+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0112 started at 09:56:16 on 20-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0112 in P2(1)/n CELL 0.71073 10.5278 5.3937 27.1476 90.000 94.292 90.000 ZERR 4.00 0.0005 0.0002 0.0014 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 64 92 16 4 V = 1537.22 F(000) = 620.0 Mu = 0.08 mm-1 Cell Wt = 1149.54 Rho = 1.242 MERG 2 OMIT -3.00 55.00 OMIT 11 0 11 SHEL 7 0.77 DFIX 0.89 0.02 N3 H3a N3 H3b EQIV_$1 x-1, y+1, z HTAB N3 O12_$1 FMAP 2 PLAN 10 SIZE 0.05 0.15 0.18 ACTA BOND $H WGHT 0.03150 2.23270 L.S. 4 TEMP -153.00 FVAR 0.59912 0.54570 PART 1 C14A 1 0.696338 -0.281746 0.078383 21.00000 0.01756 0.04094 = 0.03201 0.00398 0.00239 -0.00161 C15A 1 0.834722 -0.350885 0.074716 21.00000 0.03129 0.03892 = 0.02927 0.00228 0.00520 0.00581 AFIX 23 H15A 2 0.843063 -0.533487 0.073156 21.00000 -1.20000 H15B 2 0.886118 -0.291503 0.104415 21.00000 -1.20000 AFIX 0 C16A 1 0.884322 -0.234133 0.028352 21.00000 0.03289 0.04002 = 0.04714 0.00073 0.01622 0.00223 AFIX 23 H16A 2 0.879600 -0.051296 0.030849 21.00000 -1.20000 H16B 2 0.974767 -0.280418 0.026288 21.00000 -1.20000 AFIX 0 C17A 1 0.807685 -0.318886 -0.018138 21.00000 0.03953 0.04993 = 0.02515 0.00584 0.00871 0.00676 AFIX 23 H17A 2 0.818756 -0.499695 -0.022406 21.00000 -1.20000 H17B 2 0.839351 -0.234414 -0.047190 21.00000 -1.20000 AFIX 0 C18A 1 0.664858 -0.259385 -0.015066 21.00000 0.03921 0.04866 = 0.02652 0.00499 0.00485 0.00484 AFIX 23 H18A 2 0.652706 -0.077387 -0.015935 21.00000 -1.20000 H18B 2 0.615664 -0.330732 -0.044189 21.00000 -1.20000 AFIX 0 C19A 1 0.613346 -0.363487 0.032243 21.00000 0.02626 0.04589 = 0.02922 0.01191 0.00255 -0.00180 AFIX 23 H19A 2 0.524983 -0.304652 0.034736 21.00000 -1.20000 H19B 2 0.611607 -0.546813 0.030533 21.00000 -1.20000 AFIX 0 PART 2 C14B 1 0.662268 -0.331535 0.063163 -21.00000 0.01035 0.02768 = 0.03126 0.00626 0.00297 0.00272 C15B 1 0.758052 -0.119762 0.069397 -21.00000 0.03849 0.01715 = 0.03229 -0.00088 0.00586 -0.00500 AFIX 23 H15C 2 0.830111 -0.171437 0.092653 -21.00000 -1.20000 H15D 2 0.716734 0.025097 0.083890 -21.00000 -1.20000 AFIX 0 C16B 1 0.809615 -0.043137 0.019766 -21.00000 0.03879 0.02794 = 0.03520 0.00376 0.01446 -0.00392 AFIX 23 H16C 2 0.739435 0.027929 -0.002119 -21.00000 -1.20000 H16D 2 0.875551 0.086419 0.025821 -21.00000 -1.20000 AFIX 0 C17B 1 0.866663 -0.263725 -0.005754 -21.00000 0.03039 0.04096 = 0.03235 -0.01027 0.01005 -0.00285 AFIX 23 H17C 2 0.943919 -0.320715 0.014069 -21.00000 -1.20000 H17D 2 0.892291 -0.211745 -0.038551 -21.00000 -1.20000 AFIX 0 C18B 1 0.771595 -0.477976 -0.012183 -21.00000 0.02636 0.03637 = 0.03515 -0.01292 0.00649 -0.00111 AFIX 23 H18C 2 0.698269 -0.426784 -0.034863 -21.00000 -1.20000 H18D 2 0.812973 -0.621516 -0.027123 -21.00000 -1.20000 AFIX 0 C19B 1 0.724402 -0.554087 0.037338 -21.00000 0.03062 0.01956 = 0.03614 -0.00455 0.00402 -0.00149 AFIX 23 H19C 2 0.796824 -0.618062 0.059034 -21.00000 -1.20000 H19D 2 0.661173 -0.689174 0.032087 -21.00000 -1.20000 AFIX 0 MOLE 1 PART 0 C2 1 -0.017590 0.112304 0.168172 11.00000 0.03252 0.03414 = 0.04729 -0.00336 0.01237 0.00162 AFIX 43 H2 2 -0.057283 0.257321 0.154417 11.00000 -1.20000 AFIX 0 C3 1 -0.087703 -0.038330 0.196842 11.00000 0.02699 0.03859 = 0.03223 -0.00757 0.00822 -0.00227 C4 1 -0.029410 -0.253294 0.214008 11.00000 0.03613 0.04216 = 0.05543 0.00988 0.02028 0.00151 AFIX 43 H4 2 -0.075071 -0.367453 0.232641 11.00000 -1.20000 AFIX 0 C5 1 0.095133 -0.304550 0.204359 11.00000 0.03442 0.03887 = 0.05518 0.00463 0.01732 0.00362 AFIX 43 H5 2 0.135097 -0.453138 0.216206 11.00000 -1.20000 AFIX 0 C6 1 0.160691 -0.136705 0.177247 11.00000 0.02817 0.03242 = 0.03931 -0.01079 0.01224 -0.00312 C8 1 0.352837 -0.392826 0.186113 11.00000 0.02956 0.06232 = 0.03311 0.00594 0.01085 0.00549 AFIX 23 H8A 2 0.323143 -0.530221 0.163971 11.00000 -1.20000 H8B 2 0.329172 -0.432471 0.219837 11.00000 -1.20000 AFIX 0 C9 1 0.496512 -0.369816 0.186363 11.00000 0.03180 0.08795 = 0.03425 -0.01393 0.00837 0.00273 AFIX 23 H9A 2 0.527315 -0.247929 0.211783 11.00000 -1.20000 H9B 2 0.536225 -0.531871 0.195089 11.00000 -1.20000 AFIX 0 C11 1 0.472101 -0.063403 0.121343 11.00000 0.04941 0.03136 = 0.12149 0.00655 0.05233 0.00549 AFIX 23 H11A 2 0.495256 -0.025214 0.087488 11.00000 -1.20000 H11B 2 0.501316 0.075545 0.143170 11.00000 -1.20000 AFIX 0 C12 1 0.328420 -0.090014 0.121426 11.00000 0.04319 0.03330 = 0.06658 0.01246 0.03190 0.01083 AFIX 23 H12A 2 0.287496 0.070183 0.112090 11.00000 -1.20000 H12B 2 0.298299 -0.215051 0.096530 11.00000 -1.20000 AFIX 0 C13 1 0.634227 -0.405439 0.118970 11.00000 0.03694 0.03003 = 0.05430 0.00421 0.02004 0.00120 N1 3 0.103993 0.066587 0.158419 11.00000 0.03842 0.03229 = 0.05786 -0.00437 0.02176 -0.00115 N3 3 -0.209717 0.030001 0.209773 11.00000 0.02630 0.04815 = 0.04272 0.00572 0.00864 0.00342 N7 3 0.291127 -0.164688 0.169514 11.00000 0.02786 0.03818 = 0.04553 -0.00928 0.01450 -0.00269 N10 3 0.534685 -0.291145 0.138457 11.00000 0.03382 0.03637 = 0.05702 -0.00402 0.02000 -0.00003 O12 4 0.685286 -0.588438 0.138632 11.00000 0.04214 0.04174 = 0.04383 0.00969 0.01482 0.00667 H3A 2 -0.247160 0.140146 0.189047 11.00000 0.04200 H3B 2 -0.255154 -0.100895 0.219501 11.00000 0.05516 HKLF 4 Covalent radii and connectivity table for 2009src0112 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C14A_a - C13 C15A_a C19A_a C15A_a - C14A_a C16A_a C16A_a - C17A_a C15A_a C17A_a - C16A_a C18A_a C18A_a - C19A_a C17A_a C19A_a - C14A_a C18A_a C14B_b - C15B_b C19B_b C13 C15B_b - C14B_b C16B_b C16B_b - C17B_b C15B_b C17B_b - C16B_b C18B_b C18B_b - C19B_b C17B_b C19B_b - C18B_b C14B_b C2 - N1 C3 C3 - C4 C2 N3 C4 - C3 C5 C5 - C6 C4 C6 - N1 C5 N7 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C13 - O12 N10 C14A_a C14B_b N1 - C6 C2 N3 - C3 N7 - C6 C8 C12 N10 - C13 C9 C11 O12 - C13 Operators for generating equivalent atoms: $1 x-1, y+1, z h k l Fo^2 Sigma Why rejected -5 0 2 6.19 1.34 observed but should be systematically absent -5 0 2 6.61 1.20 observed but should be systematically absent -7 0 14 15.14 3.41 observed but should be systematically absent 15554 Reflections read, of which 999 rejected -13 =< h =< 13, -6 =< k =< 6, -35 =< l =< 34, Max. 2-theta = 54.97 3 Systematic absence violations 0 Inconsistent equivalents 3462 Unique reflections, of which 0 suppressed R(int) = 0.0464 R(sigma) = 0.0484 Friedel opposites merged Maximum memory for data reduction = 2990 / 34324 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 = 3762 / 314198 wR2 = 0.1734 before cycle 1 for 3462 data and 253 / 253 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0315 * P )^2 + 2.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.59915 0.00163 0.017 OSF 2 0.54569 0.00340 -0.002 FVAR 2 Mean shift/su = 0.005 Maximum = 0.017 for OSF Max. shift = 0.000 A for H3A Max. dU = 0.000 for H3B Least-squares cycle 2 Maximum vector length = 511 Memory required = 3762 / 314198 wR2 = 0.1734 before cycle 2 for 3462 data and 253 / 253 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0315 * P )^2 + 2.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.59916 0.00162 0.009 OSF 2 0.54569 0.00340 -0.001 FVAR 2 Mean shift/su = 0.002 Maximum = 0.009 for OSF Max. shift = 0.000 A for H3A Max. dU = 0.000 for H3B Least-squares cycle 3 Maximum vector length = 511 Memory required = 3762 / 314198 wR2 = 0.1734 before cycle 3 for 3462 data and 253 / 253 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0315 * P )^2 + 2.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.59916 0.00163 0.001 OSF 2 0.54569 0.00340 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.001 for U11 C8 Max. shift = 0.000 A for H3A Max. dU = 0.000 for C14B_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 3762 / 314198 wR2 = 0.1734 before cycle 4 for 3462 data and 253 / 253 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0315 * P )^2 + 2.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.59916 0.00163 0.000 OSF 2 0.54569 0.00340 0.000 FVAR 2 Mean shift/su = 0.000 Maximum = 0.000 for U23 C9 Max. shift = 0.000 A for H3A Max. dU = 0.000 for H3B Largest correlation matrix elements -0.762 U33 C14B_b / z C14A_a 0.596 x C14B_b / z C14A_a 0.538 U23 C14B_b / U22 C14A_a -0.705 U11 C14B_b / x C14A_a -0.579 y C14B_b / y C14A_a 0.533 U11 C17B_b / U11 C17A_a 0.700 y C14B_b / U22 C14A_a 0.577 z C14B_b / U33 C14A_a 0.527 U22 C14B_b / U12 C14A_a 0.691 x C14B_b / U11 C14A_a -0.574 U33 C14A_a / z C14A_a 0.521 U13 C11 / U11 C11 0.690 U33 C14B_b / U33 C14A_a 0.559 U33 C17B_b / U13 C17A_a 0.516 U22 C14B_b / y C14B_b -0.681 U22 C14B_b / y C14A_a 0.555 U12 C14B_b / U22 C14A_a 0.509 z C14B_b / x C14A_a 0.656 U11 C14B_b / U11 C14A_a 0.548 U13 C11 / U33 C11 0.507 U12 C17B_b / U22 C17A_a Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H15A 0.8431 -0.5335 0.0732 23 0.990 0.000 C15A_a C14A_a C16A_a H15B 0.8861 -0.2915 0.1044 23 0.990 0.000 C15A_a C14A_a C16A_a H16A 0.8796 -0.0513 0.0308 23 0.990 0.000 C16A_a C17A_a C15A_a H16B 0.9748 -0.2804 0.0263 23 0.990 0.000 C16A_a C17A_a C15A_a H17A 0.8187 -0.4997 -0.0224 23 0.990 0.000 C17A_a C16A_a C18A_a H17B 0.8393 -0.2345 -0.0472 23 0.990 0.000 C17A_a C16A_a C18A_a H18A 0.6527 -0.0774 -0.0159 23 0.990 0.000 C18A_a C19A_a C17A_a H18B 0.6157 -0.3307 -0.0442 23 0.990 0.000 C18A_a C19A_a C17A_a H19A 0.5250 -0.3047 0.0347 23 0.990 0.000 C19A_a C14A_a C18A_a H19B 0.6116 -0.5468 0.0305 23 0.990 0.000 C19A_a C14A_a C18A_a H15C 0.8301 -0.1714 0.0927 23 0.990 0.000 C15B_b C14B_b C16B_b H15D 0.7167 0.0251 0.0839 23 0.990 0.000 C15B_b C14B_b C16B_b H16C 0.7394 0.0280 -0.0021 23 0.990 0.000 C16B_b C17B_b C15B_b H16D 0.8756 0.0864 0.0258 23 0.990 0.000 C16B_b C17B_b C15B_b H17C 0.9439 -0.3207 0.0141 23 0.990 0.000 C17B_b C16B_b C18B_b H17D 0.8923 -0.2117 -0.0386 23 0.990 0.000 C17B_b C16B_b C18B_b H18C 0.6983 -0.4268 -0.0349 23 0.990 0.000 C18B_b C19B_b C17B_b H18D 0.8130 -0.6215 -0.0271 23 0.990 0.000 C18B_b C19B_b C17B_b H19C 0.7968 -0.6181 0.0590 23 0.990 0.000 C19B_b C18B_b C14B_b H19D 0.6612 -0.6892 0.0321 23 0.990 0.000 C19B_b C18B_b C14B_b H2 -0.0573 0.2573 0.1544 43 0.950 0.000 C2 N1 C3 H4 -0.0751 -0.3674 0.2326 43 0.950 0.000 C4 C3 C5 H5 0.1351 -0.4531 0.2162 43 0.950 0.000 C5 C6 C4 H8A 0.3231 -0.5302 0.1640 23 0.990 0.000 C8 N7 C9 H8B 0.3292 -0.4325 0.2198 23 0.990 0.000 C8 N7 C9 H9A 0.5273 -0.2479 0.2118 23 0.990 0.000 C9 N10 C8 H9B 0.5362 -0.5319 0.1951 23 0.990 0.000 C9 N10 C8 H11A 0.4952 -0.0252 0.0875 23 0.990 0.000 C11 N10 C12 H11B 0.5013 0.0755 0.1432 23 0.990 0.000 C11 N10 C12 H12A 0.2875 0.0702 0.1121 23 0.990 0.000 C12 N7 C11 H12B 0.2983 -0.2150 0.0965 23 0.990 0.000 C12 N7 C11 2009src0112 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C14A_a 0.69635 -0.28176 0.07839 0.54569 0.01760 0.04099 0.03201 0.00396 0.00236 -0.00162 0.03017 0.01159 0.00065 0.00158 0.00030 0.00340 0.00349 0.00436 0.00422 0.00293 0.00259 0.00284 0.00160 C15A_a 0.83473 -0.35088 0.07472 0.54569 0.03128 0.03890 0.02930 0.00227 0.00521 0.00580 0.03301 0.00863 0.00041 0.00091 0.00016 0.00340 0.00228 0.00268 0.00229 0.00205 0.00180 0.00199 0.00111 H15A_a 0.84307 -0.53348 0.07316 0.54569 0.03961 0.00340 0.00000 H15B_a 0.88612 -0.29149 0.10442 0.54569 0.03961 0.00340 0.00000 C16A_a 0.88432 -0.23414 0.02835 0.54569 0.03289 0.04004 0.04716 0.00075 0.01624 0.00224 0.03937 0.01081 0.00046 0.00100 0.00023 0.00340 0.00257 0.00296 0.00347 0.00262 0.00241 0.00217 0.00126 H16A_a 0.87960 -0.05130 0.03085 0.54569 0.04724 0.00340 0.00000 H16B_a 0.97477 -0.28043 0.02629 0.54569 0.04724 0.00340 0.00000 C17A_a 0.80768 -0.31890 -0.01814 0.54569 0.03954 0.04993 0.02514 0.00584 0.00870 0.00677 0.03789 0.01388 0.00061 0.00139 0.00021 0.00340 0.00358 0.00439 0.00293 0.00279 0.00268 0.00328 0.00144 H17A_a 0.81874 -0.49972 -0.02240 0.54569 0.04547 0.00340 0.00000 H17B_a 0.83934 -0.23445 -0.04719 0.54569 0.04547 0.00340 0.00000 C18A_a 0.66486 -0.25939 -0.01507 0.54569 0.03923 0.04865 0.02653 0.00498 0.00485 0.00484 0.03802 0.00925 0.00044 0.00101 0.00016 0.00340 0.00262 0.00306 0.00235 0.00217 0.00195 0.00227 0.00123 H18A_a 0.65271 -0.07739 -0.01594 0.54569 0.04562 0.00340 0.00000 H18B_a 0.61567 -0.33072 -0.04419 0.54569 0.04562 0.00340 0.00000 C19A_a 0.61335 -0.36350 0.03224 0.54569 0.02625 0.04593 0.02923 0.01188 0.00255 -0.00179 0.03378 0.01051 0.00046 0.00100 0.00019 0.00340 0.00233 0.00301 0.00262 0.00236 0.00217 0.00216 0.00114 H19A_a 0.52498 -0.30467 0.03473 0.54569 0.04054 0.00340 0.00000 H19B_a 0.61161 -0.54683 0.03053 0.54569 0.04054 0.00340 0.00000 C14B_b 0.66228 -0.33153 0.06317 0.45431 0.01036 0.02768 0.03126 0.00627 0.00299 0.00275 0.02303 0.01466 0.00074 0.00170 0.00031 0.00340 0.00368 0.00412 0.00570 0.00342 0.00301 0.00294 0.00170 C15B_b 0.75806 -0.11976 0.06940 0.45431 0.03850 0.01717 0.03231 -0.00089 0.00585 -0.00501 0.02917 0.00931 0.00051 0.00094 0.00019 0.00340 0.00297 0.00252 0.00276 0.00216 0.00231 0.00226 0.00125 H15C_b 0.83012 -0.17143 0.09265 0.45431 0.03500 0.00340 0.00000 H15D_b 0.71674 0.02510 0.08389 0.45431 0.03500 0.00340 0.00000 C16B_b 0.80962 -0.04314 0.01977 0.45431 0.03876 0.02797 0.03523 0.00378 0.01445 -0.00391 0.03340 0.01052 0.00055 0.00102 0.00020 0.00340 0.00300 0.00290 0.00297 0.00238 0.00238 0.00234 0.00135 H16C_b 0.73944 0.02795 -0.00212 0.45431 0.04008 0.00340 0.00000 H16D_b 0.87557 0.08640 0.02582 0.45431 0.04008 0.00340 0.00000 C17B_b 0.86665 -0.26372 -0.00576 0.45431 0.03042 0.04096 0.03233 -0.01029 0.01006 -0.00287 0.03418 0.01444 0.00070 0.00137 0.00030 0.00340 0.00372 0.00393 0.00445 0.00306 0.00319 0.00319 0.00165 H17C_b 0.94391 -0.32072 0.01406 0.45431 0.04102 0.00340 0.00000 H17D_b 0.89226 -0.21174 -0.03856 0.45431 0.04102 0.00340 0.00000 C18B_b 0.77159 -0.47798 -0.01218 0.45431 0.02639 0.03632 0.03517 -0.01292 0.00651 -0.00113 0.03242 0.01037 0.00053 0.00129 0.00022 0.00340 0.00279 0.00350 0.00317 0.00273 0.00229 0.00256 0.00134 H18C_b 0.69826 -0.42680 -0.03486 0.45431 0.03890 0.00340 0.00000 H18D_b 0.81297 -0.62152 -0.02712 0.45431 0.03890 0.00340 0.00000 C19B_b 0.72440 -0.55408 0.03734 0.45431 0.03064 0.01956 0.03618 -0.00454 0.00401 -0.00147 0.02871 0.00932 0.00050 0.00092 0.00020 0.00340 0.00266 0.00256 0.00286 0.00222 0.00218 0.00205 0.00122 H19C_b 0.79682 -0.61807 0.05903 0.45431 0.03446 0.00340 0.00000 H19D_b 0.66117 -0.68916 0.03209 0.45431 0.03446 0.00340 0.00000 C2 -0.01759 0.11230 0.16817 1.00000 0.03254 0.03415 0.04730 -0.00337 0.01237 0.00161 0.03753 0.00478 0.00024 0.00050 0.00010 0.00000 0.00128 0.00140 0.00153 0.00123 0.00114 0.00110 0.00061 H2 -0.05728 0.25731 0.15442 1.00000 0.04503 0.00000 0.00000 C3 -0.08770 -0.03833 0.19684 1.00000 0.02699 0.03860 0.03224 -0.00757 0.00821 -0.00228 0.03231 0.00439 0.00022 0.00049 0.00009 0.00000 0.00118 0.00144 0.00127 0.00111 0.00098 0.00104 0.00057 C4 -0.02941 -0.25329 0.21401 1.00000 0.03613 0.04217 0.05546 0.00987 0.02030 0.00151 0.04374 0.00552 0.00025 0.00054 0.00011 0.00000 0.00137 0.00159 0.00173 0.00137 0.00126 0.00123 0.00070 H4 -0.07507 -0.36745 0.23264 1.00000 0.05249 0.00000 0.00000 C5 0.09513 -0.30454 0.20436 1.00000 0.03445 0.03886 0.05517 0.00462 0.01732 0.00362 0.04213 0.00526 0.00024 0.00054 0.00011 0.00000 0.00136 0.00151 0.00171 0.00136 0.00124 0.00117 0.00068 H5 0.13509 -0.45314 0.21620 1.00000 0.05056 0.00000 0.00000 C6 0.16069 -0.13671 0.17725 1.00000 0.02818 0.03242 0.03931 -0.01079 0.01224 -0.00312 0.03282 0.00439 0.00022 0.00047 0.00009 0.00000 0.00119 0.00134 0.00137 0.00114 0.00103 0.00103 0.00057 C8 0.35284 -0.39282 0.18611 1.00000 0.02957 0.06232 0.03312 0.00592 0.01084 0.00548 0.04124 0.00534 0.00023 0.00058 0.00010 0.00000 0.00128 0.00189 0.00135 0.00133 0.00105 0.00127 0.00068 H8A 0.32314 -0.53022 0.16397 1.00000 0.04949 0.00000 0.00000 H8B 0.32918 -0.43246 0.21984 1.00000 0.04949 0.00000 0.00000 C9 0.49651 -0.36982 0.18636 1.00000 0.03182 0.08795 0.03427 -0.01394 0.00838 0.00272 0.05105 0.00547 0.00025 0.00070 0.00010 0.00000 0.00137 0.00246 0.00144 0.00158 0.00113 0.00151 0.00083 H9A 0.52732 -0.24795 0.21178 1.00000 0.06126 0.00000 0.00000 H9B 0.53622 -0.53188 0.19509 1.00000 0.06126 0.00000 0.00000 C11 0.47210 -0.06341 0.12134 1.00000 0.04944 0.03136 0.12154 0.00653 0.05235 0.00548 0.06514 0.00713 0.00029 0.00055 0.00016 0.00000 0.00177 0.00155 0.00312 0.00181 0.00197 0.00134 0.00109 H11A 0.49525 -0.02523 0.08749 1.00000 0.07817 0.00000 0.00000 H11B 0.50132 0.07554 0.14317 1.00000 0.07817 0.00000 0.00000 C12 0.32843 -0.09001 0.12143 1.00000 0.04319 0.03331 0.06658 0.01245 0.03190 0.01083 0.04630 0.00599 0.00026 0.00053 0.00011 0.00000 0.00151 0.00146 0.00191 0.00140 0.00142 0.00122 0.00076 H12A 0.28751 0.07020 0.11209 1.00000 0.05556 0.00000 0.00000 H12B 0.29830 -0.21503 0.09653 1.00000 0.05556 0.00000 0.00000 C13 0.63423 -0.40544 0.11897 1.00000 0.03694 0.03003 0.05431 0.00421 0.02003 0.00120 0.03959 0.00521 0.00025 0.00050 0.00011 0.00000 0.00136 0.00137 0.00169 0.00127 0.00124 0.00115 0.00065 N1 0.10399 0.06658 0.15842 1.00000 0.03843 0.03230 0.05788 -0.00437 0.02177 -0.00115 0.04196 0.00425 0.00021 0.00042 0.00009 0.00000 0.00120 0.00123 0.00147 0.00110 0.00108 0.00098 0.00058 N3 -0.20972 0.03001 0.20977 1.00000 0.02631 0.04816 0.04272 0.00572 0.00865 0.00342 0.03876 0.00439 0.00020 0.00049 0.00009 0.00000 0.00110 0.00150 0.00133 0.00117 0.00096 0.00103 0.00056 N7 0.29113 -0.16469 0.16951 1.00000 0.02787 0.03819 0.04555 -0.00929 0.01451 -0.00270 0.03661 0.00383 0.00019 0.00041 0.00008 0.00000 0.00105 0.00124 0.00126 0.00104 0.00092 0.00092 0.00053 N10 0.53469 -0.29114 0.13846 1.00000 0.03382 0.03638 0.05703 -0.00404 0.02000 -0.00004 0.04158 0.00427 0.00020 0.00043 0.00009 0.00000 0.00114 0.00126 0.00147 0.00111 0.00105 0.00097 0.00058 O12 0.68528 -0.58843 0.13863 1.00000 0.04215 0.04175 0.04384 0.00969 0.01483 0.00667 0.04200 0.00358 0.00017 0.00036 0.00007 0.00000 0.00104 0.00111 0.00107 0.00091 0.00084 0.00088 0.00049 H3A -0.24712 0.14013 0.18903 1.00000 0.04207 0.04977 0.00245 0.00455 0.00090 0.00000 0.00823 H3B -0.25513 -0.10094 0.21950 1.00000 0.05507 0.04800 0.00260 0.00445 0.00108 0.00000 0.00943 Final Structure Factor Calculation for 2009src0112 in P2(1)/n Total number of l.s. parameters = 253 Maximum vector length = 511 Memory required = 3509 / 22995 wR2 = 0.1734 before cycle 5 for 3462 data and 0 / 253 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.063; Restrained GooF = 1.063 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0315 * P )^2 + 2.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0782 for 2524 Fo > 4sig(Fo) and 0.1102 for all 3462 data wR2 = 0.1734, GooF = S = 1.063, Restrained GooF = 1.063 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 23.00 for hydrogen atoms Principal mean square atomic displacements U 0.0426 0.0305 0.0174 C14A_a 0.0427 0.0298 0.0266 C15A_a 0.0544 0.0400 0.0238 C16A_a 0.0550 0.0367 0.0219 C17A_a 0.0517 0.0372 0.0252 C18A_a 0.0523 0.0267 0.0224 C19A_a 0.0361 0.0231 0.0098 C14B_b 0.0407 0.0308 0.0160 C15B_b 0.0480 0.0320 0.0202 C16B_b 0.0497 0.0315 0.0213 C17B_b 0.0490 0.0271 0.0211 C18B_b 0.0377 0.0301 0.0183 C19B_b 0.0515 0.0350 0.0260 C2 0.0448 0.0300 0.0221 C3 0.0674 0.0398 0.0240 C4 0.0625 0.0376 0.0262 C5 0.0506 0.0274 0.0205 C6 0.0647 0.0371 0.0220 C8 0.0914 0.0374 0.0243 C9 0.1413 0.0313 0.0229 C11 0.0877 0.0292 0.0220 C12 0.0637 0.0299 0.0252 C13 0.0680 0.0321 0.0258 N1 0.0529 0.0397 0.0237 N3 0.0556 0.0335 0.0208 N7 0.0650 0.0363 0.0235 N10 0.0606 0.0355 0.0299 O12 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.010 0.015 0.022 0.029 0.037 0.047 0.065 0.102 1.000 Number in group 374. 359. 308. 390. 345. 309. 342. 349. 344. 342. GooF 1.221 1.160 1.111 1.052 0.991 0.996 0.970 1.049 1.031 1.006 K 11.606 2.091 1.630 1.166 1.083 1.060 0.993 1.010 0.997 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.15 1.32 1.66 inf Number in group 346. 348. 353. 337. 346. 352. 345. 347. 344. 344. GooF 1.101 1.228 1.123 1.126 1.027 0.966 1.034 0.861 0.978 1.144 K 1.176 1.203 1.104 1.068 0.981 0.995 1.000 0.997 1.018 1.004 R1 0.302 0.282 0.233 0.205 0.160 0.109 0.085 0.059 0.066 0.036 Recommended weighting scheme: WGHT 0.0315 2.2329 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) 8 1 11 105.52 269.30 5.85 0.099 1.10 8 1 14 37.80 108.72 4.35 0.063 1.03 10 3 2 67.24 148.74 4.24 0.074 0.90 1 1 10 28.99 6.45 3.79 0.015 2.32 9 0 15 61.95 132.69 3.68 0.070 0.95 -3 0 7 23.15 62.38 3.55 0.048 2.70 -5 6 8 36.33 4.54 3.35 0.013 0.81 -1 1 28 22.30 1.46 3.27 0.007 0.95 -1 0 5 809.47 1002.66 3.24 0.192 4.97 0 1 4 1192.15 1427.50 3.16 0.229 4.22 8 2 9 358.53 495.19 3.08 0.135 1.07 6 4 21 35.08 3.64 3.08 0.012 0.80 0 4 15 20.95 2.80 3.05 0.010 1.08 -2 4 27 39.33 6.76 3.04 0.016 0.80 -8 1 8 12.82 0.48 2.97 0.004 1.22 12 0 0 18.05 0.23 2.95 0.003 0.87 10 2 15 13.93 0.01 2.92 0.000 0.84 -2 4 24 22.15 2.08 2.89 0.009 0.86 3 3 18 18.11 0.59 2.89 0.005 1.08 -12 1 11 53.49 23.72 2.87 0.030 0.83 6 2 27 39.29 10.98 2.86 0.020 0.80 2 0 16 -0.39 16.88 2.84 0.025 1.58 12 0 12 10.07 43.12 2.81 0.040 0.80 2 6 6 39.22 85.54 2.80 0.056 0.87 -9 2 5 13.29 0.00 2.80 0.000 1.06 2 0 12 114.35 170.44 2.80 0.079 2.02 0 2 10 19.90 4.49 2.76 0.013 1.91 7 3 18 21.60 3.38 2.76 0.011 0.89 -7 1 29 19.16 0.65 2.72 0.005 0.81 6 1 28 1.16 26.49 2.71 0.031 0.81 -1 1 4 250.33 328.10 2.71 0.110 3.98 7 5 11 21.09 0.58 2.71 0.005 0.81 -10 0 4 232.36 313.98 2.71 0.107 1.05 -8 5 14 27.94 0.78 2.69 0.005 0.78 6 2 25 99.83 51.50 2.69 0.044 0.85 7 4 16 16.40 0.09 2.68 0.002 0.84 -7 1 31 44.40 14.59 2.67 0.023 0.77 -11 2 1 25.99 6.95 2.64 0.016 0.90 -4 0 10 41.07 74.29 2.63 0.052 1.96 -2 0 28 4.68 38.36 2.62 0.038 0.96 11 1 4 16.07 0.67 2.60 0.005 0.92 -5 4 24 39.37 13.23 2.60 0.022 0.82 -5 2 13 9.63 0.38 2.59 0.004 1.34 -12 3 1 63.33 26.85 2.59 0.031 0.79 -6 3 28 129.89 73.63 2.58 0.052 0.79 8 2 23 19.10 0.55 2.57 0.004 0.81 -6 5 15 27.88 5.88 2.57 0.015 0.83 11 0 5 -6.74 11.95 2.55 0.021 0.93 -1 3 29 26.13 7.28 2.52 0.016 0.83 -1 2 29 11.80 0.22 2.52 0.003 0.88 Bond lengths and angles C14A_a - Distance Angles C13 1.4813 (0.0090) C15A_a 1.5143 (0.0083) 114.74 (0.60) C19A_a 1.5374 (0.0071) 102.78 (0.46) 111.51 (0.59) C14A_a - C13 C15A_a C15A_a - Distance Angles C14A_a 1.5143 (0.0083) C16A_a 1.5336 (0.0065) 109.95 (0.48) H15A_a 0.9900 109.67 109.67 H15B_a 0.9900 109.67 109.67 108.17 C15A_a - C14A_a C16A_a H15A_a C16A_a - Distance Angles C17A_a 1.5168 (0.0080) C15A_a 1.5336 (0.0065) 111.51 (0.42) H16A_a 0.9900 109.32 109.32 H16B_a 0.9900 109.32 109.32 107.97 C16A_a - C17A_a C15A_a H16A_a C17A_a - Distance Angles C16A_a 1.5168 (0.0080) C18A_a 1.5458 (0.0071) 110.58 (0.42) H17A_a 0.9900 109.53 109.53 H17B_a 0.9900 109.53 109.53 108.09 C17A_a - C16A_a C18A_a H17A_a C18A_a - Distance Angles C19A_a 1.5373 (0.0059) C17A_a 1.5458 (0.0071) 112.00 (0.41) H18A_a 0.9900 109.21 109.21 H18B_a 0.9900 109.21 109.21 107.91 C18A_a - C19A_a C17A_a H18A_a C19A_a - Distance Angles C14A_a 1.5374 (0.0071) C18A_a 1.5373 (0.0059) 111.19 (0.53) H19A_a 0.9900 109.39 109.39 H19B_a 0.9900 109.39 109.39 108.01 C19A_a - C14A_a C18A_a H19A_a C14B_b - Distance Angles C15B_b 1.5247 (0.0092) C19B_b 1.5585 (0.0098) 109.31 (0.56) C13 1.6150 (0.0090) 104.28 (0.53) 110.14 (0.57) C14B_b - C15B_b C19B_b C15B_b - Distance Angles C14B_b 1.5247 (0.0092) C16B_b 1.5460 (0.0069) 112.09 (0.51) H15C_b 0.9900 109.19 109.19 H15D_b 0.9900 109.19 109.19 107.89 C15B_b - C14B_b C16B_b H15C_b C16B_b - Distance Angles C17B_b 1.5226 (0.0086) C15B_b 1.5460 (0.0069) 111.34 (0.48) H16C_b 0.9900 109.36 109.36 H16D_b 0.9900 109.36 109.36 107.99 C16B_b - C17B_b C15B_b H16C_b C17B_b - Distance Angles C16B_b 1.5226 (0.0086) C18B_b 1.5301 (0.0084) 111.42 (0.52) H17C_b 0.9900 109.34 109.34 H17D_b 0.9900 109.34 109.34 107.98 C17B_b - C16B_b C18B_b H17C_b C18B_b - Distance Angles C19B_b 1.5239 (0.0078) C17B_b 1.5301 (0.0084) 110.88 (0.49) H18C_b 0.9900 109.46 109.46 H18D_b 0.9900 109.46 109.46 108.05 C18B_b - C19B_b C17B_b H18C_b C19B_b - Distance Angles C18B_b 1.5239 (0.0078) C14B_b 1.5585 (0.0098) 111.40 (0.51) H19C_b 0.9900 109.35 109.35 H19D_b 0.9900 109.35 109.35 107.98 C19B_b - C18B_b C14B_b H19C_b C2 - Distance Angles N1 1.3491 (0.0030) C3 1.3772 (0.0034) 124.03 (0.26) H2 0.9500 117.99 117.99 C2 - N1 C3 C3 - Distance Angles C4 1.3767 (0.0038) C2 1.3772 (0.0034) 116.35 (0.22) N3 1.4059 (0.0030) 121.92 (0.23) 121.66 (0.25) C3 - C4 C2 C4 - Distance Angles C3 1.3767 (0.0038) C5 1.3840 (0.0034) 120.58 (0.25) H4 0.9500 119.71 119.71 C4 - C3 C5 C5 - Distance Angles C6 1.3833 (0.0035) C4 1.3840 (0.0034) 119.17 (0.26) H5 0.9500 120.41 120.41 C5 - C6 C4 C6 - Distance Angles N1 1.3320 (0.0034) C5 1.3833 (0.0035) 121.04 (0.22) N7 1.4127 (0.0029) 116.33 (0.22) 122.58 (0.24) C6 - N1 C5 C8 - Distance Angles N7 1.4476 (0.0035) C9 1.5171 (0.0034) 110.85 (0.25) H8A 0.9900 109.47 109.47 H8B 0.9900 109.47 109.47 108.05 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4530 (0.0034) C8 1.5171 (0.0034) 111.25 (0.23) H9A 0.9900 109.38 109.38 H9B 0.9900 109.38 109.38 108.00 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4536 (0.0038) C12 1.5195 (0.0038) 110.32 (0.23) H11A 0.9900 109.59 109.59 H11B 0.9900 109.59 109.59 108.12 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4482 (0.0033) C11 1.5195 (0.0038) 111.39 (0.27) H12A 0.9900 109.35 109.35 H12B 0.9900 109.35 109.35 107.98 C12 - N7 C11 H12A C13 - Distance Angles O12 1.2268 (0.0031) N10 1.3569 (0.0031) 121.46 (0.24) C14A_a 1.4813 (0.0090) 118.84 (0.38) 118.83 (0.40) C14B_b 1.6150 (0.0090) 120.12 (0.36) 117.03 (0.36) 21.45 (0.27) C13 - O12 N10 C14A_a N1 - Distance Angles C6 1.3320 (0.0034) C2 1.3491 (0.0030) 118.67 (0.22) N1 - C6 N3 - Distance Angles C3 1.4059 (0.0030) H3A 0.8898 (0.0172) 112.73 (1.81) H3B 0.9034 (0.0176) 112.43 (1.98) 119.21 (2.71) N3 - C3 H3A N7 - Distance Angles C6 1.4127 (0.0029) C8 1.4476 (0.0035) 117.59 (0.21) C12 1.4482 (0.0033) 115.88 (0.22) 111.80 (0.19) N7 - C6 C8 N10 - Distance Angles C13 1.3569 (0.0031) C9 1.4530 (0.0034) 119.32 (0.25) C11 1.4536 (0.0038) 127.17 (0.24) 112.57 (0.24) N10 - C13 C9 O12 - Distance Angles C13 1.2268 (0.0031) O12 - Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.890(17) 2.092(18) 2.978(3) 174(3) N3-H3A...O12_$1 FMAP and GRID set by program FMAP 2 3 32 GRID -0.862 -2 -2 0.862 2 2 R1 = 0.1102 for 3462 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.6792 0.9252 0.0818 [ 0.67 A from H15D ] Deepest hole -0.28 at 0.4989 0.4827 0.2004 [ 0.44 A from H9B ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3197 / 18207 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6792 -0.0748 0.0818 1.00000 0.05 0.31 0.67 H15D 0.95 C15B 1.14 C14A 1.48 C14B Q2 1 0.5758 -0.2159 0.0370 1.00000 0.05 0.25 0.72 H19A 0.90 C19A 1.28 C14B 1.67 C14A Q3 1 0.3979 -0.0913 0.1219 1.00000 0.05 0.21 0.73 C12 0.80 C11 1.38 H12B 1.46 H12A Q4 1 0.4750 -0.0377 0.1363 1.00000 0.05 0.21 0.43 C11 0.69 H11B 1.36 H11A 1.50 N10 Q5 1 0.0280 -0.3032 0.1988 1.00000 0.05 0.21 0.71 C5 0.80 C4 1.44 H5 1.51 H4 Q6 1 -0.0717 0.0451 0.1793 1.00000 0.05 0.20 0.69 C3 0.76 C2 1.34 H2 1.73 N3 Q7 1 -0.0508 -0.1478 0.1914 1.00000 0.05 0.18 0.73 C3 0.85 C4 1.59 C2 1.66 H4 Q8 1 -0.0474 -0.2953 0.2523 1.00000 0.05 0.18 0.71 H4 1.10 C4 2.01 H9B 2.06 C5 Q9 1 -0.0269 -0.3011 0.1714 1.00000 0.05 0.18 1.19 C4 1.51 C5 1.72 C3 1.81 H4 Q10 1 0.7937 -0.7337 0.0954 1.00000 0.05 0.17 1.17 H19C 1.36 H15A 1.55 H15D 1.87 O12 Shortest distances between peaks (including symmetry equivalents) 5 9 0.91 3 4 0.92 7 9 1.03 6 7 1.11 5 7 1.19 5 8 1.71 1 2 1.74 7 8 1.83 6 9 1.94 5 6 2.20 1 10 2.21 8 9 2.22 6 8 2.70 1 4 2.71 6 10 2.85 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.06: Structure factors and derivatives 1.50: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0112 finished at 09:56:20 Total CPU time: 3.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++