+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0405r started at 09:25:03 on 25-Apr-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0405r in P2(1)/c CELL 0.71073 27.4599 5.6654 11.4275 90.000 92.250 90.000 ZERR 4.00 0.0012 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F UNIT 84 80 8 12 4 V = 1776.42 F(000) = 772.0 Mu = 0.10 mm-1 Cell Wt = 1469.56 Rho = 1.374 MERG 2 OMIT -3.00 55.00 FREE C14 F1 FREE C18 F1' FMAP 2 PLAN 20 SIZE 0.03 0.20 0.60 ACTA BOND WGHT 0.06410 0.55790 L.S. 4 TEMP -153.00 FVAR 0.64024 H1N 2 -0.092540 0.179301 0.558940 11.00000 0.04040 H2N 2 -0.041846 0.045879 0.557975 11.00000 0.03412 MOLE 1 C7 1 0.400841 0.753632 1.209750 11.00000 0.01686 0.02094 = 0.02405 0.00064 0.00294 0.00390 C8 1 0.404501 0.568011 1.290227 11.00000 0.02201 0.02026 = 0.02749 0.00014 0.00396 0.00159 AFIX 43 H8 2 0.384056 0.433714 1.280036 11.00000 -1.20000 AFIX 0 C9 1 0.437514 0.577894 1.384330 11.00000 0.02916 0.02386 = 0.02307 0.00299 0.00378 0.00685 AFIX 43 H9 2 0.439199 0.452037 1.439274 11.00000 -1.20000 AFIX 0 C10 1 0.468217 0.770680 1.398995 11.00000 0.02453 0.03231 = 0.02152 -0.00477 -0.00136 0.00793 AFIX 43 H10 2 0.490956 0.776883 1.463755 11.00000 -1.20000 AFIX 0 C11 1 0.465660 0.953691 1.319212 11.00000 0.02239 0.02342 = 0.02711 -0.00311 0.00220 0.00086 AFIX 43 H11 2 0.487090 1.084611 1.328342 11.00000 -1.20000 AFIX 0 C12 1 0.431792 0.946929 1.225495 11.00000 0.01976 0.02191 = 0.02249 0.00201 0.00271 0.00183 AFIX 43 H12 2 0.429748 1.074979 1.171853 11.00000 -1.20000 AFIX 0 C13 1 0.364262 0.741735 1.110413 11.00000 0.01764 0.01791 = 0.02420 0.00432 0.00419 -0.00215 C14 1 0.329599 0.916903 1.087877 11.00000 0.02377 0.01595 = 0.02534 -0.00276 0.00452 -0.00048 AFIX 43 H14 2 0.330592 1.054407 1.135492 11.00000 -1.20000 AFIX 0 PART 1 F1 5 0.328402 1.109831 1.161908 10.50000 0.03404 0.02480 = 0.03228 -0.00523 0.00193 0.00127 PART 0 C15 1 0.293870 0.900970 0.999899 11.00000 0.01793 0.02276 = 0.02877 0.00669 0.00313 0.00155 AFIX 43 H15 2 0.270991 1.025310 0.988096 11.00000 -1.20000 AFIX 0 C16 1 0.291500 0.701429 0.928361 11.00000 0.01717 0.02285 = 0.02200 0.00517 0.00255 -0.00428 C17 1 0.326620 0.526251 0.946280 11.00000 0.02285 0.01904 = 0.02576 0.00086 0.00338 -0.00226 AFIX 43 H17 2 0.326468 0.390775 0.897278 11.00000 -1.20000 AFIX 0 C18 1 0.361497 0.550193 1.035151 11.00000 0.01652 0.01952 = 0.02895 0.00371 0.00167 0.00369 AFIX 43 H18 2 0.385045 0.428369 1.045518 11.00000 -1.20000 AFIX 0 PART 1 F1' 5 0.396571 0.377436 1.043634 10.50000 0.02398 0.01878 = 0.03435 0.00029 -0.00159 0.00795 PART 0 C19 1 0.251097 0.670181 0.834710 11.00000 0.01695 0.02576 = 0.02810 0.00038 0.00417 0.00052 AFIX 13 H19 2 0.261091 0.537858 0.782943 11.00000 -1.20000 AFIX 0 C20 1 0.242844 0.885087 0.757119 11.00000 0.02329 0.03879 = 0.03083 0.00642 0.00293 0.00223 AFIX 137 H20A 2 0.229234 1.013469 0.803115 11.00000 -1.50000 H20B 2 0.220033 0.844937 0.692053 11.00000 -1.50000 H20C 2 0.273938 0.935600 0.726094 11.00000 -1.50000 AFIX 0 C21 1 0.204458 0.592082 0.892903 11.00000 0.01940 0.02230 = 0.02248 -0.00425 -0.00083 -0.00257 O2 4 0.211756 0.401943 0.958339 11.00000 0.02062 0.02883 = 0.03834 0.00805 0.00778 -0.00139 AFIX 147 H2 2 0.186625 0.373415 0.995491 11.00000 -1.50000 AFIX 0 O3 4 0.165469 0.691772 0.880616 11.00000 0.01921 0.03157 = 0.03998 0.00194 0.00544 0.00506 MOLE 2 C1 1 -0.071382 0.499345 0.406725 11.00000 0.01700 0.01868 = 0.01997 -0.00385 0.00001 -0.00089 C2 1 -0.053824 0.623564 0.312458 11.00000 0.01824 0.02330 = 0.02157 -0.00379 0.00301 0.00148 AFIX 43 H2 2 -0.024424 0.576339 0.278087 11.00000 -1.20000 AFIX 0 C3 1 -0.079554 0.816856 0.269024 11.00000 0.02248 0.02843 = 0.02114 0.00506 0.00144 0.00006 AFIX 43 H3 2 -0.068339 0.902790 0.203970 11.00000 -1.20000 AFIX 0 C4 1 -0.121715 0.882236 0.321889 11.00000 0.02232 0.02342 = 0.02688 0.00291 -0.00185 0.00297 AFIX 43 H4 2 -0.139254 1.015089 0.291962 11.00000 -1.20000 AFIX 0 C5 1 -0.114257 0.577791 0.453879 11.00000 0.01656 0.02310 = 0.02181 -0.00013 0.00073 -0.00141 AFIX 43 H5 2 -0.126661 0.493166 0.518006 11.00000 -1.20000 AFIX 0 C6 1 -0.042413 0.293102 0.452729 11.00000 0.01807 0.02046 = 0.01951 -0.00332 0.00235 0.00036 N1 3 -0.139095 0.766497 0.413800 11.00000 0.02130 0.02322 = 0.02630 -0.00132 0.00289 0.00303 N2 3 -0.060591 0.160304 0.537345 11.00000 0.01762 0.02344 = 0.02792 0.00408 0.00501 0.00398 O1 4 -0.001994 0.253178 0.412617 11.00000 0.01800 0.02464 = 0.02777 0.00040 0.00477 0.00372 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2008src0405r in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C7 - C12 C8 C13 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - C18 C14 C7 C14 - C15 C13 F1_a - no bonds found C15 - C14 C16 C16 - C17 C15 C19 C17 - C18 C16 C18 - C17 C13 F1'_a - no bonds found C19 - C20 C16 C21 C20 - C19 C21 - O3 O2 C19 O2 - C21 O3 - C21 C1 - C5 C2 C6 C2 - C3 C1 C3 - C4 C2 C4 - N1 C3 C5 - N1 C1 C6 - O1 N2 C1 N1 - C5 C4 N2 - C6 O1 - C6 18309 Reflections read, of which 1138 rejected -35 =< h =< 35, -6 =< k =< 7, -14 =< l =< 14, 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) -1 2 6 2.35 0.45 7 2.28 4 0 12 3.88 5.11 2 49.40 2 Inconsistent equivalents 3958 Unique reflections, of which 0 suppressed R(int) = 0.0651 R(sigma) = 0.0760 Friedel opposites merged Maximum memory for data reduction = 2257 / 39799 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 = 2976 / 328045 wR2 = 0.1447 before cycle 1 for 3958 data and 263 / 263 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0641 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64022 0.00151 -0.012 OSF Mean shift/esd = 0.004 Maximum = -0.016 for x C8 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 2976 / 328045 wR2 = 0.1447 before cycle 2 for 3958 data and 263 / 263 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0641 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64020 0.00151 -0.011 OSF Mean shift/esd = 0.002 Maximum = -0.011 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 2976 / 328045 wR2 = 0.1448 before cycle 3 for 3958 data and 263 / 263 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0641 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64020 0.00151 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U11 H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 2976 / 328045 wR2 = 0.1447 before cycle 4 for 3958 data and 263 / 263 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0641 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64020 0.00151 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N 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 H8 0.3841 0.4337 1.2800 43 0.950 0.000 C8 C9 C7 H9 0.4392 0.4520 1.4393 43 0.950 0.000 C9 C8 C10 H10 0.4910 0.7769 1.4638 43 0.950 0.000 C10 C11 C9 H11 0.4871 1.0846 1.3283 43 0.950 0.000 C11 C10 C12 H12 0.4297 1.0750 1.1719 43 0.950 0.000 C12 C11 C7 H14 0.3306 1.0544 1.1355 43 0.950 0.000 C14 C15 C13 H15 0.2710 1.0253 0.9881 43 0.950 0.000 C15 C14 C16 H17 0.3265 0.3908 0.8973 43 0.950 0.000 C17 C18 C16 H18 0.3850 0.4284 1.0455 43 0.950 0.000 C18 C17 C13 H19 0.2611 0.5379 0.7829 13 1.000 0.000 C19 C20 C16 C21 H20A 0.2292 1.0135 0.8031 137 0.980 0.000 C20 C19 H20A H20B 0.2200 0.8449 0.6921 137 0.980 0.000 C20 C19 H20A H20C 0.2739 0.9356 0.7261 137 0.980 0.000 C20 C19 H20A H2 0.1866 0.3734 0.9955 147 0.840 0.000 O2 C21 H2 H2 -0.0244 0.5763 0.2781 43 0.950 0.000 C2 C3 C1 H3 -0.0683 0.9028 0.2040 43 0.950 0.000 C3 C4 C2 H4 -0.1393 1.0151 0.2920 43 0.950 0.000 C4 N1 C3 H5 -0.1267 0.4932 0.5180 43 0.950 0.000 C5 N1 C1 2008src0405r in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H1N -0.09252 0.17925 0.55891 1.00000 0.04027 0.04377 0.00100 0.00437 0.00216 0.00000 0.00702 H2N -0.04184 0.04586 0.55801 1.00000 0.03412 0.04212 0.00092 0.00447 0.00212 0.00000 0.00705 C7 0.40084 0.75363 1.20975 1.00000 0.01685 0.02094 0.02405 0.00064 0.00295 0.00390 0.02056 0.00371 0.00007 0.00035 0.00018 0.00000 0.00106 0.00106 0.00117 0.00094 0.00091 0.00083 0.00048 C8 0.40450 0.56801 1.29023 1.00000 0.02201 0.02024 0.02748 0.00013 0.00396 0.00159 0.02317 0.00386 0.00008 0.00037 0.00018 0.00000 0.00116 0.00108 0.00123 0.00098 0.00099 0.00088 0.00050 H8 0.38405 0.43372 1.28004 1.00000 0.02780 0.00000 0.00000 C9 0.43752 0.57789 1.38433 1.00000 0.02916 0.02385 0.02306 0.00298 0.00378 0.00685 0.02529 0.00399 0.00008 0.00039 0.00019 0.00000 0.00127 0.00114 0.00118 0.00096 0.00102 0.00096 0.00051 H9 0.43920 0.45204 1.43928 1.00000 0.03034 0.00000 0.00000 C10 0.46822 0.77068 1.39899 1.00000 0.02452 0.03230 0.02151 -0.00478 -0.00136 0.00792 0.02617 0.00406 0.00008 0.00039 0.00019 0.00000 0.00121 0.00128 0.00115 0.00102 0.00094 0.00097 0.00052 H10 0.49096 0.77688 1.46375 1.00000 0.03140 0.00000 0.00000 C11 0.46566 0.95370 1.31921 1.00000 0.02239 0.02341 0.02711 -0.00311 0.00220 0.00086 0.02427 0.00384 0.00008 0.00038 0.00018 0.00000 0.00119 0.00114 0.00126 0.00101 0.00099 0.00089 0.00051 H11 0.48709 1.08462 1.32834 1.00000 0.02912 0.00000 0.00000 C12 0.43179 0.94693 1.22549 1.00000 0.01975 0.02191 0.02248 0.00200 0.00271 0.00183 0.02133 0.00365 0.00007 0.00036 0.00018 0.00000 0.00113 0.00110 0.00114 0.00093 0.00093 0.00087 0.00048 H12 0.42975 1.07498 1.17185 1.00000 0.02560 0.00000 0.00000 C13 0.36426 0.74174 1.11041 1.00000 0.01763 0.01791 0.02419 0.00433 0.00419 -0.00215 0.01982 0.00365 0.00007 0.00034 0.00018 0.00000 0.00108 0.00103 0.00116 0.00092 0.00091 0.00083 0.00048 C14 0.32960 0.91690 1.08788 1.00000 0.02376 0.01595 0.02533 -0.00277 0.00452 -0.00049 0.02159 0.00377 0.00007 0.00036 0.00018 0.00000 0.00117 0.00101 0.00119 0.00092 0.00097 0.00085 0.00049 H14 0.33059 1.05440 1.13549 1.00000 0.02591 0.00000 0.00000 F1_a 0.32840 1.10983 1.16191 0.50000 0.03403 0.02478 0.03229 -0.00522 0.00192 0.00127 0.03035 0.00429 0.00009 0.00041 0.00021 0.00000 0.00152 0.00131 0.00146 0.00116 0.00120 0.00112 0.00062 C15 0.29387 0.90097 0.99990 1.00000 0.01792 0.02276 0.02876 0.00669 0.00313 0.00155 0.02309 0.00378 0.00007 0.00037 0.00019 0.00000 0.00111 0.00110 0.00122 0.00099 0.00097 0.00089 0.00049 H15 0.27099 1.02531 0.98809 1.00000 0.02771 0.00000 0.00000 C16 0.29150 0.70143 0.92836 1.00000 0.01716 0.02285 0.02199 0.00516 0.00255 -0.00429 0.02062 0.00365 0.00007 0.00036 0.00018 0.00000 0.00107 0.00108 0.00112 0.00095 0.00089 0.00086 0.00047 C17 0.32662 0.52625 0.94628 1.00000 0.02284 0.01904 0.02576 0.00086 0.00338 -0.00226 0.02248 0.00379 0.00007 0.00036 0.00019 0.00000 0.00120 0.00107 0.00118 0.00094 0.00099 0.00085 0.00050 H17 0.32647 0.39077 0.89728 1.00000 0.02698 0.00000 0.00000 C18 0.36150 0.55019 1.03515 1.00000 0.01652 0.01952 0.02893 0.00372 0.00167 0.00369 0.02164 0.00377 0.00007 0.00036 0.00019 0.00000 0.00110 0.00106 0.00123 0.00096 0.00096 0.00083 0.00049 H18 0.38505 0.42837 1.04552 1.00000 0.02596 0.00000 0.00000 F1'_a 0.39657 0.37743 1.04363 0.50000 0.02397 0.01877 0.03434 0.00030 -0.00158 0.00795 0.02577 0.00415 0.00008 0.00039 0.00021 0.00000 0.00134 0.00120 0.00144 0.00108 0.00113 0.00100 0.00058 C19 0.25110 0.67018 0.83471 1.00000 0.01693 0.02576 0.02809 0.00038 0.00416 0.00052 0.02351 0.00379 0.00007 0.00038 0.00019 0.00000 0.00108 0.00112 0.00123 0.00100 0.00093 0.00089 0.00049 H19 0.26109 0.53786 0.78294 1.00000 0.02821 0.00000 0.00000 C20 0.24284 0.88509 0.75712 1.00000 0.02329 0.03878 0.03082 0.00642 0.00293 0.00223 0.03091 0.00433 0.00008 0.00042 0.00021 0.00000 0.00123 0.00137 0.00130 0.00110 0.00102 0.00103 0.00056 H20A 0.22923 1.01347 0.80311 1.00000 0.04637 0.00000 0.00000 H20B 0.22003 0.84494 0.69205 1.00000 0.04637 0.00000 0.00000 H20C 0.27394 0.93561 0.72610 1.00000 0.04637 0.00000 0.00000 C21 0.20446 0.59208 0.89290 1.00000 0.01940 0.02229 0.02248 -0.00424 -0.00083 -0.00257 0.02143 0.00355 0.00008 0.00036 0.00018 0.00000 0.00116 0.00110 0.00116 0.00096 0.00092 0.00090 0.00049 O2 0.21176 0.40194 0.95834 1.00000 0.02061 0.02882 0.03833 0.00804 0.00778 -0.00139 0.02908 0.00277 0.00005 0.00026 0.00014 0.00000 0.00084 0.00085 0.00096 0.00074 0.00071 0.00067 0.00039 H2 0.18662 0.37338 0.99547 1.00000 0.04362 0.00000 0.00000 O3 0.16547 0.69177 0.88062 1.00000 0.01920 0.03156 0.03996 0.00194 0.00545 0.00506 0.03013 0.00276 0.00005 0.00027 0.00014 0.00000 0.00083 0.00086 0.00096 0.00076 0.00071 0.00068 0.00039 C1 -0.07138 0.49934 0.40672 1.00000 0.01699 0.01868 0.01997 -0.00385 0.00001 -0.00089 0.01856 0.00344 0.00007 0.00035 0.00017 0.00000 0.00108 0.00102 0.00108 0.00088 0.00086 0.00081 0.00046 C2 -0.05382 0.62356 0.31246 1.00000 0.01823 0.02329 0.02155 -0.00379 0.00300 0.00148 0.02097 0.00358 0.00008 0.00035 0.00018 0.00000 0.00107 0.00110 0.00113 0.00093 0.00089 0.00087 0.00048 H2 -0.02442 0.57634 0.27809 1.00000 0.02516 0.00000 0.00000 C3 -0.07955 0.81686 0.26902 1.00000 0.02247 0.02842 0.02113 0.00506 0.00144 0.00006 0.02399 0.00383 0.00008 0.00039 0.00019 0.00000 0.00116 0.00116 0.00115 0.00099 0.00092 0.00093 0.00050 H3 -0.06834 0.90280 0.20397 1.00000 0.02879 0.00000 0.00000 C4 -0.12172 0.88224 0.32189 1.00000 0.02231 0.02342 0.02687 0.00291 -0.00185 0.00297 0.02427 0.00379 0.00008 0.00038 0.00019 0.00000 0.00117 0.00111 0.00122 0.00097 0.00096 0.00090 0.00051 H4 -0.13926 1.01509 0.29196 1.00000 0.02913 0.00000 0.00000 C5 -0.11426 0.57779 0.45388 1.00000 0.01656 0.02309 0.02181 -0.00013 0.00072 -0.00141 0.02049 0.00357 0.00007 0.00036 0.00018 0.00000 0.00107 0.00108 0.00110 0.00095 0.00087 0.00086 0.00046 H5 -0.12666 0.49317 0.51801 1.00000 0.02459 0.00000 0.00000 C6 -0.04241 0.29310 0.45273 1.00000 0.01807 0.02045 0.01950 -0.00331 0.00234 0.00036 0.01930 0.00357 0.00007 0.00035 0.00018 0.00000 0.00106 0.00106 0.00108 0.00091 0.00086 0.00086 0.00046 N1 -0.13910 0.76650 0.41380 1.00000 0.02129 0.02322 0.02629 -0.00132 0.00289 0.00303 0.02355 0.00313 0.00006 0.00030 0.00015 0.00000 0.00097 0.00095 0.00103 0.00081 0.00079 0.00075 0.00043 N2 -0.06059 0.16030 0.53735 1.00000 0.01760 0.02344 0.02791 0.00409 0.00501 0.00398 0.02288 0.00329 0.00007 0.00034 0.00016 0.00000 0.00100 0.00100 0.00107 0.00087 0.00084 0.00082 0.00043 O1 -0.00199 0.25318 0.41262 1.00000 0.01799 0.02464 0.02776 0.00040 0.00476 0.00372 0.02336 0.00252 0.00005 0.00024 0.00012 0.00000 0.00079 0.00079 0.00085 0.00066 0.00064 0.00060 0.00037 Final Structure Factor Calculation for 2008src0405r in P2(1)/c Total number of l.s. parameters = 263 Maximum vector length = 511 Memory required = 2713 / 24017 wR2 = 0.1448 before cycle 5 for 3958 data and 0 / 263 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0641 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0543 for 2535 Fo > 4sig(Fo) and 0.1033 for all 3958 data wR2 = 0.1448, GooF = S = 1.040, Restrained GooF = 1.040 for all data Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0254 0.0221 0.0142 C7 0.0288 0.0218 0.0190 C8 0.0350 0.0219 0.0190 C9 0.0390 0.0204 0.0190 C10 0.0289 0.0234 0.0205 C11 0.0253 0.0202 0.0185 C12 0.0268 0.0199 0.0128 C13 0.0285 0.0211 0.0152 C14 0.0350 0.0342 0.0219 F1_a 0.0335 0.0184 0.0174 C15 0.0281 0.0211 0.0127 C16 0.0271 0.0229 0.0175 C17 0.0304 0.0205 0.0139 C18 0.0354 0.0290 0.0129 F1'_a 0.0289 0.0257 0.0159 C19 0.0427 0.0273 0.0227 C20 0.0267 0.0218 0.0158 C21 0.0439 0.0268 0.0165 O2 0.0415 0.0321 0.0167 O3 0.0232 0.0176 0.0149 C1 0.0263 0.0210 0.0156 C2 0.0310 0.0225 0.0184 C3 0.0288 0.0258 0.0181 C4 0.0234 0.0218 0.0163 C5 0.0234 0.0189 0.0156 C6 0.0269 0.0254 0.0183 N1 0.0322 0.0213 0.0151 N2 0.0295 0.0253 0.0152 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.019 0.029 0.038 0.050 0.064 0.082 0.110 0.160 1.000 Number in group 427. 392. 401. 363. 410. 383. 404. 388. 393. 397. GooF 0.851 0.929 0.922 1.042 1.092 1.085 1.225 1.173 1.056 0.978 K 1.211 1.135 0.995 0.876 0.956 0.986 0.973 1.014 1.013 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.15 1.33 1.68 inf Number in group 404. 394. 394. 391. 404. 391. 393. 401. 388. 398. GooF 1.016 0.912 1.004 1.002 1.054 0.991 1.083 0.920 1.021 1.334 K 0.980 1.011 1.022 1.015 1.041 1.011 1.015 1.012 1.026 0.980 R1 0.281 0.252 0.201 0.175 0.135 0.091 0.071 0.045 0.046 0.038 Recommended weighting scheme: WGHT 0.0639 0.5765 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) 20 0 4 33.25 150.64 5.52 0.076 1.22 1 1 1 119.10 210.81 5.39 0.090 4.97 7 0 0 65.49 130.01 5.38 0.071 3.92 17 2 8 -10.38 111.59 4.98 0.066 0.98 15 4 10 64.03 265.16 4.78 0.101 0.79 -17 1 10 20.29 75.28 4.73 0.054 0.94 -23 3 7 -6.98 67.70 4.63 0.051 0.87 0 2 0 77.97 37.23 4.52 0.038 2.83 -2 2 3 98.53 61.52 4.01 0.049 2.25 -15 1 7 169.40 254.82 3.65 0.099 1.21 20 0 6 53.28 132.40 3.64 0.071 1.09 20 1 10 65.08 176.32 3.53 0.082 0.85 -8 2 3 170.94 122.34 3.48 0.069 1.92 5 2 2 534.11 412.87 3.43 0.126 2.29 5 6 8 353.18 204.91 3.40 0.089 0.78 1 2 4 268.57 202.62 3.34 0.088 2.00 -22 3 8 408.63 262.88 3.25 0.101 0.85 -20 3 11 19.60 94.44 3.25 0.060 0.77 -5 1 1 1137.49 1436.57 3.22 0.235 3.76 13 2 12 -2.48 113.61 3.19 0.066 0.82 -26 0 8 374.35 262.54 3.18 0.101 0.86 -26 1 3 294.13 218.30 3.15 0.092 1.01 17 1 2 -6.62 8.48 3.15 0.018 1.48 -25 2 10 84.19 149.99 3.12 0.076 0.78 14 4 6 90.31 176.19 3.12 0.082 0.97 13 0 0 1360.91 1079.30 3.10 0.204 2.11 20 2 6 3.11 61.49 3.07 0.049 1.02 -8 0 4 245.71 322.30 3.07 0.112 2.24 9 1 1 275.85 356.53 3.04 0.117 2.59 1 1 5 18.91 7.64 3.03 0.017 2.11 -5 2 3 78.85 50.91 3.00 0.044 2.12 12 4 3 20.02 40.75 2.97 0.040 1.14 6 1 6 105.15 144.24 2.97 0.075 1.66 19 3 8 21.51 146.11 2.95 0.075 0.88 9 0 2 423.56 554.23 2.95 0.146 2.65 7 3 0 81.17 56.65 2.92 0.047 1.70 14 0 0 468.99 366.77 2.92 0.119 1.96 14 2 0 36.15 60.50 2.90 0.048 1.61 -28 1 6 74.59 137.59 2.89 0.073 0.87 -1 1 1 1296.54 1596.10 2.89 0.248 5.01 -24 1 11 2.44 40.37 2.83 0.039 0.78 29 1 6 345.60 213.60 2.80 0.091 0.83 21 2 7 84.78 135.83 2.79 0.072 0.94 19 4 8 31.19 145.19 2.77 0.075 0.81 12 4 0 85.19 132.94 2.75 0.072 1.20 33 1 1 23.85 74.23 2.72 0.054 0.82 0 1 4 138.48 180.49 2.70 0.083 2.55 15 5 2 0.71 23.28 2.68 0.030 0.95 25 3 1 52.19 96.91 2.67 0.061 0.94 -2 0 6 0.51 12.32 2.66 0.022 1.90 Bond lengths and angles C7 - Distance Angles C12 1.3935 (0.0029) C8 1.3980 (0.0029) 118.59 (0.20) C13 1.4875 (0.0031) 121.62 (0.18) 119.79 (0.18) C7 - C12 C8 C8 - Distance Angles C9 1.3802 (0.0030) C7 1.3980 (0.0029) 120.67 (0.20) C8 - C9 C9 - Distance Angles C8 1.3802 (0.0030) C10 1.3859 (0.0032) 120.27 (0.20) C9 - C8 C10 - Distance Angles C11 1.3807 (0.0031) C9 1.3859 (0.0032) 119.81 (0.21) C10 - C11 C11 - Distance Angles C10 1.3807 (0.0031) C12 1.3911 (0.0030) 120.19 (0.21) C11 - C10 C12 - Distance Angles C11 1.3911 (0.0030) C7 1.3935 (0.0029) 120.46 (0.19) C12 - C11 C13 - Distance Angles C18 1.3849 (0.0029) C14 1.3921 (0.0028) 115.04 (0.19) C7 1.4875 (0.0031) 121.89 (0.18) 123.04 (0.18) C13 - C18 C14 C14 - Distance Angles C15 1.3799 (0.0030) C13 1.3921 (0.0028) 123.34 (0.20) C14 - C15 C15 - Distance Angles C14 1.3799 (0.0030) C16 1.3951 (0.0030) 119.70 (0.19) C15 - C14 C16 - Distance Angles C17 1.3934 (0.0029) C15 1.3951 (0.0030) 118.36 (0.19) C19 1.5213 (0.0030) 120.13 (0.19) 121.50 (0.19) C16 - C17 C15 C17 - Distance Angles C18 1.3750 (0.0030) C16 1.3934 (0.0029) 119.75 (0.20) C17 - C18 C18 - Distance Angles C17 1.3750 (0.0030) C13 1.3849 (0.0029) 123.75 (0.19) C18 - C17 C19 - Distance Angles C20 1.5180 (0.0031) C16 1.5213 (0.0030) 113.93 (0.18) C21 1.5314 (0.0028) 112.16 (0.18) 109.11 (0.17) C19 - C20 C16 C20 - Distance Angles C19 1.5180 (0.0031) C20 - C21 - Distance Angles O3 1.2137 (0.0024) O2 1.3221 (0.0025) 123.92 (0.19) C19 1.5314 (0.0028) 124.35 (0.20) 111.73 (0.18) C21 - O3 O2 O2 - Distance Angles C21 1.3221 (0.0025) O2 - O3 - Distance Angles C21 1.2137 (0.0024) O3 - C1 - Distance Angles C5 1.3870 (0.0027) C2 1.3889 (0.0028) 117.70 (0.19) C6 1.4972 (0.0028) 124.13 (0.18) 118.16 (0.17) C1 - C5 C2 C2 - Distance Angles C3 1.3846 (0.0029) C1 1.3889 (0.0028) 119.41 (0.19) C2 - C3 C3 - Distance Angles C4 1.3775 (0.0028) C2 1.3846 (0.0029) 118.77 (0.20) C3 - C4 C4 - Distance Angles N1 1.3418 (0.0026) C3 1.3775 (0.0028) 122.87 (0.20) C4 - N1 C5 - Distance Angles N1 1.3392 (0.0027) C1 1.3870 (0.0027) 123.48 (0.19) C5 - N1 C6 - Distance Angles O1 1.2382 (0.0022) N2 1.3372 (0.0026) 122.03 (0.19) C1 1.4972 (0.0028) 118.96 (0.18) 119.00 (0.18) C6 - O1 N2 N1 - Distance Angles C5 1.3392 (0.0027) C4 1.3418 (0.0027) 117.77 (0.18) N1 - C5 N2 - Distance Angles C6 1.3372 (0.0026) N2 - O1 - Distance Angles C6 1.2382 (0.0022) O1 - FMAP and GRID set by program FMAP 2 2 16 GRID 21.154 -2 -1 3.846 2 1 R1 = 0.1033 for 3958 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.2374 0.7146 0.3770 [ 0.90 A from C19 ] Deepest hole -0.33 at 0.3492 0.4817 0.6601 [ 0.61 A from H14 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3321 / 34683 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2374 0.7854 0.8770 1.00000 0.05 0.27 0.90 C19 1.44 C21 1.49 C20 1.55 H20A Q2 1 0.3297 0.4701 1.2990 1.00000 0.05 0.23 1.53 H8 1.80 H20C 2.13 C8 2.34 H17 Q3 1 0.4500 1.2335 1.1398 1.00000 0.05 0.23 1.13 H12 1.97 C12 1.97 F1' 2.06 H10 Q4 1 -0.0202 0.4888 0.2789 1.00000 0.05 0.23 0.51 H2 1.27 C2 2.07 C1 2.08 O1 Q5 1 -0.0975 0.5208 0.5966 1.00000 0.05 0.22 1.19 H5 1.50 H3 1.71 C5 1.99 H1N Q6 1 -0.1212 0.9778 0.4814 1.00000 0.05 0.22 1.50 N1 1.63 H1N 1.90 C4 1.92 H2 Q7 1 0.2409 1.0966 0.8266 1.00000 0.05 0.21 0.62 H20A 1.44 C20 1.75 H20C 2.03 H15 Q8 1 0.2719 1.1112 1.0077 1.00000 0.05 0.20 0.54 H15 1.34 C15 2.11 C14 2.16 H14 Q9 1 0.3105 0.2117 0.7816 1.00000 0.05 0.20 1.71 H17 1.78 F1 1.95 H20C 2.18 H8 Q10 1 -0.1195 0.7228 0.2456 1.00000 0.05 0.20 1.24 C3 1.26 C4 1.82 H3 1.83 H4 Q11 1 0.3264 0.1801 0.8780 1.00000 0.05 0.20 1.21 H17 2.08 H8 2.11 C17 2.20 H15 Q12 1 0.3641 0.2889 1.3335 1.00000 0.05 0.19 1.17 H8 1.64 H17 2.00 C8 2.38 F1 Q13 1 0.3263 0.4935 0.9093 1.00000 0.05 0.19 0.46 C17 0.60 H17 1.54 C16 1.73 C18 Q14 1 0.1601 0.8379 0.8650 1.00000 0.05 0.19 0.86 O3 1.87 C21 1.87 H5 2.04 H4 Q15 1 0.4424 0.2894 1.0224 1.00000 0.05 0.19 1.38 F1' 1.67 H9 1.79 H18 1.83 H10 Q16 1 0.2750 1.1823 0.7374 1.00000 0.05 0.19 1.40 H20C 1.77 H20A 1.92 C20 2.09 F1 Q17 1 -0.0025 0.0967 0.4110 1.00000 0.05 0.19 0.89 O1 1.49 H2N 1.65 C6 2.05 H2N Q18 1 0.3916 0.1601 1.0396 1.00000 0.05 0.19 1.24 F1' 1.53 H18 1.87 H12 1.88 H9 Q19 1 0.4367 0.3559 1.3416 1.00000 0.05 0.19 1.24 H9 1.35 C9 1.59 C8 1.64 H8 Q20 1 0.4398 0.3722 1.4439 1.00000 0.05 0.19 0.46 H9 1.35 C9 2.19 F1' 2.26 C8 Shortest distances between peaks (including symmetry equivalents) 9 16 1.09 2 9 1.17 19 20 1.17 9 11 1.18 11 12 1.18 2 11 1.25 15 20 1.28 3 15 1.39 2 12 1.44 7 16 1.49 9 12 1.56 15 18 1.59 18 20 1.76 11 13 1.81 2 16 1.85 1 7 1.86 3 18 1.98 12 19 2.03 5 14 2.07 11 16 2.10 7 9 2.10 12 13 2.11 1 14 2.14 8 11 2.18 9 13 2.20 7 8 2.21 15 19 2.22 17 17 2.31 3 20 2.32 5 10 2.34 4 17 2.36 12 20 2.44 7 11 2.44 3 19 2.45 12 18 2.46 2 7 2.50 11 18 2.52 1 8 2.53 18 19 2.62 12 16 2.65 7 14 2.71 4 17 2.72 8 16 2.87 8 13 2.89 8 9 2.89 2 13 2.92 6 14 2.92 2 8 2.95 13 16 2.96 1 13 2.96 13 18 2.96 5 6 2.96 1 16 2.97 10 14 2.99 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 3.70: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.05: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.94: Structure factors and derivatives 1.56: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.45: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.16: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0405r finished at 09:25:10 Total CPU time: 7.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++