+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0655 started at 19:09:45 on 14-Jun-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0655 in P-1 CELL 0.71073 8.2012 9.0665 12.8131 83.344 84.013 72.530 ZERR 2.00 0.0001 0.0001 0.0001 0.001 0.001 0.001 LATT 1 SFAC C H N O P CL UNIT 18 36 6 4 6 8 V = 900.23 F(000) = 444.0 Mu = 0.93 mm-1 Cell Wt = 869.95 Rho = 1.605 MERG 2 OMIT -3.00 55.00 OMIT 0 0 2 OMIT -2 -2 2 OMIT 1 2 2 OMIT -1 1 2 FMAP 2 PLAN 20 SIZE 0.05 0.10 0.18 ACTA BOND WGHT 0.02790 0.47640 L.S. 4 TEMP -153.00 FVAR 1.00650 C1 1 0.668759 -0.047712 0.299395 11.00000 0.01435 0.01836 = 0.02238 0.00345 -0.00417 -0.00831 AFIX 23 H1A 2 0.795018 -0.076471 0.286323 11.00000 -1.20000 H1B 2 0.639821 -0.018423 0.372599 11.00000 -1.20000 AFIX 0 C2 1 0.587975 0.093644 0.223049 11.00000 0.01204 0.01616 = 0.01683 -0.00008 -0.00106 -0.00545 C3 1 0.403081 0.181192 0.258265 11.00000 0.01415 0.01664 = 0.02086 -0.00161 -0.00081 -0.00687 AFIX 23 H3A 2 0.397492 0.199015 0.333506 11.00000 -1.20000 H3B 2 0.370541 0.283927 0.217375 11.00000 -1.20000 AFIX 0 C4 1 0.596333 0.046653 0.110151 11.00000 0.01655 0.01763 = 0.01680 -0.00036 -0.00067 -0.00559 AFIX 23 H4A 2 0.535048 -0.032578 0.111809 11.00000 -1.20000 H4B 2 0.534650 0.138698 0.065190 11.00000 -1.20000 AFIX 0 C5 1 0.777268 -0.017856 0.059196 11.00000 0.02063 0.02275 = 0.02720 -0.00537 0.00520 -0.00568 AFIX 137 H5A 2 0.837774 0.061230 0.053951 11.00000 -1.50000 H5B 2 0.770576 -0.046162 -0.011428 11.00000 -1.50000 H5C 2 0.839479 -0.110004 0.102391 11.00000 -1.50000 AFIX 0 C6 1 0.696269 0.205560 0.231254 11.00000 0.01721 0.01996 = 0.02154 -0.00057 -0.00259 -0.00971 AFIX 23 H6A 2 0.679335 0.235189 0.304459 11.00000 -1.20000 H6B 2 0.818701 0.147428 0.218691 11.00000 -1.20000 AFIX 0 C7 1 0.659450 0.354290 0.156963 11.00000 0.02382 0.01761 = 0.02212 -0.00261 0.00062 -0.00864 AFIX 23 H7A 2 0.648682 0.329120 0.085320 11.00000 -1.20000 H7B 2 0.548830 0.426796 0.180930 11.00000 -1.20000 AFIX 0 C8 1 0.799644 0.433308 0.152497 11.00000 0.02964 0.02676 = 0.06160 0.00334 -0.00140 -0.01784 AFIX 23 H8A 2 0.910281 0.359876 0.129537 11.00000 -1.20000 H8B 2 0.809478 0.458845 0.224197 11.00000 -1.20000 AFIX 0 C9 1 0.767398 0.580885 0.078264 11.00000 0.05208 0.02519 = 0.04639 -0.00579 0.01090 -0.02286 AFIX 137 H9A 2 0.752089 0.557564 0.007761 11.00000 -1.50000 H9B 2 0.865542 0.622228 0.074906 11.00000 -1.50000 H9C 2 0.663770 0.658021 0.104258 11.00000 -1.50000 AFIX 0 N1 3 0.347896 -0.078849 0.420845 11.00000 0.01635 0.01848 = 0.01509 -0.00266 -0.00120 -0.00556 N2 3 0.108203 -0.094364 0.294814 11.00000 0.01237 0.01696 = 0.02471 -0.00398 -0.00221 -0.00354 N3 3 0.395412 -0.340758 0.322894 11.00000 0.01396 0.01613 = 0.02158 -0.00250 -0.00435 -0.00339 O1 4 0.610542 -0.183755 0.288725 11.00000 0.01518 0.01497 = 0.01940 0.00120 -0.00006 -0.00434 O2 4 0.278372 0.098707 0.244612 11.00000 0.01224 0.02099 = 0.01686 -0.00107 -0.00060 -0.00686 P1 5 0.477733 -0.229309 0.373534 11.00000 0.01313 0.01549 = 0.01375 0.00081 -0.00275 -0.00487 P2 5 0.204621 0.009310 0.341747 11.00000 0.01172 0.01542 = 0.01631 -0.00271 0.00077 -0.00432 P3 5 0.209442 -0.270914 0.283407 11.00000 0.01306 0.01569 = 0.01597 -0.00219 -0.00213 -0.00444 CL1 6 0.616182 -0.356163 0.488816 11.00000 0.02521 0.02243 = 0.01963 0.00525 -0.01042 -0.00794 CL2 6 0.032351 0.172978 0.419024 11.00000 0.01942 0.02001 = 0.02550 -0.00738 0.00584 -0.00389 CL3 6 0.219592 -0.313395 0.132431 11.00000 0.02884 0.03305 = 0.01837 -0.00810 -0.00719 0.00147 CL4 6 0.061372 -0.401944 0.350411 11.00000 0.02116 0.02279 = 0.03787 0.00099 -0.00176 -0.01241 HKLF 4 Covalent radii and connectivity table for 2007src0655 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C3 C1 C4 C6 C3 - O2 C2 C4 - C5 C2 C5 - C4 C6 - C7 C2 C7 - C8 C6 C8 - C7 C9 C9 - C8 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 O1 - C1 P1 O2 - C3 P2 P1 - O1 N1 N3 Cl1 P2 P2 - O2 N1 N2 Cl2 P1 P3 - N3 N2 Cl3 Cl4 Cl1 - P1 Cl2 - P2 Cl3 - P3 Cl4 - P3 37351 Reflections read, of which 17 rejected -10 =< h =< 10, -11 =< k =< 11, -16 =< l =< 16, Max. 2-theta = 55.00 0 Systematic absence violations 0 Inconsistent equivalents 4131 Unique reflections, of which 0 suppressed R(int) = 0.0350 R(sigma) = 0.0229 Friedel opposites merged Maximum memory for data reduction = 1950 / 41105 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 = 2490 / 240175 wR2 = 0.0633 before cycle 1 for 4131 data and 192 / 192 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0279 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.00421 0.00106 -2.156 OSF Mean shift/esd = 0.373 Maximum = -2.156 for OSF Max. shift = 0.006 A for H9A Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2490 / 240175 wR2 = 0.0631 before cycle 2 for 4131 data and 192 / 192 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0279 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.00306 0.00106 -1.086 OSF Mean shift/esd = 0.128 Maximum = -1.086 for OSF Max. shift = 0.003 A for H9A Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2490 / 240175 wR2 = 0.0630 before cycle 3 for 4131 data and 192 / 192 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0279 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.00306 0.00106 -0.003 OSF Mean shift/esd = 0.002 Maximum = -0.040 for tors H9A Max. shift = 0.001 A for H9A Max. dU = 0.000 for C5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2490 / 240175 wR2 = 0.0630 before cycle 4 for 4131 data and 192 / 192 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0279 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.00306 0.00106 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.007 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for C2 Largest correlation matrix elements -0.500 U12 C9 / U11 C9 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.7950 -0.0765 0.2863 23 0.990 0.000 C1 O1 C2 H1B 0.6399 -0.0184 0.3726 23 0.990 0.000 C1 O1 C2 H3A 0.3975 0.1989 0.3336 23 0.990 0.000 C3 O2 C2 H3B 0.3706 0.2838 0.2174 23 0.990 0.000 C3 O2 C2 H4A 0.5350 -0.0325 0.1118 23 0.990 0.000 C4 C5 C2 H4B 0.5347 0.1388 0.0653 23 0.990 0.000 C4 C5 C2 H5A 0.8374 0.0616 0.0535 137 0.980 0.000 C5 C4 H5A H5B 0.7705 -0.0470 -0.0111 137 0.980 0.000 C5 C4 H5A H5C 0.8397 -0.1094 0.1028 137 0.980 0.000 C5 C4 H5A H6A 0.6795 0.2350 0.3045 23 0.990 0.000 C6 C7 C2 H6B 0.8187 0.1473 0.2186 23 0.990 0.000 C6 C7 C2 H7A 0.6486 0.3291 0.0853 23 0.990 0.000 C7 C8 C6 H7B 0.5488 0.4267 0.1810 23 0.990 0.000 C7 C8 C6 H8A 0.9103 0.3599 0.1297 23 0.990 0.000 C8 C7 C9 H8B 0.8093 0.4590 0.2242 23 0.990 0.000 C8 C7 C9 H9A 0.7534 0.5572 0.0075 137 0.980 0.000 C9 C8 H9A H9B 0.8652 0.6227 0.0754 137 0.980 0.000 C9 C8 H9A H9C 0.6632 0.6577 0.1037 137 0.980 0.000 C9 C8 H9A 2007src0655 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.66876 -0.04768 0.29936 1.00000 0.01404 0.01813 0.02182 0.00337 -0.00407 -0.00805 0.01747 0.00202 0.00017 0.00016 0.00011 0.00000 0.00061 0.00064 0.00066 0.00052 0.00051 0.00051 0.00027 H1A 0.79502 -0.07645 0.28626 1.00000 0.02097 0.00000 0.00000 H1B 0.63988 -0.01840 0.37257 1.00000 0.02097 0.00000 0.00000 C2 0.58803 0.09356 0.22311 1.00000 0.01202 0.01558 0.01636 -0.00012 -0.00099 -0.00540 0.01446 0.00194 0.00016 0.00015 0.00010 0.00000 0.00058 0.00061 0.00060 0.00047 0.00047 0.00048 0.00025 C3 0.40312 0.18108 0.25831 1.00000 0.01416 0.01629 0.02067 -0.00169 -0.00072 -0.00684 0.01654 0.00198 0.00017 0.00015 0.00011 0.00000 0.00060 0.00062 0.00065 0.00050 0.00049 0.00050 0.00026 H3A 0.39751 0.19886 0.33356 1.00000 0.01985 0.00000 0.00000 H3B 0.37062 0.28384 0.21745 1.00000 0.01985 0.00000 0.00000 C4 0.59629 0.04670 0.11020 1.00000 0.01636 0.01705 0.01645 -0.00044 -0.00083 -0.00539 0.01662 0.00203 0.00017 0.00016 0.00010 0.00000 0.00062 0.00063 0.00062 0.00049 0.00049 0.00050 0.00026 H4A 0.53495 -0.03248 0.11181 1.00000 0.01994 0.00000 0.00000 H4B 0.53466 0.13881 0.06526 1.00000 0.01994 0.00000 0.00000 C5 0.77719 -0.01782 0.05927 1.00000 0.02072 0.02221 0.02671 -0.00509 0.00510 -0.00568 0.02361 0.00236 0.00019 0.00018 0.00012 0.00000 0.00070 0.00071 0.00075 0.00057 0.00058 0.00057 0.00030 H5A 0.83738 0.06156 0.05346 1.00000 0.03541 0.00000 0.00000 H5B 0.77052 -0.04699 -0.01111 1.00000 0.03541 0.00000 0.00000 H5C 0.83971 -0.10944 0.10280 1.00000 0.03541 0.00000 0.00000 C6 0.69633 0.20544 0.23126 1.00000 0.01661 0.01967 0.02115 -0.00061 -0.00231 -0.00942 0.01826 0.00202 0.00018 0.00016 0.00011 0.00000 0.00064 0.00066 0.00066 0.00052 0.00051 0.00053 0.00027 H6A 0.67951 0.23502 0.30448 1.00000 0.02191 0.00000 0.00000 H6B 0.81874 0.14731 0.21863 1.00000 0.02191 0.00000 0.00000 C7 0.65939 0.35426 0.15699 1.00000 0.02327 0.01717 0.02201 -0.00268 0.00067 -0.00858 0.02032 0.00214 0.00019 0.00016 0.00011 0.00000 0.00070 0.00065 0.00068 0.00053 0.00055 0.00055 0.00028 H7A 0.64863 0.32913 0.08533 1.00000 0.02438 0.00000 0.00000 H7B 0.54876 0.42672 0.18098 1.00000 0.02438 0.00000 0.00000 C8 0.79961 0.43336 0.15256 1.00000 0.02984 0.02648 0.06088 0.00363 -0.00152 -0.01782 0.03769 0.00289 0.00023 0.00020 0.00017 0.00000 0.00087 0.00084 0.00120 0.00079 0.00081 0.00071 0.00042 H8A 0.91030 0.35989 0.12972 1.00000 0.04523 0.00000 0.00000 H8B 0.80927 0.45904 0.22425 1.00000 0.04523 0.00000 0.00000 C9 0.76750 0.58086 0.07818 1.00000 0.05236 0.02456 0.04617 -0.00573 0.01083 -0.02267 0.03935 0.00298 0.00027 0.00020 0.00016 0.00000 0.00114 0.00083 0.00106 0.00074 0.00087 0.00081 0.00043 H9A 0.75340 0.55721 0.00753 1.00000 0.05902 0.00000 0.00000 H9B 0.86517 0.62273 0.07535 1.00000 0.05902 0.00000 0.00000 H9C 0.66324 0.65771 0.10370 1.00000 0.05902 0.00000 0.00000 N1 0.34791 -0.07878 0.42078 1.00000 0.01587 0.01809 0.01500 -0.00265 -0.00122 -0.00552 0.01609 0.00168 0.00015 0.00013 0.00009 0.00000 0.00053 0.00055 0.00052 0.00042 0.00042 0.00044 0.00023 N2 0.10819 -0.09435 0.29481 1.00000 0.01202 0.01647 0.02449 -0.00379 -0.00218 -0.00352 0.01757 0.00171 0.00014 0.00013 0.00009 0.00000 0.00052 0.00055 0.00059 0.00045 0.00044 0.00043 0.00023 N3 0.39546 -0.34075 0.32294 1.00000 0.01375 0.01576 0.02127 -0.00242 -0.00434 -0.00322 0.01688 0.00167 0.00014 0.00013 0.00009 0.00000 0.00053 0.00053 0.00057 0.00044 0.00044 0.00043 0.00023 O1 0.61054 -0.18371 0.28873 1.00000 0.01510 0.01482 0.01887 0.00134 0.00015 -0.00443 0.01659 0.00145 0.00012 0.00011 0.00007 0.00000 0.00045 0.00045 0.00046 0.00035 0.00036 0.00036 0.00019 O2 0.27836 0.09872 0.24461 1.00000 0.01211 0.02041 0.01661 -0.00101 -0.00062 -0.00679 0.01601 0.00139 0.00012 0.00011 0.00007 0.00000 0.00043 0.00047 0.00045 0.00036 0.00035 0.00037 0.00019 P1 0.47772 -0.22930 0.37352 1.00000 0.01288 0.01522 0.01347 0.00085 -0.00273 -0.00481 0.01374 0.00050 0.00004 0.00004 0.00003 0.00000 0.00016 0.00016 0.00016 0.00012 0.00012 0.00012 0.00008 P2 0.20462 0.00931 0.34174 1.00000 0.01145 0.01513 0.01600 -0.00271 0.00081 -0.00428 0.01413 0.00050 0.00004 0.00004 0.00003 0.00000 0.00016 0.00016 0.00016 0.00012 0.00012 0.00012 0.00008 P3 0.20943 -0.27090 0.28341 1.00000 0.01277 0.01545 0.01565 -0.00216 -0.00211 -0.00436 0.01443 0.00049 0.00004 0.00004 0.00003 0.00000 0.00016 0.00017 0.00016 0.00012 0.00012 0.00013 0.00008 Cl1 0.61621 -0.35616 0.48882 1.00000 0.02491 0.02214 0.01933 0.00528 -0.01042 -0.00784 0.02184 0.00050 0.00005 0.00004 0.00003 0.00000 0.00018 0.00017 0.00016 0.00013 0.00013 0.00014 0.00009 Cl2 0.03233 0.17297 0.41902 1.00000 0.01911 0.01971 0.02525 -0.00739 0.00590 -0.00383 0.02188 0.00053 0.00004 0.00004 0.00003 0.00000 0.00017 0.00017 0.00018 0.00013 0.00013 0.00013 0.00009 Cl3 0.21956 -0.31340 0.13243 1.00000 0.02854 0.03278 0.01802 -0.00802 -0.00714 0.00149 0.02788 0.00056 0.00005 0.00005 0.00003 0.00000 0.00019 0.00020 0.00017 0.00014 0.00014 0.00015 0.00010 Cl4 0.06134 -0.40195 0.35040 1.00000 0.02085 0.02250 0.03752 0.00101 -0.00175 -0.01228 0.02597 0.00055 0.00005 0.00004 0.00003 0.00000 0.00017 0.00018 0.00021 0.00015 0.00015 0.00014 0.00009 Final Structure Factor Calculation for 2007src0655 in P-1 Total number of l.s. parameters = 192 Maximum vector length = 511 Memory required = 2298 / 25039 wR2 = 0.0630 before cycle 5 for 4131 data and 0 / 192 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0279 * P )^2 + 0.48 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0235 for 3865 Fo > 4sig(Fo) and 0.0256 for all 4131 data wR2 = 0.0630, GooF = S = 1.064, Restrained GooF = 1.064 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0263 0.0154 0.0107 C1 0.0175 0.0150 0.0110 C2 0.0208 0.0173 0.0116 C3 0.0180 0.0167 0.0152 C4 0.0317 0.0227 0.0164 C5 0.0228 0.0201 0.0119 C6 0.0254 0.0205 0.0150 C7 0.0635 0.0354 0.0141 C8 0.0654 0.0371 0.0155 C9 0.0184 0.0157 0.0141 N1 0.0249 0.0160 0.0119 N2 0.0225 0.0157 0.0124 N3 0.0216 0.0151 0.0131 O1 0.0206 0.0167 0.0107 O2 0.0170 0.0130 0.0112 P1 0.0172 0.0144 0.0109 P2 0.0165 0.0149 0.0119 P3 0.0323 0.0218 0.0115 Cl1 0.0310 0.0220 0.0127 Cl2 0.0470 0.0224 0.0143 Cl3 0.0388 0.0260 0.0132 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.050 0.076 0.106 0.138 0.174 0.217 0.275 0.377 1.000 Number in group 414. 419. 406. 424. 406. 413. 412. 409. 413. 415. GooF 1.112 1.103 1.124 1.194 1.003 1.059 0.907 0.966 0.964 1.169 K 1.147 0.941 0.956 0.972 0.979 1.000 1.001 1.010 1.012 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 419. 407. 419. 413. 416. 404. 420. 408. 414. 411. GooF 0.940 0.862 0.891 0.879 0.822 0.944 1.001 0.956 1.091 1.866 K 0.973 1.008 1.009 1.012 1.013 1.020 1.018 1.013 1.007 0.981 R1 0.046 0.034 0.030 0.028 0.023 0.024 0.022 0.017 0.017 0.028 Recommended weighting scheme: WGHT 0.0246 0.5114 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) 0 -1 1 3663.05 4998.26 5.54 0.724 6.85 3 -1 2 388.60 504.71 5.41 0.230 2.20 -2 3 2 47.38 24.54 5.20 0.051 1.96 4 0 0 101.39 145.63 4.76 0.124 1.95 -1 3 0 132.40 182.60 4.72 0.138 2.47 2 -2 5 9.07 1.63 4.56 0.013 1.79 -3 -3 2 5.55 18.67 4.52 0.044 2.06 4 4 2 125.47 89.30 4.47 0.097 1.72 -1 4 2 15.83 5.65 4.41 0.024 1.88 3 3 4 54.46 33.54 4.27 0.059 1.99 0 4 0 346.82 279.20 4.23 0.171 2.15 4 1 1 6.09 0.78 4.12 0.009 2.04 -1 -3 2 120.06 87.76 4.07 0.096 2.59 3 1 6 114.48 83.25 4.03 0.093 1.76 4 0 3 37.38 21.58 4.00 0.048 1.82 1 0 2 6104.92 7149.91 3.98 0.865 5.11 2 3 2 304.78 245.40 3.98 0.160 2.63 1 1 8 75.89 51.92 3.96 0.074 1.59 0 2 8 79.57 55.20 3.96 0.076 1.53 -1 2 3 9.95 2.63 3.93 0.017 2.69 4 3 2 85.98 117.40 3.82 0.111 1.88 3 4 0 2351.97 2694.41 3.77 0.531 1.96 2 3 5 107.09 141.88 3.72 0.122 2.00 0 -2 1 6694.97 7647.37 3.71 0.895 3.97 1 1 6 36.89 22.39 3.69 0.048 2.10 6 7 3 1033.15 879.22 3.58 0.303 1.06 -3 -3 5 5.19 0.86 3.57 0.009 1.60 2 -1 3 54.68 78.15 3.55 0.090 2.60 4 5 2 15.46 6.88 3.54 0.027 1.54 2 2 0 4860.87 5514.59 3.52 0.760 3.43 1 -2 5 428.39 360.81 3.49 0.194 1.99 3 4 3 255.79 209.42 3.49 0.148 1.88 3 0 0 127.96 98.92 3.45 0.102 2.60 -3 0 2 864.99 751.19 3.43 0.281 2.35 3 0 5 293.74 244.79 3.38 0.160 1.89 -1 2 1 1312.64 1495.05 3.37 0.396 3.29 -1 1 0 3965.28 4431.55 3.20 0.681 5.09 1 -3 3 1096.93 970.02 3.19 0.319 2.09 2 2 3 476.37 551.71 3.17 0.240 2.86 3 3 0 2845.75 2551.13 3.16 0.517 2.29 3 1 0 828.42 944.17 3.15 0.314 2.72 4 2 3 49.86 69.00 3.15 0.085 1.90 -9 -6 1 72.83 106.26 3.12 0.106 0.85 0 -4 2 525.54 603.31 3.09 0.251 1.99 4 -1 4 125.72 98.45 3.09 0.102 1.59 3 9 3 16.28 28.42 3.08 0.055 1.00 -3 -3 4 825.35 727.89 3.06 0.276 1.75 -1 -3 1 323.14 377.68 3.05 0.199 2.84 1 5 1 49.79 68.40 3.03 0.085 1.81 0 6 5 121.25 96.04 2.99 0.100 1.30 Bond lengths and angles C1 - Distance Angles O1 1.4743 (0.0016) C2 1.5391 (0.0018) 113.12 (0.10) C1 - O1 C2 - Distance Angles C3 1.5331 (0.0018) C1 1.5391 (0.0018) 113.46 (0.11) C4 1.5438 (0.0018) 109.91 (0.11) 111.26 (0.11) C6 1.5535 (0.0018) 106.02 (0.11) 103.34 (0.10) 112.63 (0.11) C2 - C3 C1 C4 C3 - Distance Angles O2 1.4703 (0.0015) C2 1.5331 (0.0018) 113.55 (0.10) C3 - O2 C4 - Distance Angles C5 1.5279 (0.0019) C2 1.5438 (0.0018) 114.92 (0.11) C4 - C5 C5 - Distance Angles C4 1.5279 (0.0019) C5 - C6 - Distance Angles C7 1.5282 (0.0019) C2 1.5535 (0.0018) 117.08 (0.11) C6 - C7 C7 - Distance Angles C8 1.5205 (0.0021) C6 1.5282 (0.0019) 112.08 (0.13) C7 - C8 C8 - Distance Angles C7 1.5205 (0.0021) C9 1.5203 (0.0025) 113.30 (0.15) C8 - C7 C9 - Distance Angles C8 1.5203 (0.0025) C9 - N1 - Distance Angles P2 1.5942 (0.0012) P1 1.5960 (0.0012) 111.32 (0.07) N1 - P2 N2 - Distance Angles P3 1.5824 (0.0012) P2 1.5958 (0.0012) 117.57 (0.07) N2 - P3 N3 - Distance Angles P3 1.5785 (0.0011) P1 1.5965 (0.0012) 118.51 (0.07) N3 - P3 O1 - Distance Angles C1 1.4743 (0.0016) P1 1.5676 (0.0010) 120.04 (0.08) O1 - C1 O2 - Distance Angles C3 1.4703 (0.0015) P2 1.5733 (0.0010) 120.59 (0.08) O2 - C3 P1 - Distance Angles O1 1.5676 (0.0010) N1 1.5960 (0.0012) 110.90 (0.06) N3 1.5965 (0.0012) 107.76 (0.06) 116.85 (0.06) Cl1 1.9918 (0.0005) 105.30 (0.04) 108.16 (0.04) 107.21 (0.04) P2 2.6342 (0.0005) 100.58 (0.04) 34.32 (0.04) 91.42 (0.04) 141.24 (0.02) P1 - O1 N1 N3 Cl1 P2 - Distance Angles O2 1.5733 (0.0010) N1 1.5942 (0.0012) 111.87 (0.06) N2 1.5958 (0.0012) 106.45 (0.06) 116.66 (0.06) Cl2 1.9922 (0.0005) 105.42 (0.04) 106.95 (0.04) 108.92 (0.04) P1 2.6342 (0.0005) 99.28 (0.04) 34.36 (0.04) 92.31 (0.04) 140.74 (0.02) P2 - O2 N1 N2 Cl2 P3 - Distance Angles N3 1.5785 (0.0011) N2 1.5824 (0.0012) 120.10 (0.06) Cl3 2.0045 (0.0005) 108.14 (0.05) 108.93 (0.05) Cl4 2.0089 (0.0005) 109.14 (0.05) 108.51 (0.05) 100.18 (0.02) P3 - N3 N2 Cl3 Cl1 - Distance Angles P1 1.9918 (0.0005) Cl1 - Cl2 - Distance Angles P2 1.9922 (0.0005) Cl2 - Cl3 - Distance Angles P3 2.0045 (0.0005) Cl3 - Cl4 - Distance Angles P3 2.0089 (0.0005) Cl4 - FMAP and GRID set by program FMAP 2 1 22 GRID -2.632 -2 -2 2.632 2 2 R1 = 0.0255 for 4131 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.3974 0.9320 0.8343 [ 0.77 A from C4 ] Deepest hole -0.39 at 0.2397 0.0657 0.3650 [ 0.76 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2352 / 22052 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6026 0.0680 0.1657 1.00000 0.05 0.33 0.77 C4 0.78 C2 1.46 H4B 1.46 H4A Q2 1 0.6351 0.1529 0.2229 1.00000 0.05 0.31 0.75 C2 0.81 C6 1.48 H6A 1.49 H6B Q3 1 0.5033 0.1249 0.2394 1.00000 0.05 0.29 0.69 C2 0.85 C3 1.51 H3A 1.54 H3B Q4 1 0.6233 0.0222 0.2551 1.00000 0.05 0.28 0.72 C2 0.83 C1 1.49 H1A 1.52 H1B Q5 1 0.6674 0.2835 0.1999 1.00000 0.05 0.25 0.76 C6 0.79 C7 1.36 H6A 1.38 H7B Q6 1 0.7350 0.3887 0.1620 1.00000 0.05 0.25 0.75 C8 0.78 C7 1.37 H8B 1.41 H8A Q7 1 0.3167 -0.3134 0.3186 1.00000 0.05 0.25 0.62 N3 0.98 P3 1.93 P1 2.21 N2 Q8 1 0.9396 0.3558 0.1779 1.00000 0.05 0.23 0.68 H8A 1.21 C8 1.33 H8B 2.35 C7 Q9 1 0.1266 -0.1225 0.2644 1.00000 0.05 0.21 0.48 N2 1.32 P3 1.92 P2 2.46 CL3 Q10 1 0.6280 -0.1162 0.2934 1.00000 0.05 0.21 0.68 O1 0.80 C1 1.45 H1B 1.51 H1A Q11 1 0.7660 -0.1036 0.2603 1.00000 0.05 0.20 0.55 H1A 0.94 C1 1.64 O1 1.79 H1B Q12 1 0.3394 0.1402 0.2557 1.00000 0.05 0.20 0.73 C3 0.74 O2 1.37 H3A 1.42 H3B Q13 1 0.2334 0.1202 0.2206 1.00000 0.05 0.19 0.49 O2 1.77 C3 1.78 P2 2.11 H3B Q14 1 0.5493 -0.1687 0.2940 1.00000 0.05 0.19 0.48 O1 1.27 P1 1.69 C1 2.12 H1B Q15 1 0.4212 -0.3802 0.3216 1.00000 0.05 0.19 0.36 N3 1.78 P1 1.81 P3 2.58 H7B Q16 1 0.1062 -0.0620 0.3371 1.00000 0.05 0.19 0.64 N2 1.19 P2 2.00 P3 2.31 N1 Q17 1 0.9213 0.3264 0.0766 1.00000 0.05 0.19 0.76 H8A 1.52 C8 2.22 H7A 2.24 C7 Q18 1 0.4227 -0.3069 0.3518 1.00000 0.05 0.18 0.60 N3 1.02 P1 1.96 P3 2.20 O1 Q19 1 0.3459 -0.0743 0.4477 1.00000 0.05 0.17 0.35 N1 1.80 P1 1.82 P2 2.57 H1B Q20 1 0.6777 0.0189 0.0798 1.00000 0.05 0.17 0.73 C4 0.81 C5 1.35 H4B 1.39 H4A Shortest distances between peaks (including symmetry equivalents) 15 18 0.81 7 15 0.89 10 14 0.91 7 18 1.03 12 13 1.09 9 16 1.11 3 4 1.15 2 3 1.18 1 4 1.18 10 11 1.20 1 2 1.22 1 3 1.23 2 4 1.24 1 20 1.26 5 6 1.27 2 5 1.28 4 10 1.28 3 12 1.31 4 11 1.37 8 17 1.39 6 8 1.64 6 17 1.77 14 18 1.90 4 14 2.00 11 14 2.03 7 9 2.06 1 11 2.08 1 10 2.18 3 10 2.18 3 5 2.23 4 20 2.25 4 12 2.25 2 20 2.26 3 13 2.26 2 11 2.27 1 5 2.27 1 12 2.29 14 15 2.42 7 16 2.43 18 19 2.45 2 12 2.45 3 20 2.48 13 16 2.49 5 8 2.49 14 19 2.50 16 19 2.51 4 5 2.51 3 11 2.51 2 10 2.52 11 20 2.53 2 6 2.53 5 17 2.58 9 13 2.59 3 14 2.60 7 14 2.60 1 14 2.66 10 18 2.75 8 13 2.75 9 18 2.76 10 12 2.81 12 14 2.83 10 19 2.85 16 18 2.87 9 15 2.90 10 20 2.91 9 11 2.92 1 13 2.94 12 19 2.95 7 19 2.95 5 20 2.97 Time profile in seconds ----------------------- 0.06: 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. 5.58: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.15: Structure factors and derivatives 1.84: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.24: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.04: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0655 finished at 19:10:00 Total CPU time: 9.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++