+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 20:27:29 on 17-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1007 in P2(1)/c CELL 0.71073 8.7385 9.1156 16.4786 90.000 91.064 90.000 ZERR 4.00 0.0002 0.0001 0.0003 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N S UNIT 56 64 4 8 V = 1312.40 F(000) = 556.0 Mu = 0.38 mm-1 Cell Wt = 1049.59 Rho = 1.328 MERG 2 OMIT -3.00 55.00 OMIT -2 1 1 OMIT -1 1 3 OMIT -2 1 2 OMIT 1 0 8 OMIT 1 0 2 OMIT 1 1 0 OMIT 0 1 2 SIZE 0.20 0.40 0.40 ACTA BOND WGHT 0.05060 0.66170 L.S. 4 TEMP -153.00 FVAR 1.01326 0.49070 0.51959 S1 4 0.175020 0.710380 0.031595 11.00000 0.02771 0.02436 = 0.01922 0.00082 -0.00428 0.00383 S2 4 0.054910 0.485346 -0.195876 11.00000 0.03684 0.02703 = 0.02228 -0.00123 -0.00693 0.00003 N1 3 0.021779 0.759876 -0.102591 11.00000 0.02510 0.02601 = 0.01947 0.00028 -0.00174 0.00171 C2 1 0.006174 0.884346 -0.055053 11.00000 0.02283 0.02564 = 0.01710 0.00084 0.00014 -0.00016 C6 1 0.218690 0.399356 -0.072192 11.00000 0.02316 0.02340 = 0.02389 0.00115 0.00044 -0.00175 C4 1 0.105590 0.661275 -0.065454 11.00000 0.02163 0.02688 = 0.01752 0.00038 -0.00107 -0.00194 C3 1 0.083352 0.878243 0.021634 11.00000 0.02119 0.02473 = 0.01920 0.00314 -0.00039 0.00214 C5 1 0.136914 0.519424 -0.101346 11.00000 0.02549 0.02485 = 0.01878 0.00085 -0.00217 -0.00226 C1 1 0.078272 0.992049 0.077360 11.00000 0.02567 0.02793 = 0.01734 0.00224 -0.00327 0.00105 AFIX 43 H1 2 0.130064 0.985964 0.128448 11.00000 -1.20000 AFIX 0 C7 1 0.212426 0.281466 -0.129008 11.00000 0.03330 0.02437 = 0.02977 -0.00170 -0.00142 0.00045 AFIX 43 H7 2 0.261786 0.189917 -0.119919 11.00000 -1.20000 AFIX 0 C9 1 0.300832 0.391819 0.008934 11.00000 0.02688 0.02494 = 0.02361 0.00040 -0.00211 0.00192 AFIX 23 H9A 2 0.224683 0.403618 0.052192 11.00000 -1.20000 H9B 2 0.372876 0.475412 0.013107 11.00000 -1.20000 AFIX 0 C10 1 0.390060 0.249727 0.024499 11.00000 0.02834 0.02503 = 0.02583 0.00187 -0.00074 0.00178 AFIX 23 H10A 2 0.320261 0.165002 0.017237 11.00000 -1.20000 H10B 2 0.472074 0.240895 -0.015859 11.00000 -1.20000 AFIX 0 C8 1 0.129107 0.312364 -0.197486 11.00000 0.03955 0.02718 = 0.02810 -0.00484 -0.00337 -0.00321 AFIX 43 H8 2 0.114044 0.245402 -0.241082 11.00000 -1.20000 AFIX 0 C12 1 0.546300 0.101123 0.127370 11.00000 0.06799 0.03268 = 0.02758 0.00170 -0.00558 0.02023 AFIX 23 H12A 2 0.609755 0.076302 0.080152 11.00000 -1.20000 H12B 2 0.470327 0.021601 0.133813 11.00000 -1.20000 AFIX 0 C11 1 0.460894 0.245136 0.109506 11.00000 0.05258 0.02949 = 0.02687 0.00138 -0.00437 0.01210 AFIX 23 H11A 2 0.379093 0.257817 0.149677 11.00000 -1.20000 H11B 2 0.533150 0.328144 0.115980 11.00000 -1.20000 AFIX 0 PART 1 C13 1 0.653481 0.106963 0.206536 21.00000 0.02227 0.03334 = 0.02670 0.00341 -0.00170 0.00494 AFIX 23 H13A 2 0.714415 0.015683 0.211127 21.00000 -1.20000 H13B 2 0.724957 0.190912 0.203156 21.00000 -1.20000 AFIX 0 C14 1 0.551403 0.124022 0.281345 -21.00000 0.04432 0.04739 = 0.02039 0.00515 -0.00103 0.00270 AFIX 33 H14A 2 0.615920 0.128685 0.330561 -21.00000 -1.50000 H14B 2 0.482138 0.039780 0.284728 -21.00000 -1.50000 H14C 2 0.491311 0.214437 0.276265 -21.00000 -1.50000 AFIX 0 PART 2 C13 1 0.556796 0.067189 0.218876 31.00000 0.07243 0.04842 = 0.03757 0.00795 -0.00289 0.02038 AFIX 23 H13C 2 0.452921 0.063856 0.241785 31.00000 -1.20000 H13D 2 0.605925 -0.029496 0.227747 31.00000 -1.20000 AFIX 0 C14 1 0.649158 0.184438 0.259882 -31.00000 0.09207 0.06954 = 0.04984 0.00281 -0.03815 0.01447 AFIX 33 H14D 2 0.655800 0.164513 0.318282 -31.00000 -1.50000 H14E 2 0.599983 0.279784 0.250727 -31.00000 -1.50000 H14F 2 0.752304 0.185963 0.237546 -31.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2008src1007 in P2(1)/c C 0.770 H 0.320 N 0.700 S 1.030 S1 - C3 C4 S2 - C8 C5 N1 - C4 C2 C2 - N1 C1_$1 C3 C6 - C5 C7 C9 C4 - N1 C5 S1 C3 - C1 C2 S1 C5 - C6 C4 S2 C1 - C3 C2_$1 C7 - C8 C6 C9 - C6 C10 C10 - C11 C9 C8 - C7 S2 C12 - C11 C13_b C13_a C11 - C10 C12 C13_a - C14_a C12 C14_a - C13_a C13_b - C14_b C12 C14_b - C13_b Operators for generating equivalent atoms: $1 -x, -y+2, -z 17448 Reflections read, of which 620 rejected -11 =< h =< 10, -11 =< k =< 11, -21 =< l =< 20, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -6 8 7 133.12 6.23 2 36.84 1 Inconsistent equivalents 3000 Unique reflections, of which 0 suppressed R(int) = 0.0360 R(sigma) = 0.0273 Friedel opposites merged Maximum memory for data reduction = 1966 / 29854 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 = 2473 / 216396 wR2 = 0.0955 before cycle 1 for 3000 data and 174 / 174 parameters GooF = S = 1.006; Restrained GooF = 1.006 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01572 0.00194 1.271 OSF 2 0.49419 0.00586 0.595 FVAR 2 3 0.50992 0.00659 -1.466 FVAR 3 Mean shift/esd = 0.250 Maximum = -1.466 for FVAR 3 Max. shift = 0.005 A for C13_b Max. dU = 0.002 for C14_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 2473 / 216396 wR2 = 0.0950 before cycle 2 for 3000 data and 174 / 174 parameters GooF = S = 1.003; Restrained GooF = 1.003 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01539 0.00193 -0.171 OSF 2 0.49612 0.00586 0.330 FVAR 2 3 0.50521 0.00662 -0.712 FVAR 3 Mean shift/esd = 0.091 Maximum = -0.712 for FVAR 3 Max. shift = 0.002 A for C14_b Max. dU = 0.001 for C14_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 2473 / 216396 wR2 = 0.0950 before cycle 3 for 3000 data and 174 / 174 parameters GooF = S = 1.003; Restrained GooF = 1.003 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01538 0.00192 -0.006 OSF 2 0.49653 0.00587 0.069 FVAR 2 3 0.50445 0.00665 -0.115 FVAR 3 Mean shift/esd = 0.011 Maximum = -0.115 for FVAR 3 Max. shift = 0.001 A for C13_b Max. dU = 0.000 for C14_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 2473 / 216396 wR2 = 0.0949 before cycle 4 for 3000 data and 174 / 174 parameters GooF = S = 1.002; Restrained GooF = 1.002 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01538 0.00192 0.000 OSF 2 0.49663 0.00587 0.017 FVAR 2 3 0.50425 0.00665 -0.029 FVAR 3 Mean shift/esd = 0.003 Maximum = -0.029 for FVAR 3 Max. shift = 0.000 A for C13_b Max. dU = 0.000 for C14_b 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 H1 0.1302 0.9861 0.1284 43 0.950 0.000 C1 C3 C2_$1 H7 0.2619 0.1900 -0.1199 43 0.950 0.000 C7 C8 C6 H9A 0.2246 0.4035 0.0522 23 0.990 0.000 C9 C6 C10 H9B 0.3728 0.4754 0.0132 23 0.990 0.000 C9 C6 C10 H10A 0.3202 0.1650 0.0172 23 0.990 0.000 C10 C11 C9 H10B 0.4720 0.2410 -0.0159 23 0.990 0.000 C10 C11 C9 H8 0.1140 0.2454 -0.2410 43 0.950 0.000 C8 C7 S2 H12A 0.6103 0.0770 0.0801 23 0.990 0.000 C12 C11 C13_a H12B 0.4708 0.0216 0.1335 23 0.990 0.000 C12 C11 C13_a H11A 0.3791 0.2574 0.1497 23 0.990 0.000 C11 C10 C12 H11B 0.5329 0.3282 0.1161 23 0.990 0.000 C11 C10 C12 H13A 0.7143 0.0156 0.2112 23 0.990 0.000 C13_a C14_a C12 H13B 0.7250 0.1909 0.2034 23 0.990 0.000 C13_a C14_a C12 H14A 0.6159 0.1285 0.3305 33 0.980 0.000 C14_a C13_a H14A_a H14B 0.4823 0.0395 0.2846 33 0.980 0.000 C14_a C13_a H14A_a H14C 0.4913 0.2142 0.2762 33 0.980 0.000 C14_a C13_a H14A_a H13C 0.4528 0.0647 0.2418 23 0.990 0.000 C13_b C14_b C12 H13D 0.6057 -0.0290 0.2280 23 0.990 0.000 C13_b C14_b C12 H14D 0.6553 0.1642 0.3181 33 0.980 0.000 C14_b C13_b H14D_b H14E 0.5996 0.2795 0.2506 33 0.980 0.000 C14_b C13_b H14D_b H14F 0.7518 0.1856 0.2374 33 0.980 0.000 C14_b C13_b H14D_b 2008src1007 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.17503 0.71041 0.03160 1.00000 0.02755 0.02434 0.01916 0.00087 -0.00424 0.00379 0.02374 0.00063 0.00004 0.00004 0.00002 0.00000 0.00021 0.00021 0.00019 0.00013 0.00014 0.00014 0.00012 S2 0.05492 0.48536 -0.19588 1.00000 0.03680 0.02692 0.02232 -0.00118 -0.00681 0.00009 0.02877 0.00067 0.00005 0.00004 0.00002 0.00000 0.00024 0.00022 0.00020 0.00014 0.00016 0.00015 0.00013 N1 0.02181 0.75988 -0.10261 1.00000 0.02533 0.02579 0.01938 0.00021 -0.00162 0.00163 0.02353 0.00220 0.00014 0.00014 0.00007 0.00000 0.00063 0.00064 0.00058 0.00049 0.00046 0.00050 0.00027 C2 0.00628 0.88434 -0.05508 1.00000 0.02288 0.02511 0.01662 0.00080 0.00007 -0.00035 0.02154 0.00249 0.00016 0.00016 0.00008 0.00000 0.00070 0.00074 0.00064 0.00053 0.00052 0.00055 0.00030 C6 0.21871 0.39945 -0.07220 1.00000 0.02302 0.02367 0.02375 0.00107 0.00067 -0.00187 0.02347 0.00257 0.00017 0.00016 0.00009 0.00000 0.00071 0.00074 0.00070 0.00056 0.00055 0.00056 0.00031 C4 0.10573 0.66126 -0.06553 1.00000 0.02150 0.02663 0.01738 0.00077 -0.00097 -0.00212 0.02185 0.00246 0.00016 0.00017 0.00008 0.00000 0.00070 0.00075 0.00064 0.00055 0.00052 0.00055 0.00030 C3 0.08334 0.87825 0.02165 1.00000 0.02069 0.02448 0.01930 0.00339 -0.00049 0.00199 0.02150 0.00256 0.00016 0.00016 0.00008 0.00000 0.00068 0.00072 0.00065 0.00054 0.00051 0.00054 0.00029 C5 0.13695 0.51946 -0.10132 1.00000 0.02507 0.02480 0.01873 0.00077 -0.00206 -0.00210 0.02289 0.00252 0.00017 0.00016 0.00009 0.00000 0.00073 0.00075 0.00068 0.00054 0.00054 0.00056 0.00030 C1 0.07831 0.99209 0.07733 1.00000 0.02521 0.02776 0.01723 0.00209 -0.00305 0.00103 0.02344 0.00258 0.00017 0.00016 0.00009 0.00000 0.00073 0.00077 0.00067 0.00055 0.00054 0.00057 0.00031 H1 0.13025 0.98608 0.12838 1.00000 0.02813 0.00000 0.00000 C7 0.21250 0.28148 -0.12898 1.00000 0.03331 0.02415 0.02981 -0.00198 -0.00153 0.00024 0.02912 0.00274 0.00019 0.00017 0.00010 0.00000 0.00084 0.00078 0.00081 0.00062 0.00064 0.00062 0.00034 H7 0.26191 0.18996 -0.11989 1.00000 0.03494 0.00000 0.00000 C9 0.30079 0.39176 0.00897 1.00000 0.02638 0.02481 0.02369 0.00032 -0.00195 0.00166 0.02499 0.00263 0.00018 0.00017 0.00009 0.00000 0.00076 0.00076 0.00071 0.00058 0.00057 0.00058 0.00031 H9A 0.22459 0.40347 0.05221 1.00000 0.02999 0.00000 0.00000 H9B 0.37280 0.47537 0.01321 1.00000 0.02999 0.00000 0.00000 C10 0.39002 0.24974 0.02450 1.00000 0.02810 0.02511 0.02570 0.00172 -0.00064 0.00178 0.02632 0.00276 0.00018 0.00017 0.00009 0.00000 0.00079 0.00075 0.00074 0.00060 0.00059 0.00060 0.00032 H10A 0.32024 0.16501 0.01720 1.00000 0.03158 0.00000 0.00000 H10B 0.47204 0.24097 -0.01585 1.00000 0.03158 0.00000 0.00000 C8 0.12908 0.31237 -0.19746 1.00000 0.03949 0.02662 0.02827 -0.00462 -0.00298 -0.00275 0.03151 0.00283 0.00020 0.00018 0.00010 0.00000 0.00093 0.00081 0.00079 0.00064 0.00067 0.00067 0.00036 H8 0.11396 0.24538 -0.24104 1.00000 0.03781 0.00000 0.00000 C12 0.54654 0.10137 0.12732 1.00000 0.06766 0.03196 0.02728 0.00164 -0.00533 0.01970 0.04238 0.00357 0.00025 0.00020 0.00011 0.00000 0.00131 0.00095 0.00084 0.00070 0.00081 0.00088 0.00046 H12A_a 0.61027 0.07696 0.08014 1.00000 0.05085 0.00000 0.00000 H12B_a 0.47075 0.02162 0.13353 1.00000 0.05085 0.00000 0.00000 C11 0.46090 0.24501 0.10956 1.00000 0.05249 0.02956 0.02638 0.00142 -0.00444 0.01244 0.03621 0.00335 0.00023 0.00020 0.00010 0.00000 0.00108 0.00086 0.00081 0.00067 0.00073 0.00077 0.00040 H11A 0.37905 0.25740 0.14973 1.00000 0.04345 0.00000 0.00000 H11B 0.53295 0.32816 0.11611 1.00000 0.04345 0.00000 0.00000 C13_a 0.65345 0.10694 0.20666 0.49663 0.02277 0.03364 0.02676 0.00382 -0.00237 0.00513 0.02776 0.00680 0.00046 0.00041 0.00020 0.00587 0.00194 0.00189 0.00177 0.00141 0.00133 0.00138 0.00095 H13A_a 0.71432 0.01562 0.21122 0.49663 0.03331 0.00587 0.00000 H13B_a 0.72499 0.19085 0.20341 0.49663 0.03331 0.00587 0.00000 C14_a 0.55146 0.12379 0.28127 0.50337 0.04292 0.04560 0.02030 0.00576 -0.00102 0.00191 0.03629 0.00755 0.00050 0.00047 0.00020 0.00587 0.00228 0.00226 0.00174 0.00148 0.00141 0.00172 0.00105 H14A_a 0.61591 0.12846 0.33051 0.50337 0.05444 0.00587 0.00000 H14B_a 0.48228 0.03948 0.28459 0.50337 0.05444 0.00587 0.00000 H14C_a 0.49129 0.21416 0.27619 0.50337 0.05444 0.00587 0.00000 C13_b 0.55677 0.06774 0.21900 0.50425 0.06889 0.04530 0.03688 0.00825 -0.00292 0.02017 0.05040 0.00971 0.00074 0.00052 0.00025 0.00665 0.00389 0.00251 0.00238 0.00185 0.00204 0.00248 0.00152 H13C_b 0.45282 0.06469 0.24183 0.50425 0.06048 0.00665 0.00000 H13D_b 0.60566 -0.02901 0.22801 0.50425 0.06048 0.00665 0.00000 C14_b 0.64865 0.18415 0.25972 0.49575 0.09637 0.07339 0.05045 0.00190 -0.03875 0.01677 0.07390 0.01011 0.00087 0.00068 0.00036 0.00665 0.00501 0.00384 0.00311 0.00297 0.00311 0.00364 0.00217 H14D_b 0.65530 0.16423 0.31812 0.49575 0.11085 0.00665 0.00000 H14E_b 0.59956 0.27954 0.25057 0.49575 0.11085 0.00665 0.00000 H14F_b 0.75179 0.18558 0.23737 0.49575 0.11085 0.00665 0.00000 Final Structure Factor Calculation for 2008src1007 in P2(1)/c Total number of l.s. parameters = 174 Maximum vector length = 511 Memory required = 2299 / 22995 wR2 = 0.0950 before cycle 5 for 3000 data and 0 / 174 parameters GooF = S = 1.003; Restrained GooF = 1.003 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0506 * P )^2 + 0.66 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0342 for 2595 Fo > 4sig(Fo) and 0.0415 for all 3000 data wR2 = 0.0950, GooF = S = 1.003, Restrained GooF = 1.003 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0312 0.0236 0.0164 S1 0.0400 0.0270 0.0192 S2 0.0274 0.0244 0.0187 N1 0.0253 0.0228 0.0165 C2 0.0255 0.0238 0.0211 C6 0.0275 0.0210 0.0170 C4 0.0265 0.0211 0.0169 C3 0.0277 0.0231 0.0179 C5 0.0282 0.0265 0.0156 C1 0.0345 0.0294 0.0235 C7 0.0283 0.0248 0.0219 C9 0.0290 0.0271 0.0229 C10 0.0408 0.0320 0.0217 C8 0.0770 0.0293 0.0208 C12 0.0586 0.0284 0.0217 C11 0.0364 0.0282 0.0187 C13_a 0.0473 0.0426 0.0189 C14_a 0.0805 0.0444 0.0263 C13_b 0.1241 0.0718 0.0258 C14_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.036 0.054 0.075 0.097 0.126 0.158 0.207 0.286 1.000 Number in group 311. 291. 308. 297. 295. 299. 306. 293. 300. 300. GooF 0.981 0.976 1.091 1.099 1.000 1.055 0.997 0.956 0.921 0.929 K 1.134 0.936 0.945 0.970 0.970 0.994 0.996 1.017 1.017 1.012 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.14 1.31 1.64 inf Number in group 305. 306. 297. 296. 306. 290. 301. 299. 299. 301. GooF 0.814 0.924 0.903 0.924 0.812 0.882 0.898 0.904 1.187 1.548 K 0.998 1.027 1.010 1.016 1.019 1.012 1.009 1.006 1.009 1.008 R1 0.079 0.070 0.056 0.054 0.043 0.037 0.031 0.026 0.032 0.033 Recommended weighting scheme: WGHT 0.0443 0.6780 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) -1 0 2 42.17 92.22 5.35 0.098 6.05 0 2 6 75.52 41.59 5.20 0.066 2.35 -4 2 2 192.51 129.93 4.94 0.116 1.92 2 4 2 67.99 38.44 4.77 0.063 1.96 0 4 1 15.51 1.43 4.35 0.012 2.26 2 4 6 177.94 128.07 4.04 0.115 1.62 3 2 3 34.37 17.97 3.97 0.043 2.23 -4 1 5 49.77 27.99 3.94 0.054 1.80 0 0 6 215.68 160.79 3.80 0.129 2.75 3 10 2 59.67 95.41 3.80 0.099 0.86 -9 0 12 26.17 60.34 3.76 0.079 0.80 -3 2 7 22.18 9.75 3.67 0.032 1.71 -2 3 7 136.32 185.42 3.61 0.138 1.72 -5 1 5 273.32 211.75 3.53 0.148 1.53 -1 1 5 847.92 1042.38 3.53 0.328 2.94 2 1 7 156.45 205.69 3.38 0.146 2.01 3 1 3 181.95 236.06 3.35 0.156 2.46 -1 5 4 9.86 21.91 3.33 0.048 1.64 4 1 13 9.85 2.17 3.29 0.015 1.08 2 0 16 422.00 327.45 3.20 0.184 1.00 -3 4 8 23.72 12.57 3.16 0.036 1.36 0 5 7 42.61 63.94 3.16 0.081 1.44 -3 2 5 451.24 371.41 3.07 0.196 1.98 3 1 14 42.42 63.88 3.06 0.081 1.08 3 1 13 4.22 15.11 3.06 0.040 1.15 0 2 9 33.45 20.32 3.04 0.046 1.70 7 7 6 10.24 29.17 2.96 0.055 0.85 -1 6 6 25.94 41.82 2.94 0.066 1.32 4 3 6 4.96 0.90 2.93 0.010 1.48 -8 5 8 13.27 31.07 2.91 0.057 0.86 6 2 2 100.17 74.66 2.91 0.088 1.36 -1 4 3 728.12 614.53 2.89 0.252 2.05 1 3 3 759.91 896.83 2.83 0.304 2.54 5 3 4 5.54 1.04 2.81 0.010 1.41 3 2 12 43.82 28.16 2.81 0.054 1.19 -1 3 9 75.29 54.96 2.80 0.075 1.55 4 2 3 36.72 23.36 2.78 0.049 1.84 -5 1 6 16.65 28.85 2.78 0.055 1.47 -4 2 3 3320.89 2879.77 2.76 0.546 1.86 4 7 2 77.52 103.02 2.75 0.103 1.11 -3 2 6 649.95 551.71 2.74 0.239 1.84 -3 1 7 42.35 60.48 2.74 0.079 1.81 5 3 7 16.62 8.25 2.73 0.029 1.26 -1 4 4 230.81 282.12 2.73 0.171 1.95 -2 3 4 53.25 73.25 2.73 0.087 2.14 10 2 8 7.30 19.67 2.71 0.045 0.79 -3 2 10 366.18 306.15 2.70 0.178 1.38 0 4 4 677.29 579.06 2.68 0.245 1.99 3 4 1 71.27 52.79 2.67 0.074 1.78 4 3 3 473.20 560.43 2.66 0.241 1.68 Bond lengths and angles S1 - Distance Angles C3 1.7335 (0.0015) C4 1.7587 (0.0014) 89.31 (0.07) S1 - C3 S2 - Distance Angles C8 1.7052 (0.0017) C5 1.7311 (0.0015) 91.64 (0.08) S2 - C8 N1 - Distance Angles C4 1.3048 (0.0019) C2 1.3868 (0.0019) 111.05 (0.12) N1 - C4 C2 - Distance Angles N1 1.3868 (0.0019) C1_$1 1.3926 (0.0020) 124.76 (0.13) C3 1.4225 (0.0019) 114.86 (0.13) 120.38 (0.13) C2 - N1 C1_$1 C6 - Distance Angles C5 1.3873 (0.0021) C7 1.4259 (0.0021) 110.77 (0.13) C9 1.5076 (0.0020) 125.24 (0.13) 123.98 (0.14) C6 - C5 C7 C4 - Distance Angles N1 1.3048 (0.0019) C5 1.4489 (0.0022) 122.17 (0.13) S1 1.7587 (0.0014) 115.58 (0.11) 122.24 (0.11) C4 - N1 C5 C3 - Distance Angles C1 1.3864 (0.0021) C2 1.4225 (0.0019) 122.60 (0.13) S1 1.7335 (0.0015) 128.19 (0.11) 109.20 (0.11) C3 - C1 C2 C5 - Distance Angles C6 1.3873 (0.0021) C4 1.4489 (0.0022) 131.48 (0.14) S2 1.7311 (0.0015) 111.82 (0.11) 116.66 (0.11) C5 - C6 C4 C1 - Distance Angles C3 1.3864 (0.0021) C2_$1 1.3926 (0.0020) 117.02 (0.13) C1 - C3 C7 - Distance Angles C8 1.3614 (0.0023) C6 1.4259 (0.0021) 113.65 (0.15) C7 - C8 C9 - Distance Angles C6 1.5076 (0.0020) C10 1.5304 (0.0021) 114.85 (0.12) C9 - C6 C10 - Distance Angles C11 1.5223 (0.0022) C9 1.5304 (0.0021) 112.04 (0.13) C10 - C11 C8 - Distance Angles C7 1.3614 (0.0023) S2 1.7052 (0.0017) 112.11 (0.12) C8 - C7 C12 - Distance Angles C11 1.5336 (0.0023) C13_b 1.5425 (0.0043) 112.07 (0.21) C13_a 1.5935 (0.0037) 113.95 (0.18) 34.95 (0.22) C12 - C11 C13_b C11 - Distance Angles C10 1.5223 (0.0022) C12 1.5336 (0.0023) 112.87 (0.14) C11 - C10 C13_a - Distance Angles C14_a 1.5395 (0.0049) C12 1.5935 (0.0037) 108.61 (0.28) C13_a - C14_a C14_a - Distance Angles C13_a 1.5395 (0.0049) C14_a - C13_b - Distance Angles C14_b 1.4836 (0.0077) C12 1.5425 (0.0044) 108.78 (0.42) C13_b - C14_b C14_b - Distance Angles C13_b 1.4836 (0.0077) C14_b - FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0413 for 3000 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.4863 0.0149 0.1001 [ 0.57 A from H12B ] Deepest hole -0.29 at 0.4466 0.0371 0.1434 [ 0.30 A from H12B ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2244 / 17493 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4863 0.0149 0.1001 1.00000 0.05 0.35 0.57 H12B 1.04 C12 1.27 H12A 2.10 C13 Q2 1 0.0398 0.8819 -0.0131 1.00000 0.05 0.32 0.68 C3 0.75 C2 1.82 C1 1.85 N1 Q3 1 0.2223 0.3409 -0.0966 1.00000 0.05 0.30 0.67 C6 0.76 C7 1.47 H7 1.79 C5 Q4 1 0.1124 0.5141 -0.1516 1.00000 0.05 0.27 0.85 C5 0.92 S2 1.90 C6 1.95 C4 Q5 1 0.1250 0.5932 -0.0815 1.00000 0.05 0.27 0.70 C4 0.76 C5 1.80 N1 1.95 C6 Q6 1 0.2596 0.3963 -0.0333 1.00000 0.05 0.26 0.73 C6 0.78 C9 1.43 H9B 1.45 H9A Q7 1 0.1426 0.6825 -0.0291 1.00000 0.05 0.26 0.70 C4 1.06 S1 1.74 N1 1.90 C5 Q8 1 0.0881 0.3993 -0.2067 1.00000 0.05 0.25 0.86 S2 0.88 C8 1.53 H8 1.98 C7 Q9 1 0.6585 0.1036 0.0925 1.00000 0.05 0.24 0.52 H12A 1.14 C12 1.88 C13 1.94 H12B Q10 1 0.0560 0.9184 0.0500 1.00000 0.05 0.24 0.64 C3 0.83 C1 1.56 H1 1.80 C2 Q11 1 0.0103 0.8172 -0.0820 1.00000 0.05 0.23 0.63 N1 0.76 C2 1.67 C4 1.90 C3 Q12 1 0.2028 0.4666 -0.0903 1.00000 0.05 0.23 0.69 C6 0.77 C5 1.81 C7 1.96 C9 Q13 1 0.5936 0.1038 0.1656 1.00000 0.05 0.23 0.75 C12 0.85 C13 1.00 C13 1.40 H12B Q14 1 0.3467 0.3211 0.0175 1.00000 0.05 0.22 0.76 C10 0.77 C9 1.43 H9B 1.43 H9A Q15 1 0.1931 0.3126 -0.1686 1.00000 0.05 0.21 0.73 C8 0.73 C7 1.50 H7 1.50 H8 Q16 1 0.4154 0.2530 0.0659 1.00000 0.05 0.21 0.71 C10 0.82 C11 1.40 H10A 1.42 H11A Q17 1 0.1212 0.8182 0.0295 1.00000 0.05 0.21 0.65 C3 1.09 S1 1.81 C2 1.81 C1 Q18 1 -0.0615 0.9289 -0.0578 1.00000 0.05 0.20 0.72 C2 0.80 C1 1.51 H1 1.86 C3 Q19 1 0.5169 0.1824 0.1273 1.00000 0.05 0.20 0.78 C12 0.80 C11 1.35 H11B 1.44 H11A Q20 1 0.3001 0.2065 0.1417 1.00000 0.05 0.19 0.84 H11A 1.55 C11 2.10 H10A 2.13 C10 Shortest distances between peaks (including symmetry equivalents) 2 10 1.10 10 17 1.13 2 17 1.15 13 19 1.16 3 12 1.16 14 16 1.17 5 7 1.20 3 6 1.20 2 18 1.22 6 12 1.23 3 15 1.23 11 18 1.26 2 11 1.30 6 14 1.31 9 13 1.34 4 12 1.34 5 12 1.35 8 15 1.36 4 5 1.36 10 18 1.40 4 8 1.40 16 19 1.48 9 19 1.55 7 17 1.58 1 19 1.61 1 13 1.63 16 20 1.67 1 9 1.71 7 11 1.89 12 15 1.91 19 20 1.93 4 15 1.99 10 18 2.04 2 7 2.05 3 4 2.05 11 17 2.06 2 10 2.09 2 18 2.09 3 14 2.16 3 8 2.21 8 12 2.23 5 11 2.27 7 12 2.28 5 6 2.28 2 2 2.31 1 16 2.32 14 20 2.34 17 18 2.36 10 11 2.39 17 18 2.41 10 10 2.41 6 15 2.42 3 5 2.47 6 16 2.48 1 20 2.49 18 18 2.53 12 14 2.53 10 11 2.54 4 7 2.55 4 6 2.55 9 16 2.55 13 16 2.62 7 10 2.63 14 19 2.64 5 8 2.73 5 17 2.75 13 20 2.75 18 20 2.77 6 7 2.80 7 9 2.82 11 20 2.88 9 17 2.90 7 18 2.90 2 5 2.96 2 9 2.97 9 11 2.99 5 15 3.00 Time profile in seconds ----------------------- 0.20: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.03: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.02: 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 0.08: Analyse other restraints etc. 23.56: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.05: Structure factors and derivatives 2.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.13: Apply other restraints 1.91: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.36: Fourier summations 0.03: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 20:28:00 Total CPU time: 31.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++