+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0064 started at 10:12:54 on 02-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0064 in P2(1) CELL 0.71073 6.2194 7.6717 13.7114 90.000 101.551 90.000 ZERR 2.00 0.0002 0.0002 0.0005 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O S UNIT 26 28 8 2 2 V = 640.97 F(000) = 288.0 Mu = 0.25 mm-1 Cell Wt = 548.68 Rho = 1.421 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.03 0.06 0.10 ACTA HTAB 2.00000 BOND $H WGHT 0.02430 0.27210 L.S. 4 TEMP -153.00 FVAR 1.06806 MOLE 1 C2 1 0.831416 0.660869 0.748699 11.00000 0.04150 0.02954 = 0.02839 0.00422 0.01371 0.00164 AFIX 43 H2 2 0.756246 0.597229 0.791030 11.00000 -1.20000 AFIX 0 C3 1 1.046712 0.708937 0.785233 11.00000 0.04431 0.02458 = 0.02132 0.00206 0.00670 0.00709 AFIX 43 H3 2 1.120330 0.680826 0.850934 11.00000 -1.20000 AFIX 0 C4 1 1.148076 0.800299 0.720338 11.00000 0.03349 0.02360 = 0.02402 -0.00350 0.00456 -0.00019 AFIX 43 H4 2 1.296445 0.835003 0.742525 11.00000 -1.20000 AFIX 0 C6 1 0.837604 0.789813 0.599894 11.00000 0.02767 0.01477 = 0.02289 -0.00379 0.00871 0.00008 C8 1 0.843065 0.913348 0.433580 11.00000 0.02878 0.02124 = 0.01864 0.00189 0.00352 -0.00762 AFIX 23 H8A 2 0.991393 0.951643 0.467275 11.00000 -1.20000 H8B 2 0.761263 1.017158 0.403390 11.00000 -1.20000 AFIX 0 C9 1 0.862976 0.783039 0.352156 11.00000 0.01673 0.02183 = 0.01821 0.00487 0.00172 -0.00208 AFIX 23 H9A 2 0.925600 0.841434 0.299782 11.00000 -1.20000 H9B 2 0.963112 0.687392 0.380460 11.00000 -1.20000 AFIX 0 C11 1 0.533474 0.635204 0.382942 11.00000 0.01968 0.01861 = 0.02148 0.00150 0.00390 -0.00498 AFIX 23 H11A 2 0.617318 0.533307 0.414524 11.00000 -1.20000 H11B 2 0.385639 0.594632 0.349981 11.00000 -1.20000 AFIX 0 C12 1 0.512781 0.769675 0.462175 11.00000 0.02122 0.02385 = 0.02291 0.00144 0.00687 -0.00155 AFIX 23 H12A 2 0.417247 0.866578 0.431791 11.00000 -1.20000 H12B 2 0.444976 0.715385 0.514175 11.00000 -1.20000 AFIX 0 C13 1 0.526303 0.746525 0.216974 11.00000 0.01932 0.01859 = 0.01912 -0.00264 0.00317 0.00002 C14 1 0.641396 0.802301 0.137580 11.00000 0.01736 0.02305 = 0.01707 -0.00135 0.00009 0.00066 C15 1 0.840447 0.755094 0.118151 11.00000 0.01990 0.02371 = 0.02120 -0.00083 0.00094 0.00064 AFIX 43 H15 2 0.939827 0.679040 0.159413 11.00000 -1.20000 AFIX 0 C16 1 0.882855 0.831857 0.029707 11.00000 0.02098 0.03531 = 0.01972 -0.00528 0.00536 -0.00262 AFIX 43 H16 2 1.013705 0.813110 0.005413 11.00000 -1.20000 AFIX 0 C17 1 0.715777 0.934967 -0.016276 11.00000 0.02727 0.03399 = 0.02015 0.00394 0.00531 -0.00563 AFIX 43 H17 2 0.716910 0.997680 -0.075914 11.00000 -1.20000 AFIX 0 N1 3 0.723568 0.699552 0.656613 11.00000 0.03688 0.02541 = 0.02350 0.00359 0.01004 -0.00209 N5 3 1.048017 0.842181 0.628123 11.00000 0.02867 0.02104 = 0.02309 0.00005 0.00360 0.00041 N7 3 0.729546 0.836766 0.506760 11.00000 0.02578 0.02372 = 0.01976 -0.00090 0.00784 -0.00555 N10 3 0.645907 0.711268 0.308461 11.00000 0.01787 0.02121 = 0.02011 0.00127 0.00228 -0.00331 O19 4 0.325307 0.724710 0.196427 11.00000 0.01563 0.04638 = 0.02437 0.00176 0.00377 -0.00014 S18 5 0.502518 0.938889 0.045745 11.00000 0.02195 0.03283 = 0.02237 0.00470 0.00180 0.00448 HKLF 4 Covalent radii and connectivity table for 2009src0064 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C2 - N1 C3 C3 - C4 C2 C4 - N5 C3 C6 - N1 N5 N7 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C13 - O19 N10 C14 C14 - C15 C13 S18 C15 - C14 C16 C16 - C17 C15 C17 - C16 S18 N1 - C2 C6 N5 - C4 C6 N7 - C6 C12 C8 N10 - C13 C11 C9 O19 - C13 S18 - C17 C14 Floating origin restraints generated 7652 Reflections read, of which 26 rejected -8 =< h =< 7, -9 =< k =< 9, -17 =< l =< 17, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2712 Unique reflections, of which 0 suppressed R(int) = 0.0345 R(sigma) = 0.0432 Friedel opposites not merged Maximum memory for data reduction = 1788 / 27048 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 = 2272 / 215023 wR2 = 0.0833 before cycle 1 for 2712 data and 172 / 172 parameters GooF = S = 1.082; Restrained GooF = 1.082 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.06805 0.00166 -0.007 OSF Mean shift/su = 0.004 Maximum = -0.020 for U13 S18 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2272 / 215023 wR2 = 0.0833 before cycle 2 for 2712 data and 172 / 172 parameters GooF = S = 1.082; Restrained GooF = 1.082 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.06804 0.00166 -0.003 OSF Mean shift/su = 0.001 Maximum = -0.007 for U13 S18 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2272 / 215023 wR2 = 0.0833 before cycle 3 for 2712 data and 172 / 172 parameters GooF = S = 1.082; Restrained GooF = 1.082 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.06804 0.00166 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H12B Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2272 / 215023 wR2 = 0.0833 before cycle 4 for 2712 data and 172 / 172 parameters GooF = S = 1.082; Restrained GooF = 1.082 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.06804 0.00166 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for N5 Max. dU = 0.000 for O19 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 H2 0.7562 0.5972 0.7910 43 0.950 0.000 C2 N1 C3 H3 1.1203 0.6808 0.8509 43 0.950 0.000 C3 C4 C2 H4 1.2964 0.8350 0.7425 43 0.950 0.000 C4 N5 C3 H8A 0.9914 0.9516 0.4673 23 0.990 0.000 C8 N7 C9 H8B 0.7613 1.0172 0.4034 23 0.990 0.000 C8 N7 C9 H9A 0.9256 0.8414 0.2998 23 0.990 0.000 C9 N10 C8 H9B 0.9631 0.6874 0.3805 23 0.990 0.000 C9 N10 C8 H11A 0.6173 0.5333 0.4145 23 0.990 0.000 C11 N10 C12 H11B 0.3856 0.5946 0.3500 23 0.990 0.000 C11 N10 C12 H12A 0.4172 0.8666 0.4318 23 0.990 0.000 C12 N7 C11 H12B 0.4450 0.7154 0.5142 23 0.990 0.000 C12 N7 C11 H15 0.9398 0.6790 0.1594 43 0.950 0.000 C15 C14 C16 H16 1.0137 0.8131 0.0054 43 0.950 0.000 C16 C17 C15 H17 0.7169 0.9977 -0.0759 43 0.950 0.000 C17 C16 S18 2009src0064 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.83141 0.66087 0.74870 1.00000 0.04151 0.02953 0.02839 0.00422 0.01372 0.00164 0.03221 0.00485 0.00042 0.00033 0.00019 0.00000 0.00147 0.00136 0.00131 0.00105 0.00108 0.00109 0.00056 H2 0.75624 0.59723 0.79103 1.00000 0.03865 0.00000 0.00000 C3 1.04671 0.70894 0.78523 1.00000 0.04429 0.02457 0.02131 0.00206 0.00670 0.00708 0.03004 0.00466 0.00042 0.00031 0.00017 0.00000 0.00141 0.00125 0.00117 0.00101 0.00099 0.00108 0.00054 H3 1.12033 0.68083 0.85093 1.00000 0.03605 0.00000 0.00000 C4 1.14807 0.80030 0.72034 1.00000 0.03349 0.02359 0.02402 -0.00350 0.00455 -0.00018 0.02720 0.00433 0.00040 0.00030 0.00017 0.00000 0.00125 0.00123 0.00115 0.00097 0.00095 0.00099 0.00051 H4 1.29644 0.83500 0.74253 1.00000 0.03264 0.00000 0.00000 C6 0.83760 0.78981 0.59989 1.00000 0.02767 0.01476 0.02289 -0.00379 0.00871 0.00008 0.02127 0.00404 0.00036 0.00028 0.00016 0.00000 0.00111 0.00102 0.00110 0.00084 0.00087 0.00083 0.00045 C8 0.84306 0.91335 0.43358 1.00000 0.02877 0.02124 0.01864 0.00188 0.00353 -0.00761 0.02305 0.00391 0.00035 0.00030 0.00015 0.00000 0.00106 0.00123 0.00101 0.00092 0.00081 0.00095 0.00048 H8A 0.99139 0.95165 0.46727 1.00000 0.02766 0.00000 0.00000 H8B 0.76126 1.01716 0.40339 1.00000 0.02766 0.00000 0.00000 C9 0.86298 0.78304 0.35216 1.00000 0.01672 0.02183 0.01821 0.00487 0.00172 -0.00209 0.01917 0.00379 0.00033 0.00028 0.00015 0.00000 0.00096 0.00109 0.00103 0.00086 0.00077 0.00082 0.00044 H9A 0.92560 0.84143 0.29978 1.00000 0.02300 0.00000 0.00000 H9B 0.96311 0.68739 0.38046 1.00000 0.02300 0.00000 0.00000 C11 0.53347 0.63521 0.38294 1.00000 0.01968 0.01861 0.02148 0.00150 0.00390 -0.00498 0.01996 0.00392 0.00035 0.00028 0.00016 0.00000 0.00102 0.00106 0.00108 0.00085 0.00081 0.00082 0.00044 H11A 0.61732 0.53331 0.41452 1.00000 0.02395 0.00000 0.00000 H11B 0.38564 0.59463 0.34998 1.00000 0.02395 0.00000 0.00000 C12 0.51278 0.76967 0.46217 1.00000 0.02121 0.02385 0.02291 0.00144 0.00686 -0.00155 0.02232 0.00400 0.00033 0.00030 0.00016 0.00000 0.00107 0.00117 0.00113 0.00092 0.00085 0.00089 0.00047 H12A 0.41724 0.86657 0.43179 1.00000 0.02678 0.00000 0.00000 H12B 0.44498 0.71538 0.51417 1.00000 0.02678 0.00000 0.00000 C13 0.52630 0.74652 0.21697 1.00000 0.01932 0.01859 0.01911 -0.00264 0.00317 0.00002 0.01910 0.00383 0.00033 0.00028 0.00016 0.00000 0.00102 0.00107 0.00105 0.00084 0.00078 0.00084 0.00044 C14 0.64140 0.80230 0.13758 1.00000 0.01735 0.02304 0.01706 -0.00135 0.00009 0.00066 0.01962 0.00379 0.00033 0.00028 0.00015 0.00000 0.00097 0.00114 0.00100 0.00086 0.00077 0.00082 0.00044 C15 0.84044 0.75509 0.11815 1.00000 0.01989 0.02371 0.02120 -0.00084 0.00093 0.00064 0.02204 0.00395 0.00034 0.00030 0.00016 0.00000 0.00101 0.00114 0.00109 0.00088 0.00081 0.00088 0.00046 H15 0.93982 0.67904 0.15941 1.00000 0.02645 0.00000 0.00000 C16 0.88286 0.83186 0.02971 1.00000 0.02097 0.03531 0.01972 -0.00528 0.00536 -0.00263 0.02515 0.00403 0.00035 0.00033 0.00016 0.00000 0.00107 0.00132 0.00108 0.00104 0.00085 0.00097 0.00049 H16 1.01371 0.81311 0.00542 1.00000 0.03018 0.00000 0.00000 C17 0.71578 0.93496 -0.01628 1.00000 0.02727 0.03399 0.02015 0.00394 0.00532 -0.00563 0.02706 0.00428 0.00033 0.00039 0.00015 0.00000 0.00104 0.00120 0.00100 0.00122 0.00080 0.00119 0.00046 H17 0.71691 0.99768 -0.07591 1.00000 0.03247 0.00000 0.00000 N1 0.72357 0.69955 0.65661 1.00000 0.03687 0.02541 0.02350 0.00359 0.01004 -0.00209 0.02804 0.00365 0.00032 0.00026 0.00014 0.00000 0.00113 0.00104 0.00100 0.00086 0.00084 0.00087 0.00045 N5 1.04802 0.84218 0.62812 1.00000 0.02866 0.02104 0.02309 0.00004 0.00360 0.00040 0.02448 0.00352 0.00030 0.00026 0.00014 0.00000 0.00100 0.00094 0.00095 0.00081 0.00077 0.00081 0.00041 N7 0.72955 0.83677 0.50676 1.00000 0.02578 0.02372 0.01975 -0.00090 0.00784 -0.00555 0.02263 0.00336 0.00029 0.00025 0.00013 0.00000 0.00095 0.00100 0.00091 0.00082 0.00073 0.00080 0.00040 N10 0.64591 0.71127 0.30846 1.00000 0.01787 0.02121 0.02011 0.00127 0.00228 -0.00331 0.01994 0.00314 0.00027 0.00023 0.00013 0.00000 0.00085 0.00095 0.00090 0.00076 0.00068 0.00071 0.00038 O19 0.32531 0.72471 0.19643 1.00000 0.01562 0.04637 0.02437 0.00176 0.00376 -0.00014 0.02882 0.00295 0.00023 0.00024 0.00012 0.00000 0.00075 0.00108 0.00084 0.00076 0.00060 0.00070 0.00039 S18 0.50252 0.93889 0.04575 1.00000 0.02195 0.03283 0.02237 0.00470 0.00180 0.00448 0.02609 0.00102 0.00008 0.00008 0.00004 0.00000 0.00025 0.00031 0.00026 0.00027 0.00019 0.00025 0.00014 Final Structure Factor Calculation for 2009src0064 in P2(1) Total number of l.s. parameters = 172 Maximum vector length = 511 Memory required = 2102 / 26068 wR2 = 0.0833 before cycle 5 for 2712 data and 2 / 172 parameters GooF = S = 1.082; Restrained GooF = 1.082 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0243 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0375 for 2523 Fo > 4sig(Fo) and 0.0419 for all 2712 data wR2 = 0.0833, GooF = S = 1.082, Restrained GooF = 1.082 for all data Flack x parameter = 0.1389 with su 0.0775 Expected values are 0 (within 3 su's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0438 0.0306 0.0223 C2 0.0467 0.0231 0.0203 C3 0.0340 0.0273 0.0203 C4 0.0292 0.0218 0.0128 C6 0.0344 0.0193 0.0155 C8 0.0267 0.0160 0.0148 C9 0.0251 0.0211 0.0137 C11 0.0249 0.0241 0.0179 C12 0.0218 0.0193 0.0162 C13 0.0240 0.0205 0.0144 C14 0.0254 0.0229 0.0178 C15 0.0372 0.0205 0.0178 C16 0.0383 0.0249 0.0179 C17 0.0375 0.0281 0.0185 N1 0.0295 0.0229 0.0210 N5 0.0307 0.0205 0.0166 N7 0.0247 0.0193 0.0158 N10 0.0465 0.0244 0.0156 O19 0.0352 0.0255 0.0176 S18 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.042 0.055 0.066 0.079 0.094 0.112 0.140 0.188 1.000 Number in group 271. 293. 265. 267. 260. 274. 269. 278. 263. 272. GooF 1.098 1.128 1.174 1.056 0.988 1.157 1.073 0.920 1.042 1.155 K 1.221 0.991 1.002 1.006 1.003 0.999 1.010 1.001 1.012 0.995 Resolution(A) 0.77 0.81 0.85 0.89 0.94 0.99 1.07 1.18 1.36 1.71 inf Number in group 273. 270. 277. 266. 271. 270. 278. 268. 268. 271. GooF 1.216 1.159 1.048 1.045 1.047 0.961 0.958 0.832 1.096 1.368 K 1.021 1.042 1.024 1.013 1.001 0.996 1.000 1.003 1.015 0.989 R1 0.106 0.087 0.067 0.061 0.050 0.039 0.029 0.022 0.027 0.024 Recommended weighting scheme: WGHT 0.0243 0.2725 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)/su Fc/Fc(max) Resolution(A) 3 0 1 748.40 639.94 4.08 0.262 1.95 -7 -3 8 31.59 60.76 4.01 0.081 0.80 1 6 8 10.60 22.89 3.58 0.050 0.98 -2 -2 5 557.89 479.23 3.55 0.227 1.94 5 -7 2 61.87 37.03 3.47 0.063 0.80 -2 0 3 2.73 0.12 3.35 0.004 2.79 -6 -5 2 36.84 58.61 3.32 0.079 0.86 -3 3 10 9.57 19.88 3.28 0.046 1.12 2 0 0 72.14 90.50 3.24 0.098 3.05 6 -2 7 13.41 24.38 3.18 0.051 0.81 0 0 8 29.46 19.63 3.11 0.046 1.68 2 -2 2 366.93 319.94 3.10 0.185 2.14 5 -2 8 2.24 8.96 3.10 0.031 0.88 -2 -9 5 13.93 30.13 3.09 0.057 0.80 -2 2 5 541.40 478.28 3.05 0.226 1.94 4 1 0 283.14 242.48 2.99 0.161 1.49 1 -7 7 29.44 42.78 2.93 0.068 0.93 2 -2 15 21.05 7.70 2.92 0.029 0.80 5 1 10 9.20 18.33 2.89 0.044 0.82 0 -4 15 106.02 75.71 2.86 0.090 0.81 -2 7 6 66.84 93.78 2.82 0.100 0.96 -1 0 1 1049.47 1164.95 2.81 0.353 6.02 3 -8 4 11.70 3.86 2.79 0.020 0.82 -7 0 4 17.16 2.42 2.78 0.016 0.89 2 -3 0 11.43 6.54 2.78 0.026 1.96 -4 3 7 4.34 9.40 2.77 0.032 1.18 2 3 0 12.29 6.59 2.73 0.027 1.96 -5 -3 2 6.04 11.83 2.73 0.036 1.12 -5 -6 8 14.68 24.90 2.72 0.052 0.83 -4 7 7 29.35 16.38 2.68 0.042 0.85 -1 5 12 3.61 11.08 2.68 0.034 0.92 4 0 0 53.40 67.85 2.66 0.085 1.52 -3 2 6 41.90 31.85 2.63 0.058 1.54 -1 -1 4 192.69 221.66 2.61 0.154 2.97 2 0 5 248.97 218.09 2.60 0.153 1.84 1 -2 16 2.01 10.41 2.60 0.033 0.79 -5 2 10 76.43 58.93 2.59 0.079 0.98 4 -7 6 29.46 17.87 2.55 0.044 0.80 2 1 0 29.07 38.20 2.55 0.064 2.83 2 -1 0 28.87 38.02 2.55 0.064 2.83 0 -1 16 83.63 62.37 2.52 0.082 0.83 2 4 1 64.09 79.31 2.51 0.092 1.59 -4 -5 10 3.69 8.49 2.49 0.030 0.91 2 3 10 63.70 49.39 2.48 0.073 1.05 -6 -6 4 0.93 5.85 2.47 0.025 0.80 -1 -1 6 50.10 62.60 2.46 0.082 2.16 2 2 2 362.45 326.53 2.45 0.187 2.14 2 -5 10 24.55 35.63 2.44 0.062 0.92 3 -3 13 6.66 13.10 2.44 0.037 0.81 -4 -6 8 67.38 88.04 2.43 0.097 0.90 Bond lengths and angles C2 - Distance Angles N1 1.3390 (0.0031) C3 1.3825 (0.0037) 123.27 (0.23) H2 0.9500 118.37 118.37 C2 - N1 C3 C3 - Distance Angles C4 1.3802 (0.0034) C2 1.3825 (0.0037) 115.86 (0.22) H3 0.9500 122.07 122.07 C3 - C4 C2 C4 - Distance Angles N5 1.3319 (0.0029) C3 1.3802 (0.0034) 123.20 (0.22) H4 0.9500 118.40 118.40 C4 - N5 C3 C6 - Distance Angles N1 1.3447 (0.0029) N5 1.3494 (0.0028) 125.52 (0.21) N7 1.3669 (0.0028) 117.29 (0.19) 117.17 (0.19) C6 - N1 N5 C8 - Distance Angles N7 1.4609 (0.0026) C9 1.5220 (0.0031) 111.17 (0.17) H8A 0.9900 109.40 109.40 H8B 0.9900 109.40 109.40 108.01 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4700 (0.0026) C8 1.5220 (0.0031) 110.00 (0.17) H9A 0.9900 109.66 109.66 H9B 0.9900 109.66 109.66 108.17 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4691 (0.0027) C12 1.5222 (0.0031) 110.30 (0.17) H11A 0.9900 109.59 109.59 H11B 0.9900 109.59 109.59 108.13 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4581 (0.0027) C11 1.5222 (0.0031) 109.59 (0.17) H12A 0.9900 109.75 109.75 H12B 0.9900 109.75 109.75 108.22 C12 - N7 C11 H12A C13 - Distance Angles O19 1.2365 (0.0025) N10 1.3514 (0.0026) 121.86 (0.20) C14 1.4807 (0.0030) 119.15 (0.19) 118.88 (0.17) C13 - O19 N10 C14 - Distance Angles C15 1.3663 (0.0031) C13 1.4807 (0.0030) 131.07 (0.20) S18 1.7303 (0.0021) 111.00 (0.17) 117.75 (0.15) C14 - C15 C13 C15 - Distance Angles C14 1.3663 (0.0031) C16 1.4195 (0.0031) 112.78 (0.20) H15 0.9500 123.61 123.61 C15 - C14 C16 C16 - Distance Angles C17 1.3567 (0.0034) C15 1.4195 (0.0031) 112.51 (0.19) H16 0.9500 123.75 123.75 C16 - C17 C15 C17 - Distance Angles C16 1.3567 (0.0034) S18 1.7132 (0.0021) 112.12 (0.17) H17 0.9500 123.94 123.94 C17 - C16 S18 N1 - Distance Angles C2 1.3390 (0.0031) C6 1.3447 (0.0029) 115.90 (0.20) N1 - C2 N5 - Distance Angles C4 1.3319 (0.0029) C6 1.3494 (0.0028) 116.26 (0.20) N5 - C4 N7 - Distance Angles C6 1.3669 (0.0028) C12 1.4581 (0.0027) 122.62 (0.18) C8 1.4609 (0.0026) 122.20 (0.17) 112.79 (0.17) N7 - C6 C12 N10 - Distance Angles C13 1.3514 (0.0026) C11 1.4691 (0.0027) 118.33 (0.17) C9 1.4700 (0.0026) 126.39 (0.17) 113.05 (0.16) N10 - C13 C11 O19 - Distance Angles C13 1.2365 (0.0025) O19 - S18 - Distance Angles C17 1.7132 (0.0021) C14 1.7303 (0.0021) 91.57 (0.11) S18 - C17 FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0398 for 1558 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.18 at 0.2188 0.9422 0.2180 [ 1.21 A from H2 ] Deepest hole -0.21 at 0.4580 0.5195 0.9796 [ 0.77 A from S18 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2155 / 17876 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7812 0.4422 0.7820 1.00000 0.05 0.18 1.21 H2 1.78 C2 1.84 O19 2.43 C13 Q2 1 0.9606 1.0477 -0.0714 1.00000 0.05 0.18 1.55 H17 1.78 H15 2.02 C17 2.08 H16 Q3 1 0.1949 0.6955 0.2429 1.00000 0.05 0.18 1.15 O19 1.77 H15 1.86 H11B 2.20 C13 Q4 1 0.7508 0.7638 0.1349 1.00000 0.05 0.17 0.65 C15 0.75 C14 1.33 H15 1.87 C16 Q5 1 0.9836 0.7080 -0.0574 1.00000 0.05 0.17 1.17 H16 1.67 H3 1.74 C16 2.27 C3 Q6 1 0.8155 0.5144 0.8591 1.00000 0.05 0.17 1.13 H2 1.90 C2 2.31 H3 2.43 C3 Q7 1 0.7800 1.0834 0.5203 1.00000 0.05 0.16 1.66 H8B 1.72 H12B 1.86 C8 1.91 H8A Q8 1 1.0943 0.6998 0.5660 1.00000 0.05 0.16 1.45 N5 1.67 H8B 1.88 C6 2.00 H8A Q9 1 0.7968 0.5541 0.4331 1.00000 0.05 0.16 1.11 H11A 1.71 H9B 1.76 C11 1.87 H8A Q10 1 0.6126 0.7641 0.7779 1.00000 0.05 0.16 1.55 H2 1.69 C2 1.99 N1 2.00 H4 Shortest distances between peaks (including symmetry equivalents) 1 6 1.17 7 8 1.78 1 3 1.93 5 6 2.03 2 5 2.12 6 10 2.44 8 9 2.58 7 9 2.59 2 5 2.61 2 3 2.62 1 10 2.68 2 4 2.71 8 9 2.80 3 6 2.81 3 4 2.91 5 10 2.92 2 6 2.98 Time profile in seconds ----------------------- 0.02: 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. 0.38: 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 0.53: Structure factors and derivatives 0.53: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0064 finished at 10:12:56 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++