) N23 1.3277 (0.0023) 108.37 (0.15) H22 0.9500 125.82 125.82 C22 - N21 N23 C24 - Distance Angles C25 1.3556 (0.0025) N23 1.3803 (0.0022) 105.72 (0.15) C26 1.4848 (0.0024) 131.56 (0.17) 122.71 (0.16) C24 - C25 N23 C25 - Distance Angles C24 1.3556 (0.0025) N21 1.3743 (0.0022) 107.63 (0.15) H25 0.9500 126.19 126.19 C25 - C24 N21 C26 - Distance Angles C24 1.4848 (0.0024) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C24 H26A H26B N21 - Distance Angles C22 1.3187 (0.0023) C25 1.3743 (0.0022) 108.83 (0.15) H21 0.8800 125.58 125.58 N21 - C22 C25 N23 - Distance Angles C22 1.3277 (0.0023) C24 1.3803 (0.0022) 109.45 (0.15) H23 0.8800 125.28 125.28 N23 - C22 C24 O1W - Distance Angles H1W 0.9046 (0.0153) O1W - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.90 2.7376(19) 157.4 N21-H21...O1A_$1 0.88 2.34 2.9083(19) 122.7 N21-H21...O1B_$2 0.88 1.91 2.7358(19) 156.2 N23-H23...O1B_$3 0.905(15) 1.889(18) 2.7804(16) 168.1(16) O1W-H1W...O1A_$4 FMAP and GRID set by program FMAP 2 1 14 GRID -2.273 -1 -2 2.273 1 2 R1 = 0.0664 for 1488 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.0289 0.3807 0.6904 [ 0.45 A from H1W ] Deepest hole -0.30 at 0.2426 0.1015 0.9164 [ 0.90 A from N23 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1818 / 18897 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0289 0.3807 0.8096 1.00000 0.05 0.30 0.45 H1W 0.92 O1W 1.43 H1W 1.95 O1A Q2 1 0.4808 0.2699 1.1559 1.00000 0.05 0.23 0.71 H25 1.37 C25 2.15 O1A 2.18 N21 Q3 1 0.0000 0.5016 0.7500 0.50000 0.05 0.21 1.06 O1W 1.52 H22 1.72 H1W 2.47 C22 Q4 1 0.5086 0.3982 1.1573 1.00000 0.05 0.20 1.71 C25 1.76 H26B 1.92 H25 2.07 C24 Q5 1 0.0203 0.4514 1.2037 1.00000 0.05 0.20 0.95 H22 1.79 O1W 1.82 H22 1.83 C22 Q6 1 0.0000 0.3403 0.7500 0.50000 0.05 0.20 1.02 H1W 1.12 O1W 2.24 H25 2.30 O1A Q7 1 0.2500 0.2500 0.5000 0.50000 0.05 0.19 0.79 C1 1.75 O1A 1.75 O1B 2.75 H21 Q8 1 0.0438 0.2754 0.3816 1.00000 0.05 0.18 1.77 O1B 1.95 C1 2.12 H26A 2.54 C1 Q9 1 0.5000 0.3625 1.2500 0.50000 0.05 0.18 1.97 C25 2.06 H25 2.12 N21 2.27 H21 Q10 1 0.3258 0.3384 1.0155 1.00000 0.05 0.18 0.80 C24 0.86 C25 1.50 H25 1.83 N23 Shortest distances between peaks (including symmetry equivalents) 3 5 0.84 1 6 0.90 5 5 1.10 4 9 1.10 1 1 1.44 2 9 1.59 2 4 1.76 2 6 1.79 1 3 1.79 2 2 1.95 4 4 1.98 2 10 2.10 1 2 2.11 7 8 2.12 3 6 2.19 4 10 2.21 1 5 2.29 5 8 2.59 1 5 2.61 2 4 2.61 1 2 2.62 9 10 2.73 6 9 2.75 8 8 2.75 10 10 2.77 5 6 2.88 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.72: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.16: Structure factors and derivatives 0.09: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0053c2c finished at 12:50:48 Total CPU time: 1.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++