+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:17:04 on 02-Dec-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 11.2728 12.4398 13.0398 65.856 82.077 86.293 ZERR 4.00 0.0005 0.0006 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 72 68 12 16 V = 1652.63 F(000) = 712.0 Mu = 0.10 mm-1 Cell Wt = 1357.38 Rho = 1.364 MERG 2 OMIT -1 2 4 OMIT 9 3 3 OMIT 1 11 3 OMIT 5 -7 4 OMIT -1 -5 8 OMIT -6 2 4 OMIT 0 7 11 OMIT 0 11 3 OMIT -1 -3 4 OMIT 0 10 7 OMIT -1 7 11 OMIT -1 -2 4 OMIT -4 2 4 OMIT -1 6 11 OMIT 5 4 7 OMIT 5 6 7 OMIT 0 -1 8 OMIT 8 4 3 OMIT 8 3 3 OMIT 10 3 3 OMIT -1 5 11 OMIT -2 4 0 OMIT 0 5 11 OMIT -2 3 4 OMIT -1 -7 4 OMIT 0 -3 4 OMIT 0 -7 4 OMIT 7 1 7 OMIT 4 6 3 OMIT -5 1 4 OMIT 0 9 11 OMIT -2 -5 8 OMIT 1 10 3 OMIT 4 4 7 OMIT -2 -4 4 OMIT 8 6 7 SHEL 7 0.84 FMAP 2 PLAN 10 SIZE 0.04 0.16 0.22 ACTA BOND $H WGHT 0.19490 L.S. 9 TEMP -153.00 FVAR 0.13925 O1 4 0.860092 0.076439 0.300024 11.00000 0.03939 0.02821 = 0.04150 -0.00718 -0.00015 -0.01102 N2 3 0.998928 0.475758 0.134495 11.00000 0.02251 0.02413 = 0.03502 -0.00786 0.00179 0.00399 AFIX 43 H2 2 0.921726 0.474448 0.157693 11.00000 -1.20000 AFIX 0 O21 4 1.417910 0.645362 0.214152 11.00000 0.03033 0.03266 = 0.04693 -0.01654 0.00244 -0.00765 O22 4 1.746753 0.493346 0.194664 11.00000 0.02114 0.06192 = 0.04777 -0.02485 0.00179 0.00665 O23 4 0.485661 0.327007 0.547650 11.00000 0.02652 0.05979 = 0.07496 -0.03438 0.00119 0.00409 N22 3 1.009489 0.509168 0.367576 11.00000 0.01641 0.03058 = 0.02446 -0.01076 0.00167 0.00777 O3 4 1.158880 1.001383 -0.060013 11.00000 0.06804 0.02724 = 0.06633 -0.02137 -0.00722 0.00390 N1 3 1.058886 0.371800 0.147120 11.00000 0.03231 0.02286 = 0.03315 -0.01159 -0.00352 0.00117 N21 3 1.114096 0.454533 0.347976 11.00000 0.02864 0.02556 = 0.04091 -0.01110 -0.00298 -0.01080 AFIX 43 H21 2 1.117674 0.377478 0.370608 11.00000 -1.20000 AFIX 0 O2 4 0.981629 -0.246638 0.320666 11.00000 0.10560 0.02981 = 0.05423 -0.02264 0.00779 -0.00643 O24 4 0.578082 0.163175 0.565284 11.00000 0.04325 0.04489 = 0.09668 -0.03259 0.00991 -0.01487 O4 4 1.322190 0.923115 -0.110290 11.00000 0.04532 0.03240 = 0.08118 -0.00922 -0.00912 -0.01083 N3 3 1.217198 0.916115 -0.064425 11.00000 0.05121 0.03483 = 0.05089 -0.01126 -0.00724 -0.01495 C39 1 0.802708 0.506658 0.436636 11.00000 0.03819 0.02085 = 0.04315 -0.01475 -0.01270 -0.00021 AFIX 43 H39 2 0.806593 0.587439 0.423282 11.00000 -1.20000 AFIX 0 N23 3 0.578939 0.270190 0.539209 11.00000 0.03579 0.05411 = 0.06469 -0.02869 0.00038 -0.01026 C19 1 0.994307 0.680588 0.091486 11.00000 0.03061 0.03222 = 0.03683 -0.01805 -0.00349 0.00379 AFIX 43 H19 2 0.914413 0.672191 0.128063 11.00000 -1.20000 AFIX 0 C10 1 1.025737 -0.048262 0.273885 11.00000 0.05215 0.02352 = 0.04105 -0.00957 0.00694 -0.00056 C14 1 1.058124 0.581607 0.086106 11.00000 0.02527 0.02816 = 0.03384 -0.01063 -0.01053 0.00021 C34 1 0.907249 0.447889 0.412393 11.00000 0.01910 0.02585 = 0.02612 -0.01088 -0.00085 0.00493 C16 1 1.224108 0.702190 -0.022203 11.00000 0.03063 0.03123 = 0.03426 -0.00338 -0.00875 -0.00565 AFIX 43 H16 2 1.302245 0.711233 -0.062608 11.00000 -1.20000 AFIX 0 C38 1 0.697745 0.449852 0.478359 11.00000 0.03282 0.03397 = 0.03967 -0.02025 -0.00374 0.00316 AFIX 43 H38 2 0.627741 0.490552 0.493142 11.00000 -1.20000 AFIX 0 C13 1 0.996290 0.278702 0.198686 11.00000 0.02510 0.02771 = 0.03167 -0.01150 0.00392 0.00616 AFIX 43 H13 2 0.915447 0.283917 0.228675 11.00000 -1.20000 AFIX 0 C36 1 0.791528 0.270079 0.478203 11.00000 0.03538 0.02276 = 0.04669 -0.01025 -0.00762 -0.00613 AFIX 43 H36 2 0.786459 0.189347 0.491763 11.00000 -1.20000 AFIX 0 C29 1 1.426272 0.527833 0.240985 11.00000 0.02707 0.03565 = 0.03788 -0.01910 0.00057 -0.00028 C18 1 1.046834 0.788351 0.044378 11.00000 0.04712 0.02777 = 0.03448 -0.00970 -0.00829 0.00466 AFIX 43 H18 2 1.005188 0.854568 0.050906 11.00000 -1.20000 AFIX 0 C25 1 1.540159 0.351011 0.254476 11.00000 0.03706 0.04590 = 0.04212 -0.02212 -0.00638 0.01188 AFIX 43 H25 2 1.614529 0.312350 0.248082 11.00000 -1.20000 AFIX 0 C26 1 1.435004 0.289118 0.284922 11.00000 0.03430 0.03721 = 0.06426 -0.02289 0.00118 0.00436 AFIX 43 H26 2 1.436762 0.208147 0.297900 11.00000 -1.20000 AFIX 0 C37 1 0.692542 0.329769 0.499893 11.00000 0.02428 0.03201 = 0.03740 -0.02097 0.00390 -0.00961 C2 1 0.796109 -0.028417 0.385018 11.00000 0.04434 0.03152 = 0.04394 -0.01245 0.00286 -0.00923 C15 1 1.171417 0.593524 0.027671 11.00000 0.03814 0.02093 = 0.03944 -0.01520 -0.00907 0.00167 AFIX 43 H15 2 1.212827 0.526845 0.021946 11.00000 -1.20000 AFIX 0 C5 1 1.145553 -0.054796 0.238006 11.00000 0.06554 0.03215 = 0.06064 -0.02436 0.00233 0.00981 AFIX 43 H5 2 1.179510 -0.129005 0.244937 11.00000 -1.20000 AFIX 0 C23 1 1.633286 0.662170 0.200436 11.00000 0.02034 0.04711 = 0.04415 -0.01682 0.00619 -0.00486 AFIX 23 H23A 2 1.626108 0.659373 0.278014 11.00000 -1.20000 H23B 2 1.704166 0.709923 0.155851 11.00000 -1.20000 AFIX 0 C6 1 1.216953 0.041698 0.192901 11.00000 0.04411 0.03872 = 0.05919 -0.02996 0.00415 0.01361 AFIX 43 H6 2 1.299938 0.034298 0.170874 11.00000 -1.20000 AFIX 0 C7 1 1.167986 0.149673 0.179555 11.00000 0.03898 0.02765 = 0.04035 -0.00963 0.00606 -0.00420 AFIX 43 H7 2 1.218299 0.216710 0.146991 11.00000 -1.20000 AFIX 0 C8 1 1.048726 0.164634 0.211537 11.00000 0.03470 0.02615 = 0.02955 -0.01334 0.00256 -0.00704 C30 1 1.537533 0.470055 0.233091 11.00000 0.02364 0.04743 = 0.03380 -0.01570 -0.00317 0.00591 C22 1 1.522696 0.717737 0.146742 11.00000 0.01420 0.04378 = 0.05120 -0.00902 0.00743 -0.00818 C9 1 0.976547 0.062551 0.263969 11.00000 0.03878 0.02816 = 0.03529 -0.01024 0.00697 -0.00360 C33 1 1.207106 0.517939 0.295843 11.00000 0.03426 0.02710 = 0.03747 -0.00932 -0.01590 0.00407 AFIX 43 H33 2 1.201058 0.601253 0.269300 11.00000 -1.20000 AFIX 0 C27 1 1.326300 0.344734 0.296725 11.00000 0.04158 0.03050 = 0.03775 -0.00139 0.00576 -0.00980 AFIX 43 H27 2 1.254408 0.300843 0.318491 11.00000 -1.20000 AFIX 0 C17 1 1.161294 0.800751 -0.013068 11.00000 0.04597 0.02090 = 0.04053 -0.00392 -0.00658 -0.00469 C35 1 0.899403 0.328252 0.436257 11.00000 0.02937 0.03664 = 0.04490 -0.01869 -0.00405 0.00312 AFIX 43 H35 2 0.969253 0.286269 0.423462 11.00000 -1.20000 AFIX 0 C3 1 0.816178 -0.126575 0.345696 11.00000 0.06703 0.02906 = 0.05066 -0.01717 0.01221 -0.01925 AFIX 23 H3A 2 0.780327 -0.199447 0.406004 11.00000 -1.20000 H3B 2 0.774328 -0.106955 0.278223 11.00000 -1.20000 AFIX 0 C31 1 1.531184 0.727293 0.024441 11.00000 0.04932 0.05525 = 0.03557 0.00034 -0.00416 -0.00812 AFIX 137 H31A 2 1.539252 0.648283 0.024672 11.00000 -1.50000 H31B 2 1.601177 0.774225 -0.020718 11.00000 -1.50000 H31C 2 1.458523 0.765454 -0.008471 11.00000 -1.50000 AFIX 0 C28 1 1.320626 0.463803 0.277240 11.00000 0.02764 0.03329 = 0.04324 -0.01112 -0.00087 -0.00414 C12 1 0.666488 0.011337 0.392266 11.00000 0.04913 0.05268 = 0.05829 -0.01359 0.01158 -0.01505 AFIX 137 H12A 2 0.659489 0.075747 0.417710 11.00000 -1.50000 H12B 2 0.617085 -0.054807 0.446295 11.00000 -1.50000 H12C 2 0.639045 0.038786 0.317480 11.00000 -1.50000 AFIX 0 C24 1 1.649043 0.538363 0.204976 11.00000 0.02295 0.06584 = 0.03812 -0.02242 -0.00676 0.00797 C32 1 1.496058 0.838001 0.149408 11.00000 0.04283 0.03309 = 0.05974 -0.00816 0.00489 -0.01313 AFIX 137 H32A 2 1.421195 0.869375 0.117356 11.00000 -1.50000 H32B 2 1.561710 0.891727 0.104727 11.00000 -1.50000 H32C 2 1.488096 0.830428 0.227860 11.00000 -1.50000 AFIX 0 C11 1 0.844296 -0.058829 0.497686 11.00000 0.07006 0.03584 = 0.05230 -0.00638 0.00032 -0.01455 AFIX 137 H11A 2 0.927869 -0.085178 0.492398 11.00000 -1.50000 H11B 2 0.796207 -0.121891 0.557985 11.00000 -1.50000 H11C 2 0.839713 0.011078 0.514928 11.00000 -1.50000 AFIX 0 C4 1 0.944690 -0.149278 0.316791 11.00000 0.07600 0.03545 = 0.03283 -0.01433 0.00261 -0.00237 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 O1 - C9 C2 N2 - C14 N1 O21 - C29 C22 O22 - C24 O23 - N23 N22 - C34 N21 O3 - N3 N1 - C13 N2 N21 - C33 N22 O2 - C4 O24 - N23 O4 - N3 N3 - O3 O4 C17 C39 - C38 C34 N23 - O24 O23 C37 C19 - C18 C14 C10 - C5 C9 C4 C14 - N2 C15 C19 C34 - N22 C35 C39 C16 - C15 C17 C38 - C39 C37 C13 - N1 C8 C36 - C37 C35 C29 - O21 C28 C30 C18 - C19 C17 C25 - C26 C30 C26 - C25 C27 C37 - C36 C38 N23 C2 - O1 C3 C12 C11 C15 - C16 C14 C5 - C6 C10 C23 - C22 C24 C6 - C5 C7 C7 - C6 C8 C8 - C7 C9 C13 C30 - C25 C29 C24 C22 - O21 C23 C32 C31 C9 - O1 C10 C8 C33 - N21 C28 C27 - C26 C28 C17 - C18 C16 N3 C35 - C36 C34 C3 - C4 C2 C31 - C22 C28 - C29 C27 C33 C12 - C2 C24 - O22 C30 C23 C32 - C22 C11 - C2 C4 - O2 C10 C3 20735 Reflections read, of which 2466 rejected -13 =< h =< 13, -14 =< k =< 14, -15 =< l =< 15, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 5 0 0 49.47 3.33 3 20.85 2 1 0 36.99 1.09 6 7.09 5 1 0 7.43 0.99 4 5.76 1 3 0 11.60 0.45 8 3.92 1 4 0 21.28 0.88 6 7.42 0 3 3 38.37 1.02 5 10.17 0 2 4 851.65 18.76 3 724.38 3 2 4 4.19 1.00 3 10.54 0 3 4 8.34 0.72 3 10.33 0 -9 5 1.98 0.67 4 3.38 0 2 7 16.32 0.64 4 3.25 2 3 7 21.79 0.57 4 3.16 -1 4 7 85.00 4.52 4 26.89 0 5 7 22.03 1.02 3 61.14 -2 5 11 3.98 0.70 3 3.61 15 Inconsistent equivalents 5664 Unique reflections, of which 0 suppressed R(int) = 0.1796 R(sigma) = 0.2386 Friedel opposites merged Maximum memory for data reduction = 4117 / 57263 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 = 5268 / 592655 wR2 = 0.3766 before cycle 1 for 5664 data and 455 / 455 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.13863 0.00084 -0.741 OSF Mean shift/su = 0.028 Maximum = -0.741 for OSF Max. shift = 0.001 A for H11C Max. dU = 0.000 for C11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5268 / 592655 wR2 = 0.3761 before cycle 2 for 5664 data and 455 / 455 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.13847 0.00084 -0.190 OSF Mean shift/su = 0.011 Maximum = -0.190 for OSF Max. shift = 0.000 A for H11C Max. dU = 0.000 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5268 / 592655 wR2 = 0.3761 before cycle 3 for 5664 data and 455 / 455 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.13845 0.00084 -0.015 OSF Mean shift/su = 0.002 Maximum = -0.015 for OSF Max. shift = 0.000 A for H31C Max. dU = 0.000 for N23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5268 / 592655 wR2 = 0.3761 before cycle 4 for 5664 data and 455 / 455 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.13845 0.00084 -0.003 OSF Mean shift/su = 0.001 Maximum = -0.003 for OSF Max. shift = 0.000 A for H32A Max. dU = 0.000 for C31 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5268 / 592655 wR2 = 0.3761 before cycle 5 for 5664 data and 455 / 455 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.13845 0.00084 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H32A Max. dU = 0.000 for C31 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5268 / 592655 wR2 = 0.3761 before cycle 6 for 5664 data and 455 / 455 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.13845 0.00084 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H32A Max. dU = 0.000 for N23 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5268 / 592655 wR2 = 0.3761 before cycle 7 for 5664 data and 455 / 455 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.13845 0.00084 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C19 Max. shift = 0.000 A for H12A Max. dU = 0.000 for C3 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5268 / 592655 wR2 = 0.3761 before cycle 8 for 5664 data and 455 / 455 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.13845 0.00084 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H32C Max. dU = 0.000 for C22 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5268 / 592655 wR2 = 0.3761 before cycle 9 for 5664 data and 455 / 455 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.13845 0.00084 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U23 O23 Max. shift = 0.000 A for H32B Max. dU = 0.000 for N23 Largest correlation matrix elements -0.580 U23 C6 / U33 C6 -0.548 U23 O3 / U33 O3 -0.526 U23 C35 / U33 C35 -0.565 U23 C37 / U33 C37 -0.541 U23 C19 / U33 C19 -0.526 U23 C38 / U22 C38 -0.564 U23 C6 / U22 C6 -0.539 U23 C38 / U33 C38 -0.524 U23 C19 / U22 C19 -0.554 U23 O2 / U33 O2 -0.538 U23 C15 / U33 C15 -0.524 U23 C15 / U22 C15 -0.554 U23 C5 / U33 C5 -0.534 U23 C5 / U22 C5 -0.521 U23 C25 / U33 C25 -0.549 U23 O23 / U33 O23 -0.532 U23 C39 / U33 C39 -0.521 U23 C3 / U33 C3 -0.549 U23 O23 / U22 O23 -0.532 U23 C26 / U33 C26 -0.521 U23 C25 / U22 C25 -0.549 U23 C29 / U33 C29 -0.530 U23 C8 / U33 C8 -0.520 U23 C37 / U22 C37 Idealized hydrogen atom generation before cycle 10 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.9217 0.4745 0.1577 43 0.880 0.000 N2 C14 N1 H21 1.1177 0.3775 0.3706 43 0.880 0.000 N21 C33 N22 H39 0.8066 0.5875 0.4233 43 0.950 0.000 C39 C38 C34 H19 0.9144 0.6722 0.1281 43 0.950 0.000 C19 C18 C14 H16 1.3023 0.7113 -0.0626 43 0.950 0.000 C16 C15 C17 H38 0.6277 0.4906 0.4931 43 0.950 0.000 C38 C39 C37 H13 0.9154 0.2839 0.2286 43 0.950 0.000 C13 N1 C8 H36 0.7865 0.1893 0.4917 43 0.950 0.000 C36 C37 C35 H18 1.0052 0.8546 0.0510 43 0.950 0.000 C18 C19 C17 H25 1.6146 0.3123 0.2481 43 0.950 0.000 C25 C26 C30 H26 1.4368 0.2081 0.2979 43 0.950 0.000 C26 C25 C27 H15 1.2128 0.5269 0.0219 43 0.950 0.000 C15 C16 C14 H5 1.1795 -0.1290 0.2449 43 0.950 0.000 C5 C6 C10 H23A 1.6261 0.6594 0.2781 23 0.990 0.000 C23 C22 C24 H23B 1.7042 0.7099 0.1559 23 0.990 0.000 C23 C22 C24 H6 1.3000 0.0343 0.1709 43 0.950 0.000 C6 C5 C7 H7 1.2183 0.2167 0.1470 43 0.950 0.000 C7 C6 C8 H33 1.2010 0.6013 0.2693 43 0.950 0.000 C33 N21 C28 H27 1.2544 0.3008 0.3185 43 0.950 0.000 C27 C26 C28 H35 0.9693 0.2862 0.4235 43 0.950 0.000 C35 C36 C34 H3A 0.7803 -0.1995 0.4060 23 0.990 0.000 C3 C4 C2 H3B 0.7743 -0.1070 0.2782 23 0.990 0.000 C3 C4 C2 H31A 1.5392 0.6483 0.0247 137 0.980 0.000 C31 C22 H31A H31B 1.6012 0.7742 -0.0207 137 0.980 0.000 C31 C22 H31A H31C 1.4586 0.7655 -0.0085 137 0.980 0.000 C31 C22 H31A H12A 0.6595 0.0757 0.4178 137 0.980 0.000 C12 C2 H12A H12B 0.6171 -0.0548 0.4462 137 0.980 0.000 C12 C2 H12A H12C 0.6391 0.0389 0.3174 137 0.980 0.000 C12 C2 H12A H32A 1.4212 0.8694 0.1174 137 0.980 0.000 C32 C22 H32A H32B 1.5617 0.8917 0.1048 137 0.980 0.000 C32 C22 H32A H32C 1.4881 0.8304 0.2279 137 0.980 0.000 C32 C22 H32A H11A 0.9278 -0.0853 0.4924 137 0.980 0.000 C11 C2 H11A H11B 0.7961 -0.1218 0.5580 137 0.980 0.000 C11 C2 H11A H11C 0.8399 0.0111 0.5148 137 0.980 0.000 C11 C2 H11A s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.86007 0.07645 0.30001 1.00000 0.03900 0.02778 0.04113 -0.00703 -0.00008 -0.01098 0.03824 0.00806 0.00051 0.00046 0.00048 0.00000 0.00360 0.00299 0.00375 0.00267 0.00283 0.00262 0.00151 N2 0.99894 0.47576 0.13449 1.00000 0.02219 0.02379 0.03476 -0.00779 0.00183 0.00400 0.02900 0.00946 0.00055 0.00053 0.00054 0.00000 0.00344 0.00353 0.00420 0.00302 0.00300 0.00295 0.00160 H2 0.92174 0.47445 0.15768 1.00000 0.03480 0.00000 0.00000 O21 1.41790 0.64536 0.21416 1.00000 0.02988 0.03231 0.04656 -0.01637 0.00250 -0.00762 0.03650 0.00786 0.00047 0.00046 0.00048 0.00000 0.00315 0.00317 0.00382 0.00285 0.00261 0.00254 0.00144 O22 1.74677 0.49335 0.19467 1.00000 0.02078 0.06144 0.04740 -0.02469 0.00183 0.00663 0.04328 0.00859 0.00048 0.00055 0.00051 0.00000 0.00317 0.00401 0.00404 0.00325 0.00269 0.00290 0.00158 O23 0.48564 0.32703 0.54764 1.00000 0.02611 0.05938 0.07454 -0.03424 0.00136 0.00402 0.05197 0.00921 0.00053 0.00057 0.00059 0.00000 0.00348 0.00426 0.00501 0.00379 0.00319 0.00316 0.00177 N22 1.00949 0.50915 0.36757 1.00000 0.01618 0.03019 0.02410 -0.01057 0.00166 0.00769 0.02443 0.00919 0.00052 0.00053 0.00051 0.00000 0.00329 0.00346 0.00380 0.00295 0.00275 0.00288 0.00148 O3 1.15886 1.00138 -0.06001 1.00000 0.06757 0.02693 0.06589 -0.02120 -0.00707 0.00380 0.05298 0.00949 0.00062 0.00052 0.00058 0.00000 0.00466 0.00336 0.00484 0.00329 0.00357 0.00330 0.00180 N1 1.05890 0.37180 0.14712 1.00000 0.03189 0.02256 0.03273 -0.01140 -0.00341 0.00117 0.02912 0.00915 0.00057 0.00053 0.00055 0.00000 0.00373 0.00359 0.00418 0.00316 0.00313 0.00319 0.00161 N21 1.11410 0.45451 0.34797 1.00000 0.02821 0.02520 0.04057 -0.01102 -0.00291 -0.01071 0.03172 0.00914 0.00056 0.00056 0.00057 0.00000 0.00391 0.00343 0.00440 0.00322 0.00326 0.00319 0.00167 H21 1.11770 0.37745 0.37060 1.00000 0.03806 0.00000 0.00000 O2 0.98163 -0.24664 0.32067 1.00000 0.10504 0.02938 0.05387 -0.02245 0.00783 -0.00636 0.06244 0.01051 0.00072 0.00053 0.00058 0.00000 0.00598 0.00354 0.00457 0.00319 0.00394 0.00366 0.00209 O24 0.57806 0.16317 0.56529 1.00000 0.04276 0.04452 0.09614 -0.03236 0.01004 -0.01490 0.06107 0.01014 0.00057 0.00059 0.00066 0.00000 0.00392 0.00419 0.00591 0.00396 0.00366 0.00325 0.00203 O4 1.32219 0.92312 -0.11032 1.00000 0.04497 0.03191 0.08070 -0.00902 -0.00906 -0.01078 0.05643 0.00961 0.00062 0.00051 0.00063 0.00000 0.00431 0.00347 0.00528 0.00338 0.00378 0.00305 0.00191 N3 1.21720 0.91613 -0.06444 1.00000 0.05088 0.03440 0.05046 -0.01107 -0.00722 -0.01489 0.04647 0.01075 0.00078 0.00065 0.00067 0.00000 0.00548 0.00458 0.00536 0.00387 0.00420 0.00413 0.00205 C39 0.80270 0.50669 0.43664 1.00000 0.03783 0.02056 0.04280 -0.01463 -0.01262 -0.00014 0.03235 0.01119 0.00072 0.00066 0.00070 0.00000 0.00514 0.00407 0.00550 0.00396 0.00419 0.00387 0.00204 H39 0.80659 0.58747 0.42329 1.00000 0.03883 0.00000 0.00000 N23 0.57891 0.27020 0.53921 1.00000 0.03537 0.05398 0.06410 -0.02864 0.00058 -0.01035 0.04980 0.01109 0.00068 0.00074 0.00070 0.00000 0.00482 0.00547 0.00589 0.00455 0.00404 0.00428 0.00212 C19 0.99427 0.68058 0.09150 1.00000 0.03025 0.03200 0.03662 -0.01797 -0.00341 0.00376 0.03187 0.01148 0.00073 0.00068 0.00070 0.00000 0.00461 0.00465 0.00527 0.00406 0.00383 0.00383 0.00197 H19 0.91438 0.67218 0.12807 1.00000 0.03825 0.00000 0.00000 C10 1.02575 -0.04828 0.27392 1.00000 0.05190 0.02312 0.04081 -0.00939 0.00700 -0.00066 0.04107 0.01370 0.00085 0.00070 0.00077 0.00000 0.00604 0.00437 0.00573 0.00404 0.00453 0.00416 0.00227 C14 1.05813 0.58160 0.08611 1.00000 0.02488 0.02782 0.03355 -0.01052 -0.01041 0.00018 0.02870 0.01091 0.00068 0.00066 0.00069 0.00000 0.00440 0.00437 0.00494 0.00378 0.00372 0.00364 0.00190 C34 0.90725 0.44789 0.41240 1.00000 0.01877 0.02551 0.02582 -0.01077 -0.00080 0.00497 0.02368 0.01093 0.00064 0.00064 0.00064 0.00000 0.00407 0.00404 0.00456 0.00348 0.00336 0.00348 0.00176 C16 1.22412 0.70221 -0.02222 1.00000 0.03024 0.03093 0.03389 -0.00323 -0.00866 -0.00563 0.03421 0.01155 0.00074 0.00068 0.00070 0.00000 0.00451 0.00469 0.00521 0.00395 0.00382 0.00385 0.00206 H16 1.30227 0.71127 -0.06262 1.00000 0.04105 0.00000 0.00000 C38 0.69772 0.44987 0.47836 1.00000 0.03244 0.03360 0.03933 -0.02010 -0.00367 0.00313 0.03360 0.01181 0.00076 0.00071 0.00071 0.00000 0.00477 0.00466 0.00544 0.00410 0.00397 0.00392 0.00203 H38 0.62770 0.49056 0.49313 1.00000 0.04032 0.00000 0.00000 C13 0.99629 0.27870 0.19867 1.00000 0.02474 0.02752 0.03130 -0.01147 0.00393 0.00618 0.02906 0.01187 0.00070 0.00066 0.00068 0.00000 0.00427 0.00446 0.00493 0.00378 0.00359 0.00371 0.00191 H13 0.91544 0.28392 0.22863 1.00000 0.03487 0.00000 0.00000 C36 0.79154 0.27006 0.47819 1.00000 0.03506 0.02242 0.04636 -0.01008 -0.00764 -0.00607 0.03533 0.01173 0.00073 0.00069 0.00074 0.00000 0.00513 0.00417 0.00569 0.00401 0.00419 0.00387 0.00212 H36 0.78645 0.18934 0.49174 1.00000 0.04240 0.00000 0.00000 C29 1.42628 0.52785 0.24098 1.00000 0.02680 0.03529 0.03754 -0.01890 0.00063 -0.00026 0.03231 0.01157 0.00069 0.00069 0.00070 0.00000 0.00452 0.00486 0.00537 0.00421 0.00384 0.00390 0.00200 C18 1.04682 0.78836 0.04440 1.00000 0.04661 0.02738 0.03413 -0.00949 -0.00811 0.00455 0.03693 0.01218 0.00079 0.00071 0.00071 0.00000 0.00566 0.00455 0.00528 0.00398 0.00435 0.00415 0.00214 H18 1.00520 0.85457 0.05096 1.00000 0.04431 0.00000 0.00000 C25 1.54019 0.35101 0.25449 1.00000 0.03672 0.04550 0.04185 -0.02202 -0.00640 0.01190 0.04035 0.01312 0.00080 0.00078 0.00076 0.00000 0.00519 0.00543 0.00575 0.00451 0.00423 0.00445 0.00221 H25 1.61457 0.31235 0.24812 1.00000 0.04842 0.00000 0.00000 C26 1.43501 0.28911 0.28491 1.00000 0.03405 0.03685 0.06384 -0.02270 0.00118 0.00439 0.04511 0.01394 0.00078 0.00080 0.00084 0.00000 0.00536 0.00489 0.00682 0.00476 0.00458 0.00433 0.00237 H26 1.43677 0.20814 0.29786 1.00000 0.05413 0.00000 0.00000 C37 0.69255 0.32978 0.49989 1.00000 0.02405 0.03172 0.03706 -0.02082 0.00393 -0.00963 0.02901 0.01086 0.00067 0.00068 0.00070 0.00000 0.00440 0.00442 0.00510 0.00392 0.00360 0.00377 0.00191 C2 0.79608 -0.02843 0.38504 1.00000 0.04393 0.03124 0.04354 -0.01238 0.00304 -0.00929 0.04091 0.01275 0.00080 0.00072 0.00077 0.00000 0.00544 0.00465 0.00606 0.00425 0.00440 0.00413 0.00227 C15 1.17143 0.59353 0.02764 1.00000 0.03785 0.02046 0.03899 -0.01496 -0.00895 0.00164 0.03112 0.01106 0.00072 0.00065 0.00069 0.00000 0.00511 0.00415 0.00537 0.00387 0.00413 0.00370 0.00201 H15 1.21283 0.52686 0.02189 1.00000 0.03735 0.00000 0.00000 C5 1.14556 -0.05481 0.23801 1.00000 0.06512 0.03186 0.06049 -0.02432 0.00229 0.00986 0.05215 0.01498 0.00093 0.00080 0.00087 0.00000 0.00727 0.00519 0.00705 0.00493 0.00554 0.00507 0.00270 H5 1.17951 -0.12902 0.24493 1.00000 0.06258 0.00000 0.00000 C23 1.63328 0.66218 0.20047 1.00000 0.02002 0.04687 0.04383 -0.01676 0.00610 -0.00487 0.03824 0.01268 0.00069 0.00075 0.00078 0.00000 0.00436 0.00538 0.00570 0.00446 0.00387 0.00388 0.00217 H23A 1.62607 0.65935 0.27806 1.00000 0.04589 0.00000 0.00000 H23B 1.70417 0.70993 0.15592 1.00000 0.04589 0.00000 0.00000 C6 1.21699 0.04168 0.19290 1.00000 0.04372 0.03845 0.05891 -0.02985 0.00414 0.01360 0.04542 0.01404 0.00085 0.00077 0.00082 0.00000 0.00548 0.00535 0.00666 0.00492 0.00474 0.00456 0.00243 H6 1.29997 0.03427 0.17087 1.00000 0.05450 0.00000 0.00000 C7 1.16801 0.14969 0.17955 1.00000 0.03867 0.02721 0.04011 -0.00954 0.00598 -0.00415 0.03760 0.01287 0.00077 0.00071 0.00073 0.00000 0.00519 0.00445 0.00559 0.00405 0.00417 0.00397 0.00217 H7 1.21832 0.21673 0.14699 1.00000 0.04512 0.00000 0.00000 C8 1.04872 0.16464 0.21154 1.00000 0.03428 0.02574 0.02930 -0.01315 0.00264 -0.00703 0.02946 0.01109 0.00072 0.00065 0.00067 0.00000 0.00482 0.00424 0.00492 0.00373 0.00375 0.00370 0.00193 C30 1.53754 0.47004 0.23310 1.00000 0.02332 0.04710 0.03356 -0.01559 -0.00320 0.00586 0.03522 0.01223 0.00069 0.00076 0.00071 0.00000 0.00444 0.00539 0.00531 0.00429 0.00375 0.00401 0.00209 C22 1.52270 0.71777 0.14673 1.00000 0.01385 0.04340 0.05086 -0.00875 0.00741 -0.00811 0.04023 0.01300 0.00067 0.00075 0.00079 0.00000 0.00407 0.00518 0.00627 0.00451 0.00385 0.00372 0.00230 C9 0.97654 0.06257 0.26395 1.00000 0.03845 0.02782 0.03509 -0.01017 0.00700 -0.00348 0.03566 0.01262 0.00077 0.00069 0.00072 0.00000 0.00531 0.00450 0.00537 0.00395 0.00412 0.00397 0.00210 C33 1.20708 0.51796 0.29584 1.00000 0.03398 0.02671 0.03708 -0.00914 -0.01584 0.00411 0.03287 0.01159 0.00073 0.00071 0.00071 0.00000 0.00488 0.00428 0.00531 0.00390 0.00408 0.00395 0.00203 H33 1.20101 0.60127 0.26931 1.00000 0.03944 0.00000 0.00000 C27 1.32627 0.34472 0.29672 1.00000 0.04114 0.03028 0.03750 -0.00143 0.00581 -0.00972 0.04100 0.01359 0.00081 0.00071 0.00074 0.00000 0.00531 0.00469 0.00555 0.00407 0.00420 0.00420 0.00228 H27 1.25438 0.30082 0.31849 1.00000 0.04920 0.00000 0.00000 C17 1.16128 0.80073 -0.01307 1.00000 0.04566 0.02049 0.04040 -0.00385 -0.00666 -0.00465 0.03797 0.01244 0.00080 0.00067 0.00074 0.00000 0.00558 0.00419 0.00562 0.00390 0.00444 0.00399 0.00218 C35 0.89941 0.32821 0.43628 1.00000 0.02892 0.03632 0.04458 -0.01853 -0.00399 0.00313 0.03611 0.01198 0.00074 0.00071 0.00074 0.00000 0.00470 0.00490 0.00577 0.00433 0.00407 0.00399 0.00212 H35 0.96927 0.28622 0.42350 1.00000 0.04333 0.00000 0.00000 C3 0.81612 -0.12660 0.34570 1.00000 0.06672 0.02880 0.05028 -0.01706 0.01222 -0.01914 0.04934 0.01404 0.00091 0.00074 0.00086 0.00000 0.00695 0.00477 0.00632 0.00451 0.00506 0.00467 0.00259 H3A 0.78026 -0.19947 0.40600 1.00000 0.05921 0.00000 0.00000 H3B 0.77427 -0.10696 0.27822 1.00000 0.05921 0.00000 0.00000 C31 1.53120 0.72733 0.02444 1.00000 0.04877 0.05498 0.03512 0.00036 -0.00409 -0.00816 0.05217 0.01475 0.00086 0.00087 0.00078 0.00000 0.00593 0.00606 0.00607 0.00476 0.00453 0.00487 0.00262 H31A 1.53920 0.64832 0.02468 1.00000 0.07825 0.00000 0.00000 H31B 1.60123 0.77421 -0.02070 1.00000 0.07825 0.00000 0.00000 H31C 1.45856 0.76554 -0.00849 1.00000 0.07825 0.00000 0.00000 C28 1.32062 0.46382 0.27723 1.00000 0.02722 0.03296 0.04299 -0.01102 -0.00072 -0.00416 0.03601 0.01213 0.00071 0.00071 0.00075 0.00000 0.00475 0.00470 0.00563 0.00414 0.00398 0.00391 0.00213 C12 0.66649 0.01134 0.39226 1.00000 0.04868 0.05217 0.05787 -0.01338 0.01158 -0.01500 0.05700 0.01568 0.00085 0.00087 0.00091 0.00000 0.00623 0.00607 0.00702 0.00532 0.00503 0.00501 0.00281 H12A 0.65948 0.07571 0.41776 1.00000 0.08550 0.00000 0.00000 H12B 0.61706 -0.05481 0.44623 1.00000 0.08550 0.00000 0.00000 H12C 0.63909 0.03885 0.31745 1.00000 0.08550 0.00000 0.00000 C24 1.64906 0.53835 0.20498 1.00000 0.02271 0.06533 0.03765 -0.02210 -0.00666 0.00785 0.04157 0.01312 0.00076 0.00087 0.00076 0.00000 0.00474 0.00624 0.00576 0.00480 0.00397 0.00443 0.00228 C32 1.49607 0.83799 0.14942 1.00000 0.04236 0.03281 0.05928 -0.00807 0.00491 -0.01305 0.04884 0.01443 0.00084 0.00075 0.00087 0.00000 0.00547 0.00487 0.00678 0.00471 0.00475 0.00430 0.00256 H32A 1.42122 0.86937 0.11737 1.00000 0.07326 0.00000 0.00000 H32B 1.56173 0.89172 0.10476 1.00000 0.07326 0.00000 0.00000 H32C 1.48811 0.83040 0.22788 1.00000 0.07326 0.00000 0.00000 C11 0.84431 -0.05882 0.49769 1.00000 0.06955 0.03545 0.05183 -0.00626 0.00035 -0.01442 0.05618 0.01507 0.00097 0.00082 0.00086 0.00000 0.00704 0.00511 0.00681 0.00475 0.00536 0.00492 0.00278 H11A 0.92783 -0.08531 0.49243 1.00000 0.08426 0.00000 0.00000 H11B 0.79614 -0.12178 0.55803 1.00000 0.08426 0.00000 0.00000 H11C 0.83988 0.01113 0.51484 1.00000 0.08426 0.00000 0.00000 C4 0.94471 -0.14930 0.31679 1.00000 0.07552 0.03526 0.03253 -0.01421 0.00275 -0.00246 0.04847 0.01450 0.00096 0.00080 0.00077 0.00000 0.00751 0.00543 0.00572 0.00434 0.00497 0.00504 0.00254 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 455 Maximum vector length = 511 Memory required = 4813 / 22995 wR2 = 0.3761 before cycle 10 for 5664 data and 0 / 455 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1949 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1218 for 2293 Fo > 4sig(Fo) and 0.2614 for all 5664 data wR2 = 0.3761, GooF = S = 1.026, Restrained GooF = 1.026 for all data Occupancy sum of asymmetric unit = 50.00 for non-hydrogen and 34.00 for hydrogen atoms Principal mean square atomic displacements U 0.0489 0.0449 0.0209 O1 0.0440 0.0250 0.0180 N2 0.0503 0.0356 0.0236 O21 0.0631 0.0490 0.0177 O22 0.0771 0.0548 0.0240 O23 0.0374 0.0253 0.0105 N22 0.0698 0.0656 0.0235 O3 0.0338 0.0317 0.0218 N1 0.0431 0.0368 0.0153 N21 0.1131 0.0503 0.0239 O2 0.1050 0.0496 0.0286 O24 0.0944 0.0489 0.0260 O4 0.0643 0.0495 0.0255 N3 0.0480 0.0313 0.0177 C39 0.0679 0.0508 0.0307 N23 0.0379 0.0334 0.0243 C19 0.0648 0.0353 0.0231 C10 0.0382 0.0279 0.0200 C14 0.0301 0.0260 0.0150 C34 0.0513 0.0263 0.0250 C16 0.0410 0.0344 0.0254 C38 0.0426 0.0288 0.0158 C13 0.0511 0.0354 0.0195 C36 0.0408 0.0316 0.0245 C29 0.0478 0.0372 0.0257 C18 0.0543 0.0400 0.0268 C25 0.0678 0.0403 0.0272 C26 0.0455 0.0247 0.0168 C37 0.0533 0.0430 0.0264 C2 0.0422 0.0336 0.0176 C15 0.0785 0.0557 0.0223 C5 0.0499 0.0474 0.0174 C23 0.0667 0.0544 0.0152 C6 0.0538 0.0340 0.0250 C7 0.0408 0.0260 0.0216 C8 0.0504 0.0335 0.0218 C30 0.0670 0.0432 0.0105 C22 0.0513 0.0308 0.0250 C9 0.0470 0.0308 0.0208 C33 0.0573 0.0463 0.0194 C27 0.0512 0.0435 0.0192 C17 0.0447 0.0364 0.0272 C35 0.0831 0.0442 0.0207 C3 0.0792 0.0484 0.0290 C31 0.0482 0.0348 0.0251 C28 0.0764 0.0640 0.0307 C12 0.0680 0.0357 0.0210 C24 0.0727 0.0508 0.0230 C32 0.0745 0.0654 0.0286 C11 0.0791 0.0352 0.0311 C4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.004 0.007 0.010 0.014 0.018 0.023 0.030 0.041 0.061 1.000 Number in group 692. 542. 514. 612. 487. 553. 569. 592. 548. 555. GooF 1.014 0.834 1.006 0.977 1.086 1.150 1.151 1.019 1.024 0.973 K 18.779 2.747 2.195 1.464 1.296 1.359 1.090 1.082 1.288 0.984 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.42 1.76 inf Number in group 570. 564. 580. 552. 579. 557. 561. 565. 569. 567. GooF 0.807 0.807 0.902 0.997 1.035 1.048 1.088 1.055 1.257 1.176 K 1.187 1.269 1.131 1.129 1.072 1.067 1.054 1.020 1.132 1.034 R1 0.581 0.528 0.466 0.356 0.305 0.209 0.188 0.182 0.154 0.114 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.1909 0.0773 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)/su Fc/Fc(max) Resolution(A) -6 1 4 227.38 26.89 6.33 0.014 1.52 3 -5 4 249.90 0.39 6.13 0.002 1.44 -2 2 4 4151.03 1324.93 5.96 0.101 2.63 -5 3 4 218.11 31.92 5.89 0.016 1.69 11 0 3 304.17 43.91 5.87 0.018 1.01 3 6 7 328.90 98.24 5.83 0.027 1.57 -6 -7 1 263.99 59.70 5.79 0.021 1.18 0 3 0 466.46 121.16 5.76 0.030 3.78 -9 7 4 847.19 55.26 5.69 0.021 0.98 -6 0 4 455.02 83.25 5.66 0.025 1.49 0 6 7 234.20 47.38 5.56 0.019 1.63 -3 5 0 751.55 252.73 5.53 0.044 1.93 9 -1 7 369.61 12.48 5.48 0.010 1.03 -2 -7 4 833.96 1.26 5.48 0.003 1.19 -1 5 7 1800.74 378.92 5.40 0.054 1.68 6 4 7 105.50 0.01 5.39 0.000 1.40 2 -3 4 1227.28 401.25 5.35 0.055 1.91 -2 0 4 2835.26 1083.60 5.30 0.091 2.49 -2 -2 4 151.92 14.69 5.29 0.011 2.04 5 -1 11 430.48 16.97 5.20 0.011 0.98 -4 -5 8 537.44 43.39 5.20 0.018 0.96 -9 1 4 483.61 43.06 5.18 0.018 1.11 -2 -4 8 373.85 32.58 5.16 0.016 1.09 -2 1 0 6842.21 2407.30 5.13 0.136 4.99 -6 3 4 150.61 7.18 5.10 0.007 1.49 -4 -2 4 733.51 7.42 5.02 0.008 1.69 -5 4 4 314.50 72.86 5.01 0.024 1.62 0 -2 4 1782.11 659.66 4.93 0.071 2.27 -10 6 4 468.21 103.77 4.91 0.028 0.94 -10 -4 1 184.58 7.21 4.77 0.007 1.02 -6 -9 1 464.08 173.12 4.66 0.036 1.01 5 -6 4 638.01 77.16 4.62 0.024 1.19 -7 2 4 163.30 18.30 4.59 0.012 1.36 8 5 3 385.42 148.31 4.58 0.034 1.26 2 7 3 122.20 8.78 4.56 0.008 1.72 4 -3 4 1062.23 120.69 4.51 0.030 1.67 2 6 11 166.88 19.27 4.46 0.012 1.16 8 0 7 137.81 2.06 4.34 0.004 1.15 -6 4 8 343.97 11.90 4.31 0.010 1.14 -5 6 0 866.17 382.27 4.29 0.054 1.44 -6 -8 1 338.70 139.14 4.17 0.033 1.09 1 9 7 410.10 183.79 4.14 0.038 1.30 5 5 11 562.16 11.91 4.07 0.010 1.10 5 3 7 2389.61 1133.75 4.05 0.093 1.53 10 4 3 147.69 33.71 4.04 0.016 1.08 -3 2 0 182.45 40.65 3.99 0.018 3.10 5 2 3 1658.37 210.68 3.98 0.040 2.08 0 0 4 7227.79 3529.28 3.96 0.165 2.95 -5 2 0 1260.71 587.19 3.96 0.067 2.07 -5 2 4 921.02 445.03 3.95 0.058 1.72 Bond lengths and angles O1 - Distance Angles C9 1.3571 (0.0098) C2 1.4730 (0.0096) 117.59 (0.63) O1 - C9 N2 - Distance Angles C14 1.3765 (0.0098) N1 1.3784 (0.0085) 120.93 (0.62) H2 0.8800 119.54 119.54 N2 - C14 N1 O21 - Distance Angles C29 1.3569 (0.0093) C22 1.4777 (0.0092) 117.27 (0.60) O21 - C29 O22 - Distance Angles C24 1.2189 (0.0096) O22 - O23 - Distance Angles N23 1.2462 (0.0092) O23 - N22 - Distance Angles C34 1.3469 (0.0093) N21 1.3688 (0.0085) 120.85 (0.59) N22 - C34 O3 - Distance Angles N3 1.2289 (0.0095) O3 - N1 - Distance Angles C13 1.2764 (0.0096) N2 1.3784 (0.0085) 115.34 (0.64) N1 - C13 N21 - Distance Angles C33 1.2866 (0.0100) N22 1.3688 (0.0085) 118.73 (0.65) H21 0.8800 120.64 120.64 N21 - C33 N22 O2 - Distance Angles C4 1.2380 (0.0108) O2 - O24 - Distance Angles N23 1.2324 (0.0094) O24 - O4 - Distance Angles N3 1.2417 (0.0096) O4 - N3 - Distance Angles O3 1.2289 (0.0095) O4 1.2417 (0.0096) 123.27 (0.72) C17 1.4562 (0.0107) 118.74 (0.82) 117.99 (0.79) N3 - O3 O4 C39 - Distance Angles C38 1.3462 (0.0114) C34 1.4138 (0.0107) 120.95 (0.70) H39 0.9500 119.52 119.52 C39 - C38 C34 N23 - Distance Angles O24 1.2324 (0.0094) O23 1.2462 (0.0092) 122.04 (0.71) C37 1.4437 (0.0104) 118.22 (0.75) 119.74 (0.75) N23 - O24 O23 C19 - Distance Angles C18 1.3618 (0.0113) C14 1.4076 (0.0110) 120.12 (0.79) H19 0.9500 119.94 119.94 C19 - C18 C14 C10 - Distance Angles C5 1.3757 (0.0128) C9 1.4145 (0.0119) 118.39 (0.79) C4 1.4694 (0.0129) 123.42 (0.80) 118.11 (0.84) C10 - C5 C9 C14 - Distance Angles N2 1.3765 (0.0098) C15 1.3777 (0.0111) 122.31 (0.70) C19 1.4076 (0.0110) 116.93 (0.71) 120.60 (0.73) C14 - N2 C15 C34 - Distance Angles N22 1.3469 (0.0093) C35 1.3969 (0.0108) 122.97 (0.67) C39 1.4138 (0.0107) 118.90 (0.65) 118.12 (0.68) C34 - N22 C35 C16 - Distance Angles C15 1.3717 (0.0107) C17 1.4150 (0.0120) 119.54 (0.79) H16 0.9500 120.23 120.23 C16 - C15 C17 C38 - Distance Angles C39 1.3462 (0.0114) C37 1.4062 (0.0109) 119.45 (0.75) H38 0.9500 120.27 120.27 C38 - C39 C37 C13 - Distance Angles N1 1.2764 (0.0096) C8 1.4542 (0.0108) 120.01 (0.71) H13 0.9500 120.00 120.00 C13 - N1 C8 C36 - Distance Angles C37 1.3618 (0.0112) C35 1.3812 (0.0114) 119.24 (0.73) H36 0.9500 120.38 120.38 C36 - C37 C35 C29 - Distance Angles O21 1.3569 (0.0093) C28 1.3914 (0.0111) 117.68 (0.69) C30 1.4174 (0.0111) 122.33 (0.69) 119.99 (0.74) C29 - O21 C28 C18 - Distance Angles C19 1.3618 (0.0113) C17 1.3839 (0.0120) 119.52 (0.78) H18 0.9500 120.24 120.24 C18 - C19 C17 C25 - Distance Angles C26 1.3765 (0.0124) C30 1.3893 (0.0119) 119.97 (0.79) H25 0.9500 120.01 120.01 C25 - C26 C30 C26 - Distance Angles C25 1.3765 (0.0124) C27 1.3893 (0.0120) 120.18 (0.81) H26 0.9500 119.91 119.91 C26 - C25 C27 C37 - Distance Angles C36 1.3618 (0.0112) C38 1.4062 (0.0109) 121.24 (0.69) N23 1.4437 (0.0104) 119.13 (0.71) 119.52 (0.73) C37 - C36 C38 C2 - Distance Angles O1 1.4730 (0.0097) C3 1.5001 (0.0125) 108.60 (0.71) C12 1.5148 (0.0130) 104.38 (0.68) 113.45 (0.78) C11 1.5282 (0.0137) 107.67 (0.68) 112.16 (0.80) 110.11 (0.81) C2 - O1 C3 C12 C15 - Distance Angles C16 1.3717 (0.0107) C14 1.3777 (0.0111) 119.64 (0.75) H15 0.9500 120.18 120.18 C15 - C16 C14 C5 - Distance Angles C6 1.3608 (0.0129) C10 1.3757 (0.0128) 122.08 (0.81) H5 0.9500 118.96 118.96 C5 - C6 C10 C23 - Distance Angles C22 1.5020 (0.0117) C24 1.5169 (0.0128) 109.62 (0.71) H23A 0.9900 109.75 109.75 H23B 0.9900 109.75 109.75 108.22 C23 - C22 C24 H23A C6 - Distance Angles C5 1.3608 (0.0129) C7 1.3710 (0.0116) 119.35 (0.87) H6 0.9500 120.33 120.33 C6 - C5 C7 C7 - Distance Angles C6 1.3710 (0.0116) C8 1.3761 (0.0113) 122.47 (0.81) H7 0.9500 118.77 118.77 C7 - C6 C8 C8 - Distance Angles C7 1.3761 (0.0113) C9 1.4183 (0.0109) 117.65 (0.73) C13 1.4542 (0.0108) 122.82 (0.72) 119.47 (0.74) C8 - C7 C9 C30 - Distance Angles C25 1.3893 (0.0119) C29 1.4174 (0.0111) 119.85 (0.75) C24 1.4809 (0.0121) 121.53 (0.75) 118.60 (0.76) C30 - C25 C29 C22 - Distance Angles O21 1.4777 (0.0092) C23 1.5020 (0.0117) 109.02 (0.66) C32 1.5199 (0.0126) 104.85 (0.65) 111.97 (0.76) C31 1.5396 (0.0134) 108.86 (0.68) 111.69 (0.73) 110.18 (0.76) C22 - O21 C23 C32 C9 - Distance Angles O1 1.3571 (0.0098) C10 1.4145 (0.0119) 122.30 (0.73) C8 1.4183 (0.0110) 117.77 (0.70) 119.90 (0.79) C9 - O1 C10 C33 - Distance Angles N21 1.2866 (0.0100) C28 1.4447 (0.0115) 120.68 (0.72) H33 0.9500 119.66 119.66 C33 - N21 C28 C27 - Distance Angles C26 1.3893 (0.0121) C28 1.3957 (0.0116) 121.28 (0.78) H27 0.9500 119.36 119.36 C27 - C26 C28 C17 - Distance Angles C18 1.3839 (0.0119) C16 1.4150 (0.0120) 120.49 (0.72) N3 1.4562 (0.0107) 119.61 (0.79) 119.90 (0.82) C17 - C18 C16 C35 - Distance Angles C36 1.3812 (0.0114) C34 1.3969 (0.0108) 120.94 (0.76) H35 0.9500 119.53 119.53 C35 - C36 C34 C3 - Distance Angles C4 1.4855 (0.0139) C2 1.5001 (0.0125) 113.27 (0.77) H3A 0.9900 108.92 108.92 H3B 0.9900 108.92 108.92 107.74 C3 - C4 C2 H3A C31 - Distance Angles C22 1.5396 (0.0134) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - C22 H31A H31B C28 - Distance Angles C29 1.3914 (0.0111) C27 1.3957 (0.0116) 118.56 (0.76) C33 1.4447 (0.0115) 121.31 (0.73) 120.13 (0.72) C28 - C29 C27 C12 - Distance Angles C2 1.5148 (0.0130) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C2 H12A H12B C24 - Distance Angles O22 1.2189 (0.0096) C30 1.4809 (0.0121) 121.07 (0.85) C23 1.5169 (0.0128) 123.15 (0.79) 115.57 (0.72) C24 - O22 C30 C32 - Distance Angles C22 1.5199 (0.0126) H32A 0.9800 109.47 H32B 0.9800 109.47 109.47 H32C 0.9800 109.47 109.47 109.47 C32 - C22 H32A H32B C11 - Distance Angles C2 1.5282 (0.0137) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C2 H11A H11B C4 - Distance Angles O2 1.2380 (0.0108) C10 1.4694 (0.0129) 120.75 (0.94) C3 1.4855 (0.0139) 122.00 (0.87) 117.06 (0.78) C4 - O2 C10 FMAP and GRID set by program FMAP 2 3 33 GRID -1.667 -2 -2 1.667 2 2 R1 = 0.2613 for 5664 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.46 at 0.2048 0.0221 0.0671 [ 1.78 A from C6 ] Deepest hole -0.62 at 0.1207 0.3665 0.3660 [ 0.17 A from H21 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 4435 / 29337 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.2048 0.0221 0.0671 1.00000 0.05 0.46 1.78 C6 1.90 H6 1.92 O3 2.06 C5 Q2 1 1.0203 0.5222 0.1602 1.00000 0.05 0.46 0.84 N2 1.00 C14 1.30 H2 1.82 C19 Q3 1 1.0310 0.5533 0.3981 1.00000 0.05 0.44 0.86 N22 1.78 N21 1.91 C34 2.30 H33 Q4 1 1.0268 0.3024 0.4796 1.00000 0.05 0.43 1.12 H35 1.58 C35 1.61 H21 2.14 C34 Q5 1 1.4122 0.6175 -0.0521 1.00000 0.05 0.43 1.63 H16 2.00 H31A 2.25 H31C 2.36 C16 Q6 1 0.8146 0.0147 0.1999 1.00000 0.05 0.42 1.50 H3B 1.70 N3 1.90 O3 1.90 O1 Q7 1 1.0100 0.5996 0.3350 1.00000 0.05 0.40 1.03 N22 1.85 O2 2.05 N21 2.08 C34 Q8 1 1.4817 0.6940 -0.0038 1.00000 0.05 0.40 0.85 H31A 0.89 H31C 0.91 C31 1.67 H31B Q9 1 0.5619 0.3826 0.4996 1.00000 0.05 0.40 1.09 O23 1.29 N23 1.54 H38 1.57 C37 Q10 1 0.8767 0.0668 0.5575 1.00000 0.05 0.39 1.17 H11C 1.75 H36 2.08 C11 2.21 H11A Shortest distances between peaks (including symmetry equivalents) 3 7 0.84 5 8 1.62 3 3 2.45 2 7 2.80 3 4 2.84 3 4 2.86 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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 0.00: Analyse other restraints etc. 0.98: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.67: Structure factors and derivatives 13.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 1.31: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:17:23 Total CPU time: 18.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++