+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0354 started at 16:05:17 on 16-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0354 in P2(1)/c CELL 0.71073 18.5797 10.6257 8.3867 90.000 98.718 90.000 ZERR 4.00 0.0005 0.0003 0.0001 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N F P UNIT 56 60 4 36 4 V = 1636.59 F(000) = 808.0 Mu = 0.26 mm-1 Cell Wt = 1596.96 Rho = 1.620 MERG 2 OMIT -3.00 55.00 OMIT 0 2 0 OMIT -3 2 2 OMIT -1 0 2 FMAP 2 PLAN 20 SIZE 0.10 0.20 0.50 ACTA BOND WGHT 0.05090 0.68990 L.S. 4 TEMP -153.00 FVAR 0.69545 MOLE 1 C1 1 0.072710 -0.133611 0.871144 11.00000 0.01835 0.02335 = 0.05250 0.00280 0.00371 -0.00021 C2 1 0.116279 -0.051393 0.773379 11.00000 0.01773 0.02343 = 0.02413 -0.00235 0.00086 0.00090 AFIX 13 H2 2 0.122547 -0.094802 0.670583 11.00000 -1.20000 AFIX 0 C3 1 0.082559 0.078944 0.736905 11.00000 0.02203 0.02560 = 0.03496 0.00477 -0.00090 0.00231 AFIX 23 H3A 2 0.094873 0.112337 0.634188 11.00000 -1.20000 H3B 2 0.028920 0.075526 0.729814 11.00000 -1.20000 AFIX 0 C4 1 0.116240 0.160290 0.879473 11.00000 0.02501 0.01993 = 0.04580 -0.00279 0.00295 0.00418 AFIX 23 H4A 2 0.116555 0.250139 0.848347 11.00000 -1.20000 H4B 2 0.088982 0.151141 0.971499 11.00000 -1.20000 AFIX 0 C5 1 0.193452 0.110194 0.922372 11.00000 0.02371 0.01684 = 0.02714 -0.00374 0.00193 0.00016 AFIX 23 H5A 2 0.227599 0.157923 0.865381 11.00000 -1.20000 H5B 2 0.210136 0.115620 1.040012 11.00000 -1.20000 AFIX 0 C6 1 0.241844 -0.102970 0.887191 11.00000 0.02010 0.01572 = 0.01957 0.00227 0.00753 -0.00094 AFIX 43 H6 2 0.233503 -0.184143 0.840565 11.00000 -1.20000 AFIX 0 C7 1 0.312046 -0.076770 0.973240 11.00000 0.02042 0.01926 = 0.01855 0.00105 0.00411 -0.00077 AFIX 43 H7 2 0.322306 0.002318 1.024496 11.00000 -1.20000 AFIX 0 C8 1 0.363986 -0.166417 0.980868 11.00000 0.02083 0.01945 = 0.01903 0.00126 0.00499 -0.00186 AFIX 43 H8 2 0.350411 -0.243383 0.926928 11.00000 -1.20000 AFIX 0 C9 1 0.438581 -0.157284 1.063166 11.00000 0.01931 0.01998 = 0.01896 0.00358 0.00485 -0.00065 C10 1 0.464207 -0.054689 1.161733 11.00000 0.02493 0.02154 = 0.02163 0.00262 0.00444 0.00075 AFIX 43 H10 2 0.432063 0.011739 1.179107 11.00000 -1.20000 AFIX 0 C11 1 0.536437 -0.050770 1.233403 11.00000 0.02640 0.02930 = 0.02213 0.00224 0.00064 -0.00629 AFIX 43 H11 2 0.553655 0.018517 1.300041 11.00000 -1.20000 AFIX 0 C12 1 0.583865 -0.147365 1.208569 11.00000 0.01916 0.03956 = 0.02400 0.00742 0.00149 -0.00290 AFIX 43 H12 2 0.633244 -0.143958 1.258626 11.00000 -1.20000 AFIX 0 C13 1 0.559518 -0.248537 1.111248 11.00000 0.02192 0.03249 = 0.02933 0.00401 0.00601 0.00675 AFIX 43 H13 2 0.592135 -0.314087 1.093343 11.00000 -1.20000 AFIX 0 C14 1 0.487003 -0.253585 1.039865 11.00000 0.02392 0.02519 = 0.02395 -0.00067 0.00453 0.00125 AFIX 43 H14 2 0.470150 -0.323622 0.974245 11.00000 -1.20000 AFIX 0 N1 3 0.188237 -0.023168 0.868027 11.00000 0.01811 0.01757 = 0.01776 0.00078 0.00369 -0.00080 F1 4 0.245634 0.097599 0.569348 11.00000 0.04532 0.02931 = 0.02862 -0.01247 0.00672 -0.00219 F2 4 0.330135 -0.016756 0.463728 11.00000 0.02520 0.03381 = 0.06128 -0.00219 0.00708 -0.00044 F3 4 0.257330 0.118046 0.306947 11.00000 0.08145 0.02232 = 0.02923 0.00628 0.00816 -0.00593 F4 4 0.241779 -0.093530 0.272739 11.00000 0.06385 0.02511 = 0.02219 -0.00631 0.01290 -0.00478 F5 4 0.158076 0.020893 0.379099 11.00000 0.02844 0.03762 = 0.06745 -0.01374 -0.01233 0.00786 F6 4 0.231979 -0.113698 0.535817 11.00000 0.04567 0.02661 = 0.02526 0.00363 0.01171 -0.00414 F7 4 0.102972 -0.246844 0.900709 11.00000 0.03275 0.02281 = 0.09755 0.01713 0.01527 0.00222 F8 4 0.064493 -0.083844 1.013293 11.00000 0.03817 0.04994 = 0.04641 0.00792 0.02301 -0.00235 F9 4 0.005685 -0.152785 0.790248 11.00000 0.02111 0.03995 = 0.08455 0.00230 -0.00283 -0.00976 P1 5 0.244013 0.002355 0.420659 11.00000 0.02672 0.01740 = 0.01765 -0.00109 0.00308 0.00078 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 2007src0354 in P2(1)/c C 0.770 H 0.320 N 0.700 F 0.640 P 1.100 C1 - F8 F7 F9 C2 C2 - N1 C1 C3 C3 - C4 C2 C4 - C5 C3 C5 - N1 C4 C6 - N1 C7 C7 - C8 C6 C8 - C7 C9 C9 - C14 C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C13 C11 C13 - C12 C14 C14 - C13 C9 N1 - C6 C2 C5 F1 - P1 F2 - P1 F3 - P1 F4 - P1 F5 - P1 F6 - P1 F7 - C1 F8 - C1 F9 - C1 P1 - F5 F3 F2 F4 F1 F6 20512 Reflections read, of which 683 rejected -23 =< h =< 24, -12 =< k =< 13, -10 =< l =< 10, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 3737 Unique reflections, of which 0 suppressed R(int) = 0.0411 R(sigma) = 0.0323 Friedel opposites merged Maximum memory for data reduction = 1996 / 36881 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 = 2603 / 281092 wR2 = 0.1047 before cycle 1 for 3737 data and 226 / 226 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69509 0.00130 -0.276 OSF Mean shift/esd = 0.044 Maximum = -0.276 for OSF Max. shift = 0.000 A for C14 Max. dU = 0.000 for F7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2603 / 281092 wR2 = 0.1047 before cycle 2 for 3737 data and 226 / 226 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69493 0.00130 -0.125 OSF Mean shift/esd = 0.015 Maximum = -0.125 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for F7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2603 / 281092 wR2 = 0.1047 before cycle 3 for 3737 data and 226 / 226 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69493 0.00130 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U13 C8 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2603 / 281092 wR2 = 0.1048 before cycle 4 for 3737 data and 226 / 226 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69493 0.00130 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U33 C10 Max. shift = 0.000 A for H5B Max. dU = 0.000 for C10 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 H2 0.1225 -0.0948 0.6706 13 1.000 0.000 C2 N1 C1 C3 H3A 0.0949 0.1123 0.6342 23 0.990 0.000 C3 C4 C2 H3B 0.0289 0.0755 0.7298 23 0.990 0.000 C3 C4 C2 H4A 0.1166 0.2501 0.8483 23 0.990 0.000 C4 C5 C3 H4B 0.0890 0.1511 0.9715 23 0.990 0.000 C4 C5 C3 H5A 0.2276 0.1579 0.8654 23 0.990 0.000 C5 N1 C4 H5B 0.2101 0.1156 1.0400 23 0.990 0.000 C5 N1 C4 H6 0.2335 -0.1842 0.8406 43 0.950 0.000 C6 N1 C7 H7 0.3223 0.0023 1.0245 43 0.950 0.000 C7 C8 C6 H8 0.3504 -0.2434 0.9269 43 0.950 0.000 C8 C7 C9 H10 0.4321 0.0117 1.1791 43 0.950 0.000 C10 C11 C9 H11 0.5537 0.0185 1.3000 43 0.950 0.000 C11 C10 C12 H12 0.6332 -0.1440 1.2586 43 0.950 0.000 C12 C13 C11 H13 0.5921 -0.3141 1.0934 43 0.950 0.000 C13 C12 C14 H14 0.4702 -0.3236 0.9742 43 0.950 0.000 C14 C13 C9 2007src0354 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.07271 -0.13360 0.87113 1.00000 0.01833 0.02328 0.05232 0.00279 0.00367 -0.00019 0.03148 0.00342 0.00009 0.00017 0.00024 0.00000 0.00082 0.00092 0.00112 0.00080 0.00074 0.00069 0.00041 C2 0.11628 -0.05139 0.77337 1.00000 0.01763 0.02331 0.02408 -0.00236 0.00083 0.00091 0.02192 0.00288 0.00009 0.00016 0.00019 0.00000 0.00077 0.00085 0.00077 0.00063 0.00057 0.00064 0.00033 H2 0.12255 -0.09480 0.67057 1.00000 0.02630 0.00000 0.00000 C3 0.08256 0.07895 0.73692 1.00000 0.02198 0.02552 0.03489 0.00478 -0.00090 0.00231 0.02800 0.00319 0.00009 0.00017 0.00021 0.00000 0.00084 0.00093 0.00090 0.00071 0.00065 0.00070 0.00038 H3A 0.09486 0.11235 0.63420 1.00000 0.03360 0.00000 0.00000 H3B 0.02892 0.07553 0.72985 1.00000 0.03360 0.00000 0.00000 C4 0.11624 0.16029 0.87946 1.00000 0.02496 0.01983 0.04571 -0.00281 0.00298 0.00420 0.03042 0.00324 0.00010 0.00017 0.00023 0.00000 0.00091 0.00090 0.00104 0.00073 0.00073 0.00069 0.00040 H4A 0.11656 0.25013 0.84833 1.00000 0.03650 0.00000 0.00000 H4B 0.08898 0.15115 0.97149 1.00000 0.03650 0.00000 0.00000 C5 0.19345 0.11019 0.92237 1.00000 0.02370 0.01675 0.02708 -0.00378 0.00194 0.00014 0.02270 0.00288 0.00009 0.00015 0.00019 0.00000 0.00084 0.00082 0.00080 0.00061 0.00061 0.00063 0.00034 H5A 0.22760 0.15791 0.86537 1.00000 0.02725 0.00000 0.00000 H5B 0.21014 0.11562 1.04001 1.00000 0.02725 0.00000 0.00000 C6 0.24184 -0.10298 0.88719 1.00000 0.02006 0.01563 0.01951 0.00228 0.00747 -0.00092 0.01793 0.00284 0.00008 0.00015 0.00018 0.00000 0.00077 0.00077 0.00071 0.00055 0.00055 0.00059 0.00031 H6 0.23350 -0.18415 0.84057 1.00000 0.02152 0.00000 0.00000 C7 0.31205 -0.07677 0.97323 1.00000 0.02035 0.01919 0.01850 0.00105 0.00413 -0.00076 0.01923 0.00287 0.00008 0.00015 0.00017 0.00000 0.00077 0.00081 0.00072 0.00057 0.00056 0.00062 0.00032 H7 0.32230 0.00232 1.02448 1.00000 0.02307 0.00000 0.00000 C8 0.36399 -0.16641 0.98087 1.00000 0.02077 0.01935 0.01899 0.00126 0.00499 -0.00187 0.01950 0.00286 0.00008 0.00015 0.00018 0.00000 0.00078 0.00082 0.00072 0.00057 0.00056 0.00062 0.00032 H8 0.35042 -0.24338 0.92693 1.00000 0.02340 0.00000 0.00000 C9 0.43857 -0.15728 1.06316 1.00000 0.01920 0.01989 0.01891 0.00357 0.00480 -0.00067 0.01914 0.00284 0.00008 0.00015 0.00017 0.00000 0.00075 0.00081 0.00072 0.00057 0.00055 0.00061 0.00032 C10 0.46420 -0.05470 1.16173 1.00000 0.02489 0.02146 0.02153 0.00260 0.00443 0.00074 0.02253 0.00295 0.00009 0.00016 0.00018 0.00000 0.00085 0.00085 0.00077 0.00061 0.00059 0.00066 0.00034 H10 0.43206 0.01173 1.17911 1.00000 0.02704 0.00000 0.00000 C11 0.53644 -0.05077 1.23340 1.00000 0.02639 0.02921 0.02199 0.00221 0.00062 -0.00629 0.02618 0.00309 0.00009 0.00017 0.00019 0.00000 0.00088 0.00094 0.00078 0.00067 0.00061 0.00072 0.00037 H11 0.55365 0.01851 1.30005 1.00000 0.03141 0.00000 0.00000 C12 0.58387 -0.14737 1.20856 1.00000 0.01906 0.03947 0.02395 0.00740 0.00148 -0.00292 0.02768 0.00321 0.00009 0.00018 0.00020 0.00000 0.00081 0.00105 0.00081 0.00071 0.00061 0.00073 0.00038 H12 0.63325 -0.14396 1.25861 1.00000 0.03321 0.00000 0.00000 C13 0.55951 -0.24853 1.11125 1.00000 0.02187 0.03241 0.02926 0.00401 0.00601 0.00675 0.02763 0.00332 0.00009 0.00018 0.00020 0.00000 0.00086 0.00099 0.00085 0.00070 0.00064 0.00072 0.00038 H13 0.59213 -0.31409 1.09335 1.00000 0.03315 0.00000 0.00000 C14 0.48701 -0.25357 1.03987 1.00000 0.02384 0.02506 0.02389 -0.00068 0.00451 0.00125 0.02417 0.00310 0.00009 0.00016 0.00019 0.00000 0.00084 0.00091 0.00078 0.00064 0.00061 0.00068 0.00035 H14 0.47016 -0.32360 0.97423 1.00000 0.02900 0.00000 0.00000 N1 0.18823 -0.02317 0.86803 1.00000 0.01801 0.01750 0.01772 0.00077 0.00368 -0.00082 0.01764 0.00233 0.00007 0.00012 0.00015 0.00000 0.00065 0.00068 0.00061 0.00048 0.00047 0.00051 0.00027 F1 0.24564 0.09759 0.56934 1.00000 0.04526 0.02926 0.02854 -0.01249 0.00670 -0.00221 0.03424 0.00183 0.00006 0.00010 0.00012 0.00000 0.00065 0.00060 0.00054 0.00041 0.00045 0.00047 0.00026 F2 0.33013 -0.01676 0.46373 1.00000 0.02510 0.03374 0.06128 -0.00221 0.00707 -0.00044 0.03999 0.00214 0.00006 0.00011 0.00015 0.00000 0.00058 0.00065 0.00074 0.00052 0.00049 0.00046 0.00029 F3 0.25733 0.11804 0.30695 1.00000 0.08142 0.02226 0.02916 0.00634 0.00816 -0.00589 0.04430 0.00216 0.00007 0.00010 0.00013 0.00000 0.00094 0.00058 0.00056 0.00043 0.00055 0.00056 0.00032 F4 0.24178 -0.09352 0.27275 1.00000 0.06378 0.02503 0.02210 -0.00631 0.01286 -0.00478 0.03631 0.00196 0.00007 0.00010 0.00012 0.00000 0.00077 0.00057 0.00050 0.00039 0.00046 0.00051 0.00028 F5 0.15808 0.02090 0.37910 1.00000 0.02840 0.03757 0.06731 -0.01370 -0.01235 0.00786 0.04645 0.00207 0.00006 0.00011 0.00016 0.00000 0.00062 0.00068 0.00081 0.00057 0.00054 0.00050 0.00033 F6 0.23198 -0.11370 0.53581 1.00000 0.04566 0.02652 0.02517 0.00368 0.01170 -0.00414 0.03179 0.00195 0.00006 0.00010 0.00012 0.00000 0.00064 0.00057 0.00050 0.00040 0.00043 0.00047 0.00025 F7 0.10297 -0.24685 0.90069 1.00000 0.03268 0.02271 0.09740 0.01708 0.01524 0.00224 0.05037 0.00250 0.00006 0.00011 0.00018 0.00000 0.00065 0.00062 0.00103 0.00061 0.00062 0.00048 0.00035 F8 0.06449 -0.08384 1.01329 1.00000 0.03811 0.04986 0.04634 0.00790 0.02297 -0.00232 0.04306 0.00233 0.00006 0.00012 0.00014 0.00000 0.00066 0.00075 0.00068 0.00054 0.00051 0.00055 0.00030 F9 0.00568 -0.15278 0.79024 1.00000 0.02107 0.03988 0.08444 0.00230 -0.00281 -0.00980 0.04958 0.00217 0.00006 0.00012 0.00017 0.00000 0.00057 0.00072 0.00093 0.00063 0.00055 0.00049 0.00034 P1 0.24401 0.00236 0.42066 1.00000 0.02667 0.01736 0.01759 -0.00108 0.00307 0.00077 0.02057 0.00074 0.00002 0.00004 0.00005 0.00000 0.00024 0.00023 0.00021 0.00014 0.00016 0.00016 0.00013 Final Structure Factor Calculation for 2007src0354 in P2(1)/c Total number of l.s. parameters = 226 Maximum vector length = 511 Memory required = 2377 / 24017 wR2 = 0.1047 before cycle 5 for 3737 data and 0 / 226 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 0.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0395 for 3029 Fo > 4sig(Fo) and 0.0530 for all 3737 data wR2 = 0.1047, GooF = S = 1.047, Restrained GooF = 1.047 for all data Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0531 0.0230 0.0183 C1 0.0271 0.0215 0.0172 C2 0.0388 0.0264 0.0189 C3 0.0470 0.0270 0.0172 C4 0.0294 0.0232 0.0155 C5 0.0238 0.0175 0.0125 C6 0.0208 0.0199 0.0169 C7 0.0222 0.0204 0.0158 C8 0.0230 0.0198 0.0145 C9 0.0255 0.0233 0.0188 C10 0.0359 0.0219 0.0207 C11 0.0433 0.0211 0.0186 C12 0.0374 0.0270 0.0184 C13 0.0259 0.0246 0.0221 C14 0.0187 0.0184 0.0158 N1 0.0458 0.0406 0.0163 F1 0.0616 0.0336 0.0248 F2 0.0825 0.0329 0.0175 F3 0.0647 0.0278 0.0164 F4 0.0850 0.0323 0.0221 F5 0.0472 0.0295 0.0187 F6 0.1011 0.0310 0.0190 F7 0.0596 0.0492 0.0203 F8 0.0888 0.0433 0.0167 F9 0.0269 0.0186 0.0163 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.034 0.048 0.062 0.080 0.101 0.135 0.198 1.000 Number in group 407. 354. 362. 402. 347. 393. 360. 369. 366. 377. GooF 0.990 0.926 1.078 1.078 1.125 1.098 1.121 1.052 0.973 1.015 K 1.689 1.063 0.968 0.966 0.986 0.988 0.993 1.008 1.018 0.985 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.64 inf Number in group 380. 378. 362. 381. 373. 370. 371. 380. 366. 376. GooF 0.946 0.980 0.964 0.990 1.010 0.948 0.967 0.901 0.998 1.592 K 0.983 1.012 0.997 0.990 1.004 1.022 1.024 1.021 1.010 0.960 R1 0.128 0.118 0.101 0.082 0.065 0.045 0.035 0.028 0.026 0.038 Recommended weighting scheme: WGHT 0.0502 0.7023 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 1 1 3095.26 6360.40 8.63 0.520 5.65 -1 1 1 271.29 439.68 5.17 0.137 6.40 -5 1 5 6.41 0.06 4.57 0.002 1.59 -1 5 2 25.69 8.30 4.23 0.019 1.89 18 0 2 52.59 103.70 3.99 0.066 0.96 0 6 0 387.32 282.23 3.92 0.110 1.77 6 0 2 131.27 85.98 3.87 0.060 2.30 3 0 2 193.49 137.82 3.83 0.077 3.21 -4 0 4 38.66 19.89 3.82 0.029 2.01 2 0 8 32.89 58.87 3.66 0.050 1.01 1 1 1 177.15 246.63 3.60 0.102 5.94 0 3 4 115.11 80.64 3.49 0.059 1.79 -6 1 9 35.47 73.83 3.47 0.056 0.92 -5 0 2 147.00 202.75 3.43 0.093 2.98 -4 1 5 106.96 148.35 3.34 0.079 1.62 -10 0 10 25.95 85.24 3.24 0.060 0.80 0 2 2 10.67 3.00 3.23 0.011 3.27 7 1 0 68.81 45.03 3.19 0.044 2.55 8 2 0 432.71 348.13 3.14 0.122 2.11 -1 4 3 273.86 211.82 3.13 0.095 1.93 9 0 2 16.01 0.11 3.11 0.002 1.73 -6 0 4 134.73 180.09 3.10 0.088 1.85 -7 0 6 18.84 6.53 3.10 0.017 1.31 4 3 3 47.96 29.60 3.09 0.035 1.88 -1 1 3 159.38 207.38 3.08 0.094 2.70 -15 9 4 187.41 132.33 3.04 0.075 0.82 4 8 2 126.82 89.17 3.04 0.062 1.21 -3 7 5 8.90 23.22 3.00 0.031 1.12 0 5 2 237.30 187.19 2.93 0.089 1.89 1 5 2 889.98 747.06 2.89 0.178 1.87 -4 6 8 83.80 52.75 2.89 0.047 0.90 3 5 0 9.32 21.88 2.88 0.030 2.01 -12 3 7 384.63 309.93 2.88 0.115 0.97 2 4 3 9.12 1.26 2.87 0.007 1.84 -12 8 4 48.01 77.78 2.87 0.058 0.94 -2 1 5 384.09 314.18 2.86 0.116 1.66 6 2 0 26.12 13.28 2.84 0.024 2.65 -3 2 6 7.04 0.61 2.82 0.005 1.35 2 13 3 48.72 11.72 2.80 0.022 0.78 -8 6 8 182.95 239.09 2.79 0.101 0.87 14 4 5 44.75 70.79 2.78 0.055 0.90 -7 4 2 787.06 936.15 2.76 0.200 1.78 3 5 2 206.44 259.33 2.76 0.105 1.77 6 8 2 86.76 123.59 2.75 0.072 1.15 16 3 4 78.14 109.33 2.71 0.068 0.91 6 11 5 -7.14 11.99 2.69 0.023 0.79 15 1 3 310.36 381.96 2.68 0.127 1.06 -5 5 2 250.34 306.89 2.63 0.114 1.73 2 4 0 862.59 736.91 2.61 0.177 2.55 -4 1 2 116.80 149.62 2.61 0.080 3.19 Bond lengths and angles C1 - Distance Angles F8 1.3340 (0.0023) F7 1.3354 (0.0021) 107.06 (0.16) F9 1.3404 (0.0021) 106.81 (0.15) 106.84 (0.15) C2 1.5138 (0.0024) 113.48 (0.15) 112.08 (0.15) 110.22 (0.15) C1 - F8 F7 F9 C2 - Distance Angles N1 1.4784 (0.0019) C1 1.5138 (0.0024) 109.90 (0.13) C3 1.5316 (0.0024) 103.47 (0.13) 113.19 (0.14) C2 - N1 C1 C3 - Distance Angles C4 1.5300 (0.0025) C2 1.5316 (0.0024) 104.38 (0.13) C3 - C4 C4 - Distance Angles C5 1.5213 (0.0023) C3 1.5300 (0.0025) 104.27 (0.14) C4 - C5 C5 - Distance Angles N1 1.4872 (0.0020) C4 1.5213 (0.0023) 104.22 (0.13) C5 - N1 C6 - Distance Angles N1 1.2995 (0.0020) C7 1.4193 (0.0021) 124.26 (0.15) C6 - N1 C7 - Distance Angles C8 1.3506 (0.0023) C6 1.4193 (0.0021) 118.74 (0.15) C7 - C8 C8 - Distance Angles C7 1.3506 (0.0023) C9 1.4547 (0.0021) 126.72 (0.15) C8 - C7 C9 - Distance Angles C14 1.3957 (0.0023) C10 1.4067 (0.0022) 118.83 (0.15) C8 1.4547 (0.0021) 118.21 (0.14) 122.94 (0.14) C9 - C14 C10 C10 - Distance Angles C11 1.3855 (0.0023) C9 1.4067 (0.0022) 119.84 (0.15) C10 - C11 C11 - Distance Angles C10 1.3855 (0.0023) C12 1.3889 (0.0026) 120.50 (0.16) C11 - C10 C12 - Distance Angles C13 1.3836 (0.0026) C11 1.3889 (0.0026) 120.29 (0.15) C12 - C13 C13 - Distance Angles C12 1.3836 (0.0026) C14 1.3898 (0.0023) 119.54 (0.16) C13 - C12 C14 - Distance Angles C13 1.3898 (0.0023) C9 1.3957 (0.0023) 120.99 (0.16) C14 - C13 N1 - Distance Angles C6 1.2995 (0.0020) C2 1.4784 (0.0019) 123.22 (0.13) C5 1.4872 (0.0020) 124.80 (0.13) 111.68 (0.12) N1 - C6 C2 F1 - Distance Angles P1 1.6026 (0.0010) F1 - F2 - Distance Angles P1 1.5990 (0.0011) F2 - F3 - Distance Angles P1 1.5979 (0.0011) F3 - F4 - Distance Angles P1 1.6009 (0.0010) F4 - F5 - Distance Angles P1 1.5940 (0.0012) F5 - F6 - Distance Angles P1 1.6027 (0.0010) F6 - F7 - Distance Angles C1 1.3354 (0.0021) F7 - F8 - Distance Angles C1 1.3340 (0.0023) F8 - F9 - Distance Angles C1 1.3404 (0.0021) F9 - P1 - Distance Angles F5 1.5940 (0.0012) F3 1.5979 (0.0011) 90.86 (0.07) F2 1.5990 (0.0012) 179.53 (0.07) 89.56 (0.07) F4 1.6009 (0.0010) 90.10 (0.06) 90.87 (0.06) 90.10 (0.06) F1 1.6026 (0.0010) 89.55 (0.06) 89.56 (0.06) 90.25 (0.06) 179.45 (0.06) F6 1.6027 (0.0010) 90.02 (0.07) 179.11 (0.07) 89.56 (0.06) 89.29 (0.06) 90.28 (0.06) P1 - F5 F3 F2 F4 F1 FMAP and GRID set by program FMAP 2 3 21 GRID -2.778 -1 -2 2.778 1 2 R1 = 0.0528 for 3737 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.0186 0.6586 0.1902 [ 0.91 A from F9 ] Deepest hole -0.44 at 0.2322 0.0010 0.4966 [ 0.70 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2683 / 30387 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0186 -0.1586 0.6902 1.00000 0.05 0.33 0.91 F9 1.71 C1 2.08 H2 2.17 C2 Q2 1 0.0977 0.0131 0.7486 1.00000 0.05 0.26 0.76 C3 0.78 C2 1.42 H3A 1.43 H3B Q3 1 0.1535 0.1411 0.9112 1.00000 0.05 0.26 0.73 C4 0.80 C5 1.37 H4B 1.41 H4A Q4 1 0.1442 -0.0435 0.8081 1.00000 0.05 0.25 0.56 C2 0.92 N1 1.28 H2 1.78 C3 Q5 1 0.0965 -0.0892 0.8405 1.00000 0.05 0.25 0.72 C1 0.82 C2 1.57 H2 1.65 F8 Q6 1 0.1187 -0.0624 0.7301 1.00000 0.05 0.23 0.39 C2 0.62 H2 1.65 C3 1.65 N1 Q7 1 0.1074 0.1256 0.7979 1.00000 0.05 0.23 0.77 C4 0.81 C3 1.36 H3A 1.39 H4A Q8 1 0.2803 -0.0897 0.9389 1.00000 0.05 0.22 0.63 C7 0.79 C6 1.38 H7 1.49 H6 Q9 1 0.3099 -0.0052 0.3790 1.00000 0.05 0.22 0.76 F2 1.32 P1 1.69 F3 1.71 F4 Q10 1 0.2985 0.0572 1.0879 1.00000 0.05 0.22 0.94 H7 1.74 H5B 1.76 C7 2.19 F3 Q11 1 0.4134 0.0330 1.2116 1.00000 0.05 0.21 0.52 H10 1.43 C10 2.15 H7 2.32 H13 Q12 1 0.0221 0.0659 0.6639 1.00000 0.05 0.21 0.56 H3B 1.20 C3 1.49 H3A 2.23 C2 Q13 1 0.4975 -0.0610 1.2165 1.00000 0.05 0.19 0.72 C10 0.72 C11 1.43 H10 1.44 H11 Q14 1 0.3398 -0.1070 0.9395 1.00000 0.05 0.19 0.70 C7 0.82 C8 1.43 H7 1.47 H8 Q15 1 0.1829 0.0066 0.8827 1.00000 0.05 0.18 0.36 N1 1.16 C5 1.55 C2 1.60 C6 Q16 1 0.5168 -0.2573 1.1053 1.00000 0.05 0.18 0.72 C14 0.79 C13 1.47 H14 1.54 H13 Q17 1 0.1921 -0.0679 0.9117 1.00000 0.05 0.18 0.60 N1 1.05 C6 1.62 H6 1.69 C2 Q18 1 0.4053 0.0015 1.3033 1.00000 0.05 0.18 1.23 H10 1.83 C10 2.09 F2 2.14 H13 Q19 1 0.0425 -0.0961 0.9197 1.00000 0.05 0.18 0.84 F8 0.84 C1 1.34 F9 1.98 F7 Q20 1 0.3201 -0.0361 0.9824 1.00000 0.05 0.18 0.46 C7 0.54 H7 1.61 C8 1.70 C6 Shortest distances between peaks (including symmetry equivalents) 4 6 0.77 15 17 0.84 11 18 0.87 2 6 0.91 14 20 0.93 8 20 0.96 4 15 1.03 4 5 1.08 2 4 1.11 5 6 1.11 8 14 1.12 4 17 1.17 3 7 1.19 2 7 1.27 5 19 1.29 2 5 1.33 10 20 1.43 3 15 1.56 2 12 1.58 8 17 1.64 6 15 1.77 2 15 1.80 5 17 1.80 11 13 1.85 6 17 1.88 5 15 1.89 7 12 1.91 1 5 1.92 4 7 1.92 7 15 1.94 9 18 1.97 8 10 2.00 1 19 2.02 8 15 2.07 13 18 2.07 2 3 2.09 6 7 2.10 1 6 2.10 3 4 2.14 2 19 2.21 2 17 2.23 10 11 2.24 6 12 2.26 4 19 2.30 6 19 2.31 5 7 2.32 3 17 2.33 13 16 2.33 10 14 2.34 1 2 2.35 17 20 2.39 1 12 2.40 5 12 2.49 11 20 2.50 9 10 2.51 10 18 2.54 9 11 2.58 10 15 2.60 15 20 2.60 10 17 2.64 4 8 2.65 3 6 2.67 4 12 2.67 7 17 2.67 1 4 2.69 3 5 2.70 12 19 2.73 14 17 2.75 17 19 2.81 15 19 2.89 11 14 2.89 11 16 2.90 7 19 2.90 18 20 2.94 16 18 2.99 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.01: 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 0.01: Analyse other restraints etc. 3.41: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.46: Structure factors and derivatives 2.18: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.34: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.02: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0354 finished at 16:06:35 Total CPU time: 7.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++