+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0657 started at 22:08:46 on 15-Jun-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0657 in P2(1)/c CELL 0.71073 10.6315 12.0869 15.6257 90.000 101.585 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O P CL UNIT 44 88 12 8 12 16 V = 1967.03 F(000) = 952.0 Mu = 0.86 mm-1 Cell Wt = 1852.10 Rho = 1.564 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 20 SIZE 0.15 0.15 0.60 ACTA BOND WGHT 0.02690 1.59460 L.S. 4 TEMP -153.00 FVAR 0.48293 C1 1 0.108038 1.006808 -0.149304 11.00000 0.01673 0.01616 = 0.01705 0.00294 0.00272 0.00216 AFIX 23 H1A 2 0.040823 1.026646 -0.116398 11.00000 -1.20000 H1B 2 0.100228 1.058074 -0.199508 11.00000 -1.20000 AFIX 0 C2 1 0.240751 1.022160 -0.089613 11.00000 0.01295 0.01563 = 0.01720 0.00348 0.00182 0.00155 C3 1 0.246370 0.977777 0.003456 11.00000 0.01709 0.01407 = 0.01787 0.00066 0.00247 0.00015 AFIX 23 H3A 2 0.319585 1.012926 0.043350 11.00000 -1.20000 H3B 2 0.166874 0.999839 0.022849 11.00000 -1.20000 AFIX 0 C4 1 0.346930 0.968491 -0.129464 11.00000 0.01412 0.02002 = 0.01770 0.00519 0.00394 0.00254 AFIX 23 H4A 2 0.430603 0.983216 -0.090209 11.00000 -1.20000 H4B 2 0.333617 0.887392 -0.131013 11.00000 -1.20000 AFIX 0 C5 1 0.354911 1.007230 -0.221469 11.00000 0.02172 0.03213 = 0.02298 0.01069 0.00866 0.00483 AFIX 23 H5A 2 0.359589 1.089020 -0.222147 11.00000 -1.20000 H5B 2 0.275847 0.984600 -0.262778 11.00000 -1.20000 AFIX 0 C6 1 0.471877 0.959362 -0.252104 11.00000 0.01898 0.04322 = 0.02186 0.00500 0.00871 0.00058 AFIX 23 H6A 2 0.478013 0.994179 -0.308467 11.00000 -1.20000 H6B 2 0.550233 0.979537 -0.209101 11.00000 -1.20000 AFIX 0 C7 1 0.468912 0.834678 -0.263651 11.00000 0.02699 0.04716 = 0.04108 -0.01134 0.01370 0.00139 AFIX 137 H7A 2 0.468633 0.799057 -0.207349 11.00000 -1.50000 H7B 2 0.544905 0.810917 -0.285362 11.00000 -1.50000 H7C 2 0.391281 0.813533 -0.305700 11.00000 -1.50000 AFIX 0 C8 1 0.255588 1.150195 -0.079338 11.00000 0.01924 0.01509 = 0.02209 0.00361 0.00108 0.00132 AFIX 23 H8A 2 0.229660 1.183960 -0.137957 11.00000 -1.20000 H8B 2 0.194350 1.176328 -0.043666 11.00000 -1.20000 AFIX 0 C9 1 0.389158 1.194155 -0.037923 11.00000 0.02221 0.01781 = 0.03974 0.00603 -0.00130 -0.00304 AFIX 23 H9A 2 0.450309 1.173970 -0.075492 11.00000 -1.20000 H9B 2 0.418425 1.158314 0.019601 11.00000 -1.20000 AFIX 0 C10 1 0.390616 1.320142 -0.025649 11.00000 0.03728 0.01972 = 0.03692 0.00570 -0.00373 -0.00533 AFIX 23 H10A 2 0.480814 1.345988 -0.013554 11.00000 -1.20000 H10B 2 0.346481 1.354988 -0.080896 11.00000 -1.20000 AFIX 0 C11 1 0.326781 1.358671 0.047632 11.00000 0.06840 0.02852 = 0.03039 -0.00255 -0.00880 -0.00106 AFIX 137 H11A 2 0.238128 1.331584 0.037222 11.00000 -1.50000 H11B 2 0.326808 1.439711 0.049610 11.00000 -1.50000 H11C 2 0.374163 1.329612 0.103409 11.00000 -1.50000 AFIX 0 N1 3 0.012816 0.832355 -0.039234 11.00000 0.01429 0.01717 = 0.01127 -0.00067 0.00296 0.00283 N2 3 0.177555 0.658261 -0.008506 11.00000 0.02240 0.01482 = 0.01321 -0.00084 0.00137 0.00314 N3 3 0.029511 0.690098 -0.171472 11.00000 0.02314 0.01840 = 0.01264 -0.00248 0.00127 0.00389 O1 4 0.085731 0.893210 -0.182221 11.00000 0.01728 0.01968 = 0.01252 -0.00017 0.00358 0.00003 O2 4 0.260325 0.857129 0.011010 11.00000 0.01379 0.01546 = 0.01673 0.00474 0.00179 0.00226 P1 5 -0.000581 0.811295 -0.141451 11.00000 0.01308 0.01749 = 0.01093 -0.00038 0.00137 0.00183 P2 5 0.142283 0.780568 0.015839 11.00000 0.01444 0.01462 = 0.00947 0.00051 0.00246 0.00202 P3 5 0.128348 0.616737 -0.105515 11.00000 0.01996 0.01439 = 0.01273 -0.00103 0.00492 0.00153 CL1 6 -0.181186 0.848423 -0.197585 11.00000 0.01395 0.03177 = 0.01881 0.00029 -0.00151 0.00336 CL2 6 0.126222 0.780537 0.140604 11.00000 0.02320 0.02145 = 0.00989 0.00076 0.00442 0.00248 CL3 6 0.282861 0.587597 -0.158130 11.00000 0.02551 0.02629 = 0.02266 0.00037 0.01189 0.00543 CL4 6 0.053339 0.465938 -0.104649 11.00000 0.03540 0.01811 = 0.02205 -0.00144 0.00700 -0.00641 HKLF 4 Covalent radii and connectivity table for 2007src0657 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C4 C1 C3 C8 C3 - O2 C2 C4 - C5 C2 C5 - C4 C6 C6 - C7 C5 C7 - C6 C8 - C9 C2 C9 - C8 C10 C10 - C11 C9 C11 - C10 N1 - P1 P2 N2 - P3 P2 N3 - P3 P1 O1 - C1 P1 O2 - C3 P2 P1 - O1 N3 N1 Cl1 P2 P2 - O2 N2 N1 Cl2 P1 P3 - N2 N3 Cl4 Cl3 Cl1 - P1 Cl2 - P2 Cl3 - P3 Cl4 - P3 25924 Reflections read, of which 684 rejected -13 =< h =< 13, -15 =< k =< 15, -20 =< l =< 20, Max. 2-theta = 55.00 0 Systematic absence violations 0 Inconsistent equivalents 4512 Unique reflections, of which 0 suppressed R(int) = 0.0403 R(sigma) = 0.0306 Friedel opposites merged Maximum memory for data reduction = 2172 / 44802 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 = 2790 / 262234 wR2 = 0.0705 before cycle 1 for 4512 data and 210 / 210 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48293 0.00053 -0.009 OSF Mean shift/esd = 0.015 Maximum = 0.054 for U33 P3 Max. shift = 0.000 A for H11A Max. dU = 0.000 for C8 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2790 / 262234 wR2 = 0.0705 before cycle 2 for 4512 data and 210 / 210 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48294 0.00053 0.021 OSF Mean shift/esd = 0.005 Maximum = 0.021 for OSF Max. shift = 0.000 A for H7C Max. dU = 0.000 for C8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2790 / 262234 wR2 = 0.0705 before cycle 3 for 4512 data and 210 / 210 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48294 0.00053 0.002 OSF Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H7C Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2790 / 262234 wR2 = 0.0705 before cycle 4 for 4512 data and 210 / 210 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48294 0.00053 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Cl3 Max. shift = 0.000 A for H7B Max. dU = 0.000 for N2 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 H1A 0.0408 1.0266 -0.1164 23 0.990 0.000 C1 O1 C2 H1B 0.1002 1.0581 -0.1995 23 0.990 0.000 C1 O1 C2 H3A 0.3196 1.0129 0.0433 23 0.990 0.000 C3 O2 C2 H3B 0.1669 0.9998 0.0228 23 0.990 0.000 C3 O2 C2 H4A 0.4306 0.9832 -0.0902 23 0.990 0.000 C4 C5 C2 H4B 0.3336 0.8874 -0.1310 23 0.990 0.000 C4 C5 C2 H5A 0.3596 1.0890 -0.2221 23 0.990 0.000 C5 C4 C6 H5B 0.2759 0.9846 -0.2628 23 0.990 0.000 C5 C4 C6 H6A 0.4780 0.9942 -0.3085 23 0.990 0.000 C6 C7 C5 H6B 0.5502 0.9795 -0.2091 23 0.990 0.000 C6 C7 C5 H7A 0.4686 0.7991 -0.2074 137 0.980 0.000 C7 C6 H7A H7B 0.5449 0.8109 -0.2854 137 0.980 0.000 C7 C6 H7A H7C 0.3913 0.8135 -0.3057 137 0.980 0.000 C7 C6 H7A H8A 0.2297 1.1840 -0.1380 23 0.990 0.000 C8 C9 C2 H8B 0.1944 1.1763 -0.0437 23 0.990 0.000 C8 C9 C2 H9A 0.4503 1.1740 -0.0755 23 0.990 0.000 C9 C8 C10 H9B 0.4184 1.1583 0.0196 23 0.990 0.000 C9 C8 C10 H10A 0.4808 1.3460 -0.0135 23 0.990 0.000 C10 C11 C9 H10B 0.3465 1.3550 -0.0809 23 0.990 0.000 C10 C11 C9 H11A 0.2381 1.3316 0.0372 137 0.980 0.000 C11 C10 H11A H11B 0.3268 1.4397 0.0496 137 0.980 0.000 C11 C10 H11A H11C 0.3741 1.3296 0.1034 137 0.980 0.000 C11 C10 H11A 2007src0657 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.10804 1.00681 -0.14930 1.00000 0.01676 0.01614 0.01706 0.00293 0.00273 0.00215 0.01675 0.00320 0.00016 0.00014 0.00011 0.00000 0.00082 0.00082 0.00085 0.00065 0.00065 0.00066 0.00034 H1A 0.04083 1.02665 -0.11639 1.00000 0.02010 0.00000 0.00000 H1B 0.10023 1.05807 -0.19950 1.00000 0.02010 0.00000 0.00000 C2 0.24075 1.02216 -0.08961 1.00000 0.01296 0.01563 0.01719 0.00350 0.00181 0.00156 0.01543 0.00319 0.00016 0.00014 0.00011 0.00000 0.00077 0.00082 0.00083 0.00063 0.00063 0.00065 0.00033 C3 0.24637 0.97777 0.00345 1.00000 0.01710 0.01407 0.01789 0.00066 0.00249 0.00014 0.01650 0.00323 0.00016 0.00014 0.00011 0.00000 0.00082 0.00081 0.00085 0.00063 0.00065 0.00066 0.00034 H3A 0.31959 1.01292 0.04335 1.00000 0.01980 0.00000 0.00000 H3B 0.16688 0.99984 0.02285 1.00000 0.01980 0.00000 0.00000 C4 0.34693 0.96850 -0.12946 1.00000 0.01413 0.02003 0.01772 0.00518 0.00391 0.00252 0.01719 0.00337 0.00016 0.00015 0.00011 0.00000 0.00078 0.00086 0.00085 0.00066 0.00065 0.00068 0.00034 H4A 0.43060 0.98322 -0.09021 1.00000 0.02063 0.00000 0.00000 H4B 0.33362 0.88740 -0.13101 1.00000 0.02063 0.00000 0.00000 C5 0.35492 1.00722 -0.22147 1.00000 0.02172 0.03210 0.02300 0.01067 0.00865 0.00482 0.02503 0.00397 0.00018 0.00017 0.00012 0.00000 0.00092 0.00105 0.00096 0.00080 0.00075 0.00080 0.00041 H5A 0.35959 1.08901 -0.22215 1.00000 0.03003 0.00000 0.00000 H5B 0.27585 0.98459 -0.26278 1.00000 0.03003 0.00000 0.00000 C6 0.47188 0.95936 -0.25210 1.00000 0.01901 0.04324 0.02183 0.00502 0.00870 0.00058 0.02738 0.00393 0.00018 0.00018 0.00013 0.00000 0.00090 0.00121 0.00096 0.00084 0.00075 0.00085 0.00043 H6A 0.47801 0.99419 -0.30846 1.00000 0.03286 0.00000 0.00000 H6B 0.55023 0.97954 -0.20910 1.00000 0.03286 0.00000 0.00000 C7 0.46891 0.83468 -0.26365 1.00000 0.02695 0.04720 0.04108 -0.01136 0.01368 0.00135 0.03746 0.00430 0.00021 0.00020 0.00016 0.00000 0.00108 0.00138 0.00129 0.00105 0.00095 0.00099 0.00052 H7A 0.46862 0.79906 -0.20736 1.00000 0.05618 0.00000 0.00000 H7B 0.54492 0.81093 -0.28535 1.00000 0.05618 0.00000 0.00000 H7C 0.39129 0.81354 -0.30571 1.00000 0.05618 0.00000 0.00000 C8 0.25559 1.15020 -0.07934 1.00000 0.01927 0.01513 0.02208 0.00360 0.00110 0.00133 0.01925 0.00332 0.00017 0.00014 0.00012 0.00000 0.00085 0.00084 0.00091 0.00067 0.00070 0.00068 0.00036 H8A 0.22966 1.18396 -0.13796 1.00000 0.02310 0.00000 0.00000 H8B 0.19435 1.17633 -0.04367 1.00000 0.02310 0.00000 0.00000 C9 0.38915 1.19415 -0.03793 1.00000 0.02224 0.01780 0.03975 0.00602 -0.00131 -0.00306 0.02765 0.00370 0.00019 0.00016 0.00014 0.00000 0.00095 0.00091 0.00119 0.00081 0.00084 0.00076 0.00043 H9A 0.45030 1.17397 -0.07550 1.00000 0.03318 0.00000 0.00000 H9B 0.41842 1.15831 0.01960 1.00000 0.03318 0.00000 0.00000 C10 0.39061 1.32014 -0.02565 1.00000 0.03728 0.01973 0.03693 0.00571 -0.00374 -0.00532 0.03287 0.00399 0.00022 0.00016 0.00015 0.00000 0.00117 0.00098 0.00119 0.00085 0.00093 0.00088 0.00047 H10A 0.48081 1.34598 -0.01355 1.00000 0.03945 0.00000 0.00000 H10B 0.34649 1.35499 -0.08090 1.00000 0.03945 0.00000 0.00000 C11 0.32677 1.35868 0.04763 1.00000 0.06843 0.02855 0.03036 -0.00256 -0.00880 -0.00106 0.04506 0.00447 0.00027 0.00019 0.00015 0.00000 0.00172 0.00116 0.00122 0.00094 0.00115 0.00115 0.00062 H11A 0.23811 1.33160 0.03722 1.00000 0.06758 0.00000 0.00000 H11B 0.32681 1.43972 0.04961 1.00000 0.06758 0.00000 0.00000 H11C 0.37414 1.32962 0.10341 1.00000 0.06758 0.00000 0.00000 N1 0.01281 0.83235 -0.03924 1.00000 0.01429 0.01716 0.01130 -0.00067 0.00295 0.00282 0.01419 0.00261 0.00013 0.00012 0.00009 0.00000 0.00066 0.00070 0.00065 0.00053 0.00053 0.00056 0.00028 N2 0.17756 0.65826 -0.00851 1.00000 0.02238 0.01484 0.01324 -0.00083 0.00139 0.00316 0.01712 0.00272 0.00014 0.00012 0.00009 0.00000 0.00074 0.00070 0.00069 0.00054 0.00057 0.00059 0.00030 N3 0.02951 0.69010 -0.17147 1.00000 0.02313 0.01842 0.01265 -0.00249 0.00128 0.00388 0.01839 0.00275 0.00014 0.00012 0.00009 0.00000 0.00076 0.00073 0.00070 0.00056 0.00058 0.00061 0.00031 O1 0.08572 0.89321 -0.18222 1.00000 0.01729 0.01969 0.01252 -0.00017 0.00358 0.00002 0.01642 0.00220 0.00011 0.00010 0.00007 0.00000 0.00058 0.00061 0.00058 0.00046 0.00046 0.00049 0.00025 O2 0.26032 0.85713 0.01101 1.00000 0.01379 0.01547 0.01674 0.00474 0.00178 0.00227 0.01551 0.00220 0.00011 0.00009 0.00008 0.00000 0.00056 0.00058 0.00059 0.00046 0.00045 0.00046 0.00024 P1 -0.00058 0.81129 -0.14145 1.00000 0.01308 0.01751 0.01094 -0.00038 0.00137 0.00183 0.01399 0.00081 0.00004 0.00004 0.00003 0.00000 0.00020 0.00022 0.00020 0.00016 0.00015 0.00016 0.00010 P2 0.14228 0.78057 0.01584 1.00000 0.01445 0.01463 0.00948 0.00051 0.00246 0.00202 0.01284 0.00080 0.00004 0.00003 0.00003 0.00000 0.00021 0.00021 0.00020 0.00015 0.00016 0.00016 0.00010 P3 0.12835 0.61674 -0.10552 1.00000 0.01997 0.01440 0.01275 -0.00103 0.00492 0.00153 0.01548 0.00083 0.00004 0.00004 0.00003 0.00000 0.00022 0.00021 0.00021 0.00016 0.00017 0.00017 0.00010 Cl1 -0.18119 0.84842 -0.19758 1.00000 0.01395 0.03178 0.01881 0.00028 -0.00152 0.00337 0.02218 0.00081 0.00004 0.00004 0.00003 0.00000 0.00020 0.00025 0.00021 0.00017 0.00016 0.00017 0.00010 Cl2 0.12622 0.78054 0.14060 1.00000 0.02321 0.02145 0.00990 0.00077 0.00442 0.00248 0.01803 0.00080 0.00004 0.00003 0.00003 0.00000 0.00021 0.00021 0.00019 0.00015 0.00015 0.00017 0.00010 Cl3 0.28286 0.58760 -0.15813 1.00000 0.02552 0.02630 0.02267 0.00037 0.01190 0.00543 0.02384 0.00090 0.00004 0.00004 0.00003 0.00000 0.00023 0.00023 0.00023 0.00017 0.00018 0.00018 0.00011 Cl4 0.05334 0.46594 -0.10465 1.00000 0.03541 0.01811 0.02205 -0.00144 0.00700 -0.00642 0.02502 0.00085 0.00005 0.00004 0.00003 0.00000 0.00026 0.00021 0.00023 0.00017 0.00019 0.00019 0.00011 Final Structure Factor Calculation for 2007src0657 in P2(1)/c Total number of l.s. parameters = 210 Maximum vector length = 511 Memory required = 2580 / 25039 wR2 = 0.0705 before cycle 5 for 4512 data and 0 / 210 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0269 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0284 for 3904 Fo > 4sig(Fo) and 0.0360 for all 4512 data wR2 = 0.0705, GooF = S = 1.037, Restrained GooF = 1.037 for all data Occupancy sum of asymmetric unit = 23.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0197 0.0176 0.0129 C1 0.0201 0.0148 0.0114 C2 0.0189 0.0166 0.0140 C3 0.0244 0.0143 0.0129 C4 0.0402 0.0199 0.0150 C5 0.0444 0.0236 0.0141 C6 0.0559 0.0361 0.0204 C7 0.0254 0.0193 0.0131 C8 0.0464 0.0209 0.0156 C9 0.0534 0.0278 0.0175 C10 0.0808 0.0301 0.0242 C11 0.0190 0.0128 0.0107 N1 0.0247 0.0138 0.0129 N2 0.0269 0.0165 0.0117 N3 0.0197 0.0173 0.0123 O1 0.0209 0.0154 0.0103 O2 0.0184 0.0129 0.0107 P1 0.0166 0.0126 0.0094 P2 0.0204 0.0149 0.0112 P3 0.0325 0.0226 0.0114 Cl1 0.0250 0.0197 0.0094 Cl2 0.0330 0.0246 0.0140 Cl3 0.0375 0.0215 0.0160 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.036 0.054 0.074 0.096 0.121 0.148 0.189 0.257 1.000 Number in group 464. 443. 452. 463. 443. 443. 452. 447. 451. 454. GooF 0.914 1.013 1.082 1.108 1.049 1.064 1.018 1.029 0.977 1.099 K 0.926 0.889 0.927 0.958 0.967 0.985 0.990 1.008 1.016 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 455. 457. 462. 431. 456. 452. 444. 458. 444. 453. GooF 0.889 0.945 0.940 0.967 0.911 0.919 0.971 0.897 0.997 1.682 K 0.975 1.001 1.009 1.005 1.015 1.016 1.018 1.015 1.009 0.991 R1 0.078 0.062 0.049 0.047 0.036 0.031 0.030 0.020 0.020 0.028 Recommended weighting scheme: WGHT 0.0271 1.5848 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) 3 3 3 804.92 538.99 6.36 0.114 2.21 0 6 2 1242.82 963.01 5.16 0.152 1.95 4 2 1 912.50 693.90 4.84 0.129 2.30 0 4 2 38.99 89.41 4.43 0.046 2.81 2 2 5 47.58 101.71 4.23 0.049 2.26 -5 2 5 1095.61 1344.32 4.19 0.180 1.82 -3 1 5 108.06 58.98 4.15 0.038 2.51 1 5 3 233.26 155.61 4.05 0.061 2.10 -2 6 3 470.57 354.85 4.00 0.092 1.81 2 5 0 549.62 423.29 3.93 0.101 2.19 -3 0 8 639.21 820.75 3.91 0.141 1.84 11 4 4 83.34 159.25 3.86 0.062 0.84 -1 4 1 130.10 198.01 3.79 0.069 2.88 -2 2 5 369.16 275.50 3.76 0.081 2.62 1 4 5 171.65 109.33 3.74 0.051 2.05 -4 4 3 1692.47 1434.05 3.72 0.186 1.94 4 0 0 180.38 260.40 3.68 0.079 2.60 0 4 6 256.38 178.53 3.67 0.066 1.95 -2 0 2 4621.12 5287.70 3.58 0.357 4.77 -3 5 3 52.10 94.32 3.47 0.048 1.93 4 1 3 1459.59 1220.41 3.46 0.171 2.12 0 6 0 16368.66 14605.98 3.39 0.593 2.01 -6 4 4 240.05 323.80 3.32 0.088 1.49 5 0 0 336.83 435.25 3.31 0.102 2.08 1 3 6 38.80 14.65 3.28 0.019 2.04 0 11 1 235.09 316.88 3.27 0.087 1.10 2 3 3 85.13 131.89 3.19 0.056 2.56 -7 5 16 9.15 49.38 3.18 0.034 0.84 1 1 4 93.17 56.72 3.18 0.037 3.25 1 4 2 67.87 38.01 3.14 0.030 2.66 -6 14 4 68.37 205.47 3.13 0.070 0.77 1 2 8 256.90 190.41 3.10 0.068 1.74 -3 4 5 35.90 67.20 3.10 0.040 1.96 -13 1 5 63.83 0.06 3.02 0.001 0.81 2 1 0 24678.09 27340.69 3.01 0.811 4.78 1 11 11 717.96 913.97 3.00 0.148 0.85 11 2 3 16.66 50.52 2.97 0.035 0.89 7 0 6 368.52 490.84 2.96 0.109 1.19 0 6 1 76.79 119.13 2.95 0.054 2.00 0 3 9 56.52 29.98 2.95 0.027 1.57 -13 4 4 737.89 586.11 2.87 0.119 0.79 2 0 0 414.56 509.40 2.83 0.111 5.21 7 5 5 64.03 27.70 2.81 0.026 1.11 -3 3 14 1683.29 1473.53 2.81 0.188 1.07 -2 2 1 2985.41 3329.53 2.78 0.283 3.97 -2 0 4 14349.24 15861.39 2.78 0.618 3.43 -2 4 1 670.37 567.42 2.77 0.117 2.62 1 4 4 1739.06 1533.14 2.77 0.192 2.25 4 6 2 1213.00 1054.56 2.77 0.159 1.52 -2 1 2 24750.01 27143.30 2.76 0.808 4.44 Bond lengths and angles C1 - Distance Angles O1 1.4687 (0.0020) C2 1.5383 (0.0023) 112.90 (0.13) C1 - O1 C2 - Distance Angles C4 1.5379 (0.0023) C1 1.5383 (0.0023) 111.23 (0.14) C3 1.5399 (0.0023) 110.06 (0.13) 112.80 (0.14) C8 1.5607 (0.0023) 113.12 (0.14) 104.09 (0.13) 105.33 (0.14) C2 - C4 C1 C3 C3 - Distance Angles O2 1.4680 (0.0020) C2 1.5399 (0.0023) 113.96 (0.13) C3 - O2 C4 - Distance Angles C5 1.5304 (0.0024) C2 1.5379 (0.0023) 115.79 (0.14) C4 - C5 C5 - Distance Angles C4 1.5304 (0.0024) C6 1.5327 (0.0025) 112.30 (0.15) C5 - C4 C6 - Distance Angles C7 1.5173 (0.0030) C5 1.5327 (0.0025) 114.41 (0.17) C6 - C7 C7 - Distance Angles C6 1.5173 (0.0030) C7 - C8 - Distance Angles C9 1.5324 (0.0025) C2 1.5607 (0.0023) 116.95 (0.14) C8 - C9 C9 - Distance Angles C8 1.5324 (0.0025) C10 1.5345 (0.0027) 112.46 (0.16) C9 - C8 C10 - Distance Angles C11 1.5169 (0.0034) C9 1.5345 (0.0027) 113.85 (0.18) C10 - C11 C11 - Distance Angles C10 1.5169 (0.0034) C11 - N1 - Distance Angles P1 1.5952 (0.0014) P2 1.5973 (0.0014) 111.77 (0.08) N1 - P1 N2 - Distance Angles P3 1.5827 (0.0015) P2 1.5900 (0.0014) 118.39 (0.09) N2 - P3 N3 - Distance Angles P3 1.5867 (0.0015) P1 1.5901 (0.0015) 118.00 (0.09) N3 - P3 O1 - Distance Angles C1 1.4687 (0.0020) P1 1.5694 (0.0012) 120.94 (0.10) O1 - C1 O2 - Distance Angles C3 1.4680 (0.0020) P2 1.5732 (0.0012) 121.30 (0.10) O2 - C3 P1 - Distance Angles O1 1.5694 (0.0012) N3 1.5901 (0.0015) 107.02 (0.07) N1 1.5952 (0.0014) 111.34 (0.07) 117.36 (0.08) Cl1 1.9953 (0.0006) 105.61 (0.05) 108.08 (0.06) 106.79 (0.05) P2 2.6431 (0.0006) 101.10 (0.05) 91.88 (0.06) 34.14 (0.05) 139.73 (0.02) P1 - O1 N3 N1 Cl1 P2 - Distance Angles O2 1.5732 (0.0012) N2 1.5900 (0.0014) 107.86 (0.07) N1 1.5973 (0.0014) 110.67 (0.07) 117.04 (0.08) Cl2 1.9909 (0.0006) 105.85 (0.05) 107.75 (0.06) 107.07 (0.05) P1 2.6431 (0.0006) 100.82 (0.05) 91.56 (0.05) 34.09 (0.05) 139.85 (0.02) P2 - O2 N2 N1 Cl2 P3 - Distance Angles N2 1.5827 (0.0015) N3 1.5867 (0.0015) 119.56 (0.08) Cl4 1.9907 (0.0006) 109.86 (0.06) 107.59 (0.06) Cl3 2.0102 (0.0006) 107.89 (0.06) 108.74 (0.06) 101.76 (0.03) P3 - N2 N3 Cl4 Cl1 - Distance Angles P1 1.9953 (0.0006) Cl1 - Cl2 - Distance Angles P2 1.9909 (0.0006) Cl2 - Cl3 - Distance Angles P3 2.0102 (0.0006) Cl3 - Cl4 - Distance Angles P3 1.9907 (0.0006) Cl4 - FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0358 for 4512 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.8193 -0.0006 0.1112 [ 0.71 A from C2 ] Deepest hole -0.42 at 0.8263 0.4216 0.0664 [ 0.84 A from P3 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2625 / 22800 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1807 1.0006 -0.1112 1.00000 0.05 0.36 0.71 C2 0.88 C1 1.51 H1A 1.63 H1B Q2 1 0.2416 0.9994 -0.0479 1.00000 0.05 0.35 0.71 C2 0.83 C3 1.48 H3B 1.51 H3A Q3 1 0.3533 0.9797 -0.1781 1.00000 0.05 0.34 0.76 C5 0.79 C4 1.38 H4B 1.41 H5B Q4 1 0.0035 0.8192 -0.0852 1.00000 0.05 0.32 0.72 N1 0.88 P1 1.99 P2 2.10 O1 Q5 1 0.2897 0.9984 -0.1082 1.00000 0.05 0.30 0.71 C2 0.83 C4 1.48 H4A 1.49 H4B Q6 1 -0.0258 0.4786 -0.1060 1.00000 0.05 0.30 0.85 CL4 2.34 P3 2.86 N3 3.01 H5B Q7 1 0.2381 1.0734 -0.0800 1.00000 0.05 0.29 0.64 C2 0.95 C8 1.48 H8B 1.61 H8A Q8 1 0.4180 0.9763 -0.2247 1.00000 0.05 0.28 0.78 C5 0.81 C6 1.38 H6B 1.50 H5A Q9 1 0.2165 0.5976 -0.1233 1.00000 0.05 0.27 0.98 CL3 1.06 P3 2.06 N2 2.27 N3 Q10 1 0.1339 0.7774 0.0818 1.00000 0.05 0.27 0.94 CL2 1.05 P2 2.13 N2 2.13 O2 Q11 1 -0.0322 0.8242 -0.0249 1.00000 0.05 0.26 0.58 N1 1.91 P2 1.92 P1 2.20 H8B Q12 1 0.3249 1.1682 -0.0535 1.00000 0.05 0.25 0.75 C9 0.80 C8 1.36 H9B 1.43 H8B Q13 1 0.3846 1.2502 -0.0302 1.00000 0.05 0.25 0.69 C9 0.85 C10 1.36 H9B 1.43 H9A Q14 1 0.2183 0.5614 -0.1729 1.00000 0.05 0.25 0.75 CL3 1.69 P3 2.51 CL4 2.54 N3 Q15 1 -0.0126 0.7208 -0.1528 1.00000 0.05 0.24 0.69 N3 1.11 P1 1.98 P3 2.20 N1 Q16 1 0.0418 0.8589 -0.0303 1.00000 0.05 0.24 0.45 N1 1.50 P2 1.80 P1 2.22 H3B Q17 1 0.0352 0.5624 -0.0639 1.00000 0.05 0.24 1.36 CL4 1.45 P3 1.96 N2 2.27 N3 Q18 1 0.0835 1.0088 -0.2220 1.00000 0.05 0.23 0.70 H1B 1.11 C1 1.53 O1 1.81 H1A Q19 1 0.0169 0.8922 -0.1823 1.00000 0.05 0.22 0.73 O1 1.20 P1 1.71 C1 1.91 H1A Q20 1 0.4846 1.3746 0.0071 1.00000 0.05 0.22 0.47 H10A 1.22 C10 1.81 H10B 1.92 C11 Shortest distances between peaks (including symmetry equivalents) 9 14 0.89 11 16 0.91 4 16 1.00 2 7 1.02 1 2 1.07 4 11 1.09 3 8 1.10 1 7 1.12 1 5 1.15 2 5 1.16 5 7 1.19 12 13 1.19 6 17 1.31 3 5 1.41 7 12 1.48 4 15 1.58 18 19 1.75 4 19 1.79 1 18 1.83 13 20 1.87 10 16 2.08 15 19 2.16 5 12 2.23 2 12 2.23 10 11 2.24 1 19 2.28 1 3 2.30 9 17 2.34 15 17 2.36 16 19 2.37 11 15 2.40 3 7 2.43 5 8 2.50 15 16 2.52 5 18 2.53 2 3 2.56 1 12 2.59 7 18 2.60 6 18 2.66 7 13 2.67 6 17 2.72 17 17 2.72 1 16 2.73 11 19 2.74 4 10 2.74 2 16 2.78 9 15 2.81 14 17 2.83 3 18 2.83 2 18 2.90 1 4 2.97 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.01: 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. 6.67: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.97: Structure factors and derivatives 2.43: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.56: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0657 finished at 22:09:01 Total CPU time: 12.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++