+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0924 started at 11:13:20 on 28-Aug-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0924 in P2(1)2(1)2(1) CELL 0.71073 6.9529 11.4620 15.7644 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0003 0.0005 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N I UNIT 48 64 4 4 V = 1256.33 F(000) = 592.0 Mu = 2.51 mm-1 Cell Wt = 1204.63 Rho = 1.592 MERG 2 OMIT -3.00 55.00 OMIT 1 0 1 size 0.22 0.15 0.06 EXTI 0.00251 SHEL 7 0.77 FMAP 2 PLAN 5 ACTA BOND $H WGHT 0.00790 0.64320 L.S. 9 TEMP -153.00 FVAR 0.58400 C1 1 0.083630 0.568458 0.178533 11.00000 0.01310 0.01280 = 0.02061 0.00356 -0.00096 0.00595 C2 1 0.151822 0.579540 0.088097 11.00000 0.01618 0.01576 = 0.01603 0.00043 0.00167 0.00086 C3 1 0.018231 0.496481 0.043077 11.00000 0.01462 0.01646 = 0.01615 0.00091 -0.00072 0.00461 C4 1 -0.103575 0.445603 0.102121 11.00000 0.01447 0.01498 = 0.01482 0.00151 -0.00083 0.00434 C5 1 -0.237520 0.360774 0.083212 11.00000 0.01415 0.01590 = 0.02390 0.00210 -0.00396 0.00051 AFIX 43 H5 2 -0.318861 0.327834 0.125295 11.00000 -1.20000 AFIX 0 C6 1 -0.246127 0.326237 -0.001886 11.00000 0.02356 0.02086 = 0.02718 -0.00315 -0.01113 -0.00147 AFIX 43 H6 2 -0.334340 0.267120 -0.018328 11.00000 -1.20000 AFIX 0 C7 1 -0.128252 0.376729 -0.062636 11.00000 0.03092 0.02266 = 0.02008 -0.00511 -0.00847 0.00411 AFIX 43 H7 2 -0.137869 0.351981 -0.119993 11.00000 -1.20000 AFIX 0 C8 1 0.003819 0.462968 -0.041086 11.00000 0.02877 0.02049 = 0.01648 -0.00034 0.00280 0.00507 AFIX 43 H8 2 0.082459 0.498125 -0.083219 11.00000 -1.20000 AFIX 0 C9 1 -0.161879 0.464925 0.261021 11.00000 0.02097 0.02124 = 0.01924 0.00033 0.00408 0.00186 AFIX 137 H9A 2 -0.091241 0.403898 0.291436 11.00000 -1.50000 H9B 2 -0.290528 0.436320 0.246446 11.00000 -1.50000 H9C 2 -0.173281 0.534107 0.297203 11.00000 -1.50000 AFIX 0 C10 1 0.164750 0.630371 0.251762 11.00000 0.01981 0.01708 = 0.02081 -0.00203 -0.00074 0.00100 AFIX 137 H10A 2 0.066841 0.681902 0.276174 11.00000 -1.50000 H10B 2 0.275471 0.676902 0.233452 11.00000 -1.50000 H10C 2 0.206099 0.573647 0.294551 11.00000 -1.50000 AFIX 0 C11 1 0.363372 0.540178 0.078981 11.00000 0.02058 0.02094 = 0.02801 -0.00080 0.00278 -0.00010 AFIX 137 H11A 2 0.376585 0.459786 0.099327 11.00000 -1.50000 H11B 2 0.446188 0.591607 0.112629 11.00000 -1.50000 H11C 2 0.401510 0.544179 0.019205 11.00000 -1.50000 AFIX 0 C12 1 0.129441 0.707586 0.057607 11.00000 0.02959 0.01558 = 0.02445 0.00425 0.00604 -0.00177 AFIX 137 H12A 2 0.149358 0.711314 -0.003875 11.00000 -1.50000 H12B 2 0.224917 0.756726 0.086151 11.00000 -1.50000 H12C 2 -0.000084 0.735562 0.071293 11.00000 -1.50000 AFIX 0 N1 3 -0.058776 0.495303 0.183753 11.00000 0.01360 0.01337 = 0.01516 0.00073 -0.00040 0.00298 I1 4 0.674059 0.799047 0.217956 11.00000 0.01660 0.01745 = 0.02008 0.00199 0.00018 -0.00017 HKLF 4 Covalent radii and connectivity table for 2009src0924 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 I 1.330 C1 - N1 C10 C2 C2 - C3 C1 C11 C12 C3 - C8 C4 C2 C4 - C5 C3 N1 C5 - C4 C6 C6 - C7 C5 C7 - C6 C8 C8 - C3 C7 C9 - N1 C10 - C1 C11 - C2 C12 - C2 N1 - C1 C4 C9 I1 - no bonds found h k l Fo^2 Sigma Why rejected 3 0 0 44.85 10.03 observed but should be systematically absent 0 3 0 27.19 6.02 observed but should be systematically absent 9882 Reflections read, of which 46 rejected -9 =< h =< 7, -14 =< k =< 14, -20 =< l =< 18, Max. 2-theta = 54.97 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 5 14 42.63 7.67 3 44.47 1 Inconsistent equivalents 2843 Unique reflections, of which 0 suppressed R(int) = 0.0396 R(sigma) = 0.0462 Friedel opposites not merged Maximum memory for data reduction = 1626 / 28207 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 = 2019 / 166941 wR2 = 0.0520 before cycle 1 for 2843 data and 132 / 132 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58401 0.00079 0.012 OSF 2 0.00251 0.00039 0.001 EXTI Mean shift/esd = 0.004 Maximum = 0.040 for U33 I1 Max. shift = 0.000 A for H9C Max. dU = 0.000 for C12 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2019 / 166941 wR2 = 0.0520 before cycle 2 for 2843 data and 132 / 132 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58401 0.00079 0.006 OSF 2 0.00251 0.00039 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.017 for tors H9A Max. shift = 0.000 A for H9C Max. dU = 0.000 for C12 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2019 / 166941 wR2 = 0.0520 before cycle 3 for 2843 data and 132 / 132 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58401 0.00079 0.000 OSF 2 0.00251 0.00039 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.011 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2019 / 166941 wR2 = 0.0520 before cycle 4 for 2843 data and 132 / 132 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58401 0.00079 0.000 OSF 2 0.00251 0.00039 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.007 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for C10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2019 / 166941 wR2 = 0.0520 before cycle 5 for 2843 data and 132 / 132 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58401 0.00079 -0.001 OSF 2 0.00251 0.00039 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.005 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for C1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2019 / 166941 wR2 = 0.0520 before cycle 6 for 2843 data and 132 / 132 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58401 0.00079 0.000 OSF 2 0.00251 0.00039 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for C9 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2019 / 166941 wR2 = 0.0520 before cycle 7 for 2843 data and 132 / 132 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58401 0.00079 0.000 OSF 2 0.00251 0.00039 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for C4 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2019 / 166941 wR2 = 0.0520 before cycle 8 for 2843 data and 132 / 132 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58401 0.00079 -0.001 OSF 2 0.00251 0.00039 -0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for C1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2019 / 166941 wR2 = 0.0520 before cycle 9 for 2843 data and 132 / 132 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58401 0.00079 0.000 OSF 2 0.00251 0.00039 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for tors H9A Max. shift = 0.000 A for H9C Max. dU = 0.000 for C1 Largest correlation matrix elements 0.713 EXTI / OSF 0.600 U33 I1 / OSF 0.638 U22 I1 / OSF 0.593 U11 I1 / OSF Idealized hydrogen atom generation before cycle 10 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H5 -0.3189 0.3278 0.1253 43 0.950 0.000 C5 C4 C6 H6 -0.3343 0.2671 -0.0183 43 0.950 0.000 C6 C7 C5 H7 -0.1379 0.3520 -0.1200 43 0.950 0.000 C7 C6 C8 H8 0.0825 0.4981 -0.0832 43 0.950 0.000 C8 C3 C7 H9A -0.0911 0.4040 0.2915 137 0.980 0.000 C9 N1 H9A H9B -0.2905 0.4362 0.2464 137 0.980 0.000 C9 N1 H9A H9C -0.1735 0.5341 0.2972 137 0.980 0.000 C9 N1 H9A H10A 0.0669 0.6819 0.2762 137 0.980 0.000 C10 C1 H10A H10B 0.2755 0.6769 0.2335 137 0.980 0.000 C10 C1 H10A H10C 0.2061 0.5736 0.2946 137 0.980 0.000 C10 C1 H10A H11A 0.3766 0.4598 0.0993 137 0.980 0.000 C11 C2 H11A H11B 0.4462 0.5916 0.1126 137 0.980 0.000 C11 C2 H11A H11C 0.4015 0.5442 0.0192 137 0.980 0.000 C11 C2 H11A H12A 0.1494 0.7113 -0.0039 137 0.980 0.000 C12 C2 H12A H12B 0.2249 0.7567 0.0862 137 0.980 0.000 C12 C2 H12A H12C -0.0001 0.7356 0.0713 137 0.980 0.000 C12 C2 H12A 2009src0924 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.08363 0.56846 0.17853 1.00000 0.01310 0.01280 0.02062 0.00356 -0.00096 0.00595 0.01551 0.00588 0.00048 0.00027 0.00021 0.00000 0.00173 0.00158 0.00191 0.00136 0.00130 0.00121 0.00073 C2 0.15182 0.57954 0.08810 1.00000 0.01618 0.01577 0.01603 0.00042 0.00168 0.00086 0.01599 0.00564 0.00050 0.00026 0.00021 0.00000 0.00179 0.00150 0.00168 0.00126 0.00145 0.00135 0.00068 C3 0.01823 0.49648 0.04308 1.00000 0.01462 0.01648 0.01615 0.00091 -0.00072 0.00461 0.01575 0.00572 0.00048 0.00028 0.00021 0.00000 0.00176 0.00161 0.00176 0.00139 0.00139 0.00136 0.00069 C4 -0.10358 0.44560 0.10212 1.00000 0.01448 0.01499 0.01483 0.00151 -0.00083 0.00434 0.01476 0.00583 0.00046 0.00028 0.00022 0.00000 0.00171 0.00155 0.00183 0.00134 0.00134 0.00123 0.00071 C5 -0.23752 0.36077 0.08321 1.00000 0.01414 0.01592 0.02390 0.00209 -0.00396 0.00052 0.01799 0.00573 0.00048 0.00027 0.00023 0.00000 0.00176 0.00165 0.00197 0.00147 0.00142 0.00124 0.00075 H5 -0.31886 0.32783 0.12529 1.00000 0.02159 0.00000 0.00000 C6 -0.24613 0.32624 -0.00189 1.00000 0.02355 0.02088 0.02718 -0.00315 -0.01113 -0.00147 0.02387 0.00616 0.00055 0.00029 0.00025 0.00000 0.00199 0.00198 0.00216 0.00157 0.00157 0.00139 0.00087 H6 -0.33434 0.26712 -0.01833 1.00000 0.02864 0.00000 0.00000 C7 -0.12825 0.37673 -0.06264 1.00000 0.03092 0.02268 0.02007 -0.00511 -0.00847 0.00411 0.02456 0.00614 0.00055 0.00030 0.00024 0.00000 0.00237 0.00179 0.00195 0.00152 0.00158 0.00153 0.00086 H7 -0.13787 0.35199 -0.12000 1.00000 0.02947 0.00000 0.00000 C8 0.00381 0.46297 -0.04109 1.00000 0.02878 0.02050 0.01647 -0.00034 0.00281 0.00507 0.02192 0.00619 0.00054 0.00028 0.00022 0.00000 0.00216 0.00178 0.00187 0.00142 0.00167 0.00152 0.00078 H8 0.08245 0.49813 -0.08322 1.00000 0.02630 0.00000 0.00000 C9 -0.16189 0.46492 0.26102 1.00000 0.02098 0.02124 0.01924 0.00033 0.00408 0.00188 0.02049 0.00614 0.00057 0.00027 0.00021 0.00000 0.00194 0.00162 0.00188 0.00128 0.00161 0.00157 0.00075 H9A -0.09114 0.40399 0.29148 1.00000 0.03073 0.00000 0.00000 H9B -0.29046 0.43620 0.24644 1.00000 0.03073 0.00000 0.00000 H9C -0.17347 0.53413 0.29716 1.00000 0.03073 0.00000 0.00000 C10 0.16475 0.63037 0.25176 1.00000 0.01982 0.01709 0.02081 -0.00203 -0.00074 0.00099 0.01924 0.00592 0.00059 0.00027 0.00020 0.00000 0.00192 0.00154 0.00173 0.00126 0.00148 0.00154 0.00072 H10A 0.06685 0.68192 0.27616 1.00000 0.02886 0.00000 0.00000 H10B 0.27550 0.67688 0.23346 1.00000 0.02886 0.00000 0.00000 H10C 0.20605 0.57365 0.29456 1.00000 0.02886 0.00000 0.00000 C11 0.36338 0.54018 0.07898 1.00000 0.02058 0.02095 0.02801 -0.00080 0.00278 -0.00009 0.02318 0.00635 0.00050 0.00030 0.00025 0.00000 0.00217 0.00175 0.00214 0.00151 0.00161 0.00146 0.00083 H11A 0.37659 0.45979 0.09933 1.00000 0.03477 0.00000 0.00000 H11B 0.44619 0.59161 0.11263 1.00000 0.03477 0.00000 0.00000 H11C 0.40151 0.54418 0.01921 1.00000 0.03477 0.00000 0.00000 C12 0.12943 0.70758 0.05761 1.00000 0.02960 0.01559 0.02446 0.00425 0.00603 -0.00177 0.02322 0.00630 0.00052 0.00030 0.00023 0.00000 0.00206 0.00155 0.00188 0.00159 0.00150 0.00158 0.00076 H12A 0.14936 0.71131 -0.00387 1.00000 0.03482 0.00000 0.00000 H12B 0.22490 0.75673 0.08615 1.00000 0.03482 0.00000 0.00000 H12C -0.00009 0.73556 0.07129 1.00000 0.03482 0.00000 0.00000 N1 -0.05878 0.49530 0.18375 1.00000 0.01360 0.01338 0.01517 0.00072 -0.00040 0.00299 0.01405 0.00467 0.00038 0.00023 0.00017 0.00000 0.00149 0.00131 0.00143 0.00112 0.00105 0.00109 0.00058 I1 0.67406 0.79905 0.21796 1.00000 0.01660 0.01745 0.02009 0.00199 0.00018 -0.00017 0.01805 0.00035 0.00003 0.00002 0.00001 0.00000 0.00012 0.00011 0.00013 0.00009 0.00009 0.00009 0.00008 Final Structure Factor Calculation for 2009src0924 in P2(1)2(1)2(1) Total number of l.s. parameters = 132 Maximum vector length = 511 Memory required = 1889 / 25046 wR2 = 0.0520 before cycle 10 for 2843 data and 2 / 132 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0079 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0261 for 2723 Fo > 4sig(Fo) and 0.0282 for all 2843 data wR2 = 0.0520, GooF = S = 1.074, Restrained GooF = 1.074 for all data Flack x parameter = 0.0128 with esd 0.0269 Expected values are 0 (within 3 esd'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 = 14.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0223 0.0180 0.0063 C1 0.0181 0.0155 0.0144 C2 0.0203 0.0164 0.0106 C3 0.0192 0.0153 0.0098 C4 0.0256 0.0160 0.0123 C5 0.0368 0.0220 0.0128 C6 0.0380 0.0212 0.0145 C7 0.0316 0.0189 0.0153 C8 0.0250 0.0207 0.0158 C9 0.0222 0.0194 0.0161 C10 0.0290 0.0209 0.0196 C11 0.0336 0.0232 0.0129 C12 0.0165 0.0153 0.0104 N1 0.0212 0.0168 0.0162 I1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.074 0.108 0.138 0.169 0.200 0.231 0.267 0.325 0.406 1.000 Number in group 294. 284. 280. 282. 281. 290. 279. 287. 280. 286. GooF 1.033 1.212 1.077 1.156 1.075 0.984 0.925 1.051 1.127 1.078 K 0.950 0.942 0.963 0.966 0.992 1.001 1.005 1.004 1.013 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 287. 287. 286. 283. 281. 282. 283. 287. 282. 285. GooF 0.995 1.091 1.032 0.999 1.119 1.012 1.057 1.036 1.029 1.332 K 0.955 0.980 1.002 0.998 1.004 1.020 1.025 1.019 1.010 0.992 R1 0.060 0.059 0.046 0.038 0.034 0.027 0.022 0.017 0.014 0.013 Recommended weighting scheme: WGHT 0.0067 0.6712 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) 2 0 8 1140.76 891.77 4.98 0.173 1.71 8 5 2 64.92 309.01 4.52 0.102 0.81 6 2 2 7107.45 5969.44 4.03 0.448 1.12 2 7 14 390.43 607.46 3.91 0.143 0.90 3 0 4 217.37 164.99 3.71 0.075 2.00 -1 9 4 1383.50 1583.90 3.68 0.231 1.19 -1 1 6 2485.38 2751.28 3.63 0.304 2.40 8 4 5 315.70 587.27 3.53 0.141 0.80 2 0 6 3530.16 3236.37 3.44 0.330 2.10 0 1 20 163.02 365.43 3.43 0.111 0.79 8 1 8 215.60 426.09 3.26 0.120 0.79 0 3 3 1127.43 1271.63 3.26 0.207 3.09 5 0 2 -11.37 35.04 3.12 0.034 1.37 -2 3 1 2903.02 3172.37 3.05 0.327 2.54 1 1 5 2974.64 3287.87 3.00 0.333 2.79 2 8 15 213.96 344.88 2.96 0.108 0.82 3 3 0 88.33 60.60 2.94 0.045 1.98 -4 10 1 178.52 245.91 2.92 0.091 0.96 4 3 8 1778.94 1548.97 2.92 0.228 1.23 2 0 12 173.70 238.26 2.89 0.090 1.23 3 6 13 104.68 168.40 2.89 0.075 0.94 3 6 15 154.94 261.35 2.88 0.094 0.86 7 7 7 135.14 245.57 2.86 0.091 0.79 3 3 3 2465.18 2668.54 2.85 0.300 1.85 3 1 0 84.07 60.98 2.79 0.045 2.27 6 10 5 98.06 186.47 2.78 0.079 0.79 2 4 0 449.69 387.77 2.77 0.114 2.21 1 2 0 1597.87 1734.76 2.75 0.242 4.42 -5 1 14 609.71 408.36 2.73 0.117 0.87 3 9 13 109.26 223.73 2.71 0.087 0.82 1 7 0 14512.78 13785.58 2.69 0.681 1.59 2 5 5 3081.10 3317.31 2.68 0.334 1.64 -1 7 17 486.29 681.99 2.68 0.152 0.80 1 13 6 170.38 265.51 2.67 0.095 0.83 1 0 11 1130.78 996.01 2.62 0.183 1.40 -2 6 17 625.57 927.96 2.62 0.177 0.81 -2 9 9 2122.01 1877.37 2.61 0.251 0.99 -3 5 11 5094.98 4636.28 2.61 0.395 1.08 4 0 17 79.45 173.68 2.60 0.076 0.82 -7 6 1 63.69 117.89 2.59 0.063 0.88 1 2 16 234.80 308.29 2.57 0.102 0.96 2 3 0 1109.93 1218.40 2.56 0.203 2.57 4 4 16 70.76 162.54 2.56 0.074 0.82 1 4 2 1689.77 1908.08 2.55 0.254 2.51 2 11 3 986.07 1159.75 2.54 0.198 0.98 -6 7 8 2039.15 1623.24 2.49 0.234 0.85 2 3 1 3010.30 3218.31 2.48 0.329 2.54 -1 3 3 5662.15 6009.65 2.48 0.450 2.82 1 8 15 186.95 305.00 2.46 0.101 0.84 -1 2 5 1962.08 2120.32 2.46 0.267 2.57 Bond lengths and angles C1 - Distance Angles N1 1.3001 (0.0043) C10 1.4678 (0.0045) 123.69 (0.32) C2 1.5078 (0.0047) 110.71 (0.29) 125.60 (0.30) C1 - N1 C10 C2 - Distance Angles C3 1.5076 (0.0045) C1 1.5078 (0.0047) 101.43 (0.27) C11 1.5453 (0.0047) 111.00 (0.27) 111.26 (0.28) C12 1.5522 (0.0044) 112.93 (0.28) 109.94 (0.26) 110.04 (0.27) C2 - C3 C1 C11 C3 - Distance Angles C8 1.3849 (0.0046) C4 1.3870 (0.0045) 118.82 (0.32) C2 1.5076 (0.0045) 132.13 (0.32) 109.01 (0.28) C3 - C8 C4 C4 - Distance Angles C5 1.3789 (0.0045) C3 1.3870 (0.0045) 124.32 (0.33) N1 1.4414 (0.0042) 128.14 (0.31) 107.52 (0.27) C4 - C5 C3 C5 - Distance Angles C4 1.3789 (0.0045) C6 1.4000 (0.0051) 115.81 (0.33) H5 0.9500 122.09 122.09 C5 - C4 C6 C6 - Distance Angles C7 1.3870 (0.0053) C5 1.4000 (0.0051) 121.22 (0.33) H6 0.9500 119.39 119.39 C6 - C7 C5 C7 - Distance Angles C6 1.3870 (0.0053) C8 1.3913 (0.0048) 121.19 (0.34) H7 0.9500 119.41 119.41 C7 - C6 C8 C8 - Distance Angles C3 1.3849 (0.0046) C7 1.3913 (0.0048) 118.61 (0.34) H8 0.9500 120.70 120.70 C8 - C3 C7 C9 - Distance Angles N1 1.4556 (0.0041) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - N1 H9A H9B C10 - Distance Angles C1 1.4678 (0.0045) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C1 H10A H10B C11 - Distance Angles C2 1.5453 (0.0047) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C2 H11A H11B C12 - Distance Angles C2 1.5522 (0.0044) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C2 H12A H12B N1 - Distance Angles C1 1.3001 (0.0043) C4 1.4414 (0.0042) 111.28 (0.28) C9 1.4556 (0.0041) 125.61 (0.29) 123.10 (0.26) N1 - C1 C4 FMAP and GRID set by program FMAP 2 1 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0247 for 1662 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.83 at 0.1745 0.8948 0.7824 [ 1.83 A from H9C ] Deepest hole -0.50 at 0.1789 0.7011 0.8379 [ 0.88 A from I1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 2252 / 19055 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.3255 0.6052 0.2176 1.00000 0.05 0.83 1.83 H9C 2.00 H9B 2.08 C9 2.22 I1 Q2 1 -0.0016 0.3006 0.2806 1.00000 0.05 0.76 1.35 H9A 1.69 H10A 2.21 C9 2.28 I1 Q3 1 -0.1624 0.2024 -0.1574 1.00000 0.05 0.65 1.82 H7 1.97 I1 2.09 H11A 2.47 H5 Q4 1 0.1789 0.8574 0.0387 1.00000 0.05 0.45 1.41 H12B 1.78 C12 1.82 H12A 1.94 H12C Q5 1 0.3141 0.7968 0.2071 1.00000 0.05 0.39 1.46 H10B 1.76 H9B 1.98 H9A 2.06 H12B Shortest distances between peaks (including symmetry equivalents) 2 5 2.18 4 5 2.90 1 3 2.96 Time profile in seconds ----------------------- 0.14: 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 0.02: Analyse other restraints etc. 2.70: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.39: Structure factors and derivatives 1.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.55: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0924 finished at 11:13:31 Total CPU time: 6.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++