+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 15:18:59 on 15-Nov-2000 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 6.2197 8.1201 12.2081 103.178 91.760 104.153 ZERR 2.00 0.0012 0.0016 0.0024 0.030 0.030 0.030 LATT 1 SFAC C H N O S UNIT 20 22 6 4 4 V = 579.66 F(000) = 280.0 Mu = 0.45 mm-1 Cell Wt = 538.68 Rho = 1.543 MERG 2 FMAP 2 ACTA PLAN 20 BOND L.S. 4 WGHT 0.075400 1.433400 EXTI 0.006273 FVAR 0.71166 N13 3 -0.245321 0.541224 -0.073442 11.00000 0.02739 0.02338 = 0.02114 0.00569 0.00349 0.01252 N14 3 -0.422863 0.521748 -0.149710 11.00000 0.02374 0.02603 = 0.02356 0.00737 0.00178 0.00846 C18 1 -0.499857 0.657385 -0.123105 11.00000 0.02064 0.02360 = 0.02679 0.01135 0.00776 0.00561 C19 1 -0.692726 0.679367 -0.188066 11.00000 0.02350 0.03000 = 0.03656 0.00996 0.00138 0.00958 H13 2 0.231282 0.729539 0.334606 11.00000 0.03610 H17 2 -0.166589 0.458283 -0.081906 11.00000 0.05171 H15 2 -0.316318 0.912583 0.300907 11.00000 0.04225 H16 2 -0.438342 0.833208 0.466453 11.00000 0.04042 H19C 2 -0.743059 0.576717 -0.250775 11.00000 0.03539 H12 2 0.106725 0.651986 0.503532 11.00000 0.03728 H19B 2 -0.655484 0.783061 -0.214656 11.00000 0.03545 H10A 2 -0.343434 0.754389 0.637105 11.00000 0.05106 H19A 2 -0.811235 0.686821 -0.145200 11.00000 0.04785 H10C 2 -0.349218 0.565873 0.591865 11.00000 0.05619 H10B 2 -0.133785 0.681747 0.661396 11.00000 0.07606 MOLE 1 S11 5 0.064597 0.888740 0.182743 11.00000 0.02330 0.01998 = 0.02353 0.00570 0.00364 0.00860 S12 5 -0.361990 0.818308 -0.004802 11.00000 0.02355 0.02042 = 0.02734 0.00717 0.00460 0.01079 O11 4 0.303174 0.932065 0.198325 11.00000 0.02148 0.03011 = 0.03299 0.01016 0.00509 0.00748 O12 4 -0.042163 1.019532 0.163531 11.00000 0.03236 0.02144 = 0.02922 0.00568 0.00243 0.01248 N12 3 -0.009993 0.713095 0.081781 11.00000 0.02798 0.02315 = 0.01988 0.00380 0.00112 0.01342 C17 1 -0.184185 0.688267 0.008623 11.00000 0.02406 0.01918 = 0.02134 0.01022 0.00985 0.00941 C14 1 -0.034321 0.825018 0.304093 11.00000 0.02126 0.01879 = 0.02240 0.00097 0.00089 0.00358 C12 1 0.020299 0.704006 0.460668 11.00000 0.03178 0.02990 = 0.02480 0.00748 -0.00091 0.00694 C16 1 -0.301928 0.807610 0.439652 11.00000 0.02316 0.03393 = 0.03171 0.00156 0.00613 0.00602 C15 1 -0.232685 0.854593 0.341655 11.00000 0.02609 0.03052 = 0.02771 0.00306 0.00322 0.01108 C13 1 0.092293 0.749121 0.363087 11.00000 0.02343 0.02855 = 0.02705 0.00622 0.00145 0.00740 C11 1 -0.178087 0.731927 0.500536 11.00000 0.02991 0.02533 = 0.02103 -0.00192 0.00165 -0.00112 C10 1 -0.258201 0.680262 0.606052 11.00000 0.04344 0.04048 = 0.02427 0.00452 0.00936 0.00411 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 N13 - C17 N14 N14 - C18 N13 C18 - N14 C19 S12 C19 - C18 S11 - O11 O12 N12 C14 S12 - C17 C18 O11 - S11 O12 - S11 N12 - C17 S11 C17 - N12 N13 S12 C14 - C15 C13 S11 C12 - C13 C11 C16 - C15 C11 C15 - C14 C16 C13 - C12 C14 C11 - C16 C12 C10 C10 - C11 8358 Reflections read, of which 0 rejected -7 =< h =< 8, -10 =< k =< 10, -15 =< l =< 15, Max. 2-theta = 54.88 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 -1 1 31.83 0.52 5 5.13 3 -1 1 202.80 4.57 4 27.02 -5 -4 2 105.37 1.17 5 27.16 4 0 2 46.00 0.56 4 14.35 -5 -4 3 210.46 1.65 5 59.43 5 1 3 43.65 1.23 2 49.43 -5 1 5 178.98 8.54 2 63.12 -5 -2 7 50.67 1.36 3 25.09 8 Inconsistent equivalents 2576 Unique reflections, of which 0 suppressed R(int) = 0.0574 R(sigma) = 0.0536 Friedel opposites merged Maximum memory for data reduction = 1477 / 25818 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1946 / 247693 wR2 = 0.1059 before cycle 1 for 2576 data and 199 / 199 parameters GooF = S = 0.673; Restrained GooF = 0.673 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0754 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71209 0.00189 0.228 OSF 2 0.00628 0.00329 0.002 EXTI Mean shift/esd = 0.246 Maximum = 0.869 for U33 O12 Max. shift = 0.030 A for H10A Max. dU = 0.004 for H10B Least-squares cycle 2 Maximum vector length = 511 Memory required = 1946 / 247693 wR2 = 0.1054 before cycle 2 for 2576 data and 199 / 199 parameters GooF = S = 0.669; Restrained GooF = 0.669 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0754 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71242 0.00188 0.174 OSF 2 0.00626 0.00327 -0.004 EXTI Mean shift/esd = 0.093 Maximum = 0.357 for y H10B Max. shift = 0.015 A for H10B Max. dU =-0.002 for H10A Least-squares cycle 3 Maximum vector length = 511 Memory required = 1946 / 247693 wR2 = 0.1054 before cycle 3 for 2576 data and 199 / 199 parameters GooF = S = 0.669; Restrained GooF = 0.669 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0754 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71241 0.00188 -0.001 OSF 2 0.00625 0.00327 -0.004 EXTI Mean shift/esd = 0.009 Maximum = 0.109 for y H10B Max. shift = 0.005 A for H10B Max. dU = 0.000 for H10A Least-squares cycle 4 Maximum vector length = 511 Memory required = 1946 / 247693 wR2 = 0.1054 before cycle 4 for 2576 data and 199 / 199 parameters GooF = S = 0.669; Restrained GooF = 0.669 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0754 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.71241 0.00188 -0.005 OSF 2 0.00625 0.00327 0.000 EXTI Mean shift/esd = 0.003 Maximum = 0.028 for y H10B Max. shift = 0.001 A for H10B Max. dU = 0.000 for H19A No correlation matrix elements larger than 0.500 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N13 -0.24531 0.54107 -0.07354 1.00000 0.02800 0.02343 0.02131 0.00567 0.00340 0.01257 0.02312 0.00407 0.00032 0.00025 0.00015 0.00000 0.00106 0.00098 0.00092 0.00075 0.00073 0.00079 0.00041 N14 -0.42290 0.52167 -0.14972 1.00000 0.02431 0.02686 0.02355 0.00764 0.00226 0.00893 0.02424 0.00413 0.00032 0.00025 0.00016 0.00000 0.00101 0.00099 0.00095 0.00076 0.00072 0.00076 0.00041 C18 -0.49987 0.65744 -0.12302 1.00000 0.02157 0.02366 0.02656 0.01121 0.00774 0.00623 0.02289 0.00485 0.00036 0.00029 0.00019 0.00000 0.00113 0.00110 0.00112 0.00089 0.00084 0.00085 0.00046 C19 -0.69258 0.67964 -0.18798 1.00000 0.02335 0.03021 0.03671 0.00967 0.00070 0.00950 0.02941 0.00566 0.00042 0.00036 0.00023 0.00000 0.00126 0.00133 0.00138 0.00112 0.00100 0.00098 0.00052 H13 0.23276 0.73029 0.33491 1.00000 0.03537 0.05957 0.00484 0.00366 0.00229 0.00000 0.00737 H17 -0.16663 0.45603 -0.08057 1.00000 0.04853 0.06673 0.00528 0.00426 0.00257 0.00000 0.00886 H15 -0.31690 0.91133 0.30046 1.00000 0.03803 0.06094 0.00488 0.00378 0.00239 0.00000 0.00766 H16 -0.43663 0.83506 0.46824 1.00000 0.04009 0.06227 0.00503 0.00384 0.00243 0.00000 0.00784 H19C -0.74207 0.57740 -0.24941 1.00000 0.03744 0.06624 0.00480 0.00404 0.00253 0.00000 0.00763 H12 0.10517 0.64940 0.50345 1.00000 0.03899 0.06244 0.00488 0.00383 0.00246 0.00000 0.00773 H19B -0.65690 0.78135 -0.21561 1.00000 0.03983 0.06415 0.00489 0.00417 0.00247 0.00000 0.00790 H10A -0.33974 0.75955 0.63752 1.00000 0.04480 0.06712 0.00531 0.00425 0.00264 0.00000 0.00855 H19A -0.81190 0.69080 -0.14509 1.00000 0.05112 0.06999 0.00573 0.00427 0.00279 0.00000 0.00917 H10C -0.35038 0.56218 0.59069 1.00000 0.05512 0.07591 0.00578 0.00471 0.00272 0.00000 0.00964 H10B -0.13366 0.68670 0.66273 1.00000 0.08207 0.09212 0.00722 0.00531 0.00350 0.00000 0.01281 S11 0.06459 0.88882 0.18275 1.00000 0.02354 0.01998 0.02360 0.00567 0.00358 0.00864 0.02174 0.00115 0.00009 0.00007 0.00004 0.00000 0.00031 0.00028 0.00029 0.00021 0.00020 0.00021 0.00017 S12 -0.36202 0.81827 -0.00481 1.00000 0.02362 0.02068 0.02750 0.00724 0.00469 0.01092 0.02272 0.00118 0.00009 0.00007 0.00005 0.00000 0.00031 0.00029 0.00030 0.00021 0.00021 0.00021 0.00017 O11 0.30311 0.93199 0.19831 1.00000 0.02188 0.03001 0.03336 0.01045 0.00537 0.00748 0.02776 0.00353 0.00026 0.00021 0.00014 0.00000 0.00086 0.00088 0.00090 0.00070 0.00065 0.00066 0.00037 O12 -0.04233 1.01941 0.16351 1.00000 0.03239 0.02150 0.03021 0.00587 0.00228 0.01233 0.02715 0.00344 0.00027 0.00020 0.00014 0.00000 0.00093 0.00081 0.00087 0.00066 0.00066 0.00067 0.00037 N12 -0.00996 0.71295 0.08182 1.00000 0.02836 0.02277 0.02050 0.00368 0.00121 0.01366 0.02289 0.00398 0.00032 0.00024 0.00015 0.00000 0.00105 0.00094 0.00091 0.00074 0.00072 0.00078 0.00041 C17 -0.18409 0.68832 0.00875 1.00000 0.02422 0.01914 0.02073 0.01001 0.00989 0.00937 0.01965 0.00465 0.00036 0.00027 0.00017 0.00000 0.00114 0.00102 0.00103 0.00083 0.00080 0.00082 0.00043 C14 -0.03416 0.82499 0.30417 1.00000 0.02129 0.01850 0.02184 0.00100 0.00077 0.00370 0.02148 0.00445 0.00036 0.00028 0.00018 0.00000 0.00111 0.00101 0.00104 0.00080 0.00079 0.00080 0.00044 C12 0.02030 0.70410 0.46062 1.00000 0.03068 0.03070 0.02501 0.00794 -0.00077 0.00666 0.02890 0.00516 0.00042 0.00033 0.00020 0.00000 0.00131 0.00125 0.00117 0.00096 0.00092 0.00098 0.00051 C16 -0.30182 0.80762 0.43969 1.00000 0.02302 0.03454 0.03243 0.00209 0.00683 0.00640 0.03110 0.00526 0.00041 0.00033 0.00021 0.00000 0.00127 0.00134 0.00130 0.00104 0.00095 0.00099 0.00054 C15 -0.23272 0.85478 0.34173 1.00000 0.02709 0.02969 0.02835 0.00322 0.00320 0.01087 0.02837 0.00517 0.00041 0.00032 0.00020 0.00000 0.00126 0.00124 0.00119 0.00097 0.00092 0.00098 0.00051 C13 0.09236 0.74921 0.36298 1.00000 0.02384 0.02752 0.02730 0.00640 0.00175 0.00683 0.02624 0.00495 0.00039 0.00031 0.00020 0.00000 0.00122 0.00120 0.00116 0.00093 0.00089 0.00092 0.00049 C11 -0.17787 0.73193 0.50061 1.00000 0.03064 0.02592 0.02023 -0.00197 0.00147 -0.00072 0.02832 0.00464 0.00040 0.00030 0.00019 0.00000 0.00130 0.00118 0.00109 0.00089 0.00088 0.00094 0.00052 C10 -0.25832 0.68014 0.60603 1.00000 0.04422 0.04009 0.02374 0.00411 0.00909 0.00422 0.03769 0.00641 0.00053 0.00041 0.00022 0.00000 0.00166 0.00159 0.00127 0.00110 0.00111 0.00129 0.00062 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 199 Maximum vector length = 511 Memory required = 1747 / 24017 wR2 = 0.1054 before cycle 5 for 2576 data and 0 / 199 parameters GooF = S = 0.669; Restrained GooF = 0.669 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0754 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0369 for 2023 Fo > 4sig(Fo) and 0.0540 for all 2576 data wR2 = 0.1054, GooF = S = 0.669, Restrained GooF = 0.669 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0309 0.0212 0.0173 N13 0.0278 0.0237 0.0211 N14 0.0305 0.0222 0.0160 C18 0.0373 0.0302 0.0208 C19 0.0252 0.0228 0.0172 S11 0.0288 0.0245 0.0149 S12 0.0345 0.0279 0.0209 O11 0.0341 0.0301 0.0173 O12 0.0327 0.0205 0.0155 N12 0.0305 0.0160 0.0125 C17 0.0258 0.0221 0.0166 C14 0.0337 0.0300 0.0230 C12 0.0435 0.0292 0.0206 C16 0.0345 0.0283 0.0223 C15 0.0278 0.0273 0.0236 C13 0.0421 0.0268 0.0161 C11 0.0550 0.0366 0.0215 C10 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.024 0.036 0.051 0.064 0.080 0.100 0.129 0.173 1.000 Number in group 259. 260. 264. 265. 239. 268. 249. 262. 251. 259. GooF 0.758 0.757 0.720 0.666 0.582 0.637 0.637 0.601 0.600 0.692 K 1.715 0.967 0.970 0.983 0.987 0.986 0.997 0.997 1.013 1.016 Resolution(A) 0.77 0.80 0.84 0.87 0.92 0.98 1.06 1.16 1.33 1.67 inf Number in group 269. 255. 250. 264. 249. 259. 266. 250. 256. 258. GooF 0.672 0.658 0.654 0.650 0.606 0.548 0.590 0.593 0.642 0.977 K 1.000 1.005 1.028 0.994 0.991 1.002 1.016 1.017 1.021 1.005 R1 0.115 0.096 0.081 0.078 0.062 0.042 0.036 0.032 0.032 0.039 Recommended weighting scheme: WGHT 0.0497 0.1444 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 -3 1 419.50 554.53 4.35 0.194 2.62 4 0 0 137.05 93.09 4.18 0.080 1.50 3 -1 3 196.41 146.18 3.87 0.100 1.81 2 -4 3 37.95 62.85 3.83 0.065 1.80 0 -3 2 229.83 299.62 3.71 0.143 2.58 2 -2 6 57.93 37.55 3.52 0.051 1.67 -3 1 2 6.80 16.84 3.42 0.034 1.97 1 4 7 19.91 9.00 3.38 0.025 1.07 -7 7 0 1.64 17.12 3.34 0.034 0.78 -1 -4 2 0.28 6.36 3.32 0.021 1.75 3 0 3 3.53 0.03 3.29 0.001 1.72 2 -3 4 340.48 274.50 3.28 0.137 1.93 0 -4 14 73.89 44.66 3.19 0.055 0.85 0 -2 1 1319.38 1572.52 3.17 0.328 3.92 2 -2 1 61.35 85.80 3.12 0.077 2.71 -3 0 2 12.52 4.11 3.10 0.017 1.95 -6 4 6 14.98 30.42 3.02 0.046 0.88 1 6 9 -0.55 9.27 2.99 0.025 0.79 0 1 4 215.02 172.80 2.94 0.109 2.56 -3 2 3 172.15 135.91 2.93 0.096 1.76 -6 4 3 159.26 204.28 2.93 0.118 0.96 3 -9 4 15.33 0.70 2.91 0.007 0.88 -1 0 7 624.58 527.02 2.90 0.190 1.67 2 0 1 104.93 79.87 2.89 0.074 2.85 0 3 0 118.87 152.78 2.88 0.102 2.55 -1 3 4 441.64 368.92 2.86 0.159 1.78 2 0 4 28.53 17.67 2.86 0.035 2.02 -1 -1 4 5470.54 4705.73 2.82 0.567 2.69 -7 1 5 47.39 25.24 2.78 0.041 0.84 -4 -3 12 -2.93 3.12 2.77 0.015 0.83 -7 -1 1 -6.78 13.59 2.74 0.030 0.83 6 -7 2 14.82 3.30 2.72 0.015 0.86 1 0 5 57.13 41.33 2.69 0.053 2.14 2 5 6 6.09 0.21 2.68 0.004 0.95 -3 8 3 7.03 26.74 2.66 0.043 0.90 -6 3 4 5.22 12.96 2.64 0.030 0.97 1 -2 2 201.75 244.35 2.61 0.129 3.41 -3 10 0 -5.80 7.72 2.61 0.023 0.78 -1 2 1 1273.46 1471.51 2.61 0.317 3.35 -4 6 9 18.25 3.10 2.59 0.015 0.80 3 -5 3 3.76 10.26 2.58 0.026 1.39 6 0 1 1.64 17.29 2.58 0.034 0.99 -2 4 2 47.25 33.50 2.57 0.048 1.68 -1 -2 6 154.07 125.02 2.55 0.092 1.84 6 3 3 15.39 28.15 2.53 0.044 0.81 -1 10 0 18.77 4.55 2.53 0.018 0.78 3 -7 4 53.72 72.81 2.53 0.070 1.09 6 -3 9 -3.65 9.43 2.51 0.025 0.81 7 -1 4 -4.99 7.67 2.51 0.023 0.83 0 -2 5 632.34 544.94 2.46 0.193 2.27 Bond lengths and angles N13 - Distance Angles C17 1.3379 (0.0028) N14 1.3765 (0.0027) 118.23 (0.18) N13 - C17 N14 - Distance Angles C18 1.2864 (0.0029) N13 1.3765 (0.0027) 108.92 (0.19) N14 - C18 C18 - Distance Angles N14 1.2864 (0.0029) C19 1.4867 (0.0032) 123.10 (0.22) S12 1.7436 (0.0025) 115.74 (0.18) 121.15 (0.18) C18 - N14 C19 C19 - Distance Angles C18 1.4867 (0.0032) C19 - S11 - Distance Angles O11 1.4345 (0.0017) O12 1.4389 (0.0016) 118.97 (0.10) N12 1.6160 (0.0020) 106.17 (0.10) 111.07 (0.10) C14 1.7589 (0.0023) 106.83 (0.10) 107.82 (0.10) 105.09 (0.10) S11 - O11 O12 N12 S12 - Distance Angles C17 1.7335 (0.0022) C18 1.7436 (0.0025) 88.52 (0.11) S12 - C17 O11 - Distance Angles S11 1.4345 (0.0017) O11 - O12 - Distance Angles S11 1.4389 (0.0016) O12 - N12 - Distance Angles C17 1.3275 (0.0028) S11 1.6160 (0.0020) 120.41 (0.15) N12 - C17 C17 - Distance Angles N12 1.3275 (0.0028) N13 1.3379 (0.0028) 119.69 (0.19) S12 1.7335 (0.0021) 131.73 (0.17) 108.57 (0.16) C17 - N12 N13 C14 - Distance Angles C15 1.3872 (0.0032) C13 1.3845 (0.0032) 120.78 (0.22) S11 1.7589 (0.0023) 120.27 (0.18) 118.92 (0.18) C14 - C15 C13 C12 - Distance Angles C13 1.3811 (0.0033) C11 1.3898 (0.0035) 121.30 (0.23) C12 - C13 C16 - Distance Angles C15 1.3862 (0.0035) C11 1.3893 (0.0037) 121.80 (0.23) C16 - C15 C15 - Distance Angles C14 1.3872 (0.0032) C16 1.3862 (0.0035) 118.65 (0.23) C15 - C14 C13 - Distance Angles C12 1.3811 (0.0033) C14 1.3845 (0.0032) 119.44 (0.23) C13 - C12 C11 - Distance Angles C16 1.3893 (0.0037) C12 1.3898 (0.0035) 118.03 (0.22) C10 1.5057 (0.0034) 120.65 (0.24) 121.32 (0.24) C11 - C16 C12 C10 - Distance Angles C11 1.5057 (0.0034) C10 - FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0537 for 2576 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.2482 0.2377 -0.0076 [ 0.80 A from C17 ] Deepest hole -0.45 at 0.0657 0.1542 0.8257 [ 0.79 A from S11 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1837 / 17147 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2482 0.7623 0.0076 1.00000 0.05 0.38 0.80 C17 0.96 S12 1.85 N13 1.88 N12 Q2 1 -0.1287 0.8342 0.3221 1.00000 0.05 0.28 0.65 C14 0.74 C15 1.50 H15 1.79 C13 Q3 1 -0.0791 0.7003 0.0526 1.00000 0.05 0.26 0.52 N12 0.80 C17 1.86 N13 1.95 S11 Q4 1 0.0411 1.0153 0.1804 1.00000 0.05 0.26 0.56 O12 1.08 S11 1.94 O11 2.38 C14 Q5 1 -0.0022 0.8394 0.2459 1.00000 0.05 0.25 0.77 C14 1.00 S11 1.89 C13 1.89 C15 Q6 1 -0.3691 0.9653 -0.0014 1.00000 0.05 0.25 1.20 S12 2.52 C18 2.70 S12 2.70 O12 Q7 1 0.0045 0.7645 0.3224 1.00000 0.05 0.25 0.67 C14 0.78 C13 1.52 H13 1.80 C15 Q8 1 -0.5784 0.6625 -0.1566 1.00000 0.05 0.25 0.64 C18 0.85 C19 1.42 H19C 1.49 H19B Q9 1 -0.7558 0.4004 -0.3608 1.00000 0.05 0.23 1.72 H19C 1.77 C11 1.87 C16 1.91 C12 Q10 1 0.2313 0.8562 0.2176 1.00000 0.05 0.23 0.76 O11 1.22 S11 1.94 H13 1.98 C14 Q11 1 -0.4987 0.5809 -0.1198 1.00000 0.05 0.23 0.63 C18 0.79 N14 1.78 N13 1.87 C19 Q12 1 0.0032 0.5845 0.0455 1.00000 0.05 0.22 1.06 N12 1.24 H17 1.70 C17 1.79 H17 Q13 1 0.0967 0.6676 0.0795 1.00000 0.05 0.22 0.83 N12 1.19 H17 1.99 C17 2.00 S11 Q14 1 -0.0985 0.9592 0.1407 1.00000 0.05 0.22 0.54 O12 1.42 S11 2.17 N12 2.27 S12 Q15 1 -0.2805 0.9062 -0.0418 1.00000 0.05 0.21 0.98 S12 2.14 C18 2.21 C17 2.57 O12 Q16 1 0.4635 0.7430 0.1605 1.00000 0.05 0.21 2.00 O11 2.07 N14 2.13 H15 2.16 H17 Q17 1 -0.1045 1.0098 0.1614 1.00000 0.05 0.21 0.37 O12 1.66 S11 2.35 H15 2.50 S12 Q18 1 -0.4298 0.3745 -0.1467 1.00000 0.05 0.20 1.19 N14 1.60 N13 1.71 H17 2.40 C18 Q19 1 0.0336 0.6985 0.3988 1.00000 0.05 0.20 0.72 C13 0.75 C12 1.48 H13 1.51 H12 Q20 1 0.3602 0.9389 0.2069 1.00000 0.05 0.19 0.35 O11 1.78 S11 2.36 H15 2.53 H19B Shortest distances between peaks (including symmetry equivalents) 14 17 0.44 12 13 0.79 16 18 0.90 6 15 0.90 4 17 0.92 4 14 0.94 10 20 0.94 8 11 1.08 2 7 1.11 3 12 1.16 7 19 1.21 5 7 1.23 2 5 1.24 3 13 1.24 1 3 1.42 1 15 1.48 5 10 1.48 12 12 1.55 9 19 1.72 4 5 1.76 11 18 1.79 16 20 1.84 6 6 1.85 7 9 1.93 5 14 1.94 10 16 1.96 1 6 1.99 10 13 2.00 1 14 2.01 2 19 2.02 2 9 2.03 7 10 2.05 4 10 2.06 5 17 2.10 3 14 2.17 1 11 2.17 12 13 2.19 4 20 2.25 5 20 2.30 13 18 2.33 13 16 2.34 3 5 2.35 14 15 2.37 5 13 2.38 1 17 2.38 4 15 2.38 6 14 2.40 5 19 2.43 6 17 2.44 8 15 2.47 1 12 2.47 10 18 2.50 3 12 2.51 13 20 2.54 15 17 2.55 3 4 2.59 11 15 2.60 2 10 2.60 2 4 2.60 3 10 2.61 3 17 2.61 10 14 2.62 11 16 2.63 18 20 2.63 1 16 2.63 2 14 2.63 1 13 2.64 6 15 2.65 1 8 2.66 2 17 2.66 15 20 2.70 10 12 2.73 6 8 2.74 3 15 2.74 8 18 2.74 14 15 2.78 6 20 2.79 12 18 2.80 1 4 2.81 10 17 2.82 5 9 2.82 5 12 2.83 1 18 2.85 15 17 2.86 8 9 2.87 13 14 2.88 7 20 2.91 14 16 2.91 13 13 2.91 4 13 2.92 4 7 2.93 10 19 2.96 12 16 2.99 14 20 2.99 2 16 3.00 7 13 3.00 Time profile in seconds ----------------------- 0.22: 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. 1.27: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.05: Generate idealized H-atoms 2.44: Structure factors and derivatives 4.70: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.09: Apply other restraints 0.44: Solve l.s. equations 0.00: Generate HTAB table 0.11: Other dependent quantities, CIF, tables 0.59: Analysis of variance 0.17: Merge reflections for Fourier and .fcf 0.16: Fourier summations 0.17: Peaksearch 0.05: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:19:10 Total elapsed time: 10.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++