+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006src0966p-1 started at 18:09:43 on 21-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006src0966p-1 in P-1 CELL 0.71073 9.4791 10.2283 11.4144 88.423 78.172 79.694 ZERR 2.00 0.0002 0.0002 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N P CL UNIT 32 50 10 6 6 V = 1065.66 F(000) = 504.0 Mu = 0.67 mm-1 Cell Wt = 973.34 Rho = 1.517 MERG 2 OMIT -3.00 55.00 OMIT 1 0 0 OMIT 0 0 1 OMIT 0 1 0 OMIT 1 1 1 FMAP 2 PLAN 10 SIZE 0.14 0.21 0.28 ACTA BOND $H WGHT 0.03400 1.16960 L.S. 4 TEMP -153.00 FVAR 0.81945 C1 1 0.462363 1.051998 0.758182 11.00000 0.01607 0.01646 = 0.01676 0.00086 -0.00101 -0.00182 C2 1 0.488986 1.125781 0.850750 11.00000 0.02415 0.02509 = 0.01844 0.00170 -0.00766 -0.00568 AFIX 43 H2 2 0.506324 1.083050 0.922706 11.00000 -1.20000 AFIX 0 C3 1 0.490066 1.260430 0.837580 11.00000 0.02600 0.02140 = 0.02267 -0.00458 -0.00596 -0.00425 AFIX 43 H3 2 0.505524 1.310526 0.901210 11.00000 -1.20000 AFIX 0 C4 1 0.468459 1.322568 0.730883 11.00000 0.02769 0.01658 = 0.02502 0.00003 -0.00230 -0.00589 AFIX 43 H4 2 0.472337 1.414465 0.720944 11.00000 -1.20000 AFIX 0 C5 1 0.441389 1.250877 0.639424 11.00000 0.02647 0.02102 = 0.01784 0.00451 -0.00381 -0.00426 AFIX 43 H5 2 0.422879 1.294301 0.568054 11.00000 -1.20000 AFIX 0 C6 1 0.441247 1.115286 0.651862 11.00000 0.02374 0.02170 = 0.01831 -0.00026 -0.00482 -0.00641 AFIX 43 H6 2 0.426693 1.065581 0.587608 11.00000 -1.20000 AFIX 0 C7 1 0.759447 0.853478 0.705997 11.00000 0.02022 0.02368 = 0.02674 0.00098 -0.00180 -0.00604 AFIX 23 H7A 2 0.839297 0.853582 0.749917 11.00000 -1.20000 H7B 2 0.731297 0.944924 0.677661 11.00000 -1.20000 AFIX 0 C8 1 0.815098 0.759958 0.598508 11.00000 0.02746 0.04022 = 0.02363 -0.00551 0.00166 -0.01155 AFIX 23 H8A 2 0.739546 0.767395 0.549122 11.00000 -1.20000 H8B 2 0.903975 0.785968 0.548609 11.00000 -1.20000 AFIX 0 C9 1 0.850642 0.618032 0.638113 11.00000 0.02919 0.03239 = 0.05002 -0.01682 0.00299 -0.00195 AFIX 23 H9A 2 0.934284 0.608022 0.679222 11.00000 -1.20000 H9B 2 0.879144 0.558142 0.567299 11.00000 -1.20000 AFIX 0 C10 1 0.717391 0.579417 0.723207 11.00000 0.03167 0.01989 = 0.06079 -0.00066 -0.00372 -0.00316 AFIX 23 H10A 2 0.637550 0.579298 0.679280 11.00000 -1.20000 H10B 2 0.744044 0.488613 0.753491 11.00000 -1.20000 AFIX 0 C11 1 0.664375 0.676921 0.828226 11.00000 0.02142 0.02495 = 0.03192 0.01059 -0.00483 -0.00339 AFIX 23 H11A 2 0.575090 0.653262 0.879531 11.00000 -1.20000 H11B 2 0.740575 0.669437 0.876990 11.00000 -1.20000 AFIX 0 C12 1 -0.051181 0.790222 1.038518 11.00000 0.01860 0.03988 = 0.02551 -0.00444 -0.00095 -0.01081 AFIX 23 H12A 2 -0.058916 0.745780 0.964710 11.00000 -1.20000 H12B 2 -0.133958 0.865713 1.056614 11.00000 -1.20000 AFIX 0 C13 1 -0.062042 0.692223 1.141601 11.00000 0.03023 0.03693 = 0.03093 -0.00328 0.00692 -0.01761 AFIX 23 H13A 2 0.011367 0.610547 1.118637 11.00000 -1.20000 H13B 2 -0.160410 0.667326 1.158023 11.00000 -1.20000 AFIX 0 C14 1 -0.035828 0.752349 1.254788 11.00000 0.03410 0.03362 = 0.02266 0.00252 0.00454 -0.00885 AFIX 23 H14A 2 -0.034256 0.684097 1.317935 11.00000 -1.20000 H14B 2 -0.117129 0.826421 1.284300 11.00000 -1.20000 AFIX 0 C15 1 0.109339 0.803836 1.229828 11.00000 0.03061 0.02888 = 0.01901 0.00044 -0.00397 -0.00229 AFIX 23 H15A 2 0.119658 0.849508 1.302159 11.00000 -1.20000 H15B 2 0.191609 0.727983 1.211097 11.00000 -1.20000 AFIX 0 C16 1 0.116189 0.899958 1.125295 11.00000 0.02360 0.01945 = 0.01800 -0.00383 -0.00222 -0.00193 AFIX 23 H16A 2 0.042669 0.981475 1.148653 11.00000 -1.20000 H16B 2 0.214182 0.925606 1.106416 11.00000 -1.20000 AFIX 0 N1 3 0.356666 0.851647 0.901795 11.00000 0.01883 0.01861 = 0.01408 0.00030 -0.00258 -0.00487 N2 3 0.154080 0.778397 0.789399 11.00000 0.02067 0.02898 = 0.01578 -0.00086 -0.00270 -0.00760 N3 3 0.416485 0.823129 0.660224 11.00000 0.02483 0.02082 = 0.01448 -0.00255 -0.00079 -0.00714 N4 3 0.631825 0.814401 0.788459 11.00000 0.01849 0.02126 = 0.02316 0.00433 -0.00223 -0.00384 N5 3 0.088129 0.841005 1.017902 11.00000 0.01698 0.02184 = 0.01433 -0.00102 -0.00074 -0.00466 P1 4 0.462226 0.878002 0.777086 11.00000 0.01883 0.01469 = 0.01469 0.00030 -0.00087 -0.00367 P2 4 0.220118 0.782156 0.907467 11.00000 0.01763 0.01532 = 0.01347 -0.00060 -0.00130 -0.00338 P3 4 0.261208 0.787928 0.665201 11.00000 0.02481 0.01694 = 0.01361 -0.00139 -0.00314 -0.00585 CL1 5 0.286583 0.582556 0.944724 11.00000 0.03128 0.01481 = 0.02958 0.00080 -0.00033 -0.00243 CL2 5 0.284931 0.618292 0.571295 11.00000 0.04156 0.02496 = 0.02655 -0.01012 0.00100 -0.01416 CL3 5 0.151281 0.916325 0.563298 11.00000 0.03594 0.03346 = 0.02609 0.00706 -0.01446 -0.00705 HKLF 4 Covalent radii and connectivity table for 2006src0966p-1 in P-1 C 0.770 H 0.320 N 0.700 P 1.100 CL 0.990 C1 - C6 C2 P1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - N4 C8 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - N4 C10 C12 - N5 C13 C13 - C12 C14 C14 - C13 C15 C15 - C16 C14 C16 - N5 C15 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 N4 - C11 C7 P1 N5 - C16 C12 P2 P1 - N1 N3 N4 C1 P2 - N1 N2 N5 Cl1 P3 - N3 N2 Cl2 Cl3 Cl1 - P2 Cl2 - P3 Cl3 - P3 16631 Reflections read, of which 5 rejected -11 =< h =< 11, -12 =< k =< 12, -14 =< l =< 14, Max. 2-theta = 52.08 0 Systematic absence violations 0 Inconsistent equivalents 4189 Unique reflections, of which 0 suppressed R(int) = 0.0250 R(sigma) = 0.0231 Friedel opposites merged Maximum memory for data reduction = 2630 / 41876 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 = 3336 / 303763 wR2 = 0.0818 before cycle 1 for 4189 data and 244 / 244 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81878 0.00111 -0.608 OSF Mean shift/esd = 0.101 Maximum = -0.608 for OSF Max. shift = 0.001 A for C9 Max. dU = 0.000 for C15 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3336 / 303763 wR2 = 0.0817 before cycle 2 for 4189 data and 244 / 244 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81840 0.00111 -0.339 OSF Mean shift/esd = 0.035 Maximum = -0.339 for OSF Max. shift = 0.000 A for C9 Max. dU = 0.000 for C15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3336 / 303763 wR2 = 0.0818 before cycle 3 for 4189 data and 244 / 244 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81840 0.00111 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.005 for y C4 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C13 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3336 / 303763 wR2 = 0.0818 before cycle 4 for 4189 data and 244 / 244 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.81840 0.00111 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U11 C9 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C9 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 0.5063 1.0830 0.9227 43 0.950 0.000 C2 C3 C1 H3 0.5055 1.3105 0.9012 43 0.950 0.000 C3 C2 C4 H4 0.4723 1.4145 0.7210 43 0.950 0.000 C4 C5 C3 H5 0.4229 1.2943 0.5681 43 0.950 0.000 C5 C4 C6 H6 0.4266 1.0656 0.5876 43 0.950 0.000 C6 C5 C1 H7A 0.8393 0.8536 0.7499 23 0.990 0.000 C7 N4 C8 H7B 0.7313 0.9449 0.6776 23 0.990 0.000 C7 N4 C8 H8A 0.7395 0.7674 0.5491 23 0.990 0.000 C8 C9 C7 H8B 0.9040 0.7860 0.5486 23 0.990 0.000 C8 C9 C7 H9A 0.9342 0.6080 0.6793 23 0.990 0.000 C9 C8 C10 H9B 0.8792 0.5581 0.5674 23 0.990 0.000 C9 C8 C10 H10A 0.6375 0.5794 0.6792 23 0.990 0.000 C10 C11 C9 H10B 0.7440 0.4886 0.7534 23 0.990 0.000 C10 C11 C9 H11A 0.5751 0.6532 0.8795 23 0.990 0.000 C11 N4 C10 H11B 0.7406 0.6694 0.8769 23 0.990 0.000 C11 N4 C10 H12A -0.0589 0.7458 0.9647 23 0.990 0.000 C12 N5 C13 H12B -0.1340 0.8657 1.0566 23 0.990 0.000 C12 N5 C13 H13A 0.0113 0.6105 1.1186 23 0.990 0.000 C13 C12 C14 H13B -0.1604 0.6673 1.1580 23 0.990 0.000 C13 C12 C14 H14A -0.0342 0.6841 1.3179 23 0.990 0.000 C14 C13 C15 H14B -0.1171 0.8264 1.2843 23 0.990 0.000 C14 C13 C15 H15A 0.1196 0.8495 1.3021 23 0.990 0.000 C15 C16 C14 H15B 0.1916 0.7280 1.2111 23 0.990 0.000 C15 C16 C14 H16A 0.0426 0.9814 1.1487 23 0.990 0.000 C16 N5 C15 H16B 0.2141 0.9256 1.1065 23 0.990 0.000 C16 N5 C15 2006src0966p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.46241 1.05198 0.75816 1.00000 0.01589 0.01629 0.01658 0.00077 -0.00088 -0.00182 0.01675 0.00295 0.00020 0.00018 0.00017 0.00000 0.00090 0.00090 0.00095 0.00072 0.00072 0.00071 0.00038 C2 0.48899 1.12577 0.85075 1.00000 0.02397 0.02507 0.01828 0.00185 -0.00761 -0.00577 0.02181 0.00307 0.00022 0.00020 0.00018 0.00000 0.00103 0.00103 0.00101 0.00080 0.00081 0.00082 0.00042 H2 0.50630 1.08304 0.92272 1.00000 0.02617 0.00000 0.00000 C3 0.49006 1.26042 0.83758 1.00000 0.02592 0.02124 0.02251 -0.00461 -0.00605 -0.00421 0.02296 0.00312 0.00023 0.00020 0.00019 0.00000 0.00107 0.00100 0.00106 0.00081 0.00084 0.00082 0.00043 H3 0.50552 1.31051 0.90121 1.00000 0.02756 0.00000 0.00000 C4 0.46845 1.32257 0.73091 1.00000 0.02742 0.01653 0.02479 0.00009 -0.00234 -0.00594 0.02309 0.00318 0.00023 0.00020 0.00019 0.00000 0.00109 0.00095 0.00109 0.00080 0.00086 0.00080 0.00043 H4 0.47230 1.41447 0.72099 1.00000 0.02770 0.00000 0.00000 C5 0.44140 1.25087 0.63944 1.00000 0.02634 0.02079 0.01774 0.00452 -0.00375 -0.00427 0.02180 0.00317 0.00022 0.00020 0.00018 0.00000 0.00106 0.00099 0.00100 0.00078 0.00081 0.00081 0.00042 H5 0.42294 1.29429 0.56805 1.00000 0.02616 0.00000 0.00000 C6 0.44122 1.11527 0.65187 1.00000 0.02361 0.02157 0.01818 -0.00031 -0.00481 -0.00638 0.02073 0.00308 0.00022 0.00020 0.00018 0.00000 0.00101 0.00098 0.00100 0.00077 0.00079 0.00079 0.00041 H6 0.42659 1.06558 0.58764 1.00000 0.02488 0.00000 0.00000 C7 0.75943 0.85346 0.70598 1.00000 0.02010 0.02353 0.02675 0.00101 -0.00176 -0.00607 0.02363 0.00326 0.00022 0.00021 0.00019 0.00000 0.00100 0.00103 0.00113 0.00085 0.00084 0.00081 0.00044 H7A 0.83927 0.85356 0.74991 1.00000 0.02836 0.00000 0.00000 H7B 0.73129 0.94490 0.67764 1.00000 0.02836 0.00000 0.00000 C8 0.81508 0.75996 0.59853 1.00000 0.02755 0.03999 0.02346 -0.00548 0.00155 -0.01165 0.03048 0.00348 0.00025 0.00024 0.00020 0.00000 0.00114 0.00130 0.00115 0.00096 0.00090 0.00098 0.00050 H8A 0.73953 0.76738 0.54914 1.00000 0.03658 0.00000 0.00000 H8B 0.90395 0.78597 0.54863 1.00000 0.03658 0.00000 0.00000 C9 0.85064 0.61802 0.63817 1.00000 0.02915 0.03231 0.04988 -0.01665 0.00315 -0.00208 0.03883 0.00400 0.00027 0.00024 0.00025 0.00000 0.00124 0.00128 0.00159 0.00113 0.00109 0.00099 0.00060 H9A 0.93424 0.60803 0.67933 1.00000 0.04660 0.00000 0.00000 H9B 0.87919 0.55811 0.56737 1.00000 0.04660 0.00000 0.00000 C10 0.71738 0.57945 0.72319 1.00000 0.03162 0.01972 0.06062 -0.00068 -0.00360 -0.00310 0.03832 0.00410 0.00027 0.00023 0.00026 0.00000 0.00127 0.00110 0.00172 0.00108 0.00116 0.00094 0.00059 H10A 0.63755 0.57941 0.67924 1.00000 0.04598 0.00000 0.00000 H10B 0.74397 0.48863 0.75345 1.00000 0.04598 0.00000 0.00000 C11 0.66441 0.67690 0.82821 1.00000 0.02129 0.02480 0.03180 0.01068 -0.00483 -0.00336 0.02633 0.00356 0.00023 0.00021 0.00020 0.00000 0.00103 0.00107 0.00121 0.00090 0.00088 0.00083 0.00046 H11A 0.57515 0.65322 0.87954 1.00000 0.03160 0.00000 0.00000 H11B 0.74064 0.66943 0.87694 1.00000 0.03160 0.00000 0.00000 C12 -0.05118 0.79022 1.03851 1.00000 0.01859 0.03975 0.02519 -0.00455 -0.00091 -0.01073 0.02756 0.00332 0.00023 0.00023 0.00020 0.00000 0.00102 0.00126 0.00114 0.00094 0.00084 0.00091 0.00047 H12A -0.05891 0.74577 0.96470 1.00000 0.03308 0.00000 0.00000 H12B -0.13396 0.86570 1.05660 1.00000 0.03308 0.00000 0.00000 C13 -0.06206 0.69222 1.14160 1.00000 0.03008 0.03663 0.03076 -0.00329 0.00691 -0.01750 0.03286 0.00361 0.00026 0.00024 0.00021 0.00000 0.00120 0.00128 0.00125 0.00100 0.00096 0.00100 0.00053 H13A 0.01134 0.61053 1.11864 1.00000 0.03943 0.00000 0.00000 H13B -0.16044 0.66734 1.15803 1.00000 0.03943 0.00000 0.00000 C14 -0.03582 0.75236 1.25477 1.00000 0.03408 0.03337 0.02249 0.00255 0.00440 -0.00880 0.03114 0.00366 0.00026 0.00024 0.00020 0.00000 0.00126 0.00121 0.00114 0.00092 0.00093 0.00098 0.00051 H14A -0.03424 0.68411 1.31792 1.00000 0.03737 0.00000 0.00000 H14B -0.11712 0.82643 1.28428 1.00000 0.03737 0.00000 0.00000 C15 0.10930 0.80383 1.22980 1.00000 0.03024 0.02868 0.01886 0.00036 -0.00395 -0.00205 0.02648 0.00344 0.00024 0.00022 0.00019 0.00000 0.00115 0.00113 0.00105 0.00085 0.00086 0.00090 0.00046 H15A 0.11963 0.84948 1.30214 1.00000 0.03177 0.00000 0.00000 H15B 0.19156 0.72797 1.21105 1.00000 0.03177 0.00000 0.00000 C16 0.11615 0.89994 1.12532 1.00000 0.02351 0.01920 0.01790 -0.00386 -0.00214 -0.00193 0.02066 0.00304 0.00022 0.00019 0.00018 0.00000 0.00102 0.00096 0.00100 0.00078 0.00079 0.00078 0.00041 H16A 0.04262 0.98145 1.14869 1.00000 0.02479 0.00000 0.00000 H16B 0.21414 0.92559 1.10647 1.00000 0.02479 0.00000 0.00000 N1 0.35667 0.85163 0.90178 1.00000 0.01857 0.01844 0.01395 0.00029 -0.00252 -0.00484 0.01691 0.00242 0.00017 0.00016 0.00014 0.00000 0.00081 0.00079 0.00080 0.00062 0.00063 0.00063 0.00033 N2 0.15408 0.77838 0.78939 1.00000 0.02044 0.02887 0.01557 -0.00084 -0.00263 -0.00762 0.02135 0.00255 0.00018 0.00017 0.00015 0.00000 0.00085 0.00092 0.00085 0.00069 0.00067 0.00070 0.00036 N3 0.41642 0.82314 0.66022 1.00000 0.02463 0.02061 0.01432 -0.00245 -0.00077 -0.00716 0.01987 0.00249 0.00019 0.00016 0.00015 0.00000 0.00088 0.00083 0.00081 0.00064 0.00066 0.00068 0.00035 N4 0.63181 0.81439 0.78843 1.00000 0.01834 0.02097 0.02311 0.00444 -0.00208 -0.00383 0.02115 0.00267 0.00018 0.00017 0.00015 0.00000 0.00084 0.00086 0.00090 0.00068 0.00068 0.00066 0.00036 N5 0.08811 0.84101 1.01789 1.00000 0.01689 0.02160 0.01419 -0.00103 -0.00074 -0.00461 0.01774 0.00246 0.00017 0.00016 0.00014 0.00000 0.00080 0.00083 0.00081 0.00064 0.00063 0.00065 0.00034 P1 0.46223 0.87800 0.77708 1.00000 0.01870 0.01454 0.01458 0.00031 -0.00083 -0.00365 0.01623 0.00075 0.00005 0.00005 0.00004 0.00000 0.00025 0.00024 0.00025 0.00018 0.00019 0.00018 0.00012 P2 0.22013 0.78215 0.90747 1.00000 0.01752 0.01515 0.01337 -0.00062 -0.00128 -0.00335 0.01555 0.00073 0.00005 0.00005 0.00004 0.00000 0.00024 0.00023 0.00024 0.00018 0.00018 0.00018 0.00012 P3 0.26120 0.78794 0.66520 1.00000 0.02470 0.01682 0.01348 -0.00141 -0.00308 -0.00579 0.01815 0.00075 0.00006 0.00005 0.00004 0.00000 0.00027 0.00024 0.00025 0.00019 0.00020 0.00020 0.00012 Cl1 0.28658 0.58256 0.94473 1.00000 0.03119 0.01464 0.02944 0.00077 -0.00031 -0.00243 0.02616 0.00081 0.00006 0.00005 0.00005 0.00000 0.00028 0.00023 0.00028 0.00019 0.00021 0.00019 0.00013 Cl2 0.28493 0.61830 0.57130 1.00000 0.04146 0.02481 0.02643 -0.01011 0.00102 -0.01414 0.03081 0.00079 0.00006 0.00005 0.00005 0.00000 0.00032 0.00026 0.00028 0.00021 0.00022 0.00023 0.00014 Cl3 0.15126 0.91633 0.56331 1.00000 0.03585 0.03329 0.02594 0.00704 -0.01441 -0.00701 0.03053 0.00084 0.00006 0.00006 0.00005 0.00000 0.00030 0.00029 0.00028 0.00022 0.00023 0.00023 0.00014 Final Structure Factor Calculation for 2006src0966p-1 in P-1 Total number of l.s. parameters = 244 Maximum vector length = 511 Memory required = 3092 / 24017 wR2 = 0.0818 before cycle 5 for 4189 data and 0 / 244 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0340 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0316 for 3748 Fo > 4sig(Fo) and 0.0368 for all 4189 data wR2 = 0.0818, GooF = S = 1.050, Restrained GooF = 1.050 for all data Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0202 0.0159 0.0142 C1 0.0265 0.0230 0.0159 C2 0.0272 0.0254 0.0162 C3 0.0301 0.0234 0.0157 C4 0.0271 0.0237 0.0146 C5 0.0249 0.0200 0.0174 C6 0.0287 0.0242 0.0180 C7 0.0451 0.0267 0.0196 C8 0.0633 0.0337 0.0195 C9 0.0634 0.0319 0.0197 C10 0.0405 0.0214 0.0171 C11 0.0426 0.0242 0.0159 C12 0.0526 0.0303 0.0157 C13 0.0426 0.0338 0.0171 C14 0.0338 0.0267 0.0189 C15 0.0249 0.0227 0.0144 C16 0.0200 0.0168 0.0139 N1 0.0298 0.0188 0.0155 N2 0.0279 0.0183 0.0134 N3 0.0277 0.0194 0.0164 N4 0.0222 0.0178 0.0132 N5 0.0206 0.0147 0.0134 P1 0.0188 0.0150 0.0129 P2 0.0254 0.0165 0.0126 P3 0.0384 0.0254 0.0146 Cl1 0.0512 0.0274 0.0137 Cl2 0.0404 0.0332 0.0180 Cl3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.037 0.057 0.078 0.098 0.124 0.157 0.202 0.276 1.000 Number in group 430. 410. 425. 428. 405. 416. 418. 421. 415. 421. GooF 1.035 1.071 1.114 1.037 1.156 1.022 0.944 0.984 1.037 1.084 K 1.515 0.987 0.954 0.959 0.970 0.990 0.996 1.011 1.017 0.998 Resolution(A) 0.81 0.84 0.87 0.91 0.96 1.02 1.10 1.21 1.38 1.74 inf Number in group 425. 416. 427. 411. 417. 422. 418. 414. 420. 419. GooF 1.034 0.892 0.869 0.891 0.931 0.871 0.906 0.863 1.068 1.808 K 0.974 1.001 1.014 1.018 1.021 1.017 1.013 1.009 1.007 0.984 R1 0.072 0.058 0.044 0.041 0.038 0.033 0.028 0.022 0.027 0.034 Recommended weighting scheme: WGHT 0.0320 1.2012 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) 4 -1 1 42.93 6.91 7.23 0.021 2.19 -1 1 0 3595.61 6006.48 6.71 0.605 6.23 -2 -1 5 97.82 41.38 6.18 0.050 1.86 9 3 6 81.59 156.64 5.47 0.098 0.98 -3 -1 2 121.46 65.37 5.24 0.063 2.49 -1 -2 4 766.82 582.20 4.70 0.188 2.32 -2 -1 4 446.79 327.58 4.65 0.141 2.18 2 -3 2 69.05 34.42 4.42 0.046 2.39 3 -2 1 14.11 1.84 4.33 0.011 2.45 4 3 0 1452.19 1192.38 4.01 0.270 2.06 1 1 4 104.05 161.01 3.98 0.099 2.76 5 1 1 187.23 129.81 3.92 0.089 1.89 -3 2 1 352.97 459.31 3.88 0.167 2.29 3 4 0 191.11 264.97 3.85 0.127 2.13 -1 1 1 181.75 126.57 3.81 0.088 5.14 -1 12 2 -11.89 24.01 3.78 0.038 0.81 -2 2 3 80.15 46.80 3.75 0.053 2.24 5 -1 1 250.66 182.79 3.70 0.106 1.78 2 2 4 28.96 57.66 3.60 0.059 2.43 -1 -3 4 111.91 164.24 3.60 0.100 2.08 4 -2 2 665.12 810.45 3.54 0.222 1.95 0 -5 1 76.56 46.12 3.52 0.053 1.98 5 3 2 11.97 2.02 3.49 0.011 1.76 11 5 3 914.64 723.60 3.48 0.210 0.84 1 4 2 52.03 27.93 3.40 0.041 2.36 -2 3 3 800.80 958.49 3.39 0.242 1.97 7 0 3 11.27 1.25 3.38 0.009 1.32 4 0 0 1316.07 1541.36 3.35 0.307 2.28 9 5 10 25.04 62.75 3.30 0.062 0.82 3 2 1 1972.84 2303.23 3.28 0.375 2.88 2 0 1 29.39 13.36 3.28 0.029 4.56 1 3 3 1742.81 2018.80 3.26 0.351 2.57 1 3 4 3333.85 2923.01 3.22 0.422 2.22 3 3 2 1184.14 1381.98 3.19 0.290 2.42 -3 3 0 81.17 52.31 3.18 0.056 2.08 0 5 1 808.16 680.20 3.17 0.204 1.98 8 4 2 8.94 0.22 3.15 0.004 1.14 -1 -5 1 1892.07 1644.39 3.15 0.317 2.00 -5 -3 2 368.22 455.40 3.11 0.167 1.58 2 2 3 33.12 16.62 3.10 0.032 2.87 1 -2 6 70.93 107.28 3.08 0.081 1.76 5 1 2 10.98 2.64 3.08 0.013 1.88 6 2 6 16.40 2.29 3.08 0.012 1.32 7 -5 9 103.85 148.06 3.08 0.095 0.86 8 4 1 102.24 145.10 3.07 0.094 1.13 8 5 11 25.01 60.80 3.06 0.061 0.82 4 -6 1 10.97 1.33 3.05 0.009 1.26 -5 -10 3 11.95 0.23 3.03 0.004 0.90 4 2 1 527.23 437.78 3.03 0.163 2.28 1 4 0 177.18 133.01 3.02 0.090 2.54 Bond lengths and angles C1 - Distance Angles C6 1.3934 (0.0028) C2 1.4040 (0.0028) 119.21 (0.18) P1 1.7869 (0.0019) 121.34 (0.15) 119.41 (0.15) C1 - C6 C2 C2 - Distance Angles C3 1.3829 (0.0029) C1 1.4040 (0.0028) 120.24 (0.19) H2 0.9500 119.88 119.88 C2 - C3 C1 C3 - Distance Angles C2 1.3829 (0.0029) C4 1.3934 (0.0030) 119.96 (0.19) H3 0.9500 120.02 120.02 C3 - C2 C4 C4 - Distance Angles C5 1.3831 (0.0029) C3 1.3934 (0.0030) 120.20 (0.19) H4 0.9500 119.90 119.90 C4 - C5 C3 C5 - Distance Angles C4 1.3831 (0.0029) C6 1.3906 (0.0028) 120.05 (0.19) H5 0.9500 119.98 119.97 C5 - C4 C6 C6 - Distance Angles C5 1.3906 (0.0028) C1 1.3934 (0.0028) 120.27 (0.18) H6 0.9500 119.87 119.87 C6 - C5 C1 C7 - Distance Angles N4 1.4813 (0.0026) C8 1.5218 (0.0030) 112.05 (0.17) H7A 0.9900 109.20 109.20 H7B 0.9900 109.20 109.20 107.90 C7 - N4 C8 H7A C8 - Distance Angles C9 1.5091 (0.0035) C7 1.5218 (0.0030) 110.86 (0.19) H8A 0.9900 109.47 109.47 H8B 0.9900 109.47 109.47 108.05 C8 - C9 C7 H8A C9 - Distance Angles C8 1.5091 (0.0035) C10 1.5322 (0.0034) 110.15 (0.19) H9A 0.9900 109.63 109.63 H9B 0.9900 109.63 109.63 108.15 C9 - C8 C10 H9A C10 - Distance Angles C11 1.5240 (0.0034) C9 1.5322 (0.0034) 110.50 (0.19) H10A 0.9900 109.55 109.55 H10B 0.9900 109.55 109.55 108.10 C10 - C11 C9 H10A C11 - Distance Angles N4 1.4650 (0.0026) C10 1.5240 (0.0034) 111.98 (0.18) H11A 0.9900 109.22 109.22 H11B 0.9900 109.22 109.22 107.91 C11 - N4 C10 H11A C12 - Distance Angles N5 1.4765 (0.0025) C13 1.5239 (0.0033) 111.74 (0.18) H12A 0.9900 109.27 109.27 H12B 0.9900 109.27 109.27 107.94 C12 - N5 C13 H12A C13 - Distance Angles C12 1.5239 (0.0033) C14 1.5294 (0.0033) 111.09 (0.19) H13A 0.9900 109.42 109.42 H13B 0.9900 109.42 109.42 108.02 C13 - C12 C14 H13A C14 - Distance Angles C13 1.5294 (0.0033) C15 1.5299 (0.0031) 110.94 (0.18) H14A 0.9900 109.45 109.45 H14B 0.9900 109.45 109.45 108.04 C14 - C13 C15 H14A C15 - Distance Angles C16 1.5229 (0.0028) C14 1.5299 (0.0031) 110.86 (0.18) H15A 0.9900 109.47 109.47 H15B 0.9900 109.47 109.47 108.05 C15 - C16 C14 H15A C16 - Distance Angles N5 1.4728 (0.0025) C15 1.5229 (0.0028) 111.83 (0.16) H16A 0.9900 109.25 109.25 H16B 0.9900 109.25 109.25 107.93 C16 - N5 C15 H16A N1 - Distance Angles P2 1.5738 (0.0016) P1 1.6098 (0.0016) 122.19 (0.10) N1 - P2 N2 - Distance Angles P3 1.5773 (0.0017) P2 1.6023 (0.0017) 117.13 (0.11) N2 - P3 N3 - Distance Angles P3 1.5659 (0.0017) P1 1.6274 (0.0017) 122.00 (0.11) N3 - P3 N4 - Distance Angles C11 1.4650 (0.0026) C7 1.4813 (0.0026) 111.73 (0.16) P1 1.6524 (0.0017) 119.03 (0.14) 121.45 (0.14) N4 - C11 C7 N5 - Distance Angles C16 1.4728 (0.0025) C12 1.4765 (0.0025) 113.73 (0.16) P2 1.6256 (0.0016) 121.89 (0.13) 119.85 (0.14) N5 - C16 C12 P1 - Distance Angles N1 1.6098 (0.0016) N3 1.6274 (0.0017) 113.79 (0.09) N4 1.6524 (0.0017) 107.36 (0.09) 112.88 (0.09) C1 1.7869 (0.0019) 110.16 (0.09) 107.88 (0.09) 104.36 (0.09) P1 - N1 N3 N4 P2 - Distance Angles N1 1.5738 (0.0016) N2 1.6023 (0.0017) 118.79 (0.09) N5 1.6256 (0.0016) 111.04 (0.09) 108.75 (0.09) Cl1 2.0850 (0.0007) 106.63 (0.06) 104.17 (0.07) 106.57 (0.06) P2 - N1 N2 N5 P3 - Distance Angles N3 1.5659 (0.0017) N2 1.5773 (0.0017) 120.34 (0.09) Cl2 2.0184 (0.0007) 108.61 (0.07) 109.13 (0.07) Cl3 2.0214 (0.0007) 109.72 (0.07) 107.25 (0.07) 99.85 (0.03) P3 - N3 N2 Cl2 Cl1 - Distance Angles P2 2.0850 (0.0007) Cl1 - Cl2 - Distance Angles P3 2.0184 (0.0007) Cl2 - Cl3 - Distance Angles P3 2.0214 (0.0007) Cl3 - FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0366 for 4189 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.56 at 0.0614 0.9252 0.5859 [ 0.83 A from CL3 ] Deepest hole -0.53 at 0.5022 0.1013 0.1776 [ 0.73 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3015 / 21463 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0614 0.9252 0.5859 1.00000 0.05 0.56 0.83 CL3 2.34 H8B 2.46 P3 2.71 H7A Q2 1 0.9029 0.6329 0.7086 1.00000 0.05 0.48 0.45 H9A 1.05 C9 1.87 H9B 1.91 C10 Q3 1 0.7982 0.6249 0.8137 1.00000 0.05 0.44 0.89 H11B 1.26 C11 1.53 C10 1.77 H10B Q4 1 0.2134 0.6534 0.5331 1.00000 0.05 0.44 0.90 CL2 2.23 P3 2.66 CL3 2.83 H9B Q5 1 0.7181 0.7988 0.6350 1.00000 0.05 0.44 0.95 C8 1.01 H8A 1.16 C7 1.62 H7B Q6 1 0.6033 0.7783 0.7354 1.00000 0.05 0.44 0.83 N4 1.53 P1 1.58 C11 1.76 C7 Q7 1 0.4220 0.8622 0.7233 1.00000 0.05 0.43 0.82 P1 0.85 N3 2.01 N1 2.05 P3 Q8 1 0.4704 0.9804 0.7591 1.00000 0.05 0.33 0.72 C1 1.08 P1 1.84 C6 1.89 C2 Q9 1 0.8640 0.7043 0.6255 1.00000 0.05 0.29 0.77 C8 0.92 C9 1.24 H8B 1.30 H9A Q10 1 0.3514 0.8510 0.6388 1.00000 0.05 0.27 0.72 N3 1.15 P3 2.12 P1 2.23 CL3 Shortest distances between peaks (including symmetry equivalents) 2 9 1.26 7 10 1.30 2 3 1.40 5 6 1.45 7 8 1.46 5 9 1.53 6 7 1.81 6 8 2.21 3 9 2.28 2 5 2.47 8 10 2.49 3 6 2.50 6 9 2.52 5 7 2.75 1 1 2.77 3 5 2.80 6 10 2.80 5 8 2.86 1 10 2.90 1 4 2.91 2 6 2.92 4 10 3.00 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: 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 0.00: Analyse other restraints etc. 1.04: 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 1.26: Structure factors and derivatives 2.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.26: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006src0966p-1 finished at 18:09:48 Total CPU time: 5.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++