+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0016p-1 started at 16:15:15 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0016p-1 in P-1 CELL 0.71073 5.7652 8.2911 9.0772 87.558 73.569 81.599 ZERR 2.00 0.0004 0.0005 0.0004 0.004 0.004 0.003 LATT 1 SFAC C H N O UNIT 12 26 2 10 V = 411.70 F(000) = 192.0 Mu = 0.13 mm-1 Cell Wt = 358.35 Rho = 1.445 MERG 2 OMIT -3.00 55.00 OMIT 4 3 11 SHEL 7 0.77 HTAB O31A O1B EQIV_$1 x-1, y, z-1 HTAB N24 O1A_$1 EQIV_$2 -x, -y+2, -z+1 HTAB N24 O31B_$2 HTAB N24 O21_$2 EQIV_$3 x-1, y, z HTAB N24 O31B_$3 HTAB N24 O31A_$3 EQIV_$4 x, y, z-1 HTAB O21 O1B_$4 EQIV_$5 -x, -y+2, -z+2 MPLA C31 O31A O31B MPLA C31_$5 O31A_$5 O31B_$5 FMAP 2 PLAN 10 SIZE 0.01 0.08 0.14 ACTA BOND $H WGHT 0.00520 0.55700 L.S. 4 TEMP -153.00 FVAR 1.28356 MOLE 1 C1 1 0.732447 0.635977 1.141537 11.00000 0.01757 0.01447 = 0.01509 -0.00172 -0.00342 -0.00044 C2 1 0.885024 0.552759 0.992481 11.00000 0.01829 0.01954 = 0.01349 -0.00098 -0.00529 0.00134 AFIX 23 H2A 2 0.784482 0.484240 0.956976 11.00000 -1.20000 H2B 2 0.930963 0.637100 0.913232 11.00000 -1.20000 O1A 4 0.789169 0.607366 1.262199 11.00000 0.02493 0.02555 = 0.01368 -0.00275 -0.00668 0.00477 O1B 4 0.545208 0.738885 1.132962 11.00000 0.01744 0.02660 = 0.01585 -0.00165 -0.00252 0.00788 AFIX 0 MOLE 2 C22 1 0.170229 0.704556 0.469757 11.00000 0.01894 0.01642 = 0.02207 0.00004 -0.00323 -0.00153 AFIX 23 H22A 2 0.287254 0.646934 0.522363 11.00000 -1.20000 H22B 2 0.161463 0.633027 0.387465 11.00000 -1.20000 AFIX 0 C23 1 -0.078382 0.743055 0.582856 11.00000 0.01776 0.01770 = 0.01683 0.00118 -0.00640 -0.00016 AFIX 23 H23A 2 -0.130378 0.641337 0.634269 11.00000 -1.20000 H23B 2 -0.069060 0.817814 0.662535 11.00000 -1.20000 AFIX 0 N24 3 -0.262043 0.819955 0.505200 11.00000 0.01734 0.01954 = 0.01502 -0.00104 -0.00287 -0.00198 AFIX 137 H24A 2 -0.270212 0.751565 0.431589 11.00000 -1.50000 H24B 2 -0.217463 0.915469 0.461023 11.00000 -1.50000 H24C 2 -0.410847 0.839891 0.575466 11.00000 -1.50000 AFIX 0 O21 4 0.249734 0.853383 0.405534 11.00000 0.02045 0.01834 = 0.01620 0.00034 0.00069 -0.00312 AFIX 147 H21 2 0.344704 0.836050 0.316882 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 0.296709 0.888671 0.863186 11.00000 0.01369 0.01737 = 0.01554 0.00072 -0.00359 -0.00223 C32 1 0.114902 0.949479 1.011850 11.00000 0.01155 0.01749 = 0.01375 0.00046 -0.00169 0.00045 AFIX 23 H32B 2 0.193563 1.016649 1.065954 11.00000 -1.20000 H32A 2 0.068171 0.854884 1.078195 11.00000 -1.20000 AFIX 0 O31A 4 0.490593 0.790025 0.874490 11.00000 0.02049 0.03219 = 0.01476 -0.00075 -0.00487 0.00928 AFIX 147 H31 2 0.489565 0.780706 0.967175 11.00000 -1.50000 AFIX 0 O31B 4 0.268479 0.925375 0.737157 11.00000 0.02084 0.02566 = 0.01194 -0.00041 -0.00543 0.00089 HKLF 4 Covalent radii and connectivity table for 07skc0016p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C2_$6 C1 O1A - C1 O1B - C1 C22 - O21 C23 C23 - N24 C22 N24 - C23 O21 - C22 C31 - O31B O31A C32 C32 - C31 C32_$5 O31A - C31 O31B - C31 Operators for generating equivalent atoms: $1 x-1, y, z-1 $2 -x, -y+2, -z+1 $3 x-1, y, z $4 x, y, z-1 $5 -x, -y+2, -z+2 $6 -x+2, -y+1, -z+2 5633 Reflections read, of which 17 rejected -7 =< h =< 7, -10 =< k =< 10, -11 =< l =< 11, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1868 Unique reflections, of which 0 suppressed R(int) = 0.0527 R(sigma) = 0.0584 Friedel opposites merged Maximum memory for data reduction = 1787 / 18384 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 = 2112 / 137210 wR2 = 0.1267 before cycle 1 for 1868 data and 106 / 106 parameters GooF = S = 1.131; Restrained GooF = 1.131 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0052 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.28355 0.00342 -0.002 OSF Mean shift/esd = 0.004 Maximum = -0.013 for U33 O1A Max. shift = 0.000 A for H21 Max. dU = 0.000 for O21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2112 / 137210 wR2 = 0.1267 before cycle 2 for 1868 data and 106 / 106 parameters GooF = S = 1.131; Restrained GooF = 1.131 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0052 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.28354 0.00341 -0.005 OSF Mean shift/esd = 0.001 Maximum = -0.005 for OSF Max. shift = 0.000 A for H31 Max. dU = 0.000 for O21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2112 / 137210 wR2 = 0.1267 before cycle 3 for 1868 data and 106 / 106 parameters GooF = S = 1.131; Restrained GooF = 1.131 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0052 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.28353 0.00342 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H31 Max. dU = 0.000 for O21 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2112 / 137210 wR2 = 0.1267 before cycle 4 for 1868 data and 106 / 106 parameters GooF = S = 1.131; Restrained GooF = 1.131 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0052 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.28353 0.00342 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C2 Max. shift = 0.000 A for H31 Max. dU = 0.000 for O31A 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 H2A 0.7845 0.4842 0.9570 23 0.990 0.000 C2 C2_$6 C1 H2B 0.9310 0.6371 0.9132 23 0.990 0.000 C2 C2_$6 C1 H22A 0.2873 0.6469 0.5224 23 0.990 0.000 C22 O21 C23 H22B 0.1615 0.6330 0.3875 23 0.990 0.000 C22 O21 C23 H23A -0.1304 0.6413 0.6343 23 0.990 0.000 C23 N24 C22 H23B -0.0691 0.8178 0.6625 23 0.990 0.000 C23 N24 C22 H24A -0.2702 0.7516 0.4316 137 0.910 0.000 N24 C23 H24A H24B -0.2175 0.9155 0.4610 137 0.910 0.000 N24 C23 H24A H24C -0.4108 0.8399 0.5755 137 0.910 0.000 N24 C23 H24A H21 0.3447 0.8360 0.3169 147 0.840 0.000 O21 C22 H21 H32B 0.1936 1.0166 1.0660 23 0.990 0.000 C32 C31 C32_$5 H32A 0.0682 0.8549 1.0782 23 0.990 0.000 C32 C31 C32_$5 H31 0.4896 0.7807 0.9672 147 0.840 0.000 O31A C31 H31 07skc0016p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.73245 0.63598 1.14154 1.00000 0.01756 0.01447 0.01509 -0.00172 -0.00341 -0.00043 0.01608 0.00346 0.00042 0.00028 0.00026 0.00000 0.00118 0.00115 0.00111 0.00088 0.00093 0.00091 0.00048 C2 0.88502 0.55276 0.99248 1.00000 0.01829 0.01953 0.01348 -0.00098 -0.00528 0.00134 0.01731 0.00164 0.00019 0.00013 0.00011 0.00000 0.00121 0.00123 0.00110 0.00089 0.00093 0.00098 0.00050 H2A 0.78448 0.48424 0.95698 1.00000 0.02078 0.00000 0.00000 H2B 0.93096 0.63710 0.91323 1.00000 0.02078 0.00000 0.00000 O1A 0.78917 0.60737 1.26220 1.00000 0.02493 0.02555 0.01367 -0.00276 -0.00668 0.00478 0.02189 0.00164 0.00019 0.00013 0.00011 0.00000 0.00095 0.00097 0.00081 0.00068 0.00070 0.00075 0.00041 O1B 0.54521 0.73889 1.13296 1.00000 0.01744 0.02660 0.01584 -0.00165 -0.00251 0.00788 0.02149 0.00164 0.00019 0.00013 0.00011 0.00000 0.00087 0.00096 0.00083 0.00069 0.00068 0.00072 0.00040 C22 0.17023 0.70456 0.46976 1.00000 0.01893 0.01642 0.02206 0.00004 -0.00322 -0.00152 0.01976 0.00380 0.00044 0.00029 0.00028 0.00000 0.00121 0.00119 0.00123 0.00094 0.00100 0.00095 0.00052 H22A 0.28726 0.64693 0.52236 1.00000 0.02371 0.00000 0.00000 H22B 0.16146 0.63303 0.38746 1.00000 0.02371 0.00000 0.00000 C23 -0.07838 0.74306 0.58286 1.00000 0.01775 0.01770 0.01683 0.00118 -0.00639 -0.00016 0.01738 0.00363 0.00042 0.00029 0.00026 0.00000 0.00118 0.00118 0.00115 0.00090 0.00095 0.00094 0.00050 H23A -0.13038 0.64134 0.63427 1.00000 0.02086 0.00000 0.00000 H23B -0.06906 0.81782 0.66253 1.00000 0.02086 0.00000 0.00000 N24 -0.26204 0.81995 0.50520 1.00000 0.01733 0.01954 0.01501 -0.00104 -0.00287 -0.00198 0.01767 0.00298 0.00035 0.00024 0.00022 0.00000 0.00102 0.00105 0.00097 0.00078 0.00080 0.00082 0.00044 H24A -0.27021 0.75156 0.43159 1.00000 0.02650 0.00000 0.00000 H24B -0.21747 0.91547 0.46102 1.00000 0.02650 0.00000 0.00000 H24C -0.41085 0.83989 0.57546 1.00000 0.02650 0.00000 0.00000 O21 0.24974 0.85338 0.40553 1.00000 0.02044 0.01833 0.01619 0.00034 0.00069 -0.00312 0.01949 0.00255 0.00031 0.00020 0.00019 0.00000 0.00091 0.00090 0.00084 0.00065 0.00068 0.00070 0.00039 H21 0.34471 0.83605 0.31688 1.00000 0.02924 0.00000 0.00000 C31 0.29671 0.88867 0.86319 1.00000 0.01368 0.01737 0.01554 0.00072 -0.00358 -0.00223 0.01565 0.00350 0.00041 0.00028 0.00026 0.00000 0.00110 0.00117 0.00110 0.00088 0.00090 0.00091 0.00048 C32 0.11491 0.94948 1.01185 1.00000 0.01155 0.01749 0.01375 0.00046 -0.00169 0.00045 0.01492 0.00354 0.00039 0.00028 0.00025 0.00000 0.00109 0.00118 0.00108 0.00086 0.00088 0.00091 0.00048 H32B 0.19357 1.01665 1.06595 1.00000 0.01790 0.00000 0.00000 H32A 0.06818 0.85488 1.07820 1.00000 0.01790 0.00000 0.00000 O31A 0.49059 0.79002 0.87449 1.00000 0.02048 0.03218 0.01476 -0.00075 -0.00487 0.00928 0.02381 0.00281 0.00031 0.00022 0.00019 0.00000 0.00093 0.00106 0.00084 0.00073 0.00071 0.00077 0.00043 H31 0.48957 0.78071 0.96717 1.00000 0.03572 0.00000 0.00000 O31B 0.26848 0.92537 0.73716 1.00000 0.02084 0.02566 0.01193 -0.00041 -0.00543 0.00089 0.01972 0.00251 0.00030 0.00021 0.00018 0.00000 0.00088 0.00096 0.00080 0.00066 0.00068 0.00072 0.00039 Final Structure Factor Calculation for 07skc0016p-1 in P-1 Total number of l.s. parameters = 106 Maximum vector length = 511 Memory required = 2006 / 22995 wR2 = 0.1267 before cycle 5 for 1868 data and 0 / 106 parameters GooF = S = 1.131; Restrained GooF = 1.131 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0052 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0617 for 1418 Fo > 4sig(Fo) and 0.0868 for all 1868 data wR2 = 0.1267, GooF = S = 1.131, Restrained GooF = 1.131 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0190 0.0165 0.0128 C1 0.0236 0.0154 0.0130 C2 0.0349 0.0180 0.0127 O1A 0.0363 0.0171 0.0111 O1B 0.0247 0.0184 0.0162 C22 0.0205 0.0180 0.0136 C23 0.0198 0.0188 0.0144 N24 0.0269 0.0184 0.0132 O21 0.0178 0.0156 0.0136 C31 0.0197 0.0145 0.0106 C32 0.0432 0.0148 0.0135 O31A 0.0288 0.0190 0.0114 O31B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.032 0.044 0.058 0.074 0.094 0.123 0.174 1.000 Number in group 188. 189. 186. 187. 197. 182. 180. 189. 182. 188. GooF 1.087 1.068 1.135 1.155 1.242 1.133 1.142 1.209 0.846 1.229 K 4.797 1.533 1.167 1.081 1.019 0.994 0.981 1.000 1.001 1.011 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.67 inf Number in group 191. 189. 183. 189. 185. 188. 183. 186. 186. 188. GooF 1.253 1.237 1.144 1.164 1.140 1.082 0.977 0.911 1.042 1.292 K 1.059 1.053 1.084 1.024 1.026 0.997 1.002 1.005 1.019 1.000 R1 0.217 0.201 0.156 0.129 0.105 0.085 0.057 0.053 0.042 0.033 Recommended weighting scheme: WGHT 0.0049 0.5575 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 2 558.88 678.67 4.26 0.338 4.35 6 2 4 22.09 5.88 3.79 0.031 0.95 -2 2 0 536.11 452.85 3.53 0.276 2.14 5 4 9 25.27 52.77 3.52 0.094 0.82 -3 8 1 -3.44 6.21 3.20 0.032 0.83 -3 2 5 0.23 12.77 3.11 0.046 1.05 -4 -4 6 25.31 5.48 3.11 0.030 0.84 -2 2 7 35.54 56.24 2.96 0.097 0.99 1 -5 10 2.17 11.19 2.95 0.043 0.78 2 -1 1 179.06 216.90 2.90 0.191 2.58 1 -8 2 21.98 0.45 2.69 0.009 0.97 0 2 1 98.17 76.32 2.68 0.113 3.71 0 4 9 196.94 150.46 2.68 0.159 0.88 -3 -4 4 -1.95 6.42 2.67 0.033 1.11 5 0 8 76.75 50.10 2.63 0.092 0.91 -2 -5 7 34.42 56.40 2.61 0.097 0.89 6 -2 1 5.73 14.39 2.60 0.049 0.88 2 -3 11 2.83 11.38 2.58 0.044 0.78 -1 -2 5 6.43 1.81 2.57 0.017 1.46 2 7 9 8.07 19.42 2.57 0.057 0.78 -1 -6 3 8.44 1.99 2.56 0.018 1.21 -3 4 0 19.34 31.22 2.53 0.072 1.28 3 10 3 13.94 32.61 2.50 0.074 0.79 3 -6 3 32.66 49.85 2.49 0.092 1.02 -4 -9 1 40.35 22.95 2.47 0.062 0.80 1 -1 3 63.61 81.96 2.46 0.117 2.69 -4 5 2 48.46 29.41 2.44 0.070 0.92 -5 0 4 11.38 2.73 2.43 0.021 0.88 1 7 8 17.60 5.53 2.43 0.031 0.83 -3 2 7 16.81 35.90 2.42 0.078 0.88 -6 -5 1 19.94 9.15 2.42 0.039 0.82 -4 -4 7 33.48 17.11 2.42 0.054 0.78 -2 9 2 23.36 43.54 2.41 0.086 0.80 1 -2 6 383.03 336.01 2.38 0.238 1.40 3 9 2 44.37 65.01 2.36 0.105 0.87 3 3 3 1.37 5.79 2.35 0.031 1.60 7 3 4 -0.45 6.90 2.34 0.034 0.81 0 2 2 1363.28 1472.82 2.33 0.498 2.99 1 0 2 3052.25 3249.48 2.29 0.740 4.00 -2 8 4 20.34 4.61 2.29 0.028 0.82 -3 6 2 49.68 75.67 2.26 0.113 0.97 2 0 3 417.12 372.06 2.25 0.250 2.35 0 3 0 77.48 96.19 2.25 0.127 2.73 7 1 5 95.19 69.57 2.24 0.108 0.81 -5 4 3 31.12 51.65 2.23 0.093 0.82 7 4 1 29.81 18.49 2.22 0.056 0.78 1 2 1 5566.33 5941.63 2.22 1.000 3.50 3 -1 10 7.27 17.66 2.21 0.055 0.88 0 -10 3 17.25 7.90 2.19 0.036 0.79 0 10 0 1.13 13.22 2.18 0.047 0.82 Bond lengths and angles C1 - Distance Angles O1A 1.2331 (0.0024) O1B 1.2931 (0.0025) 122.79 (0.19) C2 1.5197 (0.0024) 121.00 (0.18) 116.20 (0.17) C1 - O1A O1B C2 - Distance Angles C2_$6 1.5149 (0.0020) C1 1.5197 (0.0024) 113.34 (0.13) H2A 0.9900 108.91 108.91 H2B 0.9900 108.91 108.91 107.73 C2 - C2_$6 C1 H2A O1A - Distance Angles C1 1.2331 (0.0024) O1A - O1B - Distance Angles C1 1.2931 (0.0025) O1B - C22 - Distance Angles O21 1.4232 (0.0028) C23 1.5073 (0.0032) 108.57 (0.19) H22A 0.9900 109.98 109.98 H22B 0.9900 109.98 109.98 108.35 C22 - O21 C23 H22A C23 - Distance Angles N24 1.4870 (0.0028) C22 1.5073 (0.0032) 111.22 (0.19) H23A 0.9900 109.39 109.39 H23B 0.9900 109.39 109.39 108.01 C23 - N24 C22 H23A N24 - Distance Angles C23 1.4870 (0.0028) H24A 0.9100 109.47 H24B 0.9100 109.47 109.47 H24C 0.9100 109.47 109.47 109.47 N24 - C23 H24A H24B O21 - Distance Angles C22 1.4232 (0.0028) H21 0.8400 109.47 O21 - C22 C31 - Distance Angles O31B 1.2203 (0.0027) O31A 1.3113 (0.0027) 120.18 (0.21) C32 1.5090 (0.0031) 123.20 (0.20) 116.61 (0.19) C31 - O31B O31A C32 - Distance Angles C31 1.5090 (0.0031) C32_$5 1.5248 (0.0042) 112.93 (0.23) H32B 0.9900 109.00 109.00 H32A 0.9900 109.00 109.00 107.79 C32 - C31 C32_$5 H32B O31A - Distance Angles C31 1.3113 (0.0027) H31 0.8400 109.47 O31A - C31 O31B - Distance Angles C31 1.2203 (0.0027) O31B - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.64 2.4653(19) 167.6 O31A-H31...O1B 0.91 1.91 2.805(2) 167.3 N24-H24A...O1A_$1 0.91 2.25 2.988(2) 138.3 N24-H24B...O31B_$2 0.91 2.27 2.876(3) 123.9 N24-H24B...O21_$2 0.91 2.06 2.961(3) 169.9 N24-H24C...O31B_$3 0.91 2.64 3.265(3) 126.7 N24-H24C...O31A_$3 0.84 1.88 2.6959(19) 164.5 O21-H21...O1B_$4 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 3.5767 (0.0112) x + 7.1776 (0.0114) y + 1.2892 (0.0275) z = 8.5525 (0.0277) * 0.0000 (0.0000) C31 * 0.0000 (0.0000) O31A * 0.0000 (0.0000) O31B Rms deviation of fitted atoms = 0.0000 3.5767 (0.0112) x + 7.1776 (0.0114) y + 1.2892 (0.0275) z = 8.3810 (0.0471) Angle to previous plane (with approximate esd) = 0.00 ( 0.33 ) * 0.0000 (0.0000) C31_$5 * 0.0000 (0.0000) O31A_$5 * 0.0000 (0.0000) O31B_$5 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0868 for 1868 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.4161 0.6256 0.1877 [ 1.28 A from O1B ] Deepest hole -0.36 at 0.4239 0.8062 -0.0095 [ 0.41 A from H31 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2060 / 15268 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4161 0.6256 1.1877 1.00000 0.05 0.29 1.28 O1B 1.77 C1 1.98 H22B 2.07 H21 Q2 1 0.0457 0.7357 0.5398 1.00000 0.05 0.27 0.71 C23 0.83 C22 1.29 H23B 1.44 H23A Q3 1 0.8257 0.6064 1.0640 1.00000 0.05 0.27 0.77 C2 0.78 C1 1.36 H2B 1.52 H2A Q4 1 0.8607 0.6083 1.2777 1.00000 0.05 0.26 0.47 O1A 1.60 C1 1.79 H24A 2.27 H22B Q5 1 0.5277 0.7529 1.1031 1.00000 0.05 0.25 0.33 O1B 1.32 H31 1.52 C1 2.02 H21 Q6 1 0.2113 0.9211 0.9478 1.00000 0.05 0.24 0.70 C32 0.82 C31 1.33 H32B 1.38 H32A Q7 1 0.7295 0.8335 0.8828 1.00000 0.05 0.24 1.50 O31A 1.50 H31 1.51 H32B 1.92 H2B Q8 1 0.0281 0.7640 1.0023 1.00000 0.05 0.23 1.13 H32A 1.60 H2B 1.70 C32 2.06 C2 Q9 1 0.2870 0.9677 0.3143 1.00000 0.05 0.23 1.09 H21 1.23 O21 2.00 H23B 2.20 H24B Q10 1 0.7173 0.6836 1.3144 1.00000 0.05 0.23 0.80 O1A 1.25 H24A 1.61 C1 2.15 N24 Shortest distances between peaks (including symmetry equivalents) 4 10 0.95 1 5 1.40 6 8 1.76 3 8 1.84 3 5 1.91 3 4 2.01 5 7 2.14 3 10 2.27 7 8 2.28 1 3 2.29 7 9 2.39 1 10 2.45 5 10 2.47 3 3 2.51 6 6 2.53 3 7 2.55 5 9 2.61 6 7 2.72 4 8 2.75 6 8 2.76 5 6 2.79 1 4 2.89 4 5 2.92 2 9 2.94 2 9 2.99 8 10 3.00 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.27: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.16: Structure factors and derivatives 0.19: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.03: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0016p-1 finished at 16:15:16 Total CPU time: 0.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++