+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0063 started at 09:38:22 on 02-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0063 in P2(1)2(1)2(1) CELL 0.71073 6.1453 7.8485 27.6153 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0008 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 O F UNIT 60 60 16 4 4 V = 1331.92 F(000) = 600.0 Mu = 0.10 mm-1 Cell Wt = 1145.24 Rho = 1.428 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.03 0.08 0.11 ACTA HTAB 2.00000 BOND $H WGHT 0.01300 0.86290 L.S. 8 TEMP -153.00 FVAR 0.69381 MOLE 1 C2 1 -0.264206 0.769452 -0.364222 11.00000 0.03991 0.02860 = 0.02163 0.00525 -0.00650 -0.00188 AFIX 43 H2 2 -0.351147 0.839899 -0.384428 11.00000 -1.20000 AFIX 0 C3 1 -0.064928 0.716088 -0.381347 11.00000 0.03826 0.02301 = 0.02010 0.00231 0.00001 -0.00506 AFIX 43 H3 2 -0.012445 0.748586 -0.412359 11.00000 -1.20000 AFIX 0 C4 1 0.053487 0.613021 -0.350900 11.00000 0.03150 0.02127 = 0.02335 -0.00474 0.00215 -0.00265 AFIX 43 H4 2 0.190624 0.572289 -0.361768 11.00000 -1.20000 AFIX 0 C6 1 -0.211691 0.626223 -0.293536 11.00000 0.02566 0.01523 = 0.01929 -0.00351 -0.00202 -0.00267 C8 1 -0.145183 0.501268 -0.212998 11.00000 0.02750 0.01954 = 0.01702 0.00177 -0.00027 0.00450 AFIX 23 H8A 2 -0.012802 0.456319 -0.228941 11.00000 -1.20000 H8B 2 -0.220837 0.404827 -0.197171 11.00000 -1.20000 AFIX 0 C9 1 -0.080394 0.632370 -0.174826 11.00000 0.01793 0.02162 = 0.01698 0.00102 0.00161 0.00414 AFIX 23 H9A 2 0.004716 0.576251 -0.148901 11.00000 -1.20000 H9B 2 0.011961 0.721358 -0.189765 11.00000 -1.20000 AFIX 0 C11 1 -0.420193 0.785748 -0.191018 11.00000 0.02034 0.02265 = 0.01957 0.00164 0.00071 0.00301 AFIX 23 H11A 2 -0.344412 0.881139 -0.207321 11.00000 -1.20000 H11B 2 -0.552795 0.831536 -0.175361 11.00000 -1.20000 AFIX 0 C12 1 -0.483578 0.651553 -0.228306 11.00000 0.01966 0.02666 = 0.02015 0.00256 -0.00177 0.00031 AFIX 23 H12A 2 -0.571521 0.561413 -0.212625 11.00000 -1.20000 H12B 2 -0.572688 0.704463 -0.254111 11.00000 -1.20000 AFIX 0 C13 1 -0.362448 0.673570 -0.110063 11.00000 0.01838 0.02220 = 0.01923 -0.00004 -0.00031 -0.00035 C14 1 -0.215963 0.607880 -0.070868 11.00000 0.01902 0.02361 = 0.01632 -0.00182 0.00240 0.00144 C15 1 -0.009803 0.673637 -0.062236 11.00000 0.01994 0.02374 = 0.01712 -0.00287 0.00462 0.00047 AFIX 43 H15 2 0.049396 0.755970 -0.083739 11.00000 -1.20000 AFIX 0 C16 1 0.110759 0.620257 -0.022480 11.00000 0.01685 0.02770 = 0.02176 -0.00566 -0.00073 0.00286 AFIX 43 H16 2 0.251273 0.665847 -0.016331 11.00000 -1.20000 AFIX 0 C17 1 0.021648 0.499791 0.007750 11.00000 0.02948 0.02921 = 0.01303 -0.00237 -0.00428 0.00896 C18 1 -0.182127 0.431219 0.000452 11.00000 0.03402 0.02496 = 0.02095 0.00309 0.00146 -0.00030 AFIX 43 H18 2 -0.238915 0.347438 0.021824 11.00000 -1.20000 AFIX 0 C19 1 -0.302042 0.487737 -0.038901 11.00000 0.02251 0.02509 = 0.01976 -0.00072 0.00218 -0.00428 AFIX 43 H19 2 -0.444347 0.444243 -0.044174 11.00000 -1.20000 AFIX 0 N1 3 -0.341174 0.727080 -0.320648 11.00000 0.02861 0.02562 = 0.02030 0.00197 -0.00420 0.00212 N5 3 -0.014371 0.567227 -0.306833 11.00000 0.02882 0.01877 = 0.02069 0.00107 -0.00022 0.00156 N7 3 -0.287826 0.577039 -0.249333 11.00000 0.02415 0.02119 = 0.01594 0.00095 -0.00223 0.00335 N10 3 -0.276614 0.710786 -0.154057 11.00000 0.01819 0.02100 = 0.01652 0.00122 -0.00007 0.00257 O20 4 -0.554951 0.699530 -0.100926 11.00000 0.01569 0.05920 = 0.02557 0.00899 0.00283 0.00176 F21 5 0.138773 0.446301 0.046694 11.00000 0.04029 0.04242 = 0.02244 0.00532 -0.01008 0.00844 HKLF 4 Covalent radii and connectivity table for 2009src0063 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C2 - N1 C3 C3 - C4 C2 C4 - N5 C3 C6 - N5 N1 N7 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C13 - O20 N10 C14 C14 - C15 C19 C13 C15 - C14 C16 C16 - C17 C15 C17 - F21 C16 C18 C18 - C17 C19 C19 - C18 C14 N1 - C2 C6 N5 - C4 C6 N7 - C6 C12 C8 N10 - C13 C9 C11 O20 - C13 F21 - C17 9107 Reflections read, of which 66 rejected -6 =< h =< 7, -9 =< k =< 10, -35 =< l =< 35, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1781 Unique reflections, of which 0 suppressed R(int) = 0.0390 R(sigma) = 0.0356 Friedel opposites merged Maximum memory for data reduction = 1944 / 17345 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 = 2476 / 236722 wR2 = 0.0942 before cycle 1 for 1781 data and 190 / 190 parameters GooF = S = 1.178; Restrained GooF = 1.178 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0130 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.69272 0.00143 -0.762 OSF Mean shift/su = 0.149 Maximum = -0.762 for OSF Max. shift = 0.002 A for C19 Max. dU = 0.000 for C15 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2476 / 236722 wR2 = 0.0938 before cycle 2 for 1781 data and 190 / 190 parameters GooF = S = 1.175; Restrained GooF = 1.175 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0130 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.69235 0.00142 -0.262 OSF Mean shift/su = 0.052 Maximum = -0.262 for OSF Max. shift = 0.001 A for C19 Max. dU = 0.000 for C15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2476 / 236722 wR2 = 0.0938 before cycle 3 for 1781 data and 190 / 190 parameters GooF = S = 1.175; Restrained GooF = 1.175 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0130 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.69235 0.00142 -0.003 OSF Mean shift/su = 0.003 Maximum = -0.019 for U33 C3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2476 / 236722 wR2 = 0.0938 before cycle 4 for 1781 data and 190 / 190 parameters GooF = S = 1.175; Restrained GooF = 1.175 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0130 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.69234 0.00142 -0.001 OSF Mean shift/su = 0.001 Maximum = 0.005 for U23 C11 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C11 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2476 / 236722 wR2 = 0.0938 before cycle 5 for 1781 data and 190 / 190 parameters GooF = S = 1.175; Restrained GooF = 1.175 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0130 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.69235 0.00142 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H11B Max. dU = 0.000 for C8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2476 / 236722 wR2 = 0.0938 before cycle 6 for 1781 data and 190 / 190 parameters GooF = S = 1.175; Restrained GooF = 1.175 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0130 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.69235 0.00142 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C6 Max. shift = 0.000 A for C8 Max. dU = 0.000 for O20 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2476 / 236722 wR2 = 0.0938 before cycle 7 for 1781 data and 190 / 190 parameters GooF = S = 1.175; Restrained GooF = 1.175 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0130 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.69235 0.00142 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C6 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C3 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2476 / 236722 wR2 = 0.0938 before cycle 8 for 1781 data and 190 / 190 parameters GooF = S = 1.175; Restrained GooF = 1.175 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0130 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.69235 0.00142 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H18 Max. dU = 0.000 for N7 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.3513 0.8398 -0.3845 43 0.950 0.000 C2 N1 C3 H3 -0.0126 0.7487 -0.4124 43 0.950 0.000 C3 C4 C2 H4 0.1905 0.5720 -0.3619 43 0.950 0.000 C4 N5 C3 H8A -0.0130 0.4560 -0.2289 23 0.990 0.000 C8 N7 C9 H8B -0.2211 0.4048 -0.1972 23 0.990 0.000 C8 N7 C9 H9A 0.0049 0.5764 -0.1488 23 0.990 0.000 C9 N10 C8 H9B 0.0122 0.7215 -0.1897 23 0.990 0.000 C9 N10 C8 H11A -0.3448 0.8814 -0.2073 23 0.990 0.000 C11 N10 C12 H11B -0.5531 0.8315 -0.1753 23 0.990 0.000 C11 N10 C12 H12A -0.5715 0.5614 -0.2127 23 0.990 0.000 C12 N7 C11 H12B -0.5725 0.7044 -0.2541 23 0.990 0.000 C12 N7 C11 H15 0.0495 0.7559 -0.0837 43 0.950 0.000 C15 C14 C16 H16 0.2514 0.6659 -0.0164 43 0.950 0.000 C16 C17 C15 H18 -0.2392 0.3476 0.0218 43 0.950 0.000 C18 C17 C19 H19 -0.4439 0.4437 -0.0443 43 0.950 0.000 C19 C18 C14 2009src0063 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 -0.26428 0.76945 -0.36426 1.00000 0.03968 0.02905 0.02122 0.00497 -0.00638 -0.00151 0.02998 0.00510 0.00054 0.00039 0.00010 0.00000 0.00174 0.00151 0.00128 0.00122 0.00133 0.00147 0.00068 H2 -0.35129 0.83982 -0.38447 1.00000 0.03598 0.00000 0.00000 C3 -0.06505 0.71612 -0.38136 1.00000 0.03829 0.02192 0.02008 0.00227 -0.00065 -0.00509 0.02676 0.00482 0.00051 0.00035 0.00010 0.00000 0.00168 0.00133 0.00124 0.00114 0.00125 0.00136 0.00064 H3 -0.01257 0.74872 -0.41237 1.00000 0.03212 0.00000 0.00000 C4 0.05351 0.61292 -0.35095 1.00000 0.03141 0.02137 0.02310 -0.00461 0.00226 -0.00295 0.02529 0.00470 0.00050 0.00034 0.00009 0.00000 0.00153 0.00129 0.00127 0.00115 0.00125 0.00127 0.00061 H4 0.19052 0.57203 -0.36185 1.00000 0.03035 0.00000 0.00000 C6 -0.21187 0.62629 -0.29358 1.00000 0.02576 0.01524 0.01885 -0.00354 -0.00217 -0.00296 0.01995 0.00445 0.00047 0.00032 0.00009 0.00000 0.00137 0.00118 0.00119 0.00100 0.00111 0.00113 0.00056 C8 -0.14527 0.50114 -0.21300 1.00000 0.02745 0.01933 0.01661 0.00129 -0.00016 0.00472 0.02113 0.00458 0.00046 0.00034 0.00009 0.00000 0.00146 0.00119 0.00113 0.00106 0.00113 0.00123 0.00057 H8A -0.01297 0.45604 -0.22894 1.00000 0.02536 0.00000 0.00000 H8B -0.22108 0.40479 -0.19716 1.00000 0.02536 0.00000 0.00000 C9 -0.08016 0.63246 -0.17477 1.00000 0.01762 0.02159 0.01690 0.00076 0.00173 0.00431 0.01870 0.00451 0.00043 0.00033 0.00009 0.00000 0.00129 0.00125 0.00112 0.00104 0.00104 0.00109 0.00054 H9A 0.00491 0.57636 -0.14884 1.00000 0.02245 0.00000 0.00000 H9B 0.01217 0.72146 -0.18971 1.00000 0.02245 0.00000 0.00000 C11 -0.42042 0.78589 -0.19099 1.00000 0.02030 0.02245 0.01941 0.00142 0.00067 0.00299 0.02072 0.00446 0.00043 0.00034 0.00009 0.00000 0.00129 0.00128 0.00116 0.00109 0.00105 0.00115 0.00055 H11A -0.34477 0.88140 -0.20727 1.00000 0.02486 0.00000 0.00000 H11B -0.55310 0.83148 -0.17532 1.00000 0.02486 0.00000 0.00000 C12 -0.48350 0.65155 -0.22832 1.00000 0.01969 0.02621 0.01987 0.00232 -0.00190 -0.00031 0.02192 0.00456 0.00046 0.00034 0.00009 0.00000 0.00129 0.00131 0.00116 0.00110 0.00109 0.00124 0.00056 H12A -0.57149 0.56141 -0.21265 1.00000 0.02631 0.00000 0.00000 H12B -0.57253 0.70443 -0.25414 1.00000 0.02631 0.00000 0.00000 C13 -0.36230 0.67362 -0.11004 1.00000 0.01851 0.02186 0.01864 -0.00025 -0.00024 -0.00056 0.01967 0.00458 0.00043 0.00035 0.00009 0.00000 0.00127 0.00134 0.00117 0.00110 0.00107 0.00114 0.00055 C14 -0.21590 0.60788 -0.07086 1.00000 0.01841 0.02358 0.01599 -0.00172 0.00203 0.00091 0.01933 0.00450 0.00044 0.00034 0.00009 0.00000 0.00125 0.00127 0.00114 0.00106 0.00107 0.00116 0.00054 C15 -0.00973 0.67355 -0.06223 1.00000 0.01964 0.02309 0.01681 -0.00295 0.00472 0.00028 0.01985 0.00442 0.00044 0.00033 0.00009 0.00000 0.00128 0.00126 0.00112 0.00108 0.00105 0.00121 0.00055 H15 0.04946 0.75586 -0.08374 1.00000 0.02381 0.00000 0.00000 C16 0.11085 0.62029 -0.02252 1.00000 0.01698 0.02775 0.02174 -0.00596 -0.00033 0.00223 0.02216 0.00461 0.00044 0.00035 0.00009 0.00000 0.00131 0.00144 0.00126 0.00115 0.00109 0.00120 0.00059 H16 0.25137 0.66589 -0.01638 1.00000 0.02659 0.00000 0.00000 C17 0.02161 0.49965 0.00776 1.00000 0.02920 0.02852 0.01287 -0.00234 -0.00410 0.00908 0.02353 0.00478 0.00049 0.00036 0.00009 0.00000 0.00148 0.00135 0.00108 0.00108 0.00114 0.00135 0.00059 C18 -0.18224 0.43120 0.00043 1.00000 0.03360 0.02478 0.02078 0.00269 0.00162 -0.00068 0.02639 0.00485 0.00048 0.00036 0.00010 0.00000 0.00160 0.00137 0.00128 0.00118 0.00125 0.00135 0.00063 H18 -0.23923 0.34757 0.02183 1.00000 0.03166 0.00000 0.00000 C19 -0.30178 0.48751 -0.03892 1.00000 0.02274 0.02464 0.02016 -0.00051 0.00199 -0.00437 0.02251 0.00471 0.00047 0.00035 0.00009 0.00000 0.00147 0.00136 0.00124 0.00110 0.00113 0.00125 0.00060 H19 -0.44389 0.44374 -0.04426 1.00000 0.02702 0.00000 0.00000 N1 -0.34119 0.72709 -0.32063 1.00000 0.02841 0.02562 0.02000 0.00180 -0.00455 0.00223 0.02468 0.00397 0.00039 0.00030 0.00008 0.00000 0.00126 0.00117 0.00107 0.00098 0.00101 0.00109 0.00052 N5 -0.01439 0.56725 -0.30681 1.00000 0.02827 0.01851 0.02050 0.00091 -0.00012 0.00166 0.02243 0.00390 0.00041 0.00027 0.00008 0.00000 0.00124 0.00101 0.00101 0.00092 0.00101 0.00106 0.00049 N7 -0.28775 0.57698 -0.24933 1.00000 0.02397 0.02113 0.01567 0.00105 -0.00221 0.00329 0.02026 0.00374 0.00037 0.00027 0.00007 0.00000 0.00119 0.00110 0.00098 0.00091 0.00094 0.00102 0.00049 N10 -0.27670 0.71072 -0.15406 1.00000 0.01763 0.02089 0.01662 0.00149 0.00009 0.00250 0.01838 0.00370 0.00035 0.00027 0.00007 0.00000 0.00104 0.00104 0.00095 0.00090 0.00089 0.00097 0.00045 O20 -0.55498 0.69949 -0.10093 1.00000 0.01537 0.05905 0.02543 0.00885 0.00288 0.00218 0.03328 0.00378 0.00031 0.00031 0.00007 0.00000 0.00097 0.00147 0.00099 0.00104 0.00080 0.00109 0.00054 F21 0.13878 0.44626 0.04670 1.00000 0.04020 0.04249 0.02220 0.00519 -0.01017 0.00849 0.03496 0.00310 0.00031 0.00023 0.00006 0.00000 0.00104 0.00103 0.00079 0.00077 0.00079 0.00090 0.00045 Final Structure Factor Calculation for 2009src0063 in P2(1)2(1)2(1) Total number of l.s. parameters = 190 Maximum vector length = 511 Memory required = 2288 / 26068 wR2 = 0.0938 before cycle 9 for 1781 data and 2 / 190 parameters GooF = S = 1.175; Restrained GooF = 1.175 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0130 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0467 for 1611 Fo > 4sig(Fo) and 0.0550 for all 1781 data wR2 = 0.0938, GooF = S = 1.175, Restrained GooF = 1.175 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0424 0.0300 0.0176 C2 0.0398 0.0222 0.0182 C3 0.0335 0.0249 0.0175 C4 0.0268 0.0210 0.0121 C6 0.0296 0.0182 0.0156 C8 0.0247 0.0171 0.0144 C9 0.0250 0.0191 0.0181 C11 0.0271 0.0211 0.0176 C12 0.0220 0.0188 0.0182 C13 0.0240 0.0196 0.0144 C14 0.0249 0.0219 0.0127 C15 0.0317 0.0185 0.0163 C16 0.0388 0.0199 0.0119 C17 0.0338 0.0261 0.0192 C18 0.0285 0.0208 0.0183 C19 0.0308 0.0260 0.0172 N1 0.0285 0.0208 0.0179 N5 0.0263 0.0199 0.0145 N7 0.0226 0.0169 0.0157 N10 0.0614 0.0238 0.0146 O20 0.0503 0.0395 0.0151 F21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.027 0.036 0.046 0.056 0.069 0.085 0.109 0.156 1.000 Number in group 180. 180. 183. 180. 167. 185. 173. 177. 178. 178. GooF 1.251 1.279 1.220 1.202 1.209 1.212 1.065 1.019 1.050 1.200 K 1.522 1.138 1.030 1.006 1.000 1.005 0.996 1.006 1.004 0.998 Resolution(A) 0.77 0.80 0.84 0.87 0.93 0.98 1.07 1.18 1.37 1.76 inf Number in group 182. 182. 172. 176. 180. 179. 175. 179. 177. 179. GooF 1.233 1.307 1.285 1.198 1.111 1.152 1.028 0.875 1.153 1.329 K 1.060 1.074 1.001 1.003 1.006 0.982 0.991 0.999 1.030 0.994 R1 0.129 0.137 0.109 0.087 0.062 0.050 0.033 0.031 0.032 0.024 Recommended weighting scheme: WGHT 0.0114 1.0840 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) 3 0 2 14.24 4.17 3.32 0.014 2.03 4 0 0 581.89 480.74 3.21 0.152 1.54 0 1 2 422.13 503.97 3.18 0.155 6.82 6 4 19 11.13 35.51 3.08 0.041 0.77 3 8 13 17.41 41.92 3.01 0.045 0.82 4 2 26 45.54 76.56 2.96 0.061 0.85 3 3 5 843.92 740.43 2.91 0.188 1.55 3 4 27 -4.94 10.09 2.84 0.022 0.83 5 3 25 62.83 32.17 2.84 0.039 0.78 1 9 14 30.61 9.38 2.83 0.021 0.79 7 3 10 58.81 103.67 2.78 0.071 0.80 0 4 1 7.69 1.45 2.76 0.008 1.96 5 2 18 41.79 18.74 2.76 0.030 0.93 6 0 23 28.58 57.36 2.74 0.052 0.78 1 5 29 37.35 15.93 2.72 0.028 0.81 0 0 32 0.46 15.30 2.52 0.027 0.86 0 8 10 16.48 4.19 2.51 0.014 0.92 5 3 21 2.06 15.48 2.49 0.027 0.85 1 4 30 11.13 28.72 2.48 0.037 0.83 7 3 3 -0.55 8.80 2.47 0.021 0.83 1 6 13 55.39 81.26 2.45 0.062 1.10 5 4 5 245.67 201.32 2.45 0.098 1.02 0 3 24 20.90 40.22 2.44 0.044 1.05 0 2 23 -2.27 3.66 2.42 0.013 1.15 3 7 17 104.95 139.07 2.42 0.082 0.84 3 0 30 78.59 111.19 2.38 0.073 0.84 0 7 17 16.07 0.24 2.37 0.003 0.92 1 4 29 9.51 25.14 2.37 0.035 0.85 3 1 11 334.88 288.39 2.33 0.118 1.56 4 3 25 -0.53 8.38 2.33 0.020 0.85 7 1 4 59.75 84.87 2.32 0.064 0.87 1 7 19 9.60 22.96 2.32 0.033 0.88 3 6 10 1.85 9.31 2.31 0.021 1.02 1 4 27 25.82 45.88 2.30 0.047 0.90 4 2 7 103.24 78.39 2.28 0.061 1.34 2 6 15 3.53 13.75 2.27 0.026 1.01 0 2 30 18.98 6.59 2.27 0.018 0.90 1 3 25 54.89 78.71 2.25 0.061 1.00 7 1 5 67.64 92.76 2.24 0.067 0.86 3 4 22 174.83 214.96 2.24 0.102 0.94 2 0 1 798.60 880.50 2.23 0.206 3.05 0 0 34 -8.26 6.49 2.22 0.018 0.81 2 1 9 1632.08 1508.48 2.22 0.269 2.09 1 1 13 283.06 243.24 2.21 0.108 1.95 0 6 14 21.06 6.88 2.21 0.018 1.09 4 0 25 22.93 4.63 2.21 0.015 0.90 1 3 32 37.99 58.57 2.19 0.053 0.81 3 2 12 54.81 38.79 2.18 0.043 1.43 2 9 14 0.12 9.18 2.18 0.021 0.77 0 7 20 111.65 80.53 2.17 0.062 0.87 Bond lengths and angles C2 - Distance Angles N1 1.3361 (0.0034) C3 1.3774 (0.0044) 123.23 (0.28) H2 0.9500 118.38 118.38 C2 - N1 C3 C3 - Distance Angles C4 1.3756 (0.0039) C2 1.3774 (0.0044) 116.12 (0.26) H3 0.9500 121.94 121.94 C3 - C4 C2 C4 - Distance Angles N5 1.3373 (0.0033) C3 1.3756 (0.0039) 123.30 (0.28) H4 0.9500 118.35 118.35 C4 - N5 C3 C6 - Distance Angles N5 1.3494 (0.0036) N1 1.3475 (0.0034) 125.58 (0.24) N7 1.3640 (0.0031) 116.91 (0.24) 117.50 (0.25) C6 - N5 N1 C8 - Distance Angles N7 1.4586 (0.0031) C9 1.5286 (0.0035) 110.91 (0.21) H8A 0.9900 109.46 109.46 H8B 0.9900 109.46 109.46 108.05 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4708 (0.0032) C8 1.5286 (0.0035) 109.58 (0.21) H9A 0.9900 109.75 109.75 H9B 0.9900 109.75 109.75 108.22 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4725 (0.0032) C12 1.5246 (0.0035) 110.10 (0.21) H11A 0.9900 109.64 109.64 H11B 0.9900 109.64 109.64 108.15 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4581 (0.0034) C11 1.5246 (0.0035) 109.69 (0.22) H12A 0.9900 109.73 109.73 H12B 0.9900 109.73 109.73 108.21 C12 - N7 C11 H12A C13 - Distance Angles O20 1.2275 (0.0032) N10 1.3561 (0.0031) 121.50 (0.25) C14 1.4988 (0.0036) 119.21 (0.24) 119.22 (0.23) C13 - O20 N10 C14 - Distance Angles C15 1.3884 (0.0037) C19 1.3961 (0.0036) 119.18 (0.25) C13 1.4988 (0.0036) 122.96 (0.24) 117.52 (0.24) C14 - C15 C19 C15 - Distance Angles C14 1.3884 (0.0037) C16 1.3879 (0.0036) 120.74 (0.25) H15 0.9500 119.63 119.63 C15 - C14 C16 C16 - Distance Angles C17 1.3771 (0.0039) C15 1.3879 (0.0036) 118.30 (0.26) H16 0.9500 120.85 120.85 C16 - C17 C15 C17 - Distance Angles F21 1.3603 (0.0029) C16 1.3771 (0.0039) 118.75 (0.26) C18 1.3780 (0.0040) 118.50 (0.26) 122.75 (0.25) C17 - F21 C16 C18 - Distance Angles C17 1.3780 (0.0040) C19 1.3842 (0.0038) 118.24 (0.26) H18 0.9500 120.88 120.88 C18 - C17 C19 C19 - Distance Angles C18 1.3842 (0.0038) C14 1.3961 (0.0036) 120.76 (0.27) H19 0.9500 119.62 119.62 C19 - C18 C14 N1 - Distance Angles C2 1.3361 (0.0034) C6 1.3475 (0.0034) 115.94 (0.25) N1 - C2 N5 - Distance Angles C4 1.3373 (0.0033) C6 1.3494 (0.0036) 115.81 (0.24) N5 - C4 N7 - Distance Angles C6 1.3640 (0.0031) C12 1.4581 (0.0034) 121.64 (0.22) C8 1.4586 (0.0031) 121.79 (0.23) 112.67 (0.19) N7 - C6 C12 N10 - Distance Angles C13 1.3561 (0.0031) C9 1.4708 (0.0032) 125.27 (0.21) C11 1.4725 (0.0032) 118.30 (0.22) 112.99 (0.19) N10 - C13 C9 O20 - Distance Angles C13 1.2275 (0.0032) O20 - F21 - Distance Angles C17 1.3603 (0.0029) F21 - FMAP and GRID set by program FMAP 2 3 32 GRID -0.862 -2 -2 0.862 2 2 R1 = 0.0550 for 1781 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.22 at 0.1513 0.7546 0.1728 [ 0.73 A from N10 ] Deepest hole -0.25 at 0.0566 0.5909 0.0289 [ 0.95 A from C17 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2136 / 16471 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.3487 0.7454 -0.1728 1.00000 0.05 0.22 0.73 N10 0.74 C11 1.43 H11B 1.43 H11A Q2 1 0.0010 0.7212 -0.3608 1.00000 0.05 0.22 0.70 C3 0.95 C4 1.44 H3 1.65 H4 Q3 1 -0.6172 0.7002 -0.1418 1.00000 0.05 0.19 1.19 O20 1.44 H11B 1.81 C13 1.94 C11 Q4 1 -0.4373 0.5359 -0.2965 1.00000 0.05 0.19 1.56 C6 1.63 N7 1.75 N1 1.78 H11B Q5 1 -0.0063 0.6875 -0.0322 1.00000 0.05 0.19 0.84 C15 0.93 C16 1.56 H15 1.65 H16 Q6 1 -0.1264 0.6250 -0.0648 1.00000 0.05 0.18 0.59 C14 0.81 C15 1.58 H15 1.68 C19 Q7 1 -0.6671 0.5476 -0.1630 1.00000 0.05 0.17 1.50 H12A 2.07 H9A 2.09 H2 2.20 O20 Q8 1 0.1070 0.4905 -0.2843 1.00000 0.05 0.17 1.14 N5 1.71 H11A 1.72 H8A 2.10 C4 Q9 1 -0.1133 0.5622 -0.1981 1.00000 0.05 0.17 0.66 C8 0.87 C9 1.34 H8A 1.40 H8B Q10 1 -0.5573 0.5380 -0.2016 1.00000 0.05 0.17 0.37 H12A 1.24 C12 1.95 H12B 2.14 N7 Shortest distances between peaks (including symmetry equivalents) 5 6 1.26 7 10 1.26 3 7 1.37 1 3 1.89 3 10 2.12 1 9 2.16 1 10 2.22 1 7 2.51 1 8 2.70 4 10 2.72 9 10 2.74 1 4 2.77 8 9 2.80 4 8 2.84 2 8 2.86 7 9 2.91 Time profile in seconds ----------------------- 0.00: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.44: 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 1.09: Structure factors and derivatives 0.86: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0063 finished at 09:38:25 Total CPU time: 2.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++