+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1544 started at 17:29:55 on 06-Dec-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1544 in P2(1)/n CELL 0.71073 8.4959 19.0544 13.9272 90.000 104.775 90.000 ZERR 4.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N BR AG UNIT 92 120 8 4 4 V = 2180.05 F(000) = 1056.0 Mu = 2.77 mm-1 Cell Wt = 2089.08 Rho = 1.591 MERG 2 OMIT -3.00 55.00 OMIT -1 4 2 OMIT -2 4 1 OMIT 2 2 3 OMIT 1 2 4 OMIT 2 4 3 OMIT 0 4 5 OMIT -2 4 3 OMIT 2 4 1 OMIT 0 2 5 EXTI 0.00654 FMAP 2 PLAN 20 SIZE 0.10 0.20 0.40 ACTA BOND WGHT 0.14510 30.81790 L.S. 4 TEMP -153.00 FVAR 0.40238 C1 1 0.362942 0.103959 0.227205 11.00000 0.00872 0.01262 = 0.00994 -0.00032 0.00207 -0.00221 C2 1 0.475483 -0.001848 0.337845 11.00000 0.01510 0.01133 = 0.01704 0.00573 0.00576 0.00456 AFIX 23 H2A 2 0.404551 -0.043160 0.316427 11.00000 -1.20000 H2B 2 0.515357 -0.003486 0.411091 11.00000 -1.20000 AFIX 0 C3 1 0.620441 -0.005757 0.291968 11.00000 0.01324 0.01605 = 0.01889 0.00247 0.00615 0.00713 AFIX 23 H3A 2 0.703528 -0.037648 0.332232 11.00000 -1.20000 H3B 2 0.669880 0.041428 0.293742 11.00000 -1.20000 AFIX 0 C4 1 0.572159 -0.032011 0.184601 11.00000 0.02593 0.01170 = 0.02510 -0.00328 0.01147 0.00568 AFIX 23 H4A 2 0.656851 -0.018463 0.150726 11.00000 -1.20000 H4B 2 0.564601 -0.083863 0.184079 11.00000 -1.20000 AFIX 0 C5 1 0.409438 -0.001097 0.129136 11.00000 0.02454 0.01294 = 0.01510 -0.00369 0.00404 0.00024 AFIX 23 H5A 2 0.392989 -0.009683 0.057144 11.00000 -1.20000 H5B 2 0.321196 -0.025432 0.150555 11.00000 -1.20000 AFIX 0 C6 1 0.297763 0.087809 0.381985 11.00000 0.01216 0.00975 = 0.00956 0.00457 0.00580 0.00280 C7 1 0.137563 0.064957 0.372799 11.00000 0.01342 0.01451 = 0.02039 0.00476 0.00832 0.00412 C8 1 0.049717 0.021326 0.285629 11.00000 0.01550 0.02837 = 0.02344 -0.00230 0.00557 -0.00664 AFIX 137 H8A 2 -0.055829 0.006568 0.295050 11.00000 -1.50000 H8B 2 0.115027 -0.020205 0.280333 11.00000 -1.50000 H8C 2 0.032688 0.049171 0.224678 11.00000 -1.50000 AFIX 0 C9 1 0.060914 0.085809 0.445863 11.00000 0.01455 0.02519 = 0.02126 0.00981 0.01108 0.00627 AFIX 43 H9 2 -0.047175 0.070439 0.441122 11.00000 -1.20000 AFIX 0 C10 1 0.137606 0.128300 0.525258 11.00000 0.03149 0.01596 = 0.02080 0.00824 0.01601 0.01174 C11 1 0.050209 0.150463 0.601606 11.00000 0.03996 0.02838 = 0.02814 0.00763 0.02400 0.01172 AFIX 137 H11A 2 -0.048657 0.122245 0.593984 11.00000 -1.50000 H11B 2 0.020778 0.200185 0.592312 11.00000 -1.50000 H11C 2 0.121571 0.143396 0.668260 11.00000 -1.50000 AFIX 0 C12 1 0.298238 0.149504 0.532677 11.00000 0.02616 0.01312 = 0.01384 0.00224 0.00767 0.00192 AFIX 43 H12 2 0.351974 0.178477 0.586610 11.00000 -1.20000 AFIX 0 C13 1 0.381547 0.128929 0.462286 11.00000 0.01701 0.01138 = 0.01539 0.00182 0.00597 0.00044 C14 1 0.555776 0.150798 0.473188 11.00000 0.02060 0.02474 = 0.01956 -0.00460 0.00556 -0.01023 AFIX 137 H14A 2 0.581089 0.191393 0.517670 11.00000 -1.50000 H14B 2 0.571087 0.163387 0.407944 11.00000 -1.50000 H14C 2 0.628402 0.111830 0.501035 11.00000 -1.50000 AFIX 0 C15 1 0.384565 0.121774 0.060343 11.00000 0.01460 0.01237 = 0.00655 -0.00292 0.00359 0.00013 C16 1 0.527486 0.149273 0.041279 11.00000 0.02114 0.01299 = 0.01050 -0.00499 0.00831 -0.00355 C17 1 0.693591 0.132941 0.105115 11.00000 0.01664 0.02077 = 0.01821 -0.00396 0.00521 -0.00587 AFIX 137 H17A 2 0.732335 0.088843 0.083053 11.00000 -1.50000 H17B 2 0.688710 0.128311 0.174377 11.00000 -1.50000 H17C 2 0.768519 0.170973 0.099726 11.00000 -1.50000 AFIX 0 C18 1 0.508665 0.193546 -0.041016 11.00000 0.02609 0.01389 = 0.01213 -0.00293 0.00728 -0.00380 AFIX 43 H18 2 0.602804 0.213497 -0.055083 11.00000 -1.20000 AFIX 0 C19 1 0.357087 0.209237 -0.102688 11.00000 0.03528 0.01165 = 0.01164 -0.00125 0.00940 0.00388 C20 1 0.341959 0.258117 -0.190386 11.00000 0.04786 0.02172 = 0.01781 0.00613 0.00902 -0.00085 AFIX 137 H20A 2 0.227093 0.262655 -0.226205 11.00000 -1.50000 H20B 2 0.403549 0.238943 -0.235057 11.00000 -1.50000 H20C 2 0.385450 0.304368 -0.166617 11.00000 -1.50000 AFIX 0 C21 1 0.219391 0.178110 -0.084072 11.00000 0.02173 0.01816 = 0.01295 -0.00205 0.00270 0.00761 AFIX 43 H21 2 0.115787 0.186960 -0.127970 11.00000 -1.20000 AFIX 0 C22 1 0.230137 0.134694 -0.003265 11.00000 0.01977 0.01544 = 0.01510 -0.00108 0.00506 0.00216 C23 1 0.079111 0.103080 0.016171 11.00000 0.01398 0.03647 = 0.02650 0.00826 0.00144 -0.00097 AFIX 137 H23A 2 0.067298 0.119051 0.080857 11.00000 -1.50000 H23B 2 0.087686 0.051789 0.016273 11.00000 -1.50000 H23C 2 -0.016112 0.117790 -0.035947 11.00000 -1.50000 AFIX 0 N1 3 0.378017 0.063690 0.308354 11.00000 0.01286 0.00675 = 0.01081 0.00324 0.00534 0.00224 N2 3 0.397781 0.075871 0.146234 11.00000 0.01567 0.01020 = 0.00823 0.00094 0.00439 0.00007 BR1 4 0.241471 0.329684 0.259209 11.00000 0.05621 0.03571 = 0.04765 0.00136 0.01476 0.00715 AG1 5 0.298903 0.209766 0.234763 11.00000 0.01538 0.01057 = 0.01165 0.00138 0.00492 0.00313 HKLF 4 Covalent radii and connectivity table for 2007src1544 in P2(1)/n C 0.770 H 0.320 N 0.700 BR 1.140 AG 1.440 C1 - N1 N2 Ag1 C2 - N1 C3 C3 - C2 C4 C4 - C5 C3 C5 - N2 C4 C6 - C13 C7 N1 C7 - C9 C6 C8 C8 - C7 C9 - C10 C7 C10 - C9 C12 C11 C11 - C10 C12 - C10 C13 C13 - C6 C12 C14 C14 - C13 C15 - C22 C16 N2 C16 - C18 C15 C17 C17 - C16 C18 - C19 C16 C19 - C18 C21 C20 C20 - C19 C21 - C22 C19 C22 - C21 C15 C23 C23 - C22 N1 - C1 C6 C2 N2 - C1 C15 C5 Br1 - Ag1 Ag1 - C1 Br1 h k l Fo^2 Sigma Why rejected -2 0 1 28.98 6.08 observed but should be systematically absent 2 0 1 5.67 0.94 observed but should be systematically absent 30125 Reflections read, of which 542 rejected -11 =< h =< 10, -23 =< k =< 24, -18 =< l =< 17, Max. 2-theta = 55.00 2 Systematic absence violations 0 Inconsistent equivalents 4970 Unique reflections, of which 0 suppressed R(int) = 0.0353 R(sigma) = 0.0268 Friedel opposites merged Maximum memory for data reduction = 2613 / 49713 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 = 3341 / 312667 wR2 = 0.2322 before cycle 1 for 4970 data and 251 / 251 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1451 * P )^2 + 30.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40200 0.00201 -0.192 OSF 2 0.00647 0.00119 -0.060 EXTI Mean shift/esd = 0.031 Maximum = -0.284 for U22 Br1 Max. shift = 0.010 A for H8C Max. dU = 0.000 for Br1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3341 / 312667 wR2 = 0.2322 before cycle 2 for 4970 data and 251 / 251 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1451 * P )^2 + 30.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40195 0.00200 -0.020 OSF 2 0.00645 0.00118 -0.013 EXTI Mean shift/esd = 0.013 Maximum = -0.143 for U22 Br1 Max. shift = 0.006 A for H8C Max. dU = 0.000 for Br1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3341 / 312667 wR2 = 0.2322 before cycle 3 for 4970 data and 251 / 251 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1451 * P )^2 + 30.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40195 0.00200 -0.004 OSF 2 0.00645 0.00118 0.002 EXTI Mean shift/esd = 0.002 Maximum = -0.024 for U22 Br1 Max. shift = 0.001 A for H8C Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3341 / 312667 wR2 = 0.2322 before cycle 4 for 4970 data and 251 / 251 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1451 * P )^2 + 30.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40194 0.00200 -0.001 OSF 2 0.00646 0.00118 0.002 EXTI Mean shift/esd = 0.001 Maximum = -0.006 for tors H14A Max. shift = 0.000 A for H20C Max. dU = 0.000 for C11 Largest correlation matrix elements 0.671 U33 Ag1 / OSF 0.669 U22 Ag1 / OSF 0.532 U13 C11 / U11 C11 0.671 U11 Ag1 / OSF 0.629 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.4046 -0.0432 0.3164 23 0.990 0.000 C2 N1 C3 H2B 0.5153 -0.0035 0.4111 23 0.990 0.000 C2 N1 C3 H3A 0.7037 -0.0376 0.3322 23 0.990 0.000 C3 C2 C4 H3B 0.6699 0.0415 0.2937 23 0.990 0.000 C3 C2 C4 H4A 0.6569 -0.0185 0.1507 23 0.990 0.000 C4 C5 C3 H4B 0.5647 -0.0839 0.1841 23 0.990 0.000 C4 C5 C3 H5A 0.3929 -0.0097 0.0571 23 0.990 0.000 C5 N2 C4 H5B 0.3212 -0.0254 0.1505 23 0.990 0.000 C5 N2 C4 H8A -0.0550 0.0059 0.2957 137 0.980 0.000 C8 C7 H8A H8B 0.1159 -0.0197 0.2795 137 0.980 0.000 C8 C7 H8A H8C 0.0308 0.0495 0.2249 137 0.980 0.000 C8 C7 H8A H9 -0.0471 0.0704 0.4412 43 0.950 0.000 C9 C10 C7 H11A -0.0483 0.1222 0.5942 137 0.980 0.000 C11 C10 H11A H11B 0.0207 0.2002 0.5922 137 0.980 0.000 C11 C10 H11A H11C 0.1220 0.1436 0.6682 137 0.980 0.000 C11 C10 H11A H12 0.3519 0.1785 0.5866 43 0.950 0.000 C12 C10 C13 H14A 0.5808 0.1916 0.5173 137 0.980 0.000 C14 C13 H14A H14B 0.5711 0.1631 0.4078 137 0.980 0.000 C14 C13 H14A H14C 0.6284 0.1119 0.5014 137 0.980 0.000 C14 C13 H14A H17A 0.7323 0.0889 0.0831 137 0.980 0.000 C17 C16 H17A H17B 0.6886 0.1283 0.1744 137 0.980 0.000 C17 C16 H17A H17C 0.7685 0.1710 0.0998 137 0.980 0.000 C17 C16 H17A H18 0.6027 0.2135 -0.0551 43 0.950 0.000 C18 C19 C16 H20A 0.2269 0.2624 -0.2264 137 0.980 0.000 C20 C19 H20A H20B 0.4038 0.2391 -0.2350 137 0.980 0.000 C20 C19 H20A H20C 0.3846 0.3045 -0.1667 137 0.980 0.000 C20 C19 H20A H21 0.1157 0.1870 -0.1280 43 0.950 0.000 C21 C22 C19 H23A 0.0674 0.1191 0.0809 137 0.980 0.000 C23 C22 H23A H23B 0.0878 0.0518 0.0164 137 0.980 0.000 C23 C22 H23A H23C -0.0161 0.1178 -0.0359 137 0.980 0.000 C23 C22 H23A 2007src1544 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.36304 0.10402 0.22718 1.00000 0.00882 0.01281 0.00987 -0.00033 0.00216 -0.00237 0.01054 0.01105 0.00070 0.00032 0.00043 0.00000 0.00254 0.00273 0.00259 0.00211 0.00203 0.00205 0.00108 C2 0.47549 -0.00186 0.33785 1.00000 0.01510 0.01151 0.01707 0.00575 0.00578 0.00462 0.01425 0.01291 0.00076 0.00033 0.00048 0.00000 0.00282 0.00275 0.00295 0.00230 0.00230 0.00224 0.00118 H2A 0.40458 -0.04317 0.31642 1.00000 0.01710 0.00000 0.00000 H2B 0.51535 -0.00350 0.41110 1.00000 0.01710 0.00000 0.00000 C3 0.62056 -0.00573 0.29196 1.00000 0.01320 0.01599 0.01886 0.00244 0.00617 0.00706 0.01564 0.01317 0.00077 0.00035 0.00049 0.00000 0.00279 0.00294 0.00308 0.00241 0.00233 0.00228 0.00121 H3A 0.70368 -0.03761 0.33222 1.00000 0.01877 0.00000 0.00000 H3B 0.66994 0.04146 0.29371 1.00000 0.01877 0.00000 0.00000 C4 0.57222 -0.03201 0.18459 1.00000 0.02590 0.01175 0.02526 -0.00320 0.01140 0.00588 0.02009 0.01405 0.00088 0.00036 0.00054 0.00000 0.00343 0.00288 0.00348 0.00253 0.00281 0.00253 0.00136 H4A 0.65688 -0.01846 0.15069 1.00000 0.02410 0.00000 0.00000 H4B 0.56469 -0.08386 0.18408 1.00000 0.02410 0.00000 0.00000 C5 0.40940 -0.00111 0.12911 1.00000 0.02443 0.01324 0.01500 -0.00368 0.00396 0.00023 0.01775 0.01274 0.00086 0.00035 0.00049 0.00000 0.00335 0.00294 0.00297 0.00237 0.00251 0.00248 0.00128 H5A 0.39293 -0.00968 0.05712 1.00000 0.02130 0.00000 0.00000 H5B 0.32118 -0.02545 0.15055 1.00000 0.02130 0.00000 0.00000 C6 0.29776 0.08782 0.38200 1.00000 0.01213 0.00984 0.00947 0.00459 0.00573 0.00281 0.00994 0.01179 0.00072 0.00030 0.00043 0.00000 0.00268 0.00261 0.00255 0.00201 0.00209 0.00205 0.00109 C7 0.13755 0.06494 0.37279 1.00000 0.01330 0.01472 0.02066 0.00495 0.00839 0.00436 0.01549 0.01342 0.00078 0.00034 0.00051 0.00000 0.00285 0.00288 0.00307 0.00240 0.00238 0.00229 0.00122 C8 0.04969 0.02139 0.28564 1.00000 0.01537 0.02834 0.02335 -0.00205 0.00570 -0.00665 0.02221 0.01355 0.00085 0.00040 0.00056 0.00000 0.00303 0.00379 0.00352 0.00276 0.00261 0.00262 0.00144 H8A -0.05496 0.00590 0.29566 1.00000 0.03332 0.00000 0.00000 H8B 0.11589 -0.01968 0.27954 1.00000 0.03332 0.00000 0.00000 H8C 0.03083 0.04955 0.22489 1.00000 0.03332 0.00000 0.00000 C9 0.06094 0.08578 0.44591 1.00000 0.01464 0.02531 0.02118 0.00971 0.01111 0.00649 0.01919 0.01466 0.00082 0.00038 0.00052 0.00000 0.00297 0.00352 0.00326 0.00263 0.00254 0.00249 0.00136 H9 -0.04709 0.07035 0.44124 1.00000 0.02302 0.00000 0.00000 C10 0.13757 0.12831 0.52520 1.00000 0.03149 0.01626 0.02092 0.00812 0.01602 0.01173 0.02119 0.01564 0.00094 0.00037 0.00053 0.00000 0.00374 0.00315 0.00327 0.00254 0.00286 0.00273 0.00142 C11 0.05040 0.15052 0.60163 1.00000 0.03991 0.02846 0.02806 0.00756 0.02389 0.01175 0.02938 0.01857 0.00109 0.00044 0.00062 0.00000 0.00443 0.00395 0.00386 0.00307 0.00347 0.00333 0.00172 H11A -0.04829 0.12222 0.59424 1.00000 0.04406 0.00000 0.00000 H11B 0.02070 0.20021 0.59219 1.00000 0.04406 0.00000 0.00000 H11C 0.12200 0.14360 0.66825 1.00000 0.04406 0.00000 0.00000 C12 0.29822 0.14952 0.53267 1.00000 0.02614 0.01310 0.01378 0.00219 0.00759 0.00179 0.01722 0.01341 0.00087 0.00034 0.00049 0.00000 0.00337 0.00292 0.00289 0.00227 0.00250 0.00248 0.00126 H12 0.35193 0.17849 0.58661 1.00000 0.02066 0.00000 0.00000 C13 0.38155 0.12894 0.46228 1.00000 0.01692 0.01149 0.01557 0.00182 0.00590 0.00042 0.01434 0.01252 0.00078 0.00033 0.00048 0.00000 0.00294 0.00277 0.00287 0.00224 0.00234 0.00226 0.00118 C14 0.55569 0.15079 0.47314 1.00000 0.02047 0.02484 0.01956 -0.00460 0.00556 -0.01034 0.02154 0.01301 0.00087 0.00040 0.00054 0.00000 0.00333 0.00355 0.00321 0.00265 0.00258 0.00270 0.00141 H14A 0.58084 0.19157 0.51729 1.00000 0.03231 0.00000 0.00000 H14B 0.57114 0.16309 0.40783 1.00000 0.03231 0.00000 0.00000 H14C 0.62835 0.11192 0.50137 1.00000 0.03231 0.00000 0.00000 C15 0.38450 0.12180 0.06032 1.00000 0.01442 0.01247 0.00659 -0.00293 0.00354 0.00001 0.01100 0.01129 0.00074 0.00032 0.00042 0.00000 0.00275 0.00271 0.00246 0.00206 0.00209 0.00216 0.00109 C16 0.52754 0.14928 0.04126 1.00000 0.02114 0.01307 0.01050 -0.00492 0.00822 -0.00363 0.01415 0.01197 0.00081 0.00033 0.00046 0.00000 0.00310 0.00279 0.00266 0.00220 0.00230 0.00233 0.00118 C17 0.69358 0.13295 0.10511 1.00000 0.01667 0.02081 0.01843 -0.00387 0.00536 -0.00584 0.01848 0.01265 0.00082 0.00037 0.00051 0.00000 0.00299 0.00326 0.00307 0.00250 0.00245 0.00246 0.00129 H17A 0.73235 0.08885 0.08306 1.00000 0.02772 0.00000 0.00000 H17B 0.68864 0.12831 0.17437 1.00000 0.02772 0.00000 0.00000 H17C 0.76851 0.17098 0.09975 1.00000 0.02772 0.00000 0.00000 C18 0.50863 0.19356 -0.04103 1.00000 0.02619 0.01391 0.01212 -0.00301 0.00743 -0.00385 0.01694 0.01289 0.00089 0.00035 0.00048 0.00000 0.00340 0.00287 0.00291 0.00232 0.00252 0.00254 0.00125 H18 0.60274 0.21355 -0.05509 1.00000 0.02033 0.00000 0.00000 C19 0.35707 0.20923 -0.10267 1.00000 0.03563 0.01181 0.01157 -0.00113 0.00946 0.00381 0.01905 0.01424 0.00100 0.00033 0.00051 0.00000 0.00402 0.00300 0.00293 0.00217 0.00276 0.00250 0.00140 C20 0.34175 0.25812 -0.19045 1.00000 0.04786 0.02185 0.01783 0.00599 0.00896 -0.00094 0.02908 0.01641 0.00114 0.00042 0.00056 0.00000 0.00483 0.00364 0.00336 0.00278 0.00320 0.00330 0.00168 H20A 0.22692 0.26241 -0.22644 1.00000 0.04362 0.00000 0.00000 H20B 0.40382 0.23910 -0.23495 1.00000 0.04362 0.00000 0.00000 H20C 0.38461 0.30447 -0.16668 1.00000 0.04362 0.00000 0.00000 C21 0.21933 0.17812 -0.08408 1.00000 0.02165 0.01812 0.01295 -0.00214 0.00263 0.00777 0.01790 0.01323 0.00086 0.00036 0.00049 0.00000 0.00323 0.00316 0.00290 0.00237 0.00243 0.00250 0.00130 H21 0.11573 0.18698 -0.12797 1.00000 0.02148 0.00000 0.00000 C22 0.23012 0.13471 -0.00329 1.00000 0.01984 0.01537 0.01512 -0.00109 0.00511 0.00210 0.01666 0.01299 0.00083 0.00035 0.00049 0.00000 0.00314 0.00300 0.00296 0.00234 0.00245 0.00241 0.00126 C23 0.07918 0.10310 0.01621 1.00000 0.01380 0.03629 0.02670 0.00845 0.00125 -0.00094 0.02631 0.01527 0.00085 0.00046 0.00059 0.00000 0.00318 0.00420 0.00367 0.00316 0.00270 0.00285 0.00157 H23A 0.06740 0.11910 0.08089 1.00000 0.03946 0.00000 0.00000 H23B 0.08780 0.05181 0.01635 1.00000 0.03946 0.00000 0.00000 H23C -0.01609 0.11778 -0.03590 1.00000 0.03946 0.00000 0.00000 N1 0.37802 0.06367 0.30837 1.00000 0.01313 0.00670 0.01074 0.00341 0.00538 0.00236 0.00977 0.00992 0.00062 0.00026 0.00037 0.00000 0.00231 0.00218 0.00229 0.00178 0.00184 0.00180 0.00094 N2 0.39779 0.07585 0.14625 1.00000 0.01568 0.01045 0.00808 0.00104 0.00429 0.00009 0.01117 0.00996 0.00064 0.00027 0.00037 0.00000 0.00245 0.00236 0.00227 0.00181 0.00186 0.00186 0.00098 Br1 0.24146 0.32969 0.25920 1.00000 0.05599 0.03545 0.04764 0.00138 0.01480 0.00708 0.04607 0.00221 0.00015 0.00006 0.00008 0.00000 0.00066 0.00057 0.00062 0.00040 0.00048 0.00043 0.00034 Ag1 0.29889 0.20976 0.23476 1.00000 0.01538 0.01059 0.01165 0.00138 0.00491 0.00313 0.01228 0.00087 0.00005 0.00002 0.00003 0.00000 0.00032 0.00031 0.00030 0.00015 0.00019 0.00015 0.00023 Final Structure Factor Calculation for 2007src1544 in P2(1)/n Total number of l.s. parameters = 251 Maximum vector length = 511 Memory required = 3090 / 24017 wR2 = 0.2322 before cycle 5 for 4970 data and 0 / 251 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1451 * P )^2 + 30.82 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0749 for 4469 Fo > 4sig(Fo) and 0.0807 for all 4970 data wR2 = 0.2322, GooF = S = 1.043, Restrained GooF = 1.043 for all data Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 30.00 for hydrogen atoms Principal mean square atomic displacements U 0.0139 0.0100 0.0077 C1 0.0219 0.0136 0.0073 C2 0.0229 0.0169 0.0071 C3 0.0298 0.0235 0.0070 C4 0.0251 0.0178 0.0103 C5 0.0165 0.0087 0.0047 C6 0.0249 0.0124 0.0092 C7 0.0313 0.0230 0.0123 C8 0.0352 0.0140 0.0083 C9 0.0416 0.0123 0.0097 C10 0.0536 0.0222 0.0123 C11 0.0265 0.0142 0.0109 C12 0.0180 0.0143 0.0107 C13 0.0335 0.0192 0.0120 C14 0.0144 0.0137 0.0049 C15 0.0237 0.0129 0.0058 C16 0.0258 0.0171 0.0125 C17 0.0274 0.0138 0.0096 C18 0.0362 0.0128 0.0081 C19 0.0483 0.0262 0.0127 C20 0.0295 0.0135 0.0107 C21 0.0207 0.0162 0.0130 C22 0.0424 0.0230 0.0134 C23 0.0154 0.0091 0.0048 N1 0.0157 0.0108 0.0071 N2 0.0582 0.0468 0.0332 Br1 0.0172 0.0106 0.0090 Ag1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.022 0.043 0.066 0.088 0.118 0.148 0.184 0.232 0.304 1.000 Number in group 503. 508. 493. 483. 503. 495. 504. 489. 491. 501. GooF 0.953 1.035 1.096 1.140 1.002 1.081 1.058 1.050 0.988 1.022 K 2.160 1.141 1.082 1.032 0.991 1.010 1.016 1.005 1.031 1.033 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.63 inf Number in group 500. 507. 485. 499. 502. 491. 492. 501. 494. 499. GooF 0.844 0.830 0.799 0.633 0.523 0.401 0.521 0.908 1.518 2.144 K 0.987 0.980 0.999 1.019 1.042 1.054 1.053 1.049 1.043 1.010 R1 0.108 0.101 0.087 0.067 0.051 0.036 0.042 0.061 0.096 0.122 Recommended weighting scheme: WGHT 0.1470 30.3749 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 2 1 810.49 60.98 6.78 0.030 3.43 -1 4 6 1623.23 361.56 6.37 0.074 2.09 3 4 2 1334.85 274.97 6.20 0.065 2.10 -1 6 1 395.39 2767.91 6.17 0.205 2.95 0 6 2 461.13 2987.28 6.15 0.213 2.87 -2 2 7 670.55 53.19 6.15 0.028 1.90 1 6 1 80.86 1571.72 6.12 0.155 2.84 4 4 1 544.97 24.36 6.00 0.019 1.81 1 4 2 223.24 1733.43 5.62 0.162 3.33 -2 2 1 126.35 1377.11 5.55 0.145 3.88 2 6 0 655.75 2982.67 5.54 0.213 2.51 0 2 3 319.30 1888.26 5.41 0.169 4.06 1 2 8 848.53 162.97 5.37 0.050 1.55 0 12 2 875.86 179.79 5.28 0.052 1.55 3 4 4 2555.12 948.63 5.16 0.120 1.77 -2 6 2 846.49 3131.29 5.13 0.218 2.48 0 4 3 23109.00 11127.61 5.10 0.411 3.27 3 2 4 413.18 22.28 5.08 0.018 1.86 -3 4 4 504.09 58.25 5.06 0.030 2.18 0 4 1 1296.91 4211.94 5.06 0.253 4.49 -1 12 1 1482.57 467.77 5.01 0.084 1.56 1 4 4 13201.14 6287.16 5.01 0.309 2.46 -2 2 3 745.05 2714.02 4.95 0.203 3.29 -1 4 3 327.87 11.87 4.94 0.013 3.25 3 4 0 11010.74 5253.13 4.91 0.283 2.37 1 4 1 539.12 80.85 4.90 0.035 3.81 0 12 0 2250.14 846.09 4.86 0.113 1.59 2 12 0 3571.05 1555.78 4.73 0.154 1.48 -3 2 4 41.11 725.85 4.69 0.105 2.38 -1 12 3 3569.34 1582.86 4.65 0.155 1.50 -1 2 6 132.44 960.91 4.62 0.121 2.25 -5 0 5 2072.24 813.52 4.60 0.111 1.60 -3 4 2 857.06 2673.31 4.55 0.202 2.41 2 4 5 4118.89 1944.88 4.41 0.172 1.87 -3 4 5 1199.78 405.99 4.39 0.079 2.02 -4 2 3 283.15 1184.04 4.23 0.134 2.03 -4 2 1 363.55 1367.39 4.23 0.144 2.06 1 4 6 8902.96 4655.38 4.23 0.266 1.87 2 6 2 1919.21 4685.09 4.22 0.267 2.24 -2 12 2 3044.96 1429.88 4.20 0.147 1.48 -2 4 6 713.87 195.67 4.20 0.055 2.01 1 2 2 1992.69 4797.28 4.19 0.270 4.18 4 0 0 1209.89 3151.82 4.17 0.219 2.05 -4 0 6 102.61 723.03 4.15 0.105 1.75 -1 3 2 639.95 170.73 4.13 0.051 4.37 1 12 1 3362.39 1614.10 4.10 0.157 1.54 -4 6 2 350.59 1284.46 4.09 0.140 1.76 4 4 3 1251.30 476.18 4.04 0.085 1.61 2 4 7 3143.75 1531.43 4.02 0.153 1.51 0 4 7 229.80 12.61 3.99 0.014 1.78 Bond lengths and angles C1 - Distance Angles N1 1.3464 (0.0076) N2 1.3473 (0.0077) 118.76 (0.55) Ag1 2.0969 (0.0062) 118.46 (0.42) 122.69 (0.43) C1 - N1 N2 C2 - Distance Angles N1 1.4966 (0.0074) C3 1.5280 (0.0085) 111.99 (0.50) C2 - N1 C3 - Distance Angles C2 1.5280 (0.0085) C4 1.5304 (0.0095) 112.36 (0.55) C3 - C2 C4 - Distance Angles C5 1.5205 (0.0096) C3 1.5304 (0.0095) 110.64 (0.52) C4 - C5 C5 - Distance Angles N2 1.4930 (0.0080) C4 1.5205 (0.0096) 112.82 (0.55) C5 - N2 C6 - Distance Angles C13 1.4018 (0.0088) C7 1.4036 (0.0086) 121.99 (0.57) N1 1.4439 (0.0073) 120.59 (0.53) 117.30 (0.54) C6 - C13 C7 C7 - Distance Angles C9 1.3988 (0.0090) C6 1.4036 (0.0086) 117.76 (0.63) C8 1.5023 (0.0098) 121.16 (0.61) 121.05 (0.58) C7 - C9 C6 C8 - Distance Angles C7 1.5023 (0.0098) C8 - C9 - Distance Angles C10 1.3904 (0.0109) C7 1.3988 (0.0090) 122.21 (0.64) C9 - C10 C10 - Distance Angles C9 1.3904 (0.0109) C12 1.4016 (0.0104) 118.49 (0.61) C11 1.5043 (0.0094) 120.71 (0.70) 120.80 (0.71) C10 - C9 C12 C11 - Distance Angles C10 1.5043 (0.0094) C11 - C12 - Distance Angles C10 1.4016 (0.0104) C13 1.4036 (0.0089) 121.51 (0.63) C12 - C10 C13 - Distance Angles C6 1.4018 (0.0088) C12 1.4036 (0.0089) 117.99 (0.59) C14 1.5070 (0.0090) 121.36 (0.57) 120.65 (0.60) C13 - C6 C12 C14 - Distance Angles C13 1.5070 (0.0090) C14 - C15 - Distance Angles C22 1.4047 (0.0089) C16 1.4092 (0.0085) 121.83 (0.58) N2 1.4637 (0.0075) 119.04 (0.55) 119.07 (0.54) C15 - C22 C16 C16 - Distance Angles C18 1.3991 (0.0091) C15 1.4092 (0.0085) 117.00 (0.61) C17 1.4959 (0.0094) 120.42 (0.60) 122.58 (0.58) C16 - C18 C15 C17 - Distance Angles C16 1.4959 (0.0094) C17 - C18 - Distance Angles C19 1.3858 (0.0107) C16 1.3991 (0.0091) 122.13 (0.65) C18 - C19 C19 - Distance Angles C18 1.3858 (0.0107) C21 1.3937 (0.0106) 119.00 (0.62) C20 1.5160 (0.0094) 120.47 (0.71) 120.51 (0.70) C19 - C18 C21 C20 - Distance Angles C19 1.5160 (0.0094) C20 - C21 - Distance Angles C22 1.3805 (0.0094) C19 1.3937 (0.0106) 121.46 (0.64) C21 - C22 C22 - Distance Angles C21 1.3805 (0.0094) C15 1.4047 (0.0089) 118.44 (0.63) C23 1.5029 (0.0097) 120.34 (0.63) 121.22 (0.60) C22 - C21 C15 C23 - Distance Angles C22 1.5029 (0.0097) C23 - N1 - Distance Angles C1 1.3464 (0.0076) C6 1.4439 (0.0073) 116.99 (0.48) C2 1.4966 (0.0074) 129.35 (0.51) 113.54 (0.46) N1 - C1 C6 N2 - Distance Angles C1 1.3473 (0.0077) C15 1.4637 (0.0075) 117.26 (0.50) C5 1.4930 (0.0080) 124.23 (0.52) 116.82 (0.49) N2 - C1 C15 Br1 - Distance Angles Ag1 2.3792 (0.0011) Br1 - Ag1 - Distance Angles C1 2.0969 (0.0062) Br1 2.3792 (0.0011) 174.56 (0.16) Ag1 - C1 FMAP and GRID set by program FMAP 2 2 25 GRID -1.136 -2 -2 1.136 2 2 R1 = 0.0792 for 4970 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 4.11 at 0.3085 0.2091 0.2351 [ 0.08 A from AG1 ] Deepest hole -4.32 at 0.6977 0.1695 0.7456 [ 0.37 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.28 e/A^3, Highest memory used = 3046 / 23698 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2811 0.3749 0.2220 1.00000 0.05 1.75 1.10 BR1 2.19 H2A 2.19 H8B 2.57 H11A Q2 1 0.3489 0.3316 0.2132 1.00000 0.05 1.64 1.24 BR1 2.24 H11A 2.39 AG1 2.57 H11B Q3 1 0.2492 0.2697 0.2580 1.00000 0.05 1.47 1.15 BR1 1.29 AG1 2.97 H20B 3.17 H18 Q4 1 0.2777 0.2862 0.2258 1.00000 0.05 1.43 1.03 BR1 1.47 AG1 2.99 H14A 3.11 H21 Q5 1 0.1658 0.3748 0.2454 1.00000 0.05 1.40 1.06 BR1 1.81 H2A 2.38 H5B 2.53 H4B Q6 1 0.2129 0.3867 0.2622 1.00000 0.05 1.31 1.12 BR1 1.85 H2A 2.13 H5B 2.46 H8B Q7 1 0.1380 0.3468 0.2764 1.00000 0.05 1.24 1.02 BR1 2.34 H4B 2.44 H2A 2.55 H20B Q8 1 0.1460 0.3640 0.2284 1.00000 0.05 1.22 1.05 BR1 1.89 H2A 2.61 H4B 2.67 H5B Q9 1 0.2035 0.3531 0.3238 1.00000 0.05 1.15 1.12 BR1 2.36 H5B 2.43 H18 2.55 H4B Q10 1 0.2536 0.0879 0.2586 1.00000 0.05 1.10 1.17 C1 1.20 N1 1.66 C6 1.97 H8C Q11 1 0.2540 0.3312 0.1780 1.00000 0.05 1.06 1.16 BR1 2.38 H14A 2.44 H11A 2.44 AG1 Q12 1 0.2848 0.1933 -0.0860 1.00000 0.05 0.87 0.63 C21 0.77 C19 1.41 H21 1.75 C22 Q13 1 0.2239 0.2964 0.3194 1.00000 0.05 0.87 1.09 BR1 2.21 AG1 2.25 H18 2.72 H20B Q14 1 0.1334 0.2939 0.2340 1.00000 0.05 0.83 1.13 BR1 2.13 AG1 2.19 H20B 2.78 H12 Q15 1 0.5963 0.2887 -0.2013 1.00000 0.05 0.80 1.84 H20B 2.00 H20C 2.13 AG1 2.28 C20 Q16 1 0.1825 0.2937 0.3028 1.00000 0.05 0.78 1.12 BR1 2.22 AG1 2.25 H18 2.37 H20B Q17 1 0.3764 0.0882 0.2780 1.00000 0.05 0.77 0.63 N1 0.75 C1 1.74 C6 1.90 N2 Q18 1 0.3810 0.3196 0.2769 1.00000 0.05 0.76 1.16 BR1 2.10 H21 2.24 AG1 2.80 H23C Q19 1 0.3551 0.0772 0.3531 1.00000 0.05 0.75 0.73 C6 0.74 N1 1.78 C13 1.85 C1 Q20 1 0.4339 0.2106 -0.0606 1.00000 0.05 0.69 0.70 C18 0.76 C19 1.42 H18 1.85 C16 Shortest distances between peaks (including symmetry equivalents) 5 8 0.32 13 16 0.37 5 6 0.47 3 4 0.64 7 9 0.76 5 7 0.76 7 8 0.76 6 8 0.77 2 11 0.83 2 18 0.89 1 6 0.93 14 16 0.94 10 17 1.01 1 11 1.02 1 2 1.03 6 7 1.04 3 16 1.05 3 14 1.06 3 13 1.06 4 11 1.07 6 9 1.09 2 4 1.09 9 13 1.10 1 5 1.11 7 16 1.11 17 19 1.13 5 9 1.13 7 14 1.17 4 18 1.17 9 16 1.17 1 8 1.19 13 14 1.24 7 13 1.26 4 14 1.27 12 20 1.27 8 9 1.31 8 14 1.35 10 19 1.39 8 11 1.43 3 18 1.44 1 18 1.44 4 13 1.50 4 16 1.51 11 18 1.53 5 14 1.57 5 11 1.58 11 14 1.60 3 11 1.62 13 18 1.65 2 3 1.66 8 16 1.67 1 7 1.68 9 14 1.68 6 11 1.68 1 4 1.69 15 16 1.73 5 16 1.73 1 9 1.76 3 7 1.80 5 13 1.81 8 13 1.81 2 6 1.82 4 8 1.86 16 18 1.88 14 15 1.88 6 13 1.89 6 18 1.89 2 8 1.89 6 16 1.90 6 14 1.90 9 18 1.90 3 15 1.90 7 11 1.90 2 5 1.91 4 7 1.91 3 9 1.92 13 15 1.93 4 5 1.99 3 8 2.00 1 14 2.02 2 14 2.05 5 18 2.06 4 9 2.08 4 6 2.09 14 18 2.09 1 3 2.10 11 16 2.11 8 18 2.11 3 5 2.12 7 18 2.13 2 13 2.14 11 13 2.15 1 13 2.16 1 16 2.20 2 7 2.21 9 11 2.22 2 16 2.23 2 9 2.24 3 6 2.25 4 15 2.50 7 15 2.64 10 15 2.83 9 15 2.84 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: 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 0.01: Analyse other restraints etc. 3.97: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.43: Structure factors and derivatives 3.06: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.47: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.15: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.07: Fourier summations 0.02: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1544 finished at 17:30:18 Total CPU time: 10.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++